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By J. T. Dunham

Zirconium has possible use in industry where severe corrosion conditions are encountered because it resists attack from a variety of corrosive environments. However, very little experimental testing has been done to evaluate the corrosion behavior of zirconium when simultaneously subjected to high tensile stresses and exposed to corrosive environments. This investigation was initiated for an evaluation test, but was limited to environments consisting of ferric chloride solutions which were known to attack zirconium and were shown to promote stress-corrosion cracking in preliminary tests. Tests for cracking susceptibility were conducted by the Bureau of Mines to show the effect of stress, solution concentration, air aeration of solution, and the method of mechanical processing. Tensile stress was applied to the specimens by a constant-load method which proved more reliable than a constant-strain method.

Jan 1, 1961

By R. W. Smith

The Bureau of Mines has been engaged in a systematic evaluation of the thermodynamic properties of combustion gases. These studies were designed to provide basic thermodynamic information of high accuracy, facilitating the theoretical study of flame and combustion phenomena.4 This report is the fifth of a series5/ presenting results of the study for particular fuel-oxidant systems. These calculations have as their objective the constant pressure flame temperature of acetylene-air for a range of pressures.

Jan 1, 1954

By T. L. Johnston

A review of technical literature of the last quarter century discloses that much experimental work has been carried on in an effort to develop commercial processes for making sponge iron. In addition to the work that has been recorded, other work has been done the results of which have not been published. The degree of success or failure of these investigators does not detract from the fact that the problem has its challenging aspects and practical possibilities that encourage further investigation. The purpose of this report is to record information derived from recent experimental work that .had its 'objective the development and demonstration of one method of producing sponge iron. Work of other investigators was studied and applied wherever possible.

Jan 1, 1948

By Joseph A. DeCarlo

The rapid growth of the organic chemical industry in the United States and abroad has focused attention on the future raw-material sources for this important industry. Chemical products are essential to modern civilization; and millions of tons of organic chemicals are used annually, ranging from basic raw materials to finished chemical products such as drugs, cosmetics, and soaps. Hundreds of chemical products are made directly or indirectly from coal, but in this report "coal chemicals" will be limited to crude tar, crud light oil, and ammonia recovered in the high-temperature carbonization of bituminous coal and the important principal products obtained by processing these materials. Specifically these include benzene} toluene, xylene, naphthalene, creosote oil, tar acid oil, pitch, and ammonium sulfate. Therefore the term "coal chemicals", wherever used in this report, includes only these products and does not include the secondary or intermediate products such as styrene, synthetic phenol, aniline, phthalic anhydride, or finished products made from these, such as synthetic rubber, plastics, and dyes. The United States leads the world in production and consumption of coal chemicals. In the past five years nearly one-fourth of the total output of coal-tar crudes in the world was produced in the United States. Consumption of some of the more important products derived from these crudes such as benzene, toluene, xylene, and naphthalene, however, ranged from about one-third to one-half of the world total because of imports and production of benzene, toluene, and xylene from petroleum. The synthetic organic chemical industry of the United States was established during World War I on chemical raw materials obtained by the high-temperature carbonization of bituminous coal but this source of supply currently furnishes less than 40 percent. More than 60 percent of the chemical raw materials used to produce organic and inorganic chemical is supplied by the petroleum industry and production of petrochemicals is rising rapidly.

Jan 1, 1960

By F. P. Haver

The Bureau of Mines has investigated the electrochemical reduction of lead chloride as a method for producing lead without the pollution problems associated with smelting. It was determined that high-purity metal (>99.9 pct Pb) could be obtained, using PbC12 prepared by ferric chloride leaching of galena concentrate: PbS + 2FeCl3?PbCl2 + 2FeC12 + S°. Optimum results in small-scale electrolytic tests were achieved with a bath consisting of 40 to 70 wt-pct PbCl2 dissolved in KC1-LiCl eutectic, an operating temperature of 450° C, a current density of 2.5 amp/in2, and an electrode spacing of 0.5 inch. In large-scale tests made to develop a cell design for commercial application, the optimum electrode arrangement proved to be a bipolar configuration with horizontal plates. This gave a current efficiency of 86 pct with an energy requirement of 0.52 kwhr/lb lead. To determine the effect of impurity buildup in the bath, 1,200 lb of PbC12 prepared by ferric chloride leaching of galena concentrate was electrolyzed over a period of 2 months. Little deterioration of the metal quality occurred in that time; all of the lead produced had a purity equal to or better than corroding grade (>99.94 pct Pb).

Jan 1, 1976

By D. L. Sawyer

The Bureau of Mines studied alumina extraction from uncalcined, kao-linitic clay at temperatures from 1000 to 2500 C using 20-or 27-wt-pct-HCI concentrations and with an acid-to-clay ratio of from 0.8 to 1.4 times stoichiometric. Autogenous digestion pressures ranged from atmospheric pressure to about 900 psia. Extraction of 96 pct of the alumina was obtained by HCI leaching at temperatures and leaching times that varied from 1000 C for 120 h to 2000 C for 15 min. Hydrochloric acid stoichiometry of the reaction A1203'2Si02'2H20 + 6HCI + 2AICl3 + 2Si02 + 5H20 was studied at different temperatures and leaching times in a 750-mL tetrafluoroethylene-polymer-lined autoclave. A combination of high temperature and 20 wt pct excess HCI promoted rapid and almost quantitative extraction of alumina (99 pct in some tests). Additional Bureau data obtained with 35-mL tantalum bombs and leach-ing tests with added fluoride are also provided. At high temperatures, the addition of fluoride did not result in a significant improvement over HCI alone and was deleterious to the filtering properties of the digest residue.

Jan 1, 1985

By H. C. Fuller, E. L. Anderson, F. S. Wartman, M. A. Cook

"This paper gives an account of the production of ductile-grade titanium powder in 100-pound batches by reduction of purified titanic chloride with magnesium, followed by grinding, leaching, and magnetic separation of the reaction product. Apparatus, technique, and methods of controlling product quality are described, and some data on operating costs are given.Although man has been aware of the existence of the element titanium for over 150 years, only recently has the metal itself been available in a form pure enough, particularly with reference to absorbed gases, to allow an estimate of its physical properties. In comparison with mild steel, the tensile strength of titanium is about the same, the resistance to atmospheric corrosion greater, and the specific gravity much less.These properties suggest the usefulness of titanium as a structural material for applications requiring resistance to atmospheric attack and a good strength-weight ratio. Although known reserves of titanium, high-grade enough to be useful at present are not sufficiently extensive to predicate that titanium might supplant iron, aluminum, and magnesium for structural purposes, the reserves are large enough to make its use as a structural material quite feasible in certain fields in which its unique properties are required.As a result of these considerations, the Bureau of Mines station at Tucson initiated an, investigation into the technology of titanium in 1938. First, a critical survey and small-scale trial of virtually all suggested methods7/ for producing the metal was made. The method devised by Kroll8/ seemed best adapted as a source of metallic titanium for, although the purity of the product was not as high as that of products from some other processes, it seemed that modifications in technique necessary for larger-scale production could be made more easily.Essentially, in applying the Kroll process, titanium tetrachloride was reduced to metallic titanium by adding the chloride slowly to molten magnesium contained in a molybdenum-lined iron reaction chamber filled with a protective atmosphere of argon. After reduction to the state of completion desired, the reduction mass and chamber were allowed to cool. Then the chamber was opened, and the reaction mass, consisting of titanium, magnesium chloride, and some unused magnesium, was removed by suitable means. Most of the magnesium chloride and metallic magnesium were removed by leaching in dilute hydrochloric acid. The leached sponge was then ground wet in a ball mill, releached in strong acid, and dried Removal of free iron by magnetic separation completed the production process.Development of the Kroll process by the Bureau was undertaken first at the station at Salt Lake City, in 1942 and the amount formed per run was increased in several steps from a few grams to pounds.9/ In addition to increasing the size of batch over that used by Kroll, the technique was simplified somewhat by the use of unlined reaction vessels."

Aug 1, 1949

By H. J. Kelly

[This investigation of the refractory properties of seven Pacific Northwest chrome ores and concentrates has shown that five of the ores and one of the concentrates are suitable for making refractories and that all may be used in combination with high-grade chromite. The specific objectives of the investigation were to determine the inherent physic al and chemical characteristics, to shapes using each of the chrome ores and concentrates, to compare the refractory qualities of the laboratory-prepared with commercial chrome refractories. As far as possible, standard tests were used as criteria.]

Jan 1, 1952

By Jeffrey P. Schubert

The study site in northeastern Illinois underwent surface mining for coal in 1943 and was reclaimed by the state of Illinois in 1972-1973. Additional soil amendments and seed were applied to the spoil surface in 1975-1980. Previous studies in 1975-1978 had shown that the surface spoil materials and five final-cut lakes at the site were quite acidic and the lakes contained high concentrations of sulfate and dissolved metals. Surface runoff water from monitoring plots in 1976 were only moderately acidic and the mean concentrations of most dissolved metals and sulfate in the runoff waters were less than 25% of the concentrations found in Lake B. By 1980, vegetation had become well established over most of the mined area. However, the five final-cut lakes (Lakes A-E) remained acidic. The purpose of the study reported here was to determine the physical and geochemical subsurface conditions of the spoil materials, the hydrologic flow system within the spoils, and the magnitude of acidic spoil leachate migration into the lakes and into the wetland prairie north of the mine site. Lakes A, B, C, and E were still very acidic in 1980-1981 (pH range: 2.9-3.4; aridity range: 110-860 mg/L as CaCO3). Lake B had the worst water quality, with mean concentrations of dissolved aluminum, iron, manganese, and sulfate of 75, 25, 37, and 3340 mg/L, respectively. Shallow groundwaters in spoil materials around Lake B had a lower pH and about two to four times greater concentrations of aridity, aluminum, manganese, zinc, and other metals and nearly 20 times greater dissolved iron than the water in Lake B. The shallow groundwaters in undisturbed soils and bedrock 10-30 m north of the mine site spoils generally were alkaline, but did contain occasional moderately high sulfate and metal concentrations. Pumping tests and recovery tests conducted in piezometers showed hydraulic conductivities of spoil materials ranging from less than 10- to 10-5 m/s; hydraulic conductivities of natural soils and bedrock were measured between 10-10 to 10-7 m/s. Water levels in spoil materials increased rapidly in response to rainstorm events and the recession curves were relatively quick to decline, lasting only two or three days. Quick infiltration of rainfall into the spoil surface and percolation down to the water table caused a rise in groundwater levels and movement of spoil groundwater into the lakes. This groundwater component in the lake water budgets could account for most of the water quality problems occurring in the acid lakes.

Jan 1, 1984

By Bolmerm R. L.

This information circular describes the application of modern methods and equipment in sinking a vertical, 916-foot-deep by 16-foot-diameter, concrete-lined access shaft for the Harold D. Roberts tunnel near Montezuma, Colo. Although the access shaft was merely a construction facility to expedite completion of a 23-mile water-diversion tunnel, a circular shaft of this type would be equally adaptable for mine development or other purposes. Comparable sinking methods and equipment could be used for similar shafts within a wide range of sizes and depths. SUMMARY In addition to excavation and support of the basic access shaft to tunnel grade, the overall sinking project involved initial preparation of a surface site and plant, subsequent construction of a tunnel-level station and loading pocket at the shaft bottom, and ultimate conversion of the basic shaft into a hoisting and access facility for tunnel operations. The sinking period for the basic shaft approximated one year. Actual tunnel operations through the converted shaft began on April 3, 1958, approximately 19 months after the project was initiated.

Jan 1, 1961

By M. D. Marshall

A remote heat-activated stench gas/tracer gas mine alarm system was developed to reduce the time between fire detection and personnel notification. The stench gas/ tracer gas system contains ethyl mercaptan for personnel warning and a fluorocarbon for tracer gas detection by instrumentation. A system was also developed which can be interfaced with multiplex mine phones. In-mine tests were conducted and several systems are presently installed in a hard rock mine.

Jan 1, 1983

By Davis E. Traut

TiC14, AIC13, and VC14 were coreduced simultaneously via a Kroll-type magnesium reduction to form an alloy sponge as part of a research effort by the Bureau of Mines to produce titanium alloy powder. Reduction tem-peratures of 750°, 850°, and 950° C, a range of chloride feed rates from 34 to 152 Ib/(ft2·h), and crucible diameters of 7-3/4 and 10-1/4 in were tested. Microprobe analyses using a 40-um-diam spot showed no effect on alloy microhomogeneity (distribution of Al and V in the Ti, considered critical as a powder property), due to changes in process variables within these ranges. Statistical analysis of these data for alloy sponge indicated greater variation in the chemical composition (AI and V) than that found in commercial Ti-6Al-4V plate or Plasma Rotating Electrode Process (PREP) powder. Therefore, a one-step approach to pow-der, such as grinding the Ti alloy sponge, would not produce a powder product of acceptable chemical homogeneity. An approach that homoge-nized the sponge, such as with a melting step, would produce an accept-able powder product with respect to chemical homogeneity.

Jan 1, 1987

These proceedings consist of an overview of the in situ mining research currently being carried out by the Bureau of Mines. The following papers emphasize two general aspects of the in situ mining method: the environment and productivity. Both areas are extremely important, particularly because in situ leach mining is a relatively new mining method from a commercial point of view. Topics covered include the restoration of ground water, the selection of lixiviants, in situ mining of commodities other than uranium, in situ mining costs, the application of resistance measurements to in situ mining, an acid leach mining case history, and the use of branched boreholes for in situ mining. A bibliography of Bureau of Mines publications on in situ mining is appended.

Jan 1, 1981

By J. Frederick Stampfer

Current certification testing of self-contained breathing apparatus includes tests with human subjects wearing the apparatus while exercising. During these tests, certain apparatus variables are measured during rest periods. Because of concerns that the present tests may not accurately simulate the stresses to which an apparatus is subjected in the field, the Bureau of Mines proposed new human subject tests. It was also felt that different measurement techniques would supply more reliable data on the apparatus response to these stresses. The Los Alamos National Laboratory was asked by the Bureau to evaluate the proposed tests and monitoring techniques. The major conclusions derived during this study are these: (1) The proposed tests are not too physically demanding. (2) As long as human test subjects are used, a minimum subject weight should be required for certification tests. (3) Important apparatus variables are the breathing resistance, temperature, and carbon dioxide and oxygen concentrations of the inhaled gas. (4) Continuous monitoring should be used, rather than monitoring only during rest periods. (5) New pass/fail criteria based on realistic estimates of the user's physiological requirements, as tempered by present and future engineering limitations, are needed. (6) When available, breathing machines, rather than human subjects, should be used for most certification testing. (7) A more realistic ergonomics test than that proposed is needed. (8) A gas leak test for the system and a facepiece leakage test are also needed.

Jan 1, 1983

By R. A. Cattell

The peacetime activities of the Bureau's petroleum and natural-gas program have been reoriented to serve the needs of a national-defense program. When the United Nations sent troops to Korea after the North Korean Army crossed the 38th parallel in the latter part of June 1950, the Bureau's coordinated national program on petroleum and natural gas, with each major project forming an essential member of its framework, was carefully reviewed by those in charge of the work. As a matter of fact, the era of normalcy in which the petroleum and natural-gas research of the Bureau of Mines prospered during the fiscal year 19502/ was no sedative to the need for alertness on a national-defense front. The program, although conducted along peacetime lines in general, was scanned critically and repeatedly during that period to see where - if the need should arise -the emphasis could be shifted from peace to defense or war. Judging from the experience of two wars, it would not be long before the Bureau would be asked to use its trained technical personnel in applying techniques already learned in peacetime research to the requirements of munition and fuel needs of national defense. Near the end of January 1951, petroleum and natural-gas engineers of the Bureau of Mines began a comprehensive study of reservoir conditions in the Canyon Reef fields of Scurry, Borden, and Kent Counties, Tex. This work was preceded by published analyses of crude oils from Scurry County as early as April 1950. Well-informed persons in industry have estimated that these fields hold reserves that will yield 3 to 6 billion barrels of stock-tank oil. Although generally accepted good operating practices have been followed, engineering tests have shown that the natural energy, except in some favorable parts of the reservoir, will not be adequate for obtaining a high percentage of recovery. Correct information regarding the extent and availability of this vast reservoir of hydrocarbons is therefore of great concern to the Petroleum Administration for Defense in carrying out its responsibilities under the Defense Production Act.

Jan 1, 1952

By Oliver C. Ralston

[This paper is an expmded revision of a report entitled "Froth Flota- tion and Agglomerate Tabling of Honmetdlic Idinerds, " published in Trans- actions of the Canadian Ir-stitute of Iriining and !,letdlurgy (vol. 40, November 1937, pp- 6? 1-726) and al'enared a year pr~viousl:~. Revisions en'oodied herein brinc the &ta I:T to Jn?uac"g 1, 193;. References have also been added to make the earlier paper more complete for the period it covered. This paper is an expmded revision of a report entitled "Froth Flota- tion and Agglomerate Tabling of Honmetdlic Idinerds, " published in Trans- actions of the Canadian Ir-stitute of Iriining and !,letdlurgy (vol. 40, November 1937, pp- 6? 1-726) and al'enared a year pr~viousl:~. Revisions en'oodied herein brinc the &ta I:T to Jn?uac"g 1, 193;. References have also been added to make the earlier paper more complete for the period it covered.]

Jan 1, 1938

By Oliver C. Ralston

The Nonmetals Division studies problems relating to the use of minerals, many of which are important to national defence for purposes other than the extraction of metals. In fact, virtually all of the work of the division has been diverted to investigations pertaining to better use of the Nation's natural nonmetallic is resources as weapons of defense. The experiment stations of the division are at Norris, Tenn.; Tuscaloosa, Ala.; Seattle, Wash.; and College Park, Md. Studies involving the application of electric power to the nonmetallic minerals are conducted at the Electrotechnical Laboratory at Norris, and investigations on mineral-dressing treatment are conducted mainly at the Southern Experiment Station at Tuscaloosa. The cleaning and preparation of coal are studied at both Tuscaloosa and the Northwest Experiment Station Lit Seattle (other projects relating to utilization of coal are conducted by the Coal Division of the Bureau of Mines). Problems covering the use of minerals and fundamental problems as to their properties are studied at College Park.

Jan 1, 1941

By Oliver C. Ralston

[This paper is an expanded revision of a report entitled "Froth Flotation and Agglomerate Tabling of Nonmetallic Minerals, " published in Transactions of the Canadian Institute of Mining and Metallurgy (vol. 40, November 1937, pp- 691-726) and prepared a year previously. Revisions embodied herein brine the data up to January 1, 1938. References have also been added to make the earlier paper more complete for the period it covered.]

Jan 1, 1938

By Richard A. Thomas, Michael J. Sapko, Gary L. Mowrey, William D. Monaghan, Michael A. Trevits

Over the years, more than 20,000 mine seals have been erected in underground coal mines in the United States. Seals are used extensively in underground mines to isolate worked-out areas, active mine fire zones, and to control water inundations. Seals are most often built directly in the mine and can be fabricated from blocks made of wood or cementitious material. Recently, several explosions occurred within sealed areas of underground U.S. coal mines. These explosions, believed to be initiated by lightning strikes on the surface, destroyed numerous seals and caused considerable damage external to the sealed area. The National Institute for Occupational Safety and Health is conducting research to develop design guidelines, to investigate noninvasive techniques to characterize seal strength properties, and to evaluate seal test methods. As part of this work, a 30-ft wide, 16.1-ft tall and 4-ft thick seal was built in an underground experimental mine using cement and foamed water. Two types of noninvasive techniques are currently being investigated, namely the Schmidt Hammer for measuring compressive strength and ground penetrating radar (GPR) for detecting the presence of anomalies (e.g., voids, discontinuities) within the seal. Once these noninvasive tests were completed, the seal was subjected to destructive explosion testing. This study presents the results of the Schmidt Hammer tests, GPR scans, and the characteristics of seal failure during explosion testing.

By Richard I. Barnhisel

At the Sinclair Study Site it was found that the deeper the soil the greater the yield of corn, soybeans, wheat, alfalfa, and timothy. Yields at this location were generally lower than those at the Alston Surface Mine. At Alston the non-prime land treatments generally produced greater yields for all crops than did the prime farmland treatments, however, the intermediate soil thickness, 20 cm topsoil over 40 cm of subsoil, gave the best yields, provided it's subsoil had been limed. From a chemical point of view, acidic spoils do not need to be buried by 120 cm or 4 feet of soil, provided adequate lime is applied to these spoils as a barrier prior to placement of good quality topsoil and only forage crops are to be grown. The burial depth must be increased to as much as 75 cm when grain crops such as corn or soybeans are to be grown. This response to burial depth appears to be related to water storage needed by the crop and not due to toxic effects of the spoils. A conventional farm tractor-mounted subsoiler increased yields of soybeans and corn the first one or two years, but the effect was diminished with time. Subsoiling did not produce significant increases for alfalfa or wheat. However, ripping with a bulldozer produced significant yield responses, especially for corn and soybeans, that have lasted for at least three years. The ripping effectively reduced the bulk density at least within the zones through which the ripper had passed. Liming the upper 20 cm of subsoil significantly increased yields of alfalfa, corn, and soybeans. There also appeared to be an interaction between this lime treatment and soil depth. Yields of some grain and forage crops may be high enough to meet target levels for bond release for prime farmland. Based on the present study, one should not expect corn yields to be high enough to meet bond release. This statement should not be considered final since the experiment is not complete.

Jan 1, 1983