Search Documents

By F. B. Plummer

PERHAPS the greatest progress made in the technical methods of oil production during the last year has been in handling gas from the new fields that yield light distillate fractions. At least sixteen recycling plants have been perfected and installed in South Texas fields alone during 1939 having a daily capacity of more than one billion -2 cubic feet of gas and capable of producing more than a million gallons of distillate daily. The process consists of running the gas under pres- sure through especially designed plants, separating out the condensate, then compressing the gas to 3000 lb. or more, depending on the subsurface pressure in the formation, and injecting gas back into the reservoir to be produced again later, along with more of the liquid hydrocarbons, and again recycled. Hence production in these distillate fields in sense has changed from that of producing a constantly diminishing and much-wasted product to a more or less continuous manufacturing process, in which practically all the gas is conserved-a real triumph in engineering practice.

Jan 1, 1940

By O. J. C. Runnals

The intermetallic compounds NpAl2, NpAl3, and NpAl have been prepared, and examined by X-ray diffraction methods. The compounds are isostructural with the corresponding U-Al compounds. NpAl3 is face-centered cubic with a = 7.785A and has the MgCu2 structure. NpAl is simple cubic with a = 4.2624 and has the AuCU3 structure. NpAl4 is body-centered orthorhombic with a = 4.428, b = 6.268, and c = 13.71A. The published description for the atomic positions in UAl, applies also to NpAl4 THE U-Al system has been examined by Gordon and Kaufmann.1 They identified the following intermetallic compounds: UAI2, UAl3, and a third, tentatively identified as UAl5. A structure analysis of the latter compound by Borie2 proved that the formula UAl4 was more consistent with the X-ray data. The crystal structures of UAl2 and UA have been reported by Rundle and Wilson.3 UAl2 was found to be isostructural with MgCu. The atomic positions in the simple cubic UA1, cell were found similar to those in the AuCu3 structure. Three analogous compounds exist in the binary system Np-Al. X-ray data for the compounds NpAl2, NpAl3, and NpAl4 are reported below. The neptunium used in the investigation was supplied through the courtesy of the Argonne National Laboratory as neptunium (V) nitrate. It was stated to have a radioactive content of 99.25 pct Np237. The impurity limits had been established by a spectrographic analysis given in Table I. Any titanium, boron, or bismuth impurity should be effectively removed during the fluorination of NpO2 to NpF4, and sodium, lithium, magnesium or strontium during the alloying procedure. The oxalate ignition technique, described by Westrum for the preparation of finely-divided reactive PuO2, was used.The neptunium (V) nitrate solution, containing 100 mg Np, was evaporated to dryness on oxalic acid crystals. The resulting oxalate was calcined to NpO, by heating in platinum at 650°C for 2 hr. An equimolar mixture of anhydrous hydrogen fluoride and purified hydrogen was passed over the NpO2 for 2 hr at 500°C. According to Fried and Davidson" the above fluorination conditions should produce the purple-black fluoride, NpF3 However, the light-green product showed only NpF4 lines on an X-ray diffraction pattern and contained only an estimated 5 pct of finely dispersed black NpF3 particles on microscopic examination. NpAl3: An intimate mixture of 50 mg of neptunium fluoride and aluminum powder (99.99 pct pure, —28 to $60 mesh) was heated to 900°C in a BeO crucible in vacuum by a tungsten coil for 2 hr, to allow the following reaction to proceed: NPF4 + 7Al + NpAl, + 4AlF. [1] The formation and sublimation of aluminum mono-fluoride in this system was verified from an X-ray diffraction analysis of the sublimate. The diffraction pattern was similar to one obtained in the aluminum reduction of UF4 to UF3,6 showing both Al and AlF3 lines. The resulting alloy was sintered at 1100°C for 1 hr. A powdered specimen of the crystalline product was sealed in a thin-walled quartz capillary for X-ray examination. The photograph was taken on a 14.32 cm General Electric powder diffraction camera, using filtered copper radiation. The films were calibrated in terms of a NaCl standard pattern. The wavelengths used in the calculations were 1.5418A for Cu K and 1.5405A for Cu K The powder diffraction pattern showed that NpAl is simple cubic with a = 4.262 % 0.005A, and is isostructural with UA13 where a = 4.27A1 or a =

Jan 1, 1954

By PAUL H. SHAEFF

THIS paper is presented with the idea of discussing only the basic open-hearth charge. The importance of the charging operation in producing steel is more clearly understood by dividing the principal components into four groups and discussing each separately, thereby becoming acquainted with what constitutes a charge. The significance of these components in the charge itself will then be taken up. Classification of the charge components is as follows: steel scrap; pig iron ; limestone ; refractories and coke. Steel Scarp The first component, steel scrap, according to size, analysis and cleanliness, may be classified as heavy, medium and light. Heavy melting scrap includes crop ends such as are produced in blooming ingots or the heavy crops from bar mills abovely in. in diameter; railroad scrap, which comprises rails, side-plates, car-frames, draw- bars, etc.; and such automobile forgings as axles, crank- shafts, gears, etc. This class of scrap should give a four-box charging-car (box dimension 24 by 18 by 72 in.) an average load of 10,000 to 20,000 lb.

Jan 1, 1926

By James W. Wade

THIS discussion of the future supply of lead refers only to the next ten-year period. Beyond that no prediction can be made that would be of sufficient accuracy to serve any purpose. When any commodity is by an unsatisfied demand forced to a higher price level, and the profits of those who are able to produce the commodity are greatly increased, there is awakened a new interest in the commodity on the part of both producer and consumer. The consumer attempts to reduce his costs by developing substitutes or assisting in the development of new sources of supply. Lead is now going through this stage. The lead producer is increasing development expenditure and searching for new mines. The consumer is developing substitutes as illustrated by the increasing use of zinc oxide as a pigment, and the use of dry batteries in radio sets. The search of the Ford interests for lead, by prospecting in Missouri and Idaho, is induced by the effort to develop a new source of supply. Considering the index figures of the Department of' Commerce, it is evident that lead is on a substantially higher price level. For February, 1926, the index figure of lead is 209, while the general commodity price index is only 156, 100 being taken as the base for 1913.

Jan 1, 1926

By Herbert Hoover

THERE is one problem of the new administration that has received the attention and thought of the organized engineers of America for many years past. This is the problem of the reorganization of the Federal Government. The, inadequacy, the wastefulness, and the inefficiency of our federal organization was evident, enough under pre-war conditions. These inadequacies, these inefficiencies, these wastes were exhibited to the country during the war at the cost of millions. Congress has placed the problem in the hands of a very able Congressional Joint Committee, but if this Joint Committee succeeds in securing the imminently necessary results it will only be by full insistent support to it by public opinion. Many attempts have been made at reorganization before but all, of them have gone to the same crematory-the interminable differences in opinion among the executive and legislative officials over details.

Jan 1, 1921

By AIME AIME

MOTHER example of the broad field that is covered by the mining industry is the recent erection by the Phelps Dodge Corp. of a modern hospital building at Douglas, Ariz., and an identical one at the rejuvenated mining town of Morenci. Managers of even small mining properties are often called upon to build schools, houses, stores, maybe a jail, and provide sanitary arrangements, possibly the while acting as mayor of the town. Those who direct larger properties may have to build hospitals, as in the present instance, construct sewage disposal plants, and sometimes even build and manage railroads. A mining camp achieves its reputation among mining men not entirely by the grade or amount of its ore, or the skill of the operating staff in mining and milling it at a profit-the operation soon acquires a reputation as either a desirable or an undesirable place to live, regardless of its remoteness from what is euphemistically termed civilization. Such a community is indeed fortunate if it can boast of a good hospital.

Jan 1, 1940

By E. I. Larsen, E. F. Swazy, F. R. Hensel

Experience has indicated that hard bronzes are not suitable for bearing applications where high bearing loads and speeds are involved. It is the general practice to utilize softer materials for these purposes, such as copper, lead, silver, babbitt, lead-base alloys, and more recently aluminum-base alloys, preferably supported by a steel backing. It was the objective of the present investigation to study a new material produced by powder metallurgical methods susceptible to precipitation-hardening. Test MAteriaIs Preliminary tests were made with compacts containing copper, nickel and silicon in quantities sufficient to form 3 to 5 per cent nickel silicide. It mas found that this type of alloy was susceptible to the formation of a soft surface shell when sintered in tank hydrogen. The depth of the shell depended On the length of sintering time and sintering temperature, and varied in thickness from a few thousandths to as much as One eighth inch. This soft shell resulted from the preferential oxidation of silicon, thereby reducing the efficiency of age-hardening by the nickel silicide compound. The body of the sintered compacts below the soft shell could be precipitation-hardened to a hardness of 70 to 85 Rockwell B, by quenching from goo°C. and age-hardening at 450°C. A series of tests was made with various addition agents, in order to decrease the rate of preferential oxidation, and it was found that phosphorus was most beneficial in this respect. After considerable experimentation, the following nominal com-position was accepted as standard: 2.4 per cent nickel; 0.8 silicon; 0.3 phosphorus; balance copper. The physical propertties and certain bearing properties of this alloy are described in the present paper Preparation of Compacts Several methods of incorporating the hardening ingredient (nickel silicide) were studied. Compacts formed from copper, nickel and silicon powders were found to be inferior to those fabricated from prealloyed nickel silicide master alloys, because of the rapid oxidation of pure silicon during sintering. The use of a prealloyed nickel silicide hardener containing 25 per cent silicon and 75 per cent nickel could be further improved by preparing a master alloy, incorporating nickel, silicon, phosphorus and copper, having the following nominal composition~ 25 per cent nickel; 7 silicon; 3 phosphorus 64 copper. This alloy is brittle in the cast condition and can be readily powdered. Sintering Procedure The blended powders were pressed at '5 to 40 tons per sq' in., the pressure depending on the size and shape of the compacts. Sintering was carried out in hydrogen or cracked ammonia atmospheres at

Jan 1, 1946

By E. I. Larsen, E. F. Swazy, F. R. Hensel

Experience has indicated that hard bronzes are not suitable for bearing applications where high bearing loads and speeds are involved. It is the general practice to utilize softer materials for these purposes, such as copper, lead, silver, babbitt, lead-base alloys, and more recently aluminum-base alloys, preferably supported by a steel backing. It was the objective of the present investigation to study a new material produced by powder metallurgical methods susceptible to precipitation-hardening. Test MAteriaIs Preliminary tests were made with compacts containing copper, nickel and silicon in quantities sufficient to form 3 to 5 per cent nickel silicide. It mas found that this type of alloy was susceptible to the formation of a soft surface shell when sintered in tank hydrogen. The depth of the shell depended On the length of sintering time and sintering temperature, and varied in thickness from a few thousandths to as much as One eighth inch. This soft shell resulted from the preferential oxidation of silicon, thereby reducing the efficiency of age-hardening by the nickel silicide compound. The body of the sintered compacts below the soft shell could be precipitation-hardened to a hardness of 70 to 85 Rockwell B, by quenching from goo°C. and age-hardening at 450°C. A series of tests was made with various addition agents, in order to decrease the rate of preferential oxidation, and it was found that phosphorus was most beneficial in this respect. After considerable experimentation, the following nominal com-position was accepted as standard: 2.4 per cent nickel; 0.8 silicon; 0.3 phosphorus; balance copper. The physical propertties and certain bearing properties of this alloy are described in the present paper Preparation of Compacts Several methods of incorporating the hardening ingredient (nickel silicide) were studied. Compacts formed from copper, nickel and silicon powders were found to be inferior to those fabricated from prealloyed nickel silicide master alloys, because of the rapid oxidation of pure silicon during sintering. The use of a prealloyed nickel silicide hardener containing 25 per cent silicon and 75 per cent nickel could be further improved by preparing a master alloy, incorporating nickel, silicon, phosphorus and copper, having the following nominal composition~ 25 per cent nickel; 7 silicon; 3 phosphorus 64 copper. This alloy is brittle in the cast condition and can be readily powdered. Sintering Procedure The blended powders were pressed at '5 to 40 tons per sq' in., the pressure depending on the size and shape of the compacts. Sintering was carried out in hydrogen or cracked ammonia atmospheres at

Jan 1, 1946

By Lucien Eaton

INCREASED mining activity during the past year has brought to light changes in mining practice and advances in technique, born and incubated in the period of depression from which the mining industry is now emerging. Although the tendency toward large output from individual mines has continued, a salutary trend is evident toward greater efficiency at small mines, in which the gold mines of Canada have led the way. Improvement in excavating machinery and washing plants for small placers has continued, and knowledge of the possibilities and limitations of this kind of equipment has increased. Greater portability through sectionalization has been the keynote. Power, shovels and draglines mounted on caterpillar treads move from one deposit to another under their own power, and floating washing plants mounted on pontoons can be taken down, moved, and set up again by a small crew of men in only a few days.

Jan 1, 1937

By C. H. Mathewson

THIS paper was prepared upon request as a contribution to a symposium covering the manufacture, properties, and uses of the important non-ferrous metals. In approaching a subject as broad as this, there is a natural desire to build up a comprehensive and finished production which shall constitute a dependable source of information on all questions properly belonging to this branch of metal technology. There are, however, a number of circumstances, apart from the mere routine of labor and thought involved, which operate rather effectively against the possibility of completing such an ambitious program at the present time. First of all, as far as any public record of results is concerned, the commercial rolling, drawing, and forming of zinc with relation to changes of structure and properties-and this we consider to constitute the elements of metal technology-might as well be an unpractised art. We have never seen a published photomicrograph showing the structural characteristics of either hard or soft sheet or strip, although the structure of castings has been frequently described, and other coarse-grained structures resulting from hard-hammering and annealing have been reproduced. Thus, an author in this field must proceed to his task without much assistance from the literature, and the outcome can represent only a personal estimate of principles, facts, or findings, and not a summary

Jan 9, 1919

By E. J. KENNEDY

FEBRUARY 15-18 will be the outstanding dates of the month for members of the A. I. M. E., for then the 141st Meeting of the Institute is to be held in the Engineering Societies Building, at New York. What with 41 technical sessions, the Annual Business Meeting at 4 o'clock Tuesday afternoon,, two sessions of the Section and Division delegates, minor committee meetings, and the many luncheons and dinners, the Dinner-Smoker, Informal Dance, President's Reception and the Dinner-Dance, the opportunity will be limited to do- more-than cast sheep's eyes at New York's other multitudinous attrac¬tions until the meeting is over. The technical program is diverse but well organized. The sessions are almost equally divided among the four days, with ten on Monday, Tuesday, and Wednesday, and 11 on Thursday. The meeting opens Monday morning with registration. Be sure to attend to this detail. Failure to do so may have its repercussions at the meeting and throughout the year.

Jan 1, 1932

By AIME AIME

ON Thursday a most interesting symposium on "Gases in Metals" was held, with both morning and afternoon sessions. The morning was devoted principally to the considerations of the steel maker, the nonferrous field being taken up in the afternoon period. Dr. John Johnston, as chairman, introduced the subject with "A Short Analysis of the Gas-metal Problem and Its Practical Importance." He then introduced P. H. Brace who explained in considerable detail the various vacuum fusion and other methods in use at present, both here and abroad, in the study of "gases" in metals. He was fol¬lowed immediately by H. W. Graham on "The Effect of Oxygen in Steel." The papers elicited considerable discussion, the point being particularly noted by both Dr. Rawdon and Dr. Sauveur that a knowledge of "total oxygen" alone is not sufficient information for the metallurgist, distribution of oxygen being probably the more important. Dr. Johnston, in commenting on the lack of agreement among many of the methods now in use, such as the Ledebur and vacuum fusion, spoke of the contemplated plan of the Iron and Steel Division to have a number of standard samples analyzed by many laboratories by the various methods, the Bureau of Standards acting as a clearing house, so that more definite information may be obtained on the comparative accuracy of the method.

Jan 1, 1933

By Herbert Hoover

THE Federation of Engineering Societies has been created for the sole purpose of public service. This initial meeting surely warrants some discussion of a few of the problems to which this organization, for expression of the --. engineering mind, can quite well give consideration. Some of the greatest of the problems before the country and, in fact, before the world, are those growing out of our industrial development. The enormous industrial expansion of the last fifty' years has lifted the standard of living and comfort beyond any dream of our forefathers. Our economic system under which it has been accomplished has given stimulation to invention, to enterprise, to individual improvement of the highest order, yet it presents a series of human and social difficulties for the solution of which we are groping. The congestion of population is producing subnormal conditions of life. The vast repetitive operations are dulling the human mind. The intermittency bf employment due to the bad coordination of industry, the great waves of unemployment in the ebb and flow of economic tides, produce infinite wastes and great suffering. Our business enterprises have become so large and complex that the old personal relationship between employer and worker has to a great extent disappeared. The aggregation of great wealth, with its power of economic domination, presents social, economic ills which we are constantly struggling to remedy.

Jan 1, 1920

By C. R. Kuzell

GEOGRAPHICAILY the industry of reducing and refining of copper continued to migrate from the .United States during 1931. While this country is losing the predominant position of its copper industry, our engineers still enjoy their pre-eminent position as leaders in the design and operation of the new plants being brought into production in the four quarters of the globe. Progress in the art, as indicated by the construction of the recently completed works, has not been revolutionary. Standard methods have been followed, augmented by novel features in flow-sheets demanded by the results of progress in the art of ore-dressing, and by reason of problems incidental to the peculiarities of the new ores being treated. Design and construction progress has likewise been orderly and without radical departure from less recent practice; new features in primary and secondary equipment being logical developments to provide for special conditions to keep abreast of improve¬ments in accessory apparatus. The new plants are being rapidly brought in without hazardous novelties and for the purpose of yielding the principal ingredient, copper, in as large a volume as it will he possible to market; the old United States procedure. In the meantime the domestic plants are shut down or operating at a very low capacity, threatened with untimely demise unless the metallurgist can extract and develop other valuable products from the ores. International agreements .and tariff protection may be a temporary reviving stimulant, but for many mines the days of profit will be numbered unless the ores can be made to yield as values the ingredients now being discarded. Invisible progress in this direction has been made during the past year, and it is to he hoped that time will prove that the outstanding progress of 1931 was in the development of processes for the ultimate recovery of by-products from copper ores, perhaps even relegating the value of the copper yield to secondary importance.

Jan 1, 1932

By AIME AIME

NEW YORKERS look forward to the third week of February as the time of the year when they can count on seeing their friends-from far and near gathered in the city for the four-day annual session of the Institute.., Indeed, the metropolitan district is so large that in engineer who lives in New, Jersey and has his office on the lower end of Manhattan island may easily pass a whole year without seeing an acquaintance who lives in Westchester and has an office near Forty-second Street. If the Institute served no other function than to provide a place where friendship may be renewed, ideas exchanged, and new acquaintances made it would still be worth while. But when about 30 technical sessions at which about 160 papers are read and discussed are compressed into four days the annual meeting is also entitled to high rank as an intensive course of post-graduate instruction in the newest development in mining and metallurgical technology. Last, but not least, it is the occasion of a good time for one and all, even if they do get more than a little behind on sleep before the end of the fourth day. Nine o'clock is the time set on Monday morning for the beginning of registration, but a half-hour before that a number have always 'put in an appearance, and this is fortunate, because by 10 o'clock four sessions had begun, those on mining methods, geophysics, a round table on the valuation of coal, and the session of the Local Section delegates. Three committees of the A. S. T. M. were also in simultaneous session, so the meeting may be fairly said to have started "in high."

Jan 1, 1931

By N. G. W., Cook

When an excavation is made underground the original rock stresses are removed from the surfaces of the excavation. These surfaces converge to partially close the excavation and the superincumbent rock mass moves down towards the excavation. If the convergence of the surfaces of the excavation were controlled, energy generated by their motion against the controlling forces could be extracted. Since the total forces in the rock mass are not significantly affected by the excavation, stress concentrations arise around the excavation, which compensate exactly for those stresses no longer transmitted through the excavation. These phenomena give rise to two general principles which provide the basis for analyzing the effects of making any underground excavation. The first of these is that the total force resulting from the stresses across any plane in the rock, including any plane through the excavation, must be the same before and after the excavation is made. The second of these is that energy must necessarily be released as a result of making an underground excavation.

Jan 1, 1969

By Edward Steidle

NOTHING stands still. We go forward or backward. As a distinct group of educators, our immediate concern is with the preparation of young men and women for participation in the mineral industries on a professional basis. I am going to have the temerity to state emphatically that for a long time as a whole we have remained in a static position. We are now confronted with the choice of advancement or retrogression. We are still in a position to make a choice and our ultimate fate will depend upon the course of action we elect to follow. Wars always have been great catalysts and social and scientific advancements mature under military stimulus in a fraction of the time normally consumed. We are now in the midst of a conflict whose duration or final effects cannot be estimated. However, the record already demonstrates that this war as never before is a mineral war in which incentive, strategy, and outcome are directly related to the distribution and utilization of minerals. The inevitable result is a drain upon our resources now reflected in our record production and a growing public consciousness of the importance of minerals in the role of human affairs. It is evident that we must seek new mineral frontiers beyond the borders of the United States and take every other precaution to forestall a "have-not" position in the world.

Jan 1, 1943

By A. Singh, W. M. Fleming, J. J. Santana, A. E. Torma

The present study investigated the extraction of uranium from a low-grade ore by sulfuric acid and the removal of radium from the leach residues by brine solutions. The optimum leaching conditions were found to be 1.5 mole [£]-1 H2SO4, 6.Og[9]-1NaClO3, 75°C,50% pulp density and 750 rpm with respect to the rate of uranium extraction. The maximum theoretical attainable rate of uranium extraction was determined to be V = 1.09 x 10 -2 mole [¢]-1h-1 with respect to pulp density. The order of reaction was found to be zero regarding the effect of sodium chlorate concentrations. The apparent activation energy of uranium extraction was calculated from the Arrhenius plot to be [A]E a - 2.36 kcal mole-1 (9.87 kJ mole-1). Based on a statistical design, an empirical equation has been developed describing the rate of uranium extraction with the leaching parameters. This equation can be used to generate data which may be useful for scaling up the process to pilot plant level. The most efficient brine solution for the extraction of radium - 226 from the leach residue was found to contain one mole[f] -1 CaCl2 and 0.01 mole [2] -1 HC1. The two step leaching with this solution resulted 87% removal of radium from the leach residue. On the basis of this study, a flow-sheet has been proposed for the extraction of uranium and radionuclides from the ore and leach residue to yield almost innocuous tailings.

Jan 1, 1982

By H. M. Fisher, R. E. Snow, S. C. Sun

RAPID colorimetric estimation of the amount of transparent minerals has been applied successfully to instream mill products at the cryolite flotation plant of the Pennsylvania Salt Mfg. Co., Na-trona, Pa. Apparatus used was a Bausch & Lomb monochromatic colorimeter. The optical assembly of the colorimeter, shown in Fig. 1, passes light from a 6-v, 32-cp, prefocus incandescent lamp through two condensing lenses, a heat-absorbing filter, an aperture-control diaphragm, an interference filter, and a sample container. The light finally strikes a barrier-layer photocell and the output current of the photocell is measured by a galvanometer. The engraved index line of the collective lens, located between the lamp and the galvanometer, is imaged upon the transmission scale of the colorimeter by the galvanometer mirror. Reflected light from the galvanometer mirror, the position of which is determined by the output current of the photocell, enables reading of percent transmission throughout the mineral sample being tested. The colorimeter, Fig. 1, was standardized as follows: 1—The colorimeter was' connected to a Sola constant voltage transformer, A, of 6-v output operated from a 110-v ac supply. 2—Turning the toggle switch, C, illuminated the transmission scale, B, and the control knob, D, was adjusted with a blank in the optical system until the hairline on the scale read zero. 3—A No. 430 interference filter, E, was inserted into the filter channel, F. 4—A test tube, G, containing 7 cc of distilled water was pressed into the sample space, H, and the fine adjustment knob,

Jan 1, 1955

By P. W. Bennett, E. M. Elkin

A new technique for the recovery of palladium and platinum and sludge from go12 electrolyte eliminates many of the drawbacks of the zinc-dust cementation process. In the electrolytic refining of gold by the Wohwill method, the electrolyte contains about 100 gpl gold as AuCl, and 100 gpl free hydrochloric acid. Any palladium and platinum contained in impure gold dissolve and accumulate in the electrolyte. When their concentration approaches that of gold, it becomes desirable to discard the electrolyte and to recover the gold and the palladium and platinum. As practiced at Canadian Copper Refiners until recently, discarded electrolyte was treated with sulfur dioxide to precipitate the gold. 2AuCl3 + 6H2O + 3SO2 —2Au + 6HC1 + 3H2SO4 The gold precipitate was filtered off, washed with water, and melted with scrap anodes. The wash water was added to the gold-free filtrate and treated with zinc dust to cement the palladium and platinum. PdCl2 + Zn — Pd + ZnCl2 PtCl4 + 2Zn—Pt + 2ZnCl2 The precipitate was separated and sold as Pd-Pt concentrate, and the barren filtrate and wash water were discarded. The receipts of palladium and platinum at this company were too small to warrant their refining. The process suffered from a number of disadvantages. Handling the gold-free solution was disagreeable, as it was laden with sulfur dioxide even after blowing with air overnight. Subsequent treatment with zinc dust was also troublesome. A large excess of zinc dust was required. Spray, acid mist, and vigorous evolution of hydrogen accompanied the reaction. The Pd-Pt precipitate was grossly contaminated with occluded unreacted zinc and with yellow granules of sulfur, thought to be formed by the reduction of sulfur dioxide and its derivatives. Repeated boiling of the precipitate with hydrochloric acid and washing with water decreased somewhat, but did not eliminate, the zinc. After drying overnight, the precipitate hardened to a clinkerlike mass that was difficult to grind. Grinding, handling, and packing created heavy dusting. Even weighing in an analytical balance generated dust, indicating that the powder was easily charged with static electricity. The total palladium and platinum content of the powder varied from 56 to 72 pct, with an average of 65 pct. The powder dissolved in aqua regia with difficulty, leaving a small amount of insoluble residue. However, the main drawback of the process was the strongly hygroscopic Pd-Pt product. The powder showed a marked though erratic increase in weight and a corresponding decrease in assay on exposure to air, even during the course of laboratory analysis. Such changes were the source of disagreement between Canadian Copper Refiners and the buyers of concentrate. The cause of the change in weight is believed to be hydrogen, liberated by the action of zinc dust on hydrochloric acid. Some of this hydrogen was adsorbed so strongly by the precipitate that it could not be driven off during the drying. On exposure to air it oxidized catalytically, forming water. Experiments soon showed that the entire process of treatment of discarded electrolyte then in use would have to be changed. A small quantity of apparatus was moved into the gold room, and experimentation was held to a minimum compatible with the development of a new process. PALLADIUM AND PLATINUM PRECIPITATION It was thought that zinc could be replaced with a reagent other than a hydrogen-evolving metal. Semiquantitative experiments showed that platinum and palladium could be precipitated completely from the gold-free solutions with such well-known reagents as sodium formate, formic acid, formaldehyde, and paraformaldehyde. Sodium formate was the preferred reagent, since the other three are volatile and somewhat toxic. The gold-free solutions used were those saturated with sulfur dioxide, partly freed of sulfur dioxide by aerating overnight, completely freed by boiling, as well as strongly and weakly acidic, neutral, and alkaline solutions. The reactions are complex and can be represented by these over-all equations: PdC1, + HCOONa — Pd + NaCl + HC1 + Co2 PtCl4 + 2HCOONa — Pt + 2NaCl + 2HC1 + 2CCX, Strongly acidic solutions required as much as five times the theoretical amount of sodium formate as did solutions neutralized to pH 4.5. Increasing the pH decreased the consumption of

Jan 1, 1965