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By M. J. Kovalik, D. E. Wolfson, F. Fischler

Plastometric tests were made to determine the maximum thickness of the plastic layer for different U.S. coals . The effect of test variables on the maximum thickness of the plastic layer was studied . The values for the maximum thickness of the plastic layer were found to be related to the Gieseler maximum fluidity , plastic temperature range , free swelling index , and other plastic properties of coals . Only a general relationship was observed between the plastometric parameters obtained in these tests and the coking properties of coal .

Jan 1, 1964

By W. A. Stickney, J. W. Town

Batch and continuous - circuit flotation , leaching , precipitation , and electrodeposition studies were made by the Bureau of Mines to determine optimum conditions for treatment of complex mercury - antimony sulfide and mercury- arsenic sulfide ores and concentrates . On the Red Devil ore sample over 95 percent of both the mercury and antimony sulfides were recovered in a flotation concentrate containing 35.6 percent mercury and 21.0 percent antimony . By selective flotation a mercury concentrate containing 71.0 percent mercury and 2.9 percent antimony was obtained with a mercury recovery of 90.4 percent . Leaching results show that , with 150 grams per liter of sodium sulfide and 50 grams per liter of sodium hydroxide , 95 to 99 percent of the mercury , antimony , and arsenic sulfides could be extracted from the concentrates treated . Sodium hydroxide reagent consumption was based on the sulfides generated in the dissolution of the sulfide minerals and on the method of metal recovery used . Selective leaching of the antimony and arsenic sulfides with potassium sulfide dissolved more than 95 percent of either of these two sulfides and 0.5 to 5 percent of the mercury sulfide present . Methods for recovering mercury and antimony from solution were electrodeposition of mercury followed by electrodeposition of antimony , aluminum precipitation of both mercury and antimony , or antimony precipitation of mercury followed by antimony electrodeposition . The method used in recovering the mercury depended on the mercury- antimony content of the solution being treated .Batch and continuous - circuit flotation , leaching , precipitation , and electrodeposition studies were made by the Bureau of Mines to determine optimum conditions for treatment of complex mercury - antimony sulfide and mercury- arsenic sulfide ores and concentrates . On the Red Devil ore sample over 95 percent of both the mercury and antimony sulfides were recovered in a flotation concentrate containing 35.6 percent mercury and 21.0 percent antimony . By selective flotation a mercury concentrate containing 71.0 percent mercury and 2.9 percent antimony was obtained with a mercury recovery of 90.4 percent . Leaching results show that , with 150 grams per liter of sodium sulfide and 50 grams per liter of sodium hydroxide , 95 to 99 percent of the mercury , antimony , and arsenic sulfides could be extracted from the concentrates treated . Sodium hydroxide reagent consumption was based on the sulfides generated in the dissolution of the sulfide minerals and on the method of metal recovery used . Selective leaching of the antimony and arsenic sulfides with potassium sulfide dissolved more than 95 percent of either of these two sulfides and 0.5 to 5 percent of the mercury sulfide present . Methods for recovering mercury and antimony from solution were electrodeposition of mercury followed by electrodeposition of antimony , aluminum precipitation of both mercury and antimony , or antimony precipitation of mercury followed by antimony electrodeposition . The method used in recovering the mercury depended on the mercury- antimony content of the solution being treated .

Jan 1, 1964

By D. A. O'Keefe, M. M. Wong

To obtain beryllium metal of higher purity , flakes produced from electrorefining scrap metal were used as cell feed for a second cycle of electrore fining at 500 ° C in an electrolyte composed of 51.7 mole - percent LiCl , 36.9 molepercent KC1 , and 11.4 mole - percent BeC¹ · Metallic impurities in the flakes totaled more than 108 ppm , the metallic impurities in the metal obtained from the two - cycle electrorefining were , with the exception of 35 ppm of calcium , below the spectrographic determination limits .

Jan 1, 1964

By Thomas C. Miller, Rudolph Sporcic

A relatively simple and inexpensive encapsulated hydraulic device has been developed by the Bureau of Mines to facilitate study of coal bumps , and to measure pressure changes in a coalbed as it is subjected to roof loading during mining . Construction of the device and application techniques are described . Preliminary feasibility tests in the laboratory and field indicate that the device responds satisfactorily to pressure changes in coal created by roof loading .

Jan 1, 1964

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 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 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 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 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 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 J. R. Ross

Techniques for recovering scandium from uranium plant iron sludges and from wolframite concentrates are described. The best procedure found comprised (1) dissolution with sulfuric acid, (2) preliminary concentration by solvent extraction with a primary alkyl amine, (3) further enrichment and purification by a combination of ion exchange, solvent extraction, chemical precipitation, and calcination. Recovery of scandium from these raw materials, which contained 0.058 and 0.14 percent scandium, ranged from 83 to 90 percent in products analyzing 99.6 to 99.9 percent scandium oxide.

Jan 1, 1965

By John Nagy

Results of initial research by the Bureau of Mines are given on the dust explosion hazard of float coal and on the related factors of occurrence, rate of production, sampling techniques, transport, and deposition of float coal. Tentatively, it is suggested that where float coal deposits prevail, a mini-mum of 80 percent incombustible be maintained in the top 1/8-inch layer to neutralize the explosion hazard of the surficial coal deposit.

Jan 1, 1965

By R. V. Lundquist

The specific conductance of solutions of sodium hydroxide and of sodium aluminate was directly proportional to the temperature. The specific conductance of sodium aluminate solutions with identical sodium ion concentration and at constant temperature decreased with increase in aluminum concentration. The aluminate ion population in solution was shown to consist of a mixture of monovalent and polyvalent ions. Aluminate ions did not influence the temperature dependence of pH in caustic solutions containing sodium aluminate. The density and viscosity of a solution was inversely proportional to the temperature and directly proportional to the concentrations of sodium and aluminate ions.

Jan 1, 1965

By B. B. Letson

The heats of formation of lithium chloride and lithium oxalate were determined with the aid of a Bureau-developed, glass Dewar-type solution calorimeter which uses thermistors as its temperature sensing element. Values obtained at 298.15° K were -98.38 ± 0.54 kcal/mole for lithium chloride and -329.02 ± 0.79 kcal/mole for lithium oxalate, using graphite as the standard state for carbon.

Jan 1, 1965

By W. W. Agey

An inexpensive technique that laboratory studies indicated would significantly reduce seepage in irrigation canals was devised and tested through research sponsored by the Bureau of Reclamation and the Missouri River Basin Field Committee. Laboratory tests simulating optimum field conditions determined that easily applied sodium carbonate solutions made test beds of canal lining materials virtually impermeable for long periods. The study comprised alternative laboratory treatments of 3-inch-deep test beds of canal earths with 74 water-soluble chemicals in search of one 01&apos; more that would effectively improve the water barrier characteristics of the component clays. Sodium carbonate, one of the least expensive, was among the most effective. The addition of 0,4 lb of reagent per sq yd greatly reduced the seepage from typical, highly permeable test beds. The reagent penetrated and sealed surface for about a 1.5-inch depth.

Jan 1, 1965

By John S. Berber

Tar produced as a byproduct from low-temperature carbonization of coal contains only small amounts of valuable lower boiling tar acids but relatively high percentages of high-boiling tar acids. These high-boiling tar acids are characterized by a high degree of alkylation and can be converted into the lower boiling homologs by catalytic treatment to remove the alkyl groups or decrease their chain lengths.

Jan 1, 1965

By Mulligan John J.

The Bureau of Mines investigated lode tin deposits on Potato Mountain, Seward Peninsula, Alaska. Tin was found to occur as cassiterite associated with quartz, tourmaline, pyrite, arsenopyrite, and earthy clays, but the deposits lack the varied accessory minerals commonly found in tin districts. The tin-bearing deposits are in metasediments along minor breaks and bedding planes but not in the crushed earthy filling of major faults. Cassiterite and sulfides occur with quartz in veins, both with and without earthy clays, and disseminated through tourmalinized wall rocks. The deposits are characterized by irregular segregations containing 1 to 10 percent tin within zones averaging not over 0.25 percent tin. The largest segregation exposed is on the summit of a low hill on the east-central slopes of Little Potato Mountain; most of the outcroppings are in an area trending east to west, roughly 10 to 30 feet wide and 300 feet long. Sample values ranged as high as 12 percent tin, but the average grade may be about 1 percent tin. The extreme irregularity of both grade and composition precludes a more exact determination. Similar concentrations are scattered for over 1,000 feet to the west and north, but these are smaller and lower in grade. Elsewhere on Potato Mountain, generally similar deposits occur as clusters of veinlets at widely separated points in the metasedimentary walls of major faults.

Jan 1, 1965

By Oliver Q. Leone

The effect of oxygen content in the anode metal on titanium electrorefining characteristics was studied. Increasing quantities of oxygen in the anode resulted in increased anode scale formation, decreased anode and cathode current efficiencies, lower titanium recovery efficiencies, and higher oxygen content of the cathode products. The titanium electrorefining process performed best when the anodes did not contain more than 0.5 percent oxygen, although anode dissolution was recorded for alloys containing up to 25 percent oxygen. Back emf affords a useful index of an alloy to electrorefining.

Jan 1, 1965

By H. J. Heinen

A technique offering promise as a metallurgical processing sequence the recovery of molybdenum (Mo) from the sulfide mineral--molybdenite?was investigated. The method consists of two steps: (1) electrosynthesis of pure dimolybdenum carbide (Mo2C) from molybdenite (MoS2) and (2) interaction of Mo2C and molybdic oxide (MoO3) to produce pure molybdenum metal. Two molten salt systems were satisfactory for electrosynthesizing Mo2C. The first was a mixture of potassium chloride (KCl), potassium fluoride (KY), and sodium metasilicate (Na2SiO3), and the second consisted of sodium fluoride (NaF), KF, sodium tetraborate (Na2B4O7), and sodium carbonate (Na2CO3). Yields up to 0.42 gram of Mo2C per ampere-hour were obtained. The carbide, mixed with monitored amounts of MoO3, was converted to molybdenum metal of 99.9 percent purity by sintering at 1,500° C.

Jan 1, 1965

By R. V. Lundquist

The compound 2Na2O?3CaO?5Al2O3 occurs as a minor phase in lime-soda sinters prepared for extracting aluminum from siliceous aluminum-bearing materials. About 99 percent extraction of sodium and aluminum from synthesized 2Na2O.3CaO.5Al2O3 was obtained in solutions of NaOH-Na2CO3 at leaching temperatures of 50° C and above. Extractions in water were low because insufficient NaOH was generated by hydrolysis. Extractions in NaOH solutions were limited to about 80 percent owing to the precipitation of hydrated calcium aluminates. Rapid extractions of 100 percent were obtainable in NaaC03 solutions, but the subsequent rapid precipitation of alumina trihydrate caused losses in alumina recovery.

Jan 1, 1965