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By K. K. Kelley, W. W. Weller

This report contains experimentally determined heat capacity data for four crystalline sulfides -- AsS , GeS , NiS , and Ni3 S₂ -- over the temperature range from 50 ° to 298.15 ° K. The heat capacity data were used to evaluate the entropies of the sulfides at 298.15 ° K. Entropies of formation from the metals and rhombic sulfur and from the metals and diatomic sulfur gas are also included .

Jan 1, 1964

By Richard F. Hewlett

Numerous populations of assays have been simulated for a range of assay values representative of low-grade mineral deposits to facilitate the study of problems encountered in evaluating these deposits. Analysis of these simulated populations of assays (obtained by using statistical probability models for the simulation) makes possible the quantification of the effects of (1) various composite assay intervals, (2) ore reserve computational methods, (3) uneven assay intervals, and (4) various cutoff grades on both the precision and the accuracy of the estimated average grade and tonnage of ore.

Jan 1, 1964

By Donald W. Mitchell, John Nagy, Edwin M. Murphy

Information is presented on remote sealing of a mine passageway through a borehole by five methods : PPnneeuummaattiicc injection of mineral wool and sand, ureaformaldehyde foam , balloons , urethane foam, and caving by blasting . An adaptation of the method using pneumatically conveyed mineral wool was tried in an operating mine . Further research is needed to simplify and to improve the techniques involved , as well as to explore the possibilities of other methods and combinations .

Jan 1, 1964

By J. R. Hauger, P. A. Romans, W. J. Niebuhr

With suitable instrumentation and techniques it is possible to determine the presence of tantalum in columbium to 20 ppm . This paper discusses the selection of X- ray spectrographic instrumentation and describes a technique for accomplishing the low level determination of tantalum . An ion- exchange method of separating tantalum from columbium is also described .

Jan 1, 1964

By R. L. Hopkins, H. T. Rall

A continuous method has been developed for preparing thiolacetic acid . Acetic anhydride and hydrogen sulfide are passed concurrently over an amine ion- exchange resin , under 20 - psi pressure . The thiolacetic acid , a product of the reaction , is flashed continuously from the crude reaction mixture and is purified by fractional distillation . The yield of thiolacetic acid is in excess of 80 percent based on the acetic anhydride charged . INTRODUCTION In the synthesis of reference compounds needed in the identification of sulfur compounds in petroleum , thiolacetic acid has become an important reagent because of its use in the synthesis of thiols by addition to appropriate olefins : R - CH = CH₂ + CH3 - COSH R- CH2 - CH2 - S - COCH R - CH2 - CH₂ - SH + CH3COONa NaOH (1 ) The commonly used procedures for its preparation , as described by Clark and Hartman (1 )4 and by Ellingboe (2 ) , are based on the batchwise reaction of acetic anhydride with hydrogen sulfide :

Jan 1, 1964

By Earl L. Phillips

The Bureau of Mines conducted laboratory tests on samples of pozzolaniccement concrete to develop a low- strength backfill . Results show that support costs can be lowered by replacing a portion of the portland cement in mine backfill with pozzolan ( fly ash ) and lime . Unconfined compression tests on various ratios of fly ash to cement in 84 samples produced compressivestrength curves that can be used to estimate the best backfill mix for any mine .

Jan 1, 1964

By James M. Nishi, Lloyd Carpenter

Sixteen elements were determined spectrochemically in the general range of 3 to 1,000 ppm in high - purity columbium . Samples were converted thermally to Cb2 O , mixed with graphite and Ge02 , and excited for 15 seconds using a 15 - ampere dc arc . For the molybdenum determination , the oxidized samples were mixed with NaCl and Geo₂ and excited for 30 seconds . Spectra were recorded on photographic plates , and spectral line transmittance values were measured photometrically . Relative - intensity ratios of selected analytical and internal standard spectral lines were plotted against concentrations of standards to form curves from which concentrations of impurities were read . Average precision of the method was 11.2 percent relative standard deviation .

Jan 1, 1964

By M. E. Kundick, W. E. Dieter, L. Cohen

The major details of design and maintenance of a seamless stainless steel fume hood system , developed by the Bureau of Mines , are described and illustrated . Operating and housekeeping routines are outlined .

Jan 1, 1964

By A. Gene Collins, Cynthia A. Pearson, Cathy J. Waters

The chemistry of selenium and tellurium is discussed , along with a method of preparing a synthetic oilfield brine , an oilfield brine sampling method , and methods for determining selenium and tellurium in complex oilfield brines . Selenium either can be reduced to the elemental form with sulfur dioxide and determined semiquantitatively by color comparison of the red amorphous form or can be converted to selenite and determined quantitatively by reacting it with 3,3 ' - diaminobenzidine and obtaining its spectral absorbance at 420 mu . Tellurium can be reduced to the elemental form with hypophosphorous acid , and the spectral absorbance of its red hydrosol can be measured at 400 mu . Less than 0.05 mg / 1 of selenium and 0.1 mg / 1 of tellurium can be determined by the described methods .

Jan 1, 1964

By Alla D. Mah

The energies of combustion of zirconium carbide and hafnium carbide were measured by combustion calorimetry and the heats of combustion and formation. of zirconium carbide and hafnium carbide were derived . The results are-- ZrC AH298.15 ( combustion) = -308.60 ± 0.55 kcal /mole , AH298.15 ( formation) -47.0 ± 0.6 kcal /mole , AH298.15 = HfC (combustion ) = -306.08 ± 0.20 kcal/mole , AH298.15 ( formation) -52.3 ± 0.4 kcal /mole . = INTRODUCTION This report contains the results of calorimetric measurements to obtain the heats of formation of zirconium carbide ( ZrC) and hafnium carbide ( HfC) . The work was conducted as part of a Bureau of Mines program for determining the heats of formation of oxides , carbides , and nitrides by combustion calorimetry . Combustion calorimetry is one of the most precise calorimetric techniques . The chief obstacle to obtaining accurate heat of formation values for carbides , and the chief reason for the variation in the results of different investigators , is the lack of purity of the carbide samples . Corrections for impurities always involve assumptions which lead to uncertainties . In general , a large impurity correction is accompanied by a large uncertainty in the final result .

Jan 1, 1964

By V. E. Edlund

This report presents the results obtained in a study of the technical feasibility of recovering a usable pig iron by pyrometallurgical treatment of typical copper reverberatory slags . The iron in the slag was readily reduced with carbon , but the copper and sulfur content of the metal was best controlled by a three - stage procedure comprising ( 1 ) melting the slag with pyrite to remove copper as a low- grade matte , ( 2 ) smelting the partly decopperized slag with fluxes and carbon to reduce the iron , and ( 3 ) refining the impure iron alloy from step 2 with a flush slag to remove sulfur and residual copper . Laboratory - scale tests demonstrated that washing with 8 wt pct of pyrite lowered the copper content of a typical reverberatory slag from 0.58 to 0.12 Subsequent smelting of a mixture composed of 70 pct decopperized slag , 25 pct lime , and 5 pct coke reduced 84 pct of the iron to metal containing 2.27 pct sulfur . This metal then was successfully desulfurized by treatment with a basic flush slag to produce a finished metal that contained , in percent , 93.5 Fe , 0.02 S , 0.26 Cu , and 4.9 C. Overall recovery of iron under the conditions of trial was about 80 pct . This could be increased if higher tolerances for copper could be accepted . Commercial processing would be accomplished in three furnaces with molten materials passing from one to another . Currently produced smelter slag could be treated fairly inexpensively , because the molten product would require only a little additional heat to produce an iron byproduct that undoubtedly would be attractive to local foundries .

Jan 1, 1964

By Oliver C. Fursman, Lloyd H. Banning

This research was undertaken to determine the feasibility of producing steel from hydrogen - reduced , pyrophoric iron powder . Before steelmaking tests were begun , investigations were made to develop procedures for handling the pyrophoric powder safely , and melting tests were made in a single - phase , electric - arc furnace to determine inert gas requirements for preventing powder oxidation . Steelmaking tests were conducted in a conventional electric - arc furnace , usually by a two - slag basic procedure . Results of the research indicated that ( 1 ) pyrophoric powder can be handled safely and can be prevented from oxidizing excessively during charging and melting in electric - arc steelmaking furnaces ; ( 2 ) little , if any , more electrical energy is required for melting Cerro Bolivar iron powder per unit of contained iron than is required for melting heavy melting scrap ; ( 3 ) high - quality steel can be produced readily from high- grade iron powder , having recoveries up to 95 percent of the total iron ; ( 4 ) steel can be produced from simulated titaniferous , chromiferous , and manganiferous iron powders ; and ( 5 ) the electrical energy required for melting increases with increase in the proportion of slag - forming constituents in the furnace charge .

Jan 1, 1964

By D. J. Bauer, V. E. Shaw

Bastnasite concentrate was processed to recover total rare - earth content and obtain high - purity ceric nitrate . Reaction of the concentrate with 45 percent caustic soda for 1 hour at 180 ° C in stainless steel vessels resulted in 99 - percent conversion to rare - earth hydroxides . A drying step followed by solution in nitric acid produced a tetravalent cerium fraction amenable to extraction with TBP . Single- stage separatory funnel experiments resulted in 90 -percent recovery of ceric nitrate at a purity of 99.9 percent . Fractional extraction in pressure - bubbler columns resulted in 98.5 - percent recovery of 99.5 -percent - pure ceric nitrate .

Jan 1, 1964

By H. R. Babitzke, H. Kato, M. D. Carver

A number of columbium and tantalum alloys were investigated to determine their suitability for use at elevated temperatures . Columbium-vanadium , tantalum-vanadium , and tantalum-hafnium alloys , and also columbium- 10 wt pct titanium alloys modified with additions of 0.1 to 2 mole pct ZrO2 , TiO2 , ZrB₂ , TiB , ZrC, or TiC were prepared and examined . Workability , tensile properties , and oxidation resistance were tested . Of the columbium alloys studied , the columbium- 12 at . pct vanadium exhibited the best properties ; it compared closely with the columbium- 10 at . pct vanadium alloy studied in a previous investigation.

Jan 1, 1964

By Michael G. Zabetakis, Aldo L. Furno, George H. Martindill

Hydrazine vapor is flammable in the absence of air at elevated temperatures and atmospheric pressure . The minimum concentrations of benzene , toluene , m- xylene , cumene , and n- heptane needed to inhibit flame propagation through vapor mixtures of hydrazine and hydrocarbon were determined at 125 ° C and atmospheric pressure . These concentrations can be correlated with either the heat of formation or the heat capacity of the hydrocarbon .

Jan 1, 1964

By Albert W. Deurbrouck

This report describes the preparation characteristics of the Pittsburgh and Upper Freeport coalbeds in Hancock , Brooke , Ohio , and Marshall Counties , W. Va . Over 4.5 million tons of coal was produced in these four counties in 1962. Most of this production came from the Pittsburgh coalbed . Twelve coal samples were collected for this study , 11 from the Pittsburgh bed and 1 from the Lower Freeport bed . Two of these samples could be upgraded to produce metallurgical - grade coal . The sulfur content of the Pittsburgh- bed coals was generally excessive --as high as 4.9 percent in the raw coal and 3.19 percent in the float 1.30 specific gravity fraction . The rank of the coals in this area ranges from high-volatile A to high-volatile B bituminous .

Jan 1, 1964

By Oliver Q. Leone

Three electrorefining cells were designed to investigate various factors associated with the electrorefining of reject - grade titanium sponge . Operation of the cells provided information on cell design as well as on how design and operating variables affected the quality of the titanium product . A sodium chloride - titanium chloride electrolyte was used , and the electrolyte chambers had capacities ranging from 400 to 3,500 pounds of molten salt . Major factors investigated were electrolyte composition , temperature and useful life , effect of various cathode shapes and materials of construction , methods for removing cathode deposits , effect of current density and cell potential , and the mechanics of deposit growth and crystal morphology . One of the cells was in intermittent operation over a 4 - year period and produced 2 tons of refined titanium . A product with a hardness of 80 or less Bhn (Brinell hardness number ) was consistently and easily obtained . Some metal with a hardness of less than 60 Bhn was produced . In one of the cells in which the electrolyte was held at operating temperature with an internal heater an ac input of 25 kw maintained 3,500 pounds of electrolyte at 850 ° C , but with an external heater 35 kw was required to maintain 400 pounds at 850° C.

Jan 1, 1964

By F. E. Block, Robert R. Brown, A. W. Henderson

The chlorination of Cr₂ 03 (chromic oxide ) in the presence of carbon with CC14 (carbon tetrachloride ) and COCl2 (phosgene ) chlorinating agents was investigated by employing the radioactive tracer carbon By tagging carbon mixed with Cr₂ 0з , the chlorination reaction was evaluated in terms of the competitive reaction of the elemental carbon and the carbon contained by the chlorinating agent . A unique gas - analysis train was used to separate the chlorination product gases ; CO , CO₂ , and COC12 . The C¹ activity of the gases was determined and used to calculate the reactivity of each source of carbon . Reactivities were determined for the temperature range from 600 ° to 900 ° C. The results of the investigation show that each source of carbon reacts significantly with the Cr2 03 and that the reactivity of each form of carbon depends on the reaction temperature , and each form is independent of the other . Radioisotope and gas - analysis techniques are discussed and a description of the experimental apparatus is given .

Jan 1, 1964

By Robert M. Becker

This report (the second in a series of five) presents the mathematical development in extending the theory of sample reliability from a sample consisting of a fixed number of items to a sample consisting of a fixed amount of items. Examples of a fixed amount of items per sample are samples consisting of a fixed weight or a fixed volume of unequal size particles. The probability distribution functions (those here called the compound binomial and compound multinomial functions) are developed from fundamentals. Their distributions are generalized to include some measured characteristic of the items. Infinite population moments are derived from moment-generating functions, while finite population moments are developed from corresponding infinite population moments using the finite probability operator defined in part 1 of this series.

Jan 1, 1964

By H. R. Babitzke, H. Kato, R. E. Siemens, G. Asai

The purpose of this investigation was to develop a wide variety of columbium and tantalum alloys and to determine their suitability for use at elevated temperatures . Sixty - nine columbium and tantalum alloys were investigated . For this study , columbium was alloyed with two or more of the following : nium, tungsten , vanadium , titanium, and zirconium . Tantalum was alloyed with vanadium or hafnium, or hafnium and carbon . The fabricability was determined by an arbitrary procedure . Hardness measurements , elevated - temperature tensile properties , and oxidation- resistance studies were made . Of the alloys studied , Cb - 15 Hf - 5W, Cb - 15Hf - 5W- 10Ti , Cb - 15Hf - 10W- 10Ti , Cb - 10V - 5W, Ta - 30V , and Ta - 20 to 33Hf exhibited excellent high - temperature properties . These alloys were not only easy to fabricate , but they also had good oxidation resistance and excellent high- temperature strength .

Jan 1, 1964