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By V. Runolinna, R. T. Hukki

Preliminary separation of precious metals by flotation can offer a simplification of the conventional method of treatment of anode slimes. Laboratory flotation experiments show that rich gold and silver concentrate can be obtained with excellent recoveries. THE purpose of this paper is to present the results of an investigation into the possibilities of separating precious metals from anode slimes by selective flotation. The work was carried out at the State Research Institute in Helsinki, Finland. The sample of anode slimes tested was submitted by the Outo-kumpu Co. in Finland. In 1947 the average assay of filtered and dried anode slimes in the Outokumpu refinery in Pori was as follows: Au, 0.50 pct; Ag, 9.38 pct; Cu, 11.02 pct; Ni, 45.21 pct; Pb, 2.62 pct; Fe, 0.60 pct; Sn, 1.00 pct; Sb, 0.04 pct; As, 0.70 pct; Se, 4.33 pct; S, 2.32 pct; SO,, 2.17 pct; SiO2, 2.25 pct. The daily assay naturally varies considerably from the figures presented above. The present conventional method of treatment of anode slimes consists of the steps shown in the flowsheet in fig. 1. As seen from this simplified flowsheet, the present method of treatment involves many steps by which the components of the anode slimes are removed one after another until the main products, gold and silver, may be separated. Due to the small scale of operations, the above procedure is carried out in small batches requiring considerable amount of manual labor. If, however, the anode slimes could be treated in

Jan 1, 1951

By H. B. Probst

Mechanical twins were produced in zone-refined tungsten single crystals by explosive working at room temperature. These twins are parallel to (112) planes and have irregular boundaries rather than the classical plane twin boundaries. These boundaries aye grooved surfaces in which the grooves themselves are parallel to a <111> direction and the sides of the grooves appear to be par-allel to (110) planes. TWINS were produced in tungsten single crystals by explosive working at room temperature. These twins differ in character from any previously reported for tungsten; however, they are similar to those found in molybdenum after compression at -196°C.1 Deformation twins "resembling Neumann bands in ingot iron" have been observed in tungsten by Bech-told and Shewmon.2 This observation was made with sintered polycrystalline tungsten pulled in tension to fracture at 100°C and using a strain rate of 2.8 x 10-4 sec-1. More recently Schadler3 found deformation twins in zone-refined tungsten single crystals pulled in tension at -196"&apos; and -253°C. These tests were conducted using a strain rate of 3.3 x l0-4 sec-1, and the twin bands were found to be parallel to a (112) plane. Deformation twins in tungsten&apos;s sister metal, molybdenum, were observed by Cahn.4 These twins were produced by compressing small (0.7 mm) vapor-deproducedposited molybdenum single crystals at -183°C. The compression was performed &apos;by impact." By the use of precession X-ray techniques, Cahn was able to identify the twin plane as {112} and the shear direction as <1ll>. Mueller and Parker1 produced deformation twins in polycrystalline electron-beam-melted molybdenum by compression at -196°C. Their "loading rate" was 5000 psi per min which, judging from their stress-strain curve, corresponds to a strain rate of approximately 0.3 x 10-4 sec-1. These twin bands were found to be parallel to (1 12) planes; however, they differed in appearance from previously observed twins. In place of straight and parallel twin boundaries they were found to be irregular, jagged, and sawtoothed. The sides of the saw teeth were identified as (110) planes and irrational planes of a (111) zone. The twins observed in the present work in tungsten single crystals are similar in appearance to those of Mueller and Parker in polycrystalline molybdenum. The starting material used in this investigation was 3/16-in. diam commercial tungsten rod produced by powder-metallurgy techniques. This material was converted to a single crystal by the electron-bombardment floating-zone technique.= The process was carried out in a vacuum of 10-5 mm of Hg using a traversing speed of 4 mm per min. Segments (=2 in. long and 3/16 in. in diam) of two crystals (A and B) produced in this manner were studied. Crystal A received one zoning pass, while crystal B received two passes. The two crystals were explosively worked at Bat-telle Memorial Institute in the following manner. A 1/2-in.-thick layer of plastic was applied to the crystals to serve as a buffer in an attempt to prevent cracking. The composite, crystal and buffer, was then wrapped with 1/8-in.-thick DuPont sheet explosive EL506A2 and detonated in water at room temperature. Metallographic samples of the worked crystals were prepared, and back-reflection Laue X-ray patterns were obtained using unfiltered molybdenum radiation. RESULTS AND DISCUSSION Blasting the crystals as described above failed to prevent cracking. The crystals fractured into several fragments about 3/16 to 1/2 in. long; however, the fragments were of sufficient size to be useful for the subsequent study. The diamond pyramid hardness of the crystals after blasting was in the range 430 to 450 as compared with 340 for the as-melted material, which shows a definite hardening resulting from plastic deformation. These hardness values were obtained using a 1000-g load and taking readings only in sound portions of the crystals free of cracks. The crystals exhibited profuse twinning as shown in Fig. 1. No such structure is present in the as-melted condition. Most of these twins have jagged twin boundaries and are similar in appearance to those found in molybdenum by Mueller and Parker. The twins in both crystals were found to be parallel to {112} planes. This identification was made by using the conventional two-trace method. Subsequent efforts to describe these twins more fully were carried out on crystal A. If the longitudinal axis of crystal A is placed in the (001)-(011)-(Il l) basic triangle of the standard cubic stereographic projection, as in Fig. 2, then the two sets of twins shown in Fig. 1 are parallel to the (112) and (121) planes. Fig. 3 shows a schematic representation of a twin with jagged boundaries. This type of twin with a <111>

Jan 1, 1962

By B. H. Caudle, A. B. Dyes

In a recent publication&apos; it was shown that wells with a free surface in a homogeneous gravity-drainage reservoir have a hyperbolic decline with index n &apos;. This paper reports efforts to extend this theory to practical field cases. As a first step in making the extension, a large number of lease production curves from gravity-drainage fields in the stripper stage were fitted with the general hyperbolic decline equation, q/q, = 1/(1 + y) y and n in each case being determined by statistical methods. It was found that this equation is reliable for decline curve extrapolation for periods up to at least 25 years. The resrilts obtained were disturbing in the sense that values for the index, n, were often smaller than one, which fact leads to the prediction that a well would produce all infinite amount of oil in infinite time. A theoretical investigation based on the results of the previous paper provides a suitable explanation for these low values of n. It suggests that these are obtained if production occurs from two or more layers of diflerent permeabilitv and thicktress or two lnyers having different skin effects. It is predicted that as the more permeable layers are exhausted, the index of decline, n, will rise from a value smaller than 2, to n = 2. A practical method is given for fitting the general hyperbolic decline Eq. 6 to production decline data. When this method is used, the index of decline observed in gravity-drainage reservoirs in the stripper stage when wing only data over early years 01 decline usually agrees quite closely with that determined using data over 25 years or more. This indicates that the hyperbolic decline equation is reliable for predicting behavior of such reservoirs. A method is also suggested for taking into account any changes in the value of the index INTRODUCTION As a result of both experimental work with models and theoretical deductions, it was recently concluded&apos; that wells having a free surface in a homogeneous reservoir producing by pure gravity drainage should have a hyperbolic decline with n = 2. The present report details efforts to extend this work on ideal homogeneous reservoirs to actual field cases. It should be remembered that both the previous work and the present extension are based on the assumption that the reservoir is at very low pressure, and hence, nearly all the potential available for driving fluid to the well is the gravity head. Attempts to apply conclusions of this study to reservoirs which have considerable pressures supplementing the gravity drive may lead to difficulty. WELLS WITH NO FREE SURFACE In a dipping gravity-drainage reservoir such as that shown in Fig. 1, some of the down-dip wells have no free surface. The previous study&apos; showed that the up-dip wells, which have a free surface, should follow Eq. 1. The following approximate analysis, of a type which was justified experimentally for up-dip wells in the work just mentioned, leads to results for the down-dip wells.

By David Mitchell

THE production of fluorspar is one of the smaller nonmetallic indus-tries in the United, States with a capital investment-about $10,000,000. Shipments from United States mines1 in 1936 totaled 176,231 short tons valued at $3,111,268, an average price of $17.65 per ton. The United States produces about 40 per cent of the world&apos;s fluorspar, of which about 90 per cent comes from the Illinois and Kentucky deposits along the Ohio River.2 Further detailed information on the fluorspar industry in the United States is given by Hatmaker and Davis.28 Fluorspar is marketed according to the following relative quantities and specifications: Consump- Specifications, Per Cent Use Form tion in 1936, Per Cent CaF2 SiO2 Fe2O3 Metallurgical Gravel 79 +85 -5 or lump Ceramic.. Ground 10 +95 -3 -0.1 Acid Ground 11 +98 -1 The concentration of the coarser sizes presents relatively little diffi-culty, good recoveries being obtained with jigs and tables. However, sizes smaller than about 10 mesh cannot be successfully treated by ordinary gravity separation methods and so have been accumulating as

Jan 1, 1938

By Garth M. Crosby, F. McIntosh Galbraith, Bronson Stringham

THE Hercules mine is located in the northeastern section of the Coeur d&apos;Alene district, approximately 1 1/2 miles north of the town of Burke, Idaho. Surface indications of the ore deposit were first discovered in 1886, but regular mine production was not started until 1902 and was continuous until April 1925, when the known ore had been extracted. Incomplete records show that from 1912 until operations were suspended the mine produced 2 1/2 million tons of ore containing 9.4 pct lead and 7.7 oz of silver per ton, together with an estimated 2 pct zinc, 0.3 pct copper, and 20 pct iron. This operation was the first in a series of mining enterprises culminating in October 1947 with the consolidation of Day Mines, Inc. In the same year it was decided to unwater the levels below the collar of the Hercules shaft in the hope of finding some indication of a recurrence of ore. The unwatering operation has been described in a previous paper.1 The initial exploration, following recapture of the workings, showed sufficient promise to warrant a detailed study of the mineralogy with modern techniques.

Jan 12, 1953

By David Mitchell

THE production of fluorspar is one of the smaller nonmetallic indus-tries in the United States with a capital investment-about $10,000,000. Shipments from United States mines&apos; in 1936 totaled 176,231 short tons valued at $3,111,268, an average price of $17.65 per ton. The United States produces about 40 per cent of the world&apos;s fluorspar, of which about 90 per cent comes from the Illinois and Kentucky deposits along the Ohio River.2 Further detailed information on the fluorspar industry in the United States is given by Hatmaker and Davis.28 Fluorspar is marketed according to the following relative quantities and specifications: Consump- Specifications, Per Cent Use Form tion in 1936, Per Cent CaF2 SiO2 Fe2O3 Metallurgical Gravel 79 +85 -5 or lump Ceramic,. Ground 10 +95 -3 -0,1 Acid Ground 11 +98 -1 The concentration of the coarser sizes presents relatively little diffi-culty, good recoveries being obtained with jigs and tables. However, sizes smaller than about 10 mesh cannot be successfully treated by ordinary gravity separation methods and so have been accumulating as

Jan 1, 1938

By Wilbur Jurden

THE writer&apos;s first experience with a nonferrous reduction plant of great magnitude was at the Washoe reduction works of Anaconda some 35 years ago. Here was a plant which had been planned with remarkable skill and foresight considering the time and the state of development of copper-plant practice in the year 1902. The designer utilized topography to fullest extent to provide proper sequence of operations and, what is most remarkable, to leave adequate space for future developments, most of which at that time were unknown. However, the practice then was to locate the various units of the reduction works at the most advantageous points of the existing terrain with little regard for tramming or other auxiliaries and then connect these various units by the essential trackage, conveyor systems, piping, etc., as the need developed. This occasionally led to undesirable track arrangements, sharp curves, and steep grades, especially when it became necessary to extend various portions of the plant. Conveyor systems also became rather complicated, running as they did at various angles, and such items as piping and electrical distribution were often found to be in the wrong place, entirely inadequate in size, or awkwardly arranged for any kind of extension. This condition was not peculiar to Anaconda, for all copper plants at that time were built in the same manner and it was the constant association with these difficulties which, in the year 1925, influenced the layout of the Andes Copper Mining Co. plant. In that plant all trackage was laid out straight and level, all conveyors at right angles to each other with minimum length and number of transfers. All buildings were placed parallel and the main structures were complete for all purposes so that auxiliary buildings and dog houses would not be added later. Piping and electrical work was provided for in the original layout and carefully designed to avoid additions and alterations, and careful study given to every movement of material throughout the entire plant so that it would be accomplished with the least possible effort. Naturally it was hardly expected to attain all these objectives perfectly but our efforts did succeed in creating a plant which was unique and outstanding for its time-1927. It was also most gratifying to find that these design principles contributed to considerable savings starting right in the drafting room, carrying through the construction and ultimately yielding savings in operations and manpower. Not only that, but such a plant gives the observer an impression of symmetry and order, is more attractive to the workmen, and unquestionably eliminates many accident hazards. However, the Andes plant buildings were fitted to the existing terrain instead of having terrain created to fit the buildings-an item which we found advantageous to correct on the next large plant. At Morenci in 1939, all of the desirable features of the Andes plant such as parallel buildings, etc., were incorporated; but we went one step further-power shovels were brought in to make the terrain fit the reduction works. The result at Morenci is well-known and needs no elaboration here, but the success achieved by the design methods used for this and previous plants naturally influenced and guided the layout of the Chuquicamata sulphide plant which is the largest yet conceived. Chuquicamata Plant Design At Chuquicamata several factors not encountered previously complicated the problem to a great extent. The most desirable location for the smelter would allow smelter gases to blow directly into the open-pit mine already producing 60,000 tons of oxide ore per day and employing 1550 men. This, of course, would be a serious condition and, therefore, we were forced to move the smelter to a less desirable location but followed our previous experience at Morenci and made the terrain fit the job. The most difficult problem, however, was the provision for receiving various types of ore both by rail and conveyor. These consisted of: 1-Sulphide-bearing residue from the stockpile from which oxide copper had previously been leached. 2-Sulphide-bearing residue coming direct from the leaching vats. 3-Sulphide ore crushed at the existing crushing plants and hauled to the concentrator in cars. 4-Sulphide ore from the new crushing plant adjacent to the concentrator. 5-Sulphide ore obtained

Jan 1, 1952

By W. C. Leslie

The textures of cold-rolled and of annealed iron are compared with those of an iron-0.8 pct copper alloy in which the amount of precipitation after cold rolling was controlled. Previously published pole figures -for cold-rolled and for annealed iron are confirmed. The effects of precipztatiotz after cold rolling are to retain the cold-rolled texture after annealing, to inhibit the formation of the usual allnealing texture, and to produce elongated recrys-tallized ferrite grains. It is suggested that the inhibition of new textures by precipitation after cold rolling is a general phenomenon. A great deal of attention has been paid to the development of texture during the secondary or tertiary recrystallization of ferritic alloys, but very little work seems to have been done on the control of texture during primary recrystallization. If such control were attained, it might be possible to simplify the processing of oriented materials or to change the characteristics of current cold-rolled and an-nealed products. From previous experience, it seemed likely that texture could be controlled by recrystallizing a supersaturated solid solution. Green, Liebmann, and Yoshidal found that the formation of preferred orientation in aluminum (40 deg rotation about <111> relative to the deformed matrix) was inhibited when iron was retained in supersaturated solid solution in the strained aluminum. The authors attributed this inhibition to iron atoms in solid solution. There is, however, an alternative explanation. Green et al, took a highly supersaturated solution of iron in strained aluminum and heated it to an unspecified temperature for recrystallization. It is probable that precipitation occurred prior to and during recrystallization, and it is proposed that the inhibiting agent is this precipitate, rather than the iron atoms in solid solution. It is important to note that precipitation before cold work is ineffective; the effective precipitate is that formed after cold working and either before or during recrystallization. The location and distribution of the precipitate are critical. Precipitation in such a manner has been found to have profound effects upon kinetics of recrystallization and the microstruc-ture of the recrystallized alloys.2-4 It would be surprising, indeed, if this were accomplished with no change in texture. Because of the relative simplicity of the system, and because of previous experience,4-7 it was decided to determine the effect of precipitation on texture in an alloy of iron and copper. Bush and Lindsay5 found an unspecified change in texture in cold-rolled and annealed low-carbon rimmed steel sheets when the copper content exceeded 0.1 pct. MATERIALS In earlier work, the rate of recrystallization of a low-carbon steel was greatly decreased by 0.80 pct copper, and, after the proper treatment, the recrystallized ferrite grains were greatly elongated.4 Accordingly, it was decided to investigate the effect of precipitation on texture at this level of copper content. The iron and the iron-copper alloy were made from high-quality electrolytic iron and OFHC copper, vacuum-melted in MgO crucibles, cast, hot-rolled to 0.2 in., then machined to 0.150 in. The compositions are given in Table I. The plates were heated to 925°C and brine quenched, twice. This produced a ferrite grain size of ASTM 0 in the iron and ASTM 1 in the Fe-Cu alloy. Disk specimens were cut from the heat-treated plates, repeatedly polished and etched, then used to determine (110) and (200) pole figures by reflection. Despite the complication of large grain size, these pole figures strongly indicated a random texture. PROCEDURES The copper content in solid solution in ferrite before cold rolling and recrystallization, and hence, the amount that could precipitate during the recrys-tallization anneal, was controlled at three levels by heat treatment. The specimens as quenched from 925° C were presumed to have all the copper, 0.80 pct, in solid solution. Other samples of the quenched alloy were aged 5 hr at 700°C to retain about 0.5 pct Cu in solid solution.6 A third set of quenched specimens was reheated to 700°C, then slowly cooled in steps, to reduce the amount of copper in solid solution to a very low level. All specimens were cold-rolled 90 pct, from 0.150 to 0.015 in. thick. The rolling was done in one direction only, i.e., the strip was not reversed between passes, with a jig on the table of the mill to keep the short specimens at 90 deg to the rolls. The rolls were 5 in. in diameter and speed was 35 ft. per min. Machine oil was used as a lubricant. In a supersaturated alloy, the maximum effect of the copper precipitate on microstructure and on recrystallization can be developed by a treatment at 500°C, after cold rolling and before recrystallization.&apos;

Jan 1, 1962

By E. A. Ernst, N. F. Carpenter

The benefits derived from an acidizing treatment are a function of the penetration achieved by the acid before complete spending. Additional penetration may be achieved by (1) controlling acid leak-08 into formation pores in the channel faces, and (2) retarding the reaction rate of the acid. A recently developed chemical additive consists of a synthetic polymeric material which absorbs hydrochloric-acid solutions, when suspended therein, swelling up to 40 times its original volume. These swollen particles have the ability to deform and seal-08 formation pores, providing fluid-loss control. In addition, they provide a diffusion barrier between the fracture face and the acid solution, prolonging the spending time of the acid. Field applications of this new technique have shown promising results. A method of conducting acid fluid-loss tests, using carbonate cores, is believed to provide fluid-loss data that are more representative of formation conditions than the conventional filter-paper determinations. INTRODUCTION The concept of oilwell acidizing has changed since its first commercial application, 30 years ago. Originally, it was visualized that the acid penetrated thousands of tiny pores and flow channels in the matrix rock, enlarging them by dissolving the carbonate walls. The resultant permeability increase was assumed to be the responsible factor in increasing production from the well. Recent laboratory studies,&apos; however, have shown that this does not provide the complete picture. Although this type of individual pore penetration by the acid does take place during acid "soaks", designed to overcome "skin effect" due to mud invasion in the immediate vicinity of the wellbore, many years of experience have shown that considerable pressure is required to attain any appreciable injection rate into the fine capillary pores of the rock. During most acidizing treatments, the bottom-hole pressure build-up due to the restriction of flow into the formation exceeds the "breakdown" pressure of the rock so that a fracture is induced. In most cases, such fractures open up along natural, incipient fissures and zones of weakness in the rock and, therefore, tend to follow the natural stress pattern of the rock—whether it be horizontal, vertical or inclined. Because of the comparatively greater permeability of the channel in relation to that of the matrix, the bulk of the acid volume is diverted into the newly opened fracture. Here it quickly penetrates the formation, opening and ex- tending the fracture in much the same manner as a conventional fracturing fluid. Unlike the fracturing fluid, however, most acidizing solutions contain no propping agent; thus, the open fracture will again close when the injection pressure is relieved. Laboratory studies2 have shown that in many cases the etching of the fracture faces, resulting from the reaction between the acidizing solution and the carbonate rock, is nonuniform due to the heterogeneity of the rock structure. As a result, the two fracture faces no longer match when pressure is released, and support pillars and intermediate voids remain, forming a high-conductivity channel for well fluids. Unfortunately, this is not true over the entire area of the fracture, but only over that portion of the fracture where the rock has been partially dissolved by the acid. The acid solution spends as its travels away from the wellbore; once it has completely spent, even though it may provide additional mechanical fracture extension, no additional benefit due to etching of fracture faces can be expected. Studies of acid reaction rates under formation conditions,3 observing the effect of different variables upon spending time, have shown that the reaction was often so rapid that very little penetration of the formation occurred before the acid was spent. Study was undertaken to devise methods of increasing the penetration of the acid before spending, so as to provide greater benefit from the acidizing treatment by etching a greater portion of the fracture faces. Several techniques were devised to accomplish this purpose. First, chemical additives were developed which were designed to retard the reaction rate of the acid, causing it to penetrate a greater distance from the wellbore before finally becoming spent. Another method was to increase the injection rate of the acid. However, it was found that the resultant increased shear tended to accelerate the reaction rate of the acid, partially offsetting the benefits of the higher injection rate insofar as achieving increased penetration before spending was concerned.&apos; Another approach to the problem of achieving increased penetration was the development of fluid-loss additives for acid solutions, which would minimize the volume of acid lost into formation pores in the fracture faces and provide maximum fracture extension for the volume of acid injected during the treatment. The use of fluid-loss additives is now considered the most effective method of providing maximum fracturing-fluid efficiency.~ Unfortunately, this latter technique does not solve the problem of rapid reaction rate, with consequent limitation of the fracture area benefited by reaction with unspent acid. A newly developed acid additive overcomes many of these limitations by providing the dual benefits of fluid-loss control and mechanical retardation of acid reaction

By E. V. Daveler

The milling plant of the Alaska-Gastineau Mining Co. is located at the town of Thane, Alaska, on Gastineau Channel, 4 mi. south of Juneau and directly across the channel from the Ready Bullion mine of the Treadwell mines on Douglas Island. Previous to the organization of the Alaska-Gastineau Mining Co., in 1912, the milling was done at the stamp mill of the Alaska Perseverance Co. located at the mine in Silver Bow Basin. But the contemplated increase in production made it necessary to locate the mill on Gastineau Channel, as not enough water was available at the mine during the winter months, nor was there room for taking care of the large tonnage of tailings that would ultimately be discarded from the mill. Character of Ore The gold and silver values occur in quartz lenses associated with pyrrhotite, galena, arsenical pyrites, and zinc blende. These lenses occur in large bodies of slate, schist, and metagabbro, which also carry some valuable metallic contents. With the essential low cost of mining, it was necessary to mine large bodies of low-grade material containing the high-grade streaks. Of the minerals, pyrrhotite, the magnetic sulfide of iron, is predominant, and galena is the next sulfide present in quantity. The gold occurs free and coarse and associated with the iron sulfide in its finer state. The silver occurs with the lead or is alloyed with the gold. A chemical analysis of the ore shows Silver............ 0.10 oz. Magnesia......... 0.4 per cent. Silica............. 59.7percent. Sulfur............ 1.2 per cent. Iron.............. 5.2 per cent. Lead............. 0.1 per cent. Alumina.......... 21.4percent. Zinc............. 0.2percent.. Lime............. 5.0 per cent. Experimental Work Investigations at the old Perseverance stamp mill had developed the following points: Roughing concentration following stamping gives a fair recovery.

Jan 1, 1920

By Edwin C. Holden

In making the original estimates for a report recommending the cyanidation of Ymir stamp-mill tailings, the writer was unable to find in any of the standard works on cyanide-practice certain data applicable to the local conditions; nor has he as yet seen quite the same practice recorded in the rapidly growing literature of cyanidation. To present these figures, together with a few novel features of local practice, the present paper is offered. The ore treated is obtained from a fissure-vein of steep dip, occurring in a slate country. The ore-body is lenticular in plan, swelling from 4 ft. in width at one end to a maximum of 42 ft., and tapering irregularly to less than 18 in., where payvalues cease. In the wider portions of the fissure the ore is mixed with more or less horse-matter from the walls. The clean ore is white, massive quartz, with from 8 to 12 per cent of sulphurets; the latter being pyrite, sphalerite and galena, the predominance being in the order given. The precious metal tenor is variable, the gold more closely following the pyrite, the silver the galena. The present mill-supply is practically all from below the oxidized zone. The unavoidable admixture of horse-matter and stope-filling with the ore as mined, affects more or less the character of the mill-feed, which sometimes contains from 10 to 25 per cent of slate. During the last three months of 1902, the mill-feed carried 0.3977 oz. gold and 1.903 oz. silver per ton of 2,000 lb., 2.65 per cent lead and 2.92 per cent zinc. The iron, unfortunately, was not determined. The Ymir mill and mine have been fully described elsewhere;* suffice it to say of the milling that the crushed ore,

Jan 1, 1904

By A. Steiner, E. Miller, K. L. Komarek

Equations have been derived to calculate the chemical potentials of the components of liquid binary alloys from liquidus and enthalpy data. The equations are applicable to systems with intermetal-lic compounds of limited solid solubility. The liquidus curve of the Mg-Sn system was accurately redetermined, and the melting point of the compound Mg2Sn was found to be 770.5° * 0.3°C. The thermo-dynamic properties of the liquid alloys were calcu -lated from the liquidus data. The activity of tin shows both positive and negative deviations from Raoult&apos;s law and the relative integral entropy is positive. THE phase boundaries in an equilibrium phase diagram are functions of the thermodynamic properties of the coexisting phases. Specifically, the shape of the liquidus curve near an intermediate compound is determined by the properties of the compound and the liquid phase. Hauffe and wagnerl have derived an equation for the chemical potential differences (ui) of the liquid alloys near the congruent melting point when the heat of fusion of the compound and the liquidus curve are known. In their derivation the temperature dependence of the ui value was neglected, and liquid of stoichio-metric composition was chosen as the reference state. To obtain chemical potentials over the ntire composition range of the phase diagram with the pure components as the reference state, equations have been derived which incorporate the temperature dependence of the chemical potentials. Such a thermodynamic analysis can be carried out when the liquidus curve and the enthalpy values are known. The equations have been applied to the redetermined liquidus curve of the Mg-Sn system to obtain the thermodynamic properties of liquid Mg-Sn alloys. The Mg-Sn phase diagram has been studied by various investigators and the results have been compiled and critically assessed by Hansen.2 Preliminary thermal analyses showed that the basic features of the diagram were correct. The system has one congruent melting compound, Mg2Sn, two eutectics, and some solid solubility of tin in magnesium. However, the published liquidus temperatures show considerable scatter. In order to perform an accurate thermodynamic analysis, the liquidus curve between the magnesium-rich and tin-rich eutectic compositions was therefore redetermined by careful thermal analysis using highest-purity starting materials. EXPERIMENTAL PROCEDURE The magnesium metal (Dominion Magnesium Ltd, Toronto, Canada) had a purity of 99.99+ pct with the following impurities (in ppm): 20 Al, 30 Zn, 10 Si, <1 Ni, <1 Cu, <10 Fe; tin (Cominco Products, Spokane, Wash.) contained 99.999+ pct Sn. The graphite crucibles were machined from graphite rods (United Carbon Products Corp., Bay City, Mich.) which had an average total ash content of less than 30 ppm. All the graphite parts were baked out in vacuum at 950" to 1000°C for a minimum of 24 hr to remove volatile organic materials. The graphite crucibles (3 in. long, 1-5/8 in. OD, 1-3/8 in. ID) were tightly closed with a threaded cover (1/2 in. thick) which had a central thermocouple well (2-1/4 in. long, 5/16 in. OD, 3/16 in. ID). Cover and thermocouple well were machined from one piece of graphite. A thin sheath of quartz was inserted in the well to protect the thermocouple

Jan 1, 1964

By D. M. Boulin, E. S. Greiner

Single crystals of vanadium were bent at 293" and 77°K to a maximum fiber strain of about 1 pct. Analysis of slip line and etch markings of- crystals deformed at either temperature show the slip planes are {112}. The slip directions at 298° and 77°K, deterwined from the asterism axes of rotation of crystals compressed in a {110} direclion, were (111). Etch pits, associated with dislocations, were observed in the plastically deformed vanadium. There was no evidence of mechanical twinning. THIS paper presents results on single crystals of vanadium plastically deformed by bending and compressing at 298° and 77°K. Bcc metals have been observed to slip on {110}, (1121, and (123) planes while the slip direction has invariably been found to be ( 111) 1 Lindley and smallman2 have studied the deformation intension of polycrystalline vanadium between 298° and 20°K and reported that at and above 77°K the deformation is predominantly by slip, but at 20°K the deformation is associated with twinning. Later, Edington and smallman3 found that single crystals of vanadium compressed in a (111) direction at 77°K deformed by twinning on { 112}( 111) systems. Clough and pavlovic4 have reported that mechanical twins were observed in vanadium loaded by impact at 77°, 173°, and 195°K, respectively. PREPARATION OF SINGLE CRYSTALS The vanadium single crystals were made from commercial vanadium reported to contain 0.03 pct C, 0.03 pct 0, 0.02 pct N, 0.0X* pct Ca, 0.0X pct Si, proximately 0.8 cm diam, 4 cm long and were grown in (100) and (110) directions. A crystal for studies of etch pits was gound to have a face parallel to a {l00} plane by the Bond crystal-orienting technique.7 In order to avoid straining, the crystals were placed on the steel mount with a low-melting organic compound (glycol phthalate) before grinding. Crystals for the bending experiments were ground to have the four side faces parallel to ( 100) planes. The crystals were electropolished8 in 10 pct H2So4 using a current density of about 3 amp per sq cm to remove the strained surface material. The crystals were bent slowly by three-point loading in a stainless-steel jig designed by Sylwestrowicz.9 The end rollers of the jig were 3.8 cm apart. DEFORMATION AT 298°K The bent vanadium crystal, after removal from the jig, had a radius of curvature of 20.4 cm over the 2-cm length close to the center loading roller, where the maximum bending moment occurred. This radius of curvature corresponded to a maximum fiber strain of 0.9 pet. The side faces contained slip bands as shown in Fig. 1. These bands are straight where the strain is high, top and bottom of micrograph, but are curved on either side of the neutral axis in the center. This curvature of the slip bands in the low-stress area may be due to cross slip. The plastically deformed crystal was subsequently electropolished and then electroetched in 10 pct H2SO4 solution, using a current density of 0.25 amp per sq cm. The structure is shown in Fig. 2. The directions of the traces on two adjoining faces were plotted stereo graphically, Fig. 3.* Since there were two sets of

Jan 1, 1968

By Thomas L. Kesler

Essentially all of the barite produced in Georgia has come from the Carters-ville district in the northwest part of the state. The earliest recorded shipment of ore, 60 tons, was made in 1894.&apos; With the exception of the four-year period 1931 to 1934, the separate yearly output has been recorded and published since 1915, whereas the total yearly output of the United States has been published since 1880. The separately recorded production of Georgia (Cartersville) through 1947 is 2,232,544 short tons valued at $14,900,746,2 but unpublished data on the period 1931 to 1934, plus the estimated unrecorded output prior to 1915, make the actual total about 2,400,000 short tons. This is about 21 pct of the total production of the United States, which, through 1947, is 11,328,440 short tons valued at $71,683,386.2 The barite-producing part of the Cartersville district is relatively small, having from north to south a length of 4.5 miles, and a width of 2 miles. This small area, containing 35 barite mines, is the source of practically all of the barite produced in the state. The area is hilly, and has a total relief of 500 ft. The west-flowing Etowah River crosses the middle of the area, and is an unfailing source of water for operations on properties near its course. Opencut mining is carried on during the entire year, but is hampered by rain in the winter and early spring. Three railroads, two U.S. highways, and a network of graded roads provide access to and within the district, as well as excellent shipping facilities for ore and supplies. In addition to the barite, the district contains deposits of manganese, brown iron, ocher, umber, and specular hematite. Geologic Setting The area containing the barite deposits is underlain by Lower Cambrian rocks and their weathered residua. These rocks are grouped in three formations; in ascending order, these are the Weisner, the Shady, and the Rome. The Weisner formation consists mainly of finely micaceous metashale containing many random beds of quartzite, a few beds of conglomerate and metasiltstone, and beds of crystalline limestone that is apparently scarce. The formation is more than 1000 ft thick, and the base is not exposed. On account of their resistance to weathering, the rocks of the Weisner formation have sustained the higher elevations and therefore crop out on the ridges that characterize the area. Nearly all of these ridges are underlain by asymmetric anticlinal folds, and conversely the intervening valleys are underlain by synclinal folds. A diagrammatic section, showing typical mode of exposure of the Weisner rocks and their relation to overlying formations, in the limb of a fold, is shown in Fig 1. The Shady formation here consists of a lithologically distinctive series of variably siliceous specular hematite beds and thin beds of dolomite, which in places contain abundant fossils. In the zone of weathering, the dolomite has been leached and most of the hematite hydrated to ocherous and umber-ous clays, hut bedding planes in these weathered materials are commonly well preserved with or without distortion effected by slumping. This preservation of structure during weathering is lacking in the residuum that rests on the Rome dolomite, which is described below. The maximum thickness of the

Jan 1, 1950

• The Venezuelan Trade Mission to the United States announced that Bethlehem Steel Corp. will begin exporting iron ore from its El Pao concession, south of the Orinoco River in Venezuela, in about three months. The ore will be transported by rail from the mines to barges on the Orinoco and transshipped to ore vessels at the coast for shipment to the Sparrows Point, Md., plant. The Latin American business men warned that projected increases in the United States tariff on petroleum imports from Venezuela would force that country into bilateral trade agreements with other countries and would mean drastic curtailment of Venezuelan imports from this country. •Bethlehem, South American Gold and Platinum Co., and U. S. Steel are investigating the possibilities of securing American foodstuff for their South American mining camp commissaries through the International Basic Economy Corp. IBEC buys in quantity to supply its subsidiary companies operating in Venezuela and Brazil. The mining companies will rid themselves of this burdensome task as well as realizing a saving from the bulk purchases of IBEC. •Oliver Iron Mining Co. has begun construction of a fine ore and taconite agglomeration plant at Virginia, Minn. It is expected to be ready in six months. The plant will be used to experiment with the making of clinker cakes and egg-sized lumps by sintering machines and nodulizing kilns respectively; about 1 million tons per year will be produced. • Roof pinning has been adopted at the iron mines of TCI, near Birmingham, to support overlying strata as mining progresses. Favorable results have been obtained in that dilution of the ore has been reduced by 50% which is attributable to this method of supporting the roof. •An American mining engineering team has gone to Turkey for a two-year assignment assisting Turkish government agencies in the $45 million ECA development, mechanization, and construction of cleaning plants for the Zonguldak coal field, 200 miles east of Istanbul on the Black Sea. The group consists of James Beeley, John E. Good, John S. Lambright, David Renshaw, and Charles R. Weir, all of the Paul Weir Co. •Arthur F. Taggart describes a new way of training engineers by emphasis on broad, basic engineering courses on page 460 of this issue. •Lawrence T. Tierney, chairman of the National Bituminous Coal Advisory Council, released a report stating that the increase in oil imports since the latter part of 194$ has caused significant damage to the U. S. fuel economy. It has reduced the strength of and employment opportunities in the coal, domestic petroleum, and transportation industries, as well as in related service and supplier fields. •Women, camels, and donkeys are the beasts of burden of the Sahara, according-to the UNESCO World Review. •Increased demand for magnesium sheet in airplane construction ana other phases of the national security program have led Alcoa to establish a sheet magnesium rolling division at its New Kensington, Pa., works which will begin operation shortly. Novel prospecting methods being used by the USGS in its search for uranium include: shock-mounted instruments in light trucks,. Geiger-counter probes lowered into augur holes, and experimental airborne prospecting.

Jan 4, 1950

By J. Waldman, M. B. Bever, A. K. Jena

The heats of formation at 273°K of 6 silver-rich Ag-Cd solid solutions and the heat of formation at 78°K of one solid solution have been measured by tin solution calorimetry. The heats of formation are analyzed in terms of the quasichemical theory. If the enthalpy diffel-ence between a hypothetical fcc form and the hcp form of cadmium is taken into account, this analysis does not lead to the conclusion put forth in the literature that electronic effects make significant contributions to the heats of formation of silver-rich Ag-Cd solid solutions. The temperature dependence of the heats of formation is appreciable and negative near 78ºK, but decreases gradually to nearly zero abore 400°K. The relative partial enthalpies per grarn -atom of silver at 541°K and cadmium at 532" and 541°K in tin have also been determined. THE composition range of the silver-rich Ag-Cd solid solutions stable at room temperature extends to about 40 at. pct Cd. Heats of formation of these solid solutions at 308" and 723°K have been measured by solution calorimetry.1,2 Heats of formation for an average temperature of 800°K have also been calculated from vapor pressures.2,3 The heats of formation deviate from the values predicted by the quasichemical theory above about 30 at. pct Cd. This deviation has been attributed to electronic effects at the Brillouin zone boundaries.2 The heats of formation of Ag-Cd alloys are essentially the same at 308", 723", and 800°K; consequently the temperature dependence of the heat of formation d?H/dT = ?Cp is vanishingly small, although from the exothermic heats of formation a negative value would have been expected. In the investigation reported here the heats of formation at 273°K of 6 silver-rich Ag-Cd solid solutions and the heat of formation at 78°K of 1 solid solution have been measured by tin solution calorimetry. The results are analyzed in terms of the quasichemical theory and the dependence of the heats of formation on temperature is discussed. The relative partial enthalpies per gram-atom of silver in tin at 541" and cadmium in tin at 532" and 541°K were obtained in the course of this investigation. The values of the temperature dependence of the relative partial enthalpies per gram-atom of silver in tin derived from the data reported by various investigators2,4-9 are contradictory. The literature contains only a value for 517°K of the relative partial enthalpy per gram-atom of solid cadmium in tin.2 EXPERIMENTAL PROCEDURES Samples of Ag-Cd solid solutions were prepared by melting weighed amounts of silver (99.99 pct pure) and cadmium (99.95 pct pure) in graphite crucibles under a flux of molten potassium chloride.10 The solidified ingots were sealed in evacuated Vycor tubes and annealed at 775°K for 10 days. The ingots were swaged and drawn into wires. The wires, sealed in evacuated Pyrex tubes, were held at 725°K for 5 hr and cooled to 365°K at an average rate of 2.5ºK per hr, followed by furnace cooling to room temperature. Chemical analysis of samples taken from different parts of each ingot gave no indication of segregation. Metallographic examination showed the samples to be homogeneous. Samples of the solid solutions or of the component elements were added to tin-rich baths in a calorimeter." At the start of a run the bath consisted of pure tin. Silver was used in the form of wire of 0.01-in. diam as supplied and cadmium in the form of lumps. Gold (99.999 pct pure) was added with the samples in order to reduce the endothermic heat effect of additions of Ag-Cd solid solutions. Samples of only one composition were added in a run and the ratio of the weight of alloy to that of gold was the same in all additions of a given run. In each run several calibrating additions of tin were made from 273°K. The heat contents of tin were calculated from the following equation, which is based on published data:12 (HTºK- H279º) = 6.70 T - 72,300/T + 20 cal/gram-atom; 505°K < T < 650°K The heat effect of each addition was plotted against the average of the sum of the atom fractions of solutes in the solution before and after that addition. The total concentration of solutes at the end of a run was less than 2 at. pct. In this range the heat effect was a linear function of the atom fraction of the solutes. The heat effect at infinite dilution and the composition dependence of the heat effect were obtained from the plots. RESULTS AND DISCUSSION Evaluation of Data. The linear dependence on composition of the heat effects of additions suggests that in the dilute range the enthalpy interaction coefficients other than the first-order coefficients of silver, cadmium, and gold are negligible, as shown in a concurrent publication.13 The heat effects at infinite dilution and the values of the composition dependence of the heat effects are listed in Table I.

Jan 1, 1970

By C. E. Lundin

The Ce-H system was investigated in the temperature range, 573° to 1023°K, and the pressure range, 10-3 to 630 Torr, as a function of &apos;composition up to 72 at. pct H. Families of isothermal arid isopleth curves were plotted from the pressure-terr~perature-composition relationships. From these curves the solubility relationships were determined for the system. The isopleths are analytically represented by equilibrium dissociation pressure equations. The relative partial molal enthalpzes and entropies of solution of hydvogen in the systerrz were calculated fronz the dissociation pressure equulions and are tabulated. The integral free energies, enthalpies, and entropies of mixing in the Ce-H system were determined from the relative partial quantities and are also tabulated. The standard free energy, enthelpy, and entvopy of reaction of the dihydride phase at kcal per kcal per mole H2, and ?S° = -34. 1 cal per deg mole H2, respectively. The equilibrium dissociation pressure equation in the two-phase region is: UNTIL recently very little was known of the detailed solubility and thermodynamic relationships of the Ce-H system. Two previous investigations1,2 are noteworthy. However, significant discrepancies and omissions exist on analyzing them. The work of Mulford and Holley1 on cerium did not clearly delineate the boundaries of the two-phase region, Cess - CeH2-x. The plateau partial pressures were not thoroughly defined and were considerably displaced in pressure compared to those from the work of Warf and Korst.2 These latter authors concentrated their studies primarily from 823° to 1023°K in the pressure range of 1 to 760 Torr. No data were determined to outline the regions of primary solid solubility and the hydride phase. Also the establishment of the plateau partial pressures was rather limited in scope. In neither work was a treatment conducted of the relative partial molal enthalpies and entropies of solution of hydrogen in the single-phase regions and the integral thermodynamic quantities of mixing throughout the system. Therefore, it was the objective of this research to determine the complete equilibrium solubility relationships and thermodynamic data for the system by pressure-temperature-composition studies. EXPERIMENTAL PROCEDURE The cerium metal for this study was donated by the Reno Metallurgy Research Center of the Bureau of Mines. Total impurity content was 0.13 pct with only 60 ppm O. The metal was checked metallographically and contained only minor amounts of second phase compared to cerium from other sources. Specimen preparation was done in a dry box flushed with argon gas. The surface of a small rectangular piece of cerium (about 0.2 g) was filed with a clean, mill file. Final weighing was done in a tared enclosed vial containing argon gas. The specimen was then loaded quickly into the reaction chamber which was purged several times with high-purity hydrogen gas and then allowed to pump to about 10-6 Torr. The furnace was heated to the reaction temperature and the run started. The equipment used to conduct the hydriding was a Sievert&apos;s-type apparatus. Basically it consisted of a source for pure hydrogen, a precision gas-measuring burette, a heated reaction chamber, a McLeod gage, and a mercury manometer. Pure hydrogen was supplied by the thermal decomposition of uranium hydride. The 100-ml precision gas burette was graduated to 0.1-ml divisions and was used to measure the quantity of gas and admit it to the chamber. The reaction chamber was a quartz tube. Prior to each run, the cerium specimen was wrapped in a tungsten foil capsule to prevent reaction of the cerium with the quartz. Control of the temperature was achieved within ±1°K. Pressures in the manometer range were measured to ±0.5 Torr and in the McLeod range (10-3 to 5 Torr) to ±3 pct. The compositions of hydrogen in cerium were calculated in terms of hydrogen to cerium atomic ratio. These compositions were estimated to be ±0.01 H/Ce ratio. The technique used to study the equilibrium pressure-temperature-composition relationships of the Ce-H system was to develop experimentally a family of isothermal curves of composition vs pressure. The range of pressure through which each isotherm was developed was from 10-9 to about 630 Torr in the temperature interval, 573° to 1023°K. RESULTS AND DISCUSSION The hydriding characteristics of cerium are iso-morphous with those of the elements of the light-rare-earth group (lanthanum, cerium, praseodymium, and neodymium) wherein the region from the dihydride to trihydride is continuously single phase.&apos; The structure of this phase is fcc.3 The heavy rare earths form a trihydride,2 which is hcp, separated by a two-phase region from the fcc dihydride phase. The Ce-H system is represented by the family of experimental isotherms in Fig. 1. Due to the small scale required to draw the curves, the experimental points are omitted; however, a total of 240 experimental data points were taken to prepare these curves. The solubility relationships can be deduced therefrom. Three distinct regions of partial pressure and composition can be seen. The region of cerium solid solution is represented by the rapidly rising isotherms in the dilute composition range. In accordance with Gibbs Phase Rule only one solid phase, the cerium solid so-

Jan 1, 1967

By L. O. Howard

Much work has been done recently on the lead-antimony system1 in connection with lead-rich alloys of commercial importance containing less than 20 per cent. antimony. Dean, Zickrick and Nix have called attention to the perpetuation in the literature of several erroneous data, such as a eutectic temperature of 228° C. at 12.5 per cent. antimony, instead of 247° at 13 per cent. The series is given as a classic example of a straight eutectiferous series in such late books as those of Heyn and Grossmann, 2 Jeffries and Archer,3 Guillet and Portevin,4 Pulsifer,5 Rosenhain,6 and Liddell,&apos; as well as the somewhat earlier works of Hof-man (1918), Wang (1909), and Williams (1920). The work of Dean has definitely shown a solid solution of antimony in lead at about 2.5 per cent. antimony. While lecturing to a class in general metallurgy at the University of Idaho, the writer had the students prepare a series of lead-antimony alloys for the purpose of illustrating methods of thermal analysis. Proper proportions of powdered antimony (sold as C.P.) and test lead were mixed and melted in graphite crucibles under a reducing cover. Cooling

By K. E. Beu

IN the measurement of retained austenite concentrations in steels using the integrated intensity method,1 Averbach has pointed out" that the absorption factor A(0) for a flat sample making a glancing angle 4 with the incident X-ray beam can be combined with his constant factor R to obtain our constant factor" G provided that "1—There is no preferred orientation in the sample, and 2—The geometric requirements [for the sample, film, and X-ray beam] have been met precisely."&apos; If A(0) can be combined with R to give G according to the equation G = R . A(0) [14] then the possibility for making non-compensating errors in the austenite determination has been eliminated. This has been described previously in a technical note." Because of the brevity of the previous note,3 it was impossible to emphasize the fact that the two conditions on preferred orientation and geometry can be easily met experimentally, contrary to Aver-bach&apos;s statement that: ". . . the necessary conditions must be tested experimentally for each determination, and this is done most easily by observing whether the apparent absorption has the form of Eq. 2 [the theoretical equation for A(0)]."" he way in which these two conditions can be met experimentally will be discussed briefly to help clear up this point. In addition to these two conditions, other factors such as sample shape, homogeneity, and grain size which also affect A will be included in this discussion. A (0) depends on sample shape. The theoretical function for A was derived originally for a flat surface.&apos; In general we have found that a flat sample surface is readily obtainable." If such a surface can * The effect of surfaces which are not flat on the measurement of retained austenite will be discussed later. be obtained, it has the following advantages: 1—it is easily reproducible from sample to sample, 2—it is the form required for metallurgical examination —this type of examination being frequently desirable for this work, and 3—it is an efficient shape for diffraction purposes. Perhaps the most important of these features is that a flat sample surface is easily reproducible; hence, this requirement on the repro-ducibility of A from sample to sample is met for all such samples. Fig. 1—Schematic diagram of the quartz crystal monochromator diffraction unit. The centerline of the main beam is at 6&apos; to the target face. The tangent to the crystal face is at 16.8&apos; to the moin beam. The centerline of the monochromatic beam is at 33.6 to the main beam. The sample surface can be rotated in its own plane. The angle of the sample surface and the monochromatic beam can be adjusted by rotating about the vertical axis, The film holder can also be rotated about B so that the film can be exposed over the desired angular range. For Fe K, X = 1.932A. 1011 planes of quartz have d = 3.35A. A(0) depends on homogeneity and grain size. If the sample is badly segregated or the grain size is large, the effect of micro-absorption and primary extinction1. &apos; must be considered. It has been shown, however, that for most plain carbon or low alloy hardened steels, neither micro-absorption nor primary extinction effects are present.&apos; A (0) depends on camera geometry. For a given angle 0, A remains theoretically constant from a geometrical viewpoint only if the following factors are kept constant: 1—the angle of inclination .+ of the sample to the X-ray beam, and 2—the centering of the sample with respect to the film cylinder. These are mechanical problems which can be solved readily if the facilities of a good machine shop are available. The arrangement used to insure that the angle 4 remains constant and the centering of the sample is reproducible is indicated schematically in Fig. 1. The sample is clamped against a thin plate with a hole in it by means of a spring-loaded pres-

Jan 1, 1954

By Y. H. Liu, R. Kiessling

The chromium, iron, and tungsten borides have been treated with ammonia at different temperatures. They are attacked, forming metal nitride and boron nitride, and the results are summarized in the tables. In the tungsten-nitrogen system a new phase has been observed, closely related to the known ß phase. THE present investigations were begun to determine whether any ternary phases exist in the transition metal-boron-nitrogen systems for the metals chromium, iron, and tungsten. Attempts to prepare such phases were made by using the borides of the metals as starting materials and ammonia as the nitriding agent. Although no new ternary phases have been found to exist, the results may be of some interest with regard to the technical use of the borides. General Procedure A steady stream of dry ammonia was passed through a silica reaction tube, the central part of which was kept at the reaction temperature while its ends were water-cooled. Weighed amounts of the borides were placed in a silica or porcelain boat and heated at different temperatures for a period of 10 to 24 hr. The boat was then rapidly removed from the reaction zone to the quenching zone, the water-cooled end of the tube, by means of a simple magnetic device. The nitrogen content of the products was determined by the increase in weight of the specimens, and the phase analysis was carried out by X-ray methods. For this analysis a Guinier-type camera, constructed at this Institute, was used with a bent, ground quartz crystal monochromator. The general reaction, which occurred in all the experiments, may be summarized as: metal boride + nitrogen -* boron nitride + metal nitride For the higher temperatures pure metal was formed instead of metal nitride. It is sometimes difficult to Discussi detect boron nitride among the reaction products by X-ray methods. Prolonged exposures of some specimens showed, however, that the strongest reflections of boron nitride were present. Additional evidence for its presence was given by the increase in weight of the specimens after nitriding. This increase was always greater than that corresponding to nitride formation only and was often in close agreement with the formula given above. Finally, a white powder, which was shown by X-ray methods to be boron nitride, was left if the reaction products after nitriding Fe,B at 448°C and FeB at 768°C were dissolved in diluted sulphuric acid. Ch rom iu m - Boron - N itrogen Five phases have been found to exist in the Cr-B system,&apos; , and all were used as starting materials. Investigations on the Cr-N system have shown the existence of two nitrides with ideal composition Cr,N and CrN.".&apos; * The results are summarized in Table I. All the borides are attacked and decomposed into chromium nitride and boron nitride, and the kind of nitride formed depends only on the temperature and not on the boride used as starting material. The lowest reaction temperature, however, is different for the different borides. Thus the 6 phase begins to react at about 735 "C, the r phase at about 800°, the S phase at about 900°, the 7, phase

Jan 1, 1952