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By M. E. Tyrrell

To promote greater use of abundant domestic raw materials in the manufacture of synthetic mullite, the Bureau of Mines has undertaken a comprehensive investigation to determine the effects of the impurity oxides TiO2, Fe203, and alkali on physical properties of sintered mullite-forming mixtures. The first part of the report presents the results of work covering a major area within the mullite study; namely, the effect of impurity oxides on volume stability, one of the outstanding characteristics of mullite refractories. The volume stability of 20 compositions in each of 3 alumina- to-silica ratios, which blanket the range commonly found in purchase specifications, has been determined following procedures of Navy Specifications B-15606 A for Grade A high-alumina refractories. Results indicated that so long as 5 percent of impurities are combined approximtely in the proportions of 3 percent Ti02, 1 percent Fe203, and 1 percent alkali, sintered mullite-forming compositions in the almina to silica range tested will be volume stable. A permissible tolerance of one-half per- cent in each impurity oxide provides a range that includes values common in the natural minerals from which sintered mullite may be made. Within the total range of 5-percent impurity mixtures, a greater number of volume-stable compositions were obtained by increasing the alumina-silica ratio.

Jan 1, 1962

By G. W. Birge

Carbonizing properties of the principal coal beds of Perry County, Ky., are described in this Bureau of Mines report. Seven samples, representing the Hindman, Flag, Haddix, and Fire Clay beds, were carbonized by the Bureau of Mines-American Gas Association (BM-AGA) method, and yields of products and physical properties of cokes were determined. Carbonizing properties of blends of Flag and Fire Clay coals, with 20 and 30 percent Pocahontas No. 3 low-volatile coal from McDowell County, W. Va., also were determined. Expanding properties of the Flag and Fire Clay coals and their blends were determined in the Bureau of Mines sole-heated oven. The Perry County coals tested are high-volatile A bituminous in rank and, with the exception of the Hindman-bed sample, which contained excessive sulfur, were chemically suitable for metallurgical use. The three coals tested in the sole-heated oven contracted less than normal for Appalachian coals of similar rank, Blending the Fire Clay and Flag coals with 20 or 30 percent low-volatile coal increased coke strength appreciably but increased the expansion beyond normal limits for industrial blends.

Jan 1, 1962

This report is the 24th in a series summarizing research on coal and related investigations3 by the Bureau of Mines. The coal programs of the Bureau of Mines include a wide range of theoretical and applied studies--such as fundamental studies of coal structure and properties, the development and evaluation of new mining techniques, and work toward more effective processing and utilization of coal. The scope of these programs is indicated, in topical outline, by the table of contents. These investigations are integrated into a broad but coordinated effort to develop information on coal that will benefit the coal mining industry and the coal consumer while promoting the wise conservation and utilization of our national coal resources. Any attempt to summarize in one volume the progress in all of the program areas indicated must necessarily be limited to a brief review of developments, without detailed reporting of the data. However, while the brief discussion in each section will present only the highlights of the Bureau's work during the year, details of many of the operations or investigations described here can be found in the publications cited throughout the text. Other work, reported here for the first time, will be covered in greater detail in later publications.

Jan 1, 1962

By G. Asai

The purpose of this Bureau of Mines investigation was to determine the properties of arc-melted iron-chromium alloys ranging in chromium content from 12 to 50 wt.-pct. Alloys were prepared by consumable-electrode arc melting of electrodes composed of high-purity chromium and high-purity iron. Alloys were fabricated to rod and sheet, and the following data were obtained: Electrical resistivity, hardness, tensile strength, and impact strength at room temperature; and creep-rupture life at 650° C. (1,200° F.). As the chromium content of the annealed alloys varied from 12 to 50 pct., the properties varied as follows: The electrical resistivity increased proportionally from 41 to 53 microhm-cm,; the Rockwell hardness varied from A 38 to A 58; the tensile strength ranged from 52,000 to 96,000 p.s.i.; the impact strength of V-notched charpy specimens varied from 140 to 405 ft.-lb., and the 100-hour creep rupture life at 1,200° F. varied from 5,000 to 16,000 p.s.i.

Jan 1, 1962

By R. L. Montgomery

Heats of solution of cerium metal and cerium (III) chloride in hydrochloric acid were measured. The standard heat of formation of the aqueous cerium (III) ion at 25° C is -166.1 ± 0.3 kcal/mole. Heats of solution of cerium (III) chloride in hydrochloric acid are consistent with the existence of a complex CeC1++ having a stability constant of 1 and a heat of complexing of 5.4 kcal/mole.

Jan 1, 1962

By D. W. Frommer

Composite samples of nonmagnetic taconite from the western Mesabi range were evaluated by reductive roasting, fine grinding, and magnetic separation to determine potential sources of concentratable material. Although large tonnages of nonmagnetic taconite are known to occur in the western Mesabi district, these materials are not as yet a commercial source of iron ore. The technique employed permits the evaluation of individual composites and blocks of composites in terms of responsiveness to a process of potential commercial significance. The 159 composites, from open-pit mines located between Grand Rapids and Chisholm, Minn., were evaluated in the following sequence: 1. Minus 8-mesh material was roasted at 500° C. in hydrogen. 2. The roasted are was ground to one or more sizes in the minus 100-to minus 400-mesh range. 3. The roasted ground ore was magnetically separated in a Davis tube. 4. Composites were classified according to degree of grinding required to produce minimal concentrates. (Minimal concentrates are herein defined as those containing less than 10 percent silica, and responsive composites as those yielding minimal concentrates.)

Jan 1, 1962

By Paul S. Lewis

The Bureau of Mines hydrogenated coals of different rank that had been irradiated with either x-rays or gamma rays. Lignite, high-volatile A and C bituminous, and low-volatile bituminous coals were exposed to l billion roent¬gens of gamma-ray radiation; specimens of high-volatile A and C bituminous coals from other sources received 6 million roentgens of X-ray radiation. Irradiated and unirradiated control specimens of those coals were hydrogenated in autoclave experiments at (6,000-p.s.i. final pressure and 400° C. with retention times of 15, 30, or 60 minutes depending on the coal rank and catalytic treatment. Comparison of results from irradiated specimens with those from the control experiments showed that the radiation had no beneficial effect on the coal. High-volatile C bituminous coal may have been affected by radiation more than the other coals. One billion roentgens appeared to reduce the amount of coal converted to liquids and gases by about 10 pct., and 6 million roentgens reduced it by about 6 pct. then catalyzed with tin. In all other cases, the conversion of irradiated coal was either reduced by as much as 4 pct. or was essentially the sank as that obtained with unirradiated coal. Irradiation during hydrogenation nay be effective for increasing the reactivity of coal and should be investigated; further work with coals irradiated prier to hydrogenation is not recommended.

Jan 1, 1962

By G. W. Birge

Carbonizing properties of the principal coal beds of Butler County, Pa., are described in this report by the Bureau of Mines. Eight samples, representing the Upper Freeport, Lower Freeport, Upper Kittanning, Middle Kittanning, Lower Kittanning, Clarion, and Brookville beds, were carbonized at 900° C. by the Bureau of Mines-American Gas Association (BM-AGA) method. Butler County coals rank as high-volatile A bituminous and are generally characterized by high sulfur content compared with Appalachian coals used for industrial coking. If cleaned, the Brookville and one sample of Upper Freeport coal would be acceptable as the major component of metallurgical coking blends. The other Butler County coals tested would be unsuitable for this purpose because of either excessive sulfur or poor coking properties.

Jan 1, 1962

By Harry R. Nicholls

The objectives of this investigation were to determine the strain propagation laws for a strain pulse in salt and to compare the seismic effects from the detonation of different explosives in salt. The investigation showed that a strain propagation law of the type, e = K(R/W 1/3 ) n, and a strain energy propagation law of the type, Ea/W 1/3 = K(R/WI/3)b , are valid in salt. A change in the regression law coefficient, n , was noted with strain level. A similar change in b was inferred because strain energy is proportional to the square of strain amplitude. Particle velocity data may be used interchangeably with strain data under the test conditions.

Jan 1, 1962

By B. C. Peterson

Calumet Division, Calumet & Hecla, Inc., whose operations are in Houghton and Keweenaw Counties, Mich., is a highly integrated and complex organization. This division operates mines, a railroad, a concentrating mill, a reverberatory smelter, and the auxiliary generating plants and shops to service these operations. In addition, it operates a sands reclamation plant, leaching plants, a foundry, and a machine shop that serves varied industries with castings and parts for many applications. Calumet & Hecla, Inc. has produced over 60 percent of all the copper that has been produced in Michigan since discovery of the ore in 1864, and in 1959 the company ranked eight among the country's producers with a production of 17,407 tons. To keep abreast of modern accounting systems developed elsewhere in industry and to combat increasing costs due to higher labor and supply costs, as well as increased costs due to deeper mines and lower grade ore, the company has developed a modern machine cost accounting system. This not only provides the usual bookkeeping and cost accounting facilities but offers accurate cost data for engineering evaluation of the mining operation. This system is credited with being instrumental in permitting continued operation of these high-cost mines in a period of increasing costs with no corresponding increase in the price of metal.

Jan 1, 1962

By R. L. Balmer

This information circular, which describes the methods and costs of sinking a small underground shaft with steel supports at the Keystone mine of American Smelting and Refining Co., near Crested Butte, Colo., is one of a series being prepared by the Bureau of Mines on current shaft-sinking practices in various mining districts of the United States. Preparations for sinking a combined exploration, development, and production shaft from the lowest level of the Keystone mine began early in 1957. This vertical, three-compartment, 6-1/4-by 16-foot rectangular shaft was to be sunk in separate stages or lifts so as to correspond with the progress of an associated lateral exploration and development program. The first section of the shaft was collared and sunk to a depth of 209 feet between September 1957 and April 1958. Because of the depressed base-metal market, the mine was shut down as soon as the initial phase of the exploration and development program had been completed and before any deeper sinking could be attempted.

Jan 1, 1962

By T. T. Campbell

This investigation was undertaken by the Bureau of Mines to determine if high-purity ductile molybdenum of uniform quality can be prepared by bomb reduction techniques. Molybdenum trioxide (Mo03) and mixtures of molybdenum dioxide (Mo02) and trioxide were reduced by magnesium in closed steel bomb reactors. Very high pressures in excess of 5,000 p.s.i. developed during magnesium reductions of Mo03. The addition of calcium oxide to the bomb charges caused a significant reduction in pressure. Reaction efficiencies higher than 95 percent were obtained during magnesium reductions of either Mo03 or mixtures of Mo02 and Mo03, but high pressures were encountered when the charges contained from 30 to 60 percent Mo02. Reaction efficiencies were usually low (less than 80 percent) when the bomb charges contained more than 40 percent Mo02. The charges with the best composition considering operating pressure, yield, and purity contained from 10 to 30 percent Mo02. The addition of small amounts of carbon to the reaction charges was helpful because some deoxidation occurred during the reduction and also during subsequent arc-melting of the regulus metal. The purity of the bomb-reduced, arc-cast molybdenum metal ranged from 99.2 to 99.8 percent and in some instances the metal contained as little as 5 parts per million oxygen.

Jan 1, 1962

By R. Lincoln

A surplus of vanadium has resulted from the tremendous output of uranium, of which vanadium is a byproduct. More knowledge of the properties and characteristics of vanadium as a pure metal has been needed so that industry can take advantage of its availability and use it according to the best principles of conservation. Besides the problem of utilization, there is the ever present need of finding new materials which will satisfy specific and demanding requirements of science and engineering; vanadium or one of its alloys may possess the latent potential for filling some of these needs. Thus this? research project was undertaken by the Bureau of Mines to determine and examine some of the physical and mechanical properties of pure vanadium. A corallary investigation was the determination of the effect of the interstitial contaminants, oxygen, nitrogen, and carbon, on unalloyed vanadium. The vanadium used for these determinations was principally the product of experimental production of the Bureau. The evaluation of this material, as small quantities became available, provided most of the data that have been obtained.

Jan 1, 1962

By E. G. King

Heat of formation values for mercuric sulfide appear in all the comprehensive listings of thermodynamic data, but experimentally determined entropy values have been lacking. Consequently, all free energy calculations involving mercuric sulfide have been based upon estimated entropy values. This paper reports Bureau of Mines measurements of the low-temperature heat capacity of red mercuric sulfide (cinnabar) and the entropy value at 298.15° K. derived therefrom. The entropy value was combined with heat data to obtain free energy values for the formation of red mercuric sulfide from liquid or gaseous mercury and from rhombic or gaseous diatomic sulfur.

Jan 1, 1962

By H. J. Seim

An ion-exchange-instrumental analysis technique is described for analyzing impurities at 1 to 1,000 parts per million level in rare-earth metals. A cation-exchange flame photometric method is used for the alkali and alkaline earth groups of metals, and an anion-exchange procedure is used in conjunction with polarographic and X-ray fluorescence techniques for selected transition elements. The standard deviation is about 6 percent, and the average error, about 5 percent.

Jan 1, 1962

By Floyd G. Anderson

This report reviews and summarizes information on prevention and suppression of dust in mining, tunneling, and quarrying published in the United States during the years 1958 through 1960. Unpublished pertinent data developed or assembled by the Bureau of Mines during this period also are included. Silicosis statistics reported by the U.S. Public Health Service indicate a sizable silicotic population in the United States and suggest a need for greater dust-control effort. A joint medical-environmental survey was begun by the U.S. Public Health Service and the Bureau of Mines to evaluate the magnitude of the silicosis problem in the metal mining industry in the United States.

Jan 1, 1962

By John J. S. Sebastian

A laboratory-scale investigation was made of the basic problems involved in developing a ceramic heat exchanger to operate at high temperatures for using nuclear heat from gas-cooled process-heat reactors. Technical data were obtained on transferring heat by forced-convection from helium to air in a single-tube vitreous-alumina heat exchanger. Coolant air was passed through the annulus parallel with, and either concurrently or counter to, the flow of helium inside the tube. The data obtained pertain to removing heat from the helium. Average inside film coefficients were determined at mean surface temperatures of 200° to 1,570° F., inlet-gas temperatures of 1,450° to 2,665° F., and Reynolds numbers up to 560. The gas-to-surface temperature ratios were varied from 1.05 to 7.6. The tabulated results are shown in the appendix at the end of this report. The film coefficients of heat transfer were correlated by taking into account the physical properties of the helium at the average fluid temperature. With experimental conditions pointing to a laminar flow, the Nusselt number was found to decrease as the ratio of gas-to-wall temperature was increased to a value of 3. However, within the range tested, gas-to-wall temperature ratios above 3 did not affect the Nusselt number, regardless of the value of the Graetz number. Thus, beyond this point any increase in this ratio ceased to influence the heat-transfer relationship.

Jan 1, 1962

By John Ward Smith

The potential economic value of oil shale depends on the products from thermal degradation of the rock, because no other practical method for producing valuable material from oil shale has been found. Detailed study of thermal degradation behavior can aid in characterizing oil shales and their deposits and in evaluating oil-shale processing methods, Numerous publications describe various pyrolysis properties of oil shales (see surveys 3, 9, 11 and articles 1, 2, 4-8, 10, 12),4 but they do not describe a generally applicable analytical procedure for detailed evaluation of thermal degradation products. The analytical method presented here for such evaluations is designed to provide for: 1. Control of retorting conditions--temperature, heating, rate, reaction atmosphere--plus some control over retort pressure and carrier-gas flow, 2. Precise direct gravimetric measurement of the thermal degradation products--oil, water, gas, and spent charge (residue after thermal treatment of the charge). 3. Samples of all products. 4. Determination of the identities and amounts of gaseous compounds produced. 5. Elemental analysis and gross heating value of all products. 6. Determination of the distribution in the retorting products of the elements present in the original samples.

Jan 1, 1962

By Donald W. Mitchell

Research shows that water neutralizes the explosion hazard of coal dust when present in sufficient quantity and when intimately mixed with the dust. The quantity of water required to neutralize coal dust and coal-rock dust mixtures is about equal to the limiting moisture adsorptive capacity of the dust; the adsorptive capacity increases with increase in the fineness and volatile content of the coal. Pools of water or high atmospheric humidity do not reduce the explosion hazard. Although wetted dust is less dispersible than dry dust, poor dispersibility cannot be relied on as the sole safeguard against explosion. Dust mixtures that contain water in excess of their limiting adsorptive capacity are dispersed and ignited by severe initiation sources. Pure coal dust adsorbs water with difficulty and retains water poorly; adsorption and retention is increased by the addition of rock dust the coal; the rock dust agglutinates wetted coal and assures that incombustible is present should drying occur. Therefore, it is advantageous to rock-dust wet areas in bituminous coal and lignite mines. When coal-rock dust mixtures are wetted and subsequently dried, the explosion hazard is about the same as for dust which was not wetted.

Jan 1, 1962

By F. L. Wideman

This report describes a computer program that is used for the calculation of the coordinates and elevations of subsidence survey pins located by intersection. This program was developed for the Federal Bureau of Mines by the Numerical Analysis Laboratory, University of Arizona. These calculations, although relatively simple, are both tedious and time-consuming when computed with a desk calculator and trigonometric tables. In this survey, a large number of pins were surveyed repeatedly, and it was evident that both time and money could be saved by using a digital computer.

Jan 1, 1962