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By Charles M. Mason

The Bureau of Mines evaluated equipment and procedures for drop-weight testing of explosive liquids as prescribed by Test 4) a widely used method. It was demonstrated that partial ignitions, originally designated as negative results, should be designated positives; it was also shown that wear or erosion of the sample cups and the type of mount used for the apparatus had important effects on the results. Relative sensitivity as measured by Test 4 was found to vary slightly with temperature. The Bureau also designed a fixed 2-kg weight and associated electromagnetic release, which subsequently were incorporated as standard in a revision of Test 4. The original concept that the test involves only adiabatic compression was found to be an oversimplification; an alternate mechanism for the initiation process is proposed in which due consideration is given to the effects of cavitation and microjets.

Jan 1, 1966

By H. J. Heinen

The Bureau of Milts studied repetitive batch electrowinning of molybdenum from molybdic oxide ) to determine the effects upon the electrolyte life, purity of metal product , and overall cell performance. The electrolyte consisted of 54.0 weight-percent sodium tetraborate (Na2B407), 23.6 weight-percent sodium chloride (NaC1), 14.9 weight-percent sodium fluoride (NaF), and 7.5 weight-percent Mo03. The feed materials were pure and technical-grade Mo03. Electrolysis was conducted at l,000° C in a graphite cell in an atmosphere of air and carbon oxides. Electrolyte degradation did not occur during repetitive winning of molybdenum from pure Mo03 in an 8-day (5,400-ampere-hour) period of operation. Electrowon metal contained <0.1 percent total impurities. The electrode configuration is a key factor in the direct conversion of technical-grade Mo03 to metal by repetitive cyclic electrolysis. The best configuration found was a cathodic crucible and a central anode. Metal purity of 99.8 percent and a current efficiency of 91 percent were maintained until the combined impurity buildup the electrolyte reached 4.7 percent silicon, l.0 percent aluminum, and 0.6 percent iron. One pound of molybdenum was produced per 1.5 pounds of solvent salts employed. About 25 percent of the initial NaCl and NaF contents of the electrolyte were lost owing to volatilization and crucible penetration.

Jan 1, 1966

By H. E. Perlee

Autoignition temperatures and limits of flammability of nine halogenated hydrocarbons in atmospheres of air, oxygen, and nitrogen tetroxide were measured in a modified standard autoignition apparatus and limit-of-flammability apparatus previously developed at the Bureau of Nines. Of the nine halogenated hydrocarbons investigates--bromochloromethane, bromotrifluoromethane, bromochlorodifluoromethane, 1,1,2-trichlorotrifluoroethane, 1-bromo-l-chloro-2,2,2-trifluoroethane, dibromodifluoromethane, l,2-dibromo-1,1,2,2-tetrafluoro-ethane, 1,1,1,3,3-pentachlorotrifluoropropane, and l-bromo-2,4-dichloro-1,1,2, 3,3,4-hexafluorobutane--two formed flammable mixtures with nitrogen tetroxide and six with oxygen; none formed flammable mixtures with air. Three of the halogenated hydrocarbons formed no flammable zones with any of the three oxidizing atmospheres. For those halogenated hydrocarbons that supported combustion in oxygen atmospheres, explosion pressures developed during constant-volume burning of mixtures near the middle of the flammable zone were observed to range from about 6 psig for dibromodifluoromethane to 158 psig for 1-bromo-1-chloro-2,2,2-trifluoroethane. In all cases, the calculated burning velocities of these mixtures were less than 8 in/sec.

Jan 1, 1966

By R. W. Van Dolah

An attempt has been made in this investigation to define the conditions under which ammonium nitrate (AN) might detonate as a result of involvement in fire. The initiation of detonation by shocks derived from explosives or from projectile impact was investigated as a function of temperature and charge diameter. A new technique was devised to investigate the burning of raw and contaminated AN under pressure. No transition, to detonation in AN was obtained in the burning experiments. The critical diameter for detonation of fertilizer-grade AN was found to be quite small when the AN was at temperatures just below melting point; this indicates that initiation of detonation may be less difficult at elevated temperatures but such initiation by gas-phase detonation was shown to be unlikely. Transition from burning to detonation was obtained with AN intimately mixed with fuels that included polyethyl-ene, paper, and fuel oil when these were contained in vessels with restricted vents. However, the experimental results supported by an analytical study indicate that the initiation of detonation in AN from fire exposure in normal storage and from transportation incidents is quite improbable. The detonation of AN in recent incidents more likely may have resulted from the effects of adjacent explosions.

Jan 1, 1966

By J. E. Tress

The Bureau of Mines prepared submicron tungsten powder by reducing tungsten hexachloride with hydrogen. The particle diameters of the resulting tungsten powders ranged from 0.015 to 0.046 micron. Within the limits of the variables investigated, no clear-cut correlation was found between process conditions and final size of the powder. Oxygen was the major contaminant in the product; being present both as an adsorbed gas and as suboxides of tungsten. Studies showed that the powder yielded compacts of approximately 45 per-cent of theoretical density when compacted mechanically. Low-temperature sintering produced more rapid densification in these compacts than in compacts prepared from conventional powders. Adding up to 20 percent ultrafine powder to conventional tungsten powder caused an increase in density upon compaction with maximum densification occurring at approximately 12 percent ultrafine powder.

Jan 1, 1966

By R. V. Higgins

A computer program is presented to calculate the shape factors and volumes of cells from a potentiometric model, using coordinates of the inter-sections of the stream lines and equal potentials and a few additional coordinates. Shape factors are used in flow computations when the geometry is complicated. The program also includes computer instructions to divide the channels into cells of equal volume and to obtain the shape factor for each of these equal volume cells. An illustrated example using the potentiometric model for the waterflood of a seven-spot well-spacing pattern is presented. The information contained in the report is of value not only to those allied to the subject but also to others, because many of the techniques can be conveniently used in formulating other computer programs.

Jan 1, 1966

By N. E. Hanna

Experience with the current version of gallery test 4, in use since 1913 to evaluate the incendivity of permissible explosives in the presence of coal dust, has shown the procedure to have inadequate discrimination. Consequently the Bureau of Mines used the up-and-down method of statistical design to investigate the incendivity of permissible explosives in the presence of coal dust and gas. A suitable device was developed to measure coal dust concentrations in the air-gas mixtures and to disperse the dust in the gallery atmosphere. A proposed testing method which uses suspended shots in a predispersed coal dust-gas-air mixture was evaluated. The new method can discriminate between different explosives with respect to their incendivity. Maximum ignitibility of the coal dust cloud by permissible explosives occurred in the vicinity of 0.3 oz/cu ft. About 10% sodium chloride in permissible explosive formulations had a very significant effect in reducing the probability of igniting coal dust. Bundled charges were more incendive than column charges.

Jan 1, 1966

By Henry C. Meeves

The nonpegmatitic sources of beryllium in Arizona, Colorado, New Mexico, Utah, and four adjacent states investigated by the Bureau of Mines are described. The investigations included 155 properties from which over 6,200 rock samples were collected; more than 5,500 samples were analyzed by the nuclear beryllium-detection technique. Twenty-four of the properties examined had rock containing more than 0.10 percent BeO. Many of the beryllium determinations were made in the field with portable detection instruments by direct scanning of outcrops and by testing samples of rock brought to the instrument. The large domestic resources of low-grade nonpegmatitic beryllium ore in Utah, which were discovered by private enterprise and which respond favorably to small-scale treatment processes, may come into commercial use and thus reduce the dependence of the United States on imported beryl.

Jan 1, 1966

By R. L. Crosby

Microscopical and X-ray diffraction techniques were used to identify two intermediate phases in that part of the solid region of the magnesium-cerium system between and Mg3Ce. Previous literature had reported only one intermediate phase for this region, 1)12t chemical analysis determined the approximate composition of the two compounds to be Mg23Ce2 and Mg17Ce2. The range in composition of the two intermediate phases was found to be limited to less than 0.3 atomic percent cerium. The study did not determine the crystal structure of Mg17Ce2, but that of Mg23Ce2 is tetragonal with a = 10.33 A and c = 19.51 A.

Jan 1, 1966

By F. L. Wideman

Output of ore and waste from metal and nonmetal mines in the United States continued an upward trend and established a new high. The tonnage of ore handled increased 6 percent over that moved in 1964 and the tonnage of waste rose almost 10 percent. Earth moving by these two activities exceeded 3.2 billion tons, an increase of 7 percent over the 1964 total. Crude material from which metal or nonmetal products were derived continued to be about 75 percent of the total material handled. In 1965, surface mining methods were used to produce about 93 percent of the ore, 99 percent of the waste, and 95 percent of the total material handled. These percentages have remained almost constant since the beginning of this decade.

Jan 1, 1966

By Oliver Q. Leone

Electrorefining tests using titanium-nitrogen alloys as anode material showed that no significant quantity of nitrogen was transferred to the cathode deposit. The nitrogen of the anode remained in the scale, and the titanium-nitrogen alloy was anodically insoluble in the electrolyte when the nitrogen content was 11 weight-percent.

Jan 1, 1966

By E. J. Kloos

The Bureau of Mines developed a test for evaluating gas masks designed to protect against phosphine gas; phosphonium iodide is used as a source of phosphine. Gas masks approved by the Bureau for respiratory protection against phosphine include the GMC-SS-1, Mine Safety Appliances Co.; the LG-10 and LG-10G, Willson Products Division, The Electric Storage Battery Co.; and the 084-PHOV-R, Acme Protection Equipment Co.

Jan 1, 1966

By J. W. Town

The Bureau of Mines conducted phosphate beneficiation studies to determine the influence of mineralogical and textural features on the recovery of phosphate from select bed and composite samples representing different phosphate rock types of the western Phosphoria Formation. Batch heavy-liquid tests showed that ore grade) pellet size, and type of interstitial material were significant parameters affecting concentrate grade and recovery. Recoveries at acid grade (31.5 percent P2O5) ranged from 98 to 56 percent. Liberation was essentially complete at 28 mesh, and recoveries tended to drop when overgrinding occurred.

Jan 1, 1966

By A. W. Deurbrouck

The Bureau of Mines analyzed 13 samples collected from three Randolph County coalbeds. The Peerless and Sewell bed samples were generally of metallurgical quality as received from the mines or could be easily upgraded. How-ever, the Lower Kittanning coa1bed samples proved to be quite inimical to upgrading to metallurgical quality.

Jan 1, 1966

By P. L. Weston

The Bureau of Mines used high-temperature reduction roasting, magnetic separation, acid-leaching, and autoclave precipitation processes to recover iron and manganese from brown Cuyana range ores of Minnesota. Wet magnetic separation concentrated over 90 percent of the iron in 3 of 4 ores as high grade products analyzing 74 to 85 percent iron, 2.5 to 6 percent manganese, and 3 to 10 percent SiO2. The nonmagnetic fractions were leached with dilute sulfuric acid extracting 83 to 93 percent of the contained manganese and small amounts of iron. The leach solutions contained Mn-to-Fe and Mn-to-SiO2 ratios favorable enough for possible consumption in metallurgical mane operations. Exceptionally pure Mn solutions were achieved by pressure precipitation of the remaining iron in an autoclave followed by lime precipitation of silica and alumina.

Jan 1, 1966

By R. R. Lowery

The Bureau of Mines developed hypereutectic aluminum-silicon alloys which 11.7.d better mechanical properties than the unmodified hypereutectic alloy. A commercial aluminum-20 weight-percent silicon LIr alloy was selected as a ary base for improvement. The primary silicon. grains were reduced from ASTM 4-5 to ASTM 8.5 by the use of phosphorus and phosphorus compounds. The remaining eutectic matrix was refined by sodium metal additions of 0.2 weight-percent. Solid solution strengthening of the alpha aluminum was obtained by adding 2 percent copper and 0.5 percent magnesium. Also, 1 percent nickel was added to harden the alloy. Optimum thermal treatment consisted of a solution treatment for 10 hour:, at 480° C with hot water quench, followed by aging for 6 hours at 175° C. The final alloy exhibited a Rockwell B hardness of 75 ±2 in the heat-treated condition. The ultimate tensile strength was 39,5O0 psi with no recordable elongation. The coefficient of linear thermal expansion was 20.4 x 10-6 per °C in the temperature range 20° to 300° C. No wear resistance data were collected.

Jan 1, 1966

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

By W. H. Tavenner

The Bureau of Mines gathered test data on the use of a continuous borer in mining an anthracite bed, which was 30 feet thick on a pitch of 15° to 45°. Gangways were driven with the continuous borer, ventilation openings between gangways were driven with a large-diameter auger, and the blocks of coal between completed gangways were mined by the long-hole method, Conveyors were used to transport the mined coal. The continuous borer operated on a coal floor that was frequently soft because of heaving. The continuous borer could not bore openings on a grade exceeding 27 percent (15° pitch). Because 150 was also the lower limit of the pitch, of the bed, the continuous borer was used only to drive gangways. The continuous borer virtually filled the workplace, leaving insufficient space to place heavy-duty timber and cushioning material between the timber and coal back to allow for normal expansion of the uncut coal. The light? weight yieldable steel arch against the coal back gave inadequate support to control convergence, which in a disturbed area sometimes occurred with explosive violence. This exposed the machine operator to a hazardous condition, since a satisfactory solution could not be found, the company discontinued the use of the continuous borer.

Jan 1, 1966

By V. E. Homme

Low- and high-temperature reduction techniques were employed by the Bureau of Mines in study of conditions favorable to the formation of massive titanium crystals. &apos;1,1,2 low-temperature method, feeding molten sodium to solidified titanium lower chloride-sodium chloride, produced higher quality and high quantity crystalline metal. The percentage of crystalline titanium was increased with increasing reactor diameter, melt depth, and titanium dichloride concentration. The high-temperature technique, feed molten sodium to melts above 8000 C, producing needle-type crystals of lower quality and with less consistent results than the low-temperature method. Layers of titanium foil, sponge, fine needles, wool, and crusts of sin-tered granules were formed during the earl, -art of the low-temperature reduction, and massive crystals were produced beneath this barrier in the latter part of the reduction. Crystalline titanium having an average hardness of Bhn 76 and representing 58 percent of the total titanium was obtained. Lamellar crystals up to 1 1/2 inches long with a hardness as low as Bhn 54 were also produced. A second-stage reduction for reclaiming titanium from offgrade sponge is described. Titanium produced by this method was comparable in quality to that from sodium reduction of titanium tetrachloride.

Jan 1, 1966

By R. L. Hopkins

The work described was performed to determine whether sulfur compounds of the thienothiophene class occur in crude oil. The presence or absence of various classes of sulfur compounds in crude oils is of interest and value to petroleum science. The Bureau of Mines, for the first time, identified hydro-carbon products of desulfurization that point directly to the identity of two individual thienothiophenes, namely 3-methylthieno[2,3-b]thiophene and 2-meth-ylthieno[3,2-b]thiophene, in Wasson, Texas, crude oil. These identifications, described in detail, were accomplished using microdesulfurization, mass spectrometry, and gas-liquid chromatography.

Jan 1, 1966