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By D. W. McGlashan, K. N. Mcleod

IN the use of free bubbles with precise temperature control and continuous pH measurement, the contact angle apparatus differs from all previous equipment. Experimental procedures differ sharply from the captive bubble method1,2 of introducing the gaseous phase in the three-phase system. When freed from the tube and captured by a solid surface, a bubble more closely conforms to the spherical ideal set up by the usual mathematical analysis of surface free energy or surface tensional relationships of the forces involved. The assembled equipment, Fig. 1, departs from the usual contact angle apparatus in providing: 1) water circulation for fixing temperature, 2) instruments to measure and record pH during testing, and 3) a system for producing and using free bubbles. The apparatus allows testing over a broad range of closely controlled conditions, and the use of free bubbles gives contact angles independent of operator manipulation, which was unavoidable in the older captive bubble method. A bubble released below the specimen rises through the liquid and contacts the mineral. If the mineral is gas-avid the bubble adheres, developing a finite contact angle. Reaction cells (1), 2x33/8x5 3/16 in. ID, are of pyrex glass 5 mm thick. To prevent optical distortion, the sides are optical flats and are planed parallel to within five wave lengths of light over the entire surface. Special cement is required to withstand chemical attack and thermal shock. The cell is placed in a thermal jacket (2) made of welded aluminum. A water seal for the optical ports is made by using O-rings tightened against the flats of the cell by fine-threaded and adjustable ports, Fig. 2. In-flow water is discharged downward from a manifold located near the bottom of the cell jacket. Water overflows the weirs at each end of the cell jacket, discharging from both sides to a collecting manifold (24). A hose (26) leads the overflow water to the thermal-conditioner well (4), which is recessed to accommodate a reaction cell and two beakers (150 ml). Both the thermal jacket and the thermal-conditioner well are insulated to minimize the effects of temperature differentials. Water, discharging from the thermal-conditioner well, returns to a thermostat bath and pump (3), from which it is pumped to the thermal jacket. The thermostat bath permits temperatures to be adjusted from 1" or 2°C to 80°C and will maintain the selected temperature within 0.2ºC. An electrode support (22) groups the four electrodes (8) so that they fit conveniently into the reaction cell, Fig. 2. This assembly holds the glass electrode, the calomel electrode, the temperature-

Jan 1, 1957

By G. E. Veins

A three-phase, continuously-operated, 250 kv.a. electric smelting furnace has been installed at the Mines Branch, Department of Mines and Technical Surveys, Ottawa, for the experimental treatment of ores and by-products of interest to the Canadian mining, metallurgical, and chemical industries. In the operation of this furnace particular emphasis is placed on the accumulation of quantitative data which will be useful in determining the most suitable smelting technique and the nature of the products, and in arriving at preliminary conclusions regarding the cast of power and electrodes. The results obtained in the experimental smelting of iron, manganese-iron, titanium- iron, nickel, and chromiumiron ores, and of a number of industrial by-products, clearly show the value of such treatment for materials of this type.

Jan 1, 1957

[Allan, Andrew Thompson Creek Coal & Coal Corp., Glenwood Springs, Colo. Allen, Earl W Mine Safety Appliances, 257 Rio Grand St., Salt Lake City, Utah Allen, Louis B C. F. & I. Corp., P.O. Box 1738, Salt Lake City, Utah Allen, Thomas Chief, State Coal Mine Inspector, Colorado, Argonaut Hotel, Denver Ambler, J.B P.O. Box 591, Denver., Colo. Anderson, A. R Jeffrey Mfg. Co., Columbus, Ohio Anderson, Merlynn D U. S. Fuel Co., Hiawatha, Utah Anderson, Nephi W Books Cliffs Coal Co., Dragerton, Utah Arnston, E. K Standard Oil Co., 4601 West 26th Ave., Denver 12, Colo. Audin. Clement, Jr Paonia,Colo.]

Jan 1, 1957

By T. S. Hutchinson, C. E. Kemp

The bottom water drive analysis presented by Muskat has been extended to include fields with wider well spacings. Curves are presented from which volumetric sweepout, water-oil ratio, and rate relations may be calculated. The effects of non-unity ratios on sweepout eficiency and productivity decline have been studied by an approximate method. Also, the effect of gravity on volumetric sweepout has been approximated for a particurlar geometry. INTRODUCTION The purpose of this paper is to report work done in applying the analysis of bottom water drive reservoirs given by Muskat1 to a larger class of reservoirs, to extend this analysis to include the effects of gravity and non-unity mobility ratios in an approximate manner, and to investigate the rate of decline of productive capacity. The bottom water drive type reservoir is one where the oil is underlain by a water zone of sufficient thickness that water movement is essentially vertical. This system is defined in more detail in the appendix and a one well element is shown diagrammatically in Fig. 1. Muskat obtained solutions to the equations describing the volumetric displacement efficiency of idealized bottom water drive systems by assuming that gravity effects due to differences in density betwecn oil and water were negligible and that the mobilities of oil and water were the same. If either of these assumptions is not made, the complexity of the system makes an analytical solution well nigh impossible at the present stage of mathematical development. Coles and Stade' developed an approximation to consider these factors. The authors have refined approximations, starting with the same basic assumption, which should give a somewhat quantitative picture of bottom water drive performance when mobilities are not equal and the effects of gravity are not negligible. The results of these approximate calculations can then be used to obtain the decline in well productivity as the field is depleted.

Jan 1, 1957

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions4/ issued by the Bureau of Mines, the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1957

By Joseph Berman

The wolframite mineral series was studied to determine the effect of the FeO - MnO ratio on unit cell symmetry and thermal stability. This work was undertaken to evaluate the analytical procedures now in use for wolframite in scheelite and to aid in the development of improved methods of analysis. Wolframite grains were hand-picked, crushed, and screened; impurities were removed by selective magnetic separations using a Frantz isodynamic separator. The samples were further checked by optical spectroscopic and microscopic examination.

Jan 1, 1957

By David B. Burrows, Francis R. Conley

INTRODUCTION A prerequisite to the evaluation and management of oil properties is accurate information derived from the analysis of core samples; but reliable data, such as porosity and permeability, can result only if all oil and water have been removed from the core samples analyzed. The most common method of core cleaning used to date has been Soxhlet extraction—a somewhat static technique, which depends upon the slow diffusion of hot solvent through the core sample. Soxhlet extraction performs satisfactorily only with highly permeable samples and at best requires long cleaning periods. The centrifuge method was developed in 1951 by Continental Oil Co. to overcome the inefficiencies inherent in the Soxhlet method. The new method is basically an operation in which hot solvents are caused to flow through the samples under the influence of centrifugal force. The centrifuge unit has proved so successful that samples which formerly required days for partial extraction can now be completely cleaned in approximately one hour. The original idea was conceived in 1950 by Elmer S. Messer, whose early experiments consisted of flowing solvent over sandstone samples suspended in a revolving basket and driven by a vertically mounted vacuum cleaner motor. Results were so outstanding that more permanent units were constructed. A modified model using this basic design was recently built by Core Laboratories, Inc., and is now used regularly in their operations. DESIGN Fig. 1 shows a photograph of the two extractors routinely used to clean small core plugs in the Production Research Div. of Continental Oil Co.'s Ponca City laboratories. For illustrative purposes, the basket from one of the units has been removed, and because both extrac- tors are of identical design only one is described in the following discussion. Each extractor unit consists of a centrifuge and a solvent still. The core basket of the centrifuge is made of mild cold rolled steel 7 1/2 in. in diameter and 1 1/8 in. deep. The basket holds 18 1-in. samples (cubical or cylindrical) and is attached directly to a cone fitted to the shaft of the motor. Both the outer rim and the hollow hub of the basket contain perforations for the passage of solvent and extract. The solvent is delivered to the perforations by means of a copper tube inserted into the hollow hub. The motor is a vertical tool post grinder motor; (115 v, 5.6 amp, 0-60 cycles, AC-DC, rated at 1/3 hp). It has a rated speed of 10,000 rpm under full load and 15,000 rpm with no load. Variation of speed is obtained by the use of a variable transformer. The solvent still was constructed from one end of a stainless steel oxygen bottle by inserting a heating element, sight glass, and piping as shown on the schematic diagram, Fig. 2. The heater used was a three-position, 1,000 w, 115-v, immersion type. Intermittent flow of solvent to the centrifuge is obtained by means of a siphon bottle inserted between the condenser and the centrifuge.

Jan 1, 1957

By Lyon R. J P

The quartz-cassiterite-wolfram veins at the Aberfoyle Tin Mine, north-eastern Tasmania, form a sheeted zone about 200 ft. wide and 1,600 ft. long in slightly contact metamorphosed shales, slates and greywackes, and are associated with a cupola of aplitic granite whose top is about 1,050 ft. below the present surface. Economic mineralization persists from the surface down to a vertical depth of 1,050 ft. to 1,100 ft., dying away in the vicinity of the cupola. Down to the 9-level there is a progressive increase in wolfram content of the veins, and a decline in cassiterite content, with increasing depth.The veins are banded or zoned, with a seivedge of muscovite on the wall. Cassiterite, wolfram and sphalerite occur inside the selvedges, projecting into a core of quartz of varying width. Other sulphides form the central part of some narrow veins, or occur as clots in the quartz. The general sequence of deposition of the ore minerals was: (1) cassiterite, wolfram; (2) arsenopyrite, pyrite, molybdenite; (3) pyrrhotite (in part); (4) blende-group minerals-chalcopyrite, sphalerite, stannite, pyrrhotite (in part)-as solid solutions; (5) galena, tetrahedrite, matildite, native bismuth, scheelite; (6) marcasite and secondary pyrite, magnetite and hematite. The sequence of deposition of the gangue minerals was: (1) fluorine-bearing minerals-muscovite topaz, apatite, triplite, fluorite-more or less contemporaneous with the cassiterite and wolfram;' (2) quartz-contemporaneous with the earlier sulphides; (3) carbonates--contemporaneous with the later sulphides. The stages overlapped somewhat.The composition of the sphalerite and heat treatment experiments with the solid solutions indicate that the blende-group sulphides were deposited at about 6000 C., and cooled rapidly, so that unmixing of the solid solutions was arrested. This accords with the likelihood that the country rock temperature was not above 2000 C. Annealing experiments at between 3500 C. and 6000 C. led to further precipitation from solid solution at the lower temperatures, and to significant segregation by solid diffusion within, a week, indicating that both deposition and cooling of the ore were rapid processes-completed in a matter of days. Since the mineralizing solutions must have lost some heat during...

Jan 1, 1957

By D. K. Deardorff, Earl T. Hayes

An improved technique is described for the accurate determination of melting points of metals in the temperature range 1500' to 2500°C. The improvements consist of gradient heating and refinements in cavity preparation to obtain true black-body conditions. The melting point of hafnium, as determined by this method, is set at 2222°±30°C. This is over 200°C higher than one of the values reported earlier. Discrepancies in the previously reported values for the melting point of hafnium are explained. The melting points of zirconium and titanium are found to be 1855O±15OC and 1668°±10°C, respectively. Reproducibility of results was ±3OC. PRIMARILY, this report is being made to correct a 1975o±25oC1 value for the melting point of hafnium, and to present an improved method for melting point determination. As a matter of interest, the technique was also applied to determining the melting point of zirconium and titanium. There is a wide difference in the melting point of hafnium as reported by competent investigators. DeBoer and Fast' reported a value of 2230°±500C, and later work of McPherson, as reported by Aden-stedt, placed the melting point at 1975o±25oC. Zwikker" calculated that the melting point was 2430°C. In resolving this discrepancy, improvements were made in the procedure for determining the melting points of refractory metals in the range 1500" to 2500°C. Special techniques are necessary to determine the melting point of these metals accurately. Since the metals oxidize in air above 900oC, the determinations must be carried out in an inert gas or vacuum. Also, every known refractory contaminates them to some extent. In addition, the attainment of true black-body conditions is always difficult. DeBoer and Fast actually determined the melting point of Hf-Zr as-deposited iodide process alloys and extrapolated to 100 pet Hf. McPherson employed a tungsten wire suspension similar to that described by Schramm, Gordon, and Kaufmann,1 and used hafnium metal produced by the iodide process. There was no apparent reason for the wide spread in melting points, since the quality of the metal was very good and the work was under the direction of highly competent investigators. Retracing some of this work revealed one understandable error in the case of hafnium, and led to development of an improved technique for determining melting points of reactive metals in the range 1500" to 2500°C. Material Crystal bar hafnium, zirconium, and titanium were used for this work, with analyses as shown in Table I. The hafnium was of the highest purity that has been prepared, though not as pure as the zirconium and titanium. At the instigation of the Pittsburgh Area Office of the AEC, a special lot of Hfo2 was purified, converted to the tetraflouride, and bomb-reduced with calcium, all at the Iowa State College Laboratories. This crude hafnium metal was then refined by the iodide process at the Foote Mineral Co. All specimens were cut with a Sic wheel, ground, pickled, and dried carefully before use. Procedure General Tungsten Suspension Method—In this method, a small specimen is suspended by a fine tungsten wire in a slender, induction-heated tungsten or tantalum cylinder, all under vacuum. The melting point is determined by heating the specimen slowly while observing it with an optical pyrometer focused upon a portion of the specimen that radiates as a black body. This means that there should be no reflected radiation, either from colder objects near the pyrometer or from hotter surfaces. The induction heater would be the only hotter object and, if it is slender enough, the specimen will attain the same temperature. Often a slender hole is drilled into the specimen as a source of black-body radiation. This was the general method used by McPherson in obtaining his value of 1975°C for the melting point of hafnium. In trying to repeat this work, it was found that the points of contact between the

Jan 1, 1957

The fundamental features of the Cable Belt Conveyor are described. It consists of independent wire ropes which take the transmission load, and a special reinforced rubber belt which acts 'only as carrier of material. The first cable belt installation in Scotland is described briefly.A general description of this type of conveyor is followed by details of the rubber belt construction and the method of joining sections of belt. The drive unit, the tensioning arrangements and the power requirements are outlined.Applications of the cable belt conveyor are 'dealt with and its advantages summarized.INTRODUCTIONThe cable belt conveyor, as its name implies is a conveyor composed of steel wire ropes and a rubber belt, in which the ropes serve as transmission members, and the belt merely as a carrier of materials.Over the years it has been the ambition of engineers connected with the belt conveyor industry to develop a conveyor that would use the high tensile strength of wire ropes to transmit the stresses involved in the driving of large capacity belt conveyors. Different lines of approach have been adopted in the United States of America and in Britain. In the United States the method adopted was to introduce a large number of flexible steel cables into the rubber belt itself, in the form of a closely packed layer arranged across the full width of the belt. These small cables are packed in a nylon filled duck envelope which is incorporated in the rubber belt. This is commonly known as the steel corded conveyor belt. In Britain, a Scottish firm developed a rubber belt conveyor in which full advantage was taken of the high tensile features of wire rope, without embodying or moulding the wire rope into the rubber belt, so that the two wire ropes and the rubber...

Jan 1, 1957

By Alla D. Mah

Titanium forms several compounds with oxygen and also is able to dissolve interstitially about 33 atomic percent of oxygen. Starting with titanium dioxide, reduction becomes increasingly difficult as oxygen is removed; and the final step, be reduction of the titanium-oxygen interstitial solutions, is by far the most difficult. The possibility of reducing titanium oxide, or of purifying titanium containing oxygen, by treatment with certain more volatile metals has been a subject of considerable interest. Theoretical appraisal of the limitations of this possibility, however, has been hampered by lack of adequate information on the thermodynamic properties of the titanium-oxygen solutions. The purpose of the present work was to remedy this difficulty by expanding the thermodynamic knowledge regarding these solutions. The experimental work involved three types of calorimetry and furnished the following information: (1) Heats of formation of 11 titanium-oxygen solutions, in the range of 0 to 10 wt.-percent oxygen, were determined at 298.15° K. As a byproduct, an improved value of the heat of formation of rutile was obtained, which, in turn, led to improved values of the heats of formation of the lower titanium-oxygen compounds. (2) Low-temperature heat-capacity data and entropies at 298.15°K in were determined for 2 representative titanium-oxygen interstitial solutions. (3) High-temperature heat-content data were obtained for 2 titanium-oxygen interstitial solutions to about 1,600° K.

Jan 1, 1957

By H. E. Lee, D. Ingvoldstad

AT Bunker Hill the original charge storage and preparation system was installed in 1917 to accommodate lead-silver gravity mill products. Only minor tonnages of wet fines such as vanner and flotation concentrates were received. Charge flux and diluent requirements were provided by an ample supply of siderite middlings and coarse lime-rock. While oversize material was crushed through %-in., the use of roll crushers in series resulted in a more or less granular, free-running charge of adequate porosity. Under such conditions, receipts could be proportioned directly from receiving bins, and suitable blending was obtained by passing the resultant layered composite through a small Stedman disintegrator. This elementary system served well for production and smelting of an extremely lead-rich sinter, in the low column blast furnace. Here sinter physical quality is less critical, and appreciable quantities of raw flux and oxidized ore may be charged directly to the blast furnace without seriously impairing furnace capacity. Prior to 1938 the relative proportions of zinc receipts were low and extraneous flux requirements at a minimum. However, subsequent war-inflated zinc demands brought marked increase in fine concentrate and slimy zinc leach residue receipts and an abrupt introduction to smelting a more refractory zinciferous charge. The higher temperature demands of the more refractory zinciferous charge required a higher smelting column and the higher column, in turn, rendered the blast furnace less receptive to improperly prepared feed. Inadequate presinter processing facilities prevented the production of acceptable sinter, and blast furnace production declined to 50 pct of former capacity. In view of a prevailing contention among lead metallurgists as to the deleterious action of high zinc slag on blast furnace capacity, it was natural to overstress this factor and to concentrate on possible changes in furnace design. Another interpretation was that primary correction should be sought through expanded sintering facilities. This divergence of opinion, together with the extreme material shortages of the 1940's, delayed corrective

Jan 1, 1957

By Herty, C. H.

No attempt will be made here to review the previous work done by investigators on the general subject of inclusions, because it was discussed sufficiently in an early cooperative bulletin of this series (No. 36, 1928), and reference was then made to general bibliographies. The work described in this present bulletin deals directly with the study of the mechanism of deoxidation of steel with aluminum and the formation of inclusions containing alumina. Unquestion- ably, such inclusions are encountered in most steel-making practices and little has been done to determine their characteristics. Aluminum is used to ensure rapid deoxidation during the solidification stages of the steel. For this reason the possibilities of inclusion elimination are slight and alumina-containing particles will undoubtedly be present in the ingot. Besides this common practice, aluminum is often used in the ladle with other deoxidizing agents such as silicon and manganese. Ladle additions of aluminum are made to rimming steels to obtain the correct partial deoxidation desired in this type of steel. In killed steels the aluminum is added to ensure soundness, as far as blowholes are concerned, in the ingot. In either rimmed or killed steels, alumina or alumina-containing inclusions are found therein, the amount and type depending on the oxidation of the metal, the amount of aluminum added, and the addition of other deoxidizers.

Jan 1, 1957

The first metal-mine accident-prevention course was prepared and published in 1942--45 as a series of seven miners' circulars (Nos. 51-57). The scope of the course has been broadened, revised, and brought up to date, and it is being published as a similar series of seven miners' Circulars (Nos. 51-57, revised) on accident prevention in metal and nonmetallic mines. These circulars are: Accident Statistics (Miners' Circular 51), dealing with general statistics on accidents and injuries at metal and nonmetallic mines, including causes, costs, and the uses of investigations and reports of all accidents.

Jan 1, 1957

By G. W. Birge

As a part of its overall program of coal carbonization, the Bureau of Mines is studying the coking properties of coals that may be used for metallurgical purposes. The objectives of this study were given in detail in a previous report.2/ The inherent suitability of coal for metallurgical use depends primarily on (1) chemical composition, (2) preparation characteristics, and (3) carbonization behavior. The first two factors, as well as the available reserves, are considered in selecting coals for carbonization tests. The selection of coal beds in Westmoreland County for coking tests was based, in part, on estimates of the coal reserves by Dowd,3/ who estimated the recoverable reserves in beds 28 inches or more thick, in thousands of tons, as follows: [ ]

Jan 1, 1957

By Larry Kaufman, Morris Cohen

THE solid phase equilibria' and the martensitic transformation in the iron-nickel system have been the subject of considerable study. In addition, there have been numerous investigations on the calorimetric and thermodynamic properties of iron-nickel alloys. The purpose of the present work is to extend the existing information concerning the martensitic reaction in the iron-nickel system, and to develop a general thermodynamic treatment which will encompass the equilibrium and non-equilibrium phase

Jan 1, 1957

By H. N. Dunning

A comprehensive production research program, now in progress at the Petroleum Experiment Station of the Bureau of Mines at Bartlesville, Okla., includes studies of the displacement of petroleum from sand by detergent solutions. An earlier report (12)2/ presented the results of an extensive research program to determine the value of detergents as floodwater additives. This report presents later results of the detergent-testing program (13, 17). Although water-flooding methods and controls are constantly being improved to increase the production of oil from secondary-recovery operations, considerable crude oil commonly remains.in place after a water flood has been terminated. Therefore, the possibility of improving the efficiency of a waterflood by the use of detergents is of increasing interest. The effects of many substances on the efficiency of water flooding have been investigated in laboratory studies (5, 11, 13, 17, 19, 24). Of the various sub-stances tested, only surface-active agents were consistently effective in removing oil from sand. Results of laboratory studies presented in earlier reports (9, 11, 12, 13) show that many detergent solutions effectively displace petroleum from sand surfaces under varying conditions encountered in centrifuging, manual and mechanical agitation, ultrasonic vibration, and imbibition.

Jan 1, 1957

By John J. Gilman

BECAUSE of their layerlike structure, zinc crystals exhibit strong anisotropies for almost all physical and chemical properties. This should, and indeed does, greatly influence the plasticity of zinc for various crystal orientations. At low temperatures, the investigator of this plastic anisotropy is plagued by the great variety of deformation modes that operate. However, at high temperatures (250° to 419°C) only two deformation modes predominate: basal (0001) and prismatic (1010) glide. Furthermore, since strain hardening is virtually absent at high temperatures, the plasticity for these two modes of deformation can be very simply described by means of two equations of state. It is the purpose of this paper to describe the experimental behavior of basal and prismatic glide in zinc crystals, and to interpret this behavior in terms of other physical properties (in particular, the thermal expansion coefficients and the elastic constants) using the theory of dislocations. Fig. 1 defines the two planes of the zinc structure that will be discussed. Glide occurs very readily on the basal planes at all temperatures, and there is a very large literature on this subject. Much of the literature has been reviewed by Schmid and Boas;' it will not be reviewed here. Kolesnikovl was the first to show that if basal glide is circumvented by stressing a zinc crystal parallel to the basal planes (giving zero shear-stress on the basal planes) then, at temperatures above about 320°C, glide on the first-order prism planes occurs. His results have recently been confirmed by Cahn, Bear, and Bell." These previous workers have established the existence and crystallographic elements of prismatic glide; the present paper is concerned with the stress, strain rate, and temperature relations of prismatic glide as contrasted with basal glide. Experimental Methods The crystals were square ones, 6x6 mm, that had been grown in precision Pyrex tubes by a method that is described in detail elsewhere.' Most of the crystals were 99.999+ pct Zn (New Jersey Zinc Co. CP grade). Some were alloyed with 0.1 -+-0.005 atomic pct Cd, and chemical analysis showed that almost all of the added cadmium persisted through the crystal-growing process. For measurements of nonbasal glide, crystals were oriented with their basal planes parallel to both the rod axis and one of the flat faces of the square cross section. However, the orientation of the close-packed directions [1210] with respect to the rod-axis was variable. For basal glide measurements, the angle between the basal plane and the specimen axis was 35". The orientations were measured by the Gren-inger back-reflection X-ray method. The problem of finding a suitable method of gripping the crystals was the most serious experimental obstacle that arose. Because of the large plastic anisotropy of zinc, the usual gripping methods were unsatisfactory. Some methods that were tried were: high melting-point solder, making heads on the ends by locally melting a crystal, and electroplating nickel on the ends to form enlarged portions. For all these methods, the regions of the grips were weaker than the crystals themselves. Finally, two methods were decided upon: bend tests and direct machining of tensile specimens. In the bend tests, specimens were loaded as simple beams so that gripping was not a problem. The beams were 1 in. long and the axis of bending was parallel to the hexagonal axis of the crystals. For the crystals that were machined into tensile specimens, brass bars with slots in them were used to support the crystals, and thereby minimize the distortions due to machining. The crystals were glued into the brass bars with plastic cement which was later dissolved away with acetone. See Fig. 2, left. No clamps were used near the crystals and the machining was done using a milling machine with a fly-cutter. The tool bit was very sharply pointed to minimize burnishing. The feed was less than 1 mil per cut. The depth of cut was 2 mil for roughing cuts, and % mil for the finishing cuts. This machining method produced surface layers of tiny recrys-tallized grains only 2 to 3 mil deep, and the bodies of the crystals were not measurably disturbed. After the crystals had been machined and removed from the brass holders, they were chemically polished until about 5 mil had been removed from all their surfaces. The polishing reagent consisted of equal parts of concentrated HNO,, 30 pct H3O and ethyl alcohol; it is described in detail elsewhere." A typical crystal is shown in Fig. 2, right. The I-shaped faces are normal to the hexagonal axis of the crystal; otherwise the projections at the ends would simply shear off when the crystal was loaded. The cross section in the 2?-in. gage length is 0.215x0.115 in. It was found that the polished

Jan 1, 1957

By F. D. Everett

The exploration work on a seleniferous tuff deposit near Lysite, Wyo., was confined chiefly to an area of approximately 1 square mile selected on the basis of prior examination and sampling work by the Bureau of Mines. This area was superficially explored by digging and sampling over 2,000 feet of trenches and 15 test pits. The surface sampling indicated that the deposit might contain a multimillion-ton reserve of easy-to-mine volcanic tuff assaying more than 0.01 percent Se. Later, 11 holes, ranging in depth from 57 to 135 feet and totaling 929.4 feet, were drilled under contract using a dry rotary drill. Samples for assay were cut at 5-foot intervals or at noticeable physical changes in the formation being drilled. Of the 206 samples assayed from the drilling, only 8 contained more than 0.005 percent selenium, and 2 of these assayed as high as 0.012 percent Se. Chemical analyses of samples obtained from six holes drilled by the Nugget Coal & Timber Co. to the south of the area explored by the Bureau of Mines showed that no selenium-bearing formations were encountered in that work. Two of 72 samples taken from 42 validation pits dug by claim holders contained more than 0.005 percent selenium. The exploratory work established that the selenium mineralization is erratically distributed in small irregular bodies and is not confined to any one tuff bed. Because of the lack of correlation between the infrequent showing of low-grade tuff, neither the extent nor grade of the reserves could be calculated.

Jan 1, 1957

By R. M. Goldhoff, J. W. Spretnak, R. Speiser

IT has been observed by Grange and Garvey' that the homogenization of boron-treated steels could lead to complete elimination of the hardenability effect caused by boron. The experimental conditions leading to this conclusion involved the heating of steel specimens with and without boron at 2350°F for 24 hr. To prevent oxidation and decarburization, the specimens were encapsulated under vacuum in silica tubes. This observation of permanent deterioration of boron effect was noted in both a 0.63 pct plain carbon steel and a 0.25 pct C low alloy steel, both of which had been treated with ferroboron and homogenized at 2350°F for 24 hr. In another series of boron-treated steels which had been homogenized for shorter times, the effect was to reduce, but not completely eliminate, the boron effect. Under these circumstances, it was presumed that longer heating times would cause permanent deterioration of the boron effect in this series of steels also. Since the characteristic grain boundary constituent could not be formed in any of these steels after homogenization, it was concluded that possibly boron was being converted into an ineffective form through chemical combination resulting from prolonged heating at high temperatures. Assuming the validity of this observation, a series of experiments to establish the relationship between temperature of homogenization and kinetics of deterioration was contemplated. Initially an attempt was made to reproduce the results just described. For this purpose commercial lots of AISI 8640 and AISI 86B40 steels were used. The analyses of these steels appear in Table I. Hardenability evaluation was on the basis of the hardness of normalized sections. Grange and Garvey' pointed out that these steels are air hardening to some extent and such a technique can be used. For these tests the specimens were held for 20 min in a salt bath at 1600°F and then cooled in still air. Several evacuated silica capsules containing pairs of the test steels were made up and heated for 24 hr at 2350°F. A number of failures occurred among these capsules, but evaluation of the specimens successfully treated indicated a complete deterioration of the boron effect. However, examination of the surface of the treated specimens showed that some reaction, probably with the silica tube, had taken place, since none of the specimens was bright. One further test was made at 2350°F for 12 hr, using a pair of specimens wrapped in tantalum foil prior to encapsulation. These specimens appeared bright after treatment, and their hardenability evaluation showed that no deterioration had taken place. Since these steels are extremely sensitive to de-boronization at high temperatures and particularly at long times of holding, the experimental observations raised some doubt as to the real occurrence of the permanent deterioration effect. To resolve this question an experiment was undertaken in which the high temperature portion of the treatment was completed in vacuum. For this purpose a molybdenum wound resistance furnace capable of maintaining good vacuum was used. All the pertinent accessories to this furnace were machined from molybdenum stock in order to withstand the high temperature involved in the experiment. With this equipment a temperature of 2400 °F was obtained and held under a pressure of 5x10-" mm Hg for 24 hr. A specimen of each of the two test steels was suspended in the furnace and both were heated simultaneously. Temperature was measured with a standardized Pt—Pt-13 pct Rh thermocouple, whose millivoltage at 2400°F was extrapolated from the standardization equation, good up to 2200°F. The complete evaluation of these specimens is shown in Table 11. The hardness values attained by each steel after normalizing, both before and after the prolonged high temperature treatment, remain the same. A microscopic study of the decomposition products present in the microstructures of specimens at various points in the heat treatment correlated with the hardness values observed. It seems that no permanent loss of boron hardenability effect occurs, at least in these Grainal-treated steels, when deboronization is circumvented. Acknowledgments This work was conducted under the sponsorship of the Aeronautical Research Laboratory, Wright Air Development Center, under Contract No. AF 18(600)-94, and their support and permission to publish is gratefully acknowledged. A note of thanks is also extended to the Republic Steel Corp. for supplying the materials used in the work. References ' R. A. Grange and T. M. Garvey: Factors Affecting the Harden-ability of Boron Treated Steels. Tro.ns. ASM, 1946, vol. 37, p. 136.

Jan 1, 1957