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By D. J. Stoops, H. Kato, M. D. Carver

The effects of impurity elements silicon , aluminum, copper , nitrogen , and manganese , at 50 to 300 ppm, on properties of the zirconium alloy Zircaloy 2 were investigated . Variations in microstructure , mechanical properties , and corrosion behavior in some inorganic acid and salt solutions were observed with variations in level of impurity element . Corrodents were solutions of sulfuric acid , phosphoric acid , copper chloride , and iron chloride . Silicon was found to modify annealed microstructures by spheroidizing and dispersion of secondphase material throughout grains . Silicon or manganese improved ultimate and yield strength of the alloy without loss in ductility . All five elements affected corrosion rates of the alloy , the effect being generally different for each element .

Jan 1, 1964

By Marvin E. Lane

This paper , which describes the mining methods and practices at the Hayden Creek lead mine of St. Joseph Lead Co. in southeast Missouri , is one of a series being prepared by the Bureau of Mines on mining methods , practices , and costs in various mining districts of the United States . The Hayden Creek mine is in the W 1/2 sec . 7 , T. 36 N. , R. 4 E. , St. Francois County , Mo. , about 1 mile southwest of the town of Frankclay ( fig . 1) . The mine is on the west edge of the mining district known as the Lead Belt . However , neither the ore body nor the underground workings are connected with those of any other mine in the district . In contrast with most operations in the district , underground haulage is entirely trackless , and nearly complete delineation of the large , well -defined ore body by drilling permitted comprehensive planning of development and mining in advance of shaft sinking . The ore differs in character and occurrence from that of the main ore deposits in the Lead Belt in that the lead mineral , galena , occurs in the dolomitic matrix enclosing granite boulders instead of in dolomite limestone .

Apr 1, 1957

By R. J. Leary

Oxidation testing of copper-clad steel strip was performed in a muffle furnace to determine whether copper in contact with steel scrap could be removed by oxidation in an airstream at high temperatures. Substantially all of the copper was oxidized before any significant iron oxidation occurred. The rate of copper oxidation was not affected by contact with iron. Copper oxide scale separated spontaneously from the underlying metal during cooling. Results indicate the possibility of removing light-gage copper coatings and components from ferrous scrap by oxidation in an incineration process.

Jan 1, 1965

By Kenneth G. Broadhead

The objective of this rare-earth oxalate study by the Bureau of Mines was to determine systematically by radiochemical techniques what effects, if any, could be attributed to the several variables--temperature, digestion time, acid concentration, rare-earth concentration, oxalic acid concentration, stirring, and the presence of other rare-earth ions. A Latin Square experimental design was used to evaluate statistically some of the variables. Precipitation losses ranged from near zero to about 7 percent, and mineral acid and rare-earth concentration were the predominant factors affecting completeness of precipitation. Quantitative oxalate precipitation of the rare-earth elements was achieved by controlling the experimental conditions as follows: (1) Maintaining rare-earth concentrations above 0.01M; (2) stirring the mixture several minutes after precipitation; (3) using an adequate (two to five-fold) excess of oxalic acid; (4) precipitating at room or iced temperature and digesting for at least 1 hour; (5) avoiding an excess of mineral acid and, if possible, maintaining the pH above 2.0; and (6) avoiding excess complexing agents such as EDTA (ethylenediaminetetraacetic acid). In the past 20 years research aimed at developing more efficient separation and purification techniques applicable to the rare-earth elements and yttrium has been extensive. Common to most of these procedures has been the use of oxalic acid to precipitate this group of elements selectively. However, this particular use of oxalic acid has a much earlier origin; its application in precipitating yttrium was first reported by Mosander (8)4 in 1843. Despite long and popular employment of this technique, only limited and somewhat conflicting data are available regarding the many factors affecting the degree of rare-earth oxalate precipitations.

Jan 1, 1961

By J. M. Kuchta

Concentrated hydrogen peroxide (H202) is a highly reactive oxidizing agent that liberates heat when it decomposes. The heat liberated may be sufficient to ignite combustibles with which the peroxide comes in contact. For this reason, concentrated hydrogen peroxide should be handled only by personnel familiar with its many unique properties.6 Hydrogen peroxide is used as a bleaching agent in the manufacture of textiles; this is its major single use in the United States. It is also employed as a reagent in chemical synthesis, as a source of free radicals to start polymerization, as a foaming agent in the manufacture of porous substances, and for its effect on biological processes. Moreover, highly concentrated hydrogen peroxide is a compact source of energy that can be utilized both as a monopropellant and as the oxidizer in a bipropellant system, During World War II, large quantities of highly concentrated hydro- gen peroxide were used as propellants, particularly in Germany. Since then, production of the peroxide has increased rapidly; in the United States alone it has more than doubled since 1950.7 Because of its widespread use, increasing interest has been shown in the hazards of handling the high- strength peroxide.

Jan 1, 1961

By M. A. Mahtab

This report presents a new procedure for analyzing the orientations of rock fractures in an engineering site. This procedure, coded in a computer program, identifies clusters or groupings among the fracture orientations and calculates (1) the mean orientation of the fractures within each cluster and (2) the dispersion or scatter among these fracture orientations. Data points are represented by intersections of joint normals with the upper hemisphere, which is divided into 100 equal-area quadrilateral patches. The points in adjacent patches where the Poisson distribution test shows significant concentrations are assigned to a single cluster. For a cluster whose fracture orientations follow Arnold's hemispherical normal distribution, a confidence interval for the fracture orientation mean is calculated by applying Fisher's estimates. The technique is applied to the treatment of three examples.

Jan 1, 1972

By C. J. Walker, Ray V. Huff

The feasibility of inert - gas cushions in underground gas storages was studied by the Bureau of Mines in accordance with a continuing program of cooperative research between the natural gas industry -- through the American Gas Association . As mixing of the inert - gas cushion with the stored natural gas is undesirable , the various mechanisms tending to bring about such mixing were the subjects of both theoretical and experimental studies . These studies indicated the practicability of such cushions is dependent upon both reservoir and operating conditions . Equations and tables of illustrative data relating the various reservoir and operating conditions to the expected time required for undesired mixing to occur in ideal reservoirs are presented . This information permits estimating the relationship of such factors in actual storage operations .

Jan 1, 1964

By K. R. Dorman

To further investigate the potential of precast concrete sets as a support medium for underground mines, the Bureau of Mines designed a five-piece precast concrete drift set for a small opening and tested it to destruction in a straining frame. Twenty-seven tests were made with three sizes of members using three loading conditions. In addition, six tests were made with sets in a distorted configuration, Test results and typical failure patterns are presented. A comparison of results with those previously reported for the three-piece set shows the five-piece set supports considerably larger total loads than does the three-piece set of equivalent cross section designed for the same size of opening. Recommendations are made for improvements in design.

Jan 1, 1969

By David Schlain

A small alumina reduction cell with a graphite crucible and boron nitride liner was developed by the Bureau of Mines as the initial phase of a study of the reactions which occur in the reduction of alumina by the Hall-Heroult process. Operating conditions in the cell such as temperature, time, current density, electrolyte composition, and electrode materials may be varied easily. Aluminum was produced in the cell at a current efficiency of about 75 percent and a cell voltage of 2.7 volts. Although the data are not wholly conclusive, the operation of the cell did not appear to be greatly affected by large changes in temperature, electrode spacing, current density, and alumina concentration in the electrolyte.

Jan 1, 1963

By P. C. McWilliams

Researchers at the U.S. Bureau of Mines investigated the use of close-range photogrammetry and subsequent stereo digitizing to obtain data from rock fracture roughness profiles. The photogrammetric process yielded results that were acceptable but somewhat inferior to those obtained by a mechanical profilometer. On the basis of this study, further pursuit of photogrammetry as a data collection method in mining is proposed. Fractal geometry was investigated as a means of measuring the roughness of rock fracture profiles. Four fractal algorithms were used: divider method, modified divider method, box method, and spectral method. A comparison of the methods gave ambiguous results. Brown's modified divider method provided the best means of obtaining the fractal dimension. Shear strength estimates were obtained using the parameters of the modified divider method and Myers' Z2 measure. Because of differences in results when comparing the different ways of obtaining the fractal dimension, future users of fractals in studies of rock fractures are advised to cross-check their results carefully.

Jan 1, 2010

By Robert C. Gabler

Evaluation of incinerated sewage sludge as a secondary resource for aluminum, phosphorus, and minor constituents such as copper and zinc was initiated as part of the Bureau of Mines secondary resource program. The elemental composition of sludge ash for 14 plants in 11 U.S. cities was determined. Comparing industrialized cities with cities where most of the sewage is domestic, significant differences in heavy metal content were noted. Various parameters were investigated affecting the extraction of metals and phosphorus from a typical industrial city sludge ash and from a Palo Alto, Calif., sludge ash with a high precious metal content. Three extraction-recovery procedures for metals and phosphorus using sulfuric acid leaching, ion exchange, and various precipitation techniques were investigated. The last procedure developed was a combination approach using a three-stage countercurrent sulfuric acid leach that recovered most of the economic values from the sludge ash and also removed the leachable fraction of elements of environmental concern.

Jan 1, 1979

By L. P. Larson

In this Bureau of Mines evaluation of the domestic supply position of tungsten, certain tungsten resources in the United States are estimated as to quantity and grade and then are systematically costed in detail (excluding exploration costs). A supply curve is developed which depicts the quantity of tungsten (WO3) up to about 15.5 million short ton units that is producible at calculated price levels ranging from about $13 to $125 per short ton unit. About 10.4 million short ton units are available at a calculated price that is less than the present market price ($40). Total known resources amount to about 40.2 million short ton units. A very large portion of that quantity was not costed due to inadequate information on either resources or processing methods. Further exploration and research would have a significant effect on the availability of tungsten in the United States.

Jan 1, 1971

By E. G. Davis

Large-scale ultrafine grinding tests of a coarse kaolin were made using the Bureau of Mines developed attrition grinding process in continuous open-and closed-circuit systems. A 20-inch diameter attrition grinder, designed and constructed at the Tuscaloosa Laboratory, was used. Studies included single- and multiple-stage open-circuit grinding, and also continuous grinding tests in closed-circuit with a 6-inch-diameter solid bowl centrifuge. Clay feed, containing 9.0 percent minus-2-micrometer esd, was used at fates up to 840 pounds per hour. Multistage grinding tests gave better results than single-stage treatment when equivalent clay feed rates were used. Closed-circuit grinding tests yielded ground products containing slightly more minus-2-micrometer-esd clay than the open-circuit grinding when using the same clay feed. Energy consumption was lower in closed-circuit grinding than in batch or open-circuit grinding. A modified two-stage closed-circuit grinding system gave the best grade of product and amount of minus -2-micrometer-esd clay produced per pound of clay feed. The ground product from this test contained 88.5 percent minus-2-micrometer-esd material and electrical energy consumption was 327 kilowatt-hours per ton of minus-2-micrometer-esd material produced.

Jan 1, 1973

By M. E. Tyrrell

Mixtures of zirconium diboride and iron, cobalt, and nickel were resistance sintered to high-density compacts using modified electric welding equipment. To evaluate the use of iron, cobalt, or nickel as binders for zirconium diboride, the sintered compacts were examined in polished section and tested for crushing strength, hardness, microhardness, oxidation rate, and resistance to mechanical shock. Each of the zirconium diboride-metal mixtures produced brittle cermets, but the hardness was generally satisfactory. The iron- and cobalt-bonded cermets exhibited rather poor oxidation resistance. Cobalt provided the least brittle bond, and nickel, the hardest and most resistant to oxidation. Iron tended to form chalky compacts with low resistance to mechanical shock.

Jan 1, 1963

By Arden D. Fugate

This work was conducted to determine a feasible process for converting siliceous fluoride offgases to a commercially usable product. The offgases were generated by pyrohydrolytic defluorination of low-grade fluorspar in a gas-fired rotary kiln, and fluorine was collected as a hydrofluoric-fluosilicic acid. A silicon-free fluoride solution for further processing was then produced by neutralizing the acidic scrubber solution with anhydrous ammonia, silicon being separated as orthosilicic acid. Ninety to ninety-nine percent of the fluorine originally present remained in solution as ammonium fluoride. Silicon was also separated from synthetic fluosilicic acids, having F-to-Si weight ratios ranging from 3.50 to 14.3. The solutions below a ratio of 4.06, the F-to-Si ratio of H2SiF6, containing dissolved silicon were desiliconized as completely as those containing less than the stoichiometric quantity of silicon. An electrolytic-grade cryolite was recovered from the ammonium fluoride solution by reacting with either sodium aluminate or alumina trihydrate and sodium hydroxide. A product containing 97 to 100 percent of the fluorine, represented by Na3A1F6, was recovered, and 94 to 99 percent of the theoretical yield was realized.

Jan 1, 1963

By J. Robert Wells

The Bureau of Mines has developed a spectrochemical procedure for determining 19 impurity elements in high-purity titanium metal, titanium oxides, and titanium halides in which all samples are converted to titanium dioxide. Determination of these impurities was studied in the general concentration range of 0 to 1,000 p.p.m., but different determination limits were found for the various elements. The procedure is quantitative for 18 elements but semi-quantitative3 for beryllium and has an overall relative standard deviation of 15.8 percent. Two mixtures were used, one composed of graphite and lithium carbonate plus gallium oxide and the other of graphite and lithium carbonate plus germanium dioxide. Each mixture was blended mechanically with an equal weight of titanium dioxide. Lithium carbonate served as buffer-diluent. Gallium was the internal standard for 1 impurity element, germanium for 7, and titanium for the remaining 11.

Jan 1, 1962

By Charles S. Allbright

This report describes hydrogenation of petroleum distillate fuels in bench scale equipment and the effects of hydrogenation on the storage stability and the composition of the fuels. Two distillate fuels were hydrogenated in laboratory equipment using a commercially available cobalt molybdate catalyst. Reactor temperatures were varied from 600° to 850° F and pressures from 100 to 600 psig. Product fuels were analyzed by ASTM, Bureau of Mines, mass, and infrared methods. Hydrogenation of a catalytically cracked fuel from Oklahoma crude oil significantly improved the storage stability, reducing insoluble gum formed during 9 months of storage at 110° F from 19.0 to 1.3 mg per 100 ml fuel, average. Conversion of the olefins to other hydrocarbon types varied with the temperature of hydrogenation--at 700° to 850° F the conversion was mainly to aromatics, at 650° F about 50:50 to saturates and aromatics, at 600° F principally to saturates. Processing a fuel composed of a mixture of virgin distillate and catalytically cracked stock, both from Illinois crude, at 700° F and 200 psig effected marked improvement in stability; the buildup of insoluble gum in storage was lowered from 18.3 to less than 1 mg per 100 ml fuel.

Jan 1, 1967

By A. R. Taylor

The Bureau of Mines has determined the heat capacity and enthalpy values for beryllium sulfate (BeS04) throughout the temperature ranges of 10° to 300° K in an adiabatic calorimeter, and 350° to 860° K in a Bunsen-type ice calorimter, The heat-capacity data were extrapolated to 0° K, and smooth values of heat capacity, entropy, enthalpy function, and free-energy function were reported at 10-degree intervals between 0° and 300° K. The method of least squares was used to fit the enthalpy data with an algebraic equation. The equation also was used to calculate values of heat capacity, entropy, enthalpy function, and free-energy function at 50-degree intervals between 300° and 900° K.

Jan 1, 1963

By Robert M. Doerr

Isothermal oxidation kinetics were determined for three grades of Ni and for 99.99 percent Co in Ca and in air from 800° to 1,200° C. The oxidation reactions followed approximately the parabolic rate law. For 99.99 percent Ni in 02 at 1,200° C, the parabolic rate constant was 2 mg cm-2 hr-2. For 99.99 percent Co in dry air, the constant ranged from 1 mg cm-2 hr-2 at 800° C to 18 mg cm-2 hr-2 at 1,200° C; for 99.99 percent Co in 02 the constant was 2 mg cm -2 hr-2 at 800° C and 10 mg cm-2 hr-2 at 1,000° C. For 99 percent Ni in dry air, the constant ranged from 0.2 mg cm 2 hr-2 at 800° C to 3 mg cm 2 hr-2 at 1,200° C. By X-ray diffraction measurements, only divalent oxides were found in the scales. Volumetric and quartz-helix gravimetric methods were used. The volumetric apparatus was designed to permit less stringent restrictions on the corrosion specimens; it was also more convenient to use. The agreement between the weight gain determined gravimetrically and the 02 consumption determined volumetrically was not good enough for direct comparison of gravimetric and volumetric results.

Jan 1, 1963

By F. R. Lee

[THE Bureau of Mines was established in July 1910 to conduct research and to Establish standards for mining equipment and practices which would conserve human life, natural resources, and property in the mineral industries. Several lists of equipment approved by the Bureau as permissible for use in gassy coal mines have a been issued since then. The lists covering all approved equipment except breathing apparatus and explosive have been consolidated info two publications: Bulletin 543, Permissible Equipment Approved to January 1, 1953, and Information Circular 5220, Permissible Mine Equipment Approved By The Bureau of Mines During 1953-62. The purpose of this publication is to supplement Bulletin 543 kind Information Circular 8220 with a listing of permissible equipment approved during 1963 and 1964. The schedules (standards) under which equipment listed herein have born approved are as follows (titles and dates of approval and revision are given in footnotes): Schedule 2F,3 schedule 6D,4 schedule 7C,5 schedule 8C,6 schedule 9B,7 schedule 10C,8 schedule 12D,9 schedule 22,10 schedule 24,11 schedule 25B,12 schedule 28,13 schedule 29A,14 schedule 30,15 and schedule 31.16]

Jan 1, 1966