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By J. Leja, J. H. Schulman

FROTH flotation is usually effected by the addition of a collector agent and a frothing agent to an aqueous suspension of suitably comminuted mineral ores. The action of collectors is to adsorb onto the surfaces of minerals to be separated, sensitizing them to bubble adherence. The action of frothers has, in the past, been accepted as that of froth formation only, brought about by a lowering of the air/water interfacial tension. Substances capable of producing froth are classed1a,b according to their relative capacities for production of froth-volume and froth stability in the simple frother-water system. The purpose of this paper is to show that the surface active agents acting as frothers become effective only when there is a suitable degree of molecular interaction taking place between collector molecules and frother molecules at the air/water and solid/ water interfaces. Further, the discussion will demonstrate that the actual mechanism of adherence of an air bubble to a suitably collector-coated particle is due to the molecular interaction collector-frother. This leads to the formation of a continuous interfacial film of associated molecules, anchored to the mineral by polar groups of the collector, and enveloping the whole bubble. The tenacity of adhesion mineral-to-bubble results from the strength and the visco-elasticity of this mixed film.

Jan 2, 1954

By S. H. Ash

SAFETY records have improved in all branches of the mineral industry. While annual production was rising from $2 billion in 1910 to nearly $12 billion in 1950, fatalities decreased from 3539 in 1911 to 974 in 1951. And, although safety progressed under hand methods, it progresses more effectively under modern, mechanized methods. But powered devices such as electric or diesel units can in themselves create new hazards unless proper safeguards are instituted. Health Use of diesels underground is increasing. Diesel equipment has been used in construction of 34 tunnels in 16 states in the last 17 years. The 77 noncoal underground mines in 24 states using diesels underground range from mines with large open stopes to those with narrow veins, so that the ventilating problems represent a good cross-section of U. S. mining. The U. S. Bureau of Mines has received no report that anyone has suffered ill effects from the proper use of properly maintained equipment. The necessity for correct maintenance and use of satisfactory exhaust conditioners cannot be emphasized too strongly.

Jan 2, 1954

By George M. Schwartz

WHEN reviewing the progress made in mining geology for the year 1953, one might say that not much has been accomplished and, indeed, in a subject such as economic geology not much progress should be expected in the 10 months of the year which elapsed before this article was prepared. This seeming lack of progress, however, disappears when the facts are investigated a bit. There undoubtedly are more economic geologists at work than ever before. It is probably not an exaggeration to say that more geologists are now employed by a single company in the Lake Superior district than were employed in the whole district 20 years ago. In most mining districts geologists are busy with numerous problems of production, development, and exploration and some give an occasional thought to the scientific problems of the science, or rather the art, of mining geology. In fact, this very intense activity of mining geologists is one reason why progress seems slow; they do not have time to write up results of investigations. There is also a great amount of work being done which is not released because of company policy. Conditions have improved very much in recent years but mining corporations, in general, have some distance to go before attaining par with the petroleum industry in this respect.

Jan 2, 1954

PRODUCTION of nonmetallic mineral raw materials used by the fertilizer, ceramic, chemical, and construction industries and many others, was greater during 1953 than in any previous year. Production of fertilizer minerals was the highest in history despite somewhat decreased consumption in the second half of the year. Marketable phosphate rock production increased 10 pct to an estimated total of 13.1 million LT, valued at $78.5 million, and potash production was estimated at 1.8 million tons of K2O equivalent, valued at over $60 million. Crude gypsum output exceeded the 1952 total and approached the record of 8.66 million tons mined in 1951, with indications that 1953 will show a new all-time high. Gains and losses among gypsum products were irregular, with major gains in plate- glass and terra-cotta plasters, sanded building plasters and miscellaneous building plasters, and principal declines in base-coat plasters, prepared finishes and tile. Lath and wallboard outputs were each about 20 pct higher than in 1952.

Jan 2, 1954

By R. L. Loofbourow, Roger V. Pierce

THE degree to which our mineral requirements are being met by mining leaner, more complex or more remote deposits is indicated by developments during 1953. Heavy capital investment, skilled technical advice, planning, and able execution are requirements for the typical venture. Producers, faced with rising costs and with softer prices, are seeking improved mining and recovery. Developments in production of iron ore are typical of the course being followed in metal and nonmetal mining. Iron ore development in the U. S. is concentrated on the spectacular work with Lake Superior taconite, while in Canada new production is expected from Labrador and output from Steep Rock, Algoma, and Newfoundland is being increased. Shipment of iron will soon be made from Venezuela.

Jan 2, 1954

By J. E. Andersen, J. Halpern, C. S. Samis

In the presence of oxygen, galena is oxidized in an aqueous medium containing sodium hydroxide, in accordance with the following reaction: PbS + 2O2 + 3OH ? HPbO2 + SO4 = + H2O A novel method was devised for following this reaction which takes place in an autoclave under oxygen pressure, by measuring the concentration of HPbO2- in the solution with a cathode ray polarograph employing stationary platinum electrodes. Using this procedure a study was made of the kinetics of the reaction, in which the effect of a number of variables, including temperature, oxygen pressure, NaOH concentration, and agitation, on the rate, were determined. The results of this study are described and discussed, in terms of possible mechanisms for the reaction. IT is known that sulphide minerals can be oxidized in aqueous media in the presence of oxygen under pressure. Reactions of this type can be classified in two categories depending upon whether the products of oxidation are insoluble or soluble in the aqueous medium. An example of the first type of reaction is the oxidation of pyrite in alkaline solutions, giving rise to an insoluble iron oxide. The kinetics of this reaction have been investigated and its mechanism established.' It has been applied in the oxidation of iron sulphides present in refractory gold ores to improve the subsequent recovery of gold by cyanida-tion.' The second type of reaction finds application where it is desired to recover the metal by leaching during oxidation. In this case a medium is selected in which the oxidized mineral is soluble. For example, nickel, copper, and cobalt sulphide ores can be treated by oxidation in the presence of a solution of ammonia dissolving the nickel, copper, and cobalt as the metal ammine sulphate salts.:' A similar treatment has also been reported to apply to zinc sulphide ores.' It is known that lead sulphate is soluble in solutions of sodium hydroxide or ammonium acetate. It should therefore be possible to dissolve the lead from galena ores by aqueous oxidation with oxygen under pressure using either of these solutions. The applicability of the ammonium acetate treatment has been investigated and confirmed in a recent study.' The present paper describes the results of a similar study in which the kinetics of the oxidation of galena in sodium hydroxide solutions have been investigated. The object of this investigation was pri- marily to obtain information of a fundamental nature relating to the kinetics and mechanism of this reaction. The use of pulps of comminuted ore in a study of this type is undesirable because of the difficulty in controlling and measuring the surface area. The measurements were therefore made using galena crystals of measured surface area and in this way absolute reaction rates were obtained. The reaction was found to proceed as follows: PbS + 2O2 + 3OH ? HPbO2 + SO4 + H2O [I] The products are sodium plumbite and sodium sulphate salts which dissolve in the aqueous solution. The reaction studies were carried out in an autoclave in which a desired pressure of oxygen was maintained. The reaction was followed by measuring the concentration of lead in the solution with a cathode ray polarograph. The results obtained in this investigation are presented and discussed in the present paper. Experimental Materials: The crystals of galena were obtained from Violamac Mines, Sandon, B. C. The following impurities were indicated by spectrographic analysis carried out by the Provincial Assay Office, Victoria, B. C.: Sn, 0.02 to 0.2 pct; Sb, 0.07 to 0.7; Zn, 0.01 to 0.1; Si, Fe, Mg, As, less than 0.05 pct; Ag, 126 oz per ton, the latter determined by standard fire-assaying procedure. After cutting a specimen measuring approximately 5x7x12 mm, the crystal surfaces were ground parallel to the 100 axes using No. 2 emery, washed with water, and the dimensions were measured with a micrometer. Oxygen gas was of commercial grade and supplied in cylinders by Canadian Liquid Air. Solutions were made up with chemicals of chemically pure grade and distilled water. Equipment: Autoclave: The autoclave used in these studies was constructed of stainless steel and

Jan 1, 1954

By H. M. Zoerb

Based on the belief that operating details are a definite contributing factor to major economies, this paper traces the development of crushing cavity design in Symons cone crushers to attain maximum liner utilization. Wear rates are analyzed and compared in this presentation and drawings illustrate succeeding design changes. IN these times of rising labor and material costs, it has become more and more necessary that attention be paid to some operating details which, in their obscurity, may he the key to major economies. Liner wear in crushing cavities of secondary and tertiary crushers can become an appreciable cost item when the material to be crushed is hard and abrasive. This item of cost not only includes the value of the crushing members, but also more intangible costs such as labor and lost production due to more frequent replacement. The variables which are encountered in ores and minerals to be reduced; the design of plant and machine application; the sizes, shape, and fineness, characteristics of the crushed product; the moisture; hardness; friability; and abrasiveness of the material to be crushed are all influencing factors which must be taken into consideration in the selection of a crusher, and particularly in the design of crushing cavity and liners to be used in a crusher. Through a research program undertaken in cooperation with many operators of Symons cone crushers a new approach to crusher cavity design was made, resulting in the development of liners for specific operations which showed: 1—maximum utilization, as high as 70 to 80 pct of original weight of metal, and 2— maximum capacity of unit during the greater portion of its life. It has been found that liners so designed for a given operation will show added economies in power consumption, maintenance, and general wear and tear on the crushing unit. Initial work in the so-called tailoring of crushing cavitles was begun on the tertiary or fine crushing units where as a rule reduction ratios were low, varying from 3 to 6. Parallel or sizing zones in the lower portion of the crushing cavity were too long, resulting in a tendency to pack. It was found that very little additional crushing was done in the parallel zone after the initial impact in that zone and that a relatively small amount of' additional crushing was done by attrition, which required very careful feed control. A small amount of over-feeding would result in packing which not only consumed power but caused unnecessary liner wear as well. The illustrations which follow in this discussion will show only contours of crushing cavities, and for purposes of simplification the cavities will be considered only in their closed position. The first step, therefore. was to reduce the sizing zone to a minimum. This was done by removing the lower portion of the liner as shown in Fig. 1. The result of the change was a saving of 15 to 20 pct in liner cost, less power consumption, with no change in capacity. This change in design, while an improvement, did not go far enough. As wear took place, the change in the liner was not uniform throughout its entire length, resulting in a restriction of the feed opening and thereby loss of capacity. Furthermore, progressive wear of the liner had the effect of lengthening the parallel zone until finally the entire crushing cavity was all parallel zone, see Fig. 2. It is obvious from the reduced feed opening of the worn liner that the ability of the machine to receive material is lessened considerably. Furthermore, the long parallel zone with its worn, irregular profile did not operate at its highest efficiency. The first attempt to overcome this difficulty was carried out on a 5 1/2-ft crusher installed in a plant producing roofing granules. The material being crushed was a very hard graywacke and the crusher was closed-circuited with a screen having .232-in. slotted openings. A radical change in contour was developed, as illustrated in Fig. 3. Equal wear lines on both concave and mantle are designated 1, 2, 3, etc. The method of development of this contour is as follows: Since adjustment for wear is vertical, corresponding intersections of wear lines and vertical lines developed concave and mantle contours which maintained equal but lengthening wear surfaces in the parallel zone. The ideal contour, of course, is one in which the length of the parallel zone remains constant, but because of present foundry practice and heat treating characteristics this is impossible.

Jan 1, 1954

By Frederick F. Frick

SPONGE iron as produced at Anaconda is a fine, -35 mesh, impure product, about 50 pct metallic iron, obtained from the reduction of iron calcine at a temperature of 1850°F by use of coke resulting from slack coal. The metallic iron particles are bulky and spongey and precipitate copper readily and rapidly from a copper sulphate solution. Investigation of the treatment of Greater Butte Project, Kelley, ore at Anaconda early showed the desirability of using sponge iron as a precipitant for the copper in solution resulting from desliming of the ore in a dilute sulphuric acid solution. Anaconda had done considerable work on the production of sponge iron in 1914 for use as a precipitant of copper from leach solutions. Some success and considerable experilence were attained at the time. indicating that, sponge iron might be successfully made by a modification of the process used in 1914, a batch process in which an iron calcine was reduced by means of soft coke, resulting from noncoking coal, in a Bruckner-type revolving horizontal cylindrical furnace widely used 50 years ago. The coke and calcide formed the bed in the Bruckner furnace, which was rotated at about 1 rpm. The bed was brought to a temperature of about 1800°F by means of an oil flame over the surface. Although results were reasonably satisfactory, they did not warrant full development of the process at that time. A good deal of work has been done in the last 50 years on the production of sponge iron. The objective in some cases has been the production of a precipitant for copper from solution, but the bulk of the work has been done for the production of open-hearth steel furnace stock. The production of an open-hearth stock presents two problems rather than one: first, producticon of the sponge iron, and second, what is perhaps of equal difficulty and importance, conversion of the sponge iron into a form suitable for use in the open-hearth furnace. So far as is known to the writer, none of the sponge iron processes tried in the past have proved to be economically feasible. However, Anaconda had a combination of conditions appearing to justify an attempt to produce sponge iron which would serve for the leach-precipitation-float process. It was thought that the process used in 1914, if changed to a continuous one, might work out satisfactorily. The following favorable conditions at Anaconda justified the investigation: 1—A sufficient tonnage of good grade iron calcine resulting from the roasting of a pyrite concentrate in one of the acid plants, at substantially no cost. 2—Reasonably cheap natural gas. 3-—The fact that there was no need for production of a high grade product. 4— The fact that there was no need for obtaining a consistently high reduction of' the iron in calcine. A small revolving Bruckner-type furnace about 2 ft ID by 4 ft long was set up for early pilot work at the research building. This pilot furnace showed that a satisfactory product could be obtained at reasonable cost. It also indicated a marked advantage in preceding the reduction furnace with a furnace of similar size and capacity for preheating and roasting out any residual sulphur from the feed. The small furnace was operated for several months, various details of the process were worked out. and sponge iron was produced to supply a pilot LPF plant which treated 300 lb of Kelley ore pel- hr. Later a second pilot furnace 5 ft in diam and 12 ft long inside was set up at our reverberatory furnace building. This furnace confirmed the data of the small furnace and gave a basis for design of the final plant. At Anaconda a pyrite concentrate, running about 48 pct S, is recovered from copper concentrator tailings by flotation. This concentrate is roasted to sulphur of 3 pct or less at the Chamber acid plant. The iron calcine contains about 57 pct Fe and 18 pct insoluble. The iron calcine feed, as mentioned before, is re-roasted and preheated in a reroast furnace preceding the reduction furnace. Both are of the Bruckner type. The reroasted calcine is fed into the reduction furnace at 800" to 1000°F along with 30 pct slack coal. In the feed end of the furnace the volatile is burned from the slack, giving a soft coke which readily serves for reduction of the iron. Hard metallurgical coke will not serve the purpose. since it does not reduce CO readily at a temperature of 1850°F. All indications are that the actual reduction of the iron is accomplished by carbon monoxide below the surface of the bed, which is 30 in. deep at its center. Apparently there is a constant interchange: Fe²O³ + 3CO = 2Fe - 3CO², CO² + C = 2CO Actually iron oxide is reduced by CO at somewhat lower temperature than the 1850 °F used in the process. but this temperature is necessary to obtain a satisfactory rate of furnace production. The furnace atmosphere is generally reducing, and typical blue carbon monoxide flames satisfactorily cover the bed. Gas flames from four 3-in. Denver Fire Clay Inspirator burners are played directly on the bed, which is slowly cascaded by the 1 rpm of the furnace. An excess of coke is necessary to assure maintenance of good reducing conditions in the furnace bed. Part of this coke is recovered for re-use.

Jan 1, 1954

By John D. Price

R. W. Campbell (Jones and Laughlin Steel Carp., Pittsburgh)—As usual John Price has presented an excellent paper. I know of no one who has devoted more time and conscientious thought to this subject than he has, and his efforts have produced scientific data and conclusions of real value. Results of similar studies made by the Jones and Laughlin Steel Corp. on the blending of Pennsylvania coals may be of interest. During 1935 the late F. W. Wagner and the present writer developed an empirical physical fuel value formula for evaluating the combined physical tests of metallurgical coke, see Table IV. In the development of the formula, the tumbler test, shatter test, screen test, and porosity of coke have been taken into consideration. Each of these tests brings out some physical property not expressed by the others, and in estimation of the importance of these tests as a medium for evaluating coke for the blast furnace, their worth has been graded as follows: It was thought that some additional penalty should be applied to cokes that do not show a uniform screen size, assuming that coke larger than 4 in. was not desirable and that this size was an indication of irregular size. Therefore the screen test factor is further corrected by applying a penalty of 1 pct for each 1 pct material greater than 4-in. size as shown by the screen test. The physical fitness of coke for blast furnace use depends upon four fundamental characteristics: l—gen-era1 strength, as indicated by the shatter test; 2— abradability, or the resistance of cell walls to reduction in size by attrition, as indicated by the tumbler test; 3—porosity; and 4—size and uniformity. Each of these characteristics is not of equal importance, but surely, in an attempt to determine an accurate physical value, the individual value of each should be taken into consideration. The formula is used as a yardstick, so to speak, in determining variations in the normal production of metallurgical coke and in making comparisons between normal coke and experimental blends with other coals. Table IV gives results of coking tests on raw and washed high volatile coals and these same coals with blends of coke breeze, anthracite coal, char and low volatile coals, all from Pennsylvania. The table also gives the source of the coals and coke breeze, as well as their proximate analyses. It will be noted that the washing of the raw high volatile coal increased the physical fuel value from 26.17 to 39.16, showing the effect of removing shale and slate which produces a detrimental fracturing and weakening of the coke. It is a well known fact that many Pennsylvania high volatile coals contain an excess of resinous material or binder which has a tendency to weaken the coke, owing to its high evolution of gases during carbonization. Tests were therefore made with coke breeze, an inert material, in an attempt to alleviate this condition. Blends of washed coal with 5 pct and 7.5 pct coke breeze collected from the coke plant quenching sump (82.9 pct through 1/8-in. screen) resulted in cokes with a physical fuel value of 20.75 and 16.73 respectively, lower than results obtained from 100 pct raw high volatile coal. It will be noted that the percentage of + 4-in. coke increased but that the tumbler test was very low. Undoubtedly better results could have been obtained if the coke breeze could have been crushed extremely fine. During World War II the government asked the coking industry to consider the use of anthracite coal as a substitute for high quality low volatile coal, which was extremely scarce at the time. The next series of tests was made with blends of raw and washed high volatile coals and 5, 10, and 15 pct Pennsylvania No. 5 buckwheat anthracite (100 pct through l/8-in. screen). It was necessary to use some raw high volatile coal in these blends because of insufficient washer capacity at the time. It will be noted that the physical fuel values

Jan 1, 1954

By D. F. Gibbons

THIS investigation was undertaken in order to gain further information on the mechanism of plastic deformation of iron at temperatures between room temperature and 77.2°K, and also to contribute to our understanding of the low temperature brittleness phenomenon that occurs in both the tensile and impact tests. It was decided to study as pure an iron as possible and to use the tensile test in order to simplify the problem as much as possible. Two series of iron were used throughout the investigation: iron A, obtained from the National Research Corp. and supplied as gas-free, high purity iron; and iron B, obtained from Fast' and produced by melting iron under purified hydrogen. Typical analyses of samples of both irons, after fabrication, are given in Table I. The main difference in composition of these irons is in their nickel and oxygen contents. Nickel has a very large solid solubility in iron. However, oxygen has an extremely small solid solubility. An attempt was made to reduce the oxygen content still further by remelting under purified hydrogen. This was successful in reducing the oxygen content to -0.0006 pct. However, no results on tests of this iron are included, since difficulty was encountered in fabricating the ingot. Wire specimens 1 mm in diameter were used for the investigation. The wires were produced from the ingots, as supplied, by cold rolling and swaging, with intermediate vacuum anneals at 700°C. Care was taken to reduce preferred orientation in the wires to a minimum by keeping the percentage of reduction in area between anneals of 30 to 40 pct. X-ray transmission photographs showed no indication of preferred orientation. The final grain size of iron A was 20 to 24 grains per linear mm and of iron B, 16 to 18 grains per linear mm. All specimens were tested in the decarburized and denitrided condition unless otherwise stated. The procedure was to pass hydrogen, saturated with water vapor at 26oC, over the specimens at 730°C for 2 hr. The specimens were quenched in iced water and then annealed in a vacuum of - 5x10-6 mm Hg for one day at 560°C to remove hydrogen. Higher temperatures were used for the vacuum anneal but this temperature was found to be quite satisfactory in removing hydrogen. The specimens were slow-cooled after the vacuum anneal. Where it is stated that the specimens were carburized, the specimens were given an identical decarburizing treatment and then carburized by passing hydrogen, saturated with pure n-heptane vapor at 0°C, over the specimens at 730°C. The specimens were then homogenized at 730°C for 2 hr in dry hydrogen. After the carburizing treatment the specimens were given the same vacuum anneal as for the decarburized specimens. The carbon content was determined from the maximum value of the internal friction carbon peak.2 Apparatus Fig. 1 shows a diagram of the tensile apparatus, with half the cooling coil removed. The cooling coil enabled temperatures from 200" to 77.2oK to be obtained. The apparatus was designed to fit a standard Tinius Olsen Universal tensile machine. The apparatus consisted of the rigid plate A which carried two carefully machined hooks H. These hooks attached the plate firmly to the moving crosshead of the tensile machine. The lower grip B was rigidly suspended from the plate A by three stainless steel rods. The upper grip C was joined to the upper grip of the tensile machine by the stainless steel rod E. The lower part of the apparatus was surrounded by a Dewar vessel, which was made a sliding fit inside the brass collar D. The specimen was held in a clamp which fitted into the grip, forming a ball and socket joint (see inset a). This was to attain as nearly pure

Jan 1, 1954

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

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

Jan 1, 1954

By P. A. Albert

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

Jan 1, 1954

By Merlyn B. Buhle

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

Jan 1, 1954

By Rudolph G. Wuerker

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

Jan 1, 1954

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

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

Jan 1, 1954

By J. W. Spretnak, R. Speiser

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

Jan 1, 1954

Jan 1, 1954

By N. K. Chen, R. Maddin

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

Jan 1, 1954

By N. K. Chen, R. Maddin

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

Jan 1, 1954

By C. T. Bischoff

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

Jan 1, 1954