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By D. E. Swets, R. C. Frank

It is well known that hydrogen is introduced into iron or steel as a result of many chemical processes (acid pickling, electrolytic cleaning, plating, etc.). One of the reactions that has been of recent interest1 is the reaction between an iron surface and water vapor. It was shown a few years ago2-4 that hydrogen can be introduced into steel at an accelerated rate during abrasion as a result of this reaction. Grun-berg and Scott have also observed that water in mineral oil lubricants increases pitting failure in ball bearings5 and they have suggested that hydrogen from the water is the primary cause of this effect.' In this laboratory, the question was raised as to whether or not hydrogen is also introduced into the metal surface of a bearing as a result of the decomposition of the hydrocarbon lubricant itself, and an experiment was performed to try to find a satisfactory answer. All steel parts contain some residual hydrogen. Therefore, it appeared that the best way to carry out this experiment without the need for highly accurate quantitative analyses was to use deuterium as a tracer. The natural abundance of deuterium in H2 is only 0.015 pct. The tracer was obtained in the form of deuteroparaffin (CD,(CDJ, CD,) and 0.25 g were dissolved in 20 cc of mineral oil to form the lubricant to be used in the tests. The bearings used were New Departure Type QOLOO ball bearings with a ball diam of 0.187 in. Prior to adding the mineral oil-deuteroparaffin lubricant, the bearings were cleaned in warm trichloroethylene to remove the packing grease. After packing with the new deuterated lubricant, the bearings were operated in a bearing fatigue test machine under a radial load of 190 lb and a thrust load of 190 lb at a speed of 3800 rpm. The expected life under these conditions is about 500 hr. Two tests were made; one for a period of 27 hr and the other for a period of 102 hr. The bearings achieved a temperature of 120o F during the tests. When the tests were stopped the balls were mechanically removed from the bearings and were immediately placed in liquid nitrogen to reduce degassing until the analysis for deuterium could be made. Before analyzing, the balls were warmed to room temperature and scrubbed with several degreasing agents to remove all traces of the deuteroparaffin mixture. This cleaning procedure was shown to be satisfactory by running a control test in which one ball bearing was subjected to all parts of the test except running in the fatigue machine. The hydrogen and deuterium were removed from the balls using a hot extraction apparatus attached to a mass spectrometer. Four balls from each bearing were analyzed. Each one was analyzed separately by removing it from a cold storage volume of the hot extraction apparatus and transferring it to the oven tube with a magnet. As the gases were evolved they were analyzed with the mass spectrometer. Since the hydrogen and deuterium pass through steel in the atomic form and since there are many more hydrogen atoms than deuterium atoms in the sample, the probability of forming an HD molecule is greater than forming a D2 molecule. For this reason the evolution of HD and H was followed as each ball was placed in the oven. The results showed that as each ball from the test bearing was dropped into the oven, the mass spectrometer recording of the HD evolution increased by about ten divisions. When balls from the control test bearing were dropped into the oven, the increase was about one division or less. The hydrocarbon background in the mass spectrometer was also monitored to see if hydrocarbons or deuterocarbons were given off when the balls were dropped into the oven, but no change in the hydrocarbon peaks was observed. Since the balls contained a fair amount of residual hydrogen, isotope ratio measurements were made on the gas obtained from each ball. The D/H value found for those balls which had been operated in the fatigue testing machine was consistently about 0.3

Jan 1, 1962

By J. P. McGee

The Bureau of Mines is doing research and development work on a coal-fired gas turbine plant initially developed by the Locomotive Development Committee, (LDC) of Bituminous Coal Research, Inc. The Bureau is redesigning the turbine blading and some of the auxiliary equipment, and is reerecting, the plant at the Morgantown (W. Va.) Coal Research Center. The present goal is a 1,500-hour run at virtually the same operating conditions used by the LDC in their final 1,100-hour test with the turbine. This will allow the Bureau to properly evaluate the new blade design. Erosion of the turbine blades (particularly the roots) by ash in the hot gases from the combustion of coal was the most serious problem in extended operation in earlier experimental work. New blades made of Stellite6 are being fabricated for the stator and rotor, and armored wear strips of titanium carbide will be inserted in the blades at the areas of probable maximum ash velocity and concentration. The trailing edges of the rotor and stator blades are being thickened and thinned, respectively, to induce the ash to travel to the casing and prevent it from returning to the base of the rotor blades. The first stage rotor and second stage stator blades are being removed to provide an annular space for maximum quantities of coal ash to centrifuge to the casing. Additional blades will be added to most of the rows in the stator to stop secondary flow of dust-laden gas toward the rotor. A contract has been awarded for fabrication of the new blades. The 1,500-hour run will be started as soon as the new blades are installed.

Jan 1, 1962

By Sidney Katell

Covering the period from January 1961 through December 1961, this report is a continuation of the series that began with the publication of Information Circular 7516 in October 1949. It is also the third report in the series to be prepared as a cooperative effort by the Bureau of Mines and the American Association of Cost Engineers. The cooperative agreement between the two groups provides for the publication of an annual cost bibliography with the work load involved in the preparation shared equally. The abstracted articles, concerned with all facets of cost engineering in the field of chemical and petroleum plants and related facilities, came from the following sources: 1. A.A.C.E. Bulletin. 2. Bureau of Mines Information Circulars. 3. Bureau of Mines Reports of Investigation. 4. Chemical Engineering. 5. Chemical Engineering Progress. 6. Chemical Week. 7. Coal Age. 8. Coal Utilization. 9. Cost Engineering. 10. Industrial and Engineering Chemistry. 11. Nucleonics 12. Oil and Gas Journal. 13. Petroleum Engineer for Management. 14. Petroleum Refiner. 15. World Oil.

Jan 1, 1962

By H. R. Shell

Fluorphlogopite mica was synthesized from inexpensive and abundant olivine, clay, feldspar, and sand (plus K2SiF6). The raw materials were melted in crucibles and in an internal resistance electric furnace. The melts yielded >95 percent mica. The major difficulty encountered was incomplete settling of the highly dispersed ferroalloy. This problem was not completely solved. Reducing agents tried in melts of 300 to 400 pounds were carbon, silicon, and silicon carbide. Carbon slowly reduced the iron of the raw materials, with much fuming. Silicon apparently was oxidized ahead of the melting and was ineffective under the conditions obtained. By far the best reducing agent was silicon carbide. With silicon carbide, fuming did not occur and ionic iron content of the mica flake approached 0 percent. However, even with SiC, the highly dispersed globular iron did not completely separate from the mica portion. The fluorphlogopite made during this investigation should be suitable for metallurgical use. A byproduct ferroalloy containing about 5 percent nickel, 3 to 5 percent chromium, and some cobalt was obtained. Because of the highly dispersed metallic ferroalloy, the mica was not deemed suitable for electrical or electronic uses.

Jan 1, 1962

By Charles B. Kenahan

Vanadium is subject to only light corrosion in phosphoric acid at temperatures up to 60° C. and has a moderate corrosion rate in this acid at 100° C. It is relatively corrosion resistant in sulfuric and hydrochloric acids up to 60° C, but corrodes rapidly at 100° C. It corrodes rapidly in dilute nitric acid at 35° C. Vanadium is almost inert in 10-percent solutions of formic, acetic, lactic, tartaric, and citric acids; in 9-percent oxalic acid it corrodes slowly up to 60° C. and rapidly at 100° C. Vanadium is resistant to corrosion in substitute ocean water, tapwater, and in 3-percent sodium chloride and 10-percent sodium hydroxide solutions. It is readily attacked, however, by 20-percent ferric chloride, 20-percent cupric chloride and 5-percent mercuric chloride solutions. Vanadium is protected by contact with magnesium, aluminum, and steel SAE 4130 in substitute ocean water, by magnesium and aluminum in 3-percent sodium chloride solution, and by magnesium in tapwater. Vanadium protects copper in substitute ocean water. When vanadium and stainless steel are coupled in sulfuric acid solutions, both metals are usually unaffected by contact, whereas the corrosion rate of titanium in sulfuric acid is greatly reduced by contact with vanadium.

Jan 1, 1962

By H. E. Powell

A series of alkyl-dithiocarbamic acid amine salts was prepared and tested as collector for slimed lead minerals contained in the waste material from a commercial lead ore concentrator. The reagents, members of a homologous series differing only in the number of alkyl radicals in their structure, were prepared by reacting stoichiometric amounts of primary amines and carbon disulfide in a cold alcohol solution. Subsequent purification was by recrystallization from absolute ethyl alcohol solution. Evaluation was through froth flotation of a mill tailing containing 0.2 percent lead. Results show that maximum recovery (38 percent) was obtained with the reagent containing 8 alkyl radicals, but that maximum rougher concentrate grade (4.8 percent) was obtained with the reagents of intermediate number of radicals.

Jan 1, 1962

By H. A. Dierks

Implementation of the joint Federal-State control program established in 1955 to cope with the mine water problem in the Pennsylvania anthracite region is described in this report. The increasing severity of the water problem in the anthracite mines has necessitated major adjustments as this continuing program has progressed. Since 1941 the Federal Government has recognized the mine water problem as an important factor in the worsening economic condition of the anthracite region by initiating scientific and technologic investigations and establishing the Anthracite Flood-Prevention Section in the Bureau of Mines in 1948. On the basis of comprehensive investigations and studies, the results of which were published in numerous reports and bulletins, the Anthracite Mine Drainage Commission of the Commonwealth of Pennsylvania formulated a plan that served as a background for legislative action in 1955, resulting in Public Law 162, 84th Congress (Act of July 15, 1955 (69 Stat. 352; 30 U.S.C. 571-576)), for the Federal Government, and Act No. 82 of the General Assembly, July 7, 1955, for the Commonwealth of Pennsylvania. The report covers 29 mine flood control projects approved and executed in implementing the aforementioned legislative acts. Essential engineering and cost details for each project are given, together with an evaluation of the effect that the installed facilities have on alleviating the mine water problem as it concerns individual mines and the anthracite industry as a whole.

Jan 1, 1962

By R. L. Gall

This report describes Bureau of Mines experiments in gasifying coal in a helium-heated tube-coil reactor. The purpose of this work was to investigate helium as a medium for transferring heat from a nuclear reactor to gasify coal or for use as high-temperature process heat. A laboratory-scale system was designed and constructed to demonstrate feasibility. In preliminary tests with this system, in which the coal was fed as a water slurry, the helium-heating and recycling equipment operated well. Considerable difficulty was experienced, however, in preheating coal slurry to the desired range of 400° - 1,000° F. without plugging the preheaters. Five different preheaters plugged with coke or with salts leached from the coal. The longest operating period wan 12 hours. These difficulties were partly due to the relatively small equipment and flow rates. The gasifier processed l pound per hour of low-rank coal at 300 p.s.i.g. and 1,800° F., with the carbon conversion limited to 20 to 30 percent by the short residence time and slow heat-transfer rate.

Jan 1, 1962

By Thomas P. Meloy

Floating "fines" differs from floating "sands" because the fines have a much larger surface area compared to their mass. The forces that arise from this large specific surface the key to understanding the behavior and treatment of fine particles. Though the nature of these forces is not thoroughly understood, enough work has been done to give a qualitative picture of what is happening in a flotation cell. It is the purpose of this chapter to re-examine some of the more, recent theoretical work and-to indicate its importance.

Jan 1, 1962

By L. A. Roe

The year 1867 marks the first year of commercial production of phosphate rock in the United States. South Carolina produced almost all of the domestic output of mineral phosphate until phosphate mining began in Florida in 1888. During the period 1868 to 1949 the total marketed production of domestic phosphate rock was about 186 million long tons of which 71.5 percent was produced in Florida, 18 percent in Tennessee and 7 percent in South Carolina (1). From 1949 through 1960, Florida phosphate rock production has ranged Prom 71 to 77 percent of the total domestic production. Since three-fourths of the domestic phosphate production is from the Florida field, and since most of the phosphate from the Tennessee and Western fields is not processed, but used directly as electric furnace burden, this paper will concern itself almost entirely with water requirements for mining and processing ore from Florida. Figure 1 summarizes phosphate rock production for Florida vs. total United States production over the period 1947-1960.

Jan 1, 1962

By Richard S. Watt

The Bureau of Mines is often called upon to analyze the demand for various minerals and fuels and to make projections of the future demand. Because minerals and fuels are raw materials and because the demand for raw materials [pends] on the demand for finished goods, these projections are usually [conned] with derived demand rather than final demand. In order to obtain quick [d] reasonably accurate analyses of the demand for mineral commodities, the [reau] developed a method and has used it successfully (31).4 To illustrate the [thod], this report presents a full analysis of the demand for a mineral commodity with enough general theory to permit application of the method to any mineral. Sodium chloride (common table salt) was chosen as the subject of the analysis because the demand for it is less complicated5 and permits a simple application and clear presentation of the method.

Jan 1, 1962

By D. W. Bridges

Solvent extraction has become important in recent years as a unit process in extractive metallurgy. The flexibility and simplicity of the technique have attracted widespread attention, and numerous papers describing actual and projected metallurgical applications have been published. However, differences in terminology, procedure, objectives, and standards, as reflected in reports by different operators and investigators, have sometimes made appraisals and comparisons difficult. Consequently, a need appeared for n series of basic reports on the subject. This Bureau of Mines Information Circular is the first of such a series. It deals with the status of solvent extraction in metallurgy, as well as with the rudiments and terminology of the unit operation. In analytical chemistry, extraction of molecular species from aqueous media by immiscible organic solvents has been used for many years to separate and determine chemical elements (61).4 Complex chlorides of iron and other metals are readily soluble in ethers and ketones, as are the nitrates of uranium and thorium. Most metals are extractable as complex salts of some organic reagent, such as dithizone, 8-hydroxyquinoline, or cupferron.

Jan 1, 1962

By A. C. Johnson

This circular is one of a series published by the Bureau of Mines describing mining and beneficiation methods and costs at various mining operations throughout the United States. Inclusion of the Abbott mine in this series is of particular interest, as the complex geology and the character of the deposits make their exploitation a unique operation. The mine operates on a high-cost, comparatively small-scale basis, and only the persistence of an aggressive management has enabled it to maintain its rank among the major mercury producers of California. Rising costs and decreasing metal prices, which continuously threaten the low profit margin, are reflected in increased efficiency of operation. This report summarizes past operations and describes, in detail, the geology and ore deposits; exploration and mining methods; and furnacing and condensing operations. It covers the entire operation from initial exploration to the actual production of mercury. Comparative production costs for 1944 and 1958 are of special interest.

Jan 1, 1962

By Hudson S. B

With a particular electrode configuration, and a particular combination of electrode voltage and roll speed, a relatively small increase in electrode voltage, or a relatively small decrease in roll speed, resultsin a marked improvement in the separation of zircon from ilmenite. In general, fine minerals can be separated using a higher roll speed, or a lower electrode voltage, than is required to separate coarse minerals. The ionizing electrode should be reasonably close to the point at which mineral is fed on to the roll, and nearer to the roll than the non-ionizing electrode. The optimum conditions for the separation of zircon from ilmenite may not apply for the separation of other non-conductors from other conductors.INTRODUCTIONAlthough the high tension separators used in the Australian beach sand industry are efficient, this efficiency has been gained very largely by a process of trial and error, and not by a systematic study of the effects of changes in the operating variables. The optimum roll speed for a particular electrode position and electrode voltage, and the optimum electrode voltage for a particular roll speed and electrode position, can both be determined quite readily. It is not so simple to determine the optimum electrode position for a particular electrode voltage and roll speed. The reason for this is that the electrode used in high tension separators consists of two parts-an ionizing and a non-ionizing electrode respectively. The angular and radial positions of these electrodes, relative to the feed roll and to each other, affect the behaviour of conductors and non-conductors to varying degrees.

Jan 1, 1962

By L. M. Burman

The phase-boundary pressure required to maintain a natural hydrocarbon fluid in a single phase must be considered in planning the recovery of reservoir liquids by miscible-phase processes. The change in the phase-boundary pressure at reservoir temperature that results when a light component or a mixture of light components is added to a reservoir fluid is an especially important consideration. The cricondenbar pressure (maximum phase-boundary pressure) and the critical pressure are unique correlated pressures that have been utilized to calculate the change in phase-boundary pressure that may result when the composition of a reservoir liquid is altered by an additive. In this study one reservoir oil and three gas-condensate fluids are used as examples. Correlations pertaining to the critical and cricondenbar states in chapters 4 and 5 of Bureau of Mines Monograph 10 (3)5 were used to demonstrate how butane and lighter components added to these reservoir fluids affect their phase-boundary pressures.

Jan 1, 1962

By L. H. Banning

This investigation was undertaken to obtain basic information necessary for the design and operation of a plant for recovering metallic values from nickeliferous laterite and serpentine of the Philippine Islands. It was divided into three parts: (1) Mineralogical studies and preliminary mineral dressing tests; (2) electric smelting of the ores, upgrading of ferronickel by blowing with oxygen, smelting laterite slag to produce crude iron, and the production of mild steel; and (3) nickel and cobalt recovery from upgraded ferronickel. Results of the investigation indicate that it should be feasible to recover nickel, iron, and possibly cobalt products from the laterite and ferro-nickel from the serpentine. Mineralogical studies were made on representative fractions of the laterite and serpentine tonnage samples and on five selected samples; mineral dressing tests were made only on laterite. The nickel occurs principally associated with hydrous iron oxides and chemically combined with serpentine; garnierite was the only discrete nickel mineral identified, and it was found in a highly decomposed serpentine. The bulk of the cobalt was found in wadlike manganese oxide material. Approximately twice as much chromite was found in the laterite as in the serpentine, By mineral dressing techniques, laterite was separated into two fractions: one fraction contained over 90 percent of the nickel and cobalt, and 83 percent of the iron; the other fraction contained 74 percent of the chromium. A cobalt concentrate (1.1 percent Co) was produced by a scrubbing and sizing procedure.

Jan 1, 1962

By C. R. Montgomery

Coal companies in order to supply their customers En the metallurgical market, both home and abroad, must be able to control their production in order to meet carbonization specifications over and above those of the proximate analyses which has been the prime consideration of purchases in the past. It is the purpose of this paper to review in brief some of the tests used and give data to show the application of such as it applies to the customers needs. It is now recognized that coal is not homogeneous in any of its properties and an amazing fact is that it has been used for so long a time as the principal raw material for the manufacturing of coke without more emphasis having been placed on the variation between coals; yes, even from coals in the same seam at different geographical locations, Recently Kuchta and Clendenin pointed this fact out In a study of the(1) carbonizing behavior as related to chemical and plastic properties of Alabama medium volatile coal.

Jan 1, 1962

By A. Gene Collins

Potassium, lithium, strontium, barium, and manganese are present in many oilfield brines, None of them except barium is determined routinely in brine analyses. Therefore, sensitive and accurate flame-spectrophotometric methods were developed. Potassium, lithium, and strontium were determined by a standard-addition technique in ethyl alcohol solutions. Barium and manganese were determined in ethyl alcohol and normal propyl solutions, respectively, after interfering substances were removed.

Jan 1, 1962

By R. R. Lowery

This project was proposed to provide information on the hazards associated with arc melting of thorium. A general air-sampling analysis was made to determine the separation, concentration, and distribution of thorium daughter (decay) products throughout arc melting, machining, and forging processes of a thorium handling facility. The value of well coordinated health physics program is stressed in connection with potential health hazards and personnel protection. Building, equipment, and exhaust ventilation requirements for such a facility are discussed. Special handling methods are described for thorium. INTRODUCTION The Bureau of Mines at the Albany Metallurgy Research Center has been involved in handling the naturally radioactive metals, uranium and thorium, for several years. Cooperative work for the Atomic Energy Commission has been carried out with thorium metal, and as a result the concerned laboratories of the Center have accumulated experience on the hazards associated with this metal. This report details the radioactive hazards arising from the arc melting, machining, and forging of thorium.

Jan 1, 1962

The Kingsgate molybdenite pipes are considered on petrochemical data and field occurrence to be, possibly, epi-magmatic plutonic offshoots grading into hydrothermal bodies. There is reason to believe that the ore is derived from a highly acid granite of type similar to that of the tin bearing areas of northern New England. The mineralogy, microtextures and paragenesis of the ore are discussed.INTRODUCTIONThe Kingsgate Mining Field is situated in steep, heavily timbered terrain 18 miles E.N.E. of Glen Innes and 430 miles north of Sydney. Bismuth and molybdenum ores were discovered at Kingsgate (Yarrow Creek) in 1877. Subsequently some 50 pipes were developed yielding tonnages which at the peak of operations, 1905 to 1920, rivalled production from the rich deposits of northern Queensland.Attempts to revive the field have been made periodically and small parcels of ore have been forthcoming.' During World War II demand for piezioelectric quartz again focussed attention on Kingsgate but twinning and other imperfections of the quartz prevented all but a minor exploitation of the otherwise noteworthy crystals of this locality.There is reason to believe that the ore at Kingsgate is not exhausted through exploration and mining costs would probably be high due to the capricious nature of the pipes and to the irregular distribution of rich ore shoots within them.

Jan 1, 1962