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Geochemical data on Australian granites and pegmatites, and the mineral components of these rocks, are compared with that obtained in similar studies in the U.S.S.R. and elsewhere.The geochemical character of tin granites and the trace chemistry of their component minerals, particularly biotites, have some significance as ore guides in prospecting for tin.The primary geochemical dispersion of tin can be readily tested both in the laboratory and field by colourimetric methods, after volatilization with ammonium iodide, using modifications of the method described by Wood (1958).Secondary dispersions of tin in residual soils or alluvia can likewise be readly tested by rapid colourimetric methods in the field, but simple hydraulic methods, handling larger sample volumes, give reliable outlines of dispersion patterns.INTRODUCTIONThe search for tin ores, whether lode or placer in type, is usually directed on genetic grounds to country within or adjoining acid intrusives.A long established means of prospecting is to test samples for cassiterite by panning or other hydraulic separation.These methods can be used on crushed lode material or the natural materials from placers.With the advent of new techniques for extraction and for colourimetric analysis for tin (Wood, 1958 and Ross and White, 1961) a means is available for rapid analysis of materials not susceptible to quantitative testing by hydraulic methods because of the fine sizings of cassiterite or the occurrence of tin structurally held in minerals. The new methods thus opened up the field of tin prospecting by extending the search for ore guides to genetically associated rocks and minerals, wall ror-ks of veins and a wider range of superficial deposits.

Jan 1, 1963

By J. B. Clark, A. J. McEvily, R. L. Snyder

The nonuniform distribution of precipitate particles has been recognized as a leading factor contributing to the relatively low fatigue resistance of aluminum alloys. The structure of many of these alloys is characterized by narrow precipitate-free zones adjacent to the grain boundaries. Alloys with such zones exhibit a tendency for brittle inter crystalline fracture. The interrelation between this type of structure and mechanical properties was investigated in an Al-10 wt pct Mg alloy. It was found that deformation during fatigue occurs preferentially along these zones and cracks initiate there. In Al-10wt pct Mg, the zones were found to be supersaturated even after extensive general precipitation and are due to the absence of proper precipitate nuclei in the region near the grain boundaries. Cold working the alloy prior to aging improves the mechanical properties by inducing precipitation within the zones and also by jogging of grain boundaries. The mode of fracture is changed from brittle inter crystalline to more ductile trans granular fracture. THE process of fatigue is highly structure sensitive, with the strength of the whole often dependent upon some localized discontinuity, either geometrical or metallurgical in nature. Much has been learned about the role of geometrical discontinuities, e.g., notches, in fatigue, but with the exception of the effects of inclusions or the shapes of carbides, relatively little is known about the specific effects of discontinuities in metallurgical structure such as nonuniform precipitation. In most age-hardening aluminum alloys, metallo-graphic studies have shown that the extent of precipitation adjacent to grain boundaries is much less than that which occurs in the interior of the grains. The width of these almost precipitate-free regions, which are sometimes called denuded zones, and the extent of solute depletion within them, are dependent upon the particular alloy and its aging treatment. It has been observed1 that these zones are relatively soft with the result that plastic deformation takes place preferentially within them. It has also been shown 2-4 that there exists a tendency for intercrys- talline cracking in fatigue when such zones are present. It is of interest to note that Broom et al.2,3 were able to reduce the incidence of this type of failure in an A1-4 wt pct Cu alloy by stretching the material 10 pct prior to aging. In the present study, the effects of precipitate-free regions on the fatigue properties of an A1-10 wt pct Mg alloy were studied in detail, and the effects of deformation prior to aging on the nature of the precipitation process as well as on fatigue properties were also investigated. MATERIAL AND PROCESSING An A1-10 wt pct Mg alloy was selected for this study, because it was known that well-defined precipitate-free regions along the grain boundaries are readily obtained in this alloy after aging at 200oC.5 The starting materials were 99.998 pct A1 and singly sublimed magnesium of about 99.9 pct purity. The aluminum was induction melted in a graphite crucible, and then the magnesium addition was immersed until dissolved. Chlorine gas was then bubbled through the molten alloy for 4 min to degas the melt, after which the melt was cast at a pouring temperature of 730" to 760°C into a cold, graphite-coated, tapered steel mold. Since A1-Mg alloys are difficult to homogenize,5 special care was taken to obtain a uniform composition. Two-in. cubes were cut from the ingot and heated at 446°C for 30 min. These cubes were then hot forged approximately 35 pct in each of the three cube directions and homogenized for 16 hr at 446°C. Sheet specimens were then obtained by pressing 40 pct and rolling 35 pct per pass with reheating between reduction steps to a final thickness of approximately 0.10 in. The sheet was then solution treated for 16 hr at 446°C and water quenched. The age hardening behavior of this material at 200°C was then determined, and the results are shown in Fig. 1. The age hardening of this alloy when subjected to cold work prior to aging is also shown in this figure. Preliminary work indicated that extensive deformation after quenching was required to affect drastically the precipitate-free regions in this alloy, and a rolling reduction of 50 pct was chosen. For purposes of comparison the following three conditions were studied: a) Solution treated, quenched, and aged 20 hr at 200°C

Jan 1, 1963

By Donald D. Murphy

My first contact with underground, bolt conveyors came when I was hired as a draftsman by the La-Del Conveyor & Manufacturing Company in 1935. At that tine relatively few nines were using haulage belt conveyors. Wore they were in use, they were usually loaded by chain or shaker type room conveyors which in turn were hand loaded at the working face. Duo to the low room tonnage, a gathering belt might receive who output of from six to eight rooms. For several years belts 26 and 30" in width were the favorites for coal mine use. Belt speeds very seldom exceeded 200 ft. per mm. at that time. Conveyor lengths for the majority of units lay between 1.000 and 2000 ft. For a number of years 25 H.P. drives were adequate for those conveyors. From 1940 until about 1950 loads and speeds went up slightly and 40 H.P. drives became the standard. Since the majority of mines were then using direct current power systems, we were able to use controllers with 3 or more steps of starting resistance. The slow belt speeds coupled with relatively long starting cycles kept the rate of acceleration low and gave us smooth, easy starts.

Jan 1, 1963

By Rollin E. Hook, Attwell M. Adair

The yield and fracture behavior of recrystallized chromiztm have been studied in order to gain an understanding of the recrystallization embrittlement-rheotropic recovery phenomenon. The duc tile-brittle tensile transition temperature of recrystallized chromium was found to vary from 225 ° to -80°C as the ratio of specimen diameter/mean planar grain size decreased. The applicability of this observation to other bcc metals is briefly discussed. Brittle fracture in recrystallized chromium was found to be initiated predominately from intercrystalline rupture nuclei. Single crystals exhibit a high degree of ductility at 23 "C. The experimental data indicate that grain boundaries play a significant part in the yield and fracture behavim. Pres training significantly reduces the transition temperature, and high temperature aging does not result in re-embrittle-ment until complete recovery or re crystallization occurs. SEVERAL theories have been used to explain the recrystallization embrittlement-rheotropic recovery phenomenon in chromium. Wain, Henderson, and ohnstone' propose a Cottrell dislocation locking mechanism due to nitrogen, and Weaver and Gross and weaver 3 propose a strain-induced precipitation mechanism involving a chromium nitride precipitate. The researches of many investigators seem to leave little doubt that brittleness in chromium is promoted by interstitial impurities. Smith and seybolt4 have shown that the ductile-brittle transition temperature is lowered as the interstitial content is reduced. weaver3 provides evidence for a 150°C reduction in the tensile transition temperature as the nitrogen content is reduced from 20 to 5 ppm. Maykuth and affee' have suggested that the amount and orientation of grain boundary impurities may be responsible for the brittle nature of recrystallized chromium. This suggestion was based on their findings that wrought iodide chromium possessing a fiberous grain structure is ductile in tension at room temperature while a recrystallized grain structure is completely brittle. Previous investigations have not studied this phenomenon sufficiently to determine its cause. Perhaps this has been largely due to previous experimental findings that brittle fracture observed in chromium has been almost entirely transgranular.' In addition McNeil and imb,' who investigated coarse-grained as-cast chromium, describe the point of initiation of fracture as cleavage, close to the (100) plane, near or at grain bound-daries, or at included particles or voids. However, Hook, Adair, and ipsitt found that fracture in coarse-grained recrystallized chromium is initiated by intergranular rupture and then propagates nearly entirely by cleavage. This result, together with their finding that room temperature ductility in bending is observed for single crystals and coarse-grained polycrystalline specimens for which the number of grains through the specimen diameter is small, suggests that grain boundaries may play an important role in the brittle behavior of chromium. The recrystallization embrittlement problem can be resolved into two questions. These are, whether the controlling mechanism is predominately one of crack initiation or crack propagation, and whether brittle fracture is initiated predominately by slip or twin induced intergranular rupture or by cleavage. The following research was designed to study the role of grain boundaries on the brittle fracture of chromium in an effort to resolve these questions. EXPERIMENTAL PROCEDURES, RESULTS, AND DISCUSSION General Procedure. All tensile specimens (except 0.04 in. diam wires) were prepared from 1/4 in. diam swaged rod fabricated from one ingot. Details of fabrication are given elewhere. The results of impurity analysis for the swaged rod and for the

Jan 1, 1963

By T. G. Lovering

Nonparametric statistical tests have practical application to many geological problems because, unlike the standard statistical tests, they do not require assumptions regarding the form of the population frequency distribution. Many of them do not even require that the variable be susceptible to numerical measurement. These tests are useful either 1) for geological data representing population distributions of unknown form, or otherwise not meeting the requirements for standard parametric tests; or 2) for sample attributes that cannot be measured but only ranked in order of relative magnitude. The application of two such tests will be illustrated. The Kolmogorov-Smimov test will be used to test for significant differences in copper distribution in samples of two rock types; the Spearman rank-correlation method will be used to determine whether there is a significant association between intensity of rock alteration and copper content of the rock. Nonparametric tests are, in general, quicker and easier to perform than the corresponding parametric tests, and they may be applied to a greater variety of data. They are not as powerful as the standard tests if used on data to which the latter are applicable, and computer programs utilizing them are not generally available. The use of standard or parametric statistical procedures for the interpretation of measured geological data is familiar to most mining engineers and explora- tion geologists. The computation of product moment correlation coefficients on sample assays for more-than one component is already standard procedure in some company operations, as is the use of Student's F test and Snedecor's F test for the comparison of means and variances of sample groups. The application of these three tests is limited by the prerequisites that the samples must be random, independent representatives of normally distributed populations and that the variables involved must be measurable. If such tests are applied to data which fall short of fulfilling these prerequisites, then the probability level attributed to the computed statistic is invalid and the conclusions based thereon may be erroneous. A number of nonparametric, or distribution free, statistical tests have been developed for use with data which are not amenable to standard parametric procedures. These tests have been widely used in the behavioral sciences such as psychology and sociology for some time, but their application to geologic problems is relatively new. Nonparametric tests may be grouped into two main categories: those which test for significant differences in a single variable by comparing either sample values with a standard value or representative values between two or more groups of samples; and those which test for significant association between pairs of variables in a single group of samples. The versatile chi square test, the Kolmogorov-Smirnov one and two sample tests, the Wilcox matched pairs signed ranks test, the median test, the Mann-Whitney U test and the Cochran Q test are examples of nonparametric tests with demonstrated or potential geological applications that belong in the first category. The contingency coefficient, Spearman rank correlation coefficient, Kendall rank correlation coefficient and the

Jan 1, 1963

By Martin H. Rogoff

The presence of antibiotic materials extractable with polar organic solvents was demonstrated in coals of various ranks. Since these antibiotics occur in low concentrations, 200 pounds of a high-volatile C coal was extracted with acetone at room temperature to obtain sufficient material for detailed study. The biologically active materials in the extract were concentrated by extracting with aqueous sodium hydroxide. The fractions soluble in sodium hydroxide inhibited bacterial cultures when present in concentrations comparable to those at which other antibiotics are active (5 µg/ml). Steam distillation of the extracts did not yield highly active materials, contrary to the finds of other investigators. Mass spectrometry of the extract indicated, mainly, the presence of 6-ring compounds in the region of mass 324 to 392. The predominance of 3-ring aromatic systems found by ultraviolet analysis suggests compounds such as biphenanthryl or similar structures. The activity of the hydroxide- soluble material decreased markedly when the phenolic hydroxyl groups were transformed into trimethylsilyl ethers. Hydrolysis of the ethers yielded a product having the same activity as the original material, which indicates that phenolic compounds are largely responsible for the antibiotic activity observed.

Jan 1, 1963

By John C. Machisak

THIS INFORMATION CIRCULAR contains injury and employment data for all stone quarries in the United States for the Calendar year 1960. This publication contains statistical data on injuries and employment pertinent to the stone quarries and related operations, such as the manufacture of cement and lime, rock dressing etc., but excludes statistics for clay and sand and gravel operations. Data for these commodities may be found in other Bureau publications. Reports received from the operators are voluntary responses to the Bureau's request for information; therefore, the figures may not be complete for the industry. However, since these data contribute greatly to the promotion of safety, every effort has been made to make them representative of the industry.

Jan 1, 1963

By Fred W. Shultz

In the past we have been somewhat harrassed by the terms "'quality control" and "process control". This is especially true where the industry is dependent upon the chemical analysis of their product which in turn informs them how, well they have been controlling the process. The information which they have received, in most cases, is of an historical nature rather than of current value. The word "control" is to have more significance in future operations. This is particularly true in the metals industry. As the industry continues to process lower grade ores, and processing costs continue to rise, they must obtain more information faster to exercise "control" to its fullest extent.

Jan 1, 1963

By F. J. Lecznar

An investigation of the problem of separating two minerals by a moving inclined plane has revealed that only minerals with considerable difference in sliding friction coefficients separate readily; that it is possible to separate two minerals when only one of them has a rolling friction coefficient; that difference in geometrical shape of the minerals is important to separation which improves as grain size increases; and that the thickness of the stream falling on the belt influences the grade of separation - the thinner the stream, the smaller the interference between the grains of the minerals to be separated and the higher the degree of separation. The problem of separating two minerals with different friction coefficients and shapes by a moving inclined plane has been investigated. Friction separators can be used to separate two materials that differ in shape and in friction coefficient. 1,3 Gladkov has presented some theoretical aspects of using a moving plane to clean corn and podded seeds; this method, however, did not result in practical application. When considering the separation of minerals, only those with considerable difference in sliding friction coefficients can be taken into account. Furthermore, it is possible to separate two minerals when only one of them has a rolling friction coefficient. The difference in geometrical shape of two minerals is also important to separation. It has been found that the separation of two minerals improves as the grain size increases. For example, coal and slate over 2 in. in grain size separate much better than materials of smaller grain size. As Table I indicates, the slate grains smaller than 25 mm gradually lose their flat shape with decreases in size and are more rounded than larger grains, which are almost flat. The smallest grains of slate in first and second fractions slide down the belt since their friction coefficients decrease and approach the value of the rolling coefficient. The percentage of separation of the first fraction is, therefore, low. Thickness of the coal stream falling on the belt also influences the grade of separation; the thinner the stream, the smaller the interference between the grains of the two minerals to be separated and the higher the degree of separation.

Jan 1, 1963

The Ediacara mineral field is classified as a Mississippi Valley type deposit with stratiform mineralization near the base of the Cambrian beds. Mineral deposition was contemporaneous with sedmentation and reerystallization, and mobilization took place after lithification of the sediments. Several mechanisms of deposition were possible.INTRODUCTIONThe Ediacara mineral field is located in the Mt. James Range approximately 300 miles north of Adelaide, about 12 miles west of Beltana railway siding and 10 miles east of Lake Torrens. It is isolated geographically from similar deposits of equivalent age and environment in the Flinders Range Province (Fig. 1). The climate may be described as semi arid with high summer temperatures and frequent dust storms. Occasional thunder storms are the main source of rain in the summer months.The exact date of discovery is unknown, but is believed to be about middle of the last century. Ulrich (1872) was the first geologist to report on the field. At that time only the southern portion of the field had been prospected (and abandoned). Although the prospects did not appear encouraging Ulrich advised prospecting of the shales and testing beneath the limestone.In 1888, Rosewarne, an Inspector of Mines, visited the Southern Workings and queried whether they were connected with some lode at deeper level or were merely bedded deposits. The first geological map with sections was drawn by H.Y.L. Brown (Brown 1892).Brown recognized three principal rock formations as dolomitic sandstone, kaolinised shales and sandstone, and quartzites and sandstone in descending order. These three basic units are still recognized. He recognized also the stratiform nature of the mineralization in the shales as a...

Jan 1, 1963

By F. Garofalo

It has been shown by various investigators that during constant stress creep the dependence of minimum creep rate, 6,, on stress, o, is given by em = A onat low stress levels, md by 6, = A' exp [ß s] at high stress levels. In these relations A, n, A', and ß are constant at constant temperature. A single relation has been found which satisfies conditions for both high and low stresses and agrees well with experimental results. This relation is 2, = AN (sinh a s)n, where A" is a constant at constunt temperature and a = p/n. This relation also satisfies the linear relation, 6, = k s, found at temperatures near the melting point at low stresses. EXPERIMENTAL creep results have led to a number of empirical relationships between minimum creep rate, 6,, and the applied stress, s. Under conditions of constant stress it is generally found that at low-stress levels,'-' the dependence of minimum creep rate is given by 6, = Asn. At high-stress levels'74 the experimental results fit the relation, 6, = A' exp [po l. In these relations A, n, A' and ß are constant at constant temperature. A model based on climb-of-edge dislocations from a pile-up array leads to a relation similar to that found experimentally at low stresses.' On the other hand. theories based on chemical-reaction rate,5 nonconservatively moving dislocation jogs, and jog migration and climb-of-edge dislocations4 lead to a relation similar to that found experimentally at high stresses. No difference in mechanism between low and high stress levels has been clearly defined; it is questionable whether such a difference really exists. In any event, the major argument usually given in substantiation of a change in mechanism from low to high stresses is that no single relation exists for defining the stress dependence of the creep rate over wide ranges in stress. However, such a relation has been found and is of the form, dm = A" (sinh a s)n, where A" is a constant at con- stant temperature and a = ß/n. This relation agrees well with experimental results over wide ranges in stress and temperature for copper, aluminum, an A1-3.1 pct Mg alloy, and an austenitic stainless steel. STRESS DEPENDENCE OF MINIMUM CREEP RATE At low stress levels the minimum creep rate, gm, depends on the stress, 0, under conditions of constant stress creep through the relation em=Aon [1] The quantities A and n have been defined previously. In the range in which this relation applies, a linear dependence is found in a log em,-log o plot. Above the stress range of application of relation [I], the minimum creep rate increases much mar; rapidly than predicted by relation [I]. This behavior is shown in Fig. 1 for a series of creep tests on copper4 at various temperatures ranging from 673 o to 973°K. Relation [I] is satisfied at the lower stresses, although the results at 973°K are quite limited. In all cases the transition beyond the applicable range of relation [I] is a gradual one indicating no abrupt change in mechanism. For all test temperatures, values of n have been determined from the results in Fig. 1. These are reported in Table I under Alog tm/hlog o. At high stress levels the stress dependence of minimum creep rate under conditions of constant stress is given by im = A' exp [ß a] 2] All factors have been defined previously. In a log em-0 plot, relation [2] predicts a linear function. Experimentally, a pronounced deviation from the prediction of relation [2] is found at lower stresses. As the stress is lowered, the minimum creep rate decreases more rapidly than predicted by relation [2]. This shown for copper in Fig. 2. Again it is found that the transition from high to low stresses is gradual and no really sharp change is found. Values of p determined from the high stress results are given in Table I. The dependence of minimum creep rate on stress at constant temperature for all ranges in stress

Jan 1, 1963

By G M. Thorpe

This paper discusses mine research at Inco, giving specific examples of research projects which illustrate the approach to mining problems. The first example covers the development of a new mining method, "undercut and fill," which was originated for mining badly broken-up pillars, but which is now rapidly replacing the square set method of pillar recovery. In the new method, ore is extracted in a series of successive horizontal cuts, progressing downward, a cut being completely mined and filled before the cut below is started. In the second example, improvements to the "cut and fill" method of mining are discussed. These improvements are the result of improved techniques and improved equipment, etc., with, in many cases, the former being made possible by the latter. The advances made have permitted the use of the "cut and fill" method at much greater depths than before. The third example is presented to illustrate research undertaken to obtain the earliest maximum advantage of the introduction of a new piece of equipment or material. For this purpose, the development of the "Under-ground use of AN /FO Blasting Agent " has been selected. Work on this project started in May, 1960, at a time when there was very little in-formation regarding the potentialities of AN /FO for underground blasting, either primary or secondary. By the end of 1961, AN /FO made up 64 per cent of the explosives used under-ground at Inco mines.

Jan 1, 1963

By R. C. Gifkins, A. Gittins

A. Gittins and R. C. Gifkins (University of Mel-houvne)— Evidence from somewhat similar experiments to those described in this paper has led us to the conclusion that possibility 2) of the four listed on p. 319 is a description of what happens in grain boundary sliding. That is, sliding is limited by accommodation deformation, it being necessary to the Continuance of sliding that this accommodation should take place. An example of such accommodation, though probably not the most important, is fold formation at triple points. The evidence and arguments for this point of view are set out in Refs. 14 to 16. In particular, an experiment with a lead bicrys-tall5 seems to support point 2) rather than 3). In creep of this specimen it was found that at least 90 pct of the extension of a zone 0.3 mm wide at the boundary was supplied by sliding at the boundary. The sliding was localized in a region at the boundary very much smaller than 0.3 mm, in fact, in a region too narrow to resolve optically. In poly crystalline Specimens&apos; there appears to be a surface effect, as found by Rachinger," but it appears that this may not manifest itself at low strains. "Low strains" means <10 pct for a Pb-TI alloy, <2.5 pct for magnesium or "Magnox" A12 alloy, or <40 pct for a 0 brass. Up to this extension the sliding, measured by the mean vertical step at boundaries, is proportional to extension. We are able to say this with some confidence, since the error bars on our points are statistically derived. Our results would lead us to think that the error bars on other work, including that of Mullendore and Grant, are much too large at low strains to show this

Jan 1, 1963

By F. G. Miller

It is generally accepted that sulfur exists in coal in three forms: (1) pyritic, (2) organic, and (3) sulfate sulfur. Sulfate sulfur usually makes up less than 1% of the total sulfur content. Pyritic and organic sulfur, make up almost all of the total sulfur and occur in varying amounts in different coals and can vary greatly in coal of the same seam Pyritic sulfurs of 20% to 80% of the total sulfur have been reported Other authors have shown that it is not possible to remove the organic sulfur without chemically altering the coal. Chapman and Jones (1) state: "Organic sulfur, unlike pyritic sulfur does not exist as discrete particles, but is intimately associated with the coal structure, and as such it is not possible to remove it or reduce its concentration by physical means." Any success in removing sulfur has come about by removing pyritic sulfur by physical means; therefore, removal of sulfur in the pyritic form is the subject of this investigation. The extent to which any impurities can be removed from a particular coal can be determined by a washability study. Outside of crushing coal, to finer sizes or chemically altering the coal, there are no known methods of changing this inherent washability characteristic. The efficiency of various methods used to remove impurities can be determined by comparison of results produced at a yield to the results as shown by a washability study. In recent years heavy media processes have proven their ability to wash plus 28 mesh coal and nearly produce results shown to be theoretically possible by the washability study. Therefore, it is the objective of this paper to show various methods of treating the finer fractions of the coal, in the hope of developing a process, which can effectively produce in the fine fractions the efficiency of heavy media devices in the coarse.

Jan 1, 1963

By Allan F. Smith

The influence of hydraulic fluids on spontaneous heating in bituminous coals is determined by measurement of the temperature increases produced in coal-fluid mixtures heated to a temperature sufficient for the initiation of self-heating. Similar tests on as-received coal samples and water-coal mixtures are compared with the results obtained for the various hydraulic fluids. Three of the four coals were sampled from coalbeds known to have a history of spontaneous heating. The data provide a basis for predicting the possible effects in gob or carbonaceous refuse of coal mines.

Jan 1, 1963

By Richard F. Hewlett

Computing average grade and tonnage either for an entire ore deposit or for individual blocks of ore is a continuing problem in mining. As part of a research program, investigating application of statistical techniques to mine sampling, Bureau of Mines engineers at the Denver Mining Research Center have made extensive use of an electronic digital computer for developing mine sampling theory, simulation of ore deposits, and analysis of mine sample and assay data. This report is one of a series describing use of the digital computer for rapid solution of computing problems in the mining industry.3 4 Development of a computer program to compute ore reserves by the commonly used triangular method was necessary so that results could be made available for analysis within hours.

Jan 1, 1963

By S. R. Titley

The recent emphasis placed upon the use of molybdenum as a geochemical indicator has stimulated considerable inquiry into the behavior of molybdenum in the zone of oxidation. This paper represents a summary of recent and continuing experimental work and calculations in an investigation of a portion of the system Mo-Fe-S-H20 and treats the stability of various iron and molybdenum compounds with respect to oxidation potential and pH. Using experimentally determined free energy values for ferrimolybdite, diagrams of the stability fields of this mineral have been calculated with respect to ilsemannite (?), molybdenite, pyrite and limonite. This theoretical approach is the one utilized by Garrels3&apos;4 in studies of the relationships of various minerals in the zone of oxidation. Use of this approach is particularly suited to the study of geochemistry in the zone of supergene processes because of the low temperatures, low pressures and other relatively easily determined and duplicated factors that exist in the near surface environment. Such a study of molybdenum, however, is complicated by several factors. One of these is the fact that the strong amphoteric behavior of molybdenum makes possible a wide variety of substances and complexes whose exact chemical natures are unknown. The second factor is the dearth of thermodynamic data for many of the simplest of the possible compounds and ions important to the study. For the purpose of this study, the problem of complexes has been approached through considering only the simpler possibilities realizing that the complexes and systems so treated may be gross oversimplifications. All the complexes considered, however, have been suggested in the chemical 2,7,9,12 or geologi-cal literature. EXPERIMENTAL WORK Studies of the behavior of molybdenum ions and ferrimolybdite have been carried out in aqueous sys- tems, and reactions have been followed by simultaneous measurement and recording of pH and oxidation potential. A major problem involved in this study was the long periods of time necessary for equilibrium to be established in some of the systems considered; in a few instances, these periods exceeded four weeks, that is, four weeks during which measured conditions changed continuously. Another problem, in some instances, was the indeterminate nature of the reactions that have taken place. Because of the tendency of molybdenum to complex, reactions which take place under some of the more extreme imposed conditions of oxidation and acidity or alkalinity are unknown. However, useful data for the present work were obtained from studies of the molybdate ion and ferrimolybdite between pH 2 and 8 and under only moderately oxidizing to nonoxidizing conditions. Instruments used in the experiments were a Hewlitt-Packard Model 412A VTVM, a modified Beckman Zeromatic pH Meter and two Varian model 11 recorders. pH was measured between glass and calomel electrodes and Eh was measured between calomel and platinum electrodes. Conditions of pH were varied with 1N H2SO4 and 1N NH4OH and 1N NaOH. Eh was varied with gaseous nitrogen, oxygen or aqueous H202. Ambient temperature was essentially uniform at 24ºC and was increased in the reaction vessel by the positioning of a magnetic stirrer whose temperature was sufficient to bring the temperature to 2S°C in the reaction. The temperatures of reaction did not vary more than 1/2ºfrom 25°C. Two reactions were investigated, the ferrimolybdite-limonite-water reaction and the reduction of molybdate ion. Studies of both reactions yielded useful data that were used in preparation of the Eh-pH diagrams. The traces of the reactions are shown on Fig. 1. Ferrimolybdite-Limonite- Water: Studies of this reaction involved analysis of the solution of ferrimolybdite and simultaneous formation of ferric hydroxide. The data are summarized on Fig. 1. In this reaction, equilibrium was attained at various pH&apos;s when coexistence of the two solid phases (ferrimolybdite and ferric hydroxide) was attained. At the proper pH, controlled by the amount of ferrimolybdite and thus the dissolved content of molybdate species, both phases were observed and reaction times to complete the transition were on the order of weeks. The reac-

Jan 1, 1963

By R. G. Davies

Above 500°C, where dislocation climb is rate controlling, it is observed that the activation energy for creep is independent of the apblied stress, although it varies from 62 kcal per mol at 15 pct A1 to 73 kcals per mol at 20 pctA1 due to the change in short-range ovdw with composition. Below 500°C, when the nonconservative motion of jogs upon dislocations is thought to be rate controlling, the activation energy is stress dependent. A sudden increase in the creep rate, for which no explanation is availab2e, occurs at the highest stress at all temperatures. CREEP has been the subject of numerous research publications during the past decade with most of the attention focused upon high temperature steady state creep, i.e., above 0.5 TM, where TM is the absolute melting temperature, as it is the most amenable to theory. Many of the proposed theories involve the climb of dislocations out of their slip plane, which allows them to circumvent obstacles or to annihilate dislocations of opposite sign on other slip planes.&apos; For pure metals it is observed that the activation energy for this creep is equal to the activation energy for self diffusion.&apos; The position is much more complicated in alloys as there are many possible microcreep mehanisms, as well as dislocation climb, which could be rate controlling. There has been little systematic investi- gation of alloys, but Weertman (lead and indium base alloys)3 and Lawley, Coll, and Cahn (Fe-A1 alloys)4 suggest a microcreep process as the controlling factor. A Cottrell-Jaswon atmosphere mechanism is proposed for the lead and indium alloys, and a mechanism involving crystallographic order for the Fe-A1 alloys. Lawley et al. showed that the formation of a super-lattice, either of the FeAl or Fe3A1 type. decreased the rate and increased the activation energy for creep. From the measurements of lattice parameters,= resistivity,&apos; magnetic properties,7&apos;8 internal friction: and dilatometry10 the ordered region is thought to commence at -19 at. pct Al. However, a recent investigation by the author indicates a value

Jan 1, 1963

By T. H. Alden

T. H. Alden (General Electric Research Laboratory)—This paper as well as earlier ones of Dr. Wood represent an important contribution to the experimental description of fatigue fracture. The mechanism of fracture proposed by the authors, however, is not established by this data nor supported by other data existing in the literature. Although taper section metallography provides a rather detailed picture of fatigue crack geometry, photographs so obtained must be interpreted with care. The narrow bands revealed by etching, frequently associated with surface notches, are labeled by the authors "fissures". Measurement shows, taking into account the 20 to 1 taper magnification, that the depth of these structures is at most 2 to 3 times the width. This distinction is important in the conception of a mechanism of crack formation. It is difficult, for example, to imagine a deep, narrow fissure arising from a "ratchet slip" model. A surface notch, on the other hand, may form easily by this mechanism. The notches observed in the present work are the subsurface evidence of the surface slip bands or striations in which fatigue cracks are known to originate.4-6 It is clear that an understanding of the structure of these slip bands is of key importance in understanding the mechanism of fracture. The evidence presented shows that these regions etch preferentially, possibly because they contain a high density of lattice defects, or as the authors state equivalently, because they are "abnormally distorted." However, it is not possible to conclude that the distortion consists of a high density of vacant lattice sites. The fact of a high total shear strain in itself does not assure a predominance of point defects as opposed to other defects, for example, dislocations. Other evidence in the literature which suggests unusual densities of point defects formed by fatigue7-&apos; refers not to the striations or fissures, but to the material between fissures (the "matrix"). If a choice must be made, the preferential etching would seem to be evidence for a high dislocation density, since dislocations are known to encourage chemical attack in copper;g no such effect is known for the case of point defects. A third alternative is that the slip bands are actually cracked, but that near its tip the crack is too narrow to be detected by the authors&apos; metal-lographic technique. In this case the rapid etching can be readily understood in terms of the increased chemical activity of surface atoms. Unless a vacancy mechanism is operative, the motion of dislocations to-and-fro on single slip planes will not lead to crack growth. Point defect or dislocation loop generation are the principal non-reversible effects predicted by this model. In any case, the nonuniform roughening of the surface in a slip band6 requires a flexibility of dislocation motion which is not a part of the to-and-fro fine slip idea. The same is probably true of crack growth by a shear mechanism. Either some dislocations must change their slip planes near the end of the band and return on different planes,&apos;0 or dislocations of opposite sign annihilate." The mechanism by which these processes occur in copper at room temperature or below is that of cross slip. Thus cross slip appears to be essential to fatigue crack growth.6&apos;10"12 The fact that a tensile stress opens the slip bands into broad cracks does not indicate the structure of the bands or the mechanism by which cracks form. The charactersitic concentration of slip into bands during fatigue shows a low resistance to shear strain in these regions. (This fact in itself may be inconsistent with a high concentration of vacancies.) The authors contend also that continuing shear produces an additional mechanical weakening so that the bands fracture easily (are pulled apart) under the influence of the superimposed tensile stress. It is equally possible that the only weakness is a weakness in shear, that the crack propagates by a shear mechanism, and that subsequently the tensile stress pulls the crack apart. Even the direct observation of bands opened by a tensile stress would not be conclusive since, as argued above, they may be fine cracks. The same argument applies to internal cracks, their existence in the presence of a tensile stress not indicating the mechanism of formation. Internal cracks originating in regions of heavy shear have also been seen following tensile deformation of OFHC copper,13 so that this mode of fracture is not unique to combined tensile and fatigue straining. The authors point out in their companion report14 that 90 pct of the cracks formed during pure tor-sional strain were within 8 deg of the normal to the specimen axis. If the tensile stress were an important factor in crack propagation, it is surprising that the cracks cluster about the plane in which the normal stress vanishes. Similarly, a study of zinc single crystals showed that for various orientations the life correlated well with the resolved shear stress on the basal plane,&apos;= and was not dependent on the normal stress across this plane. W. A. Wood and H. M. Bendler (Authors&apos; reply) -Dr. Alden&apos;s discussion emphasizes the essential point in the relation of slip band structure to

Jan 1, 1963

By Lawrie DC

Finely ground beryl was decomposed by mixing with ground limestone and soda ash andheating at 900¦C for,4-6, hours.The sintered material was then crushed and leached by boiling under reflux with 5N sulphuric acid for up to 4 hours. The liquor containing Be, ; Al, . Fe and, other elements as sulphates, was separated from the residue which consisted mainly of silica and gypsum, either&apos; by filtration or by decantation washing.The clarified leach liquor.was first treated to remove Fed}: , by contacting with a primary amine-kerosene solution in2 counter-current stages. The iron free liquor wa,s then passed to a 4-stage counter-current extraction unit where it was con-tacted with 0.5M di-(2 ethyl hexyl), phosphoric acid (EHPA) in kerosene. The&apos;operating conditions were such that at least 99 p&apos;br cent of the Be and only 7&apos; per&apos; cent of the Al- was, extracted The ,B6`= and. Al were ;stripped from the organic phase by sod-ium hydroxide solution of suitable concentration to form soluble "beryllate" and "aluminate" respectively. Most of the Be was subsequently precipTitated a&apos;s Bo(OH)2 by-hoating the alkaline solution to 90C, the Al remaining in solution. After filtra-tion and washing, the Bo(OH)2 could be ignited directly to BeO at about 1000 C or used as a feed to further purification stages aimed at producing "nuclear grade" BeO.A small coaAter-current extraction unit was operated con-tinuously using liquor derived from the sintering and leaching stages. Data obtained in batch laboratory tests were confirmed. A product obtained by ignition of the washed "beryllate" precip-itate contained more than&apos;99 per cent BeO.

Jan 1, 1963