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By G. H. Martindill

Complex chemical and physical changes occurring during carbonization result in a heterogeneous system composed of gaseous, liquid, and solid phases, whose relative proportions and chemical compositions change constantly as temperature increases. Studies in which the participating variables are isolated and controlled should be useful in formulating the mechanism of coal carbonization. The most characteristic property of a coking coal is its ability to form a plastic mass at a certain stage of the carbonization process. During this period it is believed that fluidity of the coal influences the properties of the resultant coke. This report gives results of an investigation by the Federal Bureau of Mines of the influence of the maximum fluidity attained by the charge on the physical quality of the coke or char produced. As a first approach to the problem, researchers investigated high-melting-point pitches, which are relatively simple carbonaceous materials. The plastic properties of these pitches, prepared specially for this work, varied greatly; their fluidities, as measured by the Gieseler plastometer, covered most of the fluidity range characteristic of coking coals. Blending these pitches with increasing pro-portions of fine coke progressively reduced their fluidities. Coal-pitch and coal-coke blends also were treated; their fluidities were varied by changing their blending ratios. The various blends were carbonized in a small-scale carbonizer and the resistance of the carbonized residue (char) to abrasion was determined in a small-scale tumbler test, using the Roga drum.

Jan 1, 1960

By Jasper L. Stuckey

GEOGRAPHICALLY, North Carolina consists of three divisions, the coastal plain on the east, the piedmont plateau in the center, and the Appalachian mountain region on the west. Geologically, the State may be divided into two main divisions, an eastern or coastal plain region, and a western or piedmont plateau and mountain region. The eastern region is underlain with unconsolidated sands, clays, marls, and shell limestones varying in age from Cretaceous to Recent. The western region is, in general, underlain with gneisses, schists, slates, sheared volcanics, and igneous intrusives of Pre-Cambrian age. In the mountain and upper piedmont portion of the western region are several areas of irregularly metamorphosed sediments of early Paleozoic age. Throughout the piedmont plateau and a part of the mountain portion of the western region, important areas are underlain with igneous intrusives of late Carboniferous age. Along the eastern edge of the piedmont plateau are two narrow belts, trending northeast-southwest, underlain with sediments of upper Triassic age. Although North Carolina contains a

Jan 1, 1947

By Ernest W. Loya

A method for preparing gravimetric primary standards of helium in the parts per trillion range has been developed by the Bureau of Mines. The standards are used to calibrate a specially modified mass spectrometer used in determining the abundance of helium-3 and helium-4 in geochemical samples and of helium-3 in isotopically purified helium-4. The desired gas standards are prepared in 5-kg metal cylinders filled to 1,800 psia. Relative errors of less than 1 pct have been attained in the parts per trillion range using a successive dilution technique.

Jan 1, 1982

By Shilpa S. Haramkar, Bhaskar N. Thorat, Sachin V. Jadhav

The filtration of phosphogypsum is a ubiquitous step in the manufacturing of phosphoric acid. It is highly desired to achieve the minimum concentration of P2O5 in the phosphogypsum cake. This work is aimed at addressing P2O5 losses in phosphogypsum (PG) along with the recovery of P2O5 from slurry by using constant pressure filtration at 1 bar pressure. Laboratory tests were carried out in the phosphoric acid production plant situated in Paradeep, India. Recycled water source near acid plant (i.e., pond water) was used for cake washing to reduce the burden on fresh water stock. The findings indicated that pressure filtration offered the most effective P2O5 recovery (nearly 93.48%). The moisture was reduced to 14–16%, and watersoluble P2O5 in the gypsum cake was found to be negligible. A narrow particle size distribution was observed, which offered effective filterability with average cake resistance of 2.38 × 1010 m/kg, indicating a moderately separable cake.

Aug 23, 2023

By Pradeep K. Rohatgi, Clyde M. Adams

Structures produced upon solidification of the eu-tectic composition (33 wt pct Cu) aluminum copper alloy have been examined as a function of freezing rate dfs /d? , the rate of change of fraction solid (fs) with time (8). Slow (dfs/d? = 0.0016 sec-1), intermediate (dfs/d? = 0.02 sec-1) and rapid (dfs/d? = 0.4 to 7.30 sec-1) freezing rates were used. The lamellar Al-Cual2 eutectic is arranged in the form of rod-shaped colonies at rapid freezing rates. The colonies are aligned parallel to the direction of heat flow, whereas the lamellae within the colonies are aligned at various angles, as high as 90 deg, to the direction of heat flow. The colony spacing (C) is proportional to the square root of inverse freezihg rate. The relationship is C = 15.5(dfs/d?)-1/2 where C is in µ and 8 is in sec. The ratio of colony spacing to lamellar spacing is greater than 20.0 and increases with a decrease in the freezing rate. A duplex dendritic structure is produced at intermediate freezing rates. A fine lamellar eutectic is arranged within the dendrites (exhibiting side branches at an angle close to 60 deg from the main stem) and a coarse irregular eutectic appears in the interdendritic regions. The duplex eutectic structure is also produced at slow freezing rates. However, at slow freezing rates there is a Platelat of CuAl2, along the center of the main stem of each dendrite and the other lamellae are arranged perpendicular to the central platelet. THE eutectic between CuA12 and a! aluminum has been reported to freeze in a lamellar form by several workers.'-3 chadwick4 has measured the interlamel-lar spacing as a function of growth rate. Kraft and Albright2 have reported on irregularities in the lamellar structures, and have proposed growth models which account for the formation of faults during solidification. In certain instances the lamellar eutectic has been found to exist in colonies. The colony formation315 has been attributed to the breakdown of a planar liquid-solid interface due to rejection of impurities. The aim of the present work is to study the structures produced from the eutectic aluminum-copper alloy under relatively fast solidification rates, such as encountered in casting and welding operations. The solid-liquid interface presumably remains planar under conditions of slow unidirectional freezing which produce lamellae aligned parallel to the direction of heat flow. The local growth velocities are the same over the entire interface and are equal to the rate of growth of the all-solid region. The spacing between the eutectic lamellae is inversely proportional to the square root of the growth rate of the all-solid region. Under the freezing conditions used in the present study, the solid-liquid interface is cellular or dendritic and the local growth velocities are different in the different regions of the interface. The relationship between the growth rate of the all solid region and the local growth velocities varies with the location and the shape of the interface. The growth rate of the all-solid region is, therefore, an inadequate parameter to describe the eutectic micro-structures which depend upon the local growth velocities. For this reason the structures have been examined as a function of freezing rate, dfs/d?, where fs is the fraction solidified at time 0. The freezing rate was varied by a factor of 4000. The relationship between the freezing rate, dfs/d?, and the growth velocit of the all solid region depends upon the specimen geometry and the shape of the interface. EXPERIMENTAL PROCEDURES The A1-33 pct Cu alloy used throughout this study was made in an induction furnace, using electrolytic copper and aluminum of commercial purity (99.7 pct), the primary impurities being silicon (0.12 pct), iron (0.14 pct), and zinc (0.02 pct). Three ranges of freezing rates were investigated: 1) A spectrum of rapid freezing rates (ranging from 0.40 to 7.30 sec-1) was obtained in arc deposits made on 2-in. thick cast plates of the eutectic alloy. The arc was operated at constant power and was made to travel at constant velocity on the surface of the plate that was in contact with the chill surface during solidification. The pool of liquid metal formed under the moving tungsten arc solidified rapidly by heat extraction through the unmelted plate. Conditions of unidirectional heat flow were achieved near the fusion zone interface, especially in the center of the arc deposits. The great advantage of the arc technique is that rapid cooling and freezing rates can be varied in a qualitative way. The correlation between the arc parameters and the solidification rate is given by the following relationship:6-8

Jan 1, 1970

By Neda Zangeneh

Production efficiency from low permeability gas shales require techniques to optimize hydraulic fracture completions. One completion strategy involves the simultaneous or near simultaneous hydraulic fracturing of multiple horizontal wells to maximize the fracture network area and stimulated reservoir volume. However, changes to the in-situ stress field caused by an earlier hydrofrac on subsequent hydraulic fractures are not accounted for in traditional hydrofrac design calculations. Presented here are the results from a set of transient, coupled hydro-mechanical simulations of a rock mass containing two wellbores using the discontinuum-based distinct-element method. The results demonstrate the influence of stress-shadows generated by a hydraulic fracture on the development of subsequent hydrofracs from an adjacent well. It is shown here that these interactions have the potential to change the size and effectiveness of the hydraulic fracture stimulation by changing the extent of the hydraulic fracture around the secondary well.

Jun 1, 2012

By K. S. Barros, D. C. R. Espinosa, J. A. S. Tenório

Over the past several decades, electrodialysis membranes have been employed for the removal of metals from galvanizing industry effluents. However, for its technical viability, it is useful to know some properties of the system to avoid, for example, precipitation of inorganic salts, destruction of the membrane and an increase in the energy consumption. The scope of the present study is to use chronopotentiometry to determine limiting current densities, transition times and resistances of the cationic membrane HDX 100 using a synthesized solution of the galvanizing industry effluent prepared with copper sulfate and sulfuric acid in different concentrations: 0.1, 0.5 and 1.0 g/L of Cu +2. The current-voltage and chronopotentiometric curves obtained have clearly defined regions and it was verified that the Cu+2 concentration causes a significant increase in the limiting current densities and in transition times. However, a high decrease in resistance occurred because at the highest concentrations, it is more difficult to reach the zero concentration value at the membrane surface. Besides, the pH increase causes a significant decrease in the limiting current density and in the transport number, but a slight increase in the resistance due to the presence of hydrogen. The results obtained confirm that the chronopotentiometry method is a valuable tool to determine membrane properties.

Mar 1, 2017

By V. Astucuri

El presente trabajo describe el proceso de extracción de plata de dos muestras de relaves antiguos empleando la cianuración. De acuerdo a este estudio, entre todos los procesos metalúrgicos utilizados para la recuperación de la plata como la tostación sulfatante, amalgamación, flotación, se encontró que la cianuración es un proceso completo ya que puede reemplazar a las anteriores, con excepción de la amalgamación de plata nativa y otras deficiencias. En consecuencia, la cianuración es el método hidrometalúrgico que aprovecha mejor el poder lixiviante de los cianuros alcalinos en soluciones diluídas y extrae la palta de los relaves. Por ello, se supedita a su contenido económico y a los minerales no económicos entre los que se encuentre asociado.

Oct 14, 1980

By Gustavo Henrique Bolognesi Donato

A utilização de materiais cerâmicos em componentes que operam em elevadas temperaturas (p. ex.: trocadores de calor cerâmicos que operam acima de 800°C) é vantajosa do ponto de vista térmico, mas não é trivial em termos estruturais, uma vez que estes materiais são frágeis e portanto, suscetíveis à fratura catastrófica. Considerando a necessidade de materiais resistentes a elevadas temperaturas e que garantam a integridade de aplicações como tais trocadores de calor, este trabalho investiga as propriedades mecânicas da alumina a (Al2O3) como função da temperatura na faixa de 23°C a 850°C. Para tal, cem ensaios de flexão em 4 pontos e ensaios adicionais selecionados em 3 pontos foram realizados em amostras de seção transversal retangular de ~ 45 mm2 produzidas por gelcasting, técnica esta que tem grande potencial para moldar peças de geometria complexa. Os ensaios foram conduzidos empregando um dispositivo fabricado em Inconel (superliga de Níquel-Cromo) especialmente desenvolvido para esta finalidade e contendo articulações objetivando autocompensação de desalinhamentos. Os resultados experimentais puderam ser muito bem descritos usando a estatística biparamétrica de Weibull e demonstram o efeito da temperatura na redução da resistência à flexão. Adicionalmente, o dispositivo proposto facilitou e dinamizou a realização dos ensaios, além de garantir pequena dispersão das propriedades mecânicas obtidas, especialmente se considerado o micromecanismo frágil de fraturamento desta classe de materiais.

Aug 8, 2018

By Sahendra Ram, Arnn Kr Singh, Dheeraj Kumar, Rajendra Singh

"Inherent existence of different rooms (openings) along the extraction line in a depillaring panel provides an easy path for the goaf to encroach the working area. Each of these openings in a mechanized depillaring (MD) operation along the extraction line is supported by the roof bolt-based breaker line support (RBBLS) to restrict the goaf encroachment. Different field studies by Council for Scientific and Industrial Research - Central Institute of Mining and Fuel Research (CSIR-CIMFR) found that the RBBLS works effectively during the depillaring under the shadow of stable surrounding ribs/fenders only. It is observed that, generally, these natural supports experience high value of induced stresses after a large amount of void creation inside the goaf. The induced stress creates spalling/loosening of the sides of the natural supports. Field studies also found that the positions of the RBBLS at the goaf edge need to be adjusted according to the depth of this spalling/ loosening. However, a systematic study in field for the correct positioning of the breaker line as per the spalling/loosening under different site conditions is difficult. Therefore, on the basis of the data and guidance provided by these field investigations, a detailed parametric investigation was conducted in the laboratory on simulated models for an effective design of RBBLS in a MD panel. FLAC3D is used for the simulation of the depillaring, and the available empirical formulations for Indian coalfields are used for subsequent calibration. An analysis of stress redistribution for different stages of the MD in simulated models showed the significance of the nature of overlying strata/induced stress for the RBBLS design. Discussing some results of field studies, this paper presents results of the laboratory investigations for an effective design of the RBBLS.INTRODUCTIONContinuous Miner (CM)-based mechanized depillaring (MD) is an important issue for Indian coalfields, where huge amounts of coal are locked up in standing pillars (Dixit and Mishra, 2010). Considerable variations in site conditions of these developed pillars bring a number of technical challenges into consideration during their final extraction. One of these challenges is goaf encroachment/overriding during caving of the competent roof strata. Goaf encroachment/overriding can effectively be controlled, mainly, by suitable design of natural supports (rib/snook/fender). However, there is a requirement of applied supports against the immediate roof as a considerable portion of this roof is exposed due to the presence of different openings along the line of extraction. These applied supports act as a fulcrum at the goaf edge between the working area and the goaf to facilitate the break out of the hanging roof inside the goaf. This is called breaker line support. An effective breaker line support is important for the efficiency of a depillaring operation. Generally, MD adopts roof bolt-based breaker line support (RBBLS) at the goaf edge (Singh, et al., 2014). For the first time in India, roof bolts were applied at the goaf edge as RBBLS in a CM-based MD (Leeming, 2003). In the beginning, three rows of roof bolts were installed as primary and secondary breaker lines support. On the basis of the observations of instrumented bolts, only two rows of roof bolts were used as secondary RBBLS (Ram, et al., 2014). Now, most of the MD operations in India are using only two rows of bolts as RBBLS (Table 1). However, the strata mechanics studies at different MD operations showed interesting characteristics resulting from this support (Ram, et al., 2015)."

Jan 1, 2016

By Ellsworth R. Spencer

A lightweight fiberglass feed leg for hand-held pneumatic percussion rock drills has been fabricated and tested by the Bureau of Mines. Its lighter weight facilitates easier handling of the rock drill apparatus, thereby reducing the potential for back injury to the driller and in- creasing drilling productivity. Current hand-held feed leg drills of the same class are 50 pct heavier than the Bureau-devised feed leg drill, which is comprised of a reduced-noise drill and the fiberglass feed leg. In-mine tests of the fiberglass leg showed that its performance and cost are comparable to those of standard aluminum feed legs.

Jan 1, 1985

By M. C. Malamphy

A general description of the activities and results of bauxite investigation by the Bureau of Mines at its bauxite project in Saline and Pulaski County, Ark., has been given in Report of Investigations 4251. The factual data obtained during the project are reported in a series of Reports of Investigations beginning with No. 4251, of which this is the eighth. The data are accompanied by maps showing the location of holes drilled and the deposits developed. Each area upon which work was done is reported by half townships. Each bauxite deposit investigated was assigned a name and a number for ready reference and identification, and its location and name are shown on the appropriate half-township map. The description of each half township is no followed by a description of each deposit developed in that half township. The 14 half township maps and 77 detail maps of the bauxite deposits in this series of reports give the locations and numbers of all the holes drilled on the project, except the deep holes drilled to test the geophysical anomalies. The locations at those holes show on figure 13 in volume I. The descriptions of the deposits developed are followed by complete detailed logs at the drill holes. Many at the widely spaced exploratory holes did not discover bauxite of minable thickness and gra.de. The pertinent information obtained from the widely spaced exploratory drill holes has been summarized and tabulated, and a table for each halt township is given with the discussion covering that area.

Jan 1, 1948

By Y L. Ma, Y Yang, M Chen, W Bruckard

To improve the understanding of the reactions and mechanisms occurring during the leaching of sulfide ores at high temperatures a range of advanced characterisation and sensing tools have been combined to provide a sophisticated and powerful methodology to examine sulfide leaching systems. These include advanced electrochemical methods, surface chemistry and materials characterisation techniques such as synchrotron X-Ray Absorption Spectroscopy (XAS), X-Ray Photoelectron Spectroscopy (XPS), Scanning Electrochemical Microscopy (SECM), and in situ X-ray diffraction (XRD), together with new robust solid state chemical sensors for in situ real time monitoring of key aqueous chemical parameters. The methodology was employed to investigate various sulfide mineral leaching processes. For example, oxidation of arsenopyrite at elevated temperature involves complicated multiple reactions and the process is strongly influenced by the solution conditions, component speciation and mineralogy. The methodology was used to study this system both ex situ and in situ to gain a detailed understanding of the complex chemical reaction mechanisms operating. These mechanisms are discussed in terms of the observed leaching efficiency. The application of this methodology enables complex sulfide leaching systems to be understood more fully such that process efficiency can be improved.

Aug 24, 2022

By Earl F. Hanson

Fires in heavily timbered mines are disastrous, involving danger to both life and property. Some mines have been completely ruined or so heavily damaged that reopening them would not pay. Though few mines are entirely free from danger of fire, the risk is minimized by proper care and good design of plant. The Tintic Standard mine is at Dividend, Utah, in the famous Tintic mining district, about 60 miles south of Salt Lake City. The development of the mine was begun in 1907 by the late Mr. E. J. Raddatz and his associates. From the beginning, the work was hampered by high rock temperatures and the presence of high concentrations of rock gases such as carbon dioxide and nitrogen. Development work was carried on with great perseverance for nine years, and resulted in the discovery of ore in 1916. The total production of the Tintic Standard mine to Jan. 1, 1936, amounted to 1,664,388 tons of ore, having a gross value of $61,996,719. General Layout of the Mine The No. 2 shaft, which is the main working shaft of the Tintic Standard, is within the main orebody and is connected with the five other shafts. Their respective positions with respect to the No. 2 shaft are as follows: North Lily, 2770 ft. northwest with drift connections on the 700 and 900-ft. levels; No. 3 shaft, 670 ft. east connected through the 700-ft. level; Eureka Standard, 4550 ft. south, connected on the 900-ft. level; No. 1 shaft, 1470 ft. southwest, with connecting drifts on the 900 and 1250-ft. levels; Eureka Lilly, 2000 ft. southwest, with connecting drift and raise through the 1250-ft. level. The Tintic Standard orebody consists essentially of one continuous oreshoot extending from the 600-ft. level to the 1450-ft. level, with a cross-sectional area of approximately 70,000 sq. ft. at both top and bottom, reaching a maximum area of 215,000 sq. ft. between the 1100

Jan 1, 1937

By E. J. Peuraniemi

Oxidation of chalcopyrite concentrate and two low-iron copper mattes were studied using a laboratory scale laminar-flow furnace simulating the phenomena taking place in different zones of the reaction shaft of a flash smelting furnace. In the experiments, screened fractions were fed into the furnace and sampled after short reaction time intervals by quenching them into a water film. Experimental conditions included temperatures of 1100 and 1300°C with reaction gas oxygen contents from 21 to 75 vol.%. Samples were analysed chemically for Cu, Fe and S to define removal rate of sulphur. Optical and scanning electron microscopy with EDS-analyser were used to examine the samples. In this paper, oxidation kinetics as well as ignition of particles are discussed. Changes in particle morphology, size, and composition are viewed to closely define the proceeding of the oxidation, and, consequently, to compose a detailed model of dust formation and reaction mechanisms. Data obtained in the experiments broadens the knowledge of physical and chemical phenomena in flash reactions and serves as reference for computer simulations.

Jan 1, 2000

By R. E. Siemens

The Bureau of Mines sought to correlate the variation of structure-sensitive superconducting properties with microstructure in selected Cb-Hf alloys and to compare the experimental results with those predicted by the GLAG theory. Alloys in wire and rod form were evaluated by critical temperature, critical current, magnetization, resistivity measurements, and optical and electron microscopy. In the absence of an external magnetic field, the current carrying capacity of columbium was greatly reduced with addition of up to 85 wt pct Hf, but a large increase in Ic occurred for Cb-90 wt pct Hf. Favorable Ic-H behavior was observed in cold-drawn alloys containing 25 and 57 wt pct Hf. Correspondingly, a maximum in Tc occurred at 10-25 and 90 wt pct Hf. Four- or five-hour heat treatment at 600° C resulted in maximum Ic values and maximum hysteresis in magnetization. Dislocation pileup, polygonization, and fine precipitates, responsible for flux pinning, are listed in order of their effectiveness as pinning sites. Sites having an average separation of 1,500 to 3,000 A and a diameter of 1,000 A or less were most effective in influencing Ic-H and M-H behavior. The resistive critical fields increased smoothly to a maximum of 80 k0e between 60 and 65 wt pct Hf. Highfield, mixed state, reversible paramagnetism was observed in some alloys; however, the GLAG theory was in good agreement with experimental results for the majority of the composition range studied.

Jan 1, 1969

By Kenneth C. G. Heath

The paper point out the economics importance of the Torco process as lubricant and fuels of the motor in the mining. It is possible to envisage an arrangement in which TORCO would be used to treat a sulphide ore, the acid used to dissolve the metallic ccoper in the concentrate and the copper produced in cathode form by electrowinning. However, there are studies point out that it would be as profitable as conventional flotation, smelting and refining. To carry out full testing of the TORCO process on anyore would be expensive, involving sending several hundred tons to one of the pilot plants located in Johann esburg or Milan. Such pilot plant testing should & be considered as confirmatory rather than exploratory, and a good economic case for using theTORCO process would have to be made out based of mallet scale testing before in curring the larger expense.

Nov 20, 1969

By John A. Breslin

Size distributions and concentrations of particulates emitted from diesel engine exhausts were measured with cascade impactors. Samples were taken from the exhaust of two types of engines using three types of fuel and operating under five different engine speed and load conditions. The measured mass median diameters of the diesel particulates were typically about 0.3 um. There was no significant difference in mass median diameter between engines or fuels and only a slight dependence on operating mode. Concentration measurements ranged from 14.2 to 250.9 mg/cu m, and calculated mass outputs, from 64 to 10,000 mg/min. Significant differences in mass output were found between engines, fuels, and especially between different operating modes. The quantity of clean dilution air that would be required to reduce the particulate mass concentration below the 2.0 mg/cu m respirable dust standard for coal mines was greater than the dilution air required to meet the standards for noxious gases for both engines tested.

Jan 1, 1976

By John A. Breslin

Size distributions and concentrations of particulates emitted from diesel engine exhausts were measured with cascade impactors. Samples were taken from the exhaust of two types of engines using three types of fuel and operating under five different engine speed and load conditions. The measured mass median diameters of the diesel particulates were typically about 0.3 um. There was no significant difference in mass median diameter between engines or fuels and only a slight dependence on operating mode. Concentration measurements ranged from 14.2 to 250.9 mg/cu m, and calculated mass outputs, from 52 to 3,443 mg/min. Significant differences in mass output were found between engines, fuels, and especially between different operating modes. The quantity of clean dilution air that would be required to reduce the particulate mass concentration below the 2.0 mg/cu m respirable dust standard for coal mines was greater than the dilution air required to meet the standards for noxious gases for both engines tested.

Jan 1, 1976

By E. T. Hayes, A. H. Roberson, M. H. Davies

ZIRCONIUM has been produced on a pilot-plant scale for only a few years, but the potential uses have led a large number of research establishments to engage in a thorough study of the metal and its alloys. The work described in this paper is part of a cooperative project between the Bureau of Mines and the Air Materiel Command. The Zr-Cr system was one of the first investigated because of the possibilities of improving the properties at elevated temperatures, the chemical corrosion resistance, and the mechanical properties of zirconium in a manner similar to the enhancement of the properties of titanium by additions of chromium. There is no published work on the Zr-Cr system but from the similarity of the metals involved it was expected that it would be similar to the Zr-Fe' and Ti-Cr' systems. The materials used in this investigation were prepared in the Bureau of Mines laboratory at Albany, Ore. Zirconium was produced by magnesium reduction of zirconium tetrachloride, and a typical analysis is as follows: Fe, 0.06 pct; Ox, 0.08; N?, 0.01; C, 0.02; and other impurities such as Al, Pb, Ni, Ti, and Si less than 0.01 pct each. High purity chromium was prepared by treating crushed electrolytic chromium in a stream of dried and purified hydrogen." The resulting powder contained about 0.01 pct 0 and about 0.1 pct total metallic impurities. All alloys were prepared by arc-melting 50 g briquetted compacts of the desired composition in a Kroll-type" arc furnace using an inert atmosphere. The furnace was evacuated twice and backfilled with helium, which was gettered by melting a center zirconium button immediately before the alloys were melted. Alloys were remelted at least once to insure greater uniformity of composition and subsequently were annealed in vacuum at 1250°C for 48 hr. Fairly homogeneous alloys were obtained by this means; a slight loss of chromium from the surface by evaporation during the high temperature homogenization was noted. All alloys were analyzed for chromium and gave results in good agreement with the nominal composition. Spot checks on tungsten and nitrogen showed pick-up of these elements to be negligible. Over 70 alloys were prepared for use in this investigation; only the critical ones are shown in Table I. Alloys containing up to 10 pct Cr were amenable to hot working at 850°C and a number of these were sheath rolled to 1/16 in. thickness. Specimens were cut from the sheet for use as metallographic samples. For the thermal analysis a differential couple was used in conjunction with an X-Y recorder, the temperature of the specimen and the difference in ternperature between it and the standard nickel body were recorded simultaneously. Heating and cooling rates of 5°C per min were used. The sensitivity of the instrument was such that a difference in temperature between the specimen and standard equivalent to 0.1 mv produced a deflection of 1 in. on the recording chart. The chromel-alumel thermocouples were checked against a Bureau of Standards calibrated thermocouple. Melting-point determinations were made in a high vacuum induction furnace using an optical pyrometer. The pyrometer, calibrated against nickel, copper, and zirconium (iodide process) under near black body conditions, was focused on the base of a hole drilled in cylindrical samples. A North American Philips Geiger counter X-ray spectrometer was used for all diffraction studies. This instrument, in addition to supplying precise intensity measurements of planar reflections, has an added advantage in that metallographic specimens mounted in bakelite can be used directly, and this

Jan 1, 1953