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By E. W. Gieseke

Coal preparation men today are confronted with problems brought about by changing feed characteristics. The size consist of the coal going to preparation plants has been getting finer and finer. In order to handle these sizes economically, operators are turning to Notation. American Cyanamid Co., in an effort to enable coal flotation plants to produce efficiently at maximum quality and capacity, wnducted experiments which demonstrated that synthetic flocculants are useful for increasing the capacity of coal and refuse filters and for clarifying coal and refuse slurries, and a wetting agent is beneficial in reducing the moisture content of filter cake. Coal preparation men are today confronted with problems brought about by the changing coal markets, changing feed characteristics, and ever increasing labor and supply costs. Small mines are finding it difficult to exist, and the larger mines are rapidly converting to fully mechanized and automated operation to survive. The size consist of the coal going to preparation plants has been getting finer and finer, and the problems facing the preparation plant personnel are growing larger and larger. Facilities can be provided to handle this plant feed in new plants, but the problems are generally not so simple in existing plants where equipment must often be used to perform tasks far beyond its rated capacity. In addition, various state conservation departments, water commission boards, and other Federal and state agencies are endeavoring to eliminate stream pollution. These problems, and many more not mentioned, have been forced on the preparation engineer for reasons of economy and the public interest. In the matter of stream pollution, a determined effort is being made by the coal industry to cooperate with the Federal, state, and local agencies. Economists predict it will be necessary to produce 600 million to 700 million tons of coal by 1970. Bear in mind that the greater proportion of this increased tonnage will have to be processed in existing plants, and you get an idea as to the problems facing the preparation engineer. Methods presently in use for preparing fine coal do an acceptable job down to 48 to 100 mesh. A very large percentage of the - 48 or -100 mesh fraction of the tonnage of coal produced now is being sent to settling ponds or sold at a low figure for reason of quality. This has caused operators to turn to flotation. Building settling ponds and impounding fines is a costly and, at times, impossible method of handling these sizes. Recently a number of flotation plants have been installed to beneficiate material finer than 48 mesh, and these plants have demonstrated that flotation can be successful and increase the plant realization. Coal is a low cost commodity and processes for its beneficiation must be low in cost. Flotation is such a process. It is easily adapted to handling fine coal, requires very little supervision when properly installed, and is economical to operate. Flotation separates coal from refuse and fine clay. For reagents, several combinations are used. Some

Jan 1, 1962

By Nicholas J. Grant, Noboru Komatsu

Metallographic and X-ray studies were made of oxide dispersion strengthened Cu-12 vol pet SiO2 and Cu-3.5 vol pet Al2O3 alloys following time exposures at temperatures approaching the melting. point of the matrix metal. Changes in hardness, oxide particle size and crystal structure were studied to determine the time-temperature stability of these alloys. An interpretation of the mechanism of oxide agglomeration is proposed. One of the most striking features of dispersion strengthened metal-metal oxide alloys is their stability at elevated temperatures, both with respect to recrystallization and maintenance of mechanical properties after exposure at high temperatures. A small amount of work has been done on the re-crystallization phenomenon in dispersion hardened metal-metal oxide alloys'l and several theoretical treatments have been advanced regarding the stability of these alloys by Lenel and Ansell,8 and by Grant and his co-workers.9, 10 This paper reports on metallographic and X-ray studies following various heat treatments of Cu-AI2D3 and Cu-SiO2 alloys at elevated temperatures and the effect of subsequent cold work on the recrystallizalion temperature. An interpretation of the recrystallization behavior of this type of alloy, based on the decomposition and agglomeration of oxides, is proposed. EXPERIMENTAL PROCEDURE Cast ingot bars of copper-1.59 pet Si and Cu-0.77 pet Al, 7/8 in in diam, were annealed in argon for 80 hr at 1000CC for homogenization. The homogenized rods were machined into fine chips and ball milled. Milled particles in the range minus 20 to plus 60 mesh were separated for internal oxidation. The internal oxidation was accomplished by the same method used by Preston and Grant,9 except that the oxidalion temperature for the Cu-Si alloy was 750°C, and for the Cu-A1 alloy was 800°C. These powders were then hydrogen-reduced at 450°C, compacted in a copper container, evacuated at room temperature to 0.04 µ, and sealed for extrusion. They were extruded at 1400°F (760°C) with a ram speed of 55 in. per min for an extrusion ratio of 15.6 to 1 to give a rod 0.38 in. diam by about 3 ft long.

Jan 1, 1962

By Robert L. Fleischer

A well known but unexplained experimental fact is the observation1 that aluminum shows a pure <111> wire texture, in contrast with other fcc metals, which have a mixed <100> <111> texture at moderate reductions. A possibly related single crystal observation on aluminum is the following:2 under tensile deformation <111> single crystals are stable (maintain their original axial orientation), while <100> crystals are unstable at room temperature and become stable at lower temperatures. This suggests that at room temperature, as proposed by Yen and Hibbard,3 the single <111> texture obtains be- cause <100> orientations are unstable in the poly-crystal. It also implies that for wire drawing at lower temperature a <100> component of the texture might be expected since that orientation is then stable. This possibility has been examined by wire drawing at temperatures near 77°K. The apparatus was designed to be used with an existing draw-bench, a steel trough acting as die holder and containing sufficient liquid nitrogen to immerse the wire entering the die. The trough is insulated by a styrofoam container to prevent excessive boiling of the bath. The wire emerging from the die enters a polyethylene tube, into the far end of which the grips are inserted. Liquid nitrogen is funneled into the tube to maintain the low tem-

Jan 1, 1962

By M. E. Tyrrell

Magnesia spinel (MgO.Al203) recovered from dusting slags in the system MgO.Al203-2Ca0.SiO2 is in the form of single crystals most of which will pass 35-mash. This investigation was undertaken by the Bureau of Mines to evaluate the concentrates as a refractory raw material. Three specific types of refractory bricks were studied: (1) dense, (2) lightweight bubble, and (3) insulating. Test specimens ware fabricated 1 by dry pressing, fired to 1,675° C., and tested by procedures common to the industry. The concentrates produced a refractor, having satisfactory density and mechanical strength; however, spinal is sensitive to thermal shock and the possibility of producing a spall-resistant brick using aggregate of such small grain-size must be considered remote. Lightweight refractorias fabricated of spinel bubbles were the most promising of the types tested. They were 30 percent lighter in sight than the dense refractory, their mechanical strength was good, and definite superiority in thermal shock resistance was indicated.

Jan 1, 1962

By Philip D. Anderson, Ralph Hultgren

Heat contents of extremely pure iron were measured over the range 300"to 1433"K, using a diphenyl ether calorimeter. Results from three samples containing widely differing impurities agreed with one another and with Previously reported results at higher temperatures (1184 ° to 1809°K) by Olette and Ferrier. From these data a table of heat contents of iron has been Prepared which is believed to be more accurate than those previously available. CP values have been derived which are consistent with these heat contents, with the best experimental Cp data, and with the thermodynamic conditions of equilibrium between bcc and fcc iron. The opinion is expressed that low-temperature extrapolations of presently known Cp values for y-Fe are not reliable. It would seem that the thermodynamic properties of iron, which is by far our most important metal, should have been well established long ago. This is not the case, however. As discussed by Olette and Ferrier,&apos; there is objection to every earlier heat content measurement. While the best true Cp determinations agree well at temperatures below the Curie point, there is wide divergence at higher temperatures. Several investigators have examined available data and attempted to calculate thermodynamic functions for iron that are consistent with the two equilibrium temperatures of bcc and fcc iron. The two primary efforts were those of Austin&apos; in 1930 and Darken and smith3 in 1948. The recommended values differ considerably; integration of Austin&apos;s Cp values leads to a heat content at 1100°K which is 300 cal per g-atom higher than the value recommended by Darken and Smith. The compilation of Fisher4 in 1949 was based on the selection of Austin. In 1956, Weiss and Tauer obtained yet another set of values by resolving Cp values into components due to dilation, lattice vibration, electronic excitation, and magnetism. The magnitude of contribution by each component and its dependence on temperature was estimated by semiempirical means. Their values are not self-consistent in that they do not form smooth curves when plotted vs temperature; moreover, their calculations cannot easily be repeated since they do not give the values of some of the parameters used. Clearly, experimental values for iron were in a most unsatisfactory state. The presently described measurements of the heat content of iron were therefore undertaken, covering temperatures as high as 1433°K. While the work was in progress, the high-temperature (1193" to 1789"K) heat content measurements of Olette and Ferrier&apos; were published; in the region of temperature overlap the present results agree with Olette and Ferrier well within experimental accuracy. It is believed that the present results, combined with those of Olette and Ferrier, provide for the first time a reliable set of heat contents of iron from room temperature to the melting point. From these data, guided by available Cp measurements, it proved possible to derive Cp, entropy, and free energy function values for @-iron from room temperature to the melting point, and for y- iron in the temperature region of its stability. Exhaustive study led to the conclusion that extrapolations of y-iron functions to room temperature were not reliable enough to be useful; hence these have been omitted from the tables. EXPERIMENTAL Materials. Three samples of extremely high purity iron from different sources, containing widely different impurities, were measured. The first of these, designated "Chipman", was kindly supplied by Dr. K. K. Kelley of the U. S. Bureau of Mines from a lot which was made many years ago by Dr. John Chipman of the Massachusetts Institute of Technology. The second, designated6&apos;Teddington", was supplied by the National Physical Laboratory, Teddington, England, from a lot zone-refined by them. The third sample, designated "Irsid", was supplied by the Institute de Recherches de la

Jan 1, 1962

By G. F. Dillion, A. F. Armington

THE present method for the ultrapurification of boron involves the formation, distillation, and decomposition of boron tribromide.&apos; However, the boron tribromide prepared contains several impurities in the ppm range, even after distillation. Some of these impurities, notably carbon, can be reduced after decomposition by zone refining. In this study, a comparison of the purity of boron tribromide at various formation temperatures is presented. The apparatus employed consisted of a bromine flask connected to a 22 mm ID horizontal quartz reaction tube packed with amorphous boron powder, which was in turn connected to a receiving flask cooled with an ice bath. Argon was used as a carrier gas. The approximate rate of passage of bromine to the reaction tube was 25 g per hr. The reaction was first investigated at several temperatures in order to determine the lowest temperature necessary to produce a colorless product which was assumed to be an indication of complete reaction of the bromine. The lowest temperature found in this study was 420oC. The amount of impurities found in the boron tribromide at various formation temperatures is shown in Table I. The data presented are emission spectroscopic results of boric oxide produced by the hydrolysis of 2 to 3 g of boron tribromide in 10 ml of distilled water. After hydrolysis, the samples were dried several hours on a hot plate. Assuming equilibrium conditions in the reactor, one can make approximate thermodynamic calculations estimatling the completeness of reaction of bromine with boron and its impurities at various temperatures. Data for these calculations were taken from Rossini,3 and must be taken as approximations since the T?S factor was not included in the calculations. The results of such calculations indicate that, with the exception of carbon bromina-tion, all impurities would react almost to completeness (> 99 pet) at all temperatures between 400" and 900oC. In the case of carbon, which cannot be accurately analyzed spectroscopically, it is estimated that only about one sixth as much carbon tetrabromide would be formed at 400" than at 900°C. Since some marked reductions in impurity content were observed at the lower reaction temperature which would not be predicted by thermo-

Jan 1, 1962

By A. Boltax

The effect of cold work on the electrical and magnetic properties of solution-treated and aged Cu-Fe alloys was studied. The electrical resistivity of solution-treated and of aged Cu-1.7 wt pct Fe samples increased by up to 25 and 140 pct, respectively, follozcing a 55 pct reduction of area. The principle contributions to the increase of resistivity of the solution-treated and aged samfiles are examined. Measurements of the .saturation induction, coercive force, and stacking fault Probability are also reported. 1 HIS paper is the second in a series which examine the behavior of the electrical and magnetic prop- erties of Cu-Fe alloys. The first paper1 was primarily concerned with the effects of thermal treatment whereas the present paper examines the effects of cold work on solution-treated and aged Cu-Fe alloys. The effects of cold work on the transformation of the coherent fcc iron precipitate to the ferromagnetic form2 and the coercive force and remanence3 have already been described, but the unusually large increases in resistivity (up to 220 pct) which occlir with cold work have not been reported previously. EXPERIMENTAL METHOD The methods used for alloy preparation, heat treatment, and electrical and magnetic measurements are described elsewhere.1 The specimens, initially 4-in. lengths of 0.0625-in. diam wire, were cold worked by swaging in hardened steel dies. Following each reduction, the samples were etched lightly in hydrochloric acid to remove surface con-

Jan 1, 1962

By M. L. Bowser

Pulse-forming circuitry is described for use in explosives research that requires precise synchronization and control of events in order to investigate detonation parameters. Included are pulse generators for oscilloscope sweep control, counterchronograph actuators, and a raster-type oscillographic method for the determination of velocities of detonation that are applicable to studies on solid, liquid, and gaseous detonations. INTRODUCTION Prom time to time, requests have been received for information on electronic circuitry used in explosives work at the Explosives Research Laboratory, Bruceton, Pa. The methods used are not entirely original;4 5 6 however, modifications of earlier techniques and some novel design aspects have resulted in time-tested methods that warrant a more detailed description.

Jan 1, 1962

By W. M. Dressel

A simple field test for detecting the presence of germanium in rocks, coals, and flue dust has been developed by the Bureau of Mines. The method consists of dissolving germanium from the samples by either acid or fusion treatment methods, adding a few drops of hematein or phenylfluorone dye, and extracting the resulting colored complex with carbon tetrachloride. INTRODUCTION Germanium is obtained commercially as a byproduct of zinc production, as a coproduct of base-metal refining from germanium-bearing mineral, and as a recovered product from the ash of some coals. The growing use of germanium in the electronics industry has increased demand for this semiconducting metal to the extent that an intensive search for new sources of supply is necessary.

Jan 1, 1962

The Bureau has published much data on sulfur (4, 15, 23)3, most of it dealing with national or international aspects of the sulfur industry. Little information, however, is available on sulfur marketing in specific States or areas, Therefore, the Bureau has conducted a survey of the resources, production, consumption, and economic future of the sulfur and sulfuric acid industry in States of the Central and Southern Rocky Mountain area - Wyoming, Colorado, Utah, Arizona, and New Mexico - and in the Northern Plains States - North Dakota, South Dakota, and Nebraska, even though these States do not represent an economic or marketing unit. The purpose of this survey is to review the demand for sulfur and primary sulfur compounds that draws upon the natural resources of the region, to discover opportunities for better use of these resources, and also to analyze and evaluate the patterns of consumption, sources of supply, and other factors that affect the demand for these mineral products. While this survey stresses the economic and marketing phases of the industry, a complementary report (32) emphasizes the resources of sulfur in Wyoming, Colorado, Utah, New Mexico, and Arizona.

Jan 1, 1962

By E. W. Davis

This paper deals with the role of the Maintenance Department in a milling operation; specifically, the Mines Development, Inc., processing plant at Edgement, South Dakota. The goal of very maintenance department is the smooth and uninterrupted operation of the plant it serves, To achieve this goal, maintenance men adapt various features and procedures into a program designed to fit the characteristics of their particular plant operation. A few of the basic elements of a sound maintenance program are: 1, A periodic preventive maintenance schedule. 2, A systematic inspection and lubrication procedure. 3. A training program for maintenance personnel. 4 A good equipment-history file system, 5. A carefully planned spare parts inventory.

Jan 1, 1962

By L. O. Bacon

This Bureau of Mines report summarizes the results of laboratory work in the design of instrumentation for obtaining the dynamic tensile strength of rock at minimum loading. Minimum loading is defined as the lowest tensile loading by pulse reflection to cause fracturing. The instrumentation for obtaining dynamic tensile strengths of rock cores evolved into the use of a compressed-air pellet gun to impact one end of a rock core, suspended by wires, at increasing increments of air pressure. Maximum strain was measured on most or all of the impacts, and the strain at fracture of the core was obtained by extrapolating the pellet velocity-strain curve to the pellet velocity at fracture. Stress at tensile fracture was obtained from the maximum s train, and the dynamic Young&apos;s modulus was calculated from the rod velocity by using simple rod theory.

Jan 1, 1962

By Elmars Ence, Harold Margolin

The titanium-aluminum system has been investigated in the composition region 0 to 34 pct Al in the temperature range 800" to 1450°C. The phases encountered in this region were: a,ß, TiAl3, The reactions observed are as follows: 13 ; L - 6T. A1, 0 (15 pct Al) + 6 (18 pct Al) - yTi Al (16.5 pct Al) at -1170°C andP (7 pctpct Al) + y (9.2 pet Al) - ah(9 pct Al) at - 1060°C. A eutectoid reaction: y — a +d belm 700°C is postulated. THE Ti-A1 system has been the sub.ect of a number of investigations. Several of these1-3 have indicated extensive solubility of A1 in both a and ß titanium. Ence and Margolin, as a result of work on the Ti-A1-0 system:&apos;5 have shown that the a solubility ofalumi-num is considerably restricted, and found that a compound, Ti2A1 existed in the region formerly designated as Q a This structure was identified as hexagonal with c/a = 0.803. Pietrokowsky confirmed the existence of this phase7 and pointed out that the structure was isomorphous with Ti3Sn.8 Although the existence of Ti,A1 has been confirmed by others,9-12 there has been considerable disagreement regarding the composition and mode of formation. A detailed reinvestigation of the Ti-A1 system has been published by Sagel et al.13 The tentative diagram indicated two phases, a, and e, occurring in the former all a region. The a, phase has the same structure as Ti2A1 and was indicated as having a broad region of solubility. Epsilon, a tetragonal phase, was shown to form within the a, solubility region. AS a result of unpublished work,14 Ence and Mugy3 olin disagreed with the interpretation of Sage1 et al., although some common features existed. The present study was conducted in an attempt to clarify prevailing uncertainties. EXPERIMENTAL PROCEDURE Alloy Preparation—Alloys were prepared from iodide titanium (99.9 pct Ti with less than 0.01 pct Zr) or Bureau of Mines electrolytic titanium (BHN-73) and high purity aluminum (99.99 pct). Alloys were arc-melted in argon or helium atmosphere as 15-g buttons in the composition range up to 34 pct Al. Depending on need, alloys were made in increments varying from 0.25 to 2 pct Al. Up to five 15-g buttons of some compositions were made. Weight losses during melting did not exceed about 1 pct of the charge and chemical analysis revealed that both titanium and aluminum were evaporated. In general, nominal and analyzed compositions agreed within 0.5 pct and therefore nominal compositions were used in plotting the data. Unavoidably, some overlap of composition occurred, particularly where small increments of A1 were used. The small increments were primarily used to obtain alloys which would fall into the narrow a -, r region and this purpose was achieved. In general, the data obtained from Bureau of Mines base titanium and iodide titanium alloys were in agreement. Forging—Both as-cast and forged samples were employed. Samples were heated for hand forging by an oxygen-hydrogen torch to the region 1200" to 1300°C. A titanium anvil and cover plate were used to prevent any iron pick-up and consequent formation of a low melting point compound. Frequent reheating kept the temperature in the desired range. Under these conditions, alloys containing up to 15.5 pct could be successfully forged. To check on the depth of contamination, forged alloys were heated slightlybelow the ß transformation temperature. Metal was removed to a depth below the contaminated surface so revealed, and the subsequent results obtained from these samples agreed closely with those secured from as-cast material. Heat Treatment—Prior to heat treatment, all alloys were vacuum annealed to remove hydrogen. Samples

Jan 1, 1962

By J. W. Rutter, K. T. Aust

In previous studies of grain boundary migration in zone-refined lead, the authors used bicrystal specimens consisting of a striated crystal which was grown from the melt, and an adjacent striation-free crystal, introduced by artificial nucleation and growth.1 While this method permits the study of the motion of individual grain boundaries, it does not provide control of the relative orientations of the grains. The present note will describe a technique for controlling the orientations of the two crystals in this type of specimen. The technique consists essentially of placing a striated crystal and a striation-free crystal of controlled orientations end-to-end in a graphite trough, then melting a short zone at the junction of the two crystals and allowing it to freeze to form the desired grain boundary. The apparatus used to carry out this process is illustrated in Fig. 1. It consists of a trough milled from high-purity graphite,with grooves in the underside for the placement of thermocouples. The graphite piece fans out on one end at the level of the bottom of the trough; the sides of the trough are completed in this region by the attachment of a mating plate with a slot cut at any desired angle to permit reorientation of the crystal placed at this end of the assembly. The joint between the crystals is made at or near the point where the slotted plate joins the rest of the trough. The thermocouple slots are deepened in this region so that the thermocouples are separated from the melt by only 1/32 in. of graphite. An induction heater, with suitable temperature control, is used to obtain the molten zone. The two single crystals used are first chemically polished in a solution consisting of eight parts glacial acetic acid and two parts 30 pct hydrogen peroxide. They are then placed in the trough with the ends to be joined at the position of the thermocouples. Next, cooling is applied to the two crystals by means of air

Jan 1, 1962

By E. J. Ostrowski

The history of ironmaking dates back to 4000 BC when an open forge was used to produce a sponge iron from a heap of ore and charcoal. Even at this early date, man recognized the need for a fuel and a reducing agent. As time passed, man developed new methods of producing iron; however, these developments were centered on the mechanical aspects, and as a result, a furnace evolved which is now known as a blast furnace. During this period of evolution,&apos; man struggled with the only fuel he knew - charcoal. Some 5600 years passed before any attempt was made to use coal as a fuel for the blast furnace. The use of coal had its beginning in 1619 when Dud Dudley of England first attempted its use in the blast furnace; as a-fuel and as a reducing agent. Coal charged to the top of the blast furnace was not satisfactory. The volatile matter of the coal choked the flues, and also the poor, strength qualities would not support the weight of the ore. Breaking up of the coal compacted the stock column to an impervious mass. One hundred and sixteen. years later in 1735, Abraham Darby of England introduced coke as the fuel and reducing agent in the blast furnace. The acceptance of coke as a fuel for the blast furnace was not spontaneous. As late as 1870, one-half of the pig iron product of the United States was made with anthracite coal, 30 per cent with raw bituminous coal and coke, and 20 per cent with charcoal. However, by 1910, 96.2 per cent of the blast furnace product was made with coke, 2.4 per cent with anthracite and coke admixture, and 1.4 per cent with charcoal. Coke became the standard fuel in the blast furnace. As the art of ironmaking progressed, more pig iron was produced and more coke was consumed. Coke oven capacity was progressively increased. In 1910, there existed approximately 4,000 coke ovens; in 1960 there was approximately 15,000 ovens. This increase in coke oven capacity was necessary to feed the mammoth appetite of modern blast furnaces.

Jan 1, 1962

By W. A. Backofen, F. de Kazinczy

FRACTURING under conditions of particular interest is identified with the junction of curves relating tensile yield and fracture stresses to test temperature; the intersection point gives the lowest stress, for brittle fracture (at the ductility transition temperature). An expression for is found in Cottrell&apos;s brittle-fracture analysis, Eq. [15],1 while measurements of this stress and temperature have been reported for a low-carbon steel heat treated to differ-

Jan 1, 1962

By R. S. Wagner, W. G. Pfann

METHODS that have been used to measure stress relaxation in metals and plastics have been reviewed recently by G. R. Gohn and A. FOX.&apos; The ideal stress relaxation test comprises placing a sample under a constant strain (usually considered

Jan 1, 1962

By B. H. Kear

All the possible ways of forming simple two-dislocation boundaries in multiple slip orientations are deduced. It is shown that the principal differences in work hardening behavior of crystals plastically deformed in these orientations can he accounted for in terms of the likelihood of formation of diffuse boundaries, or deformation bands, consisting of the products of dislocation reactions of the Lomer type. Also, it is pointed out that the break-up of boundaries under the applied stress is more likely to yield interstitial jogs than vacancy jogs, whereas glide dislocations cutting throuqh dislocations trapped in particularly stable boundam&apos;es can acquire both types of jogs. USING Frank&apos;s&apos; grain boundary formula, Ball and Hirsch2 determined the parameters of all the possible boundaries that can be built from two sets of glide dislocations in the fee structure. This paper deduces the geometrical possibilities for the formation of these two-dislocation boundaries in the different multiple slip orientations, and discusses the role of boundaries in work hardening and in jog formation. Formation of Two-Dislocation Boundaries in Mutiple Slip Orientations. The parameters of the possible two-dislocation boundaries for any crystal orientation can be deduced most conveniently using the boundary formulae due to Amelinckx,3 in conjunction with the stereographic projection shown in Fig. 1. Suppose that slip occurs in a-BC and ß-CA. According to Amelinckx, when the two systems of glide dislocations are parallel, the rotation axis, u, of the boundary is parallel to (a x ß) and the unit normal, u, defining the boundary plane is parallel to (a x ß) x (BC x CA). On the other hand, when the glide dislocations form a crossed grid, u is parallel to (BC x CA) and u is parallel to (a x CA) x (ß x BC). In Fig. 1, (a x ß) is the pole of the great circle passing through a and ß, so that u is parallel to DC, i.e., parallel to [110]. Furthermore, (a x ß) x (BC x CA) is the pole of the great circle passing through DC and 6, so that u is parallel to [110]. Hence, when all the glide dislocations are parallel, the boundary is pure tilt with parameters u = [110], v = [ 110]. Similarly, it may be shown that the corresponding crossed grid of dislocations is a mixed boundary with u = [111], u = [111]. Consider the case of a crystal compressed in the [001] orientation. In this orientation, according to Fig. 1, there are eight available slip systems. In what follows, the different types of two-dislocation boundaries that are possible in this orientation will be examined by taking different combinations of two slip systems out of the available eight, with a-BC always one of the systems. Case (i)—Slip Systems a-BC and d-CB. The formation of a tilt boundary in (101), which consists of a crossed grid of edge dislocations with vectors BC andCB, is illustrated in Fig. 2(a). As the figure shows, slip is required in the system a-BC in one part of the crystal and in d-CB in the other part, with both sets of dislocations entering the boundary from opposite sides. The rotation axis of the boundary lies in (101), depending on the relative densities of the two sets of edge dislocations in the boundary. Case (ii)-Slip Systems a-BC and ß-CA. The two possible boundaries are shown in Figs. 2(b) and (c); boundary (b) is tilt with u = [110], u = [110], and

Jan 1, 1962

By Richard D. Graves

Pitch from low-temperature carbonization of bituminous coal was hydrogenated at cracking conditions in a continuous bench-scale unit to produce low-molecular-weight oils and tar acids. The pitch contained 15.6 pct benzene-insoluble material, 4.0 pct hexane-soluble oil, and 80.4 pct asphaltene by weight. At 475° C, 7,500 psig, and 1.5 hours residence time, hydrogenation products, based on the weight of pitch, were about 36 pct oil boiling below 325° C, 24 pct hexane-soluble heavy oil, 17 pct asphaltene, 1 pct benzene insolubles, and 12 pct hydrocarbon gases. The yield of tar acids boiling below 250° C was 4.3 pct, and the yields of C6 to C8 paraffins, naphthenes, and aromatics were each less than 1.0 pct. The yield of tar acids was within the range of yields obtained by hydrogenation or high-temperature carbonization of bituminous coal (2 to 5 wt pct). Yields of oil boiling below 325° C increased with increased residence time or temperature. There was little or no effect of residence time on yields of alkali- soluble material which contained tar acids. Yields of hydro-carbon gases increased markedly with an increase in temperature from 475° to 500° C. Lowering the hydrogen pressure to 4,500 psig resulted in yields similar to those obtained at 7,500 psig.

Jan 1, 1962

By J. H. Waxweiler, L. C. Ikenberry, R. J. Bendure

Carbon which is present as insoluble carbides in austenitic stainless steels can be measured quantitatively by dissolving the steel in iodine-methanol and analyzing the residue for carbon. Severe sen-sitization was observed in Type 302 due to precipitation of only 0.003 pet carbon. Both cold work and the presence of delta ferrite caused a marked acceleration in rate of carbide precipitation. Carbide precipitation rates in 17-7 PH were stzulied for the austenite conditioning and also the aging heat treatment. CARBON and its compounds exercise a major influence on the properties of stainless steels and their response to thermal treatment. Sensitization in 18-8 type stainless steels has been the subject of numerous investigations throughout the years. Bain, Aborn, and utherford," and Binder, Brown, Frankss all studied the effects of heating austenitic stainless steels in the temperature range of 1000° to 1500°F. The primary purpose of most of these studies was the investigation of susceptibility to in-tergranular attack in acids due to these sensitizing heat treatments. Intergranular precipitation of carbides was always associated with intergranular attack but it was recognized2 that severe attack could occur with but minute quantities of precipitated carbide. Mahla and ielsen utilized the electron microscope to make a significant contribution in illustrating the appearance and method of growth of chromium carbides during sensitizing heat treatments. However, as they stated, their studies of residues could not be used to obtain a quantitative measurement of the amount of carbon which was actually precipitated. The aim of the present investigation was to devise a relatively fast, simple method for the quantitative measurement of carbides in stainless steel. EXPERIMENTAL WORK The initial investigations were made to determine the best means of separating carbides from the matrix. A number of dissolving media were tried using both chemical and electrolytic attack. Qualitative examination of the extracted residues by X-ray diffraction indicated that solution in iodine-methanol would furnish a good means of separation. Consequently, further work was pursued along this line. The method is quite simple. The sample in the form of millings or nibblings is dissolved in iodine-methanol solution at room temperature (6-g iodine, 25-ml methanol per g of sample). The insoluble residue containing the carbides is separated by suction filtration through an ultra-fine glass filter disc. This is a very fine filter medium that will retain particles as small as 0.1 to 0.2 p in diameter. After washing with methanol and drying, the filter disc and residue are placed in a conventional combustion carbon-tube furnace and the carbon determined gravimetrically. Using this technique it was found that reproducible insoluble carbon values were obtained. However, since such small amounts of insoluble carbon were obtained on Type 302 after sensitizatipn at 1250°F and 1500°F, the values were confirmed by a second method. In the second method the sample was dissolved with copper potassium chloride and filtered through a millipore paper. This treatment dissolves the matrix but leaves undissolved practically all of the carbon irrespective of how it is present in the steel. The amount of insoluble carbon present as chromium carbide is determined by calculation from the analysis of the residue for chromium and iron. The derivation of the formula used for this calculation is discussed later. The values obtained by the indirect copper-potassium-chloride method were in agreement with those obtained by the iodine-methano1 method. See Table I. It should be pointed out that the sensitivity of the direct combustion method is not too high when the amount of carbide present is small. This is due primarily to inherent blanks and to analytical errors such as weighing. For this reason it cannot be stated with any degree of certainty that there is a significant difference between values of 0.002 and 0.005 pct. Having confirmed that the iodine-methanol extraction gave a quantitative measurement of the precipitated carbides in Type 302, exploratory tests were conducted on Armco 17-7 PH stainless steel. Samples from commercial Heat 54807 were solution annealed at 2000°F, water quenched and heated at 1250" and 1500°F, and water quenched. The analysis of Heat 54808 is as follows:

Jan 1, 1962