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By John V. Beall

STREAM pollution caused by waste waters from mineral industry operations is a problem that has grown up with the industry. Its importance to each operator is dependent on the amount and type of waste he dumps into the rivers and streams; on whether this waste pollutes the waters sufficiently to make them unfit for potable water, irrigation, and conservation of wild life; and on whether this waste makes a safety or health hazard. Through the years our growing population and industry have made increasing demands on the mineral industries, the suppliers of the raw materials on which our industries are based; and we have met these demands at some sacrifice to the natural beauty and cleanliness of our country. However, that is often the unavoidable nature of the business, and along with the increased use of our

Jan 1, 1948

By Stirling Huntley, L. G. Huntley

THE controversy regarding the ,'probable future of the Mexican oil fields, and its relation to the oil industry of the United States, has led to the preparation of this paper. As has been predicted by several writers in recent papers, certain of the producing areas in the so-called "southern fields" in the Tampico Embayment have only a limited oil reserve. These areas are being pulled on by every pipe line in that region, and the length of time that they will continue to produce is a direct factor of the daily oil shipments of these companies. However, this is not the whole story, and in the following paragraphs an attempt will be made to show that the life of Mexican oil production will be a long one, and Mexican oil will continue to be a large factor n the market for an indefinite time after the areas mentioned above have been drained. The past and present producing fields will be discussed separately, in order-to establish a basis for comparison, the ,only method by which underground reserves 'can be estimated in these fields.

Jan 1, 1921

By J. F Haseman, J. E. Davenport

In the brown rock phosphate fields of Tennessee there are large deposits of phosphate matrix in which quartz is a major constituent of the gangue, and which cannot be beneficiated by the conventional washing process to yield a concentrate of suitable grade for use in the electric furnace. A huge tonnage of high-grade phosphate concentrate is produced in the Florida pebble district from low-grade siliceous feed. However, the characteristics of the low-grade siliceous Tennessee ore are such that flotation under the conditions employed in treating the Florida ore1,2 results in inadequate beneficiation. Investigation of Flotation Methods Flotation has been used in 'Tennessee primarily to produce a concentrate of premium grade by moderate enrichment of a marketable grade of phosphate. 3,4 A secondary use was to increase the recovery of phosphate from the fines (down to approximately 200 mesh) from medium-grade ores with a concomitant moderate increase in over all grade.3,5 It was considered desirable to investigate methods of improving the grade of washed products from low-grade siliceous Tennessee ore when these products were substantially below the requirements for use in the electric furnace. The present paper describes the results of a laboratory-scale study of factors that affect the beneficiation of such siliceous phosphate ore by flotation. The primary objective of the investigation was to ascertain the conditions under which the ore could be made to yield a concentrate suitable for reduction in the electric furnace. It was assumed that a phosphate concentrate for electrothermal reduction should contain at least 26 pct P2O5 and should have a weight ratio of silica to lime of not more than 0.80. Since a concentrate of moderate grade can be used in the electric furnace, and since, as Grissom4 has shown in detail, the ore will not bear the cost of expensive treatment, the study of collectors was limited to the relatively inexpensive fatty acids. A secondary objective was to determine whether a portion of the phosphate could be recovered in a grade suitable for treatment with phosphoric acid to produce 45 pct superphosphate. The ore consisted of variably cemented sand interlayered with clay. The sand layers were composed of grains of quartz, phosphate, and clay embedded in a matrix of clay and phosphate. Some clay was finely disseminated in the phosphate grains. Little massive high-grade phosphate was present. The material used in the flotation tests was a washed sand that had been separated from the ore in a bowl classifier at the TVA phosphate-washing plant. The percentage composition of the sand was as follows: P2O5, 20; SiO2, 40; CaO, 29; Fe2O3, 2; Al2O3, 3; F, 2.3. The particle-

Jan 1, 1948

By J. F. Haseman, J. E. Davenport

In the brown rock phosphate fields of Tennessee there are large deposits of phosphate matrix in which quartz is a major constituent of the gangue, and which cannot be beneficiated by the conventional washing process to yield a concentrate of suitable grade for use in the electric furnace. A huge tonnage of high-grade phosphate concentrate is produced in the Florida pebble district from low-grade siliceous feed. However, the characteristics of the low-grade siliceous Tennessee ore are such that flotation under the conditions employed in treating the Florida ore1,2 results in inadequate beneficiation. Investigation of Flotation Methods Flotation has been used in 'Tennessee primarily to produce a concentrate of premium grade by moderate enrichment of a marketable grade of phosphate. 3,4 A secondary use was to increase the recovery of phosphate from the fines (down to approximately 200 mesh) from medium-grade ores with a concomitant moderate increase in over all grade.3,5 It was considered desirable to investigate methods of improving the grade of washed products from low-grade siliceous Tennessee ore when these products were substantially below the requirements for use in the electric furnace. The present paper describes the results of a laboratory-scale study of factors that affect the beneficiation of such siliceous phosphate ore by flotation. The primary objective of the investigation was to ascertain the conditions under which the ore could be made to yield a concentrate suitable for reduction in the electric furnace. It was assumed that a phosphate concentrate for electrothermal reduction should contain at least 26 pct P2O5 and should have a weight ratio of silica to lime of not more than 0.80. Since a concentrate of moderate grade can be used in the electric furnace, and since, as Grissom4 has shown in detail, the ore will not bear the cost of expensive treatment, the study of collectors was limited to the relatively inexpensive fatty acids. A secondary objective was to determine whether a portion of the phosphate could be recovered in a grade suitable for treatment with phosphoric acid to produce 45 pct superphosphate. The ore consisted of variably cemented sand interlayered with clay. The sand layers were composed of grains of quartz, phosphate, and clay embedded in a matrix of clay and phosphate. Some clay was finely disseminated in the phosphate grains. Little massive high-grade phosphate was present. The material used in the flotation tests was a washed sand that had been separated from the ore in a bowl classifier at the TVA phosphate-washing plant. The percentage composition of the sand was as follows: P2O5, 20; SiO2, 40; CaO, 29; Fe2O3, 2; Al2O3, 3; F, 2.3. The particle-

Jan 1, 1948

Climax Molybdenum Co. has contracted with the Government to operate its property at Climax, Colo. at maximum capacity for five years. Substitution of synthetic lubricants, polyalkylene glycols and their derivatives, for petroleum products in certain industrial applications is yielding substantial savings in production costs and improved operation of mechanical equipment.

Jan 1, 1951

By John K. Hammes

INTRODUCTION From the point of view of the consumer, the cost of mineral commodities might be viewed as the total price industry pays for mine output. Similarly, the mining company engaged in the ongoing business of finding, developing and operating new mines is concerned very much today with the distribution of all the revenue paid for mine output and not just with its direct or controllable cash costs. In other words, what will the labor force, the supplier of energy, explosives, and reagents, and the supplier of government services, management, capital, and the ore reserves receive for their contribution to production? A significant amount might be categorized as what economic theory classifies as economic rent. Mining companies are finding it increasingly difficult to negotiate concession or work contracts to develop ore reserves in lesser developed countries, just as they find themselves accused of taking excess profits in their own countries. The principal difficulty in reaching mutually satisfactory agreements in many cases is the difficulty in establishing an acceptable distribution of income, in particular the distribution of economic rent. (See Chapter 7). Further, it is logical that the decisions and policies of the interested parties be they government or industry should be and will be influenced by their competitive position relative to determining the distribution of economic rent. The raising of finance for a mining project today may be inhibited by too biased an extraction of economic rent by entities other than the risk takers, the mining companies. ECONOMIC RENT A British economist (Ricardo D. McGraw-Hill, 1955) first proposed the concept of economic rent (See Drechsler, H.D. earlier in this Chapter.) Ricardo pointed out that no rent would be paid until land became scarce. Ricardo also stressed the distinction that the price of farm produce was not higher because of the rent paid on farm land but that the rent or price of more fertile farm land was higher because the price of produce is higher. This led to the concept that economic rent is not a cost and that it is therefore not price determining, but is itself price determined. Economic rent may be viewed as a cost if cost is equated with the concept of payment or distribution of income to any factor used in production. However, if it is a criterion that a payment must be made to the supplier of the factor of production, then economic rent is not truly a cost because it is not necessarily distributed or "paid" to the supplier. Consider the commodity A which occurs in three grades: Al, A2, and A3. Any grade may be used as a substitute for another grade in all of the industrial uses of A. However, in industries X and Y the different grades have different productivities. Table 1 shows the relative productivities of each grade in industries X and Y, and in all other industries [~]. [ ]

Jan 1, 1985

By R. E. Cuthbertson

AN early appreciation by the management that Climax ore presented a challenging problem of economic concentration was responsible for the establishment, in June 1926, of an ore-testing department at the experimental plant of the Colorado School of Mines at Golden, some ninety miles from Climax. An engineering office was later organized in the same community for the design of all ore-treatment units erected at Climax during the period of rapid growth. Work of the ore-testing and design staffs was effectively co-ordinated under a common head. The primary reason for having the ore-testing and plant design departments in Golden, was to place these activities under the able supervision of A. J. Weinig, consultant for the Climax Molybdenum Co., and director of the experimental plant. A secondary consideration was the availability of excellent facilities for research in ore dressing in a highly favorable environment. Concentration of molybdenite by flotation from an ore of simple mineral composition does not appear, superficially, to present a serious problem in ore dressing but experience belies this apparent simplicity. The molybdenite content of average Climax ore is low and it is finely

Jan 1, 1946

By J. T. Mackenzie

Henry Marion Howe, in whose memory we are gathered together, was one of the great thinkers who develop from time to time to whom is given the rare gift of synthesis. Analysis is given to few, but synthesis, the ability to show the relation of all parts to each other and thus to give a clear picture of the whole, is reserved for the very few. Analysis can be achieved by honesty, intelligence, and industry, but synthesis is only given to genius. Professor Howe's crowning achievement is the picture of the whole iron-carbon series shown in Fig. I, which places steel, malleable, gray iron, mottled and chilled irons in their proper relation to each other and shows the essential unity of the series. Perhaps his best statement of the case is found on page go of the Metallography of Steel and Cast Iron in these words: " Each member of the gray cast-iron series consists of the metallic matrix approximately equivalent to that member of the steel-white-cast-iron series to which it corresponds in percentage of combined carbon with its continuity broken up—by masses of graphite ..." Apparently he had taken considerable interest in this idea around the turn of the century, for he refers to a discussion at the Franklin Institute in I900 in which he said: "Though many others had probably conceived this relation between the steels and cast irons, it was here enunciated for the first time, so far as I know. It was received with great incredulity." The concept was explained in some detail in a paper on "The Constitution of Cast Iron" presented before the A.S.T.M. in 1902 when Professor Howe was retiring president of that young society. In the discussion Dr. Sauveur stated that he was "very well acquainted with Professor Howe's theory of the constitution of cast iron," and went on to say that while he "shared it to the fullest extent, some foundrymen . . . claim cast iron is a metal entirely different from steel . . . that steel and cast iron have very little in common, and that therefore the knowledge gained in the study of steel is of little or no value in the study of cast iron." Dr. Moldenke, in discussing the same paper, said he had been working on the same theory for 12 years but he laid no claim to publication. Discussing the difference in the micro-structure of the metallic matrix, Professor Howe pointed out that "such minor structural differences are indeed to be expected, because of the difference in the conditions under which these constituents are generated. "One difference in these conditions is that the steel of most micrographs has been either forged or at least treated thermally in such a way as to give a new structure radically different from that which formed during the initial solidification, whereas the cast irons have not. Hence what we see in the steels is a transformation structure, but in the cast irons a solidification structure. By giving the cast

Jan 1, 1944

By J. T. Mackenzie

Henry Marion Howe, in whose memory we are gathered together, was one of the great thinkers who develop from time to time to whom is given the rare gift of synthesis. Analysis is given to few, but synthesis, the ability to show the relation of all parts to each other and thus to give a clear picture of the whole, is reserved for the very few. Analysis can be achieved by honesty, intelligence, and industry, but synthesis is only given to genius. Professor Howe's crowning achievement is the picture of the whole iron-carbon series shown in Fig. I, which places steel, malleable, gray iron, mottled and chilled irons in their proper relation to each other and shows the essential unity of the series. Perhaps his best statement of the case is found on page go of the Metallography of Steel and Cast Iron in these words: " Each member of the gray cast-iron series consists of the metallic matrix approximately equivalent to that member of the steel-white-cast-iron series to which it corresponds in percentage of combined carbon with its continuity broken up—by masses of graphite ..." Apparently he had taken considerable interest in this idea around the turn of the century, for he refers to a discussion at the Franklin Institute in I900 in which he said: "Though many others had probably conceived this relation between the steels and cast irons, it was here enunciated for the first time, so far as I know. It was received with great incredulity." The concept was explained in some detail in a paper on "The Constitution of Cast Iron" presented before the A.S.T.M. in 1902 when Professor Howe was retiring president of that young society. In the discussion Dr. Sauveur stated that he was "very well acquainted with Professor Howe's theory of the constitution of cast iron," and went on to say that while he "shared it to the fullest extent, some foundrymen . . . claim cast iron is a metal entirely different from steel . . . that steel and cast iron have very little in common, and that therefore the knowledge gained in the study of steel is of little or no value in the study of cast iron." Dr. Moldenke, in discussing the same paper, said he had been working on the same theory for 12 years but he laid no claim to publication. Discussing the difference in the micro-structure of the metallic matrix, Professor Howe pointed out that "such minor structural differences are indeed to be expected, because of the difference in the conditions under which these constituents are generated. "One difference in these conditions is that the steel of most micrographs has been either forged or at least treated thermally in such a way as to give a new structure radically different from that which formed during the initial solidification, whereas the cast irons have not. Hence what we see in the steels is a transformation structure, but in the cast irons a solidification structure. By giving the cast

Jan 1, 1944

By JOHN R. SUMAN

I WOULD like to spend a few minutes describing to you the present condition which exists in the oil industry and then point out some aspects of this deplorable situation in which I think petroleum engineers can be helpful. As you know, the oil business at this time is in a very critical condition, .due to the tremendous potential production in excess of current demand. This is a world-wide condition as well as a national problem, as it is estimated that the surplus production available for the market in foreign countries is of about the same proportion as that existing in the United States. Due to the inability within the United States to hold production within the bounds of demand prices have been slumping for the last four years and at this time have reached the point where the sales value of the average barrel of crude oil in the United States, is far below the cost, of production. In addition to the large amount of potential production available for the market in excess of demand we have in storage in the United States about six hundred fifty millions of barrels 'of oil. Unless something can be done to limit the amount of oil coming onto the market to a point well below the demand, which point will permit the reduction of stocks, it looks as though the 'oil business is facing demoralization.

Jan 1, 1931

By G. R. Green, R. C. McDonald

The International Nickel Co., Ontario Div. mines, faced with rising production requirements, short labor supply, and ever increasing labor costs turned to mechanized mining for a solution to its problems. The degree of mechanization of ore removal has increased from 1966 with the purchase of the first diesel-powered load-haul-dump (LHD) machine to the present, with over 53% of all underground production handled by these units. Keeping pace with mechanized ore removal, there has been a parallel development of drilling equipment to complement the mucking units. This paper deals with the applications and economic advantages of mechanized drilling at the underground mines of Inco, Ontario Div. It covers the use of various types of mechanized drills in such mining methods as cut-and-fill, induced block caving, and sublevel caving. The economics of raise boring are also discussed.

Jan 1, 1974

By Mark R. Lamb

The treatment of slime is of special interest to those engaged in cyaniding gold- and silver-ores. The usual practice is to make as small a percentage of slime as possible. In many instances the slime is given no treatment, but is impounded in dams in the hope that the future will develop some method of economically treating this product. The filter-press was the first step upward from ordinary decantation, but, on account of heavy labor-charge and high cost, its use has been limited to high-grade material. The slime at the Combination mill at Goldfield averages perhaps $20 per ton, and although the values are quickly dis solved the filter-press installation was not entirely satisfactory, resulting in the erection of the canvas-cell filter, developed by Chas. Butters and his staff. This filter is a great improvement over the filter-press, and the following description of it will be of interest to those engaged in treating slime produced in crushing ores, especially in view of the fact that, by the use of this filter, slime can be treated at a lesser cost and with a higher percentage of gold- or silver-extraction than in the ordinary treatment of sand; and, moreover, the initial outlay for an all-sliming plant is less than that for the ordinary sand- and slime-plant. The economy of construction of the Butters filter-plant is clearly shown in Figs. 1 and 2, which illustrate the 20-frame filter of 40 tons capacity, now being installed by the Nevada Goldfield Reduction Co. In this construction the slime-pump is so connected that it call pump to or from either tank or the filter by changing the valve-settinga—a combination which is necessary in this particular installation, since sufficient fall is not available for filling and discharging the filter by gravity. Ordinarily, a slime-plant comprises: a filter-box with frames

Jan 1, 1908

By J. E. Metcalfe

Proceedings of the Fourth Empire Mining and Metallurgical Congress, Great Britain 1949. Part II published at the Offices of the Congress in London, England, 1139 pp. The price of these proceedings is £ 2. The parts may be purchased separately at a cost of £ 1 each.-Part I of this book covers a report of the organizing committee, the inaugural meeting and presidential address, banquet at Guildhall, welcome by Sir Richard Livingstone at Oxford. and final session. Technical session and papers are also covered in Part I. Part II covers such topics as coal, present-day trends in mineral dressing and metallurgy. Mining Engineer's Survey Manual. By J. E. Metcalfe. Published for "Mine & Quarry Engineering" by Electrical Press, London, 1951. 341 pp., illus., charts, diagrs., tables, 8 ¾ x 5 1/ in., cloth, 30s., available from Percival Marshall & Co., Ltd., London, and British Book Centre, 122 East 55th St., New York 22, N. Y. Beginning with a brief treatment of surveying fundamentals and a discussion of the correlation of surface and underground surveys, this practical manual continues with descriptions of surveying practice both above and below ground including stopes, inclined shafts; etc. Space is devoted to sampling and valuation, geological considerations, and descriptions of modern surveying instruments. The organization of survey operations is covered in the last chapter.

Jan 1, 1952

By E. C. Lee

THE safety of mine workers has received more attention from both State and Federal law-making bodies than any other industry, a fact that shows clearly the hazardous nature of the industry. The last, but by no means the least, of the measures adopted for the protection of mine workers, is workmen's compensation legislation. This is proving to be a powerful instrument for greater safety in the industries, from the fact that special stress is laid not on how the accident happened or who may have been responsible for it, but on how badly the employee is hurt by it. The injured person does not have to employ lawyers to prove his case, because the mere fact of his employment is proof of his right to compensation. The immediate effect of such legislation is the certainty confronting the mine operator that he must pay out large sums for every accident, regardless of its cause, thus adding materially to the cost of the production of his coal. This fact furnished to the operator the strongest incentive to reduce the causes of accidents; not that the operator has ever lacked reasonable consideration for the welfare of his employees and a proper humane interest in their safety, but his engrossment in earning his daily livelihood has been so great that he has not felt that he had the time to devote to the safety of the operation. This time he must now find because of the actual-cash value of the prevention of accidents in his mines. This agency alone proved inadequate to bring about a material improvement because operators have always been willing enough to improve safety conditions when possible to do so within reasonable limits of their financial ability. The requirement in the Workmen's Compensation Laws of several of the States, that the mine operator shall insure as a guarantee of his ability to meet his compensation obligations, has furnished the needed incentive, moral and financial, necessary to the prompt and effective dissemination of a more general knowledge of the causes and

Jan 10, 1917

By John McDonald

THIS report is a continuation of an earlier one with a similar title,1 to which the reader is referred for such details of procedure as do not appear here. A brief summary will be given of the objects and methods of the research at this time. It was pointed out in the previous paper that properties of magnesium alloys, as re-ported by different workers, often differ. This was thought to be due to differences in the preparation of the specimens tested. The ideal way to compare alloys would be to prepare each of them in so many ways that reasonable assurance would exist that the best properties of each alloy had been developed. The alloys would then be com-pared on the basis of these properties. The treatment actually given the alloys of these studies is necessarily a compromise with completeness. Nevertheless, enough treatments have been given so that a con-siderable degree of assurance exists that the properties obtained are representative of the alloy as such, and not merely of the manner in which it was worked and heat-treated.

Jan 1, 1940

By F. Lynwood Garrison

Except in the old Catalan forge, or its modifications, attempts to make iron and steel directly from ore in a practical and economical manner have failed so frequently and completely that such schemes are looked upon with justifiable distrust. Without exception, all have failed from one cause or another, although in some instances every indication of a practical success was manifest in the beginning. It is, therefore, necessary to carefully examine and consider every detail affecting the process, or more properly, furnace, under consideration. This I have done to the best of my ability during a long visit to Russia last summer, and after satisfactorily observing the practical success of the furnace in the iron works of Count Stroganoff at Dobriansky in the Government of Perm, I decided to investigate as completely as possible the history of similar furnaces in Finland and Russia. These data, sifted and verified with the greatest possible care, form the substance of the present paper.* An illustration on page 321 of Percy's Iron and Steel shows the old type of Osmundssmide or harkugnar, which has been in use in Northern Europe since pagan times. Fig. 1 shows a furnace of this kind. It should, perhaps, more properly be called a high-bloomary furnace or forge, the Swedish word hark meaning bloom or loupe. It was with this type of furnace that Mr. Husgafvel began his experiments at Porsaskoski in 1875. Attempts to obtain better results with larger furnaces of this type were failures, as every bloom or loupe obtained necessitated blowing out the furnace with a consequent large waste of fuel. A larger furnace of course increased this waste with no corresponding advantage. A movable hearth of threeeighth inch iron, lined with a mixture of clay, quartz and lime, was next tried, but in consequence of the frequent repairs of this lining,

Jan 1, 1888

Discussion Of the paper Of GEORGE K. BURGESS, J. J. CROWE, H. S. RAWDON, and R. G. WALTENBERG, presented at the Pittsburgh meeting, October, 1914, and printed in Bulletin NO. 93, September, 1914, pp. 2433 to 2437. ALBERT SAUVEUR, Cambridge, Mass.-The Bureau of Standards has once more rendered a public service. Manufacturers and consumers of steel rails alike should welcome the important results now laid before them by Dr. Burgess and his co-workers. Personally I welcome these results all the more that in the past, as some of the members may remember, I have never failed, when occasion arose, to call the attention of rail manufacturers to the importance of controlling the finishing temperature of their rails. The pioneer metallographic work conducted at the South Works of the Illinois Steel Co. in the early '90s clearly brought out the close relations existing between the manufacture, properties, and finishing temperature of steel rails and I think I may say without fear of being contradicted that the results of this early investigation had considerable influence in drawing the attention of manufacturers to the importance of finishing temperature and of heat treatment in general. The results now before us should be, it seems to me, of great value to rail manufacturers in their efforts to produce a better and, above all, a safer rail. It seems to be demonstrated in this paper that there is no difficulty in installing in rail mills pyrometric outfits, making it possible to record, without interfering in the mill operations, the temperature of the rails as they leave the finishing rolls, or of the ingots as they are withdrawn from the soaking pits, or at any intermediate point in the process of manufacture. The inference necessarily follows that manufacturers should see to it that such pyrometric installations are made, in order that they may actually know, instead of guessing at, the temperature of their rails;, and, for obvious reasons, rail consumers should insist upon such installations. In the rolling of heavy sections especially should care be taken to lower their finishing temperature, seeing that the present tendency is to finish them at higher temperature, whereas, owing to the slower cooling of their central portions, which makes for coarseness of grain, they should, if anything, be finished at a lower temperature than lighter rails.

Jan 4, 1915

Readers of recent Bulletins have doubtless observed that the problem of improving both material and moral condition of employees is receiving close attention from influential members of the Institute. This will lend interest to certain developments and investigations that have been reported elsewhere.

Jan 5, 1918

By K. A. SPENCER

THE production of soft coal from strip mines in the United States has shown a remarkable growth in the last sixteen years, increasing from one and one-quarter million tons in 1914 to approximately twenty-two million tons in 1929. This is a growth of approximately 1660 p& cent, as compared with a growth of approximately 20 per cent in the underground mines for the same period. But even with this marked in- crease the total tonnage produced by open-face mining represents only 4 per cent of the nation's soft coal tonnage.

Jan 1, 1931

By Milton E. Wadsworth, R. Ted Wimber

Cobalt sulfate solutions containing ammonium acetate and chloroplatinic acid were reduced by hydrogen in a pyrex-glass lined autoclave in the temperature range of 170o to 232°C and hydrogen partial pressure range of 115 to 830 psia. The reduction rate was directly proportional to the hydrogen partial pressure and surface area of the pyrex glass and was independent of the quantity of chloroplatinic acid added initially. Experiments involving the variation of the relative concentration of ammonium acetate indicated that the reducible cobalt complex was probably the diacetate complex of cobalt, Co(AC)4H20, or a new mononcetate complex Co Ac, which was in solubility equilibrium with a pink precipitate of CO(AC)-4HzO. THE reaction in which a metal is dissolved by an acid to produce gaseous hydrogen and a salt solution was discovered early in the history of chemistry. In 1859 Beketoff found experimentally that this reaction could be reversed; i.e., a salt solution could be reduced by gaseous hydrogen to produce a metal and an acid. A review of work done on this phenomenon since that time may be found elsewhere., The hydrogen reduction of a cobalt salt solution is facilitated by complexing the cobalt ion. An ammonia complex of cobalt has been reduced commercially in the recovery of cobalt metal. A new reducible complex of cobalt was discovered5 when it was found that a co-baltous sulfate solution containing ammonium acetate could be reduced by hydrogen at temperatures in the region of 200°C. When a cobalt sulfate-ammonium acetate solution was heated to a temperature below its normal boiling point, a violet color became apparent, indicating complex formation. The nature of this complex was investigated5 by the addition of NH4Ac to a CoSO4 solution maintained at 85o. During the first additions of NH, Ac, the pH of the solution remained fairly constant at about 5.85. However, as the ratio of NH,Ac to CoSO, approached two, the pH rose and then leveled off at about 6.05. The absorption spectra of a Co(Ac), solution and a CoSO,, NH Ac solution were obtained at 85°C and were compared and found to be the same. These findings suggested that the diacetate complex of cobalt, Co(Ac),.4H20, was formed at 85°C. When a cobalt sulfate-ammonium acetate solution was heated to a temperature above about 165o, a finely divided pink precipitate appeared. The X-ray diffraction pattern of this precipitate indicated that it was Co(Ac), - 4H,O. In addition, it was discovered that when chloroplatinic acid, H,PtCl;, was added initially to the cobalt sulfate-ammonium acetate solution, a faster reduction was obtained. The roles of the solution complex, pink precipitate and chloroplatinic acid in the reduction process were then investigated. APPARATUS The experimental work was carried out in a two-liter stainless-steel autoclave. Adetailed description of the autoclave and the auxiliary equipment used in maintaining constant temperature and pressure may be found elsewhere.= Because the stainless steel was corroded, and also because it acted as a hydrogena-tion catalyst, an all-glass liner was fabricated such that the solution came only into contact with flame-polished pyrex glass. EXPERIMENTAL PROCEDURE The solutions used in the experimental work were prepared by dissolving reagent grade chemicals in distilled water. Although variation of the brand of ammonium acetate appeared to have no effect on the experimental results, CoSO, 7H O from the J. T. Baker Chemical Co. of Phillipsburg, N. J.,was found to give faster reductions than that prepared by Allied Chemical and Dye Corp., N. Y. The former was used throughout the course of the experimental work and was weighed up at the outset of each experiment. The ammonium acetate was dissolved to form a 6M stock solution, which was stored under refrigeration. A 10 pct solution of chloroplatinic acid (J. T. Baker Chemical Co.) was diluted to a 1.15 x 1Q2 M stock solution, which was standardized by precipitation of K,PtCl, as outlined by Scott. The appropriate volume of the chloroplatinic acid, H,PtCl,, solution was pipetted into the clean, dry glass liner. The cobalt sulfate-ammonium acetate solution, which had previously been saturated with

Jan 1, 1962