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By J. W. Town

The Bureau of Mines determined the physical properties of southeastern Idaho phosphate fines as related to mineral composition, particle size and liberation, beneficiation, and potential use in structural clay products. The phosphate mineral in the fines was identified by unit-cell dimensions to be essentially the same as the phosphate mineral fluorapatite identified in the coarser sizes. The mean particle frequency as determined by electron-microscopy and pipet-analyses was between 0.5 and 0.2 micron. Liberation of the phosphate could not be definitely determined because of the weathered condition of the minerals and their extreme fineness. No beneficiation scheme was developed that would concentrate the phosphate into a marketable fertilizer product; therefore, forming and firing tests were made to demonstrate that the fines can be used to manufacture structural clay products.

Jan 1, 1968

By L. H. Adami

Heats of formation were obtained for four anhydrous crystalline sodium borates by hydrochloric acid solution calorimetry. The heats of formation at 298.15° K from the elements are NAB02, -233.2 ±0.6 kcal/mole; Na2B07, -786.4 ±1.0 kcal/mole; NaB305, -549.9 ±0.8 kcal/mole; and Na2B6013, -1,412.5 ±2.0 kcal/mole, The heats of formation from the constituent oxides are NaB02, -31.5 ±0.8 kcal/mole; Na2B407, -78.8 ±1.3 kcal/mole; NaB305, -44.1 ±0.8 kcal/mole; and Na2B8013, -96.7 ±1.5 kcal/mole.

Jan 1, 1968

By R. W. Freedman

The Bureau of Mines has developed a gas chromatographic method for the rapid and accurate determination of oxygen, nitrogen, carbon dioxide, methane, and, if present, carbon monoxide in mine air. This method replaces such presently used gas-reaction types as the Haldane or Orsat analysis, offering advantages in terms of precision, accuracy, speed, and convenience.

Jan 1, 1968

By Wesley T. Holmes

This report describes the second phase of an investigation aimed at obtaining a wider knowledge of the problems involved in smelting titaniferous magnetites. Liquidus temperature measurements were made on selected synthetic slag compositions in the Ti02 -A1203 -FeO-Si02 -CaO-MgO system. Both the hot-stage microscope and the strip furnace (melting-holding-quenching technique) were used during test procedure to determine the effects of CaO, MgO, and SiO2 on the liquidus temperature of slags. The liquidus temperatures of slags studied ranged from 1,241° to 1,900° C. The lowest liquidus temperature for each Ti02 plus A1203 plus FeO weight-percent generally occurred when the difference between CaO plus MgO and Si02 was less than 12 weight-percent. In this investigation substitution of either CaO or MgO for SiO2 and MgO for CaO raised the liquidus temperature of more than 50 percent of the reported base slags when Ti02, A1203, and FeO contents were held constant. The results of this investigation may serve as guidelines for determining flux requirements in smelting a wide variety of titaniferous magnetite concentrates or ores.

Jan 1, 1968

By John Nagy

Dust explosion data obtained in laboratory tests by the Bureau of Mines are presented for 181 miscellaneous materials that present an explosion hazard. Data are given also for 50 dusts that present primarily a fire hazard and for 88 dusts that did not present an explosion hazard.

Jan 1, 1968

By John Ward Smith

The Bureau of Mines drilled Wyoming Corehole No. 1 in Sweetwater County, Wyo., to sample Green River Formation oil shale. Core obtained was assayed for oil yield to determine richness and stratigraphic distribution of oil shale in the deposit. Oil shale in place at Wyoming No. 1 site represents over 200 million barrels of oil per square mile. Additional data useful in evaluating the deposit, including generalized stratigraphy and mineralogy, detailed lithologic descriptions of the core, rock specific gravity, and bore-hole logs, are presented with the oil-yield data. The sampled Wyoming oil shale resembles Mahogany-zone oil shale in rock properties and gross mineralogy. A statistically derived equation relating shale density to oil yield for the Wyoming deposit compares with a similar relationship valid for the better known Mahogany-zone oil shales in Colorado and Utah. A density log from Wyoming Corehole No. 1 is calibrated for direct oil-yield logging. The alternating rich and lean beds of shale at this site may permit creating the permeability necessary for direct production of shale oil from the shale in place.

Jan 1, 1968

By Franklin D. Cooper

This Bureau of Mines study reviews current and proposed methods of extracting copper from sub-mill-grade ore by leaching. The amount of copper produced by hydrometallurgy has increased dramatically in recent years and will probably be about 200,000 tons per year by 1970.

Jan 1, 1968

By D. H. Chambers

Digestion studies were undertaken to develop a method for the rapid dissolution of high-temperature ferroalloy scrap. Laboratory tests showed: (1) dissolution of alloy scrap with ferric ion as the leaching agent was a moderately rapid method of digestion; (2) the dissolution process can be considered as a typical reaction of a metal with chlorine gas, although evidence was obtained to show dissolution as a two-step process, one step as the reduction of ferric ion by the soluble alloy constituents and the other as the oxidation of ferrous ion with chlorine gas; and (3) the attack of ferric ion on the alloy was a function of alloy composition, ferric to ferrous ion ratio, and area of contact between leach solution and alloy. The exceedingly complex nature of alloy compositions and dissolution products generally precluded satisfactory analytical determinations. Results of moderate accuracy were obtained using complex modifications of standard analytical and spectrographic techniques.

Jan 1, 1968

By Thomas E. Green

A solvent extraction procedure using 8-hydroxyquinoline and chloroform was investigated by the Bureau of Mines as a preconcentration technique for the determination of aluminum, calcium, cobalt, copper, iron, lead, magnesium, manganese, nickel, and zinc in large samples of high purity tungsten. X-ray spectrographic and atomic absorption methods were used to determine the trace metals after preconcentration. The presence of 10 grams of tungsten had a pronounced effect on the distribution of 8-hydroxyquinoline between the aqueous and chloroform phases. This change in the 8-hydroxyquinoline distribution in turn had an adverse effect on the extraction of the trace metals. Extraction efficiencies can also be adversely affected by an increase in the quantity of extractable metals present, as shown by radiotracer tests using 65Zn. Excess 8-hydroxyquinoline in the extracts did not interfere with the determination -of the serious interference in the combined ion exchange paper--X-ray spectrographic method. Although preconcentration by 8-hydroxyquinoline extraction was found to be partially successful, other preconcentrationn methods based on ion exchange and dithizone extraction were found to be superior.

Jan 1, 1968

By R. K. Koch

The vapor pressures of liquid columbium and liquid hafnium were deter-mined by the Langmuir free evaporation method as a part of the Bureau of Mines program on the study of transition metals. An electron-beam furnace with a water-cooled copper crucible was used for melting. Temperature was measured with a two-color ratio pyrometer. Least-squares analyses of the vapor pres-sure data gave the following equations: [Logp (atm) = 5 .429 -31,310 T] for liquid columbium in the range 2,740° - 3,140° K, and [Log p (atm) = 5,690 28 T] for liquid zirconium in the range 2,500° -2,810° K. Third-law evaluations of each data set gave mean heats of sublimation (298.15° K) of 175.1±3.2 kcal/mole and 148.3±1.2 kcal/mole for columbium and hafnium, respectively. Second-law standard heats of sublimation determined from sigma plots and from sigma-prime plots agreed fairly well with the third-law values. The sigma-prime plots gave standard entropies of sublimation of 30.96±0.84 eu and 33.S6±0.44 eu for columbium and hafnium, respectively.

Jan 1, 1968

By C. B. Kenahan

The Bureau of Mines is developing methods for reclaiming the metal and mineral values contained in municipal incinerator residues. This report describes the first phase of the research, in which reliable methods for sampling and analyzing municipal residues were established and the composition and characteristics of the residues were determined. Samples were obtained from a variety of grate-type furnaces and also from a rotary kiln furnace. The samples were processed on a batch basis and separated into their natural categories by a variety of methods including screening, magnetic separation, air separation techniques, and handpicking. The main components of the residues were determined to be metal and metal oxides, glass, and ash.

Jan 1, 1968

By F. E. Brantley

Optimum autoclaving conditions were determined for separation of iron and manganese values from pregnant leach liquor produced in extracting manganese from low-grade umber are. The umber was leached with a synthetic anolyte similar to a recycle solution, used in manganese electrolysis cell operations, that had been renewed with ferrous sulfate and sulfuric acid. The equipment used and results obtained are presented for the several conditions employed. The kinetics of the separation were studied. Rate equations were derived for the formation of solid ammonium-manganese sulfate, (NH4)2 Mn2 (S04)3.

Jan 1, 1968

By Philip C. Good

Preliminary studies showed that direct hydrolysis of H2SiF6 to SiO2 and HF at elevated temperatures was subject to many mechanical difficulties, and that corrosion of construction materials was a serious problem. Elimination of SiO2 from the HF product was generally poor. An alternative procedure, hydrolysis of lime-neutralized H2SiF6 by steam at 950° to 1,100° C, yielded a product very low in SiO2. Condensates containing up to 300 g/1 HF were prepared.

Jan 1, 1968

By P. R. Jones

A computer program was written for the design of a shell and tube heat exchanger on a price optimum basis for the following conditions: (1) Triangular pitch; (2) single or multiple pass; (3) heating or cooling; (4) no change in phase; and (5) inside pumping costs immaterial. Price optimum design was obtained for four standard tube sizes and standard pitch. The inside pressure drop was fixed and outside pressure drop was computed for the optimum baffle spacing and when the baffle spacing equaled the shell diameter. Standard shells whose areas equaled or exceeded the required area were also listed. The program was made adaptable to various fluids and to various tube sizes and pitch by reading in many of the required data such as physical properties of the fluids, tube data, and standard shell data in tabular form.

Jan 1, 1968

By Andrew J. Fergus

The purpose of this study was to provide basic information to aid further research on beryllium mineral flotation. Contact-angle and microflotation (Hallimond tube) methods were used to study collector action and flotation response of beryllium minerals and associated gangue minerals with representative commercial surfactants. Chrysoberyl received prime attention. Results indicated that selective flotation of beryl and chrysoberyl from fluorite and quartz is possible with sodium isooctyl phosphate below pH 2, and fluorite and topaz are readily collected by both anionic and cationic surfactants. Several modifying reagents were studied at one pH and one level of collector concentration. Aluminum sulfate, starch, and sodium silicate proved to be depressants in chrysoberyl flotation.

Jan 1, 1968

By R. O. Dannenberg

A metallic displacement process, utilizing easily available steel wool or steel window screen, was devised and successfully used for the recovery of silver from waste photographic fixing solutions. Laboratory and prolonged commercial-scale testing established that the iron filament type unit will efficiently precipitate silver, as a high-grade sludge, from acidic waste photographic fixing solutions ranging in grade from less than 1 to over 10 grams of silver per liter. Data and design information are presented to facilitate the construction and operation of a practical unit of any desired size. A smelting process for recovering pure silver from precipitated sludge containing 27 to 80 percent silver was devised.

Jan 1, 1968

By J. J. Demeter

Anthracite from the four producing regions in Pennsylvania was both ashed in the laboratory and burned on a chain-grate stoker to determine the sulfur-retention properties of its ash. The retention of sulfur in laboratory-prepared anthracite ash was shown to be related to ashing temperature and to the amounts of sulfur and calcium present in the coal. At the usual laboratory ashing temperature of 750° C sulfur retention ranged from 0.8 to 13.2 percent of the total coal sulfur. Sulfur retention in the ash was negligible, o to 0.3 percent, at 1,200° C, which is the thermal decomposition temperature of calcium sulfate; thus calcium sulfate does not form and cannot serve as a sulfur-retaining agent. In several tests the anthracite was mixed with 6 or 10 percent dolomite prior to firing in the chain-grate stoker. The dolomite did not improve sulfur retention owing to the high temperature in the fuel bed. Sulfur retention was, however, related to the unburned carbon in the ash. The relationship of the percentage of original coal sulfur retained in the ash (Y) to the percentage of the original carbon in the coal remaining in the ash (X) is expressed by Y = -0.579 + 0.914X. The percentage of sulfur retained is almost directly proportionate to the percentage of original coal carbon in the ash.

Jan 1, 1968

By Wilbert T. Malenka

A modified factorial experiment was used to determine the effect of operating factors in hydraulic mining of anthracite. Seven basic factors at various levels were considered. The significant factors were found to be pressure-volume, pattern, and jet traverse speed. Mining data were programed for computer, and a prediction equation was determined from printout information based on the hydraulic "jumbo" operating parameters and characteristics of anthracite, The source of error is discussed. The prediction equation is general in nature and might be useful in delineating performance characteristics in the design of equipment and/or more effective utilization in a medium with characteristics similar to those of anthracite.

Jan 1, 1968

By Everett A. Sondreal

Data are presented on the characteristics of lignites with emphasis on the composition and fusion properties of the ash. Differences in the analyses of commercial-grade lignites are related primarily to variations in moisture and ash contents. Lignite ash is generally characterized by high concentra¬tions of alkaline earth oxides and a greater tendency for retention of sulfur in the ash than higher-rank coals. Composition of ash varies significantly within and between mines. The differences within mines are significant for short distances and may be eliminated under certain circumstances by normal mixing occurring during mining. The sulfur in lignite averages 0.6 percent and is found primarily in the organic or pyritic forms with only a trace of the sulfate. During the stan¬dard laboratory asking procedures, from 60 to 100 percent of the original sul¬fur is retained in the lignite ash. Trace elements, such as uranium and germanium, in the ash from commercial¬-grade lignites are present in low concentrations, but others, primarily copper and silver, are present in specific samples in concentrations approaching those found in some commercial ores.

Jan 1, 1968

By Philip C. Tully

These modifications to the Redlich-Kwong equations for pure hydrogen and neon were developed after an unsuccessful attempt to generalize a modification technique previously developed for helium. New coefficients of the B terms were developed by minimizing the residuals. No changes were made in the coefficients of the A terms. For normal hydrogen, B was changed to [0.08063Tc PcT] for temperatures from 980 to 423° K and pressures up to 1,050 atm. The average deviation in Z was 0.36 percent with maximum deviations less than 1 percent for all but a few low-temperature points. For neon, B was changed to [PCT 0.1025T], for temperatures from 120° to 973° K and pressures up to 1,500 atm. The average deviation in Z was 0.34 percent with maximum deviations less than 1 percent for all but a few high-pressure and low-temperature points. Efforts to attain a lower temperature range to comparable accuracy with this type of modification were unsuccessful. In the range of applicability, these equations should be used with caution when calculating derived thermodynamic functions, such as the isobaric specific heat.

Jan 1, 1968