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By R. S. Lang, C. C. Merrill

The recovery of zinc from oxidized zinc minerals by the caustic soda leach and electrolytic or chemical precipitation was investigated . With the exception of willemite ( 2 ZnO • Si0₂ ) oxidized zinc minerals were readily soluble in 180 to 240 g / 1 NaOH solutions . A high- grade zinc flake was recovered electrolytically from solutions which had been treated with zinc powder to precipitate copper and lead . Solutions were recycled to the leach stage with a recovery of about 85 percent of the zinc from an ore containing 21.2 percent zinc . Electrolysis was conducted at a current density of 120 amp / ft2 with a power consumption of about 1.5 kwhr /lb zinc . Zinc was also recovered from leach solutions by dilution of the solutions , carbonation of the solution , or the addition of sulfur to boiling solutions . A dilution ratio of 5 : 1 precipitated 59 percent of the zinc in 9 days . Carbonation of the solutions precipitated the zinc as zinc oxide ( ZnO ) and solutions could be recausticized for recycling . Zinc precipitated as the sulfide with sulfur was easily filtered and washed . Approximately half of the sulfur added to solutions was lost in the form of sodium thiosulfate ( Na S₂03 ) .

Jan 1, 1965

By J. A. Eisele, D. J. Bauer, D. E. Shanks

As part of its effort to produce cell - grade alumina from clay , the Bureau of Mines investigated the hydrogen chloride gas - sparging crystallization of aluminum chloride hexahydrate ( ACH ) from aluminum chloride liquor , to provide information for optimizing the crystallization operation . Four parameters important in controlling the crystallization of the aluminum chloride hexahydrate and the concentration of impurities , particularly phosphorus and magnesium , in ACH crystals are ( 1 ) aluminum chloride concentration in the feed solution to crystallization , ( 2 ) hydrogen chloride gas flow rate , ( 3 ) temperature , and ( 4 ) concentration of phosphorus and magnesium also in the feed solution . Parameters 1 , 2 , and 3 affect crystal formation . The combined effects are very important because the phosphorus and magnesium concentrate in the crystals during the early stages of crystal growth . Aluminum chloride hexahydrate of cell -grade purity was crystallized from saturated aluminum chloride solutions containing less than 0.003 wt - pct P205 and 0.010 wt - pct Mg0 . Crystallization temperatures less than 60° C decreased crystal purity .

Jan 1, 1965

By Paul W. Johnson, Ralph C. Kirby, Frank A. Peters

A series of economic evaluations of processes for producing metallurgicalgrade alumina from low- grade aluminous materials is being conducted by the Bureau of Mines to determine the relative processing costs . The two processes considered in this evaluation are concerned with the recovery of alumina from clay through the formation of ammonium alum . In the first process , dehydrated clay is leached with ammonium bisulfate solution ; in the second process , clay is baked with ammonium sulfate and then leached with water containing a small quantity of sulfuric acid . After the alumina is dissolved by either of these methods , the iron is reduced to the ferrous state to avoid crystallization of ferric sulfate with the alum . The recovery of pure alum requires two crystallization steps . The alum crystals are then redissolved and precipitated with ammonia to produce alumina hydrate , which is calcined to a - alumina . These evaluations are based on published work , and the proposed plants are designed for a capacity of 1,000 tons of alumina per day . The estimated operating cost per ton of alumina for the bisulfate leaching process is $ 117.06 , and for the sulfate baking process , $ 109.26 . Using a Marshall and Stevens chemical equipment index basis of 240.0 , the estimated fixed capital costs , in the same order , are $ 158 million and $ 146 million . Under current economic conditions , these two processes are not competitive with the Bayer process for the production of alumina from bauxite . Since small improvements will not reduce costs sufficiently to approach competitive costs , future research work with these processes should be confined to areas likely to result in major cost reductions .

Jan 1, 1965

By John K. Alley, Robert C. Johnson

The primary objective of the research was to grow aluminum borate whiskers or fibers and to determine their properties . Molten salt bath and vapor deposition methods were used for synthesis . Whiskers exceeding 25 mm in length were grown . The best results were obtained by vapor deposition and most of the data presented were determined on whiskers produced by this method of synthesis . Three different aluminum borate compositions ( 4.8A1203 B₂03 , 3.8A1203 B203 , and 2.5A120, B203 ) were identified by X- ray and chemical analyses . The aluminum borates 4.8A1203 B20, X- ray diffraction pattern was indexed . Optical data were obtained on the three aluminum borates . In addition the following whisker properties and growth factors were determined : ideal atmospheric dewpoint for vapor deposition method , near 65 ° F ; temperature range of whisker formation , 1,000 ° to 1,400 ° C for the molten bath method of synthesis , > 1,000 ° to < 1,400 ° C for the vapor deposition method ; whisker growth rates by the vapor deposition method , maximum 12 mm per hour ; raw material vaporization , 50 to 60 percent of the fluoride lost in 1 hour ; tensile strength , maximum obtained 174,162 psi ; melting points , ranged from 1,675 ° to 1,795 ° C.

Jan 1, 1965

By E. A. Rowe, G. H. Keith, B. D. Jones

An evaluation of electrowon tungsten powder was made by comparing its characteristics with conventional hydrogen - reduced tungsten powder . Electrowon tungsten powder was investigated with respect to particle size and shape , apparent density , flow rate , compressibility , green strength , and sintering characteristics . In addition , its chemical purity , absolute density , and purification by melting were determined . Significant findings were higher flow rates and better compressibility than hydrogen - reduced tungsten powder . However , the large particle size peculiar to the electrowinning process effectively prevented conventional sintering to a high- density material . The possibility of producing high - density material , using a new technique of hot swaging sheathed sintered - tungsten compacts , was demonstrated by the achievement of densities of 92 percent of theoretical .

Jan 1, 1965

By W. H. Frederic, F. H. Gibson, R. F. Abernethy

This publication contains the quantitative values for phosphorus , chlorine , sodium , and potassium in United States coals . The samples tested were taken from commercial shipments and have been selected to represent the principal coal producing areas of the country . Due to combining the analytical results from two separate surveys , values for the four elements are not available for all samples .

Jan 1, 1965

By R. P. Walters, M. J. Lynch, D. R. Flinn

The Bureau of Mines evaluated tthhee feasibility of substituting platinum- coated metals for bulk platinum shapes as a means for conserving platinum . Platinum coatings were prepared using four different methods of electrodeposition , then tested and evaluated . In order for platinum coatings to be useful in process environments , they must be thick , adherent , stress - free , and pore - free . The Bureau evaluated direct - current , current reversal , cathode shielding , and pulsed- current plating techniques for producing a pore-free platinum electrodeposit from a molten cyanide bath . Aqueous corrosion tests of Fe - 10Cr substrates coated with approximately 25 μm of platinum showed that pulse plating yielded the most corrosion- resistant and , hence , the most pore -free coatings . The morphology of coating cross sections was in all cases columnar . The average grain size of pulse -plated deposits was independent of thickness , while all other plating techniques produced grains that increased in size as the coatings became thicker . It is believed that the constant grain size in the pulse - plated deposits resulted from better mass transport during the electrodeposition .

Jan 1, 1965

By Robert A. Speirer, Richard G. Burdick

Methods of detecting geologic faults and other linear features by means of processed LANDSAT satellite images have gained prominence during the past several years . There have been numerous programs written to pick these " lineaments , " but they have been almost universally tailored to large computers . This Bureau of Mines report describes a detection method developed for use with a minicomputer . The method comprises a suite of programs that scans an image for all " potential " lineaments . From this partially analyzed data , the final lineaments are picked by another routine . The method was field tested in an area of south- central Wyoming , and results indicated good agreement between computer- picked lineaments and ground features . Most of the known geologic faults in the area were picked by the method . Such features as roads and trails were also picked but were easily distinguished from faults during field inspection . The method is relatively new but promises to be a viable reconnaissance technique for the mining industry in geologic structural analysis .

Jan 1, 1965

By Howard P. Hamlin, John W. Sweeney

Shales from 14 locations in Indiana were sampled , tested , and evaluated to determine feasibility of producing lightweight aggregates by rotary - kiln and sintering methods . Sampling procedures and the geology of the significant shale units are discussed . Preliminary testing was conducted in a muffle furnace , and continuous tests were made in a 16 - inch by 14 - foot rotary kiln . The aggregate weighed 37.0 to 47.2 pounds per cubic foot . Concrete cubes employing the aggregate were tested to determine the qualities of the concrete . Compressive strength of the concrete using seven bags of cement per cubic yard , after autoclave curing for 6 hours , ranged from 3,600 to 5,850 pounds per square inch . Four samples made suitable lightweight aggregate in the laboratory rotary kiln . Four samples tested by sintering methods made unsatisfactory aggregate .

Jan 1, 1965

By Dwight L. Sawyer, Roy T. Sorensen

The Bureau of Mines has investigated the recovery of alumina by hydrochloric acid leaching of calcined kaolinitic clay . Bench- scale studies indicated that horizontal belt filtration was a pprraaccttiiccaall method for separating the siliceous residue from aluminum chloride liquor generated in the leaching step . Miniplant -scale continuous testing was performed to evaluate the filter circuits and to compare filtration response of different calcined kaolin feed materials and of different agitatorbaffle designs in the leaching reactors . Soluble alumina recovery with a single filter ranged from 94 pct with minus 10 -mesh feed more than 96 pct with minus 35-mesh or misted feed . Process advantages were confirmed for the calcined misted kaolin feed material prepared by a Bureau-developed misting process . With two filters in series , an overall filtration rate of 100 lb solids /hr.ft - 2 of filter area was attained with a soluble alumina recovery of more than 99 pct . More than 99.5 pct alumina recovery was obtained with a thickener and a two - filter circuit for either the minus 35-mesh or the misted feed . Modifications in leaching reactor design made to decrease particle- toparticle attrition were successful and significantly increased filtration rates and decreased flocculant requirements .

Jan 1, 1965

By Van E. Shaw, D. J. Bauer

Conversion of euxenite concentrate to sulfates with sulfuric acid and solvent extraction of the yttrium- rare - earth mixture with EHPA were studied to determine extraction and separation characteristics . Digestion with 3.5 pounds of 96 percent sulfuric acid per pound of concentrate at 336 ° C for 4 hours resulted in an easily handled product with a yield in excess of 98 per- A thorium- free product was obtained by calcining the sulfated material for 3.5 hours at 650 ° C prior to leaching with water . Di ( 2 - ethylhexyl ) phosphoric acid solvent is an effective extractant with preference for cerium ( IV ) and heavy - group rare - earth elements including yttrium . Separation of complex rare - earth mixtures into light- and heavy - group fractions is feasible , and these fractions can be further processed to isolate ytterbium , neodymium , and dysprosium by changing processing conditions to obtain separation factors greater than two between these and adjacent elements .

Jan 1, 1965

By R. A. Busch, R. R. Backer, R. W. McKibbin

The Bureau of Mines conducted laboratory tests to determine the slur- ry transport and deposition properties of coal waste. A 188.5-ft pipe test loop was constructed with instruments to measure density, flow, and power and discharge, suction, and differential pressures. A 20-ton sample of Western coal waste was crushed and screened to 100 pct minus 1/2 in. Eight loop tests using this graded waste were run at slurry densities ranging from 1.15 (25 wt-pct solids) to 1.46 (60 wt-pct sol- ids). The resultant friction-pressure gradients ranged from 0.06 to 0.24 ft of water per foot of 4-in standard steel pipe. Particle-size degradation was significant. In a typical loop test lasting 25 min, the minus 200-mesh fraction increased from 19 pct to 34 pct. Deposi- tion tests showed that without the use of a flocculant, the slurries would not dewater when left to stand for 1 week. With flocculant, ad- ditional water was released; however, the settled slurries remained thixotropic. Further testing is necessary to determine their suitabil- ity for use as backfill material in active mines.

Jan 1, 1965

By Elton L. Litchfield, Milton L. Weiss

Studies were made on the projectile impact sensitivity of explosives by subjecting explosive samples to the impact of metal projectiles fired from a 0.50- caliber gun . The projectiles , in the form of right cylinders , made plane surface to plane surface contact with the explosives . Pressures in the explosive were investigated with an expendable pressure transducer in some instances . The physical model of the projectile - explosive interaction describes , in principle , the duration of the peak shock pressure in terms of the projectile and explosive geometry and the steady- state penetration of the explosive . Of the explosives studied , liquid hydrogen- solid oxygen and liquid oxygen - solid or liquid hydrocarbon fuel were the most shock sensitive ( requiring an initiating shock of about 1.0 kb or 987 atmospheres pressure ) ; cast TNT was the least sensitive ( requiring an initiating shock of more than 110 kb pressure ) . Measurements of pressure in the explosive showed some moderate space resolution by the transducer and gave pressure distributions in agreement with expectations from the model of the shock processes . The appearance of the recovered projectiles and the calculated initiation shock pressures suggest that the solid explosives were initiated directly to high- order detonation , whereas the liquid explosives were probably initiated to low- order detonation-- with a subsequent , later transition to high- order detonation .

Jan 1, 1965

By E. Morrice

The Bureau of Mines investigated methods for beneficiating platinumgroup metal ores from the Stillwater Complex , Montana , as part of its program to increase the supply of critical and strategic minerals and metals from domestic resources . This report presents results of a 5- day continuous campaign employing a pilot flotation mill to recover sulfide concentrate containing platinum- palladium values from anorthositic ore . A mercaptobenzothiazole - sulfuric acid reagent suite was used . The pilot flotation mill was operated at an average feed rate of 106 lb/ hr of ore . A rougher concentrate containing 8.5 pct of the feed was prepared ; it assayed 1.1 oz /ton Pt and 3.5 oz / ton Pd . Recovery of platinum and palladium were 91 and 87 pct , respectively .

Jan 1, 1965

By N. A. Eilertsen, Rolf S. Paine

The Bureau of Mines studied the presplitting technique used for controlling overbreakage in the walls of a vertical shaft at the U.S. Army Corps of Engineers Littleville Dam project near Huntington, Mass. The periphery of the shaft, the dimensions of which were 16-1/2 feet wide by 21 feet long and 52 feet deep, was presplit (cracked) in the solid to a depth of 48 feet prior to full-depth sinking. Presplitting prevented overbreak in a fairly soft schist and provided sound self-supporting walls which required very little scaling.

Jan 1, 1965

By Jack L. Henry, Davis E. Traut, L. R. Penner

The Bureau of Mines conducted solvent extraction batch tests to evaluate the usefulness of neodecanoic acid ( NDA) for extracting Co 3+ from ammoniacal leach liquors high in ammonium sulfate . This work is an outgrowth of previous Bureau research in which technology was devised for the recovery of cobalt , nickel , and byproduct copper from domestic laterites . The previously devised technology uses an oxidative ammoniacal sulfate leach to treat the laterite , and nickel and copper are then recovered from the leach solution by solvent extraction and electrowinning . This report deals with the subsequent solvent extraction of cobalt from the nickel - copper raffinate solution . The results showed that about 70 pct of the contained Co 3+ can be extracted batchwise at pH 8 using NDA ( a 10 - carbon - chain highly branched carboxylic acid ) . However , NDA had a solubility of approximately 0.6 to 0.8 g / L in aqueous raffinate following extraction , and this high solubility makes it impractical for use with alkaline solutions that are low in cobalt . In addition , the extracted cobalt species ( predominately cobaltic hexammine ) is not amenable to the electrolytic recovery of cobalt metal because of its extreme stability . This fundamental prob-

Jan 1, 1965

By A. D. McMahon

This survey is one of a series of Bureau of Mines publications designed to serve the needs of Government and industry for comprehensive information on mineral commodities and activities. Copper, a versatile metal, has been vital to all civilizations from prehistoric times to the present. Its essential value in antiquity and until the nineteenth century arose from its malleability and ease of working, its corrosion resistance and durability', its attractive colors in alloyed and unalloyed forms, and, of course, its availability. The principal uses were for tools, utensils, vessels, weapons, pipe, statuary and other objects of art, and for building and architectural pur£~ses where formability, permanence, and beaut)" were necessary qualities. Utilization of copper based on these physical and mechanical properties has grown tremendously for commercial, structural, mechanical, architectural, and art items; and its capacity for forming numerous alloys has led to a myriad of applications from miniature copper and brass eyelets to huge bronze battleship propellers. The early nineteenth century marks the epoch of the greatest use of copper, transmitting electrical energy. This particular property of copper is fundamental to the spectacular growth of the electrical industry and all associated industries relying on electricity for power, light, and heat. More than half of all copper produced is used for transmission of electricity. The copper industry has been able to expand along with the mounting demand because of the ever increasing discovery of resources in the world and advances in mining, metallurgical, and fabricating technologies. World production and consumption rose progressively from about 18,000 tons in 1800 to more than 4.5 million tons in 1960. The estimated world reserve of primary- copper has more than doubled since 1935, being 212 million tons in 1960. Ninety percent of this reserve is credited to eight countries-the United States, Canada, Chile, Peru, the Soviet Union, Poland, Northern Rhodesia, and the Republic of the Congo. The United States share is 32.5 million tons of copper in ore, averaging approximately 0.9 percent. Another reserve being accumulated in the industrial countries of the world is copper products now in use that will eventually be discarded as scrap and become available for recovering secondary copper. In the United States this resource of more than 30 million tons, provides about one-fourth of the annual supply.

Jan 1, 1965

By Wallace W. Key

Mineral raw materials produced in California, other States, and foreign countries were purchased for consumption in quantities valued at over $60 million at 800 of the 1,200 chemical plants operating in California in 1960, according to questionnaires completed by company officials. These and other data received from mineral consumers, producers, dealers, and Government agencies formed the basis for this the first of a series of reports designed to present the intricate features and relationships controlling mineral raw material supply and demand in California industries. The results of this study indicated certain changes in use patterns of minerals in chemica 1 manufacturing; a shift in requirements from metals to nonmeta ls, from inorganics to organics, from natura 1 to synthet ic materia ls , and from distant to local sources of supply.

Jan 1, 1965

By Richard D. Miller, Geraldine P. Norrell

This publication contains routine analyses and related source data for 295 natural gas samples from 18 States collected during calendar year 1963 as part of a continuous survey of the United States for occurrences of helium in natural gas. This survey has been conducted by the Bureau of Mines since 1917. The analyses published herein were made by mass spectrometer and a special helium analysis apparatus, which are described in Bureau of Mines Bulletins 4863 and 576.4 Five previous publications have been made to present the results of 5,998 gas analyses made by the Bureau of Mines Helium Activity , prior to 1963. The first three , Bulletin 486,5 Bulletin 576,6 and Bulletin 617,7/ contain analyses and source data on 5,214 gas samples collected from 1917 to January 1 , 1961. The fourth and fifth publications , which are published as Information Circulars , supplement the three Bulletins and contain 784 analyses of samples collected during 1961 and 1962. The present Information Circular is the third annual publication supplementing the three Bulletins .

Jan 1, 1965

By James F. O'Neill

Brown iron ore deposits in Quitman County , Ga . , were investigated by the Federal Bureau of Mines in cooperation with the State of Georgia , Department of Commerce , and the University of Alabama . Ninety- one holes were drilled , having an aggregate footage of 2,188 feet ; seventy- one holes penetrated 248 feet of iron mineralization . Average thickness of the ore zone was 3.5 feet under an average thickness of 14.7 feet of overburden . The drilling developed inferred reserves containing nearly 30 million long tons of crude ore with an average analysis of 28 percent iron plus minor quantities of manganese . Test work done by the Bureau on the crude ore samples indicated that they would upgrade by current log washer practice , with the use of a 1 /8 - inch screen , and yield 4.4 million dry long tons of concentrate with an average analysis of 52.1 percent iron plus manganese . The weight recovery obtained was 14.7 percent . Research studies made by the Bureau showed that the weight recovery would be increased by changing the screen size without any appreciable sacrifice of grade . The average weight recovery was increased to 18 percent with a 10 - mesh screen and 22.8 percent with a 20 - mesh screen . Screen tests studies indicated that there was no appreciable interlocking of the iron and manganese minerals and the clay and silica waste particles of the materials retained on a 200- mesh screen . Clay was prominent in micron - size slimes . Silica was deleterious in the minus 20 - mesh size .

Jan 1, 1965