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By W. C. Wahl, M. M. Fine

Leonardite , a naturally occurring , partially oxidized form of lignite with a high content of humic acids , was investigated as a binder for iron ore pellets . Although insoluble in original condition , leonardite forms watersoluble salts with good binding properties when treated with certain alkalis such as sodium hydroxide . Soluble leonardite imparts excellent dry strength to pellets , but green strength is somewhat lower than that obtainable with bentonite . However , green strength can be improved by adding a small amount of calcium hydroxide to the leonardite - concentrate mixture . Leonardite binders were used successfully on three of the four different concentrates tested .

Jan 1, 1964

By T. E. Green, E. F. Spano, W. J. Campbell

A combined ion exchange X- ray spectrographic method was evaluated for the determination of 11 metallic elements in high - purity tungsten : Aluminum , calcium , chromium , cobalt , copper , iron , magnesium , manganese , nickel , titanium , and zinc . Copper , nickel , and manganese in the 5- to 100 - microgram range ( 1 to 20 parts per million based on 5 - gram samples of tungsten ) , calcium in the 10- to 100 - microgram range , and cobalt in the 5- to 20 - microgram range can be determined within an accuracy of ± 10 percent of the amount present . Limits of detection of these elements are 0.05 to 0.14 microgram . The overall method was unsatisfactory for the determination of aluminum , chromium , iron , magnesium , titanium and zinc in tungsten .

Jan 1, 1964

By R. V. Lundquist, A. E. Morris, E. L. Singleton

This experimental research was performed to determine rate - of - reaction constants on the MnO - C and Mn , C₂ - 3MnO systems at 1,100 ° , 1,150 ° , and 1,185 ° C. Reactions were conducted at atmospheric pressure under controlled flow of purified helium through the furnace chamber . The weight - loss method defined reduction percentages , and reaction products were identified by X- ray methods . The system Mn0 - C followed a linear reaction rate , and experimental results produced an apparent activation energy of 55.8 kcal per mole of Mn0 . The system Mn, C - 3Mn0 followed a parabolic rate of reaction law and yielded an apparent activation energy of 114.4 kcal per mole for the reaction .

Jan 1, 1964

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 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 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 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. 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 Manuel Gomez

Carbon number distributions were obtained for tar acid fractions from five low-temperature tars by low-ionizing voltage mass spectrometry. Quantitative data for phenols representing seven structural compound types were examined by statistical analysis. It was shown that for the phenols discussed, the data could be represented by regression equations expressing phenolic concentration as a function of the reciprocal of the carbon number and the carbon-to-hydrogen ratio of the parent coal. The total concentration of each structural type present was found to depend on the molecular weight and boiling point of the initial member of the group. Carbon distribution data for the tar acid fractions studied support the view that low-temperature tars contain the same chemical compounds but in different proportions.

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 James S. Browning

The Bureau of Mines conducted laboratory batch and small-scale continuous flotation tests of weathered mica pegmatite ores from Alabama and North Carolina to determine the technical feasibility of recovering commercial-grade mica concentrates. A new anionic-catonic method was developed for recovering mica in the presence of clay slimes. In continuous tests, concentrates containing 98.1 percent mica were obtained from the Alabama pegmatite ore; the North Carolina pegmatite ore concentrates contained 97.2 percent mica. The recoveries were 83.8 and 81.6 percent, respectively.

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 Tilman M. M.

The effects of substituting cobalt for nickel on the acid corrosion resistance of two types of austenitic stainless steel were determined. Cobalt substitutions to a maximum 2.2 weight-percent were made in types 302 and 309 stainless steels. Total immersion corrosion tests were made in 10 volume-percent hydrochloric acid, and boiling-acid tests were conducted in 65 weight-percent nitric acid and in undiluted glacial acetic acid. For modified type 309 in acetic acid, corrosion rates decreased for additions greater than 0.57 weight-percent cobalt. Corrosion rates increased as cobalt was increased up to about 1 weight percent for modified type 302 in nitric and hydrochloric acids and for modified type 309 in nitric acid, but these rates decreased with a further increase in cobalt content. A gradual increase in corrosion rates with increasing cobalt content was shown for type 302 in acetic acid and for type 309 in hydrochloric acid. Cobalt substitutions in larger amounts (above a ratio of 8 Ni to 1 Co) may increase the corrosion resistance of the austenitic stainless steels.

Jan 1, 1965

By L. B. Pankratz

Heat content measurements were conducted for GaPo.996 and InPo.986 over the temperature range from 298° to 1,100° K, and for In2S2.897 over the range from 298° to 1,200° K. Both the actual experimental data and values adjusted to conform with the stoichiometric compositions (GaP, InP, and In2S3) were reported. Entropy increments above 298.15° K were calculated for the stoichiometric compounds, and heat content and heat capacity equations were derived.

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

By R. C. Buehl

A pyrometallurgical process for recovering manganese from open-hearth furnace slags or low-grade manganiferous iron ores is described. The slag or ore is smelted in a blast furnace to produce spiegeleisen; the speigeleisen is then blown with air in a basic converter to give an oxide slag. This slag product contains 60 to 75 percent manganous oxide and may be considered a synthetic manganese ore. In the smelting operations coke rates for five test periods ranged from 3,255 to 4,130 lb per ton of spiegeleisen. The recovery of manganese in the spiegeleisen varied from 60 to 76 percent. Recovery increased to 83 percent when the open-hearth slag feed to the blast furnace was diluted with a high-? grade iron ore sinter to facilitate smelting. In blowing the spiegeleisen a cyclic procedure was developed that gave nearly 90 percent recovery of manganese in the slag product (synthetic ore) yet prevented excessive contamination of the slag by phosphorus and iron. The overall recovery of manganese was about 75 percent when iron ore sinter was used with the open-hearth slag in the smelting step. The metal remaining after oxidizing the manganese from the spiegeleisen contained approximately 3.5 percent phosphorus. It was refined in a basic converter by blowing with air in the presence of lime" A high--grade iron and a basic phosphate slag were produced.

Jan 1, 1965

By John Nagy

Dust explosion data obtained in laboratory studies by the Bureau of Mines are presented for activated carbon, asphalt, charcoal, carbon black, coal, coke, gilsonite, graphite, lignite, miscellaneous carbons, pitch, tunnel dust, and mixtures of these materials with other ingredients. The explosion hazard is shown to increase as the volatile content of the dusts increases.

Jan 1, 1965

By H. Dolezal

An investigation was made on the use of magnesium for the direct reduction of rutile to make low-cost, offgrade titanium which could be upgraded to an acceptable grade of metal by electrorefining. Reductions made with charges containing magnesium chloride under hydrogen yielded products with oxygen con-tests close to the theoretical equilibrium composition. Two reduction products were made from rutile for use in electrorefining amenability tests: (1) a product from reduction in an inert atmosphere which contained 88.9 percent titanium and 4.42 percent oxygen, and (2) a product from reduction in a hydro-gen atmosphere which contained 92.5 percent titanium and 2.40 percent oxygen. Reduction products obtained under both of these conditions were amenable to electrorefining.

Jan 1, 1965