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The behavior of some reagents in non-sulfide flotation 1946

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"THE BEHAVIOUR. OF SOME REAGENTS IN NON-SULFIDE FLOTATION" A Thesis Presented as P a r t i a l Requirement f o r the Degree of Master of Applied Science hy P. Raymond R. Jones, 3.A., JB.A.Sc., U n i v e r s i t y of B r i t i s h Columbia A p r i l , 1940. TABLE OE CONTENTS Page Acknowledgement 1 Porword 2 Conclusions 4 Recommendations f o r Future I n v e s t i g a t i o n 7 Reagents 8 Preparation of the Ore 9 General Procedure i n Tests 1. G r i n d i n g 10a 2. F l p a t i n g 10a Teets and Graphs 11 Assay Methods 65 1 ACKffOWLKDC-K&iKNT- The w r i t e r wirher to express hie thank? to a l l thore who have a s s i s t e d i n any way i n doing t h i s work. The WOK was c a r r i e d on under the supervision of Mr. G-. A G r i l l i e s , Professor of Ore Dressing, at the U n i v e r s i t y of B r i t i s h Columbia, and to him the author expresses sincereet appreciation f o r help and advice. The assistance of Mr. A. G-. C. L y l e , who worked as the author's colleague during the e a r l i e r part of t h i s work, cannot De overestimated. Many of the ideas worked out in t h i s t h e s i s are h i e , arid of hie u n f a i l i n g energy and capacity f o r work too much cannot be s a i d . To Mr. P. A. forward,.Assistant Professor of Metallurgy, U n i v e r s i t y of B r i t i s h Columbia, many thanks are due f o r help and advice i n aseaying. 2 JTORvYOHD The research which i a described i n t h i s report was begun as an e f f o r t to carry on the work of Elfetrora and Dayton i n the f i e l d of hon-Sulfide F l o t a t i o n , c a r r i e d on during the previous U n i v e r s i t y term. During the course of t h e i r research they made numerous t e s t s , ueir.g various reagents, to i n v e s t i g a t e the separation by f l o t a t i o n of s i l i c a , D a r i t e , and c a l c i t e . For the sake of s i m p l i c i t y i n p r e l i m i n a r y i n v e s t i g a t i o n , they used a synthetic ore, composed of crushed b a r i t e aficl lime et one, and pare s i l i c a s;.nd. An examination of t h e i r report showed that they had made an e x c e l l e n t survey of the use fulness of various reagents i n the f l o t a t i o n of the aoove minerals. However, as. they covered a great deal of ground i n the course of t h e i r work, they did not make a very f u l l i n v e s t i g a t i o n of the action of any of the reagents they used. For example, i n f l o a t i n g o f f a concentrate, they very of- ten added eo much reagent that the f l o t a t i o n of too large a bulk of concentrate prevented t h e i r o b taining a good recovery, as expressed by the Three-Mineral Index ( i . e . the sura of the recovery of the desired mineral i n the concentrate, and the losses of the undeeired minerals to the t a i l s ) . At other times the product obtained was too small to give a good r e - covery. In such cases, i t was seen that good recoveries might be obtained, using the same reagents, but in d i f f e r e n t amounts. 3 tfith t h i s object i n view, the author and h i e colleague oe- gan to check over the teete g i v i n g promise of oeet r e s u l t s . The method used to check these r e s u l t s , i . e . - - t h e removal of a number of concentrates, and the drawing of graphs, showed some very i n t r i g u i n g p o s s i b i l i t i e s , and throughout t h i s work more a t t e n t i o n i e paid to the method of i n v e s t i g a t i o n , and to i t e p o s s i b l e value as a research t o o l , than to the making of good separations. 4 CON CLUE 10 Kg 1. By talcing o f f a number of concentrates from a s i n g l e t e s t , smooth graphs may be p l o t t e d , showing (a) Recovery vs. weight of concentrate. (b) Weight of product vs. amount of reagent used. 2. 'With some combinations of reagents the graphs (a) above are p a i r s of i n t e r s e c t i n g s t r a i g h t l i n e s , or, i n other words, the recovery i s i n d i r e c t r a t i o to the weight of con- centrate removed up to a c e r t a i n p o int, where there i s a sharp break: i n the curve, and the recovery v a r i e s from that point as a new.direct r a t i o of the weight of concentrate removed. 3. The "recovery vs. weight of c o n c e n t r a t e " curve may break e i t h e r up or down, or may continue as a s t r a i g h t l i n e , depending on the mineral f o r which the recovery i s being p l o t - ted, and on the reagents used. 4. The break-points i n the recovery graphs f o r s i l i c a , b a r i t e , and limestone may occur at very n e a r l y the same weight of product, i n which case a graph showing the Three Mineral Index f o r any one of the minerals w i l l also show a sharp break- point, u s u a l l y a maximum. I f the recovery graphs, when produced, pass through zero recovery at zero weight of concentrate, and through 100$ re- covery at f u l l weight of product, then the Three M i n e r a l Index graph w i l l pass through 200 at zero concentrate, and 100 at the point where the f u l l charge has been ( t h e o r e t i c a l l y ) f l o a t e d . 5. For combinations of reagents which give these broken l i n e s , the maximum Three M i n e r a l Index obtainable by v a r y i n g 5 one reagent ( f r o t h e r - c o l l e c t o r i n these t e s t s ) may be found from a graph, and f o r t h i s graph i t may be necessary to take o f f only two concentrates, one on e i t h e r side of the maximum index. 6. The maximum obtainable Index may always be found from the r e s u l t s of a s i n g l e t e s t , provided care i s taken to f l o a t s u f f i c i e n t product to p l o t r e c o v e r i e s on both sides of the maximum. 7. When a t e s t i s run using a reagent A as a f r o t h e r - c o l l e c t o r , and reagents 3 and C as depressor and a c t i v a t o r , a curve may be obtained showing d i r e c t l y the r e c o v e r i e s obtain- able by f l o a t i n g d i f f e r e n t q u a n t i t i e s of concentrate (by vary- i n g the amount of A ) . A t e s t may then be run u s i n g d i f f e r e n t amounts of B or C, or with a d d i t i o n of a new reagent D, and a s i n g l e concen- t r a t e taken o f f . I f the Three M i n e r a l Index from t h i s t e s t l i e s above the Three Mineral Index curve from the f i r s t t e s t , i t i s i n d i c a t i v e that a higher maximum Index may be obtained with t h i s a l t e r a t i o n i n B or 0, or the a d d i t i o n of D, than was obtainable with the o r i g i n a l combination of 3 and G. 8. A given q u a n t i t y of a f r o t h i n g - c o l l e c t i o n reagent brings up a l a r g e r amount of product when added a l l at once and a s i n g l e concentrate removed, than when added in s e v e r a l f r a c t i o n s , and a concentrate removed a f t e r each a d d i t i o n . 9. Sodium metaphoephate i s not a completely s a t i s f a c t o r y depressor f o r limestone, i n the presence of s i l i c a and b a r i t e , u s ing Emuleol X - l to f l o a t b a r i t e . Probably sodium hexa- metaphosphate w i l l be found to be more s a t i s f a c t o r y . 10. G r i n d i n g i n an i r o n m i l l does not appear to i n h i the a c t i o n of the reagents used i n b a r i t e f l o t a t i o n . 7 RECOMHBKDATIOhg' FOR FUTURE IMVEPTIGATIOK 1. More work should he done i n i n v e s t i g a t i o n of the use- fulness of the "recovery v s . weight of product" curves, tfork along t h i s l i n e could be combined with continued research into the use of various c a t i o n i c reagents in non-sulfide f l o t a t i o n . The author recommends that other reagents than those used be t r i e d , to see i f the curves obtained u s i n g Lissolamine A and Emulsol X - l ean also be obtained using other reagents. 2. I f p o s s i b l e , a commercial ore, of as simple a comp- o s i t i o n as can be obtained, should be used instead of a syn- t h e t i c ore. 3. The a p p l i c a t i o n of the graphs used i n t h i s research to s u l f i d e f l o t a t i o n should be looked i n t o . In separation of one s u l f i d e from an ore containing other s u l f i d e s and gangue, i t i s possible that the gangue minerals might be considered as a s i n g l e component i n p l o t t i n g r e c o v e r i e s . 4. Regulation of the a i r i n l e t of the fagergren c e l l might r e s u l t i n better s e l e c t i v i t y i n some t e s t s . In the work done the a i r i n l e t was kept f u l l open during a l l t e s t s , f o r the sake of uni f o r m i t y . 5. Regulation of PH i s suggested as a possible means of obtaining a b e t t e r limestone-barite separation. 8 RBASENTS L i s sola-mine "A" ( c e t y l t r i m e t h y l ammonium bromide—manufact- ured by C. I . L . ) . This substance has good f r o t h i n g proper- t i e s , and e x c e l l e n t c o l l e c t i n g properties f o r a c t i v a t e d s i l - i c a . I t i s f a i r l y soluble i n water, and was added as a water s o l u t i o n to the f l o t a t i o n c e l l . Copper Sulfate--This reagent was used as an a c t i v a t o r f o r s i l i c a . Experience has shown that s i l i c a w i l l not f l o a t unless a c t i v a t e d by a base-metal s a l t . Emulsol X - l - - a sulphated higher a l c o h o l (composition not given), manufactured by The Emulsol Corporation of Chicage, 111. This reagent was used as a c o l l e c t o r f o r b a r i t e . I t ' s chief draw-back i s a d e f i n i t e tendency to f l o a t limestone. I t needs no f r o t h e r . Sodium Metaphosphate—used as a depressor f o r limestone. This reagent did not seem very s a t i s f a c t o r y . Three Mineral Index curves obtained from t e s t s where t h i s reagent was used were f i t t e d i n same cases by t e s t s made by Elftom & Dayton, i n which they used no depressor. Sodium Hexa-Metaphosphate--used as a depressor f o r limestone. This reagent was not very f u l l y i n v e s t i g a t e d , but seems to show p o s s i b i l i t i e s of being a b e t t e r reagent than the meta- phosphate . Sulfonated Cod O i l—(f r o m Cave & Co., Vancouver, B . C ) . This reagent was used as a c o l l e c t o r f o r b a r i t e . I t seems to have some c o l l e c t i n g action f o r both b a r i t e and limestone, with a marked tendency tc prefer the b a r i t e i n the presence of sodium metaphosphate. 9 ' PREPARATION OF THE ORE (a) M a t e r i a l s . To carry on work: done by Elftom & Dayton, a synthetic ore was used. This ore was a mixture of s i l i c a sand, crushed white marble, and crushed b a r i t e . Assays on the limestone and b a r i t e were as f o l l o w s : Limestone B a r i t e CaCO^ ....96.4$ BaSO 90.2$ BaSO? 0.6 CaCO 0.6 SiOo 3.0 SiOg 5  8.1 100.0% * 98.9% The s i l i c a sand was assumed to be free of c a l c i t e and b a r i t e , but may have contained small amounts of other s i l i c - a t e s . (b) Crushing. The marble and b a r i t e were crushed i n a small l a b - oratory jaw crusher, then reduced by r o i l s . They were mechan- i c a l l y screened a f t e r each reduction u n t i l a l l was minus ten mesh. The crushed limeetone and b a r i t e and the s i l i c a sand were mixed i n the approximate proportions of 30:30:40 r e s p e c t i v e l y . The f o l l o w i n g assays were obtained from the mixture: 03.00 ry ••••••• 31 • (Z^O BaSO^ 29.3 SiO p 38. 6 99.1$ (c) G r i n d i n g . For the most part, the ore was ground i n a small por- c e l a i n pebble m i l l , i n s ide dimensions approximately 6" long x diameter, with a charge of pebbles weighing 1425 grams. 10 The charge in a l l cases was 500 grams of ore and 500 grams of water. The grind was for 30 minuteB, at 70 r.p.m. An automatic stop clock was used to time the grinding. Two tests were ground in an iron rod m i l l , inside dim- ensions 11" x 10" diameter, with thirteen 1" rods. The grind was for 15 minutes at 44 R. P. M. Complete screening tests were not made. A one hundred gram sample of a 30-minute pebble mill grind showed the f o l - Screen Size f0 Weight A s s a y  u/o BaS04 SiOg CaCO, o -200 -150,+200 + 150 62.9 23.6 13.5 38.9 18.4 6.9 26.5 51.6 63.0 35.1 29.0 24.6 A sample of a rod mill grind—20 minutes at 44 S. P. M., with 13 rods, showed the following: Screen Size fo Weight -200 69.3 -150,+ 200 21.5 +-150 9.2 This grind was too fine to run comparative tests with pebble mill grinds, so the tests were made on a 15-minute grind, which was assumed roughly comparable to the 30-min- ute pebble mill grind. 10 a GENERAL PROCEDURE IN TESTS 1. G r i n d i n g . The g r i n d i n g process was ae described i n the pre- ceding s e c t i o n . In some cases reagents were added to the m i l l (copper s u l f a t e and sodium metaphosphate). The usual charge c o n s i s t e d only of 500 grams of ore and 500 grams of water. The f u l l charge of pebbles was used at a l l times i n the pebble m i l l * When the automatic stop clock stopped the motor, the m i l l was undamped from the frame, and removed to a sink. The cover was removed, and adhering pulp washed i n t o a pan, u s i n g a f i n e stream of water. The pebbles were next removed from the m i l l (by hand) and"placed on a heavy wire screen over the same pan, where the pulp was c a r e f u l l y washed from them. The m i l l was now t i p p e d up over the pan, and the r e - mainder of the pulp washed i n t o the pan. 2. g l o a t i n g . (a) The C e l l The f l o t a t i o n c e l l used was a Laboratory Fagergren F l o t a t i o n Machine, with a molded pyrex glass f l o t a t i o n cham- ber. The c a p a c i t y was just s u f f i c i e n t f o r a 500 gram charge at 4:1 d i l u t i o n . T h i s machine has the advantages of very simple and convenient operation and easy cleaning, but gives l e s s oppor- t u n i t y of s e l e c t i v e d r a i n i n g of the f r o t h than does a Ruth f l o t a t i o n machine. I t i s also more d i f f i c u l t to skim. 11 TESTS Test Ho 72 (Repeat of Test Ho. 8) To pebble m i l l - - Ore 500 gms. Water 500 gms. CuS0 4 0. 50# I t on G r i n d — 3 0 min. © 70 R. P. M. To c e l l — l a t e r — s u f f i c i e n t to give d i l u t i o n 4:1 #1 Gone. Liseolamine A 0.16# 1 ton Conditioned 1 min. Skimmed 3 l/3 min. F r o t h . — l a r g e bubbles, not p l e n t i f u l . #2 Cone. hissolamime A 0.16# 1 ton. Conditioned 1 min. Skimmed 3 l / 3 min. F r o t h — S m a l l e r bubbles, f a i r l y p l e n t i f u l . #5 Gone. l i s s o l a m i n e A 0.16# 1 ton. Conditioned 1 min. Skimmed 3 l / 3 min. F r o t h — V e r y f i n e bubbles, so p l e n t i f u l that very l i t t l e skimming was necessary. Ph Gone. #1 #2 #3 = 12.0 T a i l s = 12.2 12 Wt. of Gone. #l + #2+#3 = 253.3 gms. T a i l s = 245.2 gms. 498.5 Test 1o A S S A Y % RECOVERY 6Jo 3 Min. IHDBX 72 Wt. BaS0 4 GaGO^ o s i o 2 BaSO. 4 GaC0 3 S i O g Peed 100.0 27.9 29.4 42.7 100.0 100.0 100.0 G 49.2 10.7 13.0 72.0 18.8 22.5 88.5 247.2 T 50.8 44.7 46.2 9.1 81.2 77.5 11.6 Purpose of T e s t — t o repeat Test #8, which gave the best 3- mineral index f o r S i l i c a f l o t a t i o n i n work done by E l f e t r o m & Dayton. Summary of Test. I t was evident from the r e s u l t s of Test #8 that the Lissolamine A was not added a l l at once, but data as to how i t was added was not given. A p r e l i m i n a r y t e s t was run adding the f u l l amount of Lissolamine A at the beginning. The concentrate obtained was too small to give any p o s s i b i l i t y of a good recovery, so the products were not assayed. A t e s t was then run adding 0.16# 1 ton L i s s o l . (1/3 the amount used i n t e s t #8) at a time. The f i r s t a d d i t i o n was not enough to give much of a concentrate. The second a d d i t i o n brought up a f a i r concentrate, which was added to the f i r s t . The f i n a l a d d i t i o n brought up a very heavy f r o t h - - f i n e bubbles - - r i s i n g i n the machine and overflowing the l i p without skimm- in g . This was added to the f i r s t two. • . I t appeared that the f i r s t a d d i t i o n was almost e n t i r e l y 13 adsorbed, l e a v i n g l i t t l e or none to form a f r o t h . The second a d d i t i o n a l s o l e f t l i t t l e Lissolamine to f r o t h . On the 3rd a d d i t i o n enough Lissolamine appears to have accumulated i n the c e l l to give a good f r o t h . The assays of the combined concentrates, and of the t a i l s , showed an 88.5% SiOg recovery, and a grade of 72.0% i n the concentrate (from a heads of 40% S i 0 2 ) . There was £2.5% of the GaCO_ and 18.8$ of the Ba80„ i n the cone. The 3-mineral 6 4 index was £47.2--lower than f o r t e s t #8. 14 Test Mo. 73 To Pebble M i l l — Ore 500 gme. tfater 500 gme. CuS0 4 0. 50# / ton. Grind--30 min. & 70 B. P. M. To c e l l — l a t e r s u f f i c i e n t to give d i l u t i o n 4:1 #1 Gone, l i s s o l a m i n e A. 0.24# /ton Conditioned 3 min. Fr o t h poor so no skimming attempted. Lissolamine A--0.12# / ton Conditioned 3 min. Skimmed 3 min. F r o t h — f a i r l y p l e n t i f u l , bubbles coarse. #2 Cone. Lissolamine A 0.12# / ton Conditioned 3 min. Skimmed 3 min. F r o t h — v e r y p l e n t i f u l , bubbles f i n e . #3 Gone. Lissolamine A 0.16# / ton Conditioned 3 min. Skimmed 2 min. F r o t h — v e r y p l e n t i f u l , bubbles very f i n e and w e l l m i n e r a l i z e d f o r -| min. 15 #4 Cone. Liseolamine A--0.16# / ton. Conditioned 3 min. Skimmed 2 min. F r o t h — v e r y p l e n t i f u l , bubbles very f i n e but poorly m i n e r a l i z e d . #5 Cone. LiBEolamine A—0.16# /ton. Conditioned 3 min. Skimmed 2 min. F r o t h — v e r y p l e n t i f u l , bubbles very f i n e but poorly m i n e r a l i z e d . Cone—PH = 12.3 T a i l s — P H =10.9 1 wt. Wt. L i e s . A (gms) (%) # /ton Gone. #1 " f2 " #3 " #4 " #5 T a i l s 34.0 6.8 0.36 135.4 26.9 0.12 141.5 28.0 0.16 105.0 20.8 0.16 69.4 13.7 0.16 19.1 3.8 (Weight x Assay) y (*) .. A S s a y % R e c o v e r y Wt. R e c o v e r BaS04 CaC0 3 SiO 2 BaSO, 4 GaG0 3 SiO g BaS0 4 CaCO^ S i 0 2 8.2 10.9 69.7 2.8 3.7 23.7 2.0 2.8 11.7 11.2 12.6 70.0 - 15.2 17.1 94.8 10.8 12.8 46.7 24.5 21.3 49.2 34.7 30.1 69.6 24.6 22.6 34.2 46.5 39.9 9.6 48.9 41.0 10.1 34.7 30.8 5.0 44.6 48.2 4.6 30.9 33.4 3.2 21.9 25.1 1.6 |43.9 40.4 8.3 8.4 7.7 1.6 6.0 5.9 0.8 Grade of Accum. Accum. Accum , Accumulative y (#>. Product 3 Min. Product Wt. % Wt. R e c o v e r G r a d e ( (gms) BaSO, A 0aC0 3 SiO 2 BaS0 4 CaC0„ 6 SiO 2 Index Cone. #1 34.0 6.8 2.0 2.8 11.7 8.2 10.9 69.7 206.8 #2 #3 169.4 33.7 12.8 15.6 58.4 10.7 12.3 69.9 230.0 310.9 61.7 37.4 38.2 92.6 17.0 16.4 60.5 217. 2 #4 415.9 82.5 72.1 69.0 97.6 24.4 21.9 47.8 156.7 #5 485.3 96.2 94.0 ' 94.1 99.2 27.3 25.9 41.4 111.3 T a i l s 504.4 100.0 100.0 100.0 100.0 28.0 26.4 40.3 1C0.0 i — 1  e o - T E S T T 3 — -4 s - . O s . - ? z U 0 K ul 5 i J Z 3 J U < 4 0 20 - C a C O - I 0 0 2 0 4.0 6 0 e o IOO A c c U M U L A T I V E re 1 ISl  17 Purpose of Test Prom the r e s u l t of #7 2 i t was seen that a l a r g e number of t e s t s would have to be run to f i n d the best p o s s i b l e index to be obtained using Lissolamine A as a SiOg c o l l e c t o r . There- fore i t was sought to devise a method by which the desired quantity of Lissolamine might be c l o s e l y estimated from the r e s u l t s of a s i n g l e t e s t . Summary of Test With the above object i n view, a t e s t was run u s i n g small a d d i t i o n s of Lissolamine at i n t e r v a l s , c o n d i t i o n i n g a f t e r each a d d i t i o n . ( i . e . - - e q u i l i b r i u m e s t a b l i s h e d between L i s s . i n e o l . and L i s s . r e a c t i n g with i n t e r v a l surfaces.) Prom t e s t #72 i t was seen that adding l e s s than 0.32# /ton of L i e s , would give very l i t t l e recovery, but to make sure of ob t a i n i n g a good s e r i e s of r e s u l t s 0.24# /ton was added f o r the f i r s t concentrate, and was conditioned f o r 3 min. The F r o t h formed when the a i r - v a l v e was opened was very weak and small i n amount, and no skimming was attempted. - A second a d d i t i o n of 0.12# /ton L i s s . was made, and the f r o t h t h i s time was f a i r l y p l e n t i f u l , with coarse bubbles. A concentrate was taken o f f . For the 2nd concentrate another 0.12# /ton was added, and a very f i n e f r o t h formed, r i s i n g i n the c e l l and over- flowing the l i p . Three f u r t h e r a d d i t i o n s of 0.16# /ton L i e s o l . were made, and a concentrate taken o f f a f t e r each a d d i t i o n . Toward the end the f r o t h , while very p l e n t i f u l , was very poorly mineral- 18 i z e d . The f i v e concentrates and the t a i l s were assayed. From the r e s u l t s the f o l l o w i n g graphs were p l o t t e d : — 1. Grade vs. recovery f o r three products. 2. Lissolamine added vs. weight of product. 3. Weight of concentrate vs. 3- Min. Index. In "1" the CaCO^ and 3aS0 grades increased as the recov- a 4 ° ery went up f o r the whole range of the t e s t s — u p to 100% r e - c o v e r y — i n a smooth curve, n e a r l y a s t r a i g h t l i n e i n both cases. The SiOg curve was a s t r a i g h t l i n e up to about 89$ recovery, Out there showed a sudden break, the grade decreasing r a p i d l y with recovery, again i n approx. a s t r a i g h t l i n e . In "2" a smooth curve was obtained, showing a tendency to l e v e l o f f at the t o p — d u e probably to the decreasing weight of Eolids i n the pulp. No. 3 i n d i c a t e d a sharp maximum 3-raineral index, r i s i n g in a s t r a i g h t l i n e to the max., and f a l l i n g i n a s t r a i g h t l i n e again. From t h i s graph i t looked as though i t might be poss- i b l e to p r e d i c t the best t e s t with a given reagent by making only two concentrates and a t a i l i n g — a s two points on the graph are already given by the i n i t i a l index of 200 and the f i n a l index of 100. 19 Test No. 74 To Pebble M i l l . Ore 500 gms. Water 500 gms. Grind--30 min. @ 70 H. P. M. To C e l l . Water to give d i l u t i o n 4:1 Sod. Metaphosphate—1.0# /ton. Conditioned 3 min. Proth--very poor eo no skimming attempted. #1 Cone. Emulsol(X-l) - 1 drop. (1 drop - 0.033 gm.) Conditioned 3 min. Skimmed -J- min. Proth--poorly m i n e r a l i z e d , no skimming attempted. Emulsol X - l - 1 drop. Conditioned 3 min. Skimmed -g- min. F r o t h — f a i r l y w e l l m i n e r a l i z e d . #2 Cone. Emulsol X-l-1 drop. Conditioned 3 min. Skimmed % min. #3 Cone. Emulsol X-l-2 drops. Water--500 c. c. Conditioned 3 min. Skimmed |- min. so #4 Gone. Emulsol X-l-3 drops. Water--500 c.c. Conditioned 3 min. Skimmed min. #5 Cone. Emulsol X-l-3 drops. Water--500 c. c. Conditioned 3 min. Skimmed -g- min. #6 Cone. Emulsol X.-1 -3 drops. Water—500 c.c. Conditioned 3 min. Skimmed lr min. #7 Cone. Emulsol X-l-3 drops. Water—500 c. e. Conditioned 3 min. Skimmed -| min. si Test No. 74 (Con 1d) PH = 11.0 Prod. Cone.#1 #2 #3 • #4 #5 #6 #7 T a i l s Wt. 77.1 58.0 74.2 46.9 24.9 4.5 11.4 196.6 Emulsol X - l (drops)A 2 1 2 3 3 3 3 4 1 drop s 0.033 gm Emulsol X - l Accu P - l . Drops of Product wt. Emulsol X - l (gms) (accumulative) Cone. #1 77.1 2 135.1 3 #3 209.3 5 #4 256.2 8 #5 281.1 11 #6 285.6 14 #7 297.0 17 | T a i l s 4-93-6 Purpose and Summary. Test #71 ( E l f s t r o m & Dayton) showed a good r e s u l t u s i n g Emulsol X - l as a b a r i t e c o l l e c t o r , and Sodium Metaphosphate as a limestone depressor. I t was run at 40°, but there was no evidence that the high temperature was re s p o n s i b l e f o r the good r e s u l t . I t was decided to run a t e s t u s i n g the reagents Emul- s o l X - l and NaPO^. Test #74 was run to f i n d j u s t about where the Dest concen- t r a t e should l i e from a curve of "Wt. of product vs. drops of reagent". A smooth curve was obtained, and i t was seen that between 3 and 4 drops should give the best r e s u l t (about 150 (1 dr. Em.--X-1 = o.l32# Ton.). 23 Test Ho. 75 To Pebble M i l l Ore , . . . .500 gms. Water 500 gms. Grind--30 min. <g> 70 R. P. M. To C e l l Water to give d i l a t i o n 4:1 Sod. Metaphosphate 1.0# / t o n . #1 Gone. Emulsol X - l -3 drops. (ldrop - 0.033 gm.) Conditioned 3 min. Skimmed 1 min. #2 Gone. Emulsol X - l -3 drops Conditioned 3 min. Skimmed 1 min. #3 Gone. Emulsol X - l -3 drops Water--500 grams. Conditioned 3 min. Skimmed 1 min. #4 Gone. Emulsol X - l -3 drops l a t e r — 8 0 0 grams. Conditioned 3 min. Skimmed 1 min. 24 #5 Cone. Emulsol X - l -3 drops. Sodium metaphosphate 1.0# /ton water--800 grams. Conditioned 3 min. Skimmed 1 min. PH—8.55 Product Wt. Emulsol X - l (gms) (drops) 4 Cono#l. 163.2 3 #2 86.0 3 #3 42.0 3 #4 9.0 3 #5 3.3 3 T a i l s 193.6 & 1 drop = 0.033 gnu Emulsol X - l Accum. Drops of Product Wt. Bmulsol('X-l^ ;i; (gms) (accumulative) Cone. #1 163.2 3 #2 249.2 6 #3 291.2 9 #4 300.2 12 #5 303.5 15 T a i l s 497.1 Purpose and Summary of Test To cheek the c o l l e c t i n g p r o p e r t i e s of HaP0 3 a t e s t was run with a second a d d i t i o n of t h i s reagent a f t e r 12 drops of Em-X-1 had been added. The curve obtained showed no i r r e g u l a r i t y at the point where the EaP0 3 was added, so i t was assumed that the amount of t h i s reagent i n the pulp had l i t t l e or no e f f e c t on the shape of the product-reagent graph, (provided i t be present i n s u f f i c i e n t amount to depress the Is.) 25 Test No. 76 To Pebble M i l l . Ore 500 gms. Water 500 gms. Grind--30 min. @ 70 E. P. M. To C e l l . Water to give 4:1 d i l u t i o n . Sod. Metaphosphate—1.0# /ton. fl Gone. Emulsol X - l 2 drops. (1 drop - 0.033 gm.) Conditioned 3 min. Skimmed 1 min. P r o t h - - p l e n t i f u l , bubbles f i n e and w e l l m i n e r a l i z e d . #2 Gone. Emulsol X-1--1 drop. Water--500 grams. Conditioned 3 min. Skimmed 1 min. P r o t h — f a i r l y p l e n t i f u l , bubbles f i n e and f a i r l y w e l l m i n e r a l i z e d . #3 Cone. Emulsol X-1--1 drop. Water—500 grams. Conditioned 3 min. Skimmed 1 min. P r o t h — p l e n t i f u l , bubbles very f i n e but poorly m i n e r a l i z e d . 26 #4 C o n c . Emulsol X-1--3 drops. Water--500 grams. Conditioned 3 min. Skimmed 1 min. Pro t h . - - p l e n t i f u l , bubbles very f i n e and w e l l mine r a i l zed. #5 Cone. Emulsol X - l — 3 drops. Conditioned 3 min. Skimmed 1 min. F r o t h — p l e n t i f u l , bubbles f i n e but not w e l l m i n e r a l i z e d , #6 Cone. Emulsol X-1--6 drops. Conditioned 3 min. Skimmed 1 min. F r o t h — p l e n t i f u l , bubbles f i n e and f a i r l y w e l l m i n e r a l i z e d . PH— 6 . 6 Wt. (gms) Wt. (%) A s i 3 a y Assay x Weight Recovery ( i) BaS© 4 CaC©„ o sio 2 BaS0 4 CaC0„ o S i 0 g BaS0 4 CaCOg S I C Cone. #1 107.8 21.5 62.7 23.0 13.5 67.5 24.8 14.5 45.6 17.7 7.1 #2 40.2 8.0 61.3 23.9 16.7 24.6 9.6 6.7 16.7 6.8 3.3 #3 23.3 4.7 63.4 22.8 17.4 14.8 5.3 4.1 10.0 3.8 2.0 . #4 51.8 10.4 45.3 28.5 23.9 23.4 14.7 12.4 15.8 10.5 6.0 #5 33.7 6.7 24.2 44.0 29.5 8.2 14.8 10.0 5.6 10.5 4.9 #6 83. 5 16.6 3.7 53.5 31.2 3.1 44.7 26.0 2.1 31.9 12.5 T a i l s 160.6 32.1 0.38 16.6 62.0 6.1 26.6 132.0 4.2 18.8 64.2 Product Accum. Wt. (gms) Accum. Wt. (fo) Accumulative Recovery (fo) Grade of Accum. Product {*&) 3 Min. Index BaS0 4 CaC0 3 S10 o BaS0 4 CaC0 3 S10 ? Cone. #1 107.8 21.5 45.6 17.7 7.1 62.7 23.0 13.5 220.8 #2 #3 148.0 29.5 62.3 24.5 10.4 62.1 23.2 14.3 227.4 171.3 34.2 72.3 28.3 12.4 62.4 23.2 14.8 231.6 • #4 223.1 44.6 88.1 38.8 18.4 58.5 24.4 16.9 230.9 #5 256.8 51.3 93.7 49.3 23.3 54.0 26.9 18.6 221.1 #6 340.3 67.9 95.8 81.2 35.8 41.3 33.2 21.8 178.8 T a i l s 500.9 100.0 100.0 . 100.0 100.0 28.5 28.1. 41.0 100.0  i  28 Purpose To eee i f curves s i m i l a r to those obtained f o r L i e s o l - amine A might be drawn f o r Emulsol X - l . Summary Prom the r e s u l t s of t e s t #7 5 i t was seen that the best index could not be obtained with l e s s than 2 drops of Em. X - l , so t h i s amount was added f i r s t , with l#/ton of NaPOg. Two f u r t h e r a d d i t i o n s of 1 drop were made, two of 3 drops, and one of 6 drops. The l a s t a d d i t i o n was made i n an attempt to check the shape of the product-reagent curve at the upper end, as a tendency to r i s e a f t e r f l a t t e n i n g was n o t i c e d from t e s t #74. It was r e a l i z e d l a t e r that t h i s a d d i t i o n should have been c a r r i e d f a r t h e r . The graph showed the r i s e a l l r i g h t , but another reason might have caused i t . I t was n o t i c e d prev- i o u s l y that a s i n g l e l a r g e a d d i t i o n of reagent seems to b r i n g up a l a r g e r bulk of product than two smaller ones g i v i n g the same t o t a l reagent. graphs Graphs were drawn as f o r t e s t 73. P l o t t i n g the accum- u l a t i v e recovery against the c a l c u l a t e d grade of combined products showed the sharp break in the BaSO^ curve that was shown i n t e s t #73 f o r s i l i c a . A corresponding point was i n - dicated f o r limestone, while the s i l i c a curve continued as a s t r a i g h t l i n e throughout the range of the t e s t s . I n t e r p r e t a t i o n of the above seems r a t h e r . d i f f i c u l t at present. I t seems to represent some d i f f e r e n c e i n the a c t i o n of the reagents used on s i l i c a on the one hand, and on lime- 29 stone and b a r i t e on the other. The grade of s i l i c a i n c r e a s - es as a l i n e a r f u n c t i o n of the product taken up. The grades of limestone and b a r i t e increase up to a point (where the re- covery = approx. 94$ f o r eaeh of these minerals) and then suddenly f a l l o f f . The graph of recovery vs. weight of cone, showed some i n t e r e s t i n g p o s s i b i l i t i e s : - - The Three-Mineral Index curve p l o t t e d two s t r a i g h t l i n e s , passing through 200 and 100 as before, and i n t e r s e c t i n g to give a max. index of 240 f o r these reagents under these c o n d i t i o n s , but the graph showing the l o s s e s of limestone and s i l i c a to the t a i l s d i d not pass through the 100 point, although they p l o t t e d s t r a i g h t l i n e s as before, with the break i n the curve at the product g i v i n g the maximum Three-Min. Index, as i n te s t 73. The GaG0 3 l o s s graph crosses the l i n e of zero recovery at 380 g. of p r o d u c t — a n d may be i n t e r p r e t e d as meaning that i f a product were made con t a i n i n g 380 g., i t would contain a l l - t h e limestone. The s i l i c a l o s s graph d i d not cross the l i n e of zero r e - covery at a l l . I t cut the 500 gm. product l i n e at 40$—seem- ing to i n d i c a t e that a l l the s i l i c a could not be f l o a t e d with these reagents. I t was no t i c e d that Lissolamine A. brought up n e a r l y the whole at the charge during the t e s t (#73)—whereas Emulsol X - l began to b r i n g up very l i t t l e toward the end of the t e s t (#76) --and yet l e f t a large t a i l i n g . This d i f f e r e n c e i s well i l l - 30 u s t r a t e d by the i r r e g u l a r i t i e s of the graphs f o r Emulsol X - l . When the limestone curve i s produced to cross the 500g. product l i n e , i t cuts at -40%-- which accounts f o r the balance b r i n g i n g the Three-Mineral Index curve to the 100% mark as be f o r e . This may be a c c i d e n t a l , and very p o s s i b l y the index curve does not always go through 100. 31 Test No. 7 7 To Pebble M i l l . Ore 500 gms. Water 500 gms. Grind--30 min. @ 70 R. P. M. To C e l l . Water to give 4:1 d i l u t i o n . Sodium Metaphoephate 1.0# /ton. #1 Cone. Emulsol X - l 5 drops ( 1 drop = 0.033 gms.) Conditioned 3 min. Skimmed 1 min. P r o t h — v e r y p l e n t i f u l , bubbles f i n e and w e l l m i n e r a l i z e d . Wt. of Cone #1 = 236.7 T a i l s = 261.7 Test 77 - Wt. % Assay % Recovery % 3 Min. Index BaS0 4 CaCO, S i O g BaSO 4 CaCO „ o SiGg Peed C T 100.0 47.5 52.5 27.9 53.7 5.7 , 29.4 26.4 32.1 42.7 17.0 65.6 100.0 89.5 10.5 100.0 42.7 57.3 100.0 19.0 81.0 227. £ 32 This t e s t was run to compare the e f f e c t of adding a l a r g e s i n g l e amount of reagent with that of adding the same t o t a l reagent i n smaller q u a n t i t i e s . We had some i n d i c a t i o n pre- v i o u s l y ( t e s t s 72 compared to t e s t 73, and the r i s e i n the pro- duct-reagent curve f o r t e s t 76) that a l a r g e r product would be obtained by the s i n g l e a d d i t i o n , and we wished to f i n d i f t h i s was t r u l y the case, and a l s o i f the product obtained by the larg e a d d i t i o n would s a t i s f y the product-recovery graph obtain- ed by the smaller a d d i t i o n s . A point near the max. 3-mineral index was chosen, and 5 drops of reagent added, as i n d i c a t e d by the product-reagent graph, to give the d e s i r e d product. The product was l a r g e r than that obtained by the small additions—236.7 gm. against 210 gm. shown by the graph. 33 Test Ro. 78. To Pebble M i l l . Ore p 500 gms. Water - 500 gme. Sodium Metaphosphate = 1.0# /ton. Grind--30 min. @ 70 fi. P. M. To C e l l . Water to give 4:1 d i l u t i o n . #1 Gone. Emulsol X - l — 1 drop ( ldrop - 0.033 gm.) Conditioned 3 min. Skimmed 1 min. #2 Gone. Emulsol X-1--1 drop. Water--700 grams. Conditioned 3 min. Skimmed 1 min. #3 Gone. Emulsol X - l — 1 drop. l a t e r - - 6 0 0 grams. Conditioned 3 min. Skimmed 1 min. #4 Cone. Emulsol X-1--1 drop". l a t e r - - 2 0 0 grams. Conditioned 3 min. Skimmed 1 min. 34 #5 Gone. Emulsol X-1--1 drop. Water—300 grams. Conditioned 3 min. Skimmed 1 min. #6 Gone. Emulsol X-1--1 drop Water—200 grams. Conditioned 3 min. Skimmed 1 min. Wt. (gms) Wt. {%) A S S a y (fa) Assay x Weight Secevery BaSO^ CaCO, o SiO 2 BaSO, 4 CaCOg SiOo 2 BaSO, 4 OaCO, 3 sio2 Gone. #1 90.0 18.0 66.5 22.9 10.9 59.8 20.6 9.8 42.5 13.7 4.7 #2 64.2 12.8 58.2 27.1 16.2 37.3 17.4 10.4 26.4 11.5 4.9 #3 24.6 4.9 68.3 23.4 12.4 16.8 5.8 3.1 11.9 3.8 1.5 #4 21.8 4.4 58.2 31.4 9.1 12.7 6.9 2.0 9.0 4.6 1.0 #5 6.9 1.4 54.0 32.9 12.9 3.7 2.3 0.9 2.6 1.5 0.4 #6 3.6 0.7 51.5 31.6 21.3 1.9 1.1 0.8 1.4 0.7 0.4 T a i l s 289.9 57.8 3.02 53.4 62.4 8.8 96.5 181.0 6.2 64.2 87.1 Product Accum. Wt. Accum. Wt. Accumulative Recovery (%) Grade of iAccum. Product {fo) 3 Min. (gms (%) CaCO„ SiOo BaS0 4 CaCO^ S i O p Index Cone. #1 #2 #3 ' #4 #5 #6 T a i l s 90.0 154.2 178.8 200.6 207.5 211.1 501.0 18.0 30.8 35.7 40.1 41.5 42.2 100.0 42.6 68.9 80.8 89.8 92.4 93.8 100.0 13.7 25.2 29.0 33.6 35.1 35.8 100.0 4.7 9.6 11.1 12.1 12.5 12.9 100.0 66.5 63.0 63.6 63.3 62.8 62.7 28.2 22.9 24.6 24.5 25.3 25.6 25.6 30.1 fa 10.9 13.1 13.1 12.7 12.6 12.8 41.6 224.1 234.1 240.7 244.1 244.8 245.1 100.0  loo 20 n o 6 0 R E C O V E R Y (Accur*) . ) i w 90  36 Tests 69 and 70 (ElfStrom & Dayton), u s i n g the reagent we used'(Emulsol X-l) without any HaPOg were found to f i t our 3-mineral index curve almost e x a c t l y (although they were run at temperatures of 40° and 60° r e s p . ) . A l s o , s e v e r a l roughly comparable t e s t s u s i n g l a PO i n the m i l l , or c o n d i t i o n i n g i t s e v e r a l minutes Defore adding Em. X - l gave a b e t t e r index than our max. They p l o t t e d a rough curve i n d i c a t i n g a max. index of about 270. Consideration of these data l e d us to b e l i e v e that quite p o s s i b l y our I s . depressant was prevented from r e a c t i n g f u l l y with the I s . by adding Em. X - l simultaneously or soon a f t e r i t . Test #78 was run to f i n d out i f our surmise was c o r r e c t , and to see i f a b e t t e r index could be obtained by pre-cond- i t i o n i n g the charge with NaPOg. To t h i s e f f e c t the Na^Po^ (Iff /ton) was added to the pebble m i l l . Products were taken o f f with a d d i t i o n s of 1 drop, of Em. X - l per product--6 con- centrates and a t a i l i n g oeing removed. The r e s u l t s of t h i s t e s t showed a max. index of about 2455 with 3 points very close to the apex. This index was f a r below what was expected from the longer c o n d i t i o n i n g of the NaPOg. I t was reasoned that perhaps the KaPO^ coa t i n g on the surface of the I s . (or mono-molec. f i l m — a d s o r p t i o n l a y e r — or whatever..) was formed, but was worn o f f by continued g r i n d i n g . Or perhaps f o r some other reason the HaPO deter- i o r a t e d before the a c t u a l f l o t a t i o n . , To check t h i s l i n e of reasoning reference was made to r 37 te s t e by E l f S t r o m & Dayton: — #60—0.5# ton of HaPO^ was added to the m i l l — t o g e t h e r ' 3 with Ha SiO„. The weight of product taken o f f i n t h i s t e s t 3 <3 gives, from our graph showing the r e l a t i o n between product and index f o r T. 78, almost p r e c i s e l y the index they obtained. #69 and #70—Ho HaP0_ was used i n these t e s t s — y e t the r e s u l t s f i t the curve we obtained by adding NaPOg to the m i l l . The above c o n s t i t u t e s f a i r l y strong evidence that the HaP0 3 added to the m i l l was almost equivalent to adding none at a l l . 38 Test # 79 To Pebble M i l l Ore 500 g. Water 500 g. G r i n d — f u l l charge of pebbles—70 H. P. M.--30 m. To G e l l Water to b r i n g pulp d i l . to 4:1. HaP03—1# / t o n . Co n d i t i o n lOjmin. . Cone. #1. Emulsol X - l — 2 drops, ( l dr. = 0.033 g.) Condition 3 min. Skim 2 min. PH cone. =8.55 F r o t h as u s u a l — f i n e and copious, becoming coarser. Cone. #2. Emulsol X - l — 2 drops. Water 900 grams. Conditioned 3 min. Skimmed 2 min. ; PH cone. =8.50 ! Cone. #3. Water 800 g. Emulsol X - l — 2 min. Conditioned 3 min. i Skimmed 2 min. 39 Gone.#4. Water 300 g. Emulsol X-1--2 drops. Conditioned 3 min. Skimmed 2 min. Cone. #5. and Cone # 6 — a s f o r cone. #4, except that only 200 g. water was added f o r each. T a i l s — p H = 8.05 Product Weight % Wt. A s s a y 1 i) $ Wt. x Assay Recovery fo BaS0 4 CaC0 3 S i 0 2 SaS0 4 CaC0„ sio 2 BaB0 4 CaC0„ o SiO, Cone. #1 174.3 35.3 57.2., 27.7 22.0 20.2 9.7 7.7 68.0 32.1 20.9 #2 72.9 14.8 46.6 33.0 26.6 . 6.9 4.9 3.9 23.2 16.1 10.6 #3 11623 3.3 43.6 34.2 21.0 1.5 1.1 0.7 5.0 3.6 1.9 #4 6.2 1.3 42.0 39.4 24.8 0.5 0.5 0.3 1.7 1.6 0.8 #5 6.0 1.2 23.4 50.2 26.8 0.2 0.5 0.3 G.7 1.6 0.8 #6 3.4 0.7 16.9 55.4 23.9 0.1 0.4 0.2 0.3 1.3 0.5 T a i l s 214.5 43.5 0.7 30.4 j 54.9 0.3 13.2 23.8 1.1 43.7 64.6 493.6 100.0 1 29.7 30.3 36.9 100.0 100.0 100.0 Product Accum. Wt. Accum. $ Wt. Accumulative Recovery Accum. Loss 3-Min. Index (Barite) Accum. Grade of Prod. BaSO^ BaS0 4 CaC0 3 SiO 2 CaC0 3 sio 2 Cone. #1 #2 #3 #4 #5 #6 T a i l s 174.3 247.2 263.£ 269.7 275.7 279.1 493.6 35.3 50.1 53.4 54.7 55.9 56.6 100.0 68.0 91.3 96.4 98.0 98.7 99.0 100.0 32.0 48.2 51.8 53.4 55.1 56.4 100.0 21.0 31.4 33.4 34.2 35.0 35.5 100.0 68.0 51.8 48.2 46.6 44.9 43.6 0.0 79.0 68.6 66.6 65.8 65.0 64.5 0.0 215.0 211.7 211.2 210.4 208.6 207.1 100.0 57.2 54.0 53.6 53.2 52.5 51.8 29.7  ioo 41 This t e s t was run. to see i f c o n d i t i o n i n g i n the c e l l before adding Emulsol might enhance the a c t i o n of the NaPO^. Before adding Em. X - l the HaPO was conditioned f o r 10 minutes. Two drops of Em. X - l were added, and the mixture con- d i t i o n e d f o r a f u r t h e r 3 minutes. #1 cone, was, taken o f f . The f r o t h was very heavy, and f i l l e d two pans with f i n e foam, be- coming coarser toward the end. F i v e more cone, were removed-- adding two drops of Em. X - l f o r each cone. The r e s u l t s of t h i s t e s t were d i s a p p o i n t i n g i n regard to improvement of 3-min. index. The curves obtained i n d i c a t e a a max. of about S20. The BaSO^ recovery was very good, but the curves showing l o s s o f CaC0 3 and SiOg f a l l o f f much too ra< i d l y to allow f o r a h i g h index. The low r e s u l t here suggests that the Em. X - l , kept i n a warm place, has l o s t i t s s e l e c t i v e powers. This idea i s born out by subsequent t e s t s . 42 est 80. To.Pebble M i l l Ore 500 g. Water 500 g. G r i n d — 3 0 m i n . - - f u l l charge — 7 0 H. P. M. To F l o t a t i o n C e l l Water to give 4:1 d i l u t i o n . MaPOg—2#/ton. Conditioned 10 minutes. Gone #1. pH - 8.3 Emulsol X - l — 5 drops. Conditioned 3 min. Skimmed 3 min. T a i l s pH-= 8.3 N o t e — T h i s concentrate f i l l e d .t\NO pans with f r o t h , and these p o r t i o n s were separately assayed. They weighed 208.3 g. and 46.4 g. Product 'Weight A s s a y ' % fo Wt. x Assay Recovery fo CaCO- BaSG. SiO. 3 4 2 Ca00 3 BaS04 S i O g CaC0 3 BaSo 4 SiOg Gone. l a . n l b . T a i l s £08.3 46.4 241.8 42.0 9.3 48.7 26.6 56.4 20.4 37.8 42.0 22.6 36.0 5.3 58.4 11.2 23.6 8.6 4; • 15 3*9 2*1 17.5 2.6 28.5 33.7 78.5 21.9 13.5 12.9 5.4 52.7 8.6 72.7 496.5 100.0 33.2 30.1 39.2 100.0 100.0 100.0 Product Accumulative Accumulative Recovery 3-Ivlin. Index 3aS0 4 Weight BaS0 4 CaC0 3 BaS0 4 Cone, l a Cone, l b T a i l s 208.3 254.7 496.5 78.5 66.3 78.1 91.4 52.7 72.7 100.0 0.0 0.0 222.9 216.8 100.0 44 -a s i n g l e concentrate was taken o f f — u s i n g 2#/ton NaPO^ — conditioned 3 minutes. The concentrate f i l l e d two pans with f r o t h , and the pans were kept separate f o r assay purposes. The assays show that the f i r s t f r o t h to come up i s high- er i n B a r i t e and lower i n Limestone than the l a s t to come up. The s i l i c a was a l s o s l i g h t l y h i g h e r i n the f i r s t p a n - f u l l . The index obtained f i t s the curve from t e s t #79—show- i n g t h at a d d i t i o n a l amounts of NaPO^ do not Increase the s e l e c t - i v i t y of the Em. X - l . This t e s t also i n d i c a t e s a d i f f e r e n c e i n the a c t i o n of the Em. X - l as compared to t e s t #76 and t e s t #77. The point i t gives on the 3-Min. index vs. weight of product graph i s w e l l below the curve f o r t e s t #76. 45 Test #81 i Iron M i l l . To M i l l - Ore 500 g. Water 500 g. HaPO_ 2#/ton. 6 Grind 15 min. @ 44 H. P. M. with 13 rods. P o r c e l a i n Pebble M i l l . Ore 500 g. Water 500 g. NaP0 3 2#/ton. Grind 30 min. © 70 fi. P. M., with f u l l charge. To C e l l (same f o r both) Water to b r i n g p. d. to 4:1 Emulsol X - l — 4 drops. Condition 3 minutes. Skim 2 minutes. pH = 8.5. Iron Mill.—Gone. 226.5 g. T a i l s 267,0 Pore. M i l l . - - C o n e . 222.8 g. \ •?i T a i l s 270.9 g. \ A. Iron M i l l — ~pi Product Wt. $> wt. A s s a y % % Wt. x Assay Recovery % CaC0 3 BaS0 4 S i O g GaCO^ BaS0 4 -SIO CaCO, BaSO, S i O P Gone. T a i l s 226.5 26?.0 46.0 54.0 26.8 55.0 25.4 36.8 7.6 58.5 12.3 25.3 11.7 19.9 4.1 31.6 38.2 86.0 27.0 61.8 14.0 73.0 493.5 100.0 32.2 29.4 43.3 100.0 100.0 100.0 3-Mln. Index f o r B a £ 0 4 : 220.8 B. P o r c e l a i n M i l l Product Wt. fo Wt. A s s a y % fo Wt. x Assay Recovery fo CaCO,. BaSO. SiOp 3 4: <s CaCO, BaSO, S i 0 9 3 4 <i CaC0 3 BaS0 4 SiOg Gone. T a i l s 227.8 270.9 45.6 53 « 4: 27.8 56.6 17.9 37.6 6.8 53.1 12.7 25.8 8.2 20.0 3.6 28.4 38.9 87.8 22.4 61.1 12.2 77.6 498.7 100.0 32.7 29.4 36.6 IOO.O IOO.O lOoToj 3-Min. Index f o r BaS0 4 r 226.5 47 Test #81 was run with the two purposes; (1) to compare g r i n d i n g i n a p o r c e l a i n pebble m i l l to g r i n d i n g i n an i r o n rod m i l l — ( a s regards s e l e c t i v i t y of Em. X -1), and (2) to check again the apparent l o s s i n s e l e c t i v i t y of the Em. X - l . 2#/ton I a P 0 3 was added i n the m i l l , and 4 drops e f Em. X - l i n the c e l l . The r e s u l t s show l i t t l e d i f f e r e n c e i n the r e s u l t s from the d i f f e r e n t g r i n d s — a n d such d i f f e r e n c e s as appear may he a r e s u l t of d i f f e r e n t fineness of gr i n d i n g , not to any i r o n s a l t s formed i n the m i l l . The greatest d i f f e r e n c e was shown by the SiOg recovery — b e i n g 27$ i n the cone, from the rod m i l l grind, and only 22.4$ i n the cone, from the pebble m i l l g r i n d . The d i f f e r e n c e may be due to a c t i v a t i o n of SiQ by i r o n s a l t s . 2 The 3-Min. index obtained was 226.5 f o r the pebble m i l l , against 220.8 f o r the i r o n rod m i l l . Both i n d i c e s are w e l l be- low the curve obtained i n t e s t #78, where l#/ton KaP0 3 was add- ed to the b a l l m i l l charge. 48 Test #82. A. Pebble M i l l Tp_ M i l l — Ore 500 g. Water 500 g. Grind 30 min. & 70 R. P. M. — f u l l charge of peobles. Tc_ C e l l - Water to b r i n g p. d. to 4:1. •'NaPO — l # / t o n . 3 Cond i t i o n 10 min. Cone. #1— Sulfonated Cod O i l - 2 drops. (1 dr. = 0.036 g.) (pH = 8.3) ( = 0.144#/T) Condition 3 min. Skim 3 min. F r o t h as f o r Emulsol X - l , but not quite so p l e n t i f u l , and a l i t t l e tougher. Cone. #2.-- Sulfonated Cod O i l — 2 drops. Condition 3 min. Skim 2 min. Frot h as above. Cone.#3.— Sulfonated Cod O i l — 2 drops. Condition 3 min. Skim 2 min. Cone. #4.--Same as Cone #3. Cone. #5.— Sulfonated Cod O i l -- 5 drops. •• Conditioned 3 min.--Skim 2 min. Proth was becoming poorer—much more b r i t t l e , but s t i l l w e l l m i n e r a l i z e d . 49 T a i l s -- pH = 8.2. N. B. A f t e r each concentrate was removed, water was added to b r i n g the l e v e l of the pulp up to the o r i g i n a l 4:1 mark. B. Bod M i l l . Duplicate t e s t to 8 2T A . Grind 13 rods --44'R. P f o r 15 min. The f r o t h was not so w e l l m i n e r a l i z e d toward the en as i n the pebble m i l l g r i n d . Test #82—A Product Wt. fo Wt. A s s a y % % Wt. x Assay Recovery fo CaCO 3 BaSQ4 SiOg CaC0 3 BaS0 4 ?i0g CaCO BaSO. £10 c 3 4 c Cone. 1 2 3 4 5 T a i l s 63.7 60.8 65.3 47.1 54.8 204.7 12.8 12.2 13.2 9.5 11.1 41.2 36.4 56.4 14.7 37.6 58.2 13.3 42.4 54.1 9.3 49.2 48.2 9.8 62.2 19.2 22.6 10.8 18.9 75.0 4.66 7.22 1.88 4.59 7.10 1.63 5.59 7.16 1.23 4.68 4.59 0.93 6.92 2.13 2.51 4.45 7.80 30.8 15.1' 20.0 4.8 14.9 19.8 4.2 18.1 19.9 3.2 15.1 12.8 2.4 •22.4 5.8 6.4 14.4 21.7 79.0 ...20,89 36.00 39.0 OQO^IL .100.0 100.0 Product Accum. Wt. Cone. 1 2 3 4 . 5 T a i l s 63.7 124.5 189.8 236.9 291.7 496.4 ACcum. /O Wt . 12.8 25.0 38.2 47. 7 58.8 100.0 Accum. K e c o v . CaCO, ?i0. BaSO 4 15.1 30.0 48.1 63.2 85.6 100.0 4.8 9.0 12.2 14.6 21.0 20.0 39.8 59. 7 72.5 78.3 100.0 100.0 Accum. Loss C a C O 3 SiOg 84.9 70.0 51.9 36.8 14.4 0.0 9 5»2 91.0 87.8 85.4 79.0 0.0 3-Min. Index f o r BaSO, 4 200.1 200.8 197.4 194.7 181.7 100.0 Grade of BaS0 4 i n Accum. ProductJ 56.2 57.2 56.3 54.6 48.0 36.0 Product Wt. (/o Wt. Cone. 1 52.4 10.4 2 59.1 11.8 3 51.7 10.3 4 43.1 8.6 5 96.5 19.2 T a i l s 199.8 39.7 502.6 100.0 Test #82—B a 7 I'O CaCo 3 BaS0 4 SiO '/o wt. x Assay CaCor, B a S O . SiO. 28.8 33.8 38.4 45.6 56.8 14.8 67.3 62.8 56.1 48.5 c? 2 * 2.6 6. 7 13.2 12.2 10.5 25.9 85.2 3.00 4.00 3.96 3.93 10.90 5.88 7.00 7.40 5.79 4.17 4.40 1.03 0.70 1.56 1.26 0.90 4.98 33.40 31.67 29.79 43.501L00.P0 100 .^~10070 Recovery y0 CaC0„ BaSO, SIO 9.50 12.60 12.50 12.40 34.40 18.60 23.5 24.8 19.4 14.0 14.8 3.5 1.6 3.6 2.9 2.1 11.5 78.3 1 Test 82-3.--Cont'd Product Accum. Wt. Accum. • % Wt. Accum. Recovery Accum. l o s s 3-Min. Index f o r B a r i t e . Grade of BaS0 4 i n Accum. Prod, CaC0„ o BaS0 4 SiOg CaCO 3 Cone. #1 52.4 10.4 9.5 1.6 23.5 98.4 90.5 212.4 67.3 2 111.5 22.2 22.1 5.2 48.3 94.8 77.9 221.0 64.9 3 163.2 32.5 34,6 8.1 67.7 91.9 65.4 225.0 62.2 4 206.3 41.1 47.0 10.2 81.7 89.8 53.0 224.5 59.2 5 302.8 60.3 81.4 21.7 96.5 78.3 18.6 193.4 47.8 T a i l s 502.6 100.0 100.0 100.0 100.0 0.0 0.0 100.0 29.8  N O . a G R A P H P A P E R . C . P . C . 6CM DROPS O P 5O L C O N A T « D COD On. (fl O B O P = O . 0 3 6 G « M ^ ) NO. *4« GRAPH PAK*. T M B C L A R K E ft S T U A R T C O . . L T D . . V A N C O U V E R , R . C  52 s The purpose of t h i s t e s t was to cheek the work of E l f ^ t r o m & Dayton u s i n g sulfonated cod o i l to f l o a t B a r i t e , with HaP0 3 as a l e . depressant; and to check the comparative r e s u l t s ob- tained by g r i n d i n g i r o n and p o r c e l a i n m i l l s . Duplicate t e s t s were run, u s i n g a p o r c e l a i n m i l l f o r one, and an i r o n rod m i l l f o r the other. The r e s u l t s obtained were not very good from the stand- point of f l o a t i n g B a £ 0 4 away from CaCO^, The best 3-rnineral index obtainable, as i n d i c a t e d by the graphs of 3-Min. Index vs. Accum. Wt. of Product, i s about 227 f o r the rod m i l l g r i n d . The pebble m i l l g r i n d i n d i c a t e d an index of about 200.1 as a maximum. Tests #38 and #39, ( E l f e t r o m & Dayton) give i n d i c e s above the curve we obtained here (using an i r o n m i l l ) . They used Wag SiO_ i n the m i l l , and t h i s may have had some a d d i t i o n a l dep-3 r e s s i n g e f f e c t on SiO , and perhaps on CaCO . c 3 Why such poor r e s u l t s were obtained with the pebble m i l l g r i n d i s not apparent, and a check on t h i s t e s t seems ad v i s a b l e . The "break-points'* i n the S i O g and CaCO^ curves f o r s u l f . c. c., do not occur at the same weight of product as the c o r r - esponding point i n the BaS0 4 curve; consequently the 3-Min. Index curve does not show a sharp maximum point, but r a t h e r a broader region of maximum 3-Min. Index. This i r r e g u l a r i t y as compared to the curves f o r L i s s o l . A w i l l hamper Eomewhat the use of these curves i n p r e d i c t i n g - t h e best obtainable i n d e x — and the r i g h t wt. of product to give t h i s index. The same i r r - e g u l a r i t y a p p e a r s — t h o ' not to so marked a degree, i n the Em* XI curves. 52 Test #83 To M i l l . Ore 500 g. l a t e r 500 g. Grind 30 min U 70 B. P. M f u l l charge of pebbles. To C e l l . Water to b r i n g p. d. to 4:1. Cond i t i o n 10 min. Cone. #1. Added Emulsol X - l — 1 drop. Condition 3 min. Skim 2 min. F r o t h as i n Test # 79. Cone. #2. Added Emulsol X - l — 1 drop. Condition 3 min. Skim 2 min. Same f o r Cone. #^ #4, #5, and #6. Water was added each time, to b r i n g l e v e l of pulp up to the o r i g i n a l 4:1 mark. Weights of Products: Cone. #1 = 70.9 g. Cone. #2 = 65.5 g. Cone. #3 = 51.6 g. T a i l s Cone. #4 - 19-3 g. Cone. #5 = 8.9 g. Cone. #6 - 11.4 g. 268.7 Product Wt. fo Wt. Assay % x Wt. A S S a y f Recc-yery % CaC0 3 ' BaSO SiO 2 CaCO, a BaS0 4 2 CaCO^ o 3aS0 4 s i o 2 Gone. #1 70.9 14.3 4.27 8.84 1.73 29.8 61.7 12.1 13.0 30.0 3.6 2 65.5 13.2 3.28 8.38 2.54 24.8 63.4 19.2 10.0 28.4 5.3 3 51.6 10.4 2.79 5.84 2.86 26.8 56.1 27.5 8.5 19.8 6.0 4 19.3 3.9 1.13 2.03 1.07 29.0 52.6 27.5 3.5 7.1 2.2 5 8.9 1.8 0.49 1.03 0.38 27.2 57.2 20.9 1.5 3.5 0.8 6 11.4 2.3 0.66 1.24 0.69 28.8 53.9 29.9 . 2.0 4.2 1.5 T a i l s 268.7 54.1 20.15 2.06 38.40 37.2 3.8 70.9 61.5 7.0 80.6 496.3 100.0 32.77 29.42 47.67 100.0 100.0 100.0 Product Accum. Wt. Aeeum. fo Wt. Recovery iccum. Loss 3-Min. Index Crade of Accum, Product. (BaS0 4) CaC0 3 SiOg BaSO 4 CaCO^ SiOg (Barite) Cone. #1 70.9 14.3 13.0 3.6 30 .0 87.0 96.4 213.4 61.7 2 136.4 27.5 23.0 8.9 58.4 77.0 91 .1 226.5 62.5 3 188.0 37.9 31.5 14.9 78 .2 68.5 85.1 231.8 60.8 4 207.3 41.8 35.0 17.1 85.3 65.0 82.9 233.2 59.9 5 216.2 43.6 36.5 17.9 88.8 63.5 82.1 234.4 59.6 6 227.6 45.9 38.5 19.4 93.0 61.5 80.6 235.1 59.2 T a i l s 496.3 100.0 100.0 100.0 100.0 0.0 0.0 100.0 29.3 54 The purpose of t h i s t e s t was to repeat t e s t 79, u s i n g 1 newly -purchased Emulsol X - l , to see i f the new Em. had b e t t e r s e l e c t - ive p r o p e r t i e s than the o l d . In comparing the product-reagent curves of t h i s t e s t with those from Test #79, the following i s shown: — 1. ' The s i l i c a l o s s l i n e s f o r both t e s t s are very n e a r l y s t r a i g h t l i n e s , tho' both show a s l i g h t break downwards. The curve f o r t e s t 83, i n d i c a t i n g a greater s e l e c t i v i t y of the o l d Em. X - l f o r s i l i c a . 2. The L s . l o s s l i n e s are both much steeper than the s i l i c a curves, with the curve f o r t e s t 79 again f a l l i n g o f f more r a p i d l y toward the r i g h t . There was a sharper break i n the curve than f o r SiO , o c c u r r i n g with about 45 gm. l e s s product than the corresponding point f o r BaSO^. The curves show that CaCOg i s s t i l l by f a r the more d i f f i c u l t to keep down, and use of a b e t t e r depressor i s necessary i f BaS0 4 i s to be s u c c e s s f u l l y f l o a t e d away from CaCO^. 3. The BaS0 4 recovery l i n e s i n both t e s t s r i s e very r a p i d l y to t h e i r maximum, which i s n e a r l y 100% recovery, with the curve f o r t e s t 83 r i s i n g a l i t t l e more steeply, and reach- i n g a max. at about 250 gm. of product, as against 280 gm. f o r t e s t 79. 33 TT TT. "TT*| — - 1 - 1 • — - T* Q - 1 C O 1 a y \ a - M I N E R A L . I N O E X F - O R 8 CQ 1 x UJ Q Z -I < UJ z f «5 2 > UJ > 0 u Ul DC 100 BaSQ^ R E C O V E R Y IOO 200 300 40O ACCUMULATIVE W T : O P P R O D U C T I M G R A M 5 5 0 0 n i n 1 1 1 n 1 N o . 24* G R A P H P A P E R . T H I « ft DO Test #84 To M i l l Ore 500 g. Water 500 g. Grind 30 min. @ 70 r . P. M. — f u l l charge. To C e l l — Water to b r i n g p. d. to 4:1. Sodium Hexametaphosphate —2#/ton. Condition 10 min. pH = 9.4 Cone. #1 Emulsol X - l — 1 drop. Condition 3 min. Skim 2 min. Proth--not as much as with UaPO^ d e p r e s s o r — a n d very p o o r l y m i n e r a l i z e d . QoflQ» #2 Emulsol X - l — 1 drop. Condition 3 min. Skim 2 min. Proth--as above. Cone. #5 Emulsol X - l — 2 drops. Condition 3 min. Skim 2 min. Pr o t h somewhat tougher—and f i n e r at f i r s t . Concj. #4 56 Cone. #4 Emulsol X - l — 3 drops. Condition 3 min. Skim 2 min. F r o t h more copious, tougher. Cone. #5 Emulsol X - l — 3 drops. C o n d i t i o n 3 min. Skim 2 min. F r o t h f i n e r . Cone. #6 Emulsol X - l — 3 d r o p s . Condition 3 min. Skim 2 min. Larger v o l . — f i n e r f r o t h . Weights of Products. Cone. #1 — 4.1 g. Cone. #4 — 22.9 2 -- 4.4 g. 5 — 25.6 3 —11.2 g. 6 — 25.8 T a i l s -- 401.5 An assay was run on Cone. 1+-2-J-3. There was not enough t o t a l product to be worthwhile working out r e c o v e r i e s . Product Wt. A s s a y  ujo BaSO. CaCO, SiO Cone. 1 2 3 19.7 27.1 53.8 15.8 57 Purpose — To i n v e s t i g a t e NagPgO as a depressor f o r limestone. Sodium hexametaphosphate was used by ElfStrom & Dayton i n an attempt to f l o a t s i l i c a from b a r i t e and l . s . u s i n g L i s s o l . A. The q u a n t i t y ueed (2#/ton) showed a general depressing a c t - ion, and the r e c o v e r i e s were a l l very s m a l l . In t h i s t e s t -- (#84) — the same quantity of Na^P^O-^ — 2#/ton — was added and conditioned i n the c e l l f o r 1C min. A drop of Emulsol X - l was added, and while a f a i r amount of f r o t h formed, i t was poorly m i n e r a l i z e d . Six concentrates were taken o f f , with increased amounts of Em. X - l , but a l l f r o t h s were very poorly m i n e r a l i z e d , and the t o t a l product removed was only 94.0 gm. T h i s was obviously too l i t t l e to give a good BaSQ 4 recovery, so complete assays were not run. An assay on G1-V-Gg+G3 showed BaS0 4 27.1$, GaC0 3 53.8$, and Si© g 15.8$. The CaCO^ seemed to be depressed l e s s than the BaSO^ or SisQ g. 68 Test #86 To M i l l Ore -- 500 g. Water 500 g. Grind — 30 min. © 70 E. P. M. — f u l l charge. To C e l l — Water to b r i n g p. d. to 4:1. Sodium hexaroetaphosphate — 0.5#/ton» Conditioned 10 min. pH = 9.0 Gone. #1 — Emulsol X - l — 1 drop. Conditioned 3 min. F r o t h was p o o r — l i t t l e of i t , and p o o r l y mineralized, so no skimming was attempted. Added Emulsol X - l — 3 drops. Conditioned 3 min. Skim 2 min. F r o t h — one panful — w e l l m i n e r a l i z e d . Cone. #2. -- Emulsol X - l -- 4 drops. Conditioned 3 min. Skim 2 min. F r o t h as f o r #1. Cone. #3. Emulsol X - l — 4 drops." Conditioned 3 min. Skim 2 min. Froth f i n e r . Cone. #4. Emulsol X - l -- 4 drops. Conditioned 3 min. Skim 2 min. Froth, hot so s e l l m i n e r a l i z e d — not so p l e n t i f u l , tougher. Cone. #5. Emulsol X - l — 4 drops. Conditioned 3 min. Skim. 2 min. F r o t h as above. Weights of Products: Cone. #1 — 59.9 Cone. #4 — 38.1 2 — 80.0 5 — 31.9 3 — 65.2 T a i l s —221.1 Product I t . % Wt. A S S a y i io wt. x Assay Be covery fo GaC0 3 SiOg BaSO, 4 CaCO" 3 sios JBaS04 Ca0O3 SiOg BaSO. 4 Gone. #1 59.9 H a 18.8 7.1 75.1 2.3 0.9 9.1 7.3 2.2 30.7 I 80.0 16.1 20.6 15.0 71.9 3.3 2.4 11.6 10.6 5.9 39.2 65.2 13.2 32.6 23.6 46.6 4.3 3.1 6.2 13.8 7.6 21.0 4 38.1 7.7 46.8 34.1 20.1 5.6 2.6 1.5 11.5 6.4 5.1 i 31.9 6.4 46.2 46.4 6.9 2.9 3.0 0.4 9.3 7.3 1.3 T a i l s 22111 44.5 33.4 65.0 1.9 14.8 28.9 0.8 47.5 70.6 2.7 496.2 31.2 40.9 29.6 100.0 100.0 100.0 Accum. Accum. Product Wt. 7% Wt. Cone. #1 59.9 12.1 2 139.9 28.2 S 205.1 41.4 4 243.2 49.1 5 275.1 55.5 T a i l s 296.2 100.0 Accum. Recov. jo CaC0„ SiO BaSO [Accum. l o s s 7.3 17.9 31.7 52.5 100.0 2.2 8.1 15.7 22.1 29.4 4 30.7 69.9 90.9 96.0 97.3 100.0 100.0 CaCO 92.7 82.1 68.3 56.8 47.5 0.0 SiO 2 97.8 91.9 84.2 77.9 70.6 0.0 p-LIin. In. For BaSO 243,9 243.5 230.7 215.4 100.0 Accum. Grade of Product. &5.1 73.5 65.1 57.8 52.0 29.6 Purpose — To repeat #84, with l e s s Na-P-O-, In t h i s t e s t only 0.5 #/ton NagPgO-^ w a E u 8 e d * T l i e f r o t h with a d d i t i o n of 1 drop Em. X - l was small i n amount and poorly m i n e r a l i z e d , so 3 more drops were added, and the f r o t h obtained was b e t t e r m i n e r a l i z e d and greater i n amount. Five concentr- ates were removed, with 4 drops Em. X - l per cencentrate. A t o t a l of 275.1 gm. of cone, was taken o f f . The curves obtained did not show the tendency to s t r a i g h t l i n e s , as e x h i b i t e d by previous t e s t s , but were quite regular, and showed a p o s s i b l e maximum 3-Mineral index f o r BaSO^ of 246. Due to the f a c t that the weight of Product vs. Recovery graphs f o r Ba8© 4, GaCOg, and S i O g were not s t r a i g h t l i n e s with break-points, the 3-Min. Index curve showed a f a i r l y wide range of nearimaximum, i n s t e a d of a sharp point, as i n some prev- ious t e s t s . The l o s s curve f o r S i O g , when produced to cut the r e - covery l i n e , passes n e a r l y through the 500 gram mark, whereas the CaOOg curve passes cuts t h i s axis at 315 gm. — i n d i c a t - i n g a r a p i d increase i n CaCO^ recovery with the amount of 3 product removed. I t would be i n t e r e s t i n g , from the t h e o r e t i c a l stand- p o i n t , to keep removing products u n t i l n e a r l y a l l the charge has been f l o a t e d . I f the curves continue as i n d i c a t e d , the I.e. would be e n t i r e l y removed i f 315 gm. of Gone, were removed, and pure SiOg would be l e f t . I t i s quite p o s s i b l e t h a t 0 s m a l l e r quantity of sodium hexametaphosphate, and a smaller amount of Em. X - l might give a b e t t e r separation than the above, and an i n v e s t i g a t i o n would 62 be a d v i s a b l e . By running s e v e r a l t e s t s , removing and assaying only one concentrate f o r each, and n o t i n g whether the 3-min. index f e l l above or below the curve f o r Test 85, a b e t t e r com- b i n a t i o n of reagents might be e a s i l y obtained, and the amount of product to give the beet recovery (3-Min. Index) could then be determined from a graph s i m i l a r to the above.   63  65 ASSAY PROCEDURES The simple composition of the syn t h e t i c ore used allowed the use of s p e c i a l adaptations of commercial assay procedures. Such procedures were developed by Elf e t r o m and Dayton, and were used with minor a l t e r a t i o n s i n t h i s research. Determination of Calcium Weigh out 0.5 grams of ore i n t o a 400 c.c. beaker. Add 10 c.c. HOi, cover with a watch gla s s u n t i l a l l a c t i o n ceases, add 5 c.c. EiNO and b o i l u n t i l brown fumes are a l l o f f . Place beaker on a low p l a t e , r i n s e o f f cover g l a s s , and take assay to dryness. Bake on a high p l a t e f o r hour, c o o l , add 10 c.c. flCl and 40 c.c. water, b o i l t i l l c l e a r , f i l t e r through a 12.5 cm. r a p i d f i l t e r , and wash with b o i l i n g water, with hot 1:1 HC1, and then with water four times. Make the f i l t r a t e ammonaical; then 5 c.c. i n excess. B o i l , f i l t e r , and wash with b o i l i n g water. To the f i l t r a t e add EC1 u n t i l a c i d , then one c.c. excess. Add 3 grams ammonium oxalate, b r i n g to b o i l , and add ammonia drop by drop t i l l a l k a l i n e . Allow the p r e c i p i t a t e to s e t t l e out f o r -§- hour, decant the s o l u t i o n through the f i l t e r , wash the p r e c i p i t a t e into the f i l t e r , and wash well ( 5 times at l e a s t ) with b o i l i n g water. Rinse out the beaker, washing i t at l e a s t eight times, to remove a l l the ammonium oxalate. Wash the p r e c i p i t a t e into the o r i g i n a l beaker, f o l d the paper over the edge of the beaker, add 100 c.c. hot water 66 and 5 o.c. 1:1 H gEG^, and heat n e a r l y to b o i l i n g . T i t r a t e to a pink c o l o u r with KMnO^, add the f i l t e r paper, and f i n i E h t i t r a t i o n . Determination of B a r i t e and t^uarta Fuse 1 gram of ore with 3 grams of sodium carbonate i n a platinum c r u c i b l e at 950° C. u n t i l the melt i s c l e a r . Pour the fused m a t e r i a l i n t o the c r u c i b l e cover, immerce both- cruc- i b l e and cover, with contents, i n a 250 c.c. beaker of hot water. Digest f o r 10 minutes (or l o n g e r — o v e r n i g h t i f convenient) remove the cover and c r u c i b l e , and scrub and r i n s e w e l l . When s o l u t i o n i s complete, ( i . e . a l l lumps have d i s i n t e - grated) f i l t e r through a 12.5 cm. #1,.Whatman f i l t e r , and wash w e l l with hot water. Reserve the f i l t r a t e f o r determination of s i l i c a . 'Wash the residue back i n t o the o r i g i n a l beaker and d i s s - olve with 1:1 H.C1, adding 10c.c. fre e HG1 i n excess. B o i l f o r 10 minutes. Add 4 c.c. HgSO^ i n 20 c.c. water to the hot barium c h l o r i d e s o l u t i o n . Cover the beaker, place on a medium plate and allow to s e t t l e f o r -§• hour. Decant the s o l u t i o n into a f i l t e r , wash the p r e c i p i t a t e into the beaker, and wash at l e a s t eight times with b o i l i n g water. Ig n i t e and weigh as barium s u l f a t e . 67 Determination of S i l i c a A c i d i f y the f i l t r a t e reserved f o r s i l i c a determination, adding 20 c.c. HOI i n excess. Evaporate to dryness, and bake f o r jj hour on a high p l a t e . Add 15 c.c. 1:1 H'Cl, 150 c.c. water, and heat to b o i l i n g . F i l t e r , and wash the residue. To the f i l t r a t e , add 10 c.c. HG1 and again evaporate to dryness. Take up with 15 c.c. 1:1 EGl, and 150 c.c. water, heat to b o i l i n g , and f i l t e r through the same f i l t e r paper. Wash s i x times with b o i l i n g water. I g n i t e , and weigh as SiOg. Note. Some s i l i c a may be contained i n the barium carbonate residue, hence i n the high s i l i c a s , the f i l t r a t e from the barium s u l f a t e f i l t r a t i o n i s beet f u r t h e r a c i d i f i e d , taken to dryness, d i s s o l v e d i n 14 c.c. 1:1 E G l and 150 c.c. water, f i l t e r e d , i g n i t e d , and the r e s u l t a n t s i l i c a obtained added to the r e g u l a r s i l i c a assay. 9 August

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