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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 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 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 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 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

By F. H. Gibson

An investigation was made by the Federal Bureau of Mines of methods for determining phosphorus in coal, coal ash, and coke ash. Several of these methods are being considered for international standardization. As might be expected, methods and proposals from other countries for determining phosphorus differ considerably from those accepted an standard in the United States. Some of the methods differ fundamentally in principle from the American Society for Testing Materials (ASTM) standard used in the United States; others differ only in details of procedure. Because the Bureau considered that certain of the proposed methods might offer advantages in obtaining increased accuracy and precision or in decreasing the time required for making analyses, these methods were investigated, and the results compared with those obtained by the ASTM method. The methods investigated may be grouped into three types--volumetric, colorimetric, and gravimetric. All were about equally accurate and may be used alternatively. From a practical viewpoint, when only a limited number of analyses are made intermittently, the gravimetric procedure probably is the most suitable because no special apparatus or standard solutions are required. The volumetric methods are more rapid when more analyses are made. For mass production, the colorimetric methods, although requiring a suitable photometer or spectrophotometer, are more suitable because a large throughput should be feasible.

Jan 1, 1961

By J. B. Gayle

During the past several decades, there has been a steady increase in the number and size of experimental ovens used for carbonization research. Although many were originally intended principally for studies of coal expansion, current practice usually includes determinations of the properties of the experimental cokes. With respect to size and shatter characteristics, the cokes from the larger experimental ovens closely approximate those from duplicate charges carbonized in commercial ovens; however, they are consistently lighter and frequently less resistant to degradation by abrasive forces. To minimize these differences, some operators dry the experimental charges before carbonization. The resulting higher dry coal charge densities do, in fact, yield cokes with gravities closely approximating those produced commercially from the same coal or blend but without drying. The drying of the experimental charges may be criticized on the grounds that it represents a departure from commercial practice and may result in oxidation of the samples; for these reasons, the practice has not been universally adopted.

Jan 1, 1961

By S. L. May

Investigations by the Federal Bureau of Mines indicate that hafnium and zirconium compounds of acceptable purity can be extracted from Nigerian zircon concentrates. Chlorination and caustic soda fusion techniques were used to extract 85 to 95 percent of the valuable metals from the concentrate. The extracted hafnium and zirconium compounds were purified by recrystallization of the oxychlorides or by formation of complex salts during chlorination. The zirconium-hafnium product of the recrystallization method contained 15 parts per million of uranium, and the product of the salt-complex method contained less than 10 parts per million of uranium. The hafnium was separated from zirconium by solvent extraction methods. A zirconium product containing 0.3 percent hafnium and a hafnium product containing 4 percent zirconium were obtained. At the request of the Atomic Energy Commission (AEC), work was started to develop techniques for processing Nigerian zircon concentrates in commercial installations presently engaged in producing zirconium and hafnium metals from ores. The Nigerian zircon has a high hafnium content, but the presence of uranium and thorium is a problem not normally encountered in processing zircon concentrates.

Jan 1, 1961

By F. W. Wood

A program of research was conducted by the Bureau of Mines to investigate anomalies in electrical-discharge behavior during consumable-electrode arc melting of titanium and to study the effects of these irregularities on arc-furnace explosions. A major effort was devoted to an experimental survey of arc behavior and a qualitative definition of discharge phenomena.3/ An important conclusion was that the "glow" of industrial arc-melting terminology is not a glow discharge but a skittering arc in a displaced position. The conditions that permit displaced skittering were tentatively defined. The displaced skittering arcs tended to damage melting crucibles in two ways, and details of possible mechanisms leading to crucible rupture and explosive reactions have been proposed accordingly. However, no acceptable means of preventing crucible damage was discovered.

Jan 1, 1961

By J. S. Browning

Laboratory and pilot-plant tests of spodumene-beryl pegmatites of the Kings Mountain, N. C., area resulted in development of a new and improved method by the Bureau of Mines for separating and recovering spodumene, mica, and beryl. The process was successfully applied to other domestic pegmatites and a spodumene flotation-plant tailing containing about 0.5 percent beryl. The method comprised soap flotation of the spodumene, using combinations of sodium fluoride and lignin sulfonate as conditioning agents to recover 80 to 85 percent of the contained lithia in concentrates assaying over 6 percent Li20. About 80 percent or more of the beryl was retarded in the spodumene tailing. The beryl subsequently was activated, floated, and cleaned in a secondary circuit to yield beryl concentrates containing 6 to 7 percent BeO. The tests also demonstrated that a good recovery of high-grade mica could be produced.

Jan 1, 1961

By R. T. Johansen

The wettability of petroleum reservoir materials by water and crude oil has been recognized as an important factor in determining waterflood behavior. The problem of simulating and studying reservoir conditions and characteristics, to produce laboratory results congruous with field experience, has been examined by many methods. (1, 2, 3, 4).4/ The most generally accepted approach to this problem is determining wettability of the porous medium by imbibition methods; or, after solvent extraction, predetermining the wettability of the samples by coating the surface of the medium to render it preferentially oil-or water-wet (3, 5). The emphasis of wettability studies has been placed on the characteristics of the reservoir materials with little consideration being given to the fluids themselves. Therefore, the wetting tendencies of crude oils have been investigated by a recently developed method (6). Imbibition and the more general phenomena of capillary pressure are the most direct ways to measure wettability. The simplest type of capillary pressure observations involves the use of an interfacial-tension capillarimeter, which does not produce as separate values either interfacial tension or contact angle. Actually, these quantities do not have independent significance in reservoir engineering, and the property of wettability they are intended to evaluate is given, immediately by capillarimetric measurements.

Jan 1, 1961

By Murray Jacobson

Data obtained by the Federal Bureau of Mines on the dust explosion hazard in air are presented for 220 samples of agricultural products. Information is given on ignition temperature of dust clouds and layers, minimum explosive concentration, minimum electrical energy for ignition, explosion pressure and rates of pressure rise, amount of inert dust required to prevent flame propagation, and, in a few instances, the permissible oxygen concentration in an atmosphere to prevent ignition by spark and by heated surface. The effects of particle size and source of sample on explosibility are shown. The relative ignition sensitivity, severity of explosion, and overall explosibility of the materials are characterized by empirical indexes. This report contains Ma obtained by the Bureau in laboratory studies on the explosion hazards of agricultural dusts. Recognition of the dangers will encourage adoption of adequate measures to prevent ignition and explosion during preparation, processing, and utilization of the materials. Agricultural products constitute one of the largest groups of materials used in America. More than 260 million tons of various grains, much of which now exists in dust form, was grown in 1958.6/ Over 600,000 tons of the annual production of 200

Jan 1, 1961

By D. A. Wilson

Several promising systems for selectively oxidizing the iron in an iron-tin alloy commonly called "hardhead" were investigated in a research project conducted to devise a method for recovering tin from this troublesome alloy. A satisfactory oxidation method was developed and tested successfully on melts of 2,000 grams. Molten hardhead (near 1,080° C.) was blown with air to oxidize iron and leave tin in the reduced state. Recovery of available tin was 96 to 98 percent. Tin products contained 2 to 0.1 percent iron which was reduced to 0.06 percent by filtration at 250° C. Iron oxide formed during oxidation was absorbed by a fluid flux cover composed of 43 percent silica, 17 percent burned limestone, and 40 percent fused borax. Less successful but nevertheless promising results were obtained with mixtures of steam and hydrogen which were sufficiently selective at temperatures between 600° and 950° C. but did not result in complete oxidation of iron. Carbon dioxide-carbon monoxide mixtures also oxidized iron selectively but incompletely. Both stern and carbon dioxide systems produced sufficiently encouraging results to additional research on these systems.

Jan 1, 1961