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Bioleaching of enargite Steer, Cheryl Ann 2002

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B I O L E A C H I N G OF E N A R G I T E by C H E R Y L A N N STEER B . S c , University of Alberta, 2000  A THESIS SUBMITTED IN P A R T I A L F U L F I L M E N T OF THE REQUIREMENTS FOR THE D E G R E E OF M A S T E R OF APPLIED SCIENCE in THE F A C U L T Y OF G R A D U A T E STUDIES (Department of Metals and Materials Engineering) We accept this thesis as conforming to the required standard  THE UNIVERSITY OF BRITISH C O L U M B I A December 2002 © Cheryl Ann Steer, 2002  In presenting this thesis in partial fulfilment of the requirements for an advanced degree at the University of British Columbia, I agree that the Library shall make it freely available for reference and study. I further agree that permission for extensive copying of this thesis for scholarly purposes may be granted by the head of my department or by his or her representatives. It is understood that copying or publication of this thesis for financial gain shall not be allowed without my written permission.  Department of Metals and Materials Engineering The University of British Columbia Vancouver, Canada  Date  Qece.^ht-.'r- '-Zo, xOC ^, j  Abstract Enargite (C113ASS4) is a refractory mineral that has not been investigated extensively with respect to copper leaching. The two main challenges to its leaching is its very refractory nature, which some sources consider to be more refractory than chalcopyrite; and the mineral contains arsenic, and possibly small amounts of antimony, which will pose a challenge for the processing and the ultimate disposal of these elements.  Initially, the leaching of enargite as discussed in the literature has been reviewed. It was found that the information on the leaching of enargite is sparse, and the research that has been conducted indicates that enargite is not viable to leaching. The purpose of the current work is to determine the leachability of enargite, concentrating on the bioleaching aspects. In this respect, mesophiles, moderate thermophiles, and extreme thermophiles were used at their respective temperatures using various pulp densities (19, 33, 48 and 95 g/L) and particle sizes (nominal Pgo sizes of 10, 15, and 37 microns).  Under these experimental conditions, it was determined that almost complete extraction of copper could be achieved using extreme thermophiles, with low pulp densities and smaller particle sizes. For the mesophiles, the decrease in particle size caused a small increase in copper extraction than that reported in the literature. Other important observations have been noted: in the mesophile and moderate thermophile leach solutions, it is very clear that pyrite is being leached preferentially to the enargite and the iron is reporting to solution. In the extreme thermophiles, however, the iron is reporting to the solid residue, possibly as a precipitate.  ii  More work will be needed to determine the viability of bioleaching enargite in a commercial process.  Furthermore, many other methods by which enargite may potentially be leached  have yet to be explored. For instance, chloride leaching or sulphate leaching using finer grinds and a variety of conditions may need to be considered in the future.  iii  Table of Contents Abstract  ii  Table of Contents  iv  List of Tables  vii  List of Figures  viii  Acknowledgements  x  1. Introduction  1  2. Literature Review  6  2.1 Mineralogy  6  2.2 Impurity Elements: Arsenic and Antimony  7  2.2.1 Arsenic  8  2.2.2 Antimony  13  2.2.3 Analysis  15  2.3 Sulphuric Acid Leaching  15  2.3.1 Leaching Reactions  16  2.3.2 Pressure Leaching  20  2.3.3 Leaching of Enargite  22  2.4 Biological Leaching  25  2.4.1 Bacteria Involved in Bioleaching  27  2.4.2 Microbial Growth  32  2.4.3 Bioleaching Reactions  34  2.4.4 Variables and Leaching Conditions  37  2.4.5 Enargite Bioleaching  43  iv  2.5 Chloride Leaching  46  2.5.1 Industrial Processes  49  2.5.2 Advantages  49  2.5.3 Disadvantages  50  2.6 Ammonia Leaching 2.6.1 Leaching of Enargite  52 53  2.7 Sodium Sulphide Leaching  55  2.8 Discussion  57  2.9 Objective  59  3. Experimental Methods  60  3.1 Enargite Sample  60  3.2 Bacteria and Culture Medium  61  3.3 Bacterial Culturing  63  3.4 Bacterial Leaching Experiments  66  3.5 Analysis of Samples  68  4. Results and Discussion  69  4.1 Head Analysis  69  4.2 Mesophiles  70  4.3 Moderate Thermophiles  81  4.4 Extreme Thermophiles  90  4.5 Discussion and Summary 5. Conclusions and Recommendations for Future Work 5.1 Conclusions  101 103 103  v  5.1.1 Mesophilic Bacteria  103  5.1.2 Moderate Thermophiles  104  5.1.3 Extreme Thermophiles  104  5.1.4 Overall Conclusions  105  5.2 Future Work  106  5.2.1 Bioleaching  106  5.2.2 Atmospheric Leaching  107  5.2.3 Pressure Leaching  107  5.2.4 Arsenic Removal  108  6. References  •  110  Appendix A : Enargite Leaching Reactions  120  Appendix B: Trace Nutrient Solution Analysis  124  Appendix C: Mass Balance Calculations  125  Appendix D : Extraction Data Summary  127  Appendix E: Raw Data from Bioleaching Experiments  136  vi  List of Tables Table 1.1: Some Common Copper Minerals [19, 20, 38]  2  Table 2.1: Hydrolysis constants at 298.15 K (25°C) [25].  10  Table 2.2: Typical nutrients and concentrations for bacterial leaching [23]  39  Table 3.1: Nutrient medium composition  62  Table 3.2: Thermophile Trace Nutrient Solution Composition  62  Table 3.3: Light's Solution Composition  64  Table 3.4: Pulp Densities used in Bacterial Leaching Experiments  66  Table 4.1: Head analysis of the enargite samples used for testing  69  Table 4.2: Estimate of the enargite and pyrite content in the head samples  70  Table 4.3: Final extraction values for mesophilic bacteria  78  Table 4.4: Solid residue analysis for mesophilic bacteria  79  Table 4.5: Sulphur analysis for the 10 g experiments, mesophilic bacteria  80  Table 4.6: Final extraction values for moderate thermophilic bacteria  88  Table 4.7: Solid residue mass analysis for moderate thermophilic bacteria  89  Table 4.8: Final extraction values for extreme thermophilic bacteria  98  Table 4.9: Solid residue mass analysis for extreme thermophilic bacteria  99  Table 4.10: Sulphur analysis for 95 g/L experiments, extreme thermophilic bacteria  100  vii  List of Figures Figure 2.1: Structure of Enargite [ 1 ]  7  Figure 2.2: Eh-pF£ diagram of the arsenic-water system [6]  9  Figure 2.3: Typical growth curve of a bacterial population in a culture [56]  34  Figure 2.4: Eh-pH diagram for the enargite-ammonia-water system at 75°C [1]  54  Figure 4.1: pH versus time for mesophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  71  Figure 4.2: Potential versus time of mesophiles, for particle size of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  73  Figure 4.3: Copper extraction versus time of mesophiles, for particle size of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  74  Figure 4.4: Iron extraction versus time of mesophiles, for particle size of Pso equals (a) 10 microns, (b) 15 microns and (c) 37 microns  76  Figure 4.5: Arsenic extraction versus time of mesophiles, for particle size of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  77  Figure 4.6: pH versus time for moderate thermophiles, with particle sizes of Pso equals (a) 10 microns, (b) 15 microns and (c) 37 microns  82  Figure 4.7: Potential versus time for moderate thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  83  Figure 4.8: Copper extraction versus time for moderate thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  84  Figure 4.9: Iron extraction versus time for moderate thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  86  viii  Figure 4.10: Arsenic extraction versus time for moderate thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  87  Figure 4.11: pH versus time for extreme thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  91  Figure 4.12: Potential versus time for extreme thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  92  Figure 4.13: Copper extraction versus time for extreme thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  94  Figure 4.14: Iron extraction versus time for extreme thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  95  Figure 4.15: Arsenic extraction versus time for extreme thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns  97  ix  Acknowledgements I would like to acknowledge the National Science and Research Council and Noranda for financial support for this program.  I would like to thank Dr. David Dreisinger, my supervisor, for his support and advice during this progect.  I would also like to acknowledge the numerous other people in the  hydrometallurgy and biohydrometallurgy groups for their assistance and enlightening conversations.  I would like to thank my family for their support in this endeavour. I would like to especially thank my dad, Greg Steer, and my husband, Mark Smith, for their care and support as I worked through the experimentation and the writing of this thesis. I would also like to thank my two cats, Yoshi and Marbles, for being there when needed.  1. Introduction There is a growing interest in the processing of more complex ores and minerals in order to extract metals economically. Hydrometallurgical techniques have offered an advantage over pyrometallurgical ones in these areas, especially in the handling of sulphide ores and the avoidance of SO2 emissions [9]. Furthermore, there are often unwanted components in ores and concentrates such as arsenic, antimony, and selenium. These need to be treated in an environmentally acceptable manner [24], and hydrometallurgy can offer alternatives for handling such elements.  The challenge in hydrometallurgy is to leach the valuable metals from the minerals present so that a pure product can result from the process in an economical fashion. Table 1.1 lists some of the common copper minerals that are often found in ores and concentrates from which copper is extracted. A number of different strategies have been developed to leach copper from such minerals.  The most common reagent for leaching copper ores is an aqueous solution of sulphuric acid (H2SO4). It is an effective solvent that is readily available at a relatively low cost. Sulphuric acid rapidly attacks oxidized copper ores and may be regenerated when sulphate or sulphide minerals are leached. Furthermore, it is easy to handle and process losses are low [19, 20]. Sulphide ores tend to leach slowly in sulphuric acid, and usually require ferric sulphate or other oxidants to aid in the leaching process. These ores may also require harsher conditions for leaching, such as higher temperatures and pressures in an autoclave. Bioleaching, which  1  is done in an acidified ferric sulphate-based system, utilizes bacteria that can break down the minerals and regenerate the ferric ion during leaching.  Table 1.1: Some Common Copper Minerals [19, 20, 38]. Mineral Name azurite bornite brochantite chalcocite chalcopyrite chrysocolla covellite cuprite dioptase enargite malachite tennantite tenorite tetrahedrite  Chemical Formula 2CuC0 Cu(OH) Cu FeS CuS0 -3Cu(OH) Cu S CuFeS CuSi0 -2H 0 CuS Cu 0 CuSi0 H 0 3  2  5  4  4  2  2  2  3  2  2  3  2  CU3ASS4  CuC0 Cu(OH) Cu As4Si CuO Cui Sb4Si 3  ]2  2  2  3  3  Ammonia (NH ) and hydrochloric acid (HC1) are other proposed reagents for the leaching of 3  copper ores. Hydrochloric acid is harder to handle than sulphuric acid and higher losses are more likely. Ammonia is hard to handle because it is very volatile [19, 20] and tends to contaminate process effluents. Other reagents have also been considered for use in leaching systems.  There is an increasing interest in the leaching of more complex ores with the aim of economically extracting their valuable metals. Enargite, the focus of the current study, is one such mineral. One source ranked the extractability of copper minerals as follows [17]:  2  chalcocite  (C112S) >  covellite (CuS) > bornite (CusFeS^  > chalcopyrite  Chalcopyrite  (CuFeS2)  (CuFeS2)  > enargite  (CU3ASS4)  is often considered a refractory mineral for copper extraction;  enargite is considered even more refractory than chalcopyrite. This poses a challenge for the extraction of copper from enargite. Another challenge will be the presence of arsenic in enargite, as well as other impurity elements such as antimony that can substitute for arsenic. After the extraction of copper, arsenic and other impurity elements need to be converted to a form for safe disposal.  Enargite is only recently gaining interest in regards to copper extraction, and therefore there is not a great deal of information available in the literature. Bioleaching has been researched more than other areas because enargite is also associated with gold ores. However, for a gold ore bioleaching is used to leach enough of the minerals present to expose the gold for a subsequent cyanide leach. Copper extraction from enargite, whether from bioleaching or some other leaching method, has been poorly researched.  Future work will be needed in other areas for enargite leaching. Ideally, the process to leach enargite will be compatible with current copper hydrometallurgy. A sulphate based process would allow the copper to be extracted directly and would be compatible with current solvent extraction/electrowinning (SX/EW) copper processing. Because of the serious disadvantages of chloride processing and its problems with compatibility with copper processes, it may not  3  be the route used to process enargite. However, it will eventually warrant future study as enargite behaviour in this system has been hardly researched.  An overview of the literature relevant to enargite leaching is first presented. First, a brief overview of the mineralogy of enargite and the chemistry of arsenic and antimony is provided. Following this is a discussion of the systems that either have been used to leach enargite or may potentially leach enargite.  These systems involve sulphate, chloride,  ammonia, and sodium sulphide; a special discussion on bioleaching is also included. Chloride has been included even though it has not been used to leach enargite as it has the potential for leaching more refractory minerals; sodium sulphide has been included as it has been tested for extracting arsenic from enargite, though it does not appear to be a widely used process.  The experimental work focuses on the bioleaching of enargite. Using shake flask tests, the leachability of enargite under bioleaching conditions present was determined.  Three  different groups of bacteria (mesophiles, moderate thermophiles, and extreme thermophiles) at their respective growth temperatures were used; other conditions varied include the particle size and the pulp density. It was found in this work that, under certain conditions, enargite can be leached; these results are more promising than those found in the literature, which indicate that copper extraction via enargite bioleaching might not be viable.  As illustrated by the literature review, enargite leaching has not been extensively researched, and the little research that has been done suggests that enargite is not viable to leaching  4  processes. Thus, there are many areas open for further investigation into the leaching of enargite.  Some potential areas for future work have been included. It is hoped that work  such as this would provide a foundation into future studies into the leaching behaviour of enargite, and potentially lead to an economical means of extracting copper from this mineral.  5  2 . Literature Review 2.1  Mineralogy  Enargite belongs to the enargite-luzonite-famatinite Cti3(As, Sb)S4.  series of minerals of composition  These minerals can co-exist in nature and can often be intergrown with each  other. Of these three minerals, enargite is the most common.  Enargite is a dark brown or black mineral that forms elongated, prismic crystals. orthorhombic  CU3ASS4  It is  with a hexagonal close-packed (hep) structure. It is of the wurtzite-  type structure (wurtzite = a-ZnS) that is derived by ordered substitution, or alternate replacement of metals. Figure 2.1 shows the structure of enargite. Antimony can substitute for arsenic up to 6 weight percent antimony or about 20 mol percent  Cu3SbS4.  The existence  of an orthorhombic form of Cu3SbS4, however, is uncertain. Bismuth has also been cited as a potential impurity element [11, 21, 22, 26, 27].  6  Figure 2.1: Structure of Enargite [ 1 ].  Luzonite and famatinite (also called stibio-luzonite) are the tetragonal forms of CU3ASS4 and CU3SI5S4  respectively. They have a cubic close-packed structure and are of the sphalerite-  type structure. There is a continuous solid-solution series between luzonite and famatinite. Visually, luzonite looks like pinkish grey masses in polished mineral sections [21, 22, 26].  It is worth noting that enargite and luzonite are polytypes of  CU3ASS4  and are intergrown in  many ore deposits, in many cases very intimately on a microscopic scale. Note that stacking faults in the hexagonal close-packed matrix (enargite) result in cubic close-packed lamella (luzonite) and vice versa.  Thus, a heavily disordered luzonite or enargite structure is  considered a structure intermediate between enargite and luzonite, especially since enargite and luzonite differ only in the stacking sequence of identical layers. When enargite and luzonite coexist, luzonite will generally be richer in antimony, although the compositional range can overlap [21, 22, 26]. Geologically, enargite is the high temperature modification of  CU3ASS4  with the inversion temperature lying between 280-300°C.  The formation of  enargite or luzonite-famatinite is determined geologically by the Sb/As ratio of the fluid [21, 22, 26].  2.2  Impurity Elements: Arsenic and Antimony  Note that enargite  (CU3ASS4)  contains a significant amount of arsenic.  previously, antimony can also be present as an impurity in enargite.  As discussed  These elements are  7  "nuisance" elements during processing and it is desirable to remove these elements when possible. What follows is a brief discussion on the chemistry of these elements."  2.2.1 Arsenic Arsenic is usually an unwanted component in most metallurgical processes. Although is a fairly scarce element in the earth's crust, it is found in complex sulphide minerals from ores and concentrates of metals such as copper, lead, zinc, and gold [6]. Metallurgically, arsenic is a contaminant and a high purity final product can be difficult to obtain when it is present. Environmentally, arsenic is highly toxic, and there is a risk of atmospheric release and water contamination. During roasting and smelting, arsenic can be released into the atmosphere as arsenic trioxide. After a hydrometallurgical process, arsenic can appear as ions in aqueous solutions [6, 11].  In nature, arsenic occurs rarely in the free state and is usually associated in compounds containing sulphur, oxygen, and or iron [55]. It has been estimated that less than 2% of arsenic emissions are from natural sources, and the majority of emissions have been linked to coal combustion and ore smelting [67]. Many toxic effects have been found to be caused by arsenic exposure [55, 67]; it is for this reason that the ability to deal with and dispose of arsenic is an important area when processing minerals such as enargite.  Arsenic is an element with atomic number 33. It is in the group V B elements with nitrogen, phosphorous, antimony, and bismuth. There are three main valence states: -3 as arsenide, +3 as arsenite, and +5 as arsenate [6, 24]. Arsenite is approximately 60 times more toxic than  8  arsenate, although only limited toxicity data is available [55]. There are two oxides of arsenic that can form in an aqueous solution:  AS2O3  and two hydroxides of  AS2O5,  A s 0 - 4 H 0 < 25.9°C and 3 A s 0 - 5 H 0 > 25.9°C [6]. A n E -pH diagram of the arsenic2  5  2  2  5  2  h  water system is found in Figure 2.2.  Despite the fact that arsenic is an important impurity element in hydrometallurgical processing, there are serious gaps in arsenic thermodynamic data.  One source [25],  investigating thermodynamic data for arsenic, actually concluded that there was a need for a complete re-analysis of thermodynamic data for arsenic species. The thermodynamic data for many solid arsenic compounds is poorly known and in need of a thorough investigation; the same was true for many of the ions. Thus, it can be difficult to obtain an accurate picture of the speciation of arsenic-containing ions and compounds in a system.  9  There are a large number of metal-arsenic compounds. Ferric arsenate (FeAsO^Ff^O), for instance, is used extensively for removing arsenate because it is a low solubility compound. Not all compounds are stable: for instance, calcium arsenates (formed by removing arsenate with lime) can decompose to calcium carbonate in alkaline solutions with atmospheric carbon dioxide [6].  2.2.1.1 Arsenic (V) The predominant As(V) species in water are H3ASO4, H2ASO4", HASO4 ", and ASO4 ", 2  3  depending on the Eh and pH of the solution [24]. Thermodynamic data for the hydrolysis of arsenic acid (H3ASO4) is known to a high degree of certainty in the literature. Table 2.1 shows solubility data for arsenic acid and compares it to phosphoric acid. Phosphorous, like arsenic, is a group VB element; note the similarities between the data [25].  Table 2.1: Hydrolysis constants at 298.15 K (25°C) [25]. log Id logK logK 2  3  Arsenic Acid 2.24 ± 0.06 6.96 ± 0.02 11.50  Phosphoric Acid 2.148 ±0.001 7.199 + 0.002 12.35 ± 0.02  The largest gap in the thermodynamic data is for arsenic species complexation; in many cases, there is no thermodynamic data, nor information to tell if these aqueous metal complexes are significant in the speciation of arsenic in solution. As discussed above, arsenic (V) has a similar chemistry to phosphorous (V); it is also believed to have a similar  10  aqueous chemistry to antimony and bismuth [6, 25].  One source estimated the  thermodynamic data using analogous phosphorous compounds, and used these values in speciation calculations. It was found that free arsenic concentrations (HAsO/" or H2ASO4") decreased by about 50% [25]. Therefore, arsenic complexes are likely important in a given system, although the data to calculate them are not available. This also influences the reactions that can be considered in a given system.  Arsenate can be removed from solution and stabilized with iron. Studies on the Fe203AS2O5-H2O system have revealed three crystalline ferric arsenates [24]:  FeAs0 -2H 0  As(V) < 0.22 M  FeH (As0 )2 - IOH2O  As(V) = 0.22 - 1 . 4 M  Fe(H As0 )3-5.5H 0  As(V)>l'.4M.  4  2  4  3  2  4  2  Ferric arsenate, or scorodite (FeAs04-2H.20), exists as a stable solid phase at a pH above 1.5 and has a very low solubility at higher pH values [6, 24].  A common method for removing arsenic from solution is by the formation of scorodite. A solution of dissolved iron is added to the solution to be treated. The arsenate will not only form scorodite but will also adsorb to ferric hydroxide surfaces, which will also form during the process [24]. The solid can then be separated by a thickener. This process has been used commercially to reliably produce solutions with arsenic concentrations below 50 ppb (part per billion) [29]. Operational factors that can compromise arsenic removal are the poor oxidation of Fe(II), poor arsenic-ferric hydroxide particle settling charactaristics, and arsenic in solution in forms other than arsenate [29].  11  Scorodite can form under lower temperature conditions and at higher temperatures found in autoclaves.  At lower temperatures, it is generally amorphous.  At higher temperatures,  crystalline scorodite can be formed. Although crystalline scorodite has the lowest solubility of arsenic minerals, this and high iron ferric arsenates have comparable order-of-magnitude solubility [43].  One important parameter in the removal of arsenic from solution is the ratio of Fe(III) to As(V).  As this ratio increases, arsenic precipitation increases and the residual As(V)  decreases [24, 29]. The pH is also important in the process. One study noted that at too high of a pH, although ferric hydroxide/scorodite particles are formed, the particles are too fine. This can cause problems in operation: an initial pH of less than 10.7 produced coarser particles more easily removed in a thickener [29].  It is believed that other components in the system may affect the removal of arsenate from solution; there may be the formation of arsenic complexes that do not adsorb onto ferric hydroxide. For instance, dissolved sulphate can interfere with arsenic co-precipitation [29]. However, it is often hard to predict because the thermodynamic data may not be reliably known. For instance, NBS fluoroarsenate data suggests that co-precipitation can be affected at 1 ppm fluoride; however, experimentally no effect was found. This was attributed to either faulty thermodynamic data or fluoroarsenates that also co-precipitate onto ferric hydroxide [29].  12  Other elements can also form arsenates, such as cadmium, copper, zinc, and especially calcium.  However, most elements are not suitable for long-term stability of disposal,  especially non-iron containing arsenates and the whole family of arsenites [43].  In many  cases, atmospheric carbon dioxide can destabilize these metal arsenates; this is not the case with ferric arsenates [43].  2.2.1.2 Arsenic (III) The predominant arsenite (As(III)) species in water are A s O , H A s 0 2 , and ASO2", depending +  on the E h and p H of the solution [24]. log K i = 9.29 at 298.15 K [25].  There is one hydrolysis constant for arsenious acid:  Arsenite is generally believed to form weaker complexes  than arsenate; however, no measurements of arsenite complexes have been reported [25].  Arsenite can co-precipitate with ferric hydroxide, but removal is less complete than arsenate [29].  One should note that there is no ferric arsenite mineral found in nature, and there is  little reliable information on the formation for ferric arsenites from aqueous solution, although this appears to only occur at higher p H values (ideally about p H 8) [24].  2.2.2 Antimony Antimony, like arsenic, is a nuisance element and is also a problem when disposed of in the environment.  13  Antimony has atomic number 51 and is in Group V B (as does arsenic).  The common  valance forms is the +3 and the +5 states [24]. Like arsenic, antimonite (+3 valence state) is more toxic than antimonate (+5 valence state) [55].  2.2.2.1 Antimony (III) Antimony trioxide has an amphoteric nature. Antimony (III) dissolves as SbO in a very +  acidic solution of pH below 1. At a pH from 1 to 10 and Sb(III) = 10" M , Sb2C>3 (cubic 4  form) is a stable antimony (III) species. In a more alkaline solution, it exists as SbCV [24].  Ferric ion can also be used to eliminate antimony from solution. Ferric antimonite has neither been identified in nature nor synthesized; the elimination of antimony (III) is by adsorption to ferric hydroxide.  Again, the important variables are the pH and the  Fe(III)/Sb(III) concentration [24].  2.2.2.2 Antimony (V) Antimony pentaoxide (Sb205) has a very small stability domain. In very acidic solutions, it exists as SbC>2 ; in neutral and alkaline solutions, it exists as SbCV [24]. +  In the pH range for antimony elimination (optimally pH between 3 and 4), antimony concentration decreases gradually with time, even after 24 hours. In the literature, there are fluctuations of the observed concentrations of antimony (V) reported [24]. Thus, it may be difficult to remove antimony (V) from solutions with ferric. However, it is known that a higher Fe(III)/As(V) concentration promotes the elimination of arsenic.  14  2.2.3 Analysis Arsenic and antimony, despite being significant impurity elements, are not well understood. Arsenic in particular has been identified as a problem in processing.  Despite this,  complexation of metals by arsenic species is largely unexplored and thermodynamic data available is not reliable enough to provide useful information. These complexes may be important in the leaching of enargite. Thus, it may be hard to predict the actual reactions in enargite systems.  Furthermore, note that for effective removal of arsenic, the dissolved arsenic must be in the +5 valence state, and ferric appears to effectively remove the arsenic from solution. The removal of antimony is less understood, and the removal of antimony in the +5 valance state with ferric iron is very slow.  2.3 Sulphuric Acid Leaching The most common reagent for leaching copper ores is an aqueous solution of sulphuric acid (H2SO4). It offers a system with low cost, minimal corrosion problems, and the ability to regenerate sulphuric acid during the electrowinning of copper from solution [23]. Sulphuric acid may also be regenerated during the leaching of sulphate or sulphide minerals. Finally, excess sulphur may be removed as elemental sulphur or as complex basic iron sulphates Fe(S04)OH and Fe3(S04)2(OH)5 [23]. In the electrowinning step, the copper is recovered from a C u S 0 / H S 0 electrolyte [33]: 4  2  4  CuS0 + H 0 ->Cu + H SO + Y 0 4  2  2  A  2  2{)  [2-1 ]  15  2.3.1  Leaching Reactions  Since sulphuric acid is one of the most common leaching reagents for copper, the reactions involving many of the copper minerals are well known.  Solutions of acidified ferric sulphate are very common in leaching. For a general case, in a ferric sulphate solution, the thermodynamically stable chemical reaction is [61]: MS + SFe  3+  + 4H 0 -» M  2+  2  + SOf + SH + SFe +  2+  [2-2]  But, i f elemental sulphur (S°) is produced [61]: MS + 2Fe  -> M  i+  2 +  + 2Fe  2+  + S°  [2-3]  However, elemental sulphur is not thermodynamically stable and is predicted to be oxidized to sulphate [23, 61]: S°+y 0 + 2  2  H 0 -> H S0 2  2  4  [2-4]  This reaction normally does not occur in ferric leaching systems as elemental sulphur is a metastable product and can persist in residues from leaching [61]. The amount of sulphur oxidized to elemental sulphur (S°) and sulphate (SO4") depends on the reaction conditions. A n increase in acid concentration and an increase in sulphate concentration typically results in an increase in the stability of S°.  If elemental sulphur is preferred, a high acid  concentration is therefore desirable to increase the rate of copper dissolution and depress the oxidation of S to SO4 ". Elemental sulphur may be preferred in some instances, such as i f 2  excess acid production is not desired [23].  16  In a sulphate solution, oxygen can also act as the oxidant [23]; however, the reactions are generally slower than when ferric is the oxidant.  Azurite, malachite, tenorite, and chrysocolla are completely soluble at room temperature and at normal acid strength.  The leaching reactions for azurite, malachite, and chrysocolla  respectively in sulphuric acid are as follows [20]: Cw (OH) • ( C 0 ) + 3H S0 3  2  3  2  2  4  Cu (OH) • C0 + 2H S0 2  2  3  2  -> 3CuS0 + 2C0 + 4H 0 4  2  2  -> 2CuS0 + 2C0 + 3H 0  4  4  2  3  2  2  A  4  2  [2-6]  2  CuSiQ • 2H 0 + H SO -» CuS0 + Si0 + 3H 0 2  [2-5]  (slow reaction)  [2-7]  Cuprite can be completely dissolved in acid ferric sulphate. The leaching reactions can be described as follows [20]: Cu 0 + H S0 2  2  -> CuS0 + Cu + H 0  4  4  [2-8]  2  Cu + Fe (S0 ) -> CuS0 + 2FeS0 2  4  Cu 0 + H S0 2  2  4  3  4  [2-9]  4  + Fe (S0 ) -> 2CuS0 + H 0 + 2FeS0 2  4  3  4  2  4  [2-10]  Not that ferric is used as an oxidizing agent in reactions [2-9] and [2-10].  Chalcocite, bornite, and covellite are leached in acid ferric sulphate solutions and elevated temperature (35-50°C) for nearly complete extraction [20].  17  For chalcocite, the leaching reactions are as follows [20, 23, 59, 61]: Cu S + Fe (SO ) -> CuS + CuSO + 2FeS0  [2-11 a]  CuS + Fe (S0 ) -> CuS0 + 2FeS0 + S  [2-11 b]  2  2  A  2  4  3  A  3  4  4  4  Cw 5 + 2Fe(S0 ) -> 2CwS0 + 4FeS0 + S 2  4  3  4  (overall reaction)  4  [2-11 c]  (The first reaction is faster, while the CuS formed is different than covellite.) +Y 0  Cu S + H S0 2  2  2  4  CuS + CuS0 + H 0  2  4  (very slow)  2  [2-12]  The leaching reactions for covellite are as follows [20, 23, 61]: CuS + Fe (S0 ) 2  4  -> CuS0 + 2FeS0 + S  3  4  CuS + H SO +y 0 2  A  2  [2-13]  4  -> CuS0 +S°+ H 0  2  4  (very slow)  2  [2-14]  Finally, the leaching of bornite can proceed as follows [23]: Cu FeS + 6Fe (S0 ) 5  4  2  Cu FeS + 5H S0  4  5  4  2  ->5CuS0 +\3FeS0  3  4  4  + 4S°  [2-15]  + %0 ^> 5CuS0 + Fe{OH\ +4S°+y H 0 x  4  2  4  2  2  [2-16]  In all three cases, the presence of an oxidizing reagent (such as ferric or oxygen) is required for the reactions to proceed.  Chalcopyrite is only partially leached under mild conditions in acid and ferric iron solutions, and often harsher conditions with higher pressures and temperatures in an autoclave are required for practical extraction. The extraction reactions involving chalcopyrite are as follows [20, 23, 33]:  18  2CuFeS + / 0 +5H S0 5  2  2  2  2  4  2  2  2  CaFeS + H S0 2  2  4  -» 2CuS0 + Fe (S0 )  [2-18]  2  4  CuFeS + 2Fe (S0 ) 2  4  2  2  4  3  2  + 5# 0  3  2  CuSO +Fe(OH)  5  4  4  2  + /0 +/H0  4  2  [2-17]  A  2CuFeS + "/ 0 + H S0 2  -> 2CuSO + Fe (S0 ) +4S + 5H 0  2  4  + 2S°  3  [2-19]  -> C « 5 0 + 5Fe,S0 + 2S°  3  4  [2-20]  4  The presence of ferric sulphate (Fe2(S04)3) can lead to other solids forming as it is prone to hydrolysis and precipitation [33]. Also, note in the above reactions how iron can sometimes increase in a system, depending on the minerals being leached.  There can be the  precipitation of ferric hydroxide [33]: Fe (S0 ) + 6H 0 -> 2Fe(OH) + 3H S0 2  4  3  2  i  2  [2-21]  4  with the precipitation of ferric oxy-hydroxide (goethite) [33]: Fe (S0 ) +4H 0^>2FeO(OH) 2  4  3  + 3H S0  2  2  [2-22]  4  and/or the precipitation of ferric oxide (hematite) [23, 33]: Fe (S0 ) 2  4  + 3H 0 -> 2Fe 0 + 3H S0  2  2  2  }  2  [2-23]  4  and/or the precipitation of ferric hydroxy-sulphate (jarosite) [23, 33]: X S0 +3Fe (S0 ) +\2H 0 2  4  2  4  i  -> 2XFe (S0 ) (OH) +6H S0  2  3  4  2  6  2  4  [2-24]  where X = Na+, K NFL; , H 3 0 , etc, depending on acidity. +  +  +  Finally, other precipitation reactions that have been proposed are as follows [23]: F e ( 5 0 ) + 2H 0 -> 2Fe(S0 )OH + H S0 2  4  3  2  4  2  [2-25]  4  (At high T and high acidity) 3Fe (S0 ) +10H O -> 2Fe (S0 ) OH + 5H S0 2  4  3  2  3  4  2  5  2  4  [2-26]  19  Therefore, the compounds formed by the precipitation of iron from the sulphate system can be numerous and complex. High acid concentrations will reverse the iron precipitation reactions; it also dissolves ferro-hydroxides produced, which results in high iron concentration in solution and excessive acid consumption [23].  Finally, sulphur can be oxidized to sulphate, as was shown in Equation 2-4 [23]: S + y O + H 0 -> H S0  [2-4]  0  2  2  2  2  4  The percentage of sulphur oxidized to S° and SO4" depends on the reaction conditions. A n increase in acid concentration and an increase in sulphate concentration results in an increase in area of stability of S°. A high acid concentration will therefore increase the rate of copper dissolution and depress the oxidation of S to SO4 " [23]. 2  Although the reactions involved in sulphate systems have been investigated extensively, there is still ongoing work into the mechanisms involved in the leaching of copper minerals. In general, variables that can influence the reactions include particle size, acidity, concentration of Fe(III), oxygen partial pressure, and temperature [23].  2.3.2  Pressure Leaching  Pressure leaching involves the leaching of ores at high temperatures and elevated oxygen partial pressures.  In most cases during leaching, kinetics is the limiting factor, not  thermodynamics. The increase of temperature and oxygen partial pressure will, in general, increase the kinetics of the reactions involved; thus, this is often used for hard-to-leach minerals. Furthermore, in general an increase in partial pressure predominantly increases the  20  reaction rates and only slightly affects equilibrium; it also results in high slurry oxidation potentials, and high heat generation rates [42, 59].  Temperature is critical for two reasons. temperature.  First, leaching reactions are functions of  At temperatures greater than 175°C, metal sulphides oxidize completely to  sulphate; at temperatures less than about 175°C, elemental sulphur forms [59]. Secondly, sulphur melts at 119°C.  The molten sulphur can coat the sulphide surface with an  impermeable film that must be oxidized before the dissolution of copper can continue [23]. In some cases, a surfactant may be used to disperse the molten sulphur so that it does not coat the sulphide surfaces.  In Total Pressure Oxidation (TPO), high temperatures (200 to 230°C) and high oxygen partial pressures (100-200 psig O2) are used to destroy the refractory sulphide matrix. Sulphur is converted to sulphate (SO4 ") in this process [42]. This is generally the most extreme case used in pressure leaching systems.  Pressure leaching is conducted in an autoclave. It is often the most expensive method of leaching due to higher capital and operating costs involved.  Industrially, autoclaves are  generally run in a continuous process, with 3 to 6 compartments per autoclave and impellers in each compartment for agitation and gas dispersion [58]. Materials for an autoclave are typically carbon steel with a lining such as lead/brick or thermoplastic/brick. Stainless steel or titanium are also often needed to make the internal components (such as propellers) due to the corrosive nature of the leach solutions used [42, 58].  21  Some industrial processes for the leaching of copper sulphide ores utilize pressure oxidation. •  The Dynatec process involves medium temperature autoclaving at 150°C and oxygen over pressure. Coal is used as a surfactant to disperse the molten sulphur [33, 36].  •  The INCO process involves leaching at 115°C and at a total gauge pressure of 1034 kPa, including 966 kPa 0 [32]. 2  •  The Activox Process involves ultrafine grinding plus oxygen pressure oxidation under mild conditions [63].  2.3.3  Leaching of Enargite  2.3.3.1 Leaching Reactions Enargite is very refractory when leached in sulphuric acid in the presence of ferric iron. Upon leaching, arsenic and copper dissolve from the enargite at approximately the same rate. The suggested reaction for the ferric leaching of enargite in sulphuric acid is as follows [2, 8, 11]: Cu AsS +1 \Fe  + 4H 0 o 3Cu  3+  3  2+  4  2  + As0 r + 4S° + &H +1 \Fe 3  +  1+  [2-27]  This is assuming that the arsenic enters solution in the 5+ valence state. However, some arsenic occurs as A s , suggesting the following reaction also occurs [8]: 3+  Cu AsS + 9Fe  3+  3  4  + 2H 0 o 3Cu  2+  2  + AsO; + 4S° + 4H + 9Fe +  2+  [2-28]  Not all the sulphur, however, goes to elemental sulphur. A small fraction of sulphur is oxidized to sulphate [2, 8]: S + 3Fe (S0 ) +4H 0^> 2  4  3  2  6FeS0 + 4H S0 4  2  4  [2-29]  22  The elemental sulphur from the reaction has been found to form locally on the enargite surface as small crystal agglomerates [8, 11].  More details on the proposed leaching reactions of enargite are discussed in Appendix A .  2.3.3.2 Observations on Enargite Leaching Copper is extracted from enargite at a very slow rate. It was reported by one source that there was 50% copper extraction for -100 mesh enargite after 7 days at 80-85°C [2]. This study examined pure enargite synthesized in the laboratory. The conditions that favoured the dissolution of enargite were a high leaching temperature and a high ferric ion concentration. A high acid strength slightly accelerated dissolution but mainly prevented hydrolysis and precipitation of Fe  (which is expected for any ferric-sulphuric acid system).  It was  believed that the kinetics is probably controlled by a chemical reaction on the surface: there were linear kinetics, a low dissolution rate, and a moderately high activation energy [2].  The same group that leached pure, synthetic enargite also compared their results to samples of relatively pure natural enargite. In two cases, it was found they had similar similar rates and activation energies; however, there was more scatter in the data. One of these samples came from Poopo, Bolivia, with coarsely crystalline enargite; the other came from Butte, Montana, which was enargite with occasional patches of CuS. A third sample of enargite from Butte, Montana actually dissolved rapidly; however, there were fine veins of covellite within the enargite that were attacked preferentially, exposing the surface of the enargite and  23  thus allowing for faster dissolution [2]. This brief review demonstrates the importance of the mineralogy in the leaching of enargite samples.  A different group examined a sample of enargite from the Department of Geology at the University of Chile [8]. According to the analysis, this sample contained 46.2% copper, 16.3% arsenic, and 0.55% iron.  Mineralogically, some inclusions of chalcopyrite were  present along with a few particles of quartz. The particle size was -100/+150 mesh. Tests were conducted at 30°C, and were mainly done to compare with biological leaching tests (which will be discussed later, in Section 2.4.5). dissolution in acid medium  (H2SO4)  Without iron, arsenic and copper  was slow, with 1.1% copper extraction at 500 hours.  With ferric iron, dissolution was faster but the rate decreased continuously. There was 4.9% copper extraction reported at 500 hours [8].  The second test gave less favourable extraction than that found in the first test. The particle size may have been somewhat larger for the second test (-100/+150 mesh compared to -100 mesh), but the difference is probably not that significant compared to other factors. The first test was done at a higher temperature (80-85°C for the first test, 30°C for the latter), and temperature was cited as being a very important factor. Secondly, very little information is given on the mineralogy of the sample; only the chemical composition was given. As discussed previously, mineralogy of the ore or concentrate may influence the apparent leaching behaviour of the enargite.  24  Finally, one source has investigated the total pressure oxidation of an ore with enargite present.  The ore investigated, an E l Indio ore, contained pyrite (FeS2), scorodite  (FeAsCvEbO), enargite (Q13ASS4), tetrahedrite ((Cu, F e ^ S t ^ S ^ ) , and tennantite ((Cu, Fe)i2As4Si3). Gold was also present as fine particles associated with sulphide minerals and silver as acanthite (Ag2S) enclosed in enargite [42].  Variables studied were the leach  temperature (200-220°C), reaction time (0-180 minutes), and pulp density (100-325 g ore using 1000 mL of 2 g/L H S 0 ) . 2  4  In general, high copper extractions were reported, in some cases greater than 95%. Iron had re-precipitated as iron-sulphate hydroxide/jarosite. Furthermore, arsenic had dissolved and much of it had reprecipitated with the iron; however, levels in solution were still high enough to require lime treatment to re-precipitate arsenic as a stable ferric arsenate/gypsum product. Antimony reported almost entirely to the residue, probably as a ferric antimonate-type compound. To recover the silver and gold, a lime boil of the residue was required to release silver from argentojarosite; then, the silver and gold could be recovered from a cyanidation leach. In fact, the nearly complete recovery of gold suggested that the refractory matrix had been destroyed during total pressure oxidation [42].  2.4 Biological Leaching Bioleaching is a process by which the mineral is leached with the aid of bacteria. These bacteria are generally acidophilic and oxidize ferrous iron (Fe(II)) to ferric iron (Fe(III)) [15]. Some bacteria also oxidize sulphur to sulphate.  Initial bacterial leaching studies were  performed using Thiobacillus ferrooxidans, which is mesophilic (grows optimally at room-  25  temperature) and autotropic (utilizes carbon dioxide as a carbon source). It was originally thought to be the only microorganism involved in bioleaching [19, 56]. Other bacteria have since been found to play a role in bacterial leaching. Furthermore, there is a growing interest in the use of thermophiles (higher temperature bacteria) because they may give higher leaching rates than mesophiles [15, 35, 56].  Bacterial leaching can be used in the context of heap, dump, in-situ, or reactor leaching [15, 56]. There are many reasons why bioleaching is being considered for many applications [28, 66]: •  Bioleaching can yield potentially low capital and operating costs  •  Biohydrometallurgy can be efficient at a small scale. The process can be operated at the mine site in small, readily expandable modular units; this also eliminates the transportation of the ore or concentrate, which may be important for some isolated mines.  •  Lower grade ores and concentrates can potentially be used in the bioleaching process.  •  Biohydrometallurgy is often more environmentally friendly as it does not produce SO2 and produces residues that are stable or easy to handle.  •  Biohydrometallurgical processes can be easier to operate as it does not have sophisticated hardware associated with conventional technologies and therefore does not require a highly trained workforce. It has more favourable safety considerations compared to those processes with high pressures, high temperatures, or dangerous off-gases.  •  If coupled with SX/EW for copper ores and concentrates, copper can be produced directly.  26  The disadvantage is that, as a new technology, bioleaching is not as well understood and therefore  associated  with perceived risks that may prevent  implementation  [66].  Furthermore, the reaction rate is an important factor. A slow rate results in a longer retention time, which results in a large, expensive leaching tank and large inventories of concentrate and thus large sums of money tied up in working capital [23].  One example of a process that uses biohydrometallurgy is B I O X Technology. This process uses mesophilic bacteria at 35-40°C to oxidize pyrite/arsenopyrite concentrates for gold recovery. The advantages include the absence of noxious off-gasses or toxic effluent, the simplicity of plant operation and maintenance, the ability to use the process on a smaller scale, a tolerance to a wide range of sulphur grade feed, and the production of a stable Fe/As residue.  However, some problems include sensitivity to water quality, especially with  cyanide and thiocyanate, there can be significant neutralization costs, and lengthy residence times measured in days may be required [66].  2.4.1  Bacteria Involved in Bioleaching  There are three kingdoms of bacteria:  archaeobiota, eucaryotes, and eubacteria. Cells of  "higher" organisms are eucaryotic cells, while archaeobiota and eubacteria are procaryotic cells. It is the procaryotic bacteria that play a major role in biohydrometallurgy. Some features that distinguish them from eucaryotic cells include the absense of internal membranes separating the separate cell mechanisms, nuclear division by fission instead of mitosis (possibly due to a single structure with all the genetic information), and a cell wall with a specific strengthening agent [56].  27  There are two major subgroups of procaryotic cells: "Gram-negative" and "Gram-positive". This is the ability to resist discolourization by a Gram stain (use the crystal-violet iodine complex using alcohol or acetone).  These which easily lose their colour are " G r a m -  negative"; those that retain it are "Gram-positive" [56]. Gram-positive cells have a cell wall with a thick single structure; Gram-negative cells have a multi-layered cell wall structure. A s most bacteria in biohydrometallurgy are Gram-negative, it is believed that this cell wall structure plays a major role in many of the processes, especially since transport through this wall is essential for conducting processes for extracting life energy [56]. The exact mechanisms of what occurs in the cell are beyond the scope of this discussion; it is enough to appreciate that it plays a major role in bioleaching.  Most bacteria found in biohydrometallurgy are chemolithoautotrophs, which means they use carbon dioxide as their carbon source for the synthesis of new cell material and can grow strictly in a mineral environment in the absence of light. meaning they  can only  grow  autotropically.  M a n y are obligate autotrophs,  Some microorganisms, however,  are  heterotrophs, which obtain carbon from organic substances. Facultative heterotrophs are autotrophs that can also grow heterotrophically.  Finally, since many leaching processes are  done in acid solutions, bacteria of interest are generally acidophiles, meaning that they can grow optimally at a p H less than 3 [56].  28  2.4.1.1 Mesophiles Mesophiles are bacteria that survive and grow at an optimum temperature between 20° and 45°C. In bioleaching, this is the most well-researched group of bacteria.  The Thiobacillus genus in particular has received the most attention in bioleaching. These are Gram-negative bacteria, non-spore forming rods which grow under aerobic conditions; many are chemolithoautotropic. Thiobacilli obtain energy from the oxidation of sulphur and reduced sulphur compounds.  Some species may oxidize iron and other elements in their  reduced states. The result is that natural but generally slow oxidative reactions are catalyzed and accelerated.  The genus Thiobacillus is of commercial interest since under optimal  conditions of microbial growth the amount of mineral solubilized in the unit time is considerable, and resistance to metal ion concentrations is of the same order of magnitude as those typical of hydrometallurgical processes. For instance, for copper, these bacteria can survive at 55 kg/m of copper [56]. 3  This feature is not commonly shared by all  microorganisms.  Thiobacillus ferrooxidans is the most commonly researched microorganism within the bioleaching literature and has been investigated the most extensively.  It is an obligate  autotroph and can grow in strictly autotropic conditions. Biologically, T. ferrooxidans is relatively diverse, and being highly polymorphic can take a variety of shapes such as rods, spheres, and ovoids [56].  29  T. ferrooxidans can oxidize reduced sulphur compounds and elemental sulphur. It can also promote the enzymatic oxidation of iron.  Although it is not the organism capable of  oxidizing iron, it is this feature that allows it to play a very significant role in biohydrometallurgical processes. It is also tolerant to many metal cations, which is attributed to the ability of cells to exclude the metal cations from their internal structure. However, T. ferrooxidans is relatively more sensitive to metallic anions than to heavy metal cations. The sensitivity to first time exposure and tolerance limits after adaptation can vary between strains of the same species [56].  T. thiooxidans is another commonly investigated species from the Thiobacillus genus. These bacteria primarily oxidize elemental sulphur and reduced sulphur compounds. A result of such oxidation is the production of sulphuric acid [49, 52].  Other acidophilus in the Thiobacillus genus include T. acidophilus, T. kabolus, T. albertis, T. concretivorus, and T. organoparus. T. prosperus are halotolerant, and T. cuprinus are facilitatively chemolithoautotropic bacteria which oxidized metal suphides but does not oxidize ferrous iron. There are also species that grow optimally at intermediate to high pH values [49, 56].  Another important genus is Leptospirillum. Leptospirillum ferrooxidans are Gram-negative, acidophilic chemolithotropic bacteria which oxidizes ferrous to ferric iron. Compared to T. ferrooxidans, they can tolerate lower pH and higher concentrations of uranium, molybdenum, and silver. They are, however, more sensitive to copper and unable to oxidize sulphur or  30  sulphur compounds. It must therefore work in cooperation with other bacteria (such as T. ferrooxidans or T. thiooxidans) in order to attack minerals [49, 56].  Heterotropic organisms have also been found to be present and are believed to aid in metal leaching processes, although their exact role is obscure [56]. Some believe that although they aid in bioleaching, they may not benefit directly from metal solubilization reactions [49].  It is important to note that often it is a number of different species interacting together to dissolve the mineral instead of a single species. These interactions may be cooperative and or competitive. As conditions change, the community of microorganisms present may also change [56].  2.4.1.2 Thermophiles Thermophiles are bacteria that have an optimum growth temperature starting from 30-40°C to a maximum of 100°C. Moderate thermophilic bacteria live at temperatures around 50°C, while extremely thermophilic bacteria live at temperatures greater than 50°C [49, 56]. Much less is known or has been researched on these bacteria.  Moderate thermophiles grow optimally at temperatures higher than that of mesophiles, but less than 50°C. One genus in particular, the Acidiphilium genus, consists of acidophilic and strictly heterotropic bacteria. Another bacteria in this group, Thiobacillus acidophilus, are facilitative autotrophs that can utilize either powdered sulphur or glucose (and other organic  31  compounds); it, however, cannot grow on Fe  or metal sulphides alone.  Interestingly,  autotropic growth on elemental sulphur is not inhibited by ferrous iron, although it does inhibit growth on glucose [56].  Extreme thermophilic bacteria live at temperatures greater than 60°C. The Sulfolobus genus is commonly associated with this group of bacteria. For instance, Sulfolobus acidocaldarius is a facilitative heterotroph, and is able to grow on both elemental sulphur and iron [56]. Acidianus brierleyi is an obligate autotrophy that can grow on ferrous iron, elemental sulphur and metal sulphides [49, 56]. There are many other extremely thermophilic bacteria that are involved in bioleaching. The largest problems in the use of these bacteria is the lack of understanding of their behaviour compared to mesophiles, and the requirement for a lower pulp density; many of these bacteria have a weak cell wall and may suffer abrasive mortality from the minerals during mixing [47, 48].  As with mesophilic bacteria, it is generally a number of different species interacting together (whether cooperatively or competitively) that aids in leaching, and not simply a single species.  2.4.2  Microbial Growth  When microbial cells are introduced into fresh medium, a certain time elapses before cell division starts; this is called a "lag phase". The length of the lag phase depends on the organisms present and the state of the cells innoculated (since old cells take longer than active ones). It can depend also on a number of other factors such as the nature of the  32  innoculum, the size and composition of the culture medium, the gases available, and the temperature. The length of the delay is believed to be related to the time required by the microorganisms to orient the adaptive enzymes to the new conditions [56].  At the end of the lag phase, the population starts to grow and microorganisms double by cell division. This is called the "exponential phase" or the "logrithmic phase". A straight line on a semilogarithmic plot of number of viable organisms per unit volume versus time is observed [56]. Mathematically: N =2"-N n  [2-30]  0  where No = initial number per unit volume N„ = number per unit volume at time t„ after n generations  A period follows where no further growth occurs; either cell division stops or the rate of viable cell formation equals the death rate. This is called the "stationary phase", and it is indicated by a line parallel to the "t" axis in the N versus t graph. The medium becomes n  modified as nutrients become depleted and microbial metabolism products increase; there are also changes in pH and a decrease in 0 and CO2 availability in the medium [56]. 2  Finally, the "death phase" occurs when the medium becomes unsuitable for bacteria. If the bacteria are not transferred to fresh medium, they die and lysis may occur [56].  Figure 2.3 illustrates these various stages of growth graphically.  33  lag  exponential  stationary  death  E V 1*  c  1  '3 • ©  .  1 S  O  Time  Figure 2.3: Typical growth curve of a bacterial population in a culture [56].  2.4.3  Bioleaching Reactions  There are two modes of bacterial attack: direct and indirect leaching. In indirect leaching, it is believed that the bacteria recycles reagents such as H and Fe +  3+  and thus aids in the  dissolution of the minerals of interest. The bacteria need not be in contact with the mineral as it only recycles the catalytic agents.  In fact, many bacteria (such as Thiobacillus  ferrooxidans) derive its life energy from the conversion of ferrous iron to ferric iron. Other bacteria gain energy from the conversion of sulphur to sulphate. The proposed mechanism for indirect attack is as follows [15, 19, 30, 48, 49, 51, 52, 54, 56, 68]:  a)  Ferrous ions enter the solution, possibly by attack of H2SO4 and O2 on iron sulphide minerals: e.g.  CuFeS + 40 -> CuS0 + FeS0 2  2  4  [2-31 ]  4  FeS + \4Fe + SH 0 -> l5Fe +16H + 2S0 ~ 3+  2  2+  2  +  4  [2-32]  34  b)  The bacteria catalyzes the oxidation of the ferrous ions: 2FeSO, + H SO, + y 0 2  2  "  2  a / a c  " ° " >Fe (SOJ + H 0 2  3  2  [2-33]  This reaction is generally very slow without the action of bacteria. c)  The Fe(III) acts as a leachant for sulphide minerals present in the ore: 2Fe + M S  2Fe + M  3+  2+  2+  + S°  [2-34]  Note that reactions involved in (b) and (c) are cyclic, and that although elemental sulphur is shown in the above reaction, sulphate may be formed.  Some bacteria are involved in the oxidation of sulphur. In this manner the elemental sulphur may be transformed to sulphate [15, 34, 48, 49, 54, 68]: S +y O + H 0 -> H SO 0  2  2  2  2  A  [2-35]  There are a number of different sulphur mechanisms that have been proposed, and two notable ones are the thiosulphate and the polysulphide mechanisms [51, 54]. The exact details of these mechanisms will not be discussed in this paper; it is sufficient to say that the end result is the formation of sulphate or sulphur, and intermediate sulphur compounds (e.g. S 0 6 \ S2O3 ", H S ) may be formed as oxidation products [51, 54]. Of course, the final 2  4  2  2  n  sulphur product will depend on the sulphide mineral being leached as well as the leaching conditions present. The fate of such sulphur species, however, may cause passivation, and this may play a role in the kinetics of the leaching of a mineral as the bacteria will need to remove this layer [51].  Direct leaching involves bacterial attachment to the metal sulphide surface with the bacteria oxidizing the mineral via the action of enzymes [15, 49, 51, 52, 54, 68]. The ferric/ferrous  35  reaction is similar to that described for indirect leaching, but is bound in the cell envelope. This envelope is sometimes referred to as the extracellular polysaccaride (EPS) layer or as consisting of extracellular polymeric substances that are excreted by the microorganisms [15, 51, 54]. The sulphur reactions described above may also occur in this layer. Intimate contact between the bacteria and the mineral is required for direct attack. It has been suggested that the bacteria may condition the surroundings within the formed layer to facilitate dissolution of the mineral. However, these mechanisms that occur during attachment and the initiation of solubilization are not completely understood.  More likely both mechanisms occur together, and in fact models do exist that suggest this [52, 68].  One source suggests even that co-operative leaching occurs, where attached  bacteria liberate energy-carrying species; ones that do not get used by them feed the free bacteria [52].  Although this overview summarizes the mechanisms involved in bioleaching, these mechanisms are actually very complex and are still a major area of research. However, it can be seen that there are two important sub-processes:  bacterial ferrous iron oxidation, and  chemical ferric leaching of the sulphide minerals.  According to the Nernst equation,  assuming pseudo steady-state [35]:  [Fe ] 2+  = exp  [2-36]  At 25°C [56]: a .3+ E = 0.771 + 0.05911og 'Fea  [2-37]  36  Thus, the potential of the solution can be an indication of the activity of the bacteria: as the bacteria oxidize more ferrous ions to ferric ions, the potential of the solution will increase.  Many of the reactions involved in ferric sulphate leaching can be applied to bacterial leaching. Note that the cyclic nature of the reactions can lead to the build-up of  H2SO4  and  dissolved iron. Just as in ferric sulphate leaching, a build-up of iron can lead to precipitation reactions and the formation of iron compounds such as jarosite.  Thiobacillus ferrooxidans is the most used microbe for bacterial leaching commercially, and has been shown to catalyze the oxidation of chalcopyrite, chalcocite, covellite, bornite, enargite, stannite, and tetrahedrite [23]. Chalcocite, covellite, and bornite are bioleached rapidly and completely.  Chalcopyrite is only partially leached due to slow bioleaching  kinetics and the formation of a passivation layer. Some sources even consider it nonviable due to the long leach times required, although efforts have been made to improve recovery through bioleaching in heaps. One source suggested that fine grinding to less than 10 urn may be needed [28, 30, 33]. More recent literature appears to be more optimistic about the bioleaching of chalcopyrite.  2.4.4  Variables and Leaching Conditions  2.4.4.1 Acidity The pH of a solution for bacterial leaching is typically 1.5 to 3.5 [19, 23, 49]. It should be noted, however, that above a pH of 2.5 ferric iron precipitates. The lower limit may be the  37  tolerance of bacteria to H [23]. Some report the lower limit for T'. ferrooxidans as pH 2.0; +  however, it can be adapted to lower pH values [49].  2.4.4.2 Aeration Oxygen and carbon dioxide are essential nutrients and are important for bacteria growth. Oxygen is required for some of the reactions (as discussed previously); it is for good growth and high activity of the leaching bacteria. Carbon dioxide is required to provide a carbon source for the bacteria, and in some cases the growth of bacteria may be limited by carbon dioxide. Although high carbon dioxide concentrations can be inhibitory, a degree of carbon dioxide enrichment can be helpful. To increase the supply of oxygen and carbon dioxide, forced aeration may be needed [10, 19, 23, 30, 49, 56].  2.4.4.3 Nutrients Other than oxygen and carbon dioxide, bacteria need nutrients such as nitrogen (from ammonium), phosphate, calcium, magnesium, and potassium. Many of these elements have different physiological functions and are therefore important for survival. If the bacteria are generally chemolithoautotropic, only inorganic compounds are required; this kind of medium is called a mineral base since the source of nutrients is in inorganic form [23, 30, 49, 56].  There are many different kinds of culture medium and broth recipes. There are two different kinds of mediums.  A minimal or synthetic medium is a medium entirely composed of  chemically defined compounds, trace amounts of several ions, and potentially organic compounds that may be required by particular strains. A medium considered a broth, or is  38  rich or complex when it is chemically undefined or has ingredients of unknown chemical composition, such as milk, yeast, or meat. Furthermore, a selective medium inhibits growth of a group or groups of microorganisms; elective mediums encourage the growth of the required organism without positively deterring the growth of others [56].  Many of the mediums used in biohydrometallurgy appear to be synthetic mediums that are generally elective.  Some typical nutrients and concentrations for bioleaching culture  mediums are listed in Table 2.2.  Table 2.2: Typical nutrients and concentrations for bacterial leaching [23]. Component (NH ) S0 K HP0 KCI A1 (S0 ) T8H 0 MgS0 -7H 0 MnS0 H 0 Ca(N0 ) -4H 0 Na S0 4  2  2  2  4  4  4  3  2  4  2  4  3  2  2  2  2  4  Concentration (g/L) 0.1-5 0.5-5 0.05-0.1 1.0-8.0 0.01-3.0 0.05 0.01 0.05  In general, as long as the nutrients are above a certain threshold they do not affect the growth rate [56].  2.4.4.4 Organic Compounds Some have tried surfactants to increase the wettability of minerals by decreasing the contact angle and lowering the surface tension of the leaching solution [23]. It is known, however, that many surfactants, flotation reagents, and organic extracts used in solvent extraction generally have an inhibitory effect on leaching bacteria. The decrease in surface tension can  39  also lead to a reduction of oxygen mass transfer. Therefore, organics present from solvent extraction need to be removed before bioleaching [49, 56].  2.4.4.5 Temperature Temperature can affect the chemical reaction rates and O2/CO2 solubility. As well, bacteria are sensitive to temperature and can only operate within a specific range. Each species has its own temperature range it can tolerate and a temperature for optimal growth; the rate of reaction will actually go through a peak within this range.  For mesophiles such as T.  ferrooxidans and T. thiooxidans, the temperature optimum range is between 20-35°C. At much lower temperatures, there is a decrease in solubilization; however, some solubilization has been found to occur even at 4°C. Microorganisms may survive at lower temperatures (e.g. -40°C) although with a very reduced growth rate and metabolic activity. At too high of a temperature (e.g. greater than 50°C) the bacteria may be destroyed.  As discussed  previously, thermophilic bacteria can tolerate higher temperatures [19, 23, 30, 49, 56].  2.4.4.6 Ore or Concentrate Characteristics A decrease in particle size results in an increase in surface area and an increase in leaching. A n increase in pulp density may increase metal extraction but some metals are toxic to bacteria and inhibit at higher concentrations [49, 56]. The limit on pulp density is normally about 20-25% for mesophiles, possibly due to oxygen mass transfer characteristics [64]. The use of a low pulp density can increase the capital and operating costs. Extreme thermophiles are more sensitive to an increase in pulp density. This may be due to an abrasive effect of the mineral on the bacteria, as some thermophilic bacteria do not have a cell wall [47].  40  Other minerals present in the ore can also affect the bioleaching process. For instance, with high carbonate, the pH will increase during leaching and inhibit the bacteria [49].  2.4.4.7 Tolerance of Bacteria to Ions The effect of heavy metals depends on the concentration in solution.  They can be  bactericidal, where microorganisms are killed and do not grow upon removal. They can also be bacteriostatic, where microorganism growth is inhibited but not killed [56].  Different species have different sensitivities, and strains can be adapted to specific can be adapted to specific metals or substances at higher concentrations. There are two different means by which a microbial population adapts. Physiological adaptation is where nearly all cells of the population assume a new phenotype (observable characteristics); this change is reversible, and the original condition is restored when the stimulus is removed. Genetic adaptation, or mutation and selection, involves the emergence of new genotypes (genetic make-up); this is generally very rare.  Mutant cells with enhanced resistance survive the  addition of the metal cation. This change is permanent, and it has been observed for T. ferrooxidans cultures in increasing concentrations of uranium; it is also believed to be involved for cadmium and mercury [56]. These processes of adaptation are important as many of the elements being leached can be toxic to the bacteria. For instance, copper is potentially a toxic ion to bacteria, but with adaptation bacteria have been found in solutions with greater than 20 g/L copper [23, 49].  41  2.4.4.8 Arsenic Toxicity One challenge in the bioleaching of arsenic-bearing minerals is that arsenic in solution is toxic to organisms, including those that are used in bioleaching such as T. ferrooxidans and Sulfolobus BC [8, 9]. Adaptation can aid in allowing bacteria to survive. However, one source claimed it was very difficult to adapt cultures of moderate thermophiles to arsenic [64].  Work in the literature has been performed to examine the toxicity of arsenic on Sulfolobus BC unconditioned to high arsenic levels. It was found that As(III) is 2 to 3 times more toxic than As(V) [16].  Other studies have indicated similar results:  a similar study using  Sulfolobus BC found a 90% decrease in growth rate at 600 mg/L As(III), but a significant toxicity for As(V) only at 1000 mg/L [9]. The larger toxicity of arsenite than arsenate has also been observed in other bacteria [14]. It appears that arsenate influences the maximum growth capacity while arsenite primarily influences the growth rate [14].  Experiments with arsenopyrite with Sulfolobus B C have shown that arsenic is released initially as arsenite but is eventually converted to arsenate.  Thus, in the process of  bioleaching with an arsenic source, arsenite will eventually be oxidized to arsenate.  It  appears that there is a well-defined role for bacteria in the presence of ferric. Exactly how this oxidation takes place is generally not well understood, but it is known that the cells do need to be alive (dead cells and Fe(III) could not oxidize arsenite) and that ferric needs to be present (alive cells without ferric provided negligible oxidation of arsenite over an extended time period) [14, 16].  42  The decrease in toxicity in the presence of iron is also observed with T. ferrooxidans [8]. However, in general mesophiles are more tolerant to arsenic in solution than thermophiles [64].  2.4.5 Enargite Bioleaching Recall the study of the leaching of enargite in sulphuric acid on the sample from the Department of Geology at the University of Chile [8, 11]. Also recall that the enargite had a chemical analysis of 46.2% copper, 16.3% arsenic, and 0.55% iron; some inclusions of chalcopyrite were present along with a few particles of quartz.  The particle size was -  100/+150 mesh, and tests were conducted at 30°C with T. ferrooxidans. Strong and rapid adherence of the bacteria to the mineral surface was observed. After 500 hours of leaching with bacteria there was 11% dissolution of the copper and arsenic [8, 11].  The leaching of enargite with Sulfolobus BC, a high temperature thermophilic bacteria, was also tested on the same enargite sample as mentioned above at 70°C. Cell attachment to the enargite surface was observed as was bacterial growth. After a certain point, however, the rate of copper dissolution increased strongly until ferric iron decreased due to coprecipitation with arsenic as ferric arsenate. After 552 hours, 52% of the copper dissolved. In the absence of ferric during bioleaching, only 12% of the copper dissolved [9].  It is interesting to note that in a study of leaching using synthetically pure enargite in hot sulphuric acid (80-85°C), there was 50% extraction after 7 days, or 168 hours [2]. In the  43  best-case scenario for bioleaching discussed above, there was 52% extraction at 70°C with Sulfolobus BC after 552 hours [9]. There might be something odd about the mineralogy of the samples obtained that makes this particular enargite sample exceptionally refractory; there may also be other factors that are not being accounted for that are strongly influencing the bioleaching reactions.  Another study using T'. ferrooxidans examined an enargite-pyrite concentrate from Minera El Indio from L a Serena, Chile [10]. A rather detailed chemical analysis and mineralogical spectrum were given for the sample: 42.0 ug/g gold, 21.2% Cu, 22.6% Fe, 37.8% S, 7.7% As, 40.7% Cu AsS , 42.8% FeS , and 3.9% CuFeS . While varying the enrichment of the air 3  4  2  2  with carbon dioxide (from none to 4% enrichment), the extractions obtained were 16.17 to 19.28% copper after 24 hours. No particle size data was given, making it hard to compare with the above data. However, note that only 9% was extracted after 550 hours in the above study. Some factors that could have influenced this include a mineralogy more favourable for enargite extraction and a (potentially) smaller particle size. The leaching conditions were also not well reported in this study, making it hard to compare to the above data.  In another study [44], a gold concentrate (El Indio Mining Company, L a Serena, Chile) was used containing 40.7% enargite, 42.8% pyrite, 3.9% chalcopyrite, 0.8% chalcocite, 0.3% covellite; 42 g/ton Au, 440 g/ton Ag, 21.1% Cu, 22.6% Fe, 37.8% S, and 7.7% As. This was studied using a T. ferrooxidans R2 culture adapted for several months in 9K medium; tests were conducted using an air-lift column. Particle size was -200 mesh; pulp densities were 6, 18, and 24% w/v; the pH was 2.4, and the temperature was 33°C. It was determined that the  44  ore was difficult to leach, with no more than 5% of the arsenic, 17% of the copper and 20% of the iron solubilized after 24 days. It was believed due to the linear leaching kinetics that the leaching of enargite was probably controlled by a surface reaction.  One study on Sulfolobus B C used a copper concentrate from Chuquicamata Division of CODELCO-Chile [47]; the composition was 31.82% pyrite, 18.31% covellite, 15.29% chalcopyrite, 14.22% chalcocite, 13.02% enargite, 35.2 wf% copper, 19.48% iron, 36.4 % sulphur, and 2.48% arsenic.  The temperature was 68-70°C; the particle size was -212  microns (70 Tyler mesh) with 67% under 38 microns (400 mesh). Batch reactor experiments were performed; the conditions were acid, ferric, bacterial, and bacterial-ferric. After 150 hours, 30% copper was extracted from acid (from the leaching of chalcocite) and 42% from the acidic ferric solution.  Bioleaching generated 90% extraction after 300 hours.  Pulp  density was a major factor in these experiments; at pulp densities of 0.5, 2, and 5% w/v, the copper recoveries obtained were 85%, 72%, and 32% respectively. This is likely because of the abrasive effect of the mineral upon Sulfolobus, as it is an archaebacteria and lacks a cellular wall.  Other studies have been performed into the bioleaching of enargite and enargite concentrates; however, information into the extraction rates and the leaching conditions are usually incomplete. One important observation with T. ferrooxidans using a mostly enargite and pyrite sample (41% enargite, 43% pyrite) is that pyrite is bioleached over enargite. The lack of arsenic in solution, low levels of copper and the increase in iron in solution was seen as evidence for this [34].  45  Overall, bioleaching does appear to show some promise for the extraction of copper from enargite.  Since arsenic appears predominantly as arsenate, the removal of arsenic from  solution will be straightforward. Furthermore, the rates of leaching appear to be higher than that for ferric sulphate leaching, although the information on the amount of extraction is inconsistent and in need of further investigation.  2.5 Chloride Leaching Ferric chloride is a better oxidizing agent than ferric sulphate due to the high solubility of metal chlorides and because chloride ions can readily complex copper ions [23].  For  instance, the solubility of CuCh is 107.9 g in 100 g of hot water; for FeCb, it is 535.8 g in 100 g of hot water [23]. Furthermore, chloride acts as a complexant for many metals, and the high ionic activities present in acidic chloride solutions contributes to the fast dissolution of many minerals [40].  Example reactions of copper minerals in chloride systems are as follows: For covellite [23, 58]: CuS + FeCl -> CuCl + FeCl + S o 3  2  -0  CuS + CuCl -> ICuCl + S'  [2-39]  2  CuS + FeCi; -> CuCF + Fe + S° + 2CI 2+  2  [2-38]  [2-40]  46  For chalcopyrite [23, 61]: CuFeS + 4FeCl -> CuCl + 5FeCl + 2S•o  [2-41]  CuFeS + 3FeC/ -> CwC/ + 4FeC/ + 25'-o  [2-42]  2  3  2  2  2  3  2  2CuFeS + 1C1 -> 2CuCl + 2FeCl + 3S C/ 2  2  2  2S Cl + 4H 0 + Cl 2  2  2  2  3  2  [2-43]  2  6HCI + H S0 + 35' 2  [2-44]  4  (The limiting step is the constantly thickening layer of sulphur on the surface [61].)  In acid-chloride solutions, important leaching variables include temperature, pH, and chloride concentration. The effect of temperature is pronounced above 55°C, where the rate of reaction increases as the temperature increases. Very often, the above reactions will be controlled by mass transport [23].  The predominant sulphur species produced is elemental sulphur.  For instance, in the  M I N T E X process, less than 5% of oxidized sulphur occurs as SO4 " and more than 95% as 2  S°. In small scale test work performed by Cominco, 75-90% of the oxidized sulpure occurs as elemental sulphur [37].  Other processes also predominantly form elemental sulphur.  Separation of sulphur can occur by flotation or physical separation methods such as hot filtration, pelletization, and flotation [37].  Other elements can also be dissolved in the chloride solution. Antimony and arsenic can be dissolved by chloride solutions; some reactions involving specific arsenic and antimony minerals are as follows [59]:  47  FeAsS + 5FeCl -> 6FeCl + AsCl + S  [2-45]  As S + 6FeCl -> 2AsCl + 6FeCl + 3S  [2-46]  Sb S + 6FeCl -> 256C/ + 6FeCl + 35  [2-47]  3  2  2  3  3  3  3  2  3  3  3  2  2  Chalcopyrite, a refractory copper mineral, can more easily be dissolved in chloride solutions, and its leaching is strongly dependent on temperature [37]. It is this potential for leaching refractory minerals that makes the use of chloride solutions so appealing. However, despite the interest in chloride hydrometallurgy, there has not been any work found on the leaching of enargite in these solutions.  Only one source discussed the effects of a chloride salt solution on enargite. When placing various minerals in 10% ferric chloride solution with HC1, enargite was completely unaltered in appearance [53]. This work was dealing more with mineral identification as opposed to mineral leaching; however, this is the earliest work available describing enargite in a chloride solution.  One can not assume, however, that because chalcopyrite can be leached enargite can be leached as well. A n investigation of tennantite (Q112AS4S13) and tetrahedrite (Cui2Sb4Si3) in ferric chloride-hydrochloric acid solutions showed that both minerals are  extremely  refractory to ferric chloride, with slow rates even at higher temperatures and immeasurably slow rates at lower temperatures [38].  48  2.5.1 Industrial Processes Chloride systems, as far as it is known, are not in commercial practice for copper extraction, despite the large number of processes that have been developed. Some processes that have been developed are as follows [37, 39, 40]: C L E A R Process (Copper Leach, Elecrolysis And Regeneration) by the Duval Corporation Cymet Process by Cyprus Metallurgical Corporation Minemet Recherche Process by Imetal Corporation Cuprex Process, jointly developed by Imperial Chemical Industries, Technicas Runidas and the Nerco Minerals Company -  The M I N T E X process The UBC-Cominco Process The Dextec process The Elkem process The Intec process (using Halex, a mixture of chloride and brominde)  -  The U S B M (US Bureau of Mines) process The G C M (Great Central Mines) process  2.5.2  Advantages  There are some distinct advantages to the use of a chloride process for copper (usually involving a F e C V C u C b leach). First of all, the kinetics are rapid since the chloride appears to accelerate the "corrosion" leaching of the copper sulphide minerals. The resulting chloride salts are highly soluble, which may result in high metal recoveries. Furthermore, there is a  49  lack of pyrite attack. Elemental sulphur (as opposed to sulphate) is generated in the process. Finally, the electrowinning of copper is from the cuprous state instead of the cupric state in sulphate systems, which may provide an energy benefit [33, 37, 40].  2.5.3 Disadvantages Despite the potential advantages of the leaching of copper in chloride media, there are serious disadvantages that have prevented their use commercially.  First, there are serious concerns about the purity of the final copper product.  Chloride  leaching is not highly specific, and elements such as silver, lead, zinc, arsenic, and antimony are all soluble in concentrated chloride media. These solutions are difficult to purify, and in fact solvent extraction, which is extremely effective for sulphate solutions, is not as effective for chloride solutions. Furthermore, in electrowinning, elements such as selenium, tellurium, and silver have similar deposition potentials and will co-deposit with copper to some extent [33, 37, 39]. In the Cymet and Cominco processes, CuCl precipitate is produced to purify the solution, but some impurities still report to crystals and some co-precipitation occurs, implying the need for further purification steps [37].  In electrowinning, copper will tend to plate as a granular or powdered product. The high surface area of the powdered copper increases the chance of contamination. The resulting copper is also difficult to recover from plating cells.  Furthermore, this copper must be  treated before being sold, usually be pressing and sintering or melting [33, 37, 39].  50  Furthermore, electrowinning with chloride solutions can be expensive.  High current  densities are required, resulting in a higher energy cost. As well, chlorine can result from the electrowinning process, which is extremely toxic and corrosive. Extensive hooding and venting is required to capture the chlorine and to maintain a safe working environment [39].  In general, acidic chloride solutions are also volatile, and extensive hooding, venting, and vapour recovery systems are required. Chloride solutions are also much more corrosive than sulphate solutions, and corrosion concerns do play a role when designing the plant [33, 39]. The final leach residues can also be environmentally abusive, and considerable cost may be required before these can be disposed of safely [39].  In chloride solutions, silver and copper have very similar behaviour. Silver will also dissolve in chloride media, albeit slower than copper, depending of course on the mineral form of silver. Unfortunately, silver recovery methods are not well defined [37]. As for gold, it is virtually insoluble in chloride media unless a very high oxidation potential is maintained (with, for instance, CI2, H2O2, etc.). Total sulphur removal is required for gold leaching. The sulphur recovered is often contaminated with selenium, which means a purification step may be required in order to sell the sulphur as a by-product [37]. Overall, precious metal recovery from chloride systems can be difficult to perform.  These disadvantages are very serious, and in fact this is why chloride systems are not generally used for copper hydrometallurgy.  51  2.6 Ammonia Leaching Ammonia leaching has been proposed for copper systems, although it would more likely be used in mixed copper concentrates such as nickel-copper-cobalt, copper-zinc, and nickelcopper concentrates [19, 23]. It is harder to handle because it is more volatile, but it is a common reagent in other hydrometallurgical systems.  Overall reactions in the ammonia system are as follows [19, 23, 59]: For chalcocite: Cu S + 6NH + (NH, ) SO, + / 0 -+ 2Cu(NH ), SO, + H 0 5  2  3  2  2  2  3  2  [2-48]  For covellite: CuS + 4NH + 20 ^Cu (NH ), SO, 3  2  [2-49]  3  Forbornite: 2Cu FeS + 36NH + 2(NH,) SO, + ^/ 0 5  4  3  2  2  +(2-  2  n)H 0 2  ->\0Cu(NH ),SO , + Fe 0 • nH 0 +  3  2  3  [2-50]  2  For chalcopyrite: 2CuFeS + \2NH +"/ 0 + (2- n)H 0 2  3  2  2  2  -> 2Cu(NH ),SO, + 2(NH,) SO, + Fe 0 • nH 0 3  2  2  3  [2-51]  2  The reactions for chalcocite, covellite, and bornite will be complete at lower temperatures; higher temperatures are required for chalcopyrite, and increasing the oxygen partial pressure will certainly increase the initial extraction of copper. Other important variables in ammonia systems include the ammonia concentration and SO4 " concentration. One should note that in 2  52  this system, ammonia can remain as free NH3, be neutralized to N H or be complexed with 4  copper ions to form ammines such as Cu(NH ) 3  4  and Cu(NH ) 3  2  [23, 40].  For a copper-zinc concentrate pressure leached in a N F f - N H 3  4  sulphate solution, pyrite  remained unreacted and was in found in the residue. The iron associated with copper and zinc minerals formed a ferric oxide and remained in the residue.  Alumina, silica, lime,  magnesia, gold, and silver also reported to the residue. Finally, in the presence of ferric ions, arsenic and antimony formed insoluble ferric arsenate and antimonite, which also reported to the residue [23].  2.6.1  Leaching of Enargite  The leaching of enargite in ammonia solutions with small oxygen overpressure is believed to occur by the following reaction [1, 17]: Cu.AsS, + \3NH, + 8.750 + 2.5H.O 2  [2-521 -> 3Cu(NH )l 3  +  + NH,H AsO 2  + 4S0 ~ +2H 2  A  +  Note that both copper and arsenic forms are soluble. According to the literature, only a maximum of 60% of the copper is extracted after a 24 hour leach at 82°C [1]; lower extractions are realized at lower temperatures. Figure 2.4 shows an Eh-pH diagram for the enargite-ammonia-water system.  53  Experimental work done on the leaching conditions revealed that the ideal conditions were set to oxygen partial pressure of 5-50 psi, at 82°C and pH 10. Above a concentration of 0.3044 total NH3, there was no influence on the rate of dissolution of enargite indicating that the rate is likely not chemically controlled. Furthermore, as the temperature was increased, there was a significant increase in the extraction of copper from enargite. As well, a decrease in particle size resulted in an increase in the rate and the extent of copper extraction from enargite. For instance, after 8 hours, 24% of the copper was extracted from the -100/+150 mesh fraction, but 51% for the -270/+400 mesh size fraction [1].  A n electrochemical mechanism was proposed for the oxidative leaching of enargite with ammonia. This mechanism was described as follows [1]:  54  anode  Cu AsS + 390H~ o 3Cu + \9H 0 + HAs0 ~ + S0 r + 35e'  cathode  0 +2H 0 + 4e" o40H~  2+  3  2  2  4  2  2  [2-53] [2-54]  2  The 60% extraction of copper seems very appealing compared to other processes discussed previously. However, ammonia solutions are not as common for copper leaching as sulphate solutions. It should also be noted that this was the only study found that examined the relationship between particle size and the reaction rate, and as expected a decrease in particle size increased the rate.  This study is also impressive because it actually proposes a  mechanism and the kinetics were examined carefully (careful analysis of the kinetics indicated that a surface chemical reaction was the rate controlling step). This type of careful study is needed for enargite in other systems.  2.7 Sodium Sulphide Leaching Sodium sulphide in an alkaline solution is not a conventional means of leaching copper ores. However, it has caught the attention of some because it selectively leaches the arsenic from enargite, leaving covellite [3], which can be processed by known means.  The alkaline  leaching of enargite in sodium sulphide is as follows [17]: 2Cu AsS + 3Na S -> Cu S + 2Na AsS 3  A  2  2  3  4  [2-55]  Cu S is recovered as a solid and arsenic enters the liquid in the pentavalent or trivalent form 2  of thioarsenic compounds (depending on the reaction conditions) [17].  One source studied an enargite concentrate from E l Indio, Chili, containing mainly enargite with some quartz [17]. It was leached in 400 mL solution, with 4 g enargite at 90°C. The  55  best results was 90.73% of the arsenic after 60 minutes, at Na S/NaOH = 2 (with 100 g/L:50 2  g/L).  On average, copper in solution was not greater than 0.5%.  After grinding in an  attrition mill for 60 minutes, 96% As and 72% Sb was recovered after 10 minutes of leaching; for the as-received, it was 61% As and 41% Sb. Unfortunately, no particle size information was given for any of the leaching experiments, making it hard to objectively analyze the results.  Another source cited the work of the Leparnto Consolidated Mining Company on an enargite-pyrite concentrate from the Republic of the Philippines in Northern Luzon [4]. They investigated a number of ways of extracting the arsenic from enargite, and reported primarily on their work with alkaline sodium sulphide leaching. The leaching conditions involved no more than 2.5 molar sodium sulphide and 0.25 molar NaOH; temperatures were greater than 80°C. They found that more than 90% of the arsenic was extracted in 3 to 4 hours with 2 times the stoichiometric sodium sulphide.  Antimony was also dissolved in the leach  solution, although the kinetics of this was believed to be slower. Again, no particle size data was given for the samples being leached.  At greater than 80°C, the sodium thioarsenate (Na3AsS4) is dissolved in the solution, and will precipitate upon cooling [4]: 3H SO + 2Na AsS -> 3H S + 3Na S0 + As S 2  A  3  4  2  2  4  2  5  [2-56]  It was estimated that 5-6% of silver and 8% of the gold was leached in the process of leaching the enargite. This is not surprising because the solubility of gold in sodium sulphide  56  is well known [4]. Although this was claimed to be recoverable in an industrial process, no details were given as to how this would take place.  The advantage of the sodium sulphide leach is that the arsenic is preferentially leached from the enargite, leaving a mineral that can easily be leached by conventional processes or processed by pyrometallurgical means.  2.8  Discussion  Enargite has certainly not attracted attention as has chalcopyrite and other refractory minerals. Studies to date have also concluded that enargite is very refractory in sulphate solutions. Because the removal and disposal of elements such as arsenic can be troublesome, there has been little motivation to continue such work. However, with a need to extract metals from more refractory minerals, enargite may again become of interest.  Although some work has been done on the leaching behaviour of enargite, it is interesting to note what these studies do not cover. Although enargite has been found to be refractory in sulphuric acid solutions, the investigated particle sizes are just under 100 mesh, or 149 mircons. Studies using finer particle sizes have not been covered. There has also not been a study on the effect of temperature. The fact that there are wide variations in results reported by various sources may be accounted by either a change in these variables and or differences in mineralogy.  57  Bioleaching has been more extensively researched with respect to enargite leaching. Much of the work done has been with respect to refractory gold ores where enargite may be present. In these cases, the goal is to dissolve enough of the enargite and other minerals to access the gold. With respect to leaching copper, there is a potential for developing such a process since experiments with bacteria seem to yield better results than those in sulphuric acid solutions under similar conditions. However, in some cases the leaching variables are not well described. Again, most of the particle sizes (if reported) are just under 100 mesh (149 microns). Since the fine grinding of chalcopyrite has been recommended for bacterial leaching, perhaps the same applies for enargite. Again, variations in leaching variables and mineralogy may account for differences in the percentage of copper leached between different studies.  Other reagents have been considered for use in the leaching of enargite, and unfortunately these have been researched more thoroughly. Temperature and particle size appear to be important variables in these systems. This may provide a clue for the leaching of enargite in more conventional (sulphate) systems:  perhaps with smaller particle sizes and higher  temperatures enargite might be leached.  Coupled with a lack of knowledge of the enargite mineral leaching behaviour is a lack of knowledge of the arsenic-water system. It is therefore difficult to predict how arsenic species will behave in the described leaching systems, especially since the data available is unreliable or incomplete. The presence of arsenic and other impurity elements will also possess  58  additional processing challenges since this will have to be converted to a form for safe disposal.  Overall, the leaching behaviour of enargite is not well known. If it is to be successfully leached in an industrial process, there is a need to investigate its behaviour in conventional systems that are used industrially instead of in exotic systems that will likely never be used in an industrial setting.  2.9 Objective It was decided that bioleaching would be the focus of the experimental work. In this context, the purpose of this work is to determine the leachability of enargite under bioleaching conditions. First, it will be determined i f enargite can be leached. Secondly, i f enargite is leached, the conditions present as well as the leaching behaviour of enargite will be examined closely. As the work on enargite leaching is limited, it is hoped that such work will provide a foundation for future studies into the viability of leaching enargite on a larger scale.  59  3. Experimental Methods Shake flask tests on natural enargite were conducted using three different groups of bacteria: mesophiles, moderate thermophiles, and extreme thermophiles at 35°C, 48°C, and 68°C respectively. In order to determine the leachability of enargite and the associated minerals, complete mass balances were performed to determine the extraction of copper, iron, and arsenic. Potential and pH readings were also taken throughout the experiments.  This chapter covers the experimental methods used to conduct the bioleaching experiments. It also explains in more detail the experimental plan used to conduct the investigation.  3.1 Enargite Sample Enargite was purchased from the Mineral Resource Company located in California, and was obtained from the Butte Mine in Montana. Pyrite and quartz are naturally associated with the mineral, and visually pyrite and quartz was observed with the black enargite mineral.  Wet grinding of the enargite sample was performed at P R A (Process Research Associates) in Vancouver, B C . Grinding was done wet, and a slurry was returned. This slurry was then filtered and air dried so that dry solid could be added to the respective experiments. Approximately 1 kg of enargite for each particle size was ground to a nominal Pgo of 10, 20, and 37 microns.  60  Chemical analysis of the head samples were performed by Chem Met Consultants Inc. in Vancouver. Atomic Absorption (AA) analysis for copper, iron, arsenic and antimony was performed; sulphur species was also determined.  3.2 Bacteria and Culture Medium The various bacteria cultures for this work were adapted from pre-existing cultures available in the biohydrometallurgy lab at the University of British Columbia.  These cultures  originated from Little Bear Labs in Colorado and were bacteria cultures originally grown on either sphalerite or pyrite. These were used to start the new cultures for the enargite leaching experiments by allowing the bacteria to adapt to enargite; this process is discussed under bacterial culturing.  The three cultures  of bacteria—mesophiles,  moderate  thermophiles, and  extreme  thermophiles—were drawn from and maintained in separate flasks in separate shakers and were therefore kept separate from each other. These cultures consist of groups of bacteria as opposed to a single species. Bacterial speciation was not done for a number of reasons: the analysis was deemed to be very expensive, and over time the composition of the bacterial cultures would change as adaptation to the leach environment occurred.  The medium used for bacterial growth were taken from recipes adapted from those provided with the bacteria; the version used in the culturing and the leaching experiments are shown in Table 3.1.  61  Table 3.1: Nutrient medium composition. Mesophilic Medium 2.0 0.8 0.3 1.0 1  M g S 0 - 7 H 0 (g/L) ( N H ) S 0 (g/L) K H P 0 (g/L) FeS0 -7H 0 (g/L) Mesophile nutrient solution (mL/L) Thermophile nutrient solution (mL/L) pH adjusted to 1.6 by 6 M H S 0 4  4  2  2  4  2  4  4  2  2  Thermophilic Medium 0.8 0.8 0.1 0.5 1  4  The trace nutrient solutions were made in-the lab at the Univeristy of British Columbia; the recipe for the thermophile trace nutrient solution is found in Table 3.2.  This solution  appeared to contain a brown precipitate, and the solution required shaking before the needed amount was withdrawn to compose the nutrient medium.  The mesophile trace nutrient  solution was pink, and the primary change is the addition of E D T A to suppress precipitation of the brown precipitate.  Table 3.2: Thermophile Trace Nutrient Solution Composition Compound MnCl -4H 0 Na B O T0H O ZnS0 -7H 0 CuCl -2H 0 VOS0 -2H 0 CoS0 2  2  4  2  7  2  4  2  2  2  4  2  4  Composition (g/L) 1.8 4.5 0.22 0.05 0.03 0.01  62  3.3  Bacterial Culturing  As discussed previously, elements such as copper and arsenic can be toxic to many bacteria. Before experiments could begin, culturing was required to adapt the bacteria to the conditions that would result from the leaching of enargite.  Section 2.4.4.7 discussed the  adaptation mechanisms that are typically found in bacterial leaching.  For each culture, 2 to 7 grams of enargite was used with addition of a small amount of elemental sulphur (approximately 0.1 to 0.3 g). The amount of enargite in initial cultures was low (about 2 grams) and larger amounts were used in later cultures. Approximately 20 to 25 mL of inoculum as slurry (solid plus liquid from previous shake flask culture) was used with 75 to 80 mL fresh medium. The first inoculum used was taken from the bacterial cultures in the laboratory; successive cultures used inoculum from previous bacterial cultures.  Erlenmeyer flasks (250 mL) with bevelled bottoms were used as bioreactors. The flasks were covered with porous foam lids during experiment (to allow ingress of air with minimum evaporation). Separate rotary shakers at set temperatures of 35°C, 48°C, and 68°C were used to grow the mesophiles, moderate thermophiles, and extreme thermophiles respectively.  The pH and Eh (potential) were monitored during the course of the culturing; these measurements were taken at room temperature.  Potential was measured with respect to  silver/silver chloride (Ag/AgCl) with a Corning Redox Platinum Electrode. Calibration was  63  done in Light's solution. The Light's solution was made in the lab; the composition can be found in Table 3.3. It was made so that the potential was 474 mV versus Ag/AgCl/4M KCI.  Table 3.3: Light's Solution Composition Chemical Fe(NH )2(S04)2-6H 0 Fe(NH )2(S0 )2T2H 0 H S0 4  19.61 g per 500 mL (to make 0.1 M ) 24.11 g per 500 mL (to make 0.1 M ) 28.1 mL (18 M ) per 500 mL or 51.62 g  2  4  4  2  2  4  For the silver/silver chloride reaction [70]: AgCl  (s)  + e »Ag  (s)  + Cr  E° = 0.222 V  [3-1]  Thus, to convert the potentials obtained to potentials versus the standard hydrogen potential, 220 mV were added to the readings. As all potentials were recorded when the solutions were at room temperature, no adjustments in the calculations were needed for temperature.  The pH was measured with a " V W R Scientific" pH probe. Calibration of the probe was conducted using 3 different- solutions buffer solutions of pH values 1.68, 4.00, and 7.00. These solutions were deemed adequate for calibrating the probe to measure pH in weakly acidic solutions.  The bacteria were considered to be active as the potential (Eh) would rise during the culturing for the mesophiles and the moderate thermophiles; for the extreme thermophiles, the potential would increase after a number of days. As discussed previously, some bacteria catalyze the reaction of ferrous (Fe ) to ferric (Fe ); a high potential indicates a larger ferric 2+  3+  to ferrous ratio. Transfers occurred when the potential reached a high level, generally after  64  the potential levelled off. This levelling of the potential is typical when the bacteria cultures have grown exponentially and adapted to the sample and solution in the leach reactor. Seven to ten days was typically when successive transfers would occur. Evaporative losses were also monitored for, and water was added to make up for water lost by this means.  At first, the pH was adjusted when necessary: when the pH was greater than 2, 6 M sulphuric acid would be added until the pH was approximately 1.6. However, it was also noted that this increase in pH was temporary and the pH would begin to drop approximately three days into the experiment. It was then decided that adjusting the pH was not necessary and only caused the p H to become extremely low once leaching had progressed further. Furthermore, this effect seemed to decrease over time as the cultures adapted to the leaching conditions present.  Samples were taken from the earlier bacterial cultures in order to determine the performance of the system.  When it was determined that the bacteria was indeed leaching enargite  (indicated by the presence of copper and arsenic in solution), the cultures were simply maintained with successive transfers every 7 to 10 days.  The cultures were maintained for several months before being used in bacterial leaching experiments.  65  3 . 4 Bacterial Leaching Experiments Bacterial leaching experiments were shake-flask tests modeled after the bacterial culturing methods.  Mesophiles, moderate thermophiles, and extreme thermophiles were used at  temperatures of 35°C, 48°C, and 68°C respectively. The medium used was the same as that used for culturing (refer to Table 3.1). As in culturing, no carbon dioxide was blown into the system, and the shaking action was assumed to be adequate for supplying the required oxygen and carbon dioxide from the atmosphere.  First, a carefully weighed sample (2 g, 3.5 g, 5 g, or 10 g) of natural enargite of a certain particle size (Pgo = 5-10, 15, and 37 microns) was placed in a 250 mL Erlenmeyer flask with a bevelled bottom. Then, 95 mL of medium was added. Finally, inoculation was done with 10 mL of solution from the stock culture.  The stock culture was taken from bacterial  culturing, and allowed to settle in order to only use the liquid for the inoculation. A liquid sample was also taken of this stock culture for chemical analysis.  The pulp densities used in the experiments are described in Table 3.4.  Table 3.4: Pulp Densities used in Bacterial Leaching Experiments Mass of Enargite Added (g) 2 3.5 5 10  Pulp Density (g/L) 19.0 33.3 47.6 95.2  66  During testing, the pH and the potential were measured, and evaporative losses were tracked by weighing the test flasks and comparing the mass to the total mass at the start of the test. It was assumed that most of the mass loss was due to evaporative losses. The difference was made up with deionized water by weight.  Samples were also taken from the experiments approximately once a week. A sample of 5 mL of liquid was taken by a pipette; the sample was then replaced by 5 mL of medium. Records of the subtraction and addition were kept in order to calculate the final mass balance.  Although pH readings were taken, it was found that acid addition to maintain the pH was not necessary, as was discussed with bacterial culturing. Total test length was 36 days. After testing, the tests were vacuum filtered with the filtrate being collected, measured, and analyzed. The remaining solids were washed with 250 mL of deionized water. These were then dried and weighed; the weight of the filter paper (weighed before testing) was subtracted to arrive at the weight of the solids. These solids were then collected for further analysis; the wash water was also sampled for further compositional analysis.  No sterile test was conducted. It would have provided useful information as to what effects could be attributed to the presence of bacteria. However, there were some concerns with the bactericide (thymol) being very volatile, and this bactericide may contaminate other existing cultures and tests in the laboratory.  67  3.5 Analysis of Samples Liquid samples were sent to International Plasma Laboratories (IPL) in Vancouver, BC for 30 element Inductively Coupled Plasma (ICP) analysis. The samples removed during testing as well as the filtrate was diluted by a factor of 5 (5 mL solution with water to make 25 mL of solutions). It was believed that as the four elements of interest (copper, iron, arsenic and antimony) were in higher concentrations, it would introduce negligible error; in fact, for some samples, the copper concentration would exceed the limits of analysis and thus would not be accurate.  Wash solution samples were not diluted as the concentrations of the  elements of interest were already low and the amount of liquid available for sampling was abundant.  Solid samples were sent out for analysis to either International Plasma Laboratory Ltd. (IPL) or Chem Met Consultants Inc., both in Vancouver, BC. Chem Met performed atomic adsorption (AA) analysis some of the solid samples (the head samples plus some of the mesophile and extreme thermophile 10 g tests); sulphur analysis was also performed on those samples. On the rest of the solid samples, a modified acid digestion method followed by ICP analysis was used to determine the solid composition.  Mass balances were based on the head analysis, the composition of the medium and inoculum, the composition of samples taken through the test, the final filtrate and wash analysis, and the final solid analysis. Details on the mass balance calculations can be found in Appendix C.  68  4. Results and Discussion Following is a presentation and discussion of the results of the bioleaching experiments. After the head analysis is discussed, the results from the three different groups of bacteria— mesophiles, moderate thermophiles, and extreme thermophiles—are presented.  The full data collected from these experiments can be found in Appendices D and E.  4.1 Head Analysis The results of the head analysis are shown in Table 4.1. Note for all head samples that most of the sulphur appears as sulphide; there is negligible elemental sulphur and very little sulphur as sulphate.  Table 4.1: Head analysis of the enargite samples used for testing. Particle Size Copper Iron Arsenic (microns, Pso) 31.2 10 11.6 10.5 30.4 15 10.6 10.5 32.4 7.2 12 37  Analysis (weight percent) Antimony Sulphur Total Sulphate Elemental Sulphide (S0 -) (S ) (S°) CS ") 0.55 32.2 0.13 <0.01 32.0 0.55 32.4 O.01 0.01 32.3 0.02 0.39 29.1 <0.01 29.0 2  T  2  4  If it is assumed that all of the arsenic and antimony appears as enargite (Cu3(As, Sb)S4) and all the iron appears as pyrite (FeS2), a rough approximation on the amount of enargite and pyrite in the sample can be generated, as well as the amount of copper that is likely not associated with enargite. Table 4.2 shows the results of such calculations. It can be seen based on these calculations that the samples contain a large amount of enargite  69  (approximately 57 to 64% by weight) with a significant amount of pyrite (approximately 15 to 25% by weight). Visually, the samples were mainly black (enargite) with some grains that appeared to be pyrite and some that appeared to be quartz.  Table 4.2: Estimate of the enargite and pyrite content in the head samples. Particle Size (microns, Pgo) 10 15 37  Enargite (wt. %) (Cu (As, Sb)S ) 57.2 57.2 64.5 3  4  Pyrite (wt. %) (FeS ) 24.9 22.8 15.5 2  Copper not in enargite (% of total copper) 11.6 9.3 3.9  As expected, some of the copper present is likely not associated with enargite. Based on these calculations, i f all the copper not associated with enargite is leached (recalling that enargite is considered to be a very refractory mineral), approximately 4 to 12% copper extraction is to be expected. Of course, these numbers will be higher i f not all of the arsenic and antimony are associated with enargite. It is believed, however, that this gives a good standard to compare with the results from leaching tests.  4.2  Mesophiles  Figure 4.1 shows the pH of the solutions in the bioleaching tests using mesophiles as a function of time. In most cases there was an initial rise in the pH, which indicates at this point that acid consuming reactions were dominating.  Recall that enargite dissolution  reactions that produce elemental sulphur are acid consuming. The pH only rose over 2 in one instance; no acid was used to lower the pH. One possible explanation is that the bacteria that predominantly oxidizes sulphur and sulphur reduced compounds underwent a lag phase at  70  this time. After this short time, the pH dropped throughout the remainder of the test. It is believed that acid producing reactions were dominating for this period. The final pH was generally between 1.1 and 1.4, with it being higher for those experiments with a lower pulp density as there were less solids available to leach and thus produce acid from.  — * — 1 9 g/L  -19 g/L  — * — 1 9 g/L (2)  -19 g/L (2)  — a — 3 3 g/L  -33 g/L  — a — 48 g/L  -48 g/L  —x — 95 g/L  -95 g/L  0  5  10  15  20  25  30  — > - 9 5 g / L (2)  35  0.00  10.00  Time (days)  20.00  30.00  40.00  Time (days)  (a)  (b)  - • — 1 9 g/L - * — 1 9 g/L (2) -B—  33 g/L 48 g/L  -x--95g/L -»-95g/L(2)  5  10  15  20  25  30  35  Time (days)  (c) Figure 4.1: pH versus time for mesophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  71  Figure 4.2 shows the potential as a function of time. The potential rises throughout, although there might be a drop within the first three days of the experiment.  The initial drop in  potential may also indicate a lag phase as discussed with the initial rise in pH. The final potentials are well over 825 mV, with some reaching higher than 900 mV. The potential is controlled by a number of factors, although a very important one is the ferric/ferrous ratio. A high potential may indicate high activity of the iron-oxidizing bacteria present, as they dissolve iron from iron-bearing minerals such as pyrite and oxidize dissolved ferrous iron to ferric.  The copper extraction is shown in Figure 4.3. Note that extraction is most rapid in the first 10 to 15 days, and then it slows. For 10 microns, it is 10 to 15 days; for 15 microns, 10 days; and for 37 microns, less than about 10 days. This may be partially due to copper being leached from minerals other than enargite.  Extractions are greater than 15% but are no  greater than 30%.  72  575 "  1  1  1  .  1  1  r-  0  5  10  15  20  25  30  35  Time (days)  (C)  -  Figure 4.2: Potential versus time of mesophiles, for particle size of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  73  Time (days)  (C)  Figure 4.3: Copper extraction versus time of mesophiles, for particle size of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  In the literature, extractions reported include 17% after 24 days [44], 9% after 550 hours (22.9 days) [8, 11], and 11% after 500 hours (20.8 days) [10].  In the current work,  extractions after approximately 20 days were between 13 and 25%, with most of the extraction values around 20%. The literature extraction values were obtained using much  74  coarser particle sizes (-100 or -200 mesh) than what was used in these experiments. Also, it was noted in this work that the smaller particle sizes in general yielded better extractions than the larger ones.  Although smaller particle sizes may improve the leaching behaviour of  enargite, this improvement is relatively small. It is also expected as smaller particle sizes will yield a greater surface area for leaching.  Figure 4.4 shows a plot of the extraction of iron versus time. Although the amount of iron extracted varies, the amount is greater than 50% and sometimes over 90%. (Those extraction values over 100% result because intermediate extraction values are based on solution assays.) Also note that there is typically a lag period for iron extraction; this may be attributed to a lag period where iron oxidizing bacteria begin to release the iron from the minerals present. Recall that a lag period was noticed with the pH and potential measurements in many cases. It is believed that these high iron extractions may contribute to the high potentials that were observed and discussed previously. Higher iron extractions than copper were also observed in the literature using T. ferrooxidans, a mesophilic bacteria [34]. In these experiments, the high iron extractions may be an indication that pyrite is being leached preferentially to the enargite.  75  100  -19 g/L -19 g/L (2) •  33 g/L  —A—48 g/L --x--95g/L - - » - - 9 5 g/L (2)  5  10  15  20  25  30  35  Time (days)  (c) Figure 4.4: Iron extraction versus time of mesophiles, for particle size of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  Figure 4.5 shows the extraction of arsenic. Arsenic extraction to solution is lower than that for copper. If it is assumed that the literature findings are correct; that is, that copper and arsenic are not leached preferentially; then these results can be explained either by not all the  76  copper associated with enargite (as discussed previously) and or arsenic absorbed in other compounds, possibly with iron oxides that may form and report to the solids.  — • — 1 9 g/L  - 1 9 g/L  — * — 1 9 g/L (2)  - 1 9 g/L (2)  — o — 33 g/L  - 3 3 g/L  — a — 48 g/L  - 4 8 g/L  --x--95g/L  - 9 5 g/L  --»--95g/L(2)  10  15  20  25  40  Time (days)  (a)  (b)  — • — 1 9 g/L — * — 1 9 g/L (2) — Q — 33 g/L &  48 g/L  —x--95g/L - - » — 9 5 g / L (2)  0  5  10  15  20  25  30  35  Time (days)  (c) Figure 4.5: Arsenic extraction versus time of mesophiles, for particle size of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  77  Table 4.3 summarizes the final extraction values for the experiments with the mesophiles. Since extraction values are higher than 4% to 11%, it is believed that enargite was indeed being leached in these experiments.  Table 4.3: Final extraction values for mesophilic bacteria Particle Size (microns, Pgo) 10  15  37  Pulp Density (R/L) 19 19(2) 33 48 95 19 19(2) 33 48 95 95 (2) 19 19(2) 33 48 95 95 (2)  Element, Percent Extraction to Solution Copper Iron Arsenic 24.96 94.85 13.47 24.21 93.17 12.29 25.55 92.04 14.54 23.99 60.13 10.59 26.08 14.14 75.70 22.96 75.48 8.66 20.94 93.04 8.43 24.41 93.45 10.28 20.99 8.44 87.28 27.68 56.40 13.69 26.06 92.94 11.17 15.82 79.22 8.59 22.88 84.10 .8.02 15.98 86.15 8.08 23.20 12.42 65.19 19.12 7.54 39.38 18.40 82.82 10.20  Table 4.4 shows the solid analysis results of the solid residues that result from the experiments, and compares it to the measured head values (shown originally in Table 4.1). Note that the weight ratio of copper to arsenic in pure enargite is 2.54. Although the ratio of copper to arsenic decreases, in general the ratio in the final analysis are not drastically different than those of the measured head, and are no lower than 2.52 (which is close to that of enargite).  Thus, the residues are not enriched with arsenic with respect to copper.  78  Furthermore, i f arsenic were to be leached and re-precipitated, it would most likely be in the form of scorodite or some other iron-arsenic oxide, as has been found in other studies and discussed previously.  The iron, however, shows very high extractions to solution.  Therefore, it is believed that the arsenic leached while leaching the mesophiles is mostly remaining as dissolved arsenic, although some may be precipitated.  Table 4.4: Solid residue analysis for mesophilic bacteria. Particle Size (microns) 10  15  37  Pulp Density (R/L)  (Head) 19 19(2) 33 48 95 (Head) 19 19(2) 33 48 95 95 (2) (Head) 19 19(2) 33 48 95 95 (2)  Element in Residue (wt. %) Copper Iron Arsenic Antimony 31.2 11.6 10.5 0.55 39 0.86 14 0.7 39 14 1.03 0.7 14 38 0.66 0.7 35 6.3 13 0.6 35.2 1.8 13.9 0.67 30.4 10.6 10.5 0.55 36 3.96 13 0.7 39 0.95 14 0.7 39 0.52 14 0.7 14 39 1.91 0.7 34 4.6 13.1 0.69 14 38 0.87 0.7 32.4 7.2 12 0.39 0.4 35 2.25 13 36 2.56 13 0.7 36 1.24 0.4 13 35 5.4 12 0.6 32 4.4 12.7 0.42 36 1.38 13 0.4  Ratio of Cu:As 2.97 2.79 2.79 2.71 2.69 2.53 2.90 2.77 2.79 2.79 2.79 2.60 2.71 2.70 2.69 2.77 2.77 2.92 2.52 2.77  Table 4.5 shows the sulphur analysis for the head samples and for the residues of the 10 g experiments only. It is interesting to note that although there is negligible elemental sulphur in the measured head samples, there is a small but measurable quantity in the residue,  79  although most of the sulphur does remain as sulphide. Thus, it appears that most of the sulphur during leaching with the mesophiles is likely converted to sulphate (as indicated by the acid production given by the pH values throughout the experiment) or some other dissolved intermediate form, with only small amounts of elemental sulphur being formed.  Table 4.5: Sulphur analysis for the 10 g experiments, mesophilic bacteria. Particle Size (microns) 10 15 37  Sulphur Analysis , weight % Sample Head  S 32.2  (S0 ")S 0.13  S° <0.01  S~ 32  Residue Head Residue Head Residue  26.8 32.4 28.2 29.1 27.4  <0.01 <0.01 0.2 0.02 O.01  0.44  26.4  <0.01 0.31 O.01 0.16  32.3 27.7 29 27.3  T  2  4  2  In summary, for the mesophilic bacteria: Copper extractions were no greater than 30%. -  It is believed that enargite has been leached, with much of the arsenic reporting to solution. Smaller particle sizes show a small improvement in the leaching behaviour; this improvement is to be expected as it provides a greater surface area for leaching. Sulphur is being oxidized to sulphate, as indicated by the constantly lowering of pH values throughout the experiment and the sulphur analysis completed for some of the solids.  -  Much of the iron in the other minerals is also being extracted, and as a result of this plus the action of iron oxidizing bacteria, the potential increases throughout the experiment. It is believed that pyrite is being leached preferentially to the enargite.  80  4.3  Moderate Thermophiles  At the beginning of the experiments, there was a rise in the pH for about the first 10 days; this was followed by a drop in the pH. This is also indicative of a lag period, though the rise in pH appears to last longer than that for the mesophiles. The rise in pH is also higher, often reaching higher than 2, but dropping after approximately 5-10 day. As with the mesophilic bacteria, the final p H values (1.1 to 1.5) are lower for higher pulp densities. This can be observed in Figure 4.6.  The potential underwent a short drop at the beginning, and then it continued to rise for the rest of the experiments, as can be seen in Figure 4.7. As discussed previously, this drop may indicate a lag time where the bacteria are adapting to the new environment. This drop is also very distinct in these experiments.  The final potentials are lower than that for the  mesophiles: they are normally between 750 and 870 mV.  81  82  880  - • — 1 9 g/L  -19 g/L  - B — 33 g/L  - 33 g/L  - A — 4 8 g/L  -48 g/L  -x--95g/L  -95 g/L  580 0  5  10  15  20  25  30  35  0  5  10  15  20  Time (days)  Time (days)  (a)  (b)  25  30  35  - • — 1 9 g/L - o — 33 g/L - a — 4 8 g/L - x - - 9 5 g/L  10  15  20  25  30  35  Time (days)  (c) Figure 4.7: Potential versus time for moderate thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  Copper extraction also slows down after the first 10 to 15 days as with the mesophiles (Figure 4.8). The extractions then continue to increase. The final extraction values of 34% to 60% are higher than those found for the mesophiles. Note that the 95 g/L experiments showed the worst extraction in all cases, and that the final extractions from the other experiments were very similar.  Unfortunately, no literature values were found for the  83  bioleaching of enargite with moderately thermophilic bacteria, and in general the role of such bacteria is not reported on extensively. It is sufficient to note, however, that there is a great improvement in leaching by using such bacteria as compared to the mesophiles. As well, there is a greater improvement in the leaching behaviour as particle size increases than what was observed in the mesophiles.  — • — 1 9 g/L — a — 33 g/L a  48 g/L  --x--95g/L  Time (days)  (C)  Figure 4.8: Copper extraction versus time for moderate thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  84  Iron extraction also shows a 10-15 day lag time with slow extractions, as seen in Figure 4.9. With the exception of the 95 g/L experiments, final iron extractions were very high, being over 60% in all cases and over 80% for the smaller particle sizes.  With the 95 g/L  experiments, iron extractions were very low. Interestingly, the final potentials were also lower for the 95 g/L experiments as well (refer to Figure 4.6). It appears that, as with the mesophiles, most of the pyrite is being leached, and it appears that pyrite is leached preferentially to the enargite.  Arsenic extractions again were also much less than copper (Figure 4.10). Again, extractions for the 95 g/L experiments were lower than those of the other experiments with lower pulp densities.  85  — • — 1 9 g/L — o — 33 g/L —a—48 g/L —x — 95 g/L  Time (days)  '  -  (c)  Figure 4.9: Iron extraction versus time for moderate thermophiles, with particle sizes of Pso equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  86  40  5  10  15  20  25  30  - » — 1 9 g/L  - • — 1 9 g/L  - a — 33 g/L - A — 4 8 g/L -x--95g/L  - a — 33 g/L 48 g/L - x —95 g/L  35  5  Time (days)  10  15  20  25  30  35  Time (days)  (a)  (b) 40 35 30 - • — 1 9 g/L - a — 3 3 g/L -6—48 g/L - X - - 9 5 g/L  5  10  15  20  25  30  35  Time (days)  (c) Figure 4.10: Arsenic extraction versus time for moderate thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  Table 4.6 summarizes the extraction data for the moderate thermophiles.  Note the  similarities between the 2, 3.5, and 5 g experiments that were discussed previously; also note how the 10 g experiments showed lower extractions than those of the other experiments.  87  Also note that the extractions of all the elements are generally higher than for the mesophiles (refer to Table 4.3).  Table 4.6: Final extraction values for moderate thermophilic bacteria. Particle Size (microns, Pso) 10  15  37  Pulp Density (g/L) 19 33 45 95 19 33 45 95 19 33 45 95  Element, Percent Extraction to Solution Copper Iron Arsenic 60.15 34.14 88.91 59.79 92.06 36.83 58.36 84.08 37.80 50.93 30.42 27.37 48.51 96.71 23.30 46.94 93.71 25.05 47.75 83.87 26.63 41.94 49.47 19.41 98.34 40.51 16.73 40.23 78.08 17.05 39.74 67.39 17.39 34.07 13.54 24.08  Table 4.7 compares the solid residue analysis to that of the measured head for each respective particle size. Again, the ratio of copper to arsenic is close to or higher than 2.54, which is the mass ratio of copper to arsenic in enargite. As with the mesophiles, much of the arsenic that is leached is in solution, although some may have re-precipitated with iron. However, with the very high iron extractions in some cases, it is likely that most of the arsenic leached is indeed in solution.  88  Table 4.7: Solid residue mass analysis for moderate thermophilic bacteria. Particle Size (microns) 10  15  37  Pulp Density (g/L) (Head) 19 33 48 95 (Head) 19 33 48 95 (Head) 19 33 48 95  Copper 31.2 32 33 32 27 30.4 36 36 34 32 32.4 33 32 32 30  Element Iron Arsenic 11.6 10.5 12 2.06 12 1.71 12 3.23 11 11 10.6 10.5 1.06 13 0.94 13 12 2.87 7.2 12 7.2 12 0.80 12 2.22 12 2.92 12 6.1 12  Antimony 0.55 0.9 0.7 0.6 0.6 0.55 0.8 0.8 0.7 0.6 0.39 0.5 0.5 0.4 0.4  Ratio of Cu:As 2.97 2.67 2.75 2.67 2.45 2.90 2.77 2.77 2.83 2.67 2.70 2.75 2.67 2.67 2.50  In summary, for the moderately thermophilic bacteria: The behaviour of enargite with moderately thermophilic bacterial leaching solutions parallels that of leaching in mesophilic solutions, with generally higher extractions overall using moderate thermophiles. It is believed that enargite is being leached, with copper extractions of 34-60% being realized. This is an improvement over those for the mesophiles. Iron extractions were much higher than that of the mesophilic bacteria, sometimes nearing completion. It is believed that pyrite is being leached preferentially to the enargite in these experiments. -  Arsenic extractions were also higher than that found in the mesophiles. It is believed that much of the leached arsenic reports to solution.  89  Sulphur is being oxidized to sulphate, as indicated by the pH values dropping throughout the experiments. -  Between the various pulp densities, the final results were very similar for all except for the 95 g/L experiment, which had much lower extractions in all cases.  4.4  Extreme Thermophiles  In general, the trend for the pH tends to follow that of the mesophiles and the moderate thermophiles (Figure 4.11), and decreases continuously throughout the tests. Final values, however, are slightly lower than those found for the mesophiles and the moderate thermophiles.  The potential tends to behave differently than that of the other bacteria (Figure 4.12). Examining the smallest particle size (Figure 4.12a), for the 95 g/L experiment, the potential remains under 670 mV throughout the experiment. For the 19 g/L experiments, however, the potential remains low for a time and then rises very quickly to over 800 mV. Variations on these responses were observed for the other experiments.  In general, for the lower pulp  densities, the potential will remain low for a significant amount of time (10 to 20 days), then it may begin to rise more or less quickly to a higher potential. For the higher pulp densities, the potential may remain low throughout the experiment. This trend is more pronounced with the lower particle size but can still be distinguished with the larger one. This type of behaviour is much different than with the mesophiles and moderate thermophiles, where there is typically a small drop in potential in the first couple days, after which the potential continuously increases.  90  — • — 1 9 g/L  - 1 9 g/L  — » — 1 9 g / L (2)  - 1 9 g/L (2)  33 g/L  - 3 3 g/L  — A — 4 8 g/L  - 4 8 g/L  --x--95g/L  - 9 5 g/L  — e —  0  5  10  15  20  25  30  35  0  Time (days)  5  10  15  20  25  30  35  Time (days)  (a)  (b)  - 1 9 g/L - 1 9 g/L (2) - 3 3 g/L - 4 8 g/L - 9 5 g/L  1.00 0.00  10.00  20.00  30.00  Time (days)  (c) Figure 4.11: pH versus time for extreme thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  91  580 -I 0  .  1  10  20  :  r30  Time (days)  (c) Figure 4.12: Potential versus time for extreme thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  92  The copper extraction trends are much different from those found in previous experiments, as shown in Figure 4.13. For the smallest particle size, the extraction is just under 100% for the 19 g/L and 33 g/L experiments, and in fact is near completion after approximately 20 days. However, for the 48 g/L and 95 g/L experiments, the extraction of copper remains low and never rises above 40%. For the other particle sizes, the results are more spread out; however, it is clear that the lower pulp densities leach much better than the higher pulp densities. This conclusion is consistent with that found in the literature: one source, using stirred reactor tests with Sulfolobus B C , found that the extraction was a strong function of pulp density [47]. It was believed that since Sulfolobus B C is an archaebacteria and therefore lacks a cellular wall, the abrasive effect of the mineral had an adverse effect, especially at higher pulp densities.  One literature source reported 52% extraction of enargite with Sulfolobus B C with 100/+150 mesh material after 552 hours (23 days) [9]. Clearly, the current work is an improvement, with almost complete extraction in some cases after approximately 20 days. A different source reports up to 90% extraction after 300 hours (12.5 days) [47]; however, as the material also contained a large amount of other copper bearing minerals such as covellite, chalcopyrite, and chalcocite, it is difficult to compare with the current work.  93  100 -19 g/L -19 g/L (2) — o — 33 g/L  - • — 1 9 g/L  60  —a—48 g/L  - * — 1 9 g/L (2) -B—  --x--95g/L  33 g/L  —•—19 g/L  - A — 48 g/L  40  - * — 1 9 g/L (2)  - x —95 g/L  —o—33 g/L - A — 4 8 g/L  20  -x--95g/L  0  5  10  15  20  25  30  35  0  Time (days)  5  10  15  20  25  30  35  Time (days)  (a)  (b) 100  - • — 1 9 g/L - * — 1 9 g/L (2) - a — 33 g/L - a — 4 8 g/L -x--95g/L  0  5  10  15  20  25  30  35  Time (days)  (c) Figure 4.13: Copper extraction versus time for extreme thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  Iron extractions are shown in Figure 4.14. Clearly, iron extraction is much lower for the extreme thermophiles than for the other bacteria, and it is never above 30%. It is interesting to note that this is true even for those experiments that reach potentials over 820 mV. It was noted for the mesophiles and the moderate thermophiles that pyrite is leached preferentially  94  to enargite. In this case, there are two possible explanations for the fate of pyrite: either pyrite is not leached preferentially to enargite, or the iron that is leached from the pyrite reports to the solids as a precipitate.  — » — 1 9 g/L — * — 1 9 g/L (2) — o — 33 g/L ^ a — 4 8 g/L --x--95g/L  0  5  10  15  20  25  30  35  Time (days)  (c) Figure 4.14: Iron extraction versus time for extreme thermophiles, with particle sizes of Pso equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  95  Arsenic extractions are also much lower for the extreme thermophiles than for other bacteria (Figure 4.15). Final extractions to the liquid are never above 10%. Note that in many cases the extraction of arsenic over time actually decreases after an initial increase.  Table 4.8 summarizes the extraction data for the extreme thermophiles. Note that, as discussed previously, copper extractions are very high for low pulp densities, and that iron and arsenic extractions are very low. Note that some iron extractions are also negative. This is reasonable because iron is entering the system through the medium (refer to Table 3.1); despite the negative extractions, the solution composition of iron is not zero. This type of extraction also seems to suggest that iron is precipitating to a solid form.  96  30  30  25  25  g  Extr:  c 20 o B  — « — 1 9 g/L — * — 1 9 g/L (2) — o — 33 g/L  15  —a—48 g/L  seni  u  --x--95g/L  10  < 5 0 0  5  10  15  20  25  30  35  5  Time (days)  10  15  20  25  30  35  Time (days)  (a)  (b)  - • — 1 9 g/L - * - - 1 9 g / L (2) - a — 33 g/L  -fi— 48 g/L - X - - 9 5 g/L  10  15  20  25  Time (days)  (C)  Figure 4.15: Arsenic extraction versus time for extreme thermophiles, with particle sizes of Pgo equals (a) 10 microns, (b) 15 microns and (c) 37 microns.  97  Table 4.8: Final extraction values for extreme thermophilic bacteria Particle Size (microns, Pso) 10  15  37  Pulp Density (g/L) 19 19(2) 33 48 95 19 19(2) 33 48 . 95 19 19(2) 33 48 95  Element, Percent Extraction to Solution Copper Iron Arsenic 1.64 99.31 22.01 99.12 26.56 1.17 24.92 99.13 1.36 38.05 15.44 1.87 37.09 13.82 1.73 7.34 1.32 97.83 95.15 17.89 2.49 86.43 3.71 4.10 11.44 43.98 1.98 28.15 8.79 0.89 4.11 93.19 -24.77 84.94 14.67 3.08 63.82 -8.24 7.27 51.19 15.29 6.07 29.10 -1.93 3.09  98  Table 4.9 summarizes the solid mass residue analysis. For lower pulp densities, there is almost no copper left in the solid residue, and almost complete extraction for the copper. Arsenic, on the other hand, does not appear to report to the liquid but tends to remain with the solids. Iron extraction is also much lower. It is likely that the arsenic, once leached to solution, re-precipitates with iron to form an iron-arsenic oxide, which reports to the residue. The ratio of copper to arsenic in Table 4.9 shows that the residues are enriched with arsenic with respect to copper, which supports this hypothesis.  Table 4.9: Solid residue mass analysis for extreme thermophilic bacteria. Particle Size (microns) 10  15  37  Pulp Density (g/L) (Head) 19 19(2) 33 48 95 (Head) 19 19(2) 33 48 95 (Head) 19 19(2) 33 48 95  Copper 31.2 0.53 0.62 0.63 26 25.6 30.4 1.53 3.4 8.6 25 28 32.4 4.4 10 18 23 26.8  Element Iron Arsenic 11.6 10.5 17 20 21 18 21 18 12 13 11.6 13.8 10.6 10.5 16 16 18 19 18 17 12 13 11.4 12.8 7.2 12 14 18 17 16 11 15 13 14 13.4 8.6  Antimony 0.55 0.5 0.4 0.8 0.6 0.62 0.55 0.6 0.8 0.9 0.6 0.65 0.39 0.6 0.8 0.5 0.6 0.44  Ratio of Cu:As 2.97 0.03 0.03 0.03 2.00 1.86 2.90 0.10 0.18 0.51 1.92 2.19 2.70 0.24 0.63 1.20 1.64 2.00  99  Table 4.10 shows the sulphur analysis for the residues of the 95 g/L experiments compared to the measured head.  It appears that elemental sulphur is not formed; the sulphur that is  oxidized reports to the solution, likely as sulphate (as indicated by the low pH values due to acid formation) or as some other intermediate sulphur compound.  Table 4.10: Sulphur analysis for 95 g/L experiments, extreme thermophilic bacteria. Particle Size 10 15 37  Sulphur Analysis , weight % Sample Head Residue Head Residue Head Residue  S 32.2 27.1 32.4 29.5 29.1 25.9 T  (S0 ")S 0.13 0.05 <0.01 0.21 0.02 0.01 2  4  S° O.01 <0.01 <0.01 <0.01 O.01 <0.01  S" 32.0 27.0 32.3 29.2 29.0 25.9 2  100  In summary, for the extreme thermophiles: -  The copper extraction behaviour is a strong function of pulp density, with little leaching occurring at higher pulp densities and almost complete extraction at the lower pulp densities. The extraction of iron and arsenic are very low. It is believed that the arsenic is reprecipitating with iron to the solid residue, possibly as an iron-arsenic oxide. The sulphur is being oxidized to sulphate, as indicated by the decrease in pH over time and the sulphur analysis of some of the solids, which did not detect elemental sulphur remaining in the residue.  4.5  Discussion and S u m m a r y  It appears that enargite is viable to bioleaching under certain circumstances.  The ideal  conditions for bioleaching for maximum copper extraction appears to be the use of extreme thermophiles, low pulp densities, and long residence times.  Overall, mesophile behaviour is better understood based on the information in the literature. It was observed that smaller particle sizes cause a slight improvement in the leaching of enargite.  This improvement is expected as a decrease in particle size increases the area  available for leaching. Furthermore, the high iron extractions and high potentials can be explained by the action of iron oxidizing bacteria; the low pH values and low amounts of elemental sulphur in the residue can be explained by the action of sulphur oxidizing bacteria. The behaviour then is reasonable compared to what has been observed in the literature. Furthermore, it appears that pyrite is leached preferentially to enargite.  101  Moderate thermophile behaviour is much less understood; however, the trends in the data parallels that found in the mesophiles. It also appears that pyrite is leached preferentially to the enargite.  Extreme thermophiles, though investigated to some degree, are also not well understood. In this case, it is unclear whether enargite is leached preferentially to the pyrite, or i f the iron from pyrite is precipitated from solution and reports to the solids.  The fact that iron  extractions are low seems to indicate that iron is likely precipitating into the solids. The extraction of arsenic is also much lower, implying that arsenic does report to the solids. It is possible that arsenic is precipitating with the iron, based on the data available. Finally, for the extreme thermophiles, copper extraction is very sensitive to pulp density, with lower pulp densities showing almost complete extraction and higher pulp densities showing much lower extraction values. It is believed that, as noted in the literature, at higher pulp densities the abrasion effect on the cell wall may cause shearing of the cells, as some species of extreme thermophiles have a weak cell wall [47].  102  5. Conclusions and Recommendations for Future Work 5.1  Conclusions  5.1.1 Mesophilic Bacteria It is believed that copper has been leached from enargite, with copper extractions no greater than 30% after 36 days.  These results are an improvement over those reported in the  literature; this is attributed to the smaller particle sizes used in the current study. Thus, it appears that smaller particle sizes do improve the leaching behaviour of enargite, although this effect is small. The increased surface area available for leaching that results from a smaller particle size is believed to be the cause of this. Arsenic was also extracted from enargite, with much of it reporting to solution.  Based on the high iron extractions, it is believed that pyrite it preferentially dissolved over enargite in the mesophile leaching solutions. High potentials are realized in the mesophile leach solutions; the action of iron oxidizing bacteria on the dissolution of pyrite and the conversion of ferrous iron to ferric is believed to be the cause. The fact that iron extractions are higher than copper extractions is not unusual; this has also been reported in the literature [34].  Finally, sulphur from the sulphide minerals leached is being oxidized to sulphate, as indicated by the constant drop in pH values throughout the experiment and by the sulphur analysis done on some of the solids. This seems to indicate the action of sulphur oxidizing bacteria within the leach solutions.  103  5.1.2 Moderate Thermophiles Copper was also being leached from the enargite present, and copper extractions of 34-60% were realized.  This was an improvement over the values obtained by the mesophiles.  Arsenic extractions were also higher than those for the mesophiles.  Furthermore, iron  extractions were much higher than that of the mesophilic bacteria, sometimes nearing completion. Again, it is believed that pyrite is leached preferentially to the enargite. Finally, sulphur is being oxidized to sulphate, as indicated by the pH values dropping throughout the experiments.  Overall, the behaviour of the moderate thermophiles modeled that of the mesophiles, although the final extraction values were higher. Furthermore, comparing the various pulp densities used, the final results were very similar for all except for the 95 g/L experiments, which had much lower extractions in all cases.  5.1.3 Extreme Thermophiles The extraction behaviour is strongly dependent on pulp density, with little leaching occurring at higher pulp densities and almost complete extraction of copper at the lower pulp densities. It is believed that at higher pulp densities, the abrasion of the mineral on the weak cell walls may be shearing the cells and thus reducing the bacteria available for leaching [47].  Furthermore, the extraction of iron and arsenic are very low. It is believed that the arsenic is re-precipitating with iron to form an iron-arsenic oxide in the solid residue, although further  104  study is required in order to confirm this hypothesis. Finally, the sulphur is being oxidized to sulphate, as indicated by the decrease in pH over time and by the sulphur analysis conducted on some of the leach residues.  5.1.4  Overall Conclusions  Enargite can be leached via bacterial leaching, and finer grinds yield better results. This effect is to a smaller degree for the mesophiles and to a greater degree for the thermophiles.  The behaviour of the mesophilic bacteria appears to correspond well with what is understood and reported on in the literature. In the case of the thermophiles, their behaviour has not been researched well and therefore not well understood.  In the case of the mesophiles and the moderate thermophiles, pyrite is clearly leached preferentially to the enargite. The leaching behaviour for these do not appear to be highly dependent on pulp density, although a slight effect was noted in the moderate thermophiles.  The use of extreme thermophiles can greatly improve extraction and may aid in arsenic removal as arsenic tends to appear in the residue. However, the leaching of copper from enargite using extreme thermophiles is highly dependent on pulp density.  At low pulp  density, almost complete copper extractions are realized; at high pulp densities, abrasion reduces the bacteria available for leaching.  105  5.2 Future Work 5.2.1 Bioleaching The next step in the work that has been done is possibly tank reactor work to scale up the bioleaching experiments and to determine i f it is viable to leach enargite on a larger scale. There are some disadvantages that may be demonstrated by such tests. First, the residence times are relatively long. Secondly, at low pulp densities, larger tank sizes are required for a given throughput; as well, more of the copper is tied up in working capital with the large volumes of leach solution present. Finally, fine grinding is considered to be very expensive in many cases.  It should be noted, however, that as more refractory minerals are being  considered for leaching, more extreme methods are required to remove the elements of interest, and despite the disadvantages, leaching may be deemed viable.  Currently, although extreme thermophiles have the potential for successful bioleaching, they are poorly researched and not well understood. Unfortunately, this has been a hurdle towards their large-scale use, and more work in understanding their mechanisms and behaviours would prove to be very useful.  In the current work, kinetics was not investigated as the purpose was to determine i f enargite could be leached, as well as to provide clues to further investigations. More careful kinetic studies may be necessary to confirm the literature assertion that the leaching reactions are surface reaction controlled. Furthermore, further study into the products of the reactions will be necessary, possibly using x-ray diffraction to confirm the various compounds present. Finally, the fact that pyrite is leached preferentially to enargite in the mesophiles and  106  moderate thermophiles seems to indicate that an electrochemical mechanism may be involved, since electrochemically one mineral may passivate while the other is leached. The fact that enargite is being leached at a lower potential in the extreme thermophiles than for the mesophiles and moderate thermophiles also seems to indicate that this is an area for which further study may be warranted.  5.2.2 Atmospheric Leaching As can be seen from the current results, fine grinding can improve leaching behaviour. Other sources have proposed such a procedure for sulphate leaching systems. Further study into the leaching of enargite by such systems would be very useful.  As discussed previously, chloride solutions have been proposed for the leaching of various refractory minerals, although it has not been tested specifically on enargite. Furthermore, in chloride processing, arsenic and antimony will dissolve.  The removal of arsenic and  antimony from such solutions for disposal must be addressed as well.  5.2.3 Pressure Leaching The behaviour of enargite in pressure leaching systems has not been well examined. To date, one paper examines the total pressure oxidation of an enargite concentrate, with copper extractions greater than 90% [42].  107  A number of industrial systems have been found to be effective in the pressure leaching of chalcopyrite (which is considered to be less refractory than enargite). Some of these systems are as follows: The Activox process: fine grinding and pressure leaching C E S L copper process: chloride-activated pressure leaching in a sulphate system -  Dynatec process: Leaching at 150°C [33, 36], oxygen overpressure, coal/carbon as a surfactant to disperse the elemental sulphur [33, 36].  -  The Anglo American/University of British Columbia process:  Leaching at 150°C  after fine grinding to 5 - 10 um particle size with the addition of sulphur dispersing surfactants such as lignin sulfonate. Total Pressure Oxidation Process:  Temperatures  of 200-220°C with oxygen  overpressure [42].  It is hoped that such systems may be successful in the leaching of enargite.  It should be  remembered, however, that enargite is likely more refractory than chalcopyrite for different reasons: the literature has hinted that enargite leaching is controlled by a surface reaction [2, 44], while chalcopyrite leaching is controlled by a passivating layer [28, 30, 33]. Despite this, tests based on these systems may prove useful in determining i f enargite can be leached successfully in a pressure leaching system.  5.2.4  Arsenic Removal  One issue during the processing of enargite is the fate of nuisance elements such as arsenic and antimony. In hydrometallurgy, arsenic can report either to the solution or to the solid  108  residue. It is also possible that, even though arsenic reports to the residue, the residual in solution requires further treatment for safe disposal.  There has been some research into the fate of arsenic in hydrometallurgical processes, but this area has been limited. Furthermore, since the thermodynamic data for arsenic species has gaps in it, the prediction of the species present is difficult. More work may be required in this area in order to allow for the processing of minerals such as enargite.  109  6. References 1.  S. Gajam and S. 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Ballester (Eds.), Proceedings of st  the International Biohydrometallurgy Symposium IBS '99, San Lorenzo de E l Escorial, Madrid, Spain, June 20-23, 1999, pp. 301-308. 45.  T. Havlik and R. Kammel, "Procedure  for Selective Copper Recovery from  Tetrahedrite", Metall, Vol 54 No. 1-2, February 2000, pp. 26-29. 46.  D. Fornasiero, D. Fullston, C. L i , and J. Ralston, "Separation of enargite and tennantite from non-arsenic copper sulfide minerals by selective oxidation or dissolution", Int. J. Miner. Process. 61 (2001) 109-119.  47.  Blanca Escobar, Jesus M . Casas, Jorge Mamani and Ricardo Badilla-Ohlbaum, "Bioleaching of a Copper Concentrate with Sulfolobus B C " , Biohydrometallurgical Technologies, Volume 1:  Bioleaching Processes, A . E . Torma, J.E. Wey, V.I.  Lakshamanan (Eds.)Proceeding of International  Biohydrometallurgy Symposium,  Jackson Hole, Wyoming, U S A , August 22-25, 1993, pp.195-204.  116  48.  Corale L . Brierley and James A . Brierley, "Copper bioleaching:  state-of-the-art",  Proceedings of COPPER 99-COBRE 99 International Conference, Volume III— Hydrometallurgy of Copper, S.K. Young, D.B. Dreisinger, R.P Hackl, and D.G. Dixon (Ed.), October 10-13, 1999, Phoenix, Arizona, U S A , pp. 59-68. 49.  Klaus Bosecker, "Bioleaching:  metal solubilization by microorganisms", FEMS  Microbiology Reviews 20 (1997) 591 -604. 50.  Marja Riekkola-Vanhanen and Seppo Heimala, "Electrochemical Control in the Biological Leaching of Sulfidic Ores", Biohydrometallurgical Technologies, Volume 1: Bioleaching Processes, A.E. Torma, J.E. Wey, V.I. Lakshamanan (Eds.)Proceeding of International Biohydrometallurgy Symposium, Jackson Hole, Wyoming, U S A , August 22-25, 1993, pp. 561-570.  51.  G.S. Hansford and T. Vargas, "Chemical and electrochemical basis of bioleaching processes", Hydrometallurgy 59 (2001) 135-145.  52.  Helmut Tributsch, "Direct versus indirect bioleaching", Hydrometallurgy 59 (2001) 177-185.  53.  H . N . 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Silverman and Donald G. Lundgren, "Studies on the Chemoautotropic Iron Bacterium Ferrobacillus Ferrooxidans I. A n Improved Medium and a Harvesting Procedure for Securing High Cell Yields", Journal of Bacteriology, Vol. 77, 1959, pp.  642-647. 61.  J.E. Dutrizac and R.J.C. MacDonald, "Ferric Ion as a Leaching Medium", Minerals Sci. Engng, Vol. 6, No. 2, April 1974, pp. 59-100.  62.  G. Rossi, "The design of bioreactors", Hydrometallurgy 59 (2001) 217-231.  63.  P. Balaz, "Mechanical Activation in Technology of Metals Extraction", Metall, V o l . 54, April 2000, pp. 190-195.  64.  M . A . Jordan, S. McGinness and C V . Phillips, "Acidophilic Bacteria—Their Potential Mining and Environmental Applications", Minerals Engineering, Vol. 9, No. 2, 1996,  pp. 169-181. 65.  P. Velasquez, J.R. Ramos-Barrado, R. Cordova and D. Leinen, " X P S analysis of an electrochemically modified electrode surface of natural enargite", Surf. Interface Anal.  30 (2000) 149-153.  118  66.  R. Poulin  and  R.W. Lawrence,  "Economic  and  Environmental  Niches  of  Biohydrometallurgy", Minerals Engineering Vol. 9 No. 8, 1996, pp. 799-810. 67.  J6rg Matschullat, "Arsenic in the geosphere—a review", The Science of the Total Environment 249 (2000) 297-312.  68.  Henry L . Ehrlich, "Past, present and future of biohydrometallurgy," Hydrometallurgy 59 (2001) 127-134.  69.  R.P. Hackl, D.B. Dreisinger, E. Peters, and J.A. King, "Passivation of chalcopyrite during oxidative leaching in sulfate media", Hydrometallurgy 39 (1995) 25-48  70.  Daniel C. Harris, Quantitative Chemical Analysis. 3  rd  Edition, W.H. Freeman and  Company, 1991, p. AP41.  119  Appendix A: Enargite Leaching Reactions Reactions for enargite leaching have been derived based on a number of sources [41, 57]. What follows is a list of the chemical reactions that may occur during the leaching of enargite. Oxygen (O2) and ferric iron (Fe ) are present as the oxidizing agents in these 3+  examples.  In the following reactions: •  Enargite as C u 3 ( A s , Sb)S4  •  Copper as C u  •  Sulphur as S° or SO4 "  •  Arsenic (III) as A s O or  •  Arsenic (V) as  •  Antimony (III) as SbO or H S b 0  •  Antimony (V) as S b 0  •  Oxidizing agents are 0 and F e  •  H and H 2 O are also present  2 +  2  +  H2ASO4"  HASO2  or  H3ASO4  +  + 2  2  or Sb0 " 3  3+  2  +  For Arsenic (III) species: If oxygen is the oxidant: Cu AsS +y 0 3  A  A  +y H S0 ->3CuS0 +/ (AsO) SO  2  2  2  4  Cu AsS + %0 +y H 0->3CuSO  4  3  3  A  2  2  2  A  2  2  +4S°+y H 0  A  + y (AsO) SO  2  2  2  A  +y H SO 2  2  A  2  [Al] [A2]  120  Cu AsS +%0 + 3H S0 -> 3CuS0 + HAs0 + 4S° + / H 0  [A3]  Cu AsS + % O +y H 0 -» 3CuS0 + HAs0 + H S0  [A4]  5  3  4  2  2  4  4  2  2  2  3  i  a  4  2  2  4  2  2  4  If ferric iron is the oxidant: Cu AsS + %Fe (S0 ) 3  4  2  4  +H0  3  2  [A5]  -> 3CuS0 + Y (AsO) S0 + 4S° + H S0 + 9FeS0 4  2  2  4  2  4  4  Cu AsS + % Fe (S0 ) + \lH 0 3  3  4  2  4  3  2  -> 3CuS0 +y (AsO) S0 4  2  2  Cu AsS + %Fe (S0 ) 3  4  2  4  4  [A6]  + \1H S0 + 33FeS0 2  4  4  + 2H 0  3  2  [A7]  -> 3CuS0 + HAs0 + 4S° + y H S0 + 9FeS0 4  2  2  Cu AsS + ^y Fe (S0 ) 3  4  2  2  4  2  4  4  + \SH 0  3  2  [A8]  -> 3CuS0 + HAsQ + 4S0 ~ + %H S0 + 33FeS0 2  4  2  3  4  2  4  4  For Arsenic (V) species: If oxygen is the oxidant: Cu AsS +%0 + 3H S0 3  4  2  2  4  3CuS0 + H As0 + 4S° + y H 0 4  3  4  2  Cu AsS + y 0 +y H 0^> 3CuS0 + H As0 + H S0 i  3  4  4  2  2  2  4  3  4  2  4  2  [A9] [A10]  If ferric iron is the oxidant: Cu AsS + %Fe {S0 ) 3  4  2  4  + 4H 0  3  2  [All]  -> 3CuS0 + H As0 +4S°+y H S0 +1 \FeS0 4  3  4  2  2  4  4  121  Cu AsS + / Fe (S0 ) + 20H O 35  3  4  2  2  4  3  2  -> 3CuS0 + H As0 4  3  + % H S0  4  2  [A12]  + 35FeSO  4  A  For Antimony (III) species: If oxygen is the oxidant: Cu SbS +%0 +y H S0 3  4  2  2  Cu ASbS + y 0 3  4  4  2  -> 3CuSO + y (SbO) S0  4  A  +y H 0  2  2  4  2  2  Cu SbS +iy 0 3  4  4  4  2  + 4S° + y H 0  4  2  2  2  [Al3]  2  +y H S0  4  2  2  [A14]  4  ->3CuS0 + HSb0 +4S° + / H 0  [Al5]  5  4  4  +y H 0^>  2  2  -> 3CuS0 +y (SbO) S0  2  Cu SbS +%0 + 3H S0 3  2  2  2  2  3CuS0 + HSb0 + H S0  2  4  2  2  [ A l 6]  4  If ferric iron is the oxidant: Cu SbS + % Fe (S0 ) 3  4  2  4  + H0  3  2  -> 3CuS0 + y (SbO) S0 + 4S° + H S0 4  2  2  4  Cu SbS + %Fe (S0 ) 3  4  2  4  2  3  4  2  4  [A17]  + 9FeS0  4  2  2  Cu SbS +%Fe (S0 )  4  +\1H 0  3  -> 3CuS0 +y (SbO) S0 4  2  +17 H S0  4  2  [A18]  + 33FeS0  4  4  + 2H 0  3  2  -->3CuSO +HSbO +4S +y H S0 +9FeS0 0  4  2  2  2  4  4  Cu SbS + K Fe (S0 ) + 1 8 # 0 -> 3CuS0 + HSb0 + % H S0 3  3  4  2  4  3  2  4  2  2  4  + 33FeS0  4  [A20]  122  For Antimony (V) species: If oxygen is the oxidant: Cu SbS + / 0 + 3H S0 -> 3CuS0 + HSb0 +4S° +  /H0  u  3  4  4  2  2  4  4  [A21 ]  5  3  2  2  Cu SbS +iy 0 +y H 0^> 3Cu + HSb0 + H S0  [A22]  2+  3  4  4  2  2  2  3  Cu SbS + A0 +y H S0 4  2  2  2  4  ->3CuS0 + y (Sb0 ) S0 +4S°  n  3  2  4  4  2  2 2  +  4  AH 0  [A23]  7  2  Cu SbS + y 0 +y H 0^> 3CuS0 + (Sb0 ) SO + y H S0  [A24]  i  3  4  4  2  2  2  4  2  2  A  2  2  4  If ferric iron is the oxidant: Cu SbS + y Fe (S0 )  + 3H 0  u  3  4  2  2  4  3  2  [A25]  3CuS0 + HSbQ + 4S° + 5H S0 +1 \FeS0 4  3  2  Cu SbS +y Fe (S0 ) 3  4  2  2  4  4  4  4  +\9H O-+3CuS0  3  z  CwSZ>S + % FeJS0 ) 3  4  +HSb0 +%H S0  4  3  2  4  +35FeS0 [A26] 4  + 2H 0  3  2  3CuS0 + y (Sb0 ) S0 + 4S° + 2H S0 +1 \FeS0 4  2  Cu AsS + % Fe (S0  2  3  4  2  4  2  4  2  4  4  ) +lSH 0 3  2  -> 3CuS0 + y (Sb0 ) S0 +1SH S0 + 35FeS0 4  2  2  2  4  2  4  4  The reactions where oxygen acts as the oxidant are likely slower than those where ferric iron acts as the oxidant, as is the case with the other minerals discussed.  123  Appendix B: Trace Nutrient Solution Analysis Table B. 1 contains the analysis of the trace nutrient solutions used for the mesophiles and the thermophiles. After diluting a sample of the solution by a factor of 5, the chemical analysis was determined by International Plasma Laboratories (IPL) in Vancouver, B C using 30 element Inductively Coupled Plasma (ICP) analysis.  Table B. 1: Chemical Analysis of the Trace Nutrient Solutions Element Present Aluminum (Al) Arsenic (As) Bismuth (Bi) Calcium (Ca) Cobalt (Co) Copper (Cu) Iron (Fe) (La) Magnesium (Mg) Manganese (Mn) (Mo) Nickel (Ni) Phosphorous (P) Potassium (K) Sodium (Na) (Sr) Tungsten (W) Vanadium (V) Zinc (Zn) (Zr)  Thermophile Trace Nutrient Mesophile Trace Nutrient Solution (Composition in mg/L) Solution (Composition in mg/L) 8.5 7.5 12.5 4.5 1.5 4.0 52.5 1.20 40.15 17.50 5.45 15.65 11.85 0.35 466.5 1.0 144.95 233.40 2.00 4.85 0.25 1.5 2.0 25 875 1185 0.10 1.00 0.5 5.20 0.10 48.80 35.95 0.15 0.10  124  Appendix C: Mass Balance Calculations All mass balances were calculated using the following: mass of element in = mass of element out An elemental mass balance was performed for the elements copper, iron, and arsenic.  Let: rrifeed  = mass of the feed solids  Mhead  = mass of the metal in the head sample  Mieach  = mass of metal found in the feed leach solution  Mfihrate  M ash W  M  r e s  = mass of metal in the wash water  idue  M ampie S  = mass of metal in the filtrate  = mass of metal in the residue = total mass of metal found in the samples  The mass of the metal found in a solid sample is determined by M = m * wt% of element  [Cl]  For a liquid sample, the mass of the metal is determined by: M = Cm/vVljquid  [C2]  Then, assuming that samples are taken during the course of the test, the mass balance as follows: Mhead + Mieach = M  r e s  i d u e + Mfihrate + M a s h + M W  s a m  ple  [C3]  Again using the full mass balance, the calculated head can then be derived from the metal found in sampling, the final filtrate, the wash, and the residue, less that added to the system via the feed leach solution. In other words: Wt%Metal =  M f  '"  r {  "  e  +  M  w  "  S  h  ™ »e °<"»P'e  +M  id  ~ 'eacH  +M  M  m  %  [  c  4  ]  feed  m  This is sometimes referred to as the actual head, while the assay head is referred to as the indicated head.  Extraction is calculated as follows: %Extraction = " Mfi  ra,e  + M w a s h  + M  ~  M  . 100%  [C5]  head  M  If the measured head is used, this is the indicated extraction; if the calculated head is used, this is the actual extraction.  Alternately: M -M %Extraction = — ^  [C6]  head  M  Equation C5 was used to determine the percent extraction in the current work.  126  Appendix D: Extraction Data Summary Mesophiles  Table D. 1: Extraction data for mesophile experiments with 2 g of sample. Indicated Extractions B3-M10  B3-M15  B3-M37  Actual Extractions  Cu  Fe  As  Sb  Cu  Fe  As  Sb  0.00 8.02 14.00 26.01 36.34 0.00 8.02 14.00 26.01 36.34 0.00 8.02 14.00 26.01 36.34  (%) 0.00 17.31 20.71 23.42 25.03 0.00 20.81 24.70 26.95 22.59 0.00 10.11 12.36 14.01 14.95  (%) 0.00 7.47 19.15 81.33 90.22 0.00 8.31 19.23 67.07 68.38 0.00 9.61 23.30 55.08 74.80  (%) 0.00 5.74 4.84 10.84 12.49 0.00 4.37 3.75 6.54 7.51 0.00 3.49 3.07 4.34 7.50  (%) 0.00 1.76 1.84 10.03 11.51 0.00 1.08 1.12 6.17 7.20 0.00 1.16 1.87 3.98 7.46  (%) 0.00 17.26 20.65 23.35 24.96 0.00 21.15 25.11 27.39 22.96 0.00 10.70 13.09 14.82 15.82  (%) 0.00 7.85 20.13 85.50 94.85 0.00 9.17 21.23 74.04 75.48 0.00 10.18 24.68 58.34 79.22  (%) 0.00 6.19 5.21 11.69 13.47 0.00 5.04 4.33 7.54 8.66 0.00 4.00 3.52 4.98 8.59  (%) 0.00 2.00 2.09 11.38 13.07 0.00 1.22 1.27 6.96 8.12 0.00 1.39 2.25 4.80 8.99  0.00 11.87 20.19 25.85 35.81 0.00 11.87 20.19 25.85 35.81 0.00 11.87 20.19 25.85 35.81  0.00 17.08 20.16 22.15 24.24 0.00 17.36 19.63 20.18 21.24 0.00 15.39 16.80 18.86 21.27  0.00 9.62 49.63 67.24 96.76 0.00 15.03 48.02 64.81 91.32 0.00 19.59 61.83 78.80 123.73  0.00 1.27 3.21 6.11 10.51 0.00 -0.14 2.72 5.20 7.24 0.00 1.15 3.91 6.05 11.54  0.00 17.06 20.14 22.13 24.21 0.00 17.11 19.35 19.89 20.94 0.00 16.57 18.07 20.29 22.88  0.00 9.26 47.78 64.74 93.17 0.00 15.32 48.92 66.03 93.04 0.00 13.32 42.02 53.56 84.10  0.00 2.73 2.64 2.46 12.29 0.00 1.41 1.62 2.07 8.43 0.00 1.27 2.96 1.82 8.02  0.00 1.45 3.66 6.97 11.97 0.00 -0.16 3.13 5.99 8.34 0.00 0.90 3.07 4.76 9.07  Time (days)  " ~"  B4-M10  B4-M15  B4-M37  0.00 2.52 2.44 2.27 11.34 0.00 1.28 1.47 1.88 7.67 0.00 0.97 2.25 1.38 6.09  127  Table D.2: Extraction data for mesophile experiments with 3.5 g of sample. Indicated Extractions.  B6-M10  B6-M15  B6-M37  Actual Extractions  ;  Time (days)  Cu  Fe  As  Sb  Cu  Fe  (%)  (%)  (%)  (%)  (%)  (%)  0.00 7.07 19.96 27.97 35.99 0.00 7.07 19.96 27.97 35.99 0.00 7.07 19.96 27.97 35.99  0.00 12.74 19.04 21.96 25.55 0.00 12.84 18.43 21.47 25.09 0.00 7.87 12.19 14.44 16.31  0.00 3.00 34.94 95.56 83.61 0.00 2.89 31.84 92.07 87.89 0.00 3.86 24.22 68.16 85.30  0.00 2.24 4.39 11.87 13.87 0.00 1.73 3.13 7.90 9.25 0.00 1.92 2.00 5.12 7.35  0.00 0.22 1.88 11.09 0.57 0.00 0.49 2.16 7.79 0.44 0.00 0.69 0.34 3.84 0.16  0.00 12.74 19.03 21.95 25.55 0.00 12.49 17.93 20.88 24.41 0.00 7.71 11.94 14.14 15.98  0.00 3.30 38.46 105.19 92.04 0.00 3.07 33.85 97.89 93.45 0.00 3.89 24.46 68.83 86.15  As  Sb  (%)  (%)  0.00 2.35 4.60 12.45 14.54 0.00 1.93 3.48 8.77 10.28 0.00 2.11 2.20 5.63 8.08  0.00 0.28 2.39 14.15 0.73 0.00 0.63 2.78 10.04 0.57 0.00 0.87 0.43 4.84 0.21  Table D.3: Extraction data for mesophile experiments with 5 g of sample. Indicated Extractions Time (days)  B5-M10  B5-M15  B5-M37  0.00 7.80 13.17 18.81 28.79 35.81 0.00 7.80 13.17 18.81 28.79 35.81 0.00 7.80 13.17 18.81 28.79 35.81  Cu  Fe  As  (%)  (%)  (%)  0.00 1.39 6.00 12.20 25.27 56.96 0.00 3.67 15.07 22.85 55.59 80.62 0.00 1.72 9.68 19.74 28.51 92.77  0.00 2.74 1.96 1.95 1.22 10.42 0.00 0.57 0.99 1.00 2.78 7.98 0.00 2.03 1.55 1.78 1.09 9.63  0.00 15.62 18.39 19.22 20.24 25.16 0.00 15.35 17.05 18.97 19.44 22.13 0.00 13.55 18.04 19.00 19.70 22.15  Actual Extractions Sb  Cu  Fe  As  Sb  (%)  (%)  (%)  (%)  0.00 14.89 17.53 18.33 19.30 23.99 0.00 14.56 16.17 17.99 18.44 20.99 0.00 14.20 18.90 19.90 20.64 23.20  0.00 1.47 6.33 12.88 26.68 60.13 0.00 3.97 16.31 24.74 60.18 87.28 0.00 1.21 6.80 13.87 20.03 65.19  (%) 0.00 2.78 1.99 1.98 1.24 10.59 0.00 0.60 1.05 1.06 2.94 8.44 0.00 2.62 2.00 2.30 1.40 12.42  0.00 -0.12 0.13 0.37 2.07 -0.08 0.00 0.11 0.75 1.58 4.93 9.07 0.00 -0.11 -0.11 0.35 1.74 8.82  0.00 -0.09 0.10 0.29 1.61 -0.06 0.00 0.10 0.68 1.44 4.48 8.24 0.00 -0.13 -0.13 0.40 1.99 10.10  128  Table D.4: Extraction data for mesophile experiments with 10 g of sample. Indicated Extractions Time (days)  B2-M10  B2-M15  B2-M37  0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02 0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02 0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  Cu  Fe  (%) 0.00 6.15 14.03 15.57 19.20 21.91 24.23 24.71 26.98 26.80 25.47 0.00 6.20 16.87 22.23 25.67 27.03 27.32 27.58 29.07 28.49 27.52 0.00 1.95 1.96 0.99 4.20 13.57 27.55 32.94 38.01 39.55 36.37  (%) 0.00 1.18 1.05 1.83 14.94 27.95 34.20 49.10 64.55 75.05 69.57 0.00 0.82 0.60 1.16 18.56 52.81 52.62 53.93 58.59 56.70 53.64 0.00 0.29 3.83 5.15 6.16 1.32 5.08 5.88 6.62 6.96 6.95  As  (%) 0.00 0.32 1.95 1.49 3.51 6.41 8.78 12.96 14.54 14.43 13.95 0.00 0.09 1.96 2.91 5.16 12.82 11.78 12.18 13.23 13.03 12.73 0.00 -0.08 -0.08 -0.08 -0.08 -0.08 0.98 1.82 1.92 2.26 4.54  Actual Extractions Sb  Cu  Fe  (%) 0.00 0.22 0.23 -0.03 0.71 1.92 3.39 12.93 14.71 14.75 14.40 0.00 -0.05 0.04 0.04 1.34 9.74 12.47 13.18 13.79 13.94 13.62 0.00 4.46 11.94 14.82 17.37 18.11 18.78 19.19 20.21 19.74 19.12  (%) 0.00 6.29 14.36 15.94 19.65 22.43 24.81 25.29 27.62 27.43 26.08 0.00 6.24 16.97 22.36 25.82 27.19 27.48 27.74 29.23 28.65 27.68 0.00 2.11 2.12 1.07 4.55 14.69 29.83 35.67 41.15 42.82 39.38  (%) 0.00 1.29 1.14 1.99 16.26 30.41 37.21 53.42 70.23 81.66 75.70 0.00 0.86 0.63 1.22 19.52 55.54 55.33 56.71 61.61 59.63 56.40 0.00 0.32 4.16 5.58 6.68 1.43 5.51 6.37 7.17 7.54 7.54  As  Sb  (%) 0.00 0.32 1.97 1.51 3.56 6.50 8.90 13.14 14.73 14.62 14.14 0.00 0.10 2.11 3.14 5.55 13.79 12.67 13.11 14.23 14.02 13.69 0.00 -0.08 -0.08 -0.08 -0.08 -0.08 1.07 2.00 2.10 2.48 4.97  (%) 0.00 0.24 0.25 -0.03 0.77 2.08 3.68 14.00 15.92 15.97 15.59 0.00 -0.06 0.04 0.04 1.42 10.33 13.22 13.98 14.62 14.78 14.44 0.00 4.39 11.75 14.59 17.10 17.82 18.48 18.89 19.89 19.43 18.81  129  Table D.5: Extraction data for mesophile experiments with 10. g of sample (continued). Indicated Extractions  B7-M15  B7-M37  Time (days)  Cu  Fe  As  (%)  (%)  (%)  0.00 6.95 14.98 21.96 27.94 35.98 0.00 6.95 14.98 21.96 27.95 35.98  0.00 17.86 24.10 26.58 27.20 26.46 0.00 12.00 16.78 17.63 18.79 19.16  0.00 1.26 16.54 34.32 67.34 85.80 0.00 0.03 11.55 37.63 62.29 75.99  0.00 0.46 3.09 7.90 10.81 10.06 0.00 2.21 2.35 5.17 8.91 9.40  Actual Extractions Sb  Cu  Fe  As  Sb  (%)  (%)  (%)  (%)  (%)  0.00 17.59 23.75 26.19 26.79 26.06 0.00 11.53 16.12 16.94 18.05 18.40  0.00 1.37 17.92 37.17 72.95 92.94 0.00 0.03 12.58 41.01 67.89 82.82  0.00 0.51 3.43 8.76 12.00 11.17 0.00 2.39 2.54 5.60 9.66 10.20  — ... ... ...  — ...  — ... ... ... ...  — ... __. ... ...  — ... ...  — — ...  Moderate Thermophiles Table D.6: Extraction data for moderate thermophile experiments with 2 g of sample. Indicated Extractions  B9-T10  B9-T15  B9-T37  Time (days)  Cu  Fe  As  (%)  (%)  (%)  0.00 12.92 19.97 28.03 35.99 0.00 12.92 19.97 28.03 35.99 0.00 12.92 19.97 28.03 35.99  0.00 41.83 49.13 51.66 62.39 0.00 31.87 35.79 42.13 52.74 0.00 27.84 29.54 33.23 41.62  0.00 18.02 73.71 69.78 58.99 0.00 12.68 41.44 69.15 66.71 0.00 22.20 53.30 66.59 54.50  0.00 15.97 23.36 25.13 23.87 0.00 10.21 10.75 17.01 17.77 0.00 11.47 10.84 13.63 12.06  Actual Extractions Sb  Cu  Fe  (%)  (%)  (%)  As (%)  (%)  0.00 40.33 47.37 49.80 60.15 0.00 29.31 32.92 38.75 48.51 0.00 27.10 28.75 32.35 40.51  0.00 27.16 111.10 105.18 88.91 0.00 18.38 60.08 100.26 96.71 0.00 40.06 96.17 120.15 98.34  0.00 22.84 33.40 35.94 34.14 0.00 13.39 14.09 22.30 23.30 0.00 15.92 15.04 18.91 16.73  0.00 -1.31 4.72 4.33 -0.73 0.00 0.02 1.97 5.93 -0.66 0.00 -0.80 -0.75 0.08 -1.44  0.00 -0.86 3.09 2.84 -0.47 0.00 0.01 1.35 4.05 -0.45 0.00 -0.61 -0.57 0.06 -1.09  Sb  130  Table D.7: Extraction data for moderate thermophile experiments with 3.5 g of sample. Indicated Extractions  B6-T10  B6-T15  B6-T37  Cu  Fe  As  Actual Extractions  Time (days)  (%)  (%)  (%)  (%)  (%)  (%)  0.00 12.91 19.96 28.03 35.99 0.00 12.91 19.96 28.03 35.99 0.00 12.91 19.96 28.03 35.99  0.00 34.93 51.55 52.90 62.47 0.00 40.73 52.29 56.80 50.28 0.00 23.98 33.56 35.43 41.66  0.00 7.95 29.16 54.08 68.27 0.00 9.66 46.18 94.34 74.00 0.00 4.56 17.57 39.10 53.59  0.00 12.31 16.48 21.25 26.46 0.00 10.78 15.29 27.41 19.87 0.00 10.61 11.45 12.21 12.88  0.00 -0.49 0.01 2.29 -0.32 0.00 -0.49 1.45 9.63 -0.01 0.00 -0.01 -0.66 -0.66 -0.66  0.00 33.43 49.34 50.63 59.79 0.00 38.03 48.82 53.02 46.94 0.00 23.16 32.40 34.21 40.23  0.00 10.72 39.32 72.92 92.06 0.00 12.24 58.48 119.47 93.71 0.00 6.64 25.59 56.96 78.08  Sb  Cu  Fe  As (%)  0.00 17.14 22.93 29.58 36.83 0.00 13.59 19.28 34.57 25.05 0.00 14.04 15.16 16.17 17.05  Sb (%)  0.00 -0.98 0.03 4.57 -0.65 0.00 -0.71 2.08 13.79 -0.02 0.00 -0.01 -0.82 -0.82 -0.82  Table D.8: Extraction data for moderate thermophile experiments with 5 g of sample. Indicated Extractions  B8-T10  B8-T15  B8-T37  Cu  Fe  Actual Extractions  Time (days)  (%)  (%)  (%)  (%)  (%)  0.00 12.91 19.96 28.03 35.99 0.00 12.91 19.96 28.03 35.99 0.00 12.91 19.96 28.03 35.99  0.00 28.98 44.53 49.23 63.25 0.00 20.83 36.24 40.19 51.93 0.00 16.18 26.53 32.27 42.30  0.00 5.92 17.49 38.42 64.12 0.00 3.12 10.92 44.80 68.61 0.00 2.22 6.03 22.20 46.75  0.00 10.34 17.62 22.83. 30.56 0.00 3.30 10.57 16.12 21.07 0.00 6.40 12.27 13.21 13.67  0.00 -0.35 0.01 1.63 -0.23 0.00 0.19 -0.32 2.16 -0.19 0.00 -0.49 -0.49 -0.49 -0.49  0.00 26.74 41.09 45.42 58.36 0.00 19.16 33.32 36.96 47.75 0.00 15.20 24.93 30.32 39.74  As  Sb  Cu  Fe  As  (%)  (%)  0.00 0.00 7.76 12.79 22.94 21.80 50.38 . 28.24 84.08 37.80 0.00 0.00 3.82 4.18 13.36 13.36 54.77 20.37 83.87 26.63 0.00 0.00 3.21 8.15 8.70 15.61 32.00 16.80 67.39 17.39  Sb (%)  0.00 -0.72 0.01 3.41 -0.48 0.00 0.29 -0.49 3.35 -0.30 0.00 -0.73 -0.73 -0.73 -0.73  131  Table D.9: Extraction data for moderate thermophile experiments with 10 g of sample. Indicated Extractions Time (days)  B7-T10  B7-T15  B7-T37  0.00 12.91 19.96 28.02 35.99 0.00 12.91 19.96 28.02 35.99 0.00 12.91 19.96 28.02 35.99  Cu  (%)  0.00 18.05 31.54 40.91 56.13 0.00 15.00 28.99 34.98 45.70 0.00 13.17 21.09 27.86 36.85  Fe  As .  (%)  (%)  0.00 2.93 8.85 18.61 25.87 0.00 2.14 6.56 21.07 39.74 0.00 1.85 4.41 9.12 20.10  0.00 2.38 11.09 18.19 24.68 0.00 0.05 6.73 11.57 16.54 0.00 2.86 8.42 12.21 12.07  Actual Extractions Sb  (%)  0.00 -0.08 0.01 0.74 -0.11 0.00 0.09 0.20 0.72 -0.10 0.00 -0.24 -0.24 -0.24 -0.24  Cu  Fe  (%)  (%)  0.00 16.38 28.62 37.12 50.93 0.00 13.76 26.60 32.10 41.94 0.00 12.17 19.50 25.76 34.07  0.00 3.45 10.41 21.89 30.42 0.00 2.67 8.17 26.23 49.47 0.00 2.22 5.28 10.92 24.08  As  (%)  0.00 2.64 12.30 20.18 27.37 0.00 0.05 7.90 13.58 19.41 0.00 3.21 9.45 13.71 13.54  Sb  (%) 0.00 -0.12 0.02 1.09 -0.17 0.00 0.14 0.31 1.10 -0.15 0.00 -0.31 -0.31 -0.31 -0.31  132  Extreme  Thermophiles  Table D.10: Extraction data for extreme thermophile experiments with 2 g o f sample.  B3-E10  B3-E15  B3-E37  Time (days) 0.00 8.04 14.01 26.01 36.36 0.00 8.04 14.01 26.01 36.36 0.00 8.04 14.01 26.01 36.36  Indicated Extractions Cu Fe As  Sb  Actual Extractions Cu Fe As  (%)  (%)  (%)  (%)  (%)  (%)  (%)  0.00 30.15 78.06 113.11 109.03 0.00 20.32 36.76 99.09 106.07 0.00 59.11 75.78 93.69 104.11  0.00 16.81 11.38 20.31 17.25 0.00 6.83 6.27. 3.19 5.08 0.00 -1.69 -25.54 -20.81 -18.95  0.00 14.76 13.82 1.64 1.41 0.00 5.75 9.60 2.39 0.95 0.00 26.31 6.40 3.97 3.60  0.00 0.08 0.07 9.49 0.97 0.00 2.28 -0.29 11.45 6.08 0.00 -2.31 0.93 4.74 5.23  0.00 27.46 71.10 103.02 99.31 0.00 18.74 33.90 91.39 97.83 0.00 52.91 67.83 83.86 93.19  0.00 21.45 14.52 25.91 22.01 0.00 9.85 9.05 4.60 7.34 0.00 -2.21 -33.37 -27.19 -24.77  0.00 17.13 16.04 1.91 1.64 0.00 7.96 13.29 3.31 1.32 0.00 30.03 7.30 4.53 4.11  0.00 0.20 0.17 22.91 2.33 0.00 3.99 -0.50 20.05 10.66 0.00 -2.53 1.02 5.19 5.73  0.00 92.46 101.84 99.49 104.62 0.00 26.69 37.20 80.88 100.85 0.00 17.57 46.79 73.77 91.84  0.00 15.78 26.42 23.91 24.56 0.00 7.81 4.97 2.74 15.07 0.00 6.65 5.90 9.34 19.15  0.00 8.48 0.96 0.69 1.12 0.00 5.10 1.62 5.06 2.13 0.00 2.19 1.77 2.66 2.23  0.00 4.86 11.48 5.73 1.09 0.00 0.00 5.16 9.18 10.38 0.00 1.87 7.29 12.71 16.99  0.00 87.59 96.48 94.25 99.12 0.00 25.18 35.10 76.30 95.15 0.00 16.25 43.28 68.23 84.94  0.00 17.07 28.57 25.85 26.56 0.00 9.27 5.90 3.25 17.89 0.00 5.09 4.51 7.15 14.67  (%)  *  B4-E10  B4-E15  B4-E37  0.00 11.89 20.23 25.88 35.83 0.00 11.89 20.23 25.88 35.83 0.00 11.89 20.23 25.88 35.83  Sb  ' ' " ' i t . ^ '  0.00 8.87 1.01 0.73 1.17 0.00 5.97 1.89 5.93 2.49 0.00 3.02 2.44 3.66 3.08  •• •  0.00 . 13.69 32.38 16.15 3.06 0.00 0.00 6.68 11.88 13.43 0.00 1.50 5.82 10.16 13.58  133  Table D . l l : Extraction data for extreme thermophile experiments with 3.5 g of sample. Actual Extractions  Indicated Extractions  B7-E10  B7-E15  B7-E37  Time (days)  (%)  Cu  0.00 8.01 15.01 23.05 30.02 36.00 0.00 8.01 15.01 23.05 30.02 36.00 0.00 8.01 15.01 23.05 30.02 36.00  0.00 29.10 80.91 114.09 115.00 108.31 0.00 15.33 25.03 41.80 72.98 98.58 0.00 14.40 38.90 57.22 63.97 67.00  Fe (%)  0.00 13.76 10.83 15.53 24.94 23.26 0.00 3.11 6.57 12.73 6.60 3.43 0.00 2.33 -3.29 -7.31 -7.38 -7.37  As (%)  0.00 4.27 3.78 3.26 1.49 1.29 0.00 0.82 1.65 5.38 2.67 3.78 0.00 1.81 8.21 4.82 5.92 6.70  Sb  Cu  Fe  (%)  (%)  (%)  0.00 26.63 74.05 104.42 105.26 99.13 0.00 13.44 21.95 36.65 63.98 86.43 0.00 13.72 37.05 54.50 60.94 63.82  0.00 14.74 11.60 16.64 26.72 24.92 0.00 3.36 7.10 13.76 7.13 3.71 0.00 2.61 -3.68 -8.17 -8.25 -8.24  0.00 -0.81 -0.81 -0.81 -0.81 -0.81 0.00 -0.80 -0.80 -0.80 -0.80 -0.80 0.00 -1.13 -1.13 -1.13 -1.13 -1.13  As  Sb  (%)  (%)  0.00 4.49 3.98 3.43 1.57 1.36 0.00 0.89 1.79 5.82 2.89 4.10 0.00 1.97 8.91 5.23 6.42 7.27  0.00 -1.20 -1.20 -1.20 -1.20 -1.20 0.00 -0.91 -0.91 -0.91 -0.91 -0.91 0.00 -1.31 -1.31 -1.31 -1.31 -1.31  Table D.12: Extraction data for extreme thermophile experiments with 5 g of sample. Indicated Extractions  B5-E10  B8-E15  B5-E37  Time (days)  Cu  Fe  (%)  (%)  0.00 7.81 13.19 18.83 28.80 35.82 0.00 9.87 14.98 21.96 27.94 35.98 0.00 7.81 13.19 18.84 28.80 35.82  0.00 18.10 24.39 20.95 35.18 38.90 0.00 9.18 21.84 26.59 31.49 47.59 0.00 17.69 23.19 34.81 38.94 51.33  0.00 5.26 13.17 9.47 11.16 14.10 0.00 1.82 6.49 8.40 12.00 10.43 0.00 10.73 18.26 25.33 19.78 21.81  As (%)  0.00 0.32 0.61 0.53 1.53 1.79 0.00 0.44 1.28 0.35 0.74 1.84 0.00 1.68 3.17 2.80 2.69 5.20  Actual Extractions Sb  Cu  Fe  (%)  (%)  (%)  0.00 -0.27 1.40 1.62 3.24 2.97 0.00 0.00 0.00 0.00 0.00 0.00 0.00 -0.39 -0.39 2.89 4.82 7.40  0.00 17.70 23.85 20.49 34.41 38.05 0.00 8.49 20.18 24.57 29.10 43.98 0.00 17.64 23.13 34.71 38.84 51.19  0.00 5.76 14.42 10.37 12.22 15.44 0.00 1.99 7.13 9.22 13.17 11.44 0.00 7.52 12.80 17.75 13.87 15.29  As (%)  0.00 0.33 0.64 0.55 1.60 1.87 0.00 0.47 1.38 0.37 0.79 1.98 0.00 1.96 3.71 3.27 3.15 6.07  Sb (%)  0.00 -0.32 1.63 1.89 3.78 3.46 0.00 0.00 0.00 0.00 0.00 0.00 0.00 -0.34 -0.34 2.55 4.25 6.52 134  Table D-13: Extraction data for extreme thermophile experiments with 10 g of sample.  B2-E10  B2-E15  B2-E37  Time (days) 0.00 3.01 8.01 11.15 14.27 19.03 22.03 26.08 29.00 33.09 36.05 0.00 3.01 8.02 11.15 14.27 19.03 22.03 26.04 29.00 33.09 36.02 0.00 3.01 8.01 11.15 14.27 19.03 22.03 26.08 29.00 33.09 36.02  Indicated Extractions Cu Fe As (%) 0.00 11.21 19.10 20.56 23.80 26.47 28.71 31.89 34.45 38.11 37.05 0.00 5.94 8.14 10.85 13.96 19.14 20.48 23.59 26.63 29.25 28.44 0.00 6.43 11.37 12.58 13.94 17.17 18.07 22.14 26.87 29.14 28.82  (%) 0.00 5.69 6.71 7.85 9.61 13.01 11.91 13.52 15.45 16.16 13.31 0.00 2.34 4.60 3.54 6.15 7.44 6.29 7.20 8.87 9.65 8.42 0.00 4.61 2.76 1.00 0.96 1.63 0.61 -0.13 -0.58 -1.36 -1.90  (%) 0.00 3.03 0.61 0.54 0.72 0.88 1.08 1.35 1.49 1.71 1.78 0.00 0.26 1.75 0.20 0.54 0.31 2.58 0.55 0.63 0.76 0.86 0.00 2.20 1.42 0.57 0.71 0.91 1.17 1.73 2.34 2.79 3.02  Sb (%) 0.00 -0.26 0.74 0.94 1.64 1.96 2.73 3.10 3.50 3.65 2.75 0.00 0.03 -0.18 -0.24 0.63 0.53 0.79 1.12 1.69 1.94 1.61 0.00 -0.08 -0.13 0.26 0.58 1.04 1.36 1.69 1.98 1.87 1.36  Actual Extractions Cu Fe As (%) 0.00 11.22 19.11 20.58 23.82 26.49 28.74 31.92 34.48 38.15 37.09 0.00 5.88 8.06 10.74 13.82 18.95 20.27 23.35 26.36 28.95 28.15 0.00 6.49 11.48 12.70 14.08 17.34 18.24 22.35 27.12 29.42 29.10  (%) 0.00 5.91 6.97 8.15 9.99 13.52 12.37 14.05 16.05 16.78 13.82 0.00 2.44 4.80 3.70 6.42 7.76 6.57 7.52 9.27 10.08 8.79 0.00 . 4.67 2.79 1.02 0.97 1.65 0.62 -0.13 -0.59 -1.38 -1.93  (%) 0.00 2.96 0.59 0.52 0.70 0.86 1.05 1.31 1.45 1.67 1.73 0.00 0.27 1.80 0.21 0.56 0.32 2.66 0.57 0.65 0.78 0.89 0.00 2.25 1.45 0.59 0.73 0.93 1.20 1.77 2.39 2.85 3.09  Sb (%) 0.00 -0.30 0.83 1.05 1.84 2.20 3.06 3.47 3.93 4.09 3.09 0.00 0.03 -0.19 -0.25 0.67 0.56 0.83 1.18 1.78 2.05 1.70 0.00 -0.08 -0.13 0.27 0.60 1.07 1.40 1.74 2.04 1.93 1.40  135  Appendix E: Raw Data from Bioleaching Experiments Following is the raw data and calculations used in this thesis from which all the experimental data was drawn from and considered.  136  Mesophiles, 2 g Enargite, P Test UB3-M10  Date  Hour  Time . Initial (days) Mass (g)  14-Feb 18-Feb 21-Feb 22-Feb 26-Feb 28-Feb 5-Mar 7-Mar 11-Mar 12-Mar 14-Mar 15-Mar 19-Mar 21-Mar 22-Mar  10:15 9:20 11:25 10:40 9:55 10:10 10:25 11:30 12:35 10:30 11:00 12:00 12:25 20:30 18:30  0.00 3.96 7.05 8.02 11.99 14.00 19.01 21.05 25.10 26.01 28.03 29,07 33.09 35.43 36.34  Enargite In (g):  2.01  Total Water (g):  13.96  Vol (mL) Mass (g) Flask Weight (g): ,-.>• ' • 118.97 Innoculum in: 10 10 Medium in: 95.03 95.03 Total Final Weight (g) 224.88 Filtrate Volume (mL) 101.29 ' 'y. Wash Volume (mL) 250 ' . ! • Solid Residue (g)  e o  of 10 microns  Mesophiles  1.21  225.88 224.17 224.46 225.72 223.96 225.35 223.43 225.22 223.60 226.09 225.22 225.66 223.99 225.46 224.88  E Sample Medium Added Final (mL) Added (mL) Water (g) Mass (g) (Ag/AgCI) E„ (mV) h  pH  1.69 1.66 1.60 1.59 1.51 1.55 1.43 1.47 1.41 1.47 1.52 1.32 1.42 1.36 1.36  453 461 525 521 550 569 630 641  673 681 745 741 770 789 850 861  666 672 678 678 679 678  886 892 898 898 899 898  5  5  5  5  5  Copper  Iron  Arsenic  Antimony  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  31.2 191.70 0  11.6 54.85 0.10  10.5 8.0 0  0.55 1.5 0  116.5 93.0 208.5 240.5  2.0 2.0 10.5 12.0  14  •'• *i.<~.  Weight of Element Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g) Calculated Head (g) % Difference  % Extraction  Calculated Head Measured Head  Copper Iron 0.62712 0.23316 0.0019 0.0005 0 0.00954  0.005274 0.00086 0.000583 0.00606 0.00217 0.000465 0.006538 0.00905 0.001043 0 0 0 0.1375 0.003513 0.4719 0.629 -0.282 24.96 25.03  0.0005 0.0005 0.0005 0.2086 0.00231 0.0104  , . itiSL  0.7 • -  Arsenic 0.21105 0.0001 0  0 0 0 0.0244 0 0.1694  v.v.  225.71 226.09  2.06  226.02  2.50  225.93  2.82  226.42  0.83  226.05  2.58  226.57  5  Analysis  1054.85 171.50 1212.00 433.05 1307.65 1809.40 1357.70 2059.45 14.05 9.24 39 0.8599  1.54 1.63  ..#:."  Antimony 0.011055 0.0000 0 0.00001 0.00001 0.0000525 0 0 0 0.0012 0 0.00847  0.222 4.878  0.196 7.240  0.010 11.868  95.31 90.66  13.47 12.49  13.07 11.51  Copper Output Sample #  Time (days) Sol'n Vol. (mL) 0.00 8.02 14.00 26.01 36.34  1 2 3 Filtrate Wash  104.90 104.74 104.37 105.11 101.29 250.00  g Cu sampled  Tot. Cu Sampled (g)  0.00527425 0.00606 0.00653825  0.00527 0.01133 0.01787  Cu in sol'n (g) Cu(aq) total (g)  %Cu indicated  %Cu actual  0.110 0.126 0.137 0.138 0.004  0.109 0.130 0.147 0.153 0.157  17.31 20.71 23.42  17.26 20.65 23.35  25.03  24.96  Iron Output Sample # 1 2 3 Filtrate Wash  Arsenic  Time (days) Sol'n Vol. (mL) 0.00 104.90 8.02 104.74 14.00 104.37 26.01 105.11 36.34 101.29 250.00  g Fe sampled  Tot. Fe Sample  Fe in sol'n (g)  Fe(aq)total  %Fe indicated  %Fe actual  0.000355299 0.001663049 0.008544799  0.00036 0.00202 0.01056  0.01796291 0.045197429 0.190186034 0.2086 0.00231  0.02 0.04 0.19 0.21 0.21  7.47 19.15 81.33  7.85 20.13 85.50  90.22  94.85  As(aq) total  %As indicated  %As actual  0.01 0.01 0.02 0.03 0.03  5.74 4.84 10.84  6.19 5.21 11.69  12.49  13.47  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  1.76 1.84 10.03  2.00 2.09 11.38  11.51  13.07  Output  Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.00 104.90 8.02 104.74 14.00 104.37 26.01 105.11 36.34 101.29 250.00  g As sampled 0.0005825 0.000465 0.0010425  Tot. As Sample As in sol'n (g) 0.00058 0.00105 0.00209  0.01220221 0.00970641 0.021915435 0.02 0.00  Antimony Output Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.0000 8.02 14.00 26.01 36.34  104.90 104.74 104.37 105.11 101.29 250.00  g Sb sampled 0.00001 0.00001 0.0000525  Tot. Sb Sample Sb in sol'n (g) 0.00001 0.00002 0.00007  0.00020948 0.00020874 0.001103655 0.00 0.00  Mesophiles, 2 g Enargite (2), P Test UB4-M10 Date 4-Apr 8-Apr 12-Apr 15-Apr 16-Apr 18-Apr 23-Apr 24-Apr 26-Apr  Hour 15:00 12:50 10:10 10:40 11:55 11:05 10:05 19:40 11:10  29-Apr 30-Apr 3-May 7-May 10-May  10:20 11:20 10:45 10:25 10:20  Enargite In (g):  2.01  Total Water (g):  20.33  Vol (mL) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  8 0  of 10 microns  Mesophiles  :  •  10 95.05  Time (days)  Initial Mass (g)  0.00 3.91 7.80 10.82 11.87 13.84 18.80 20.19 21.84  250.53 249.70 248.08 251.20 250.58 249.12 247.47 250.34 243.44  PH 1.57 1.67 1.65 1.58 1.66 1.54 1.53 1.52 1.45  24.81 25.85 28.82 32.81 35,81  249.60 249.26 247.65 248.97 249.41  1.49 1.37 1.48 1.35 1.40  Mass (g) 144.83 10 95.05 249.41  101.72 250  E„ (Ag/AgCI) 409 407 505 536 560 573 602 609 623  E (mV) 629 627 725 756 780 793 822 829 843  636 628 626 621 630  856 848 846 841 850  Sample (mL)  Medium Added Added (mL) Water (g)  5  5  5  5  5  Copper  Iron  Arsenic  Antimony  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  31.2 179.75 0  11.6 464.20 0.10  10.5 24.0 0  0.55 1.5 0  1050.00 1188.40 1264.60 1306.30 13.73 39  261.00 1162.80 1576.15 2246.80 6.84 1.0332  53.5 49.5 44.0 229.5 0.4 14  1.5 3.5 6.5  Weight of Element Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g) Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  11.0 0.7  •>•  Copper 0.62712 0.0018 0  Iron 0.23316 0.0046 0.00955  Arsenic 0.21105 0.0002 0  Antimony 0.011055 0.0000 0  0.00525 0.005942 0.006323  0.00131 0.00581 0.00788  0.000268 0.000248 0.00022  0.0000075 0.0000175 0.0000325  0 0 0 0.1329 0.003433 0.4758  0.0005 0.0005 0.0005 0.2285 0.00171 0.01261  0 0 0 0.0233 0.0001 0.1708  0 0 0 0.0011 0 0.00854  i. -;«}«isif?,,. ">'!' ':"..•'  ••(?  0.628 -0.113  '  , -3--  24.21 24.24  •' .-'  Final Mass (g)  4.74  252.82  3.38  250.85  7.32  250.76  3.09 1.80  250.74 250.77  5  Analysis  . •' :.M-'.S#  1.22  h  '.  0.242 -3.862  0.195 7.728  0.010 12.244  94.79 98.46  12.29 11.34  11.97 10.51  Copper Output Sample #  Time (days) Sol'n Vol. (mL)  0.00 11.87 20.19 25.85 35.81  1 2 3 Filtrate Wash  103.69 103.74 103.50 102.42 101.72 250.00  g Cu sampled  Tot. Cu Sampled (g)  0.00525 0.005942 0.006323  0.00525 0.01119 0.01752  Cu in sol'n (g) Cu(aq) total (g)  %Cu indicated  %Cu actual  0.109 0.123 0.130 0.133 0.003  0.107 0.126 0.139 0.149 0.152  17.08 20.16 22.15  17.06 20.14 22.13  24.24  24.21  Fe in sol'n (g)  Fe(aq) total  %Fe indicated  %Fe actual  0.02707614 0.1203498 0.161429283 0.2285 0.00171  0.02 0.12 0.16 0.22 0.23  9.62 49.63 67.24  9.26 47.78 64.74  96.76  93.17  As(aq)total  %As indicated  %As actual  0.01 0.01 0.00 0.02 0.02  2.52 2.44 2.27  2.73 2.64 2.46  11.34  12.29  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  1.27 3.21 6.11  1.45 3.66 6.97  10.51  11.97  Iron Output Sample #  Time (days) Sol'n Vol. (mL)  0.00 11.87 20.19 25.85 35.81  1 2 3 Filtrate Wash  103.69 103.74 103.50 102.42 101.72 250.00  g Fe sampled  0.000802799 0.005311799 0.007378549  Tot. Fe Sample  0.00080 0.00611 0.01349 '  Arsenic Output Sample #  1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL)  0.00 11.87 20.19 25.85 35.81  103.69 103.74 103.50 102.42 101.72 250.00  g As sampled Tot. As Sample As in sol'n (g)  0.0002675 0.0002475 0.00022  0.00027 0.00052 0.00074  0.00555009 0.00512325 0.00450648 0.02 0.00  Antimony Output Sample #  1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL)  0.0000 11.87 20.19 25.85 35.81  103.69 103.74 103.50 102.42 101.72 250.00  g Sb sampled  0.0000075 0.0000175 0.0000325  Tot. Sb Sample Sb in sol'n (g)  0.00001 0.00003 0.00006  0.00015561 0.00036225 0.00066573 0.00 0.00  Mesophiles, 2 g Enargite, P Test XB3-M15  8 0  of 15 microns  Mesophiles  Date  Hour  Time Initial (days) Mass (g)  PH  14-Feb 18-Feb 21-Feb 22-Feb 26-Feb 28-Feb 5-Mar 7-Mar 11-Mar 12-Mar 14-Mar 15-Mar 19-Mar 21-Mar 22-Mar  10:15 9:20 11:25 10:40 9:55 10:10 10:25 11:30 12:35 10:30 11:00 12:00 12:25 20:30 18:30  0.00 ' 3.96 7.05 8.02 11.99 14.00 19.01 21.05 25.10 26.01 28.03 29,07 33.09 35.43 36.34  1.71 1.69 1.65 1.64 1.56 1.56 1.45 1.57 1.48 1.64 1.43 1.43 1.46 1.47 1.45  Enargite In (g): Total Water (g):  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  2.00 17.88  Vol (mL) Mass (g) 114.82 10 10 95.04 95.04 250.76 103.08 250 1.28  251.60 249.62 250.20 251.06 248.85 250.50 248.24 250.79 248.90 253.54 252.38 251.81 249.60 251.67 250.76  Sample Eh (Ag/AgCI) E (mV) (mL) h  430 460 517. 500 556 560 578 645  650 680 737 720 776 780 798 865  649 664 681 674 677 675  869 884 901 894 897 895  5  5 5  Medium Added Final Added (mL) Water (g) Mass (g) -  Iron  Arsenic  Antimony  30.4 191.70 0  10.6 54.85 0.10044  10.5 8.0 0  0.55 1.5 0  956.75 1101.90 1137.00 1162.80 13.60 36  135.25 309.05 1044.00 1394.05 7.26 3.9606  69.0 57.0 96.5 143.0  1.0 1.0 5.0 7.0 0.2 0.7  it.-'  % Extraction  Calculated Head Measured Head  251.37  3.57  251.81  5.03  253.93  3.43  253.03  5  Copper  Calculated Head (g) % Difference  2.52 5  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  Weight of Element Copper Iron Arsenic Head (g) 0.608 0.212 0.21 Innoculum (g) 0.0019 0.0005 0.0001 Medium (g) 0 0.00955 0 Samples (g): #1 0.004784 0.00068 0.000345 #2 0.00551 0.00155 0.000285 #3 0.005685 0.00522 0.000483 Medium Added (g): #1 0 0.0005 0 #2 0 0.0005 0 #3 0 0.0005 0 0.1199 PLS (g) 0.1437 0.0147 Wash (g) 0.0034 0.00182 0 0.4608 Solid Residue (g) 0.0507 0.1664  251.72 251.43  5  Analysis  13  2.10 1.23  Antimony 0.011 0.0000 0 0.000005 0.000005 0.000025 0 0 0 0.0007 0.00005 0.00896  ' -.•'  0.598 1.625  0.192 9.410 >-  22.96 22.59  0.182 13.251  0.010 11.349  - , ' t • . . . . '„..,;,;,->  73.60 66.68  8.66 7.51  8.12 7.20  141  Copper Output Sample #  Time (days) Sol'n Vol. (mL) 0.00 8.02 14.00 26.01 36.34  1 2 3 Filtrate Wash  134.78 134.24 133.68 136.72 103.08 250.00  g Cu sampled  Tot. Cu Sampled (g)  0.00478375 0.0055095 0.005685  0.00478 0.01029 0.01598  Cu in sol'n (g) Cu(aq) total (g)  %Cu indicated  %Cu actual  0.128 0.147 0.155 0.120 0.003  0.127 0.150 0.164 0.134 0.137  20.81 24.70 26.95  21.15 25.11 27.39  22.59 •  22.96  Iron Output Sample # 1 2 3 Filtrate Wash  Arsenic  Time (days) Sol'n Vol. (mL) 0.00 134.78 8.02 134.24 14.00 133.68 26.01 136.72 36.34 103.08 250.00  g Fe sampled  Tot. Fe Sample  Fe in sol'n (g)  Fe(aq)total  %Fe indicated  %Fe actual  0.000174049 0.001043049 0.004717799  0.00017 0.00122 0.00593  0.018 0.041 0.143 0.1437 0.001815  0.02 0.04 0.14 0.14 0.14  8.31 19.23 67.07  9.17 21.23 74.04  68.38  75.48  As(aq)total  %As indicated  %As actual  0.01 0.01 0.01 0.02 0.02  4.37 3.75 6.54  5.04 4.33 7.54  7.51  8.66  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  1.08 1.12 6.17  1.22 1.27 6.96  7.20  8.12  Output  Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.00 134.78 8.02 134.24 14.00 133.68 26.01 136.72 36.34 103.08 250.00  g As sampled 0.000345 0.000285 0.0004825  Tot. As Sample As in sol'n (g) 0.00035 0.00063 0.00111  0.00926256 0.00761976 0.01319348 0.01 0.00  Antimony Output Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.0000 8.02 14.00 26.01 36.34  134.78 134.24 133.68 136.72 103.08 250.00  g Sb sampled 0.000005 0.000005 0.000025  Tot. Sb Sample Sb in sol'n (g) 0.00001 0.00001 0.00004  0.00013424 0.00013368 0.0006836 0.00 0.00  Mesophiles, 2 g Enargite (2), P  Test #B4-M15  8 0  of 15 microns  Mesophiles  Date  Hour  Time Initial (days) Mass (g)  pH  4-Apr 8-Apr 12-Apr 15-Apr 16-Apr 18-Apr 23-Apr 24-Apr 26-Apr  15:00 12:50 10:10 10:40 11:55 11:05 10:05 19:40 11:10  0.00 3.91 7.80 10.82 11.87 13.84 18.80 20.19 21.84  223.85 222.49 223.19 222.22 221.68 220.30 222.91 223.49 222.74  1.54 1.73 1.70 1.62 1.62 1.65 1.49 1.51 1.59  411 400 518 555 574 591 577 586 624  631 620 738 775 794 811 797 806 844  29-Apr 30-Apr 3-May 7-May 10-May  10:20 11:20 10:45 10:25 10:20  24.81 25.85 28.82 32.81 35.81  223.04 222.81 221.75 223.24 222.16  1.48 1.46 1.66 1.47 1.43  627 638 634 628 620  847 858 854 848 840  Enargite In (g):  2.00  Total Water (g):  10.69  Vol (mL) Mass (g) Flask Weight (g): It;!-',#!»: Si 116.88 Innoculum in: 10 10 Medium in: 95.12 95.12 222.16 Total Final Weight (g):r: > . Filtrate Volume (mL) 102.53 »¥'3<f|:;; \. . " Wash Volume (mL) 250 Solid Residue (g)  1.25  Sample Medium Added Final E (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) h  5  5  Copper  Iron  Arsenic  Antimony  30.4 179.75 0  10.6 464.20 0.10044  10.5 24.0 0  0.55 1.5 0  1044.10 1108.05 1094.10 1090.65 11.50 39  355.20 1017.55 1366.75 1912.80 8.47 0.9482  28.5 30.5 37.5 154.0 0.3 14  0.0 3.0 5.5 7.5  Copper 0.608 0.0018 0  Iron 0.212 0.0046 0.00955  0.7 -  Arsenic 0.21 0.0002 0  °j"  ...,^  Antimony 0.011 0.0000 0  0.005221 0.00178 0.000143 0.00554 0.00509 0.000153 0.005471 0.00683 0.000188  0 0.000015 0.0000275  0 0.0005 0 0 0.0005 0 0 0.0005 0 0.1118 0.1961 0.0158 0.002875 0.00212 0.000075 0.4875 0.01185 0.175  0 0 0 0.0008 0 0.00875  '••Mtf'T-j*',.,  Calculated Head (g) % Difference  % Extraction  Calculated Head Measured Head  224.35 223.91  1.27  224.01  2.49  224.24  5  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt % ; , -L* ' Weight of Element Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g)  •fe.  4.05 1.00 5  5  '  224.37  5  Analysis  i~ -  1.88  •>  0.617 -1.420  0.208 1.847  0.191 8.997  0.010 13.214  20.94 21.24  94.30 92.56  8.43 7.67  8.34 7.24  Copper Output Sample #  Time (days) Sol'n Vol. (mL) 0.00 11.87 20.19 25.85 35.81  1 2 3 Filtrate Wash  104.97 102.80 104.61 103.93 102.53 250.00  g Cu sampled  Tot. Cu Sampled (g)  0.0052205 0.00554025 0.0054705  0.00522 0.01076 0.01623  Cu in sol'n (g) Cu(aq) total (g)  %Cu indicated  %Cu actual  0.107 0.116 0.114 0.112 0.003  0.106 0.119 0.123 0.126 0.129  17.36 19.63 20.18  17.11 19.35 19.89  21.24  20.94  Iron Output Sample # 1 2 3 Filtrate Wash  Arsenic  Time (days) Sol'n Vol. (mL) 0.00 104.97 11.87 102.80 20.19 104.61 25.85 103.93 35.81 102.53 250.00  g Fe sampled  Tot: Fe Sample  Fe in sol'n (g)  Fe(aq) total  %Fe indicated  %Fe actual  0.001273799 0.004585549 0.006331549  0.00127 0.00586 0.01219  0.037 0.106 0.142 0.1961 0.0021175  0.03 0.10 0.14 0.19 0.19  15.03 48.02 64.81  15.32 48.92 66.03  91.32  93.04  As(aq)total  %As indicated  %As actual  0.00 0.00 0.00 0.02 0.02  1.28 1.47 1.88  1.41 1.62 2.07  7.67  8.43  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  -0.14 2.72 5.20  -0.16 3.13 5.99  7.24  8.34  Output  Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.00 104.97 11.87 102.80 20.19 104.61 25.85 103.93 102.53 35.81 250.00  g As sampled 0.0001425 0.0001525 0.0001875  Tot. As Sample As in sol'n (g) 0.00014 0.00030 0.00048  0.0029298 0.003190605 0.003897375 0.02 0.00  Antimony Output Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.0000 11.87 20.19 25.85 35.81  104.97 102.80 104.61 103.93 102.53 250.00  g Sb sampled 0 0.000015 0.0000275  Tot. Sb Sample Sb in sol'n (g) 0.00000 0.00002 0.00004  0 0.00031383 0.000571615 0.00 0.00  Mesophiles, 2 g Enargite, P  Test #B3-M37 Date  Hour  Time Initial (days) Mass (g)  14-Feb 18-Feb 21-Feb 22-Feb 26-Feb 28-Feb 5-Mar 7-Mar 11-Mar 12-Mar 14-Mar 15-Mar 19-Mar 21-Mar 22-Mar  10:15 9:20 11:25 10:40 9:55 10:10 10:40 11:30 12:35 10:30 11:00 12:00 12:25 20:30 18:30  0.00 3.96 7.05 8.02 11.99 14.00 19.02 21.05 25.10 26.01 28.03 29.07 33.09 35.43 36.34  Enargite In (g):  2.01  Total Water (g):  16.86  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  8 0  of 37 microns  Mesophiles  Vol (mL) Mass (g) 137.36 10 10 95.06 95.06 242.41 • • 95.33 250 1.48  244.30 242.18 242.52 244.94 242.57 243.61 241.44 241.32 241.40 244.29 243.34 243.95 242.09 243.06 242.41  PH 1.74 1.63 1.58 1.60 1:51 1.52 . 1.44' 1.52 1.46 1.52 1.53 1.39 1.45 1.44 1.42  E,, Sample Medium Added Final (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 467 472 525 533 541 580 640 645  687 692 745 753 761 800 860 865  654 661 685 659 670 670  874 881 905 879 890 890  5  Analysis  Copper  Iron  Arsenic  Antimony  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  32.4 191.70 0  7.2 54.85 0.10044  12 8.0 0  0.39 1.5 0  641.85 760.10 820.90 905.15 7.57 35  136.95 328.80 765.00 1126.45 5.63 2.2498  80.5 68.0 93.5 175.5 0.9 13  1.0 1.5 3.0 6.0  Arsenic 0.2412 0.0001 0  Antimony 0.007839  Weight of Element Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g) Calculated Head (g) % Difference  % Extraction  Calculated Head Measured Head  Copper Iron 0.65124 0.14472 0.0019 0.0005 0 0.00955  • 5  5  5  5  0.003209 0.00068 0.000403 0.003801 0.00164 0.00034 0.004105 0.00383 0.000468 0 0 0 0.0863 0.001893 0.518  0.0005 0 0.0005 0 0.0005 0 0.1074 0.0167 0.00141 0.000225 0.0333 0.1924  1.99 2.80  244.17 245.32  2.00  244.57  3.07  244.51  3.25  244.65  1.18  244.52  2.57  244.66  5  0.4  o.ooOo 0  0.000005 0.0000075 0.000015 0 0 0 0.0006 0 0.00592  0.615 5.507  0.137 5.583  0.210 12.734  0.007 17.024  15.82 14.95  75.63 71.41  8.59 7.50  8.99 7.46  Copper Output Sample #  Time (days) Sol'n Vol. (mL) 0.00 8.02 14.00 26.01 36.34  1 2 3 Filtrate Wash  104.93 105.57 104.24 104.92 95.33 250.00  g Cu sampled  Tot. Cu Sampled (g)  0.00320925 0.0038005 0.0041045  0.00321 0.00701 0.01111  Cu in sol'n (g) Cu(aq) total (g) .  %Cu indicated  %Cu actual  0.068 0.079 0.086 0.086 0.002  0.066 0.081 0.091 0.095 0.097  10.11 •12.36 14.01  10.70 13.09 14.82  14.95  15.82  Iron Output Sample # 1 2 3 Filtrate Wash  Arsenic  Time (days) Sol'n Vol. (mL) 0.00 104.93 8.02 105.57 14.00 104.24 26.01 104.92 36.34 95.33 250.00  g Fe sampled  Tot. Fe Sample  Fe in sol'n (g)  Fe(aq) total  %Fe indicated  %Fe actual  0.000182549 0.001141799 0.003322799  0.00018 0.00132 0.00465  0.014457812 0.034274112 0.0802638 0.1074 0.0014075  0.01 0.03 0.08 0.11 0.11  9.61 23.30 55.08  10.18 24.68 58.34  74.80  79.22  As(aq)total  %As indicated  %As actual  0.01 0.01 0.01 0.02 0.02  3.49 3.07 4.34  4.00 3.52 4.98  7.50  8.59  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  1.16 1.87 3.98  1.39 2.25 4.80  7.46  8.99  Output  Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.00 104.93 8.02 105.57 14.00 104.24 26.01 104.92 36.34 95.33 250.00  g As sampled 0.0004025 0.00034 0.0004675  Tot. As Sample As in sol'n (g) 0.00040 0.00074 0.00121  0.008498385 0.00708832 0.00981002 0.02 0.00  Antimony Output Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.0000 8.02 14.00 26.01 36.34  104.93 105.57 104.24 104.92 95.33 250.00  g Sb sampled 0.000005 0.0000075 0.000015  Tot. Sb Sample Sb in sol'n (g) 0.00001 0.00001 0.00003  0.00010557 0.00015636 0.00031476 0.00 0.00  Mesophiles, 2 g Enargite (2), P Test UB4-M37  8 0  Date  Hour  Time Initial (days) Mass (g)  PH  4-Apr 8-Apr 12-Apr 15-Apr 16-Apr 18-Apr 23-Apr 24-Apr 26-Apr 29-Apr 30-Apr 3-May 7-May 10-May  15:00 12:50 10:10 10:40 11:55 11:05 10:05 19:40 11:10 10:20 11:20 10:45 10:25 10:20  0.00 3.91 7.80 10.82 11.87 13.84 18.80 20.19 21.84 24.81 25.85 28.82 32.81 35.81  1.54 1.73 1.72 1.63 1.63 1.62 1.50 1.52 1.57 1.50 1.47 1.58 1.44 1.44  Enargite In (g):  2.00  Total Water (g):  13.12  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  of 37 microns  Mesophiles  236.23 234.55 237.25 236.03 235.60 234.24 235.51 236.16 235.68 235.34 234.96 233.70 235.49 234.24  E„ (Ag/AgCI) E (mV)  Analysis  Vol (mL) Mass (g) 129.13 10 10 95.11 95.11 • . . 234.24 102.69 250 1.29  Sample Medium Added Final (mL) Added (mL) Water (g) Mass (g)  h  412 395 527 564 577 594 600 596 620 634 637 636 628 626  632 615 747 784 797 814 820 816 840 854 857 856 848 846  Copper  5 5  5  Arsenic  Antimony  12 24.0 0  0.39 1.5 0  314.50 891.90 1137.55 1769.70 4.32 2.5608  24.5 52.5 30.5 139.5  1.0 3.0 4.5 8.5  13  0.7  Weight of Element Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g)  Iron 0.144 0.0046 0.00955  Arsenic 0.24 0.0002 0  Antimony 0.0078 0.0000 0  0.004861 0.00157 0.000123 0.000005 0.005036 0.00446 0.000263 0.000015 0.005494 0.00569 0.000153 0.0000225  •.  Calculated Head (g) % Difference  % Extraction  Calculated Head Measured Head  '.•.„•  . '  0.602 7.067  n  ...  0.212 -47.127  '-  0 0 0 0.0009 0 0.00903  V , ; ' . > , t SIA ... : .-  0.182 24.032  0.010 -27.312  8.02 6.09  9.07 11.54  •i',''".' ;„"?' v v • -vf'i c  22.88 . 21.27  84.41 124.19  237.46 236.66  0.57  236.25  3.49  237.19  5  7.2 464.20 0.10044  0 0 0 0.0143 0 0.1677  3.22 1.15 5  Iron  0 0.0005 0 0.0005 0 0.0005 0.1214 0.1817 0.002783 0.00108 0.4644 0.03303  239.24  5  Head (wt %) 32.4 Innoculum (mg/L) 179.75 Medium (g/L) 0 Samples (mg/L): #1 972.10 #2 1007.10 #3 1098.85 PLS (mg/L) 1182.50 Wash (mg/L) 11.13 Solid Residue (wt % 36 Copper 0.648 0.0018 0  4.69  •  Copper Output Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (niL) 0.00 105.10 11.87 104.47 20.19 105.03 25.85 103.83 35.81 102.69 250.00  g Cu sampled  Tot. Cu Sampled (g)  0.0048605 0.0050355 0.00549425  0.00486 0.00990 0.01539  Time (days) Sol'n Vol. (n»-) 0.00 105.10 11.87 104.47 20.19 105.03 25.85 103.83 35.81 102.69 250.00  g Fe sampled 0.001070299 0.003957299 0.005185549  Cu in sol'n (g) Cu(aq) total (g)  %Cu indicated  %Cu actual  0.102 0.106 0.114 0.121 0.003  0.100 0.109 0.122 0.135 0.138  15.39 16.80 18.86  16.57 18.07 20.29  21.27  22.88  Tot. Fe Sample  Fe in sol'n (g)  Fe(aq)total  %Fe indicated  %Fe actual  0.00107 0.00503 0.01021  0.032855815 0.093676257 0.118111817 0.1817 0.00108  0.03 0.09 0.11 0.18 0.18  19.59 61.83 78.80  13.32 42.02 53.56  123.73  84.10  As(aq) total  %As indicated  %As actual  0.00 0.01 0.00 0.01 0.01  0.97 2.25 1.38  1.27 2.96 1.82  6.09  8.02  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  1.15 3.91 6.05  0.90 3.07 4.76  11.54  9.07  Iron Output Sample # 1 2 3 Filtrate Wash  Arsenic  Output  Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.00 105.10 11.87 104.47 20.19 105.03 25.85 103.83 35.81 102.69 250.00  g As sampled 0.0001225 0.0002625 0.0001525  Tot. As Sample As in sol'n (g) 0.00012 0.00039 0.00054  0.002559515 0.005514075 0.003166815 0.01 0.00  Antimony Output Sample # 1 2 3 Filtrate Wash  Time (days) Sol'n Vol. (niL) 0.0000 105.10 11.87 104.47 20.19 105.03 25.85 103.83 35.81 102.69 250.00  g Sb sampled 0.000005 0.000015 0.0000225  Tot. Sb Sample Sb in sol'n (g) 0.00001 0.00002 0.00004  0.00010447 0.00031509 0.000467235 0.00 0.00  Mesophiles, 3.5 g Enargite, P Test UB6-M10  Date  21-May 24-May 27-May 28-May 30-May 3-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun  Hour  of 10 microns  Time  Initial  (days)  M a s s (g)  PH  (Ag/AgCI)  E„ (mV)  224.15 223.39 224.39 223.96 223.32 226.31 225.26 224.62 223.70 221.97 225.53 224.98 223.32 224.42  1.57 1.67 1.78 1.93 1.76 1.74 1.62 1.54 1.44 1.32 1.31 1.21 1.23 1.27  404 385 488 518 535 564 604 575 627 639 625 640 635 641  624 605 708 738 755 784 824 795 847. 859 845 860 855 861  12:00 0.00 10:20 2.93 10:25 5.93 13:40 7.07 10:30 8.94 12:35 13.02 10:25 16.93 11:00 19.96 11:20. . 22.97 10:05 26.92 27.97 11:10 12:00 30.00 11:15 33.97 11:45 35.99  E n a r g i t e In (g):  3.50  Total Water (g):  11.15  E„  2.14  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %) ' f . - . '  .'•  Sample  Copper  Analysis  Vol (mL) Mass (g) Flask Weight (g): • . -\ 115.77 Innoculum in: 10 10 Medium in: 95.01 95.01 Total Final Weight (g): 224.42 Filtrate Volume (mL) 104.37 Wash Volume (mL) 250 Solid Residue (g)  8 0  Mesophiles  •  Iron  (mL)  5  Medium  Final  1.62  225.01  3.87  227.19  3.74  225.71  1.92  225.24  5  5  5  5  5  Arsenic  Added  A d d e d ( m L ) W a t e r (g) M a s s (g)  Antimony  31.2 169.25 0  11.6 444.10 0.10  10.5 24.5 0  0.55 1.0 0  1345.00 1925.65 2118.35 2365.90 27.51 38  158.85 1388.75 3692.80 3245.00 20.88 0.6639  81.0 151.5 402.0 459.5 0.4 14  0.5 3.5 20.0 0.7  '• ' . ''.'-v."  ,• "•  Weight of Element Copper Head (g) 1.092 Innoculum (g) 0.0017 Medium (g) 0 Samples (g): #1 0.006725 #2 0.0096283 #3 0.0105918 Medium Added (g): #1 0 #2 0 #3 0 0.2469 PLS (g) Wash (g) 0.0068775 Solid Residue (g) 0.8132  Iron Arsenic 0.406 0.3675 0.0044 0.0002 0.009543 0 0.000794 0.000405 0.006944 0.000758 0.018464 0.00201  Antimony 0.01925 0.0000 0 0.0000025 0.0000175 0.0001  0.000502 0.000502 0.000502 0.3387 0.00522 0.014207  0 0 0 0.0480 0.0001 0.2996  0 0 0 0.0000 0 0.01498  0.369 9.158  0.351 4.603  0.015 21.610  ':*''«i«if.{  ;  Calculated Head (g) % Difference %  1.092 -0.024  Extraction  Calculated Head Measured Head  25.55 25.55  • *:,3r"\ "  96.15 87.34  • •  14.54 13.87  ij-,-.:-**Sf..  0.73 0.57  149  Copper Output  Tot. Cu Sample # Time (days) Sol'n Vol. (mL) g Cu sampled Sampled (g) Cu in sol'n (g)Cu(aq) total (g) %Cu indicated %Cu actual 1 2 3 Filtrate Wash  0.00 7.07 19.96 27.97 35.99  104.88 104.69 105.35 106.26 104.37 250.00  0.006725 0.00962825 0.01059175  0.00673 0.01635 0.02695  0.141 0.203 0.225 0.247 0.007  0.139 0.208 0.240 0.272 0.279  12.74 19.04 21.96  12.74 19.03 21.95  25.55.  25.55  Iron Output  Sample # Time (days) Sol'n Vol. (IT 1 2 3 Filtrate Wash  0.00 7.07 19.96 27.97 35.99  104.88 104.69 105.35 106.26 104.37 250.00  g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total 0.000292049 0.006441549 0.017961799  0.00029 0.00673 0.02470  0.016630007. 0.146304813 0.392396928 0.3387 0.00522  0.01 0.14 0.39 0.33 0.34  %Fe indicated %Fe actual 3.00 34.94 95.56  3.30 38.46 105.19  83.61  92.04  Arsenic Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) As(aq)total 1 2 3 Filtrate Wash  0.00 7.07 19.96 27.97 35.99  104.88 104.69 105.35 106.26 104.37 250.00  0.000405 0.0007575 0.00201  0.00041 0.00116 0.00317  0.00847989 0.015960525 0.04271652 0.05 0.00  0.01 0.02 0.04 0.05 0.05  %As indicated %As actual 2.24 4.39 11.87  2.35 4.60 12.45  13.87  14.54  Antimony Output  Sample # Time (days) Sol'n Vol. (IT»L) g Sb sampled Tot. Sb Sample Sb in sol'n (g) Sb(aq) total %Sb indicated %Sb actual 1 2 3 Filtrate Wash  0.0000 8.94 19.96 27.97 35.99  104.88 104.05 105.35 106.26 104.37 250.00  0.0000025 0.0000175 0.0001  0.00000 0.00002 0.00012  0.000052025 0.000368725 0.0021252 0.00 0.00  0.00 0.00 0.00 0.00 0.00  0.22 1.88 11.09  0.28 2.39 14.15  0.57  0.73  Mesophiles, 3.5 g Enargite, P Test #B6-M15  8 0  of 15 microns  Mesophiles  Date  Hour  Time Initial (days) Mass (g)  pH  21-May 24-May 27-May 28-May 30-May 3-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun  12:00 10:20 10:25 13:40 10:30 12:35 10:25 11:00 11:20 10:05 11:10 12:00 11:15 11:45  0.00 2.93 5.93 7.07 8.94 13.02 16.93 19.96 22.97 26.92 27,97 30.00 33.97 35.99  1.55 1.70 . 1.84 1.98 1.84 1.72 1.71 1.61 1.55 1.41 1.36 1.31 1.29 1.31  Enargite In (g):  3.50  Total Water (g):  11,63  Analysis  Vol (mL) Mass (g) Flask Weight (g): 116.5 Innoculum in: 10 10 Medium in: 95.11 95.11 Total Final Weight (g):| :•;>. -"-« 226.28 Filtrate Volume (mL) 104.40 V-7. 250 . / e £ Wash Volume (mL) Solid Residue (g)  225.10 224.33 224.45 224.98 224.37 224.46 223.59 225.02 224.40 224.18 226.00 225.30 223.92 226.28  E  "I' ":  :;  2.12  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %)  h  (Ag/AgCI) Eh (mV) 324 369 465 521 546 556 583 587 624 632 631 645 642 645  Copper  544 589 685 741 766 776 803 807 844 852 851 865 862 865  Iron  Sample Medium Added Final (mL) Added (mL) Water (g) Mass (g)  5  5  % Extraction  Calculated Head Measured Head  225.38  2.34  225.93  1.12 2.24  225.52 226.42  3.14  227.06  5  Arsenic  Antimony  10.6 444.10 0.10044  10.5 24.5 0  0.55 1.0 0  1317.75 1820.25 2022.60 2258.90 27.99 39  144.40 1167.00 3264.20 3123.75 17.62 0.5207  63.0 109.0 268.0 307.0 0.0 14  1.0 4.0 14.0 0.7 Antimony 0.01925 0.0000 0  0.00072 0.000315 0.00584 0.000545 0.01632 0.00134  0.000005 0.00002 0.00007  0.0005 0.0005 0.0005 0.3261 0.00441 0.01104  0 0 0 0.0321 0 0.2968  0 0 0 0.0000 0 0.01484  1.094 -2.795  0.349 5.946  0.331 9.985  0.015 22.468  24.41 25.09  96.84 91.08  10.28 9.25  0.57 0.44  •  Calculated Head (g) % Difference  1.01 5  5  Iron Arsenic 0.371 0.3675 0.0044 0.0002 0.00955 0  225.30 225.26  5  30.4 169.25 0  Weight of Element Copper Head (g) 1.064 Innoculum (g) 0.0017 Medium (g) 0 Samples (g): #1 0.0065888 #2 0.0091013 #3 0.010113 Medium Added (g): #1 0 #2 0 #3 0 PLS (g) 0.2358 Wash (g) 0.0069975 0.8268 Solid Residue (g)  0.97 0.81  Copper Output  Tot. Cu Sample # Time (days) Sol'n Vol. (mL) g Cu sampled Sampled (g) Cu in sol'n (g)Cu(aq) total (g) %Cu indicated %Cu actual 1 2 3 Filtrate Wash  0.00 7.07 19.96 27.97 35.99  105.10 104.98 105.02 106.00 104.40 250.00  0.00658875 0.00910125 0.010113  0.00659 0.01569 0.02580  0.138 0.191 0.214 0.236 0.007  0.137 0.196 0.228 0.260 0.267  12.84 18.43 21.47  12.49 17.93 20.88  25.09  24.41  Iron Output  Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total 1 2 3 Filtrate Wash  0.00 7.07 19.96 27.97  35.99  105.10 104.98 105.02 106.00 104.40 250.00  0.000219799 0.005332799 0.015818799  0.00022 0.00555 0.02137  0.015 0.123 0.346 0.3261 0.004405  0.01 0.12 0.34 0.32 0:33  %Fe indicated %Fe actual 2.89 31.84 92.07  3.07 33.85 97.89  87.89  93.45  Arsenic Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) As(aq) total %As indicated %As actual 1 2 3 Filtrate Wash  0.00 7.07 19.96 27.97 35.99  105.10 104.98 105.02 106.00 104.40 250.00  0.000315 0.000545 0.00134  0.00032 0.00086 0.00220  0.00661374 0.01144718.' 0.028408 0.03 0.00  0.01 0.01 0.03 0.03 0.03  1.73 3.13 7.90  1.93 3.48 8.77  9.25  10.28  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) Sb(aq) total %Sb indicated %Sb actual 1 2 3 Filtrate Wash  0.0000 8.94 19.96 27.97 35.99  105.10 104.37 105.02 106.00 104.40 250.00  0.000005 0.00002 0.00007  0.00001 0.00003 0.00010  0.00010437 0.00042008 0.001484 0.00 0.00  0.00 0.00 0.00 0.00 0.00  0.49 2.16 7.79  0.63 2.78 10.04  0.44  0.57  Mesophiles, 3.5 g Enargite, P  Test #B6-M37 Date 21-May 24-May 27-May 28-May 30-May 3-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun  Enargite In (g): Total Water (g):  8 0  of 37 microns  Mesophiles  Hour 12:00 10:20 10:25 13:40 10:30 12:35 10:25 11:00 11:20 10:05 11:10 12:00 11:15 11:45  Time (days) 0.00 2.93 5.93 7.07 8.94 13.02 16.93 19.96 22.97 26.92 27.97 30.00 33.97 35.99  3.51 14.33  Vol(mL) Mass(g) Flask Weight (g): 145.92 10 10 Innoculum in: 95.05 95.05 Medium in: Total Final Weight (g): I 254.30 103.39 Filtrate Volume (mL) 250 Wash Volume (mL) Solid Residue (g) •• - j 2.71  Initial Mass (g) 254.20 253.20 253.77 254.04 253.34 253.01 251.49 253.53 252.26 252.61 255.13 254.28 252.41 254.30  E„ (Ag/AgCI) E„ (mV) 385 605 382 602 458 678 505 725 529 749 567 787 582 802 592 812 615 835 629 849 626 846 636 856 640 860 641 861  PH 1.54 1.59 1.71 1.89 1.69 1.67 1.60 1.58 1.56 1.45 1.39 1.32 1.32 1.34  Analysis  Copper  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %)  Iron  5  5  Arsenic  Antimony  872.10 1306.55 1466.55 1592.90 17.13 36  135.60 630.65 1671.60 2112.35 6.44 1.2374  79.5 79.5 199.0 284.5 0.0 13  1.0 0.5 5.0  0.0005 0.0005 0.0005 0.2184 0.00161 0.03353  . . . . '.'wvv '. ; >';i"'& .. /,'„ ; i X * & A . !' :  0.4 :<:•.-?.-.•  0.00068 0.000398 0.00315 0.000398 0.00836 0.000995 0 0 0 0.0294 0 0.3523 ..  1.02  254.36  3.01  254.50  2.27 3.00  254.53 255.61  2.94  255.35  5  0.39 1.0 0  Iron Arsenic 0.25272 0.4212 0.0044 0.0002 0.00955 0  254.71 254.35  5  12 24.5 0  ;'  1.51 0.58 5  7.2 444.10 0.10044  Weight of Element Copper Head (g) 1.13724 Innoculum (g) 0.0017 Medium (g) 0 Samples (g): #1 0.0043605 #2 0.0065328 #3 0.0073328 Medium Added (g): #1 0 #2 0 #3 0 PLS (g) 0.1647 Wash (g) 0.0042825 Solid Residue (g) 0.9756 ;  5  Medium Added Final Added (mL) Water (g) Mass (g)  32.4 169.25 0  . ••  Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  Sample (mL)  -  Antimony 0.013689 0.0000 0 0.000005 0.0000025 0.000025 0 0 0 0.0000 0 0.01084 :>',•"<  1.161 -2.099  0.250 0.984  0.383 9.008  0.011 20.648  15.98 16.31  86.60 85.75  8.08 7.35  0.21 0.16  Copper Output  Sample # Time (days) Sorn Vol. (mL) g Cu sampled 0.00 104.77 1 7.07 104.61 0.0043605 2 19.96 104.10 0.00653275 3 27.97 105.70 0.00733275 Filtrate 35.99 103.39 Wash 250.00  Iron Output  "  Sample # Time (days) Sol'n Vol. (mL) 0.00 104.77 1 7.07 104.61 2 19.96 104.10 3 27.97 105.70 35.99 103.39 Filtrate Wash 250.00  Tot. Cu Sampled (g) 0.00436 0.01089 0.01823  Cu In sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.091 0.136 0.155 0.165 0.004  0.090 0.139 0.164 0.181 0.186  7.87 12.19 14.44  7.71 11.94 14.14  16.31  15.98  Fe(aq) total  %Fe indicated  %Fe actual  0.01 0.06 0.17 0.21 0.22  3.86 24.22 68.16  3.89 24.46 68.83  85.30  86.15  As(aq) total  %As indicated  %As actual  0.01 0.01 0.02 0.03 0.03  1.92 2.00 5.12  2.11 2.20 5.63  7.35  8.08  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  0.69 0.34 3.84  0.87 0.43 4.84  0.16  0.21  .  g Fe sampled 0.000175799 0.002651049 0.007855799  Tot. Fe Sample Fe in sol'n (g) 0.00018 0.00283 0.01068  0.014185116 0.065650665 0.17668812 0.2184 0.00161  Arsenic Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 104.77 1 7.07 104.61 0.0003975 0.00040 0.008316495 2 19.96 104.10 0.0003975 0.00080 0.00827595 3 27.97 105.70 0.000995 0.00179 0.0210343 Filtrate 35.99 103.39 0.03 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 104.77 1 7.07 104.61 0.000005 0.00001 0.00010461 2 19.96 104.10 0.0000025 0.00001 0.00005205 3 27.97 105.70 0.000025 0.00003 0.0005285 Filtrate 35.99 103.39 0.00 Wash 250.00 0.00  Mesophiles, 5 g Enargite, P Test #B5-M10  8 0  of 10 microns  Mesophiles  Date  Hour  Time Initial (days) Mass (g)  11-Apr 15-Apr 18-Apr 19-Apr 23-Apr 24-Apr 26-Apr 29-Apr 30-Apr 3-May  15:50 10:45 11:10 11:05 10:10 19:50 11:20 10:25 11:20 10:50  0.00 3.79 6.81 7.80 11.76 13.17 14.81 17.77 18.81 21.79  243.65 242.16 240.60 243.53 241.61 243.53 242.86 243.10 242.56 241.16  1.59 1.81 1.73 1.81 1.55 1.57 1.61 1.50 1.45 1.46  365 398 505 509 552 524 538 542 546 534  585 618 725 729 772 744 758 762 766 754  7-May 10-May 14-May 16-May 17-May  10:25 10:45 11:20 10:30 11:15  25.77 28.79 32.81 34.78 35.81  242.39 242.59 242.56 243.32 242.66  1.39 1.40 1.34 1.26 1.27  575 609 630 637 647  795 829 850 857 867  Analysis  Copper 31.2  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 PLS (mg/L) Wash (mg/L) Solid Residue (wt"/  178.60 0  Enargite In (g):  5.01 14.18  Total Water (g):  Vol (mL) Mass (g) Flask Weight (g): •• '•' i"*l*">< 133.91 Innoculum in: 10 10 Medium in: 95.04 95.04 242.66 Total Final Weight (g): ,s j . . . 102.76 Filtrate Volume (mL) Wash Volume (mL) 250 •~ . . ' ^ 3.56 Solid Residue (g) ;  Added Sample Medium Final E (Ag/AgCI) E (mV) (mL) Added (mL) Water (g) Mass (g) h  PH  Head (wt %)  h  Weight of Element  l  f  e  . - - . V - i i s . - •. • . ! . ' " * . - .  Calculated Head (g % Difference  % Extraction  Calculated Head Measured Head  5  5  5  Iron 11.6  Arsenic 10.5  Antimony 0.55  489.60 0.10  28.5 0  2.5 0  ;  140.5 94.5 91.5 49.5 519.5 0.3 13  0.5 1.0 4.5  0.6  • " l i f e  Iron  Arsenic  Antimony  0.58116 0.52605 0.0049 0.0003 0.00955 0  0.027555 0.0000 0  0.00062 0.0019 0.00371 0.00733  0.000703 0 0.000473 0.0000025 0.000458 0.000005 0.000248 0.0000225  0.0005 0 0.0005 0 0.0005 0 0.3310 0.0534 0.00492 0.000075 0.22428 0.4628 -  0 0 0 0.0000 0 0.02136  *«.: # !  1.639 -4.876  0.550 5.282  23.99 25.16  59.26 56.13  0.518 1.605 . . .  10.59 10.42  3.31  243.91  2.35  243.96  1.30  244.16  2.87  244.03  1.60 1.44 1.31  243.99 244.03 243.87  5  5  Copper  Head (g) 1.56312 Innoculum (g) 0.0018 Medium (g) 0 Samples (g): #1 0.011756 #2 0.013262 #3 0.01356 #4 0.013675 Medium Added (g): #1 0 #2 0 #3 0 0.3459 PLS (g) Wash (g) 0.010643 1.246 Solid Residue (g)  5  5  2351.20 124.00 2652.30 380.00 2711.95 741.45 2734.95 1466.80 3366.10 3220.95 42.57 19.68 35 6.3 H  5  0.021 22.546 • •'  4 i  - ••  -0.08 -0.06  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 104.73 0.00 1 7.80 104.61 0.011756 2 13.17 104.61 0.0132615 3 18.81 102.24 0.01355975 4 28.79 102.24 0.01367475 35.81 102.76 Filtrate Wash 250.00  Tot. Cu Sampled (g) 0.01176 0.02502 0.03858 0.05225  Cu in sol'n (g) Cu(aq) total (g) 0.246 0.277 0.277 0.280 0.346 0.011  %Cu indicated %Cu actual  0.244 0.287 0.301 0.316 0.383 0.393  15.62 18.39 19.22 20.24  14.89 17.53 18.33 19.30  25.16  23.99  Fe(aq) total  %Fe indicated  %Fe actual  0.01 0.03 0.07 0.15 0.33 0.33  1.39 6.00 12.20 25.27  1.47 6.33 12.88 26.68  56.96  60.13  As(aq) total  %As indicated  %As actual  0.01 0.01 0.01 0.01 0.05 0.05  2.74 1.96 1.95 1.22  2.78 1.99 1.98 1.24  10.42  10.59  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00 0.00  -0.09 0.10 0.29 1.61  -0.12 0.13 0.37 2.07  -0.06  -0.08  Iron Output  Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.00 104.73 1 7.80 104.61 0.000117799 0.01297164 0.00012 13.17 104.61 0.001397799 2 0.00152 0.0397518 3 18.81 102.24 0.003205049 0.00472 0.075805848 4 28.79 103.47 -0.323650822 -0.31893 0.151769796 Filtrate 35.81 102.76 0.3310 Wash 250.00 0.00492  Arsenic Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 104.73 1 7.80 104.61 0.0007025 0.00070 0.014697705 13.17 104.61 0.0004725 2 0.00118 0.009885645 3 18.81 102.24 0.0004575 0.00163 0.00935496 4 28.79 102.24 0.0002475 0.00188 0.00506088 Filtrate 35.81 102.76 0.05 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 104.73 104.61 1 7.80 0 0.00000 0 2 13.17 104.61 0.0000025 0.00000 0.000052305 0.00010224 3 18.81 102.24 0.000005 0.00001 4 28.79 102.24 0.0000225 0.00003 0.00046008 35.81 102.76 0.00 Filtrate 250.00 0.00 Wash  Mesophiles, 5 g Enargite, P Test UB5-M15  8 0  of 15 microns  Mesophiles  Date  Hour  Time (days)  Initial Mass (g)  pH  11-Apr 15-Apr 18-Apr 19-Apr 23-Apr 24-Apr 26-Apr 29-Apr 30-Apr 3-May  15:50 10:45 11:10 11:05 10:10 19:50 11:20 10:25 11:20 10:50  0.00 3.79 6.81 7.80 11.76 13.17 14.81 17.77 18.81 21.79  225.49 224.35 223.33 226.27 225.30 225.01 224.69 224.43 224.19 222.59  1.58 1.92 1.85 1.83 1.60 1.66 1.61 1.59 1.50 1.58  367 404 532 539 563 558 571 569 584 569  587 624 752 759 783 778 791 789 804 789  7-May 10-May 14-May 16-May 17-May  10:25 10:45 11:20 10:30 11:15  25.77 28.79 32.81 34.78 35.81  224.97 224.12 224.65 224.99 224.82  1.47 1.38 1.30 1.25 1.25  629 639 629 638 639  849 859 849 858 859  Copper 30.4 178.60 0  Enargite In (g):  Total Water (g):  4.99 10,15  Vol (mL) Mass (g) Flask Weight (g): 115.83 ' „ * ^ ' , . Innoculum in: 10 10 Medium in: 95.04 95.04 224.82 Total Final Weight (g): Filtrate Volume (mL) 101.39 •, , " '''}• Wash Volume (mL) 250 • "3 Solid Residue (g) 3.24 S3  Sample (mL)  E (Ag/AgCI) E h(mV) h  Analysis  Head (wt %)  Medium Added Final Added (mL) Water (g) Mass (g)  5  5  5  5  5  5  Iron 10.6  Arsenic 10.5  Antimony 0.55  489.60 0.10044  28.5 0  2.5 0  31.0 51.0 50.5 139.5 405.0 1.4 14  0.5 2.0 4.0 12.0 21.5 0.3 0.7  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 PLS (mg/L) Wash (mg/L) Solid Residue (wt °/  2224.65 230.50 2393.10 812.00 2617.85 1235.65 2559.45 2870.20 2868.45 4126.75 41.75 51.65 39 1.9084  Weight of Element  Copper  Arsenic  Antimony  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g) <s?'V" ^vfsc? Calculated Head (g % Difference  1.51696 0.52894 0.52395 0.0018 0.0049 0.0003 0 0.00955 0  0.027445 0.0000 0  0.011123 0.011966 0.013089 0.012797  .  1.599 -5.425  0.489 7.627  20.99 22.13  87.34 80.68  0.62  225.31  3.18  225.77  1.61 1.00 0.55  225.73 225.65 225.54  0.000155 0.0000025 0.000255 0.00001 0.000253 0.00002 0.000698 0.00006  0 0.0005 0 0 0.0005 0 0 0.0005 0 0.2908 0.4184 0.0411 0.010438 0.01291 0.00035 1.2636 0.06183 0.4536  % Extraction  Calculated Head Measured Head  0.00115 0.00406 0.00618 0.01435  226.52  5  5  Iron  3.19  ;  0 0 0 0.0022 0.000075 0.02268  :K<~ '•  0.495 5.451  0.025 9.119 . • ~4-~ i •  .~H.'. .-. :  8.44 7.98  9.07 8.24  157  Copper Output Sample #  Time (days) Sol'n Vol. (mL) 0.00 7.80 13.17 18.81 28.79 35.81  1 2 3 4 Filtrate Wash  104.67 105.45 104.19 101.77 101.77 101.39 250.00  g Cu sampled  Tot. Cu Sampled (g)  0.01112325 0.0119655 0.01308925 0.01279725  0.01112 0.02309 0.03618 0.04898  Cu in sol'n (g) Cu(aq) total (g)  %Cu indicated  %Cu actual  0.235 0.249 0.266 0.260 0.291 0.010  0.233 0.259 0.288 0.295 0.325 0.336  15.35 17.05 18.97 19.44  14.56 16.17 17.99 18.44  22.13  20.99  Iron Output Sample # 1 2 3 4 Filtrate Wash  Arsenic  Time (days) Sol'n Vol. (mL) 0.00 104.67 7.80 105.45 13.17 104.19 18.81 101.77 28.79 104.15 35.81 101.39 250.00  g Fe sampled  Tot. Fe Sample  Fe in sol'n (g)  Fe(aq) total  %Fe indicated  %Fe actual  0.000650299 0.003557799 0.005676049 -0.404060183  0.00065 0.00421 0.00988 -0.39418  0.024 0.085 0.126 0.299 0.4184 0.0129125  0.02 0.08 0.12 0.29 0.41 0.43  3.67 15.07 22.85 55.59  3.97 16.31 24.74 60.18  80.62  87.28  As(aq) total  %As indicated  %As actual  0.00 0.01 0.01 0.01 0.04 0.04  0.57 0.99 1.00 2.78  0.60 1.05 1.06 2.94  7.98  8.44  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00 0.00  0.10 0.68 1.44 4.48  0.11 0.75 1.58 4.93  8.24  9.07  Output  Sample # 1 2 3 4 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.00 104.67 7.80 105.45 13.17 104.19 18.81 101.77 28.79 101.77 35.81 101.39 250.00  g As sampled 0.000155 0.000255 0.0002525 0.0006975  Tot. As Sample As in sol'n (g) 0.00016 0.00041 0.00066 0.00136  0.00326895 0.00531369 0.005139385 0.014196915 0.04 0.00  Antimony Output Sample # 1 2 3 4 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.0000 104.67 7.80 105.45 13.17 104.19 18.81 101.77 28.79 101.77 35.81 101.39 250.00  g Sb sampled 0.0000025 0.00001 0.00002 0.00006  Tot. Sb Sample Sb in sol'n (g) 0.00000 0.00001 0.00003 0.00009  0.000052725 0.00020838 0.00040708 0.00122124 0.00 0.00  Mesophiles, 5 g Enargite, P Test #BS-M37  8 0  of 37 microns  Mesophiles  Date  Hour  Time Initial (days) Mass (g)  11-Apr 15-Apr 18-Apr 19-Apr 23-Apr 24-Apr 26-Apr 29-Apr 30-Apr 3-May  15:50 10:45 11:10 11:05 10:10 19:50 11:20 10:25 11:20 10:50  0.00 3.79 6.81 7.80 11.76 13.17 14.81 17.77 18.81 21.79  256.08 254.49 253.12 255.73 254.94 256.91 256.16 255.26 254.81 253.31  1.60 1.84 1.73 1.74 1.55 1.56 1.55 1.51 1.46 1.51  367 404 508 526 540 531 538 544 554 551  587 624 728 746 760 751 758 764 774 771  7-May 10-May 14-May 16-May 17-May  10:25 10:45 11:20 10:30 11:15  25.77 28.79 32.81 34.78 35.81  225.46 254.51 254.77 255.54 256.13  1.40 1.37 1.30 1.25 1.24  586 625 627 637 644  806 845 847 857 864  Analysis Head (wt %)  Copper 32.4  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 PLS (mg/L) Wash (mg/L) Solid Residue (wt °/  178.60 0  Weight of Element  Copper  Enargite In (g):  Total Water (g):  5.01 13.61  Vol(mL) Mass(g) Flask Weight (g): 146.07 "• Innoculum in: 10 10 Medium in: 95.05 95.05 256.13 Total Final Weight (g): • 100.95 Filtrate Volume (mL) Wash Volume (mL) 250 3.40 Solid Residue (g) ":*yfV... •  PH  E„ Sample Medium Added Final (Ag/AgCI) E(mV) (mL) Added (mL) Water (g) Mass (g) h  5  5  5  5  5  5  5  5  Iron 7.2  Arsenic 12  Antimony 0.39  489.60 0.10044  28.5 0  2.5 0  2119.20 106.00 2683.45 376.20 2798.90 744.30 2774.20 1448.25 3072.60 3254.30 52.67 44.05 35 5.4  119.5 85.0 97.5 52.0 556.5 1.9 12  0.0 0.0 1.0 4.0 19.0 0.3 0.6  Iron  Arsenic  Antimony  0.36072 0.0049 0.00955  0.6012 0.0003 0  0.019539 0.0000 0  0.00053 0.00188 0.00372 0.00724  0.000598 0.000425 0.000488 0.00026  0 0 0.000005 0.00002  Head (g) 1.62324 Innoculum (g) 0.0018 Medium (g) 0 Samples (g): #1 0.010596 #2 0.013417 #3 0.013995 #4 0.013871 Medium Added (g): #1 0 #2 0 #3 0 PLS (g) 0.3102 Wash (g) 0.013168 Solid Residue (g) 1.19 ' .• - : Calculated Head (g 1.550 % Difference 4.539 % Extraction • . •:.'<!!?* • Calculated Head 23.20 Measured Head 22.15  '• 7i ':  0.0005 0 0.0005 0 0.0005 0 0.3285 0.0562 0.01101 0.000475 0.1836 0.408 ...'.li •"; \:..>:^ 0.513 0.466 -42.303 22.509 64.23 91.41  ti  ''rfp  12.42 9.63  0 0 0 0.0019 0.000075 0.0204 V • 0.022 -14.505 "" - X F 8.82 10.10  3.10  256.22  2.46  257.40  3.65  256.96  1.68 1.74 0.98  256.19 256.51 256.52  Copper Output Sample #  Time (days) Sol'n Vol. (mL) 0.00 7.80 13.17 18.81 28.79 35.81  1 2 3 4 Filtrate Wash  105.00 104.65 105.83 102.23 102.23 100.95 250.00  g Cu sampled  Tot. Cu Sampled (g)  0.010596 0.01341725 0.0139945 0.013871  0.01060 0.02401 0.03801 0.05188  Cu in sol'n (g) Cu(aq) total (g)  %Cu indicated  %Cu actual  0.222 0.284 0.286 0.284 0.310 0.013  0.220 0.293 0.308 0.320 0.346 0.360  13.55 18.04 19.00 19.70  14.20 18.90 19.90 20.64  22.15  23.20  Iron Output Sample # 1 2 3 4 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.00 105.00 7.80 104.65 13.17 105.83 18.81 102.23 28.79 74.38 35.81 100.95 250.00  g Fe sampled  Tot. Fe Sample  Fe in sol'n (g)  Fe(aq)total  %Fe indicated  %Fe actual  2.77986E-05 0.001378799 0.003219299 -0.321280335  0.00003 0.00141 0.00463 -0.31665  0.0110929 0.039813246 0.076089789 0.107720835 0.3285 0.0110125  0.01 0.03 0.07 0.10 0.32 0.33  1.72 9.68 19.74 28.51  1.21 6.80 13.87 20.03  92.77  65.19  As(aq)total  %As indicated  %As actual  0.01 0.01 0.01 0.01 0.06 0.06  2.03 1.55 1.78 1.09  2.62 2.00 2.30 1.40  9.63  12.42  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00 0.00  -0.13 -0.13 0.40 1.99  -0.11 -0.11 0.35 1.74  10.10  8.82  Arsenic Output Sample # 1 2 3 4 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.00 105.00 7.80 104.65 13.17 105.83 18.81 102.23 28.79 102.23 35.81 100.95 250.00  g As sampled 0.0005975 0.000425 0.0004875 0.00026  Tot. As Sample As in sol'n (g) 0.00060 0.00102 0.00151 0.00177  0.012505675 0.00899555 0.009967425 0.00531596 0.06 0.00  Antimony Output Sample # 1 2 3 4 Filtrate Wash  Time (days) Sol'n Vol. (mL) 0.0000 105.00 7.80 104.65 13.17 105.83 18.81 102.23 28.79 102.23 35.81 100.95 250.00  g Sb sampled 0 0 0.000005 0.00002  Tot. Sb Sample Sb in sol'n (g) 0.00000 0.00000 0.00001 0.00003  0 0 0.00010223 0.00040892 0.00 0.00  Mesophiles, 10 g Enargite, P Test MB2-M10 T i m e D a t e  20-Dec 23-Dec 28-Dec 31-Dec 3-Jan 8-Jan 11-Jan 15-Jan 18-Jan 22-Jan 25-Jan  E n a r g i t e  I n (g):  Total Water (g):  B 0  of 10 microns  Mesophiles  H o u r  9:30 9:30 9:45 12:55 15:50 10:05 10:05 11:25 9:25 11:30 10:05  ( d a y s )  0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  10.00 • 24.87  Vol (mL) Mass (g) Flask Weight (g): 132.12 Innoculum in: io' 10 Medium in: 95.01 95.01 Total Final Weight (g): '' ^Vfv.f:" 245.24 Filtrate Volume (mL) 98.72 i-'.-'-jy'fjl Wash Volume (mL) 250 Solid Residue (g) 6.40  I n i t i a l M a s s  E „ ( g )  P H  246.64 244.14 241.18 243.09 243.86 242.05 245.52 245.34 245.61 245.12 245.24  S a m p l e  ( A g / A g C I )  1.56 1.76 1.68 1.60 1.42 1.32 1.32 1.26 1.21  430 442 531 558 633 657 580 651 677 691 672  1.16  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 #5 #6 #7 #8 #9 PLS (mg/L) Wash (mg/L) Solid Residue (wt %)  -•IIS.  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 #5 #6 #7 #8 #9 Medium Added (g): #1 #2 #3  #4 #5 #6 #7 #8 #9 PLS (g) Wash (g) Solid Residue (g)  E x t r a c t i o n  ( m L )  5 5 5 5 5 5 5 5 5  Arsenic  Antimony  11.6 1291.15 0.10  10.5 39.5 0  0.55 3.0 0  2010.85 4452.85 4622.60 5473.20 6146.05 6343.35 6189.95 6561.10 6217.85 5418.35 132.81 35.2  260.90 253.10 337.80 1830.35 3373.50 3962.10 5642.50 7359.95 8577.95 7932.3 147.55 1.8  36.5 208.5 146.5 347.0 641.0 828.5 1215.5 1313.5 1245.0 1171 5.6 13.9  1.5 1.5 0.0 4.0 10.5 17.5 67.5 73.5 70.5 66.5 0.6 0.67  R-4  . ..;  Copper  .:  Iron  3.12 0.0134 0  Arsenic  Antimony  1.16 1.05 0.0129 0.0004 0.00954 0  0.055 0.0000 0  0.0100543 0.0222643 0.023113 0.027366 0.0307303 0.0317168 0.0309498 0.0328055 0.0310893  0.0013 0.00127 0.00169 0.00915 0.01687 0.01981 0.02821 0.0368 0.04289  0.00018 0.00104 0.00073 0.00174 0.00321 0.00414 0.00608 0.00657 0.00623  0.0000075 0.0000075 0 0.00002 0.0000525 0.0000875 0.0003375 0.0003675 0.0003525  0 0 0  0.0005 0.0005 0.0005  0 0 0  0 0 0  0 0 0 0 0 0 0.5349 0.0332025 2.2528  % Difference Calculated Head Measured Head  M e d i u m A d d e d  5 5 5 5 5 5 5 5 5  Iron  tmij,, -:,!mm3.048 Calculated Head (g) %  ( m L )  31.2 1337.45 0  ,.  Weight of Element  ( m V )  650 662 751 778 853 877 800 871 897 911 892  Copper  A n a l y s i s  E „  •••  0 0 0 0 0 0 0.0066 0.00015 0.04288 trtjt  2.320 '  0.0005 0 0.0005 0 0.0005 0 0.0005 0 0.0005 0 0.0005 0 0.7831 0.1156 0.03689 0.0014 0.1152 0.8896  * J o * •.  26.08 25.47  1.066 8.088  1.036 1.322  •  : -sp".  89.20 81.98  14.14 13.95  -  •  0.051 7.641 15.59 14.40  A d d e d W a t e r  F i n a l ( g )  2.54 5.53 3.73 2.94 4.83 1.24 1.25 1.14 1.67  M a s s  ( g )  246.68 246.71 246.82 246.80 246.88 246.76 246.59 246.75 246.79  Copper Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  Sol'n Vol. (mL) 104.52 102.02 99.06 100.97 101.74 99.93 103.40 103.22 103.49 103.00 98.72 250.00  Total Cu g Cu sampled Removed (g)  Sol'n Vol. (mL) 104.52 102.02 99.06 100.97 101.74 99.93 103.40 103.22 103.49 103.00 98.72 250.00  Sol'n Vol. (mL) 104.52 102.02 99.06 100.97 101.74 99.93 103.40 103.22 103.49 103.00 98.72 250.00  Time Sol'n Vol. (days) (mL) 0.0000 104.52 3.0000 102.02 8.0104 99.06 11.1424 100.97 14.2639 101.74 19.0243 99.93 22.0243 103.40 26.0799 103.22 28.9965 103.49 33.0833 103.00 36.0243 98.72 250.00  0.01005 0.02226 0.02311 0.02737 0.03073 0.03172 0.03095 0.03281 0.03109  0.01005 0.03232 0.05543 0.08280 0.11353 0.14524 0.17619 0.20900 0.24009  Cu in sol'n (g)  Cu (aq) %Cu total (g) indicated  %Cu actual  0.205 0.441 0.467 0.557 0.614 0.656 0.639 0.679 0.640 0.535 0.033  0.192 0.438 0.486 0.599 0.684 0.756 0.771 0.842 0.836 0.762 0.795  6.15 14.03 15.57 19.20 21.91 24.23 24.71 26.98 26.80 24.41 25.47  6.29 14.36 15.94 19.65 22.43 24.81 25.29 27.62 27.43 24.99 26.08  g Fe Total Fe sampled Removed (g)  Fe in sol'n (g)  Fe (aq) total  %Fe indicated  %Fe actual  0.0008 0.00076 0.00119 0.00865 0.01637 0.01931 0.02771 0.0363 0.04239  0.026617 0.025072 0.034108 0.18622 0.337114 0.409681 0.582419 0.761681 0.883529 0.7831 0.036888  0.01 0.01 0.02 0.17 0.32 0.40 0.57 0.75 0.87 0.77 0.81  1.18 105 1.83 14.94 27.95 34.20 49.10 64.55 75.05 66.39 69.57  1.29 1.14 1.99 16.26 30.41 37.21 53.42 70.23 81.66 72.24 75.70  Total As g As sampled Removed (g)  As in sol'n (g)  As(aq) total  %As indicated  %As actual  0.00018 0.00104 0.00073 0.00174 0.00321 0.00414 0.00608 0.00657 0.00623  0.003724 0.020654 0.014792 0.035304 0.064055 0.085667 0.125464 0.135934 0.128235 0.12 0.00  0.00 0.02 0.02 0.04 0.07 0.09 0.14 0.15 0.15 0.15 0.15  0.32 1.95 1.49 3.51 6.41 8.78 12.96 14.54 14.43 13.82 13.95  0.32 1.97 1.51 3.56 6.50 8.90 13.14 14.73 14.62 14.01 14.14  gSb Total Sb sampled Removed (g)  Sb in sol'n (g)  Sb (aq) total  %Sb indicated  %Sb actual  7.5E-06 7.5E-06 0 0.00002 5.3E-05 8.8E-05 0.00034 0.00037 0.00035  0.000153 0.000149 0 0.000407 0.001049 0.00181 0.006967 0.007607 0.007262 0.01 0.00  0.00 0.00 0.00 0.00 0.00 0.00 0.01 0.01 0.01 0.01 0.01  0.22 0.23 -0.03 0.71 1.92 3.39 12.93 14.71 14.75 14.12 14.40  0.24 0.25 -0.03 0.77 2.08 3.68 14.00 15.92 15.97 15.29 15.59  Iron Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  0.00080 0.00157 0.00275 0.01140 0.02777 0.04708 0.07479 0.11108 0.15347  Arsenic Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  0.00018 0.00123 0.00196 0.00369 0.00690 0.01104 0.01712 0.02369 0.02991  Antimony Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  0.00001 0.00002 0.00002 0.00004 0.00009 0.00018 0.00051 0.00088 0.00123  162  Mesophiles, 10 g Enargite, P  Test #B2-M15  8 0  of 15 microns  Mesophiles Time  Initial  Date  Hour  (days)  M a s s (g)  pH  (Ag/AgCI)  E„  20-Dec  9:30  0.00  245.48  1.54  420  640  23-Dec  9:30  3.00  242.70  1.93  473  28-Dec  9:45  8.01  239.62  1.78  526  31-Dec  12:55  11.14  242.60  1.62  3-Jan  15:50  14.26  242.41  8-Jan  10:05  19.02  11-Jan  10:05  15-Jan  Sample  Medium  Added  Final  (mL)  A d d e d (mL)  W a t e r (g)  M a s s (g)  693  5  5  2.45  245.15  746  5  5  6.53  246.15  550  770  5  5  2.82  245.42  1.37  652  872  5  5  3.02  245.43  240.85  1.26  675  895  5  5  5.99  246.84  22.02  245.40  1.20  672  892  5  5  1.35  246.75  11:25  26.08  244.93  1.35  698  918  5  5  1.48  246.41  18-Jan  9:25  29.00  245.19  1.21  704  924  5  5  1.38  246.57  22-Jan  11:30  33.08  244.73  5  5  1.38  246.11  25-Jan  10:05  36.02  244.43  1.21  E n a r g i t e In (g):  10.00  Analysis  Total W a t e r (g):  26.40  H e a d (wt %)  674  Copper  Innoculum (mg/L) M e d i u m (g/L)  E  (mV)  h  894  Iron  Arsenic  Antimony  30.4  10.6  10.5  0.55  1337.45  1291.15  39.5  3.0  0  0.10044  0  0  S a m p l e s (mg/L): V o l (mL)  M a s s (g)  #1  1985.55  212.60  13.0  0.0  130.99  #2  5236.00  195.75  212.0  0.5  10  10  #3  6428.45  247.65  294.0  0.5  95.01  95.01  #4  7153.05  2067.00  512.5  7.5  244.43  #5  7322.05  5735.45  1300.5  53.5  •{'.  #6  6736.85  5465.75  1076.5  63.0  f 6.43 ;  #7  6517.60  5624.40  1070.5  64.0  #8  6622.65  6084.50  1122.0  64.0  #9  6164.30  5918.30  1052.5  62.0  P L S (mg/L)  5499.85  5613.5  994  58  99.67  63.26  2.4  0.4  34  4.6  Flask W e i g h t (g): Innoculum in: M e d i u m in: Total Final W e i g h t (g): Filtrate V o l u m e (mL) W a s h V o l u m e (mL) Solid R e s i d u e (g)  100.77 250  • f  W a s h (mg/L) Solid R e s i d u e (wt %)  13.1  ' i ' •' ' Weight of Element  H e a d (g)  Copper  Iron  Arsenic  0.69 .  ',- - »  v  Antimony  3.04  1.06  1.05  0.055  0.0134  0.0129  0.0004  0.0000  0  0.00954  0  0  #1  0.0099278  0.00106  6.5E-05  0  #2  0.02618  0.00098  0.00106  0.0000025  #3  0.0321423  0.00124  0.00147  0.0000025  #4  0.0357653  0.01034  0.00256  0.0000375  #5  0.0366103  0.02868  0.0065  0.0002675  #6  0.0336843  0.02733  0.00538  0.000315  #7  0.032588  0.02812  0.00535  0.00032  #8  0.0331133  0.03042  0.00561  0.00032  #9  0.0308215  0.02959  0.00526  0.00031  #1  0  0.0005  0  0  #2  0  0.0005  0  0  #3  0  0.0005  0  0  #4  0  0.0005  0  0  #5  0  0.0005  0  0  #6  0  0.0005  0  0  #7  0  0.0005  0  0  #8  0  0.0005  0  0  #9  0  0.0005  0  0  0.5542  0.5657  0.1002  0.0058  0.0249175  0.01582  0.0006  0.0001  2.1862  0.29578  0.84233  0.044367  Calculated H e a d (g)  3.023  1.008  0.976  0.052  % Difference  0.566  4.901  7.051  5.715  % Extraction Calculated H e a d  u:.27.68  70.66  13.69  14.44  Measured Head  27.52  67.20  12.73  13.62  Innoculum (g) M e d i u m (g) S a m p l e s (g):  M e d i u m A d d e d (g):  P L S (g) W a s h (g) Solid R e s i d u e (g)  :•»-•  '-;'  Copper Output Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  Sol'n Vol. g Cu (mL) sampled  Total Cu Removed (g)  Cu in sol'n (g)  Cu (aq) total (g)  %Cu indicated  %Cu actual  0.00993 0.03611 0.06825 0.10402 0.14063 0.17431 0.20690 0.24001 0.27083  0.202 0.516 0.653 0.725 0.731 0.703 0.677 0.690 0.639 0.554 0.025  0.189 0.513 0.676 0.780 0.822 0.831 0.838 0.884 0.866 0.812 0.837  6.20 16.87 22.23 25.67 27.03 27.32 27.58 29.07 28.49 26.70 27.52  6.24 16.97 22.36 25.82 27.19 27.48 27.74 29.23 28.65 26.85 27.68  Sol'n Vol. g Fe (mL) sampled 104.49 101.71 0.00056 98.63 0.00048 101.61 0.00074 101.42 0.00983 99.86 0.02818 104.41 0.02683 103.94 0.02762 104.20 0.02992 103.74 0.02909 100.77 250.00  Total Fe Removed (g)  Fe in sol'n (g)  Fe (aq) total  %Fe indicated  %Fe actual  0.00056 0.00104 0.00177 0.01161 0.03978 0.06661 0.09423 0.12415 0.15324  0.022 0.019 0.025 0.210 0.573 ' 0.571 0.585 0.634 0.614 0.5657 0.015815  0.01 0.01 0.01 0.20 0.56 0.56 0.57 0.62 0.60 0.55 0.57  0.82 0.60 1.16 18.56 52.81 52.62 53.93 58.59 56.70 52.15 53.64  0.86 0.63 1.22 19.52 55.54 55.33 56.71 61.61 59.63 54.83 56.40  Sol'n Vol. g As (mL) sampled 104.49 101.71 6.5E-05 98.63 0.00106 101.61 0.00147 101.42 0.00256 99.86 0.0065 104.41 0.00538 103.94 0.00535 104.20 0.00561 103.74 0.00526 100.77 250.00  Total A s Removed (g)  As in sol'n (g)  As (aq) total  %As indicated  %As actual  0.00007 0.00113 0.00260 0.00516 0.01166 0.01704 0.02240 0.02801 0.03327  0.001322 0.02091 0.029873 0.051978 0.129868 0.112397 0.111268 0.116912 0.109186 0.10 0.00  0.00 0.02 0.03 0.05 0.13 0.12 0.13 0.14 0.14 0.13 0.13  0.09 1.96 2.91 5.16 12.82 11.78 12.18 13.23 13.03 12.67 12.73  0.10 2.11 3.14 5.55 13.79 12.67 13.11 14.23 14.02 13.63 13.69  Sol'n Vol. gSb (mL) sampled 104.49 101.71 0 98.63 2.5E-06 101.61 2.5E-06 101.42 3.8E-05 99.86 0.00027 104.41 0.00032 103.94 0.00032 104.20 0.00032 103.74 0.00031 100.77 250.00  Total Sb Removed (g)  Sb in sol'n (g)  Sb (aq) total  %Sb indicated  %Sb actual  0.00000 0.00000 0.00001 0.00004 0.00031 0.00063 0.00095 0.00127 0.00158  0 4.93E-05 5.08E-05 0.000761 0.005343 0.006578 0.006652 0.006669 0.006432 0.01 0.00  0.00 0.00 0.00 0.00 0.01 0.01 0.01 0.01 0.01 0.01 0.01  -0.05 0.04 0.04 1.34 9.74 12.47 13.18  -0.06 0.04 0.04 1.42 10.33 13.22 13.98  13.79 13.94 13.44 13.62  14.62 14.78 14.25 14.44  104.49 101.71 98.63 101.61 101.42 99.86 104.41 103.94 104.20 103.74 100.77 250.00  0.00993 0.02618 0.03214 0.03577 0.03661 0.03368 0.03259 0.03311 0.03082  Iron Output Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  Arsenic Output Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  Antimony Output Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.0000 3.0000 8.0104 11.1424 14.2639 19.0243 22.0243 26.0799 28.9965 33.0833 36.0243  Mesophiles, 10 g Enargite (2), P Test XB7-M15  8 0  of 15 microns  Mesophiles Initial Mass (g) 245.86 244.90 246.29 246.09 244.85 246.11 245.98  12:00 12:00  Time (days) 0.00 1.93 5.88 6.95 9.87 13.91 14.98 16.94 20.94  245.04 243.96  pH 1.60 2.25 1.94 1.90 1.66 1.52 1.42 1.46 1.43  7-Aug  12:30  21.96  245.66  1.39  612  832  9-Aug 12-Aug 13-Aug 16-Aug 20-Aug 21-Aug  12:45 12:10 12:10 13:50 13:15 13:05  23.97 26.94 27.94 31.01 34.99 35.98  244.90 245.54 245.35 244.16 245.84 245.65  1.30 1.23 1.26 1.21 1.22 1.22  664 685 693 700 711 708  884 905 913 920 931 928  Analysis Head (wt-%)  Copper 30.4  Iron 10.6  Arsenic 10.5  Antimony 0.55  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 PLS (mg/L) Wash (mg/L)  383.25 0  1305.50 0.1004  55.5 0  0  5193.50 6757.20 7174.55 7031.45 6628.95 99.91  251.10 1791.50 3593.95 6953.55 8613.40 116.39  51.0 311.5 779.0 1037.0 956.5  38  0.8654  Date 16-Jul 18-Jul 22-Jul 23-Jul 26-Jul 30-Jul 31-Jul  Hour 13:30 11:55 10:35 12:20 10:20 11:15 13:05  2-Aug 6-Aug  Enargite In (g): Total Water (g):  10.01 9.50  Vol (mL) Mass (g) Flask Weight (g): 130.70 • •' . Innoculum in: 10 10 Medium in: 95.06 95.06 Total Final Weight (g): v". ••• . . . 245.65 " : — Filtrate Volume (mL) 103.83 !  1  Wash Volume (mL) Solid Residue (g)  1  250  E„  Solid Residue (wt % 6.01 Weight of Element  (Ag/AgCI) E (mV) 449 669 362 582 491 711 509 729 540 760 523 743 549 769 558 778 625 845 h  ••jt'v";;i.. VCopper *<t'.i. Iron  Sample (mL)  Medium Added Added (mL) Water (g)  5  5  5  5  5  5  5  247.53  2.79  247.64  1.96  245.92  0.62  246.16  1.50  247.34  5.2 14 •".',!: " - '  0.7 ^ v ;  ;Hi:  s  Arsenic  Antimony  3.04304 0.0038 0  1.0611 0.0131 0.0095  1.05105 0.0006 0  0.055055 0.0000 0  0.025968 0.033786 0.035873 0.035157  0.0013 0.009 0.018 0.0348  0.000255 0.001558 0.003895 0.005185  0 0 0 0  Medium Added (g): #1 #2 #3 #4 PLS (g) Wash (g) Solid Residue (g)  0 0 0 0 0.6883 0.024978 2.2838  0.0005 0.0005 0.0005 0.0005 0.8943 0.0291 0.052  0 0 0 0 0.0993 0.0013 0.8414  0 0 0 0 0.0000 0 0.04207  • ...  2.63 5  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4  Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  Final Mass (g)  ...  3.089 -1.506  0.980 7.686  0.947 9.884  0.042 23.586  26.06 26.46  94.69 87.41  11.17 10.06  0.00 0.00  165  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.15 1 6.95 105.38 0.0259675 14.98 2 105.27 0.033786 3 21.96 104.95 0.03587275 4 27.94 104.64 0.03515725 Filtrate 35.98 103.83 Wash 250.00  Tot. Cu Sampled (g) 0.02597 0.05975 0.09563 0.13078  Cu in sol'n (g) Cu(aq) total (g) 0.547 0.711 0.753 0.736 0.688 0.025  %Cu indicated %Cu actual  0.543 0.733 0.809 0.828 0.780 0.805  17.86 24.10 26.58 27.20  17.59 23.75 26.19 26.79  26.46  26.06  Fe(aq) total  %Fe indicated  %Fe actual  0.01 0.18 0.36 0.71 0.88 0.91  1.26 16.54 34.32 67.34  1.37 17.92 37.17 72.95  85.80  92.94  As(aq) total  %As indicated  %As actual  0.00 0.03 0.08 0.11 0.10 0.11  0.46 3.09 7.90 10.81  0.51 3.43 8.76 12.00  10.06  11.17  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00 0.00  0.00 0.00 0.00 0.00  0.00 0.00 0.00 0.00  0.00  0.00  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.15 1 6.95 105.38 14.98 2 105.27 3 21.96 104.95 4 27.94 . 104.64 35.98 Filtrate 103.83 Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.000753299 0.008455299 0.017467549 0.034265549  0.00075 0.00921 0.02668 0.06094  0.026 0.189 0.377 0.728 0.8943 0.0290975  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.15 1 6.95 105.38 0.000255 0.00026 0.00537438 2 14.98 105.27 0.0015575 0.00181 0.032791605 3 21.96 104.95 0.003895 0.00571 0.08175605 4 27.94 104.64 0.005185 0.01089 0.10851168 Filtrate 35.98 103.83 0.10 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb 0.00 105.15 1 6.95 105.38 2 14.98 105.27 3 21.96 104.95 4 27.94 104.64 35.98 Filtrate 103.83 Wash 250.00  sampled Tot. Sb Sample Sb in sol'n (g) 0 0 0 0  0.00000 0.00000 0.00000 0.00000  0 0 0 0 0.00 0.00  166  Mesophiles, 10 g Enargite, P Test #B2-M37  8 0  of 37 microns  Mesophiles  Date  Hour  20-Dec 23-Dec 28-Dec 31-Dec 3-Jan 8-Jan 11-Jan 15-Jan 18-Jan 22-Jan 25-Jan  9:30 9:30 9:45 12:55 15:50 10:05 10:05 11:25 9:25 11:30 10:05  Time (days) 0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  Initial Mass (g)  PH  252.70 249.69 229.94 236.34 248.98 247.16 251.43 251.31 251.74 250.96 251.26  1.56 1.68 1.59 1.50 1.46 1.28 1.26 1.36 1.29  Copper  10.00  Analysis  Total Water (g):  57.92  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 #5 #6 #7 #8 #9 PLS (mg/L) Wash (mg/L) Solid Residue (wt %)  2 4 5  439 440 514 534 606 659 665 683 699  659 660 734 754 826 879 885 903 919 220 220  1.29  Enargite In (g):  Vol (mL) Mass (g) Flask Weight (g): Ci' • '-"fi 138.23 Innoculum in: 10 10 Medium in: 94.98 94.98 Total Final Weight (g): I 251.26 Filtrate Volume (mL) 99.72 •. . .'. Wash Volume (mL) , iL^_Ji£i Solid Residue (g) iffi\\;;jj! 8.06  E„ Sample Medium Added (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g)  Weight of Element  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 #5 #6 #7 #8 #9 Medium Added (g): #1 #2 #3  #4 #5 #6 #7 #8 #9 PLS (g) Wash (g) Solid Residue (g) '  •.  .  5 5 5 5 5 5 5 5 5  Arsenic  Antimony  32.4 1337.45 0  7.2 1291.15 0.10044  12 39.5 0  0.39 3.0 0  1534.10 4730.65 5161.10 5063.85 5137.55 4885.00 4780.25 4844.40 4498.20 3984.8 91.49 32  265.40 330.60 227.05 428.35 1118.15 2047.00 2426.20 2768.50 2897.65 2673.4 33.40 4.4  38.5 565.5 671.0 674.5 65.0 497.0 566.5 622.5 636.5 620 1.4 12.7  0.0 0.0 0.0 0.0 0.0 4.0 7.0 7.0 8.0 16 0.3 0.42  Arsenic  Antimony  Copper  Iron  3.24 0.0134 0  0.72 0.0129 0.00954  1.2 0.0004 0  0.039 0.0000 0  0.0076705 0.0236533 0.0258055 0.0253193 0.0256878 0.024425 0.0239013 0.024222 0.022491  0.00133 0.00165 0.00114 0.00214 0.00559 0.01024 0.01213 0.01384 0.01449  0.00019 0.00283 0.00336 0.00337 0.00033 0.00249 0.00283 0.00311 0.00318  0 0 0 0 0 0.00002 0.000035 0.000035 0.00004  0 0 0  0.0005 0.0005 0.0005  0 0 0  0 0 0  0 0 0 0 0 0 0.3974 0.0224151 2.5792  0.0005 0 0.0005 0 0.0005 0 0.0005 0 0.0005 0 0.0005 0 0.2666 0.0618 0.00818 0.00034 0.35464 1.02362 "  ' *'/'"*'•  Calculated Head (g) % Difference  Iron  5 5 5 5 5 5 5 5 5  . *>"  3.189 1.581  0.665 7.641  1.107 7.743  19.12 18.81  46.67 43.10  7.54 6.95  0 0 0 0 0 0 0.0016 0.0000735 0.033852  .'-"jiv•• 0.036 8.664  % Extraction  Calculated Head Measured Head  4.97 4.54  3.53 22.84 16.37 3.28 5.83 1.59 1.62 0.98 1.88  Final Mass (g)  253.22 252.78 252.71 252.26 252.99 253.02 252.93 252.72 252.84  Copper Output Sample No.  Time (days)  0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  1 2 3 4 5 6 7 8 9 Filtrate Wash  Sol'n Vol. g Cu (mL) sampled  104.47 101.46 81.71 88.11 100.75 98.93 103.20 103.08 103.51 102.73 99.72 245.00  0.00767 0.02365 0.02581 0.02532 0.02569 0.02443 0.0239 0.02422 0.02249  Total Cu Removed (g)  Cu in sol'n (g)  Cu (aq) total (g)  %Cu indicated  %Cu actual  0.00767 0.03132 0.05713 0.08245 0.10814 0.13256 0.15646 0.18068 0.20318  0.156 0.387 0.455 0.510 0.508 0.504 0.493 0.501 0.462 0.397 0.022  0.142 0.381 0.473 0.554 0.577 0.599 0.612 0.645 0.629 0.587 0.610  4.39 11.75 14.59 17.10 17.82 18.48 18.89 19.89 19.43 18.12 18.81  4.46 11.94 14.82 17.37 18.11 18.78 19.19 20.21 19.74 18.41 19.12  Total Fe Removed (g)  Fe in sol'n (g)  Fe (aq) total  %Fe indicated  %Fe actual  0.00082 0.00198 0.00261 0.00425 0.00934 0.01907 0.03070 0.04404 0.05802  0.026927 0.027013 0.020005 0.043156 0.110619 0.21125 0.250093 0.286567 0.297676 0.2666 0.008183  0.01 0.01 0.01 0.03 0.10 0.20 0.24 0.27 0.28 0.25 0.26  1.95 1.96 0.99 4.20 13.57 27.55 32.94 38.01 39.55 35.23 36.37  2.11 2.12 1.07 4.55 14.69 29.83 35.67 41.15 42.82 38.15 39.38  Total As Removed (g)  As in sol'n (g)  As(aq) total  % As indicated  % As actual  0.00019 0.00302 0.00638 0.00975 0.01007 0.01256 0.01539 0.01850 0.02169  0.003906 0.046207 0.059122 0.067956 0.00643 0.05129 0.058395 0.064435 0.065388 0.06 0.00  0.00 0.05 0.06 0.07 0.02 0.06 0.07 0.08 0.08 0.08 0.08  0.29 3.83 5.15 6.16 1.32 5.08 5.88 6.62 6.96 6.93 6.95  0.32 4.16 5.58 6.68 1.43 5.51 6.37 7.17 7.54 7.51 7.54  Total Sb Removed (g)  Sb in sol'n (g)  Sb (aq) total  %Sb indicated  %Sb actual  0.00000 0.00000 0.00000 0.00000 0.00000 0.00002 0.00006 0.00009 0.00013  0 0 0 0 0 0.000413 0.000722 0.000725 0.000822 0.00 0.00  0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00  -0.08 -0.08 -0.08 -0.08 -0.08 0.98 1.82 1.92 2.26 4.35 4.54  -0.08 -0.08 -0.08 -0.08 -0.08 1.07 2.00 2.10 2.48 4.76 4.97  Iron Output Sample No.  1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days)  0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  Sol'n Vol. g Fe (mL) sampled  104.47 101.46 81.71 88.11 100.75 98.93 103.20 103.08 103.51 102.-73 99.72 245.00  0.00082 0.00115 0.00063 0.00164 0.00509 0.00973 0.01163 0.01334 0.01399  Arsenic Output Sample No.  1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days)  0.00 3.00 8.01 11.14 14.26 19.02 22.02 26.08 29.00 33.08 36.02  Sol'n Vol. g As (mL) sampled  104.47 101.46 81.71 88.11 100.75 98.93 103.20 103.08 103.51 102.73 99.72 245.00  0.00019 0.00283 0.00336 0.00337 0.00033 0.00249 0.00283 0.00311 0.00318  Antimony Output Sample No.  1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days)  0.0000 3.0000 8.0104 11.1424 14.2639 19.0243 22.0243 26.0799 28.9965 33.0833 36.0243  Sol'n Vol. gSb (mL) sampled  104.47 101.46 81.71 88.11 100.75 98.93 103.20 103.08 103.51 102.73 99.72 245.00  0 0 0 0 0 0.00002 3.5E-05 3.5E-05 0.00004  168  Mesophiles, 10 g Enargite (2), P Test UB7-M37  Date  Hour  Time (days)  Initial Mass (g)  PH  16-Jul 18-Jul 22-Jul 23-Jul 26-Jul 30-Jul 31-Jul 2-Aug 6-Aug 7-Aug 9-Aug 12-Aug 13-Aug 16-Aug 20-Aug 21-Aug  13:30 11:55 10:35 12:20 10:20 11:15 13:05 12:00 12:00 12:30 12:45 12:15 12:15 13:50 13:15 13:05  0.00 1.93 5.88 6.95 9.87 13.91 14.98 16.94 20.94 21.96 23.97 26.95 27.95 31.01 34.99 35.98  249.20 248.48 248.20 247.64 246.10 248.97 248.54 247.83 249.46 249.18 248.37 249.02 248.70 247.36 248.06 249.52  1.61 1.85 1.67 1.75 1.58 1.45 1.34 1.38 1.33 1.32 1.27 1.23 1.27 1.18 1.21 1.22  Enargite In (g):  Total Water (g):  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  8 0  of 37 microns  Mesophiles  10.02 13.46  Vol (mL) Mass (g) 133.95 10 10 95.11 95.11 '' C' ' 249.52 103.68 250 7.66  E„ (Ag/AgCI) E„ (mV)  Analysis  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): • #1 #2 #3 #4 PLS (mg/L) Wash (mg/L) Solid Residue (wt % '.•  • •'":  :  Sample (mL)  Medium Added Added (mL) Water (g)  464 370 499 508 531 586 585 606 636 629 664 671 655 692 700 698  684 590 719 728 751 806 805 826 856 849 884 891 875 912 920 918  Copper 32.4 383.25 0  Iron 7.2 1305.50 0.1004  Arsenic 12 55.5 0  3796.25 127.75 5064.30 921.45 5056.60 2704.10 5197.40 4415.30 5137.10 5293.25 94.08 49.94 36 1.3837  261.5 262.5 571.0 976.0 1038.5 1.9 13  0.4  '  '•  5 5  5  5  4.20  250.30  2.94  250.77  1.34  249.71  2.09 1.70  249.45 249.76  5  5  Antimony 0.39 0  I  Copper  Iron  Arsenic  Antimony  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 Medium Added (g): #1 #2 #3 #4 PLS (g) Wash (g) Solid Residue (g)  3.24648 0.0038 0  0.7214 0.0131 0.0096  1.2024 0.0006 0  0.039078 0.0000 0  0.018981 0.025322 0.025283 0.025987  0.0006 0.0046 0.0135 0.0221  0.001308 0.001313 0.002855 0.00488  0 0 0 0  0 0 0 0 0.5326 0.02352 2.7576  0.0005 0.0005 0.0005 0.0005 0.5488 0.0125 0.106  0 0 0 0 0.1077 0.000475 0.9958  0 0 0 0 0.0000 0 0.03064  3.379 -4.097  0.662 8.248  1.109 7.779  0.031 21.593  18.40 19.16  83.99 77.06  10.20 9.40  0.00 0.00  ,  % Extraction  Calculated Head Measured Head  249.67  5  ' '  ' *  1.19 5  Weight of Element  Calculated Head (g) % Difference  Final Mass (g)  Copper Output  Sample #  Time (days) Sol'n Vol. (mL)  0.00 6.95 14.98 21.96 27.95 35.98  1 2 3 4 Filtrate Wash  105.23 103.67 104.57 105.21 104.73 103.68 250.00  g Cu sampled  Tot. Cu Sampled (g)  0.01898125 0.0253215 0.025283 0.025987  0.01898 0.04430 0.06959 0.09557  Cu in sol'n (g) Cu(aq) total (g)  %Cu indicated  %Cu actual  0.394 0.530 0.532 0.544 0.533 0.024  0.390 0.545 0.572 0.610 0.598 0.622  12.00 16.78 17.63 18.79  11.53 16.12 16.94 18.05  19.16  18.40  Iron Output Sample #  Time (days) Sol'n Vol. (mL)  0.00 6.95 14.98 21.96 27.95 35.98  1 2 3 4 Filtrate Wash  105.23 103.67 104.57 105.21 104.73 103.68 250.00  g Fe sampled  Tot. Fe Sample  Fe in sol'n (g)  Fe(aq)total  %Fe indicated  %Fe actual  0.000136549 0.004105049 0.013018299 0.021574299  0.00014 0.00424 0.01726 0.03883  0.013243843 0.096356027 0.284498361 0.462414369 0.5488 0.012485  0.00 0.08 0.27 0.45 0.54 0.55  0.03 11.55 37.63 62.29  0.03 12.58 41.01 67.89  75.99  82.82  As(aq)total  %As indicated  %As actual  0.03 0.03 0.06 0.11 0.11 0.11  2.21 2.35 5.17 8.91  2.39 2.54 5.60 9.66  9.40  10.20  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00 0.00  0.00 0.00 0.00 0.00  0.00 0.00 0.00 0.00  0.00  0.00  Arsenic Output Sample #  1 2 3 4 Filtrate Wash  •  Time (days) Sol'n Vol. (mL)  0.00 6.95 14.98 21.96 27.95 35.98  105.23 103.67 104.57 105.21 104.73 103.68 250.00  g As sampled  0.0013075 0.0013125 0.002855 0.00488  Tot. As Sample As in sol'n (g)  0.00131 0.00262 0.00548 0.01036  0.027109705 0.027449625 0.06007491 0.10221648 0.11 0.00  Antimony Output Sample #  1 2 3 4 Filtrate Wash  Time (days) Sol'n Vol. (nnL)  0.00 6.95 14.98 21.96 27.95 35.98  105.23 103.67 104.57 105.21 104.73 103.68 250.00  g Sb sampled  0 0 0 0  Tot. Sb Sample Sb in sol'n (g)  0.00000 0.00000 0.00000 0.00000  0 0 0 0 0.00 0.00  Moderate Thermophiles, 2 g Enargite, P Test #B9-T10 Date  Hour  Time (days)  Initial Mass (g)  pH  4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun 28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  12:25 10:40 10:50 11:30 10:25 11:20 12:15 11:35 12:55 12:50 13:10 13:20 11:45 12:15  0.00 2.93 5.93 8.96 12.92 13.95 15.99 19.97 22.02 24.02 28.03 30.04 34.97 35.99  241.39 233.46 234.01 234.26 232.46 239.67 234.18 232.88 236.00 236.88 232.34 236.86 229.35 239.17  1.58 1.79 1.79 1.75 1.62 1.55 1.35 1.36 1.31 1.40 1.42 1.30 1.37 1.41  Enargite In (g):  Total Water (g):  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  8 0  of 10 microns  Moderate Thermophiles  2.01 92.28  Vol (mL) Mass (g) 133.84 10 10 95.01 95.01 •• • .*»tJ , 239.17 102.02 250 0.81  E (Ag/AgCI) E h  (mV)  h  484 401 454 480 512 508 537 593 624 625 608 621 620 621  704 621 674 700 732 728 757 813 844 845 828 841 840 841  Copper 31.2 2617.25 0  2986.40 3291.45 3303.50 3533.95 36.09 Solid Residue (wt "A 32  Analysis  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L)  „.-; ,'u  Medium Added Final Added (mL) Water (g) Mass (g)  5  5  5  5  Iron 11.6  Arsenic 10.5  Antimony 0.55  1996.30 0.201  459.5 0  9.5 0  641.50 1976.85 1893.00 1522.25 8.77 2.0608  396.5 535.0 549.0 456.5 4.0 12  •<.-,  4.5 4.0 0.9  ...  Iron  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g)  0.23316 0.0200 0.01909  Arsenic  Antimony  0.21105 0.0046 0  0.011055 0.0001 0  0.014932 0.00321 0.001983 0.016457 0.00988 0.002675 0.016518 0.00947 0.002745  0 0.0000225 0.00002  0 0.001 0 0.001 0 0.001 0.3605 0.1553 0.009023 0.00219 0.2592 0.01669  0 0 0 0.0466 0.001 0.0972  0 0 0 0.0000 0 0.00729 ,,  Calculated Head (g) % Difference  ; „•  -  0.650 -3.727  0.155 33.659  0.148 30.074  0.007 34.532  60.15 62.39  89.21 59.18  34.14 23.87  -0.73 -0.47  % Extraction  Calculated Head Measured Head  8.46 7.91 8.66 9.89  241.92 241.92 242.92 242.35  9.03 8.67 5.97 5.96 9.74 5.43 12.56  243.21 241.55 241.97 242.84 242.08 242.29 241.91  5  5  Weight of Element Copper 0.62712 0.0262 0  Sample (mL)  Copper  Output Tot. Cu  Sample #  Time (days)  Sol'n Vol. (mL)  0.00  105.54  g Cu sampled  Sampled (g)  Cu in sol'n (g)  Cu(aq) total (g)  %Cu indicated  %Cu actual  1  12.92  96.61  0.014932  0.01493  0.289  0.262  41.83  40.33  2  19.97  97.03  0.01645725  0.03139  0.319  0.308  49.13  47.37  3  28.03  96.49  0.0165175  0.04791  0.319  0.324  51.66  49.80  35.99  102.02  0.361  0.382  250.00  0.009  0.391  62.39  60.15  Fe(aq) total  %Fe indicated  %Fe actual  Filtrate Wash  Iron Output Sample #  Time (days) 0.00  Sol'n Vol. (r  g Fe sampled  Tot. Fe Sample  Fe in sol'n (g)  105.54  1  12.92  96.61  0.002203097  0.00220  0.061975315  0.04  18.02  27.16  2  19.97  97.03  0.008879847  0.01108  0.191813756  0.17  73.71  111.10  3  28.03  96.49  0.008460597  0.01954  0.18265557  0,16  69.78  105.18  35.99  102.02  0.1553  0.14  250.00  0.0021925  0.14  58.99  88.91  %As indicated  %As actual  Filtrate Wash  Arsenic  Output  Sample #  Time (days)  Sol'n Vol. (nnL)  0.00  105.54  g As sampled  Tot. As Sample  A s in sol'n (g)  As(aq)total  1  12.92  96.61  0.0019825  0.00198  0.038305865  0.03  15.97  22.84  2  19.97  97.03  0.002675  0.00466  0.05191105  0.05  23.36  33.40  3  28.03  96.49  0.002745  0.00740  0.05297301  0.05  25.13  35.94  35.99  102.02  0.05  0.05  250.00  0.00  0.05  23.87  34.14  Sb in sol'n (g)  Sb(aq) total  %Sb indicated  %Sb actual  Filtrate Wash  Antimony Sample #  Output Time (days)  Sol'n Vol. (rnL)  0.0000  105.54  g Sb sampled  Tot. Sb Sample  1  12.92  96.61  0  0.00000  0  0.00  -0.86  2  19.97  97.03  0.0000225  0.00002  0.000436635  0.00  3.09  4.72  3  28.03  96.49  0.00002  0.00004  0.00038596  0.00  2.84  4.33  35.99  102.02  0.00  0.00  250.00  0.00  0.00  -0.47  -0.73  Filtrate Wash  ' -1.31  Moderate Thermophiles, 2 g Enargite, P Test#B9-T15  8 0  of 15 microns  Moderate Thermophiles  Date  Hour  Time (days)  Initial Mass (g)  pH  4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun  12:25 10:40 10:50 11:30 10:25 11:20 12:15 11:35 12:55  0.00 2.93 5.93 8.96 12.92 13.95 15.99 19.97 22.02  255.38 248.00 248.46 248.92 246.31 254.28 248.81 245.29 250.90  1.58 1.83 1.86 1.85 1.70 1.66 1.51 1.45 1.38  479 395 436 479 512 521 545 576 609  699 615 656 699 732 741  28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  12:50 13:10 13:20 11:45 12:15  24.02 28.03 30.04 34.97 35.99  250.57 245.36 250.21 243.80 254.10  1.48 1.48 1.37 1.44 1.45  597 615 627 624 620  817 835 847 844 840  5  5  Copper •30.4  Iron 10.6  Arsenic 10.5  Antimony 0.55  2617.25 0  1996.30 0.20088  459.5 0  9.5 0  2288.95 2444.50 2720.20 2960.00 30.32 36  486.85 1133.85 1750.90 1558.65 8.93 1.0616  271.0 271.5 395.5 357.5 3.0 13 , i ",' ' Arsenic  1.0 2.5 5.5  Enargite In (g): Total Water (g):  2.01 92.10  Vol (mL) Mass (g) Flask Weight (g): 147.80 Innoculum in: 10* ' 10 Medium in: 95.06 95.06 Total Final Weight (g): •• : > 254.10 102.56 Filtrate Volume (mL) Wash Volume (mL) 250 Solid Residue (g) 0.95  E (Ag/AgCI) E (mV) h  Analysis Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt"/(  h  765 796 829  Medium Sample Added Final (mL) Added (mL) Water (g) Mass (g)  5  5  5  Iron 0.21306 0.0200 0.0191  0.21105 0.0046 0  0.011055 0.0001 0  0.00243 0.00567 0.00875  0.001355 0.001358 0.001978  0.000005 0.0000125 0.0000275  0.001 0.001 0.001 0.1599 0.00223 0.01009  0 0 0 0.0367 0.00075 0.1235  0 0 0 0.0000 0 0.0076  0.147 31.025  48.51 52.74  93.14 64.24  % Extraction Calculated Head Measured Head  6.94 11.11 4.96  255.75 256.40 255.86  5.11 10.06 5.75 12.83  255.68 255.42 255.96 256.63  0.8  Head (g) 0.61104 Innoculum (g) 0.0262 Medium (g) 0 Samples (g): #1 0.011445 #2 0.012223 #3 0.013601 Medium Added (g): #1 0 #2 0 #3 0 PLS (g) 0.3036 Wash (g) 0.00758 Solid Residue (g) 0.342 0.664 -8.709  256.44 257.00 256.62 256.97  5  Weight of Element Copper  Calculated Head (g) % Difference  8.44 8.54 7.70 10.66  Antimony  0.161 0.008 23.710 31.705 i- -: • • - ' T J i l S f M 23.30 -0.66 17.77 -0.45  173  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.57 1 12.92 96.50 0.01144475 2 19.97 95.48 0.0122225 3 28.03 95.55 0.013601 35.99 102.56 Filtrate Wash 250.00  Tot. Cu Sampled (g) 0.01144 0.02367 0.03727  Cu in sol'n (g) Cu(aq) total (g) 0.221 0.233 0.260 0.304 0.008  %Cu indicated %Cu actual  0.195 0.219 0.257 0.315 0.322  31.87 35.79 42.13  29.31 32.92 38.75  52.74  48.51  Fe(aq) total  %Fe indicated  %Fe actual  0.03 0.09 0.15 0.14 0.14  12.68 41.44 69.15  18.38 60.08 100.26  66.71  96.71  As(aq) total  %As indicated  %As actual  Iron Output  Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.00 105.57 1 12.92 96.50 0.001429847 0.00143 0.047 2 19.97 95.48 0.004664847 0.00609 0.108 3 28.03 95.55 0.007750097 0.01384 0.167 35.99 Filtrate 102.56 0.1599 Wash 250.00 0.0022325  Arsenic  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.57 1 12.92 96.50 0.001355 0.00136 0.0261515 2 19.97 95.48 0.0013575 0.00271 0.02592282 3 28.03 95.55 0.0019775 0.00469 0.037790025 35.99 102.56 Filtrate 0.04 Wash 250.00 0.00  0.02 0.02 0.04 0.04 0.04  10.21 10.75 17.01 .  13.39 14.09 22.30  17.77  23.30  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  0.01 1.35 4.05  0.02 1.97 5.93  -0.45  -0.66  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.57 1 12.92 96.50 0.000005 0.00001 0.0000965 19.97 2 95.48 0.0000125 0.00002 0.0002387 3 28.03 95.55 0.0000275 0.00005 0.000525525 Filtrate 35.99 102.56 0.00 Wash 250.00 0.00  Moderate Thermophiles, 2 g Enargite, P Test UB9-T37  Date 4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun 28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  Enargite In (g): Total Water (g):  Moderate  Hour 12:25 10:40 10:50 11:30 10:25 11:20 12:15 11:35 12:55 12:50 13:10 13:20 11:45 12:15  Time (days) 0.00 2.93 5.93 8.96 12,92 13.95 15.99 19.97 22.02 24.02 28.03 30.04 34.97 35.99  2.00 98.95  Vol (mL) Mass (g) Flask Weight (g): 137.36 Innoculum in: 10 10 Medium in: 95.08 95.08 Total Final Weight (g): 243.43 Filtrate Volume (mL) 102.87 Wash Volume (mL) 250 Solid Residue (g) 1.20 i^... * '  Initial Mass (g) 245.00 236.45 237.81 238.27 234.84 243.38 237.46 235.15 240.40 239.77 234.11 239.63 231.06 243.43  8 0  of 37 microns  Thermophiles  PH 1.58 1.77 1.77 1.75 1.65 1.59 1.45 1.43 1.36 1.48 1.48 1.35 1.43 1.47  E„ (Ag/AgCI) E (mV) 482 702 426 646 466 686 505 725 535 755 546 766 573 793 599 819 615 835 616 836 620 840 629 849 623 843 620 840 h  Sample Medium Added Final (mL) Added (mL) Water (g) Mass (g)  5 5  5  5  5  Copper 32.4  Iron 7.2  Arsenic 12  Antimony 0.39  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  2617.25 0  1996.30 0.201  459.5 0  9.5 0  2163.55 2158.40 2320.85 2489.35 26.26 33  543.90 1009.60 1222.65 949.10 3.25 0.7962  336.5 302.0 360.0 276.0 0.6 12  0.5 0.5 1.0  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g) Calculated Head (g % Difference % Extraction Calculated Head Measured Head  0.648 0.0262 0  Iron 0.144 0.0200 0.0191  Arsenic 0.24 0.0046 0  0.010818 0.00272 0.001683 0.010792 0.00505 0.00151 0.011604 0.00611 0.0018 0 0.001 0 0.001 0 0.001 0.2561 0.0976 0.006565 0.00081 0.396 0.00955  245.86 246.02 245.67 246.03  8.53 11.07 4.92 5.77 11.28 6.06 15.11  245.99 246.22 245.32 245.54 245.39 245.69 246.17  5  Analysis Head (wt %)  Weight of Element Copper  9.41 8.21 7.40 11.19  0.5 Antimony 0.0078 0.0001 0 0.0000025 0.0000025 0.000005  0 0 0 0.0284 0.00015 0.144  0 0 0 0.0000 0 0.006  0.666 -2.729  0.080 44.579  0.173 27.942  0.006 24.167  40.51 41.62  88.03 48.79  16.73 12.06  -1.44 -1.09  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.64 1 12.92 95.48 0.01081775 2 19.97 95.79 0.010792 3 28.03 94.75 0.01160425 35.99 Filtrate 102.87 Wash 250.00  Tot. Cu Sampled (g) 0.01082 0.02161 0.03321  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.207 0.207 0.220 0.256 0.007  0.180 0.191 0.215 0.263 0.270  27.84 29.54 33.23  27.10 28.75 32.35  41.62  40.51  Fe(aq) total  %Fe indicated  %Fe actual  0.03 0.08 0.10 0.08 0.08  22.20 53.30 66.59  40.06 96.17 120.15  54.50  98.34  As(aq)total  %As indicated  %As actual  0.03 0.03 0.03 0.03 0.03  11.47 10.84 13.63  15.92 15.04 18.91  12.06  16.73  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  -0.61 -0.57 0:06  -0.80 -0.75 0.08  -1.09  -1.44  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.64 1 12.92 95.48 2 19.97 95.79 3 28.03 94.75 35.99 102.87 Filtrate Wash 250.00  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.001715097 0.004043597 0.005108847  0.00172 0.00576 0.01087  0.052 0.097 0.116 0.0976 0.0008125  Arsenic Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.64 1 12.92 95.48 0.0016825 0.00168 0.03212902 2 19.97 95.79 0.00151 0.00319 0.02892858 3 28.03 94.75 0.0018 0.00499 0.03411 Filtrate 35.99 102.87 0.03 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.64 1 12.92 95.48 0.0000025 0.00000 0.00004774 2 19.97 95.79 0.0000025 0.00001 0.000047895 3 28.03 94.75 0.000005 0.00001 0.00009475 35.99 102.87 Filtrate 0.00 Wash 250.00 0.00  Moderate Thermophiles, 3.5 g Enargite, P Test UB6-T10  Date 4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun 28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  Enargite In (g): Total Water (g):  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  Moderate  Hour 12:20 10:30 10:40 11:25 10:15 11:15 12:05 11:20 12:35 12:45 13:00 13:05 11:20 12:05  Time (days) 0.00 2.92 5.93 8.96 12.91 13.95 15.99 19.96 22.01 24.02 28.03 30.03 34.96 35.99  3.50 90.77  Vol (mL) Mass (g) 132.14 10 10 95.01 95.01 239.25 102.94 240 1.39  Initial Mass (g) 241.36 234.12 234.14 234.78 232.15 242.92 237.55 233.25 236.35 238.81 232.31 237.87 230.46 239.25  8 0  of 10 microns  Thermophiles  PH 1.66 1.85 1.74 1.76 1.63 1.47 1.33 1.36 1.30 1.37 1.34 1.21 1.28 1.31  E„ (Ag/AgCI) E (mV) 489 709 393 613 434 654 465 685 495 715 487 707 503 723 525 745 516 736 543 763 571 791 598 818 624 844 627 847 h  Medium Sample Added Final (mL) Added (mL) Water (g) Mass (g)  5  5  5  5  5  Copper 31.2  Iron 11.6  Arsenic 10.5  Antimony 0.55  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  2617.25 0  1996.30 0.201  459.5 0  9.5 0  4223.50 5819.10 5726.85 5961.50 65.79 33  541.35 1417.50 2477.70 2862.50 10.29 1.7145  516.5 641.0 795.5 893.5 0.4 12  Weight of Element Copper  Iron  Head (g) 1.092 0.406 Innoculum (g) 0.0262 0.0200 Medium (g) 0 0.01909 Samples (g): #1 0.021118 0.00271 #2 0.029096 0.00709 #3 0.028634 0.01239 Medium Added (g): #1 0 0.001 #2 0 0.001 #3 0 0.001 0.6137 0.2947 PLS (g) Wash (g) 0.01579 0.00247 Solid Residue (g) 0.4587 0.02383 Calculated Head (g % Difference % Extraction Calculated Head Measured Head  Arsenic  242.24 242.24 242.06 245.82  5.75 8.31 8.48 3.69 10.70 5.18 11.49  243.30 241.56 244.83 242.50 243.01 243.05 241.95  5  Analysis Head (wt %)  .. v  8.12 8.10 7.28 13.67  ,. .  1.0 5.5 0.7 Antimony  0.3675 0.0046 0  0.01925 0.0001 0  0.002583 0.003205 0.003978  0 0.000005 0.0000275  0 0 0 0.0920 0.000096 0.1668  0 0 0 0.0000 0 0.00973  1.141 -4.473  0.301 25.840  0.264 28.152  0.010 49.779  59.79 62.47  92.08 68.29  36.83 26.46  -0.65 -0.32  177  Copper Output  Sample # Time (days) Sol'n Vol. (nnL) g Cu sampled 0.00 105.72 1 12.91 96.51 0.0211175 2 19.96 97.61 0.0290955 3 28.03 96.67 0.02863425 35.99 Filtrate 102.94 Wash 240.00  Tot. Cu Sampled (g) 0.02112 0.05021 0.07885  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.408 0.568 0.554 0.614 0.016  0.381 0.563 0.578 0.666 0.682  34.93 51.55 52.90  33.43 49.34 50.63  62.47  59.79  Fe(aq) total  %Fe indicated  %Fe actual  0.03 0.12 0.22 0.27 0.28  7.95 29.16 54.08  10.72 39.32 72.92  68.27  92.06  As(aq)total  %As indicated  %As actual  0.05 0.06 0.08 0.10 0.10  12.31 16.48 21.25  17.14 22.93 29.58  26.46  36.83  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  -0.49 0.01 2.29  -0.98 0.03 4.57  -0.32  -0.65  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.72 1 12.91 96.51 2 19.96 97.61 3 28.03 96.67 Filtrate 35.99 102.94 Wash 240.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.001702347 0.006083097 0.011384097  0.00170 0.00779 0.01917  0.052245689 0.138362175 0.239519259 0.2947 0.0024696  Output  Sample # Time (days) Sol'n Vol. (nnL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.72 1 12.91 96.51 0.0025825 0.00258 0.049847415 2 19.96 97.61 0.003205 0.00579 0.06256801 3 28.03 96.67 0.0039775 0.00977 0.076900985 Filtrate 35.99 102.94 0.09 Wash 240.00 0.00  •  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.72 1 12.91 96.51 0 0.00000 0 2 19.96 97.61 0.000005 0.00001 0.00009761 3 28.03 96.67 0.0000275 0.00003 0.000531685 Filtrate 35.99 102.94 0.00 Wash 240.00 0.00  Moderate Thermophiles, 3.5 g Enargite, P Test #B6-T15  Date 4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun 28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  Enargite In (g): Total Water (g):  Moderate  Hour 12:20 10:30 10:40 11:25 10:15 11:15 12:05 11:20 12:35 12:45 13:00 13:05 11:20 12:05  Time (days) 0.00 2.92 5.93 8.96 12.91 13.95 15.99 19.96 22.01 24.02 28.03 30.03 34.96 35.99  3.50 95.68  Vol (mL) Mass (g) Flask Weight (g): ,,. .v.;. 114.83 Innoculum in: 10 10 Medium in: 95.05 95.05 Total Final Weight (g): - ••• 251.81 Filtrate Volume (mL) 102.27 ••' •':.:¥ Wash Volume (mL) 250 Solid Residue (g) 1.68  Initial Mass (g) 253.98 246.33 246.22 245.65 243.22 252.16 245.95 243.34 249.08 249.83 243.05 247.55 241.36 251.81  8 0  of 15 microns  Thermophiles  pH 1.63 1.89 1.91 1.88 1.78 1.62 1.48 1.47 1.40 1.42 1.40 1.27 1.35 1.35  E„ (Ag/AgCI) E (mV) 453 673 383 603 421 641 466 686 493 713 514 734 519 739 557 777 577 797 581 801 589 809 624 844 618 838 631 851 h  Medium Sample Added Final (mL) Added (mL) Water (g) Mass (g)  5  5  5  5  5  Copper 30.4  Iron 10.6  Arsenic 10.5  Antimony 0.55  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  2617.25 0  1996.30 0.201  459.5 0  9.5 0  3679.80 4512.85 4727.00 4696.15 64.98 36  446.95 1530.30 2966.35 2842.10 15.35 0.9415  354.0 472.0 811.5 677.0 0.7 13  Weight of Element Copper Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g)  1.064 0.0262 0  '  Iron 0.371 0.0200 0.01909  0.018399 0.00223 0.022564 0.00765 0.023635 0.01483  ' <''''?;  8.20 10.88 5.85 4.82 9.87 6.84 13.09  254.15 254.22 254.93 254.65 252.92 254.39 254.45  3.0 15.5 0.8 •  Arsenic  Antimony  0.3675 0.0046 0  0.01925 0.0001 0  0.00177 0.00236 0.004058  0 0.000015 0.0000775  0 0.001 0 0 0.001 0 0 0.001 0 0.4803 0.2907 0.0692 0.016245 0.00384 0.000175 0.6048 0.01582 0.2184  Calculated Head (g) 1.140 % Difference -7.119 ' % Extraction Calculated Head 46.94 Measured Head 50.28  254.32 253.98 254.35 254.90  5  Analysis Head (wt %)  :*:.T ..  7.99 7.76 8.70 11.68  0 0 0 0.0000 0 0.01344  0.293 21.034  0.291 20.706  0.013 30.195  94.60 74.70  25.05 19.87  -0.02 -0.01  179  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 135.65 12.91 124.89 1 0.018399 19.96 125.01 2 0.02256425 3 28.03 124.72 0.023635 35.99 102.27 Filtrate Wash 250.00  Tot. Cu Sampled (g) 0.01840 0.04096 0.06460  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.460 0.564 0.590 0.480 0.016  0.433 0.556 0.604 0.519 0.535  40.73 52.29 56.80  38.03 48.82 53.02  50.28  46.94  Fe(aq) total  %Fe indicated  %Fe actual  0.04 0.17 0.35 0.27 0.27  9.66 46.18 94.34  12.24 58.48 119.47  74.00  93.71  As(aq)total  %As indicated  %As actual  0.04 0.06 0.10 0.07 0.07  10.78 15.29 27.41  13.59 19.28 34.57  19.87  25.05  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  -0.49 1.45 9.63  -0.71 2.08 13.79  -0.01  -0.02  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 135.65 1 12.91 124.89 2 19.96 125.01 3 28.03 124.72 35.99 102.27 Filtrate Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.001230347 0.006647097 0.013827347  0.00123 0.00788 0.02170  0.056 0.191 0.370 0.2907 0.0038375  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 135.65 1 12.91 124.89 0.00177 0.00177 0.04421106 2 19.96 125.01 0.00236 0.00413 0.05900472 3 28.03 124.72 0.0040575 0.00819 0.10121028 Filtrate 35.99 102.27 0.07 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 135.65 1 12.91 124.89 0 0.00000 0 2 19.96 125.01 0.000015 0.00002 0.00037503 3 28.03 124.72 0.0000775 0.00009 0.00193316 Filtrate 35.99 102.27 0.00 Wash 250.00 0.00  0  Moderate Thermophiles, 3.5 g Enargite, P Test UB6-T37  Date 4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun 28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  Enargite In (g): Total Water (g):  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  80  of 37 microns  Moderate Thermophiles  Hour 12:20 10:30 10:40 11:25 10:15 11:15 12:05 11:20 12:35 12:45 13:00 13:05 11:20 12:05  Time (days) 0.00 2.92 5.93 8.96 12.91 13.95 15.99 19.96 22.01 24.02 28.03 30.03 34.96 35.99  3.51 106.20  Vol (mL) Mass (g) 130.98 ••• 10 10 95.13 95.13 237.57 100.88 245 2.20  Initial Mass (g) 240.21 231.88 233.10 231.76 228.54 238.99 232.34 229.05 234.47 239.83 229.92 236.29 225.69 237.57  pH 1.61 1.81 1.80 1.78 1.71 1.59 1.47 1.48 1.39 1.49 1.48 1.32 1.40 1.39  E„ (Ag/AgCI) E (mV) 491 711 407 627 441 661 468 688 485 705 497 717 509 729 535 755 567 787 572 792 579 799 613 833 603 823 621 841 h  Sample Medium Added Final (mL) Added (mL) Water (g) Mass (g)  5 5  5  5  5  Copper 32.4  Iron 7.2  Arsenic 12  Antimony 0.39  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  2617.25 0  1996.30 0.201  459.5 0  9.5 0  3178.15 4144.35 4113.25 4257.50 54.09 32  334.70 680.60 1244.60 1527.25 5.41 2.2206  524.0 531.0 532.0 503.0 0.7 12  1.0 0.0 0.0  Iron  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g)  0.25272 0.0200 0.01911  Calculated Head (g % Difference % Extraction Calculated Head Measured Head  1.13724 0.0262 0  0.015891 0.00167 0.020722 0.0034 0.020566 0.00622  Arsenic  0.5 Antimony  0.4212 0.0046 0  0.013689 0.0001 0  0.00262 0.002655 0.00266  0.000005 0 0  0 0.001 0 0 0.001 0 0 o.ooi 0 0.4295 0.1541 0.0507 0.013252 0.00133 0.000172 0.704 0.04885 0.264  241.65 240.55 240.46 242.07  10.04 11.98 10.91 1.99 12.12 4.64 15.07  242.38 241.03 245.38 241.82 242.04 240.93 240.76  5  Analysis Head (wt %)  Weight of Element Copper  9.77 7.45 8.70 13.53  0 0 0 0.0000 0 0.011  1.178 -3.563  0.173 31.362  0.318 24.441  0.011 20.301  40.23 41.66  71.84 49.31  17.05 12.88  -0.82 -0.66  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.72 1 12.91 94.05 0.01589075 2 19.96 94.56 0.02072175 28.03 95.43 0.02056625 3 Filtrate 35.99 100.88 Wash 245.00  Tot. Cu Sampled (g) 0.01589 0.03661 0.05718  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.299 0.392 0.393 0.429 0.013  0.273 0.382 0.403 0.461 0.474  23.98 33.56 35.43  23.16 32.40 34.21  41.66  40.23  Fe(aq)total  %Fe indicated  %Fe actual  0.01 0.04 0.10 0.13 0.14  4.56 17.57 39.10  6.64 25.59 56.96  53.59  78.08  As(aq)total  %As indicated  %As actual  0.04 0.05 0.05 0.05 0.05  10.61 11.45 12.21  14.04 15.16 16.17  12.88  17.05  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  -0.01 -0.66 -0.66  -0.01 -0.82 -0.82  -0.66  -0.82  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.72 1 12.91 94.05 2 19.96 94.56 3 28.03 95.43 Filtrate 35.99 100.88 Wash 245.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.000669097 0.002398597 0.005218597  0.00067 0.00307 0.00829  0.031478535 0.064357536 0.118772178 0.1541 0.00132545  Output  Sample # Time (days) Sol'n Vol. (n 0.00 105.72 1 12.91 94.05 2 19.96 94.56 3 28.03 95.43 Filtrate 35.99 100.88 Wash 245.00  g As sampled Tot. As Sample As in sol'n (g) 0.00262 0.002655 0.00266  0.00262 0.00528 0.00794  0.0492822 0.05021136 0.05076876 0.05 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (n 0.0000 105.72 1 12.91 94.05 2 19.96 94.56 3 28.03 95.43 35.99 100.88 Filtrate Wash 245.00  g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.000005 0 0  0.00001 0.00001 0.00001  0.00009405 0 0 0.00 0.00  M o d e r a t e T h e r m o p h i l e s , 5 g Enargite, P Test UB8-T10  Moderate  8 0  of 10 microns  Thermophiles  Date  Hour  Time (days)  Initial Mass (g)  PH  4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun  12:25 10:35 10:45 11:30 10:20 11:20 12:15 11:30 12:50  0.00 2.92 5.93 8.96 12,91 13.95 15.99 19.96 22.02  243.35 236.49 236.64 236.71 232.47 241.70 236.50 234.59 238.52  1.60 1.86 1.89 1.87 1.65 1.55 1.38 1.36 1.25  483 379 417 449 471 472 484 496 506  703 599 637 669 691 692 704 716 726  28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  12:50 13:05 13:15 11:40 12:10  24.02 28.03 30.03 34.97 35.99  239.63 235.59 239.08 232.28 241.16  1.37 1.30 1.20 1.25 1.22  523 545 561 589 599  743 765 781 809 819  5  5  Copper 31.2  Iron 11.6  Arsenic 10.5  Antimony 0.55  2617.25 0  1996.30 0.201  459.5 0  9.5 0  5048.80 7181.90 7490.30 8639.60 91.98 32 I,: '-u.<;».>.•.. • •'-"i%s-. , . Weight of Element Copper  572.85 1253.50 2480.95 3762.60 14.84 3.2272  621.5 970.5 1190.5 1460.5 1.8 12  Enargite In (g): Total Water (g):  Analysis  5.00 87.16  Vol (mL) Flask Weight (g): . •• w v Innoculum in: 10 Medium in: 95.11 Total Final Weight (g): Filtrate Volume (mL) 103.16 W a s h Volume (mL) 250 Solid Residue (g)  Head (wt %)  M a s s (g) 132.73 10 95.11 241.16 '' ,'  * j * •?i<#  2.20  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 P L S (mg/L) W a s h (mg/L) Solid Residue (wt °/<  E„ (Ag/AgCI) E„ (mV)  Head (g) 1.56 Innoculum (g) 0.0262 Medium (g) 0 Samples (g): #1 0.025244 #2 0.03591 #3 0.037452 Medium Added (g): #1 0 #2 0 #3 0 0.8913 P L S (g) W a s h (g) 0.022995 Solid Residue (g) 0.704 Calculated Head (g; % Difference  % Extraction Calculated Head Measured Head  1.691 -8.377 , ~'?K , " 58.36 63.25  Sample Medium Added Final (mL) Added (mL) Water (g) Mass (g)  5  5  244.23 243.78 244.36  5.72 8.49 5.10 11.21  245.35 244.08 244.18 243.49  0.6  •-.  • • '*!,';*' •• -  Antimony  0.525 0.0046 0  0.0275 0.0001 0  0.00286 0.00627 0.0124  0.003108 0.004853 0.005953  0 0.000005 0.0000275  0.001 0.001 0.001 0.3881 0.00371 0.071  0 0 0 0.1507 0.00045 0.264  0 0 0 0.0000 0 0.0132  0.424 19.156 . V 37.80 30.56  0.013 52.227  83.95 64.02  7.73 9.19 5.84  1.0 5.5  0.58 0.0200 0.01911  0.442 23.739  244.05 244.00 243.97 244.17  5  5  \ ' V ' •• ' ' ••' -'<r» Iron Arsenic  7.56 7.36 7.26 11.70  -0.48 -0.23  183  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.62 1 12.91 94.74 0.025244 19.96 2 96.86 0.0359095 3 28.03 97.86 0.0374515 35.99 Filtrate 103.16 Wash 250.00  Tot. Cu Sampled (g) 0.02524 0.06115 0.09861  Cu in sol'n (g) Cu(aq) total (g) 0.478 0.696 0.733 0.891 0.023  %Cu indicated %Cu actual  0.452 0.695 0.768 0.964 0.987  28.98 44.53 49.23  26.74 41.09 45.42  63.25  58.36  Fe(aq)total  %Fe indicated  %Fe actual  0.03 0.10 0.22 0.37 0.37  5.92 17.49 38.42  7.76 22.94 50.38  64.12  84.08  As(aq) total  %As indicated  %As actual  0.05 0.09 0.12 0.16 0.16  10.34 17.62 22.83  12.79 21.80 28.24  30.56  37.80  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  -0.35 0.01 1.63  -0.72 0.01 3.41  -0.23  -0.48  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.62 1 12.91 94.74 2 19.96 96.86 3 28.03 97.86 35.99 103.16 Filtrate Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.001859847 0.005263097 0.011400347  0.00186 0.00712 0.01852  0.054271809 0.12141401 0.242785767 0.3881 0.00371  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.62 1 12.91 94.74 0.0031075 0.00311 0.05888091 2 19.96 96.86 0.0048525 0.00796 0.09400263 3 28.03 97.86 0.0059525 0.01391 0.11650233 35.99 103.16 Filtrate 0.15 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.62 1 12.91 94.74 0 0.00000 0 2 19.96 96.86 0.000005 0.00001 0.00009686 3 28.03 97.86 0.0000275 0.00003 0.00053823 Filtrate 35.99 103.16 0.00 Wash 250.00 0.00  Moderate Thermophiles, 5 g Enargite, P Test#B8-T15  Moderate  Date  Hour  4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun 28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  12:25 10:35 10:45 11:30 10:20 11:20 12:15 11:30 12:50 12:50 13:05 13:15 11:40 12:10  Enargite In (g):  Total Water (g):  Initial Mass (g)  PH  0.00 2.92 5.93 8.96 12.91 13.95 15.99 19.96 22.02  226.70 220.46 221.91 220.49 218.97 225.65 221.00 220.89 223.11 223.52 218.64 222.94 217.08 226.10  1.59 1.95 2.04 2.04 1.91 1.80 1.63 1.57 1.41 1.50 1.40 1.25 1.28 1.31  5.00 74.44  Vol(mL) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  Time (days)  24.02 28.03 30.03 34.97 35.99  10 95.02 104.53 250  Head (wt %)  ' >*'"'.'''  2.54  of 15 microns  E (Ag/AgCI) Eh(mV)  Sample (mL)  h  Analysis  Mass(g) 116.25 10 95.02 226.10  8 0  Thermophiles  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  480 387 408 430 458 459 477 508 525 537 579 599 613 614  700 607 628 650 678 679 697 728 745 757 799 819 833 834  Copper 30.4  5  7.67 4.95 6.39 8.67  228.13 226.86 226.88 227.64  8.35 6.37 4.44 3.41 8.41 4.73 11.05  229.35 227.26 227.55 226.93 227.05 227.67 228.13  5  5  5  5  5  Iron 10.6  Arsenic 10.5  Antimony 0.55  2617.25 0  1996.30 0.20088  459.5 0  9.5 0  3508.00 5614.75 6073.25 6831.40 101.63 34  373.75 781.45 2643.10 3623.25 19.33 2.8748  224.5 592.0 874.0 1020.0 0.5 12  1.5  BMBRUV'- »:."* •'  7.0 0.7  " t"  Weight of Element Copper  Iron  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g) V ^ . ' - V ' • ''" Calculated Head (g % Difference  0.53 0.0200 0.01909  ;  Medium Added Final Added (mL) Water (g) Mass (g)  1.52 0.0262 0  Arsenic 0.525 0.0046 0  0.01754 0.00187 0.001123 0.028074 0.00391 0.00296 0.030366 0.01322 0.00437 0 0.001 0 0 0.001 0 0 0.001 0 0.7141 0.3787 0.1066 0.025408 0.00483 0.000125 0.8636 0.07302 0.3048  Antimony 0.0275 0.0001 0 0.0000075 0 . 0.000035 0 0 0 0.0000 . 0 0.01778  %  % Extraction  Calculated Head Measured Head  1.653 -8.744 : •'  47.75 51.93  0.434 18.204 \T^/  : ;  • * *  83.16 68.02  0.415 20.876  0.018 35.536  .-;.*''.• >•.:  26.63 21.07  -0.30 -0.19  185  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.45 1 12.91 97.72 0.01754 2 19.96 99.64 0.02807375 3 28.03 97.39 0.03036625 35.99 104.53 Filtrate Wash 250.00  Tot. Cu Sampled (g) 0.01754 0.04561 0.07598  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.343 0.559 0.591 0.714 0.025  0.317 0.551 0.611 0.764 0.789  20.83 36.24 40.19  19.16 33.32 36.96  51.93  47.75  Fe(aq) total  %Fe indicated  %Fe actual  0.02 0.06 0.24 0.36 0.36  3.12 10.92 44.80  3.82 13.36 54.77  68.61  83.87  As(aq)total  %As indicated  %As actual  0.02 0.06 0.08 0.11 0.11  3.30 10.57 16.12  4.18 13.36 20.37  21.07  26.63  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  0.19 -0.32 2.16  0.29 -0.49 3.35  -0.19  -0.30  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.45 1 12.91 97.72 19.96 2 99.64 3 28.03 97.39 35.99 104.53 Filtrate Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.000864347 0.002902847 0.012211097  0.00086 0.00377 0.01598  0.037 0.078 0.257 0.3787 0.0048325  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.45 1 12.91 97.72 0.0011225 0.00112 0.02193814 2 19.96 99.64 0.00296 0.00408 0.05898688 3 28.03 97.39 0.00437 0.00845 0.08511886 35.99 104.53 Filtrate 0.11 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.45 1 12.91 97.72 0.0000075 . 0:00001 0.00014658 2 19.96 99.64 0 0.00001 0 3 28.03 97.39 0.000035 0.00004 0.00068173 Filtrate 35.99 104.53 0.00 Wash 250.00 0.00  Moderate Thermophiles, 5 g Enargite, P Test UB8-T37  Moderate  Date 4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun  Hour 12:25 10:35 10:45 11:30 10:20 11:20 12:15 11:30 12:50  28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  12:50 13:05 13:15 11:40 12:10  Enargite In (g): Total Water (g):  Time (days)  Initial Mass (g)  0.00 2.92 5.93 8.96 12.91 13.95 15.99 19.96 22.02  228.40 222.14 238.90 232.43 224.08 230.53  PH 1.59 1.87 1.90 1.82 1.78 1.68  226.12 224.29 224.40  1.55 1.52 1.39  24.02 28.03 30.03 34.97 35.99  224.75 219.53 225.12 217.88 227.19  1.51 1.45 1.29 1.32 1.34  5.02 76.67  Vol (mL) Mass (g) Flask Weight (g): 117.83 :•" Innoculum in: 10 10 Medium in: 95.05 95.05 ,-y, f g 227.19 Total Final Weight (g): 102.51 Filtrate Volume (mL) W a s h Volume (mL) 250 3.26 Solid Residue (g)  8 0  of 37 microns  Thermophiles E„ (Ag/AgCI) E h(mV) 488 708 396 616 435 655 450 670 462 682 462 682 477 697 498 718 509 729  Sample (mL)  Medium Added Final Added (mL) Water (g) Mass (g)  5  5  5  743 769 806 829 823  5  5  Analysis Head (wt %)  Copper 32.4  Iron 7.2  Arsenic 12  Antimony 0.39  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 P L S (mg/L) W a s h (mg/L) Solid Residue (wt %  2617.25 0  1996.300.201  459.5 0  9.5 0  2857.85 4371.40 5325.75 6175.90 73.20 32  276.60 411.75 1036.55 1830.80 5.07 2.9224  426.5 753.0 809.5 749.0 0.8 12  0.4  Weight of Element Copper  Iron  Head (g) 1.62648 Innoculum (g) 0.0262 Medium (g) 0 Samples (g): #1 0.014289 #2 0.021857 #3 0.026629 Medium Added (g): #1 0 #2 0 #3 0 0.6331 P L S (g) W a s h (g) 0.0183 Solid Residue (g) 1.0432  0.36144 0.0200 0.01909  0.6024 0.0046 0  0.019578 0.0001 0  0.00138 0.00206 0.00518  0.002133 0.003765 0.004048  0 0 0  0.001 0.001 0.001 0.1877 0.00127 0.09527  0 0 0 0.0768 0.0002 0.3912  0 0 0 0.0000 0 0.01304  .  •• •  -.•  1.731 -6.438  0.251 30.620 ; ' .  39.74 42.30  Antimony  Arsenic  v-  •  62.01 43.02  ..  -<•  0.474 21.393 •-  .  0.013 33.880  '." - . . . .  17.39 13.67  245.19  8.65  232.73  6.72 4.30 4.60  232.84 228.59 229.00  3.73 9.82 4.44 11.36  228.48 229.35 229.56 229.24  5  523 549 586 609 603  Calculated Head (g % Difference % Extraction Calculated Head Measured Head  23.05  -0.73 -0.49  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.55 1 12.91 101.23 0.01428925 2 19.96 101.44 0.021857 3 28.03 96.68 0.02662875 Filtrate 35.99 102.51 Wash 250.00  Tot. Cu Sampled (g) 0.01429 0.03615 0.06278  Cu in sol'n (g) Cu(aq) total (g) 0.289 0.443 0.515 0.633 0.018  %Cu indicated %Cu actual  0.263 0.432 0.525 0.670 0.688  16.18 26.53 32.27  15.20 24.93 30.32  42.30  39.74  Fe(aq)total  %Fe indicated  %Fe actual  0.01 0.02 0.08 0.17 0.17  2.22 6.03 22.20  3.21 8.70 32.00  46.75  67.39  As(aq)total  %As indicated  %As actual  0.04 0.07 0.08 0.08 0.08  6.40 12.27 13.21  8.15 15.61 16.80  13.67  17.39  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  -0.49 -0.49 -0.49  -0.73 -0.73 -0.73  -0.49  -0.73  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.55 1 12.91 101.23 2 19.96 101.44 3 28.03 96.68 Filtrate 35.99 102.51 Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.000378597 0.001054347 0.004178347  0.00038 0.00143 0.00561  0.028 0.042 0.100 0.1877 0.0012675  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.55 1 12.91 101.23 0.0021325 0.00213 0.043174595 2 19.96 101.44 0.003765 0.00590 0.07638432 3 28.03 96.68 0.0040475 0.00995 0.07826246 Filtrate 35.99 102.51 0.08 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb 0.0000 105.55 1 12.91 101.23 2 19.96 101.44 3 28.03 96.68 Filtrate 35.99 102.51 Wash 250.00  sampled Tot. Sb Sample Sb in sol'n (g) 0 0 0  0.00000 0.00000 0.00000  0 0 0 0.00 0.00  Moderate Thermophiles, 10 g Enargite, P Test#B7-T10  Moderate  Time (days)  Initial Mass (g)  0.00 5.93 8.96 12.91 13.95  232.54 226.51 226.48 228.26 225.67 231.25  12:10 11:25 12:45  15.99 19.96 22.01  12:45 13:00 13:10 11:20 12:10  24.01 28.02 30.03 34.95 35.99  Date  Hour  4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun  12:25 10:30 10:45 11:25 10:20 11:15  20-Jun 24-Jun 26-Jun 28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  Enargite In (g):  2.92  Vol (mL) Flask Weight (g): Innoculum in: Medium in:  10 95.07  Total Final Weight (g): Filtrate Volume (mL)  105.61  W a s h Volume (mL) Solid Residue (g)  s  ;  -  233.03  :  V;  250 '  '.  1  ' ,* 6.25  of 10 microns  E„ (Ag/AgCI) E (mV) h  Sample Medium Added Final (mL) Added (mL) Water (g) Mass (g)  446 376 394 425 442 450  666 596 614 645 662 670  227.36 226.08 228.83  1.62 2.04 2.05 1.99 1.79 1.66 1.48 1.37 1.27  463 469 469  683 689 689  229.41 225.68 228.87 223.75 233.03  1.32 1.30 1.15 1.20 1.18  480 496 494 519 527  700 716 714 739 747  5  5  Copper 31.2  Iron 11.6  Arsenic 10.5  Antimony 0.55  Innoculum (mg/L) Medium (g/L) Samples (mg/L):  2617.25 0  1996.30 0.201  459.5 0  9.5 0  #1 #2 #3 P L S (mg/L)  5968.50 9886.45 12384.60 14906.80  546.25 1236.35 2387.90 2991.25 16.39 11  300.0 1205.0 1904.0 2317.5 7.7 11  0.5 1.0 5.0  Head (wt %)  M a s s (g) 116.91 10 95.07  •  PH  Analysis  10.00 70.56  Total Water (g):  8 0  Thermophiles  W a s h (mg/L) Solid Residue (wt °/<  247.96 27  5  6.26 7.41 4.83 7.54  232.77 233.89 233.09 233.21  6.50 6.55 4.24  233.86 232.63 233.07  4.03 7.53 4.26 11.41  233.44 233.21 233.13 235.16  5  5  5  0.6  „!*"" •  Weight of Element Copper Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 ' #3 P L S (g) W a s h (g) Solid Residue (g)  Iron  Arsenic  1.16 0.0200 0.0191  1.05 0.0046 0  0.055 0.0001 0  0.029843 0.049432 0.061923  0.00273 0.00618 0.01194  0.0015 0.006025 0.00952  0.0000025 0.000005 0.000025  0 0 0 1.5743 0.06199 1.6875  0.001 0.001 0.001 0.3159 0.0041 0.6875  0 0' 0 0.2448 0.001925 0.6875  0 0 0 0.0000 0 0.0375  ! BIi..>>... 0.986 14.976  0.947 9.845  .,MI»<J '-<-*>;S 0.037 31.932  30.29 25.76  27.37 24.68  111*-., v• ' Calculated Head (g; 3.439 % Difference -10.219  :  % Extraction Calculated Head Measured Head  Antimony  3.12 0.0262 0  50.93 56.13  'is  -0.17 -0.11  189  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.63 1 12.91 98.76 0.0298425 19.96 99.17 2 0.04943225 3 28.02 98.77 0.061923 105.61 Filtrate 35.99 Wash 250.00  Tot. Cu Sampled (g) 0.02984 0.07927 0.14120  Cu in sol'n (g) Cu(aq) total (g) 0.589 0.980 1.223 1.574 0.062  %Cu indicated %Cu actual  0.563 0.984 1.276 1.689 1.751  18.05 31.54 40.91  16.38 28.62 37.12  56.13  50.93  Fe(aq)total  %Fe indicated  %Fe actual  0.03 0.10 0.22 0.30 0.30  2.93 8.85 18.61  3.45 10.41 21.89  25.87  30.42  As(aq)total  %As indicated  %As actual  0.03 0.12 0.19 0.26 0.26  2.38 11.09 18.19  2.64 12.30 20.18  24.68  27.37  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  -0.08 0.01 0.74  -0.12 0.02 1.09  -0.11  -0.17  Iron Output  Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.00 105.63 1 12.91 98.76 0.001726847 0.00173 0.05394765 2 19.96 99.17 0.005177347 0.00690 0.12260883 3 28.02 98.77 0.010935097 0.01784 0.235852883 35.99 105.61 Filtrate 0.3159 Wash 250.00 0.0040975  Arsenic  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.63 1 12.91 98.76 0.0015 0.00150 0.029628 2 19.96 99.17 0.006025 0.00753 0.11949985 3 28.02 98.77 0.00952 0.01705 0.18805808 Filtrate 35.99 105.61 0.24 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.63 1 12.91 98.76 0.0000025 0.00000 0.00004938 2 19.96 99.17 0.000005 0.00001 0.00009917 3 28.02 98.77 0.000025* 0.00003 0.00049385 . Filtrate 35.99 105.61 0.00 Wash 250.00 0.00  Moderate Thermophiles, 10 g Enargite, P Test#B7-T15 Date 4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun  Hour 12:25 10:30 10:45 11:25 10:20 11:15 12:10 11:25 12:45  28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  12:45 13:00 13:10 11:20 12:10  Enargite In (g): Total Water (g):  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  8 0  of 15 microns  Moderate Thermophiles Time (days)  Initial Mass (g)  0.00 2.92 5.93 8.96 12.91 13.95 15.99 19.96 22.01  231.19 225.19 225.95 226.34 223.21 230.31 226.09 225.03 227.31  pH 1.63 2.31 2.34 2.36 2.25 2.13 1.92 1.65 1.42  24.01 28.02 30.03 34.95 35.99  227.99 219.96 227.85 221.77 230.28  1.49 1.37 1.24 1.31 1.23  10.00 72.56  Analysis Head (wt %)  Vol (mL) Mass (g) ;• .) 115.57 10 10 95.06 95.06 ;  •  • H  104.50 250  r  230 28  6.01  E„ (Ag/AgCI) Eh(mV) 462 362 368 385 402 428 456 488 492  682 582 588 605 622 648 676 708 712  512 536 545 556 566  732 756 765 776 786  Copper 30.4  Innoculum (mg/L) 2617.25 Medium (g/L) 0 Samples (mg/L): #1 4937.80 #2 8875.85 #3 10810.85 PLS (mg/L) 11897.30 Wash (mg/L) 196.61 32 Solid Residue (wt % • , •' . Weight of Element Copper Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g) Calculated Head (g % Difference % Extraction Calculated Head Measured Head  Sample (mL)  5  Medium Added Final Added (mL) Water (g) Mass (g) 232.46 232.65 232.01 232.37  6.77 6.26 4.45  232.86 231.29 231.76  11.82 4.07 10.39  231.78 231.92 232.16  5  5  5  5  5  Iron 10.6  Arsenic 10.5  Antimony 0.55  1996.30 0.20088  459.5 0  9.5 0  52.0 436.85 900.25 754.0 2577.10 1293.5 4152.20 1601.5 29.01 1.8 7.2 12 i • •. . Iron Arsenic  7.27 6.70 5.67 9.16  1.5 2.0 5.0  0.6 Antimony  3.04 0.0262 0  1.06 0.0200 0.0191  1.05 0.0046 0  0.055 0.0001 0  0.024689 0.044379 0.054054  0.00218 0.0045 0.01289  0.00026 0.00377 0.006468  0.0000075 0.00001 0.000025  0 0 0 1.2433 0.049153 1.9232  0.001 0.001 0.001 0.4339 0.00725 0.43272  0 0 0 0.1674 0.00045 0.7212  0 0 0 0.0000 0 0.03606  3.313 -8.966  0.851 19.681  0.895 14.771  0.036 34.532  41.94 45.70  49.17 39.50  19.41 16.54  -0.15 -0.10  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.62 1 12.91 97.64 0.024689 19.96 99.46 2 0.04437925 3 28.02 94.39 0.05405425 35.99 104.50 Filtrate Wash 250.00  Tot. Cu Sampled (g) 0.02469 0.06907 0.12312  Cu in sol'n (g) Cu(aq) total (g) 0.482 0.883 1.020 1.243 0.049  %Cu indicated %Cu actual  0.456 0.881 1.063 1.340 1.389  15.00 28.99 34.98  13.76 26.60 32.10  45.70  41.94  Fe(aq) total  %Fe indicated  %Fe actual  0.02 0.07 0.22 0.41 0.42  2.14 6.56 21.07  2.67 8.17 26.23  39.74  49.47  As(aq)total  %As indicated  %As actual  0.00 0.07 0.12 0.17 0.17  0.05 6.73 11.57  0.05 7.90 13.58  16.54  19.41  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  0.09 0.20 0.72  0.14 0.31 1.10  -0.10  -0.15  Iron Output  Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.00 105.62 1 12.91 97.64 0.001179847 0.00118 0.043 2 19.96 99.46 0.003496847 0.00468 0.090 3 28.02 94.39 0.011881097 0.01656 0.243 Filtrate 35.99 104.50 0.4339 Wash 250.00 0.0072525  Arsenic  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.62 1 12.91 97.64 0.00026 0.00026 0.00507728 2 19.96 99.46 0.00377 0.00403 0.07499284 3 28.02 94.39 0.0064675 0.01050 0.122093465 35.99 104.50 Filtrate 0.17 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.62 1 12.91 97.64 0.0000075 0.00001 0.00014646 2 19.96 99.46 0.00001 0.00002 0.00019892 3 28.02 94.39 0.000025 0.00004 0.00047195 35.99 104.50 Filtrate 0.00 Wash 250.00 0.00  Moderate Thermophiles, 10 g Enargite, P Test UB7-T37  Moderate  Date 4-Jun 7-Jun 10-Jun 13-Jun 17-Jun 18-Jun 20-Jun 24-Jun 26-Jun  Hour 12:25 10:30 10:45 11:25 10:20 11:15  28-Jun 2-Jul 4-Jul 9-Jul 10-Jul  12:45 13:00 13:10 11:20 12:10  12:10 11:25 12:45  Enargite In (g): Total Water (g):  0.00 2.92 5.93 8.96  229.31 226.85 219.52 223.28 223.28 228.65  pH 1.74 1.99 1.97 1.94 1.82 1.70  223.87 223.72 225.31 226.42 221.94 225.65 219.36 229.26  13.95 15.99 19.96 22.01 24.01 28.02 30.03 34.95 35.99  10.01  ;  :  10 95.07  Total Final Weight (g): II Filtrate Volume (mL) 103.13 Wash Volume (mL) Solid Residue (g)  Initial Mass (g)  250 . / *''f?t  Mass (g) 113.76 10 95.07 229.26  7.71  of 37 microns  Eh (Ag/AgCI)  Sample (mL)  Medium Added Final Added (mL) Water (g) Mass (g)  470 379 405 435 447 447  Eh (mV) 690 599 625 655 667 667  1.57 1.54 1.39  458 477 481  678 697 701  1.52 1.44 1.28 1.32 1.29  496 513 517 553 560  716 733 737 773 780  5  5  Copper 32.4  Iron 7.2  Arsenic 12  Antimony 0.39  Innoculum (mg/L) 2617.25 Medium (g/L) 0 Samples (mg/L): #1 4553.90 #2 6878.55 #3 8889.30 10371.40 PLS (mg/L) Wash (mg/L) 200.02 Solid Residue (wt "A 30  1996.30 0.201  459.5 0  9.5 0  334.90 517.40 872.70 1572.75  391.5 1038.5 1468.0 1278.5 12.8 12  0.0 0.0 0.0  Weight of Element Copper  Iron  Analysis Head (wt %)  77.99  Vol (mL) Flask Weight (g): Innoculum in: Medium in:  Time (days)  12.91  8 0  Thermophiles  10.56 6.1  5  5  Arsenic  5  0.4 Antimony  0.72072 0.0200 0.0191  1.2012 0.0046 0  0.039039 0.0001 0  0.02277 0.034393 0.044447  0.00167 0.00259 0.00436  0.001958 0.005193 0.00734  0 0 0  Medium Added (g): #1 0 0 #2 #3 0 PLS (g) 1.0696 Wash (g) 0.050005 Solid Residue (g) 2.313  0.001 0.001 0.001 0.1622 0.00264 0.47031  0 0 0 0.1319 0.0032 0.9252  0 0 0 0.0000 ' 0 . 0.03084  3.508 -8.165  0.602 16.514  1.070 10.910  0.031 21.245  34.07 36.85  21.84 18.23  13.54 12.07  -0.31 -0.24  Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  229.86 229.81 231.70 230.94  8.60 6.20 5.29  232.47 229.92 230.60  4.05 7.98 4.51 11.98  230.47 229.92 230.16 231.34  5  3.24324 0.0262 0  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3  3.01 10.29 8.42 7.66  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.54 1 12.91 99.51 0.0227695 2 19.96 99.95 0.03439275 98.17 0.0444465 3 28.02 35.99 Filtrate 103.13 Wash 250.00  Tot. Cu Sampled (g) 0.02277 0.05716 0.10161  Cu in sol'n (g) Cu(aq) total (g) 0.453 0.688 0.873 1.070 0.050  %Cu indicated %Cu actual  0.427 0.684 0.904 1.145 1.195  13.17 21.09 27.86  12.17 19.50 25.76  36.85  34.07  Fe(aq)total  %Fe indicated  %Fe actual  0.01 0.03 0.07 0.14 0.14  1.85 4.41 9.12  2.22 5.28 10.92  20.10  24.08  As(aq)total  %As indicated  %As actual  0.03 0.10 0.15 0.14 0.14  2.86 8.42 12.21  3.21 9.45 13.71  12.07  13.54  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  -0.24 -0.24 -0.24  -0.31 -0.31 -0.31  -0.24  -0.31  Iron Output  Sample # Time (days) Sol'n Vol. (nIL) 0.00 105.54 1 12.91 99.51 2 • 19.96 99.95 3 28.02 98.17 Filtrate 35.99 103.13 Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.000670097 0.001582597 0.003359097  0.00067 0.00225 0.00561  0.033 0.052 0.086 0.1622 0.00264  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.54 1 12.91 99.51 0.0019575 0.00196 0.038958165 2 19.96 99.95 0.0051925 0.00715 0.103798075 3 28.02 98.17 0.00734 0.01449 0.14411356 35.99 103.13 Filtrate 0.13 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (nnL) g Sb 0.0000 105.54 1 12.91 99.51 2 19.96 99.95 3 28.02 98.17 Filtrate 35.99 103.13 Wash 250.00  sampled Tot. Sb Sample Sb in sol'n (g) 0 0 0  0.00000 0.00000 0.00000  0 0 0 0.00 0.00  Extreme Thermophiles, 2 g Enargite, P Test UB3-E10  Date 14-Feb 18-Feb 21-Feb 22-Feb 26-Feb 28-Feb 5-Mar 7-Mar 11-Mar 12-Mar 14-Mar 15-Mar 19-Mar 21-Mar 22-Mar  Extreme  Hour 10:00 9:30 11:35 10:55 10:10 10:20 10:50 11:35 12:45 10:10 11:05 12:05 12:40 20:40 18:40  Enargite In (g):  2.00  Total Water (g):  468.89  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g) Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  Time Initial (days) Mass (g) 0.00 238.47 3.98 195.02 7.07 203.67 8.04 227.51 12.01 192.75 14.01 221.81 19.03 185.16 21.07 215.90 25.11 195.01 26.01 229.30 28.05 215.84 29.09 227.29 33.11 196.08 35.44 213.66 36.36 236.18  Vol (mL) Mass (g) 130.98 10 10 95.01 95.01 ____ 236.18  E (Ag/AgCI) E„ (mV) 477 697 387 607 420 640 402 622 398 618 412 632 404 624 649 869 h  pH 1.53 1.60 1.30 1.23 1.19 1.12 1.17 1.21 1.24 1.25 1.20 1.23 1.28 1.27  661 655 682 646 645 641  Sample (mL)  Medium Added Final Added (mL) Water (g) Mass (g)  5  5  5  5  881 875 902 866 865 861  5  5  56.17 47.60 23.78 58.35 29.79 65.88 24.15 44.24 9.65 22.80 11.41 42.67 32.40  Analysis  Copper  Iron  Arsenic  Antimony  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  31.2 2690.40 0  11.6 4107.10 0.201  10.5 255.5 0  0.55 18.0 0  2274.75 5658.60 7195.00 6010.55 76.58 0.5335  847.05 759.50 915.60 779.35 6.71 17  355.0 335.5 26.5 19.0  2.0 2.0 12.5 2.0  20  0.5  Arsenic 0.21 0.0026 0  Antimony 0.011 0.0002 0  0.011374 0.00424 0.028293 0.0038 0.035975 0.00458  0.001775 0.001678 0.000133  0.00001 0.00001 0.0000625  0 0.001 0 0.001 0 0.001 0.6125 0.0794 0.019145 0.00168 0.004748 0.1513  0 0 0 0.0019 0 0.178  0 0 0 0.0002 0 0.00445  250  ,v  0.89  of 10 microns  8 0  Thermophiles  Weight of Element Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g) Lf*«:  •V  Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  r  '  , v»•-'.':  Copper 0.624 0.0269 0  ••  Iron 0.232 0.0411 0.01909  f '  '-. i .  0.685 -9.793  0.182 21.623 «  99.31 109.03  0.181 13.826  •;.  16.79 13.16  0.005 58.579 '  ,.,  1.64 1.41  2.33 0.97  251.19 251.27 251.29 251.10 251.60 251.04 240.05 239.25 238.95 238.64 238.70 238.75 246.06  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.49 1 8.04 94.53 0.01137375 2 14.01 88.83 0.028293 26.01 3 96.32 0.035975 Filtrate 36.36 101.90 Wash 250.00  Tot. Cu Sampled (g) 0.01137 0.03967 0.07564  Cu in sol'n (g) Cu(aq) total (g) 0.215 0.503 0.693 0.612 0.019  %Cu indicated %Cu actual  0.188 0.487 0.706 0.661 0.680  30.15 78.06 113.11  27.46 71.10 103.02  109.03  99.31  Fe(aq)total  %Fe indicated  %Fe actual  0.04 0.03 0.05 0.04 0.04  16.81 11.38 20.31  21.45 14.52 25.91  17.25  22.01  As(aq) total  %As indicated  %As actual  0.03 0.03 0.00 0.00 0.00  14.76 13.82 1.64  17.13 16.04 1.91  1.41  1.64  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  0.08 0.07 9.49  0.20 0.17 22.91  0.97  2.33  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.49 1 8.04 94.53 2 14.01 88.83 3 26.01 96.32 Filtrate 36.36 101.90 Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.003230847 0.002793097 0.003573597  0.00323 0.00602 0.00960  0.080071637 0.067466385 0.088190592 0.0794 0.0016775  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.49 1 8.04 94.53 0.001775 0.00178 0.03355815 2 14.01 88.83 0.0016775 0.00345 0.029802465 3 26.01 96.32 0.0001325 0.00359 0.00255248 Filtrate 36.36 101.90 0.00 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.49 1 8.04 94.53 0.00001 0.00001 0.00018906 2 14.01 88.83 0.00001 0.00002 0.00017766 3 26.01 96.32 0.0000625 0.00008 0.001204 36.36 101.90 Filtrate 0.00 Wash 250.00 0.00  196  Extreme Thermophiles, 2 g Enargite (2), P Test #B4-E10  8 0  of 10 microns  Extreme Thermophiles  Date 4-Apr 8-Apr 12-Apr 15-Apr 16-Apr 18-Apr 23-Apr 24-Apr 26-Apr  Hour 14:40 13:00 10:15 11:05 12:00 11:20 10:25 20:10 11:35  29-Apr 30-Apr 3-May 7-May 10-May  10:40 11:40 11:10 10:55 10:30  Enargite In (g):  Time (days)  Initial Mass (g)  0.00 3.93 7.82 10.85 11.89 13.86 18.82 20.23 21.87  226.63 196.00 194.53 203.74 218.58 211.18 192.38 216.50 214.84  24.83 25.88 28.85 32,84 35.83  203.94 219.28 202.56 194.29 202.74  2.01 268.64  Total Water (g):  Vol (mL) Mass (g) Flask Weight (g): • 118.97 10 10 Innoculum in: 95.00 95.00 Medium in: 202.74 Total Final Weight (g): 79.52 I , '1 Filtrate Volume (mL) 250 Wash Volume (mL) Solid Residue (g) ' ! 0.95  1 '."  :  E  h  (Ag/AgCI)  Eh (mV)  1.14 1.22 1.19  444 419 469 501 566 588 590 596 598  664 639 689 721 786 808 810 816 818  1.22 1.13 1.17 1.18 1.14  608 588 580 571 573  828 808 800 791 793  PH 1.57 1.74 1.56 1.34 1.22 1.26  Sample (mL)  Medium Added Added (mL) Water (g)  5  5  5  5  5  5  Analysis  Copper  Iron  Arsenic  Antimony  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  31.2 2428.20 0  11.6 979.30 0.201  10.5 98.5 0  0.55  6189.70 6616.40 5942.55 6998.30 120.55 0.6158  477.35 747.45 666.65 813.70 9.40 18  193.5 21.5 14.0 25.5 0.7 21  5.5 13.0 5.5 0.0  Copper 0.62712 0.0243 0  Iron 0.23316 0.0098 0.01908  Arsenic 0.21105 0.0010 0  Antimony 0.011055 0.0000 0  0.030949 0.033082 0.029713  0.00239 0.00374 0.00333  0.000968 0.000108 0.00007  0.0000275 0.000065 0.0000275  0 0 0 0.5565 0.030138 0.00585  0.001 0.001 0.001 0.0647 0.00235 0.171  0 0 0 0.0020 0.000175 0.1995  0 0 0 0.0000 0 0.0038  0.662 -5.555  0.216 7.522  0.202 4.353  0.004 64.541  99.12 104.62  20.69 19.14  1.17 1.12  3.06 1.09  Weight of Element Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g)  0  0.4  ••<. faup* Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  Final Mass (g)  32.67 35.19 23.53 9.80 18.03 36.39 11.33 12.84  228.67 229.72 227.27 228.38 229.21 228.77 227.83 227.68  23.39 7.54 25.17 32.76  227.33 226.82 227.73 227.05  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.65 1 11.89 97.60 0.0309485 2 20.23 95.52 0.033082 3 25.88 98.30 0.02971275 35.83 Filtrate 79.52 Wash 250.00  Tot. Cu Sampled (g) 0.03095 0.06403 0.09374  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.604 0.632 0.584 0.557 0.030  0.580 0.639 0.624 0.626 0.656  92.46 101.84 99.49  87.59 96.48 94.25  104.62  99.12  Fe(aq) total  %Fe indicated  %Fe actual  0.04 0.06 0.06 0.05 0.06  15.78 26.42 23.91  17.07 28.57 25.85  24.56  26.56  As(aq)total  %As indicated  %As actual  0.02 0.00 0.00 0.00 0.00  8.48 0.96 0.69  8.87 1.01 0.73  1.12  1.17  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  4.86 11.48 5.73  13.69 32.38 16.15  1.09  3.06  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.65 1 11.89 97.60 2 20.23 95.52 3 25.88 98.30 35.83 Filtrate 79.52 Wash 250.00  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.001382347 0.002732847 0.002328847  0.00138 0.00412 0.00644  0.04658936 0.071396424 0.065531695 0.0647 0.00235  Arsenic Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.65 1 11.89 97.60 0.0009675 0.00097 0.0188856 2 20.23 95.52 0.0001075 0.00108 0.00205368 3 25.88 98.30 0.00007 0.00115 0.0013762 35.83 79.52 Filtrate 0.00 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.65 1 11.89 97.60 0.0000275 0.00003 0.0005368 2 20.23 95.52 0.000065 0.00009 0.00124176 3 25.88 98.30 0.0000275 0.00012 0.00054065 Filtrate 35.83 79.52 0.00 Wash 250.00 0.00  Extreme Thermophiles, 2 g Enargite, P Test UB3-E15  8 0  of 15 microns  Extreme Thermophiles  Date  Hour  14-Feb 18-Feb 21-Feb 22-Feb 26-Feb 28-Feb 5-Mar 7-Mar 11-Mar 12-Mar 14-Mar 15-Mar 19-Mar 21-Mar 22-Mar  10:00 9:30 11:35 10:55 10:10 10:20 10:50 11:35 12:45 10:10 11:05 12:05 12:40 20:40 18:40  Enargite In (g):  2.01  Total Water (g):  385.33  Time (days) 0.00 3.98 7,07 8.04 12.01 14,01 19.03 21.07 25.11 26,01 28.05 29,09 33.11 35.44 36.36  Vol (mL) Mass (g) Flask Weight (g): 145.88 .Innoculum in: 10 10 Medium in: 95.17 95.17 Total Final Weight (g): fipflll"'.; . 244.92 Filtrate Volume (mL) 93.77 * 4 i ' \ " Wash Volume (mL) 250 0.94 Solid Residue (g) v  Initial Mass (g)  253.63 205.12 215.97 243.92 209.37 231.87 197.13 233.12 218.50 245.54 234.01 243.81 214.04 231.82 244.92  •  PH  E„ (Ag/AgCI) E„ (mV)  1.70 1.80 1.76 1.85 1.43 1.50 1.36 1.43  464 405 416 416 444 446 460 486  684 625 636 636 664 666 680 706  1.43 1.35 1.32 1.30 1.32 1.32  648 651 671 643 642 647  Sample (mL)  Medium Added Final Added (mL) Water (g) Mass (g)  5  5  5  5  868 871 891 863 862 867  5  5  Analysis  Copper  Iron  Arsenic  Antimony  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  30.4 2690.40 0  10.6 4107.10 0.20088  10.5 255.5 0  0.55 18.0 0  1573.15 2901.10 6246.80 6525.40 38.17 1.5316  579.25 648.20 490.15 546.20 2.75 16  153.0 262.5 56.5 23.5  4.5 1.5 14.5 8.0  -  Weight of Element Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g)  • .- :  Copper 0.61104 0.0269 0  16 0.6 '•" • .'-."0 it, .; iv'AiJ,:- >'.' Iron Arsenic Antimony 0.21306 0.21105 0.011055 0.0411 0.0026 0.0002 0.01912 0 0 "  -  i.  -  0.007866 0.0029 0.014506 0.00324 0.031234 0.00245  0.000765 0.001313 0.000283  0.0000225 0.0000075 0.0000725  0 0.001 0 0.001 0 0.001 0.6119 0.0512 0.009543 0.00069 0.014397 0.1504  0 0 0 0.0022 0 0.1504  0 0 0 0.0008 0 0.00564  0.152 27.786  0.006 42.898 wV^^S"-' •• 10.66 6.08  -  Calculated Head (g) % Difference  0.663 -8.426  0.148 30.681  97.83 106.07  -1.83 -1.27  % Extraction  Calculated Head Measured Head  48.85 38.04 10;98 46.43 21.64 58.53 24.27 35.31 8.56 19.92 9.86 40.58 22.36  ,.  w*'  1.32 0.95  '  253.97 254.01 254.90 255.80 253.51 255.66 257.39 253.81 254.10 253.93 253.67 254.62 254.18  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.74 1 8.04 96.03 0.00786575 2 14.01 83.98 0.0145055 3 26.01 97.65 0.031234 Filtrate 36.36 93.77 Wash 250.00  Tot. Cu Sampled (g) 0.00787 0.02237 0.05361  Cu in sol'n (g) Cu(aq) total (g) 0.151 0.244 0.610 0.612 0.010  %Cu indicated %Cu actual  0.124 0.225 0.605 0.639 0.648  20.32 36.76 99.09  18.74 33.90 91.39  106.07  97.83  Fe(aq)total  %Fe indicated  %Fe actual  0.01 0.01 0.01 0.01 0.01  6.83 6.27 3.19  9.85 9.05 4.60  5.08  7.34  As(aq) total  %As indicated  %As actual  0.01 0.02 0.01 0.00 0.00  5.75 9.60 2.39  7.96 13.29 3.31  0.95  1.32  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  2.28 -0.29 11.45  3.99 -0.50 20.05  6.08  10.66  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.74 1 8.04 96.03 2 14.01 83.98 3 26.01 97.65 Filtrate 36.36 93.77 Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.001891847 0.002236597 0.001446347  0.00189 0.00413 0.00557  0.056 0.054 0.048 0.0512 0.0006875  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.74 1 8.04 96.03 0.000765 0.00077 0.01469259 2 14.01 83.98 0.0013125 0.00208 0.02204475 3 26.01 97.65 0.0002825 0.00236 0.005517225 Filtrate 36.36 93.77 0.00 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.74 1 8.04 96.03 0.0000225 0.00002 0.000432135 2 14.01 83.98 0.0000075 0.00003 0.00012597 3 26.01 97.65 0.0000725 0.00010 0.001415925 36.36 93.77 0.00 Filtrate Wash 250.00 0.00  Extreme Thermophiles, 2 g Enargite (2), P Test#B4-E15  Date 4-Apr 8-Apr 12-Apr 15-Apr 16-Apr 18-Apr 23-Apr 24-Apr 26-Apr 29-Apr 30-Apr 3-May 7-May 10-May  Enargite In (g): Total Water (g):  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  Extreme  Hour 14:40 13:00 10:15 11:05 12:00 11:20 10:25 20:10 11:35 10:40 11:40 11:10 10:55 10:30  Time (days) 0.00 3.93 7.82 10.85 11.89 13.86 18.82 20.23 21.87 24.83 25.88 28.85 32.84 35.83  2.00 289.66  Vol (mL) Mass (g) 132.12 10 10 95.03 95.03 221.65 -*n,.y 74.95 250 0.92  Initial Mass (g) 239.96 200.90 208.90 242.20 232.37 221.31 196.08 228.80 226.72 216.43 232.08 212.03 201.32 221.65  8 0  of 15 microns  Thermophiles  PH 1.58 1.85 1.86 1.66 1.63 1.69 1.45 1.38 1.47 1.40 1.27 1.34 1.24 1.18  Analysis Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt % • • ~ r.")»f; Weight of Element Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g) Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  E„ (Ag/AgCI) E„ (mV) 444 664 370 590 386 606 437 657 445 665 432 652 447 667 449 669 478 698 511 731 555 775 592 812 606 826 619 839  Sample Medium Added Final (mL) Added (mL) Water (g) Mass (g)  5  5  5  5  5  5  Antimony  Copper  Iron  30.4 2428.20 0  10.6 979.30 0.20088  Arsenic 10.5 98.5 0  1898.90 2545.15 5040.85 7582.55 86.93 3.4  268.20 214.70 159.25 536.40 6.19 18  119.0 40.0 110.5 52.5 0.7 19  Copper 0.608 0.0243 0  Iron 0.212 0.0098 0.01909  '  0.55 0  r  '  Arsenic 0.21 0.0010 0  0.0 6.0 10.0 13.5 0.2 0.8 ... ...^ Antimony 0.011 0.0000 0  0.009495 0.00134 0.000595 0.012726 0.00107 0.0002 0.025204 0.0008 0.000553  0 0.00003 0.00005  0 0.001 0 0 0.001 0 0 0.001 0 0.5683 0.0402 0.0039 0.021733 0.00155 0.000175 0.03128 0.1656 0.1748  0 0 0 0.0010 0.00005 0.00736  0.644 -5.998  0.179 15.724  95.15 100.85  7.31 6.16  0.179 14.632  0.009 22.711  ''VlklMP;".  2.49 2.13  13.43 10.38  45.29 32.69  246.19 241.59  8.43 22.54 45.92 12.62 19.82 25.58 8.33 29.07 39.37  240.80 243.85 242.00 241.42 246.54 242.01 240.41 241.10 240.69  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.84 1 11.89 98.25 0.0094945 2 20.23 94.68 0.01272575 3 25.88 97.96 0.02520425 35.83 74.95 Filtrate Wash 250.00  Tot. Cu Sampled (g) 0.00949 0.02222 0.04742  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.187 0.241 0.494 0.568 0.022  0.162 0.226 0.492 0.591 0.613  26.69 37.20 80.88  25.18 35.10 76.30  100.85  95.15  Fe(aq)total  %Fe indicated  %Fe actual  0.02 0.01 0.01 0.03 0.03  7.81 4.97 2.74  9.27 5.90 3.25  15.07  17.89  As(aq)total  %As indicated  %As actual  0.01 0.00 0.01 0.00 0.00  5.10 1.62 5.06  5.97 1.89 5.93  2.13  2.49  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  0.00 5.16 9.18  0.00 6.68 11.88  10.38  13.43  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.84 1 11.89 98.25 2 20.23 94.68 3 25.88 97.96 35.83 74.95 Filtrate Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.000336597 6.90973E-05 -0.000208153  0.00034 0.00041 0.00020  0.026 0.020 0.016 0.0402 0.0015475  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.84 1 11.89 98.25 0.000595 0.00060 0.01169175 2 20.23 94.68 0.0002 0.00080 0.0037872 3 25.88 97.96 0.0005525 0.00135 0.01082458 Filtrate 35.83 74.95 0.00 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.84 1 11.89 98.25 0 0.00000 0 20.23 94.68 2 0.00003 0.00003 0.00056808 3 25.88 97.96 0.00005 0.00008 0.0009796 35.83 74.95 0.00 Filtrate Wash 250.00 0.00  Extreme Thermophiles, 2 g Enargite, P Test #B3-E37  Date 14-Feb 18-Feb 21-Feb 22-Feb 26-Feb 28-Feb 5-Mar 7-Mar 11-Mar 12-Mar 14-Mar 15-Mar 19-Mar 21-Mar 22-Mar  Hour 10:00 9:30 11:35 10:55 10:10 10:20 10:50 11:35 12:45 10:10 11:05 12:05 12:40 20:40 18:40  Enargite In (g):  2.00  Total Water (g):  418.76  Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  Time Initial (days) Mass (g) 0.00 ' 236.80 3.98 198.78 7.07 210.60 8.04 228.25 199.16 12.01 14.01 215.34 19.03 189.46 21.07 219.25 25.11 191.66 26,01 228.39 28.05 217.02 29.09 225.17 33.11 192.72 35,44 214.22 36.36 231.57  Vol (mL) Mass (g) , • ; • 129.14 10 10 95.07 95.07 231.57 99.15 250  111.12 1*11  Extreme  8 0  of 37 microns  Thermophiles  E (Ag/AgCI) E (mV) 482 702 429 649 486 706 496 716 477 697 481 701 500 720 571 791 h  pH 1.70 1.56 1.49 1.52 1.71 1.26 1.24 1.34  h  Sample (mL)  Medium Added Final Added (mL) Water (g) Mass (g)  5  5  5  5  1.32 1.34 1.28 1.29 1.34 1.34  620 620 630 607 622 632  840 840 850 827 842 852  5  5  Analysis Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  Copper  Iron  Arsenic  Antimony  32.4 2690.40 '0  7.2 4107.10 0.201  12 255.5 0  0.39 18.0 0  4221.20 5901.00 5998.70 6053.85 82.89 4.4  397.90 51.05 114.20 135.65 1.31 14  676.5 172.5 80.5 64.0 0.8 18  0.0 3.0 5.5 5.0 0.2 0.6  Copper 0.648 0.0269 0  Iron 0.144 0.0411 0.0191  sfev-sillita,-J«ili  Weight of Element Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g) «LV,:.;»J %V, .^re:  tam< r i Arsenic 0.24 0.0026 0  0.021106 0.00199 0.003383 0.029505 0.00026 0.000863 0.029994 0.00057 0.000403 0 0.001 0 0.001 0 0.001 0.6002 0.0134 0.020723 0.00033 0.04928 0.1568 ;•.  '«-•',»'•.  0 0 0 0.0063 0.0002 0.2016  - '?K, *, r  ;  calculated Head (g) 0.724 0.110 -11.719 % Difference 23.465 % Extraction . ,V''E;.< "fSS,*:: 93.19 -42.27 Calculated Head 104.11 -32.35 Measured Head  47.45 35.65 17.75 47.12 30.84 57.24 17.68 47.25 10.60 20.28 12.01 46.53 28.38  0.210 12.401  Antimony 0.0078 0.0002 0  0 0.000015 0.0000275 0 0 0 0.0005 0.00005 0.00672 SS.:. ." i.'M* 0.007 8.612 ;. ...... . - j 5 i i r  :  4.11 3.60  5.73 5.23  246.23 246.25 246.00 246.28 246.18 246.70 236.93 238.91 238.99 237.30 237.18 239.25 242.60  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.66 97.11 0.021106 1 8.04 2 14.01 84.20 0.029505 97.25 3 26.01 0.0299935 Filtrate 36.36 99.15 Wash 250.00  Tot. Cu Sampled (g) 0.02111 0.05061 0.08060  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.410 0.497 0.583 0.600 0.021  0.383 0.491 0.607 0.654 0.675  59.11 75.78 93.69  52.91 67.83 83.86  104.11  93.19  Fe(aq)total  %Fe indicated  %Fe actual  0.00 -0.04 -0.03 -0.03 -0.03  -1.69 -25.54 -20.81  -2.21 -33.37 -27.19  -18.95  -24.77  As(aq)total  %As indicated  %As actual  0.06 0.02 0.01 0.01 0.01  26.31 6.40 3.97  30.03 7.30 4.53  3.60  4.11  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  -2.31 0.93 4.74  -2.53 1.02 5.19  5.23  5.73  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.66 1 8.04 97.11 14.01 84.20 2 3 26.01 97.25 Filtrate 36.36 99.15 Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.000985097 -0.000749153 -0.000433403  0.00099 0.00024 -0.00020  0.039 0.004 0.011 0.0134 0.0003275  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.66 1 8.04 97.11 0.0033825 0.00338 0.065694915 2 14.01 84.20 0.0008625 0.00425 0.0145245 3 26.01 97.25 0.0004025 0.00465 0.007828625 36.36 99.15 Filtrate 0.01 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.66 0 0.00000 0 1 8.04 97.11 0.000015 0.00002 0.0002526 2 14.01 84.20 0.00004 0.000534875 3 26.01 97.25 0.0000275 36.36 99.15 0.00 Filtrate Wash 250.00 0.00  Extreme Thermophiles, 2 g Enargite(2), P Test #B4-E37  Date 4-Apr 8-Apr 12-Apr 15-Apr 16-Apr 18-Apr 23-Apr 24-Apr 26-Apr 29-Apr 30-Apr 3-May 7-May 10-May  Extreme  Hour 14:40 13:00 10:15 11:05 12:00 11:20 10:25 20:10 11:35 10:40 11:40 11:10 10:55 10:30  Enargite In (g):  2.01  Total Water (g):  313.37  Time (days) 0.00 3.93 7.82 10.85 11.89 13.86 18.82 20.23 21.87 24.83 25.88 28.85 32.84 35.83  Vol(mL) Mass(g) Flask Weight (g): K. ."• :-. 145.87 10 Innoculum in: 10 95.10 Medium in: 95.10 225.85 Total Final Weight (g): 75.46 Filtrate Volume (mL) 250 Wash Volume (mL) Solid Residue (g) 1.06  Initial Mass (g) 253.52 217.41 214.80 229.55 245.80 234.97 210.30 241.83 238.59 228.90 243.78 226.48 215.90 225.85  8 0  of 37 microns  Thermophiles  pH 1.56 1.84 1.86 1.74 1.70 1.74 1.44 1.40 1.47 1.40 1.26 1.27 1.30 1.22  E„ (Ag/AgCI) E (mV) 442 662 373 593 384 604 399 619 426 646 443 663 451 671 456 676 490 710 522 742 562 782 603 823 608 828 615 835 h  Medium Added Sample Final (mL) Added (mL) Water (g) Mass (g) >  5  5  5  5  5  5  Analysis  Copper  Iron  Arsenic  Antimony  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  32.4 2428.20 0  7.2 979.30 0.201  12 98.5 0  0.39  1416.45 3426:70 5010.05 7287.80 92.62 10  198.25 195.05 243.05 484.30 3.85 17  Weight of Element Copper Iron Head (g) 0.65124 0.14472 Innoculum (g) 0.0243 0.0098 Medium (g) 0 0.0191 Samples (g): #1 0.007082 0.00099 #2 0.017134 0.00098 #3 0.02505 0.00122 Medium Added (g): #1 0 0.001 #2 0 0.001 #3 0 0.001 0.5499 0.0365 PLS (g) Wash (g) 0.023155 0.00096 0.106 0.1802 Solid Residue (g) "' ' ,:-.\r„:' • •• ' . ...a . . . . ..j * ' • . * . Calculated Head (g) 0.704 0.189 -8.113 -30.583 % Difference % Extraction 84.94 Calculated Head 4.65 91.84 6.07 Measured Head  0  64.0 1.5 52.5 6.0 71.0 10.0 69.0 15.5 0.9 0.3 16 0.8 :ei<Sff? ..•„.t'»r- ' • .,- ;. Arsenic 0.2412 0.0010 0  Antimony 0.007839 0.0000 0  0.00032 0.000263 0.000355  0.0000075 0.00003 0.00005  0 0 0 0.0052 0.000225 0.1696  0 0 0 0.0012 0.000075 0.00848  J..  -' '  0.175 27.453 iSBk3.08 2.23  0.010 -25.171 .,  ^ ^ ^...  13.58 16.99  37.60 43.52 25.89 8.16 21.14 44.58 12.36 20.25 24.65 9.93 27.57 37.72  255.01 258.32 255.44 253.96 256.11 254.88 254.19 258.84 253.55 253.71 254.05 253.62  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.64 1 11.89 97.92 0.00708225 20.23 93.95 2 0.0171335 3 25.88 95.90 0.02505025 35.83 75.46 Filtrate Wash 250.00  Tot. Cu Sampled (g) 0.00708 0.02422 0.04927  Cu in sol'n (g) Cu(aq) total (g) 0.139 0.322 0.480 0.550 0.023  %Cu indicated %Cu actual  0.114 0.305 0.480 0.575 0.598  17.57 46.79 73.77  16.25 43.28 68.23  91.84  84.94  Fe(aq) total  %Fe indicated  %Fe actual  0.01 0.01 0.01 0.03 0.03  6.65 5.90 9.34  5.09 4.51 7.15  19.15  14.67  As(aq)total  %As indicated  %As actual  0.01 0.00 0.01 0.01 0.01  2.19 1.77 2.66  3.02 2.44 3.66  2.23  3.08  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00  1.87 7.29 12.71  1.50 5.82 10.16  16.99  13.58  Iron Output  Sample # Time (days) Sol'n Vol. (n 0.00 105.64 1 11.89 97.92 2 20.23 93.95 3 25.88 95.90 Filtrate 35.83 75.46 Wash 250.00  g Fe sampled Tot. Fe Sample Fe in sol'n (g) -1.31527E-05 -2.91527E-05 0.000210847  -0.00001 -0.00004 0.00017  0.019 0.018 0.023 0.0365 0.0009625  Arsenic Output  Sample # Time (days) Sol'n Vol. (nnL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.64 1 11.89 97.92 0.00032 0.00032 0.00626688 2 20.23 93.95 0.0002625 0.00058 0.004932375 3 25.88 95.90 0.000355 0.00094 0.0068089 Filtrate 35.83 75.46 0.01 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (rnL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 105.64 1 11.89 97.92 0.0000075 0.00001 0.00014688 2 20.23 93.95 0.00003 0.00004 0.0005637 3 25.88 95.90 0.00005 0.00009 0.000959 Filtrate 35.83 75.46 0.00 Wash 250.00 0.00  Extreme Thermophiles, 3.5 g Enargite, P of 10 microns 80  Test#B7-E10  Date  8-Jul 10-Jul 12-Jul 15-Jul 16-Jul 18-Jul 22-Jul 23-Jul 26-Jul 30-Jul 31-Jul 2-Aug 6-Aug 7-Aug 9-Aug 12-Aug 13-Aug  Enargite In (g):  Total Water (g):  Extreme Time (days)  Hour  12:00 0.00 12:30 2.02 14:10 4.09 12:40 7.03 12:20 ' 8.01 10.01 12:10 10:45 13.95 12:20 15.01 10:20 17.93 11:15 21.97 13:10 • 23.05 12:05 25.00 12:05 29.00 12:35 30.02 12:50 32.03 12:15 35.01 12:00 36.00  3.50 238.80  Vol (mL) Mass (g) Flask Weight (g): .fyrtS:."} 116.89 Innoculum in: 10 10 Medium in: 95.00 95.00 Total Final Weight (g): l i f t ; - . . V - l 219.03 96.37 Filtrate Volume (mL) 250 Wash Volume (mL) '«•>- ' .."-i 1.64 Solid Residue (g) 1  Thermophiles  Initial Mass (g)  PH  225.65 221.31 210.45 204.92 228.75 213.67 196.50 230.98 209.68 196.25 217.82 211.69 196.48 218.44 226.35 203.61 219.03  1.58 1.86 1.41 1.28 1.44 1.39 1.02 1.25 1.34 1.23 1.04 1.08 1.16 1.16 1.20 1.18 1.16  E„ (Ag/AgCI) E„ (mV)  479 384 409 429 437 492 454 476 470 508 509 609 620 624 642 644 637  Analysis Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 PLS (mg/L) Wash (mg/L) Solid Residue (wt %  :  699 604 629 649 657 712 674 696 690 728 729 829 840 844 862 864 857  Copper Iron 11.6 31.2 6542.25 2541.90 0 0.201 3535.90 8420.65 12845.15 12210.45 11147.15 199.58 0.6323 :  Sample (mL)  5 5  Medium Added Added (mL) Water (g)  4.66 16.90 31.25  225.97 227.35 236.17  12.39 42.08  226.06 238.58  17.07 29.71 8.38 15.64 30.02 7.64  226.75 225.96 226.20 227.33 226.50 226.08  23.06  226.67  5 5  5  5  5  5  Arsenic 10.5 160.5 0  Antimony 0.55 15.5 0  750.20 627.30 908.00 1292.00 1197.15 17.96 18  159.5 133.0 124.5 51.0 43.0 0.5 21  0.8  "*?-*,.."  Weight of Element  Copper  Iron  Arsenic  Antimony  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 Medium Added (g): #1 #2 #3 #4 PLS (g) Wash (g) Solid Residue (g)  1.092 0.0654 0  0.406 0.0254 0.0191  0.3675 0.0016 0  0.01925 0.0002 0  0.01768 0.042103 0.064226 0.061052  0.0038 0.0031 0.0045 0.0065  0.000798 0.000665 0.000623 0.000255  0 0 0 0  0 0 0 0 1.0743 0.049895 0.01037  0.001 0.001 0.001 0.001 0.1154 0.0045 0.2952  0 0 0 0 0.0041 0.000125 0.3444  0 0 0 0 0.0000 0 0.01312  1.193 -9.258  0.379 6.657  0.349 4.993  0.013 32.649  99.13 108.31  22.10 20.63  1.36 1.29  -1.20 -0.81  '•-  Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  Final Mass (g)  .  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.26 1 8.01 108.36 0.0176795 2 15.01 110.59 0.04210325 3 23.05 97.43 0.06422575 4 30.02 98.05 0.06105225 Filtrate 36.00 96.37 Wash 250.00  Tot. Cu Sampled (g) 0.01768 0.05978 0.12401 0.18506  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.383 0.931 1.252 1.197 1.074 0.050  0.318 0.883 1.246 1.256 1.133 1.183  29.10 80.91 114.09 115.00  26.63 74.05 104.42 105.26  108.31  99.13  Fe(aq) total  %Fe indicated  %Fe actual  0.06 0.04 0.06 0.10 0.09 0.09  13.76 10.83 15.53 24.94  14.74 11.60 16.64 26.72  23.26  24.92  As(aq) total  %As indicated  %As actual  0.02 0.01 0.01 0.01 0.00 0.00  4.27 3.78 3.26 1.49  4.49 3.98 3.43 1.57  1.29  1.36  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00 0.00  -0.81 -0.81 -0.81 -0.81  -1.20 -1.20 -1.20 -1.20  -0.81  -1.20  Iron Output  Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.00 105.26 1 8.01 108.36 0.002746597 0.00275 0.081291672 2 15.01 110.59 0.002132097 0.00488 0.069373107 3 23.05 97.43 0.003535597 0.00841 0.08846644 4 30.02 98.05 0.005455597 0.01387 0.1266806 Filtrate 36.00 96.37 0.1154 Wash 250.00 0.00449  Arsenic Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.26 1 8.01 108.36 0.0007975 0.00080 0.01728342 2 15.01 110.59 0.000665 0.00146 0.01470847 3 23.05 97.43 0.0006225 0.00209 0.012130035 4 30.02 98.05 0.000255 0.00234 0.00500055 Filtrate 36.00 96.37 0.00 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb 0.00 76.09 1 8.01 108.36 15.01 2 110.59 3 23.05 97.43 4 30.02 98.05 36.00 Filtrate 96.37 Wash 250.00  sampled Tot. Sb Sample Sb in sol'n (g) 0 0 0 0  0.00000 0.00000 0.00000 0.00000  0 0 0 0 0.00 0.00  Extreme Thermophiles, 3.5 g Enargite, P Test#B7-E15  Date 8-Jul 10-Jul 12-Jul 15-Jul 16-Jul 18-Jul 22-Jul 23-Jul 26-Jul 30-Jul  Hour 12:00 12:30 14:10 12:40 12:20 12:10 10:45 12:20 10:20 11:15  31-Jul 2-Aug 6-Aug 7-Aug 9-Aug 12-Aug 13-Aug  13:10 12:05 12:05 12:35 12:50 12:20 12:00  Enargite In (g): Total Water (g):  8 0  of 15 microns  Extreme Thermophiles Time (days)  Initial Mass (g) 224.35 209.54 209.03 208.33 217.61 209.68 194.59 217.28 209.12  PH 1.52 2.02 1.62 1.49 1.65 1.68 1.40 1.54 1.76  21.97  193.06  1.66  23.05  217.44 209.99 194.05 218.23 209.06 202.27 217.54  1.44 1.50 1.41 1.36 1.39 1.28 1.26  0.00 2,02 4.09 7,03 8.01 10.01 13,95 15.01 17.93  25.00 29.00 30.02 32.03 35.01 36.00  3.51 270.47  Vol(mL) Mass(g) Flask Weight (g): W? ' -."1 115.54 10 10 Innoculum in: 95.02 95.02 Medium in: Total Final Weight (g): j . - , . . . • ,- [ 217.54 96.95 ' Filtrate Volume (mL) Wash Volume (mL) 250 Solid Residue (g) v ' 'I 1.92  E„ (Ag/AgCI) Eh ( ) 516 736 384 604 381 601 383 603 400 620 402 622 400 620 397 617 400 620 454 674 m V  Sample (mL)  Medium Added Added (mL) Water (g)  5  5  5  5  443 459 473 487 500 506 524  663 679 693 707 720 726 744  5  5  5  5  Analysis Head (wt %)  Copper 30.4  Iron 10.6  Arsenic 10.5  Antimony 0.55  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 PLS (mg/L) Wash (mg/L)  6542.25 0  2541.90 0.2009  160.5 0  15.5 0  2323.45 3266.90 4913.90 7981.40 10583.40 155.05  375.45 507.65 739.85 503.75 384.15 3.77  47.0 76.0 211.5 98.5 138.5 1.8  8.6  18  17  0.9  Weight of Element  Copper  Iron  Arsenic  Antimony  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4  1.06704 0.0654 0  0.3721 0.0254 0.0191  0.36855 0.0016 0  0.019305 0.0002 0  0.011617 0.016335 0.02457 0.039907  0.0019 0.0025 0.0037 0.0025  0.000235 0.00038 0.001058 0.000493  0 0 0 0  Medium Added (g): #1 #2 #3 #4 PLS (g) Wash (g) Solid Residue (g)  0 0 0 0 1.0261 0.038763 0.16512  0.001 0.001 0.001 0.001 0.0372 0.0009 0.3456  0 0 0 0 0.0134 0.00045 0.3264  0 0 0 0 0.0000 0 0.01728  1.217 -14.058  0.344 7.439  86.43 98.58  -0.35 -0.33  Solid Residue (wt %  • •  Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  '  0.340 7.653 i. J'ft'-kllfci 4.10 3.78  .;.«*SfS 0.017 11.292  •' . ' >3S3» -0.91 -0.80  Final Mass (g)  15.46 22.17 16.65 7.40 15.79 31.37 13.91 15.92 32.38  225.00 231.20 224.98 225.01 225.47 225.96 231.19 225.04 225.44  7.80 14.76 31.77 6.50 15.92 22.67  225.24 224.75 225.82 224.73 224.98 224.94  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.30 1 8.01 98.56 0.01161725 2 15.01 98.23 0.0163345 3 23.05 98.39 0.0245695 4 30.02 99.18 0.039907 36.00 Filtrate 96.95 Wash 250.00  Tot. Cu Sampled (g) 0.01162 0.02795 0.05252 0.09243  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.229 0.321 0.483 0.792 1.026 0.039  0.164 0.267 0.446 0.779 1.013 1.052  15.33 25.03 41.80 72.98  13.44 21.95 36.65 63.98  98.58  86.43  Fe(aq) total  %Fe indicated  %Fe actual  0.01 0.02 0.05 0.02 0.01 0.01  3.11 6.57 12.73 6.60  3.36 7.10 13.76 7.13  3.43  3.71  As(aq)total  %As indicated  %As actual  0.00 0.01 0.02 0.01 0.01 0.01  0.82 1.65 5.38 2.67  0.89 1.79 5.82 2.89  3.78  4.10  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00 0.00  -0.80 -0.80 -0.80 -0.80  -0.91 -0.91 -0.91 -0.91  -0.80  -0.91  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.30 1 8.01 98.56 2 15.01 98.23 3 23.05 98.39 4 30.02 99.18 36.00 Filtrate 96.95 Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.000872847 0.001533847 0.002694847 0.001514347  0.00087 0.00241 0.00510 0.00662  0.037 0.050 0.073 0.050 0.0372 0.0009425  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.30 1 8.01 98.56 0.000235 0.00024 0.00463232 2 15.01 98.23 0.00038 0.00062 0.00746548 3 23.05 98.39 0.0010575 0.00167 0.020809485 4 30.02 99.18 0.0004925 0.00217 0.00976923 36.00 Filtrate 96.95 0.01 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb 0.00 75.00 1 8.01 98.56 2 15.01 98.23 3 23.05 98.39 4 30.02 99.18 36.00 Filtrate 96.95 Wash 250.00  sampled Tot. Sb Sample Sb in sol'n (g) 0 0 0 0  0.00000 0.00000 0.00000 0.00000  0 0 0 0 0.00 0.00  Extreme Thermophiles, 3.5 g Enargite, P Test #B7-E37  Date 8-Jul 10-Jul 12-Jul . 15-Jul 16-Jul 18-Jul 22-Jul 23-Jul 26-Jul 30-Jul 31-Jul 2-Aug 6-Aug 7-Aug 9-Aug 12-Aug 13-Aug  Enargite In (g): Total Water (g):  Extreme  Time (days) 0.00 2.02 4.09 7.03 8.01 10.01 13.95 15.01 17.93 21.97 23.05 25.00 28.92 30.02 32.03 35.01 36.00  Hour 12:00 12:30 14:10 12:40 12:20 12:10 10:45 12:20 10:20 11:15 13:10 12:05 10:05 12:35 12:50 12:15 12:00  3.51 341.58  Vol (mL) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g) Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  Mass (g) | 146.07 10 10 95.01 95.01 ' i ' 245 84 93 25 ' 248 5 "' "'•) 2.40  I  Initial Mass (g) 254.91 236.68 235.91 225.5 246.38 236.19 217.16 247.58' 228.49 216.43 245.31 234.41 216.05 247.05 236.41 226.69 245.84  PH 1.52 1.90 1.48 1.41 1.55 1.76 1.49 1.39 • 1.43 1.45 1.26 1.33 1.39 1.38 1.45 1.37 1.32  Analysis Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 PLS (mg/L) Wash (mg/L) Solid Residue (wt % t-'>"  8 0  of 37 microns  Thermophiles  - '  E„ (Ag/AgCI) E (mV) 508 728 388 608 390 610 404 624 406 626 395 615 '404 624 546 766 459 679 449 669 451 671 462 682 457 -677 467 687 480 700 478 698 495 715  Sample (mL)  Copper Iron 32.4 7.2 6542.25 2541.90 0 0.201  h  2367.90 5060.35 7092.55 7390.35 7791.70 113.53 18  323.55 174.50 72.55 69.50 70.80 0.75 11  St '.' " •„ •'3*?,!' •"-  18.84 20.57 31.40 8.90 19.15. 40.71 8.81 26.22 39.24 9.99 20.92 40.78 8.75 18.97 28.33  5  5  5  5  5  5  5  5  Arsenic 12 160.5 0  Antimony 0.39 15.5 0  95.5 364.5 205.0 238.0 273.5 4.0 15  0.5  >,!»,  :  Medium Final Added Added (mL) Water (g) Mass (g)  =  ..  V •'  Weight of Element  Copper  Iron  Arsenic  Antimony  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 Medium Added (g): #1 #2 #3 #4 PLS (g) Wash (g) Solid Residue (g)  1.13724 0.0654 0  0.2527 0.0254 0.0191  0.4212 0.0016 0  0.013689 0.0002 0  0.01184 0.025302 0.035463 0.036952  0.0016 0.0009 0.0004 0.0003  0.000478 0.001823 0.001025 0.00119  0 0 0 0  0 0 0 0 0.7266 0.028155 0.432  0.001 0.001 0.001 0.001 0.0066 0.0002 0.264  0 0 0 0 0.0255 0.000992 0.36  0 0 0 0 0.0000 0 0.012  *  Calculated Head (g) 1.194 % Difference -4.983 % Extraction VifcN*.- • Calculated Head 63.82 Measured Head 67.00 -  f  f  , .  i  0.226 10.524 %'}",, -•' .  -16.75 -14.99  0.388 7.831 •'fJ.'..;  7.27 6.70  . - . , •«  0.012 13.471 •  "' ^ . 1 * *  *'  -1.31 -1.13  ''1  255.52 256.48 256.90 255.28 255.34 257.87 256.39 254.71 255.67 255.30 255.33 256.83 255.80 255.38 255.02  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.33 1 8.01 96.80 0.0118395 2 15.01 98.00 0.02530175 3 23.05 95.73 0.03546275 4 30.02 97.47 0.03695175 Filtrate 36.00 93.25 Wash 248.00  Tot. Cu Sampled (g) 0.01184 0.03714 0.07260 0.10956  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.229 0.496 0.679 0.720 0.727 0.028  0.164 0.442 0.651 0.728 0.734 0.762  14.40 38.90 57.22 63.97  13.72 37.05 54.50 60.94  67.00  63.82  Fe(aq) total  %Fe indicated  %Fe actual  0.01 -0.01 -0.02 -0.02 -0.02 -0.02  2.33 -3.29 -7.31 -7.38  2.61 -3.68 -8.17 -8.25  -7.37  -8.24  As(aq)total  %As indicated  %As actual  0.01 0.03 0.02 0.02 0.03 0.03  1.81 8.21 4.82 5.92  1.97 8.91 5.23 6.42  6.70  7.27  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00 0.00  -1.13 -1.13 -1.13 -1.13  -1.31 -1.31 -1.31 -1.31  -1.13  -1.31  Iron Output  Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.00 105.33 1 8.01 96.80 0.000613347 0.00061 0.031 2 15.01 98.00 -0.000131903 0.00048 0.017 3 23.05 95.73 -0.000641653 -0.00016 0.007 4 30.02 97.47 -0.000656903 -0.00082 0.007 36.00 Filtrate 93.25 0.0066 Wash 248.00 0.000186  Arsenic  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.33 1 8.01 96.80 0.0004775 0.00048 0.0092444 2 15.01 98.00 0.0018225 0.00230 0.035721 3 23.05 95.73 0.001025 0.00333 0.01962465 4 30.02 97.47 0.00119 0.00452 0.02319786 36.00 93.25 Filtrate 0.03 Wash 248.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb 0.00 66.47 1 8.01 96.80 2 15.01 98.00 3 23.05 95.73 4 30.02 97.47 Filtrate 36.00 93.25 Wash 248.00  sampled Tot. Sb Sample Sb in sol'n (g) 0 0 0 0  0.00000 0.00000 0.00000 0.00000  0 0 0 0 0.00 0.00  Extreme Thermophiles, 5 g Enargite, P Test#B5-E10  Extreme  Date 11-Apr 15-Apr 18-Apr 19-Apr 23-Apr 24-Apr 26-Apr 29-Apr 30-Apr 3-May  Hour 15:45 11:10 11:25 11:15 10:30 20:15 11:40 10:45 11:45 11:15  7-May 10-May 14-May 16-May 17-May  11:00 11:00 11:25 10:35 11:25  Enargite In (g): Total Water (g):  21.81  Initial Mass (g) 225.90 216.27 212.47 221.30 192.68 213.14 210.24 196.51 221.40 199.89  PH 1.57 1.65 1.64 1.56 1.36 1.44 1.35 1.34 1.21 1.24  25.80 28.80 32.82 34.78 35.82  187.02 198.02 185.53 207.31 222.38  1.21 1.03 1.30 1.25 1.26  0.00 3.81 6,82 7.81 11.78 13.19 14.83 17.79 18.83  5.00 316.89  Vol (mL) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g) Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g)  Time (days)  ,  10 95.01  Mass (g) J 137.34  10 95.01 222.38  79.10 250  8 0  of 10 microns  Thermophiles  E (Ag/AgCI) E 413 633 379 599 410 630 398 618 400 620 401 621 403 623 407 627 400 620 408 628 h  Sample Medium Added Final (mL) Added (mL) Water (g) Mass (g)  5  5  5  5  5  5  5  5  407 407 428 421 413  627 627 648 641 633  Analysis Head (wt %)  Copper 31.2  Iron 11.6  Arsenic 10.5  Antimony 0.55  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 PLS (mg/L) Wash (mg/L) Solid Residue (wt °/  1645.85 0  854.90 0.201  80.5 0  7.5 0  3783.85 5338.95 5172.25 8581.20 6637.75 107.40 26  494.40 1199.60 1102.75 1640.30 1102.95 12.29 12  31.5 54.5 54.5 141.5 117.0 1.0 13  0.0 6.5 8.5 15.5 10.0 0.1 0.6  Weight of Element  Copper  Iron  Arsenic  Antimony  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g)  1.56 0.0165 0  0.58 0.0085 0.01909  0.525 0.0008 0  0.0275 0.0001 0  3.80  .'* . •  ;  .•  ..  0.018919 0.00247 0.000158 0.026695 0.006 0.000273 0.025861 0.00551 0.000273 0.042906 0.0082 0.000708  0 0.0000325 0.0000425 0.0000775  0 0 0 0.5250 0.02685 0.988  0 0 0 0.0008 0.000025 0.0228  i " ••-.5t*H*  Calculated Head (g % Difference % Extraction Calculated Head Measured Head .  1.595 -2.238 38.05 38.90  0.001 0.001 0.001 0.0872 0.00307 0.456  0 0 0 0.0093 0.00025 0.494 -' a Jl'*>«••. •' ' 0.530 0.503 8.681 4.114 13.91 12.70  1.87 1.79  0.024 14.124 3.46 2.97  22.71 16.97 4.95 35.78 14.08 18.04 35.06 6.27 26.33  238.98 229.44 226.25 228.46 227.22 228.28 231.57 227.67 226.22  40.19 28.48 41.81 26.22  227.21 226.50 227.34 233.53  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 83.56 78.96 1 7.81 0.01891925 2 13.19 70.80 0.02669475 3 18.83 57.55 0.02586125 4 28.80 57.55 0.042906 Filtrate 35.82 79.10 Wash 250.00  Tot. Cu Sampled (g) 0.01892 0.04561 0.07148 0.11438  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.299 0.378 0.298 0.494 0.525 0.027  0.282 0.380 0.327 0.549 0.580 0.607  18.10 24.39 20.95 35.18  17.70 23.85 20.49 34.41  38.90  38.05  Fe(aq)total  %Fe indicated  %Fe actual  0.03 0.08 0.05 0.06 0.08 0.08  5.26 13.17 9.47 11.16  5.76 14.42 10.37 12.22  14.10  15.44  As(aq)total  %As indicated  %As actual  0.00 0.00 0.00 0.01 0.01 0.01  0.32 0.61 0.53 1.53  0.33 0.64 0.55 1.60  1.79  1.87  Iron Output  Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.00 83.56 1 7.81 78.96 0.001467597 0.00147 0.039037824 2 13.19 70.80 0.004993597 0.00646 0.08493168 3 18.83 0.004509347 57.55 0.01097 0.063463263 4 28.80 44.68 -0.079041845 -0.06807 0.073288604 79.10 Filtrate 35.82 0.0872 Wash 250.00 0.0030725  Arsenic Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 83.56 1 7.81 78.96 0.0001575 0.00016 0.00248724 2 13.19 70.80 0.0002725 0.00043 0.0038586 3 18.83 57.55 0.0002725 0.00070 0.003136475 4 28.80 57.55 0.0007075 0.00141 0.008143325 Filtrate 35.82 79.10 0.01 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 83.56 1 7.81 78.96 0 0.00000 0 2 13.19 70.80 0.0000325 0.00003 0.0004602 3 18.83 57.55 0.0000425 0.00008 0.000489175 4 28.80 57.55 0.0000775 0.00015 0.000892025 35.82 79.10 Filtrate 0.00 Wash 250.00 0.00  Sb(aq) total 0.00 0.00 0.00 0.00 0.00 0.00  %Sb indicated %Sb actual -0.27 1.40 1.62 3.24  -0.32 1.63 1.89 3.78  2.97  3.46  Extreme Thermophiles, 5 g Enargite, P Test#B8-E15  Extreme  Date  Hour  16-Jul 18-Jul 22-Jul 23-Jul 26-Jul 30-Jul 31-Jul 2-Aug 6-Aug 7-Aug 9-Aug 12-Aug 13-Aug 16-Aug 20-Aug 21-Aug  13:30 11:55 10:35 12:20 10:20 11:15 13:05 12:00 12:00 12:30 12:45 12:10 12:10 13:50 13:15 13:05  Enargite In (g):  5.02  Total Water (g):  362.30  Time (days) 0.00 1.93 5.88 6.95 9.87 13.91 14.98 16.94 20.94 21.96 23.97 26.94 27.94 31.01 34.99 35.98  Vol (mL) Mass (g) Flask Weight (g): 145.93 Innoculum in: 10 10 Medium in: 95.12 95.12 256.25 Total Final Weight (g): 103.52 Filtrate Volume (mL) Wash Volume (mL) 250 Solid Residue (g) 3.70 S#x  Initial Mass (g)  pH  256.15 238.31 213.88 246.32 229.10 216.08 246.14 233.57 216.02 245.84 236.67 229.47 248.34 227.85 219.55 256.25  1.68 1.53 1.21 1.62 1.88 1.87 1.66 1.77 1.69 1.67 1.76 1.62 1.53 1.50 1.42 1.43  of 15 microns  E„ (Ag/AgCI) E„ (mV)  Analysis  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 PLS (mg/L) Wash (mg/L) Solid Residue (wt % ••  8 0  Thermophiles  ...  467 427 458 434 392 396 397 387 390 385 404 427 429 443 461 470  687 647 678 654 612 616 617 607 610 605 624 647 649 663 681 690  Copper 30.4 3000.55 0 2177.25 3701.45 4282.50 4721.20 6593.05 91.88 25  Sample (mL)  Medium Added Final Added (mL) Water (g) Mass (g)  18.62 43.07 10.76 28.32 41.06 10.88 23.61 40.83 10.94 21.62 28.19 8.75 29.24 46.41  5  5  5  5  5  5  5  5  Iron 10.6 1469.30 0.2009  Arsenic 10.5 81.0 0  Antimony 0.55  311.65 517.40 693.00 806.55 665.15 5.35 12  40.0 77.5 24.0 41.0 93.0 0.8 13  .'.v.-.-ffVi..-.vi,.',.•.:...;>.-.  0  0.6 •-.  Weight of Element  Copper  Iron  Arsenic  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 Medium Added (g): #1 #2 #3 #4 PLS (g) Wash (g) Solid Residue (g)  1.52608 0.0300 0  0.5321 0.0147 0.0191  0.5271 0.0008 0  0.02761 0.0000 0  0.010886 0.018507 0.021413 0.023606  0.0016 0.0026 0.0035 0.004  0.0002 0.000388 0.00012 0.000205  0 0 0 0  0 0 0 0 0.6825 0.02297 0.925  0.001 0.001 0.001 0.001 0.0689 0.0013 0.444  0 0 0 0 0.0096 0.0002 0.481  0 0 0 0 0.0000 0 0.0222  1.651 -8.204  0.485 8.857  0.491 6.901  0.022 19.594  43.98 47.59  8.45 7.70  1.98 1.84  0.00 0.00  Calculated Head (g) % Difference % Extraction  Calculated Head Measured Head  ••*-.''.'.••'"••  Antimony  "  i  256.93 256.95 257.08 257.42 257.14 257.02 257.18 256.85 256.78 258.29 257.66 257.09 257.09 265.96  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 105.20 1 9.87 78.15 0.01088625 2 14.98 95.19 0.01850725 3 21.96 94.89 0.0214125 4 27.94 97.39 0.023606 Filtrate 35.98 103.52 Wash 250.00  Tot. Cu Sampled (g) 0.01089 0.02939 0.05081 0.07441  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.170 0.352 0.406 0.460 0.683 0.023  0.140 0.333 0.406 0.481 0.703 0.726  9.18 21.84 26.59 31.49  8.49 20.18 24.57 29.10  47.59  43.98  Fe(aq) total  %Fe indicated  %Fe actual  0.01 0.03 0.04 0.06 0.05 0.06  1.82 6.49 8.40 12.00  1.99 7.13 9.22 13.17  10.43  11.44  As(aq) total  %As indicated  %As actual  0.00 0.01 0.00 0.00 0.01 0.01  0.44 1.28 0.35 0.74  0.47 1.38 0.37 0.79  1.84  1.98  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00 0.00  0.00 0.00 0.00 0.00  0.00 0.00 0.00 0.00  0.00  0.00  Iron Output  Sample # Time (days) Sol'n Vol. (mL) 0.00 105.20 1 9.87 78.15 2 14.98 95.19 3 21.96 85.72 4 27.94 97.39 Filtrate 35.98 103.52 Wash 250.00  Arsenic  g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.000553847 0.001582597 0.002460597 0.003028347  0.00055 0.00214 0.00460 0.00763  0.024 0.049 0.059 0.079 0.0689 0.0013375  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 105.20 1 9.87 78.15 0.0002 0.00020 0.003126 2 14.98 95.19 0.0003875 0.00059 0.007377225 3 21.96 85.72 0.00012 0.00071 0.00205728 4 27.94 97.39 0.000205 0.00091 0.00399299 Filtrate 35.98 103.52 0.01 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb 0.00 105.20 1 9.87 78.15 2 14.98 95.19 3 21.96 85.72 4 27.94 97.39 35.98 Filtrate 103.52 Wash 250.00  sampled Tot. Sb Sample Sb in sol'n (g) 0 0 0 0  0.00000 0.00000 0.00000 0.00000  0 0 0 0 0.00 0.00  Extreme Thermophiles, 5 g Enargite, P Test UB5-E37  Extreme  8 0  of 37 microns  Thermophiles  Time  Initial  Date  Hour  (days)  M a s s (g)  pH  (Ag/AgCI)  Eh ( m V )  11-Apr 15-Apr 18-Apr 19-Apr 23-Apr 24-Apr 26-Apr 29-Apr 30-Apr 3-May  15:45 11:10 11:25 11:15 10:30 20:15 11:40 10:45 11:50 11:15  0.00 3.81 6.82 7.81 11.78 13.19 14.83 17.79 18.84 21.81  247.49 200.63 229.05 251.41 222.18 241.74 236.73 215.67 223.83 236.56  1.59 1.72 1.82 1.77 1.62 1.55 1.59 1.48 1.31 1.42  392 378 385 396 417 417 474 438 435 434  612 598 605 616 637 637 694 658 655 654  7-May 10-May 14-May 16-May 17-May  11:00 11:00 11:25 10:35 11:25  25.80 217.95 28.80 225.92 32.82 221.28 34.78 i 23o:oa,| 35.82 242.06  1.34 1.25 1.40 1.39 1.34  441 451 490 570 590  661 671 710 790 810  Copper 32.4  E n a r g i t e In (g):  Total Water (g):  4.99 305.90  Vol (mL) Mass (g) Flask Weight (g): 115.57 Innoculum in: 10 10 Medium in: 95.24 95.24 Total Final Weight (g): 242.06 Filtrate Volume (mL) 115.63 ;.: ,/?,> Wash Volume (mL) 250 i' tit!?'.' Solid Residue (g) 3.44 iiv-*-*.:, I  E„  Analysis  Head (wt %)  Sample (mL)  Medium  5  5  5  5  5  5  5  5  Iron 7.2  Arsenic 12  Antimony 0.39  Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 PLS (mg/L) Wash (mg/L) Solid Residue (wt "/  1645.85 0  854.90 0.201  80.5 0  7.5 0  2311.65 3134.30 4758.20 5129.90 6617.90 120.35 23  359.90 611.90 858.15 817.60 734.20 8.01 13  83.0 160.0 141.0 129.5 252.5 3.2 14  5.5 8.5 12.0 0.4 0.6  Weight of Element  Copper  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 Medium Added (g): #1 #2 #3 PLS (g) Wash (g) Solid Residue (g)  1.61676 0.35928 0.0165 0.0085 0 0.01913  Calculated Head (g % Difference  ,.-v*, i •'vC'':.'-'-  0.011558 0.015672 0.023791 0.02565  '  Iron  -  *  Arsenic  Antimony  0.5988 0.0008 0  0.019461 0.0001 0  0.0018 0.000415 0.00306 0.0008 0.00429 0.000705 0.00409 0.000648  0 0.001 0 0.001 0 0.001 0.7652 0.0849 0.030088 0.002 0.7912 0.4472  0 0 0.0000275 0.0000425  0 0 0 0.0292 0.0008 0.4816  0 0 0 0.0014 0.0001 0.02064  1.621 -0.267  0.513 -42.661  0.513 14.377  0.022 -13.458  51.19 51.33  12.75 18.19  6.07 5.20  6.52 7.40  % Extraction  Calculated Head Measured Head  Added  A d d e d ( m L ) W a t e r (g)  Final M a s s (g)  49.46 29.26  250.09 258.31  29.70 6.14 16.83 32.00 32.28 11.35  251.88 247.88 253.56 247.67 256.11 247.91  29.87 21.74 27.63 19.64  247.82 247.66 248.91 249.64  Copper Output  Sample # Time (days) Sol'n Vol. (mL) g Cu sampled 0.00 126.93 7.81 1 130.85 0.01155825 2 13.19 121.18 0.0156715 3 18.84 116.00 0.023791 4 28.80 116.00 0.0256495 Filtrate 35.82 115.63 Wash 250.00  Tot. Cu Sampled (g) 0.01156 0.02723 0.05102 0.07667  Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.302 0.380 0.552 0.595 0.765 0.030  0.286 0.375 0.563 0.630 0.800 0.830  17.69 23.19 34.81 38.94  17.64 23.13 34.71 38.84  51.33  51.19  Fe(aq) total  %Fe indicated  %Fe actual  0.04 0.07 0.09 0.07 0.08 0.08  10.73 18.26 25.33 19.78  7.52 12.80 17.75 13.87  21.81  15.29  As(aq)total  %As indicated  %As actual  0.01 0.02 0.02 0.02 0.03 0.03  1.68 3.17 2.80 2.69  1.96 3.71 3.27 3.15  5.20  6.07  Sb(aq) total  %Sb indicated  %Sb actual  0.00 0.00 0.00 0.00 0.00 0.00  -0.39 -0.39 2.89 4.82  -0.34 -0.34 2.55 4.25  7.40  6.52  Iron Output  Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) 0.00 126.93 7.81 1 130.85 0.000795097 0.00080 0.047 2 13.19 121.18 0.002055097 0.00285 0.074 3 18.84 116.00 0.003286347 0.00614 0.100 4 28.80 97.39 -0.080807546 -0.07467 0.080 Filtrate 35.82 115.63 0.0849 Wash 250.00 0.0020025  Arsenic  Output  Sample # Time (days) Sol'n Vol. (mL) g As sampled Tot. As Sample As in sol'n (g) 0.00 126.93 1 7.81 130.85 0.000415 0.00042 0.01086055 2 13.19 121.18 0.0008 0.00122 0.0193888 3 18.84 116.00 0.000705 0.00192 0.016356 4 28.80 116.00 0.0006475 0.00257 0.015022 35.82 115.63 Filtrate 0.03 Wash 250.00 0.00  Antimony Output  Sample # Time (days) Sol'n Vol. (mL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) 0.0000 126.93 1 7.81 130.85 0 0.00000 0 2 13.19 121.18 0 0.00000 0 3 18.84 116.00 0.0000275 0.00003 0.000638 4 28.80 116.00 0.0000425 0.00007 0.000986 Filtrate 35.82 115.63 0.00 Wash 250.00 0.00  Extreme Thermophiles, 10 g Enargite, P Test UB2-E10  Date  Hour  20-Dec 23-Dec 28-Dec 31-Dec 3-Jan 8-Jan 11-Jan 15-Jan 18-Jan 22-Jan 25-Jan  9:40 9:50 10:00 13:10 16:10 10:20 10:25 11:40 9:40 11:45 10:50  Enargite In (g):  8 0  of 10 microns  Extreme Thermophiles  Time Initial (days) Mass (g) 0.00 250.96 219.03 3.01 8.01 198.10 11.15 14.27 19.03 22.03 26.08 29.00 33.09 36.05  10.00  Total Water (g):  Vol(mL) Mass(g) Flask Weight (g): ':. • /I 135.56 Innoculum in: 10 10 Medium in: 95.00 95.00 219.95 Total Final Weight (g): Filtrate Volume (mL) 72.51 Wash Volume (mL) 250 Solid Residue (g) ''•'I/'A 7.66  E„ Sample Medium Added Final (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g)  pH 1.53 1.60 1.30 1.23 1.19 1.12 1.17 1.16 1.16  221.75 221.96 206.52 223.56 212.89 224.82 212.33 219.95  477 387 420 402 398 412 404 411 408 408 407  1.04  Copper  Analysis  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 #5 #6 #7 #8 #9 PLS (mg/L) Wash (mg/L) Solid Residue (wt %)  •mK*:  - '•'  Weight of Element  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 #5 #6 #7 #8 #9 Medium Added (g): #1 #2 #3  #4 #5 #6 #7 #8 #9  « V j r > .  \>";  Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  5 5 5 5 5 5 5 5 5  Iron  Arsenic  5 5 5 5 5 5 5 5 5  32.16 53.17 29.54 29.14 45.08 27.48 39.22 26.95 39.04  Antimony  31.2 3895.65 0  . 116 2833.85 0.201  10.5 170.5 0  0.55 14.5 0  5291.85 11577.40 7823.70 8611.80 11453.15 9113.60 11355.45 9936.25 12762.45 9844.75 165.88 25.6  1284.60 2020.85 1566.65 1830.45 2941.35 2134.00 2750.85 2618.80 3231.15 2396.55 35.66 11.6  456.0 110.0 59.0 80.5 122.0 114.0 165.5 148.5 200.0 175.5 1.4 13.8  0.0 10.5 8.0 12.5 17.5 18.0 22.5 20.5 24.0 13 0.2 0.62  Copper  Iron  Antimony  Arsenic  3.12 0.0390 0  1.16 0.0283 0.01908  1.05 0.0017 0  0.055 0.0001 0  0.0264593 0.057887 0.0391185 0.043059 0.0572658 0.045568 0.0567773 0.0496813 0.0638123  0.00642 0.0101 0.00783 0.00915 0.01471 0.01067 0.01375 0.01309 0.01616  0.00228 0.00055 0.0003 0.0004 0.00061 0.00057 0.00083 0.00074 0.001  0 0.0000525 0.00004 0.0000625 0.0000875 0.00009 0.0001125 0.0001025 0.00012  0 0 0  0.001 0.001 0.001  0 0 0  0 0 0  0 0 0 0 0 0 0.7138 0.04147 1.96096  PLS (g) Wash (g) Solid Residue (g)  697 607 640 622 618 632 624 631 628 628 627  -.7 . .  0 0.001 0.001 0 0.001 0 0.001 0 0.001 0 0 0.001 0.1738 0.0127 0.00892 0.00035 0.88856 1.05708  «  0 0 0 0 0 0 0.0009 0.00005 0.047492  ' . ' M . „*IS  *  3.117 0.098  1.117 3.734  37.09 37.05  20.43 19.67  • .  1.076 -2.450  •:'  0.049 10.896 ,  1.73 1.78  '*  - ' • J*  3.09 2.75  251.19 251.27 251.29 251.10 251.60 251.04 252.11 251.77 251.37  Copper  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Output  Time (days) 0.00 3.01 8.01 11.15 14.27 19.03 22.03 26.08 29.00 33.09 36.05  Sol'n Vol. (mL) 105.40 73.47 52.54 76.19 76.40 60.96 78.00 67.33 79.26 66.77 72.51 250.00  Total Cu g Cu sampled Removed (g) 0.02646 0.05789 0.03912 0.04306 0.05727 0.04557 0.05678 0.04968 0.06381  0.02646 0.08435 0.12346 0.16652 0.22379 0.26936 0.32613 0.37582 0.43963  0.389 0.608 0.596 0.658 0.698 0.711 0.765 0.788 0.852 0.714 0.041  0.350 0.596 0.641 0.742 0.826 0.896 0.995 1.075 1.189 1.115 1.156  11.21 19.10 20.56 23.80 26.47 28.71 31.89 34.45 38.11 35.72 37.05  11.22 19.11 20.58 23.82 26.49 28.74 31.92 34.48 38.15 35.76 37.09  Sol'n Vol. (mL) 105.40 73.47 52.54 76.19 76.40 60.96 78.00 67.33 79.26 66.77 72.51 250.00  g Fe sampled  Total Fe Removed (g)  Fe in sol'n (g)  Fe (aq) total  %Fe indicated  %Fe actual  0.00542 0.0091 0.00683 0.00815 0.0137 0.00967 0.01275 0.01209 0.01515  0.00542 0.01452 0.02135 0.02950 0.04320 0.05286 0.06561 0.07770 0.09285  0.09438 0.106175 0.119363 0.139846 0.179305 0.166452 0.185215 0.207566 0.215744 0.1738 0.008915  0.07 0.08 0.09 0.11 0.15 0.14 0.16 0.18 0.19 0.15 0.15  5.69 6.71 7.85 9.61 13.01 11.91 13.52 15.45 16.16 12.54 13.31  5.91 6.97 8.15 9.99 13.52 12.37 14.05 16.05 16.78 13.02 13.82  Sol'n Vol. (mL) 105.40 73.47 52.54 76.19 76.40 60.96 78.00 67.33 79.26 66.77 72.51 250.00  g As Total As sampled Removed (g)  As in sol'n (g)  As (aq) total  %As indicated  %As actual  0.00228 0.00055 0.0003 0.0004 0.00061 0.00057 0.00083 0.00074 0.001  0.00228 0.00283 0.00313 0.00353 0.00414 0.00471 0.00554 0.00628 0.00728  0.033502 0.005779 0.004495 0.00615 0.007437 0.008892 0.011143 0.01177 0.013354 0.01 0.00  0.03 0.01 0.01 0.01 0.01 0.01 0.01 0.02 0.02 0.02 0.02  3.03 0.61 0.54 0.72 0.88 1.08 1.35 1.49 1.71 1.74 1.78  2.96 0.59 0.52 0.70 0.86 1.05 1.31 1.45 1.67 1.70 1.73  gSb sampled  Total Sb Removed (g)  Sb in sol'n (g)  Sb (aq) total  %Sb indicated  %Sb actual  0 5.3E-05 0.00004 6.3E-05 8.8E-05 0.00009 0.00011 0.0001 0.00012  0.00000 0.00005 0.00009 0.00016 0.00024 0.00033 0.00045 0.00055 0.00067  0 0.000552 0.00061 0.000955 0.001067 0.001404 0.001515 0.001625 0.001602 0.00 0.00  0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00  -0.26 0.74 0.94 1.64 1.96 2.73 3.10 3.50 3.65 2.66 2.75  -0.30 0.83 1.05 1.84 2.20 3.06 3.47 3.93 4.09 2.99 3.09  Cu in sol'n (g)  Cu (aq) %Cu total (g) Indicated  %Cu actual  Iron Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Arsenic  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.01 8.01 11.15 14.27 19.03 22.03 26.08 29.00 33.09 36.05  Output  Time (days) 0.00 3.01 8.01 11.15 14.27 19.03 22.03 26.08 29.00 33.09 36.05  Antimony Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time Sol'n Vol. (mL) (days) 0.0000 105.40 3.0069 73.47 8.0139 52.54 11.1458 76.19 14.2708 76.40 19.0278 60.96 22.0313 78.00 26.0833 67.33 29.0000 79.26 33.0868 66.77 36.0486 72.51 250.00  Extreme Thermophiles, 10 g Enargite, P Test#B2-E15  Extreme  Date  Hour  Time (days)  Initial Mass (g)  20-Dec 23-Dec 28-Dec 31-Dec 3-Jan 8-Jan 11-Jan 15-Jan 18-Jan 22-Jan 25-Jan  9:40 9:50 10:05 13:10 16:10 10:20 10:25 10:40 9:40 11:45 10:15  0.00 3.01 8.02 11.15 14.27 19.03 22.03 26.04 29.00 33.09 36.02  233.71 209.43 197.78 210.46 208.70 189.17 212.33 210.25 212.79 203.37 213.67  Enargite In (g):  10.01  Total Water (g):  266.49  Vol (mL) Mass (g) Flask Weight (g): i - , - J 118.36 Innoculum in: 10 10 95.00 95.00 Medium in: Total Final Weight (g): T-r;r-7r~] 213.67 83.77 Filtrate Volume (mL) 250 • ' • ,• Wash Volume (mL) 7.89 Solid Residue (g)  8 0  of 15 microns  Thermophiles E (Ag/AgCI) E„ (mV) h  pH  1.52 1.79 1.60 1.61 1.49 1.30 1.40 1.48 1.39 1.30  471 373 416 391 391 380 369 . 394 395 401 399  691 593 636 611 611 600 589 614 615 621 619  Copper  Analysis  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 #5 #6 #7 #8 #9 Medium Added (g): #1 #2 #3 #4 #5 #6 #7 #8 #9 PLS (g) Wash (g) ' Solid Residue (g) Calculated Head (g) % Difference  5 5 5 5 5 5 5 5 5  Iron  Head (wt %) 30.4 Innoculum (mg/L) 3895.65 Medium (g/L) 0 Samples (mg/L): #1 2709.00 #2 3934.40 #3 4090.85 #4 5106.25 #5 8919.70 #6 6411.50 #7 7339.90 #8 7780.10 #9 9299.25 PLS (mg/L) 7063.95 Wash (mg/L) 138.52 Solid Residue (wt %) 28 :'.:..*.i".v ' - , .. .... Weight of Element Copper  Antimony  10.6 2833.85 0.20088  10.5 170.5 0  0.55 14.5 0  655.25 1111.70 802.70 1165.05 1763.65 1132.85 1279.40 1451.05 1743.20 1342.8 20.76 11.4  55.0 285.0 26.0 69.0 46.5 315.0 42.5 48.5 69.5 68.5 0.8 12.8  2.0 0.5 0.0 6.0 6.5 6.0 8.0 11.0 13.5 8.5 0.2 0.65 ;--v.;. Antimony  Arsenic  1.06106 1.05105 0.0283 0.0017 0.01908 0  0.055055 0.0001 0  0.013545 0.019672 0.0204543 0.0255313 0.0445985 0.0320575 0.0366995 0.0389005 0.0464963  0.00328 0.00556 0.00401 0.00583 0.00882 0.00566 0.0064 0.00726 0.00872  0.00028 0.00143 0.00013 0.00035 0.00023 0.00158 0.00021 0.00024 0.00035  0.00001 0.0000025 0 0.00003 0.0000325 0.00003 0.00004 0.000055 0.0000675  0 0 0  0.001 0.001 0.001  0 0 0  0 0 0  0 0 0 0 0 0 0.5917 0.03463 2.2092 -* '•" - •  3.075 -1.036  0.001 0 0.001 0 0.001 0 0.001 0 0.001 0 0.001 0 0.1125 0.0057 0.00519 0.0002 0.89946 1.00992 .  28.15 28.44  0 0 0 0 0 0 0.0007 0.00005 0.051285 :'i<viis .„,:.  •  k  1.016 4.228  1.019 3.055  11.49 11.00  0.89 0.86  % Extraction  Calculated Head Measured Head  5 5 5 5 5 5 5 5 5  Arsenic  Iron  3.04304 0.0390 0  Sample Medium Added (mL) Added (mL) Water (g)  0.052 5.241 ' . . e^lSsi'; 1.70 1.61  24.37 36.04 24.26 25.16 45.98 30.97 23.27 25.88 30.56  Final Mass (g)  233.80 233.82 234.72 233.86 235.15 243.30 233.52 238.67 233.93  Copper Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Sol'n Vol. (mL) 105.34 81.06 69.41 82.09 80.33 60.80 83.96 81.88 84.42 75.00 83.77 250.00  g Cu Total Cu sampled Removed (g)  Sol'n Vol. (mL) 105.34 81.06 69.41 82.09 80.33 60.80 83.96 81.88 84.42 75.00 83.77 250.00  Sol'n Vol. (mL) 105.34 81.06 69.41 82.09 80.33 60.80 83.96 81.88 84.42 75.00 83.77 250.00  Time Sol'n Vol. (days) (mL) 0.0000 105.34 3.0069 81.06 8.0174 69.41 11.1458 82.09 14.2708 80.33 19.0278 60.80 22.0313 83.96 26.0417 81.88 29.0000 84.42 33.0868 75.00 36.0243 83.77 250.00  Time (days) 0.00 3.01 8.02 11.15 14.27 19.03 22.03 26.04 29.00 33.09 36.02  0.01355 0.01967 0.02045 0.02553 0.0446 0.03206 0.0367 0.0389 0.0465  0.01355 0.03322 0.05367 0.07920 0.12380 0.15586 0.19256 0.23146 0.27795  Cu in sol'n (g)  Cu (aq) %Cu total (g) indicated  %Cu actual  0.220 0.273 0.336 0.410 0.542 0.538 0.601 0.657 0.697 0.592 0.035  0.181 0.248 0.330 0.425 0.583 0.623 0.718 0.810 0.890 0.831 0.865  5.94 8.14 10.85 13.96 19.14 20.48 23.59 26.63 29.25 27.30 28.44  5.88 8.06 10.74 13.82 18.95 20.27 23.35 26.36 28.95 27.02 28.15  g Fe Total Fe sampled Removed (g)  Fe in sol'n (g)  Fe (aq) total  %Fe indicated  %Fe actual  0.00227 0.00455 0.00301 0.00482 0.00781 0.00466 0.00539 0.00625 0.00771  0.053 0.077 0.066 0.094 0.107 0.095 0.105 0.122 0.131 0.1125 0.00519  0.02 0.05 0.04 0.07 0.08 0.07 0.08 0.09 0.10 0.08 0.09  2.34 4.60 3.54 6.15 7.44 6.29 7.20 8.87 9.65 7.93 8.42  2.44 4.80 3.70 6.42 7.76 6.57 7.52 9.27 10.08 8.28 8.79  Total As g As sampled Removed (g)  As in sol'n (g)  As (aq) total  %As indicated  % As actual  0.00028 0.00143 0.00013 0.00035 0.00023 0.00158 0.00021 0.00024 0.00035  0.004458 0.019782 0.002134 0.005543 0.002827 0.026447 0.00348 0.004094 0.005213 0.01 0.00  0.00 0.02 0.00 0.01 0.00 0.03 0.01 0.01 0.01 0.01 0.01  0.26 1.75 0.20 0.54 0.31 2.58 0.55 0.63 0.76 0.84 0.86  0.27 1.80 0.21 0.56 0.32 2.66 0.57 0.65 0.78 0.87 0.89  gSb Total Sb sampled Removed (g)  Sbin sol'n (g)  Sb (aq) total  %Sb indicated  %Sb actual  0.00001 2.5E-06 0 0.00003 3.3E-05 0.00003 0.00004 5.5E-05 6.8E-05  0.000162 3.47E-05 0 0.000482 0.000395 0.000504 0.000655 0.000929 0.001013 0.00 0.00  0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00  Iron Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.01 8.02 11.15 14.27 19.03 22.03 26.04 29.00 33.09 36.02  0.00227 0.00683 0.00984 0.01466 0.02247 0.02713 0.03252 0.03877 0.04648  Arsenic Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.01 8.02 11.15 14.27 19.03 22.03 26.04 29.00 33.09 36.02  0.00028 0.00170 0.00183 0.00218 0.00241 0.00398 0.00420 0.00444 0.00479  Antimony Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  0.00001 0.00001 . 0.00001 0.00004 0.00008 0.00011 0.00015 0.00020 0.00027  0.03 -0.18 -0.24 0.63 0.53 0.79 1.12 1.69 1.94 • 1.52 1.61  0.03 -0.19 -0.25 0.67 0.56 0.83 1.18 1.78 2.05 1.60 1.70  222  Extreme Thermophiles, 10 g Enargite, P Test UB2-E37  Date 20-Dec 23-Dec 28-Dec 31-Dec 3-Jan 8-Jan 11-Jan 15-Jan 18-Jan 22-Jan 25-Jan  Enargite In (g):  Extreme  Hour 9:40 9:50 10:00 13:10 16:10 10:20 10:25 11:40 9:40 11:45 10:15  Initial Time (days) Mass (g) 0.00 245.95 3.01 216.27 8.01 199.61 11.15 218.18 14.27 216.51 19.03 202.98 22.03 218.37 26.08 208.32 29.00 218.54 33.09 209.09 36.02 219.38  Total Water (g):  Vol (mL) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) |Wash Volume (mL) Solid Residue (g)  10 95.01  PH 1.56 1.52 1.37 1.36 1.35 1.20 1.26 1.28 1.26 1.15  Mass (g) 130.72 10 95.01 219.38  of 37 microns  E„ Medium Sample Added Final (mL) Added (mL) Water (g) Mass (g) (Ag/AgCI) E„ (mV) 453 673 385 605 5 5 29.96 246.23 420 640 5 5 46.64 246.25 408 628 5 5 27.82 246.00 412 632 5 5 29.77 246.28 411 631 5 5 43.20 246.18 415 635 5 5 28.33 246.70 439 659 5 5 37.51 245.83 443 663 5 5 29.26 247.80 443 663 5 5 36.82 245.91 447 667  Copper  Analysis  10.01  8 0  Thermophiles  Head (wt %) Innoculum (mg/L) Medium (g/L) Samples (mg/L): #1 #2 #3 #4 #5 #6 #7 #8 #9 PLS (mg/L) Wash (mg/L) Solid Residue (wt %) Weight of Element  Head (g) Innoculum (g) Medium (g) Samples (g): #1 #2 #3 #4 #5 #6 #7 #8 #9 Medium Added (g): #1 #2 #3  #4 #5 #6 #7 #8 #9 PLS (g) Wash (g) Solid Residue (g)  Iron  Antimony  32.4 3895.65 0  7.2 2833.85 0.201  12 170.5 0  0.39 14.5 0  3275.80 6646.85 5128.70 5488.95 7923.80 6216.20 8635.90 8917.05 10576.80 8219.8 156.79 26.8  815.20 819.10 459.30 465.45 643.60 422.00 405.40 310.05 270.95 183.6 3.00 8.6  372.0 286.5 68.5 87.0 137.0 142.5 252.5 297.0 395.5 350.5 5.4 13.4  1.5 1.5 3.0 4.5 8.0 7.5 10.0 9.5 9.5 5 0.1 0.44  Arsenic  Antimony  Copper  Iron  3.24324 0.0390 0  0.72072 0.0283 0.01909  1.2012 0.0017 0  0.039039 0.0001 0  0.016379 0.0332343 0.0256435 0.0274448 0.039619 0.031081 0.0431795 0.0445853 0.052884  0.00408 0.0041 0.0023 0.00233 0.00322 0.00211 0.00203 0.00155 0.00135  0.00186 0.00143 0.00034 0.00044 0.00069 0.00071 0.00126 0.00149 0.00198  0.0000075 0.0000075 0.000015 0.0000225 0.00004 0.0000375 0.00005 0.0000475 0.0000475  0 0 0  0.001 0.001 0.001  0 0 0  0 0 0  0 0 0 0 0 0 0.0265 0.0013 1.139  0 0 0 0 0 0 0.0004 0.000024 0.0374  0 0.001 0 0.001 0 0.001 0 0.001 0 0.001 0 0.001 0.6221 0.0139 0.0376296 0.00072 2.278 0.731 i  Calculated Head (g) % Difference % Extraction Calculated Head Measured Head  Arsenic  . I I , . ,  ;  3.213 0.939  0.712 1.181  1.175 2.155  0.038 2.835  29.10 28.82  -2.64 -2.61  3.09 3.02  1.40 1.36  223  Copper Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.01 8.01 11.15 14.27 19.03 22.03 26.08 29.00 33.09 36.02  Sol'n Vol. (mL) 105.22 75.54 58.88 77.45 75.78 62.25 77.64 67.59 77.81 68.36 75.68 240.00  Total Cu g Cu sampled Removed (g)  Sol'n Vol. (mL) 105.22 75.54 58.88 77.45 75.78 62.25 77.64 67.59 77.81 68.36 75.68 240.00  Sol'n Vol. (mL) 105.22 75.54 58.88 77.45 75.78 62.25 77.64 67.59 77.81 68.36 75.68 240.00  Time Sol'n Vol. (days) (mL) 0.0000 105.22 3.0069 75.54 8.0139 58.88 11.1458 77.45 14.2708 75.78 19.0278 62.25 22.0313 77.64 26.0833 67.59 29.0000 77.81 68.36 33.0868 36.0243 75.68 240.00  0.01638 0.03323 0.02564 0.02744 0.03962 0.03108 0.04318 0.04459 0.05288  0.01638 0.04961 0.07526 0.10270 0.14232 0.17340 0.21658 0.26117 0.31405  Cu in sol'n (g)  Cu (aq) %Cu total(g) indicated  %Cu actual  0.247 0.391 0.397 0.416 0.493 0.483 0.584 0.694 0.723 0.622 0.038  0.208 0.369 0.408 0.452 0.557 0.586 0.718 0.871 0.945 0.897 0.935  6.43 11.37 12.58 13.94 17.17 18.07 22.14 26.87 29.14 27.66 28.82  6.49 11.48 12.70 14.08 17.34 18.24 22.35 27.12 29.42 27.92 29.10  Total Fe g Fe sampled Removed (g)  Fe in sol'n (g)  Fe (aq) total  %Fe indicated  %Fe actual  0.00307 0.00309 0.00129 0.00132 0.00221 0.00111 0.00102 0.00055 0.00035  0.062 0.048 0.036 0.035 0.040 0.033 0.027 0.024 0.019 0.0139 0.00072  0.03 0.02 0.01 0.01 0.01 0.00 0.00 0.00 -0.01 -0.01 -0.01  4.61 2.76 1.00 0.96 1.63 0.61 -0.13 -0.58 -1.36 -2.00 -1.90  4.67 2.79 1.02 0.97 1.65 0.62 -0.13 -0.59 -1.38 -2.03 -1.93  g As Total As sampled Removed (g)  As in sol'n (g)  As (aq) total  %As indicated  %As actual  0.00186 0.00143 0.00034 0.00044 0.00069 0.00071 0.00126 0.00149 0.00198  0.028101 0.016869 0.005305 0.006593 0.008528 0.011064 0.017066 0.02311 0.027036 0.03 0.00  0.03 0.02 0.01 0.01 0.01 0.01 0.02 0.03 0.03 0.04 0.04  2.20 1.42 0.57 0.71 0.91 1.17 1.73 2.34 2.79 2.91 3.02  2.25 1.45 0.59 0.73 0.93 1.20 1.77 2.39 2.85 2.98 3.09  gSb Total Sb sampled Removed (g)  Sb in sol'n (g)  Sb (aq) total  %Sb indicated  %Sb actual  7.5E-06 7.5E-06 1.5E-05 2.3E-05 0.00004 3.8E-05 0.00005 4.8E-05 4.8E-05  0.000113 8.83E-05 0.000232 0.000341 0.000498 0.000582 0.000676 0.000739 0.000649 0.00 0.00  0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00  -0.08 -0.13 0.26 0.58 1.04 1.36 1.69 1.98 1.87 1.30 1.36  -0.08 -0.13 0.27 0.60 1.07 1.40 1.74 2.04 1.93 1.34 1.40  Iron Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.01 8.01 11.15 14.27 19.03 22.03 26.08 29.00 33.09 36.02  0.00307 0.00616 0.00745 0.00878 0.01099 0.01210 0.01312 0.01367 0.01402  Arsenic Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  Time (days) 0.00 3.01 8.01 11.15 14.27 19.03 22.03 26.08 29.00 33.09 36.02  0.00186 0.00329 0.00364 0.00407 0.00476 0.00547 0.00673 0.00822 0.01019  Antimony Output  Sample No. 1 2 3 4 5 6 7 8 9 Filtrate Wash  0.00001 0.00002 0.00003 0.00005 0.00009 0.00013 0.00018 0.00023 0.00028  

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