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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 Murray Jacobson

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

Jan 1, 1961

By F. W. Wessel

Manganiferous carbonate slates of the Cuyuna range, which are part of the unoxidized thin-budded iron formation, represent a large potential source of manganese. This report details recent bench-scale research by the Federal Bureau of Mines in applying mineral-dressing techniques to these materials in order to investigate their potential uses. Work outlined in the report was directed toward the production of concentrates usable as iron-blast furnace feed, but an equally important objective might have been to furnish an enriched feed for extractive processes for recovering manganese. Flotation concentrates were prepared that contained 11.1 percent manganese, 27.8 percent iron, and 12.2 percent silica, with recoveries of 73 percent of the manganese and 48 percent of the iron. Calculated analysis for a simulated sinter suggests a product containing 16.0 percent manganese, 40.2 percent iron, and 17.6 percent silica, with 31 percent recovery of the dry weight of the ore. The silica in the flotation concentrates was due to quartz and iron silicates. Substantial quantities of the iron silicates (stilpnomelane and smaller amounts of minnesotaite) were present in the slate, and the need to reject these minerals limited the recovery of iron. The sintered flotation concentrate would be usable as ferruginous manganese ore for iron blast-furnace feed because of its favorable manganese silica ratio. The unsintered flotation concentrates, representing 45 percent of the feed weight and containing manganese enriched in the ratio of 1.6 : 1, also could be used as feed to processes for extracting manganese.

Jan 1, 1961

By R J. Tremblay, R. R. Hoffman

This paper deals with materials of construction and problems encountered and overcome in leaching and filtration of oxidized sulphuric acid slurry in the Port Radium mill after eight years of operation. The slurry is characterized by a high calcium sulphate content as well as a high chloride level under oxidized conditions, both of which affected initial design and subsequent changes. Leach agitation tanks are of wood with a mild steel superstructure and stainless steel agitator and moving parts below solution level. Electro-polished 316 stainless steel cooling coils are used for temperature control of the slurry. The string filters are of the Oliver type with wood decking. Extensive use is made of wood, Linatex lined mild steel and stainless steel for the slurry handling. A typical analysis of the slurry solution follows:(pH-1.30) ClOa Fe+++ Free Acid UaOs c1-so.--0.10 gms/litre 10.2 gms/litre 6. 7 gms/litre 3.5 gms/litre 2.0 gms/litre 155 gms/litre

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 W. M. Deaton

The Keyes Helium Plant of the Federal Bureau of Mines was constructed under an expedited schedule, to supply the urgent and growing demand for helium in atomic energy, missiles, aerology, space exploration, shielded-arc welding, and low-temperature research. Construction began in December 1958 and ended in August 1959. The plant, near Keyes, Okla., processes 2 percent helium-bearing natural gas from the Keyes gasfield. In 1960 the plant produced and shipped 263 million cubic feet of helium (equivalent to an annual rate of 290 million cubic feet). Production cost was $9.11 a thousand cubic feet of helium. A low-temperature process involving two steps is used; the first separates a crude-helium product from the natural gas at about -250° F. and 225 pounds per square inch gage (p.s.i.g.); and the second purifies the crude helium to a high-purity product (Grade-A helium, 99.995 percent helium) at about -320° F. and 2,750 p.s.i.g.

Jan 1, 1961

By H. H. Klepfer, M. E. Snyder

UNTIL very recently, the commercial availability of the rare earths as metals has been very limited. Fabrication of mill products from these metals has not been studied in most cases. This note reports the results of the development of fabrication techniques for thulium. Thulium has a melting point of about 1550°C and a hexagonal close-packed crystal structure. It oxidizes in air to give a black oxide (TmzO,). The procedures for producing thin thulium foil were developed on one ingot weighing about 220 g and were subsequently applied in processing about a pound of metal to foil. Several alternates for the various fabrication steps were investigated and will be discussed. The metal fabricated was in the form of commercial chill-cast ingots 1 in. in diam and 2 in. long weighing approximately 220 g. Impurities in the ingots were reported by the vendor to be 4000 ppni tantalum, 2000 ppm calcium, 200 ppm nickel, 100 to 200 ppm iron, 100 ppm europium, and less than 100 ppm copper, lutetium, and ytterbium. In addition to these impurities, several salt-like inclusions as large as l/8 in. in diam were revealed along the center line of the one ingot sectioned. Preliminary tests indicated that small wafers cut from the as-cast ingot would not fabricate readily by rolling. Forging of copper-jacketed wafers was therefore attempted. At 1550"F forging was satisfactory but an apparent reaction of copper with thulium demanded investigation of lower temperatures. Therefore, the remainder of the test ingot was forged at 1450°F—with only minor cracking. All ingots forged were inserted into copper tubes of 1 in. 1D and 0.125-in. wall thickness. The jackets were sealed by flattening the ends of the tubes and welding under helium. Heating time at 1450°F was 30 min. Press forgings of 1/8 in. per pass were used, followed by 10 min reheats. When the ingots had been squared and reduced to 0.250 in. in thickness, the original copper jacket was stripped off and replaced by a new jacket in preparation for hot rolling. Hot rolling at 1450" F without edge cracking was readily accomplished after forging. Excellent results were obtained with 10 pct reductions of thickness followed by 5 to 10 min reheats. After reduction of thickness from 0.250 to 0.100 in. the copper jacket was removed. It was found, in fact, that hot rolling in air was possible. A tenacious black oxide similar to that seen on zirconium was formed during 3 min reheats at 1450°F. Reduction in air to 0.010 in. foil was possible taking 10 pct reductions per pass. The oxide coat formed during hot rolling in air could best be removed by sand blasting and pickling. Common pickling solutions containing polar solvents were found to attack the metal too rapidly and a concentrated nitric-hydrofluoric acid mixture attacked neither the oxide nor the metal. The most satisfactory pickling solution was 52 vol pct concentrated nitric acid-48 vol pct glacial acetic acid. After forging to 0.250 in., vacuum annealing and cold rolling was found to be another satisfactory alternate to hot rolling in copper jackets. After forging. a hardness of Rockwell B76 was found. Annealing in vacuum (2 X l0-5 mm of Hg) for 1 hr at 1200"F did not alter this value. Annealing at 1470"F for 1 hr brought the hardness down to R;]63. With cold rolling (5 pct per pass) the hardness returned to about R,1:76 after 20 pct reduction and edge cracking became noticeable. However, cold rolling to a total of 40 pct reduction in thickness (RI,,83) was possible before edge crack propagation became serious. Good surface finish was obtained, and the metal loss due to oxidation was minimized by cold rolling and vacuum annealing. Using this procedure the yield of 1.25 in. wide by 0.010 in. thick foil from a 1-in. diam ingot was about 40 pct.

Jan 1, 1961

By William J. Orlandi

The intent and scope of this paper is to present to you, as concisely as possible, the problems and requirements -- and what we consider advantages -- of all-belt haulage in a modern underground coal mine. Mine No, 10, at Pawnee, Illinois, was opened in 1951; consequently, all the planning and consideration given to haulage selection was based on information then available and on Peabody Coal Company? s experience to that date,

Jan 1, 1961

By James S. Browning

The purpose of this investigation was to develop a dependable and economic method for recovering spodumene and mica from pegmatites of the type found in Gaston County, N. C. Laboratory batch tests and continuous flotation tests were made by the Federal Bureau of Mines to determine the feasibility of treating the ore by flotation to recover high-grade spodumene and mica concentrates. The spodumene flotation circuit yielded concentrates containing 6.50 percent lithia (Li20), with an overall recovery of 81.8 percent of the lithia in the ore, The mica circuit yielded concentrates containing 97.5 percent mica, with a recovery of 82.5 percent of the mica in the spodumene tailing.

Jan 1, 1961

By 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 Scott W. Hazen

In recent years many mining companies have recognized that their chance for continued economic survival depends on the adaptation of technological advances in their operations. Increased productivity through new developments in mining methods and improvements in equipment has made mining and processing of lower grade ores possible. Cost analysis has produced accurate data on the costs for development, production, and processing of ore. All of these changes and cost studies have shown the necessity for increased accuracy in determining the grade of ore. Methods of estimating grade in a mineral deposit have not kept pace with the technological advances in the other areas. The same methods are in use today as in the past. Experience and judgment are major criteria of accuracy and the results are highly subjective. In 1953, as part of its research program to develop a better understanding of fundamentals of mining technology, the Federal Bureau of Mines began a sampling method research project at its Denver Mining Research Center. The basic objective of the project is to investigate sampling methods and to study the adaptation of the techniques of statistical analysis to mine sampling.

Jan 1, 1961

By Barbara A. Thompson

A previously reported high-resolution method for the location of boron-rich areas in metallurgical and biological specimens was been adapted for general use on a routine basis. The rnetlzod utilizes neutron activation and autoradiograpizy. Alpha-particles emitted by boron nuclei upon neutron capture are recorded on a photographic emulsion. The resulting a-particle tracks show the location of boron-rich areas. Experimental techniques, interferences, and limitations of the method are discussed in detail. The method is most useful where there is marked segregation of boron. In this type of sample, the segregation can be observed when the nominal boron concentration is as low as 0.0006 pct. THE positive identification and location of boron-rich areas in metals is frequently of great interest in metallurgical work. Unequivocal identification is often difficult to make by conventional metallo-graphic methods. Recently, a method has been described which accomplishes this objective by neutron activation and autoradiography.l-3 The method can be described briefly as follows. Upon neutron capture, a -particles are emitted by boron nuclei according to the following reaction: ,Blo + n - ,a4 + 3Li7 + 2.4 mev The energy is dissipated as kinetic energy of the products. By irradiating a boron-containing sample in contact with a photographic emulsion and subsequently developing this emulsion, a-particle tracks are obtained whose location corresponds to the location of boron-rich areas in the sample. Two factors combine to make the reaction extremely specific for boron. The first is the unusually high (755 barns) cross section of boron for thermal neutron capture. The second is the higher neutron energy required to produce (n, a ) reactions in essentially all other nuclei except lithium. These two factors make the method specific for boron by six to seven orders of magnitude when a predominantly thermal neutron source such as the Brookhaven reactor is used. The reported limit of detection of this method is of the order of 0.01 pct B., The present work was originally undertaken to determine whether this limit could be lowered by use of a thinner emulsion. However, initial experiments showed that in order to use the method at all, it was necessary to reestablish the optimum experimental conditions in terms of the available irradiation facilities. It is the purpose of this paper to describe these experimental conditions in detail, to discuss the factors influencing sensitivity, and to evaluate several techniques for increasing sensitivity. EXPERIMENTAL A) Preliminary Experiments—The first measure-ments were made using samples of crystal oriented silicon steel containing various concentrations of boron. In the later experiments, samples of various high-temperature alloys such as M-252, hcoloy 901, Nichrome V, and so forth, were used. Faraggi, et al.,2 reported that the lower limit of sensitivity in this type of sample was about 0.01 pct B using nuclear emulsions of 50- u thickness. but that it should be possible to extend this limit by the use of thinner emulsions. Accordingly, we first used Kodak Auto-radiographic Stripping Film (Permeable Base) which has an emulsion thickness of only 5 µ. This was mounted on the metallographic specimens according to the technique described by Boyd.4 The emulsion remained in contact with the metal surface throughout exposure and development. Since the emulsion is transparent after development, the autoradiograph and metal surface can be viewed simultaneously and any correlation between film blackening and structure of the metal can be made directly with no problems of realignment. Because the silicon steel is readily attacked by moisture alone, it was necessary to apply a protective coating to the metal surfaces before mounting the emulsion. The coating was made extremely thin in order to absorb as few a-particles as possible. Boyd4 and Gomberg5 have discussed various plastics used for this purpose; however, none was sufficiently impermeable to prevent chemical attack of the steel during the developing process. This attack resulted in the production of gross chemical artifacts in the emulsion. It was, therefore, necessary to use the method of Wolfsberg and John6 as follows. A very thin (approximately 1 µ) coating of Plexiglas II was applied by dipping the sample in a 2 pct solution of Plexiglas II in dichloroethylene. Then, because the emulsion will not adhere to Plexiglas 11, a thin coating of Parlodion was applied in a similar manner using 2 pct Parlodion in iso-amyl acetate. No protective coating was necessary with the high-tem-

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

By R. M. Becker

As part of the Bureau of Mines program for examining the Nation's iron and titanium resources, magnetic, gravity, and geologic surveys were made to permit an estimate of the extent and magnitude of the Iron Mountain, Colorado, titaniferous magnetite deposit. Gabbro is the dominant rock type of the area. Within the gabbro are lenses of titaniferous magnetite, 5 to 25 feet wide and as much as several hundred feet long. These lenses comprise a zone which has scattered occurrences of magnetite for 2,200 feet. To the west, the gabbro grades into a strip of pyroxenite that in turn borders a large monzonite mass. A wedgelike broadening of the pyroxenite with depth accompanied by little or no increase in the titaniferous magnetite is considered a reasonable interpretation of the field data. The iron deposits appear to be limited and discontinuous.

Jan 1, 1961

By A. Simkovich, R. W. Lindsay

The possibility of using sodium sulfide slags to remove copper from ferrous alloys has been investigated by Jordan1 and by Langenberg.2, 3 In these studies, such slags were determined to be capable of removing copper and sulfur from the melt. The present work represents additional effort to clarify the effects of temperature on copper removal. The experiments were performed in a 17-lb induction furnace. Graphite crucibles contained the melts and kept the baths saturated with carbon. Temperatures were measured with a calibrated optical pyrometer and were controlled by manipulation of power input to the furnace. Estimated accuracy of temperatures in this investigation is ± 10°C (18°F) for measurements prior to slag additions, and + 20°C (36°F) after slag formation. The procedure consisted of melting 800 g of electrolytic iron. During this step, powdered graphite covered the exposed iron surface. After a predetermined temperature was reached, copper shot was added. A sample of the molten alloy for chemical analysis was then aspirated into a silica sheath. Next, a slag-forming mixture of sodium sulfite and graphite was added instantaneously to the melt. The sodium sulfite amounted to one-tenth the charge weight of iron; sufficient graphite was added to combine with oxygen in the sodium sulfite, assuming formation of carbon monoxide and reduction of the sulfite to sulfide. Subsequent to the slag addition, the molten alloy was sampled periodically, with the exception of heat A in which no intervening samples were taken between the slag addition and the end of the run. The iron was poured into a graphite mold, and the ingots sectioned and drilled for samples. Results of selected heats are presented in Table I. Analyses of samples drawn from the iron prior to slag addition are listed under zero time. Two samples from heat D were reported with copper contents greater than the initial concentration in the bath. Owing to the gradual but complete disappearance of slag during this heat, it is believed copper momentarily became more concentrated in the upper portion of the bath while reverting from the slag. This is the region from which samples were drawn. It should be noted that analysis of the ingot was equal to the copper content at the time of slag addition. The terminal temperatures of heats D and E, and the initial sulfur content of heat A are also to be noted. Because of the large temperature drop which occurred when slag was formed in heat D, power input to the furnace was increased in heat E after the slag addition, causing a higher terminal temperature. In heat A, the initial sulfur concentration was relatively high as compared to heats B through E owing to contamination by some slag remaining in the crucible from a previous heat. It is evident from Table I that copper was removed at the onset of slag formation. Roughly 30 pct of the copper was taken into the slag, with the exception of heat D, which had approximately 50 pct removed. For a comparatively short time of slag-metal contact, it appears that no gain is to be made in copper removal through use of high or low temperatures. If the slag initially formed remains in contact with the iron for an extended period, temperature has a marked effect upon copper removal, as can be seen by studying results for the two extremes in temperature. At about 1425°C, the copper level remained relatively constant after the initial removal by the slag. However, in the region of 1670°C, a definite reversion of copper occurred. Reversion was incomplete in heat D, and complete in heat E. The final temperatures of heats D and E differed by about 75°C. This temperature difference is thought to be the reason for only partial copper reversion in heat D. It is believed the effects of temperature noted above are related to the evolution of a white fume, which appeared in every run except heat A. (In the case of heat A, the fume was practically indiscernible.) After each slag addition, a yellow flame formed for about 5 sec. When the flame subsided, a white fume appeared. Upon contact with surrounding cooler surfaces, this fume deposited as a white solid. In the experiments made at 1425°C, evolution of fume continued unchanged to the end of the runs. However, heats D and E exhibited a different behavior. A very noticeable decrease in fume evolution from heat D was observed. Furthermore, this heat had much less slag remaining than did runs A through C when the experiments were terminated. No slag remained at the end of heat E; evolution of fume from this heat ceased prior to pouring. Spec-trographic analysis of the white deposit indicated sodium to be the major metallic element, with the maximum concentration of iron and copper as 0.1 and 0.01 pct, respectively. It is supposed the white fume observed in these experiments is principally sodium oxide (Na2O), formed by oxidation of sodium in the slag and subsequent sublimation. (Sodium oxide is a white to gray substance in the solid state; at 1275oC, it sublimes.4) According to this mechanism, elevated temperatures would accelerate removal of sodium from the slag, sulfur pickup by the

Jan 1, 1961

By J. W. Town

This report summarizes the results of laboratory investigations conducted by the Federal Bureau of Mines to obtain hydrometallurgical information on the dissolution of mercury sulfides from ores, flotation concentrates, and pure mercuric sulfides. Statistical methods were used to design the experiments and evaluate the resulting data. Studies demonstrated that cinnabar is readily soluble in sodium sulfide, partly soluble in potassium sulfide, and essentially insoluble in ammonium sulfide. Additions of sodium hydroxide or potassium hydroxide to sodium sulfide solutions increased mercury extraction slightly; when either was added to potassium sulfide or ammonium sulfide solutions, mercury extraction was equal to that of sodium sulfide. Tests at the Albany Metallurgy Research Center showed that sodium sulfide would completely dissolve chemically pure mercuric sulfide, more than 95 percent of the cinnabar in 5-percent mercury flotation concentrates, and 60 to 90 percent of the cinnabar in low-grade ores. The double-leach tests showed that potassium sulfide would dissolve over 90 percent of the arsenic in mercury-arsenic products and 1 to 10 percent of the mercury; then sodium sulfide-hydroxide solutions would dissolve 80 to 90 percent of the remaining mercury and 5 to 10 percent of the arsenic.

Jan 1, 1961

By R. H. Gautschi, F. C. Langenberg

Rare-earth additions were made to laboratory heats of Type 310 stainless to observe their effect on as-cast ingot structure, nitrogen and sulfur contents, and nonmetallic inclusions. Lanthanum had a grain-refining effect in 30-lb ingots, but results with 200-lb ingots were inconsistent. Cerium, lanthanum, and misch metal lowered the sulfur content when the sulfur exceeded 0.015 pct and the rare-earth addition was greater than 0.1 pct. The rare-eardh content in the metal dropped very rapidly within the first few minutes after the addition. The size, shape, and distribution of nonmetallic inclusions was not changed in 30-lb ingots, but changes were noticed in larger ingots. RARE-earth* additions have been made to austenitic Cr-Ni and Cr-Mn steels to improve their hot workability. The high alloy content of these steels often results in a considerable resistance to deformation and inherent hot shortness at rolling temperatures, particularly in larger ingots. Rare earths in the metallic, oxide, or halide form are usually added to the steel in the ladle after deoxidation although they can be added in the furnace prior to tap or in the molds during teeming. The literature- indicates that the effects of rare-earth treatments on these stainless steels are not consistent, and sometimes even contradictory. Since no mechanism has been presented which satisfactorily accounts for the claimed improvements, the effects of rare earths are a qualitative matter. The work described in this paper was initiated to expand the knowledge of the effects of rare-earth additions on melting variables such as ingot structure, chemical analysis, and nonmetallic inclusions. REVIEW OF LITERATURE Ingot Structure—Rare-earth additions to stainless steels have been reported to cause a change in primary ingot structure in that there are fewer coarse columnar grains. However, the results are inconsistent. While one investigation1 has shown a large reduction in coarse columnar crystals, another2 has been unable to observe this effect, particularly when small ingots were poured. Post and coworkers3 observed ingot structures for a number of years and found that the columnar type of structure is not definitely a cause of any particular trouble in rolling or hammering, provided the alloy is ductile. Knapp and Bolkcom4 found rare-earth additions to be quite effective in preventing grain coarsening in Type 310 stainless steel. Chemical Analysis—Many effects of rare-earth treatment on chemical analysis have been claimed in the literature. Russell5 observed that some sulfur is removed by rare-earth metals, and that a high initial sulfur content improved the efficiency of sulfur removal. Lillieqvist and Mickelson6 report that rare-earth treatment causes sulfur removal in basic open-hearth furnaces, but not in basic lined induction furnaces. Knapp and Bolkcom found no sulfur removal in acid open-hearth and acid electric furnaces, probably because the acid slag can not retain sul-fides. snellmann7 showed that sulfur could be lowered apprecfably with rare-earth additions; however, a sulfur reversion occurred with time. Langenberg and chipman8 studied the reaction CeS(s) = Ce(in Fe) + S(in Fe), and found the solubilit product [%Ce] [%S] equal to (1.5 + 0.5) X 10-3'at 1600°C. Results in 17 Cr-9 Ni stainless were about the same as those in iron. Beaver2 treated chromium-nickel steels with 0.3 pct misch metal and observed some reduction in the oxygen content. He also noted an inconsistent but beneficial effect of rare earths when tramp elements were present in amounts sufficient to cause difficulty in hot working. It is not known whether rare earths reduce the content of the tramp elements or change the form in which these elements appear in the final structure. No quantitative data are available concerning a possible effect of rare-earth treatment on hydrogen and nitrogen contents. However, Schwartzbart and sheehan9 stated that additions of rare earths had no effect on impact properties when the nitrogen content was low (0.006 pct), but served to counteract the adverse effects of high nitrogen content (0.030 pct) on these properties. Knapp and Bolkcom4 analyzed open-hearth heats in the treated and untreated conditions and found the nitrogen content (0.006 pct) to be unaffected. These two results lead to the speculation that rare-earth additions can reduce the nitrogen content to a certain level. Decker and coworkers10 have observed that small amounts of boron or zirconium, picked up from magnesia or zirconia crucibles, increased high-tem-

Jan 1, 1961

By C. G. Dunn, P. K. Koh

THE primary recrystallization texture in cold-rolled silicon iron, which is the matrix texture for developing the Goss texture or the cube-on-edge texture by secondary recrystallization at temperatures near 900°C,1-5,21 has not been adequately described. Thus from the present available information, it is not possible to explain satisfactorily both the grain-growth selectivity of the matrix and the often observed magnetic torque curve, which itself provides some information on the texture. Also lacking is information on the special annealing texture that develops in this material when the annealing temperature is 1200°C or higher and the rate of rise to temperature is extremely rapid. From the work of May and Turnbull5 and from unpublished work, it was known that isothermal annealing near 1200°C tends to reduce the extent of secondary recrystallization and that a much weaker cube-on-edge texture results if appreciable normal grain growth replaces secondary recrystallization. Koh and Dunn6,7 have obtained additional information on complex primary recrystallization textures from further studies made after normal grain growth. In these instances the initial textures were retained during normal grain growth. A similar result reasonably could be expected in the present study except for the presence of a grain growth ihibitor1-5,8,9.21 and its tendency to allow only a few grains to grow. However, any information on the orientations of grains in the special annealing texture, even if far from representative of the initial matrix texture, would provide useful information on the nature of the matrix texture. In the present texture study the method of Newkirk and Bruce,10 which is based on the methods of Geisler" and Schwartz, 12 is used to obtain a complete (110) pole figure of the primary recrystallization texture. The high-temperature annealing texture is determined simply from the orientations of a large number of selected grains. The kinetic nature of the process that produces the annealing texture is treated elsewhere13 and it is shown that a form of secondary recrystallization with a very high rate of nucleation occurs during rapid annealing at high temperatures. EXPERIMENTAL PROCEDURE Commercial 0.014-in. cold-rolled silicon iron strip (3.16 wt pct Si), prepared by two stages of cold rolling with an intermediate short anneal, was given a decarburizing 3-min anneal at 800°C. Me-tallographic studies indicated complete recrystallization. Short-time anneals at 900° C and at higher temperatures proved that secondary recrystallization had not begun at 800°C, in fact, the short additional anneals were still in the induction period of secondary recrystallization. A rapid rise to an annealing temperature of 1260°C (2300°F) was obtained in a BaC12and NaCl fused salt bath. The structures that resulted from anneals in the range 12- to 1000-sec duration were relatively finegrained, even though the growth was a form of exaggerated grain growth13 or secondary recrystallization with a high nucleation frequency.= Many of the grains were large enough for an X-ray study using a 5-mil X-ray beam. A transmission Laue Camera and an optical-mechanical stage for moving the grains into the X-ray beam were used. A total of 325 grains were X-rayed in this manner and the grain orientations determined. Complete (110) pole figures were obtained for the primary recrystallization texture using CoKa radiation at 30 kv in the back-reflection range, such as (220) for (110) poles, as described recently by Newkirk and Bruce.10 The low voltage serves to reduce the spurious white radiation to a minimum. A filter of 0.001-inch iron foil was located in front of the detector slit for transmission and in front of the beam slit for back reflection. A new and improved specimen holder extended the useful tilting angle range for transmission to 70 deg instead of 60 deg as previously reported.' A torque magnetometer was used to obtain the magnetic torque curves for a number of l-in. diam disk specimens. RESULTS The (110) pole figure of the material after recrystallization at 800°C is shown in Fig. 1. The positions of the pole concentrations are found to be

Jan 1, 1961

By C. S. Smith

QUANTITATIVE methods were used to good effect in the earliest days of metallography1-3 but they mysteriously passed into virtual disuse until the important paper4 by Howard and Cohen in 1947. Various devices for the measurements of integrated linear intercepts have been constructed, primarily by petrographers. The hydraulically operated stage designed by the writer5 was satisfactory, but prolonged use caused air bubbles to become entrapped, which introduced back-lash. A new stage has been constructed which avoids this defect and provides better integration when measuring directional structures. This utilizes a circular traverse, and integration is achieved by counting electrical pulses produced by a photocell and a light chopper.* The stage is shown diagramatically in Fig. 1 and in photograph, Fig. 2. It is of simple construction. Mounted on a plate with clamps to fit the stage of a standard metallurgical microscope is a worm and 100-tooth worm gear, the latter supporting the specimen to be measured. The worm is manually actuated by a knob which contains inside it three

Jan 1, 1961

By J. M. Kuchta

Concentrated hydrogen peroxide (H202) is a highly reactive oxidizing agent that liberates heat when it decomposes. The heat liberated may be sufficient to ignite combustibles with which the peroxide comes in contact. For this reason, concentrated hydrogen peroxide should be handled only by personnel familiar with its many unique properties.6 Hydrogen peroxide is used as a bleaching agent in the manufacture of textiles; this is its major single use in the United States. It is also employed as a reagent in chemical synthesis, as a source of free radicals to start polymerization, as a foaming agent in the manufacture of porous substances, and for its effect on biological processes. Moreover, highly concentrated hydrogen peroxide is a compact source of energy that can be utilized both as a monopropellant and as the oxidizer in a bipropellant system, During World War II, large quantities of highly concentrated hydro- gen peroxide were used as propellants, particularly in Germany. Since then, production of the peroxide has increased rapidly; in the United States alone it has more than doubled since 1950.7 Because of its widespread use, increasing interest has been shown in the hazards of handling the high- strength peroxide.

Jan 1, 1961