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By F. E. Block

The metallic reduction of vanadium chlorides was investigated by the Federal Bureau of Mines as a possible new route for preparing vanadium metal in an effort to develop a production process that would be adaptable to large-scale plant production and would yield metal of uniformly high quality. Vanadium tetrachloride was usually prepared by chlorinating vanadium pentoxide in the presence of carbon. Although oxygen-?free tetrachloride was difficult to prepare this way, it could be prepared by the direct chlorination of vanadium carbide. Lower valent vanadium trichloride was prepared by the thermal decomposition of vanadium tetrachloride. Vanadium dichloride was also prepared by the thermal disproportionation of vanadium trichloride.

Jan 1, 1961

By W. J. Wenger

Oil fields in the Powder River Basin of Wyoming have produced 731 million barrels of petroleum through 1959. Production in 1959 was 32 million barrels, the highest production since 1924. The record production was in 1923, when the Basin produced 38 million barrels of oil and the Salt Creek field, then at its peak, produced 35 million barrels. In this report, the characteristics of crude oils found in the Basin are used as a basis for determining the best re-fining uses for the oils and for predicting the characteristics of oils that may be discovered in the Basin in the future. Analyses of 108 oils sampled over a period of 30 years are presented Crude oils of two major types are produced from the Powder River Basin. One has a low sulfur content and occurs in younger formations, and the other has a high sulfur content and occurs in older formations. The oils with low sulfur contents are generally light colored and waxy, and may be either paraffinic or naphthenic. The oils with high sulfur contents are usually dark colored and asphaltic; only their low boiling fractions are paraffinic. Alteration appears to account for the anomalous properties of some oils found at shallow depths. Shapes and slopes of correlation index curves classify the oils into the same two groups as their sulfur contents, with gently sloping curves representing the low-sulfur oils and steep curves representing high-sulfur, asphaltic oils,

Jan 1, 1961

By Miles B. Royert

Crude Minnesota taconite was charged in the Bureau of Mines experimental blast furnace so that smelting characteristics of such highly siliceous raw materials could be studied and smelting costs compared with those of a standard Mesabi ore. The Bureau recognized that the highly siliceous nature of the crude ore and its relatively low metallic content would be serious economic deterrents to commercial use of the raw taconite, but compensating factors would be low capital investment in production facilities, large tonnage available on short notice, high recoveries of iron, and low delivered cost. Crude taconite smelted readily in the experimental blast furnace. Coke consumption per ton of metallic product was very high, compared with the average established requirements for smelting normal grades of metalliferous raw materials. Slag rates were also inordinately high. Metal quality was erratic as to silicon, and sulfur contents were objectionably high.

Jan 1, 1961

By John Ward Smith

This paper describes and evaluates a method that the Federal Bureau of Mines used to determine the ultimate composition of the organic material in 10 samples of oil shale from the Mahogany zone of the Green River formation in Colorado and Utah. Since interest has centered on the Mahogany zone, the richest section of the deposit, these 10 samples were chosen to provide a broad representation of this zone with the objective of obtaining generally valid ultimate composition values. The most probable organic composition for the Mahogany zone and the 95-percent confidence limits for each component average (in weight-percent of organic material) are: Carbon 80.5 ± .4 Hydrogen 10.3 ± .1 Nitrogen 2.4 ± .1 Sulfur 1.0 ± .1 Oxygen 5.8 ± .5 As only minor variations in composition were observed, the organic material of this particular bed is quite similar over a wide geographic area.

Jan 1, 1961

By P. G. Clites

A laboratory furnace was developed by the Federal Bureau of Mines for use in studying the interrelationships among variables associated with skull melting and casting high-temperature metals. Although additional work is necessary to determine the extent to which the information obtained by using this furnace can be extrapolated to larger furnaces of the same type, many casting characteristics of metals and alloys can be determined on equipment of this size. This furnace is a laboratory-size, consumable-electrode, skull-casting furnace equipped with a water-cooled copper ladle. The ladle, which is a tilt-pour or over-the-lip type, has a volume of approximately 30 cubic inches and provides up to 20 cubic inches of molten metal for castings. Castings of various reactive and refractory metals, including zirconium, titanium, hafnium, columbium, molybdenum, tantalum, and tungsten, have been produced. In addition, castings of iron, chromium, and copper have been made. The simplicity and versatility of the apparatus would make it useful to metallurgical laboratories preparing cast specimens.

Jan 1, 1961

By R. J. Gajan

As part of its research program on secondary metal refining, the Federal Bureau of Mines has developed a fast method for determining aluminum, iron, copper, cadmium, and lead in zinc-base alloys. The new method is intended for use by trained technicians in laboratories with inexpensive equipment. It can be used either in the analytical laboratories of the many small plants that are characteristic of the secondary metals industry or in laboratories engaged in basic research to improve refining processes. A complete analysis for the foregoing elements can be made in less than 3 hours from a single sample in solution. The method is especially helpful when a small amount of sample is available. Aluminum and iron are determined spectrophotometrically and the other elements polarographically. The new method is now being used for control analysis in metallurgical research, and the results compare favorably with previously used spectrographic methods. Luke and Braun4/ described a photometric method for the determination of aluminum in zinc diecasting alloys in which the aluminum was complexed with Aluminon reagent (ammonium salt of aurintricarboxylic acid), forming a red lake. An adaptation of this method was used for determining aluminum. Beers law is obeyed between 0.01 and 0.06 milligram of aluminum.

Jan 1, 1961

By G. V. Sullivan

This report summarizes the results of metallurgical investigations by the Federal Bureau of Mines of manganese oxide ore, averaging 23 to 25 percent manganese, stockpiled at the Butte-Philipsburg depot of General Services Administration (GSA). The oxide ores were stockpiled in two general classifications, straight oxide ore and mixed oxide-carbonate ore. Continuous-circuit flotation tests at the Albany (Oreg.) Metallurgy Research Center of the Bureau of Mines showed that each of these ore types could be concentrated by an oil-emulsion scheme to produce a concentrate that could be sintered to meet program specifications. About 88 percent of the manganese was recovered in the concentrate from the straight oxide sample, with the sintered concentrate containing 48 percent Mn. The sintered concentrate from the mixed oxide-carbonate sample contained 41 percent Mn with a recovery in the concentrate of 95 percent.

Jan 1, 1961

By James S. Browning

The purpose of this investigation was to develop a dependable and economic method for recovering spodumene and mica from pegmatites of the type found in Gaston County, N. C. Laboratory batch tests and continuous flotation tests were made by the Federal Bureau of Mines to determine the feasibility of treating the ore by flotation to recover high-grade spodumene and mica concentrates. The spodumene flotation circuit yielded concentrates containing 6.50 percent lithia (Li20), with an overall recovery of 81.8 percent of the lithia in the ore, The mica circuit yielded concentrates containing 97.5 percent mica, with a recovery of 82.5 percent of the mica in the spodumene tailing.

Jan 1, 1961

By A. S. Moore

The Bureau of Mines is doing research and development work on removing acid-gas impurities from synthesis gas made directly from coal. Since conventional gas scrubbers, packed towers and bubble-cap columns, are expensive to construct and difficult to operate with viscous solutions, one aspect of the work was developing a compact, agitated, gas-liquid contactor for use with concentrated absorbents. The efficacy of the agitated contactor for absorbing carbon dioxide in diethanolamine increased with increasing solution rate, turbine speed, diethanolamine concentration, and carbon dioxide concentration in feed gas, and with decreasing liquid-gas ratio. It was unaffected by pressure between 200 and 300 p.s.i.g. and little affected by temperature between 115 and 190° F.

Jan 1, 1961

By W. S. Landers

This report presents a study by the Federal Bureau of Mines of technical factors related to the production of special carbon and tar from selected Wyoming coals. Certain Wyoming high-volatile bituminous and subbituminous coals were processed in bench-scale apparatus to determine potential carbonization yields and in pilot plant retorts to produce sufficient char and tar for testing. These tests have shown that a critical selection of coal is necessary when the coal is processed for a specialized carbon. Generally high yields of tar are obtained from low-temperature carbonization of Wyoming high-volatile bituminous and subbituminous coals, and the yield of tar usually increases with increase in rank within this range of coals. The production and evaluation of industrial carbons from Wyoming coals by using pilot plant and bench-scale techniques is part of the continuous program of upgrading western coals. It has been found that: 1. Most Wyoming coals are nonagglomerating and may be carbonized in fluidized systems. Chars produced in pilot plant retorts at low temperatures contain about 17 to 23 pct, residual volatile matter and are easily ignited. These chars appear suitable as power plant fuel. The tar-plus-light-oil yields range from 14 to 40 gal./ton of raw coal processed. 2. Wyoming high-volatile coals produce a slightly smaller and somewhat weaker coke than currently mined Western United States high-volatile coals used commercially as blending stock in metallurgical coke production.

Jan 1, 1961

By M. R. Geer

The use of the cyclone as a dense-medium cleaning device was first described by Driessen6/ in 1945, after development of the process in the Netherlands during the German occupation of World War II. A pilot plant was built in the Netherlands soon thereafter, and the first commercial plant was built in 1948. By 1958, 18 plants were operating or under construction.7/ Thus, economic factors in Europe, where the high cost of coal places a premium on efficient cleaning, dictated rapid adoption of the cyclone. American reception of the process differed. The Bureau of Mines presented the results of its own small-scale cyclone experiments in 1946;8/ showing a sharp separation between coal and impurity; adoption by industry now is taking place. There is now much greater emphasis on the efficient cleaning of fine coal, and the first American cyclone plant has begun operating; others are planned or under construction. With the present interest in improved treatment of fine coal, the Bureau of Mines felt that additional performance data on the cyclone would be helpful to industry. Therefore, a complete, open-circuit pilot plant was built to make cleaning trials on American coals covering a wide range of washability characteristics. Five raw coals and one middling product were included in the investigation, and each was cleaned at several densities; 17 cleaning trials are reported.

Jan 1, 1961

By F. E. Armstrong

This report describes development and application by the Bureau of Mines of techniques and instruments for using radioactive inert-gas tracers to determine flow paths through petroleum reservoirs that have natural fracture systems and for which water injection has been selected as the stimulative production method. A field test was made to prove the techniques and evaluate instrumentation. The feasibility of applying the techniques and instruments to the solution of reservoir problems in other stimulative methods of production also is discussed. Oil commonly is displaced from sandstone host rocks by the action of a driving force that causes the oil to move through interstices of the rock and into production wells. In addition to the requirements of oil being trapped within the sand pores and the presence of an effective displacement mechanism, the rock itself must have adequate permeability to permit flow of oil and other fluids.

Jan 1, 1961

By Dale W. Richardson

Ductile hafnium was not obtained consistently by the conventional Kroll process. The bimetal reduction modification produced a more ductile hafnium by lowering the impurities, especially oxygen, in the sponge metal. Hafnium oxide was chlorinated in the presence of carbon to form anhydrous hafnium tetrachloride, which was reduced by sodium and magnesium in an inert atmosphere to produce sponge hafnium metal. After vacuum distillation to remove the byproducts, the sponge was arc-melted into ingot and rolled into strip. Metallic impurities were decreased by evaporating the hafnium tetrachloride from a fused salt. An excessive amount (over 1,200 parts per million (p.p.m.)) of aluminum was contained in some of the hafnium oxide, much of which remained as aluminum chloride in the hafnium tetrachloride during chlorination. Evaporation of the hafnium tetrachloride from a fused NaCI-KCI mixture during the Mg-Na reduction greatly lowered its aluminum content, as most of the aluminum and some of the other metallic impurities were retained by the fused salt.

Jan 1, 1961

By D. Bienstock

In connection with air-pollution studies, the Bureau of Mines is cooperating with the U.S. Public Health Service in investigating the use of solids for removing sulfur dioxide in concentrations of less than 0.5 percent from combustion and waste gases. Removal of sulfur dioxide at flue-gas tempera¬tures would no longer result in the cooling of scrubbed gas, which is inherent to liquid scrubbing processes used exclusively in industry today. Results are reported of extensive investigation, using metallic oxides as absorbents, adsorbents, and oxidation catalysts at 130° and 330° C. (temperatures at which flue gas may be treated in powerplant practice). The most active absorbents tested were the oxides of manganese, cobalt, copper, and alkalized alumina; 23 to 33 grams of sulfur dioxidn were removed by 100 grams of absorbent at 130° C., while scrubbing more than 90 percent of the sulfur dioxide from a simulated flue gas, and 19 to 61 grams of sulfur dioxide were removed at 330° C. A more detailed study is reported on absorption and regeneration, using manganese oxides and alkalized alumina. Adsorption of sulfur dioxide on activated carbons and molecular sieves at elevated temperatures is considerably less efficient than removal by absorption--a maximum of 7 to 8 grams of sulfur dioxide could be removed with 100 grams of adsorbent at 130° C. A potash-promoted vanadium pentoxide is effective in converting sulfur dioxide to trioxide; complete conversion in a simulated flue gas containing 0.35 percent sulfur dioxide was obtained at 365° C. Pilot-plant and cost studies are being made by the Bureau to determine the economic feasibility of removing on an industrial scale the sulfur dioxide present in gases in low concentrations.

Jan 1, 1961

By David M. Gullikson

Since publication of the paper on the composition of California oilfield waters by Jensen (6)3/ in 1934 the only other information on the subject was published recently by Chave (4). To supply needed information on the composition of California waters in areas of current drilling activity, the Federal Bureau of Mines collected formation water samples for analysis. Thirty-eight samples from oil-and gas-producing formations in 12 fields located in Ventura, Kern, Glenn, and Colusa counties were analysed by the Bureau's San Francisco Petroleum Research Laboratory. The samples were selected particularly from fields where the water composition was not well known or where interpretation of electrical logs has been difficult and the interpretation may be affected by unusual composition of the water. These samples were obtained from rocks ranging in geologic age from Cretaceous to Upper Pliocene. Fifteen constituents of these waters were determined including sodium, potassium, calcium, magnesium, strontium, barium, lithium, chloride, iodide, bromide, carbonate, bicarbonate, sulfate, borate, and residual acidity. These analyses are the first to be published on California oilfield waters in which determinations for potassium, strontium, bromide, iodide, boron) and naphthenates were made on a significant number of samples. The electrical resistivities of tae samples were determined at 75° F. and 175° F.

Jan 1, 1961

By David M. Gullikson

As part of its program of petroleum production research the Federal Bureau of Mines has long been engaged in the study and development of systems of analysis of oilfield waters (8, 12, 20, 21, 22, 27, 30).21 However, many of the early chemical procedures developed by the Bureau and widely adopted by the petroleum industry are time consuming, and some are unreliable for determining certain constituents found in California oilfield waters. Because of the need for more rapid and more accurate methods having greater sensitivity with low concentrations of some constituents, a study has been made by the Bureau's Petroleum Research Laboratory at San Francisco, in developing new techniques and modifying previously published techniques for analyzing oilfield waters by flame spectrophotometric, potentiometric, and colorimetric methods. Test solutions were synthesized for testing the suitability and accuracy of the procedures, and the effect of interfering ions. These solutions contained known quantities of characteristic constituents of oilfield waters including sodium, magnesium, potassium, calcium, lithium, strontium, barium, sulfate, chloride, bromide, iodide, carbonate, bicarbonate and borates in a wide range of concentrations. The compositions of these synthetic brines are listed in table 22. Many California oilfield waters contain salts of petroleum-derived organic acids and several synthetic oilfield waters also were prepared to which large quantities of naphthenates or salts of petroleum acids were added.

Jan 1, 1961

By William J. Campbell

This study was a part of two programs: The first, to develop and evaluate high-temperature refractories; the second, to investigate reaction-rate kinetics and phase equilibria in the sinter step of the lime-soda process for the recovery of alumina. High-temperature X-ray diffractometer techniques are to be used extensively in both programs. This paper summarizes developments in the field of high-temperature X-ray diffractometers through 1959, evaluates various furnace designs, and describes briefly the X-ray diffraction facilities of the Federal Bureau of Mines. A more detailed description of the equipment and its calibration is planned in a future paper on thermal expansion and phase inversion of rare-earth oxides.

Jan 1, 1961

By William J. Campbell

The purpose of this investigation by the Federal Bureau of Mines was to design and construct a fluorescent X-ray spectrograph for dynamic rate studies of selective oxidation in molten metals and to establish basic principles for interpretation of data obtained by this method. An X-ray spectrograph was constructed in which the sample holder is a resistance wound furnace; it was operated up to 800° C. in oxidizing atmospheres. No difficulties were experienced with the cooling or heating systems nor with the protective layer of mica around the X-ray tube window, even though the oxidizing surface of the metal is only 0.5 inch from the X-ray tube window, Means are provided for heating under controlled atmospheres for selected time? temperature cycles.

Jan 1, 1961

By K. K. Kershner

Sulfide ore concentrates containing cobalt, nickel, copper, lead, and iron were salt roasted and leached on a laboratory scale. More than 95 percent of the cobalt, nickel, and copper was recovered. Heating patterns for salt roasting different concentrates were established. More cobalt, nickel, and copper were recovered from a bulk concentrate composed of a mixture of copper concentrate and iron concentrate. This mixture corresponded roughly with the mixture of these materials in stockpiles in southeastern Missouri. A temperature range of 375° to 400° C. was best for salt roasting. Metal chlorides were leached at a pH of 1 from chloridized charges of concentrates, Although the amounts of cobalt, nickel, and copper extracted were high, the amount of iron dissolved simultaneously interfered with subsequent separation and recovery of these metals. The amount of dissolved iron was reduced substantially by steam treating chloridized charges of bulk concentrate at 300° C. In this way, the ratios of cobalt, nickel, and copper to iron in leach liquors permitted satisfactory separation and recovery of these metals. INTRODUCTION The Federal Bureau of Mines is experimenting with chloridizing reactions.4 5 6 7/ Salt roasting of sulfide ores and concentrates, or their calcines, to form metal chlorides has certain advantages. Chlorides of

Jan 1, 1961

By E. R. Palowitch

A centrifugal float-and-sink test procedure has been developed by the Bureau of Mines to reduce the time for the gravimetric separation of coals finer than l4-mesh from as long as 24 hours to less than 1 hour. Comparative tests indicated that centrifuging a minus 14-mesh Pittsburgh-bed coal for 20 minutes at 1,500 revolutions per minute produced results that compared favorably with static float-and-sink test results. Standard deviations of the mean recovery and ash content of the float obtained centrifugally ranged from 1.31 and 0.04 percent, respectively, at 1.30 specific gravity to 0.21 and 0.05 percent, respectively, at 1.60 specific gravity. As in static separations, retreatment of the products separated at low specific gravities was required.

Jan 1, 1961