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By H. L. Gilbert

Zircon sand may be reacted with sodium hydroxide at 600° C. to form sodium zirconate and sodium silicate. Sodium zirconate is water insoluble and so may be washed free of sodium silicate. The sodium zirconate may then be converted to zirconyl chloride by the action of hydrochloric acid and the zirconyl chloride crystals separated by cooling the solution. This approach produces zirconyl chloride of satisfactory purity with less cost than is involved in buying anhydrous zirconium chloride and converting it. A proposed design for a plant is given, INTRODUCTION This work was conducted by the Rare Metals Branch as a part of research on zirconium at the Bureau of Mines Northwest Electrodevelopment Laboratories, Albany, Oreg., under the guidance of S. M. Shelton, Regional Director. The work was supervised by W. W. Stephens, head of the Rare Metals Branch (now with Carborundum Metals Corp.).

Jan 1, 1954

By W. H. Mathews

"The Hardie group of cinnabar claims is in the interior of British Columbia; 25 miles northwest of the city of Kamloops. It is one of a number of mercury; properties scattered along a north trending belt 20 miles long and up to 5; miles wide. In all but one of these properties cinnabar is associated with; dolomite veinlets in zones of carbonate alteration in bedded rocks of Triassic; and Cretaceous (?) age; or in intrusives cutting these bedded rocks. No dolomite alteration or cinnabar mineralization is known in the undoubted Tertiary rocks adjacent to the mercury belt.The mercury showings of the Hardie group lie for the most part in a granitic stock cutting Cretaceous (?) volcanics. The rock in this intrusive shows marked variations in texture and has been described in earlier reports as granite and granodiorice, granite porphyry, and trachyte or dacite porphyry. At Hardie mountain the cinnabar mineralization, unlike that of the other properties, is associated with a fine-grained, almost chalcedoni c, quartz; carbonates, though present, are of minor importance. Some of the most interesting showings are found in an adit in the southeastern part of the property where cinnabar mineralization shows a very distinct structural but not a genetic relationship to a brown porphyry dyke 2 to 8 feet wide cutting a phase of the stock that may best be described as aplitic"

Jan 1, 1954

By M. S. Hunter, D. L. Robinson

An extremely fine subgrain structure found in aluminum and aluminum alloys is shown and a method for revealing this structure is described. The appearance and some of the characteristics of this structure are described and the possible significance of subgrain structure in terms of chemical, electrochemical, and metallurgical processes is considered. GRAINS and grain boundaries, which constitute the principal manifestations of the crystalline aggregates known as metals, play such an important part in determining the characteristics and properties of metals and alloys that their nature and behavior have long been of much concern to the met-allographer. Many investigators have speculated on the possible existence of a finer structure within the usual grain structure and, through X-ray diffraction and metallographic techniques, have revealed evidence that such finer structures exist. Among these structures are the mosaic blocks and domains described by Burgers1 and others in their contributions on crystalline structure and the dislocation theory, the small units associated with polygoniza-tion described by Cahn,2 and the intragranular blocks revealed more recently by Lacombe and Beaujard.3 his paper describes some novel methods for clearly revealing a very fine granular substructure within the usual grains of pure aluminum and aluminum alloys. It also compares the characteristics and behavior of this subgrain structure with those of the ordinary grain structure and gives some examples of the manner in which this substructure may influence the characteristics of aluminum alloys. Metallographic investigations of aluminum and its alloys have dealt extensively with the functions and behavior of grains and grain boundaries and have evolved a definite concept of the relation between grain structure, orientation and physical, mechanical, chemical, and electrochemical behavior. During the examination of etched samples, a roughening or mottling of the body of certain grains has occasionally been observed. Such roughening obviously represented differential attack by the etching solution, but its true significance was not at first realized. It is now known that this roughening probably rep- resented a subgrain structure, although the particular etching treatments used were not capable of revealing this subgrain structure clearly. Also, in practically all cases, the subgrains were apparently far too small to be resolved by the light microscope. Recently, a method has been developed for revealing clearly the subgrain structure of most aluminum alloys. This method is somewhat unique in that it eliminates much of the usual tedious mechanical polishing and the attendant danger of a surface layer of flowed metal and at the same time is simple, rapid, and effective. It involves the use of the Alcoa R5 Bright Dip, a patented chemical polishing treatment licensed by Aluminum Co. of America. This treatment produces a bright, highly polished surface at least the equal of any mechanical polish and also etches the subgrain boundaries as well as the ordinary grain boundaries to reveal both the grain and subgrain structure simultaneously. Metallographic specimens to be examined are taken through the customary grinding and polishing operations used for aluminum alloys.' The usual care required in the final polishing operation to prevent a flowed surface layer and to obtain a high polish is not necessary, however, because any flowed layer is eliminated and a high polish is produced by the final immersion in the Alcoa R5 Bright Dip. Depending on alloy type, this dip takes from a few seconds to about 3 min, after which the sample is rinsed well, blown dry, and is ready for examination. The substructure can be revealed by some of the usual metallographic methods such as electropolish-ing or mechanical polishing and etching but no method has been found which is the equal of the new chemical polishing treatment. Mechanical polishing followed by the usual metallographic etching is not entirely satisfactory for revealing this substructure, probably because of the flowed surface layer resulting from the mechanical polish. If the usual etching methods are prolonged sufficiently to remove this layer, the specimen surface becomes quite rough and the substructure is not defined clearly.

Jan 1, 1954

By P. A. Albert

THE to a transformation has been investigated by Newkirk1 in sponge titanium alloys which had been relatively slow-cooled so that several grains formed in a former grain. For a nucleated from , Newkirk assumed the following relationships and found them consistent with his experimental results: (00.1)a (110)Pll.01. II [111] Liu and Margolin,' in their investigation, found that the habit planes of martensitic in titanium consisted of planes of the families (3341, and (3441,. Using Newkirk's orientation relationship, the (3341 habit plane is found to correspond to the (1450) plane of a.

Jan 1, 1954

By R. M. Creamer

Attempts have been made to electroplate titanium and zirconium from aqueous, nonaqueous, and fused-salt electrolytes. Metals were produced only in fused-salt electrolytes, the major product being sponge metal. All other electrolytes gave only partial reduction of the metal ions. Fused alkali borate electrolytes containing titanium salts gave titanium boride powders and coatings of poor adherence. Some of the problems encountered in the deposition of these metals and some of the aspects of titanium and zirconium chemistry involved are discussed. INTRODUCTION Titanium and zirconium are both relatively light, noncorrosive metals with both military and civilian uses. This has led to intensive investigations into the metallurgy of these metals. Both metals are high in the Electrochemical Displacement Series and are difficult to prepare in a pure state. At present they are prepared by reducing their chlorides, using magnesium. Electrolytic reductions have resulted in the preparation of fine powders or sponge of variable quality. It is believed that a good process of electroplating these metals on a baser metal would result in a very desirable product. The objective of the research summarized in this report was to investigate methods of electrodepositing these metals, with the idea of producing uniform, coherent plates. Most of the work was concentrated on titanium, the more abundant of the two metals. A system developed for titanium should be applicable to zirconium owing to their chemical similarity. Information gained from these experiments may also be applicable to the electro-winning of the metal.

Jan 1, 1954

By M. R. KEYS

"The property is about 120 miles north of Red Lake in the Favourable Lake area, district of Kenora ( Patricia part) , Ontario. The original discovery was staked by K. Murray in December, 1927. The first development work was done by the Favourable Lake Mining and Exploration Company. In 1936 Newmont Mining Corporation acquired control of the property and developed it to production by September, 1939. Production to the end of 1945 had a value of $7,534,656 from 441,457 tons of ore, an average value of $17.04 a ton . This production was mainly from gold and silver, with lead and zinc of subordinate importance.The rocks in the vicinity of the mine trend in a north-south direction. From east to west the sequence is: (1) A dark-coloured, massive rock, presumably a flow, composed mainly of quartz and biotite. ( 2) A buff- coloured, scricitized rock locally containing quartz phenocrysts and black hornblende. This is an alteration product of the dark variety and is later than the folding. It occurs mainly within the dark rock. (3) A series of sediments comprising thin beds of greywacke, grit, quartzite, conglomerate, and iron formation. ( 4) A gabbro sill, now largely altered to amphibolite.With the exception of the buff type, these rocks dip 80°E. The buff rock has a very irregular outline in comparison with the other rocks and appears to dip somewhat more flatly east. Felsite and diorite dykes are also present. These have a general strike of S.60°E. and dip 65°S .W. A post-ore diorite dyke trending N.15°E. occurs about 2,000 feet east of the mine area."

Jan 1, 1954

By Merlyn B. Buhle

The value of the earth resistivity method in groundwater studies in Illinois has long been recognized. Owing to the sharp electrical contrasts between sand and gravel deposits and glacial till, alluvial silt or underlying shale, much of the earth resistivity prospecting has been of a relatively elementary nature and has been highly successful. Approximately 90 pct of earth resistivity interpretations by the State Geological Survey have been accurate for practical purposes. Four studies involving fairly simple geologic situations are presented in this paper as typical cases. FOR the past 20 years electrical earth resistivity exploration has been used in Illinois in many phases of study undertaken by the State Geological Survey, chiefly in locating and outlining deposits of water-bearing sand and gravel from which to obtain ground water for municipal and industrial supplies. At least 43 municipalities in the state derive their total water supply from deposits of sand and gravel discovered by resistivity methods. These deposits occur in both Quaternary and preglacial valleys and within much of the glacial drift which covers a large portion of the state. In recent years there has been much demand from rapidly growing municipalities for help from the Illinois Geological Survey to extend existing well fields. Water supplies for many and varied industries constitute a considerable portion of the Survey's studies. The diminishing need of water supplies for railroads has 'been accompanied by an increasing demand by the oil industry for water for secondary recovery programs. The instruments used by the Illinois Geological Survey follow closely the commutated direct current circuits developed by O. H. Gish and W. J. Rooney' using the Wenner2 electrode configuration. More recently replacement of the hand-driven commutator by a synchronous vibrator has led to increased ease of operation and accuracy. Continuing improvement of equipment and technique has led to many changes in the instruments, but the operating theory remains the same. In the field operation at a selected station, four electrodes are set at equal distances in the ground 6 to 10 in. deep, in a straight line. A 16 to 20-cycle current is applied to the two outside steel electrodes

Jan 1, 1954

By D. D. Blue

To insure domestic production of aluminium for, essential civilian and defense uses, the Government, under authority of the Defense Production Act of 1950, programed and promoted an aluminum-expansion program that will more than double the primary production capacity that existed in 1949. In view of this vastly increased production, the raw materials, with respect to both quantity and sources, are reviewed. The raw-material consumption pattern, the requirements during an expansion period when excess quantities of materials for starting up new facilities are consumed, and the probable requirements for production of 1.7 million tons per year of primary aluminum are discussed. The raw materials that presented the most difficult supply problems were bauxite, electrical power, and fluoride salts, and the supply pattern for these materials probably will undergo changes. A major part of the electrical energy for the increased capacity was to come from thermal generation, Jamaica-was to become a major source of bauxite, and synthetic fluoride salts were replacing natural cryolite in increasing quantities. Other raw-material requirements discussed are: Soda ash; lime, and limestone; starch; filter cloth; fuel; alumina; the carbonaceous materials, green and calcined petroleum coke, high-and low-temperature pitch and coke or anthracite; cryolite; aluminum fluoride; the materials going into production of synthetic fluorides, acid-grade fluorspar, and sulfuric acid; and labor. INTRODUCTION The raw materials for the aluminum industry that have received the most publicity are bauxite, the ore that supplies elemental aluminum, and electrical energy, the means by which aluminum oxide is reduced to metal. A number of other important materials are, however, required in large quantities in the production of primary aluminum metal.

Jan 1, 1954

By J. D. Sargent

Selenium might be described as a paradoxical element, being a metal or a nonmetal, a conductor or nonconductor, amorphous or crystalline, colorant or decolorant, and a hydrogenator or dehydrogenator. Selenium was discovered in 1817 by the Swedish chemist, Berzelius, while studying flue dust from the lead chambers of the sulfuric acid works at Gripsholm, Sweden.

Jan 1, 1954

By Rudolph G. Wuerker

The progress made in testing the strength of rocks and minerals as they are encountered in mine operation is reviewed. An attempt is made to correlate these physical measurements with abrasive hardness, grindability, and behavior in comminution on one hand and fracture of rocks in pillars and roof control on the other. THIS paper reviews the progress made in testing the strength of rocks, ores, coal, salts, and other minerals as they are encountered in mine operations. It attempts to correlate the results of these physical measurements with technological properties more useful to the mining engineer: abrasive hardness, grindability, and behavior in comminution on one hand, and roof control, fracture of rocks in pillars, and mining methods with controlled caving on the other. In the following pages, the materials discussed will be referred to as rocks. Basic to rock mechanics and comminution are the problems of strength, elastic behavior, and failure, common to all brittle materials. A distinction will be drawn as to theoretical and applied research, and discussion of the progress made in each field will include test data obtained by the U.S. Bureau of Standards,1-1 the U.S. Bureau of Mines," the Iowa Engineering Experiment Station,"." the Committee on Geophysical Research at Harvard University,'" Basic Industries Research of the Allis-Chalmers Manufacturing Co.,11,12 by Philipps,13 and by Mueller," to name only a few. With refinements of testing methods and increased standardization. more useful and more comparable results have been achieved. This is especially important in testing a material like rock, as the inherent heterogeneity demands careful and exacting procedures. New measuring procedures that appear to supersede well known standard methods have contributed to faster and less costly testing yet have introduced new concepts, with implications as to comparability of results which must be watched. Reference is made to the sonic method for determining elastic properties," to be discussed in detail below. Basic Investigations Historically, all work in the field has started with the simplest determinations such as those for crushing strength, abrasive hardness, and grindability. These serve the limited objectives in the researcher's field of specialization: building construction, road ballast, roof control in mines, comminution, and seismic prospecting. Occasionally, fundamental properties like the modulus of elasticity E and Poisson's ratio v have been determined with the idea that they might have some bearing on the technological properties of the material under investigation. But it was not until the work of Philipps,13 of Harvard University,'" and of the U.S. Bureau of Mines"' that sufficient basic data were collected to allow researchers to go beyond the technological test and find the fundamental laws behind the behavior of rocks in mine and mill operations. The properties to be looked for are those that describe the elastic behavior of any material, the modulus of elasticity E and Poisson's ratio v being the ones determinable with least difficulties. Only two such properties are required to compute any other property such as the shear modulus, the modulus of rigidity, and the bulk modulus, all of which are related to each other according to well known equations of the theory of elasticity." In spite of their heterogeneous character, all rocks tested have possessed elastic properties. This does not mean that rocks of the same type always have the same modulus of elasticity, which varies exactly as the crushing strength or any other physical property of a rock can spread over a wide range. This has been explained by imperfections of the material always found in rocks, but to some extent this scattering of data is caused by inaccuracies inherent in the testing methods. Modulus of Resilience, a Criterion of Failure Increased availability of E values should allow us to test the validity of the quantity of strain energy theory which has been used in the solution of roof control problems by Philipps13 and by Holland.'" Recently Bond and Wang12 have applied this theory to explain the failure of an elastic material in comminution. Actually it is a very old theory, proposed as far back as 1885 by Beltrami.16 By its assumption the condition of yielding is determined by the term S2 M, = — x volume. Here M, is the modulus of 2E resilience, and its dimension is inch-pounds per cubic inch, that is, work per unit volume. Its numerical value is equal to the area under the stress-strain diagram. In the foregoing equation S is the yield stress (in psi) in tension or compression, whatever the case may be. E, the modulus of elasticity, is in psi. The great appeal of Beltrami's concept of stored energy lies in the fact that the two properties which seem to influence failure most, strength and elasticity, occur in the formula for the modulus of resilience. As an illustration of this, the moduli of resilience in compression of some typical materials tested by the U.S. Bureau of Mines" have been plotted in Fig. 1. The sample of concrete of conventional mix is shown only for the sake of comparison. Its determination was made in the Department of Mining and Metallurgical Engineering, University of Illinois. The values of the moduli of resilience of the various specimens in the plot are:

Jan 1, 1954

By H. W. Maynor, C. J. McHargue

DURING the course of an investigation of materials suitable for use as thermocouples at elevated temperatures by one of the authors, several nlolybdenum-rhenium alloys were prepared. Micrographs of an annealed alloy containing 25 pct Re (intended concentration; analysis not obtained) showed a number of twins, Fig. 1, suggesting a face-centered cubic structure. This note reports the structure and recrystallized wire texture of an alloy containing 25 wt pct Re. Alloys were prepared from 99.9 pct Mo (Fansteel Metallurgical Corp.) and rhenium obtained from the University of Tennessee (purity unreported). Powders were combined and briquetted at 56,000 psi and sintering was carried out at 2400°C for 5 hr in vacuum. Ingots so prepared were swaged at 982.2" to 1037.8oC into wires 0.036 in. diameter, a reduction in diameter of 85.6 pct. These wires were vacuum-annealed 1 hr at 2000°C. A North American Philips 114.59 mm powder camera and nickel-filtered copper radiation were used for structure determination. For the texture determination a Laue-type camera was used with zirconium-filtered molybdenum radiation and, because of the high background, aluminum foil was mounted next to the film. Exposures were taken with the wire perpendicular to the X-ray beam and tilted by 10". It was found that the X-ray pattern could be indexed on the basis of a face-centered cubic structure. Because of difficulties associated with obtaining a good X-ray pattern for this material, accurate parameter determinations were not made. An indicated parameter value of 3.70A was obtained. The X-ray data are given in Table I. The annealed wire texture was observed to be a sharp [111] texture. The spread about this fiber axis was k8" at the surface of the 0.036 in. wire. The annealed wire textures of aluminum have been reported as retention of the [Ill] deformation texture for anneals below 500°C and a new [1121 texture for anneals above 600°C.1 In copper wires, with a [Ill] plus [loo] deformation texture, results indicate a retention of this texture for annealing at lower temperatures and new components or the disappearance of components for annealing at higher temperatures.' The presence of the strong [I111 texture in the molybdenum-rhenium alloy after a 2000 °C anneal suggests that the deformation texture was the same. Acknowledgment The wires used in this study were prepared and heat-treated at the Institute for Atomic Research, and Ames Laboratory, Iowa State College, and the authors wish to express their thanks to the Institute for allowing the use of the material and permission to publish the results.

Jan 1, 1954

By J. W. Spretnak, R. Speiser

IT has been suggested that boron in steel may form a film entirely around the austenite grain and that this film is responsible for the boron hardenability effect. In this connection, it is of interest to examine some of the ramifications of the concentration range of boron usually employed in hardenable steels, namely 0.0005 to 0.003 pct in a grain size range of ASTM grain size No. 1 through No. 10. The ratio of the iron to boron atoms and the number of unit cells of y iron per boron atom are listed in Table I. Even at the highest concentration considered, there are 1600 unit cells of y iron per boron atom, assuming a uniform distribution of boron. To investigate the possibility of the boron film formation, the number of boron atoms required to cover the grain surface completely must be calculated. With some transition elements, boron crystallizes in sheets composed of equilateral hexagons very much like graphite.' The selected value for the length of a side is 1.80Å. A simple calculation shows that two boron atoms cover an area of 8.4x l0 -16 sq cm. Table II lists the number of atoms of boron required for the formation of the monatomic film and Table III lists the number of boron atoms per grain. The hypothetical cases of 100 pct and 10 pct adsorption are calculated (all boron atoms in a grain and 10 pct of all boron atoms in a grain are located at the grain surface respectively). In Table 111, all combinations of grain size and composition below and to the left of the solid line (100 pct adsorption) and the dashed line (10 pct adsorption) are excluded as to the possibility of covering the grain surface with a continuous boron film. Thus, even for 100 pct adsorption, the smaller grains can form the film only at the higher concentrations. For the best case, grain size No. 1 and 0.0030 pct B, the required degree of adsorption is 3.9 pct. The above calculations deal only with the number of boron atoms required to form a monatomic film and do not take into account the mechanism of concentration of boron at the grain surface and the possible limitations to the extent of this concentration at a constant temperature, as for example in the austenitizing process. The question next arises as to how this surface concentration can occur during an isothermal treatment. Such surface enrichment of boron must occur through the phenomenon of surface adsorption, i.e., the concentration of solute atoms in solid solution in the vicinity of the surface without precipitation. A solute atom will tend to concentrate at the grain boundary if it reduces the interfacial tension. The possibility of adsorption effects involving both boron and carbon in iron has been discussed.' In general, the tendency for a sol-

Jan 1, 1954

Jan 1, 1954

By E. J. Gleim

The construction of explosion-proof electric mine equipment for operation in gassy coal mines of the United States was begun as early as 1903. In 1.906, similar equipment with special protective devices was built for export. An investigation of explosion-proof motors was conducted by the United States Bureau of Mines during 1910 and 1911. In other words, this was among the first efforts of the Bureau directed toward the saving of life and property subsequent to its establishment by act of Congress in 1910. In these early motors, those with special devices for relief of explosion pressures predominated. At that time it was generally considered that, by providing for pressure relief, the enclosures could be made lighter in weight because of the lower explosion pressures developed within.

Jan 1, 1954

By W. P. Corking

"The purpose of this paper is to describe the relationship of the goldbearing ore to structure at the Pickle Crow mfoe. Information beyond this scope may be found in the reports and papers of Hurst( l), Bothwell(2), Thomson(3) , and Monette( 4).The property lies on Crow river, in Patricia district, 80 miles northeast of Allanwater, and about 125 miles northeast of Sioux Lookout on the Canadian National railway. From April of 1935, when the mill began operation, to the end of 1944, a total of 564,890 oz. gold and 49,275 oz. silver were recovered from 958,416 tons of ore.Mining on the property is at present carried on in two separate orebodies, the Howell and the No. 2 vein. Stoping has been carried on from every level on the Howell vein to a depth ot 2,450 feet below the surface and from several levels on the No. 2 vein through a mile long cross-cut on the 750-foot level to the Howell vein workings. A steadily increasing volume of ore is being obtained from the No. 2 vein.Each of the two orebodies consists of vein quartz with small amounts of other gangue minerals either in a single vein or a stockwork of veins. Both lie within sheared walls and carry gold in the free state. Fig. 1 shows the position of the veins with respect to the surrounding rocks. It will be noted that the delineation of the beds of iron formation shows that the lava flows and minor, interbedded sediments that make up most of the country rocks are areally folded and contorted.STRUCTURENearly all gold found to date in sufficient quantity and concentration to make ore in the Pickle Crow area is confined to these major quartz veins . Both strike a little north of east and dip north, and in both cases the attitude of the enclosing rocks is somewhat more north of east in strike and more steeply north in dip than that of the veins. As a result of this disposition both veins migrate across their enclosing rocks at a moderate angle in both dip and strike. (In this connection it should be noted that No. 2 vein dips at a considerably flatter angle than its host rock, but has a very pronounced rake to the northeast, effecting the same result as in the Howell vein.)"

Jan 1, 1954

By N. K. Chen, R. Maddin

THE textures of straight-rolled and of cross-rolled molybdenum were first determined with the aid of pole figures by Custers and Riemersma.' These authors have shown that for straight-rolling, the main texture was (100) [0111 with a considerable spread about the rolling direction. After cross-rolling a second texture was obtained in which there was a [111] axis perpendicular to the rolling plane, possessing a rotary symmetry. Recently Semchy-shen and Timmons2 in their study of preferred orientation of arc-cast molybdenum sheet obtained similar pole figures. In these two investigations, polycrystalline materials were used. In the main, the textures of molybdenum in these cases are qualitatively consistent with rolling textures of other body-centered cubic metals, such as iron and Fe-Si alloys." In the present investigation, single crystals of molybdenum were deformed by rolling with respect to specific crystallographic planes and directions. Since the deformation textures of polycrystalline aggregates have been related intimately to the behavior of individual grains,4 a study of possible correlations of final textures with respect to the initial orientations of the single crystals might conceivably lead to a better understanding of the textures. Annealing treatments were carried out after deformation in order to study the recrystallization characteristics as well as the recrystallization texture. Rolling of Single Crystals Single crystals of molybdenum (about 1/8 in. in diarn x 1-in. long), grown by the method previously described,5 were cold-rolled without intermediate anneals. Except for specimens MR-1 and MR-2, which were rolled at random in the preliminary test in order to find a proper rate of reduction, all other specimens were carefully documented as to their respective orientation before deformation by means of X-ray Laue back-reflection methods. A stereo-graphic projection was constructed from which it was possible to determine a particular plane and direction to be considered for rolling. Parallel flat surfaces were then polished metallographically with respect to a reference scratch on the specimen which was mounted in sealing wax. These flat surfaces contained the plane chosen for rolling. After etching, a Laue back-reflection photogram was again made of one of the flat surfaces to determine the exact plane of rolling. The initial orientations of all the specimens (specified by two elements for each crystal, direction of rolling and the pole of the rolling plane) are summarized in Fig. 1. The specimens were mounted in plasticene between two hardened Si-Fe plates. The sandwich was then rolled down, keeping the direction constant in the case of straight-rolling. In cross-rolling (MR-10, MR-11, and MR-12) the sandwich was rotated 90" after each pass so that every first and third pass contained the same rolling direction. Specimens MR-14, MR-15, and MR-16 were compression-rolled following the manner of Barrett." In these cases the direction of the sandwich through the rolls was changed by 3" to 5" for each pass until the specimens were rolled to the desired reduction in thickness. It was found that if extreme care was exercised in rolling, i. e., the amount of deformation per pass was extremely small, the specimens could be rolled to a large reduction in thickness. The rate of reduction used, with a single exception of MR-1. was generally 0.001 in. per 10 passes. Thus, it took about 800 passes to reduce a specimen to a final reduction in thickness of 87 to 98 pct. The results of rolling are shown in Table I. Cold-Rolling Textures The final orientations were determined by the conventional Laue transmission method," using molybdenum radiation, with or without a zirconium filter. Pole figures were plotted from (1101 and (200) reflections in which three degrees of intensity— heavy, medium, and light—were determined visually. Three main types of textures have been observed from the deformed single crystals. These are: 1—a

Jan 1, 1954

By N. K. Chen, R. Maddin

Columbium single crystals were deformed in tension and compression. Reorientation by X-rays and stereographic projections of slip traces indicate that plane of slip may be considered as (110). The plastic behavior is shown to be quite similar to the deformation of molybdenum single crystals. STUDIES on the crystallography of the deformation process in body-centered cubic metals have been renewed recently with investigations of iron single crystals1-" and molybdenum single crystals.4 It is now apparent that too many exceptions to the rationalization based upon the ratio of absolute testing temperature to absolute melting point by Andrade5 exist to permit more serious discussion of this type of analysis. The considerations of resolved shear stress utilizing only planes of the type {ll0}, {112), and {123)³,6 permit analysis of the deformation only on the basis of those three types of planes. The suggestions made by Elam7 and by Greninger8 in which the slip process is envisioned as a composite slip on two nonparallel {110) planes can be illustrated schematically in Fig. 1. It may be seen that an unresolved trace on any plane containing a <111> direction may be accomplished by varying the number of atoms participating in the composite process. By further varying the number of atoms in each plane but keeping the ratio of participating atoms constant, jogs could be obtained in the traces and hence wavy slip lines could be produced. Vogel and Brick&apos; studied the behavior of a iron single crystals in which they suggest that the plane of glide is "non-crystallographic" and may be predicted from the intersection between the great circle joining the slip direction and specimen axis with the great circle whose zone axis is the slip direction. In a more recent investigation on iron single crystals, Steijn and Brick" suggest that the slip mechanism may be considered as made up of a type of composite slip occurring on {110} and {112} planes. Evidence for a possible composite nature of the slip process has been presented for the case of molybdenum in the form of analysis of asterism and specimen axis rotation." Definite proof of a composite slip process must, however, await good electron microscopic resolution of the individual traces making up the unresolved optical trace used in determining the acting slip plane. The present investigation was undertaken to study the behavior of columbium single crystals not only in tension but also in compression since the specimen axis migration should indicate the plane or planes of glide in the same manner that the specimen axis migration in tension indicates the direction of glide. The orientations of eleven crystals investigated are shown in Fig. 2. Specific orientations are missing (those in the vicinity of [Ill] and [001] and consequently the effect of orientation on the crystallography of deformation could not be considered. Experimental Procedure The 1/8 in. rods (7 in. long) were subjected to an axial tension in vacuo while at temperatures in the vicinity of 2000°C for 2 to 4 hr. This treatment resulted in large cylindrical grains (about ½ in. long) occupying the entire cross section. A number of these rods were used for the tension studies by observing the behavior of the individual grains. For the compression studies, single crystals approximately % in. long by 1/8 in. in diameter were cut from the rods; the ends were ground parallel. All specimens were polished electrolytically in a solution of 15 cc HF(48 pct) and 85 cc H2SO4 (concentrated) using a platinum cathode, a current density of 0.04 amp per sq cm and a temperature between 25" and 60°C.10 Orientations were obtained using a Laue back-reflection method (3 cm film to specimen distance) with a ½ mm collimator 9 cm long. For the compression specimens, a reference mark was scratched on one of the compression sur-

Jan 1, 1954

By B. R. Klahold

Each year hundreds of mineral specimens and numerous inquiries regarding tests and analyses of minerals and related inorganic substances are received by the Bureau of Mines. In response to this demand, in years past Information Circulars were published containing a list of laboratories. This paper is a revised version of Information Circular 7523, The listing has been changed from a regional basis to one of States arranged alphabetically and grouped by cities, again alphabetically, with Alaska and Canada listed at the end. All the services given at these laboratories are listed on one page for convenience and brevity. This list is compiled as a public service, and none of the laboratories listed herein are recommended over any other nor can the Bureau of Mines vouch for their results.

Jan 1, 1954

By C. T. Bischoff

DURING the past few years geochemical testing for traces of heavy metals in water, soil, rock, and vegetation has aroused increasing interest. Various techniques for field and laboratory determinations have been described in the literature, as have some of the results of application. However, little information has been published regarding application to glacial terrain. Over 90 pct of the Canadian Shield is overburdened, resulting in high costs for mineral exploration once the outcropping ore deposits have been found. This has been largely responsible for the widespread application of mining geophysics in Canada, permitting concentration of effort on area or zones considered most favorable. However, geophysical interpretation has its limitations, since at least 90 pct of the structures indicated thereby contain no valuable minerals. A more direct approach is therefore highly desirable. If underlying base metal mineralization can be detected by sampling soil or vegetation at moderate cost this should prove of great help in locating new discoveries or extending known ones. A large proportion of Canadian ore deposits contain appreciable copper or zinc, even where these are not the principal economic metals. Consequently the field of application is a broad one.

Jan 1, 1954

By R. I. Jaffee, F. C. Holden, H. R. Ogden

ECENT papers dealing with the properties of unalloyed iodide titanium have been directed primarily at the determination of base-line properties for alloy investigations. Early work was limited to a few tests because of the limited availability of iodide titanium at the time. In the results of papers by Campbell et al.,1 Gonser and Litton,2 Jaffee and Campbell,3 inlay and Snyder,4 and Jaffee, Ogden, and Maykuth, data on mechanical properties are presented for unalloyed iodide titanium in the annealed and cold-worked conditions. Data are presented in this paper which show the effects of heat treatment on the structure and mechanical properties of commercially produced iodide titanium. Correlation is made between microstruc-tural variables and the mechanical properties. Experimental Procedures Melting Stock: The melting stock used was as-deposited iodide titanium, produced by New Jersey Zinc Co. The furnished analysis showed the following range of impurities: N, 0.004 to 0.008 pct; Mn, 0.005 to 0.013; Fe, 0.0035 to 0.025; Al, 0.013 to 0.015; Mo, 0.0015; Pb, 0.0045 to 0.0065; Cu, 0.0015 to 0.002; Sn, 0.001 to 0.01; Mg, 0.0015 to 0.002; and Ni, 0.003. Hydrogen content as determined by vacuum-fusion analysis was 0.0091 wt pct (0.44 atomic pct) after arc melting and fabrication. Nitrogen analysis on the arc-melted and fabricated titanium showed a content of less than 0.002 pct N. The average hardness of the furnished stock was Rf 70, or approximately 85 VHN. Melting Procedure: The as-deposited rods were rolled, sheared, and degreased in preparation for arc melting. The charge was arc-melted with a tungsten electrode in a water-cooled copper crucible under a positive pressure of high purity (99.96 pct) argon. The final ingot was approximately 2 in. in diameter and showed no increase in hardness over that of the initial stock. Fabrication: Heating for fabrication was done in air. It was begun by forging the ingot into a 3/4 in. diam rod, at an initial temperature of 1600°F. Scale was removed by sandblasting. The rod was then swaged to 1/4 in. diam at room temperature through a series of 20 dies, with approximately 10 pct reduction in area between each die. An anneal of 1 hr at 850 °C in air was given after the 1/2 in. die, such that the final cold reduction was 75 pct. Sections cut from this rod were used for test and microstructure specimens. Heat Treatment: Heat treatments were carried out in resistance tube furnaces with stainless-steel linings, under an atmosphere of gettered argon. As further protection against contamination, the specimens were packed in titanium turnings in a titanium sleeve. Control experiments have shown negligible hardness increases with this method, indicating that contamination from oxygen and nitrogen is slight. Three cooling rates were employed in this work; these have been designated as water quenching, argon cooling (to simulate air cooling under a controlled atmosphere), and furnace cooling. The cooling rate for an argon cool is 100°C per min for the first minute, with an average cooling rate of 35°C per min over a 15-min period. A furnace cool requires about 10 hr, with an average cooling rate of 3.6oC per min during the first hour, and an average cooling rate of 1.2°C per min over the 10-hr period. Microimpact Test: The specimen adopted was based on the cylindrical Izod Type Y specimen (ASTM, E23-41T). All dimensions were reduced to half scale, including the notch radius. Specifications are shown in Fig. 1. The specimen is held vertically in an adapter and broken as a cantilever beam. Impact tests were run on a constant-velocity (11.34 ft per sec) Tinius Olsen impact testing machine with a total available energy of 100 in.-lb. Tests were made to determine the correlation between this microimpact and the standard V-notch Charpy impact test. Curves showing impact energy as a function of temperature for both impact tests are plotted in Fig. 2. Transition temperatures, when they occur, are about the same for both impact tests. All three titanium-rich materials have the same conversion factor, 10. Tensile Testing: Tensile tests were conducted on Baldwin-Southwark testing machines using the 600, 2400, or 3000 1b range. Specifications for the test specimen were taken from the 1948 edition of the ASM Metals Handbook, and are shown in Fig. 1. Strain measurements were made using an SR-4 resistance gage (Type A-7) cemented to the reduced section in conjunction with a lever-type extenso-meter. Readings on the SR-4 strain indicator were

Jan 1, 1954