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By R. D. Berkenkotter

Titanium and iron assays obtained from cores of three diamond-drill holes from the Cebolla Creek titaniferous iron deposit were evaluated by statistical techniques to obtain information concerning the mineral characteristics of the deposit and to make a preliminary determination of sampling requirements for the deposit. A range of sample volumes representing sizes from one-sixth NX core 2 feet in length through full NX core 10 feet in length were prepared by split-ting the NX core with a diamond saw and combining pulverized splits. Results indicate the existence of at least two statistical populations having different average grades of iron and titanium. Each has an assay frequency distribution that is not normal but is highly peaked (leptokurtic). Frequency distributions of assays from specific altered zones of the drill holes appear to be normally distributed. Increasing the cross-sectional area of the sample unit to change assay volume did not result in significant changes either in assay values or the resulting frequency distributions of assays. However, when assay volume is increased by increasing sample interval, the shape of the assay frequency distribution changes, and a normal distribution of assays is approached. Positive correlation exists between titanium and iron assays. The degree of correlation, although very significant, is too low to use for prediction purposes. Although the amount of data from three widely separated drill holes is not sufficient to establish an average grade for this large deposit, it indicates a range of expected assay values and provides some information for determining requirements of future sampling for evaluation purposes.

Jan 1, 1963

By Robert C. Johnson

Water-swelling fluormicas and fluormontmorillonoids were synthesized and described. They were found predominantly in the system Mg0 - MgF2 - Si02, with varying amounts of Li+ or Na+, Some water-swelling synthetic minerals were prepared with only strontium or lead in the twelvefold position, Water- swelling compounds containing either K+ or Ba+ were not found. The synthesized water-swelling products were shown by electron microscopy, X-ray diffraction, and chemical analysis to be typically two-silica-layer, platy compounds, Except for the complete substitution of fluoride for hydroxyl, the compounds were similar to the natural micas or montmorillonites. The stability and properties of the compounds were further established by electrodialysis, by differential thermal analysis, and by anion and cation exchange methods. Fluoride in the interlayer positions was nonexchangeable except through decomposition of the product. Exchanging the sodium or the lithium of the synthetic fluormicas or fluormontmorillonoids with potassium ion, particularly those derived from KOH provided a product from which a completely inorganic paper of extraordinary flexibility was fabricated. This paper had excellent mechanical and electrical properties except for water adsorption and a high power factor. Neither of these problems was solved during this investigation. However, papers with dielectric strength from 1,500 to 5,000 volts per mil were readily fabricated, particularly from the lithium containing fluormicas or fluormontmorill onoids.

Jan 1, 1963

By Carl Rampacek

The conversion of dilute sulfur dioxide gas into sulfuric acid by autoxidation in mechanical cells of the flotation or gas absorber types was investigated. Bench-scale tests were made with sulfur dioxide-air mixtures to determine the influence of several factors on autoxidation of sulfur dioxide, using iron and manganese salts as catalysts. The laboratory investigation subsequently was extended to pilot plant acid-making tests, using a modified turbomixer gas absorber having a 12-inch-diameter impeller. Sulfur dioxide gas was produced for the tests by roasting pyrite in a fluidized-bed reactor. In the better tests, made with manganese sulfate as the catalyst, the equivalent of 1,000 pounds of anhydrous H2SO4 was produced per 24 hours as a 10-percent solution; power consumption was 0.2 kwhr per pound of equivalent anhydrous acid synthesized. The batch and continuous tests demonstrated the technical feasibility of producing dilute sulfuric acid by autoxidation of sulfur dioxide gas in mechanical cells when converting pyrite roaster or waste smelter gases.

Jan 1, 1963

By H. C. Carpenter

Lignite tar made by low-temperature Lurgi-Spülgas carbonization of North Dakota lignite was hydrocracked in single-pass, fixed-bed operation at 3,000 pounds per square inch over cobalt molybdate catalyst to produce gasoline, and at the same pressure, over zinc chromite catalyst to crack the high-boiling phenolic compounds to low-boiling phenolics. Hydrocracking the raw tar or the creosote-oil fraction from the tar over cobalt molybdate removed most of the oxygen, sulfur, and nitrogen in the forms of water, hydrogen sulfide, and ammonia, and produced gasoline yields from 31 to 59 volume-percent. The gasoline fractions contained from 0.1 to 7.7 volume-percent tar acids, but tar-base percentages were too low for reliable measurement; removal of these materials with dilute caustic and acid solutions also reduced the sulfur and nitrogen to 0.01 weight-percent or less.

Jan 1, 1963

By Robert S. Warfield

The Bureau of Mines investigated a geologically favorable area in the Beluga River coalfield in south-central Alaska to determine if there were sufficient minable coal reserves for onsite utilization to meet the projected thermal power needs of the Anchorage area. A program of diamond core drilling and sampling delimited a shallow saucerlike structure estimated to contain indicated reserves of more than 20 million tons of subbitminous coal in a seam over 50 feet thick that could be mined by opencut methods. A large sample of fresh coal was taken across the full width of the seam for washability studies. This sample, with 4 volume-percent of clay partings eliminated, contained 24.4 percent moisture and 16.8 percent ash and had a calorific value of 7,162 Btu per pound. The studies indicated that mechanical cleaning would be of doubtful value.

Jan 1, 1963

By A. W. Deurbrouck

Five preparation plants employing concentrating tables for washing 3/8- inch to 0 raw coal were tested. Two of the plants were washing Pittsburgh-bed coal, two were washing Pocahontas-bed coal, and one was washing Elkhorn-bed coal. Samples of the feed to and products from the tables were collected over the normal operating shift. These samples were analyzed, and complete performance criteria were determined. The results of this study show that the concentrating table is an effective fine-coal cleaner even when operating at 40 percent over the recommended 10 tons per hour feed rate. Recovery efficiencies for the 3/8-inch to 200- mesh size fraction ranged from 97.3 to 99.3 percent; maximum yield errors and ash errors were 2.4 and 1.0 percent, respectively; probable errors ranged from 0.074 to 0.115 specific gravity units and error areas from 52 to 73 square centimeters. The amount of minus 200-mesh material in the water used for feed water and dressing water to the table had no significant effect on the sharpness of the separation achieved but did have an effect on the ash content of the clean- coal product. In the one plant studied, the substitution of fresh water for plant circulating water reduced the ash content of the clean coal by about 6 percentage points.

Jan 1, 1963

By L. J. E. Hofer

This Bureau of Mines study, part of a broad program of research in air pollution related to minerals, was conducted to determine the nature and extent of the poisoning of catalysts when used to remove certain air pollutants from exhaust gases. The poisoning examined in this investigation occurs when leaded gasoline is used as a fuel for automotive engines. This research was conducted in cooperation with the Public Health Service. The smog in the Los Angeles area is attributed to the effect of radiant energy on the mixture of hydrocarbons and nitrogen oxides found in the atmosphere there. A large portion of the hydrocarbons is believed to originate in the exhaust gases of automobiles. To prevent the escape of these hydrocarbons into the atmosphere catalytic mufflers have been proposed. In principle, these are simple and nonmechanical, consisting of a vessel charged with a catalyst capable of destroying the exhaust hydrocarbons by catalyzing their oxidation. However, these catalysts are severely affected by the particulate matter, mainly in the form of lead sulfate (PbS04), lead oxysulfate (PbS04.Pb0), and Lead chlorobromide (Pb(Cl,Br)2), contained in the exhaust gas. Deposition of lead on the catalyst as PbS04, PbS04, PbS0, and Pb(Cl,Br)2 restricts catalytic activity. As a result,after 20,000 miles of operation the temperature necessary to achieve 50-percent conversion of isopentane in a mixture of 0.2 percent isopentane, 2 percent carbon monoxide and 4 percent oxygen, and the balance nitrogen at 10,000 hourly space velocity has risen from 400° C. to 500° C. even with a catalyst taken from the exit portion of the catalyst bed. The rest of the catalyst was more severely affected. Therefore, it would appear that operation for 20,000 miles is near the limit for a catalyst.

Jan 1, 1963

By G. W. Birge

Twenty-eight samples, representing the Pittsburgh, Lower Kittanning, Stockton-Lewiston, Coalburg, Winifrede, Cedar Grove, Peerless, No. 2 Gas, Powellton, and Eagle 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. Expanding characteristics of 22 of the samples were determined in the Bureau of Mines sole-heated oven. The Kanawha County coals tested were high-volatile A bituminous in rank, with dry, mineral-matter- free fixed- carbon contents ranging from 53.9 to 66.3 percent. With few exceptions, they were chemically satisfactory for metallurgical use, and most of the coke-strength indexes were within the industrially accepted range for high-volatile blending coals.

Jan 1, 1963

By W. W. Weller

Low-temperature heat capacities of scandium sesquioxide (Sc203) and a mixture of cerium sesquioxide (Ce203) and cerium dioxide (CeO2) were measured over the temperature range from 50° to 298° K. The entropy of scandium sesquioxide at 298.15° K was evaluated directly as S°298.15 = 18.4 ± 0.1 cal/deg mole. That of cerium sesquioxide was extracted by combining the heat-capacity data for the mixture with those for pure cerium dioxide; the result was S298.15 36.0 ± 1.0 cal/deg mole.

Jan 1, 1963

By P. E. Churchward

Rhenium sources and recovery methods were investigated by the Bureau of Mines to delineate potential resources of the metal. The only significant rhenium resource appears to be about 28,000 lb of rhenium contained in the domestic annual output of approximately 20,000 tons of byproduct molybdenite concentrates from porphyry copper operations. An estimated 70 to 80 pct of this rhenium is potentially recoverable by processing the rhenium-bearing fumes and dusts obtained during conventional roasting of molybdenite concentrate. At 70 pct recovery this would amount to 19,600 lb of rhenium. A more conservative estimate by the Committee on Refractory Metals of the National Research Council (1513 is that 12,000 lb of rhenium metal could be produced annually from current production of molybdenite from porphyry copper operations in the United States. A procedure was developed in the laboratory for recovering rhenium in the form of electrolytic flake by electrowinning the metal from a solvent extraction strip solution. The procedure included (1) water leaching of molybdenite roaster flue dust, (2) selective extraction of rhenium from the leach liquor by contacting it with a kerosine solution of a quaternary amine, (3) stripping of rhenium from the loaded organic solution by a perchloric acid solution, and (4) electrodeposition of rhenium from the loaded strip liquor. Raw material for the studies was flue dust containing 0.48 pct Re, 35 pct Mo, and 23 pct S in sulfide and sulfate form, and small amounts of numerous metallic impurities. Water leaching dissolved 85 pct of the Re and yielded a solution that was 13 in sulfuric acid and contained, 1 g/l Re and 16 g/l Mo. The solvent extraction strip solution that was electrolyzed for rhenium deposition was 1 molar in perchloric acid and 1 molar in ammonium sulfate and contained 13 g/l Re and 0.01 g/l Mo.

Jan 1, 1963

By L. B. Pankratz

High-temperature heat-content values of pure lutetium sesquioxide and dysprosium sesquioxide were measured over the temperature range from 298° to 1,800° K. Similar data for cerium sesquioxide were calculated from measurements of a mixture of cerium sesquioxide and dioxide and known values for cerium dioxide. The results for lutetium sesquioxide are regular. Dysprosium sesquioxide has a minor thermal anomaly near 1,590° K, the extra heat absorption being 220 cal/mole, Hexagonal cerium sesquioxide undergoes a transformation around 1,050° K, which is only slowly reversible; consequently results were obtained for both the low- and high-temperature varieties. The original heat-content data are reported, and smooth values of heat content and the corresponding entropy increments are tabulated. Equations were derived to represent the heat-content values.

Jan 1, 1963

By Edward W. Parsons

Conventional rock-bolt anchors often fail when installed in weak formations. The purpose of this work was to develop an anchor that would utilize an explosive charge to secure anchorage in any type of rock. Laboratory work to develop a rock-bolt anchored by explosive forming was initiated using rock-bolt models which had a drilled explosive chamber and were composed of various metals. This was followed by the use of several types of seamless tubing which were expanded with a water-coupled explosive capsule. By attaching a length of solid bolt to the anchor tube, a prototype explosive-anchored rock bolt was made. More than 150 laboratory models were expanded during this phase of development, During two field tests in underground mines (A and B) and one in an open- cut mine (C), 87 explosive-anchored bolts, 9 slot-and-wedge bolts, 2 bolts anchored with expanding grout, and 28 expansion-shell bolts consisting of three types of shells were installed and subjected to pull tests. The field tests were run to determine the effects of variables such as the amount and placement of the explosive charge, design changes in the bolt, and the effect on anchorage of different pull-test techniques. The field tests revealed the following: Mine A. The explosive-anchored rock bolt was feasible, but changes were necessary in bolt materials and in some details of bolt design. Mine B. The design and materials of the bolt gave excellent results in hard fractured rock, but no information was obtained concerning variations in the dimensions of the anchor unit or in the explosive charge. Nine C. Varying the explosive charge to produce a beaded surface on the bolt tube and tightening of the anchored bolt before pull-testing were found to increase significantly the anchorage obtained in soft ground.

Jan 1, 1963

By C. J. Thompson

Two sulfur compounds--the 2,2,5-trimethyl- and the 2,2,5,5-tetramethyl derivatives of thiacyclopentane--were identified in Wilmington, Calif., crude oil, using microdesulfurization and gas-liquid chromtography techniques.

Jan 1, 1963

By G. T. Krempasky

This report covers the installation and evaluation of lb reinforced concrete sets, 6 in each of 3 mines in the Goeur d'Alene mining district, Shoshone County, Idaho, and is the second of a series to determine the feasibility of a more permanent type of mine support. Closure measurements, where applicable, were made periodically of the concrete-set installations and were compared to the initial cross section of the sets. A different method of blocking was used at each test site; at one test site the type of blocking was changed several times during the test. Results from each test site are reported separately. No attempt was made to compare the cost of the concrete installations with the cost of other types of support used in the district. Such an evaluation of permanent types of support would require a longer period of time. At this time, tests are not complete enough to determine the applicability of underground concrete supports. However, results to date tend to confirm the general opinion that precast concrete mine supports could be used to advantage in openings that require support and must have long life, especially where decay of timber is an important factor.

Jan 1, 1963

By A. A. Cochran

The objective of the research was to determine the final distribution of cerium additions to steel, their effect on sulfide inclusions, and the usefulness of radiotracer methods in investigating steel problems. Fifty-gram heats of steel were prepared that contained either cerium 141 and nonradioactive sulfur, or sulfur 35 and nonradioactive cerium. These steels were studied by autoradiography, measurements of their surface radioactivities, optical microscopy, and chemical analysis. Samples of the crucibles were analyzed quantitatively for cerium or sulfur by radioactivity counting methods. The addition of cerium to steel melts reduced the size and number of iron sulfide inclusions in the resulting steel. A significant fraction of the sulfur and most of the cerium penetrated into the MgO crucible during the melting operation, The cerium inclusions in steel were identified as cerium sulfide. Radiotracer methods were found to be versatile and highly sensitive.

Jan 1, 1963

By M. J. Kovalik

The effect of oxidation by air at temperatures ranging from 200° to 390° C on the change of chemical and physical properties of Pittsburgh-bed coal was studied as a function of processing time and temperature. The goal was to prepare a nonagglomerating fuel from a strongly coking coal for use in continuous carbonizing processes and in fixed-bed gasifiers. The oxidized coal was carbonized in a bench-scale apparatus, and the coke strength was evaluated in a Roga tumbler. Strength of the coke was progressively reduced with time of oxidation until the coking power of the coal was apparently destroyed. Time requirements to obtain an essentially nonagglomerating product were inversely related to processing temperature. Gaseous products released from the coal during oxidation reduced the yield of the desired nonagglomerating product, which decreased with time of oxidation at constant temperature and with increase in processing temperature at equal time. Oxidation at a temperature slightly above the lower limit of the plastic temperature range of Pittsburgh-bed coal was most effective because of the short processing time required and moderate processing losses.

Jan 1, 1963

By Charles Prasky

This report describes fluidized bed techniques employed by the Bureau of Mines at Minneapolis to differentially sulfatize the manganese in two samples of low-grade manganiferous ferruginous carbonate slates from the Cuyuna Range district, Minn. Suitable mechanics of operation were established. A space rate of 1.25 to 1.5 fps, a retention time of 3 to 3.5 hours, a temperature of 700° C, and a 10 percent sulfur dioxide gas in air were adequate for sulfatizing the slates by fluidization. Under these conditions the overflow product removal rate from the 4-inch-diameter reactor was 4 to 5 pounds per hour. The sulfur dioxide was used more efficiently in the two-stage treatment than in the single-stage treatment. However, approximately 80 percent of the manganese was converted to sulfate by either treatment.

Jan 1, 1963

By R. E. Mussier

This investigation was made to study new methods to prepare high-purity yttrium metal, Various methods were used to prepare pure intermediate compounds, primarily chlorides, bromides, and iodides, which were subsequently reduced to metal. The process found most suitable for the preparation of pure anhydrous yttrium chloride involved thermal dehydration of a mixture of hydrated yttrium chloride and ammonium chloride while under vacuum. Yttrium bromide and iodide were prepared most effectively by the direct halogenation of yttrim carbide. Yttrim carbide was obtained by reacting and melting yttrium oxide-carbon mixtures in a carbon-arc furnace. Yttrium halides were purified by vacuum distillation and reduced by alkali or alkaline-earth metals. Lithium and sodium proved to be the best reductants from the standpoint of yield (>95 pct) and purity (>99.8 pct) of the yttrium. The product of the reduction step was sponge metal, which was consolidated readily by conventional cold-mold, arc-melting procedure. The purest yttrium obtained in laboratory scale work was prepared by sodium reduction of yttrium chloride and contained only 125 pp oxygen; other impurities did not exceed 1,000 ppm. In larger scale tests yttrium containing only 800 to 1,000 ppm total impurities was obtained by lithium reduction of yttrium chloride. The tensile properties of high-purity yttrium were determined. Mechanical tests showed that yttrium can be forged, extruded, rolled, spot welded, and deep drawn.

Jan 1, 1963

By G. W. Birge

Carbonizing properties of the principal coalbeds of Elk, Clarion, Jefferson, Clearfield, and Centre Counties, Pa,, are described in this Bureau of Mines report, Twenty-six samples, representing the Upper Freeport, Lower Freeport, Upper Kittanning, Middle Kittanning, Lower Kittanning, and Brookville beds, were carbonized by the Bureau of Mines--American Gas Association (BM-AM) method, and yields of products and physical properties of cokes were determined. Expansion or contraction of the majority of the samples was measured in the Bureau of Mines sole-heated oven. Chemical analyses, agglutinating values, and free-swelling indexes are given for all samples. In this area the coals generally are characterized by high sulfur and moderately high ash content, and their suitability for metallurgical use would depend largely upon satisfactory cleaning. The samples from Elk, Clarion, and Jefferson Counties were high-volatile A bituminous In rank, whereas, most samples from Clearfield County and all those from Centre County were of medium-volatile rank. Coals from Clarion County had dry, mineral- matter-free fixed-carbon contents ranging from 56.5 to 60.3 percent and were weakly coking. With the exception of two samples which contained excessive ash, the medium-volatile coals of Clearfield and Centre Counties were strongly coking and, as indicated by sole-oven expansion results, would require blending with lower rank coal to avoid oven damage.

Jan 1, 1963

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