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By R. Ward Stahl

This publication is a revision of Report of Investigations 5363 updated to reflect the improvement in fire protection at selected coal mines and contains suggestions on what may be considered good fire protective equipment, suggested methods of organizing the attack on fires at various locations underground, and helpful hints on testing and evaluating firefighting facilities.

Jan 1, 1968

By R. F. Abernethy

A chemical method of determining microgram quantities of arsenic in coal was investigated by the Bureau of Mines to supplement a semiquantitative spectrographic method of determining arsenic in coal ash. In accordance with a method recommended by the International Organization for Standardization, 1-gram samples of coal are decomposed by wet oxidation with boiling sulfuric acid (H2S04) and nitric acid (HN03) to remove the organic matter. After heating to fumes of SO3 to remove HN03, the arsenic is separated as arsine by the action of zinc in H2S04 solution. The arsine is absorbed in dilute iodine solution in which the arsenic is determined colorimetrically by the molybdenum-blue reaction. Two modifications of the method for obtaining the arsenic in solution, in addition to the wet oxidation method, give satisfactory results. The modifications are (1) furnace ashing with MgO added to the coal, followed by treatment with H2S04, and (2) extraction of arsenic from the coal by dilute HNO3 without ashing. Float-and sink-tests show that arsenic is associated mainly with mineral matter in the three coals examined. High-temperature ashing tests show that very little arsenic is volatilized from coal ash below 1,000° C, but it is virtually all removed from the ash at 1,300° C.

Jan 1, 1968

By Frank G. Horino

This report describes an instrument designed by the Bureau of Mines for quantitatively identifying texture of rock surfaces produced by grinding or extremely rough surfaces beyond the range of commercial surface measuring instruments. The transducer for the instrument is a linear variable differential transformer that converts mechanical motion caused by surface roughness, waviness, and lay to an electrical output. The electrical output is recorded graphically as an X-Y plot of the line traversed on the rock surface. Details of the synthesized device and its calibration are given. The sensitivity of the unit is 2 percent of the scale setting of the amplifier. The horizontal scale is adaptable from ¼ inch to 15 inches of specimen length with a sensitivity of 0.01 inch if a 10 to 1 magnification is used and 0.1 inch if a 1 to 1 magnification is used.

Jan 1, 1968

By Jerry J. Gray

Transportation charges for mineral commodity movements in western Oregon and western Washington were determined mainly by a stratified random sample canvass of producers. Total 1965 mineral production value for this area was $53.3 million; the cost or charge to move this production from the mine to the consumer or to the point of consumption was determined to be an additional $38.7 million. Thirty seven companies were contacted as a sample out of a total population of 349; the statistically expanded sample production value deviated 3.6 percent from that obtained by the Bureau's annual canvass. The agreement between the sample results and the canvass totals demonstrated the effectiveness of the sampling method for obtaining data with a predesigned level of accuracy. For comparison, the north-central Idaho and western Montana area was studied, A random sample experiment was designed, but because of the dominance of a few major companies, a random sample technique would have required more visits to producers than if only the larger firms were contacted. Eighty-four percent of the 1966 mineral value ($198.6 million) was accounted for by interviewing 27 firms out of a total population of 199. Total transportation costs or charges for the area were $26.7 million. The significant difference observed between the relationship of minerals production value and transport charges between the two areas investigated can be attributed to the difference in the minerals produced. The western Oregon and western Washington region is a nonmetals-producing area as opposed to the predominance of metals production in the Idaho-Montana region.

Jan 1, 1968

By M. O. Magnuson

As part of an experiment in the restoration of lands strip-mined for coal, revegetation studies were conducted at three backfilled strip-mine sites in north-central Pennsylvania. The sites were subdivided into plots that were given varying amounts of lime and fertilizer. In tests conducted cooperatively with State and Federal agronomy experts, the plots were then planted with a variety of trees, shrubs, and grass-legume mixtures. Initial tree and shrub survival was not appreciably affected by lime and fertilizer applications where the spoil pH was above 4.5. Of 14 species of trees and shrubs tested, Norway spruce, black locust, Japanese larch, pitch pine, and white pine were the hardiest. The ground-cover percentage of grass-legume mixtures in the second growing season was substantially increased by using lime and fertilizer. Mixtures comprised partly of fescue were the most satisfactory.

Jan 1, 1968

By K. R. Dorman

To develop the potential of precast concrete sets as a support medium in underground mines, a three-piece precast concrete drift set was designed for a small opening and tested to destruction in an underground straining frame. Thirty-six tests were made with three sizes of members using three different loading conditions. In addition, 14 members were tested individually in the laboratory. Test results are compared with theoretical calculations. A cost comparison shows the use of concrete sets would be advantageous where conventional wooden timber requires excessive replacement.

Jan 1, 1968

By R. W. Van Dolah

The feasibility of formulating cap-sensitive slurry explosives for use in underground mines with potentially flammable gas atmospheres was examined. Formulations containing aluminum metal as sensitizer and sodium chloride to reduce incendivity were prepared; some were cap-sensitive and had adequate air-gap. Flaked aluminum metal rather than the atomized type proved to be the more effective sensitizing agent of the formulations tested for incendivity in the large gallery of the Bureau of Mines, some were found to be suitably nonincendive.

Jan 1, 1968

By R. R. Brown

The Bureau of Mines undertook a limited feasibility study to determine the practicality of removing copper from automobile scrap by thermal treatment. Test specimens, prepared by wrapping bare and insulated copper wire around small steel coupons, were heated at 600° to 1,150° C in various atmospheres for different lengths of time under both static and dynamic conditions. The tests indicated that adequate removal of copper cannot be effected by thermal treatment of scrap above the melting point of copper. Tests showed that copper present in scrap as insulated wire is embrittled by thermal treatment at 800° to 900° C if the insulation contains lead, and that the embrittled copper is almost completely removed by a mechanical action such as tumbling. Also chemical pretreatment of specimens to effect embrittlement of copper and the magnetic separation of oxide scale were studied. Tests showed that bare copper can be embrittled by depositing waterglass (Na, Si409) on copper prior to thermal treatment.

Jan 1, 1968

By J. L. Reuss

The Bureau of Mines derived information on the softening characteristics of both unfired and indurated iron ore pellets as measured by hot compression strength in a laboratory study. A surprisingly high hot strength (240 1b per ½ -inch spheroid) was developed by unfired magnetite pellets near 900° C; lesser maxima were developed by pellets made from hematite and specularite concentrates near 1,000° C. Those from goethite remained weak throughout the pre induration heating. Fully indurated commercial pellets retain a high resistance to softening when heated in air. On the contrary, in a hot reduing atmosphere their high cold crushing strength dissipates rapidly. At 1,000° C, for example, the average compression strength of seven different commercial pellets was 110 lb; at 1,100° C, the hot strength was only 60 lb. After a rather sharp initial drop, the loss of strength with increase of temperature was gradual. There was no sudden collapse, nor any significant difference, in behavior of commercial pellets whether made from magnetite or hematite concentrates.

Jan 1, 1968

By John B. Shutack

In an effort to improve the performance of the explosive-anchored rock bolt, the Bureau of Mines studied the effect of the detonation velocity of the explosive and type of charge (linear or nonlinear) on the fracturing tendency of the anchor tube. Also, different types of tubing were compared to determine the one most suitable for use as an anchor tube. The Bruceton up-and-down method was applied in tests in which steel shooting blocks having boreholes ranging from 1-3/8 to 2-1/8 inches in diameter were used. Of the four types of tubing evaluated, a welded A-178 tubing that was drawn over a mandrel and renormalized gave the most promising results. The A-179 seamless tubing that is normally used with the explosive bolt was the most inferior. Both types, however, gave significantly better anchorage than the conventional shell when tested in both laboratory and underground experiments. Within the range of velocities studied (5,000 to 7,000 m/sec), the type of explosive showed no significant effect on anchor-tube performance. In general; linear explosive charges provided better anchorage than nonlinear charges.

Jan 1, 1968

By Karl C. Dean

The Bureau of Mines studied the precipitation of copper from dilute acidic sulfate solutions using shredded automobile scrap in a rotary drum. The tests established that the scrap in the rotary drum precipitated copper faster and more completely than shredded, detinned, tinplate scrap in a launder, with comparable iron consumption. Although power is required to rotate the drum, the faster precipitation and continuous recovery of cement copper are advantages of the tumbler method. Cost evaluation indicates that the rotary drum method, which uses relatively low-cost and readily available shredded automobile scrap, is competitive with the launder method, which uses relatively high-cost shredded tinplate scrap or detinned shredded cans.

Jan 1, 1968

By R. B. Schluter

Magnetite pellets were simultaneously reduced and indurated on a laboratory scale in order to determine the effects of temperature, induration time, degree of metallization, and sulfur content upon the physical and chemical properties of prereduced pellets. The reductants were commercially-pure tank gases. Among the findings were these: 1,100° C is the minimum temperature that will produce acceptably hard pellets using carbon monoxide as the reduc-ing gas. Prolonged treatment time improves the pellets' crushing strength, but the rate of improvement falls off sharply after 2 hours' induration. At 1,120° C, 75-percent metallization produces the maximum crushing strength; there was no corresponding peak at 900° or 1,050° C. Sulfur in the furnace atmosphere lowers the required induration temperature. A few tenths of 1 percent sulfur in the pellet increases the sintering rate of metallic iron in pellets by forming a liquid FeS phase that facilitates iron transfer.

Jan 1, 1968

By Andrew J. Fergus

A study of the flotation characteristics of columbium-tantalum minerals was made by contact-angle and microflotation methods, and the findings were confirmed by flotation of two natural ores. In the contact-angle study conditions for collection of columbite, pyrochlore, and tantalite were determined for (1) sodium oleate with a sulfonate; (2) sodium isooctyl phosphate; (3) a short-chain primary amine; (4) a long-chain primary amine; and (5) a quaternary amine. These conditions were confirmed in microflotation tests. Information about collector action on common gangue minerals was also obtained by these two methods. In batch flotation tests on a pyrochlore ore and a columbite ore, it was demonstrated that collectors selected on the basis of contact-angle and micro-flotation studies would float columbium minerals from a complex natural ore. However, multiple cleaner and scavenger flotation steps will be necessary to produce commercial concentrates. From a pyrochlore ore containing 0.54 percent Cb2O5, a 44.4 percent Cb2O5 concentrate was made containing 36.4 percent of the total Cb2O5. For a columbite are the corresponding values were: 4.35, 54.6, and 67.1 percent. During the batch flotation study, wetting agents were found to aid in the gangue-ore mineral separations.

Jan 1, 1968

By R. V. Mrazek

The heat of formation of vanadium trichloride was determined at 298.15° K. Measurements were made in a solution calorimeter in which an aqueous hydrochloric acid-potassium dichromate solvent was employed. Data are presented for the heats of solution of vanadium trichloride and the vanadium trioxide "backup" compound, and for appropriate dilution reactions needed to preserve stoichiometry. The resulting heat of formation of vanadium trichioride (VCI3) at 298.15° K was found to be ?H°298.15° K = -138.89 ±0.37 kcal/g mole.

Jan 1, 1968

By Basil Dimitriades

Five recently developed methods for determining nitrogen oxides in automotive exhausts have been evaluated from the standpoint of accuracy and applicability in current exhaust studies. Results showed that methods requiring conversion of nitric oxide to nitrogen dioxide as a part of the analytical procedure are subject to errors introduced by the instability of NO2. The extent of some of these errors has been determined and procedures have been developed to minimize undesirable influences. On the basis of the results obtained from this study, recommendations are made regarding procedures for batch type or continuous measurement of nitrogen oxides in exhaust streams.

Jan 1, 1968

By Herbert R. Babitzke

As part of a project to develop refractory metal alloys suitable for high-temperature structural applications, the Bureau of Mines applied solid solution and precipitation-hardening techniques to columbium and tantalum alloys. Thirty-three alloys were evaluated to determine their formability, strength, and oxidation resistance. Three alloys had tensile strengths near 40,000 psi at 1,200° C: Cb-1N-5W-5V-10Hf (No.4), Cb-15Hf-5W-0.5B (No. 31), and Cb-15Hf-SW-IB (No. 32). Oxidation resistance of the high-strength alloys was good. Alloy4 gained only 34 mg/cm2 at 1,200° C, and 21 mg/cm2 at 1,000° C in 2 hours. Hot forming was done without any protection from oxidation.

Jan 1, 1968

By Perry N. Halstead

This report describes two goniometers that, by simple manipulation, can be used to ascertain the attitude of a joint, vein, or fracture plane observed on the planar projection of a borehole photograph taken with an NX borehole camera of the type developed by the U.S. Army Corps of Engineers. One goniometer was designed to interpret photographs taken in vertical drill holes and the other for photographs taken in inclined drill holes. In practice, several measurements are made on each photograph with the goniometer. These data are then substituted into mathematical equations, which are derived in this report and the attitudes of fracture planes are determined.

Jan 1, 1968

By Paul Sands

Single- and two-stage tests were made with 6-inch, coal-cleaning hydrocyclones to determine the effect of hydrocyclone geometry, operating conditions, and feed composition on performance. Most of the testing was conducted in an open-circuit pilot plant that had a maximum capacity of about 9 tons per hour. The coals used in the investigation had top sizes of 1/4 inch and 28 mesh. Considerable latitude was found in the range of geometry variables that could be used without affecting performance adversely, although a certain minimum ratio of overflow to underflow openings had to be maintained for best operation. Two-stage cleaning proved distinctly better than operation with a single hydrocyclone, because clean coal lost in the refuse product of the primary unit can be partly recovered in the secondary. There is an unusually great difference in the specific gravities at which the individual sizes of the feed are separated in the hydrocyclone. This militates against high efficiency because maximum yield occurs when all sizes are cleaned at the same specific gravity. The size composition of the feed and, more particularly, the size composition of the impurity have a greater influence on the efficiency attainable in the hydrocyclone than in most other types of fine-coal cleaners.

Jan 1, 1968

The principal activities of the Bureau of Mines Explosives Research Center during fiscal year 1967 (July 1, 1966, to June 30, 1967) arc reviewed in a part 1. Part 2 presents short abstracts of the publications issued during this period in the Bureau series and in other media. Part 3 describes a short study on the shock initiation of hydrogen peroxide not destined for publication elsewhere. ACKNOWLEDGMENTS The Bureau of Mines gratefully acknowledges the support received through cooperative agreement in fiscal year 1967 from The Dow Chemical Company Manufacturing Chemists' Association, Inc.

Jan 1, 1968

By H. E. Powell

The magnetic susceptibilities of 57 minerals containing titanium, zirconium, vanadium, columbium, tantalum, chromium, molybdenum, and tungsten were determined. The source and petrographic analysis of each sample are given. Included are values for isomorphous series of minerals showing wide ranges of composition and for a few high-purity synthetic minerals.

Jan 1, 1968