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By Wallace W. Key

The California pesticide industry in 1962 consumed about 30,000 tons of clay, talc, limestone, diatomite, sulfur, and other minerals as fillers (carriers and diluents) in pesticide formulation. This was 10 percent of the U.S. filler requirement for pesticides. About two- thirds of the California total was supplied by a few local mineral producers; the remainder came mainly from Florida, Georgia, and Wyoming. The objectives of this report are to provide data on quantities, sources, specifications, and market conditions for minerals used as fillers by California pesticide formulators. The study disclosed that specifications for mineral fillers have become more rigid and formulators have become more numerous in recent years. During 1962 over 1,200 firms registered 16,000 pesticide products with the Bureau of Chemistry in California. Factors which will tend to diminish future need for mineral fillers include the trend toward greater use of organic sprays rather than dusts and further development of biological controls, such as the development of sterile insect strains.

Jan 1, 1965

By D. R. Mathews

Electrorefined vanadium was evaluated with respect to tensile properties and the effects of interstitial contaminants in the temperature range of 77° to 273° K. The yield strength of 18,500 psi and hardness of 63 diamond pyra-mid hardness (DPH) of electrorefined vanadium are approximately equal to that of iodide crystal bar vanadium. The ductile-brittle transition temperature was found to be below 77° K, but with 0.175 weight-percent oxygen or 0.10 weight-percent nitrogen, it increased to between 123° and 190° K. With carbon content up to 0.11 weight-percent, the transition temperature remained below 77° K. The yield strength of the interstitial-containing alloys can be expressed by: au = 7.5 + 480 (pct N) + 290 (pct 0) + 280 (pct C), where au is the upper yield stress in 1,000 psi at 273° K. Profuse deformation twinning occurred in the alloys tested at 77° K. However, twinning could be suppressed by dissolved oxygen or nitrogen in excess of 0.15 and 0.086 weight-percent, respectively. Carbon, even though present in excess of the solubility limit, did not affect twinning.

Jan 1, 1965

By John E. Crawford

A year ago, if I had the pleasure of addressing you, I would have discussed ocean mineral resources from a promotional standpoint. I would have described exciting indications of mammoth tonnages of sea-floor industrial minerals. I would have attempted to fire your imaginations as to the potential of a nation having the technologic know-how to exploit its submerged boundaries. As a first step toward this capability, I would have solicited your support for a Bureau of Mines? program aimed at determining the industrial worth of marine minerals and devising techniques and hard- ware for their recovery. We still need your support, but recently we have ventured out of the realm of planning and into your Government's first program in marine mineral engineering. Today, I wish to describe what we have done within the framework of existing research problems and our possible goals. I will be brief so as to allow ample time for questions, and I can do this with confidence because our program is so new that I need not be chagrined at not having all the answers.

Jan 1, 1965

By B. Ramaswami

INTERNAL oxidation occurs readily in silver due to the rapid diffusion of oxygen in silver.' It has a marked effect on creep in polycrystalline silver2 and raises the critical resolved shear stress in single crystals of silver.3 However, the effect of oxygen on the work-hardening parameters of silver is not known. It is the aim of this paper to describe the effect of internal oxidation on the work-hardening characteristics of single crystals of silver and an Ag-0.1 at. pct A1 alloy. The materials used were: 99.99 pct Ag from Handy and Harman and 99.993+ pct A1 from Alcoa. Single crystals, 6 mm by 6 mm in cross section of silver and Ag-0.1 at. pct A1 of mo.5 orientation, i.e., the orientation with the Schmidt factor m = 0.5. were grown by the Chalmers technique.4 One set of specimens, referred to herein as oxidized specimens, was annealed at 940°C for 24 hr in a muffle furnace, in air, and furnace-cooled to room temperature. Another set of specimens, referred to as nonoxidized specimens, was annealed in oxygen-free helium at 940°C for 24 hr and furnace-cooled over a period of 7 hr to room temperature. The annealed single crystals were tested at room temperature in a floor-model Instron testing machine. The results are presented in Figs. 1 and 2. A

Jan 1, 1965

By Albert W. Deurbrouck

This report describes the preparation characteristics of 23 coal samples collected from nine of the more significant coalbeds of Fayette County, W. Va. In 1963 almost 5.4 million tons of medium to high volatile B coals of excellent quality for metallurgical and steam markets were produced in Fayette County. Of the 23 coal samples collected 11 would require some upgrading to pro-vide metallurgical quality products, 11 were acceptable as received, and 1 was a noncaking coal. Cleaning these coals to metallurgical standards would require only the removal of the sink 1.58 specific gravity material which would be quite easy as very little near-separating-gravity material was present at this gravity.

Jan 1, 1965

By R. C. Buehl

A pyrometallurgical process for recovering manganese from open-hearth furnace slags or low-grade manganiferous iron ores is described. The slag or ore is smelted in a blast furnace to produce spiegeleisen; the speigeleisen is then blown with air in a basic converter to give an oxide slag. This slag product contains 60 to 75 percent manganous oxide and may be considered a synthetic manganese ore. In the smelting operations coke rates for five test periods ranged from 3,255 to 4,130 lb per ton of spiegeleisen. The recovery of manganese in the spiegeleisen varied from 60 to 76 percent. Recovery increased to 83 percent when the open-hearth slag feed to the blast furnace was diluted with a high-? grade iron ore sinter to facilitate smelting. In blowing the spiegeleisen a cyclic procedure was developed that gave nearly 90 percent recovery of manganese in the slag product (synthetic ore) yet prevented excessive contamination of the slag by phosphorus and iron. The overall recovery of manganese was about 75 percent when iron ore sinter was used with the open-hearth slag in the smelting step. The metal remaining after oxidizing the manganese from the spiegeleisen contained approximately 3.5 percent phosphorus. It was refined in a basic converter by blowing with air in the presence of lime" A high--grade iron and a basic phosphate slag were produced.

Jan 1, 1965

By W. E. Anable

The Bureau of Mines studied the purification of commercially available yttrium by melting it in a 100-kw electron-beam furnace. Button-scale melts were made to determine the ultimate purification that could be attained by melting yttrium at 1,733° to 1,770° C at low pressure (0.05 to 0.1 micron) for 1 to 120 minutes. In addition, numerous melts were made to study the effect of doping yttrium with carbon, 17 selected metallic additions, and 3 compounds. Except for nickel and zirconium, the metallic impurities in yttrium were lowered significantly on extended treatment; silicon was lowered only slightly. The nonmetallic impurities} oxygen, nitrogen, and carbon, were not lowered except on short exposures. In isolated instances, the oxygen content was lowered from 5,860 ppm to about 5,000 ppm. In most instances the carbon con-tent was lowered from 545 to about 220 ppm in 20 minutes and then increased again. It was concluded that yttrium cannot be purified by direct heating or by the doping technique employed.

Jan 1, 1965

By Thomas A. Morgan

The distribution of stress adjacent to each of 25 mine openings was determined by the borehole stress-relief method in the FMC Corp. Westvaco trona mine at Westvaco, Wyo. The purpose of the stress determinations was twofold: First, to study the effect on these distributions of various factors such as opening shape, stress level, and loading history; and second, to estimate the distribution of stresses adjacent to extensive high-extraction (85 to 100 percent) areas. Stress distributions in areas of low average stress correspond closely to the theoretical distributions based on elastic theory. However, in areas of high average stress, the stress distributions are of a type associated with plastic failure. The stresses adjacent to a mined-out area supported by remnant pillars were significantly higher than the stresses adjacent to another area in which the remnant pillars were removed.

Jan 1, 1965

By Manuel Gomez

The heat contents of thermally dried lignite, subbituminous B coal, and their corresponding low-temperature chars were determined at various temperatures below the highest temperature to which these materials had been exposed before testing. Similar studies were made on high-temperature char and coke, spent shale, and ash prepared from both coal and spent shale. Heat content of the carbonaceous materials tested correlated well with temperature. Heat con-tent results for spent shale compared well with the published results. Statistical analysis of experimental data together with published information showed moisture, volatile matter, carbon content, and temperature to be the principal variables influencing the specific heat of coal. The specific heat of devolatilized carbonaceous substances, char and coke, approached that of graphite as the carbonization temperature was increased. The elemental specific heats of coal constituents, estimated from the ultimate analysis and the specific heat of coal, compared favorably with published elemental specific heats.

Jan 1, 1965

By T Salman

The construction and use of the B.E.T. (gas adsorption) apparatus is described. Examples are given for the determination of large and small surface areas using nitrogen and krypton. Introduction A NY study of the milling of ores from crushing to grinding, classification, and concentration and finally dewatering of the products involves solid particles which are either in contact with a gas or a liquid phase. The surface area of the solid and its characteristics constitute important parameters in all mineral dressing operations. The success of any particular operation is dependent on the interaction of the surface of the solid particles with the gas or the liquid phase. Particle size and specific surface (surface area per unit weight) continue to be important parameters in the flotation research associated with the adsorption of collector molecules or ions on mineral particles, as in the early years of mineral dressing research (1). In order to understand the mechanism of the flotation process, it is essential that the surface properties of the adsorbent be known.

Jan 1, 1965

By Curt D. Edgerton

This study was made to determine trends in fresh water usage by California petroleum refineries, to forecast fresh water requirements to 1975, and to evaluate water conservation practices. Statistical data used in the study were obtained largely from published sources and from records of selected companies. An adequate sampling of the State's refining capacity was obtained, and the data were extrapolated to the total California refining capacity. A breakdown of the data was then made on the basis of the following refining regions: (1) the Los Angeles Basin and Southern Coastal region, (2) the Southern San Joaquin Valley, and (3) the San Francisco Bay area. An unpublished forecast of crude oil input to refineries by a major oil company operating on the West Coast was used as a basis for predicting fresh-water usage. The 1963 fresh water intake by California petroleum refineries was 84 million gallons per day. This is expected to increase to 128 million gallons per day by 1975. The fresh-water to crude-oil ratio is increasing in all regions except the Southern San Joaquin Valley. At present, the supply of fresh water available to almost all of the State's petroleum refineries, mostly from surface sources and company-owned wells, is adequate, although shortages may develop within the foreseeable future. Present conservation methods are centered around the following four objectives: (1) minimum intake of fresh water of the lowest possible quality commensurate with sound technologic practice; (2) optimum recirculation; (3) proper treatment before discharge; and (4) substitution of air cooling for water cooling.

Jan 1, 1965

By D. H. Baldwin, R. E. Reed-Hill

DURING the course of experiments involving oxygen equilibrations with a high-purity Pd-5 at. pct Rh alloy, the appearance of a subscale was noted. Most of the heat treatments in a pure oxygen atmosphere were performed at 900°C. The presence of the subscale was noted when the oxygen partial pressure was in excess of approximately 95 mm, up to 1 atm, the highest pressure used. According to available thermodynamic information' on the free energy of formation of Rh2O3 (the only reliably reported solid oxide of rhodium), this oxide should not be stable under these conditions, nor, of course, any oxide of palladium. Extraction of the subscale from the matrix was affected by treatment with aqua regia, and the resulting X-ray diffraction powder pattern is shown in Table I. This pattern is not that of Rh2O3, nor that of any known rhodium or palladium oxide. It can be indexed on a hexagonal lattice with a. = 5.22Å and co = 6.0Å. In addition to this unknown material, there was a weak Rh2O3 pattern. An X-ray fluorescence analysis of the powder gave 3214 palladium counts per sec and 5381 rhodium counts per sec, thus indicating the likelihood of a double oxide of palladium and rhodium. In view of the fact that the above result was obtained on a single sample, it is perhaps best not to insist upon the above ratio of about 0.6, but possibly to tentatively assume 0.5 or 1/1. The small amount of Rh2O3 in the X-ray pattern might have occurred on cooling, and it seems possible that the double oxide, below some temperature level, is not as stable as Rh2O3. To examine this point, some of the extracted double oxide was heated on a sheet of pure palladium in air at 900°C, and allowed to furnace-cool over a period of several hours. The X-ray diffraction pattern of the powder showed approximately the same intensity of Rh2O3 and the "hexagonal" oxide as before, but, in addition, a rather faint pattern of another crystalline species made its appearance. This finding again suggests partial transformation of the major (double) oxide to other oxides on cooling from 900°C. Application of the phase rule shows that only one equilibrium oxide (subscale) could have been present at temperature. Vacuum-fusion, oxygen analysis of the extracted subscale showed 7.7 ± 0.7 pct O. Combining this information with that of the X-ray fluorescence analysis suggests the formula PdRhO. This compound should have an oxygen content of 7.07 pct, which is within the range of error of the oxygen analysis. However, until a more careful stoichiometric study is made, it is suggested that the formula be written

Jan 1, 1965

By G. W. Birge

Fifteen coal samples, representing the Winifrede, Chilton, Alma, No. 2 Gas, Powellton, Eagle, Douglas, Sewell, Beckley, Pocahontas No.4, and Pocahontas No.3 beds in Wyoming County, and five samples, representing the Fire Creek, Pocahontas No.6, and Pocahontas No.3 beds in Mercer County, W. Va., were carbonized at 9000 C by the Bureau of Mines-American Gas Association (BM-AGA) method, and yields of products and physical properties of cokes were determined. Expansion characteristics of the majority of samples were determined in the Bureau of Mines sole-heated oven. Chemical analyses and agglutinating values were determined for all coals. The coals were mostly strongly coking and low in ash and sulfur content. Dry, mineral-matter-free fixed-carbon content of the Wyoming County coals ranged from 63.0 to 83.4 percent. The Mercer County samples were all low volatile in rank. Yields of carbonization products were generally in accord with yields from similar rank coals of the Appalachian region. Because of their expanding tendencies, most of the medium-and low-volatile coals would require blending with lower rank coal for normal coke production.

Jan 1, 1965

By H D. Smith

T HE production of coal in Canada was slightly higher in 1964 than in the immediate past, and the major users continue to be the electric utility and metallurgical industries. There are continuing trends toward the increased use of cokes and chars in various metallurgical applications. Geological Research During 1964, the coal drilling program of the Research Council of Alberta (RCA) was concentrated in the extreme south of the Province (notably in the Milk River area and the region immediately to the northeast of this area). Field work commenced on June 1 and was completed at the end of September, by which time a total of 376 holes, aggregating some 48,500 ft., were drilled in 132 townships. Although no new major coal occurrences were intersected, the pro-gram yielded useful data for defining the extent of the known coal deposits in the area. Detailed results will be analyzed during the winter and reported in due course. Meanwhile, a full report on the

Jan 1, 1965

By Joseph A. Cavallaro

This report describes the timed release analysis technique that was developed to serve as a tool for assessing the froth flotation cleaning potentials of fine-size coals. Using this developed technique, 16 coals from 10 different coalbeds were tested. All of the coals included in this study were quite amenable to froth flotation with float coal yields ranging from 80.7 to 99.5 percentage points. Float-and-sink analyses of the coals tested are shown to be of limited value in predicting froth flotation cleaning potential. Generally the float-and-sink analyses indicated a better product could be obtained than froth flotation could provide; although, in four of the coals tested froth flotation results were superior to those expected from the gravimetric analysis. The fixed carbon content of the samples collected was found to correlate with the floatability of the coals. The higher rank coals were the most readily floatable coals while the lower rank coals did not respond quite as well to flotation.

Jan 1, 1965

By Frank A. Jerabek

Problems of mine backfilling and fill material deposited underground, the characteristics and relationship between the deposited fill material and overlying ground, and the practical applications and limitations of hydraulic backfilling as ground support are discussed. A great variety of materials ranging from coal washery refuse to concentrator tailings is used as hydraulic fill. Some materials will solidify and cement; others will resemble quicksand, Hydraulic fill as ground support is more efficient in inclined mine openings than in horizontal mine openings, where it cannot be placed tightly to the back. This and other deficiencies of hydraulic backfilling led to the development of pneumatic stowing. Research work in hydraulic backfilling at the Pennsylvania State University is also discussed. This research work includes the investigation of segregation in the discharged fill slurry, the quantity of solids escaping in the drain liquid, the relationship of escaping solids to slurry concentration and discharge rate, and the compressibility of fine fill material.

Jan 1, 1965

The principal activities of the Bureau of Mines Explosives Research Center from July 1, 1962, to June 30, 1963, are described briefly in part 1. Part 2 gives short abstracts of publications that appeared during fiscal year 1963; in general, the research reported in these publications antedates the report period.

Jan 1, 1965

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grind-ability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions4 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1965

By Wallace W. Key

The California pesticide industry in 1962 consumed about 30,000 tons of clay, talc, limestone, diatomite, sulfur, and other minerals as fillers (carriers and diluents) in pesticide formulation. This was 10 percent of the U.S. filler requirement for pesticides. About two-thirds of the California total was supplied by a few local mineral producers; the remainder came mainly from Florida, Georgia, and Wyoming. The objectives of this report are to provide data on quantities, sources, specifications, and market conditions for minerals used as fillers by California pesticide formulators. The study disclosed that specifications for mineral fillers have become more rigid and formulators have become more numerous in recent years. During 1962 over 1,200 firms registered 16,000 pesticide products with the Bureau of Chemistry in California. Factors which will tend to diminish future need for mineral fillers include the trend toward greater use of organic sprays rather than dusts and further development of biological controls, such as the development of sterile insect strains.

Jan 1, 1965

By T E. Tibbetts

This paper deals with coal sampling in general and with mechanical coal sampling in particular. The necessity of obtaining representative samples is emphasized. Other sections of the paper are devoted to the design and selection of automatic samplers, with a consideration of the three main types, and the testing, operation and maintenance of these samplers. The cost of the installation of an automated sampling system must be related to the value of the material to be sampled, to the volume of coal involved, and to the savings in labour and economy which can be achieved. Introduction T HE Committee?:; on Coal Sampling of the Coal Study Subsection, Thermal Power Section (Eastern Zone), Canadian Electrical Association, was established in November, 1963, to "study the various problem areas of coal sampling." The first undertaking of the Committee was to at-tempt to survey the problem areas of coal sampling through an evaluation of coal sampling difficulties as experienced at both the plant design and operational levels within the electric utilities represented on the Committee. The results of this enquiry indicated that satisfactory answers to almost any conceivable

Jan 1, 1965