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By A. N. Fried

With the growing importance of fluid injection in recent years, the petroleum industry has been investigating and field- testing a variety of new methods designed to modify the physical properties of reservoir oil to improve the efficiency of gas and water injection. These procedures include condensing-gas drive, LPG (liquefied petroleum gas) injection, alcohol-slug process, high-pressure-gas displacement, detergent-solution flooding, and in situ combustion (30, 37).3 A new and different method to increase the effectiveness of gas and water injection has been tested by the Bureau of Mines, Consideration of both fundamental and practical factors that operate to limit the oil recovery attain- able by conventional oil-displacement mechanisms led to the concept of a displacement mechanism called the foam-drive method. This report describes the experimental study that tested this concept in the laboratory.

Jan 1, 1961

By J. G. Walters

In 1928, the Coal Carbonization Section of the Federal Bureau of Mines, in cooperation with the American Gas Association, began a survey of the carbonizing properties of American coals. A standard test method for evaluating the carbonizing properties of coals that met the following conditions was developed: To yield products similar to those obtained in commercial operations. To produce yields sufficient to permit analyses and tests of quality. To be laboratory size. To be convenient to operate. To permit reproducible control of test conditions and results. This test method has become known as the Bureau of Mines-American Gas Association (BM-AGA) test (53),3/ and more coals of greater variety have been tested in this apparatus than in any other of similar scale.

Jan 1, 1961

By D. A. Pirttinen

The promotion of improved coal quality for thermal generation can benefit our national economy. The construction of electric generating facilities in Canada is expanding at a rapid rate to satisfy the demands of a rising population and new uses for electrical energy. With remaining economic water power resources in the process of development, generation from thermal sources continues to grow. The increase in thermal capability has been somewhat arrested by a de-pressed economy, widening of inter-provincial and state transmission networks and decisions to exploit certain water resources before high capital investment is further in-creased by rising construction costs. The introduction of extra high volt-age transmission lines will further delay thermal generation planning, but in due course, when the effects of restrictive factors have been dissipated, steam-electric generation from fossil fuels will rise to considerable proportions. In time, nuclear sources will contribute a growing share to thermal power, but, it is doubtful if nuclear participation will ever displace conventional fuels for steam rising, unless it can be adapted to operate efficiently for variable outputs in peaking service. It appears certain that fossil fueled

Jan 1, 1961

By Rudolph G. Wuerker

Charles T. Holland (Head, Dept. of Mining Engineeri*, Virginia Polytechnical Inst., Blacksburg, Va.) Mr. Wuerker has presented a very interesting discussion of the use of triaxial test methods for investigating the strength properties of rocks. Such methods, no doubt, eventually will develop considerable information of interest to those concerned with the design of mine layouts, particularly in the field of pillar design. From his discussion of my recent article, "Cause and Occurrence of Coal Mine Bumps" (Holland Mining Engineering 1958, p. 933-1002), it is evident that in one place at least I did not make my meaning clear to him and perhaps others. To clear the matter up I think it best to quote from the article, somewhat more fully than did Mr. Wuerker, as follows: "4) In actual operations — because rocksare not perfectly elastic, homogeneous, nor isotropic and because local yield does occur — the maximum stress as demonstrated by Phillips (Ref. 22, pp. 64, 65) and indicated by much experience in mining, does not occur at the walls of the opening but at a short distance inside the pillar. Furthermore, the maximum stress does not reach as great a value as theoretical considerations and laboratory experimental methods indicate.* Actual distance inside the pillar, measured from the wall, at which the maximum stress exists, has not been determined. Observations in many mines, however, indicate that this distance could have a mini-value of one to six or eight times the bed thickness and that it is probably affected by width and height of the opening, depth of cover, and relative values of the elasticity and plasticity of materials comprising the roof, floor, and coal seam. The actual value of the stress produced probably lies between the theoretical maximum and the average stress concentration that would be produced if the weight of the strata above the unsupported opening were evenly distributed over the pillars for a distance equal to the opening width." The footnote reference in the above quotation referred to the following: "*For example, the Pocahontas No. 4 coal bed in southern West Virginia is mined under cover up to 1800 ft thick. Development openings are driven 18 to 20 ft wide, and the bed is about 6 ft thick. According to the work of Panek, the tangential wall stress at mid-bed height under these conditions would reach values between 4000 and 5000 psi. Actual tests of 3-in. cubes of this coal show its compressive strength would be much less than this, perhaps as low as 400 psi. Yet the pillars usually show no evidence of failure in these headings. In this same bed at a depth of 800 ft, the author has seen an opening 225 ft between supports lying between two old groves approximately 1100 ft apart. According to the theoretical considerations, the stress in the pillar walls would have been about 18,000 psi, yet the pillar showed little or no evidence of weight. In view of these observations, it is clear that the wall stress does not attain the maximum values indicated by theory." (Underlining added to original wording.) By referring to Fig. 2A of my paper it will be noted that theoretically the maximum pillar stress would occur at the pillar wall, i.e., at the passageway surface of the pillar. Obviously this cannot be correct in the cases of stress ranging from 4000 to 18000 psi since the coal at the surface of the pillar is under no constraint and cannot have a strength much greater than 400 or 500 psi. Hence, my conclusion that the maximum stress does not occur at the wall but back in the pillar some distance from the wall. Since these stresses are pushed back in the pillar from the wall, it is also obvious that the loads transferred to the pillar from the opening will be spread over a greater area and hence Pillar stresses will not rise to the values postulated by theory and photoelastic experiment. Further since to visual inspection the coal along the pillar wall did not appear to be failed the conclusion was reached that the stress shift was caused by local elastic or plastic yield and by difference in the elastic modulus of the rocks composing the mine floor, mine roof, and coal bed. Later on under the heading "Strength of Mine Pillars" (pages 1000-1002) the effects of constraint is briefly described. Also a formula taking into account constraint is developed relating pillar strength to the uniaxial strength of coal and the L/T ratio of the pillar. Since my paper was written, reports of experiments conducted in South Africa (Denkhaus, et. al., 1959), in Sweden (Hast 19581, and in Canada (McInnes, et.al., 1959) reveal that the conclusion expressed relative to the existence of a low stress area existing around the edges of pillars and solid faces as described above is generally correct. But it seems possible that where the wall stress developed is less than the unconfined strength of the rock composing the pillar and where the roof, floor, and pillar

Jan 1, 1961

By J. R. Hornaday, A. E. Morris, N. A. Parlee, D. C. Carmichael

Rates of absorption and effusion of hydrogen in solid iron were measurede by a Sieverts type of apparatus. With clean a iron these rates are diffusion controlled down to 420°C and are represented by the equation D = 6.70 x e-'100' crn2 sec-I Certain surface impurities can affect these rates at all temper-atuves. Thin oxide films lower, the apparent diffusivity of annealed iron markedly. Cold-worked iron (75 pct) annealed at 430°C has practically the same solubility and diffusivity as anealed iron. THE mechanism of absorption and evolution of hydrogen in solid iron alloys is not fully understood despite the large number of investigations on the subject. While there appear to be many instances of simple solid-state diffusion control of rate, there are many cases where investigators have either concluded that surface reactions are rate controlling or that some "nondiffusible" hydrogen resides in discontinuities. The purposes of this research were 1) to develop a sound method for studying this absorption and evolution behavior, 2) to examine it in pure annealed iron, and 3) to determine the effects of important variables, such as cold work, surface condition, and composition. This paper relates the progress toward these objectives. Much of the present knowledge of the movement of hydrogen through iron alloys comes from permeability studies which involve the measurement of the rate of passage (under steady state conditions) through membranes of the order of 1 mm in thickness. This method is open to question on various grounds. If surface reactions are involved, two different surfaces operating under two different conditions must be considered. The presence of defects in the membrane even of microscopic dimensions may lead to erroneous results. A few people have studied evolution of hydrogen into vacuum, under carefully controlled (unsteady state) conditions, and some of the best diffusivity data come from these sources. Most of these methods measure rates of evolution only and thus do not make a rigorous test for reversibility of behavior. It appeared that an "unsteady state" method that would permit the measurement of both rates of evolution and absorption under controlled temperature, pressure, and other conditions would offer several advantages. Accordingly the modified Sieverts apparatus described below was designed and built. APPARATUS This apparatus is shown in Fig. 1. The sample bulb is detailed in Fig. 2. Hydrogen of 99.5 pct purity and argon of 99.99 pct purity were used. The hydrogen was deoxidized and dried by means of a Deoxo unit followed by a "Dri-erite" tower. The argon was only dried. The gas burette was graduated in tenths of a cubic centimeter, and, with the aid of a travelling magnifier, readings could be estimated to the nearest 0.01 cc. The level of mercury in the burette was adjusted by means of a leveling bulb operated by a fine screw adjustment. An electrical system, consisting of two slightly separated platinum electrodes inserted in one leg of the manometer and a small light bulb was used to obtain rapid accurate adjustment of the pressure. The capillary tubing of the Vycor sample bulb was 3 mm bore as was all tubing back to the gas burette. The samples were discs made from vacuum-melted Ferrovac-E iron of greater than

Jan 1, 1961

By G. W. Govier

The origin and limitations of the conventional and empirical equation for the interpretation of the results of back pressure tests on gas wells are discussed. Difficulties in data interpretation arise from many causes, including Jack of flow stabilization, uncertainties in connection with the friction calculation, and the effect of turbulence near the sand face in the reservoir. A procedure is developed to ac-count for the turbulence effect. This is based upon the theoretical equation for laminar steady state flow and current knowledge of turbulent steady state flow. The procedure involves the expression of the equation for combined laminar-turbulent steady state flow in terms of a turbulence contribution factor. This factor. is shown to be dependent mainly upon the flow rate per unit of pay thickness and the reservoir permeability. The method of interpretation permits the use of judgment based upon the theory and present day under-standing of laminar-turbulent flow and is considered an improved method

Jan 1, 1961

By Urie R. W

Fluidized bed roasting of copper concentrates from Mt. Morgan, Mt. Lyell, Mt. Isa, and Peko was performed in a 3 ft 6 in diameter, slurry fed, pilot plant roaster operated under autogenous conditions to produce calcines with desirable leaching properties. A 12 in. diameter, externally heated roaster, provided with a dry feed system, was also used.An account is given of important factors which influence roaster behaviour and performance, and the effects of operating variables on calcine composition and leaching properties are described. Due to copper ferrite formation, a maximum of approximately 50 per cent of the copper in the calcines may be in the form of CuO before the copper leach efficiency falls significantly below lOO' per cent. Recovery of gold by cyanidation of leach residues was consistently high and independent of roasting conditions.INTRODUCTIONIn traditional practice copper is produced by pyrometallurgical techniques when the ,copper minerals in the ore or concentrate are predominantly sulphides, and by hydrometallurgy when the minerals are oxidized. Copper smelting is most suited to large scale operations, and for many years small to medium size mines with sulphide orebodies have been interested ill; alternative processes.Since hydrometallurgical plants (ie. leaching and electrowinning plants) are essentially unitized, they may be scaled down in output without much loss in efficiency or increase in processing cost, and many proposals have been made for the application of this type of process following roasting of the sulphides to render the copper soluble. However, until the advent of fluidized roasting, it was not possible to control the roasting operations sufficiently precisely to produce calcines consistently of the required leaching characteristics.

Jan 1, 1961

By J. E. Reeves, J H. Morgan

Certain non-metallic minerals are used widely as fillers in the manufacture of many Canadian products. The first part of this paper deals in a general way with deposits of such minerals and their mining, with the concentration and preparation of the minerals for market, with specifications of the consumers, and with methods of control of the products to meet the specifications. The second part of the paper de-scribes talc as a specific example of mineral filler. Its production and uses in Canada and the possibility of producing higher grades of talc are discussed. Some suggestions are made for meeting the needs for mineral fillers as Canada's industry expands. RELATIVELY few people are sufficiently aware of the vast and important role that is being played in our everyday lives by mineral fillers. Many kinds of paints, papers and plastics, to mention three major classes of industrial products, are literally loaded

Jan 1, 1961

By J. W. Town

As part of the Federal Bureau of Mines titanium resources examination program, samples from seven deposits in the Pacific Northwest were tested for amenability to various beneficiation techniques. The samples obtained by the Bureau's Office of Mineral Resources at Spokane, Washington represent a large potential source of titanium. This report summarizes the results of tests at the Bureau's Metallurgy Research Center, Albany, Oregon. Recoveries from tabling placer samples were about 50 percent at grades of 30 percent titanium dioxide. Flotation was the most effective method for concentrating the fine ilmenite in clay samples; recoveries of approximately 50 30 percent titanium dioxide. Flotation was the most effective method for concentrating the fine ilmenite in clay samples; recoveries of approximately 50

Jan 1, 1961

By A. R. Orban, R. B. Engdahl, J. D. Hummell

The initial phase of a research program on smoke abatement from Bessemer converters is described. In work sponsored by the American Iron and Steel Institute, a 300-lb experimental Bessemer converter was assembled to simulate blowing conditions in a commercial vessel. Measurements of smoke and dust were also made in the field on a 30-ton commercial vessel. During normal blows the dust loading from the laboratory converter averaged 0.51 lb per 1000 lb of exhaust gas. This was similar to the exhaust-gas loading of a commercial vessel. The addition of hydrogen to the blast gas of the laboratory converter caused a decided decrease in smoke density. Smoke was also reduced markedly when methane or ammonia was added instead of hydrogen. The research is continuing on a bench-scale investigation of the mechanism of smoke formation in the converter process. DURING the past 2 years, on behalf of the American Iron and Steel Institute, Battelle has been conducting a research program on the control of emissions from pneumatic steelmaking processes. The objective of the research program is to discover a practical method for reducing to an unobjectionable level the emission of smoke and dust from Bessemer converters. PRELIMINARY INVESTIGATION Although conceivably some new collecting technique may be devised which would be economically practicable for cleaning Bessemer gases, no such system based on presently known principles seems feasible because of the extremely large volume of high-temperature gases involved. Hence, the research is being directed toward prevention of smoke formation at the source. A thorough review was first made of former work to determine the present status of the cleaning of converter gases. No published work was found on work done in the United States on collecting smoke or on preventing its formation in the bottom-blown, acid-Bessemer converter. In Europe, however, a number of investigations have been made on the basic-Bessemer converter. Kosmider, Neuhaus, and Kratzenstein1 conducted tests on a 20-ton converter to obtain characteristic data for dust removal and the utilization of waste heat. They concluded that because of the submicron size of the dust, special equipment would be necessary to clean the exhaust gases. Dehne2 conducted a large number of smoke-abatement experiments at Duisburg-Huckingen in a 36-ton Thomas converter discharging into a stack. A number of wet-scrubbing and dry collectors were tried unsuccessfully. A waste-heat boiler and electrostatic collector with necessary gas precleaners was felt to be the best solution for this particular plant. Meldau and Laufhutte3 determined that the particle size was all below 1 µ in the waste gas of a bottom-blown converter. Sel'kin and zadalya4 describe the use of oxygen-water mixtures injected into a molten bath in refining open-hearth steel. They claim that with use of oxygen-water mixtures the amount of dust formed was reduced between 33.3 and 20 pct of its previous level, and emission of brown smoke almost ceased. Pepperhoff and passov5 attempted unsuccessfully to find some correlation between the optical absorption of the smoke, the flame emission, and the composition of the metal in a Thomas converter in order to determine automatically the metallurgical state in the melt. In a recent U. S. Patent (NO. 2,831,762)' issued to two Austrian inventors, Kemmetmuller and Rinesch, the inventors claim a process for treating the exhaust gases from a converter. By their method the inventors claim that the exhaust gases from the converter are cooled immediately after leaving the converter to a degree that oxidation of the metal vapors and metal particles to form Fe2O3 is inhibited in the presence of surplus oxygen. Gledhill, Carnall, and sargent7 report on cleaning the gases from oxygen lancing of pig iron in the ladle. They claim the Pease-Anthony Venturi scrubber removed 99.5 + pct of the smoke, thereby reducing the concentration to 0.1 to 0.2 grain per cu ft, which resulted in a colorless stack gas after the evaporation of water. Fischer and wahlster8 developed a small basic converter and compared the metallurgical behavior of the blow with that of a large converter. Later work by Kosmider, Neuhaus, and Hardt9 on the use of steam for reduction of smoke from an oxygen-enriched converter confirmed that the cooling effect of steam is detrimental to production. From review of all of the published information on the subject, it was concluded that a practical solution to the smoke-elimination problem had not been found. Accordingly, it was deemed desirable to investigate the feasibility of preventing the initial formation of smoke in the converter.

Jan 1, 1961

By C. S. Finney, John Mitchell

The decline of the beehive coking industry was inevitable, but it had filled the needs and economy of its day. A beehive plant required neither large capital investment to construct nor an elaborate and expensive organization to run. The ovens were built near mines from which large quantities of easily-won coking coal of excellent quality could be taken, and handling and preparation costs were thus at a minimum. The beehive process undoubtedly produced fine metallurgical coke, and low yields were considered to be the price that had to be paid for a superior product. Few could have foreseen that the time would come when lack of satisfactory coking coal would force most of the beehive plants in the Connellsville district, for example, to stay idle; and if there were those like Belden who cried out against the enormous waste which was leading to exhaustion of the country's best coking coals, there were many more to whom conservation was almost the negation of what has since become popularly known as the spirit of free enterprise. As for the recovery of such by-products as tar, light oil, and ammonia compounds, throughout much of the beehive era there was little economic incentive to move away from a tried and trusted carbonization method simply to produce materials for which no great market existed anyway. With the twentieth century came changes that were to bring an end to the predominance of beehive coking. Large new steel-producing corporations were formed whose operations were integrated to include not only the making and marketing of iron or steel but also the mining of coal and ore from their own properties, the quarrying of their own limestone and dolomite, and the production of coke at or near their blast furnaces. As the steel industry expanded so did the geographic center of production move westward. By 1893 it had moved from east-central to western Pennsylvania, and by 1923 was located to the north and center of Ohio. This western movement led, of course, to the utilization of the poorer quality coking coals of Illinois, Indiana and Ohio. These coals could not be carbonized to produce an acceptable metallurgical coke in the beehive oven, but could be so treated in the by-product oven. By World War I the technological and economic limitations of the beehive oven as a coke producer were being widely recognized. After the war the number of beehive ovens in existence dropped steadily to a low of 10,816 in 1938, in which year the industry produced only some 800,000 tons of coke out of a total US production of 32.5 million tons. The demands of the second World War led to the rehabilitation of many ovens which had not been used for years, and in 1941, for the first time since 1929, beehive ovens produced more than 10 pet of the country's total coke output. Production fell off again after 1945, but the war in Korea made it necessary once more to utilize all available carbonizing capacity so that by 1951 there were 20,458 ovens with an annual coke capacity of 13.9 million tons in existence. Since that time the iron and steel industry has expanded and modernized its by-product coking facilities, and by the end of 1958 only 64 pet of the 8682 beehive ovens still left were capable of being operated. Because beehive ovens are cheap and easy to build and can be closed down and started up with no great damage to brickwork or refractory, it is likely that they will always have a place, albeit a minor one, in the coking industry. The future role of the beehive oven would seem to be precisely that predicted forty years ago by R. S. McBride of the US Geological Survey. Writing with considerable prescience, McBride declared: "A by-product coke-oven plant requires an elaborate organization and a large investment per unit of coke produced per day. Operators of such plants cannot afford to close them down and start them up with every minor change in market conditions. It is not altogether a question whether beehive coke or by-product coke can be produced at a lower price at any particular time. Often by-product coke will be produced and sold at less than cost simply in order to maintain an organization and give some measure of financial return upon the large investment, which would otherwise

Jan 1, 1961

By Stephan I. Zajac, Roger A. Blais, John B. Stubbins

THE iron deposits of central Labrador occur within a relatively small area, herein called the Knob Lake Iron Range, in which a northwest-trending series of low hills and ridges defines the height-of-land at the boundary between provinces of Quebec and Newfound-land. Approximately two-thirds of the deposits are in Quebec and the remainder in Labrador, with several deposits straddling the inter-provincial boundary. These deposits are being exploited in open-pit mines by the Iron Ore Company of Canada centered at Schefferville, Quebec. Since 1954 this company has produced more than 56 million tons of iron ore to become Canada's leading iron ore producer. With indicated reserves of more than 375 million tons of direct-shipping ore and large tonnages of iron formation amenable to beneficiation, this mining district is assured of a long life. This paper describes the Knob Lake iron ores and their geological settings and stresses the features that lead to a better understanding of their origin. The

Jan 1, 1961

By J. A. Boyle

In the Frick District of U, So Steel Corporation, we have had more than 37 years of experience in the use of multiple-fan ventilation systems, in our coal mines. In our Colonial field, with a long belt installation, we have mined 85 million tons of coal with the use of the multiple fan system of ventilation. In our Palmer field, with the use of the same arrangement, we have mined 90 million tons of coal--a total of 175 million tons without one accident attributable to improper mine ventilation. The same system, fundamentally, has been installed in our expanding Robena operations and at its present stage of development we are using eight fans to ventilate this area. To date we have mined 55 million tons of coal with very encouraging results and again without any accidents attributable to ventilation.

Jan 1, 1961

By W. M. Dressel

The objective of the research reported in this publication of the Federal Bureau of Mines was to devise a mineral dressing procedure that would concentrate zinc silicate minerals from certain deposits in southwestern Missouri. The best flotation results were obtained by batch laboratory flotation using sulfidizing agents and ethoxylated cocoamine. The flotation concentrate contained 70 percent of the zinc at a grade of 47.8 percent. Gravity concentration tests showed that 55 percent of the zinc could be recovered at a grade of 48.3 percent.

Jan 1, 1961

By Robert K. Koch

The reactions of alumina and alumina monohydrate with wet hydrogen fluoride gas were studied by the Federal Bureau of Mines to determine the feasibility of producing commercial-grade aluminum fluoride from offgases generated by pyrohydrolysis of siliceous fluorspars. The test results showed than an aluminum fluoride reactor operating at maximum efficiency could retain 96 percent of the fluorine contained in off-gases generated by pyrohydrolysis of siliceous fluorspar. The requirements are a reactor temperature of 200° C. and a reactor entrance gas containing 5 mole-percent hydrogen fluoride. Partial pressure equilibrium constants were determined for the reaction of alumina monohydrate and wet hydrogen fluoride gas from 200° to 350° C. and for the reaction of alumina and wet hydrogen fluoride gas from 350° to 700° C. Both reactions are reversible, and they proceed in directions that are dependent upon the temperature and the relative HF:H2O concentration. Logarithms of the equilibrium constants were used to plot the reaction isobars; these can be used to calculate the theoretical maximum efficiency of a reactor processing wet hydrogen fluoride gas between 200° and 700° C. The theoretical maximum efficiency decreases with increasing temperature.

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 W. R. Huff

This report describes the development and operation by the Bureau of Mines of a pilot plant designed for using high-volatile A bituminous coal-in-water suspensions as a source of preheated coal and superheated steam in the pressure gasification of coal with oxygen. Figure 1 on page 2 is a block diagram of the integrated gasification process, in which a total of 70 tons of coal was fed from slurry and gasified. The present work included (1) development of equipment and methods both for mixing pulverized coal and water to produce slurry and for pumping and metering the slurry at gasification pressure; (2) development of equipment for heating the flowing slurry and, because slurry that can be pumped produces more steam than is necessary as a gasification reactant, developing equipment for removing and metering the excess steam; and (3) demonstration of the process under actual gasifier operating conditions, at a coal rate of about 800 pounds per hour and gasification pressures in the range 100 to 300 pounds per square inch gage. By using the forced-convection principle, a flow of slurry made from a caking, high-volatile A bituminous coal can be continuously heated to 600° F. in a coil-type heater. The flow rate and concentration of the slurry and the temperature gradient along the length of the heating coil must be closely controlled. In a radiant-type heater, involuntary reductions in flow rate, even momentary, can lead to coking and plugging of the heater coil.

Jan 1, 1961

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 C. P. Mabie

This report summarizes studies by the Bureau of Mines in developing a simple method for estimating the phosphorus pentoxide (P205) content of finely ground sedimentary phosphate ores and beneficiated products. The method used involved leaching, filtration, and precipitation. The Bureau found that measurement of the volume of ammonium phosphomolybdate precipitate obtained from samples containing 16.8 to 37.7 percent P205 and the use of an appropriate calibration curve permitted estimates of percentage of P205 content accurate within ± 1.1 to ± 2.6 percent, respectively, at the 95-percent confidence limits. Incidental to mineral dressing and petrographic investigations of western phosphate ores in 1959, the Bureau of Mines undertook development of a simple process-control method for rapid on-the-spot evaluation of phosphate-mineral recovery. Because of the fine-grained and obscure character of western phosphate ores, chemical, rather than microscopic or petrographic, techniques were investigated. The described method involves acid decomposition of the ore or product, filtration, addition of ammonium molybdate reagent to the filtrate, and centrifuging and measuring the volume of yellow ammonium phosphomolybdate precipitate produced.

Jan 1, 1961

By V. M. Benson

A simplified, routine method for determining lithium in lithium-bearing rock is presented. The sample is decomposed by repeated treatments with nitric, hydrofluoric, and perchloric acids. Since this procedure does not appreciably dissolve beryl, interference by beryllium (the principal interfering cation) is minimized for most samples. The salts are brought into solution with water and enough citric acid-ammonium citrate buffer is added to make the final volumetric dilution 0.20 M with respect to citrate. The addition of citrate greatly reduces anion interference in the hydrogen-oxygen flame, slightly increases the intensity of the lithium 671 millimicron emission line, and reduces the effect of most of the interfering cations to the extent that analytical separations are not necessary. The accuracy of results of single determinations of lithium in a pegmatite containing spodumene, lithium-bearing mica, and beryl are approximately equal to that obtained by other flame methods, INTRODUCTION This investigation was undertaken in Bureau of Mines laboratories to develop a reliable, rapid, routine analytical method for determining lithium in lithium-bearing minerals. The requirements of the procedure were that the method should be applicable to the analysis of a variety of lithium-bearing ores and test products, and the results would be reasonably accurate for materials containing 0.05 to 8 percent Li20.

Jan 1, 1961