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Bioleaching of enargite Steer, Cheryl Ann 2002

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BIOLEACHING OF ENARGITE by C H E R Y L A N N STEER B.Sc , University of Alberta, 2000 A THESIS SUBMITTED IN PARTIAL FULFILMENT OF THE REQUIREMENTS FOR THE DEGREE 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, xOCj^, 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. i i 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. i i i Table of Contents Abstract i i Table of Contents iv List of Tables vii List of Figures vii i 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 52 2.6.1 Leaching of Enargite 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 101 5. Conclusions and Recommendations for Future Work 103 5.1 Conclusions 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 Chemical Formula azurite 2CuC0 3 Cu(OH) 2 bornite Cu 5FeS 4 brochantite CuS0 4-3Cu(OH) 2 chalcocite Cu 2S chalcopyrite CuFeS 2 chrysocolla CuSi0 3 -2H 2 0 covellite CuS cuprite C u 2 0 dioptase C u S i 0 3 H 2 0 enargite CU3ASS4 malachite CuC0 3 Cu(OH) 2 tennantite Cu ] 2As4Si 3 tenorite CuO tetrahedrite Cui2Sb4Si3 Ammonia (NH 3) and hydrochloric acid (HC1) are other proposed reagents for the leaching of 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 (CuFeS2) > enargite (CU3ASS4) Chalcopyrite (CuFeS2) 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 series of minerals of composition Cti3(As, Sb)S4. 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. It is orthorhombic CU3ASS4 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. As discussed previously, antimony can also be present as an impurity in enargite. 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: A S 2 O 3 and two hydroxides of A S 2 O 5 , A s 2 0 5 - 4 H 2 0 < 25.9°C and 3As 2 0 5 -5H 2 0 > 25.9°C [6]. An E h -pH diagram of the arsenic-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 2", and ASO43", 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]. Arsenic Acid Phosphoric Acid log Id logK 2 logK 3 2.24 ± 0.06 6.96 ± 0.02 11.50 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 Fe203-AS2O5-H2O system have revealed three crystalline ferric arsenates [24]: FeAs0 4-2H 20 As(V) < 0.22 M FeH3(As04)2 - IOH2O As(V) = 0.22 - 1 . 4 M Fe(H2As04)3-5.5H20 As(V)>l ' .4M. 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]. There is one hydrolysis constant for arsenious acid: log K i = 9.29 at 298.15 K [25]. 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"4 M , Sb2C>3 (cubic 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 4 / H 2 S 0 4 electrolyte [33]: CuS04 + H20 ->Cu + H2SOA + Y2 02{) [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 + SFe3+ + 4H20 -» M2+ + SOf + SH+ + SFe2+ [2-2] But, i f elemental sulphur (S°) is produced [61]: MS + 2Fei+ -> M 2 + + 2Fe2+ + S° [2-3] However, elemental sulphur is not thermodynamically stable and is predicted to be oxidized to sulphate [23, 61]: S°+y202+ H20 -> H2S04 [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. An 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 SO42". Elemental sulphur may be preferred in some instances, such as i f 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]: Cw3(OH)2 • (C0 3 ) 2 + 3H2S04 -> 3CuS04 + 2C02 + 4H20 [2-5] Cu2 (OH)2 • C03 + 2H2S04 -> 2CuS04 + 2C02 + 3H20 [2-6] CuSiQ3 • 2H20 + H2SOA -» CuS04 + Si02 + 3H20 (slow reaction) [2-7] Cuprite can be completely dissolved in acid ferric sulphate. The leaching reactions can be described as follows [20]: Cu20 + H2S04 -> CuS04 + Cu + H20 [2-8] Cu + Fe2 (S04 )3 -> CuS04 + 2FeS04 [2-9] Cu20 + H2S04 + Fe2 (S04)3 -> 2CuS04 + H20 + 2FeS04 [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]: Cu2S + Fe2 (SOA )3 -> CuS + CuSOA + 2FeS04 [2-11 a] CuS + Fe2 (S04 )3 -> CuS04 + 2FeS04 + S [2-11 b] Cw25 + 2Fe(S0 4) 3 -> 2CwS04 + 4FeS04 + S (overall reaction) [2-11 c] (The first reaction is faster, while the CuS formed is different than covellite.) Cu2S + H2S04 + Y2 02 CuS + CuS04 + H20 (very slow) [2-12] The leaching reactions for covellite are as follows [20, 23, 61]: CuS + Fe2(S04)3 -> CuS04 + 2FeS04 + S [2-13] CuS + H2SOA +y202 -> CuS04 +S°+ H20 (very slow) [2-14] Finally, the leaching of bornite can proceed as follows [23]: Cu5FeS4 + 6Fe2(S04)3 ->5CuS04 +\3FeS04 + 4S° [2-15] Cu5FeS4 + 5H2S04 + x%02^> 5CuS04 + Fe{OH\ +4S°+y2H20 [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 2CuFeS2 + 5/202 +5H2S04 -> 2CuSOA + Fe2 (S04 )3+4S + 5H20 [2-17] 2CuFeS2 + "/202+ H2S04 -» 2CuS04 + Fe2(S04)3 + 5# 20 [2-18] CaFeS 2 + H2S04 + 5/402 + /2H20 CuSO 4+Fe(OH)3 + 2S° [2-19] CuFeS2 + 2Fe2 (S04)3 -> C«50 4 + 5Fe,S04 + 2S° [2-20] 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]: Fe2 (S04)3 + 6H20 -> 2Fe(OH)i + 3H2S04 [2-21] with the precipitation of ferric oxy-hydroxide (goethite) [33]: Fe2 (S04)3+4H20^>2FeO(OH) + 3H2S04 [2-22] and/or the precipitation of ferric oxide (hematite) [23, 33]: Fe2(S04)2 + 3H20 -> 2Fe20} + 3H2S04 [2-23] and/or the precipitation of ferric hydroxy-sulphate (jarosite) [23, 33]: X2S04+3Fe2(S04)i+\2H20 -> 2XFe3(S04)2(OH)6+6H2S04 [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]: Fe 2 (50 4 ) 3 + 2H20 -> 2Fe(S04)OH + H2S04 [2-25] (At high T and high acidity) 3Fe2 (S04 ) 3 +10H2O -> 2Fe 3 (S04 )2 OH5 + 5H2S04 [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]: S0 + y2O2+ H20 -> H2S04 [2-4] The percentage of sulphur oxidized to S° and SO4" depends on the reaction conditions. An 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 SO42" [23]. 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. First, leaching reactions are functions of temperature. 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 2 [32]. • 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]: Cu3AsS4 +1 \Fe3+ + 4H20 o 3Cu2+ + As03r + 4S° + &H+ +1 \Fe1+ [2-27] This is assuming that the arsenic enters solution in the 5+ valence state. However, some arsenic occurs as A s 3 + , suggesting the following reaction also occurs [8]: Cu3AsS4 + 9Fe3+ + 2H20 o 3Cu2+ + AsO; + 4S° + 4H+ + 9Fe2+ [2-28] Not all the sulphur, however, goes to elemental sulphur. A small fraction of sulphur is oxidized to sulphate [2, 8]: S + 3Fe2 (S04)3 +4H20^> 6FeS04 + 4H2S04 [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). Without iron, arsenic and copper dissolution in acid medium (H2SO4) 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, Fe^St^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 2 S0 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 BIOX 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 "Gram-negative"; those that retain it are "Gram-posit ive" [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 wal l 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. Many are obligate autotrophs, meaning they can only grow autotropically. Some microorganisms, however, are heterotrophs, which obtain carbon from organic substances. Facultative heterotrophs are autotrophs that can also grow heterotrophically. Final ly, 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/m3 of copper [56]. 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: Nn=2"-N0 [2-30] 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 n versus t graph. The medium becomes modified as nutrients become depleted and microbial metabolism products increase; there are also changes in pH and a decrease in 0 2 and CO2 availability in the medium [56]. 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 E lag exponential stationary death 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. CuFeS2 + 402 -> CuS04 + FeS04 [2-31 ] FeS2 + \4Fe3+ + SH20 -> l5Fe2+ +16H+ + 2S04~ [2-32] 34 b) The bacteria catalyzes the oxidation of the ferrous ions: 2FeSO, + H2SO, + y202 " a / a c " ° " >Fe2(SOJ3 + H20 [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: 2Fe3+ + MS 2Fe2+ + M2+ + 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]: S0+y2O2+ H20 -> H2SOA [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 4 06 2 \ S2O3 2", H 2 S n ) may be formed as oxidation products [51, 54]. Of course, the final 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]: [Fe2+] = exp [2-36] At 25°C [56]: a 'Fe-.3+ E = 0.771 + 0.05911og [2-37] a 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 Concentration (g/L) (NH 4 ) 2 S0 4 0.1-5 K 2 H P 0 4 0.5-5 KCI 0.05-0.1 A1 2 (S0 4 ) 3 T8H 2 0 1.0-8.0 MgS0 4 -7H 2 0 0.01-3.0 M n S 0 4 H 2 0 0.05 Ca(N0 3 ) 2 -4H 2 0 0.01 N a 2 S 0 4 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. An 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 co-precipitation 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 E l Indio from La 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 3 AsS 4 , 42.8% FeS 2, and 3.9% CuFeS 2. While varying the enrichment of the air 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, La 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 BC 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 + FeCl3 -> CuCl + FeCl2 + S o [2-38] CuS + CuCl2 -> ICuCl + S' -0 [2-39] CuS + FeCi; -> CuCF2 + Fe2+ + S° + 2CI [2-40] 46 For chalcopyrite [23, 61]: CuFeS2 + 4FeCl3 -> CuCl2 + 5FeCl2 + 2S •o [2-41] CuFeS2 + 3FeC/ 3 -> CwC/ + 4FeC/ 2 + 25' -o [2-42] 2CuFeS2 + 1C12 -> 2CuCl2 + 2FeCl3 + 3S 2C/ 2 [2-43] 2S2Cl2 + 4H20 + Cl2 6HCI + H2S04 + 35' [2-44] (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 SO42" and more than 95% as 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 + 5FeCl3 -> 6FeCl2 + AsCl3 + S [2-45] As2S3 + 6FeCl3 -> 2AsCl3 + 6FeCl2 + 3S [2-46] Sb2S3 + 6FeCl3 -> 256C/3 + 6FeCl2 + 35 [2-47] 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. An 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 FeCVCuCb 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 nickel-copper 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: Cu2S + 6NH3 + (NH, )2 SO, + 5/202 -+ 2Cu(NH3 ), SO, + H20 [2-48] For covellite: CuS + 4NH3 + 202 ^Cu (NH3 ), SO, [2-49] Forbornite: 2Cu5FeS4 + 36NH3 + 2(NH,)2 SO, + ^ /202 +(2- n)H20 ->\0Cu(NH3),SO+, + Fe203 • nH20 For chalcopyrite: 2CuFeS2 + \2NH3 +"/202 + (2- n)H20 -> 2Cu(NH3),SO, + 2(NH,)2SO, + Fe203 • nH20 [2-50] [2-51] 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 SO42" concentration. One should note that in 52 this system, ammonia can remain as free NH3, be neutralized to N H 4 or be complexed with 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 NFf 3 -NH 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, + 8.7502 + 2.5H.O [2-521 -> 3Cu(NH3)l+ + NH,H2AsOA + 4S02~ +2H+ 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]. An electrochemical mechanism was proposed for the oxidative leaching of enargite with ammonia. This mechanism was described as follows [1]: 54 anode Cu3AsS4 + 390H~ o 3Cu2+ + \9H20 + HAs02~ + S02r + 35e' [2-53] cathode 02+2H20 + 4e" o40H~ [2-54] 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]: Cu 2S is recovered as a solid and arsenic enters the liquid in the pentavalent or trivalent form of thioarsenic compounds (depending on the reaction conditions) [17]. One source studied an enargite concentrate from El Indio, Chili, containing mainly enargite with some quartz [17]. It was leached in 400 mL solution, with 4 g enargite at 90°C. The 2Cu3AsSA + 3Na2S -> Cu2S + 2Na3AsS4 [2-55] 55 best results was 90.73% of the arsenic after 60 minutes, at Na 2S/NaOH = 2 (with 100 g/L:50 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]: 3H2SOA + 2Na3AsS4 -> 3H2S + 3Na2S04 + As2S5 [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 if 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 PRA (Process Research Associates) in Vancouver, BC. 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 Thermophilic Medium Medium MgS0 4 -7H 2 0 (g/L) 2.0 0.8 (NH 4 ) 2 S0 4 (g/L) 0.8 0.8 K H 2 P 0 4 (g/L) 0.3 0.1 FeS0 4 -7H 2 0 (g/L) 1.0 0.5 Mesophile nutrient solution (mL/L) 1 Thermophile nutrient solution (mL/L) 1 pH adjusted to 1.6 by 6M H 2 S 0 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 EDTA to suppress precipitation of the brown precipitate. Table 3.2: Thermophile Trace Nutrient Solution Composition Compound Composition (g/L) MnCl 2 -4H 2 0 1.8 N a 2 B 4 O 7 T 0 H 2 O 4.5 ZnS0 4 -7H 2 0 0.22 CuCl 2 -2H 2 0 0.05 V O S 0 4 - 2 H 2 0 0.03 CoS0 4 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(NH4)2(S04)2-6H20 Fe(NH 4)2(S0 4)2T2H 20 H 2 S 0 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 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 2 +) to ferric (Fe 3 +); a high potential indicates a larger ferric 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, 6M 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 pH 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 Pulp Density Added (g) (g/L) 2 19.0 3.5 33.3 5 47.6 10 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 Analysis (weight percent) Size Copper Iron Arsenic Antimony Sulphur (microns, Pso) Total (ST) Sulphate (S0 4 2-) Elemental (S°) Sulphide CS2") 10 31.2 11.6 10.5 0.55 32.2 0.13 <0.01 32.0 15 30.4 10.6 10.5 0.55 32.4 O.01 0 .01 32.3 37 32.4 7.2 12 0.39 29.1 0.02 <0.01 29.0 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) Enargite (wt. %) (Cu 3(As, Sb)S4) Pyrite (wt. %) (FeS2) Copper not in enargite (% of total copper) 10 57.2 24.9 11.6 15 57.2 22.8 9.3 37 64.5 15.5 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. -19 g/L -19 g/L (2) -33 g/L -48 g/L -95 g/L 0 5 10 15 20 25 30 35 Time (days) —*—19 g/L —*—19 g/L (2) — a — 3 3 g/L — a — 48 g/L —x — 95 g/L —>-95g /L (2) 0.00 10.00 20.00 30.00 40.00 Time (days) (a) (b) - •—19 g/L -*—19 g/L (2) -B— 33 g/L 48 g/L -x - -95g/L - » - 9 5 g / 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 5 10 15 20 25 30 35 Time (days) -19 g/L -19 g/L (2) • 33 g/L —A—48 g/L - - x - - 9 5 g / L - - » - - 9 5 g/L (2) (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. 10 15 20 25 Time (days) - 1 9 g/L - 1 9 g/L (2) - 3 3 g/L - 48 g/L - 9 5 g/L — • — 1 9 g/L — * — 1 9 g/L (2) — o — 33 g/L — a — 48 g/L - - x - - 9 5 g / L - - » - - 9 5 g / L ( 2 ) 40 (a) (b) 0 5 10 15 20 25 30 35 Time (days) — • — 1 9 g/L — * — 1 9 g/L (2) — Q — 33 g/L & 48 g/L — x - - 9 5 g / L - - » — 9 5 g / L (2) (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) Pulp Density (R/L) Element, Percent Extraction to Solution Copper Iron Arsenic 10 19 24.96 94.85 13.47 19(2) 24.21 93.17 12.29 33 25.55 92.04 14.54 48 23.99 60.13 10.59 95 26.08 75.70 14.14 15 19 22.96 75.48 8.66 19(2) 20.94 93.04 8.43 33 24.41 93.45 10.28 48 20.99 87.28 8.44 95 27.68 56.40 13.69 95 (2) 26.06 92.94 11.17 37 19 15.82 79.22 8.59 19(2) 22.88 84.10 .8.02 33 15.98 86.15 8.08 48 23.20 65.19 12.42 95 19.12 39.38 7.54 95 (2) 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 Pulp Density (R /L) Element in Residue (wt. %) Ratio of (microns) Copper Iron Arsenic Antimony Cu:As 10 (Head) 31.2 11.6 10.5 0.55 2.97 19 39 0.86 14 0.7 2.79 19(2) 39 1.03 14 0.7 2.79 33 38 0.66 14 0.7 2.71 48 35 6.3 13 0.6 2.69 95 35.2 1.8 13.9 0.67 2.53 15 (Head) 30.4 10.6 10.5 0.55 2.90 19 36 3.96 13 0.7 2.77 19(2) 39 0.95 14 0.7 2.79 33 39 0.52 14 0.7 2.79 48 39 1.91 14 0.7 2.79 95 34 4.6 13.1 0.69 2.60 95 (2) 38 0.87 14 0.7 2.71 37 (Head) 32.4 7.2 12 0.39 2.70 19 35 2.25 13 0.4 2.69 19(2) 36 2.56 13 0.7 2.77 33 36 1.24 13 0.4 2.77 48 35 5.4 12 0.6 2.92 95 32 4.4 12.7 0.42 2.52 95 (2) 36 1.38 13 0.4 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 Sulphur Analysis , weight % (microns) Sample S T (S04 2")S S° S2~ 10 Head 32.2 0.13 <0.01 32 Residue 26.8 <0.01 0.44 26.4 15 Head 32.4 <0.01 <0.01 32.3 Residue 28.2 0.2 0.31 27.7 37 Head 29.1 0.02 O.01 29 Residue 27.4 O.01 0.16 27.3 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 pH 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 82 880 580 0 5 10 15 20 25 30 35 Time (days) (a) - •—19 g/L - B — 33 g/L - A — 4 8 g/L - x - - 9 5 g / L 0 5 10 15 20 25 30 35 Time (days) (b) - •—19 g/L - o — 33 g/L -a—48 g/L - x - - 9 5 g/L 10 15 20 25 30 35 Time (days) -19 g/L - 33 g/L -48 g/L -95 g/L (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. —•—19 g/L — a — 33 g/L a 48 g/L - - x - - 9 5 g / 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 —•—19 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 5 10 15 20 25 30 35 Time (days) (a) 40 35 30 - » — 1 9 g/L - a — 33 g/L - A — 4 8 g/L -x - -95g/L 40 - •—19 g/L - a — 33 g/L 48 g/L -x —95 g/L 5 10 15 20 25 30 35 Time (days) (b) - •—19 g/L -a—33 g/L -6—48 g/L -X - -95 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) Pulp Density (g/L) Element, Percent Extraction to Solution Copper Iron Arsenic 10 19 60.15 88.91 34.14 33 59.79 92.06 36.83 45 58.36 84.08 37.80 95 50.93 30.42 27.37 15 19 48.51 96.71 23.30 33 46.94 93.71 25.05 45 47.75 83.87 26.63 95 41.94 49.47 19.41 37 19 40.51 98.34 16.73 33 40.23 78.08 17.05 45 39.74 67.39 17.39 95 34.07 24.08 13.54 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) Pulp Density (g/L) Element Ratio of Cu:As Copper Iron Arsenic Antimony 10 (Head) 31.2 11.6 10.5 0.55 2.97 19 32 2.06 12 0.9 2.67 33 33 1.71 12 0.7 2.75 48 32 3.23 12 0.6 2.67 95 27 11 11 0.6 2.45 15 (Head) 30.4 10.6 10.5 0.55 2.90 19 36 1.06 13 0.8 2.77 33 36 0.94 13 0.8 2.77 48 34 2.87 12 0.7 2.83 95 32 7.2 12 0.6 2.67 37 (Head) 32.4 7.2 12 0.39 2.70 19 33 0.80 12 0.5 2.75 33 32 2.22 12 0.5 2.67 48 32 2.92 12 0.4 2.67 95 30 6.1 12 0.4 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 Thermophi les 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 0 5 10 15 20 25 30 35 Time (days) (a) 1.00 — • — 1 9 g/L — » — 1 9 g / L (2) — e — 33 g/L — A — 4 8 g/L - - x - - 9 5 g / L -19 g/L -19 g/L (2) -33 g/L -48 g/L -95 g/L 0 5 10 1 5 20 25 30 35 Time (days) (b) - 1 9 g/L - 1 9 g/L (2) - 3 3 g/L - 48 g/L - 9 5 g/L 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 . 1 : r-0 10 20 30 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 BC, found that the extraction was a strong function of pulp density [47]. It was believed that since Sulfolobus BC 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 60 40 20 0 5 10 15 20 25 30 35 Time (days) (a) 100 - •—19 g/L -*—19 g/L (2) -B— 33 g/L - A — 48 g/L -x —95 g/L 0 5 10 15 20 25 30 35 Time (days) (b) - •—19 g/L -*—19 g/L (2) - a — 33 g/L -a—48 g/L -x - -95g/L 0 5 10 15 20 25 30 35 Time (days) -19 g/L -19 g/L (2) —o— 33 g/L —a—48 g/L - -x - -95g/L —•—19 g/L - * — 1 9 g/L (2) —o—33 g/L - A — 4 8 g/L -x - -95g/L (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 —*—19 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 25 0 5 10 15 20 25 30 35 Time (days) (a) 30 25 g c o 20 B Extr: 15 u seni 10 < 5 0 — « — 1 9 g/L —*—19 g/L (2) — o — 33 g/L —a—48 g/L - - x - - 95g /L 5 10 15 20 25 30 35 Time (days) (b) - •—19 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) Pulp Density (g/L) Element, Percent Extraction to Solution Copper Iron Arsenic 10 19 99.31 22.01 1.64 19(2) 99.12 26.56 1.17 33 99.13 24.92 1.36 48 38.05 15.44 1.87 95 37.09 13.82 1.73 15 19 97.83 7.34 1.32 19(2) 95.15 17.89 2.49 33 86.43 3.71 4.10 48 . 43.98 11.44 1.98 95 28.15 8.79 0.89 37 19 93.19 -24.77 4.11 19(2) 84.94 14.67 3.08 33 63.82 -8.24 7.27 48 51.19 15.29 6.07 95 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) Pulp Density (g/L) Element Ratio of Cu:As Copper Iron Arsenic Antimony 10 (Head) 31.2 11.6 10.5 0.55 2.97 19 0.53 17 20 0.5 0.03 19(2) 0.62 18 21 0.4 0.03 33 0.63 18 21 0.8 0.03 48 26 12 13 0.6 2.00 95 25.6 11.6 13.8 0.62 1.86 15 (Head) 30.4 10.6 10.5 0.55 2.90 19 1.53 16 16 0.6 0.10 19(2) 3.4 18 19 0.8 0.18 33 8.6 18 17 0.9 0.51 48 25 12 13 0.6 1.92 95 28 11.4 12.8 0.65 2.19 37 (Head) 32.4 7.2 12 0.39 2.70 19 4.4 14 18 0.6 0.24 19(2) 10 17 16 0.8 0.63 33 18 11 15 0.5 1.20 48 23 13 14 0.6 1.64 95 26.8 8.6 13.4 0.44 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 Sulphur Analysis , weight % Sample S T (S04 2")S S° S2" 10 Head 32.2 0.13 O.01 32.0 Residue 27.1 0.05 <0.01 27.0 15 Head 32.4 <0.01 <0.01 32.3 Residue 29.5 0.21 <0.01 29.2 37 Head 29.1 0.02 O.01 29.0 Residue 25.9 0.01 <0.01 25.9 100 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 re-precipitating 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 D i s c u s s i o n a n d 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 CESL 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]. 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King, "Passivation of chalcopyrite during oxidative leaching in sulfate media", Hydrometallurgy 39 (1995) 25-48 70. Daniel C. Harris, Quantitative Chemical Analysis. 3 r d 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 3 +) are present as the oxidizing agents in these examples. In the following reactions: • Enargite as Cu3 (As, Sb)S4 • Copper as C u 2 + • Sulphur as S° or SO42" • Arsenic (III) as A s O + or H A S O 2 • Arsenic (V) as H 2 A S O 4 " or H 3 A S O 4 • Antimony (III) as SbO + or HSb0 2 • Antimony (V) as Sb0 2 + or Sb0 3" • Oxidizing agents are 0 2 and Fe 3 + • H + and H 2 O are also present For Arsenic (III) species: If oxygen is the oxidant: Cu3AsSA+yA02 +y2H2S04->3CuS04+/2(AsO)2SOA +4S°+y2H20 [Al] Cu3AsSA + 3%0 2 +y2H20->3CuSOA + y2(AsO)2SOA +y2H2SOA [A2] 120 Cu3AsS4 +%02+ 3H2S04 -> 3CuS04 + HAs02 + 4S° + 5/2H20 CuiAsS4 + 3 % O a +y2H20 -» 3CuS04 + HAs02 + H2S04 [A3] [A4] If ferric iron is the oxidant: Cu3AsS4 + %Fe2(S04)3 + H20 -> 3CuS04 + Y2 (AsO)2 S04 + 4S° + H2S04 + 9FeS04 Cu3AsS4 + 3% Fe2 (S04 )3 + \lH20 -> 3CuS04 +y2(AsO)2S04 + \1H2S04 + 33FeS04 Cu3AsS4 + %Fe2(S04)3 + 2H20 -> 3CuS04 + HAs02 + 4S° + y2 H2S04 + 9FeS04 Cu3AsS4 + ^y2Fe2(S04)3 + \SH20 -> 3CuS04 + HAsQ2 + 4S024~ + 3%H2S04 + 33FeS04 If ferric iron is the oxidant: Cu3AsS4 + %Fe2{S04)3 + 4H20 -> 3CuS04 + H3As04 +4S°+y2 H2S04 +1 \FeS04 [A5] [A6] [A7] [A8] For Arsenic (V) species: If oxygen is the oxidant: Cu3AsS4 +%02+ 3H2S04 3CuS04 + H3As04 + 4S° + y2H20 [A9] Cu3AsS4 +iy402 +y2H20^> 3CuS04 + H3As04 + H2S04 [A10] [Al l ] 121 Cu3AsS4 + 35/2 Fe2 (S04 )3 + 20H2O -> 3CuS04 + H3As04 + % H2S04 + 35FeSOA [A12] For Antimony (III) species: If oxygen is the oxidant: Cu3SbS4 +%02+y2H2S04 -> 3CuSOA + y2(SbO)2S04 + 4S° + y2H20 [Al3] Cu3ASbS4 + y402 +y2H20 -> 3CuS04 +y2(SbO)2S04 +y2H2S04 [A14] Cu3SbS4 +%02+ 3H2S04 ->3CuS04 + HSb02 +4S° +5/2H20 [Al5] Cu3SbS4 +iy402 +y2H20^> 3CuS04 + HSb02 + H2S04 [ A l 6] If ferric iron is the oxidant: Cu3SbS4 + % Fe2(S04)3 + H20 -> 3CuS04 + y2 (SbO)2 S04 + 4S° + H2S04 + 9FeS04 Cu3SbS4 + %Fe2(S04)3 +\1H20 -> 3CuS04 +y2(SbO)2S04 +17 H2S04 + 33FeS04 [A17] [A18] Cu3SbS4 +%Fe2(S04)3 + 2H20 -->3CuSO4+HSbO2+4S0+y2H2S04+9FeS04 Cu3SbS4 + 3 K Fe2 (S04 ) 3 +18# 2 0 -> 3CuS04 + HSb02 + % H2S04 + 33FeS04 [A20] 122 For Antimony (V) species: If oxygen is the oxidant: Cu3SbS4 +u/402 + 3H2S04 -> 3CuS04 + HSb03 +4S° + 5/2H20 [A21 ] Cu3SbS4 +iy402 +y2H20^> 3Cu2+ + HSb03 + H2S04 [A22] Cu3SbS4 +nA02+y2H2S04 ->3CuS04 + y2(Sb02)2S04+4S° + 7AH20 [A23] Cu3SbS4 +iy402 +y2H20^> 3CuS04 + (Sb02 )2 SOA + y2 H2S04 [A24] If ferric iron is the oxidant: Cu3SbS4 + uy2Fe2(S04)3 + 3H20 3CuS04 + HSbQ3 + 4S° + 5H2S04 +1 \FeS04 [A25] Cu3SbS4 +y2Fe2(S04)3 +\9HzO-+3CuS04 +HSb03+%H2S04 +35FeS04 [A26] Cw3SZ>S4 + % FeJS04)3 + 2H20 3CuS04 + y2 (Sb02 )2S04+ 4S° + 2H2S04 +1 \FeS04 Cu3AsS4 + % Fe2 (S04 )3+lSH20 -> 3CuS04 + y2 (Sb02 )2 S04 +1SH2S04 + 35FeS04 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, BC using 30 element Inductively Coupled Plasma (ICP) analysis. Table B. 1: Chemical Analysis of the Trace Nutrient Solutions Element Present Thermophile Trace Nutrient Solution (Composition in mg/L) Mesophile Trace Nutrient Solution (Composition in mg/L) Aluminum (Al) 8.5 7.5 Arsenic (As) 12.5 4.5 Bismuth (Bi) 1.5 Calcium (Ca) 4.0 52.5 Cobalt (Co) 1.20 40.15 Copper (Cu) 17.50 5.45 Iron (Fe) 15.65 11.85 (La) 0.35 Magnesium (Mg) 1.0 466.5 Manganese (Mn) 144.95 233.40 (Mo) 2.00 4.85 Nickel (Ni) 0.25 Phosphorous (P) 1.5 2.0 Potassium (K) 25 Sodium (Na) 875 1185 (Sr) 0.10 1.00 Tungsten (W) 0.5 Vanadium (V) 5.20 0.10 Zinc (Zn) 48.80 35.95 (Zr) 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 = mass of metal in the filtrate M W a s h = mass of metal in the wash water M r e s i d u e = mass of metal in the residue M Sampie = 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 For a liquid sample, the mass of the metal is determined by: M = Cm/vVljquid [C l ] [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 W a s h + M s a m p l e [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 +M™id»e+M°<"»P'e ~M'eacH m % [ c 4 ] mfeed 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] Mhead If the measured head is used, this is the indicated extraction; i f the calculated head is used, this is the actual extraction. Alternately: M -M %Extraction = — ^ [C6] Mhead 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 Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B3-M10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 8.02 17.31 7.47 5.74 1.76 17.26 7.85 6.19 2.00 14.00 20.71 19.15 4.84 1.84 20.65 20.13 5.21 2.09 26.01 23.42 81.33 10.84 10.03 23.35 85.50 11.69 11.38 36.34 25.03 90.22 12.49 11.51 24.96 94.85 13.47 13.07 B3-M15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 8.02 20.81 8.31 4.37 1.08 21.15 9.17 5.04 1.22 14.00 24.70 19.23 3.75 1.12 25.11 21.23 4.33 1.27 26.01 26.95 67.07 6.54 6.17 27.39 74.04 7.54 6.96 36.34 22.59 68.38 7.51 7.20 22.96 75.48 8.66 8.12 B3-M37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 8.02 10.11 9.61 3.49 1.16 10.70 10.18 4.00 1.39 14.00 12.36 23.30 3.07 1.87 13.09 24.68 3.52 2.25 26.01 14.01 55.08 4.34 3.98 14.82 58.34 4.98 4.80 36.34 14.95 74.80 7.50 7.46 15.82 79.22 8.59 8.99 " ~ " B4-M10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 11.87 17.08 9.62 2.52 1.27 17.06 9.26 2.73 1.45 20.19 20.16 49.63 2.44 3.21 20.14 47.78 2.64 3.66 25.85 22.15 67.24 2.27 6.11 22.13 64.74 2.46 6.97 35.81 24.24 96.76 11.34 10.51 24.21 93.17 12.29 11.97 B4-M15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 11.87 17.36 15.03 1.28 -0.14 17.11 15.32 1.41 -0.16 20.19 19.63 48.02 1.47 2.72 19.35 48.92 1.62 3.13 25.85 20.18 64.81 1.88 5.20 19.89 66.03 2.07 5.99 35.81 21.24 91.32 7.67 7.24 20.94 93.04 8.43 8.34 B4-M37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 11.87 15.39 19.59 0.97 1.15 16.57 13.32 1.27 0.90 20.19 16.80 61.83 2.25 3.91 18.07 42.02 2.96 3.07 25.85 18.86 78.80 1.38 6.05 20.29 53.56 1.82 4.76 35.81 21.27 123.73 6.09 11.54 22.88 84.10 8.02 9.07 127 Table D.2: Extraction data for mesophile experiments with 3.5 g of sample. Indicated Extractions. ; Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B6-M10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 7.07 12.74 3.00 2.24 0.22 12.74 3.30 2.35 0.28 19.96 19.04 34.94 4.39 1.88 19.03 38.46 4.60 2.39 27.97 21.96 95.56 11.87 11.09 21.95 105.19 12.45 14.15 35.99 25.55 83.61 13.87 0.57 25.55 92.04 14.54 0.73 B6-M15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 7.07 12.84 2.89 1.73 0.49 12.49 3.07 1.93 0.63 19.96 18.43 31.84 3.13 2.16 17.93 33.85 3.48 2.78 27.97 21.47 92.07 7.90 7.79 20.88 97.89 8.77 10.04 35.99 25.09 87.89 9.25 0.44 24.41 93.45 10.28 0.57 B6-M37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 7.07 7.87 3.86 1.92 0.69 7.71 3.89 2.11 0.87 19.96 12.19 24.22 2.00 0.34 11.94 24.46 2.20 0.43 27.97 14.44 68.16 5.12 3.84 14.14 68.83 5.63 4.84 35.99 16.31 85.30 7.35 0.16 15.98 86.15 8.08 0.21 Table D.3: Extraction data for mesophile experiments with 5 g of sample. Indicated Extractions Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B5-M10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 7.80 15.62 1.39 2.74 -0.09 14.89 1.47 2.78 -0.12 13.17 18.39 6.00 1.96 0.10 17.53 6.33 1.99 0.13 18.81 19.22 12.20 1.95 0.29 18.33 12.88 1.98 0.37 28.79 20.24 25.27 1.22 1.61 19.30 26.68 1.24 2.07 35.81 25.16 56.96 10.42 -0.06 23.99 60.13 10.59 -0.08 B5-M15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 7.80 15.35 3.67 0.57 0.10 14.56 3.97 0.60 0.11 13.17 17.05 15.07 0.99 0.68 16.17 16.31 1.05 0.75 18.81 18.97 22.85 1.00 1.44 17.99 24.74 1.06 1.58 28.79 19.44 55.59 2.78 4.48 18.44 60.18 2.94 4.93 35.81 22.13 80.62 7.98 8.24 20.99 87.28 8.44 9.07 B5-M37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 7.80 13.55 1.72 2.03 -0.13 14.20 1.21 2.62 -0.11 13.17 18.04 9.68 1.55 -0.13 18.90 6.80 2.00 -0.11 18.81 19.00 19.74 1.78 0.40 19.90 13.87 2.30 0.35 28.79 19.70 28.51 1.09 1.99 20.64 20.03 1.40 1.74 35.81 22.15 92.77 9.63 10.10 23.20 65.19 12.42 8.82 128 Table D.4: Extraction data for mesophile experiments with 10 g of sample. Indicated Extractions Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B2-M10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 3.00 6.15 1.18 0.32 0.22 6.29 1.29 0.32 0.24 8.01 14.03 1.05 1.95 0.23 14.36 1.14 1.97 0.25 11.14 15.57 1.83 1.49 -0.03 15.94 1.99 1.51 -0.03 14.26 19.20 14.94 3.51 0.71 19.65 16.26 3.56 0.77 19.02 21.91 27.95 6.41 1.92 22.43 30.41 6.50 2.08 22.02 24.23 34.20 8.78 3.39 24.81 37.21 8.90 3.68 26.08 24.71 49.10 12.96 12.93 25.29 53.42 13.14 14.00 29.00 26.98 64.55 14.54 14.71 27.62 70.23 14.73 15.92 33.08 26.80 75.05 14.43 14.75 27.43 81.66 14.62 15.97 36.02 25.47 69.57 13.95 14.40 26.08 75.70 14.14 15.59 B2-M15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 3.00 6.20 0.82 0.09 -0.05 6.24 0.86 0.10 -0.06 8.01 16.87 0.60 1.96 0.04 16.97 0.63 2.11 0.04 11.14 22.23 1.16 2.91 0.04 22.36 1.22 3.14 0.04 14.26 25.67 18.56 5.16 1.34 25.82 19.52 5.55 1.42 19.02 27.03 52.81 12.82 9.74 27.19 55.54 13.79 10.33 22.02 27.32 52.62 11.78 12.47 27.48 55.33 12.67 13.22 26.08 27.58 53.93 12.18 13.18 27.74 56.71 13.11 13.98 29.00 29.07 58.59 13.23 13.79 29.23 61.61 14.23 14.62 33.08 28.49 56.70 13.03 13.94 28.65 59.63 14.02 14.78 36.02 27.52 53.64 12.73 13.62 27.68 56.40 13.69 14.44 B2-M37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 3.00 1.95 0.29 -0.08 4.46 2.11 0.32 -0.08 4.39 8.01 1.96 3.83 -0.08 11.94 2.12 4.16 -0.08 11.75 11.14 0.99 5.15 -0.08 14.82 1.07 5.58 -0.08 14.59 14.26 4.20 6.16 -0.08 17.37 4.55 6.68 -0.08 17.10 19.02 13.57 1.32 -0.08 18.11 14.69 1.43 -0.08 17.82 22.02 27.55 5.08 0.98 18.78 29.83 5.51 1.07 18.48 26.08 32.94 5.88 1.82 19.19 35.67 6.37 2.00 18.89 29.00 38.01 6.62 1.92 20.21 41.15 7.17 2.10 19.89 33.08 39.55 6.96 2.26 19.74 42.82 7.54 2.48 19.43 36.02 36.37 6.95 4.54 19.12 39.38 7.54 4.97 18.81 129 Table D.5: Extraction data for mesophile experiments with 10. g of sample (continued). Indicated Extractions Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B7-M15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 6.95 17.86 1.26 0.46 — 17.59 1.37 0.51 — 14.98 24.10 16.54 3.09 . . . 23.75 17.92 3.43 . . . 21.96 26.58 34.32 7.90 . . . 26.19 37.17 8.76 _ _ . 27.94 27.20 67.34 10.81 . . . 26.79 72.95 12.00 . . . 35.98 26.46 85.80 10.06 — 26.06 92.94 11.17 . . . B7-M37 0.00 0.00 0.00 0.00 . . . 0.00 0.00 0.00 — 6.95 12.00 0.03 2.21 — 11.53 0.03 2.39 . . . 14.98 16.78 11.55 2.35 . . . 16.12 12.58 2.54 . . . 21.96 17.63 37.63 5.17 . . . 16.94 41.01 5.60 — 27.95 18.79 62.29 8.91 . . . 18.05 67.89 9.66 — 35.98 19.16 75.99 9.40 . . . 18.40 82.82 10.20 . . . Moderate Thermophiles Table D.6: Extraction data for moderate thermophile experiments with 2 g of sample. Indicated Extractions Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B9-T10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.92 41.83 18.02 15.97 -0.86 40.33 27.16 22.84 -1.31 19.97 49.13 73.71 23.36 3.09 47.37 111.10 33.40 4.72 28.03 51.66 69.78 25.13 2.84 49.80 105.18 35.94 4.33 35.99 62.39 58.99 23.87 -0.47 60.15 88.91 34.14 -0.73 B9-T15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.92 31.87 12.68 10.21 0.01 29.31 18.38 13.39 0.02 19.97 35.79 41.44 10.75 1.35 32.92 60.08 14.09 1.97 28.03 42.13 69.15 17.01 4.05 38.75 100.26 22.30 5.93 35.99 52.74 66.71 17.77 -0.45 48.51 96.71 23.30 -0.66 B9-T37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.92 27.84 22.20 11.47 -0.61 27.10 40.06 15.92 -0.80 19.97 29.54 53.30 10.84 -0.57 28.75 96.17 15.04 -0.75 28.03 33.23 66.59 13.63 0.06 32.35 120.15 18.91 0.08 35.99 41.62 54.50 12.06 -1.09 40.51 98.34 16.73 -1.44 130 Table D.7: Extraction data for moderate thermophile experiments with 3.5 g of sample. Indicated Extractions Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B6-T10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.91 34.93 7.95 12.31 -0.49 33.43 10.72 17.14 -0.98 19.96 51.55 29.16 16.48 0.01 49.34 39.32 22.93 0.03 28.03 52.90 54.08 21.25 2.29 50.63 72.92 29.58 4.57 35.99 62.47 68.27 26.46 -0.32 59.79 92.06 36.83 -0.65 B6-T15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.91 40.73 9.66 10.78 -0.49 38.03 12.24 13.59 -0.71 19.96 52.29 46.18 15.29 1.45 48.82 58.48 19.28 2.08 28.03 56.80 94.34 27.41 9.63 53.02 119.47 34.57 13.79 35.99 50.28 74.00 19.87 -0.01 46.94 93.71 25.05 -0.02 B6-T37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.91 23.98 4.56 10.61 -0.01 23.16 6.64 14.04 -0.01 19.96 33.56 17.57 11.45 -0.66 32.40 25.59 15.16 -0.82 28.03 35.43 39.10 12.21 -0.66 34.21 56.96 16.17 -0.82 35.99 41.66 53.59 12.88 -0.66 40.23 78.08 17.05 -0.82 Table D.8: Extraction data for moderate thermophile experiments with 5 g of sample. Indicated Extractions Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B8-T10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.91 28.98 5.92 10.34 -0.35 26.74 7.76 12.79 -0.72 19.96 44.53 17.49 17.62 0.01 41.09 22.94 21.80 0.01 28.03 49.23 38.42 22.83. 1.63 45.42 50.38 . 28.24 3.41 35.99 63.25 64.12 30.56 -0.23 58.36 84.08 37.80 -0.48 B8-T15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.91 20.83 3.12 3.30 0.19 19.16 3.82 4.18 0.29 19.96 36.24 10.92 10.57 -0.32 33.32 13.36 13.36 -0.49 28.03 40.19 44.80 16.12 2.16 36.96 54.77 20.37 3.35 35.99 51.93 68.61 21.07 -0.19 47.75 83.87 26.63 -0.30 B8-T37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.91 16.18 2.22 6.40 -0.49 15.20 3.21 8.15 -0.73 19.96 26.53 6.03 12.27 -0.49 24.93 8.70 15.61 -0.73 28.03 32.27 22.20 13.21 -0.49 30.32 32.00 16.80 -0.73 35.99 42.30 46.75 13.67 -0.49 39.74 67.39 17.39 -0.73 131 Table D.9: Extraction data for moderate thermophile experiments with 10 g of sample. Indicated Extractions Actual Extractions Time C u Fe As . Sb C u Fe A s Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B7-T10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.91 18.05 2.93 2.38 -0.08 16.38 3.45 2.64 -0.12 19.96 31.54 8.85 11.09 0.01 28.62 10.41 12.30 0.02 28.02 40.91 18.61 18.19 0.74 37.12 21.89 20.18 1.09 35.99 56.13 25.87 24.68 -0.11 50.93 30.42 27.37 -0.17 B7-T15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.91 15.00 2.14 0.05 0.09 13.76 2.67 0.05 0.14 19.96 28.99 6.56 6.73 0.20 26.60 8.17 7.90 0.31 28.02 34.98 21.07 11.57 0.72 32.10 26.23 13.58 1.10 35.99 45.70 39.74 16.54 -0.10 41.94 49.47 19.41 -0.15 B7-T37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 12.91 13.17 1.85 2.86 -0.24 12.17 2.22 3.21 -0.31 19.96 21.09 4.41 8.42 -0.24 19.50 5.28 9.45 -0.31 28.02 27.86 9.12 12.21 -0.24 25.76 10.92 13.71 -0.31 35.99 36.85 20.10 12.07 -0.24 34.07 24.08 13.54 -0.31 132 Extreme Thermophiles Table D.10: Extraction data for extreme thermophile experiments with 2 g of sample. Indicated Extractions Actual Extractions T ime C u Fe As Sb C u Fe A s Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B3-E10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 8.04 30.15 16.81 14.76 0.08 27.46 21.45 17.13 0.20 14.01 78.06 11.38 13.82 0.07 71.10 14.52 16.04 0.17 26.01 113.11 20.31 1.64 9.49 103.02 25.91 1.91 22.91 36.36 109.03 17.25 1.41 0.97 99.31 22.01 1.64 2.33 B3-E15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 8.04 20.32 6.83 5.75 2.28 18.74 9.85 7.96 3.99 14.01 36.76 6.27. 9.60 -0.29 33.90 9.05 13.29 -0.50 26.01 99.09 3.19 2.39 11.45 91.39 4.60 3.31 20.05 36.36 106.07 5.08 0.95 6.08 97.83 7.34 1.32 10.66 B3-E37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 8.04 59.11 -1.69 26.31 -2.31 52.91 -2.21 30.03 -2.53 14.01 75.78 -25.54 6.40 0.93 67.83 -33.37 7.30 1.02 26.01 93.69 -20.81 3.97 4.74 83.86 -27.19 4.53 5.19 36.36 104.11 -18.95 3.60 5.23 93.19 -24.77 4.11 5.73 * ' ' " ' i t . ^ ' •• • B4-E10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 . 11.89 92.46 15.78 8.48 4.86 87.59 17.07 8.87 13.69 20.23 101.84 26.42 0.96 11.48 96.48 28.57 1.01 32.38 25.88 99.49 23.91 0.69 5.73 94.25 25.85 0.73 16.15 35.83 104.62 24.56 1.12 1.09 99.12 26.56 1.17 3.06 B4-E15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 11.89 26.69 7.81 5.10 0.00 25.18 9.27 5.97 0.00 20.23 37.20 4.97 1.62 5.16 35.10 5.90 1.89 6.68 25.88 80.88 2.74 5.06 9.18 76.30 3.25 5.93 11.88 35.83 100.85 15.07 2.13 10.38 95.15 17.89 2.49 13.43 B4-E37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 11.89 17.57 6.65 2.19 1.87 16.25 5.09 3.02 1.50 20.23 46.79 5.90 1.77 7.29 43.28 4.51 2.44 5.82 25.88 73.77 9.34 2.66 12.71 68.23 7.15 3.66 10.16 35.83 91.84 19.15 2.23 16.99 84.94 14.67 3.08 13.58 133 Table D . l l : Extraction data for extreme thermophile experiments with 3.5 g of sample. Indicated Extractions Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B7-E10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 8.01 29.10 13.76 4.27 -0.81 26.63 14.74 4.49 -1.20 15.01 80.91 10.83 3.78 -0.81 74.05 11.60 3.98 -1.20 23.05 114.09 15.53 3.26 -0.81 104.42 16.64 3.43 -1.20 30.02 115.00 24.94 1.49 -0.81 105.26 26.72 1.57 -1.20 36.00 108.31 23.26 1.29 -0.81 99.13 24.92 1.36 -1.20 B7-E15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 8.01 15.33 3.11 0.82 -0.80 13.44 3.36 0.89 -0.91 15.01 25.03 6.57 1.65 -0.80 21.95 7.10 1.79 -0.91 23.05 41.80 12.73 5.38 -0.80 36.65 13.76 5.82 -0.91 30.02 72.98 6.60 2.67 -0.80 63.98 7.13 2.89 -0.91 36.00 98.58 3.43 3.78 -0.80 86.43 3.71 4.10 -0.91 B7-E37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 8.01 14.40 2.33 1.81 -1.13 13.72 2.61 1.97 -1.31 15.01 38.90 -3.29 8.21 -1.13 37.05 -3.68 8.91 -1.31 23.05 57.22 -7.31 4.82 -1.13 54.50 -8.17 5.23 -1.31 30.02 63.97 -7.38 5.92 -1.13 60.94 -8.25 6.42 -1.31 36.00 67.00 -7.37 6.70 -1.13 63.82 -8.24 7.27 -1.31 Table D.12: Extraction data for extreme thermophile experiments with 5 g of sample. Indicated Extractions Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B5-E10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 7.81 18.10 5.26 0.32 -0.27 17.70 5.76 0.33 -0.32 13.19 24.39 13.17 0.61 1.40 23.85 14.42 0.64 1.63 18.83 20.95 9.47 0.53 1.62 20.49 10.37 0.55 1.89 28.80 35.18 11.16 1.53 3.24 34.41 12.22 1.60 3.78 35.82 38.90 14.10 1.79 2.97 38.05 15.44 1.87 3.46 B8-E15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 9.87 9.18 1.82 0.44 0.00 8.49 1.99 0.47 0.00 14.98 21.84 6.49 1.28 0.00 20.18 7.13 1.38 0.00 21.96 26.59 8.40 0.35 0.00 24.57 9.22 0.37 0.00 27.94 31.49 12.00 0.74 0.00 29.10 13.17 0.79 0.00 35.98 47.59 10.43 1.84 0.00 43.98 11.44 1.98 0.00 B5-E37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 7.81 17.69 10.73 1.68 -0.39 17.64 7.52 1.96 -0.34 13.19 23.19 18.26 3.17 -0.39 23.13 12.80 3.71 -0.34 18.84 34.81 25.33 2.80 2.89 34.71 17.75 3.27 2.55 28.80 38.94 19.78 2.69 4.82 38.84 13.87 3.15 4.25 35.82 51.33 21.81 5.20 7.40 51.19 15.29 6.07 6.52 134 Table D-13: Extraction data for extreme thermophile experiments with 10 g of sample. Indicated Extractions Actual Extractions Time Cu Fe As Sb Cu Fe As Sb (days) (%) (%) (%) (%) (%) (%) (%) (%) B2-E10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 3.01 11.21 5.69 3.03 -0.26 11.22 5.91 2.96 -0.30 8.01 19.10 6.71 0.61 0.74 19.11 6.97 0.59 0.83 11.15 20.56 7.85 0.54 0.94 20.58 8.15 0.52 1.05 14.27 23.80 9.61 0.72 1.64 23.82 9.99 0.70 1.84 19.03 26.47 13.01 0.88 1.96 26.49 13.52 0.86 2.20 22.03 28.71 11.91 1.08 2.73 28.74 12.37 1.05 3.06 26.08 31.89 13.52 1.35 3.10 31.92 14.05 1.31 3.47 29.00 34.45 15.45 1.49 3.50 34.48 16.05 1.45 3.93 33.09 38.11 16.16 1.71 3.65 38.15 16.78 1.67 4.09 36.05 37.05 13.31 1.78 2.75 37.09 13.82 1.73 3.09 B2-E15 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 3.01 5.94 2.34 0.26 0.03 5.88 2.44 0.27 0.03 8.02 8.14 4.60 1.75 -0.18 8.06 4.80 1.80 -0.19 11.15 10.85 3.54 0.20 -0.24 10.74 3.70 0.21 -0.25 14.27 13.96 6.15 0.54 0.63 13.82 6.42 0.56 0.67 19.03 19.14 7.44 0.31 0.53 18.95 7.76 0.32 0.56 22.03 20.48 6.29 2.58 0.79 20.27 6.57 2.66 0.83 26.04 23.59 7.20 0.55 1.12 23.35 7.52 0.57 1.18 29.00 26.63 8.87 0.63 1.69 26.36 9.27 0.65 1.78 33.09 29.25 9.65 0.76 1.94 28.95 10.08 0.78 2.05 36.02 28.44 8.42 0.86 1.61 28.15 8.79 0.89 1.70 B2-E37 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 3.01 6.43 4.61 2.20 -0.08 6.49 . 4.67 2.25 -0.08 8.01 11.37 2.76 1.42 -0.13 11.48 2.79 1.45 -0.13 11.15 12.58 1.00 0.57 0.26 12.70 1.02 0.59 0.27 14.27 13.94 0.96 0.71 0.58 14.08 0.97 0.73 0.60 19.03 17.17 1.63 0.91 1.04 17.34 1.65 0.93 1.07 22.03 18.07 0.61 1.17 1.36 18.24 0.62 1.20 1.40 26.08 22.14 -0.13 1.73 1.69 22.35 -0.13 1.77 1.74 29.00 26.87 -0.58 2.34 1.98 27.12 -0.59 2.39 2.04 33.09 29.14 -1.36 2.79 1.87 29.42 -1.38 2.85 1.93 36.02 28.82 -1.90 3.02 1.36 29.10 -1.93 3.09 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 e o of 10 microns Test UB3-M10 Mesophiles Date Hour Time (days) . Initial Mass (g) pH Eh (Ag/AgCI) E„ (mV) Sample (mL) Medium Added (mL) Added Water (g) Final Mass (g) 14-Feb 10:15 0.00 225.88 1.69 453 673 18-Feb 9:20 3.96 224.17 1.66 461 681 1.54 225.71 21-Feb 11:25 7.05 224.46 1.60 525 745 1.63 226.09 22-Feb 10:40 8.02 225.72 1.59 521 741 5 5 26-Feb 9:55 11.99 223.96 1.51 550 770 2.06 226.02 28-Feb 10:10 14.00 225.35 1.55 569 789 5 5 5-Mar 10:25 19.01 223.43 1.43 630 850 2.50 225.93 7-Mar 11:30 21.05 225.22 1.47 641 861 11-Mar 12:35 25.10 223.60 1.41 2.82 226.42 12-Mar 10:30 26.01 226.09 1.47 666 886 5 5 14-Mar 11:00 28.03 225.22 1.52 672 892 0.83 226.05 15-Mar 12:00 29,07 225.66 1.32 678 898 19-Mar 12:25 33.09 223.99 1.42 678 898 2.58 226.57 21-Mar 20:30 35.43 225.46 1.36 679 899 22-Mar 18:30 36.34 224.88 1.36 678 898 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) 1.21 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 191.70 54.85 8.0 1.5 Medium (g/L) 0 0.10 0 0 Samples (mg/L): #1 1054.85 171.50 116.5 2.0 #2 1212.00 433.05 93.0 2.0 #3 1307.65 1809.40 208.5 10.5 PLS (mg/L) 1357.70 2059.45 240.5 12.0 Wash (mg/L) 14.05 9.24 Solid Residue (wt % 39 0.8599 14 0.7 •'• *i.<~ . • - ..#:." Weight of Element Copper Iron Arsenic Antimony Head (g) 0.62712 0.23316 0.21105 0.011055 Innoculum (g) 0.0019 0.0005 0.0001 0.0000 Medium (g) 0 0.00954 0 0 Samples (g): #1 0.005274 0.00086 0.000583 0.00001 #2 0.00606 0.00217 0.000465 0.00001 #3 0.006538 0.00905 0.001043 0.0000525 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.1375 0.2086 0.0244 0.0012 Wash (g) 0.003513 0.00231 0 0 Solid Residue (g) 0.4719 0.0104 0.1694 0.00847 , . itiSL v.v. Calculated Head (g) 0.629 0.222 0.196 0.010 % Difference -0.282 4.878 7.240 11.868 % Extraction Calculated Head 24.96 95.31 13.47 13.07 Measured Head 25.03 90.66 12.49 11.51 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 0.00 104.90 1 8.02 104.74 0.00527425 0.00527 0.110 0.109 17.31 17.26 2 14.00 104.37 0.00606 0.01133 0.126 0.130 20.71 20.65 3 26.01 105.11 0.00653825 0.01787 0.137 0.147 23.42 23.35 Filtrate 36.34 101.29 0.138 0.153 Wash 250.00 0.004 0.157 25.03 24.96 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 104.90 1 8.02 104.74 0.000355299 0.00036 0.01796291 0.02 7.47 7.85 2 14.00 104.37 0.001663049 0.00202 0.045197429 0.04 19.15 20.13 3 26.01 105.11 0.008544799 0.01056 0.190186034 0.19 81.33 85.50 Filtrate 36.34 101.29 0.2086 0.21 Wash 250.00 0.00231 0.21 90.22 94.85 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 0.00 104.90 1 8.02 104.74 0.0005825 0.00058 0.01220221 0.01 5.74 6.19 2 14.00 104.37 0.000465 0.00105 0.00970641 0.01 4.84 5.21 3 26.01 105.11 0.0010425 0.00209 0.021915435 0.02 10.84 11.69 Filtrate 36.34 101.29 0.02 0.03 Wash 250.00 0.00 0.03 12.49 13.47 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 0.0000 104.90 1 8.02 104.74 0.00001 0.00001 0.00020948 0.00 1.76 2.00 2 14.00 104.37 0.00001 0.00002 0.00020874 0.00 1.84 2.09 3 26.01 105.11 0.0000525 0.00007 0.001103655 0.00 10.03 11.38 Filtrate 36.34 101.29 0.00 0.00 Wash 250.00 0.00 0.00 11.51 13.07 Mesophiles, 2 g Enargite (2), P 8 0 of 10 microns Test UB4-M10 Mesophiles Date Hour Time (days) Initial Mass (g) PH E„ (Ag/AgCI) E h (mV) Sample (mL) Medium Added (mL) Added Water (g) Final Mass (g) 4-Apr 15:00 0.00 250.53 1.57 409 629 8-Apr 12:50 3.91 249.70 1.67 407 627 12-Apr 10:10 7.80 248.08 1.65 505 725 4.74 252.82 15-Apr 10:40 10.82 251.20 1.58 536 756 16-Apr 11:55 11.87 250.58 1.66 560 780 5 5 18-Apr 11:05 13.84 249.12 1.54 573 793 23-Apr 10:05 18.80 247.47 1.53 602 822 3.38 250.85 24-Apr 19:40 20.19 250.34 1.52 609 829 5 5 26-Apr 11:10 21.84 243.44 1.45 623 843 7.32 250.76 29-Apr 10:20 24.81 249.60 1.49 636 856 30-Apr 11:20 25.85 249.26 1.37 628 848 5 5 3-May 10:45 28.82 247.65 1.48 626 846 3.09 250.74 7-May 10:25 32.81 248.97 1.35 621 841 1.80 250.77 10-May 10:20 35,81 249.41 1.40 630 850 Enargite In (g): 2.01 Total Water (g): 20.33 Vol (mL) Mass (g) Flask Weight (g): : • 144.83 Innoculum in: 10 10 Medium in: 95.05 95.05 Total Final Weight (g): 249.41 Filtrate Volume (mL) 101.72 Wash Volume (mL) 250 Solid Residue (g) 1.22 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 179.75 464.20 24.0 1.5 Medium (g/L) 0 0.10 0 0 Samples (mg/L): #1 1050.00 261.00 53.5 1.5 #2 1188.40 1162.80 49.5 3.5 #3 1264.60 1576.15 44.0 6.5 PLS (mg/L) 1306.30 2246.80 229.5 11.0 Wash (mg/L) 13.73 6.84 0.4 Solid Residue (wt % 39 1.0332 14 0.7 . •' :.M-'.S# •>• Weight of Element Copper Iron Arsenic Antimony Head (g) 0.62712 0.23316 0.21105 0.011055 Innoculum (g) 0.0018 0.0046 0.0002 0.0000 Medium (g) 0 0.00955 0 0 Samples (g): #1 0.00525 0.00131 0.000268 0.0000075 #2 0.005942 0.00581 0.000248 0.0000175 #3 0.006323 0.00788 0.00022 0.0000325 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.1329 0.2285 0.0233 0.0011 Wash (g) 0.003433 0.00171 0.0001 0 Solid Residue (g) 0.4758 0.01261 0.1708 0.00854 i. -;«}«isif?,,. ">'!' ':".. •' ••(? •' .-' '. Calculated Head (g) 0.628 0.242 0.195 0.010 % Difference -0.113 -3.862 7.728 12.244 % Extraction ' , -3--Calculated Head 24.21 94.79 12.29 11.97 Measured Head 24.24 98.46 11.34 10.51 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 0.00 103.69 1 11.87 103.74 0.00525 0.00525 0.109 0.107 17.08 17.06 2 20.19 103.50 0.005942 0.01119 0.123 0.126 20.16 20.14 3 25.85 102.42 0.006323 0.01752 0.130 0.139 22.15 22.13 Filtrate 35.81 101.72 0.133 0.149 Wash 250.00 0.003 0.152 24.24 24.21 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 103.69 1 11.87 103.74 0.000802799 0.00080 0.02707614 0.02 9.62 9.26 2 20.19 103.50 0.005311799 0.00611 0.1203498 0.12 49.63 47.78 3 25.85 102.42 0.007378549 0.01349 ' 0.161429283 0.16 67.24 64.74 Filtrate 35.81 101.72 0.2285 0.22 Wash 250.00 0.00171 0.23 96.76 93.17 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 0.00 103.69 1 11.87 103.74 0.0002675 0.00027 0.00555009 0.01 2.52 2.73 2 20.19 103.50 0.0002475 0.00052 0.00512325 0.01 2.44 2.64 3 25.85 102.42 0.00022 0.00074 0.00450648 0.00 2.27 2.46 Filtrate 35.81 101.72 0.02 0.02 Wash 250.00 0.00 0.02 11.34 12.29 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 0.0000 103.69 1 11.87 103.74 0.0000075 0.00001 0.00015561 0.00 1.27 1.45 2 20.19 103.50 0.0000175 0.00003 0.00036225 0.00 3.21 3.66 3 25.85 102.42 0.0000325 0.00006 0.00066573 0.00 6.11 6.97 Filtrate 35.81 101.72 0.00 0.00 Wash 250.00 0.00 0.00 10.51 11.97 Mesophiles, 2 g Enargite, P 8 0 of 15 microns Test XB3-M15 Mesophiles Time Initial Eh Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) Eh (mV) (mL) Added (mL) Water (g) Mass (g) 14-Feb 10:15 0.00 251.60 1.71 430 650 18-Feb 9:20 ' 3.96 249.62 1.69 460 680 2.10 251.72 21-Feb 11:25 7.05 250.20 1.65 517. 737 - 1.23 251.43 22-Feb 10:40 8.02 251.06 1.64 500 720 5 5 26-Feb 9:55 11.99 248.85 1.56 556 776 2.52 251.37 28-Feb 10:10 14.00 250.50 1.56 560 780 5 5 5-Mar 10:25 19.01 248.24 1.45 578 798 3.57 251.81 7-Mar 11:30 21.05 250.79 1.57 645 865 11-Mar 12:35 25.10 248.90 1.48 5.03 253.93 12-Mar 10:30 26.01 253.54 1.64 649 869 5 5 14-Mar 11:00 28.03 252.38 1.43 664 884 15-Mar 12:00 29,07 251.81 1.43 681 901 19-Mar 12:25 33.09 249.60 1.46 674 894 3.43 253.03 21-Mar 20:30 35.43 251.67 1.47 677 897 22-Mar 18:30 36.34 250.76 1.45 675 895 Enargite In (g): Total Water (g): 2.00 17.88 Vol (mL) Mass (g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) 10 95.04 114.82 10 95.04 250.76 103.08 250 1.28 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 191.70 54.85 8.0 1.5 Medium (g/L) 0 0.10044 0 0 Samples (mg/L): #1 956.75 135.25 69.0 1.0 #2 1101.90 309.05 57.0 1.0 #3 1137.00 1044.00 96.5 5.0 PLS (mg/L) 1162.80 1394.05 143.0 7.0 Wash (mg/L) 13.60 7.26 0.2 Solid Residue (wt % 36 3.9606 13 0.7 Weight of Element Copper Iron Arsenic Antimony Head (g) 0.608 0.212 0.21 0.011 Innoculum (g) 0.0019 0.0005 0.0001 0.0000 Medium (g) 0 0.00955 0 0 Samples (g): #1 0.004784 0.00068 0.000345 0.000005 #2 0.00551 0.00155 0.000285 0.000005 #3 0.005685 0.00522 0.000483 0.000025 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.1199 0.1437 0.0147 0.0007 Wash (g) 0.0034 0.00182 0 0.00005 Solid Residue (g) 0.4608 0.0507 0.1664 0.00896 i t . - ' ' -.•' Calculated Head (g) 0.598 0.192 0.182 0.010 % Difference 1.625 9.410 13.251 11.349 % Extraction > - - , ' t • . . . . ' „ . . , ; , ; , -> Calculated Head 22.96 73.60 8.66 8.12 Measured Head 22.59 66.68 7.51 7.20 141 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 0.00 134.78 1 8.02 134.24 0.00478375 0.00478 0.128 0.127 20.81 21.15 2 14.00 133.68 0.0055095 0.01029 0.147 0.150 24.70 25.11 3 26.01 136.72 0.005685 0.01598 0.155 0.164 26.95 27.39 Filtrate 36.34 103.08 0.120 0.134 Wash 250.00 0.003 0.137 22.59 • 22.96 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 134.78 1 8.02 134.24 0.000174049 0.00017 0.018 0.02 8.31 9.17 2 14.00 133.68 0.001043049 0.00122 0.041 0.04 19.23 21.23 3 26.01 136.72 0.004717799 0.00593 0.143 0.14 67.07 74.04 Filtrate 36.34 103.08 0.1437 0.14 Wash 250.00 0.001815 0.14 68.38 75.48 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 0.00 134.78 1 8.02 134.24 0.000345 0.00035 0.00926256 0.01 4.37 5.04 2 14.00 133.68 0.000285 0.00063 0.00761976 0.01 3.75 4.33 3 26.01 136.72 0.0004825 0.00111 0.01319348 0.01 6.54 7.54 Filtrate 36.34 103.08 0.01 0.02 Wash 250.00 0.00 0.02 7.51 8.66 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 0.0000 134.78 1 8.02 134.24 0.000005 0.00001 0.00013424 0.00 1.08 1.22 2 14.00 133.68 0.000005 0.00001 0.00013368 0.00 1.12 1.27 3 26.01 136.72 0.000025 0.00004 0.0006836 0.00 6.17 6.96 Filtrate 36.34 103.08 0.00 0.00 Wash 250.00 0.00 0.00 7.20 8.12 Mesophiles, 2 g Enargite (2), P 8 0 of 15 microns Test #B4-M15 Mesophiles Date Hour Time (days) Initial Mass (g) pH Eh (Ag/AgCI) E„ (mV) Sample (mL) Medium Added (mL) Added Water (g) Final Mass (g) 4-Apr 15:00 0.00 223.85 1.54 411 631 8-Apr 12:50 3.91 222.49 1.73 400 620 1.88 224.37 12-Apr 10:10 7.80 223.19 1.70 518 738 15-Apr 10:40 10.82 222.22 1.62 555 775 16-Apr 11:55 11.87 221.68 1.62 574 794 5 5 18-Apr 11:05 13.84 220.30 1.65 591 811 4.05 224.35 23-Apr 10:05 18.80 222.91 1.49 577 797 1.00 223.91 24-Apr 19:40 20.19 223.49 1.51 586 806 5 5 26-Apr 11:10 21.84 222.74 1.59 624 844 1.27 224.01 29-Apr 10:20 24.81 223.04 1.48 627 847 30-Apr 11:20 25.85 222.81 1.46 638 858 5 5 3-May 10:45 28.82 221.75 1.66 634 854 2.49 224.24 7-May 10:25 32.81 223.24 1.47 628 848 10-May 10:20 35.81 222.16 1.43 620 840 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 Total Final Weight (g):r: > . 222.16 Filtrate Volume (mL) 102.53 »¥'3<f|:;; Wash Volume (mL) 250 \. . " Solid Residue (g) 1.25 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 179.75 464.20 24.0 1.5 Medium (g/L) 0 0.10044 0 0 Samples (mg/L): #1 1044.10 355.20 28.5 0.0 #2 1108.05 1017.55 30.5 3.0 #3 1094.10 1366.75 37.5 5.5 PLS (mg/L) 1090.65 1912.80 154.0 7.5 Wash (mg/L) 11.50 8.47 0.3 Solid Residue (wt % 39 0.9482 14 0.7 ; , -L* ' i~ - ' •fe . - °j" ...,^ Weight of Element Copper Iron Arsenic Antimony Head (g) 0.608 0.212 0.21 0.011 Innoculum (g) 0.0018 0.0046 0.0002 0.0000 Medium (g) 0 0.00955 0 0 Samples (g): #1 0.005221 0.00178 0.000143 0 #2 0.00554 0.00509 0.000153 0.000015 #3 0.005471 0.00683 0.000188 0.0000275 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.1118 0.1961 0.0158 0.0008 Wash (g) 0.002875 0.00212 0.000075 0 Solid Residue (g) 0.4875 0.01185 0.175 0.00875 '••Mtf'T-j*',., •> Calculated Head (g) 0.617 0.208 0.191 0.010 % Difference -1.420 1.847 8.997 13.214 % Extraction Calculated Head 20.94 94.30 8.43 8.34 Measured Head 21.24 92.56 7.67 7.24 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 0.00 104.97 1 11.87 102.80 0.0052205 0.00522 0.107 0.106 17.36 17.11 2 20.19 104.61 0.00554025 0.01076 0.116 0.119 19.63 19.35 3 25.85 103.93 0.0054705 0.01623 0.114 0.123 20.18 19.89 Filtrate 35.81 102.53 0.112 0.126 Wash 250.00 0.003 0.129 21.24 20.94 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot: Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 104.97 1 11.87 102.80 0.001273799 0.00127 0.037 0.03 15.03 15.32 2 20.19 104.61 0.004585549 0.00586 0.106 0.10 48.02 48.92 3 25.85 103.93 0.006331549 0.01219 0.142 0.14 64.81 66.03 Filtrate 35.81 102.53 0.1961 0.19 Wash 250.00 0.0021175 0.19 91.32 93.04 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 0.00 104.97 1 11.87 102.80 0.0001425 0.00014 0.0029298 0.00 1.28 1.41 2 20.19 104.61 0.0001525 0.00030 0.003190605 0.00 1.47 1.62 3 25.85 103.93 0.0001875 0.00048 0.003897375 0.00 1.88 2.07 Filtrate 35.81 102.53 0.02 0.02 Wash 250.00 0.00 0.02 7.67 8.43 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 0.0000 104.97 1 11.87 102.80 0 0.00000 0 0.00 -0.14 -0.16 2 20.19 104.61 0.000015 0.00002 0.00031383 0.00 2.72 3.13 3 25.85 103.93 0.0000275 0.00004 0.000571615 0.00 5.20 5.99 Filtrate 35.81 102.53 0.00 0.00 Wash 250.00 0.00 0.00 7.24 8.34 Mesophiles, 2 g Enargite, P 8 0 of 37 microns Test #B3-M37 Mesophiles Time Initial E,, Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 14-Feb 10:15 0.00 244.30 1.74 467 687 18-Feb 9:20 3.96 242.18 1.63 472 692 1.99 244.17 21-Feb 11:25 7.05 242.52 1.58 525 745 2.80 245.32 22-Feb 10:40 8.02 244.94 1.60 533 753 • 5 5 26-Feb 9:55 11.99 242.57 1:51 541 761 2.00 244.57 28-Feb 10:10 14.00 243.61 1.52 . 580 800 5 5 5-Mar 10:40 19.02 241.44 1.44' 640 860 3.07 244.51 7-Mar 11:30 21.05 241.32 1.52 645 865 11-Mar 12:35 25.10 241.40 1.46 3.25 244.65 12-Mar 10:30 26.01 244.29 1.52 654 874 5 5 14-Mar 11:00 28.03 243.34 1.53 661 881 1.18 244.52 15-Mar 12:00 29.07 243.95 1.39 685 905 19-Mar 12:25 33.09 242.09 1.45 659 879 2.57 244.66 21-Mar 20:30 35.43 243.06 1.44 670 890 22-Mar 18:30 36.34 242.41 1.42 670 890 Enargite In (g): 2.01 Total Water (g): 16.86 Vol (mL) Mass (g) Flask Weight (g): 137.36 Innoculum in: 10 10 Medium in: 95.06 95.06 Total Final Weight (g): • • 242.41 Filtrate Volume (mL) 95.33 Wash Volume (mL) 250 Solid Residue (g) 1.48 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 191.70 54.85 8.0 1.5 Medium (g/L) 0 0.10044 0 0 Samples (mg/L): #1 641.85 136.95 80.5 1.0 #2 760.10 328.80 68.0 1.5 #3 820.90 765.00 93.5 3.0 PLS (mg/L) 905.15 1126.45 175.5 6.0 Wash (mg/L) 7.57 5.63 0.9 Solid Residue (wt % 35 2.2498 13 0.4 Weight of Element Copper Iron Arsenic Antimony Head (g) 0.65124 0.14472 0.2412 0.007839 Innoculum (g) 0.0019 0.0005 0.0001 o.ooOo Medium (g) 0 0.00955 0 0 Samples (g): #1 0.003209 0.00068 0.000403 0.000005 #2 0.003801 0.00164 0.00034 0.0000075 #3 0.004105 0.00383 0.000468 0.000015 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.0863 0.1074 0.0167 0.0006 Wash (g) 0.001893 0.00141 0.000225 0 Solid Residue (g) 0.518 0.0333 0.1924 0.00592 Calculated Head (g) 0.615 0.137 0.210 0.007 % Difference 5.507 5.583 12.734 17.024 % Extraction Calculated Head 15.82 75.63 8.59 8.99 Measured Head 14.95 71.41 7.50 7.46 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 0.00 104.93 1 8.02 105.57 0.00320925 0.00321 . 0.068 0.066 10.11 10.70 2 14.00 104.24 0.0038005 0.00701 0.079 0.081 •12.36 13.09 3 26.01 104.92 0.0041045 0.01111 0.086 0.091 14.01 14.82 Filtrate 36.34 95.33 0.086 0.095 Wash 250.00 0.002 0.097 14.95 15.82 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 104.93 1 8.02 105.57 0.000182549 0.00018 0.014457812 0.01 9.61 10.18 2 14.00 104.24 0.001141799 0.00132 0.034274112 0.03 23.30 24.68 3 26.01 104.92 0.003322799 0.00465 0.0802638 0.08 55.08 58.34 Filtrate 36.34 95.33 0.1074 0.11 Wash 250.00 0.0014075 0.11 74.80 79.22 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 0.00 104.93 1 8.02 105.57 0.0004025 0.00040 0.008498385 0.01 3.49 4.00 2 14.00 104.24 0.00034 0.00074 0.00708832 0.01 3.07 3.52 3 26.01 104.92 0.0004675 0.00121 0.00981002 0.01 4.34 4.98 Filtrate 36.34 95.33 0.02 0.02 Wash 250.00 0.00 0.02 7.50 8.59 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 0.0000 104.93 1 8.02 105.57 0.000005 0.00001 0.00010557 0.00 1.16 1.39 2 14.00 104.24 0.0000075 0.00001 0.00015636 0.00 1.87 2.25 3 26.01 104.92 0.000015 0.00003 0.00031476 0.00 3.98 4.80 Filtrate 36.34 95.33 0.00 0.00 Wash 250.00 0.00 0.00 7.46 8.99 Mesophiles, 2 g Enargite (2), P 8 0 of 37 microns Test UB4-M37 Mesophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) Eh (mV) (mL) Added (mL) Water (g) Mass (g) 4-Apr 15:00 0.00 236.23 1.54 412 632 8-Apr 12:50 3.91 234.55 1.73 395 615 4.69 239.24 12-Apr 10:10 7.80 237.25 1.72 527 747 15-Apr 10:40 10.82 236.03 1.63 564 784 16-Apr 11:55 11.87 235.60 1.63 577 797 5 5 18-Apr 11:05 13.84 234.24 1.62 594 814 3.22 237.46 23-Apr 10:05 18.80 235.51 1.50 600 820 1.15 236.66 24-Apr 19:40 20.19 236.16 1.52 596 816 5 5 26-Apr 11:10 21.84 235.68 1.57 620 840 0.57 236.25 29-Apr 10:20 24.81 235.34 1.50 634 854 30-Apr 11:20 25.85 234.96 1.47 637 857 5 5 3-May 10:45 28.82 233.70 1.58 636 856 3.49 237.19 7-May 10:25 32.81 235.49 1.44 628 848 10-May 10:20 35.81 234.24 1.44 626 846 Enargite In (g): 2.00 Total Water (g): 13.12 Vol (mL) Mass (g) Flask Weight (g): 129.13 Innoculum in: 10 10 Medium in: 95.11 95.11 Total Final Weight (g): • . . 234.24 Filtrate Volume (mL) 102.69 Wash Volume (mL) 250 Solid Residue (g) 1.29 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 179.75 464.20 24.0 1.5 Medium (g/L) 0 0.10044 0 0 Samples (mg/L): #1 972.10 314.50 24.5 1.0 #2 1007.10 891.90 52.5 3.0 #3 1098.85 1137.55 30.5 4.5 PLS (mg/L) 1182.50 1769.70 139.5 8.5 Wash (mg/L) 11.13 4.32 Solid Residue (wt % 36 2.5608 13 0.7 Weight of Element Copper Iron Arsenic Antimony Head (g) 0.648 0.144 0.24 0.0078 Innoculum (g) 0.0018 0.0046 0.0002 0.0000 Medium (g) 0 0.00955 0 0 Samples (g): #1 0.004861 0.00157 0.000123 0.000005 #2 0.005036 0.00446 0.000263 0.000015 #3 0.005494 0.00569 0.000153 0.0000225 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.1214 0.1817 0.0143 0.0009 Wash (g) 0.002783 0.00108 0 0 Solid Residue (g) 0.4644 0.03303 0.1677 0.00903 • . '.•.„• . ' n ... ' - V , ; ' .> , t SIA ... : .- • Calculated Head (g) 0.602 0.212 0.182 0.010 % Difference 7.067 -47.127 24.032 -27.312 % Extraction •i',''".' ;„"?' v c v • -vf ' i Calculated Head 22.88 . 84.41 8.02 9.07 Measured Head 21.27 124.19 6.09 11.54 Copper Output Tot. Cu Sample # Time (days) Sol'n Vol. (n iL) g Cu sampled Sampled (g) Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.00 105.10 1 11.87 104.47 0.0048605 0.00486 0.102 0.100 15.39 16.57 2 20.19 105.03 0.0050355 0.00990 0.106 0.109 16.80 18.07 3 25.85 103.83 0.00549425 0.01539 0.114 0.122 18.86 20.29 Filtrate 35.81 102.69 0.121 0.135 Wash 250.00 0.003 0.138 21.27 22.88 Iron Output Sample # Time (days) Sol'n Vol. (n »-) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.10 1 11.87 104.47 0.001070299 0.00107 0.032855815 0.03 19.59 13.32 2 20.19 105.03 0.003957299 0.00503 0.093676257 0.09 61.83 42.02 3 25.85 103.83 0.005185549 0.01021 0.118111817 0.11 78.80 53.56 Filtrate 35.81 102.69 0.1817 0.18 Wash 250.00 0.00108 0.18 123.73 84.10 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 0.00 105.10 1 11.87 104.47 0.0001225 0.00012 0.002559515 0.00 0.97 1.27 2 20.19 105.03 0.0002625 0.00039 0.005514075 0.01 2.25 2.96 3 25.85 103.83 0.0001525 0.00054 0.003166815 0.00 1.38 1.82 Filtrate 35.81 102.69 0.01 0.01 Wash 250.00 0.00 0.01 6.09 8.02 Antimony Output Sample # Time (days) Sol'n Vol. (n iL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) Sb(aq) total %Sb indicated %Sb actual 0.0000 105.10 1 11.87 104.47 0.000005 0.00001 0.00010447 0.00 1.15 0.90 2 20.19 105.03 0.000015 0.00002 0.00031509 0.00 3.91 3.07 3 25.85 103.83 0.0000225 0.00004 0.000467235 0.00 6.05 4.76 Filtrate 35.81 102.69 0.00 0.00 Wash 250.00 0.00 0.00 11.54 9.07 Mesophiles, 3.5 g Enargite, P 8 0 of 10 microns Test UB6-M10 Mesophiles Date Hour Time (days) Initial Mass (g) PH E„ (Ag/AgCI) E„ (mV) Sample (mL) Medium Ad d e d A d d e d (mL) Water (g) Final M a ss (g) 21-May 12:00 0.00 224.15 1.57 404 624 24-May 10:20 2.93 223.39 1.67 385 605 1.62 225.01 27-May 10:25 5.93 224.39 1.78 488 708 28-May 13:40 7.07 223.96 1.93 518 738 5 5 30-May 10:30 8.94 223.32 1.76 535 755 3.87 227.19 3-Jun 12:35 13.02 226.31 1.74 564 784 7-Jun 10:25 16.93 225.26 1.62 604 824 10-Jun 11:00 19.96 224.62 1.54 575 795 5 5 13-Jun 11:20. . 22.97 223.70 1.44 627 847. 17-Jun 10:05 26.92 221.97 1.32 639 859 3.74 225.71 18-Jun 11:10 27.97 225.53 1.31 625 845 5 5 20-Jun 12:00 30.00 224.98 1.21 640 860 24-Jun 11:15 33.97 223.32 1.23 635 855 1.92 225.24 26-Jun 11:45 35.99 224.42 1.27 641 861 Enargite In (g): 3.50 Total Water (g): 11.15 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) 2.14 A n a l y s i s Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 169.25 444.10 24.5 1.0 Medium (g/L) 0 0.10 0 0 Samples (mg/L): #1 1345.00 158.85 81.0 0.5 #2 1925.65 1388.75 151.5 3.5 #3 2118.35 3692.80 402.0 20.0 PLS (mg/L) 2365.90 3245.00 459.5 Wash (mg/L) 27.51 20.88 0.4 Solid Residue (wt %) 38 0.6639 14 0.7 ' f . - . ' .'• • ,• "• '• ' . ''.'-v." Weight of Element Copper Iron Arsenic Antimony Head (g) 1.092 0.406 0.3675 0.01925 Innoculum (g) 0.0017 0.0044 0.0002 0.0000 Medium (g) 0 0.009543 0 0 Samples (g): #1 0.006725 0.000794 0.000405 0.0000025 #2 0.0096283 0.006944 0.000758 0.0000175 #3 0.0105918 0.018464 0.00201 0.0001 Medium Added (g): #1 0 0.000502 0 0 #2 0 0.000502 0 0 #3 0 0.000502 0 0 PLS (g) 0.2469 0.3387 0.0480 0.0000 Wash (g) 0.0068775 0.00522 0.0001 0 Solid Residue (g) 0.8132 0.014207 0.2996 0.01498 ':;*''«i«if.{-Calculated Head (g) 1.092 0.369 0.351 0.015 % Difference -0.024 9.158 4.603 21.610 % Extraction • *:,3r"\ " • • i j - , - . : - * * S f . . Calculated Head 25.55 96.15 14.54 0.73 Measured Head 25.55 87.34 13.87 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 0.00 104.88 1 7.07 104.69 0.006725 0.00673 0.141 0.139 12.74 12.74 2 19.96 105.35 0.00962825 0.01635 0.203 0.208 19.04 19.03 3 27.97 106.26 0.01059175 0.02695 0.225 0.240 21.96 21.95 Filtrate 35.99 104.37 0.247 0.272 Wash 250.00 0.007 0.279 25.55. 25.55 Iron Output Sample # Time (days) Sol'n Vol. (IT g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 104.88 1 7.07 104.69 0.000292049 0.00029 0.016630007. 0.01 3.00 3.30 2 19.96 105.35 0.006441549 0.00673 0.146304813 0.14 34.94 38.46 3 27.97 106.26 0.017961799 0.02470 0.392396928 0.39 95.56 105.19 Filtrate 35.99 104.37 0.3387 0.33 Wash 250.00 0.00522 0.34 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 %As indicated %As actual 0.00 104.88 1 7.07 104.69 0.000405 0.00041 0.00847989 0.01 2.24 2.35 2 19.96 105.35 0.0007575 0.00116 0.015960525 0.02 4.39 4.60 3 27.97 106.26 0.00201 0.00317 0.04271652 0.04 11.87 12.45 Filtrate 35.99 104.37 0.05 0.05 Wash 250.00 0.00 0.05 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 0.0000 104.88 1 8.94 104.05 0.0000025 0.00000 0.000052025 0.00 0.22 0.28 2 19.96 105.35 0.0000175 0.00002 0.000368725 0.00 1.88 2.39 3 27.97 106.26 0.0001 0.00012 0.0021252 0.00 11.09 14.15 Filtrate 35.99 104.37 0.00 0.00 Wash 250.00 0.00 0.00 0.57 0.73 Mesophiles, 3.5 g Enargite, P 8 0 of 15 microns Test #B6-M15 Mesophiles Time Initial E h Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) Eh (mV) (mL) Added (mL) Water (g) Mass (g) 21-May 12:00 0.00 225.10 1.55 324 544 24-May 10:20 2.93 224.33 1.70 . 369 589 0.97 225.30 27-May 10:25 5.93 224.45 1.84 465 685 0.81 225.26 28-May 13:40 7.07 224.98 1.98 521 741 5 5 30-May 10:30 8.94 224.37 1.84 546 766 1.01 225.38 3-Jun 12:35 13.02 224.46 1.72 556 776 7-Jun 10:25 16.93 223.59 1.71 583 803 2.34 225.93 10-Jun 11:00 19.96 225.02 1.61 587 807 5 5 13-Jun 11:20 22.97 224.40 1.55 624 844 1.12 225.52 17-Jun 10:05 26.92 224.18 1.41 632 852 2.24 226.42 18-Jun 11:10 27,97 226.00 1.36 631 851 5 5 20-Jun 12:00 30.00 225.30 1.31 645 865 24-Jun 11:15 33.97 223.92 1.29 642 862 3.14 227.06 26-Jun 11:45 35.99 226.28 1.31 645 865 Enargite In (g): 3.50 Total Water (g): 11,63 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. Wash Volume (mL) 250 . / e £ Solid Residue (g) "I' "::; 2.12 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 169.25 444.10 24.5 1.0 Medium (g/L) 0 0.10044 0 0 Samples (mg/L): #1 1317.75 144.40 63.0 1.0 #2 1820.25 1167.00 109.0 4.0 #3 2022.60 3264.20 268.0 14.0 PLS (mg/L) 2258.90 3123.75 307.0 Wash (mg/L) 27.99 17.62 0.0 Solid Residue (wt %) 39 0.5207 14 0.7 Weight of Element Copper Iron Arsenic Antimony Head (g) 1.064 0.371 0.3675 0.01925 Innoculum (g) 0.0017 0.0044 0.0002 0.0000 Medium (g) 0 0.00955 0 0 Samples (g): #1 0.0065888 0.00072 0.000315 0.000005 #2 0.0091013 0.00584 0.000545 0.00002 #3 0.010113 0.01632 0.00134 0.00007 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.2358 0.3261 0.0321 0.0000 Wash (g) 0.0069975 0.00441 0 0 Solid Residue (g) 0.8268 0.01104 0.2968 0.01484 • Calculated Head (g) 1.094 0.349 0.331 0.015 % Difference -2.795 5.946 9.985 22.468 % Extraction Calculated Head 24.41 96.84 10.28 0.57 Measured Head 25.09 91.08 9.25 0.44 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 0.00 105.10 1 7.07 104.98 0.00658875 0.00659 0.138 0.137 12.84 12.49 2 19.96 105.02 0.00910125 0.01569 0.191 0.196 18.43 17.93 3 27.97 106.00 0.010113 0.02580 0.214 0.228 21.47 20.88 Filtrate 35.99 104.40 0.236 0.260 Wash 250.00 0.007 0.267 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 %Fe indicated %Fe actual 0.00 105.10 1 7.07 104.98 0.000219799 0.00022 0.015 0.01 2.89 3.07 2 19.96 105.02 0.005332799 0.00555 0.123 0.12 31.84 33.85 3 27.97 106.00 0.015818799 0.02137 0.346 0.34 92.07 97.89 Filtrate 35.99 104.40 0.3261 0.32 Wash 250.00 0.004405 0:33 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 0.00 105.10 1 7.07 104.98 0.000315 0.00032 0.00661374 0.01 1.73 1.93 2 19.96 105.02 0.000545 0.00086 0.01144718.' 0.01 3.13 3.48 3 27.97 106.00 0.00134 0.00220 0.028408 0.03 7.90 8.77 Filtrate 35.99 104.40 0.03 0.03 Wash 250.00 0.00 0.03 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 0.0000 105.10 1 8.94 104.37 0.000005 0.00001 0.00010437 0.00 0.49 0.63 2 19.96 105.02 0.00002 0.00003 0.00042008 0.00 2.16 2.78 3 27.97 106.00 0.00007 0.00010 0.001484 0.00 7.79 10.04 Filtrate 35.99 104.40 0.00 0.00 Wash 250.00 0.00 0.00 0.44 0.57 Mesophiles, 3.5 g Enargite, P 8 0 of 37 microns Test #B6-M37 Mesophiles Date Hour Time (days) Initial Mass (g) PH E„ (Ag/AgCI) E„ (mV) Sample (mL) Medium Added Added (mL) Water (g) Final Mass (g) 21-May 12:00 0.00 254.20 1.54 385 605 24-May 10:20 2.93 253.20 1.59 382 602 1.51 254.71 27-May 10:25 5.93 253.77 1.71 458 678 0.58 254.35 28-May 13:40 7.07 254.04 1.89 505 725 5 5 30-May 10:30 8.94 253.34 1.69 529 749 1.02 254.36 3-Jun 12:35 13.02 253.01 1.67 567 787 7-Jun 10:25 16.93 251.49 1.60 582 802 3.01 254.50 10-Jun 11:00 19.96 253.53 1.58 592 812 5 5 13-Jun 11:20 22.97 252.26 1.56 615 835 2.27 254.53 17-Jun 10:05 26.92 252.61 1.45 629 849 3.00 255.61 18-Jun 11:10 27.97 255.13 1.39 626 846 5 5 20-Jun 12:00 30.00 254.28 1.32 636 856 24-Jun 11:15 33.97 252.41 1.32 640 860 2.94 255.35 26-Jun 11:45 35.99 254.30 1.34 641 861 Enargite In (g): Total Water (g): 3.51 14.33 Vol(mL) Mass(g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) 145.92 10 10 95.05 95.05 I 254.30 103.39 250 •• - j 2.71 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 169.25 444.10 24.5 1.0 Medium (g/L) 0 0.10044 0 0 Samples (mg/L): #1 872.10 135.60 79.5 1.0 #2 1306.55 630.65 79.5 0.5 #3 1466.55 1671.60 199.0 5.0 PLS (mg/L) 1592.90 2112.35 284.5 Wash (mg/L) 17.13 6.44 0.0 Solid Residue (wt %) 36 1.2374 13 0.4 . •• ; ' :<:•.-?.-.• -Weight of Element Copper Iron Arsenic Antimony Head (g) 1.13724 0.25272 0.4212 0.013689 Innoculum (g) 0.0017 0.0044 0.0002 0.0000 Medium (g) 0 0.00955 0 0 Samples (g): #1 0.0043605 0.00068 0.000398 0.000005 #2 0.0065328 0.00315 0.000398 0.0000025 #3 0.0073328 0.00836 0.000995 0.000025 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.1647 0.2184 0.0294 0.0000 Wash (g) 0.0042825 0.00161 0 0 Solid Residue (g) 0.9756 0.03353 0.3523 0.01084 . . . . '.'wvv '. ;;>';i"'&:.. /,'„ ; i X * & A . !' .. :>',•"< Calculated Head (g) 1.161 0.250 0.383 0.011 % Difference -2.099 0.984 9.008 20.648 % Extraction Calculated Head 15.98 86.60 8.08 0.21 Measured Head 16.31 85.75 7.35 0.16 Copper Output Tot. Cu Sample # Time (days) Sorn Vol. (mL) g Cu sampled Sampled (g) Cu In sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.00 104.77 1 7.07 104.61 0.0043605 0.00436 0.091 0.090 7.87 7.71 2 19.96 104.10 0.00653275 0.01089 0.136 0.139 12.19 11.94 3 27.97 105.70 0.00733275 0.01823 0.155 0.164 14.44 14.14 Filtrate 35.99 103.39 0.165 0.181 Wash 250.00 0.004 0.186 16.31 15.98 Iron Output " . Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 104.77 1 7.07 104.61 0.000175799 0.00018 0.014185116 0.01 3.86 3.89 2 19.96 104.10 0.002651049 0.00283 0.065650665 0.06 24.22 24.46 3 27.97 105.70 0.007855799 0.01068 0.17668812 0.17 68.16 68.83 Filtrate 35.99 103.39 0.2184 0.21 Wash 250.00 0.00161 0.22 85.30 86.15 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 0.00 104.77 1 7.07 104.61 0.0003975 0.00040 0.008316495 0.01 1.92 2.11 2 19.96 104.10 0.0003975 0.00080 0.00827595 0.01 2.00 2.20 3 27.97 105.70 0.000995 0.00179 0.0210343 0.02 5.12 5.63 Filtrate 35.99 103.39 0.03 0.03 Wash 250.00 0.00 0.03 7.35 8.08 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 0.0000 104.77 1 7.07 104.61 0.000005 0.00001 0.00010461 0.00 0.69 0.87 2 19.96 104.10 0.0000025 0.00001 0.00005205 0.00 0.34 0.43 3 27.97 105.70 0.000025 0.00003 0.0005285 0.00 3.84 4.84 Filtrate 35.99 103.39 0.00 0.00 Wash 250.00 0.00 0.00 0.16 0.21 Mesophiles, 5 g Enargite, P 8 0 of 10 microns Test #B5-M10 Mesophiles Date Hour Time (days) Initial Mass (g) PH Eh (Ag/AgCI) Eh (mV) Sample (mL) Medium Added Added (mL) Water (g) Final Mass (g) 11-Apr 15:50 0.00 243.65 1.59 365 585 15-Apr 10:45 3.79 242.16 1.81 398 618 18-Apr 11:10 6.81 240.60 1.73 505 725 3.31 243.91 19-Apr 11:05 7.80 243.53 1.81 509 729 5 5 23-Apr 10:10 11.76 241.61 1.55 552 772 2.35 243.96 24-Apr 19:50 13.17 243.53 1.57 524 744 5 5 26-Apr 11:20 14.81 242.86 1.61 538 758 1.30 244.16 29-Apr 10:25 17.77 243.10 1.50 542 762 30-Apr 11:20 18.81 242.56 1.45 546 766 5 5 3-May 10:50 21.79 241.16 1.46 534 754 2.87 244.03 7-May 10:25 25.77 242.39 1.39 575 795 1.60 243.99 10-May 10:45 28.79 242.59 1.40 609 829 5 5 1.44 244.03 14-May 11:20 32.81 242.56 1.34 630 850 1.31 243.87 16-May 10:30 34.78 243.32 1.26 637 857 17-May 11:15 35.81 242.66 1.27 647 867 Enargite In (g): 5.01 Total Water (g): 14.18 Vol (mL) Mass (g) Flask Weight (g): •  '•' i"*l*">< 133.91 Innoculum in: 10 10 Medium in: 95.04 95.04 Total Final Weight (g): ,s; j . . . 242.66 Filtrate Volume (mL) 102.76 Wash Volume (mL) 250 •~ . . ' ^ Solid Residue (g) 3.56 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 178.60 489.60 28.5 2.5 Medium (g/L) 0 0.10 0 0 Samples (mg/L): #1 2351.20 124.00 140.5 #2 2652.30 380.00 94.5 0.5 #3 2711.95 741.45 91.5 1.0 #4 2734.95 1466.80 49.5 4.5 PLS (mg/L) 3366.10 3220.95 519.5 Wash (mg/L) 42.57 19.68 0.3 Solid Residue (wt"/ 35 6.3 13 0.6 H l f e ; • " l i f e Weight of Element Copper Iron Arsenic Antimony Head (g) 1.56312 0.58116 0.52605 0.027555 Innoculum (g) 0.0018 0.0049 0.0003 0.0000 Medium (g) 0 0.00955 0 0 Samples (g): #1 0.011756 0.00062 0.000703 0 #2 0.013262 0.0019 0.000473 0.0000025 #3 0.01356 0.00371 0.000458 0.000005 #4 0.013675 0.00733 0.000248 0.0000225 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.3459 0.3310 0.0534 0.0000 Wash (g) 0.010643 0.00492 0.000075 0 Solid Residue (g) 1.246 0.22428 0.4628 0.02136 . - - . V - i i s . - •. • . ! . ' " * . - . - * « . : ! # Calculated Head (g 1.639 0.550 0.518 0.021 % Difference -4.876 5.282 1.605 22.546 % Extraction . . . • •' 4 i - •• Calculated Head 23.99 59.26 10.59 -0.08 Measured Head 25.16 56.13 10.42 -0.06 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 0.00 104.73 1 7.80 104.61 0.011756 0.01176 0.246 0.244 15.62 14.89 2 13.17 104.61 0.0132615 0.02502 0.277 0.287 18.39 17.53 3 18.81 102.24 0.01355975 0.03858 0.277 0.301 19.22 18.33 4 28.79 102.24 0.01367475 0.05225 0.280 0.316 20.24 19.30 Filtrate 35.81 102.76 0.346 0.383 Wash 250.00 0.011 0.393 25.16 23.99 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 104.73 1 7.80 104.61 0.000117799 0.00012 0.01297164 0.01 1.39 1.47 2 13.17 104.61 0.001397799 0.00152 0.0397518 0.03 6.00 6.33 3 18.81 102.24 0.003205049 0.00472 0.075805848 0.07 12.20 12.88 4 28.79 103.47 -0.323650822 -0.31893 0.151769796 0.15 25.27 26.68 Filtrate 35.81 102.76 0.3310 0.33 Wash 250.00 0.00492 0.33 56.96 60.13 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 0.00 104.73 1 7.80 104.61 0.0007025 0.00070 0.014697705 0.01 2.74 2.78 2 13.17 104.61 0.0004725 0.00118 0.009885645 0.01 1.96 1.99 3 18.81 102.24 0.0004575 0.00163 0.00935496 0.01 1.95 1.98 4 28.79 102.24 0.0002475 0.00188 0.00506088 0.01 1.22 1.24 Filtrate 35.81 102.76 0.05 0.05 Wash 250.00 0.00 0.05 10.42 10.59 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 0.0000 104.73 1 7.80 104.61 0 0.00000 0 0.00 -0.09 -0.12 2 13.17 104.61 0.0000025 0.00000 0.000052305 0.00 0.10 0.13 3 18.81 102.24 0.000005 0.00001 0.00010224 0.00 0.29 0.37 4 28.79 102.24 0.0000225 0.00003 0.00046008 0.00 1.61 2.07 Filtrate 35.81 102.76 0.00 0.00 Wash 250.00 0.00 0.00 -0.06 -0.08 Mesophiles, 5 g Enargite, P 8 0 of 15 microns Test UB5-M15 Mesophiles Time Initial E h Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E h(mV) (mL) Added (mL) Water (g) Mass (g) 11-Apr 15:50 0.00 225.49 1.58 367 587 15-Apr 10:45 3.79 224.35 1.92 404 624 18-Apr 11:10 6.81 223.33 1.85 532 752 3.19 226.52 19-Apr 11:05 7.80 226.27 1.83 539 759 5 5 23-Apr 10:10 11.76 225.30 1.60 563 783 24-Apr 19:50 13.17 225.01 1.66 558 778 5 5 26-Apr 11:20 14.81 224.69 1.61 571 791 0.62 225.31 29-Apr 10:25 17.77 224.43 1.59 569 789 30-Apr 11:20 18.81 224.19 1.50 584 804 5 5 3-May 10:50 21.79 222.59 1.58 569 789 3.18 225.77 7-May 10:25 25.77 224.97 1.47 629 849 10-May 10:45 28.79 224.12 1.38 639 859 5 5 1.61 225.73 14-May 11:20 32.81 224.65 1.30 629 849 1.00 225.65 16-May 10:30 34.78 224.99 1.25 638 858 0.55 225.54 17-May 11:15 35.81 224.82 1.25 639 859 Enargite In (g): 4.99 Total Water (g): 10,15 Vol (mL) Mass (g) Flask Weight (g): ' „ * ^ ' , . 115.83 Innoculum in: 10 10 Medium in: 95.04 95.04 Total Final Weight (g): 224.82 Filtrate Volume (mL) 101.39 •, , " '''}• Wash Volume (mL) 250 • "3 Solid Residue (g) S3 3.24 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 178.60 489.60 28.5 2.5 Medium (g/L) 0 0.10044 0 0 Samples (mg/L): #1 2224.65 230.50 31.0 0.5 #2 2393.10 812.00 51.0 2.0 #3 2617.85 1235.65 50.5 4.0 #4 2559.45 2870.20 139.5 12.0 PLS (mg/L) 2868.45 4126.75 405.0 21.5 Wash (mg/L) 41.75 51.65 1.4 0.3 Solid Residue (wt °/ 39 1.9084 14 0.7 Weight of Element Copper Iron Arsenic Antimony Head (g) 1.51696 0.52894 0.52395 0.027445 Innoculum (g) 0.0018 0.0049 0.0003 0.0000 Medium (g) 0 0.00955 0 0 Samples (g): #1 0.011123 0.00115 0.000155 0.0000025 #2 0.011966 0.00406 0.000255 0.00001 #3 0.013089 0.00618 0.000253 0.00002 #4 0.012797 0.01435 0.000698 0.00006 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.2908 0.4184 0.0411 0.0022 Wash (g) 0.010438 0.01291 0.00035 0.000075 Solid Residue (g) 1.2636 0.06183 0.4536 0.02268 <s?'V" ^vfsc? . ; :K<~ '• Calculated Head (g 1.599 0.489 0.495 0.025 % Difference -5.425 7.627 5.451 9.119 % Extraction .~H.'. :.-. . • ~4-~ i • Calculated Head 20.99 87.34 8.44 9.07 Measured Head 22.13 80.68 7.98 8.24 157 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 0.00 104.67 1 7.80 105.45 0.01112325 0.01112 0.235 0.233 15.35 14.56 2 13.17 104.19 0.0119655 0.02309 0.249 0.259 17.05 16.17 3 18.81 101.77 0.01308925 0.03618 0.266 0.288 18.97 17.99 4 28.79 101.77 0.01279725 0.04898 0.260 0.295 19.44 18.44 Filtrate 35.81 101.39 0.291 0.325 Wash 250.00 0.010 0.336 22.13 20.99 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 104.67 1 7.80 105.45 0.000650299 0.00065 0.024 0.02 3.67 3.97 2 13.17 104.19 0.003557799 0.00421 0.085 0.08 15.07 16.31 3 18.81 101.77 0.005676049 0.00988 0.126 0.12 22.85 24.74 4 28.79 104.15 -0.404060183 -0.39418 0.299 0.29 55.59 60.18 Filtrate 35.81 101.39 0.4184 0.41 Wash 250.00 0.0129125 0.43 80.62 87.28 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 0.00 104.67 1 7.80 105.45 0.000155 0.00016 0.00326895 0.00 0.57 0.60 2 13.17 104.19 0.000255 0.00041 0.00531369 0.01 0.99 1.05 3 18.81 101.77 0.0002525 0.00066 0.005139385 0.01 1.00 1.06 4 28.79 101.77 0.0006975 0.00136 0.014196915 0.01 2.78 2.94 Filtrate 35.81 101.39 0.04 0.04 Wash 250.00 0.00 0.04 7.98 8.44 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 0.0000 104.67 1 7.80 105.45 0.0000025 0.00000 0.000052725 0.00 0.10 0.11 2 13.17 104.19 0.00001 0.00001 0.00020838 0.00 0.68 0.75 3 18.81 101.77 0.00002 0.00003 0.00040708 0.00 1.44 1.58 4 28.79 101.77 0.00006 0.00009 0.00122124 0.00 4.48 4.93 Filtrate 35.81 101.39 0.00 0.00 W a s h 250.00 0.00 0.00 8.24 9.07 Mesophiles, 5 g Enargite, P 8 0 of 37 microns Test #BS-M37 Mesophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E h(mV) (mL) Added (mL) Water (g) Mass (g) 11-Apr 15:50 0.00 256.08 1.60 367 587 15-Apr 10:45 3.79 254.49 1.84 404 624 18-Apr 11:10 6.81 253.12 1.73 508 728 3.10 256.22 19-Apr 11:05 7.80 255.73 1.74 526 746 5 5 23-Apr 10:10 11.76 254.94 1.55 540 760 2.46 257.40 24-Apr 19:50 13.17 256.91 1.56 531 751 5 5 26-Apr 11:20 14.81 256.16 1.55 538 758 29-Apr 10:25 17.77 255.26 1.51 544 764 30-Apr 11:20 18.81 254.81 1.46 554 774 5 5 3-May 10:50 21.79 253.31 1.51 551 771 3.65 256.96 7-May 10:25 25.77 225.46 1.40 586 806 10-May 10:45 28.79 254.51 1.37 625 845 5 5 1.68 256.19 14-May 11:20 32.81 254.77 1.30 627 847 1.74 256.51 16-May 10:30 34.78 255.54 1.25 637 857 0.98 256.52 17-May 11:15 35.81 256.13 1.24 644 864 Enargite In (g): Total Water (g): 5.01 13.61 Vol(mL) Mass(g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) "• 10 95.05 • 146.07 10 95.05 256.13 100.95 250 ":*yfV... • 3.40 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 178.60 489.60 28.5 2.5 Medium (g/L) 0 0.10044 0 0 Samples (mg/L): #1 2119.20 106.00 119.5 0.0 #2 2683.45 376.20 85.0 0.0 #3 2798.90 744.30 97.5 1.0 #4 2774.20 1448.25 52.0 4.0 PLS (mg/L) 3072.60 3254.30 556.5 19.0 Wash (mg/L) 52.67 44.05 1.9 0.3 Solid Residue (wt °/ 35 5.4 12 0.6 '• 7i ': Weight of Element Copper Iron Arsenic Antimony Head (g) 1.62324 0.36072 0.6012 0.019539 Innoculum (g) 0.0018 0.0049 0.0003 0.0000 Medium (g) 0 0.00955 0 0 Samples (g): #1 0.010596 0.00053 0.000598 0 #2 0.013417 0.00188 0.000425 0 #3 0.013995 0.00372 0.000488 0.000005 #4 0.013871 0.00724 0.00026 0.00002 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 PLS (g) 0.3102 0.3285 0.0562 0.0019 Wash (g) 0.013168 0.01101 0.000475 0.000075 Solid Residue (g) 1.19 0.1836 0.408 0.0204 ' . • - : ...'.li •"; \:..>:^ V • Calculated Head (g 1.550 0.513 0.466 0.022 % Difference 4.539 -42.303 22.509 -14.505 % Extraction • . •:.'<!!?* • ti ''rfp "" - X F Calculated Head 23.20 64.23 12.42 8.82 Measured Head 22.15 91.41 9.63 10.10 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 0.00 105.00 1 7.80 104.65 0.010596 0.01060 0.222 0.220 13.55 14.20 2 13.17 105.83 0.01341725 0.02401 0.284 0.293 18.04 18.90 3 18.81 102.23 0.0139945 0.03801 0.286 0.308 19.00 19.90 4 28.79 102.23 0.013871 0.05188 0.284 0.320 19.70 20.64 Filtrate 35.81 100.95 0.310 0.346 Wash 250.00 0.013 0.360 22.15 23.20 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.00 1 7.80 104.65 2.77986E-05 0.00003 0.0110929 0.01 1.72 1.21 2 13.17 105.83 0.001378799 0.00141 0.039813246 0.03 9.68 6.80 3 18.81 102.23 0.003219299 0.00463 0.076089789 0.07 19.74 13.87 4 28.79 74.38 -0.321280335 -0.31665 0.107720835 0.10 28.51 20.03 Filtrate 35.81 100.95 0.3285 0.32 Wash 250.00 0.0110125 0.33 92.77 65.19 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 0.00 105.00 1 7.80 104.65 0.0005975 0.00060 0.012505675 0.01 2.03 2.62 2 13.17 105.83 0.000425 0.00102 0.00899555 0.01 1.55 2.00 3 18.81 102.23 0.0004875 0.00151 0.009967425 0.01 1.78 2.30 4 28.79 102.23 0.00026 0.00177 0.00531596 0.01 1.09 1.40 Filtrate 35.81 100.95 0.06 0.06 Wash 250.00 0.00 0.06 9.63 12.42 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 0.0000 105.00 1 7.80 104.65 0 0.00000 0 0.00 -0.13 -0.11 2 13.17 105.83 0 0.00000 0 0.00 -0.13 -0.11 3 18.81 102.23 0.000005 0.00001 0.00010223 0.00 0.40 0.35 4 28.79 102.23 0.00002 0.00003 0.00040892 0.00 1.99 1.74 Filtrate 35.81 100.95 0.00 0.00 Wash 250.00 0.00 0.00 10.10 8.82 Mesophiles, 10 g Enargite, P B 0 of 10 microns Test MB2-M10 Mesophiles T i m e I n i t i a l E „ S a m p l e M e d i u m A d d e d F i n a l D a t e H o u r ( d a y s ) M a s s ( g ) P H ( A g / A g C I ) E „ ( m V ) ( m L ) A d d e d ( m L ) W a t e r ( g ) M a s s ( g ) 20-Dec 9:30 0.00 246.64 1.56 430 650 23-Dec 9:30 3.00 244.14 1.76 442 662 5 5 2.54 246.68 28-Dec 9:45 8.01 241.18 1.68 531 751 5 5 5.53 246.71 31-Dec 12:55 11.14 243.09 1.60 558 778 5 5 3.73 246.82 3-Jan 15:50 14.26 243.86 1.42 633 853 5 5 2.94 246.80 8-Jan 10:05 19.02 242.05 1.32 657 877 5 5 4.83 246.88 11-Jan 10:05 22.02 245.52 1.32 580 800 5 5 1.24 246.76 15-Jan 11:25 26.08 245.34 1.26 651 871 5 5 1.25 246.59 18-Jan 9:25 29.00 245.61 1.21 677 897 5 5 1.14 246.75 22-Jan 11:30 33.08 245.12 691 911 5 5 1.67 246.79 25-Jan 10:05 36.02 245.24 1.16 672 892 E n a r g i t e I n ( g ) : 10.00 Total Water (g): • 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 A n a l y s i s Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 1337.45 1291.15 39.5 3.0 Medium (g/L) 0 0.10 0 0 Samples (mg/L): #1 2010.85 260.90 36.5 1.5 #2 4452.85 253.10 208.5 1.5 #3 4622.60 337.80 146.5 0.0 #4 5473.20 1830.35 347.0 4.0 #5 6146.05 3373.50 641.0 10.5 #6 6343.35 3962.10 828.5 17.5 #7 6189.95 5642.50 1215.5 67.5 #8 6561.10 7359.95 1313.5 73.5 #9 6217.85 8577.95 1245.0 70.5 PLS (mg/L) 5418.35 7932.3 1171 66.5 Wash (mg/L) 132.81 147.55 5.6 0.6 Solid Residue (wt %) 35.2 1.8 13.9 0.67 -•IIS. ,. . ..; R - 4 .: Weight of Element Copper Iron Arsenic Antimony Head (g) 3.12 1.16 1.05 0.055 Innoculum (g) 0.0134 0.0129 0.0004 0.0000 Medium (g) 0 0.00954 0 0 Samples (g): #1 0.0100543 0.0013 0.00018 0.0000075 #2 0.0222643 0.00127 0.00104 0.0000075 #3 0.023113 0.00169 0.00073 0 #4 0.027366 0.00915 0.00174 0.00002 #5 0.0307303 0.01687 0.00321 0.0000525 #6 0.0317168 0.01981 0.00414 0.0000875 #7 0.0309498 0.02821 0.00608 0.0003375 #8 0.0328055 0.0368 0.00657 0.0003675 #9 0.0310893 0.04289 0.00623 0.0003525 Medium Added (g): #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 PLS (g) 0.5349 0.7831 0.1156 0.0066 Wash (g) 0.0332025 0.03689 0.0014 0.00015 Solid Residue (g) 2.2528 0.1152 0.8896 0.04288 tmij,, -:,!mm t r t j t Calculated Head (g) 3.048 1.066 1.036 0.051 % Difference 2.320 8.088 1.322 7.641 % E x t r a c t i o n ' • • • * J o * •. - • • : -sp". Calculated Head 26.08 89.20 14.14 15.59 Measured Head 25.47 81.98 13.95 14.40 Copper Output Sample Time Sol'n Vol. g Cu Total Cu Cu in Cu (aq) %Cu %Cu No. (days) (mL) sampled Removed (g) sol'n (g) total (g) indicated actual 0.00 104.52 1 3.00 102.02 0.01005 0.01005 0.205 0.192 6.15 6.29 2 8.01 99.06 0.02226 0.03232 0.441 0.438 14.03 14.36 3 11.14 100.97 0.02311 0.05543 0.467 0.486 15.57 15.94 4 14.26 101.74 0.02737 0.08280 0.557 0.599 19.20 19.65 5 19.02 99.93 0.03073 0.11353 0.614 0.684 21.91 22.43 6 22.02 103.40 0.03172 0.14524 0.656 0.756 24.23 24.81 7 26.08 103.22 0.03095 0.17619 0.639 0.771 24.71 25.29 8 29.00 103.49 0.03281 0.20900 0.679 0.842 26.98 27.62 9 33.08 103.00 0.03109 0.24009 0.640 0.836 26.80 27.43 Filtrate 36.02 98.72 0.535 0.762 24.41 24.99 Wash 250.00 0.033 0.795 25.47 26.08 Iron Output Sample Time Sol'n Vol. g Fe Total Fe Fe in Fe (aq) %Fe %Fe No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 104.52 1 3.00 102.02 0.0008 0.00080 0.026617 0.01 1.18 1.29 2 8.01 99.06 0.00076 0.00157 0.025072 0.01 105 1.14 3 11.14 100.97 0.00119 0.00275 0.034108 0.02 1.83 1.99 4 14.26 101.74 0.00865 0.01140 0.18622 0.17 14.94 16.26 5 19.02 99.93 0.01637 0.02777 0.337114 0.32 27.95 30.41 6 22.02 103.40 0.01931 0.04708 0.409681 0.40 34.20 37.21 7 26.08 103.22 0.02771 0.07479 0.582419 0.57 49.10 53.42 8 29.00 103.49 0.0363 0.11108 0.761681 0.75 64.55 70.23 9 33.08 103.00 0.04239 0.15347 0.883529 0.87 75.05 81.66 Filtrate 36.02 98.72 0.7831 0.77 66.39 72.24 Wash 250.00 0.036888 0.81 69.57 75.70 Arsenic Output Sample Time Sol'n Vol. g As Total As As in As(aq) %As %As No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 104.52 1 3.00 102.02 0.00018 0.00018 0.003724 0.00 0.32 0.32 2 8.01 99.06 0.00104 0.00123 0.020654 0.02 1.95 1.97 3 11.14 100.97 0.00073 0.00196 0.014792 0.02 1.49 1.51 4 14.26 101.74 0.00174 0.00369 0.035304 0.04 3.51 3.56 5 19.02 99.93 0.00321 0.00690 0.064055 0.07 6.41 6.50 6 22.02 103.40 0.00414 0.01104 0.085667 0.09 8.78 8.90 7 26.08 103.22 0.00608 0.01712 0.125464 0.14 12.96 13.14 8 29.00 103.49 0.00657 0.02369 0.135934 0.15 14.54 14.73 9 33.08 103.00 0.00623 0.02991 0.128235 0.15 14.43 14.62 Filtrate 36.02 98.72 0.12 0.15 13.82 14.01 Wash 250.00 0.00 0.15 13.95 14.14 Antimony Output Sample Time Sol'n Vol. gSb Total Sb Sb in Sb (aq) %Sb %Sb No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.0000 104.52 1 3.0000 102.02 7.5E-06 0.00001 0.000153 0.00 0.22 0.24 2 8.0104 99.06 7.5E-06 0.00002 0.000149 0.00 0.23 0.25 3 11.1424 100.97 0 0.00002 0 0.00 -0.03 -0.03 4 14.2639 101.74 0.00002 0.00004 0.000407 0.00 0.71 0.77 5 19.0243 99.93 5.3E-05 0.00009 0.001049 0.00 1.92 2.08 6 22.0243 103.40 8.8E-05 0.00018 0.00181 0.00 3.39 3.68 7 26.0799 103.22 0.00034 0.00051 0.006967 0.01 12.93 14.00 8 28.9965 103.49 0.00037 0.00088 0.007607 0.01 14.71 15.92 9 33.0833 103.00 0.00035 0.00123 0.007262 0.01 14.75 15.97 Filtrate 36.0243 98.72 0.01 0.01 14.12 15.29 Wash 250.00 0.00 0.01 14.40 15.59 162 Mesophiles, 10 g Enargite, P 8 0 of 15 microns Test #B2-M15 Mesophiles T i m e Initial E„ S a m p l e M e d i u m A d d e d Final Date H o u r (days) M a s s (g) pH (Ag/AgCI) E h (mV) (mL) A d d e d (mL) Water (g) M a s s (g) 20-Dec 9:30 0.00 245.48 1.54 420 640 23-Dec 9:30 3.00 242.70 1.93 473 693 5 5 2.45 245.15 28-Dec 9:45 8.01 239.62 1.78 526 746 5 5 6.53 246.15 31-Dec 12:55 11.14 242.60 1.62 550 770 5 5 2.82 245.42 3-Jan 15:50 14.26 242.41 1.37 652 872 5 5 3.02 245.43 8-Jan 10:05 19.02 240.85 1.26 675 895 5 5 5.99 246.84 11-Jan 10:05 22.02 245.40 1.20 672 892 5 5 1.35 246.75 15-Jan 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 1.21 674 894 Enarg i te In (g): 10.00 Total Water (g): 26.40 Vol (mL) M a s s (g) Flask Weight (g): 130.99 Innoculum in: 10 10 Medium in: 95.01 95.01 Total Final Weight (g): 244.43 Filtrate Volume (mL) 100.77 • f •{'. W a s h Volume (mL) 250 f ; Solid Residue (g) 6.43 A n a l y s i s Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 1337.45 1291.15 39.5 3.0 Medium (g/L) 0 0.10044 0 0 Samples (mg/L): #1 1985.55 212.60 13.0 0.0 #2 5236.00 195.75 212.0 0.5 #3 6428.45 247.65 294.0 0.5 #4 7153.05 2067.00 512.5 7.5 #5 7322.05 5735.45 1300.5 53.5 #6 6736.85 5465.75 1076.5 63.0 #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 W a s h (mg/L) 99.67 63.26 2.4 0.4 Solid Residue (wt %) 34 4.6 13.1 0.69 ' i ' •' ' . v ',- - » Weight of Element Copper Iron Arsenic Antimony Head (g) 3.04 1.06 1.05 0.055 Innoculum (g) 0.0134 0.0129 0.0004 0.0000 Medium (g) 0 0.00954 0 0 Samples (g): #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 Medium Added (g): #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 P L S (g) 0.5542 0.5657 0.1002 0.0058 W a s h (g) 0.0249175 0.01582 0.0006 0.0001 Solid Residue (g) 2.1862 0.29578 0.84233 0.044367 : • » - • ' - ; ' Calculated Head (g) 3.023 1.008 0.976 0.052 % Difference 0.566 4.901 7.051 5.715 % Extract ion u:.-Calculated Head 27.68 70.66 13.69 14.44 Measured Head 27.52 67.20 12.73 13.62 Copper Output Sample Time Sol'n Vol. g Cu Total Cu Cu in Cu (aq) % C u % C u No. (days) (mL) sampled Removed (g) sol'n (g) total (g) indicated actual 0.00 104.49 1 3.00 101.71 0.00993 0.00993 0.202 0.189 6.20 6.24 2 8.01 98.63 0.02618 0.03611 0.516 0.513 16.87 16.97 3 11.14 101.61 0.03214 0.06825 0.653 0.676 22.23 22.36 4 14.26 101.42 0.03577 0.10402 0.725 0.780 25.67 25.82 5 19.02 99.86 0.03661 0.14063 0.731 0.822 27.03 27.19 6 22.02 104.41 0.03368 0.17431 0.703 0.831 27.32 27.48 7 26.08 103.94 0.03259 0.20690 0.677 0.838 27.58 27.74 8 29.00 104.20 0.03311 0.24001 0.690 0.884 29.07 29.23 9 33.08 103.74 0.03082 0.27083 0.639 0.866 28.49 28.65 Filtrate 36.02 100.77 0.554 0.812 26.70 26.85 Wash 250.00 0.025 0.837 27.52 27.68 Iron Output Sample Time Sol'n Vol. g Fe Total Fe Fe in Fe (aq) % F e % F e No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 104.49 1 3.00 101.71 0.00056 0.00056 0.022 0.01 0.82 0.86 2 8.01 98.63 0.00048 0.00104 0.019 0.01 0.60 0.63 3 11.14 101.61 0.00074 0.00177 0.025 0.01 1.16 1.22 4 14.26 101.42 0.00983 0.01161 0.210 0.20 18.56 19.52 5 19.02 99.86 0.02818 0.03978 0.573 0.56 52.81 55.54 6 22.02 104.41 0.02683 0.06661 ' 0.571 0.56 52.62 55.33 7 26.08 103.94 0.02762 0.09423 0.585 0.57 53.93 56.71 8 29.00 104.20 0.02992 0.12415 0.634 0.62 58.59 61.61 9 33.08 103.74 0.02909 0.15324 0.614 0.60 56.70 59.63 Filtrate 36.02 100.77 0.5657 0.55 52.15 54.83 Wash 250.00 0.015815 0.57 53.64 56.40 Arsenic Output Sample Time Sol'n Vol. g As Total As As in As (aq) % A s % A s No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 104.49 1 3.00 101.71 6.5E-05 0.00007 0.001322 0.00 0.09 0.10 2 8.01 98.63 0.00106 0.00113 0.02091 0.02 1.96 2.11 3 11.14 101.61 0.00147 0.00260 0.029873 0.03 2.91 3.14 4 14.26 101.42 0.00256 0.00516 0.051978 0.05 5.16 5.55 5 19.02 99.86 0.0065 0.01166 0.129868 0.13 12.82 13.79 6 22.02 104.41 0.00538 0.01704 0.112397 0.12 11.78 12.67 7 26.08 103.94 0.00535 0.02240 0.111268 0.13 12.18 13.11 8 29.00 104.20 0.00561 0.02801 0.116912 0.14 13.23 14.23 9 33.08 103.74 0.00526 0.03327 0.109186 0.14 13.03 14.02 Filtrate 36.02 100.77 0.10 0.13 12.67 13.63 Wash 250.00 0.00 0.13 12.73 13.69 Antimony Output Sample Time Sol'n Vol. g S b Total Sb Sb in Sb (aq) % S b % S b No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.0000 104.49 1 3.0000 101.71 0 0.00000 0 0.00 -0.05 -0.06 2 8.0104 98.63 2.5E-06 0.00000 4.93E-05 0.00 0.04 0.04 3 11.1424 101.61 2.5E-06 0.00001 5.08E-05 0.00 0.04 0.04 4 14.2639 101.42 3.8E-05 0.00004 0.000761 0.00 1.34 1.42 5 19.0243 99.86 0.00027 0.00031 0.005343 0.01 9.74 10.33 6 22.0243 104.41 0.00032 0.00063 0.006578 0.01 12.47 13.22 7 26.0799 103.94 0.00032 0.00095 0.006652 0.01 13.18 13.98 8 28.9965 104.20 0.00032 0.00127 0.006669 0.01 13.79 14.62 9 33.0833 103.74 0.00031 0.00158 0.006432 0.01 13.94 14.78 Filtrate 36.0243 100.77 0.01 0.01 13.44 14.25 Wash 250.00 0.00 0.01 13.62 14.44 Mesophiles, 10 g Enargite (2), P 8 0 of 15 microns Test XB7-M15 Mesophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E h (mV) (mL) Added (mL) Water (g) Mass (g) 16-Jul 13:30 0.00 245.86 1.60 449 669 18-Jul 11:55 1.93 244.90 2.25 362 582 2.63 247.53 22-Jul 10:35 5.88 246.29 1.94 491 711 23-Jul 12:20 6.95 246.09 1.90 509 729 5 5 26-Jul 10:20 9.87 244.85 1.66 540 760 2.79 247.64 30-Jul 11:15 13.91 246.11 1.52 523 743 31-Jul 13:05 14.98 245.98 1.42 549 769 5 5 2-Aug 12:00 16.94 245.04 1.46 558 778 6-Aug 12:00 20.94 243.96 1.43 625 845 1.96 245.92 7-Aug 12:30 21.96 245.66 1.39 612 832 5 5 9-Aug 12:45 23.97 244.90 1.30 664 884 12-Aug 12:10 26.94 245.54 1.23 685 905 0.62 246.16 13-Aug 12:10 27.94 245.35 1.26 693 913 5 5 16-Aug 13:50 31.01 244.16 1.21 700 920 20-Aug 13:15 34.99 245.84 1.22 711 931 1.50 247.34 21-Aug 13:05 35.98 245.65 1.22 708 928 Enargite In (g): 10.01 Total Water (g): 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 1 " : — Wash Volume (mL) 250 Solid Residue (g) 6.01 Analysis Copper Iron Arsenic Antimony Head (wt-%) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 383.25 1305.50 55.5 Medium (g/L) 0 0.1004 0 0 Samples (mg/L): #1 5193.50 251.10 51.0 #2 6757.20 1791.50 311.5 #3 7174.55 3593.95 779.0 #4 7031.45 6953.55 1037.0 PLS (mg/L) 6628.95 8613.40 956.5 Wash (mg/L) 99.91 116.39 5.2 Solid Residue (wt % 38 0.8654 14 0.7 V *<t'.i. ••jt'v";;i.. •".',!: " - ' ^ v ; ;Hi:s Weight of Element Copper Iron Arsenic Antimony Head (g) 3.04304 1.0611 1.05105 0.055055 Innoculum (g) 0.0038 0.0131 0.0006 0.0000 Medium (g) 0 0.0095 0 0 Samples (g): #1 0.025968 0.0013 0.000255 0 #2 0.033786 0.009 0.001558 0 #3 0.035873 0.018 0.003895 0 #4 0.035157 0.0348 0.005185 0 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 #4 0 0.0005 0 0 PLS (g) 0.6883 0.8943 0.0993 0.0000 Wash (g) 0.024978 0.0291 0.0013 0 Solid Residue (g) 2.2838 0.052 0.8414 0.04207 • ... . . . Calculated Head (g) 3.089 0.980 0.947 0.042 % Difference -1.506 7.686 9.884 23.586 % Extraction Calculated Head 26.06 94.69 11.17 0.00 Measured Head 26.46 87.41 10.06 0.00 165 Copper Output Sample # Time (days) Sol'n Vol. (mL) g Cu sampled Tot. Cu Sampled (g) Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.00 105.15 1 6.95 105.38 0.0259675 0.02597 0.547 0.543 17.86 17.59 2 14.98 105.27 0.033786 0.05975 0.711 0.733 24.10 23.75 3 21.96 104.95 0.03587275 0.09563 0.753 0.809 26.58 26.19 4 27.94 104.64 0.03515725 0.13078 0.736 0.828 27.20 26.79 Filtrate 35.98 103.83 0.688 0.780 Wash 250.00 0.025 0.805 26.46 26.06 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.15 1 6.95 105.38 0.000753299 0.00075 0.026 0.01 1.26 1.37 2 14.98 105.27 0.008455299 0.00921 0.189 0.18 16.54 17.92 3 21.96 104.95 0.017467549 0.02668 0.377 0.36 34.32 37.17 4 27.94 . 104.64 0.034265549 0.06094 0.728 0.71 67.34 72.95 Filtrate 35.98 103.83 0.8943 0.88 Wash 250.00 0.0290975 0.91 85.80 92.94 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 0.00 105.15 1 6.95 105.38 0.000255 0.00026 0.00537438 0.00 0.46 0.51 2 14.98 105.27 0.0015575 0.00181 0.032791605 0.03 3.09 3.43 3 21.96 104.95 0.003895 0.00571 0.08175605 0.08 7.90 8.76 4 27.94 104.64 0.005185 0.01089 0.10851168 0.11 10.81 12.00 Filtrate 35.98 103.83 0.10 0.10 Wash 250.00 0.00 0.11 10.06 11.17 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 0.00 105.15 1 6.95 105.38 0 0.00000 0 0.00 0.00 0.00 2 14.98 105.27 0 0.00000 0 0.00 0.00 0.00 3 21.96 104.95 0 0.00000 0 0.00 0.00 0.00 4 27.94 104.64 0 0.00000 0 0.00 0.00 0.00 Filtrate 35.98 103.83 0.00 0.00 Wash 250.00 0.00 0.00 0.00 0.00 166 Mesophiles, 10 g Enargite, P 8 0 of 37 microns Test #B2-M37 Mesophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 20-Dec 9:30 0.00 252.70 1.56 439 659 23-Dec 9:30 3.00 249.69 1.68 440 660 5 5 3.53 253.22 28-Dec 9:45 8.01 229.94 1.59 514 734 5 5 22.84 252.78 31-Dec 12:55 11.14 236.34 1.50 534 754 5 5 16.37 252.71 3-Jan 15:50 14.26 248.98 1.46 606 826 5 5 3.28 252.26 8-Jan 10:05 19.02 247.16 1.28 659 879 5 5 5.83 252.99 11-Jan 10:05 22.02 251.43 1.26 665 885 5 5 1.59 253.02 15-Jan 11:25 26.08 251.31 1.36 683 903 5 5 1.62 252.93 18-Jan 9:25 29.00 251.74 1.29 699 919 5 5 0.98 252.72 22-Jan 11:30 33.08 250.96 220 5 5 1.88 252.84 25-Jan 10:05 36.02 251.26 1.29 220 Enargite In (g): Total Water (g): 10.00 57.92 Vol (mL) Mass (g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) Ci' • '-"fi 138.23 10 10 94.98 94.98 I 251.26 99.72 •. . .'. , 2 4 5 iL^_Ji£ i i f f i \ \ ; ; j j ! 8.06 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 1337.45 1291.15 39.5 3.0 Medium (g/L) 0 0.10044 0 0 Samples (mg/L): #1 1534.10 265.40 38.5 0.0 #2 4730.65 330.60 565.5 0.0 #3 5161.10 227.05 671.0 0.0 #4 5063.85 428.35 674.5 0.0 #5 5137.55 1118.15 65.0 0.0 #6 4885.00 2047.00 497.0 4.0 #7 4780.25 2426.20 566.5 7.0 #8 4844.40 2768.50 622.5 7.0 #9 4498.20 2897.65 636.5 8.0 PLS (mg/L) 3984.8 2673.4 620 16 Wash (mg/L) 91.49 33.40 1.4 0.3 Solid Residue (wt %) 32 4.4 12.7 0.42 Weight of Element Copper Iron Arsenic Antimony Head (g) 3.24 0.72 1.2 0.039 Innoculum (g) 0.0134 0.0129 0.0004 0.0000 Medium (g) 0 0.00954 0 0 Samples (g): #1 0.0076705 0.00133 0.00019 0 #2 0.0236533 0.00165 0.00283 0 #3 0.0258055 0.00114 0.00336 0 #4 0.0253193 0.00214 0.00337 0 #5 0.0256878 0.00559 0.00033 0 #6 0.024425 0.01024 0.00249 0.00002 #7 0.0239013 0.01213 0.00283 0.000035 #8 0.024222 0.01384 0.00311 0.000035 #9 0.022491 0.01449 0.00318 0.00004 Medium Added (g): #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 PLS (g) 0.3974 0.2666 0.0618 0.0016 Wash (g) 0.0224151 0.00818 0.00034 0.0000735 Solid Residue (g) 2.5792 0.35464 1.02362 0.033852 ' • . . ' *'/'"*'• " . *>" .'-"jiv •  Calculated Head (g) 3.189 0.665 1.107 0.036 % Difference 1.581 7.641 7.743 8.664 % Extraction Calculated Head 19.12 46.67 7.54 4.97 Measured Head 18.81 43.10 6.95 4.54 Copper Output Sample Time Sol'n Vol. g Cu Total Cu Cu in Cu (aq) % C u % C u No. (days) (mL) sampled Removed (g) sol'n (g) total (g) indicated actual 0.00 104.47 1 3.00 101.46 0.00767 0.00767 0.156 0.142 4.39 4.46 2 8.01 81.71 0.02365 0.03132 0.387 0.381 11.75 11.94 3 11.14 88.11 0.02581 0.05713 0.455 0.473 14.59 14.82 4 14.26 100.75 0.02532 0.08245 0.510 0.554 17.10 17.37 5 19.02 98.93 0.02569 0.10814 0.508 0.577 17.82 18.11 6 22.02 103.20 0.02443 0.13256 0.504 0.599 18.48 18.78 7 26.08 103.08 0.0239 0.15646 0.493 0.612 18.89 19.19 8 29.00 103.51 0.02422 0.18068 0.501 0.645 19.89 20.21 9 33.08 102.73 0.02249 0.20318 0.462 0.629 19.43 19.74 Filtrate 36.02 99.72 0.397 0.587 18.12 18.41 Wash 245.00 0.022 0.610 18.81 19.12 Iron Output Sample Time Sol'n Vol. g Fe Total Fe Fe in Fe (aq) % F e % F e No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 104.47 1 3.00 101.46 0.00082 0.00082 0.026927 0.01 1.95 2.11 2 8.01 81.71 0.00115 0.00198 0.027013 0.01 1.96 2.12 3 11.14 88.11 0.00063 0.00261 0.020005 0.01 0.99 1.07 4 14.26 100.75 0.00164 0.00425 0.043156 0.03 4.20 4.55 5 19.02 98.93 0.00509 0.00934 0.110619 0.10 13.57 14.69 6 22.02 103.20 0.00973 0.01907 0.21125 0.20 27.55 29.83 7 26.08 103.08 0.01163 0.03070 0.250093 0.24 32.94 35.67 8 29.00 103.51 0.01334 0.04404 0.286567 0.27 38.01 41.15 9 33.08 102.-73 0.01399 0.05802 0.297676 0.28 39.55 42.82 Filtrate 36.02 99.72 0.2666 0.25 35.23 38.15 Wash 245.00 0.008183 0.26 36.37 39.38 Arsenic Output Sample Time Sol'n Vol. g As Total As As in As(aq) % As % As No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 104.47 1 3.00 101.46 0.00019 0.00019 0.003906 0.00 0.29 0.32 2 8.01 81.71 0.00283 0.00302 0.046207 0.05 3.83 4.16 3 11.14 88.11 0.00336 0.00638 0.059122 0.06 5.15 5.58 4 14.26 100.75 0.00337 0.00975 0.067956 0.07 6.16 6.68 5 19.02 98.93 0.00033 0.01007 0.00643 0.02 1.32 1.43 6 22.02 103.20 0.00249 0.01256 0.05129 0.06 5.08 5.51 7 26.08 103.08 0.00283 0.01539 0.058395 0.07 5.88 6.37 8 29.00 103.51 0.00311 0.01850 0.064435 0.08 6.62 7.17 9 33.08 102.73 0.00318 0.02169 0.065388 0.08 6.96 7.54 Filtrate 36.02 99.72 0.06 0.08 6.93 7.51 Wash 245.00 0.00 0.08 6.95 7.54 Antimony Output Sample Time Sol'n Vol. g S b Total Sb Sb in Sb (aq) % S b % S b No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.0000 104.47 1 3.0000 101.46 0 0.00000 0 0.00 -0.08 -0.08 2 8.0104 81.71 0 0.00000 0 0.00 -0.08 -0.08 3 11.1424 88.11 0 0.00000 0 0.00 -0.08 -0.08 4 14.2639 100.75 0 0.00000 0 0.00 -0.08 -0.08 5 19.0243 98.93 0 0.00000 0 0.00 -0.08 -0.08 6 22.0243 103.20 0.00002 0.00002 0.000413 0.00 0.98 1.07 7 26.0799 103.08 3.5E-05 0.00006 0.000722 0.00 1.82 2.00 8 28.9965 103.51 3.5E-05 0.00009 0.000725 0.00 1.92 2.10 9 33.0833 102.73 0.00004 0.00013 0.000822 0.00 2.26 2.48 Filtrate 36.0243 99.72 0.00 0.00 4.35 4.76 Wash 245.00 0.00 0.00 4.54 4.97 168 Mesophiles, 10 g Enargite (2), P 8 0 of 37 microns Test UB7-M37 Mesophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 16-Jul 13:30 0.00 249.20 1.61 464 684 18-Jul 11:55 1.93 248.48 1.85 370 590 1.19 249.67 22-Jul 10:35 5.88 248.20 1.67 499 719 23-Jul 12:20 6.95 247.64 1.75 508 728 5 5 26-Jul 10:20 9.87 246.10 1.58 531 751 4.20 250.30 30-Jul 11:15 13.91 248.97 1.45 586 806 31-Jul 13:05 14.98 248.54 1.34 585 805 5 5 2-Aug 12:00 16.94 247.83 1.38 606 826 2.94 250.77 6-Aug 12:00 20.94 249.46 1.33 636 856 7-Aug 12:30 21.96 249.18 1.32 629 849 5 5 9-Aug 12:45 23.97 248.37 1.27 664 884 1.34 249.71 12-Aug 12:15 26.95 249.02 1.23 671 891 13-Aug 12:15 27.95 248.70 1.27 655 875 5 5 16-Aug 13:50 31.01 247.36 1.18 692 912 2.09 249.45 20-Aug 13:15 34.99 248.06 1.21 700 920 1.70 249.76 21-Aug 13:05 35.98 249.52 1.22 698 918 Enargite In (g): 10.02 Total Water (g): 13.46 Vol (mL) Mass (g) Flask Weight (g): - 133.95 Innoculum in: 10 10 Medium in: 95.11 95.11 Total Final Weight (g): '' C' ' 249.52 Filtrate Volume (mL) 103.68 Wash Volume (mL) 250 Solid Residue (g) 7.66 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 383.25 1305.50 55.5 Medium (g/L) 0 0.1004 0 0 Samples (mg/L): • #1 3796.25 127.75 261.5 #2 5064.30 921.45 262.5 #3 5056.60 2704.10 571.0 #4 5197.40 4415.30 976.0 PLS (mg/L) 5137.10 5293.25 1038.5 Wash (mg/L) 94.08 49.94 1.9 Solid Residue (wt % 36 1.3837 13 0.4 '.• • • ' " : : ' • ' ' ' I Weight of Element Copper Iron Arsenic Antimony Head (g) 3.24648 0.7214 1.2024 0.039078 Innoculum (g) 0.0038 0.0131 0.0006 0.0000 Medium (g) 0 0.0096 0 0 Samples (g): #1 0.018981 0.0006 0.001308 0 #2 0.025322 0.0046 0.001313 0 #3 0.025283 0.0135 0.002855 0 #4 0.025987 0.0221 0.00488 0 Medium Added (g): #1 0 0.0005 0 0 #2 0 0.0005 0 0 #3 0 0.0005 0 0 #4 0 0.0005 0 0 PLS (g) 0.5326 0.5488 0.1077 0.0000 Wash (g) 0.02352 0.0125 0.000475 0 Solid Residue (g) 2.7576 0.106 0.9958 0.03064 ' * , Calculated Head (g) 3.379 0.662 1.109 0.031 % Difference -4.097 8.248 7.779 21.593 % Extraction Calculated Head 18.40 83.99 10.20 0.00 Measured Head 19.16 77.06 9.40 0.00 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 0.00 105.23 1 6.95 103.67 0.01898125 0.01898 0.394 0.390 12.00 11.53 2 14.98 104.57 0.0253215 0.04430 0.530 0.545 16.78 16.12 3 21.96 105.21 0.025283 0.06959 0.532 0.572 17.63 16.94 4 27.95 104.73 0.025987 0.09557 0.544 0.610 18.79 18.05 Filtrate 35.98 103.68 0.533 0.598 Wash 250.00 0.024 0.622 19.16 18.40 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.23 1 6.95 103.67 0.000136549 0.00014 0.013243843 0.00 0.03 0.03 2 14.98 104.57 0.004105049 0.00424 0.096356027 0.08 11.55 12.58 3 21.96 105.21 0.013018299 0.01726 0.284498361 0.27 37.63 41.01 4 27.95 104.73 0.021574299 0.03883 0.462414369 0.45 62.29 67.89 Filtrate 35.98 103.68 0.5488 0.54 Wash 250.00 0.012485 0.55 75.99 82.82 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 0.00 105.23 1 6.95 103.67 0.0013075 0.00131 0.027109705 0.03 2.21 2.39 2 14.98 104.57 0.0013125 0.00262 0.027449625 0.03 2.35 2.54 3 21.96 105.21 0.002855 0.00548 0.06007491 0.06 5.17 5.60 4 27.95 104.73 0.00488 0.01036 0.10221648 0.11 8.91 9.66 Filtrate 35.98 103.68 0.11 0.11 Wash 250.00 0.00 0.11 9.40 10.20 Antimony Output Sample # Time (days) Sol'n Vol. (n nL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) Sb(aq) total %Sb indicated %Sb actual 0.00 105.23 1 6.95 103.67 0 0.00000 0 0.00 0.00 0.00 2 14.98 104.57 0 0.00000 0 0.00 0.00 0.00 3 21.96 105.21 0 0.00000 0 0.00 0.00 0.00 4 27.95 104.73 0 0.00000 0 0.00 0.00 0.00 Filtrate 35.98 103.68 0.00 0.00 Wash 250.00 0.00 0.00 0.00 0.00 Moderate Thermophiles, 2 g Enargite, P 8 0 of 10 microns Test #B9-T10 Moderate Thermophiles Time Initial E h Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E h (mV) (mL) Added (mL) Water (g) Mass (g) 4-Jun 12:25 0.00 241.39 1.58 484 704 7-Jun 10:40 2.93 233.46 1.79 401 621 8.46 241.92 10-Jun 10:50 5.93 234.01 1.79 454 674 7.91 241.92 13-Jun 11:30 8.96 234.26 1.75 480 700 8.66 242.92 17-Jun 10:25 12.92 232.46 1.62 512 732 9.89 242.35 18-Jun 11:20 13.95 239.67 1.55 508 728 5 5 20-Jun 12:15 15.99 234.18 1.35 537 757 9.03 243.21 24-Jun 11:35 19.97 232.88 1.36 593 813 8.67 241.55 26-Jun 12:55 22.02 236.00 1.31 624 844 5 5 5.97 241.97 28-Jun 12:50 24.02 236.88 1.40 625 845 5.96 242.84 2-Jul 13:10 28.03 232.34 1.42 608 828 9.74 242.08 4-Jul 13:20 30.04 236.86 1.30 621 841 5 5 5.43 242.29 9-Jul 11:45 34.97 229.35 1.37 620 840 12.56 241.91 10-Jul 12:15 35.99 239.17 1.41 621 841 Enargite In (g): Total Water (g): 2.01 92.28 Vol (mL) Mass (g) Flask Weight (g): 133.84 Innoculum in: 10 10 Medium in: 95.01 95.01 Total Final Weight (g): •• • ..*»tJ , 239.17 Filtrate Volume (mL) 102.02 Wash Volume (mL) 250 Solid Residue (g) 0.81 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 2986.40 641.50 396.5 #2 3291.45 1976.85 535.0 4.5 #3 3303.50 1893.00 549.0 4.0 PLS (mg/L) 3533.95 1522.25 456.5 Wash (mg/L) 36.09 8.77 4.0 Solid Residue (wt "A 32 2.0608 12 0.9 „.-; ,'u •<.-, ... Weight of Element Copper Iron Arsenic Antimony Head (g) 0.62712 0.23316 0.21105 0.011055 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.01909 0 0 Samples (g): #1 0.014932 0.00321 0.001983 0 #2 0.016457 0.00988 0.002675 0.0000225 #3 0.016518 0.00947 0.002745 0.00002 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.3605 0.1553 0.0466 0.0000 Wash (g) 0.009023 0.00219 0.001 0 Solid Residue (g) 0.2592 0.01669 0.0972 0.00729 ,, ; „• -Calculated Head (g) 0.650 0.155 0.148 0.007 % Difference -3.727 33.659 30.074 34.532 % Extraction Calculated Head 60.15 89.21 34.14 -0.73 Measured Head 62.39 59.18 23.87 -0.47 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 0.00 105.54 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 Filtrate 35.99 102.02 0.361 0.382 W a s h 250.00 0.009 0.391 62.39 60.15 Iron Output Sample # Time (days) Sol'n Vol. (r g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.54 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 Filtrate 35.99 102.02 0.1553 0.14 W a s h 250.00 0.0021925 0.14 58.99 88.91 Arsenic Output Sample # Time (days) Sol'n Vol. (n nL) g As sampled Tot. As Sample As in sol'n (g) As(aq)total %As indicated %As actual 0.00 105.54 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 Filtrate 35.99 102.02 0.05 0.05 W a s h 250.00 0.00 0.05 23.87 34.14 Antimony Output Sample # Time (days) Sol'n Vol. (r nL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) Sb(aq) total %Sb indicated %Sb actual 0.0000 105.54 1 12.92 96.61 0 0.00000 0 0.00 -0.86 ' -1.31 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 Filtrate 35.99 102.02 0.00 0.00 W a s h 250.00 0.00 0.00 -0.47 -0.73 Moderate Thermophiles, 2 g Enargite, P 8 0 of 15 microns Test#B9-T15 Moderate Thermophiles Date Hour Time (days) Initial Mass (g) pH E h (Ag/AgCI) E h (mV) Sample (mL) Medium Added (mL) Added Water (g) Final Mass (g) 4-Jun 12:25 0.00 255.38 1.58 479 699 7-Jun 10:40 2.93 248.00 1.83 395 615 8.44 256.44 10-Jun 10:50 5.93 248.46 1.86 436 656 8.54 257.00 13-Jun 11:30 8.96 248.92 1.85 479 699 7.70 256.62 17-Jun 10:25 12.92 246.31 1.70 512 732 10.66 256.97 18-Jun 11:20 13.95 254.28 1.66 521 741 5 5 20-Jun 12:15 15.99 248.81 1.51 545 765 6.94 255.75 24-Jun 11:35 19.97 245.29 1.45 576 796 11.11 256.40 26-Jun 12:55 22.02 250.90 1.38 609 829 5 5 4.96 255.86 28-Jun 12:50 24.02 250.57 1.48 597 817 5.11 255.68 2-Jul 13:10 28.03 245.36 1.48 615 835 10.06 255.42 4-Jul 13:20 30.04 250.21 1.37 627 847 5 5 5.75 255.96 9-Jul 11:45 34.97 243.80 1.44 624 844 12.83 256.63 10-Jul 12:15 35.99 254.10 1.45 620 840 Enargite In (g): 2.01 Total Water (g): 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 Filtrate Volume (mL) 102.56 Wash Volume (mL) 250 Solid Residue (g) 0.95 Analysis Copper Iron Arsenic Antimony Head (wt %) •30.4 10.6 10.5 0.55 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.20088 0 0 Samples (mg/L): #1 2288.95 486.85 271.0 1.0 #2 2444.50 1133.85 271.5 2.5 #3 2720.20 1750.90 395.5 5.5 PLS (mg/L) 2960.00 1558.65 357.5 Wash (mg/L) 30.32 8.93 3.0 Solid Residue (wt"/( 36 1.0616 13 0.8 , i ",' ' Weight of Element Copper Iron Arsenic Antimony Head (g) 0.61104 0.21306 0.21105 0.011055 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.0191 0 0 Samples (g): #1 0.011445 0.00243 0.001355 0.000005 #2 0.012223 0.00567 0.001358 0.0000125 #3 0.013601 0.00875 0.001978 0.0000275 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.3036 0.1599 0.0367 0.0000 Wash (g) 0.00758 0.00223 0.00075 0 Solid Residue (g) 0.342 0.01009 0.1235 0.0076 Calculated Head (g) 0.664 0.147 0.161 0.008 % Difference -8.709 31.025 23.710 31.705 % Extraction i- -: • • - ' T J i l S f M Calculated Head 48.51 93.14 23.30 -0.66 Measured Head 52.74 64.24 17.77 -0.45 173 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 0.00 105.57 1 12.92 96.50 0.01144475 0.01144 0.221 0.195 31.87 29.31 2 19.97 95.48 0.0122225 0.02367 0.233 0.219 35.79 32.92 3 28.03 95.55 0.013601 0.03727 0.260 0.257 42.13 38.75 Filtrate 35.99 102.56 0.304 0.315 Wash 250.00 0.008 0.322 52.74 48.51 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.57 1 12.92 96.50 0.001429847 0.00143 0.047 0.03 12.68 18.38 2 19.97 95.48 0.004664847 0.00609 0.108 0.09 41.44 60.08 3 28.03 95.55 0.007750097 0.01384 0.167 0.15 69.15 100.26 Filtrate 35.99 102.56 0.1599 0.14 Wash 250.00 0.0022325 0.14 66.71 96.71 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 0.00 105.57 1 12.92 96.50 0.001355 0.00136 0.0261515 0.02 10.21 13.39 2 19.97 95.48 0.0013575 0.00271 0.02592282 0.02 10.75 14.09 3 28.03 95.55 0.0019775 0.00469 0.037790025 0.04 17.01 . 22.30 Filtrate 35.99 102.56 0.04 0.04 Wash 250.00 0.00 0.04 17.77 23.30 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 0.0000 105.57 1 12.92 96.50 0.000005 0.00001 0.0000965 0.00 0.01 0.02 2 19.97 95.48 0.0000125 0.00002 0.0002387 0.00 1.35 1.97 3 28.03 95.55 0.0000275 0.00005 0.000525525 0.00 4.05 5.93 Filtrate 35.99 102.56 0.00 0.00 Wash 250.00 0.00 0.00 -0.45 -0.66 Moderate Thermophiles, 2 g Enargite, P 8 0 of 37 microns Test UB9-T37 Moderate Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E h (mV) (mL) Added (mL) Water (g) Mass (g) 4-Jun 12:25 0.00 245.00 1.58 482 702 7-Jun 10:40 2.93 236.45 1.77 426 646 9.41 245.86 10-Jun 10:50 5.93 237.81 1.77 466 686 8.21 246.02 13-Jun 11:30 8.96 238.27 1.75 505 725 7.40 245.67 17-Jun 10:25 12,92 234.84 1.65 535 755 11.19 246.03 18-Jun 11:20 13.95 243.38 1.59 546 766 5 5 20-Jun 12:15 15.99 237.46 1.45 573 793 8.53 245.99 24-Jun 11:35 19.97 235.15 1.43 599 819 11.07 246.22 26-Jun 12:55 22.02 240.40 1.36 615 835 5 5 4.92 245.32 28-Jun 12:50 24.02 239.77 1.48 616 836 5.77 245.54 2-Jul 13:10 28.03 234.11 1.48 620 840 11.28 245.39 4-Jul 13:20 30.04 239.63 1.35 629 849 5 5 6.06 245.69 9-Jul 11:45 34.97 231.06 1.43 623 843 15.11 246.17 10-Jul 12:15 35.99 243.43 1.47 620 840 Enargite In (g): 2.00 Total Water (g): 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) i^... * ' 1.20 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 2163.55 543.90 336.5 0.5 #2 2158.40 1009.60 302.0 0.5 #3 2320.85 1222.65 360.0 1.0 PLS (mg/L) 2489.35 949.10 276.0 Wash (mg/L) 26.26 3.25 0.6 Solid Residue (wt % 33 0.7962 12 0.5 Weight of Element Copper Iron Arsenic Antimony Head (g) 0.648 0.144 0.24 0.0078 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.0191 0 0 Samples (g): #1 0.010818 0.00272 0.001683 0.0000025 #2 0.010792 0.00505 0.00151 0.0000025 #3 0.011604 0.00611 0.0018 0.000005 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.2561 0.0976 0.0284 0.0000 Wash (g) 0.006565 0.00081 0.00015 0 Solid Residue (g) 0.396 0.00955 0.144 0.006 Calculated Head (g 0.666 0.080 0.173 0.006 % Difference -2.729 44.579 27.942 24.167 % Extraction Calculated Head 40.51 88.03 16.73 -1.44 Measured Head 41.62 48.79 12.06 -1.09 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 0.00 105.64 1 12.92 95.48 0.01081775 0.01082 0.207 0.180 27.84 27.10 2 19.97 95.79 0.010792 0.02161 0.207 0.191 29.54 28.75 3 28.03 94.75 0.01160425 0.03321 0.220 0.215 33.23 32.35 Filtrate 35.99 102.87 0.256 0.263 Wash 250.00 0.007 0.270 41.62 40.51 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.64 1 12.92 95.48 0.001715097 0.00172 0.052 0.03 22.20 40.06 2 19.97 95.79 0.004043597 0.00576 0.097 0.08 53.30 96.17 3 28.03 94.75 0.005108847 0.01087 0.116 0.10 66.59 120.15 Filtrate 35.99 102.87 0.0976 0.08 Wash 250.00 0.0008125 0.08 54.50 98.34 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 0.00 105.64 1 12.92 95.48 0.0016825 0.00168 0.03212902 0.03 11.47 15.92 2 19.97 95.79 0.00151 0.00319 0.02892858 0.03 10.84 15.04 3 28.03 94.75 0.0018 0.00499 0.03411 0.03 13.63 18.91 Filtrate 35.99 102.87 0.03 0.03 Wash 250.00 0.00 0.03 12.06 16.73 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 0.0000 105.64 1 12.92 95.48 0.0000025 0.00000 0.00004774 0.00 -0.61 -0.80 2 19.97 95.79 0.0000025 0.00001 0.000047895 0.00 -0.57 -0.75 3 28.03 94.75 0.000005 0.00001 0.00009475 0.00 0:06 0.08 Filtrate 35.99 - 102.87 0.00 0.00 Wash 250.00 0.00 0.00 -1.09 -1.44 Moderate Thermophiles, 3.5 g Enargite, P 8 0 of 10 microns Test UB6-T10 Moderate Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E h (mV) (mL) Added (mL) Water (g) Mass (g) 4-Jun 12:20 0.00 241.36 1.66 489 709 7-Jun 10:30 2.92 234.12 1.85 393 613 8.12 242.24 10-Jun 10:40 5.93 234.14 1.74 434 654 8.10 242.24 13-Jun 11:25 8.96 234.78 1.76 465 685 7.28 242.06 17-Jun 10:15 12.91 232.15 1.63 495 715 13.67 245.82 18-Jun 11:15 13.95 242.92 1.47 487 707 5 5 20-Jun 12:05 15.99 237.55 1.33 503 723 5.75 243.30 24-Jun 11:20 19.96 233.25 1.36 525 745 8.31 241.56 26-Jun 12:35 22.01 236.35 1.30 516 736 5 5 8.48 244.83 28-Jun 12:45 24.02 238.81 1.37 543 763 3.69 242.50 2-Jul 13:00 28.03 232.31 1.34 571 791 10.70 243.01 4-Jul 13:05 30.03 237.87 1.21 598 818 5 5 5.18 243.05 9-Jul 11:20 34.96 230.46 1.28 624 844 11.49 241.95 10-Jul 12:05 35.99 239.25 1.31 627 847 Enargite In (g): Total Water (g): 3.50 90.77 Vol (mL) Mass (g) Flask Weight (g): 132.14 Innoculum in: 10 10 Medium in: 95.01 95.01 Total Final Weight (g): 239.25 Filtrate Volume (mL) 102.94 Wash Volume (mL) 240 Solid Residue (g) 1.39 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 4223.50 541.35 516.5 #2 5819.10 1417.50 641.0 1.0 #3 5726.85 2477.70 795.5 5.5 PLS (mg/L) 5961.50 2862.50 893.5 Wash (mg/L) 65.79 10.29 0.4 Solid Residue (wt % 33 1.7145 12 0.7 .. v ,. . Weight of Element Copper Iron Arsenic Antimony Head (g) 1.092 0.406 0.3675 0.01925 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.01909 0 0 Samples (g): #1 0.021118 0.00271 0.002583 0 #2 0.029096 0.00709 0.003205 0.000005 #3 0.028634 0.01239 0.003978 0.0000275 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.6137 0.2947 0.0920 0.0000 Wash (g) 0.01579 0.00247 0.000096 0 Solid Residue (g) 0.4587 0.02383 0.1668 0.00973 Calculated Head (g 1.141 0.301 0.264 0.010 % Difference -4.473 25.840 28.152 49.779 % Extraction Calculated Head 59.79 92.08 36.83 -0.65 Measured Head 62.47 68.29 26.46 -0.32 177 Copper Output Tot. Cu Sample # Time (days) Sol'n Vol. (n nL) g Cu sampled Sampled (g) Cu in sol'n (g) Cu(aq) total (g) %Cu indicated %Cu actual 0.00 105.72 1 12.91 96.51 0.0211175 0.02112 0.408 0.381 34.93 33.43 2 19.96 97.61 0.0290955 0.05021 0.568 0.563 51.55 49.34 3 28.03 96.67 0.02863425 0.07885 0.554 0.578 52.90 50.63 Filtrate 35.99 102.94 0.614 0.666 Wash 240.00 0.016 0.682 62.47 59.79 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.72 1 12.91 96.51 0.001702347 0.00170 0.052245689 0.03 7.95 10.72 2 19.96 97.61 0.006083097 0.00779 0.138362175 0.12 29.16 39.32 3 28.03 96.67 0.011384097 0.01917 0.239519259 0.22 54.08 72.92 Filtrate 35.99 102.94 0.2947 0.27 Wash 240.00 0.0024696 0.28 68.27 92.06 Arsenic Output Sample # Time (days) Sol'n Vol. (n nL) g As sampled Tot. As Sample As in sol'n (g) As(aq)total %As indicated %As actual 0.00 105.72 1 12.91 96.51 0.0025825 0.00258 0.049847415 0.05 12.31 17.14 2 19.96 97.61 0.003205 0.00579 0.06256801 0.06 16.48 22.93 3 28.03 96.67 0.0039775 0.00977 0.076900985 0.08 21.25 29.58 Filtrate 35.99 102.94 0.09 0.10 Wash 240.00 0.00 • 0.10 26.46 36.83 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 0.0000 105.72 1 12.91 96.51 0 0.00000 0 0.00 -0.49 -0.98 2 19.96 97.61 0.000005 0.00001 0.00009761 0.00 0.01 0.03 3 28.03 96.67 0.0000275 0.00003 0.000531685 0.00 2.29 4.57 Filtrate 35.99 102.94 0.00 0.00 Wash 240.00 0.00 0.00 -0.32 -0.65 Moderate Thermophiles, 3.5 g Enargite, P 8 0 of 15 microns Test #B6-T15 Moderate Thermophiles Date Hour Time (days) Initial Mass (g) pH E„ (Ag/AgCI) E h (mV) Sample (mL) Medium Added (mL) Added Water (g) Final Mass (g) 4-Jun 12:20 0.00 253.98 1.63 453 673 7-Jun 10:30 2.92 246.33 1.89 383 603 7.99 254.32 10-Jun 10:40 5.93 246.22 1.91 421 641 7.76 253.98 13-Jun 11:25 8.96 245.65 1.88 466 686 8.70 254.35 17-Jun 10:15 12.91 243.22 1.78 493 713 11.68 254.90 18-Jun 11:15 13.95 252.16 1.62 514 734 5 5 20-Jun 12:05 15.99 245.95 1.48 519 739 8.20 254.15 24-Jun 11:20 19.96 243.34 1.47 557 777 10.88 254.22 26-Jun 12:35 22.01 249.08 1.40 577 797 5 5 5.85 254.93 28-Jun 12:45 24.02 249.83 1.42 581 801 4.82 254.65 2-Jul 13:00 28.03 243.05 1.40 589 809 9.87 252.92 4-Jul 13:05 30.03 247.55 1.27 624 844 5 5 6.84 254.39 9-Jul 11:20 34.96 241.36 1.35 618 838 13.09 254.45 10-Jul 12:05 35.99 251.81 1.35 631 851 Enargite In (g): Total Water (g): 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 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 3679.80 446.95 354.0 #2 4512.85 1530.30 472.0 3.0 #3 4727.00 2966.35 811.5 15.5 PLS (mg/L) 4696.15 2842.10 677.0 Wash (mg/L) 64.98 15.35 0.7 Solid Residue (wt % 36 0.9415 13 0.8 :*:.T .. ' • Weight of Element Copper Iron Arsenic Antimony Head (g) 1.064 0.371 0.3675 0.01925 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.01909 0 0 Samples (g): #1 0.018399 0.00223 0.00177 0 #2 0.022564 0.00765 0.00236 0.000015 #3 0.023635 0.01483 0.004058 0.0000775 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.4803 0.2907 0.0692 0.0000 Wash (g) 0.016245 0.00384 0.000175 0 Solid Residue (g) 0.6048 0.01582 0.2184 0.01344 ' <''''?; Calculated Head (g) 1.140 0.293 0.291 0.013 % Difference -7.119 21.034 20.706 30.195 % Extraction ' -Calculated Head 46.94 94.60 25.05 -0.02 Measured Head 50.28 74.70 19.87 -0.01 179 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 0.00 135.65 1 12.91 124.89 0.018399 0.01840 0.460 0.433 40.73 38.03 2 19.96 125.01 0.02256425 0.04096 0.564 0.556 52.29 48.82 3 28.03 124.72 0.023635 0.06460 0.590 0.604 56.80 53.02 Filtrate 35.99 102.27 0.480 0.519 Wash 250.00 0.016 0.535 50.28 46.94 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 135.65 1 12.91 124.89 0.001230347 0.00123 0.056 0.04 9.66 12.24 2 19.96 125.01 0.006647097 0.00788 0.191 0.17 46.18 58.48 3 28.03 124.72 0.013827347 0.02170 0.370 0.35 94.34 119.47 Filtrate 35.99 102.27 0.2907 0.27 Wash 250.00 0.0038375 0.27 74.00 93.71 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 0.00 135.65 1 12.91 124.89 0.00177 0.00177 0.04421106 0.04 10.78 13.59 2 19.96 125.01 0.00236 0.00413 0.05900472 0.06 15.29 19.28 3 28.03 124.72 0.0040575 0.00819 0.10121028 0.10 27.41 34.57 Filtrate 35.99 102.27 0.07 0.07 Wash 250.00 0.00 0.07 19.87 25.05 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 0.0000 135.65 1 12.91 124.89 0 0.00000 0 0.00 -0.49 -0.71 2 19.96 125.01 0.000015 0.00002 0.00037503 0.00 1.45 2.08 3 28.03 124.72 0.0000775 0.00009 0.00193316 0.00 9.63 13.79 Filtrate 35.99 102.27 0.00 0.00 Wash 250.00 0.00 0.00 -0.01 -0.02 0 Moderate Thermophiles, 3.5 g Enargite, P 8 0 of 37 microns Test UB6-T37 Moderate Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E h (mV) (mL) Added (mL) Water (g) Mass (g) 4-Jun 12:20 0.00 240.21 1.61 491 711 7-Jun 10:30 2.92 231.88 1.81 407 627 9.77 241.65 10-Jun 10:40 5.93 233.10 1.80 441 661 7.45 240.55 13-Jun 11:25 8.96 231.76 1.78 468 688 8.70 240.46 17-Jun 10:15 12.91 228.54 1.71 485 705 13.53 242.07 18-Jun 11:15 13.95 238.99 1.59 497 717 5 5 20-Jun 12:05 15.99 232.34 1.47 509 729 10.04 242.38 24-Jun 11:20 19.96 229.05 1.48 535 755 11.98 241.03 26-Jun 12:35 22.01 234.47 1.39 567 787 5 5 10.91 245.38 28-Jun 12:45 24.02 239.83 1.49 572 792 1.99 241.82 2-Jul 13:00 28.03 229.92 1.48 579 799 12.12 242.04 4-Jul 13:05 30.03 236.29 1.32 613 833 5 5 4.64 240.93 9-Jul 11:20 34.96 225.69 1.40 603 823 15.07 240.76 10-Jul 12:05 35.99 237.57 1.39 621 841 Enargite In (g): 3.51 Total Water (g): 106.20 Vol (mL) Mass (g) Flask Weight (g): • • • 130.98 Innoculum in: 10 10 Medium in: 95.13 95.13 Total Final Weight (g): 237.57 Filtrate Volume (mL) 100.88 Wash Volume (mL) 245 Solid Residue (g) 2.20 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 3178.15 334.70 524.0 1.0 #2 4144.35 680.60 531.0 0.0 #3 4113.25 1244.60 532.0 0.0 PLS (mg/L) 4257.50 1527.25 503.0 Wash (mg/L) 54.09 5.41 0.7 Solid Residue (wt % 32 2.2206 12 0.5 Weight of Element Copper Iron Arsenic Antimony Head (g) 1.13724 0.25272 0.4212 0.013689 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.01911 0 0 Samples (g): #1 0.015891 0.00167 0.00262 0.000005 #2 0.020722 0.0034 0.002655 0 #3 0.020566 0.00622 0.00266 0 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 o.ooi 0 0 PLS (g) 0.4295 0.1541 0.0507 0.0000 Wash (g) 0.013252 0.00133 0.000172 0 Solid Residue (g) 0.704 0.04885 0.264 0.011 Calculated Head (g 1.178 0.173 0.318 0.011 % Difference -3.563 31.362 24.441 20.301 % Extraction Calculated Head 40.23 71.84 17.05 -0.82 Measured Head 41.66 49.31 12.88 -0.66 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 0.00 105.72 1 12.91 94.05 0.01589075 0.01589 0.299 0.273 23.98 23.16 2 19.96 94.56 0.02072175 0.03661 0.392 0.382 33.56 32.40 3 28.03 95.43 0.02056625 0.05718 0.393 0.403 35.43 34.21 Filtrate 35.99 100.88 0.429 0.461 Wash 245.00 0.013 0.474 41.66 40.23 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.72 1 12.91 94.05 0.000669097 0.00067 0.031478535 0.01 4.56 6.64 2 19.96 94.56 0.002398597 0.00307 0.064357536 0.04 17.57 25.59 3 28.03 95.43 0.005218597 0.00829 0.118772178 0.10 39.10 56.96 Filtrate 35.99 100.88 0.1541 0.13 Wash 245.00 0.00132545 0.14 53.59 78.08 Arsenic Output Sample # Time (days) Sol'n Vol. (n g As sampled Tot. As Sample As in sol'n (g) As(aq)total %As indicated %As actual 0.00 105.72 1 12.91 94.05 0.00262 0.00262 0.0492822 0.04 10.61 14.04 2 19.96 94.56 0.002655 0.00528 0.05021136 0.05 11.45 15.16 3 28.03 95.43 0.00266 0.00794 0.05076876 0.05 12.21 16.17 Filtrate 35.99 100.88 0.05 0.05 Wash 245.00 0.00 0.05 12.88 17.05 Antimony Output Sample # Time (days) Sol'n Vol. (n g Sb sampled Tot. Sb Sample Sb in sol'n (g) Sb(aq) total %Sb indicated %Sb actual 0.0000 105.72 1 12.91 94.05 0.000005 0.00001 0.00009405 0.00 -0.01 -0.01 2 19.96 94.56 0 0.00001 0 0.00 -0.66 -0.82 3 28.03 95.43 0 0.00001 0 0.00 -0.66 -0.82 Filtrate 35.99 100.88 0.00 0.00 Wash 245.00 0.00 0.00 -0.66 -0.82 Moderate Thermophiles, 5 g Enargite, P 8 0 of 10 microns Test UB8-T10 Moderate Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 4-Jun 12:25 0.00 243.35 1.60 483 703 7-Jun 10:35 2.92 236.49 1.86 379 599 7.56 244.05 10-Jun 10:45 5.93 236.64 1.89 417 637 7.36 244.00 13-Jun 11:30 8.96 236.71 1.87 449 669 7.26 243.97 17-Jun 10:20 12,91 232.47 1.65 471 691 11.70 244.17 18-Jun 11:20 13.95 241.70 1.55 472 692 5 5 20-Jun 12:15 15.99 236.50 1.38 484 704 7.73 244.23 24-Jun 11:30 19.96 234.59 1.36 496 716 9.19 243.78 26-Jun 12:50 22.02 238.52 1.25 506 726 5 5 5.84 244.36 28-Jun 12:50 24.02 239.63 1.37 523 743 5.72 245.35 2-Jul 13:05 28.03 235.59 1.30 545 765 8.49 244.08 4-Jul 13:15 30.03 239.08 1.20 561 781 5 5 5.10 244.18 9-Jul 11:40 34.97 232.28 1.25 589 809 11.21 243.49 10-Jul 12:10 35.99 241.16 1.22 599 819 Enargite In (g): 5.00 Total Water (g): 87.16 Vol (mL) Mass (g) Flask Weight (g): . •• w v - 132.73 Innoculum in: 10 10 Medium in: 95.11 95.11 Total Final Weight (g): 241.16 Filtrate Volume (mL) 103.16 '' * j * Wash Volume (mL) 250 , ' •?i<# Solid Residue (g) 2.20 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 5048.80 572.85 621.5 #2 7181.90 1253.50 970.5 1.0 #3 7490.30 2480.95 1190.5 5.5 P L S (mg/L) 8639.60 3762.60 1460.5 Wash (mg/L) 91.98 14.84 1.8 Solid Residue (wt °/< 32 3.2272 12 0.6 I,: - '-u.<;».>.•.. • •'-"i%s-. , . \ ' V ' •• ' ' ••' -'<r» • - . • • '*!, ';*' •• -Weight of Element Copper Iron Arsenic Antimony Head (g) 1.56 0.58 0.525 0.0275 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.01911 0 0 Samples (g): #1 0.025244 0.00286 0.003108 0 #2 0.03591 0.00627 0.004853 0.000005 #3 0.037452 0.0124 0.005953 0.0000275 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 P L S (g) 0.8913 0.3881 0.1507 0.0000 Wash (g) 0.022995 0.00371 0.00045 0 Solid Residue (g) 0.704 0.071 0.264 0.0132 Calculated Head (g; 1.691 0.442 0.424 0.013 % Difference -8.377 23.739 19.156 52.227 % Extraction , ~'?K , " . V Calculated Head 58.36 83.95 37.80 -0.48 Measured Head 63.25 64.02 30.56 -0.23 183 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 0.00 105.62 1 12.91 94.74 0.025244 0.02524 0.478 0.452 28.98 26.74 2 19.96 96.86 0.0359095 0.06115 0.696 0.695 44.53 41.09 3 28.03 97.86 0.0374515 0.09861 0.733 0.768 49.23 45.42 Filtrate 35.99 103.16 0.891 0.964 Wash 250.00 0.023 0.987 63.25 58.36 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.62 1 12.91 94.74 0.001859847 0.00186 0.054271809 0.03 5.92 7.76 2 19.96 96.86 0.005263097 0.00712 0.12141401 0.10 17.49 22.94 3 28.03 97.86 0.011400347 0.01852 0.242785767 0.22 38.42 50.38 Filtrate 35.99 103.16 0.3881 0.37 Wash 250.00 0.00371 0.37 64.12 84.08 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 0.00 105.62 1 12.91 94.74 0.0031075 0.00311 0.05888091 0.05 10.34 12.79 2 19.96 96.86 0.0048525 0.00796 0.09400263 0.09 17.62 21.80 3 28.03 97.86 0.0059525 0.01391 0.11650233 0.12 22.83 28.24 Filtrate 35.99 103.16 0.15 0.16 Wash 250.00 0.00 0.16 30.56 37.80 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 0.0000 105.62 1 12.91 94.74 0 0.00000 0 0.00 -0.35 -0.72 2 19.96 96.86 0.000005 0.00001 0.00009686 0.00 0.01 0.01 3 28.03 97.86 0.0000275 0.00003 0.00053823 0.00 1.63 3.41 Filtrate 35.99 103.16 0.00 0.00 Wash 250.00 0.00 0.00 -0.23 -0.48 Moderate Thermophiles, 5 g Enargite, P 8 0 of 15 microns Test#B8-T15 Moderate Thermophiles Time Initial E h Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E h(mV) (mL) Added (mL) Water (g) Mass (g) 4-Jun 12:25 0.00 226.70 1.59 480 700 7-Jun 10:35 2.92 220.46 1.95 387 607 7.67 228.13 10-Jun 10:45 5.93 221.91 2.04 408 628 4.95 226.86 13-Jun 11:30 8.96 220.49 2.04 430 650 6.39 226.88 17-Jun 10:20 12.91 218.97 1.91 458 678 8.67 227.64 18-Jun 11:20 13.95 225.65 1.80 459 679 5 5 20-Jun 12:15 15.99 221.00 1.63 477 697 8.35 229.35 24-Jun 11:30 19.96 220.89 1.57 508 728 6.37 227.26 26-Jun 12:50 22.02 223.11 1.41 525 745 5 5 4.44 227.55 28-Jun 12:50 24.02 223.52 1.50 537 757 3.41 226.93 2-Jul 13:05 28.03 218.64 1.40 579 799 8.41 227.05 4-Jul 13:15 30.03 222.94 1.25 599 819 5 5 4.73 227.67 9-Jul 11:40 34.97 217.08 1.28 613 833 11.05 228.13 10-Jul 12:10 35.99 226.10 1.31 614 834 Enargite In (g): Total Water (g): 5.00 74.44 Vol(mL) Mass(g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) 10 95.02 116.25 10 95.02 226.10 104.53 250 ' >*'"'.''' 2.54 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.20088 0 0 Samples (mg/L): #1 3508.00 373.75 224.5 1.5 #2 5614.75 781.45 592.0 #3 6073.25 2643.10 874.0 7.0 PLS (mg/L) 6831.40 3623.25 1020.0 Wash (mg/L) 101.63 19.33 0.5 Solid Residue (wt % 34 2.8748 12 0.7 BMBRUV'- »:."* •' " t" Weight of Element Copper Iron Arsenic Antimony Head (g) 1.52 0.53 0.525 0.0275 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.01909 0 0 Samples (g): #1 0.01754 0.00187 0.001123 0.0000075 #2 0.028074 0.00391 0.00296 0 . #3 0.030366 0.01322 0.00437 0.000035 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.7141 0.3787 0.1066 0.0000 . Wash (g) 0.025408 0.00483 0.000125 0 Solid Residue (g) 0.8636 0.07302 0.3048 0.01778 V ; ^ % . ' - V ' • ''" -Calculated Head (g 1.653 0.434 0.415 0.018 % Difference -8.744 18.204 20.876 35.536 % Extraction : •' \ T ^ / : ; • * * .-;.*''.• >•.: Calculated Head 47.75 83.16 26.63 -0.30 Measured Head 51.93 68.02 21.07 -0.19 185 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 0.00 105.45 1 12.91 97.72 0.01754 0.01754 0.343 0.317 20.83 19.16 2 19.96 99.64 0.02807375 0.04561 0.559 0.551 36.24 33.32 3 28.03 97.39 0.03036625 0.07598 0.591 0.611 40.19 36.96 Filtrate 35.99 104.53 0.714 0.764 Wash 250.00 0.025 0.789 51.93 47.75 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.45 1 12.91 97.72 0.000864347 0.00086 0.037 0.02 3.12 3.82 2 19.96 99.64 0.002902847 0.00377 0.078 0.06 10.92 13.36 3 28.03 97.39 0.012211097 0.01598 0.257 0.24 44.80 54.77 Filtrate 35.99 104.53 0.3787 0.36 Wash 250.00 0.0048325 0.36 68.61 83.87 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 0.00 105.45 1 12.91 97.72 0.0011225 0.00112 0.02193814 0.02 3.30 4.18 2 19.96 99.64 0.00296 0.00408 0.05898688 0.06 10.57 13.36 3 28.03 97.39 0.00437 0.00845 0.08511886 0.08 16.12 20.37 Filtrate 35.99 104.53 0.11 0.11 Wash 250.00 0.00 0.11 21.07 26.63 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 0.0000 105.45 1 12.91 97.72 0.0000075 . 0:00001 0.00014658 0.00 0.19 0.29 2 19.96 99.64 0 0.00001 0 0.00 -0.32 -0.49 3 28.03 97.39 0.000035 0.00004 0.00068173 0.00 2.16 3.35 Filtrate 35.99 104.53 0.00 0.00 Wash 250.00 0.00 0.00 -0.19 -0.30 Moderate Thermophiles, 5 g Enargite, P 8 0 of 37 microns Test UB8-T37 Moderate Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E h(mV) (mL) Added (mL) Water (g) Mass (g) 4-Jun 12:25 0.00 228.40 1.59 488 708 7-Jun 10:35 2.92 222.14 1.87 396 616 23.05 245.19 10-Jun 10:45 5.93 238.90 1.90 435 655 13-Jun 11:30 8.96 232.43 1.82 450 670 17-Jun 10:20 12.91 224.08 1.78 462 682 8.65 232.73 18-Jun 11:20 13.95 230.53 1.68 462 682 5 5 20-Jun 12:15 15.99 226.12 1.55 477 697 6.72 232.84 24-Jun 11:30 19.96 224.29 1.52 498 718 4.30 228.59 26-Jun 12:50 22.02 224.40 1.39 509 729 5 5 4.60 229.00 28-Jun 12:50 24.02 224.75 1.51 523 743 3.73 228.48 2-Jul 13:05 28.03 219.53 1.45 549 769 9.82 229.35 4-Jul 13:15 30.03 225.12 1.29 586 806 5 5 4.44 229.56 9-Jul 11:40 34.97 217.88 1.32 609 829 11.36 229.24 10-Jul 12:10 35.99 227.19 1.34 603 823 Enargite In (g): 5.02 Total Water (g): 76.67 Vol (mL) Mass (g) Flask Weight (g): :•" 117.83 Innoculum in: 10 10 Medium in: 95.05 95.05 Total Final Weight (g): ,-y, f g 227.19 Filtrate Volume (mL) 102.51 Wash Volume (mL) 250 Solid Residue (g) 3.26 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 2617.25 1996.30- 459.5 9.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 2857.85 276.60 426.5 #2 4371.40 411.75 753.0 #3 5325.75 1036.55 809.5 P L S (mg/L) 6175.90 1830.80 749.0 Wash (mg/L) 73.20 5.07 0.8 Solid Residue (wt % 32 2.9224 12 0.4 Weight of Element Copper Iron Arsenic Antimony Head (g) 1.62648 0.36144 0.6024 0.019578 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.01909 0 0 Samples (g): #1 0.014289 0.00138 0.002133 0 #2 0.021857 0.00206 0.003765 0 #3 0.026629 0.00518 0.004048 0 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 P L S (g) 0.6331 0.1877 0.0768 0.0000 Wash (g) 0.0183 0.00127 0.0002 0 Solid Residue (g) 1.0432 0.09527 0.3912 0.01304 . •• • v - - . • . . -<• . Calculated Head (g 1.731 0.251 0.474 0.013 % Difference -6.438 30.620 21.393 33.880 % Extraction ; ' . • •- '." - . . . . Calculated Head 39.74 62.01 17.39 -0.73 Measured Head 42.30 43.02 13.67 -0.49 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 0.00 105.55 1 12.91 101.23 0.01428925 0.01429 0.289 0.263 16.18 15.20 2 19.96 101.44 0.021857 0.03615 0.443 0.432 26.53 24.93 3 28.03 96.68 0.02662875 0.06278 0.515 0.525 32.27 30.32 Filtrate 35.99 102.51 0.633 0.670 Wash 250.00 0.018 0.688 42.30 39.74 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.55 1 12.91 101.23 0.000378597 0.00038 0.028 0.01 2.22 3.21 2 19.96 101.44 0.001054347 0.00143 0.042 0.02 6.03 8.70 3 28.03 96.68 0.004178347 0.00561 0.100 0.08 22.20 32.00 Filtrate 35.99 102.51 0.1877 0.17 Wash 250.00 0.0012675 0.17 46.75 67.39 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 0.00 105.55 1 12.91 101.23 0.0021325 0.00213 0.043174595 0.04 6.40 8.15 2 19.96 101.44 0.003765 0.00590 0.07638432 0.07 12.27 15.61 3 28.03 96.68 0.0040475 0.00995 0.07826246 0.08 13.21 16.80 Filtrate 35.99 102.51 0.08 0.08 Wash 250.00 0.00 0.08 13.67 17.39 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 0.0000 105.55 1 12.91 101.23 0 0.00000 0 0.00 -0.49 -0.73 2 19.96 101.44 0 0.00000 0 0.00 -0.49 -0.73 3 28.03 96.68 0 0.00000 0 0.00 -0.49 -0.73 Filtrate 35.99 102.51 0.00 0.00 Wash 250.00 0.00 0.00 -0.49 -0.73 Moderate Thermophiles, 10 g Enargite, P 8 0 of 10 microns Test#B7-T10 Moderate Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E h (mV) (mL) Added (mL) Water (g) Mass (g) 4-Jun 12:25 0.00 232.54 1.62 446 666 7-Jun 10:30 2.92 226.51 2.04 376 596 6.26 232.77 10-Jun 10:45 5.93 226.48 2.05 394 614 7.41 233.89 13-Jun 11:25 8.96 228.26 1.99 425 645 4.83 233.09 17-Jun 10:20 12.91 225.67 1.79 442 662 7.54 233.21 18-Jun 11:15 13.95 231.25 1.66 450 670 5 5 20-Jun 12:10 15.99 227.36 1.48 463 683 6.50 233.86 24-Jun 11:25 19.96 226.08 1.37 469 689 6.55 232.63 26-Jun 12:45 22.01 228.83 1.27 469 689 5 5 4.24 233.07 28-Jun 12:45 24.01 229.41 1.32 480 700 4.03 233.44 2-Jul 13:00 28.02 225.68 1.30 496 716 7.53 233.21 4-Jul 13:10 30.03 228.87 1.15 494 714 5 5 4.26 233.13 9-Jul 11:20 34.95 223.75 1.20 519 739 11.41 235.16 10-Jul 12:10 35.99 233.03 1.18 527 747 Enargite In (g): 10.00 Total Water (g): 70.56 Vol (mL) Mass (g) Flask Weight (g): • 116.91 Innoculum in: 10 10 Medium in: 95.07 95.07 Total Final Weight (g): ; s -: 233.03 Filtrate Volume (mL) 105.61 V; ' ,* Wash Volume (mL) 250 Solid Residue (g) ' '. 1 6.25 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 5968.50 546.25 300.0 0.5 #2 9886.45 1236.35 1205.0 1.0 #3 12384.60 2387.90 1904.0 5.0 P L S (mg/L) 14906.80 2991.25 2317.5 Wash (mg/L) 247.96 16.39 7.7 Solid Residue (wt °/< 27 11 11 0.6 „ ! * " " • Weight of Element Copper Iron Arsenic Antimony Head (g) 3.12 1.16 1.05 0.055 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.0191 0 0 Samples (g): #1 0.029843 0.00273 0.0015 0.0000025 #2 0.049432 0.00618 0.006025 0.000005 #3 0.061923 0.01194 0.00952 0.000025 Medium Added (g): #1 0 0.001 0 0 #2 ' 0 0.001 0' 0 #3 0 0.001 0 0 P L S (g) 1.5743 0.3159 0.2448 0.0000 Wash (g) 0.06199 0.0041 0.001925 0 Solid Residue (g) 1.6875 0.6875 0.6875 0.0375 111*-., v- • ' !:BIi..>>... .,MI»<J '-<-*>;S Calculated Head (g; 3.439 0.986 0.947 0.037 % Difference -10.219 14.976 9.845 31.932 % Extraction 'is Calculated Head 50.93 30.29 27.37 -0.17 Measured Head 56.13 25.76 24.68 -0.11 189 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 0.00 105.63 1 12.91 98.76 0.0298425 0.02984 0.589 0.563 18.05 16.38 2 19.96 99.17 0.04943225 0.07927 0.980 0.984 31.54 28.62 3 28.02 98.77 0.061923 0.14120 1.223 1.276 40.91 37.12 Filtrate 35.99 105.61 1.574 1.689 Wash 250.00 0.062 1.751 56.13 50.93 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.63 1 12.91 98.76 0.001726847 0.00173 0.05394765 0.03 2.93 3.45 2 19.96 99.17 0.005177347 0.00690 0.12260883 0.10 8.85 10.41 3 28.02 98.77 0.010935097 0.01784 0.235852883 0.22 18.61 21.89 Filtrate 35.99 105.61 0.3159 0.30 Wash 250.00 0.0040975 0.30 25.87 30.42 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 0.00 105.63 1 12.91 98.76 0.0015 0.00150 0.029628 0.03 2.38 2.64 2 19.96 99.17 0.006025 0.00753 0.11949985 0.12 11.09 12.30 3 28.02 98.77 0.00952 0.01705 0.18805808 0.19 18.19 20.18 Filtrate 35.99 105.61 0.24 0.26 Wash 250.00 0.00 0.26 24.68 27.37 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 0.0000 105.63 1 12.91 98.76 0.0000025 0.00000 0.00004938 0.00 -0.08 -0.12 2 19.96 99.17 0.000005 0.00001 0.00009917 0.00 0.01 0.02 3 28.02 98.77 0.000025* 0.00003 0.00049385 0.00 0.74 1.09 Filtrate 35.99 105.61 . - 0.00 0.00 Wash 250.00 0.00 0.00 -0.11 -0.17 Moderate Thermophiles, 10 g Enargite, P 8 0 of 15 microns Test#B7-T15 Moderate Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E h(mV) (mL) Added (mL) Water (g) Mass (g) 4-Jun 12:25 0.00 231.19 1.63 462 682 7-Jun 10:30 2.92 225.19 2.31 362 582 7.27 232.46 10-Jun 10:45 5.93 225.95 2.34 368 588 6.70 232.65 13-Jun 11:25 8.96 226.34 2.36 385 605 5.67 232.01 17-Jun 10:20 12.91 223.21 2.25 402 622 9.16 232.37 18-Jun 11:15 13.95 230.31 2.13 428 648 5 5 20-Jun 12:10 15.99 226.09 1.92 456 676 6.77 232.86 24-Jun 11:25 19.96 225.03 1.65 488 708 6.26 231.29 26-Jun 12:45 22.01 227.31 1.42 492 712 5 5 4.45 231.76 28-Jun 12:45 24.01 227.99 1.49 512 732 2-Jul 13:00 28.02 219.96 1.37 536 756 11.82 231.78 4-Jul 13:10 30.03 227.85 1.24 545 765 - 5 5 4.07 231.92 9-Jul 11:20 34.95 221.77 1.31 556 776 10.39 232.16 10-Jul 12:10 35.99 230.28 1.23 566 786 Enargite In (g): Total Water (g): 10.00 72.56 Vol (mL) Mass (g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) ; ;• .) 115.57 10 10 95.06 95.06 • • H 230 28 104.50 r 250 6.01 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.20088 0 0 Samples (mg/L): #1 4937.80 436.85 52.0 1.5 #2 8875.85 900.25 754.0 2.0 #3 10810.85 2577.10 1293.5 5.0 PLS (mg/L) 11897.30 4152.20 1601.5 Wash (mg/L) 196.61 29.01 1.8 Solid Residue (wt % 32 7.2 12 0.6 • , • ' . i • • . . Weight of Element Copper Iron Arsenic Antimony Head (g) 3.04 1.06 1.05 0.055 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.0191 0 0 Samples (g): #1 0.024689 0.00218 0.00026 0.0000075 #2 0.044379 0.0045 0.00377 0.00001 #3 0.054054 0.01289 0.006468 0.000025 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 1.2433 0.4339 0.1674 0.0000 Wash (g) 0.049153 0.00725 0.00045 0 Solid Residue (g) 1.9232 0.43272 0.7212 0.03606 Calculated Head (g 3.313 0.851 0.895 0.036 % Difference -8.966 19.681 14.771 34.532 % Extraction Calculated Head 41.94 49.17 19.41 -0.15 Measured Head 45.70 39.50 16.54 -0.10 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 0.00 105.62 1 12.91 97.64 0.024689 0.02469 0.482 0.456 15.00 13.76 2 19.96 99.46 0.04437925 0.06907 0.883 0.881 28.99 26.60 3 28.02 94.39 0.05405425 0.12312 1.020 1.063 34.98 32.10 Filtrate 35.99 104.50 1.243 1.340 Wash 250.00 0.049 1.389 45.70 41.94 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.62 1 12.91 97.64 0.001179847 0.00118 0.043 0.02 2.14 2.67 2 19.96 99.46 0.003496847 0.00468 0.090 0.07 6.56 8.17 3 28.02 94.39 0.011881097 0.01656 0.243 0.22 21.07 26.23 Filtrate 35.99 104.50 0.4339 0.41 Wash 250.00 0.0072525 0.42 39.74 49.47 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 0.00 105.62 1 12.91 97.64 0.00026 0.00026 0.00507728 0.00 0.05 0.05 2 19.96 99.46 0.00377 0.00403 0.07499284 0.07 6.73 7.90 3 28.02 94.39 0.0064675 0.01050 0.122093465 0.12 11.57 13.58 Filtrate 35.99 104.50 0.17 0.17 Wash 250.00 0.00 0.17 16.54 19.41 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 0.0000 105.62 1 12.91 97.64 0.0000075 0.00001 0.00014646 0.00 0.09 0.14 2 19.96 99.46 0.00001 0.00002 0.00019892 0.00 0.20 0.31 3 28.02 94.39 0.000025 0.00004 0.00047195 0.00 0.72 1.10 Filtrate 35.99 104.50 0.00 0.00 Wash 250.00 0.00 0.00 -0.10 -0.15 Moderate Thermophiles, 10 g Enargite, P 8 0 of 37 microns Test UB7-T37 Moderate Thermophiles Time Initial Eh Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) Eh (mV) (mL) Added (mL) Water (g) Mass (g) 4-Jun 12:25 0.00 229.31 1.74 470 690 7-Jun 10:30 2.92 226.85 1.99 379 599 3.01 229.86 10-Jun 10:45 5.93 219.52 1.97 405 625 10.29 229.81 13-Jun 11:25 8.96 223.28 1.94 435 655 8.42 231.70 17-Jun 10:20 12.91 223.28 1.82 447 667 7.66 230.94 18-Jun 11:15 13.95 228.65 1.70 447 667 5 5 20-Jun 12:10 15.99 223.87 1.57 458 678 8.60 232.47 24-Jun 11:25 19.96 223.72 1.54 477 697 6.20 229.92 26-Jun 12:45 22.01 225.31 1.39 481 701 5 5 5.29 230.60 28-Jun 12:45 24.01 226.42 1.52 496 716 4.05 230.47 2-Jul 13:00 28.02 221.94 1.44 513 733 7.98 229.92 4-Jul 13:10 30.03 225.65 1.28 517 737 5 5 4.51 230.16 9-Jul 11:20 34.95 219.36 1.32 553 773 11.98 231.34 10-Jul 12:10 35.99 229.26 1.29 560 780 Enargite In (g): 10.01 Total Water (g): 77.99 Vol (mL) Mass (g) Flask Weight (g): ; : 113.76 Innoculum in: 10 10 Medium in: 95.07 95.07 Total Final Weight (g): II 229.26 Filtrate Volume (mL) 103.13 Wash Volume (mL) 250 Solid Residue (g) . / *''f?t 7.71 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 2617.25 1996.30 459.5 9.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 4553.90 334.90 391.5 0.0 #2 6878.55 517.40 1038.5 0.0 #3 8889.30 872.70 1468.0 0.0 PLS (mg/L) 10371.40 1572.75 1278.5 Wash (mg/L) 200.02 10.56 12.8 Solid Residue (wt "A 30 6.1 12 0.4 Weight of Element Copper Iron Arsenic Antimony Head (g) 3.24324 0.72072 1.2012 0.039039 Innoculum (g) 0.0262 0.0200 0.0046 0.0001 Medium (g) 0 0.0191 0 0 Samples (g): #1 0.02277 0.00167 0.001958 0 #2 0.034393 0.00259 0.005193 0 #3 0.044447 0.00436 0.00734 0 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 1.0696 0.1622 0.1319 0.0000 ' Wash (g) 0.050005 0.00264 0.0032 0 . Solid Residue (g) 2.313 0.47031 0.9252 0.03084 Calculated Head (g) 3.508 0.602 1.070 0.031 % Difference -8.165 16.514 10.910 21.245 % Extraction Calculated Head 34.07 21.84 13.54 -0.31 Measured Head 36.85 18.23 12.07 -0.24 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 0.00 105.54 1 12.91 99.51 0.0227695 0.02277 0.453 0.427 13.17 12.17 2 19.96 99.95 0.03439275 0.05716 0.688 0.684 21.09 19.50 3 28.02 98.17 0.0444465 0.10161 0.873 0.904 27.86 25.76 Filtrate 35.99 103.13 1.070 1.145 Wash 250.00 0.050 1.195 36.85 34.07 Iron Output Sample # Time (days) Sol'n Vol. (n IL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.54 1 12.91 99.51 0.000670097 0.00067 0.033 0.01 1.85 2.22 2 • 19.96 99.95 0.001582597 0.00225 0.052 0.03 4.41 5.28 3 28.02 98.17 0.003359097 0.00561 0.086 0.07 9.12 10.92 Filtrate 35.99 103.13 0.1622 0.14 Wash 250.00 0.00264 0.14 20.10 24.08 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 0.00 105.54 1 12.91 99.51 0.0019575 0.00196 0.038958165 0.03 2.86 3.21 2 19.96 99.95 0.0051925 0.00715 0.103798075 0.10 8.42 9.45 3 28.02 98.17 0.00734 0.01449 0.14411356 0.15 12.21 13.71 Filtrate 35.99 103.13 0.13 0.14 Wash 250.00 0.00 0.14 12.07 13.54 Antimony Output Sample # Time (days) Sol'n Vol. (n nL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) Sb(aq) total %Sb indicated %Sb actual 0.0000 105.54 1 12.91 99.51 0 0.00000 0 0.00 -0.24 -0.31 2 19.96 99.95 0 0.00000 0 0.00 -0.24 -0.31 3 28.02 98.17 0 0.00000 0 0.00 -0.24 -0.31 Filtrate 35.99 103.13 0.00 0.00 Wash 250.00 0.00 0.00 -0.24 -0.31 Extreme Thermophiles, 2 g Enargite, P 8 0 of 10 microns Test UB3-E10 Extreme Thermophiles Time Initial E h Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 14-Feb 10:00 0.00 238.47 1.53 477 697 18-Feb 9:30 3.98 195.02 1.60 387 607 56.17 251.19 21-Feb 11:35 7.07 203.67 1.30 420 640 47.60 251.27 22-Feb 10:55 8.04 227.51 1.23 402 622 5 5 23.78 251.29 26-Feb 10:10 12.01 192.75 1.19 398 618 58.35 251.10 28-Feb 10:20 14.01 221.81 1.12 412 632 5 5 29.79 251.60 5-Mar 10:50 19.03 185.16 1.17 404 624 65.88 251.04 7-Mar 11:35 21.07 215.90 1.21 649 869 24.15 240.05 11-Mar 12:45 25.11 195.01 44.24 239.25 12-Mar 10:10 26.01 229.30 1.24 661 881 5 5 9.65 238.95 14-Mar 11:05 28.05 215.84 1.25 655 875 22.80 238.64 15-Mar 12:05 29.09 227.29 1.20 682 902 11.41 238.70 19-Mar 12:40 33.11 196.08 1.23 646 866 42.67 238.75 21-Mar 20:40 35.44 213.66 1.28 645 865 32.40 246.06 22-Mar 18:40 36.36 236.18 1.27 641 861 Enargite In (g): 2.00 Total Water (g): 468.89 Vol (mL) Mass (g) Flask Weight (g): 130.98 Innoculum in: 10 10 Medium in: 95.01 95.01 Total Final Weight (g) ____ 236.18 Filtrate Volume (mL) Wash Volume (mL) 250 Solid Residue (g) 0.89 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 2690.40 4107.10 255.5 18.0 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 2274.75 847.05 355.0 2.0 #2 5658.60 759.50 335.5 2.0 #3 7195.00 915.60 26.5 12.5 PLS (mg/L) 6010.55 779.35 19.0 2.0 Wash (mg/L) 76.58 6.71 Solid Residue (wt % 0.5335 17 20 0.5 , v r ' , v »•-'.': •• f ' Weight of Element Copper Iron Arsenic Antimony Head (g) 0.624 0.232 0.21 0.011 Innoculum (g) 0.0269 0.0411 0.0026 0.0002 Medium (g) 0 0.01909 0 0 Samples (g): #1 0.011374 0.00424 0.001775 0.00001 #2 0.028293 0.0038 0.001678 0.00001 #3 0.035975 0.00458 0.000133 0.0000625 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.6125 0.0794 0.0019 0.0002 Wash (g) 0.019145 0.00168 0 0 Solid Residue (g) 0.004748 0.1513 0.178 0.00445 L f * « : • V '-. i . Calculated Head (g) 0.685 0.182 0.181 0.005 % Difference -9.793 21.623 13.826 58.579 % Extraction « •;. ,., ' Calculated Head 99.31 16.79 1.64 2.33 Measured Head 109.03 13.16 1.41 0.97 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 0.00 105.49 1 8.04 94.53 0.01137375 0.01137 0.215 0.188 30.15 27.46 2 14.01 88.83 0.028293 0.03967 0.503 0.487 78.06 71.10 3 26.01 96.32 0.035975 0.07564 0.693 0.706 113.11 103.02 Filtrate 36.36 101.90 0.612 0.661 Wash 250.00 0.019 0.680 109.03 99.31 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.49 1 8.04 94.53 0.003230847 0.00323 0.080071637 0.04 16.81 21.45 2 14.01 88.83 0.002793097 0.00602 0.067466385 0.03 11.38 14.52 3 26.01 96.32 0.003573597 0.00960 0.088190592 0.05 20.31 25.91 Filtrate 36.36 101.90 0.0794 0.04 Wash 250.00 0.0016775 0.04 17.25 22.01 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 0.00 105.49 1 8.04 94.53 0.001775 0.00178 0.03355815 0.03 14.76 17.13 2 14.01 88.83 0.0016775 0.00345 0.029802465 0.03 13.82 16.04 3 26.01 96.32 0.0001325 0.00359 0.00255248 0.00 1.64 1.91 Filtrate 36.36 101.90 0.00 0.00 Wash 250.00 0.00 0.00 1.41 1.64 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 0.0000 105.49 1 8.04 94.53 0.00001 0.00001 0.00018906 0.00 0.08 0.20 2 14.01 88.83 0.00001 0.00002 0.00017766 0.00 0.07 0.17 3 26.01 96.32 0.0000625 0.00008 0.001204 0.00 9.49 22.91 Filtrate 36.36 101.90 0.00 0.00 Wash 250.00 0.00 0.00 0.97 2.33 196 Extreme Thermophiles, 2 g Enargite (2), P 8 0 of 10 microns Test #B4-E10 Extreme Thermophiles Time Initial E h Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) Eh (mV) (mL) Added (mL) Water (g) Mass (g) 4-Apr 14:40 0.00 226.63 1.57 444 664 8-Apr 13:00 3.93 196.00 1.74 419 639 32.67 228.67 12-Apr 10:15 7.82 194.53 1.56 469 689 35.19 229.72 15-Apr 11:05 10.85 203.74 1.34 501 721 23.53 227.27 16-Apr 12:00 11.89 218.58 1.22 566 786 5 5 9.80 228.38 18-Apr 11:20 13.86 211.18 1.26 588 808 18.03 229.21 23-Apr 10:25 18.82 192.38 1.14 590 810 36.39 228.77 24-Apr 20:10 20.23 216.50 1.22 596 816 5 5 11.33 227.83 26-Apr 11:35 21.87 214.84 1.19 598 818 12.84 227.68 29-Apr 10:40 24.83 203.94 1.22 608 828 23.39 227.33 30-Apr 11:40 25.88 219.28 1.13 588 808 5 5 7.54 226.82 3-May 11:10 28.85 202.56 1.17 580 800 25.17 227.73 7-May 10:55 32,84 194.29 1.18 571 791 32.76 227.05 10-May 10:30 35.83 202.74 1.14 573 793 Enargite In (g): Total Water (g): 2.01 268.64 Vol (mL) Mass (g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) • 118.97 10 10 95.00 95.00 202.74 79.52 I , '1 250 1 '." : ' ! 0.95 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 2428.20 979.30 98.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 6189.70 477.35 193.5 5.5 #2 6616.40 747.45 21.5 13.0 #3 5942.55 666.65 14.0 5.5 PLS (mg/L) 6998.30 813.70 25.5 0.0 Wash (mg/L) 120.55 9.40 0.7 Solid Residue (wt % 0.6158 18 21 0.4 Weight of Element Copper Iron Arsenic Antimony Head (g) 0.62712 0.23316 0.21105 0.011055 Innoculum (g) 0.0243 0.0098 0.0010 0.0000 Medium (g) 0 0.01908 0 0 Samples (g): #1 0.030949 0.00239 0.000968 0.0000275 #2 0.033082 0.00374 0.000108 0.000065 #3 0.029713 0.00333 0.00007 0.0000275 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.5565 0.0647 0.0020 0.0000 Wash (g) 0.030138 0.00235 0.000175 0 Solid Residue (g) 0.00585 0.171 0.1995 0.0038 ••<. faup* Calculated Head (g) 0.662 0.216 0.202 0.004 % Difference -5.555 7.522 4.353 64.541 % Extraction Calculated Head 99.12 20.69 1.17 3.06 Measured Head 104.62 19.14 1.12 1.09 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 0.00 105.65 1 11.89 97.60 0.0309485 0.03095 0.604 0.580 92.46 87.59 2 20.23 95.52 0.033082 0.06403 0.632 0.639 101.84 96.48 3 25.88 98.30 0.02971275 0.09374 0.584 0.624 99.49 94.25 Filtrate 35.83 79.52 0.557 0.626 Wash 250.00 0.030 0.656 104.62 99.12 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.65 1 11.89 97.60 0.001382347 0.00138 0.04658936 0.04 15.78 17.07 2 20.23 95.52 0.002732847 0.00412 0.071396424 0.06 26.42 28.57 3 25.88 98.30 0.002328847 0.00644 0.065531695 0.06 23.91 25.85 Filtrate 35.83 79.52 0.0647 0.05 Wash 250.00 0.00235 0.06 24.56 26.56 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 0.00 105.65 1 11.89 97.60 0.0009675 0.00097 0.0188856 0.02 8.48 8.87 2 20.23 95.52 0.0001075 0.00108 0.00205368 0.00 0.96 1.01 3 25.88 98.30 0.00007 0.00115 0.0013762 0.00 0.69 0.73 Filtrate 35.83 79.52 0.00 0.00 Wash 250.00 0.00 0.00 1.12 1.17 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 0.0000 105.65 1 11.89 97.60 0.0000275 0.00003 0.0005368 0.00 4.86 13.69 2 20.23 95.52 0.000065 0.00009 0.00124176 0.00 11.48 32.38 3 25.88 98.30 0.0000275 0.00012 0.00054065 0.00 5.73 16.15 Filtrate 35.83 79.52 0.00 0.00 Wash 250.00 0.00 0.00 1.09 3.06 Extreme Thermophiles, 2 g Enargite, P 8 0 of 15 microns Test UB3-E15 Extreme Thermophiles Time Initial • E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 14-Feb 10:00 0.00 253.63 1.70 464 684 18-Feb 9:30 3.98 205.12 1.80 405 625 48.85 253.97 21-Feb 11:35 7,07 215.97 1.76 416 636 38.04 254.01 22-Feb 10:55 8.04 243.92 1.85 416 636 5 5 10;98 254.90 26-Feb 10:10 12.01 209.37 1.43 444 664 46.43 255.80 28-Feb 10:20 14,01 231.87 1.50 446 666 5 5 21.64 253.51 5-Mar 10:50 19.03 197.13 1.36 460 680 58.53 255.66 7-Mar 11:35 21.07 233.12 1.43 486 706 24.27 257.39 11-Mar 12:45 25.11 218.50 35.31 253.81 12-Mar 10:10 26,01 245.54 1.43 648 868 5 5 8.56 254.10 14-Mar 11:05 28.05 234.01 1.35 651 871 19.92 253.93 15-Mar 12:05 29,09 243.81 1.32 671 891 9.86 253.67 19-Mar 12:40 33.11 214.04 1.30 643 863 40.58 254.62 21-Mar 20:40 35.44 231.82 1.32 642 862 22.36 254.18 22-Mar 18:40 36.36 244.92 1.32 647 867 Enargite In (g): 2.01 Total Water (g): 385.33 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 v ' \ " Wash Volume (mL) 250 Solid Residue (g) 0.94 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 2690.40 4107.10 255.5 18.0 Medium (g/L) 0 0.20088 0 0 Samples (mg/L): #1 1573.15 579.25 153.0 4.5 #2 2901.10 648.20 262.5 1.5 #3 6246.80 490.15 56.5 14.5 PLS (mg/L) 6525.40 546.20 23.5 8.0 Wash (mg/L) 38.17 2.75 Solid Residue (wt % 1.5316 16 16 0.6 - • .- : " - i. '•" • .'-."0 it,-.; iv'AiJ,:- >'.' Weight of Element Copper Iron Arsenic Antimony Head (g) 0.61104 0.21306 0.21105 0.011055 Innoculum (g) 0.0269 0.0411 0.0026 0.0002 Medium (g) 0 0.01912 0 0 Samples (g): #1 0.007866 0.0029 0.000765 0.0000225 #2 0.014506 0.00324 0.001313 0.0000075 #3 0.031234 0.00245 0.000283 0.0000725 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.6119 0.0512 0.0022 0.0008 Wash (g) 0.009543 0.00069 0 0 Solid Residue (g) 0.014397 0.1504 0.1504 0.00564 - ' Calculated Head (g) 0.663 0.148 0.152 0.006 % Difference -8.426 30.681 27.786 42.898 % Extraction , . w*' wV^ S^"-' •• Calculated Head 97.83 -1.83 1.32 10.66 Measured Head 106.07 -1.27 0.95 6.08 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 0.00 105.74 1 8.04 96.03 0.00786575 0.00787 0.151 0.124 20.32 18.74 2 14.01 83.98 0.0145055 0.02237 0.244 0.225 36.76 33.90 3 26.01 97.65 0.031234 0.05361 0.610 0.605 99.09 91.39 Filtrate 36.36 93.77 0.612 0.639 Wash 250.00 0.010 0.648 106.07 97.83 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.74 1 8.04 96.03 0.001891847 0.00189 0.056 0.01 6.83 9.85 2 14.01 83.98 0.002236597 0.00413 0.054 0.01 6.27 9.05 3 26.01 97.65 0.001446347 0.00557 0.048 0.01 3.19 4.60 Filtrate 36.36 93.77 0.0512 0.01 Wash 250.00 0.0006875 0.01 5.08 7.34 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 0.00 105.74 1 8.04 96.03 0.000765 0.00077 0.01469259 0.01 5.75 7.96 2 14.01 83.98 0.0013125 0.00208 0.02204475 0.02 9.60 13.29 3 26.01 97.65 0.0002825 0.00236 0.005517225 0.01 2.39 3.31 Filtrate 36.36 93.77 0.00 0.00 Wash 250.00 0.00 0.00 0.95 1.32 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 0.0000 105.74 1 8.04 96.03 0.0000225 0.00002 0.000432135 0.00 2.28 3.99 2 14.01 83.98 0.0000075 0.00003 0.00012597 0.00 -0.29 -0.50 3 26.01 97.65 0.0000725 0.00010 0.001415925 0.00 11.45 20.05 Filtrate 36.36 93.77 0.00 0.00 Wash 250.00 0.00 0.00 6.08 10.66 Extreme Thermophiles, 2 g Enargite (2), P 8 0 of 15 microns Test#B4-E15 Extreme Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 4-Apr 14:40 0.00 239.96 1.58 444 664 8-Apr 13:00 3.93 200.90 1.85 370 590 45.29 246.19 12-Apr 10:15 7.82 208.90 1.86 386 606 32.69 241.59 15-Apr 11:05 10.85 242.20 1.66 437 657 16-Apr 12:00 11.89 232.37 1.63 445 665 5 5 8.43 240.80 18-Apr 11:20 13.86 221.31 1.69 432 652 22.54 243.85 23-Apr 10:25 18.82 196.08 1.45 447 667 45.92 242.00 24-Apr 20:10 20.23 228.80 1.38 449 669 5 5 12.62 241.42 26-Apr 11:35 21.87 226.72 1.47 478 698 19.82 246.54 29-Apr 10:40 24.83 216.43 1.40 511 731 25.58 242.01 30-Apr 11:40 25.88 232.08 1.27 555 775 5 5 8.33 240.41 3-May 11:10 28.85 212.03 1.34 592 812 29.07 241.10 7-May 10:55 32.84 201.32 1.24 606 826 39.37 240.69 10-May 10:30 35.83 221.65 1.18 619 839 Enargite In (g): 2.00 Total Water (g): 289.66 Vol (mL) Mass (g) Flask Weight (g): 132.12 Innoculum in: 10 10 Medium in: 95.03 95.03 Total Final Weight (g): 221.65 Filtrate Volume (mL) 74.95 -*n,.y Wash Volume (mL) 250 Solid Residue (g) 0.92 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 2428.20 979.30 98.5 Medium (g/L) 0 0.20088 0 0 Samples (mg/L): #1 1898.90 268.20 119.0 0.0 #2 2545.15 214.70 40.0 6.0 #3 5040.85 159.25 110.5 10.0 PLS (mg/L) 7582.55 536.40 52.5 13.5 Wash (mg/L) 86.93 6.19 0.7 0.2 Solid Residue (wt % 3.4 18 19 0.8 • • ~ r.")»f; ' ' r ... ...^ Weight of Element Copper Iron Arsenic Antimony Head (g) 0.608 0.212 0.21 0.011 Innoculum (g) 0.0243 0.0098 0.0010 0.0000 Medium (g) 0 0.01909 0 0 Samples (g): #1 0.009495 0.00134 0.000595 0 #2 0.012726 0.00107 0.0002 0.00003 #3 0.025204 0.0008 0.000553 0.00005 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.5683 0.0402 0.0039 0.0010 Wash (g) 0.021733 0.00155 0.000175 0.00005 Solid Residue (g) 0.03128 0.1656 0.1748 0.00736 Calculated Head (g) 0.644 0.179 0.179 0.009 % Difference -5.998 15.724 14.632 22.711 % Extraction ''VlklMP;". Calculated Head 95.15 7.31 2.49 13.43 Measured Head 100.85 6.16 2.13 10.38 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 0.00 105.84 1 11.89 98.25 0.0094945 0.00949 0.187 0.162 26.69 25.18 2 20.23 94.68 0.01272575 0.02222 0.241 0.226 37.20 35.10 3 25.88 97.96 0.02520425 0.04742 0.494 0.492 80.88 76.30 Filtrate 35.83 74.95 0.568 0.591 Wash 250.00 0.022 0.613 100.85 95.15 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.84 1 11.89 98.25 0.000336597 0.00034 0.026 0.02 7.81 9.27 2 20.23 94.68 6.90973E-05 0.00041 0.020 0.01 4.97 5.90 3 25.88 97.96 -0.000208153 0.00020 0.016 0.01 2.74 3.25 Filtrate 35.83 74.95 0.0402 0.03 Wash 250.00 0.0015475 0.03 15.07 17.89 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 0.00 105.84 1 11.89 98.25 0.000595 0.00060 0.01169175 0.01 5.10 5.97 2 20.23 94.68 0.0002 0.00080 0.0037872 0.00 1.62 1.89 3 25.88 97.96 0.0005525 0.00135 0.01082458 0.01 5.06 5.93 Filtrate 35.83 74.95 0.00 0.00 Wash 250.00 0.00 0.00 2.13 2.49 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 0.0000 105.84 1 11.89 98.25 0 0.00000 0 0.00 0.00 0.00 2 20.23 94.68 0.00003 0.00003 0.00056808 0.00 5.16 6.68 3 25.88 97.96 0.00005 0.00008 0.0009796 0.00 9.18 11.88 Filtrate 35.83 74.95 0.00 0.00 Wash 250.00 0.00 0.00 10.38 13.43 Extreme Thermophiles, 2 g Enargite, P 8 0 of 37 microns Test #B3-E37 Extreme Thermophiles Time Initial E h Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E h (mV) (mL) Added (mL) Water (g) Mass (g) 14-Feb 10:00 0.00 ' 236.80 1.70 482 702 18-Feb 9:30 3.98 198.78 1.56 429 649 47.45 246.23 21-Feb 11:35 7.07 210.60 1.49 486 706 35.65 246.25 22-Feb 10:55 8.04 228.25 1.52 496 716 5 5 17.75 246.00 26-Feb 10:10 12.01 199.16 1.71 477 697 47.12 246.28 28-Feb 10:20 14.01 215.34 1.26 481 701 5 5 30.84 246.18 5-Mar 10:50 19.03 189.46 1.24 500 720 57.24 246.70 7-Mar 11:35 21.07 219.25 1.34 571 791 17.68 236.93 11-Mar 12:45 25.11 191.66 47.25 238.91 12-Mar 10:10 26,01 228.39 1.32 620 840 5 5 10.60 238.99 14-Mar 11:05 28.05 217.02 1.34 620 840 20.28 237.30 15-Mar 12:05 29.09 225.17 1.28 630 850 12.01 237.18 19-Mar 12:40 33.11 192.72 1.29 607 827 46.53 239.25 21-Mar 20:40 35,44 214.22 1.34 622 842 28.38 242.60 22-Mar 18:40 36.36 231.57 1.34 632 852 Enargite In (g): 2.00 Total Water (g): 418.76 Vol (mL) Mass (g) Flask Weight (g): , • ; • 129.14 Innoculum in: 10 10 Medium in: 95.07 95.07 Total Final Weight (g): 231.57 Filtrate Volume (mL) 99.15 Wash Volume (mL) 250 111*11 Solid Residue (g) 1.12 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 2690.40 4107.10 255.5 18.0 Medium (g/L) ' 0 0.201 0 0 Samples (mg/L): #1 4221.20 397.90 676.5 0.0 #2 5901.00 51.05 172.5 3.0 #3 5998.70 114.20 80.5 5.5 PLS (mg/L) 6053.85 135.65 64.0 5.0 Wash (mg/L) 82.89 1.31 0.8 0.2 Solid Residue (wt % 4.4 14 18 0.6 s f e v - s i l l i t a , - J « i l i tam< r i Weight of Element Copper Iron Arsenic Antimony Head (g) 0.648 0.144 0.24 0.0078 Innoculum (g) 0.0269 0.0411 0.0026 0.0002 Medium (g) 0 0.0191 0 0 Samples (g): #1 0.021106 0.00199 0.003383 0 #2 0.029505 0.00026 0.000863 0.000015 #3 0.029994 0.00057 0.000403 0.0000275 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.6002 0.0134 0.0063 0.0005 Wash (g) 0.020723 0.00033 0.0002 0.00005 Solid Residue (g) 0.04928 0.1568 0.2016 0.00672 «LV,:.;»J :%V, .^re- ;•. ' « - • ' , » ' • . -r'?K,;*, SS.:. ." i . 'M* calculated Head (g) 0.724 0.110 0.210 0.007 % Difference -11.719 23.465 12.401 8.612 % Extraction . ,V''E;.:< "fSS,*:: ;. ...... . - j5 ir i Calculated Head 93.19 -42.27 4.11 5.73 Measured Head 104.11 -32.35 3.60 5.23 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 0.00 105.66 1 8.04 97.11 0.021106 0.02111 0.410 0.383 59.11 52.91 2 14.01 84.20 0.029505 0.05061 0.497 0.491 75.78 67.83 3 26.01 97.25 0.0299935 0.08060 0.583 0.607 93.69 83.86 Filtrate 36.36 99.15 0.600 0.654 Wash 250.00 0.021 0.675 104.11 93.19 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 105.66 1 8.04 97.11 0.000985097 0.00099 0.039 0.00 -1.69 -2.21 2 14.01 84.20 -0.000749153 0.00024 0.004 -0.04 -25.54 -33.37 3 26.01 97.25 -0.000433403 -0.00020 0.011 -0.03 -20.81 -27.19 Filtrate 36.36 99.15 0.0134 -0.03 Wash 250.00 0.0003275 -0.03 -18.95 -24.77 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 0.00 105.66 1 8.04 97.11 0.0033825 0.00338 0.065694915 0.06 26.31 30.03 2 14.01 84.20 0.0008625 0.00425 0.0145245 0.02 6.40 7.30 3 26.01 97.25 0.0004025 0.00465 0.007828625 0.01 3.97 4.53 Filtrate 36.36 99.15 0.01 0.01 Wash 250.00 0.00 0.01 3.60 4.11 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 0.0000 105.66 1 8.04 97.11 0 0.00000 0 0.00 -2.31 -2.53 2 14.01 84.20 0.000015 0.00002 0.0002526 0.00 0.93 1.02 3 26.01 97.25 0.0000275 0.00004 0.000534875 0.00 4.74 5.19 Filtrate 36.36 99.15 0.00 0.00 Wash 250.00 0.00 0.00 5.23 5.73 Extreme Thermophiles, 2 g Enargite(2), P 8 0 of 37 microns Test #B4-E37 Extreme Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E h (mV) (mL) Added (mL) Water (g) Mass (g) 4-Apr 14:40 0.00 253.52 1.56 442 662 8-Apr 13:00 3.93 217.41 1.84 373 593 > 37.60 255.01 12-Apr 10:15 7.82 214.80 1.86 384 604 43.52 258.32 15-Apr 11:05 10.85 229.55 1.74 399 619 25.89 255.44 16-Apr 12:00 11.89 245.80 1.70 426 646 5 5 8.16 253.96 18-Apr 11:20 13.86 234.97 1.74 443 663 21.14 256.11 23-Apr 10:25 18.82 210.30 1.44 451 671 44.58 254.88 24-Apr 20:10 20.23 241.83 1.40 456 676 5 5 12.36 254.19 26-Apr 11:35 21.87 238.59 1.47 490 710 20.25 258.84 29-Apr 10:40 24.83 228.90 1.40 522 742 24.65 253.55 30-Apr 11:40 25.88 243.78 1.26 562 782 5 5 9.93 253.71 3-May 11:10 28.85 226.48 1.27 603 823 27.57 254.05 7-May 10:55 32.84 215.90 1.30 608 828 37.72 253.62 10-May 10:30 35.83 225.85 1.22 615 835 Enargite In (g): Total Water (g): 2.01 313.37 Vol(mL) Mass(g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) K. ."• :-. 10 95.10 145.87 10 95.10 225.85 75.46 250 1.06 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 2428.20 979.30 98.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 1416.45 198.25 64.0 1.5 #2 3426:70 195.05 52.5 6.0 #3 5010.05 243.05 71.0 10.0 PLS (mg/L) 7287.80 484.30 69.0 15.5 Wash (mg/L) 92.62 3.85 0.9 0.3 Solid Residue (wt % 10 17 16 0.8 :ei<Sff? - ' • ..•„.t'»r- .,- ;. Weight of Element Copper Iron Arsenic Antimony Head (g) 0.65124 0.14472 0.2412 0.007839 Innoculum (g) 0.0243 0.0098 0.0010 0.0000 Medium (g) 0 0.0191 0 0 Samples (g): #1 0.007082 0.00099 0.00032 0.0000075 #2 0.017134 0.00098 0.000263 0.00003 #3 0.02505 0.00122 0.000355 0.00005 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.5499 0.0365 0.0052 0.0012 Wash (g) 0.023155 0.00096 0.000225 0.000075 Solid Residue (g) 0.106 0.1802 0.1696 0.00848 "' ' ,:-.\r„:' • •'• . . a .. . . . . ..j * ' • . * . J.. -' ' Calculated Head (g) 0.704 0.189 0.175 0.010 % Difference -8.113 -30.583 27.453 -25.171 % Extraction iSBk- . , ^ ^ ^... Calculated Head 84.94 4.65 3.08 13.58 Measured Head 91.84 6.07 2.23 16.99 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 0.00 105.64 1 11.89 97.92 0.00708225 0.00708 0.139 0.114 17.57 16.25 2 20.23 93.95 0.0171335 0.02422 0.322 0.305 46.79 43.28 3 25.88 95.90 0.02505025 0.04927 0.480 0.480 73.77 68.23 Filtrate 35.83 75.46 0.550 0.575 Wash 250.00 0.023 0.598 91.84 84.94 Iron Output Sample # Time (days) Sol'n Vol. (n g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.64 1 11.89 97.92 -1.31527E-05 -0.00001 0.019 0.01 6.65 5.09 2 20.23 93.95 -2.91527E-05 -0.00004 0.018 0.01 5.90 4.51 3 25.88 95.90 0.000210847 0.00017 0.023 0.01 9.34 7.15 Filtrate 35.83 75.46 0.0365 0.03 Wash 250.00 0.0009625 0.03 19.15 14.67 Arsenic Output Sample # Time (days) Sol'n Vol. (n nL) g As sampled Tot. As Sample As in sol'n (g) As(aq)total %As indicated %As actual 0.00 105.64 1 11.89 97.92 0.00032 0.00032 0.00626688 0.01 2.19 3.02 2 20.23 93.95 0.0002625 0.00058 0.004932375 0.00 1.77 2.44 3 25.88 95.90 0.000355 0.00094 0.0068089 0.01 2.66 3.66 Filtrate 35.83 75.46 0.01 0.01 Wash 250.00 0.00 0.01 2.23 3.08 Antimony Output Sample # Time (days) Sol'n Vol. (r nL) g Sb sampled Tot. Sb Sample Sb in sol'n (g) Sb(aq) total %Sb indicated %Sb actual 0.0000 105.64 1 11.89 97.92 0.0000075 0.00001 0.00014688 0.00 1.87 1.50 2 20.23 93.95 0.00003 0.00004 0.0005637 0.00 7.29 5.82 3 25.88 95.90 0.00005 0.00009 0.000959 0.00 12.71 10.16 Filtrate 35.83 75.46 0.00 0.00 Wash 250.00 0.00 0.00 16.99 13.58 Extreme Thermophiles, 3.5 g Enargite, P 8 0 of 10 microns Test#B7-E10 Extreme Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 8-Jul 12:00 0.00 225.65 1.58 479 699 10-Jul 12:30 2.02 221.31 1.86 384 604 4.66 225.97 12-Jul 14:10 4.09 210.45 1.41 409 629 16.90 227.35 15-Jul 12:40 7.03 204.92 1.28 429 649 31.25 236.17 16-Jul 12:20 ' 8.01 228.75 1.44 437 657 5 5 18-Jul 12:10 10.01 213.67 1.39 492 712 12.39 226.06 22-Jul 10:45 13.95 196.50 1.02 454 674 42.08 238.58 23-Jul 12:20 15.01 230.98 1.25 476 696 5 5 26-Jul 10:20 17.93 209.68 1.34 470 690 17.07 226.75 30-Jul 11:15 21.97 196.25 1.23 508 728 29.71 225.96 31-Jul 13:10 • 23.05 217.82 1.04 509 729 5 5 8.38 226.20 2-Aug 12:05 25.00 211.69 1.08 609 829 15.64 227.33 6-Aug 12:05 29.00 196.48 1.16 620 840 30.02 226.50 7-Aug 12:35 30.02 218.44 1.16 624 844 5 5 7.64 226.08 9-Aug 12:50 32.03 226.35 1.20 642 862 12-Aug 12:15 35.01 203.61 1.18 644 864 23.06 226.67 13-Aug 12:00 36.00 219.03 1.16 637 857 Enargite In (g): Total Water (g): 3.50 238.80 Vol (mL) Mass (g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) .fyrtS:."} 116.89 10 10 95.00 95.00 l i f t ; - . . V - l 219.03 96.37 1 250 '«•>- ' : .."-i 1.64 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 6542.25 2541.90 160.5 15.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 3535.90 750.20 159.5 #2 8420.65 627.30 133.0 #3 12845.15 908.00 124.5 #4 12210.45 1292.00 51.0 PLS (mg/L) 11147.15 1197.15 43.0 Wash (mg/L) 199.58 17.96 0.5 Solid Residue (wt % 0.6323 18 21 0.8 : "*?-*,. ." Weight of Element Copper Iron Arsenic Antimony Head (g) 1.092 0.406 0.3675 0.01925 Innoculum (g) 0.0654 0.0254 0.0016 0.0002 Medium (g) 0 0.0191 0 0 Samples (g): #1 0.01768 0.0038 0.000798 0 #2 0.042103 0.0031 0.000665 0 #3 0.064226 0.0045 0.000623 0 #4 0.061052 0.0065 0.000255 0 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 #4 0 0.001 0 0 PLS (g) 1.0743 0.1154 0.0041 0.0000 Wash (g) 0.049895 0.0045 0.000125 0 Solid Residue (g) 0.01037 0.2952 0.3444 0.01312 ' • - . Calculated Head (g) 1.193 0.379 0.349 0.013 % Difference -9.258 6.657 4.993 32.649 % Extraction Calculated Head 99.13 22.10 1.36 -1.20 Measured Head 108.31 20.63 1.29 -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 0.00 105.26 1 8.01 108.36 0.0176795 0.01768 0.383 0.318 29.10 26.63 2 15.01 110.59 0.04210325 0.05978 0.931 0.883 80.91 74.05 3 23.05 97.43 0.06422575 0.12401 1.252 1.246 114.09 104.42 4 30.02 98.05 0.06105225 0.18506 1.197 1.256 115.00 105.26 Filtrate 36.00 96.37 1.074 1.133 Wash 250.00 0.050 1.183 108.31 99.13 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.26 1 8.01 108.36 0.002746597 0.00275 0.081291672 0.06 13.76 14.74 2 15.01 110.59 0.002132097 0.00488 0.069373107 0.04 10.83 11.60 3 23.05 97.43 0.003535597 0.00841 0.08846644 0.06 15.53 16.64 4 30.02 98.05 0.005455597 0.01387 0.1266806 0.10 24.94 26.72 Filtrate 36.00 96.37 0.1154 0.09 Wash 250.00 0.00449 0.09 23.26 24.92 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 0.00 105.26 1 8.01 108.36 0.0007975 0.00080 0.01728342 0.02 4.27 4.49 2 15.01 110.59 0.000665 0.00146 0.01470847 0.01 3.78 3.98 3 23.05 97.43 0.0006225 0.00209 0.012130035 0.01 3.26 3.43 4 30.02 98.05 0.000255 0.00234 0.00500055 0.01 1.49 1.57 Filtrate 36.00 96.37 0.00 0.00 Wash 250.00 0.00 0.00 1.29 1.36 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 0.00 76.09 1 8.01 108.36 0 0.00000 0 0.00 -0.81 -1.20 2 15.01 110.59 0 0.00000 0 0.00 -0.81 -1.20 3 23.05 97.43 0 0.00000 0 0.00 -0.81 -1.20 4 30.02 98.05 0 0.00000 0 0.00 -0.81 -1.20 Filtrate 36.00 96.37 0.00 0.00 Wash 250.00 0.00 0.00 -0.81 -1.20 Extreme Thermophiles, 3.5 g Enargite, P 8 0 of 15 microns Test#B7-E15 Extreme Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E h ( m V ) (mL) Added (mL) Water (g) Mass (g) 8-Jul 12:00 0.00 224.35 1.52 516 736 10-Jul 12:30 2,02 209.54 2.02 384 604 15.46 225.00 12-Jul 14:10 4.09 209.03 1.62 381 601 22.17 231.20 15-Jul 12:40 7,03 208.33 1.49 383 603 16.65 224.98 16-Jul 12:20 8.01 217.61 1.65 400 620 5 5 7.40 225.01 18-Jul 12:10 10.01 209.68 1.68 402 622 15.79 225.47 22-Jul 10:45 13,95 194.59 1.40 400 620 31.37 225.96 23-Jul 12:20 15.01 217.28 1.54 397 617 5 5 13.91 231.19 26-Jul 10:20 17.93 209.12 1.76 400 620 15.92 225.04 30-Jul 11:15 21.97 193.06 1.66 454 674 32.38 225.44 31-Jul 13:10 23.05 217.44 1.44 443 663 5 5 7.80 225.24 2-Aug 12:05 25.00 209.99 1.50 459 679 14.76 224.75 6-Aug 12:05 29.00 194.05 1.41 473 693 31.77 225.82 7-Aug 12:35 30.02 218.23 1.36 487 707 5 5 6.50 224.73 9-Aug 12:50 32.03 209.06 1.39 500 720 15.92 224.98 12-Aug 12:20 35.01 202.27 1.28 506 726 22.67 224.94 13-Aug 12:00 36.00 217.54 1.26 524 744 Enargite In (g): Total Water (g): 3.51 270.47 Vol(mL) Mass(g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) W? ' -."1 115.54 10 10 95.02 95.02 j . - , . . . • ,- [ 217.54 96.95 ' 250 v ' 'I 1.92 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 6542.25 2541.90 160.5 15.5 Medium (g/L) 0 0.2009 0 0 Samples (mg/L): #1 2323.45 375.45 47.0 #2 3266.90 507.65 76.0 #3 4913.90 739.85 211.5 #4 7981.40 503.75 98.5 PLS (mg/L) 10583.40 384.15 138.5 Wash (mg/L) 155.05 3.77 1.8 Solid Residue (wt % 8.6 18 17 0.9 Weight of Element Copper Iron Arsenic Antimony Head (g) 1.06704 0.3721 0.36855 0.019305 Innoculum (g) 0.0654 0.0254 0.0016 0.0002 Medium (g) 0 0.0191 0 0 Samples (g): #1 0.011617 0.0019 0.000235 0 #2 0.016335 0.0025 0.00038 0 #3 0.02457 0.0037 0.001058 0 #4 0.039907 0.0025 0.000493 0 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 #4 0 0.001 0 0 PLS (g) 1.0261 0.0372 0.0134 0.0000 Wash (g) 0.038763 0.0009 0.00045 0 Solid Residue (g) 0.16512 0.3456 0.3264 0.01728 • • ' .;.«*SfS Calculated Head (g) 1.217 0.344 0.340 0.017 % Difference -14.058 7.439 7.653 11.292 % Extraction i. J'ft'-kllfci •' . ' >3S3» Calculated Head 86.43 -0.35 4.10 -0.91 Measured Head 98.58 -0.33 3.78 -0.80 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 0.00 105.30 1 8.01 98.56 0.01161725 0.01162 0.229 0.164 15.33 13.44 2 15.01 98.23 0.0163345 0.02795 0.321 0.267 25.03 21.95 3 23.05 98.39 0.0245695 0.05252 0.483 0.446 41.80 36.65 4 30.02 99.18 0.039907 0.09243 0.792 0.779 72.98 63.98 Filtrate 36.00 96.95 1.026 1.013 Wash 250.00 0.039 1.052 98.58 86.43 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.30 1 8.01 98.56 0.000872847 0.00087 0.037 0.01 3.11 3.36 2 15.01 98.23 0.001533847 0.00241 0.050 0.02 6.57 7.10 3 23.05 98.39 0.002694847 0.00510 0.073 0.05 12.73 13.76 4 30.02 99.18 0.001514347 0.00662 0.050 0.02 6.60 7.13 Filtrate 36.00 96.95 0.0372 0.01 Wash 250.00 0.0009425 0.01 3.43 3.71 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 0.00 105.30 1 8.01 98.56 0.000235 0.00024 0.00463232 0.00 0.82 0.89 2 15.01 98.23 0.00038 0.00062 0.00746548 0.01 1.65 1.79 3 23.05 98.39 0.0010575 0.00167 0.020809485 0.02 5.38 5.82 4 30.02 99.18 0.0004925 0.00217 0.00976923 0.01 2.67 2.89 Filtrate 36.00 96.95 0.01 0.01 Wash 250.00 0.00 0.01 3.78 4.10 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 0.00 75.00 1 8.01 98.56 0 0.00000 0 0.00 -0.80 -0.91 2 15.01 98.23 0 0.00000 0 0.00 -0.80 -0.91 3 23.05 98.39 0 0.00000 0 0.00 -0.80 -0.91 4 30.02 99.18 0 0.00000 0 0.00 -0.80 -0.91 Filtrate 36.00 96.95 0.00 0.00 Wash 250.00 0.00 0.00 -0.80 -0.91 Extreme Thermophiles, 3.5 g Enargite, P 8 0 of 37 microns Test #B7-E37 Extreme Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E h (mV) (mL) Added (mL) Water (g) Mass (g) 8-Jul 12:00 0.00 254.91 1.52 508 728 10-Jul 12:30 2.02 236.68 1.90 388 608 18.84 255.52 12-Jul 14:10 4.09 235.91 1.48 390 610 20.57 256.48 . 15-Jul 12:40 7.03 225.5 1.41 404 624 31.40 256.90 16-Jul 12:20 8.01 246.38 1.55 406 626 5 5 8.90 255.28 18-Jul 12:10 10.01 236.19 1.76 395 615 19.15. 255.34 22-Jul 10:45 13.95 217.16 1.49 '404 624 40.71 257.87 23-Jul 12:20 15.01 247.58' 1.39 • 546 766 5 5 8.81 256.39 26-Jul 10:20 17.93 228.49 1.43 459 679 26.22 254.71 30-Jul 11:15 21.97 216.43 1.45 449 669 39.24 255.67 31-Jul 13:10 23.05 245.31 1.26 451 671 5 5 9.99 255.30 2-Aug 12:05 25.00 234.41 1.33 462 682 20.92 255.33 6-Aug 10:05 28.92 216.05 1.39 457 -677 40.78 256.83 7-Aug 12:35 30.02 247.05 1.38 467 687 5 5 8.75 255.80 9-Aug 12:50 32.03 236.41 1.45 480 700 18.97 255.38 12-Aug 12:15 35.01 226.69 1.37 478 698 28.33 255.02 13-Aug 12:00 36.00 245.84 1.32 495 715 Enargite In (g): Total Water (g): 3.51 341.58 Vol (mL) Mass (g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g) Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) | 146.07 10 10 95.01 95.01 ' i ' 245 84 93 25 ' 248 I 5 "' "'•) 2.40 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 6542.25 2541.90 160.5 15.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 2367.90 323.55 95.5 #2 5060.35 174.50 364.5 #3 7092.55 72.55 205.0 #4 7390.35 69.50 238.0 PLS (mg/L) 7791.70 70.80 273.5 Wash (mg/L) 113.53 0.75 4.0 Solid Residue (wt % 18 11 15 0.5 t - ' > " - ' St:'.' " •„ •'3*?,!' •"- > , ! » , = .. V •' Weight of Element Copper Iron Arsenic Antimony Head (g) 1.13724 0.2527 0.4212 0.013689 Innoculum (g) 0.0654 0.0254 0.0016 0.0002 Medium (g) 0 0.0191 0 0 Samples (g): #1 0.01184 0.0016 0.000478 0 #2 0.025302 0.0009 0.001823 0 #3 0.035463 0.0004 0.001025 0 #4 0.036952 0.0003 0.00119 0 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 #4 0 0.001 0 0 PLS (g) 0.7266 0.0066 0.0255 0.0000 Wash (g) 0.028155 0.0002 0.000992 0 Solid Residue (g) 0.432 0.264 0.36 0.012 * f f i , . . - . , •« Calculated Head (g) 1.194 0.226 0.388 0.012 % Difference -4.983 10.524 7.831 13.471 % Extraction V i f c N * . - - • %'}",, -•' . •'fJ.'..; • "' ^ . 1 * * *' ''1 Calculated Head 63.82 -16.75 7.27 -1.31 Measured Head 67.00 -14.99 6.70 -1.13 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 0.00 105.33 1 8.01 96.80 0.0118395 0.01184 0.229 0.164 14.40 13.72 2 15.01 98.00 0.02530175 0.03714 0.496 0.442 38.90 37.05 3 23.05 95.73 0.03546275 0.07260 0.679 0.651 57.22 54.50 4 30.02 97.47 0.03695175 0.10956 0.720 0.728 63.97 60.94 Filtrate 36.00 93.25 0.727 0.734 Wash 248.00 0.028 0.762 67.00 63.82 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.33 1 8.01 96.80 0.000613347 0.00061 0.031 0.01 2.33 2.61 2 15.01 98.00 -0.000131903 0.00048 0.017 -0.01 -3.29 -3.68 3 23.05 95.73 -0.000641653 -0.00016 0.007 -0.02 -7.31 -8.17 4 30.02 97.47 -0.000656903 -0.00082 0.007 -0.02 -7.38 -8.25 Filtrate 36.00 93.25 0.0066 -0.02 Wash 248.00 0.000186 -0.02 -7.37 -8.24 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 0.00 105.33 1 8.01 96.80 0.0004775 0.00048 0.0092444 0.01 1.81 1.97 2 15.01 98.00 0.0018225 0.00230 0.035721 0.03 8.21 8.91 3 23.05 95.73 0.001025 0.00333 0.01962465 0.02 4.82 5.23 4 30.02 97.47 0.00119 0.00452 0.02319786 0.02 5.92 6.42 Filtrate 36.00 93.25 0.03 0.03 Wash 248.00 0.00 0.03 6.70 7.27 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 0.00 66.47 1 8.01 96.80 0 0.00000 0 0.00 -1.13 -1.31 2 15.01 98.00 0 0.00000 0 0.00 -1.13 -1.31 3 23.05 95.73 0 0.00000 0 0.00 -1.13 -1.31 4 30.02 97.47 0 0.00000 0 0.00 -1.13 -1.31 Filtrate 36.00 93.25 0.00 0.00 Wash 248.00 0.00 0.00 -1.13 -1.31 Extreme Thermophiles, 5 g Enargite, P 8 0 of 10 microns Test#B5-E10 Extreme Thermophiles Time Initial E h Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E (mL) Added (mL) Water (g) Mass (g) 11-Apr 15:45 0.00 225.90 1.57 413 633 15-Apr 11:10 3.81 216.27 1.65 379 599 22.71 238.98 18-Apr 11:25 6,82 212.47 1.64 410 630 16.97 229.44 19-Apr 11:15 7.81 221.30 1.56 398 618 5 5 4.95 226.25 23-Apr 10:30 11.78 192.68 1.36 400 620 35.78 228.46 24-Apr 20:15 13.19 213.14 1.44 401 621 5 5 14.08 227.22 26-Apr 11:40 14.83 210.24 1.35 403 623 18.04 228.28 29-Apr 10:45 17.79 196.51 1.34 407 627 35.06 231.57 30-Apr 11:45 18.83 221.40 1.21 400 620 5 5 6.27 227.67 3-May 11:15 21.81 199.89 1.24 408 628 26.33 226.22 7-May 11:00 25.80 187.02 1.21 407 627 40.19 227.21 10-May 11:00 28.80 198.02 1.03 407 627 5 5 28.48 226.50 14-May 11:25 32.82 185.53 1.30 428 648 41.81 227.34 16-May 10:35 34.78 207.31 1.25 421 641 26.22 233.53 17-May 11:25 35.82 222.38 1.26 413 633 Enargite In (g): 5.00 Total Water (g): 316.89 Vol (mL) Mass (g) Flask Weight (g): , J 137.34 Innoculum in: 10 10 Medium in: 95.01 95.01 Total Final Weight (g) 222.38 Filtrate Volume (mL) 79.10 Wash Volume (mL) 250 Solid Residue (g) 3.80 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 11.6 10.5 0.55 Innoculum (mg/L) 1645.85 854.90 80.5 7.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 3783.85 494.40 31.5 0.0 #2 5338.95 1199.60 54.5 6.5 #3 5172.25 1102.75 54.5 8.5 #4 8581.20 1640.30 141.5 15.5 PLS (mg/L) 6637.75 1102.95 117.0 10.0 Wash (mg/L) 107.40 12.29 1.0 0.1 Solid Residue (wt °/ 26 12 13 0.6 .'* . • .. Weight of Element Copper Iron Arsenic Antimony Head (g) 1.56 0.58 0.525 0.0275 Innoculum (g) 0.0165 0.0085 0.0008 0.0001 Medium (g) 0 0.01909 0 0 Samples (g): #1 0.018919 0.00247 0.000158 0 #2 0.026695 0.006 0.000273 0.0000325 #3 0.025861 0.00551 0.000273 0.0000425 #4 0.042906 0.0082 0.000708 0.0000775 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.5250 0.0872 0.0093 0.0008 Wash (g) 0.02685 0.00307 0.00025 0.000025 Solid Residue (g) 0.988 0.456 0.494 0.0228 ; . • i " ••-.5t*H* -' a Jl'*>«••. •' ' Calculated Head (g 1.595 0.530 0.503 0.024 % Difference -2.238 8.681 4.114 14.124 % Extraction Calculated Head 38.05 13.91 1.87 3.46 Measured Head . 38.90 12.70 1.79 2.97 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 0.00 83.56 1 7.81 78.96 0.01891925 0.01892 0.299 0.282 18.10 17.70 2 13.19 70.80 0.02669475 0.04561 0.378 0.380 24.39 23.85 3 18.83 57.55 0.02586125 0.07148 0.298 0.327 20.95 20.49 4 28.80 57.55 0.042906 0.11438 0.494 0.549 35.18 34.41 Filtrate 35.82 79.10 0.525 0.580 Wash 250.00 0.027 0.607 38.90 38.05 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq)total %Fe indicated %Fe actual 0.00 83.56 1 7.81 78.96 0.001467597 0.00147 0.039037824 0.03 5.26 5.76 2 13.19 70.80 0.004993597 0.00646 0.08493168 0.08 13.17 14.42 3 18.83 57.55 0.004509347 0.01097 0.063463263 0.05 9.47 10.37 4 28.80 44.68 -0.079041845 -0.06807 0.073288604 0.06 11.16 12.22 Filtrate 35.82 79.10 0.0872 0.08 Wash 250.00 0.0030725 0.08 14.10 15.44 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 0.00 83.56 1 7.81 78.96 0.0001575 0.00016 0.00248724 0.00 0.32 0.33 2 13.19 70.80 0.0002725 0.00043 0.0038586 0.00 0.61 0.64 3 18.83 57.55 0.0002725 0.00070 0.003136475 0.00 0.53 0.55 4 28.80 57.55 0.0007075 0.00141 0.008143325 0.01 1.53 1.60 Filtrate 35.82 79.10 0.01 0.01 Wash 250.00 0.00 0.01 1.79 1.87 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 0.0000 83.56 1 7.81 78.96 0 0.00000 0 0.00 -0.27 -0.32 2 13.19 70.80 0.0000325 0.00003 0.0004602 0.00 1.40 1.63 3 18.83 57.55 0.0000425 0.00008 0.000489175 0.00 1.62 1.89 4 28.80 57.55 0.0000775 0.00015 0.000892025 0.00 3.24 3.78 Filtrate 35.82 79.10 0.00 0.00 Wash 250.00 0.00 0.00 2.97 3.46 Extreme Thermophiles, 5 g Enargite, P 8 0 of 15 microns Test#B8-E15 Extreme Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 16-Jul 13:30 0.00 256.15 1.68 467 687 18-Jul 11:55 1.93 238.31 1.53 427 647 18.62 256.93 22-Jul 10:35 5.88 213.88 1.21 458 678 43.07 256.95 23-Jul 12:20 6.95 246.32 1.62 434 654 5 5 10.76 257.08 26-Jul 10:20 9.87 229.10 1.88 392 612 28.32 257.42 30-Jul 11:15 13.91 216.08 1.87 396 616 41.06 257.14 31-Jul 13:05 14.98 246.14 1.66 397 617 5 5 10.88 257.02 2-Aug 12:00 16.94 233.57 1.77 387 607 23.61 257.18 6-Aug 12:00 20.94 216.02 1.69 390 610 40.83 256.85 7-Aug 12:30 21.96 245.84 1.67 385 605 5 5 10.94 256.78 9-Aug 12:45 23.97 236.67 1.76 404 624 21.62 258.29 12-Aug 12:10 26.94 229.47 1.62 427 647 28.19 257.66 13-Aug 12:10 27.94 248.34 1.53 429 649 5 5 8.75 257.09 16-Aug 13:50 31.01 227.85 1.50 443 663 29.24 257.09 20-Aug 13:15 34.99 219.55 1.42 461 681 46.41 265.96 21-Aug 13:05 35.98 256.25 1.43 470 690 Enargite In (g): 5.02 Total Water (g): 362.30 Vol (mL) Mass (g) Flask Weight (g): 145.93 Innoculum in: 10 10 Medium in: 95.12 95.12 Total Final Weight (g): 256.25 Filtrate Volume (mL) 103.52 Wash Volume (mL) 250 Solid Residue (g) S # x 3.70 Analysis Copper Iron Arsenic Antimony Head (wt %) Innoculum (mg/L) Medium (g/L) 30.4 10.6 10.5 0.55 3000.55 1469.30 81.0 0 0.2009 0 0 Samples (mg/L): #1 #2 #3 #4 2177.25 311.65 40.0 3701.45 517.40 77.5 4282.50 693.00 24.0 4721.20 806.55 41.0 PLS (mg/L) Wash (mg/L) Solid Residue (wt % 6593.05 665.15 93.0 91.88 5.35 0.8 25 12 13 0.6 •• ... . ' . v . - . - f f V i . . - . v i , . ' , . • . : . . . ; > . - . •-. Weight of Element Copper Iron Arsenic Antimony Head (g) Innoculum (g) Medium (g) 1.52608 0.5321 0.5271 0.02761 0.0300 0.0147 0.0008 0.0000 0 0.0191 0 0 Samples (g): #1 #2 #3 #4 0.010886 0.0016 0.0002 0 0.018507 0.0026 0.000388 0 0.021413 0.0035 0.00012 0 0.023606 0.004 0.000205 0 Medium Added (g): #1 #2 #3 #4 0 0.001 0 0 0 0.001 0 0 0 0.001 0 0 0 0.001 0 0 PLS (g) Wash (g) Solid Residue (g) 0.6825 0.0689 0.0096 0.0000 0.02297 0.0013 0.0002 0 0.925 0.444 0.481 0.0222 Calculated Head (g) % Difference 1.651 0.485 0.491 0.022 -8.204 8.857 6.901 19.594 % Extraction ••*-.''.'.••'"•• " i Calculated Head Measured Head 43.98 8.45 1.98 0.00 47.59 7.70 1.84 0.00 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 0.00 105.20 1 9.87 78.15 0.01088625 0.01089 0.170 0.140 9.18 8.49 2 14.98 95.19 0.01850725 0.02939 0.352 0.333 21.84 20.18 3 21.96 94.89 0.0214125 0.05081 0.406 0.406 26.59 24.57 4 27.94 97.39 0.023606 0.07441 0.460 0.481 31.49 29.10 Filtrate 35.98 103.52 0.683 0.703 Wash 250.00 0.023 0.726 47.59 43.98 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 105.20 1 9.87 78.15 0.000553847 0.00055 0.024 0.01 1.82 1.99 2 14.98 95.19 0.001582597 0.00214 0.049 0.03 6.49 7.13 3 21.96 85.72 0.002460597 0.00460 0.059 0.04 8.40 9.22 4 27.94 97.39 0.003028347 0.00763 0.079 0.06 12.00 13.17 Filtrate 35.98 103.52 0.0689 0.05 Wash 250.00 0.0013375 0.06 10.43 11.44 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 0.00 105.20 1 9.87 78.15 0.0002 0.00020 0.003126 0.00 0.44 0.47 2 14.98 95.19 0.0003875 0.00059 0.007377225 0.01 1.28 1.38 3 21.96 85.72 0.00012 0.00071 0.00205728 0.00 0.35 0.37 4 27.94 97.39 0.000205 0.00091 0.00399299 0.00 0.74 0.79 Filtrate 35.98 103.52 0.01 0.01 Wash 250.00 0.00 0.01 1.84 1.98 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 0.00 105.20 1 9.87 78.15 0 0.00000 0 0.00 0.00 0.00 2 14.98 95.19 0 0.00000 0 0.00 0.00 0.00 3 21.96 85.72 0 0.00000 0 0.00 0.00 0.00 4 27.94 97.39 0 0.00000 0 0.00 0.00 0.00 Filtrate 35.98 103.52 0.00 0.00 Wash 250.00 0.00 0.00 0.00 0.00 Extreme Thermophiles, 5 g Enargite, P 8 0 of 37 microns Test UB5-E37 Extreme Thermophiles T i m e Initial E„ S a m p l e M e d i u m A d d e d Final Date H o u r (days) M a s s (g) p H (Ag/AgCI) E h ( m V ) (mL) A d d e d (mL) Water (g) M a s s (g) 11-Apr 15:45 0.00 247.49 1.59 392 612 15-Apr 11:10 3.81 200.63 1.72 378 598 49.46 250.09 18-Apr 11:25 6.82 229.05 1.82 385 605 29.26 258.31 19-Apr 11:15 7.81 251.41 1.77 396 616 5 5 23-Apr 10:30 11.78 222.18 1.62 417 637 29.70 251.88 24-Apr 20:15 13.19 241.74 1.55 417 637 5 5 6.14 247.88 26-Apr 11:40 14.83 236.73 1.59 474 694 16.83 253.56 29-Apr 10:45 17.79 215.67 1.48 438 658 32.00 247.67 30-Apr 11:50 18.84 223.83 1.31 435 655 5 5 32.28 256.11 3-May 11:15 21.81 236.56 1.42 434 654 11.35 247.91 7-May 11:00 25.80 217.95 1.34 441 661 29.87 247.82 10-May 11:00 28.80 225.92 1.25 451 671 5 5 21.74 247.66 14-May 11:25 32.82 221.28 1.40 490 710 27.63 248.91 16-May 10:35 34.78 i 23o:oa,| 1.39 570 790 19.64 249.64 17-May 11:25 35.82 242.06 1.34 590 810 Enarg i te In (g): 4.99 Total Water (g): 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) i i v - * - * . : , I 3.44 A n a l y s i s Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 1645.85 854.90 80.5 7.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 2311.65 359.90 83.0 #2 3134.30 611.90 160.0 #3 4758.20 858.15 141.0 5.5 #4 5129.90 817.60 129.5 8.5 PLS (mg/L) 6617.90 734.20 252.5 12.0 Wash (mg/L) 120.35 8.01 3.2 0.4 Solid Residue (wt "/ 23 13 14 0.6 ,.-v*, i •'vC'':.'-'- ' - * Weight of Element Copper Iron Arsenic Antimony Head (g) 1.61676 0.35928 0.5988 0.019461 Innoculum (g) 0.0165 0.0085 0.0008 0.0001 Medium (g) 0 0.01913 0 0 Samples (g): #1 0.011558 0.0018 0.000415 0 #2 0.015672 0.00306 0.0008 0 #3 0.023791 0.00429 0.000705 0.0000275 #4 0.02565 0.00409 0.000648 0.0000425 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 PLS (g) 0.7652 0.0849 0.0292 0.0014 Wash (g) 0.030088 0.002 0.0008 0.0001 Solid Residue (g) 0.7912 0.4472 0.4816 0.02064 Calculated Head (g 1.621 0.513 0.513 0.022 % Difference -0.267 -42.661 14.377 -13.458 % Extract ion Calculated Head 51.19 12.75 6.07 6.52 Measured Head 51.33 18.19 5.20 7.40 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 0.00 126.93 1 7.81 130.85 0.01155825 0.01156 0.302 0.286 17.69 17.64 2 13.19 121.18 0.0156715 0.02723 0.380 0.375 23.19 23.13 3 18.84 116.00 0.023791 0.05102 0.552 0.563 34.81 34.71 4 28.80 116.00 0.0256495 0.07667 0.595 0.630 38.94 38.84 Filtrate 35.82 115.63 0.765 0.800 Wash 250.00 0.030 0.830 51.33 51.19 Iron Output Sample # Time (days) Sol'n Vol. (mL) g Fe sampled Tot. Fe Sample Fe in sol'n (g) Fe(aq) total %Fe indicated %Fe actual 0.00 126.93 1 7.81 130.85 0.000795097 0.00080 0.047 0.04 10.73 7.52 2 13.19 121.18 0.002055097 0.00285 0.074 0.07 18.26 12.80 3 18.84 116.00 0.003286347 0.00614 0.100 0.09 25.33 17.75 4 28.80 97.39 -0.080807546 -0.07467 0.080 0.07 19.78 13.87 Filtrate 35.82 115.63 0.0849 0.08 Wash 250.00 0.0020025 0.08 21.81 15.29 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 0.00 126.93 1 7.81 130.85 0.000415 0.00042 0.01086055 0.01 1.68 1.96 2 13.19 121.18 0.0008 0.00122 0.0193888 0.02 3.17 3.71 3 18.84 116.00 0.000705 0.00192 0.016356 0.02 2.80 3.27 4 28.80 116.00 0.0006475 0.00257 0.015022 0.02 2.69 3.15 Filtrate 35.82 115.63 0.03 0.03 Wash 250.00 0.00 0.03 5.20 6.07 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 0.0000 126.93 1 7.81 130.85 0 0.00000 0 0.00 -0.39 -0.34 2 13.19 121.18 0 0.00000 0 0.00 -0.39 -0.34 3 18.84 116.00 0.0000275 0.00003 0.000638 0.00 2.89 2.55 4 28.80 116.00 0.0000425 0.00007 0.000986 0.00 4.82 4.25 Filtrate 35.82 115.63 0.00 0.00 Wash 250.00 0.00 0.00 7.40 6.52 Extreme Thermophiles, 10 g Enargite, P 8 0 of 10 microns Test UB2-E10 Extreme Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 20-Dec 9:40 0.00 250.96 1.53 477 697 23-Dec 9:50 3.01 219.03 1.60 387 607 5 5 32.16 251.19 28-Dec 10:00 8.01 198.10 1.30 420 640 5 5 53.17 251.27 31-Dec 13:10 11.15 221.75 1.23 402 622 5 5 29.54 251.29 3-Jan 16:10 14.27 221.96 1.19 398 618 5 5 29.14 251.10 8-Jan 10:20 19.03 206.52 1.12 412 632 5 5 45.08 251.60 11-Jan 10:25 22.03 223.56 1.17 404 624 5 5 27.48 251.04 15-Jan 11:40 26.08 212.89 1.16 411 631 5 5 39.22 252.11 18-Jan 9:40 29.00 224.82 1.16 408 628 5 5 26.95 251.77 22-Jan 11:45 33.09 212.33 408 628 5 5 39.04 251.37 25-Jan 10:50 36.05 219.95 1.04 407 627 Enargite In (g): Total Water (g): 10.00 Vol(mL) Mass(g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) ':. • /I 10 95.00 135.56 10 95.00 219.95 72.51 250 ''•'I/'A 7.66 Analysis Copper Iron Arsenic Antimony Head (wt %) 31.2 . 116 10.5 0.55 Innoculum (mg/L) 3895.65 2833.85 170.5 14.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 5291.85 1284.60 456.0 0.0 #2 11577.40 2020.85 110.0 10.5 #3 7823.70 1566.65 59.0 8.0 #4 8611.80 1830.45 80.5 12.5 #5 11453.15 2941.35 122.0 17.5 #6 9113.60 2134.00 114.0 18.0 #7 11355.45 2750.85 165.5 22.5 #8 9936.25 2618.80 148.5 20.5 #9 12762.45 3231.15 200.0 24.0 PLS (mg/L) 9844.75 2396.55 175.5 13 Wash (mg/L) 165.88 35.66 1.4 0.2 Solid Residue (wt %) 25.6 11.6 13.8 0.62 •mK*: - '•' Weight of Element Copper Iron Arsenic Antimony Head (g) 3.12 1.16 1.05 0.055 Innoculum (g) 0.0390 0.0283 0.0017 0.0001 Medium (g) 0 0.01908 0 0 Samples (g): #1 0.0264593 0.00642 0.00228 0 #2 0.057887 0.0101 0.00055 0.0000525 #3 0.0391185 0.00783 0.0003 0.00004 #4 0.043059 0.00915 0.0004 0.0000625 #5 0.0572658 0.01471 0.00061 0.0000875 #6 0.045568 0.01067 0.00057 0.00009 #7 0.0567773 0.01375 0.00083 0.0001125 #8 0.0496813 0.01309 0.00074 0.0001025 #9 0.0638123 0.01616 0.001 0.00012 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 #4 0 0.001 0 0 #5 0 0.001 0 0 #6 0 0.001 0 0 #7 0 0.001 0 0 #8 0 0.001 0 0 #9 0 0.001 0 0 PLS (g) 0.7138 0.1738 0.0127 0.0009 Wash (g) 0.04147 0.00892 0.00035 0.00005 Solid Residue (g) 1.96096 0.88856 1.05708 0.047492 « V j r > . \ > " ; -.7 . . « * ' . ' M . „*IS Calculated Head (g) 3.117 1.117 1.076 0.049 % Difference 0.098 3.734 -2.450 10.896 % Extraction • . •:' , ' * - ' • J * Calculated Head 37.09 20.43 1.73 3.09 Measured Head 37.05 19.67 1.78 2.75 Copper Output Sample Time Sol'n Vol. g Cu Total Cu Cu in Cu (aq) %Cu %Cu No. (days) (mL) sampled Removed (g) sol'n (g) total (g) Indicated actual 0.00 105.40 1 3.01 73.47 0.02646 0.02646 0.389 0.350 11.21 11.22 2 8.01 52.54 0.05789 0.08435 0.608 0.596 19.10 19.11 3 11.15 76.19 0.03912 0.12346 0.596 0.641 20.56 20.58 4 14.27 76.40 0.04306 0.16652 0.658 0.742 23.80 23.82 5 19.03 60.96 0.05727 0.22379 0.698 0.826 26.47 26.49 6 22.03 78.00 0.04557 0.26936 0.711 0.896 28.71 28.74 7 26.08 67.33 0.05678 0.32613 0.765 0.995 31.89 31.92 8 29.00 79.26 0.04968 0.37582 0.788 1.075 34.45 34.48 9 33.09 66.77 0.06381 0.43963 0.852 1.189 38.11 38.15 Filtrate 36.05 72.51 0.714 1.115 35.72 35.76 Wash 250.00 0.041 1.156 37.05 37.09 Iron Output Sample Time Sol'n Vol. g Fe Total Fe Fe in Fe (aq) %Fe %Fe No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 105.40 1 3.01 73.47 0.00542 0.00542 0.09438 0.07 5.69 5.91 2 8.01 52.54 0.0091 0.01452 0.106175 0.08 6.71 6.97 3 11.15 76.19 0.00683 0.02135 0.119363 0.09 7.85 8.15 4 14.27 76.40 0.00815 0.02950 0.139846 0.11 9.61 9.99 5 19.03 60.96 0.0137 0.04320 0.179305 0.15 13.01 13.52 6 22.03 78.00 0.00967 0.05286 0.166452 0.14 11.91 12.37 7 26.08 67.33 0.01275 0.06561 0.185215 0.16 13.52 14.05 8 29.00 79.26 0.01209 0.07770 0.207566 0.18 15.45 16.05 9 33.09 66.77 0.01515 0.09285 0.215744 0.19 16.16 16.78 Filtrate 36.05 72.51 0.1738 0.15 12.54 13.02 Wash 250.00 0.008915 0.15 13.31 13.82 Arsenic Output Sample Time Sol'n Vol. g As Total As As in As (aq) %As %As No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 105.40 1 3.01 73.47 0.00228 0.00228 0.033502 0.03 3.03 2.96 2 8.01 52.54 0.00055 0.00283 0.005779 0.01 0.61 0.59 3 11.15 76.19 0.0003 0.00313 0.004495 0.01 0.54 0.52 4 14.27 76.40 0.0004 0.00353 0.00615 0.01 0.72 0.70 5 19.03 60.96 0.00061 0.00414 0.007437 0.01 0.88 0.86 6 22.03 78.00 0.00057 0.00471 0.008892 0.01 1.08 1.05 7 26.08 67.33 0.00083 0.00554 0.011143 0.01 1.35 1.31 8 29.00 79.26 0.00074 0.00628 0.01177 0.02 1.49 1.45 9 33.09 66.77 0.001 0.00728 0.013354 0.02 1.71 1.67 Filtrate 36.05 72.51 0.01 0.02 1.74 1.70 Wash 250.00 0.00 0.02 1.78 1.73 Antimony Output Sample Time Sol'n Vol. gSb Total Sb Sb in Sb (aq) %Sb %Sb No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.0000 105.40 1 3.0069 73.47 0 0.00000 0 0.00 -0.26 -0.30 2 8.0139 52.54 5.3E-05 0.00005 0.000552 0.00 0.74 0.83 3 11.1458 76.19 0.00004 0.00009 0.00061 0.00 0.94 1.05 4 14.2708 76.40 6.3E-05 0.00016 0.000955 0.00 1.64 1.84 5 19.0278 60.96 8.8E-05 0.00024 0.001067 0.00 1.96 2.20 6 22.0313 78.00 0.00009 0.00033 0.001404 0.00 2.73 3.06 7 26.0833 67.33 0.00011 0.00045 0.001515 0.00 3.10 3.47 8 29.0000 79.26 0.0001 0.00055 0.001625 0.00 3.50 3.93 9 33.0868 66.77 0.00012 0.00067 0.001602 0.00 3.65 4.09 Filtrate 36.0486 72.51 0.00 0.00 2.66 2.99 Wash 250.00 0.00 0.00 2.75 3.09 Extreme Thermophiles, 10 g Enargite, P 8 0 of 15 microns Test#B2-E15 Extreme Thermophiles Time Initial E h Sample Medium Added Final Date Hour (days) Mass (g) pH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 20-Dec 9:40 0.00 233.71 1.52 471 691 23-Dec 9:50 3.01 209.43 1.79 373 593 5 5 24.37 233.80 28-Dec 10:05 8.02 197.78 1.60 416 636 5 5 36.04 233.82 31-Dec 13:10 11.15 210.46 1.61 391 611 5 5 24.26 234.72 3-Jan 16:10 14.27 208.70 1.49 391 611 5 5 25.16 233.86 8-Jan 10:20 19.03 189.17 1.30 380 600 5 5 45.98 235.15 11-Jan 10:25 22.03 212.33 1.40 369 . 589 5 5 30.97 243.30 15-Jan 10:40 26.04 210.25 1.48 394 614 5 5 23.27 233.52 18-Jan 9:40 29.00 212.79 1.39 395 615 5 5 25.88 238.67 22-Jan 11:45 33.09 203.37 401 621 5 5 30.56 233.93 25-Jan 10:15 36.02 213.67 1.30 399 619 Enargite In (g): Total Water (g): 10.01 266.49 Vol (mL) Mass (g) Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) Wash Volume (mL) Solid Residue (g) i - , -J 118.36 10 10 95.00 95.00 T-r;r-7r~] 213.67 83.77 250 • ' • ,• 7.89 Analysis Copper Iron Arsenic Antimony Head (wt %) 30.4 10.6 10.5 0.55 Innoculum (mg/L) 3895.65 2833.85 170.5 14.5 Medium (g/L) 0 0.20088 0 0 Samples (mg/L): #1 2709.00 655.25 55.0 2.0 #2 3934.40 1111.70 285.0 0.5 #3 4090.85 802.70 26.0 0.0 #4 5106.25 1165.05 69.0 6.0 #5 8919.70 1763.65 46.5 6.5 #6 6411.50 1132.85 315.0 6.0 #7 7339.90 1279.40 42.5 8.0 #8 7780.10 1451.05 48.5 11.0 #9 9299.25 1743.20 69.5 13.5 PLS (mg/L) 7063.95 1342.8 68.5 8.5 Wash (mg/L) 138.52 20.76 0.8 0.2 Solid Residue (wt %) 28 11.4 12.8 0.65 :'.:..*.i".v ' - , .. . . . . ;--v.;. Weight of Element Copper Iron Arsenic Antimony Head (g) 3.04304 1.06106 1.05105 0.055055 Innoculum (g) 0.0390 0.0283 0.0017 0.0001 Medium (g) 0 0.01908 0 0 Samples (g): #1 0.013545 0.00328 0.00028 0.00001 #2 0.019672 0.00556 0.00143 0.0000025 #3 0.0204543 0.00401 0.00013 0 #4 0.0255313 0.00583 0.00035 0.00003 #5 0.0445985 0.00882 0.00023 0.0000325 #6 0.0320575 0.00566 0.00158 0.00003 #7 0.0366995 0.0064 0.00021 0.00004 #8 0.0389005 0.00726 0.00024 0.000055 #9 0.0464963 0.00872 0.00035 0.0000675 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 #4 0 0.001 0 0 #5 0 0.001 0 0 #6 0 0.001 0 0 #7 0 0.001 0 0 #8 0 0.001 0 0 #9 0 0.001 0 0 PLS (g) 0.5917 0.1125 0.0057 0.0007 Wash (g) ' 0.03463 0.00519 0.0002 0.00005 Solid Residue (g) 2.2092 0.89946 1.00992 0.051285 -* '•" - • . • :'i<viisk.„,:. Calculated Head (g) 3.075 1.016 1.019 0.052 % Difference -1.036 4.228 3.055 5.241 % Extraction ' . . e^ lSs i ' ; Calculated Head 28.15 11.49 0.89 1.70 Measured Head 28.44 11.00 0.86 1.61 Copper Output Sample Time Sol'n Vol. g Cu Total Cu Cu in Cu (aq) %Cu %Cu No. (days) (mL) sampled Removed (g) sol'n (g) total (g) indicated actual 0.00 105.34 1 3.01 81.06 0.01355 0.01355 0.220 0.181 5.94 5.88 2 8.02 69.41 0.01967 0.03322 0.273 0.248 8.14 8.06 3 11.15 82.09 0.02045 0.05367 0.336 0.330 10.85 10.74 4 14.27 80.33 0.02553 0.07920 0.410 0.425 13.96 13.82 5 19.03 60.80 0.0446 0.12380 0.542 0.583 19.14 18.95 6 22.03 83.96 0.03206 0.15586 0.538 0.623 20.48 20.27 7 26.04 81.88 0.0367 0.19256 0.601 0.718 23.59 23.35 8 29.00 84.42 0.0389 0.23146 0.657 0.810 26.63 26.36 9 33.09 75.00 0.0465 0.27795 0.697 0.890 29.25 28.95 Filtrate 36.02 83.77 0.592 0.831 27.30 27.02 Wash 250.00 0.035 0.865 28.44 28.15 Iron Output Sample Time Sol'n Vol. g Fe Total Fe Fe in Fe (aq) %Fe %Fe No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 105.34 1 3.01 81.06 0.00227 0.00227 0.053 0.02 2.34 2.44 2 8.02 69.41 0.00455 0.00683 0.077 0.05 4.60 4.80 3 11.15 82.09 0.00301 0.00984 0.066 0.04 3.54 3.70 4 14.27 80.33 0.00482 0.01466 0.094 0.07 6.15 6.42 5 19.03 60.80 0.00781 0.02247 0.107 0.08 7.44 7.76 6 22.03 83.96 0.00466 0.02713 0.095 0.07 6.29 6.57 7 26.04 81.88 0.00539 0.03252 0.105 0.08 7.20 7.52 8 29.00 84.42 0.00625 0.03877 0.122 0.09 8.87 9.27 9 33.09 75.00 0.00771 0.04648 0.131 0.10 9.65 10.08 Filtrate 36.02 83.77 0.1125 0.08 7.93 8.28 Wash 250.00 0.00519 0.09 8.42 8.79 Arsenic Output Sample Time Sol'n Vol. g As Total As As in As (aq) %As % As No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 105.34 1 3.01 81.06 0.00028 0.00028 0.004458 0.00 0.26 0.27 2 8.02 69.41 0.00143 0.00170 0.019782 0.02 1.75 1.80 3 11.15 82.09 0.00013 0.00183 0.002134 0.00 0.20 0.21 4 14.27 80.33 0.00035 0.00218 0.005543 0.01 0.54 0.56 5 19.03 60.80 0.00023 0.00241 0.002827 0.00 0.31 0.32 6 22.03 83.96 0.00158 0.00398 0.026447 0.03 2.58 2.66 7 26.04 81.88 0.00021 0.00420 0.00348 0.01 0.55 0.57 8 29.00 84.42 0.00024 0.00444 0.004094 0.01 0.63 0.65 9 33.09 75.00 0.00035 0.00479 0.005213 0.01 0.76 0.78 Filtrate 36.02 83.77 0.01 0.01 0.84 0.87 Wash 250.00 0.00 0.01 0.86 0.89 Antimony Output Sample Time Sol'n Vol. gSb Total Sb Sbin Sb (aq) %Sb %Sb No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.0000 105.34 1 3.0069 81.06 0.00001 0.00001 0.000162 0.00 0.03 0.03 2 8.0174 69.41 2.5E-06 0.00001 3.47E-05 0.00 -0.18 -0.19 3 11.1458 82.09 0 . 0.00001 0 0.00 -0.24 -0.25 4 14.2708 80.33 0.00003 0.00004 0.000482 0.00 0.63 0.67 5 19.0278 60.80 3.3E-05 0.00008 0.000395 0.00 0.53 0.56 6 22.0313 83.96 0.00003 0.00011 0.000504 0.00 0.79 0.83 7 26.0417 81.88 0.00004 0.00015 0.000655 0.00 1.12 1.18 8 29.0000 84.42 5.5E-05 0.00020 0.000929 0.00 1.69 1.78 9 33.0868 75.00 6.8E-05 0.00027 0.001013 0.00 1.94 2.05 Filtrate 36.0243 83.77 0.00 0.00 • 1.52 1.60 Wash 250.00 0.00 0.00 1.61 1.70 222 Extreme Thermophiles, 10 g Enargite, P 8 0 of 37 microns Test UB2-E37 Extreme Thermophiles Time Initial E„ Sample Medium Added Final Date Hour (days) Mass (g) PH (Ag/AgCI) E„ (mV) (mL) Added (mL) Water (g) Mass (g) 20-Dec 9:40 0.00 245.95 1.56 453 673 23-Dec 9:50 3.01 216.27 1.52 385 605 5 5 29.96 246.23 28-Dec 10:00 8.01 199.61 1.37 420 640 5 5 46.64 246.25 31-Dec 13:10 11.15 218.18 1.36 408 628 5 5 27.82 246.00 3-Jan 16:10 14.27 216.51 1.35 412 632 5 5 29.77 246.28 8-Jan 10:20 19.03 202.98 1.20 411 631 5 5 43.20 246.18 11-Jan 10:25 22.03 218.37 1.26 415 635 5 5 28.33 246.70 15-Jan 11:40 26.08 208.32 1.28 439 659 5 5 37.51 245.83 18-Jan 9:40 29.00 218.54 1.26 443 663 5 5 29.26 247.80 22-Jan 11:45 33.09 209.09 443 663 5 5 36.82 245.91 25-Jan 10:15 36.02 219.38 1.15 447 667 Enargite In (g): Total Water (g): 10.01 Flask Weight (g): Innoculum in: Medium in: Total Final Weight (g): Filtrate Volume (mL) |Wash Volume (mL) Solid Residue (g) Vol (mL) Mass (g) 130.72 10 10 95.01 95.01 219.38 Analysis Copper Iron Arsenic Antimony Head (wt %) 32.4 7.2 12 0.39 Innoculum (mg/L) 3895.65 2833.85 170.5 14.5 Medium (g/L) 0 0.201 0 0 Samples (mg/L): #1 3275.80 815.20 372.0 1.5 #2 6646.85 819.10 286.5 1.5 #3 5128.70 459.30 68.5 3.0 #4 5488.95 465.45 87.0 4.5 #5 7923.80 643.60 137.0 8.0 #6 6216.20 422.00 142.5 7.5 #7 8635.90 405.40 252.5 10.0 #8 8917.05 310.05 297.0 9.5 #9 10576.80 270.95 395.5 9.5 PLS (mg/L) 8219.8 183.6 350.5 5 Wash (mg/L) 156.79 3.00 5.4 0.1 Solid Residue (wt %) 26.8 8.6 13.4 0.44 Weight of Element Copper Iron Arsenic Antimony Head (g) 3.24324 0.72072 1.2012 0.039039 Innoculum (g) 0.0390 0.0283 0.0017 0.0001 Medium (g) 0 0.01909 0 0 Samples (g): #1 0.016379 0.00408 0.00186 0.0000075 #2 0.0332343 0.0041 0.00143 0.0000075 #3 0.0256435 0.0023 0.00034 0.000015 #4 0.0274448 0.00233 0.00044 0.0000225 #5 0.039619 0.00322 0.00069 0.00004 #6 0.031081 0.00211 0.00071 0.0000375 #7 0.0431795 0.00203 0.00126 0.00005 #8 0.0445853 0.00155 0.00149 0.0000475 #9 0.052884 0.00135 0.00198 0.0000475 Medium Added (g): #1 0 0.001 0 0 #2 0 0.001 0 0 #3 0 0.001 0 0 #4 0 0.001 0 0 #5 0 0.001 0 0 #6 0 0.001 0 0 #7 0 0.001 0 0 #8 0 0.001 0 0 #9 0 0.001 0 0 PLS (g) 0.6221 0.0139 0.0265 0.0004 Wash (g) 0.0376296 0.00072 0.0013 0.000024 Solid Residue (g) 2.278 0.731 1.139 0.0374 i . I I , . , ; Calculated Head (g) 3.213 0.712 1.175 0.038 % Difference 0.939 1.181 2.155 2.835 % Extraction Calculated Head 29.10 -2.64 3.09 1.40 Measured Head 28.82 -2.61 3.02 1.36 223 Copper Output Sample Time Sol'n Vol. g Cu Total Cu Cu in Cu (aq) %Cu %Cu No. (days) (mL) sampled Removed (g) sol'n (g) total(g) indicated actual 0.00 105.22 1 3.01 75.54 0.01638 0.01638 0.247 0.208 6.43 6.49 2 8.01 58.88 0.03323 0.04961 0.391 0.369 11.37 11.48 3 11.15 77.45 0.02564 0.07526 0.397 0.408 12.58 12.70 4 14.27 75.78 0.02744 0.10270 0.416 0.452 13.94 14.08 5 19.03 62.25 0.03962 0.14232 0.493 0.557 17.17 17.34 6 22.03 77.64 0.03108 0.17340 0.483 0.586 18.07 18.24 7 26.08 67.59 0.04318 0.21658 0.584 0.718 22.14 22.35 8 29.00 77.81 0.04459 0.26117 0.694 0.871 26.87 27.12 9 33.09 68.36 0.05288 0.31405 0.723 0.945 29.14 29.42 Filtrate 36.02 75.68 0.622 0.897 27.66 27.92 Wash 240.00 0.038 0.935 28.82 29.10 Iron Output Sample Time Sol'n Vol. g Fe Total Fe Fe in Fe (aq) %Fe %Fe No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 105.22 1 3.01 75.54 0.00307 0.00307 0.062 0.03 4.61 4.67 2 8.01 58.88 0.00309 0.00616 0.048 0.02 2.76 2.79 3 11.15 77.45 0.00129 0.00745 0.036 0.01 1.00 1.02 4 14.27 75.78 0.00132 0.00878 0.035 0.01 0.96 0.97 5 19.03 62.25 0.00221 0.01099 0.040 0.01 1.63 1.65 6 22.03 77.64 0.00111 0.01210 0.033 0.00 0.61 0.62 7 26.08 67.59 0.00102 0.01312 0.027 0.00 -0.13 -0.13 8 29.00 77.81 0.00055 0.01367 0.024 0.00 -0.58 -0.59 9 33.09 68.36 0.00035 0.01402 0.019 -0.01 -1.36 -1.38 Filtrate 36.02 75.68 0.0139 -0.01 -2.00 -2.03 Wash 240.00 0.00072 -0.01 -1.90 -1.93 Arsenic Output Sample Time Sol'n Vol. g As Total As As in As (aq) %As %As No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.00 105.22 1 3.01 75.54 0.00186 0.00186 0.028101 0.03 2.20 2.25 2 8.01 58.88 0.00143 0.00329 0.016869 0.02 1.42 1.45 3 11.15 77.45 0.00034 0.00364 0.005305 0.01 0.57 0.59 4 14.27 75.78 0.00044 0.00407 0.006593 0.01 0.71 0.73 5 19.03 62.25 0.00069 0.00476 0.008528 0.01 0.91 0.93 6 22.03 77.64 0.00071 0.00547 0.011064 0.01 1.17 1.20 7 26.08 67.59 0.00126 0.00673 0.017066 0.02 1.73 1.77 8 29.00 77.81 0.00149 0.00822 0.02311 0.03 2.34 2.39 9 33.09 68.36 0.00198 0.01019 0.027036 0.03 2.79 2.85 Filtrate 36.02 75.68 0.03 0.04 2.91 2.98 Wash 240.00 0.00 0.04 3.02 3.09 Antimony Output Sample Time Sol'n Vol. gSb Total Sb Sb in Sb (aq) %Sb %Sb No. (days) (mL) sampled Removed (g) sol'n (g) total indicated actual 0.0000 105.22 1 3.0069 75.54 7.5E-06 0.00001 0.000113 0.00 -0.08 -0.08 2 8.0139 58.88 7.5E-06 0.00002 8.83E-05 0.00 -0.13 -0.13 3 11.1458 77.45 1.5E-05 0.00003 0.000232 0.00 0.26 0.27 4 14.2708 75.78 2.3E-05 0.00005 0.000341 0.00 0.58 0.60 5 19.0278 62.25 0.00004 0.00009 0.000498 0.00 1.04 1.07 6 22.0313 77.64 3.8E-05 0.00013 0.000582 0.00 1.36 1.40 7 26.0833 67.59 0.00005 0.00018 0.000676 0.00 1.69 1.74 8 29.0000 77.81 4.8E-05 0.00023 0.000739 0.00 1.98 2.04 9 33.0868 68.36 4.8E-05 0.00028 0.000649 0.00 1.87 1.93 Filtrate 36.0243 75.68 0.00 0.00 1.30 1.34 Wash 240.00 0.00 0.00 1.36 1.40 

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