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By Marvin L. Whisman

This report describes the preparation of tritium-labeled organic compounds to be used by the Federal Bureau of Mines in studying the role of certain gasoline constituents in gum-forming mechanisms. The gasoline constituents that have been investigated boil within a range of approximately 90 to 230° C. and can be classified as paraffins. naphthenes, olefins, diolefins, monocyclic aromatics, polycyclic aromatics, and organic sulfur, nitrogen,: and oxygen compounds. The technique of Wilzbach has been applied to more than 50 samples. Purification techniques have been developed that accomplish rapid and effective purification as well as removal of labile tritium in a one-step operation. Data are presented to show the rate of exchange between tritium and hydrogen that can be expected for a variety of compounds common to a full-boiling-range gasoline. These values should be useful to other investigators using tracer programs involving tritium labeled compounds.

Jan 1, 1961

By D. N. Collins, J. R. Stevens

New expressions in the technical assessment of mineral concentration processes have been defined as Concentration Efficiency: Concentration Index: where h is the percentage of head grade; c, percentage of concentrate grade; maximum percentage of concentrate grade obtainable at 100 pct recovery; and R, percentage of recovery. In developing these expressions, the basic requirements for the technical assessment of concentration operations have been defined and the various expressions suggested by others for asses-sing the results of such operations reviewed and criticized. The derived expression for E, depends on a simple combination of recovery (R) and a new term selectivity (s), where S is (c-h)/(c,,, -h), by definition. Limitations of the new expressions are discussed and examples given of applications to concentration operations. It is also shown that the formulae for E, and I, can be applied to scatter diagrams, multi-component systems, size-assay analyses, and classification data. Many methods of quantifying concentrating operations have been proposed. These include direct presentation of weights and assays together with the derived data for other items such as ratio of concentration, recovery, rejection losses, and enrichment ratio. These terms are now accepted mineral dressing nomenclature, and in the assessment of the results of concentration processes, concentrate grade and recovery are together the most widely accepted measures of concentration efficiency. For practical purposes when the concentrate grade is equal to or greater than a predetermined acceptable value, test or operation results may be assessed by the recovery figures alone. Similarly when recovery is within specification, the operation can be assessed by concentrate grade. The ultimate assessment and selection of a concentration operation is—admittedly with a few ex-ceptions—a matter of economics. There is however an intermediate stage in laboratory and pilot plant testing when evaluations must be made without the assistance of an economic yardstick. Numerous techniques are employed to facilitate such evaluations among which may be mentioned graphical plots of grade vs recovery, cumulative weight vs cumulative recovery, scatter diagrams, etc. The desirability of combining metallurgical results and product weights and assays into a single value has been recognized and discussed by many workers1-" with the resultant suggestion and use of such terms as Metallurgical Efficiency ,' Summation Index,' Selectivity Index,'- and Absolute Efficiency B None of these expressions completely satisfies all the requirements of a selectivity or efficiency formula and it is proposed in this report to define the terms, relating to the technical efficiency of a concentrating operation, concentration index and concentration efficiency. Examples are given of their application and a comparison is made of their use in relation to other formulae. All product grades in this paper will be referred to in terms of mineral percentages and a list of symbols is given in Table I. CONSIDERATION OF EXISTING FORMULAE A number of the existing efficiency and index terms used in quantifying concentrating operations are considered below. Metallurgical Efficiency:

Jan 1, 1961

By Lowell Stroud

Since 1929, the Helium Activity of the Bureau of Mines has operated a helium-extraction plant at Amarillo, Tex. The natural gas that supplies this plant is obtained from the Cliffside geologic structure 12 miles to the northwest and over the years, has become known simply as "Cliffside gas," There is need for published data on the low-temperature phase equilibria of helium-bearing natural gases. To date, little information has been published on the equilibrium phase compositions, solution of helium in condensed natural gas, condensation characteristics, or equilibrium vaporization coefficients for methane, nitrogen, and helium in helium-containing systems. A windowed phase equilibrium apparatus (8)6 was used to obtain 105 equilibrium samples, representing 35 experimental conditions of condensed Cliffside gas at pressures of 100, 200, 300, 400, and 500 p.s.i.a. and temperatures from 0° to -270° F. Data on equilibrium vapor-liquid composition for Cliffside gas are presented in both tabular and graphic form and are discussed in detail to show their relationship to certain criteria that must be met to effect an efficient separation of helium from natural gas by means of low-temperature processes. Facts about condensation characteristics and solution of helium in the liquid phases are included, The important relationship of these two factors in decreasing the percentage of total helium lost by solution in the liquid phase is discussed.

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 Donald J. Frendzel

The post-World War II expansion of the Soviet petroleum industry has established the U.S.S.R. as a major oil-producing nation and has led to Russian reentry into the international petroleum trade. The rapid growth of Soviet petroleum production will allow the U.S.S.R. to displace Venezuela as the world's second largest oil-producer in 1960 and to narrow further the gap between Soviet and U.S. crude-oil production. U.S.S.R. crude oil output was only a tenth of U.S. production in 1946, but it will be more than a third at the end of 1960 and more than half in 1965. The Soviet Seven-Year Plan (1959-65) for oil provides for substantial increases in petroleum production, refining, storage, and distribution facilities. Crude oil production and primary distillation capacity are to double, considerable storage capacity is planned, and pipelines for crude oil and petroleum products are to increase threefold. According to the Soviets, the initial phases of this plan (1959 and 1960) have been completed successfully. However, this progress has been achieved with difficulty.

Jan 1, 1961

By R. A. Swalin, L. A. Neimark

The research work presented in this paper had initially a two-fold goal. First, further data concerning the low-temperature recovery of cold work was desired. Recovery phenomena have been extensively studied in face-centered-cubic metals but at the time of initiation of this research, no investigation concerning the low-temperature recovery in body-centered-cubic metals had been made. During the course of the investigation a paper by Martin on the recovery of point defects in molybdenum appeared.&apos; Comparison of our results on tungsten with Martin&apos;s results on molybdenum will be made. Secondly, knowledge concerning the influence of a particular type of impurity addition on the recovery kinetics was desired. It has been known for a long time that extremely small amounts of certain impurity additions exert a profound influence on the recrystallization behavior and the resulting microstructure of tungsten. Small amounts of potassium silicate and aluminum chloride added prior to the reduction of tungsten oxide to the metal have been found by Smithells to raise the recrystallization temperature markedly,2 and yield an ultimate microstructure in which grains several millimeters long are produced in fine wires of say 10 mil diam. If the impurities are added singly, ordinary secondary recrystallization results with none of the spectacular properties of the wire to which special additions were made. Swalin and Geisler3 and Rieck4 have studied the recrystallization behavior of such doped wire in some detail. The former workers found that small amounts of these impurities raised the recrystallization temperature over 400°C and electron microscopic examination revealed no obvious inclusions in the microstructures. In fact. chemical analysis showed that there was <0.001 pct K, <0.002 pct Al, trace of Si, and <0.0003 pct 0 in the wire studied. The possibility that the role of the special impurities is to keep the structure open by void formation and that submicroscopic porosity acts as the inhibiting agent has been discussed.2&apos;3 Meijering and Rieck5 have suggested that the impurities are strung out as second-phase particles in a direction parallel to the drawing direction. It was thought that a kinetic study of recovery could perhaps elucidate the role of the impurities to some extent. When a metal is deformed by cold work three basic types of defects are thought to be introduced into the crystal lattice, namely, interstitials, vacancies, and dislocations. Van Bueren6 has proposed that recovery of cold-worked metal is a four-stage process, each step being the result of the annealing of a primary defect or a combination of defects and having a unique activation energy. The steps in order of increasing activation energy are attributed to a) the diffusion of interstitials recombining with vacancies, b) diffusion of vacancy pairs, c) the diffusion of single vacancies, and d) climb of dislocations. In metals with relatively low- or medium-range melting points the temperatures for recovery are low enough so that the first three steps may occur during room-temperature deformation. For tungsten, because of the high melting point and subsequently high recovery temperature, it was calculated, using Nowick&apos;s approach7 that this recovery would occur in the temperature range 200" to 600°C. It is also known that recovery of X-ray line broadening, presumably due to dislocation climb, occurs at about 600°C.8 EXPERIMENTAL METHOD Two types of cold-rolled 10-mil-diam tungsten wire were used in the investigation; a) pure tungsten, (called undoped) and b) G. E. No. 218 wire (called

Jan 1, 1961

By E. Peters

Roasting processes are divided into several elementary mechanisms, any of which could be significant or pre-dominant in a particular roast. The elementary processes considered in-elude beat transfer, gas-solid inter-actions with accompanying mass transfer between the bed and furnace atmosphere, vapor phase transport processes in solid-solid interactions, and solid phase diffusion processes. Examples are chosen of processes in which one of these mechanisms pre-dominates and some recently obtained data is presented to support the existence and significance of these mechanisms. Proposals are also made for future research in these areas, and for utilizing the information in the improvement of roaster capacities’ OASTING of ores as a preparative treatment for smelting or leaching has been practiced for so long that its origin has been lost in antiquity, but little has been under-stood of its basic nature until fair-ly recent times. The nominal chemistry of roasting processes is now understood; that is, the initial chemical com-pounds present in the ores or con-

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 H. U. Ross

ROASTING is usually thought of as a process in which finely crushed or ground ore is heated with air in a suitable furnace in which the ore is rabbled or agitated in such a way as to insure complete reaction between the oxygen of the air and the oxidisable constituents of the ore. Roasting in this sense is used only to a very limited extent in the iron and steel industry. This is because, in most iron ore deposits mined today, the ore is of a type that does not require roasting. Where this process is used, it is usually because of some special circumstance, such as a peculiar economic condition, that warrants it. If roasting is looked upon in the broader sense as a gas-solid chemical reaction carried out at an elevated temperature in which both gaseous and solid products are formed, then the process is used in the iron and steel industry to a greater extent

Jan 1, 1961

By K. E. Tame

A resume of the history and state of the art of physical beneficiation of uranium ores is presented along with a detailed description of research on concentration of uranium ores by attrition grinding. The information on flotation, gravity concentration, electronic sorting, and selective grinding was gathered to complement the study of attrition grinding methods. Both dry and wet grinding procedures were investigated as potential methods of upgrading a variety of ore types, ranging in grade from 0.02 to 0.42 percent U308. A Mardun4 disintegrator that employs high-speed rotating paddles in a cylindrical shell lined with interrupter bars was used in most of the dry grinding studies. Attrition scrubbing devices, which impart a violent mixing or attritioning action to ore pulps, and cylindrical mills, employing rods or punchings as grinding media, were used in the wet grinding tests.

Jan 1, 1961

By W. W. Fowkes

The Federal Bureau of Mines examined a low-temperature tar obtained from a small-scale commercial unit for carbonizing North Dakota lignite for products that might be important to the economic processing of the tar. Tie tar may be divided into three distinct parts: (1) Tar acids, 45 volume-percent; (2) tar bases, 1 volume percent; and (3) neutral compounds, 54 volume-percent. It has a boiling range of approximately 150° to 380° C. (the decomposition temperature) and yields 18 weight-percent as hard pitch. The tar distillate up to 365° C. may be separated as: (1) Tar acids, 48 volume-percent; (2) tar bases, 1 volume-percent; and (3) hydrocarbons, 51 volume-percent. The tar-acid distillate, boiling to approximately 265° C., was characterized in some detail; the neutral fractions and the tar bases were less thoroughly examined. In general, as might be expected of a primary low-temperature tar, the lower boiling fractions are less in quantity compared with the usual high-temperature tar. The homologous series of each major class appears to be rather complete, although some components are present in very small amounts. The tar is quite unstable thermally, and might be more conveniently processed by extraction methods rather than by distillation procedures. The neutral fraction of the tar is highly aromatic, and might be considered as base stock for the production of liquid fuels.

Jan 1, 1961

By W. A. Roliff

The renewed interest of the past few years in the Appalachian and Michigan oil provinces has not, as yet, created any marked increase in activity in Southwestern Ontario. During 1960 development drilling in-creased somewhat over 1959, but exploratory drilling decreased slightly. More attention was devoted to the deeper horizons, but lake drilling de-creased considerably. Oil production reached a new peak and gas production increased slightly. During 1960 an interesting oil and gas discovery was made in the Cambrian and gas discoveries six miles off-shore in the eastern part of Lake Erie were made in the Clinton-Cataract zone of the Silurian. This paper reviews activities during 1960, summarizes the discoveries made to-date and the pertinent exploration data relating to the prospects of the region and discusses some of the economic aspects of exploration and development. D URING the last few years there has •been a marked renewal of interest in the old petroleum

Jan 1, 1961

By John P. Powell

A comprehensive study of the effects of hydraulically fracturing water-flood wells in Oklahoma has been made by the Federal Bureau of Mines. This report presents results of that study and an analysis of some of the factors governing the results of fracture treatment on waterflood properties. Originally, hydraulic fracturing was used to stimulate oil production from old wells producing by primary methods, and its application to water-flooding was regarded with skepticism by most producers. However, since 1953 the number of fracture treatments of both oil and input wells in waterfloods has increased steadily. Hydraulic-fracture treatments in waterfloods have generally been successful in stimulating production from oil wells and increasing the rate of injection into input wells. Hydraulic fracturing has enabled several producers to turn probable failures into economically successful projects.

Jan 1, 1961

By H. P. Pew

THE Pembina oil field is in west-central Alberta, about 88 miles west-southwest of Edmonton. The field, about 35 miles long by T HE Pembina oil field is in west-central Alberta, about 88 miles west-southwest of Edmonton. The field, about 35 miles long by 85 miles wide, is the largest in Canada in areal extent, in the amount of oil in place and in the current producing rate. The discovery well was completed in the middle of 1953. The field has grown until its present area is 369,820 acres. There are 74 working interest owners in the field. Early in the producing history of the Pembina field a committee of operators was formed on a permanent basis. The Pembina Operators' Committee has established a permanent staff, which compiles and distributes pertinent field information on a regular basis to all participants. The Alberta Oil and Gas Conservation Board has dealt with field-wide problems primarily through this committee. Expansion of the field was rapid as shown by the number of wells completed -from 135

Jan 1, 1961

By H. C. Fuller

Depletion of iron ore in the Nation&apos;s large deposits has directed attention to other sources. One of these is the titaniferous iron ore of the Iron Mountain, Wyo., area. Tests were made to determine the feasibility of smelting this ore, which contains about 20 percent titanium dioxide (Ti02), in an electric-arc furnace to produce pig iron. Initial tests, which were made in a 30-pound-capacity induction furnace, demonstrated that the iron could be easily reduced to metal and that limestone was a suitable and effective flux. Larger scale tests then were made in a 50-pound-capacity electric-arc furnace to obtain the more detailed information necessary for the planned continuous operation of a still larger arc furnace. The principal facts determined by preliminary batch-smelting studies were that (1) 9 pounds of limestone flux was required for each 100 pounds of ore smelted, (2) expensive coke was not required because coal proved to be a satisfactory reductant (near stoichiometric carbon was optimum), and (3) overreduction, which produced a viscous slag, must be avoided.

Jan 1, 1961

By H. Kenworthy

The purpose of the study described in this publication is to develop methods for recovering simple master alloys or single metal components from discarded and scrapped S-816 alloy, The Bureau of Mines started this investigation late in 1955 after the need became apparent for a method of reclaiming high-temperature alloys from an ever-increasing accumulation of rejected and wornout jet engine turbine buckets. Laboratory studies showed the following: (1) Pyrometallurgical separations are not selective enough, (2) several methods can be used for effective chemical dissolution of the major constituents of the alloy, (3) a master alloy or complex salts of cobalt and nickel can be separated, (4) chromium, contaminated by several other metals, may be segregated, and (5) more time and effort need to be expended in separating the minor constituents and improving the purity of the major metals removed. Difficult and incomplete chemical separations were attributed to the complexity of alloy composition, as were the long tedious chemical analyses o&apos; products. For determination of several of the metallic components, standard methods of separation and routine analytical procedures had to be considerably modified to achieve satisfactory results. The overall technical problems involved in separating S-816 components do not appear to be insurmountable; however, refinement of several of the methods used in this investigation is desirable.

Jan 1, 1961

By J. P. Capp

The Federal Bureau of Mines and the Alabama Power Company conducted an experiment in underground gasification of coal at Gorgas, Ala. involving the use of hydraulic fracturing to increase the air acceptance of a coalbed for the introduction of combustion air and removal of product gases. Air acceptance is defined as the flow rate of air which can be injected into the coalbed at 65 p.s.i.g. This was the second time the hydraulic-fracturing technique was used at Gorgas. Sand suspended in a heavy oil served as the fracturing fluid in the first experiment; in the second the sand was two to six times larger and was suspended in a water-starch gel. In addition to providing further tests of the underground-gasification process, the purpose of the second experiment was to determine the effects of the larger sand and greater volumes of a water-base fluid on (1) the extent of the fractured area, (2) the air acceptance of the coal, and (3) the rate at which a gasification path could be carbonized (linked) through the coal, and to compare these results with those of the first experiment. The coal was fractured by injecting 11,000 lb. of sand and 33,580 gal. of water and water-gel at 200 to 600 g.p.m. and 900 to 1,000 p.s.i. The fluid fractured the coal and the sand served as a propping agent to hold the cracks and crevices open. Pressures during the fracturing operation at test boreholes indicated that the fracturing fluid extended only about 150 ft. from borehole H, the point of application of the fracture. Injection of air revealed that the air acceptance of the coalbed within this e t was materially increased. On the other hand, increased air acceptance also was noted at boreholes up to 280 ft. from borehole H and at the electrolinking area 300 to 400 ft. away, indicating that the fracture effects extended considerably farther than was evident from observation. Similar effects were noted at approximately the same distances after the first hydraulic fracture.

Jan 1, 1961

By K. C. Li

The scope of this subject is a broad one. The demand for a metal with high refractory properties, great strength at elevated temperatures and high nuclear cross section, has put tungsten in the foreground as: the most promising metal to fill some of these requirements. Recently developed techniques have made it possible to roll large tungsten sheet and-the availability of fabricated tungsten is already upon us. More and more, the demand is for purer and still purer metals. Tungsten is no exception. As technology improves, we are learning more about the effect of foreign elements in minor amounts upon the chemical and physical properties of metals. As equipment and technology improve, specifications become more rigid, and reasonably so. Pure metals have revealed properties hitherto unknown in metals produced by former technology.

Jan 1, 1961

By J. D. Ramsdell

The object of this investigation by the Federal Bureau of Mines was to evaluate the workability, recrystallization characteristics, and mechanical and physical properties of high-purity electrorefined vanadium. The low level of interstitially soluble elements in electrorefined vanadium results in a soft ductile metal which responds readily to cold working by rolling, swaging, and press-forging. Hardness, strength, and resistivity increased with an increase in impurity content, but thermal expansion was independent of impurity content. The work-hardening of vanadium occurs rapidly. Most of the hardness increase occurs in the first 15 pct. of reduction in area. When vanadium is annealed, its hardness increases to a maximum when the annealing temperature is between 200° to 400° C. A sharp decrease in hardness develops as the annealing temperature is increased. An anomaly in the hardness versus annealing temperature curve is present in the 600° to 800° C. range, while all evidence of cold-work is removed at annealing temperatures above 900° C.

Jan 1, 1961

By R. I. Cavanagh, A J. Last

THE USE of higher grade charges in blast furnaces in the form of sintered or pelletized concentrates has been increasing rapidly. The question of beneficiation of iron ores for this purpose is therefore receiving much attention as more deposits are developed. Many iron ores may respond well to magnetic roasting procedures followed by magnetic concentration, however, in most cases other more standard ore dressing methods are competitive and cheaper. For magnetic roasting as applied to iron ore beneficiation, the present question is "Can it be economically justified in situations where it appears to produce good results?" The following collection of information on the general status and operations of magnetic roasting methods may be helpful in considering this question. Magnetic Roasting Magnetic roasting involves the transformation of non-magnetic iron oxides, hydrated oxides and carbonates by means of heat and suitable

Jan 1, 1961