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By Foster Fraas

The Bureau of Mines investigated a method for calculating values of adsorption energy; the goal was to devise an equation consistent with experimental data accumulated in the investigation of adsorption as related to ore separation processes. Numerical identification of the constants of a previously formulated equation provided an equation by which values of adsorption energy could be calculated. Values thus calculated checked with those obtained by calorimetric measurement.

Jan 1, 1965

By S. R. Goodman, Hsun Hu

A study has hem made of the formation of annealing textures in an 18-8 austenitic stainless steel (Type 304L) from various deformation textures obtained by rolling at different temperatures. When the deformation texture is a mixture of the ferritic type and the brass type owing to the pres -ence of both martensitic ferrite and retained aus-tenite in the specimen, recrystallization takes place by the growth of the existing austenite phase. In a previous report,' it was shown that the rolling texture of austenitic stainless steel (Type 304L) changed gradually from the brass type to the copper type with increasing temperature of deformation above 200°C. These changes are similar to those in high-purity silver2,3 and electrolytic copper;4 a brass-type texture is favored at low rolling temperatures, whereas a copper-type texture is favored During the course of rolling -texture transition from the brass type to the copper type, the subsequent recrystallization textures change accordingly. The orientation relationship between the annealing textures and the various rolling textures, being consistent with previous observations on various fcc metals, can be described as [Ill] rotations of approximately 25 to 40 deg. Carhide precipitation may influence the annealing textures. at high rolling temperatures. Furthermore, the annealing textures in high-purity silver5 and electrolytic copper4 were found to depend entirely on the prior deformation texture. From a copper-type rolling texture a strong cube texture will form upon recrystallization, whereas from a brass-type rolling texture the annealing texture will be quite different from the cube orientation. In an earlier comm~nication,6 the formation of a strong cube texture in 18-8 austenite stainless steels (Types 304 and 304L) was reported briefly by the authors. The present paper constitutes the results of a complete study of the annealing textures obtained from a

Jan 1, 1965

By R. D. Pehlke, P. D. Goodell, R. W. Dunlap

The rate of dissolution of steel bars in molten pig iron has been measured experimentally in the temperature range 2300° to 2650° F. The rate of solution is shown to be a .function of bath composition, temperature, and stirring. A kinetic model based on carbon diffusion in the liquid phase has been derived to fit the experimental results. THE rate of scrap melting has long been an important variable in steelmaking operations. With the advent of the oxygen steelmaking process and the accompanying shorter heat times, the rate of scrap melting has now become one of the rate-limiting factors in steel production. As observed in commercial practice, the solution rate is influenced by the compositions of liquid and solid, the temperature, agitation, and time. However, no definitive work has been done on the Fe-C system, and there is very little information in the literature regarding the relative effects of these variables in steelmaking systems. A number of questions have been raised in regard to scrap utilization in basic oxygen steelmaking operations. Consideration has been given to the optimum size and shape of scrap, and to the use of preheated scrap as a means for decreasing the pig-iron requirement in oxygen blowing. The determination of an optimum scrap practice for a specific installation depends to a large extent upon the economics of the scrap market and also upon the behavior of scrap in the vessel. The present research was undertaken as a preliminary study in evaluating the behavior of steel in a pig-iron bath under various conditions of temperature, composition, and agitation, as might be encountered in oxygen converter operations or in any steelmaking operation where scrap behavior is an important process variable. Related studies have been carried out on non-ferrous systems. The solution rate of solid aluminum in a molten A1-Si alloy has been studied.' Furthermore, the increasing use of liquid metals has created considerable interest in studies related to dissolution of a solid in a liquid, or mass transfer taking place between a solid interface and a liquid metallic phase.2-10 In an effort to clarify the relative importance of factors influencing the dissolution of scrap in Fe-C alloys, this paper presents the results of a study of the rate of dissolution of a low-carbon steel cylinder in a molten Fe-C bath at various bath compositions, temperatures, and conditions of agitation. An attempt has been made to determine the mechanism of solution, and a model has been derived to fit the experimental results. The rate of heat transfer between the molten pig-iron bath and the solid-steel cylinder has also been studied. EXPERIMENTAL PROCEDURE A molten bath of pig iron (nominal composition 4.2 pct C, 0.5 pct Mn, 0.8 pct Si)* was held in a 200- *In view of the fact that the composition of the pig-iron bath was slowly changing with time because of steel dissolution and reaction with the surrounding atmosphere, intermittent samples of the liquid bath were taken throughout each experiment, Table 1. lb induction melting unit. The internal diameter of the furnace was 8-1/2 in. and the bath depth approximately 14 in. Cold-finished 1020 steel cylinders of 1/2-, 3/4-, 1-, 1-1/2-, and 2-in. diameters were cut into 1 -ft lengths for use as test specimens. One end of each bar was machined to fit a hand-driven, mechanical stirring device which rested on top of the furnace. This fixture permitted 7 to 8 in. of the bar to be immersed in the melt. The steel cylinders were cleaned to free the surface of grease and oxide. The rods, at ambient temperature, were immersed into the molten pig-iron bath. The melt temperatures studied in this investigation were 2300°, 2500°, and 2650°F. Different agitation conditions were achieved by operating with a) the power to the furnace, giving induction stirring; b) induction stirring plus mechanical stirring, using hand rotation with a chain and sprocket assembly at approximately 200 rpm; c) mechanical stirring alone with the power off; and d) the power off and no mechanical stirring resulting in minimum agitation, i.e., only that caused by natural convection currents in the bath. The samples were immersed in the melt for prescribed times ranging from 30 sec up to 6 min. Immersion times were measured with a stopwatch and temperature control of the melt was achieved by power adjustment following temperature measurement with an optical pyrometer. The measurements with the calibrated pyrometer were checked out to within less than 10°F with simultaneous thermocouple measurements. Following immersion, the bars were water-quenched and the diameters were measured with a micrometer at several positions on the reduced area, and by volumetric displacement. The dissolution rates calculated from the

Jan 1, 1965

By Thon T. Gin

The lithologic, mineralogic, and magnetic beneficiation characteristics of the iron formation at U. S. Steel's Atlantic City Ore Mine, Fremont County, Wyoming, have been determined. The iron formation averages about 30 percent Fe content, and varies from 125 feet to about 500 feet in thickness. It is composed of interbedded magnetite-rich quartzites, magnetite-quartz-amphibole schists, and amphibole-chlorite schists. Quartz, actinolite-tremolite, chlorite, and magnetite are the essential mineral constituents. These rocks are differentiated into four major ore types on the basis of their relative quartz and amphibole content. The iron content of the magnetic concentrate decreases and the silica content increases with decreasing grain size and increasing amphibole content in each ore type at the same fineness of grind. Criteria were developed to enable the mine operator to recognize the ore types and to blend them to produce a more uniform concentrator feed. This results in less variation in product quality and requires fewer changes in operating conditions-in the concentrator.

Jan 1, 1965

By Martin H. Stanczyk

The Bureau of Mines studied continuous closed-circuit attrition grinding of a coarse commercial filler-grade kaolin to produce paper-coating-grade clay having a particle size analysis of at least 70 percent minus 2-micron equivalent spherical diameter (esd). The coarse clay, containing about 12 percent minus 2-micron-esd material, was ground in a Bureau-developed 10-inch-diameter attrition grinder in closed circuit with a 5-foot-diameter bowl classifier. In the best test, a finished product containing 82.7 percent minus 2-micron-esd material was obtained when grinding 20 pounds of raw clay per hour at percent solids with a 100-percent circulating load. Energy consumption was about 341 kilowatt-hours per ton of clay feed, or 487 kilowatt-hours per ton of minus 2-micron-esd material produced. Closed-circuit grinding gave some-what greater particle size reduction and lower energy consumption than either batch or continuous open-circuit grinding.

Jan 1, 1965

By L. A. Dale, D. A. Dahlstrom

Closed-water circuits are justified today from two standpoints: economical operation and prevention of stream pollution. In today's modern preparation plant, it has been found very desirable to have the plant circulating water maintained at a relatively low solids concentration of around 3%. In so doing, bene-ficiation equipment can operate at a much higher efficiency. However, makeup water requirements would become excessive if the fines were to be removed from the preparation plant by bleeding a 3% solids concentration to a tailings pond. With the ever increasing percentage of —200 mesh coal, clay and slimes in the raw coal, coupled with the creation of these fines within the preparation plant, the need for water conservation for economy reasons becomes even more important. Because of stream pollution laws, tailings ponds have become very costly to operate and maintain, resulting in the necessity of employing an in-plant method of water recovery. Accordingly, the primary system employed in water recovery in the coal preparation plant today consists of a solids concentration device to thicken refuse solids while at the same time producing a sufficiently clarified effluent that can go back to the preparation plant for water reuse. The thickened product is then normally passed to a dewatering device that will produce a handleable solid that can be disposed of

Jan 1, 1965

By H. E. Powell

Basic data were recorded on the decompositions that take place during thermal decomposition of siderite (FeC03). Both the naturally occurring and a synthetically prepared mineral were studied by differential thermal, thermo-gravimetric, X-ray-diffraction, and chemical (including gas) analyses. Thermal decomposition was studied in the media of dry air, moist air, dry carbon dioxide, dry helium, and dry carbon monoxide and at atmospheric and at reduced pressures. Results showed the thermal decomposition of FeC03 to be an extremely complex process, dependent on environmental factors and side reactions that cannot now be completely controlled. Therefore, full understanding of the reaction involved must depend on additional research with advanced evaluation techniques.

Jan 1, 1965

By Lawrie D. C

Finely ground beryl was decomposed by mixing with ground limestone and soda ash and heating at 900°C for 4-6 hr. The sintered mater:al was then crushed and leached by boiling under reflux with 5N sulphuric acid for up to 4 hr. The liquor containing Be, AI, Fe and other elements as sulphates, was separated from the residue which consisted mainly of silica and gypsum, either by filtration or bydecantation washing.The clarified leach liquor was first treated to remove Fe+++ by contacting with a primary amine-kerosene solution in 2 countercurrent stages. The iron free liquor was then passed to a 4-stage counter-current extraction unit where it was contacted with O·5M di- (2 ethyl hexyl) phosphoric acid (EHPA) in kerosene. Under the operating conditions, 99 per cent of the Be and 7 per cent of the Al was extracted.The Be and Al were stripped from the organic phase by sodium hydroxide solution of suitable concentration to form soluble "beryllate" and "aluminate" respectively. Most of the Be was subsequently precipitatedas Be(OH)2 by heating the alkaline solution to 90°C, the Al remaining in solution. After filtration and washing, the Be(OH)2 could be ignited directly to BeO at about 1000°C or used as a feed to further purification stages if required.A small counter-current extraction unit was operated continuously using liquor derived from the sintering and leaching stages. Dataobtained in batch laboratory tests were confirmed. A product obtained by ignition of the washed "beryllate" precipitate contained more than 99 per cent BeO.INTRODUCTIONIn 1958 an investigation was commenced into the recovery of beryllium oxide from beryl, as part of a programme to utilize mineral resources of South Australia. A survey of the literature indicated that little work had been done on direct solvent extraction of beryllium from aqueous liquors, so it was decided to apply the experience gained in this field in uranium processing to the current problem.Preliminary extraction tests on solutions of beryllium...

Jan 1, 1965

By J. L. Eakin

The Bureau of Mines determined agents that are effective in foaming heavy brines and oil from gas wells in severe concentrations of sodium chloride, in severe concentrations of calcium chloride, or in moderate oil-brine mixtures. Dynamic foam tests were designed to select the more effective foaming agents. Numerous foaming agents were tested in concentrated simulated brines, in oilfield brines having varied concentrations of ions, in heavy natural brines, and in a commercial brine generally used as a reservoir pressure-balancing fluid. Several agents were detected that could perform efficiently in the field under the most severe saline conditions. Agents that promote foaming in oil-brine mixtures were also determined.

Jan 1, 1965

By G. E. Rennick

A siphon-type laboratory airlift well was designed and operated by the Bureau of Mines to study the concurrent flow of air and oil in small-diameter pipes. Glass flowstrings ranging from to 1 inch in diameter and from L4 to 64 feet in length were equipped with various-sized air-entry jets. Liquid holdup volumes were used to correlate vertical-flow data, and empirical equations for computing gas requirements were derived. The effect of flowstring length on flow efficiency, oil- and gas-production rates, and gas-oil ratios was relatively minor at all flowing pressures. Air-jet sizes and flowstring diameters, however, had a marked effect on flow efficiency and oil- and gas-production rates. The small air-jet sizes increased maximum flow efficiency and its associated flowing pressures but decreased oil- and gas-production rates. An increase in flowstring diameter increased maximum flow efficiency with its associated flowing pressure and also increased the production rates of oil and gas.

Jan 1, 1965

By W. W. Agey

An inexpensive technique that laboratory studies indicated would significantly reduce seepage in irrigation canals was devised and tested through research sponsored by the Bureau of Reclamation and the Missouri River Basin Field Committee. Laboratory tests simulating optimum field conditions determined that easily applied sodium carbonate solutions made test beds of canal lining materials virtually impermeable for long periods. The study comprised alternative laboratory treatments of 3-inch-deep test beds of canal earths with 74 water-soluble chemicals in search of one 01' more that would effectively improve the water barrier characteristics of the component clays. Sodium carbonate, one of the least expensive, was among the most effective. The addition of 0,4 lb of reagent per sq yd greatly reduced the seepage from typical, highly permeable test beds. The reagent penetrated and sealed surface for about a 1.5-inch depth.

Jan 1, 1965

By H. E. Rudi

The advent of open nit mining permitted the development and processing of minerals never before thought possible. New equipment was needed; new techniques were devised; new methods were called for. This development and acquisition of new techniques, methods and equipment did not, however, stir the souls of our industry and educational leaders sufficiently to a recognition of the problem of people, especially the future development of the people needed in open-pit mining. The people problem has been and will be with us as long as there are two of them. The development of people will be required for the same reason. The problem of developing future personnel for open-pit mining is not what must be developed; that is known to all of us and can be briefly stated ashore and better of everything." As I see it, the real problem lies in determining (1) what personnel are really critical, (2) why are they critical and (3) how can we develop them.

Jan 1, 1965

The purpose of this paper is to present the methods used in ground water control and the considerations that affected the development of these techniques. Production at Knob Lake is currently proceeding at depths which may be as much as 200 feet below the original standing water table. In order to produce a more saleable product and to improve operating and maintenance conditions, it is necessary to depress the water table below the mining level. Considerable success has been achieved by drilling deep wells in strategic locations and installing vertical tur-bine pumps at depths of up to 400 feet. This method is especially suitable for operation under severe winter conditions and has reduced the detrimental effects by a far greater extent than other methods of water control, Spring runoff is handled in open sumps, but all other water from four mines, with flows exceeding 16,000 g.p.m., is pumped all year 'round from about thirty-five wells. THE Knob Lake operation of the. Iron Ore Company of Canada is located on the Quebec-Labrador border, 320 miles north of Sept-lies, a seaport

Jan 1, 1965

By Norman G. Foster

The mass spectra of 14 previously unreported alkylthiophenes are pre-sented. Low ionization voltage data of selected compounds from these 14 and 23 previously reported alkylthiophenes are presented and discussed for their value in supporting fragmentation mechanisms analytical correlations. A comparison with and corroboration of earlier correlations is made. Additional correlations concerning detection of side chain branching and the detection of ethyl-alkyl and propyl-alkylthiophenes are made. A discussion of the possible fragmentation routes and mechanism of fragmentation is given. Speculative structures are inferred s out some of the ions and hence this work provides a basis for suggesting fation mechanisms for the alkylthiophenes according to modern theories ass spectrometry. Verification of these mechanisms must await the availability of isotopically labeled molecules which are labeled in specific lotions that permit the definition of the paths of frag-mentation. Some suggestions for further work to generalize on the correlations and studies made to this point are presented.

Jan 1, 1965

By S. L. May

Tantalum and columbium can be extracted from several of their ores or concentrates by chlorination procedures. Direct chlorination of high-grade minerals in the presence of carbon at temperatures between 500° and 800° C will extract up to 99 percent of the tantalum and columbium. Metallurgical beneficiation of low-grade source materials by carbothermic reduction produces a ferroalloy that is amenable to chlorination at a temperature of 500° C. Over 90 percent of the tantalum and columbium can be recovered.

Jan 1, 1965

By G. Krauss, W. Pitsch

The fine structure of the bcc martensite formed in an Fe-33 wt pct ATi single crystal of arrstenite is sho~on by transmission electron microscoPy to consist of combinations of transformation twins, stacking faults, deformation twins, and regular arrays of parallel screw dislocations. These structures constitute evidence for the multiple lattice-invariant deformations which operating during the formation of martensite could produce the real habit-plane scatter measured by a two-surface analysis of the plates formed in the single crystal of this investigation and reported in the literature for other Fe-Ni rnartensites. CRYSTALLOGRAPHIC theories1,2 of martensitic transformation show that the habit plane of martensite in a parent lattice is dependent in part upon an inhomogeneous distortion or lattice-invariant deformation which takes place on a fine scale within a martensite plate during its formation. Several recent theoretical papers3,4 have addressed themselves to an analysis of a wide variety of conceivable lat-tice-invarient deformations and the habit planes which they produce, while experimental investigation have been concerned with either the measurement of habit planes or the description and identification of the martensitic fine structure which reflects the nature of the lattice-invariant deformation operating during transformation. In Fe-Ni alloys with subzero Ms temperatures, the group of alloys with which this paper concerns itself, habit planes have often been found to scatter an amount greater than might be expected from possible experimental errors,5-7 and fine twinning has been identified as a major constituent of the fine structure of martensite.8-11 It has been suggested3,4 that more than one type of invariant shear occurs during martensitic transformation. This possibility has been experimentally supported12,13 by the observation of both dislocation configurations and twinning in a single martensite plate. The purpose of this paper is to report additional evidence for multiple lattice-invariant deformations in martensite and so to account for the real scatter in the habit planes of the martensite plates formed in Fe-Ni alloys. EXPERIMENTAL PROCEDURE The Fe-Ni single crystal was produced by pulling a high-purity iron and nickel charge through a single-crystal vacuum furnace in an alumina crucible. The crystal was double-melted to promote homogeneity and to increase its size by further additions on the second pass. In its final form the crystal was 4 cm in diam and 5 cm long. The nickel and carbon contents were analyzed at 32.9 and 0.006 wt pct, respectively. The austenite of this alloy first transformed to martensite by bursts at about -120°C, and, to preserve as much of the austenite as possible, all transformation was performed just below -120°C. Some observations were made on transformed samples which had been heated for 2 min at 340°C. It is assumed that the features of the martensite of these samples, Figs. 1 and 4, are the same as those of the as-quenched martensite. Orientation of the crystal by X-ray diffraction established 10.735 0.609 0.3161? as the axis of the crystal, an orientation that was checked within 2 deg by neutron diffraction. Further checks by electron diffraction of samples cut normal to the axis confirmed this orientation within the larger limits of error inherent in electron diffraction of thin foils. The X-ray orientation was the one used for the two-surface analysis of the martensite habit planes. A two-surface analysis was performed on the quadrant of the single crystal which had been oriented by both X-ray and neutron-diffraction techniques. Photomicrographs at X50 were made on two surfaces along an edge 2 cm long. Fiducial marks and the fact that many of the plates were almost completely surrounded by retained austenite made good matching of individual plates on two surfaces possible. The habit-plane trace on a surface was taken as the best line parallel to the long axis of a plate. A measure of the accuracy afforded by this criterion was provided by a family of very large plates which appeared at intervals along the entire 2 cm length of the edge. The plates all had habit-plane traces within 2 deg of one another. Many of the plates did not show midribs and, therefore, the use of midribs7 to represent habit-plane traces was not feasible in this investigation. The over-all experimental accuracy is estimated to be better than ±2 deg. Samples for transmission examination in a Siemens Elmiskop I at 100 kv were prepared by cutting 2-mm-thick discs from the single crystal, removing about 0.5 mm by chemical polishing,14 trans-

Jan 1, 1965

By A. T. Harris

Ground quartzite, known in the industry as amorphous silica, is produced from a quartzite deposit near Honey Brook, Pa., by George F. Pettinos, Inc., of Bala-Cynwyd, Pa. The quartzite is mined by the open pit method and processed in a mill at the mine. The operation regularly produces five standard grades of sand and one grade of crushed stone; however, the company accepts special orders and will produce material to meet the customer's specifications. Beneficiation (chiefly crushing and screening) is controlled by laboratory screen tests on samples taken during preparation of the sand. The chief uses of the sand are for foundry operations, furnace lining, concrete aggregate, and other specialized uses. The quartzite in this deposit is of uniform composition and does not require control by chemical analysis. However, for special purposes, analysis will be furnished.

Jan 1, 1965

By Hyung Sup Choi

The preparation of high-purity zirconyl compounds was studied in order to develop an economical process for obtaining pure zirconium via the caustic fritting of zircon sand. The direct dissolution of caustic frits with concentrated hydrochloric or nitric acid at 80c. followed by the addition of a small amount of acidified gelatin, gave high-purity zirconyl chloride or nitrate. The addition of a small amount of gelatin caused a mutual flocculation between colloidal silica and gelatin. The precipitation of this silica floc markedly lowered the content of silica in the product. The silica content of the compounds (or solution) so produced, generally less than 100 ppm., was sufficiently low for tributyl phosphate extraction for nitrate solutions. It was found that the degree of purification de-pends not only on the procedures employed but also on the nature of the frit itself. Silica was more effectively eliminated from the fritted product produced at higher temperatures, and less silica was present in the com-pound prepared from the frit produced in a shorter heating time. In order to ascertain the nature of the

Jan 1, 1965

By R. J. Leary

Oxidation testing of copper-clad steel strip was performed in a muffle furnace to determine whether copper in contact with steel scrap could be removed by oxidation in an airstream at high temperatures. Substantially all of the copper was oxidized before any significant iron oxidation occurred. The rate of copper oxidation was not affected by contact with iron. Copper oxide scale separated spontaneously from the underlying metal during cooling. Results indicate the possibility of removing light-gage copper coatings and components from ferrous scrap by oxidation in an incineration process.

Jan 1, 1965

By N. A. D. Parlee, I. D. Shah, W. C. Phelps

THIS note reports on a continuation of a program on the thermodynamics of Fe-S-X systems in the "steel-burning" temperature range begun by Bock, Barloga, and parlee.' Small coils of 0.039-in.-diameter pure iron (Ferrovac-E) wire were equilibrated with Fe-S-0 melts in ingot iron crucibles under argon at 1324°C in the assembly shown in Fig. 1, the lower part of which was heated in a large Globar furnace. Fig. 1 shows (R) the coiled iron wire sample, (M) the Fe-S-0 melt prepared from desired proportions of ferrous sulfide and ferric oxide, (K) the iron crucible, (I) a mullite guide tube, (J) an alumina crucible, (L) alundum sand, (N) crushed mullite, (Q) hollow cylinders of K30 brick, (C) a steel rod, (B), (El, (F), (G), (P), and (O), details of brass water-cooled head, and (H) a mullite tube 2-3/4 in. ID and 26 in. long. The rod (C) bearing the sample could be removed at will and be replaced by a tube for sampling the melt, or by a thermocouple for comparing the melt temperature with a control thermocouple not far from the 2-3/4-in. mullite tube. After equilibration the iron coils were treated with acid to remove the outer layer of metal and then they were analyzed for sulfur by a standard combustion method. The melt samples were analyzed for oxygen by a variation of Lander's2 hydrogen-reduction method for mattes, and for sulfur by the ASTM combustion-iodometric method NO. E 30-47. When the results of some forty-two runs were examined it was found that the sulfur and oxygen contents of the equilibrated melts showed good consistency, in that the plotted compositions fell along the smooth curve shown in Fig. 2. The points on this curve represent the experimental compositions of melts in equilibrium with ?-iron (Fe-S-0) solid solutions. These solid solutions are saturated with sulfur and oxygen with respect to the melt and therefore have the same sulfur and oxygen activities as the melt. The curve drawn through the points therefore delineates the ? liquidus. It falls in such a position as to roughly confirm the liquidus curves of Hilty and crafts3 at 1200" and 1300°C which are

Jan 1, 1965