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By Ruth F. Brinkley

This circular describes the activities and publications of the Bureau of Mines, Explosives Research Laboratory4 for the fiscal year 1960 (July 1, 1959 -June 30, 1960). Part 1 describes briefly the principal projects that were active during the report period, and presents some data not scheduled for publication elsewhere in the near future. Certain of the results are only preliminary and should be regarded as tentative, pending the findings of the completed investigation. Publications that appeared during the report period are listed and described briefly in part 2. In general, the research activities reported in these publications antedate fiscal year 1960. The published material relating to activities that are still current is indicated by references in part 1.

Jan 1, 1962

By Clyde L. Brown

The ignition source of fires and explosions in coal mines is sometimes difficult to explain because resulting widespread destruction often erases valuable evidence that might reveal the cause. However, through years of experience, investigators have been able to piece together enough evidence to establish the reasons and, thereby, have been equipped to recommend corrective or preventative measures. The pattern of hazards is not constant. It changes with the development of new practices and new equipment. Important among the new hazards to coal mining are those introduced by electricity. In addition to the dangers of electric shock, fires and explosions from heat and arcs, and premature blasts, certain others have developed as a result of stray electric currents from direct-current traction systems. The conventional direct-current power-distribution system in coal mines is conducive to electrolysis damage to mine tracks, metallic pipelines, grounded power conductors, and structures in a position to become conductors of stray currents. The voltage drop resulting from power demand on intentionally grounded power conductors and accidental grounds on insulated conductors are common sources of stray currents in coal mines. Uncontrolled electric cur-rents flowing through the earth and metallic structures can be a menace, and these contribute to the estimated $6,000,000,000 annual loss caused by corrosion. The purpose of this publication is to discuss some of the electrolysis hazards in the coal-mining industry and to outline corrective measures to alleviate them.

Jan 1, 1962

By Frank A. Peters

This Bureau of Mines report is the second of a series of process evaluations planned to determine the relative processing costs of producing metallurgical-grade alumina from low-grade aluminous materials. Included in these evaluations are recommendations for additional research and development to improve the processes and to lower their costs. The design for each process is based on published work. The processes considered in this report are designed to extract alumina as aluminum chloride from calcined clay with 20 percent hydrochloric acid and to remove the silica residue by filtration. Iron is removed by one of the following processes: Isopropyl ether extraction, in which iron chloride is extracted before decomposing the aluminum chloride; gas precipitation, in which the aluminum chloride is precipitated with hydrogen chloride while leaving the iron chloride in solution; gas precipitation-isopropyl ether extraction, in which the aluminum chloride from precipitation is extracted with isopropyl ether, if necessary; caustic purification, in which a crude alumina is produced and then purified by a modified Bayer operation; or sinter purification, in which a crude alumina is produced and then purified by a lime-soda sinter operation. For plants producing 1,000 tons of alumina a day the estimated operating costs per ton of alumina are: [Isopropyl ether extraction process $ 65.09 Gas precipitation process 89.04 Gas precipitation-isopropyl ether extraction process 119.65 Caustic purification process 73.79 Sinter purification process 80.47] The estimated fixed capital costs per annual ton for these plants on a Marshall and Stevens chemical equipment basis of 240.0 are: [Isopropyl ether extraction process $229.03 Gas precipitation process 287.16 Gas precipitation-isopropyl ether extraction process 356.59 Caustic purification process 266.48 Sinter purification process 279.13]

Jan 1, 1962

By Hsun Hu, R. S. Cline

A detailed studj) of texture formation in 2 pet Al-Fe single crystals with initial orientations of approximately (111) [112], (112) [111], and (112) [111] was made by examining the textures developed on the surface and at various interior sections of the crystal after rolling to various amounts. Depending' upon the initial orientation of the crystal, the surface and interior textures may differ only in sharpness, or may differ essentially in orientation. The orientation of the (111) [112] crystal does not change upon rolling up to 70 pet, but after rolling more than 90 pet a distinct component of (001) (110] orientation is developed. The texture formed in the two (112) (1111 type crystals consists of (111) (1121 and (001) (1101 components. The latter, however, is largely confined to the surface layers. The textures formed on both sides of the crystal are identical, and the texture composition profile is approximately symmetrical with respect to the central section of the strip thickness. The formation of these texture components is analyzed. DURING the past seven or eight years, deformation and recrystallization textures in rolled Si-Fe single crystals have been extensively studied by various investigators.1-7 From these studies, much knowledge on texture formation in bee crystals of various initial orientations was obtained. However, these results also raised many questions, regarding particularly the correlation between deformation and recrystallization textures, as well as the deformation texture itself of some particular crystals. To take a (111) [112] type crystal as an example, it was shown by Dunn and Koh2, 3 that this orientation does not change during deformation by rolling. This finding is consistent with the conclusion reached by Barrett and Leven-son8 with respect to iron crystals that (111) [112] is one of the stable end orientations. However, different recrystallization textures were observed by Dunn and Koh3 in (111) [112] type crystals of different initial thickness, which widened differently during rolling even though their deformation textures were identical. Another interesting example, also from the results of Dunn and Koh2'3 is that of texture formation in a (112) [111] crystal. This crystal developed a two-component deformation texture of (111) [112] plus (001) [110]. Its recrystallization texture, however, was found to be predominantly (110) [001], which is related to the (111) [112] component by a simple [110] rotation. This crystal, therefore, behaved as if the other deformation texture component, (001) [110], were not present. There are also discrepancies among the results of different investigators, as well as numerous unexplained fine features of the deformation texture of crystals of various initial orientations. In order to have a better understanding of all of these points, a detailed study of deformation textures is greatly needed. One of the obvious things that has been completely overlooked in previous texture studies is the possible effect of surface texture. All past work on the texture of Si-Fe single crystals was conducted in a rather simple manner, i.e., the rolled crystals were etched to a very thin sheet; then their textures were examined by transmission X-ray techniques. For recrystallization texture studies, unless precautions are taken by etching off a sufficient amount of the surface layer before annealing, the texture developed in the interior may be affected by the surface layer, which may well have a different initial texture and which may have undergone recrystallization earlier than the interior of the specimen. Because of this effect, it is now planned to reexamine the texture of various rolled and annealed single crystals at the surface, and at various sections below the surface by using reflection techniques. In some cases, both surfaces of the rolled crystal will be examined. In one of Dunn's early papers,9 he noted that at an early stage of rolling the crystal seems to divide roughly through the middle to become a sample which in effect consists of two layers having some what different orientations. This effect has never been further explored. The investigation described in the present paper constitutes the beginning of a series of thorough investigations of texture formation in deformed bee single crystals designed to clear up some of the uncertainties which have been discussed. We have chosen a high-purity 2 pet Al-Fe alloy for this investigation. It is known that the allotropic transformation of iron is eliminated by alloying with approximately 1petAl. Such an alloy, being very similar to silicon ferrite, can be heated to the solidus temperature without phase transformation. One reason for choosing A1-Fe instead of Si-Fe for the present investigation is that we have been able to make single crystals of a vacuum-melted high-purity A1-Fe alloy by the strain-anneal method without much difficulty, but were not successful in doing so with a vacuum-melted high-purity Si-Fe alloy. For many research purposes,

Jan 1, 1962

By M. R. Geer

Efforts to evaluate washery performance are nearly as old as the art of coal cleaning, and in former years there was no uniformity in either the methods used or the basic terminology employed. This situation, and the con- fusion it bred, prevailed until about the time of the First International Coal Preparation Conference in 1950, Largely because of the interest of the French coal research organization Cerchar, the subject of evaluating performance was given prime importance at this conference. As a result, there is now a much greater degree of uniformity in terminology and methods of expressing cleaning results. The International Standards Organization currently is working toward international standards of terminology and methods that should improve the situation even more. The various criteria that are used to evaluate the performance of coal- cleaning equipment fall into three categories, depending upon the extent to which they are dependent on the density composition of the raw coal; some are directly dependent, others are only indirectly dependent, and still others are substantially indenpendent.

Jan 1, 1962

By Bruce I. Thomas

Reconnaissance studies of beach sands along the eastern part of the Gulf of Alaska were conducted by the Bureau of Mines to determine if any of these coastal areas warranted investigations as possible sources of valuable minerals. Because of difficult access and limited transportation facilities only a minimum of sampling, surveying, and camping equipment is utilized to obtain spot samples from key areas as well as information indicating the location, size, and character of the deposits. Such data were obtained from beaches located along approximately 247 miles of the Gulf of Alaska coastline during parts of the 1957 and 1958 field seasons. A total of 201 3-inch-diameter auger holes, spaced roughly at 1 mile intervals, were bored by hand methods to depths ranging from 3 feet to 27 feet; also 33 shovel samples were collected from selected localities. Samples were reduced to a rough concentrate in the field by panning; the rough concentrates were shipped to the Bureau of Mines laboratory at Juneau for further concentration and for petrographic and chemical analyses. Particular attention was given to the heavy-mineral content of the concentrates, although the types and relative amounts of rock-forming minerals were also determined. The reconnaissance indicated that, generally, the valuable mineral content of the beach deposits was too low to be of further interest except in the vicinity of Yakutat and Lituya Bays where erratic but possibly significant concentrations of magnetite and/or ilmenite were found. At Yakutat, about 20 miles of beachline extending southeasterly from Ocean Cape, yielded samplas containing from 1 pound to over 300 pounds of iron and from a trace to over 100 pounds of titanium dioxide (TiO2) per cubic yard of beach material. However, the higher grade samples represented local concentrations of minor importance. The general tenor of the Yakutat beach, as indicated by the airthmetical average of 27 auger-hole samples, is about 35 pounds of iron and 20.5 pounds of titanium dioxide per cubic yard of beach material. Ilmenite is the predominant heavy mineral of the beach deposits in the vicinity of Lituya Bay, but it was found in concentrations only in limited areas near the

Jan 1, 1962

By Joseph M. Singer

This research project had two main objectives: (1) To identify the smoke limits of gaseous fuel-air mixtures and (2) to obtain and evaluate basic chemical information on the formation of smoke in very rich flames near the smoke limit. Such information would do much to establish the circumstances for car-bon deposition in gas appliances and in other types of combustors. Based on tests with ethylene and propane, these studies showed the following: 1. Smoke limits are related to the yellow-tip limits of the fuel. Previous research established sufficient data to permit prediction of yellow-tip limits on gas burners using a wide variety of fuels. The present study of smoke limits deals only with ethylene-air flames, but the concept that was developed is probably applicable to other fuels.

Jan 1, 1962

By William A. Beck

The Construction Aggregates Corp. operates a plant for processing sand and gravel from two deposits in Ottawa County, Mich. The bulk of the sand is obtained from a sand dune on the shore of Lake Michigan, and the gravel is dug from a glacial-drift deposit farther inland. Mining is done with draglines, and the material, both at the digging site and in the plant, is moved mainly by systems of conveyors. The Ferrysburg plant serves customers along the Great Lakes, which is unusual for a business normally local in character. Annual production exceeds 1-1/2 million tons of sand and gravel as concrete aggregate and 200,000 tons of core sand for foundry use.

Jan 1, 1962

By W. A. McKinney

The segregation process consists of heating crushed oxidized or mixed oxide-sulfide copper are with a copper-volatilizing salt and carbonaceous material at about 750° C. to produce metallic copper which is recovered from the furnace calcines by conventional sulfide flotation. The Bureau of Mines made a number of bench-scale laboratory tests on two copper ores to determine the relative merits of using halogen salts, potassium chlorate, or various salt mixtures as volatilizing agents in segregation of the copper. Laboratory investigation of typical siliceous and calcareous oxidized ores revealed that sodium chloride was a better segregating agent than the other salts. Calcium chloride, magnesium chloride, sodium fluoride, or potassium chlorate gave nearly as good segregation as the sodium chloride on the siliceous ore. Segregation of the calcareous ore with calcium chloride was nearly as good as that obtained with sodium chloride, but inferior segregation resulted when magnesium chloride, sodium bromide, or potassium chlorate was employed. The use of sodium bromide or sodium iodide on the siliceous ore, and of sodium fluoride or sodium iodide on the calcareous are, gave appreciably poorer segregation than sodium chloride or the other salts. Other tests of the ores, using mixtures of sodium chloride and the other halogen salts or potassium chlorate, gave segregation approaching that obtained with sodium chloride.

Jan 1, 1962

By Michael G. Zabetakis

Limits of flammability of normal propyl nitrate (NPN) vapor were investigated at ambient and elevated temperatures. Minimum spontaneous ignition and decomposition temperatures were determined with laboratory apparatus over the pressure range from 0 to 4,000 p.s.i.g. Flame speeds and the detonation susceptibility of NPN vapor were measured at elevated temperatures. Stable detonation was obtained with liquid NPN at elevated temperatures, and the detonation velocity was determined to be between 4,700 and 5,100 m./sec.

Jan 1, 1962

By K. K. Kelley

Thermodynamics data for silicates have applications in the fields of extractive metallurgy, ceramics, and geochemistry. To facilitate these applications, up-to-date tables of heats and free energies of formation are needed. It is the purpose of this report to supply such tables for anhydrous silicates. During the last 15 years the heats of formation of a substantial number of anhydrous silicates have been reliably determined at or near room temperature. This resulted from the development (first by the Bureau of Mines and later by the Geophysical Laboratory of the Carnegie Institution of Washington, by the Institute of Geology of the University of Helsinki, Finland, and by the Department of Geology of the University of Chicago) of accurate solution calorimeters, employing hydrofluoric acid as the reaction medium. Specific references to work of these laboratories will be made in the next section of this report. Also, entropy data at 298.150 K. and high-temperature heat-content values are available for many of these silicates, mainly owing to work of the Bureau of Mines. Most of these entropy and heat-content data have been compiled in Bureau of Mines Bulletins (13, 15).3

Jan 1, 1962

By John C. Machisak

INJURY experience and employment data at all metal mines in the United States and Alaska are presented in this Information Circular for the calendar year 1958. This publication covers the metal mining industries, and contains statistical data on injuries and employment pertinent to metal mines, ore-dressing plants, and primary nonferrous smelters, refineries, and reduction plants. These operations report injury and employment information annually to the Bureau of Mines on a voluntary basis. The Bureau is authorized to make requests for such data, and the information submitted contributes immeasurably to the promotion of safety in the metal mining industry. Every effort has been made to make the annual canvass as complete as possible. This publication contains, along with production and development workers, the office employees at the mine location. The metal mines identified in this publication are classified according to the mineral ores mined; that is, copper, iron, lead-zinc, gold-silver lode, gold placer, and miscellaneous metals.

Jan 1, 1962

By B. K. Shibler

During a research program to develop improved methods for recovering elemental sulfur and useful sulfur compounds from secondary source materials, the technical literature was searched for pertinent articles on processing methods. This report summarizes results of the literature survey and describes the more important processes that have been used or suggested for recovering sulfur and sulfur compounds from all non-Frasch sources. The bibliography presented represents a survey of the available English language literature on the subject through 1958, with particular attention focused on the period 1950 through 1958. Engineering Index and Industrial Arts Index were the principal guides used in the survey of this period. Chemical Abstracts was used to a limited extent to identify a few key foreign articles and patents. The Sulfur Symposium (4)4 published in November 1950 by Industrial and Engineering Chemistry includes a broadly representative selection of the literature up to 1949. Therefore, this reference was used extensively to locate and list pertinent articles on processing methods reported in the period prior to 1950.

Jan 1, 1962

By Scott W. Hazen

This report describes the design, analysis, and results of a special experimental mine-sampling project conducted as part of the Bureau of Mines continuing program on sample-methods research. The experimental project was conducted at the Bureau?s Denver Mining Research Center and at the Climax molybdenum mine within the framework of a cooperative research agreement between the Bureau and Climax Molybdenum Co., Division of American Metals-Climax, Inc. The primary objective of the project was to investigate the interrelation-ship between sample volume, number of samples, the standard deviation of an assay distribution, and the precision required for an estimate of grade of ore, and to develop this interrelationship into a relatively simple method of application for use in mine sampling.

Jan 1, 1962

By M. R. Geer

Information on the performance of coal-cleaning equipment is necessary to provide a basis for evaluating the performance of existing plants and projecting that of new plants. Performance data can contribute greatly to the wise selection and effective use of coal-washing equipment. The Bureau of Mines has published information on the performance of several commercial plants, as well as of some laboratory-scale equipment, 5 (2-9, 11, 12, 17-12, 21-25) from time to time for a number of years. A more intensive program to provide such information for all the principal types of cleaning equipment is underway. The present evaluation of table performance is part of this program.

Jan 1, 1962

By F. W. Mueller

It seems to be a matter of general understnading that title extraction or use of ground water may not be used as the basis of a depletion deduction under the United States Revenue Code And indeed, I have been unable to find any precedent upon which to base such a deduction. It is for this reason that the Shurbet case, which is the subject of my discussion and is now before the Court, may well become a precedent as authority for the allowance or disallowance of a depletion deduction for income purposes. It is well known that the law recognized that capital is consumed in the process of extracting minerals, oil and has, other natural deposits, and timber (underscoring supplied). This exhaustion, or depletion, is likened to the using up of raw materials in manufacturing. The law, therefore, provides a deduction for depletion which is intended as compensation for the exhaustion of assets consumed in the production of income through severance of minerals, oil and gas, other natural deposits, and timber.

Jan 1, 1962

By C. S. Tout

While investigating methods for determining the best temperatures for hot-working experimental stainless steels, the Bureau of Mines Albany Metallurgy Research Center developed a machine in which hot-twist tests could be made in a few minutes. This machine is similar to some used previously except that specimens are heated by induction instead of by radiation, and their temperature is measured by a calibrated radiation-detection unit instead of by a thermocouple. In. developing the technique for using the new machine, tests were made on specimens of medium-carbon steel, mild steel, and AISI (American Iron and Steel Institute) type 304 stainless steel. Tests also were made on as-cast specimens and preworked specimens of experimental AISI type 202, low austenitic stainless steel, and as-cast specimens of AISI type 301 experimental stainless steel. The optimum hot-working temperatures were determined for all types of steel tested. Also, data were gathered on the effects of test speed and temperature on torsional strength and the effect of twisting on tensile stress in the specimen.

Jan 1, 1962

A nine-month investigation was conducted into the effect on coke quality and blast furnace operation of the addition of bentonite and southern coal to the northern coal fed to the coke ovens at the Newcastle steelworks.Additions of 0·3 per cent bentonite or 25 per cent southern coal to the northern coal increased the coke strength from 15-20 A.S.T.M. stability to 25-30 A.S.T.M. stability. It is likely that improved mixing and blending facilities would, in both cases, give a coke of over 30 A.S.T.M. stability.For the same coke strength, the use of 0 3 per cent imported Wyoming bentonite was considerably cheaper than the use of 25 per cent southern coal, but the use of Australian bentonite promises the same coke strength for still lower costs. Other additives such as coke breeze, charcoal, iron ore fines, and certain other finely divided materials, gave relatively minor improvements in coke quality.There appeared to be sufficient improvement in blast furnace operation and production to justify full scale addition of bentonite to improve coke quality, although other variables, particularly iron ore physical quality, overshadowed on many occasions the effect of coke quality. Further coke trials with southern or bentonite will be carried out when ore quality has been improved by the introduction of ore sintering at Newcastle.INTRODUCTIONDuring the period of operation of the Newcastle coke ovens and blast furnaces from April 1960 (when No. 3 blast furnace was blown in after rebuilding) to December 1960, a bentonite coke trial was carried out based on earlier research findings (Gregory, 1959a, 1959b; Felton and Gregory, 1960; Gregory, 1960) that as little as 0 3 per cent to 05 per cent bentonite clay added to northern N.S.W. high volatile coking coals gave a significant increase in coke strength. The bentonite coke trial was followed by trials...

Jan 1, 1962

By E. T. Turkdogan, P. Grieveson

It is shown experimentally that, by making use of the coupled S-O reaction in ionic melts, it is possible to transfer slclJur or oxygen from a lozv to a high chemical potential through an ionic nzenzbrane. This uphill transfer of sulfur is accompanied by a counter downhill transfer of oxygen and vice versa. The Materials balance shows that the amoulits of sul -fur and oxygen lost or gained by one system are the same as those gained or lost by the other systenz — the two systejns being separated by an iofzic membmne. The systems used in these experi?nents were solid Mn-MnS-Mno and liquid Fe-S-0. Sufficient results were obtained Lo study the kinetics of the transfer and the indications are that the counter diffusion of sulfide and oxide iojzs in the membrane is the rate controlling process. WHEN an ionic oxide-melt reacts with an atmosphere containing sulfur and oxygen-bear ing gases the following reaction occurs: 1/2 S2 (gas) +O2- (melt) = S2- (melt) + 1/2 0, (gas) [1] Under the restrictions that i) electric conductance in the melt is purely ionic and ii) each constituent element in the melt does not change valence, the solution of an atom of sulfur in the melt will result in the evolution of an atom of oxygen, so that the electric neutrality is maintained. For a given temperature and melt composition, the equilibrium concentration of sulfur in the melt is determined by the ratio, po2 /ps2 , in the gas phase and not by the individual partial pressures of oxygen and sulfur. This has been demonstrated by a number of investigators, for example by Richardson and withers', Fincham and Richardson,la by St Pierre and Chipman,' and by Turkdogan and Darken.3 In his Howe Memorial Lecture for 1961, Darken discussed the possibility of uphill pumping of sulfur through an ionic membrane at the expense of oxygen. TO test the validity of this concept associated with coupled reactions, experiments were carried out in the following manner. A presintered mixture of Mn-MnS-MnO and prefused mixture of Fe-S-0, contained in platinum and iridium crucibles, respectively, and separated by a thin layer of soda-glass (to act as an ionic membrane), were placed side by side in an evacuated silica capsule and sealed. This was then kept at 1400°K for a required time to allow Reaction [11 to occur via the ionic membrane. When partial equilibrium is reached, the ratios Po2 /pS2, for systems on either side of the membrane, are equal and the flux of sulfur and oxygen through the membrane becomes zero, although the individual partial pressures po2 andp,, in these two systems may differ considerably.

Jan 1, 1962

By M. Clair Smith

This report is one of a series being prepared by the Bureau of Mines on exploration, development, mining methods, and costs at various open-pit mines in the United States. These reports have been prepared in cooperation with various mining companies. A similar program, conducted from 1928 to 1939, was generally conceded to have contributed to improving the efficiency of mining operations. The purpose of these reports is to promote development and conservation of our mineral resources by disseminating technological information on mining methods and practices. This report describes exploration, development, equipment, and mining by open-pit methods of the remainder of an ore body that had been previously worked by underground methods. The Tripp pit of the Consolidated Coppermines Corp. is located at Kimberly, Nev., a small mining company town having an elevation of 7,250 feet, 9 miles by road west of Ely, Nev. (fig. 1). The pit extends over the area formerly mined by underground methods from the Morris and Brooks shafts.

Jan 1, 1962