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By J. P. McCullough

In 1943, the Federal Bureau of Mines began a program of thermodynamic investigations of petroleum constituents and related compounds. These systematic, long-range studies, which were conducted in the thermodynamics laboratory of the Bartlesville Petroleum Research Center and are still continuing, have resulted in a substantial quantity of data valuable to the petroleum industry and science in general. As separate phases of these studies were completed, the findings were promptly reported in the scientific press. During the past 16 years, 89 journal articles, giving the results obtained for individual compounds and small groups of related compounds, were published, mainly in the Journal of the American Chemical Society and the Journal of Physical Chemistry. In addition, members of the Bureau staff have contributed six chapters to specialized reference books. This circular, prepared in response to many requests, lists these 95 published papers, giving an abstract of the contents of each, as well as titles, authors, and literature citations. The journal articles are listed in the order of their preparation, which closely approximates the chronological order of their publication; hence, the item number to the left of each citation corresponds to the assigned contribution number. For the convenience of the reader, the abstract section is followed by a condensed bibliography, arranged alphabetically by senior author and keyed to the abstracts by appropriate contribution numbers in parentheses after the entry.

Jan 1, 1961

By Leo F. Reinartz

Part II of a four-part series on the history of steelmaking in the US, points out the inadequate safety and living conditions that existed in steel mills at the turn of the Century. Also defined are furnace and process developments. OPERATIONS in steel plants today are highly mechanized. Men work in light, clean, orderly melting shops, making it difficult for old timers to convince young men that primitive, hazardous conditions existed in steel plants at the turn of the century. Working conditions then were very poor as compared to present day standards. In small plants especially, sanitary, locker, and washroom facilities, first-aid practices and stations were un- known Accidents were frequent and severe. Workers had a fatalistic attitude toward getting hurt. He who had an accident was looked upon as a hero. A dirty bandanna often served as a bandage. Infections were frequent. Electric cranes were in their infancy and broke down often Cables had not as yet replaced chains. Pig iron and scrap iron were loaded by hand in the stockyard, and stockyard locomotives were un- known; mules served as the usual motive power. It was not unusual to see recorded a delay of ½ hr in charging a furnace because of a balky mule. Furnace operations A few plants had primitive charging machines, but most furnaces were charged by placing scrap or pig iron on the paddle of a long peel, which rested on a bar across the furnace door opening. Laborers at the handle end of the peel, using the bar as a fulcrum, would heave the material into the furnace by a down and sideward motion of the peel handle. In time they became expert in placing these materials in the furnace, but it was hard, hot work, and a long time was required for charging. Cold charges of 25 tons required more than 12 hr for melting and re- fining the steel. Ports, doors, and frames were not water cooled. The charging and working area in front of the furnace was covered with steel plates. They were hot and often warped by the intense heat of the un- insulated checker chambers directly below. In the summer, working conditions on the charging floor were almost unbearable. Silica refractories were of poor quality. Because of this, and the inadequate training of furnace men in fuel control and furnace operations, roofs, front and back walls, and ends burned out rapidly. Dolomite machines were unknown; consequently, furnace banks and hearths were fettled with dolomite by the use of hand shovels. The round system required six or more men. Each man took a shovelful of dolomite and, in his turn, deposited it on the back wall and bank by a dexterous forward swing and twist of the shovel. The upward swing of the shovel partially protected his face from the searing heat of the furnace coming out through the wide-open door. Considerable skill and stamina were required to do this job properly. Reverse valves, usually of the cast-iron butterfly type, were located below the charging floor. They were operated by long levers on the charging floor level men they became warped, because of heat and abuse, great strength and skill were required to reverse them. Furnace operations were difficult. The quality and quantity of producer gas coming from irregularly stoked, hand-operated gas producers was uncertain and unreliable. Furnace Linings and ports were quickly burned out. Poor bottom and side-wall refractories, indifferent and inexperienced crews, as well as irregular re-

Jan 1, 1961

Factors of importance in the ntilization of coal fines are mentioned, and the results of flotation tests on coal fines from three important coal seams in New South Wales are presented.INTRODUCTIONEconomic utilization of fine coal is an important problem in the Australian coal industry, particularly as the proportion of fines mined is increasing with progressive mechanization.While the use of uncleaned coal fines may be economic, it may be preferable to beneficiate them, but the most economic process must be selected.For beneficiating coal finer than about 28 mesh, froth flotation can be applied, but mining engineers should avoid practices that may be detrimental to flotation. Such practices include the indiscriminate use of water, particularly that containing a wetting' agent, for dust suppression. In addition, clay stemming in wet conditions may produce slimes which could adsorb on coal surfaces, while the use of oils and greases as well as the application of stone dust and chlorides in roadway consolidation may influence adversely fine coal beneficiation.This paper deals with the application of flotation to samples of fine coal from the Bulli, Greta, and Victoria Tunnel seams. In addition a discussion is given of the mineralogical constitution, size analysis, and degree of liberation of ash constituents of the various samples.COAL SAMPLESRepresentative samples of coal from the Bulli, Greta, and Victoria Tunnel seams were obtained for testing.

Jan 1, 1961

By W. L. Schmidt

The effect of a water-repellent film in sandstone cores on the effective permeability-saturation relationship was investigated as part of a cooperative research program between the Bureau of Mines and the American Gas Association. The repellent film was formed by the reaction of methyltrichlorosilane3 with the connate water in the core. Other researchers have reported on the use of silicone chemicals to alter the flow characteristics of porous media (1-3, 5-7, 9, 10).4 The previous studies, however, dealt almost entirely with oil-water or oil-gas systems and not with water-gas systems. The primary purpose of this study was to determine the feasibility of using silane to retard the influx of water into natural-gas storage wells and to determine the necessary requirements for achieving this result. The success or failure of silane treatment as a remedial measure depends on its effect on gas-production rate and attendant water production.

Jan 1, 1961

By J. T. Dunham

Zirconium has possible use in industry where severe corrosion conditions are encountered because it resists attack from a variety of corrosive environments. However, very little experimental testing has been done to evaluate the corrosion behavior of zirconium when simultaneously subjected to high tensile stresses and exposed to corrosive environments. This investigation was initiated for an evaluation test, but was limited to environments consisting of ferric chloride solutions which were known to attack zirconium and were shown to promote stress-corrosion cracking in preliminary tests. Tests for cracking susceptibility were conducted by the Bureau of Mines to show the effect of stress, solution concentration, air aeration of solution, and the method of mechanical processing. Tensile stress was applied to the specimens by a constant-load method which proved more reliable than a constant-strain method.

Jan 1, 1961

By M. van Swaay, C. E. Birchenall

Palladium has a large capacity for the dissolution or occlusion of hydrogen; the gas also diffuses very rapidly through the metal. Palladium thimbles are widely used in the laboratory for purification of hydrogen by diffusion. The use of palladium filters could be extended to several large-scale applications if greater stability of the permeation process could be attained. In this paper a number of aspects contributing toward this goal are discussed, and new data on solubility and diffusivity are given. Palladium sheets of 0.005, 0.010, or 0.020 in. thickness were prepared by three procedures: casting and rolling, sintering palladium powder, and sintering palladium powder to which 0.1 pct thorium oxide had been added. Half-inch diam circular specimens were cut and clamped in a stainless steel holder provided with knife edges to seal the palladium sheet with soft copper gaskets. The seals were tested for leaks at l0-5 mm Hg. No difficulties from this source were encountered even after many temperature cycles in the system. The holder was silver-soldered to Kovar-glass seals and attached to the system through glass ball joints. Each joint was sealed with Apiezon wax and was adjacent to a cold trap. In several experiments the holders were fused directly into the system, eliminating the ball joints, to show that the wax did not affect the filter. Three filter holders were supported in holes in a stainless steel cylinder, which also acted as a temperature equalizing block inside the resistance wound furnace. The measuring thermocouple was inserted in one of the holders. A potentiometric controller with control thermocouple on the furnace heater winding maintained ± 0.2oC. Electrolytic hydrogen was purified and stored as shown in the flow diagram, Fig. 1. It could be admitted to either or both sides of the palladium specimens. Only a mechanical pump was used, for even high pumping speeds would not bring the pressure on the off-gas side of the filter below 10 to 50p Hg owing to the rapid hydrogen flow through the filters. A series of steady-state permeability studies allowed identification of several conditions of permeability loss. A constant fore pressure was maintained while the low-pressure face was pumped. After enough time had elapsed for a steady flow to be established the pump was cut off, and the rate of pressure increase in a thermostated bulb was measured to determine the flow rate. The time delay method of Daynes1,9 was adopted since it offered the possibility of determining solubilities and diffusivities. For each measurement both sides of the filter were evacuated for 15 min, which gave about 10-4mm Hg residual pressure. Hydrogen was admitted to one side or the other of the filter at a fixed pressure. The pressure on the off-gas side was observed as a function of time. A

Jan 1, 1961

By Joseph A. Sutton

This study was undertaken by the Bureau of Mines to determine whether the sulfur-oxidizing bacterium Thiobacillus thiooxidans could use sulfur compounds to produce sulfuric acid in sufficient quantities to leach valuable metals from low-grade ores. The results of extended tests indicated that the bacterium is capable of extracting appreciable amounts of copper and cobalt from ore and mineral samples when sulfur is available in a state that can be readily assimilated by the organisms. Under the conditions of these tests, this organism was not able to assimilate and oxidize the sulfur as it occurred in the ores and minerals. Ores containing copper minerals in the silicate, carbonate, and oxide forms, in the presence of elemental sulfur, were more susceptible to bacterial action than ores containing copper minerals in the sulfide form. Thiobacillus thiooxidans remained active on elemental sulfur in the presence of some of the ores which were tested, but could not tolerate others. Therefore, strains of the bacterium were progressively adjusted to increasing concentrations (0.5 to 10 grams) of the individual ores until they could remain active on 10-gram portions of all ores being tested.

Jan 1, 1961

By Perry D. Teitelbaum

In two earlier studies the Federal Bureau of Mines undertook to explore comprehensively the dimensions of the Nation's energy balance. The first of these studies, published in 1950 as Bureau of Mines Information Circular 7582, by Harold J, Barnett, was primarily concerned with projections of future domestic energy requirements and supplies, because these related to projected growth in major fuel-consuming sectors of the economy, changing rates of energy-use efficiency, and interfuel substitution patterns. But, to provide the essential background for these projections, it was first necessary to assemble and examine in some detail the quantitative information on the size and shape of the current United States fuel economy. Among other things, Barnett's path-breaking study indicated the need to consider energy as an entity, particularly for public and private policy makers, industry and commodity analysts, economists, and others concerned with long range questions of domestic and international energy supply and demand. The study also spotlighted a gap in the fabric of current economic intelligence; no comprehensive collation and reconcilation in any single report of available published statistical information covering the origin -a disposition of all energy materials existed. In response to this latter need, the Bureau of Mines prepared the second of the two studies referred t3 above. This was published in 1951 as Report of Investigations 4805, by W, H, Lyon and D, S. Colby, and it consisted of statistical information on the production and use of each of the various fuels and electric energy in the United States for 1929, 1939, and 1947; all were presented in tabular form and on a uniform basis. The three years selected were chosen largely on the basis of data availability.

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 B. A. Strathdee

An arsenical ore containing both pyrite and arsenopyrite was heated to a temperature at which decomposition and distillation took place. The condensate consisted of metallic arsenic and arsenic disulphide, although the analysis of the ore showed that volatile arsenic and sulphur were present in proportion to produce a condensate of arsenic trisulphide and sulphur. Distillation tests on the mineral arsenopyrite also produced a condensate of metallic arsenic and arsenic disulphide. This arsenic sulphide gave a distinct x-ray diffraction pattern which was not listed in the A.S.T.M. data file. This same sulphide can be produced by heating a mixture of arsenic and sulphur in vacuo. Its chemical analysis corresponds to As2S2. The dissociation pressures of arsenopyrite and the vapour pressures of arsenic disulphide and arsenic metal were measured, using a quartz "spoon" gauge. The dissociation pressures of arsenopyrite were compared with the published data for the dissociation pressures of pyrite to account

Jan 1, 1961

By Harry R. Nicholls

A simple economical method has been developed for determining the in situ longitudinal and shear velocities in rock from which its elastic constants can be calculated. By detonating small charges of high explosives in shallow drill holes near a free surface, both longitudinal and shear waves were generated simultaneously. Accelerometers and velocity gages mounted to the rock surface were used to record the arrival time for both waves over travel path lengths from 50 to 450 feet, Measurements were made in two rock types. From the arrival time measurements, the longitudinal and shear wave velocities were calculated. From these velocities and the density of the rock, the elastic constants were calculated. The dynamic elastic constants of drill core samples of the two rock types were determined in the laboratory by the resonant-frequency method, The lab- oratory and in situ elastic constants are compared and significant differences noted. In general, there is less spread in the in situ data than in the laboratory data, and Poisson's ratio does not fall outside the theoretical limits for the in situ data as is often the case for laboratory-determined elastic constants.

Jan 1, 1961

By R. K. Linn

The New Idria Mining and Chemical Co. owns and operates the New Idria mine in southern San Benito County, Calif. During 1957-59, the New Idria mine was the largest producer of mercury in the United States and its alltime production of over a half-million flasks was exceeded only by one mine. It is one of the oldest and most consistent producers in California. With the exception of 1921-22, the mine has an annual production of mercury dating back to 1854. This paper by the Federal Bureau of Mines describes the exploration, development, mining, and furnacing of mercury ore at the New Idria mine. Figure 1 is a view of the furnace plant of the New Idria mine. The purpose of this report is to promote the development and conservation of our mineral resources by dissemination of technological information on mining and processing procedures, and related practices at operating mines.

Jan 1, 1961

By Paul L. Campbell

Investigations by the Federal Bureau of Mines of methods of upgrading tar obtained by low-temperature carbonization of lignite showed that ß,ß?-oxydipropionitrile, ß,ß?-iminodipropionitrile, and ß,ß'-thiodipropionitrile were effective solvents for extracting aromatics (aromatic hydrocarbons plus polar compounds) from coal-tar neutral distillate fractions. Batch extraction showed that these solvents extracted approximately the same percentage of aromatics from various neutral oil fractions boiling between approximately 170° and 350° C. In continuous countercurrent extractions using oxydipropionitrile and iminodipropionitrile, approximately 30 to 35 vol.-pct, and 65 to 70 vol.-pct, of the aromatics in 170° to 350° C. neutral distillate oil were extracted at room temperature when solvent-to-oil ratios were 2:1 and 12:1, respectively. As the concentration of aromatics in the neutral distillate oil fraction decreased, the capacities and, to some extent, the selectivities of these solvents for the remaining aromatics decreased. Aromatics were isolated from the extracts and the solvents recovered by washing the extract fractions with a low-boiling paraffinic hydrocarbon such as heptane, using hydrocarbon-to-extract ratios of at least 2:1. The heptane wash removed most of the aromatics but only part of the polar compounds (compounds containing oxygen, sulfur, and nitrogen) from the extracts. The recovered oxydipropionitrile and iminodipropionitrile, containing polar compounds, were effective in extracting aromatics from neutral distillate oils. The contaminated solvents showed essentially the same capacities and selectivities as the pure solvents.

Jan 1, 1961

By K. H. J. Clarke

SINCE the beginning of this century the non-ferrous mineral industry has contributed $17,809,-000,000 to the economic growth of Canada. To contemplate the vast amount of investment capital required and the resultant beneficial distribution of these billions of dollars for labour, transportation, supplies, taxes and dividends, challenges the imagination. It is the purpose of this paper, (a) to trace the development of the industry since its formative period to the present; (b) to discuss the current situation and problems; and ( c) to attempt to peer into the hazy future. Although there are 21 metals currently being produced in Canada which are classified as non-ferrous, or as alloying metals, copper, lead, zinc, nickel-the metals which will be discussed in this paper-constitute almost 60 per cent of their total value. ;The story

Jan 1, 1961

By W. L. Dare

This publication is one of a series prepared by the Federal Bureau of Mines on methods and costs of producing uranium ore on the Colorado Plateau. The information it contains was gathered in 1955-58 and applies to eight small operations. (See fig. 1.) Mining costs have increased since the data were I collected, but the information should be helpful in estimating future costs I at similar deposits. The Bureau of Mines had early experience in the production of carnotite-type ores on the Colorado Plateau.3 4/ Under a cooperative agreement with the National Radium Institute in 1914-16, the Bureau mined and concentrated carnotite ore for recovery of radium, uranium, and vanadium. The ore was taken from claims in or near Long Park Montrose County, Colo., about 3 mi. south of La Salle Mining Co.'s La Salle mine, which is one of the mines described in this report. The Bureau leased the claims from Crucible Steel Mining & Milling Co., a subsidiary of Crucible Steel Co. of America, and from 1914 to 1916 produced 990 tons of high-grade ore, containing 2.6 pct. U308, and about 2,000 tons of mill-grade ore, containing 0.85 pct. U308. The high-grade ore was shipped directly to a radium-recovery plant built in Denver in 1914 under the cooperative agreement. There, commercial methods of extracting uranium, vanadium, and radium from carnotite ores were developed by Bureau personnel. The lower grade ore was concentrated at a small mill in Long Park before being shipped to Denver. The final recovery was 69,000 lb. of U308 and 8.8 g. of radium. The direct mining cost of producing the high-grade ore, including the labor to hand sort and sack it, was $35.96 per ton. Freighting the ore 58 miles to Placerville, Colo., the nearest rail point on the Rio Grande Southern Railway, cost $25.28 per ton, which included $4.55 per ton for ore bags and twine. Four-or six-horse teams pulled two wagons in tandem and made the

Jan 1, 1961

By C. G. Cheriton

The Bathurst mining district is located near the town of Bathurst on the north shore of the province of New Brunswick in eastern Canada. This region is the northeasterly extension of the Appalachian mountain system. The area is heavily forested and covered with a fairly uniform layer of glacial gravels and boulder clay. The relief is low, increasing to a few hundred feet in the north west and several hundred feet in the extreme southwest. Thus, rock outcrops are scarce and occur mostly along streams and ridges. These factors made conventional prospecting difficult and resulted in the district becoming an excellent place for the application of regional geological studies, air photo techniques, airborne and gound geophysical methods and soil sampling. Late in 1952, The Brunswick Mining and Smelting Company discovered a very large base metal sulphide body presently known as their No. 6 orebody. Early in 1953, another and even larger sulphide body was discovered and is known as the No. 12 ore body. Mining exploration was very active thoughout 1953 and in 1954, The American Metal Company discovered the orebodies which have been developed into The Heath Steele 'Mines. The location of these deposits is shown on figure one. In the latter part of 1954, The Anaconda Company became interested in the district and decided to make a geological study of this new and promising base rrietal area. The following paper presents the story of the application of modern geological and geophysical techniques, leading to the discovery of a large sul-nhidp liodv. The Bathurst district is generally underlain by the Tetagouche group of Middle Ordovician rocks.

Jan 1, 1961

[NORTH AMERICA UNITED STATES ALABAMA Birmingham CORD, Richard H DISMUKES, Edward B Citronelle PERRIN, Huey P Fairfield PAGEL, Herbert Ervin Huntsville ENG, Harvard KELLEY, Dean W WAGGONER, J B Mobile HORNER, William L PETROUTSON, Peter C Montgomery GAMBLE, Halbert R Redstone RAWLINGS, William E Tuscaloosa MASON, William L University CUDWORTH, James R JONES, Walter B]

Jan 1, 1961

By A. S. Prokopovitsh

A spectrophotometric method for the determination of small amounts of copper in tungsten metal powder using the principle of solvent extraction has been developed by the Federal Bureau of Mines. The metallic sample is dissolved in hydrogen peroxide, tartaric acid added, the pH adjusted, and the excess peroxide destroyed by boiling. Copper is reduced to the cuprous state, and the reagent neocuproine (2,9-dimethy1-1,10-phenanthroline) is added to form a colored complex with the copper. This colored complex is then extracted into chloroform and the absorbance of the separated chloroform layer measured on a spectrophotometer. Copper contents as low as 1 p.p.m. (parts per million) can be determined. The method is limited to finely divided tungsten powder. The interest of the Bureau of Mines in developing more sensitive methods for the determination of trace impurities in high-purity tungsten prompted an investigation of the possibility of using solvent extraction-colorimetric methods. The organic reagents now commercially available make possible many extremely sensitive colorimetric methods for the determination of metallic ions. Extraction of the colored complex into a small volume of organic phase can be used to further increase sensitivity (4) .4/ This general approach has the added advantage that no special equipment beyond that normally found in an analytical laboratory is required.

Jan 1, 1961

By F. D. Everett

The Federal Bureau of Mines reviewed the status of tungsten deposits of Utah in 1959. Industrial requirements of tungsten during emergencies have exceeded the domestic supply, and a knowledge of the sources of this strategic element may be helpful in the future. Tungsten occurs as the mineral scheelite in deposits that have been developed or explored on approximately 60 properties in 10 of the Great Basin ranges of Utah, none of which were being worked in 1957-59. Ores from most of the productive areas are similar in that they are contained in tactite deposits on or near the contact of calcareous and acidic intrusive rocks. The tactite ores consist predominantly of the silicate minerals garnet, epidote, and diopside and the carbonate rocks limestone or dolomite. Scheelite, where present, is disseminated irregularly in the tactite. Tungsten ores from Utah mainly have been produced from small deposits worked in World Wars I and II and the Korean campaign. The ores were either hand sorted to a grade ranging from 0.5 to 1.0 percent tungsten trioxide (W03) or were beneficiated in small mills to higher grade concentrates. The largest reserve appears to be in the area of the Notch Peak intrusive in the House Range, Millard County. A large part of the reserve in the House Range is mineralized tactite containing 0.2 to 0.3 percent W03. Research on flotation by the Bureau of Mines has indicated a method of concentrating scheelite in tactite ores that average 0.25 percent W03, with at least 85 percent recovery. The concentrate assays more than 5 percent W03 and can be processed into artificial scheelite ready for industrial use.

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