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By James W. Ballard, H. H. Schrenk

"The X-ray method of quantitative determination is advantageous because it permits determination of compounds rather -than ions or elements; for example, the direct determination of quartz in silicates,4/,5/,6/ The method also takes into account the finest particles of a sample, which may be lost in wet chemical methods because of solubility or in petrographic methods because of limitation of the microscope. The sample is usually reduced to a powder and is easily prepared,7/ only a few milligrams of material being necessary. The sample and its chemical composition are not destroyed and may be used for further analysis by X-ray diffraction or by other methods.This paper presents in detail some of the more essential problems that arise in the application of X-ray diffraction to quantitative chemical analysis, Photometric measurements are discussed in connection with line intensities and the choice of X-ray film. The internal standard method, successfully used in spectrographic analysis, is applied.Copper K-alpha X-rays from a demountable research-type X-ray tube were used with a camera of 20 centimeters radius with a cast-lead-slit collimating system. A combination of a tilted wedge and a lead-slit collimating system permitted irradiation of a large amount of sample with X-rays. This tended to minimize errors due to possible inhonogeneity of the sample, to decrease the time of exposure, and to keep the lines on the X-ray film to a minimum width. There was sufficient dispersion of the lines for satisfactory analysis of most samples. Power was furnished the tube by a. source of constant high potential consisting of a synchronous motor generator furnishing 500-cycle power to a 100-kv. transformer, rectifying valves, and a condenser filter circuit. The X-ray tube was operated as a gas-type tube at 35 kv, and 20 ma,, the exposure times varying from 1 to 2 hours. The constant output of X-rays from the tube, indicated bar an exposure meter built for the purpose, was satisfactory.The recording microphotometer8/has been described. It was found preferable to a nonrecording instrument for measuring blackening of lines above a background on X-ray films. This background, which usually occurs, is sometimes complicated by numerous peaks from lines of complex diffraction patterns. is microphotometer record of the pattern, therefore, facilitates the location of the background 'and the measurement of the heights of the peaks and thus contributes to the accuracy of a determination."

Jun 1, 1946

By H. E. Powell

This Bureau of Mines study describes two processes for recovering zinc, copper, silver, and iron from the magnetic fraction of a waste generated by the primary smelting of zinc in horizontal retort distillation furnaces. The laboratory-scale procedures include reduction melting to produce a high-copper iron and matte smelting to produce a copper-silver-iron matte and metallic iron. Zinc is fumed in each process and recovered as the oxide. Direct reduction melting yields a metallic iron high in copper and a small rich matte from the sulfur contained in the waste. The products of the second process are a matte containing essentially all of the silver, about 80 pct of the copper and 37 pet of the iron, and an iron-copper alloy containing all of the remaining copper. Extraction with metallic lead or sodium sulfate recovers essentially all of the copper from the molten high-copper iron and yields an acceptable foundry iron.

Jan 1, 1973

By C. C. Clark

This report presents the results of tests conducted by the U.S. Bureau of Mines to determine the transport characteristics of highly concentrated paste backfill mixes made from dewatered total mine tailings. The slurry concentrations of the mixes were all above 78 pct by weight with slumps ranging from 6.4 to 16.5 cm (2.5 to 6.5 in). Laboratory material property tests and full-scale pumping tests were conducted using pipe diameters of 102, 128, and 154 mm (4, 5, and 6 in) and a positive-displacement pump. The results indicated that the tested backfill mixes can be successfully transported as a stiff paste and identified the influence of and the interaction among the various mix and system variables.

Jan 1, 2010

By F. W. Smith

This paper is based largely on a study of experimental data obtained by the Bureau of Mines in its comprehensive 25-year survey of the carbonizing properties of American coals. Although the Bureau was interested in and conducted carbonization research-from time to time ever since it was organized in 1910 (1),4/ no systematic studies of the coke-, gas-, and byproduct-making properties of American coals were undertaken until 1927, when the American Gas Association appointed an advisory committee (2) to cooperate with the Bureau in developing equipment and techniques to obtain-data for the accurate assessment of the behavior of coals on carbonization. It was found, in general, that small-scale laboratory tests were unsuitable for the complete evaluation of the coking properties of coal; hence, larger pilot-plant-scale equipment was designed and used (3). It was decided that the scale of the test should be large enough to determine both the yield and quality of the products and yet small enough to maintain adequate control of the process variables (4). These considerations led to development of a carbonizing retort and furnace-of 80 to 200 pounds of coal capacity, suitable for operation at various temperatures up to 1,100° C. (2,0120 F.) and equipment for recovery and measurement of gas and byproducts. This apparatus and the standardized procedure for its operation became known as the Bureau of Mines-American Gas Association (EM-AGA) method or retort (5).

Jan 1, 1955

By D. W. Bridges, Donald R. Peterson, Masami Hayashi

Techniques are described for recovering about 80 pct of the cobalt and nickel contained in superalloy scrap by anodic dissolution of the scrap and simultaneous electrodeposition of a pure cobalt - nickel alloy at the cathodes in an electrolytic cell partitioned by permeable diaphragms into separate anode and cathode compartments . Superalloy scrap was alternatively prepared for subsequent anodic dissolution either by melting and casting massive scrap into suitably sized anodes , by packing moderate - sized discard scrap in inert metal baskets that subsequently served as anodes , or after concentrating the superalloy portion of grinding debris , by magnetic separation to reject corundum or other abrasives , slagging any remaining abrasives from molten grindings , and finally casting the superalloy metal into anodes . In the processing , purified electrolyte -- 1 N in NiSO4 and in NiCl₂ , and 0.1 N in CoSO4 and in CoCl2 --was charged to the cathode compartments and discharged from the anode compartments at a rate sufficient to overcome the backward migration of ionic impurities from the anodes to the cathodes . Discharged electrolyte was purified by reacting it first with SO2 and next with limestone , and then recirculated to the cathode compartments , in which a 50 pct cobalt - 50 pct nickel alloy was deposited on either blanks of stainless steel or starting sheets of cobalt - nickel alloy . The process was made self - sustaining by either adding H2SO4 to the catholyte feed to throttle the rate of cobalt - nickel deposition , thereby compensating for the slower rate of cobalt - nickel dissolution from the anode and losses occurring in electrolyte purification , or alternatively , adding H₂SO4 to

Jan 1, 1964

By G. St. J. Perrott, N. A. Tolch

"PURPOSE OF TESTSThe propulsive strength4 developed by the Cardox blasting device depends on the thickness of disk, weight of heater element, and weight of carbon dioxide charge. It might be supposed that the maximum weight of carbon dioxide that can be charged into the shell should give the greatest strength. However, according to the ballistic pendulum, the maximum weight of carbon dioxide with certain conditions of heater and disk has less propulsive strength than a smaller charge; in one condition of test a loss of 39 per cent in propulsive strength was noted. It is therefore of interest to study the effect of the variables that determine the strength of Cardox.ACKNOWLEDGMENTGrateful acknowledgment is made to A. B. Coates, associate mechanical engineer who developed the testing method for measuring pressures in the Cardox shell.DESCRIPTION OF DEVICEThe Cardox blasting device as fully described by the bureau in Report of Investiga¬tions 2920 (1929), consists essentially of hollow—steel shell, cylindrical in shape, an electrode, valve assembly, shearing disk, and discharge cap. The shell is prepared for use by inserting a heater element, closing the open end with a shearing disk, and screwing in place the discharge cap. The charge of carbon dioxide enters the shell through the electrode.The heater element is fired by an electric igniter of the match—head type. The heat released by the heater element completely gasifies the carbon dioxide and raises the pressure of the gas until it is enough to shear the disk."

Apr 1, 1931

By John E. Miller

A high accuracy Burnett apparatus for use at 12,000 psi and 0° to 65° C has been constructed at the Bureau of Mines Helium Research Center. The apparatus is patterned after Burnett's original apparatus, but the working pressure is much higher and elastic distortion can be essentially eliminated. An operating procedure to permit faster experimental measurements is suggested.

Jan 1, 1967

By J. R. Koehler

The U.S. Bureau of Mines (USBM) ground control research program includes several projects focused on developing design criteria for yielding-pillar-based longwall gate road systems. As part of this program, mining practices at the Sunnyside Mines, Sunnyside Reclamation and Salvage Co., Sunnyside, UT, are being documented to preserve the long history of yield pillar system evolution on the property. Published information describing the specific in-mine performance of the numerous gate road configurations utilized at the Sunnyside Mines is very limited. To overcome this deficit, USBM personnel interviewed 30 longtime mine employees representing nearly 700 years of mining experience at the Sunnyside operations. Mining conditions in 12 specific areas in the Nos. 1, 2, and 3 Mines were discussed in the interviews. Also, broad topics such as general mining practices, safety, and geology were often addressed during the discussions. Comprising the body of this report is an extensive record of the events and conditions experienced while mining the identified areas. In addition, eight significant conclusions were developed that accurately summarize the general opinions of the interviewed personnel regarding mining conditions and practices at Sunnyside.

Jan 1, 1994

By T. F. Anstett

The Bureau of Mines estimated the potential availability of rare-earth oxides (EtEO), including yttrium, and thorium, which is also contained in the rare-earth bearing minerals monazite and bastnasite, from 38 'properties in market economy countries (MEC's). Only nine of the properties evaluated produce or would produce REO as the primary product; the others contain REO as a byproduct, chiefly from mineral sands operations recovering rutile, ilmenite, and zircon. Nearly 77% (2,578,000 mt) of the total 3,355,000 mt of recoverable RE0 evaluated is from producing properties. It is estimated that 21% (705,000 mt) of this total is from properties that could not realize a positive rate of return at the January 1984 market prices for the recovered commodities. At production capacities assumed for this evaluation, the amount of RE0 potentially available from producers ranges from an estimated 46,500 mt in 1986, to a peak of 50,900 mt in 1992, to 49,900 mt by the year 2000. Total MEG production in 1984 was estimated at 40,700 mt. Assuming demand does not increase sharply, producing properties can continue to fulfill overall REO demand through at least the end of this century.

Jan 1, 1986

By John M. Gomes

A two-phase molten halide-silicate technique for extracting tungstic oxide (WO3) from scheelite (CaW04) and wolframite [(Fe, Mn)W04] was investigated. The halide phase extracted over 99 percent of the was, whereas the lower silicate phase retained about 90 percent of the calcium, iron, or manganese oxides. The most efficient extraction and separation of tungsten from scheelite was accomplished at 1,080° C in a molten system containing, in mole-percent, 9 calcium tungstate (CaW04), 42 sodium chloride (NaCl), 28 sodium fluoride (NaF), 17 sodium metasilicate (Na2SiO3), and 4 alumina (Al2O3). Wolframite was also treated at 1,0800°C; the molten system contained, in mole-percent, 11 (Fe, Mn)W04, 74 NaCl, and 15 Na2 SiO3.

Jan 1, 1968

By John C. Machisak

Employment and related injury experience of the coking industry in the United States for 1957 contained in this publication is summarized under three general sections: (A) General injury experience: Tables 1 to 9: Current and comparable statistics on operating data, number, frequency, and degree of severity of injuries and major accident agencies involved in the cause of Injuries. Data are presented for the industry as a whole, for each type of oven, and for the States in which coke was produced.

Jan 1, 1959

By Stephenson. E. L.

"INTRODUCTION In the spring of 1942 a series of magnetometer surveys on deposits of black sand underlying Pleistocene raised marine terraces along the coast of southwestern Oregon was nada by the Division of Geophysical Exploration of the Federal Bureau of Mines in cooperation with the Oregon Department of Geology and Mineral Industries. A few preliminary tests had been made in the same area in May 1940 and December 1941.The sands contain fine gold and metals of the platinum group, and, beginning in 1852, extensive, but spasmodic mining and exploration have been done for these precious metals. There are many old placer, mines and prospects, although for the most part the yield of the metals has been small. The sands also contain other minerals of potential value, including ilmenite, magnetite, garnet, zircon, and particularly chromite, and the wartime demand for domestic chromite resulted in extensive testing and development of the known deposits. The purpose of the magnetometer surveys was to determine the efficacy of, magnetic methods in tracing and outlining these known deposits and in prospecting for new ones. The field work was done between March 17 and May 29, 1942, by the author assisted by W.W. Paulsen of the Oregon Department of Geology and Mineral Industries."

Jun 1, 1945

By T. E. Gray

This report describes preparation characteristics of the significant coalbeds in Marion County, W. Va., as determined by the Bureau of Mines. It is one in a series telling what coals are suitable for producing metallurgical coke, either as mined or after beneficiation. Over 9.4 million tons of coal was produced in Marion County, W. Va., in 1958, of which almost 6 million tons was cleaned mechanically in nine cleaning plants. All of the coal mechanically cleaned came from the Pittsburgh bed. The Bureau of Mines estimated that 1,578 million tons of recoverable coal remained in the county in beds 28 inches or more thick as of January 1, 1955.

Jan 1, 1960

By H. R. Beard

The Bureau of Mines investigated the absorption of radium and thorium from waste uranium leach liquor by clays and other materials. This work was conducted in support of the Bureau's goal of minimizing the environmental conflicts, impacts, and occupational hazards associated with mining and milling operations. Tailing and soil samples from New Mexico were evaluated for their potential to absorb radium and thorium from tailing liquors. Absorption ranged from 0 to 97 pct for radium and 0 to 60 pct for thorium. Some samples that readily absorbed radium were contacted with various salt solutions that could be present in tailing solutions to determine whether desorption would be a potential problem. The desorption of radium ranged from 0 to 75 pct. An alpha spectrometric method was used to determine the radium and thorium concentrations in the solutions and solids.

Jan 1, 1980

USBM Contract H0133045 consists of the design, build and test of 50 waveform generators. The waveform generator is a small ULF transmitter operating in the 1 to 3 KHz frequency range for the purpose of locating trapped miners during a mine disaster. This contract provided for the design, test, and building of 50 waveform generators using a discrete component construction with an option of using hybrid construction techniques within 105 days after the effective date of the contract. Because of large quantity economic considerations, this option was not initiated. Two engineering models were designed, constructed and tested and 50 final production units were fabricated using discrete construction. Complete documentation is supplied under a separate package which includes final schematics, parts list, layout information, equipment specification, production test procedures and qualification test procedures. Ten units have been delivered to the USBM. The remaining 40 units are being retained for packaging under contract H0242010 Transmitter Package and Receivers. A great deal of experience has been gained as a result of this contract. A final discrete potted printed circuit configuration has been arrived at that is now ready for field testing. After field testing, any desired changes should be incorporated into a final design. However, as a result of the current experience gained building and testing the production units, this printed circuit package together with potting procedure could be improved to reduce future costs. For example, the printed circuit board could be increased in size by 0.125 to 0.2 inches and all components could be mounted directly to the board eliminating costly hand stacking of components. The new printed

By Warren M. Mahan

A rotary kiln process was developed by the Federal Bureau of Mines to produce consistently an iron product containing 3 to 7 percent nickel. Cuban laterite and serpentine ores were smelted in a gas-fired batch-rotary kiln) 5 feet in diameter and 9 feet long. The metal contained 2 to 4 percent carbon, with little or no silicon, and could be produced on a large scale with modest capital investment. A total of 121 tests was run using this procedure. The tests were conducted with a maximum temperature of 2,625° F., using linings of firebrick containing 40 to 70 percent alumina. Slags in the kiln were acid to neutral. The material in each batch passed through three stages: (1) Sponge metal, (2) carburization, and (3) balling and meltdown. Half the tests were made while firing the kiln with atmospheric-temperature air; the remainder were fired with preheated air. Tests showed that preheated air decreased fuel requirements, dust losses, and reducing agent, and increased the capacity of the kiln.

Jan 1, 1960

By John C. Machisak

The National Safety Competition is sponsored and conducted annually by the Bureau of Mines, U.S. Department of the Interior, to give greater impetus to the building of programs safeguarding the employees of the mineral industries from disabling work injuries. The results of the 1960 National Safety Competition are presented in this publication. Mines and quarries that were awarded the Sentinels of Safety trophy for the best safety record in their competitive group and those mineral operations that ranked second, third, fourth, and fifth in the competition are listed with a summary of their achievements in preventing disabling work injuries. In addition, this publication presents statistical data on disabling work-injury experience in all other mines and quarries participating in the annual competitions.

Jan 1, 1962

By L. A. Haas

The U.S. Department of the Interior, Bureau of Mines, is conducting laboratory-scale research to determine the leaching conditions required with sulfuric acid for extracting base metal from a matte with a copper-to-nicke1 ratio of 6 to 1. The matte (61.2 pct Cu, 9.7 pct Ni, 3.3 pct Fe, 21 pct S, and about 5 oz of precious metals per ton) was prepared from Duluth Complex (Minnesota) ore by smelting a bulk sulfide flotation concentrate. The matte was pre leached at atmospheric pressure to selectively extract 20 pct of the nickel, and the undissolved solids were referred to as the matte residue. Autoclave leaching of the matte residue extracted over 95 pct of the nickel, copper, and iron. The remaining leach residue in the autoclave contained over 100 oz of precious metals per ton. The leaching conditions required were matte grind of greater than 98 pct minus 325 mesh, pulp concentration of 50 g/1, total pressure of 100 psig with oxygen at 150° C or 400 psig with air at 180° C, 50 g/1 H2S04, 700 rpm agitator speed, and 6 hours of leaching time. The leaching time was decreased to 2 hours by increasing the agitator speed to 1,300 rpm. Sulfuric acid concentration greater than 50 g/1 did not appreciably enhance the base metal extraction, but with less acid, residues with higher iron concentrations were obtained. Supersaturation of the liquor was prevented at 150° C by using a 1ixiviant that contained 30 g/l Ni and 20 g/1 Cu.

Jan 1, 1979

By A. L. Engel

This investigation was undertaken to assess the feasibility of processing an extensive deposit of iron ore near Palisades, Eureka County, Nev., previously penalized for high phosphorus content. The experiments described indicate a satisfactory accomplishment of objective. Chemical treatment will permit a high-phosphorus iron ore to be used. Leaching with acid solution effectively lowers the phosphorus content with a [gligible] loss of iron. The use of hydrochloric acid is preferred because [ ] does not contaminate the ore and the cost is lower. Minus-1/2-inch ore was satisfactorily leached in 24 hours, minus-1/4-inch ore, in 8 hours, and minus-10-mesh ore, in 3 hours. About 40 pounds of acid per ton of ore was consumed in each instance.

Jan 1, 1959

By J. Bruce Clemmer, M. F. Williams, B. H. Clemmons, Carl Rampacek, R. H. Stacy

"INTRODUCTION This report is the first of several dealing with the application of flotation methods for beneficiating the calcareous and siliceous red iron ores and ferruginous sandstones of the Birmingham district. The flotation study was part of a general investigation of the concentratability of various iron ores of Alabama and other Southeastern States undertaken by the Southern Experiment Station of the Bureau of Mines, United States Department of the Interior, in cooperation with the University of Alabama, Tuscaloosa, Ala.Batch testing and pilot-plant flotation testing of the calcareous red ores of the Birmingham district have been in progress for several years, and although some phases of the study are not yet completed, enough data are available to indicate that many of the ores will yield marketable-grade concentrates with good recovery.The first flotation tests on the calcareous red ores employing conventional methods either the iron oxides or the siliceous gangue materials failed to give the desired results. The inferior separations obtained or prohibitive reagent requirements made the methods unattractive. Other more effective flotation methods were sought. A laboratory study of various reagents was undertaken. It resulted in the development of two attractive methods embracing anionic flotation of the activated siliceous gangue from the retarded iron oxides. The methods were similar in that fatty acid or soap-collecting agents were employed in strongly alkaline pulps to float the naturally activated quartz from the iron-ore pulps. The methods differed, however, in the addition agent employed to retard the hematite or hematite and calcite. By proper choice and quantity of the addition agent, the calcite could be floated with the quartz or retarded with the hematite as desired. Ability to recover or reject the calcite gives added flexibility to the separation. Although the methods have their limitations and cannot be considered ""cure-alls,"" they have given encouraging results on a number of calcareous red ores that heretofore proved difficult to concentrate by conventional flotation procedures."

Mar 1, 1945