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By M. G. Zabetakis

The use of liquid hydrogen as a high-energy fuel introduces numerous hazards not ordinarily associated with the use of other more conventional fuels. These hazards are attributable to the unique properties of hydrogen in the liquid and gas states (table 1). Since little work has been conducted on explosion and related hazards of cryogenic fuels, a research program was undertaken to obtain basic data on such dangers for hydrogen and other combustibles under these conditions. These data were used to outline emergency procedures for protecting personnel and equipment when an accidental spillage of liquid hydrogen occurs and to establish a quantity-distance table for the storage of this fuel. The vaporization of liquid hydrogen from a surface is treated as a prob¬lem in heat transfer theory. Two extreme cases are briefly considered: (1) The transfer of heat occurs at constant temperature drop between, the boiling liquid and the hot surface, and (2) the transfer of heat is limited by the rate at which it can flow to the surface from a hot insulating medium. The available data indicate that the former case (1) is applicable when vaporizing from a conducting surface and, initially, when vaporizing from an insulating medium; the latter case (2) is applicable after initial flash vaporization has occurred from the insulating medium. The vaporization rate determines in part the rate at which flammable hydrogen vapor-air mixtures are formed above a spill area. However, the rates at which heat is transferred to the vapor, and air is brought in contact with it also are of importance. Accordingly, the distribution of flammable mixtures above a spill area was determined experimentally. In general, flammable mixtures were found to be both above and within the visible vapor cloud.

Jan 1, 1961

By William J. Campbell

This study was a part of two programs: The first, to develop and evaluate high-temperature refractories; the second, to investigate reaction-rate kinetics and phase equilibria in the sinter step of the lime-soda process for the recovery of alumina. High-temperature X-ray diffractometer techniques are to be used extensively in both programs. This paper summarizes developments in the field of high-temperature X-ray diffractometers through 1959, evaluates various furnace designs, and describes briefly the X-ray diffraction facilities of the Federal Bureau of Mines. A more detailed description of the equipment and its calibration is planned in a future paper on thermal expansion and phase inversion of rare-earth oxides.

Jan 1, 1961

By C. N. Adams

The purpose of this investigation was to evaluate the physical and mechanical properties of high-purity titanium made by two processes. Sodium-reduced metal with 58 Brinell hardness number (B.h.n.) and electrorefined metal with 60 B.h.n. and 70 B.h.n. were used. Titanium of these hardness levels did not work-harden excessively, and beyond 40 percent cold work the hardening effect was not great. Rapid softening occurred when the metal was annealed at temperature between 300° and 600° C. Full annealing, as determined by property and microstructure studies, was accomplished after 30 minutes at 700° C. A recrystallization diagram is presented which is based on determinations of annealed grain size as a function of rolling reduction and annealing time. For reductions of less than 20 percent, exaggerated grain growth occurred during annealing; for reductions greater than 20 percent, the variation in grain size for each annealing temperature was minor.

Jan 1, 1961

By K. K. Kershner

The purpose of this research by the Federal Bureau of Mines was to investigate the recovery of tin from mine-run ores and low-grade concentrates. Over 95 percent of the total tin in such materials was volatilized to tin chlorides at temperatures ranging from 520° to 565° C. Gaseous mixtures of hydrogen and hydrogen chloride were used for reducing cassiterite to stannous oxide and for converting this compound to tin chlorides. The chlorides were swept from the reaction zone of an oscillating kiln by a rapid flow of reactant gases and collected in a condensing system. Losses of tin that occur in current metallurgical processing were prevented. Approximately the same time of treatment was required for minus 35-mesh mine-run ores and low-grade concentrates. In a continuous process, the circulating gases would require some enrichment.

Jan 1, 1961

By H. D. Kline

This publication describes mining and milling methods and costs at the Madison mine of National Lead Co., St. Louis Smelting & Refining Division, in the Fredericktown district of southeast Missouri and is one of a series prepared by the Federal Bureau of Mines on methods, practices, and costs of mining and milling throughout the United States. The are bodies of the Madison mine are known for the complexity and diversity of their are minerals. Sulfides of copper, nickel, and cobalt occur in commercial quantities with lead sulfide, which is the most valuable metallic mineral in are bodies of the Bonne Terre formation in southeast Missouri. Several attempts were made by various operators to mine the complex ores and separate the sulfide minerals before 1927 when National Lead Co. became interested in the Fredericktown district. Operating then as the St. Louis Smelting & Refining Co., the company began mining and milling ores from the Madison mine in 1944 and has operated continuously since then. A recently built refinery produces copper, nickel, and cobalt metal from a concentrate containing iron sulphides and small quantities of copper, nickel, and cobalt sulphides.

Jan 1, 1961

A spectrographic procedure applicable to the semiquantitative determination of 29 elements in tungsten is presented. The method is designed to give estimates of impurity concentrations up to 500 p.p.m. Limits of detectability range from 0.3 p.p.m. for the more sensitive elements to 100 p.p.m. for the less sensitive ones. Tungsten metal samples varying in particle size from minus 300-to 30-mesh are excited in the presence of 5 percent germanium with a direct current arc. Germanium acts to stabilize the arc, minimizes the volatilization of tungsten, and serves as an efficient carrier to sweep impurities from the tungsten into the excitation zone. Curves are presented that show the volatilization behavior of germanium, tungsten, and impurities in tungsten at different concentration levels. Data obtained were used as guides in establishing the method of analysis. In the absence of established reliable analytical procedures for determining many impurities in tungsten in the parts per million concentration range, the spectrographic method described here should prove to be helpful in evaluating high-purity tungsten.

Jan 1, 1961

By W. S. Sanner

Anthracite was used extensively as a fuel in iron metallurgy from 1840 to 1880. In 1874, 226 of the 680 blast furnaces in the United States were operating on anthracite and producing almost one-half of the Nation's pig iron. However, by 1890, railroad expansion, the development of western iron-ore reserves, and the growing use of coke decreased the importance of anthracite as a metallurgical fuel. As a result, the last blast furnace designed exclusively for anthracite use was built in 1891. Because of the increased energy requirements of our expanding national economy, the abnormally high demands during national emergencies, and the proximity of anthracite deposits to eastern steel-producing areas, interest has grown in again using anthracite in iron metallurgy. Estimates of anthracite reserves indicate a 300-yr. supply at a production rate of 30 million tons per year. These large reserves dictate the development of an adequate technology for the use of anthracite by the metallurgical industry.

Jan 1, 1961

The paper outlines the development of a solvent extraction process for the recovery of scandium, yttrium, thorium, and heavy lanthanides from waste sulphate liquor at the Port Pirie uranium treatment plant. A summary is given of known solvents for these elements, including the recently developed alkyl-phosphoric acid esters which are applicable to sulphate solutions.A kerosene solution of di- (2'-ethylhexyl) phosphoric acid (EHPA) has been suggested by some workers as a suitable solvent for fractionation of the lanthanides. Experimental work with this solvent showed that it could be used for initial recovery of the above elements from low concentrations in the complex sulphate liquor. In particular, scandium could be recovered as a high grade product by extraction with 0·lM EHPA, followed by a purification strip with 9N sulphuric acid, and final stripping of scandium with sodium hydroxide solution.To enable alkaline stripping to be used successfully, the kerosene solution of the reagent was modified by the addition of a small proportion of nonanol. Experimental work included laboratory scale batch tests and small pilot scale continuous tests.A proposed extension of the process for the separate recovery of individual heavy lanthanides, yttrium, and thorium is described.INTRODUCTIONAt the Port Pirie uranium treatment plant of the South Australian Government, large volumes of "barren liquor", free from 'uranium, are at present run to waste. This "barren liquor" results from sulphuric acid leaching of Radium,Hill uranium concentrate, followed by separation of solid residues and removal of uranium from the clear solution by ion exchange. The mineral davidite, from which the uranium is derived, contains other potentially valuable components, notably vanadium, chromium, thorium, yttrium, scandium, and the lanthanides. These constituents are...

Jan 1, 1961

Present roof bolting practices in the collieries of Australian Iron and Steel Pty. Ltd. are outlined. Roof support has been improved since introducing roof bolts and it is hoped to increase the reliability of the bolts still further.Expansion-shell, and split and wedge roof bolts five to eight feet long are placed by "Atlas Falcon" and "Fletcher" roof bolters. Both anchorage and tightening have presented some problems.Good panel supervision is required if systematic roof bolting is to be properly co-ordinated with coal production without unnecessary delay to either. Successful roof bolting can only be the product of conscientious men and supervisors who are all convinced of its value. A rigid operational code should be established early and maintained.INTRODUCTIONRoof bolting is a method of support which is permanent and reduces or eliminates the need for other support; The method was pioneered in America and was first experimentally investigated in Australian collieries at Elrington in 1949 (McKensey, 1953). Pneumatic installation methods were employed. Subsequently, a method of using standard hand-held electric coal drills was developed at John Darling Colliery (Horseman, 1954). Pneumatic roof bolting equipment was first operated in the collieries of Australian Ironand Steel Pty. Ltd (A.I. &. S.) in 1951. Since then various hydraulically operated mobile machines have been installed in Australian collieries and these, together with improved pneumatic equipment, form the two present basic methods of placing ,roof bolts. Roof bolt anchorage is achieved by either split and wedge or expansion-shell bolts.The two broad types of roof bolting are 1. consolidation of strata, and 2. suspension support.

Jan 1, 1961

By R. J. Leary

Significant improvements in surface conditions or mechanical properties of steels have been attributed by several investigators to ladle additions of small quantities of rare-earth metals or their oxides. To investigate systematically these effects in wrought and in cast plain carbon and alloy mechanical steels containing approximately 0.35 percent carbon, heats of four representative compositions were melted by the Bureau of Mines in a 4-ton open-hearth furnace. Each heat was cast into three sets of ingots to exemplify respectively, treatments with (1) rare-earth metals, (2) rare-earth metal oxides, and (3) an untreated set as a control. The development of melting, casting and rolling practices is described and discussed. Lance injection of oxygen shortly after melt raised the temperature of the metal immediately as much as 500° F., principally because mechanical agitation exposed the high-carbon metal to the flame and furnace root. An exceptional degree of superheat in the metal at the termination of the refining period was attributed to oxygen injection during the refining period. Bath temperatures higher than industrial practice were permitted by the all-basic furnace lining. Rates of carbon elimination as high as 0.036 percent carbon per minute were achieved by oxygen injections.

Jan 1, 1961

By Beverly W. Dunning

The effect of vacuum melting on the elimination of gases and nonmetallic inclusions for six low-alloy steels was investigated. The purpose of these studies was the analysis and comparison of differences in gas content and inclusions in air-melted and vacuum-melted steel. Data obtained from melts of 1-1/4 to 20 pounds indicate that vacuum melting decreases the number and size of nonmetallic inclusions and at the same time increases the degree of dispersion of the remaining inclusions. These improvements are undoubtedly related to the elimination of approximately 80 percent of the nitrogen and 90 percent of the oxygen as well as most of the undesirable metallic trace impurities.

Jan 1, 1961

By Howard W. Wainwright

The Bureau of Mines is engaged in a research program on the characterization of tars produced by low-temperature carbonization of coal and their economical upgrading to more valuable materials, Throughout the years, hydrogenation has played an important role in the treatment of these tars, mainly as a means of converting the whole crude tar or selected fractions to motor fuels; diesel oil, lubricating oil, or various solvents. In some instances, production of specialty chemicals has been the objective. The purpose of this report is to summarize, without critical review, the information of the past 25 years on the hydrogenation of low-temperature tars and related substances as presented in the literature or its English translation. Published articles and patents not abstracted in the main body of this report are included in a bibliography at the end. HYDROGENATION REACTIONS The hydrogenation of tar follows three general types of reactions; 1. The removal of oxygen, sulfur, and nitrogen in the tar to form water, hydrogen sulfide, and ammonia, respectively: [ ]

Jan 1, 1961

By Charles B. Kenaban

The possibility of using ultrasonic energy as a tool to improve the electrolytic deposition of copper and zinc from several electrolytes was investigated by the Federal Bureau of Mines. Sound with frequencies of 20, 26, 38, and 400 kilocycles per second and acoustical intensities of 0.25 to 1.5 watts per square centimeter was employed. Measurements of cell voltage, anode and cathode current efficiencies, and electrode potentials were made at various current densities. Effects of ultrasonics on the quality of the deposit and on anode corrosion also was noted. In the electrolytic recovery of copper from an acid copper sulfate solution at 50° C., adherent, well-consolidated deposits are normally obtained up to a current density of 30 amperes per square foot. As the current density is increased above this value, the deposits normally become progressively more spongy and less adherent. Ultrasonic irradiation resulted in adherent and well-consolidated deposits at current densities up to 300 amperes per square foot. Radiation also produced smaller grain size and preferred orientation of the copper crystals. In addition, radiation caused as much as 3-volt decreases in cell voltages at the higher current densities. These decreases were caused chiefly by depolarization of the anode, although small depolarization effects were also noted at the cathode. Radiation apparently did not greatly affect cathode-current efficiencies, but prevented excessive anode corrosion at the higher current densities and resulted in more uniform corrosion. Ultrasonic radiation at a frequency of 400 kilocycles per second was not as effective as radiation at the lower frequencies. Circulation of the electrolyte at rates up to 5 percent of the cell capacity per minute did not produce results comparable to those effected by ultrasonic radiation. Rapid rotation of the cathode up to 1,800 revolutions per minute gave results approaching those obtained with ultrasonics.

Jan 1, 1961

By F. M. Morris

A large reserve of thick coal in southwest Virginia was developed by Clinch-field Coal Co. in 1957-1958 to produce a nominal rate of 1500 tph raw coal. Operation features coal cleaning in transit. Refuse removed averages 35 pct. Evolution of plant from initial conception to completion is discussed, selection of means applied is explained, and performance to date us design expectation is described. The long-range plan calls for ultimate handling capacity of 40,000 tpd raw coal with anticipated clean coal capacity of 26,000 tpd on a three-shift basis. From a materials handling viewpoint, the Moss No. 3 operation is principally of interest as an ensemble. Generally speaking, it uses time-tested equipment and ideas but some of these are employed on a scale that may be new in the industry. At present about 20,000 tpd of raw coal are being handled. This is expected to increase to 40,000 tpd as soon as business conditions justify it. The purpose of this paper is to discuss the evolution of the plant as to materials handling practices, to describe briefly the equipment and methods used, and to comment on performance in certain areas. The subject divides itself naturally into four phases: 1) operations at the mines, 2) transportation from mines to plant, 3) raw coal handling into the plant, and 4) transportation of refuse away from the plant. OPERATIONS AT THE MINES The coal reserves for Moss 3 are in southwest Virginia where Dickenson, Russell, and Buchanan Counties come together. This area contains about 15 square miles and over 100,000,000 tons of coal. Here the No. 4 (Tiller) and No. 5 (Jawbone) seams of the Norton Formation lie so closely together that for practical purposes, they constitute one seam of coal. This seam, which is called the Thick Tiller, varies from 10 to 18 ft in thickness and underlies Sandy Ridge, a mountain cresting between 2400 and 3300 ft above sea-level. At 18-ft seam height (which is considered to be the maximum practical mining height) the parting between seams will be about 3 1/2 ft thick and each bench of coal will be about 7 ft thick. Depending on the amount of impurities in the seams Drover. total reject in this height coal may approximate 50 pet by wt. It will average about 35 pet for the property as a whole. The first move in developing this resource was made in 1953 when contour maps of several square miles around Duty, Va., including all the known outcrop, were made by photogrammetry. At this time, it was felt the prospective operation would be served by the Clinchfield Railroad and a photogrammetric route survey was made by this railroad from Haysi to Duty. Study of the resulting maps indicated only one site—adversely owned—which might accommodate the size washing plant to be erected. Water resources of a dependable nature seemed nonexistent. In 1954 bulk washability tests were made on the Tiller Bench at the Moss No. 1 preparation plant. The tests indicated this portion of the seam, mined separately, would wash to 4 pet ash with good recovery. Also in 1954, development of Moss No. 2, south of Sandy Ridge, was begun. This mine is in the Tiller Seam where it is about 100 ft below the Jawbone Seam. The reasons for developing a mine in the normal Tiller Seam before tackling the Thick Tiller seemed compelling: Railroad service could be established quickly, communications were better (though not good!), more was known of the seam (it had been mined in the years 1911 to 19241, and there was no essential property to be acquired. After some legal skirmishing, the Norfolk & Western Railroad was granted the right to serve the new mine. Three decades earlier the old mine had been served by the Clinchfield Railroad. The event which triggered active development of Moss 3 was the Appalachian Power Co.'s decision in 1956 to build a 450,000-kva power plant on Clinch River at Carbo. This solved the problem of marketing the steam coal which inevitably must be a product of a mine in the Thick Tiller. Management promptly decided to build the preparation plant at Carbo where an excellent site was owned; where railroad service existed; where telephone service could be obtained; and where roads, bridges, and water supply were tolerable.

Jan 1, 1961

By John C. Machisak

Injury data and experience, with related employment statistics, at coal mines in the United States for 1959 are presented in this publication under the following general sections: (A) General injury experience: Tables 1 to 6: Current data on number of injuries degree of injury, frequency and severity rates, average severity, and related employment and production data by work location. (B) Selected injury experience: Tables 7 to 38: Current data on principal agencies of injuries, distribution of injuries by part of body injured, days of disability, extent of hand and machine loading, experience by employment and production groups, and various other operating factors and physical conditions related to the occurrence of injuries at the Nation's coal mines.

Jan 1, 1961

Solvent extraction has recently been introduced into Australian hydrometallurgical practice for the production of a high grade uranium concentrate from El Sherana ore by a sulphuric acid leach and solvent extraction process. The solvent is a 5 per cent solution of tri(iso-octyl)amine in kerosene modified with 4 per cent of a long chain alcohol. The stripping reagent is a molar solution of sodium chloride.Preliminary testing for the development of the process showed that the leach liquor was quite amenable to the solvent extraction process and that the equilibrium and rate considerations of both the extraction and stripping steps were very favourable.The industrial plant contains four stages of extraction, three stages of chloride stripping and one stage of secondary carbonate stripping. An internal type of mixer-settler is used for the stagewise contact, the design being based on tests with model equipment.The performance and control of the industrial plant is satisfactory; 99·7 per cent of the uranium is recovered for a loss of 0·3 gallons of kerosene and 0· 4 pounds of amine per 1,000 gallons of liquor treated.INTRODUCTIONThe processing of El Sherana uranium ore from the South Alligator River valley commenced in April, 1959, and thereby introduced into Australian hydrometallurgical practice the unit operation of solvent extraction on an industrial scale. Although there are now some twelve mineral processing plants in the United States and Canada using solvent extraction, its application to the field of primary hydrometallurgy is quite new. Prior to 1956 none of these twelve plants was operating and hydrometallurgical application waslimited to the refining of comparatively high grade uranium compounds and fission products from nitrate and nitric acid solutions.

Jan 1, 1961

By Marvin L. Whisman

This report describes the preparation of tritium-labeled organic compounds to be used by the Federal Bureau of Mines in studying the role of certain gasoline constituents in gum-forming mechanisms. The gasoline constituents that have been investigated boil within a range of approximately 90 to 230° C. and can be classified as paraffins. naphthenes, olefins, diolefins, monocyclic aromatics, polycyclic aromatics, and organic sulfur, nitrogen,: and oxygen compounds. The technique of Wilzbach has been applied to more than 50 samples. Purification techniques have been developed that accomplish rapid and effective purification as well as removal of labile tritium in a one-step operation. Data are presented to show the rate of exchange between tritium and hydrogen that can be expected for a variety of compounds common to a full-boiling-range gasoline. These values should be useful to other investigators using tracer programs involving tritium labeled compounds.

Jan 1, 1961

By Robert H. Merrill

Measurement of the deformation of a borehole in rock subjected to a change in applied stress can be used to calculate the magnitude and direction of the applied stress, provided a satisfactory deformation-applied stress relationship exists , In this investigation by the Bureau of Mines the deformation of a bore- hole in a rock model subjected to a known applied stress was compared with the theoretical deformation of a hole in an elastic, isotropic plate and was found to be in good agreement. Hence, this relationship can be used to calculate the applied stress on a borehole from borehole deformation measurements.

Jan 1, 1961

By K. K. Kershner

Sulfide ore concentrates containing cobalt, nickel, copper, lead, and iron were salt roasted and leached on a laboratory scale. More than 95 percent of the cobalt, nickel, and copper was recovered. Heating patterns for salt roasting different concentrates were established. More cobalt, nickel, and copper were recovered from a bulk concentrate composed of a mixture of copper concentrate and iron concentrate. This mixture corresponded roughly with the mixture of these materials in stockpiles in southeastern Missouri. A temperature range of 375° to 400° C. was best for salt roasting. Metal chlorides were leached at a pH of 1 from chloridized charges of concentrates, Although the amounts of cobalt, nickel, and copper extracted were high, the amount of iron dissolved simultaneously interfered with subsequent separation and recovery of these metals. The amount of dissolved iron was reduced substantially by steam treating chloridized charges of bulk concentrate at 300° C. In this way, the ratios of cobalt, nickel, and copper to iron in leach liquors permitted satisfactory separation and recovery of these metals. INTRODUCTION The Federal Bureau of Mines is experimenting with chloridizing reactions.4 5 6 7/ Salt roasting of sulfide ores and concentrates, or their calcines, to form metal chlorides has certain advantages. Chlorides of

Jan 1, 1961

By H. F. Yancey

Traditionally the Pacific Northwest has relied on hydroelectric power, which has been both abundant and cheap. However, comparatively few hydroelectric sites capable of providing low-cost power remain, therefore the need for supplemental thermal generation, perhaps within the next decade, is generally recognized. Based on the present cost and availability of competing fuels, coal seems to be the logical choice for projected thermal power plants. Power companies and public utilities have become interested in establishing reserves of coal for future use. One deposit explored in 1958-59 lies in southern Thurston and northern Lewis Counties, Wash., near Centralia. Drilling, totaling 22,700 feet, proved the existence of 70 million tons of strippable coal--an ample reserve for the projected power plant. The coal, like most others and particularly those of Washington and Oregon, when mined in full seam section by mechanical methods, would require cleaning to make it suitable for use. The amount and nature of the impurities in this coal dictated a thorough investigation of its cleaning characteristics to establish economic factors and to insure proper preparation-plant design. Therefore, arrangements were made through a cooperative agreement to conduct such work at the Seattle Coal Research Laboratory of the Bureau of Mines. This report describes that investigation. The results are of interest primarily in connection with the utilization of this particular deposit, but some of the information developed is applicable to other deposits of low-rank coals in the West, because the impurities in these coals differ greatly in behavior from those generally associated with the higher rank coals of the Appalachian field.

Jan 1, 1961