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Major activities of the Bureau of Mines Explosives Research Center during fiscal year 1966 (July 1, 1965 to June 30, 1966) are reviewed briefly. Part 1 summarizes significant accomplishments of the projects that were active during the report period. Part 2 presents short abstracts of the publications that appeared in the Bureau series and in other media during fiscal year 1966. Publications issued after June 30, 1966, are noted where pertinent in foot- notes but are not abstracted. ACKNOWLEDGMENTS The Bureau of Mines gratefully acknowledges the support given through cooperative agreements by the following organizations to investigations conducted by the Explosives Research Center during fiscal year 1966: Manufacturing Chemists' Association. The Sulphur Institute.

Jan 1, 1967

By d&apos, Kathleen J. Amico

This summary appears in Minerals Year-book volumes I-II, and III, which cover mineral production in the United States, its island possessions, the Canal Zone, and the Commonwealth of Puerto Rico, as well as the principal minerals imported into and exported from the United States. The sections of this chapter and the area chapters in volume III contain further details on production. A summary table comparing world and U.S. mineral production also is included. Mineral production may be measured at any of several stages of extraction and processing. The stage of measurement used in the chapter is normally what is termed "mine output." It usually refers to minerals in the form in which they are first extracted from the ground, but customarily includes for some minerals the product of auxiliary processing operations at or near mines.

Jan 1, 1967

By P. Rama Rao, D. H. Sastry, T. R. Anantharaman

Deformation (a) and twin (a') stacking-fault densities in cold - wor ked filings of fcc silver alloys containing 2, 4, and 6 wt pct Sb have been estimated from Debye-Scherrer peak shifts and asymmetries, respectively. Evidence has been obtained for a possible strain-induced transformation in a two-phase alloy containing 9.0 zut pct Sb. Using Fourier analysis of X-ray line profiles, the effective particle sizes and root mean square strains have been determined for the three fcc alloys in the cold-worked condition. The values of the compound fault probability 0.5a + a') evaluated from peak shifts and asymmetries are in reasonable apeement with those derived from peak broadening. COLD work of fcc metals may produce both deformation and twin (also called growth) stacking faults, which can be detected and quantitatively estimated by X-ray diffraction techniques.' In addition to peak broadening, deformation faults produce a shift in peak positions and twin faults an asymmetry of the Debye-Scherrer reflections. Besides stacking faults, a reduction in the size of coherently diffracting domains and distortion within these also broaden the powder reflections of deformed fcc metals and alloys. Fourier analysis' of peak shapes provides quantitative infor- mation about the effective domain sizes, lattice strains, and also the compound fault probability (1.5a + a'), where a and a' represent deformation-and growth-fault density, respectively. The Paterson method2 for determination of a from peak shifts, the warren3 or wagner4 method for evaluation of a' from peak asymmetries, and the Fourier analysis for quantitative estimates of all the contributory causes of peak broadening have, in the course of the last decade, been extensively applied to obtain data for a number of deformed fcc metals and alloys. One of the useful results of earlier measurements of a in several solid solutions is a correlation between a and the solute valence as well as electron concentration per atom (p) in alloy systems based on a particular solvent. The work of Smallman and westmacott5 on Cu-Zn, Cu-A1, and Cu-Sn, of Foley, Cahn, and ~aynor' on Cu-Si and Cu-Ge, and of Rama Rao and Anantharaman7 on Cu-Si and Cu-Sb has revealed a common trend in the increase of a with p and also a with valency of the solute. Cahn and Davies' and Ad-ler and wagnerg have observed similar trends for silver alloys containing cadmium, indium, and tin. Data on a for silver alloys with a pentavalent solute element are not, however, available. It is primarily to fill this need that the present investigation on Ag-Sb alloys was undertaken. Utilizing the Patersonand Warren methods, values of a and a', respectively, have been determined in three silver alloys containing 2, 4, and 6 wt pct Sb. By Fourier analysis of the broadening of Debye-Scherrer peaks, effective particle sizes, lattice strains, and the compound fault probability (1.5a +a') have also been evaluated.

Jan 1, 1967

By K. Hodgson, N. C. Joughin

The detailed mechanism of rockbursts and other forms of damage due to rock failure in underground mining is as yet unknown. Studies of the energy changes which necessarily occur when an excavation is made underground seem to provide the best understanding of the phenomena leading to rock failure and damage (see Cook 1). It is common knowledge that the damage and rockburst hazard increases with depth and is greatest at remnants and in regions mined in an irregular manner. The rate at which energy is released as an excavation is enlarged provides an objective parameter to describe mining geometry in terms which are significant to studies of rock failure. In this paper, it is shown empirically that the rate of energy release per unit area increase in the size of an excavation is closely related to seismicity and incidence of damage in the mine. Consequently, it is suggested that the energy release rate is an important parameter in the design of underground mine layouts. Observations were made at two mines: the East Rand Proprietary Mines, Ltd. (E.R.P.M.), at a depth of about 9000 ft, and at Harmony Gold Mining Co., Ltd., at a depth of about 5000 ft. At both of these mines continuous recording seismic networks were in operation. (See Cook and Joughin.3) DESCRIPTION At E.R.P.M. the gold-bearing reef dips at approximately 35 degrees and is presently being mined at depths from 8000 ft to 11,000 ft below surface. The rock surrounding the excavation consists of a very homogeneous quartzite extending far into the hangingwall and footwall. The stoping width is approximately 40 in.

Jan 1, 1967

Jan 1, 1967

Jan 1, 1967

By R. L. Andrews

The Bureau of Mines investigated means of electrodepositing iridium to form thick coatings suitable for the protection of such metals as tungsten and molybdenum, which oxidize rapidly at high temperatures. Using a fused sodium cyanide bath, thick, adherent, and coherent deposits of iridium up to 15 mils thick were plated on tungsten and molybdenum substrates at 600° C and current densities of 10 to 100 ma/cm2. Limited oxidation testing of molybdenum encapsulated with pure iridium indicates that the coating may offer protection to approximately l,000° C in flowing air, but that at higher temperatures, the volatility of its oxide limits use of pure iridium. Alloy coatings of iridium with platinum, palladium, and rhodium up to 4 mils thick were formed from a fused sodium cyanide electrolyte; because their oxides are less volatile, these alloys may protect substrates at higher temperatures. Deposits made from aqueous electrolytes either had very low rates of deposition or were highly stressed and cracked when heavy deposits were made.

Jan 1, 1967

By N. F. Fiore, M. F. McGuire

THIS communication describes a series of experiments in which dislocation etch pitting was used to ascertain the depth of damage in crystals which were mechanically polished or which were cut with either a commercial metallographic cut-off wheel,* a com- All specimens were cut from single crystals of American Smelting and Refining Co. 99.999+ pct pure copper which were grown from the melt by the Bridge-man technique. The test specimens were disks, with faces being (111) planes and the disk axis a (111) direction. The disks were annealed in a vacuum of 10-5 Torr for 24 hr at 950°C prior to cutting or polishing and were given a light electropolishing in an ortho-phosphoric acid bath before etch pitting. Both Youngs1 and Livingston's2 reagents were used for etch pitting and the reagents gave identical quantitative results; however Livingston's reagent produced less staining and so all photomicrographs shown are of {111) surfaces etched with this solution. The surface of the annealed crystals showed well-defined subboundaries and a density of dislocations of about 1 X 106 per sq cm excluding those present in subboundaries, Fig. 1. The depth of cold work produced during mechanical polishing was determined after an annealed specimen was mounted in a paraffin holding block to protect it from extraneous damage. The exposed (111) surface was ground on metallographic papers and then polished on billiard cloth through 0.05-p alumina abrasive. It was necessary to remove about 0.3 mm (-0.01 in.) to obtain a structure representative of the annealed sur- face, indicating that the crystal was damaged to this depth during mechanical polishing. The cold work caused by standard cutting methods was measured in another series of tests in which cuts

Jan 1, 1967

By William A. Edmiston, R. E. Grace

A simplified model for the theory of reaction rates near equilibrium has been applied to the reduction of wustite. A linear relationship between the net rate of reaction and the Gibbs free-energy change, ?F, is predicted. The reduction of wustite in H2 -H2O gas mixtures was studied with a microbalance technique at temperatures from 850° to 950 °C. The predicted model was found to be valid to -?F/RT = 0.1 or approximately -200 cal per mole away from equilibrium. ThE theory of reaction rates near equilibrium has been developed by a number of authors. Prigogine, Outer, and Herbo1 have studied the catalytic hydrogena tion of benzene in an attempt to deduce some intrinsic connection between reaction rates near equilibrium and thermodynamics. Manes, Hofer, and weller2 have derived more general expressions for reaction rates near equilibrium from classical thermodynamics. Hollingsworth3,4 has commented briefly on the work of Manes et al. Benson5 has summarized in a general way the results of the earlier contributions. It is the purpose of this paper to apply the theory of reaction rates near equilibrium specifically to the reduction of wustite in H2-H2O gas mixtures. The basic premise is that the reduction of wustite proceeds by a surface reaction, rather than by solid-state diffusion ,or gaseous diffusion. Richardson and Dancy6 and Gellner and Richardson7 have suggested that the reduction of wustite may be governed by iron diffusion in wustite. Mckewan8-11 has proposed that reduced iron layers on various oxides are sufficiently porous to offer a negligible impedance to the reducing gas. The linear motion of interfaces reported by McKewan and discussed by Themelis and Gauvin12 indicates the lack of diffusive control during reduction. The reduction studies of magnetite reported by Quets, Wadsworth, and Lewis13 give additional evidence that reduction rates are linear when the reaction products are porous and nonprotective. The interpretation of measurements reported in this paper is predicated upon a surface-controlled reduction reaction, at least in the earliest stages of reduction when the reduced iron layer is thin.

Jan 1, 1967

By S. Gstalder, J. Raynal

Consideration was given to simple tests which could be performed on rocks to give a measure of rock drillability. Various methods of breaking rocks were considered and the hardness test developed by Schreiner was selected for this study. The test involves application of an increasing load on the rock face through a flat-faced cylindrical punch until rupture occurs. Test results show that hardness is a good measure of the breaking strength of rocks. Useful relationships are shown to exist between hardness and other physical quantities such as specific disintegration, Young's modulus and sonic velocity. Specific disintegration (volume of rock broken per unit of work input) provides a possible means of comparing the effectiveness of other methods of rock breakage. The relationship between hardness and sonic velocity may be very significant for it may be possible to deduce rock drillability from sonic log data. provided that a mineralogical factor is taken into account. TO test further the results of the work, laboratory drilling tests were performed which closely simulated down-hole pressure conditions. Correlations of drilling results with rock hardness measurements were quite good. It was concluded that rock hardness, as measured in the laboratory or as deduced from sonic logs, could be used in relations for predicting rock drilling performance. INTRODUCTION Drillability of rocks cannot be defined in an absolute manner by a single quantity or measured by a single test. Resistance of rock to drilling depends to a large extent upon the means used for rock destruction. This complicates drillability classification of rocks for there may be as many classifications as there are methods of rock breakage without known functional relations between them. The objective of this work was to develop. in terms of rock destruction behavior, means of selecting the best drilling method for a given rock or the conditions for optimum output from a given drilling method. ANALYSIS OF ROCK DESTRUCTION TESTS Gauthier and Baron' have reviewed the many test methods which have been developed for determining the resistance of rocks to breakage. These include drilling tests, punch tests, scratch tests, resistance to shock, wear tests, etc. A standard drilling test might be to determine the time required to drill a standard depth (1/16 in.) in a rock using a bi-cone microbit (1 1/4-in. diameter) when a standard load (417 Ib) is applied at a standard speed of bit rotation (110 rpm). From the standpoint of similarity, the results of microbit drilling tests would seem to be most representative of the several methods suggested above. However, evaluation of drilling performance by this method is only qualitative and cannot be applied directly to actual drilling conditions. Punch tests basically measure rock hardness. Punches of various shapes and sizes, including small cones for Vickers' and Knoop's tests, the wedge for Epstein's test and the right circular cylinder for Schreiner's test, have been used. Results of these tests lead to a quantitative hardness classification which would seem to be related to the resistance of rock to bit-tooth penetration. Scratch tests are related to the resistance of rocks to abrasion such as would be encountered in drilling with diamonds. Either the width of the scratch obtained at a fixed load or the load required to give a scratch of a fixed width may be used to evaluate surface hardness of the rock. This should be related to the resistance of the rock to wear. The above tests, and probably many others. give relative measurements of the breakage or destruction characteristics of rocks. There is no direct relation between results of these tests and the drillability of rocks. Also, the tests each measure different quantities which have different dimensions and they do not permit direct comparison of numerical values. As one step in rectifying the above difficulties. it is proposed that the results of all test methods be expressed in terms of volume of rock destroyed per unit of work required; this is referred to as "specific disintegration". Test results may then be reported in a form which shows both a classification of rocks in regard to each method and a comparison of methods with regard to each rock. The disadvantage in using specific disintegration is the difficulty of measuring this quantity with accuracy. The volume of rock damage is difficult to measure. as is the true value of work input. Rock heterogeneity adds to the

Jan 1, 1967

By K. E. Stanfield

Oil-yield results are presented for 65 oil-shale sections in Piceance Creek Basin, Colorado, sampled during the period 1957 through 1963. Including previously published data, oil-yield results for 203 sampled sections have now been released by the Bureau of Mines to aid in appraising the shale oil potential of the basin. Oil yields of core samples (135 sets) were regarded as reliable bases for appraising the Mahogany-zone interval, but only 5 sets of cores sampled the deeper, lower-zone oil shales. Drill cuttings (68 sets) sampled the lower-zone oil shales, but their oil yields are principally indicative and should be confirmed by analyses of cores. More complete core sampling of the lower-zone oil shales is needed.

Jan 1, 1967

By J. M. Singer

Methods are proposed for predicting concentrations of nitrogen oxides and carbon monoxide in the combustion gases of flames, specifically of lean, stoichiometric, and rich propane-air flames. Calculations are based on kinetic and thermodynamic theory. These theoretical data are compared with concentrations observed experimentally downstream of flat grid-type burner flames (approximately 25,000 Btu/hr) that were used to simulate gas appliances such as water and space heaters. Air pollutant concentrations are also computed for (1) flames chemically perturbed by recycling flue gases into the primary fuel-air mixtures; (2) flames thermally perturbed by cooling the burned gases at different rates; and (3) flames perturbed by combination of these two effects. In general, experimental and computed concentrations agree to within a factor of 2 to 7 with the experimental values always being higher than the theoretical. The theoretical analysis indicates that cooling the primary flame by recycling cold flue gases (with and without excess air) reduces the relative emission of nitric oxide and increases emission of carbon monoxide if the flame stoichiometry does not radically change. Cooling rates of about 5,500° to 10,000° R/sec starting at about 3,500° R generally suffice to prevent nitric oxide concentrations in lean flames from increasing much above the initial values at the combustion zone; these same cooling rates do not prevent oxidation of most of the initial carbon monoxide.

Jan 1, 1967

By O. Terichow

A pendulum sclerometer designed by the Bureau of Mines is described. Its method of operation is given, along with the results of tests made on representative mineral samples of Mohs' hardness scale to determine the applicability of the device for research on rock testing. The sclerometer hardness values obtained from the tests indicated that reproducibility and accuracy were good. A quantitative comparison of the pendulum hardness values with microhardness and surface energy values published by other investigators showed good agreement on minerals with Mohs' hardness numbers of 2 to 9.

Jan 1, 1967

By B. E. Sundquist

The various methods based on solution models for obtaining free energies of mixing from miscibility-gap data have been applied to a number of binary-alloy systems. For nine of these systems there exist experimental thermodynamic data that permit a comparison of the results to experiment. It was found that the method of van der Toorn and Tiedema almost invariably leads to results that are physically unacceptable and that vary drastically with small changes in the miscibility-gap parameters. The subregular solution model is found in all cases, except the Al-Zn, Fe-Cr, and Cu-Pb systems, to exaggerate the free energy of mixing by 30 pct or more. The model developed by Lumsden is found to give results that are often in excellent agreement with experiment and which exaggerate the free energy of mixing by no more than 30 pct. These results and others give evidence that the Lumsden treatment of the effect of unequal atomic sizes and of imperfect configurational randomness due to deviations of AB bond energies from the mean of AA and BB bond energies is adequate for most systems. ANALYTIC expressions are frequently proposed for the dependence on composition of the activities of the components of a solution. Because the development of solution theory is incomplete, these expressions contain parameters which must be determined by experiment. The measurement of activities is often difficult and consequently such measurements are less readily available than are measurements of phase equilibria which, under certain conditions, can also be used to evaluate these parameters. For example, suppose it is known that two structurally dissimilar phases, each of known composition, in an n-com-ponent system are at equilibrium at a given temperature and pressure. n equations can be set up in terms of these parameters expressing the equality of the chemical potential of each component in the two phases. In addition, one can write the Gibbs-Duhem equation for each phase that also contains these parameters. Thus, if these n + 2 equations contain n + 2 parameters, these parameters can be determined (at the temperature in question) from the phase diagram alone. If the average number of parameters in each expression for the activity of a given component in a given phase is V then there will be 2nV parameters involved. Equating 2nV to n + 2 shows that, for n + 2, V = 1. If the temperature dependence of each parameter were to be expressed in some explicit form one could use equilibrium conditions at a number of temperatures to increase V. The situation is much improved when the two phases in equilibrium are structurally similar. It can then be assumed that, stably or metastably, two phases will become one at higher temperatures. Thus the number of parameters involved becomes nV instead of 2nV. Hence, V = 2 for n = 2 using only one temperature. (It is implied here that the activity expressions used are valid over the entire composition range.) In this investigation only the equilibrium of two structurally similar, two-component phases (miscibility-gap systems) will be considered. The various proposed solution models will be applied to a number of these systems and the results compared with available experimental results. All of the analytic expressions that have been proposed for the free energy of mixing of a two-component system are of the form where ?Gmix is the free energy of mixing per mole of solution, N1 and N2 are the mole fractions of components 1 and 2, respectively, and f(Ni, T) is some function of composition and temperature. In the "ideal" solution model f = 0. In the "regular" solution model f = a constant. Since these two models permit only a symmetric equilibrium diagram they will not be considered further here. The simplest model that permits a nonsymmetric miscibility envelope is the so-called "subregular" solution model proposed by Hardy.1 This model gives where the Ci(T) are functions of temperature only. The same expression for f is obtained from the "linear a function" model proposed by Darken and Gurry2 and applied to miscibility-gap systems by Wriedt.3 This model requires that the a function defined by be a linear function of composition (yi is the activity coefficient of component i). This model is not purely hypothetical for it has been found2 to hold true for a number of systems. It is readily shown3 that the f(Nl, T) obtained from this model is of the form given in Eq. [2]. It will be noted that the subregular solution model contains only two parameters and hence both of them can be determined at any desired temperature below the critical temperature, Tc, for a miscibility-gap systems in the manner described previously. At T, the two constants can be determined by equating the second and third derivatives of ?Cmix with composition to zero. Another two-parameter model was proposed by Lumsden4 who set

Jan 1, 1967

By J. W. Town

Recrystallization studies on chrome-bearing spinel materials were made by the Bureau of Mines to determine the effects of certain fluxing agents and cooling rates on the chromium-to-iron ratio of recrystallized spinel. Statistically designed and evaluated tests showed that the ratio of chromium to iron in naturally occurring chrome spinel could be increased from 1.5 to 1 to over 7 to 1 and that the ratio of chromium to iron in the chrome-spinel in a stain-less steel slag could be raised to over 18 to 1. Silica, magnesia, and lime had significant positive effects, while alumina had a significant negative effect. Cooling rates of 200 C per hour in a programmed spiral globar electric furnace were satisfactory for growing crystals of recoverable size.

Jan 1, 1967

By M. Gangal, B. Paul

It may be seen from Maurer's survey (Maurer,l 1966) that most of the common methods used in rock drilling today depend upon mechanical loading of the rock. In order to predict the behavior of rock under an imposed system of stresses, it is necessary to have a valid criterion which delineates those combinations of stress which cause macroscopic rock failure from those which do not. Admittedly, the conditions under which brittle materials fracture depend very much upon statistically variable local effects such as inclusions, grain boundaries, minute imperfections, etc. However, it is extremely desirable to be able to predict fracture under complex states of stress by means of a stress-criterion of failure, where, for a given material, the effects of the other variables mentioned are incorporated into a small number of experimentally observable parameters. One of the most successful of these "macroscopic stress criteria" has been the Coulomb-Mohr theory 2,3 (also see Jaeger 4 and Terzaghi 5), modified by the addition of tension cutoffs (Paul 6). At first thought it might seem rather odd that a macroscopic theory is capable of predicting fractures which originate at highly localized random imperfections at an atomic level (or more likely at the level of individual mineral grains in rocks). However, Griffith7 showed that fractures originating near the tips of randomly oriented elliptical cracks lead to the macroscopic stress criterion of failure indicated in Fig. 1 (a). Fig. I (a) is to be interpreted in the following way: P and Q represent the maxi mum and minimum principal stresses (compression is considered positive) in a macroscopically isotropic body; fracture will not occur for any combination of principal stresses lying within the 'fracture curve' shown, but

Jan 1, 1967

By James A. Wasson

The Mitchell and Berea sands were cored and logged in Fred Link well K-l, Lower Newport field, Washington County, Ohio. Core and reservoir fluid analyses and available field data were studied to determine if these sands could be successfully waterflooded. The results of the study indicate that there is insufficient oil in place to form an oilbank in either the western Mitchell pool or the Berea sand, and that no commercial recovery of oil by waterflooding can be obtained in these reservoirs.

Jan 1, 1967

By I. K. Choi

In a recent paper by Smith and Wen(1) the adsorption of sodium dodecylsulfate and trimethyldodecylammonium chloride on kaolinite was studied. As would be expected considering the general negative character of kaolinite, except perhaps at quite' acid pH values (2,3,4), it was found that trimethyldodecylammonium chloride adsorbed strongly on kaolinite at basic pH values. Furthermore, it was found that sodium dodecylsulfate adsorbed strongly on kaolinite at acid pH values, particularly at initial 1H values below pH 3 (final pH values near pH 4). It is interesting to note that adsorption of the anionic surfactant was strong under conditions where the kaolinite was apparently slightly negatively charged (2). The present paper reports on an extension of the work by Smith and Wen. In this paper the effects of the presence of dodecyl alcohol and sodium hexametaphosphate on adsorption of sodium dodecylsulfate and trimethyldodecylammonium chloride on kaolinite are considered.

Jan 1, 1967

Cores of pre-Tertiary basement from ten oil exploration wells are related petrologically to the "axial", "marginal" and "shelf" facies of the New Zealand Geosyncline.A NW. Nelson-type basement is inferred beneath peninsular Taranaki and the western continental shelf. The terms Taranaki Basin and Wanganui Basin are re-defined and the terms North Wanganui Basin, South Wanganui Basin, Pipiriki High, Taranaki Fault, and Turakina Fault are proposed. Major faults are interpreted as of mainly transcurrent type and appear to form the western part of a splay at the northern end of the Alpine Fault. Evidence for a major Cook Strait Fault is reviewed.

Jan 1, 1967

By W. M. McKewan, R. G. Olsson

In order to improve the understanding of the iron oxide reduction mechanism, the rate of equal molar diffusion of hydrogen and water vapor was measured through disks of porous iron and alumina. The measuretneizts were made at atmospheric pressure at 800°, 900- , and 1000°C. It is shown tint the reduction of dense hematite pellets with hydrogen at these temperatures and at atmospheric pressure is to a great extent limited by gaseous diffusion between the bulk-gas phase and the iron-wustile interface. THE investigation of the reduction of iron oxides with hydrogen has been the subject of numerous papers. Although the effects of temperature, pressure, and gas composition on the rate of iron oxide reduction have been studied, the actual mechanism of the reduction process has not been definitely determined. As a means of improving the understanding of the mechanism, the rate of equal molar counterdiffusion of hydrogen and water vapor was measured through porous iron and porous alumina disks at reduction temperatures. The alumina was used as a basis of compari-son because its pore structure is homogeneous and independent of temperature. The porous iron was prepared by the reduction of dense hematite disks with hydrogen at the temperature of the subsequent diffusion experiment. The hematite disks were made from pellets that were identical to those used by McKewan1,2 in his study of iron oxide reduction with hydrogen. In these investigations the weight loss and rate of movement of the various interfaces were measured as a function of the reduction temperature and gas composition. With these reduction data and the presently reported diffusion data it is possible to determine the importance of H2-H2O transport between the bulk-gas phase and the Fe/FeO interface to the reduction of dense hematite. APPARATUS AND PROCEDURE A porous iron or alumina sample was held in the base plate of a sealed canister containing porous granular wustite, as illustrated schematically in Fig. 1. The canister was suspended from an automatic recording balance in a vertical tube furnace through which flowed hydrogen and water-vapor mixtures of known composition at atmospheric pressure (0.96 atm). Hydrogen from the gas stream diffused through the porous sample, reducing the wustite in the interior of the canister. The water vapor that was formed diffused back to the gas stream. The rate of diffusion was determined from the recorded weightloss data. The furnace, automatic balance, and gas-metering equipment have been described previously.2 The main body of the canister and the tubing extension were made of stainless steel while the base plate was made of high-purity iron. The main body of the canister was % in. in diam. It held approximately 6 g of porous granular wustite that was prepared by reducing 0.1- to 0.2-cm-diam specular hematite particles at 900°C with an H2-H2O mixture of a composition near the iron-wustite equilibrium value. The upper end of the 1/8-in.-diam tubing extension was sealed with a segment of plastic tubing and a tubing clamp. The temperature at the top of the furnace was sufficiently high so that no water vapor condensed inside the extension. In the experiments with porous iron, iron oxide samples were prepared from reagent-grade hematite that was pressed and sintered in a manner previously described.' The resulting pellets had a density of 5.15 ± 0.05 g per cu cm. Each pellet was centerless-ground

Jan 1, 1967