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By L. H. Adami

The heats of formation of anhydrous cadmium sulfate, cobalt sulfate, copper sulfate, nickel sulfate, and zinc sulfate were determined by hydrochloric acid solution calorimetry. The values at 298.15° K for formation from the metal, rhombic sulfur, and oxygen gas follow (cal/mole): CdS04J -222.0 ± 0.3; CoS04, -212.0 ± 0.4; CuS04) -183.4 ± 0.6; NiS04, -208.1 ± 0.2; and ZnS04, -233.1 ± 0.2. Corresponding heats of decomposition to form the metal oxide, sulfur dioxide, and oxygen were derived from these results; heats of decomposition to form the metal oxide and sulfur trioxide were also derived.

Jan 1, 1965

By R. Barany

The heats of formation of goethite, ferrous vanadate, and manganese molybdate at 298.15° K were determined by solution calorimetry. For formation from the elements, the heat values were -133.7 ±0.3 kcal/mole for goethite, -453.8 ±0.5 kcal/mole for ferrous vanadate, and -284.8 ±0.2 kcal/mole for manganese molybdate. For formation from the oxides, the heat values were -0.9 ±0.1 kca1/mole for goethite, -19.4 ±0.3 kca1/mole for ferrous vanadate, and -14.6 ±O.l kcal/mole for manganese molybdate.

Jan 1, 1965

By Clark F. Grain

The monoclinic to tetragonal inversion of zirconium dioxide was studied by single-crystal X-ray methods, high-temperature X-ray diffractometry, and differential thermal analysis. The unusual features of the inversion, such as no definite transition Lperature, hysteresis, and athermal kinetics, were confirmed for powders who mean crystallite size was greater than 1,000 A. Samples of mean crystallite size below 1,000 A displayed classical kinetics, obeying a logarithmic rate law. A detailed mechanism based on Ubbelohde's theory of continuous phase transformations was proposed which is consistent with all the experimental facts.

Jan 1, 1965

By J. B. Gayle

The Bureau of Mines studied the effects of air oxidation on the recovery of float coal. Both batch-and continuous-type tests were made on six bituminous coals, representing the range in rank of coals now commercially used for carbonization, and on one anthracite coal. The effects on flotation recovery of oxidation at 1000 C for periods up to 50 days were investigated using an alcohol-type frother and a kerosine-pine oil reagent. Two series of release analysis tests were made, using one medium-volatile bituminous coal. Float coal recovery was adversely affected by oxidation in all tests where the alcohol-type frother was used. Conversely, a small degree of oxidation improved recovery with kerosine-pine oil frother for some of the coals in continuous tests. Prolonged oxidation (beyond about 14 days) adversely affected float coal recovery for all coals, the effect being more pronounced for batch-type tests and for tests using alcohol-type frother. Reagent selectivity for the rejection of both ash forming and sulfur bearing minerals was reduced by oxidation. Severe reduction of reagent selectivity required only about 3 days' oxidation for alcohol-type frother but more than 10 days' oxidation when the kerosene-pine oil reagent was used.

Jan 1, 1965

By T. E. Sterner

The Bureau of Mines investigated the use of a chromatographic gas analyzer in determining the concentration of combustion products in gas produced during field and laboratory thermal oil-recovery tests. Several parameters (carrier-gas flow, cell current, sample size, and temperature) known to affect quantitative analyses were studied using a commercially available dual-column, dual-detector chromatographic gas analyzer which had been modified to provide close control of these variables. The apparatus made possible a much closer control of air-and gas-injection rates and provided adequate data for performing material-balance calculations and for determining oxygen utilization during the laboratory and field combustion tests. The chromatographic analysis also aided materially in evaluating and measuring bypassing and gas travel times and in detecting high-permeability zones that were present in the reservoir.

Jan 1, 1965

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grind-ability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions4 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1965

By M. R. Geer

Samples of coal from six beds in the Roslyn-Cle Elum field of Washington were subjected to float-and-sink tests to determine their amenability to the production of high-ash boiler fuel for on-site power generation. Grindability tests and analyses of ash were made. All of the coals would require some degree of cleaning to insure a product of 25 percent ash. With two of the coals the entire size range would have to be washed. With the other four, it would suffice to clean only the coarse coal and bypass the raw fines.

Jan 1, 1965

By R. E. Campbell

Uranium metal of improved purity was prepared by electrorefining commercial magnesium-reduced uranium in a molten sodium chloride-uranium trichloride electrolyte. The best operating conditions for the preparation of refined metal were established as follows: an electrolyte containing 8.7 to 13.3 weight-percent uranium; initial cathode current densities from 300 to 1,500 amp/sq ft; and a molten salt temperature of 860° C. Ingots produced from electrorefined uranium crystals prepared with these operating conditions were substantially free of metallic impurities. The only impurities in the refined and consolidated metal were present in low or undetectable amounts.

Jan 1, 1965

By B. W. Naugle

The Bureau of Mines investigated the changes that occur in decomposition products when coal is carbonized in a fluidized bed with steam as the fluidizing medium and the vapors are subsequently cracked without condensation in a fluidized bed of high-temperature coke. The coal used was from the High Splint bed, High Splint mine, Harlan County, Ky. Since this coal is agglomerating, it was blended with char. The integrated unit used in this investigation consisted of a 3-inch-diameter fluidized coal carbonizer, a 3.5-inch-diameter cracker containing a bed of high-temperature coke fluidized by the tar vapors and steam from the carbonizer, and gas-cleaning and product-recovery systems. The carbonizer was operated at 485° C and the cracker at 600°, 700°, and 800° C. The process variables investigated were temperature, residence time, and concentration (pound of tar vapors per pound of steam to the cracker) of tar vapors in the cracker. The total tar yields decreased as the temperature of the cracker increased, and at a constant cracker temperature of 600° C the yield of paraffins, acids, aromatics, and olefins in the distillate increased directly with the tar vapor concentration in the cracker. At 700° and 800° C only the acids and aromatics increased with increased concentration. Bases remained essentially constant regardless of the temperature and concentration. Similar results were obtained when the tar from the carbonizer was condensed prior to feeding to the cracker.

Jan 1, 1965

By Jr. Oitto

A polyester-type resin and deformed-steel reinforcing bars (rebars) were used in to strengthen and to stabilize bolted, fractured wall rock along pas 1:'y. in a western gold mine. Reinforcing bars were placed in boreholes drilled into fractured rock and then were surrounded by resin pumped under pressure into the holes and intersecting fractures until the wall rock was thoroughly impregnated. Pumping and injection equipment and infusion procedures are described. Visual examinations for movement in bonded and adjacent unbonded rock were made for 3 years. Fractured walls containing resin-rebar installations were strengthened. The results suggest that resin-rebar support can be used advantageously and economically in repairing fractured or broken rock when compared with rock bolting or timbering.

Jan 1, 1965

By Robert M. Becker

Particle mixtures were sampled in the laboratory, using ordinary sampling procedures, to determine whether or not the compound-multinomial probability distribution and other developments of part 2 agreed with experimental results. The objective was accomplished by the Bureau of Mines by comparing the moments and moment relationships of the appropriate probability models with their corresponding experimental values over a fairly wide range. The overall agreement between the corresponding theoretical and experimental values is both good and complete. The results demonstrate that sampling to a constant amount, such as weight, of items per sample is not the same, in general, as sampling to some constant number of items per sample. The results seem to confirm all the developments of part 2 and the application of the compound-multinomial function to bulk sampling.

Jan 1, 1965

By D. R. Mathews

The solubility of carbon in electrorefined vanadium was determined to be approximately 0.27 wt pct at the eutectic temperature 1,650° C and 0.03 wt pct at 700° C. The tensile strength and hardness of vanadium increased with car-bon content to the solubility limit, but this effect was small, probably because of the narrow solubility range. Between the solubility limit and 0.3 weight-percent carbon, the second phase had essentially no strengthening effect in vanadium. The second phase, observed metallographically at the grain boundaries and within the grains, was shown by autoradiography to contain high-carbon concentrations. This second phase was identified as VgC by X-ray analysis. The VgC in the grain boundaries contributed largely to the poor cold-and-hot workability of vanadium-carbon alloys. Increased concentrations of V2C occurred at the grain boundaries of the high-carbon alloy ingots as a result of homogenization at 1,600° C for 1 hour. Alloy ingots containing more than 0.36 wt pet carbon (a calculated 2.9 wt pct VaC) following homogenization, cracked severely and failed by intergranular fracture upon swaging at 900° C.

Jan 1, 1965

By Joseph Grumer

The range of composition of gases synthesized from solid fuels which are exchangeable with natural gas on current gas appliances was evaluated by theoretical principles. These principles consider primarily the flashback, blowoff, and yellow-tipping characteristics of air-entraining burner flames. It was found that complete identity between the synthetic and natural product is not necessary. Gases such as may be obtained by hydrogasification of coal and other solid fuels without the removal of unreacted hydrogen offer advantages in flame characteristics. Between 25 to 37 percent hydrogen can be tolerated in the sendout gas.

Jan 1, 1965

By G. A. Crowder

Far infrared spectra, most of them in the region 15-200 microns and for both the liquid or solution state and for the vapor state, were obtained for twenty-seven compounds.

Jan 1, 1965

By T. A. Sullivan

High-purity vanadium metal was prepared by electrorefining commercial vanadium in a molten sodium bromide, potassium bromide, and vanadium dibromide electrolyte. Variables investigated were operating temperature, current densities, electrolyte composition, and condition of the anode. The purity of the refined metal was in the range of 99.95 percent vana-dium. Iron and oxygen in the 50- to 250-ppm range were the only major impurities. Metal with hardness numbers of 50 to 60 in the Rockwell F scale was prepared from feed material with a Rockwell B hardness of 90. The arc-melted metal was highly ductile and could be cold-worked into sheet or foil.

Jan 1, 1965

By Jr. Gabler

Methods for the direct spectrochemical determination of impurities at the parts-per-million level in tungsten metal and oxide are presented. Several published procedures were investigated and numerous modifications were made in establishing procedures with improved precision and extended lower levels of determinability. Details of standards preparation are presented, experimental work is described, and three preferred methods are described in detail. A germanium carrier-distillation procedure is applicable to the determination of 13 elements in tungsten powder; a silver chloride carrier-distillation procedure provides for the determination of 24 elements in tungstic oxide, and a sustaining ac arc method is applicable to 26 elements in tungstic oxide. The choice of methods to be used depends upon sample form, elements and concentrations to be determined, and the precision and accuracy required. The investigations reported here were undertaken to develop direct spec-trochemical methods with increased accuracy and precision to determine impurities in high-purity tungsten and tungstic oxide, to define the lower concentration levels of detectability and measurement for the common impurities in tungsten by direct spectrographic means, and to present the details of the developed or modified methods that have proved applicable.

Jan 1, 1965

By T. C. Davis

Nine organic derivatives of fluorine, silicon, boron, and aluminum were purified for thermodynamic studies using distillation, zone melting, and gas liquid chromatography, The unusual properties of these compounds required the development of special techniques for handling and purification. To determine purities of purified samples, new techniques for analyzing spectral data were developed.

Jan 1, 1965

By Richard F. Hewlett

This report describes how a limited number of preliminary exploration drill-hole assays from a mineral deposit can be used to design grid spacing that is both economic and efficient for subsequent evaluation drilling of that deposit. Relationships between desired precision of the estimate of grade of ore and drilling cost are used to determine the economic drill-hole spacing. The statistical concept of precision in estimating grade of ore is used to determine the efficient drill-hole spacing. Assay data from approximately 50 known copper deposits were studied, and the relationships of the statistical parameters of these deposits were computed. Drilling requirements for various precisions of the estimates of grade of ore were computed for some of these known deposits to serve as guides for drilling future copper deposits. The effect of various geologic factors on the trend in grade of ore and, therefore, on the drilling requirements is shown for certain deposits.

Jan 1, 1965

By S. L. May

Tantalum and columbium can be extracted from several of their ores or concentrates by chlorination procedures. Direct chlorination of high-grade minerals in the presence of carbon at temperatures between 500° and 800° C will extract up to 99 percent of the tantalum and columbium. Metallurgical beneficiation of low-grade source materials by carbothermic reduction produces a ferroalloy that is amenable to chlorination at a temperature of 500° C. Over 90 percent of the tantalum and columbium can be recovered.

Jan 1, 1965

By M. Copeland

Phase relations of gadolinium alloyed, up to 40 weight-percent (wt pct), with AISI 304-type stainless steel were established. Body-and face-centered cubic iron-rich solid solution phases and several intermetallic gadolinium-containing compounds of variable composition that approximated the formulas Fe9Gd, Ni7Gd2, Ni3Gd, Fe2Gd, NiGd, and NiGd3 were identified. The intermetallic phases Fe9Gd and Ni7Gd2 were noted to melt at about 1,080° C at about 0 to 2 wt pct gadolinium. The melting temperature of Fe9Gd increased with increas-ing gadolinium content to a plateau at about 1,230°C and 30 wt pct gadolinium, and the melting point of Ni7Gd2 decreased to a plateau at 900° C and 30 wt pct gadolinium where Ni3Gd, NiGd, and Fe2Gd coexist. Body-centered cubic iron solid solution was stable from 1 to 2 wt pct gadolinium to higher contents, 30 wt pct gadolinium or possibly more, and face-centered cubic iron up to 12 wt pct gadolinium below 1,200° C. The stability of these phases above 1,200° C was not resolved except for the mel points. A limited number of fabrication variables as well as mechanical and corrosion properties of alloys containing up to 5 wt pct gadolinium were studied. Equilibrating and forming operations were best conducted at about 940° to 1,080° C. Some variability in the yield and tensile strengths of alloys was noted; however, there was a continual decrease in ductility and impact resistance with increasing gadolinium contents. The resistance of gadolinium alloys to corrosion in water at 354° C was about the same as stainless steel.

Jan 1, 1965