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As REVISED IN CONFERENCE FEB. 17, 1931 REPORT OF SUBCOMMITTEE ON MINE VENTILATION CODE OF A, I. M. E. COMMITTEE ON VENTILATION ALFRED W. HESSE, Chairman THOMAS G. FEAR GEORGE S. RICE E. A. HOLBROOK WILLIAM A. ROWE HOWARD ECKFELDT R. V. NORRIS CADWALLADER EVANS, JR. H..1. SMITH, Secretary REALIZING, from the safety and health standpoint, the need of furnishing air of good quality to workers underground and of diluting and carrying away dangerous and noxious gases, the following code is offered to unify regulatory measures in coal mine ventilation, so far as is practicable, in the United States of America.

Jan 1, 1931

The Institute should feel honored that one of its distinguished members, Auguste J. Rossi, has been awarded the Perkin Medal of the Society of Chemical Industry. The medal was presented at a meeting of the New York Section of the Society on Jan. 18, at the Chemists' Club. Mr. F. A. J. Fitzgerald, Past President of the American Electrochemical Society; described the work of Mr. Rossi, while the presentation address was delivered by William H. Nichols, Past President of the Society of Chemical Industry.

Jan 2, 1918

THE great development of the mines and metallurgical works of this country during the last few years, accompanied as it has been by the investment of enormous sums of money in purchasing lands, and in the erection of improvements, requires that advantage should be taken of the accumulated knowledge of engineers, superintendents, and' others, in mastering &he problems which are constantly presenting themselves for our action. Among those may be mentioned the consideration of more economical systems of mining in our coal and metal-liferous mines, improved methods of transportation above and below ground, unwatering and ventilating mines, the mechanical preparation of coal and other minerals, the various metallurgical processes, and, in fact, every question tending to the attainment of two great objects : 1st. The more economical production of the useful minerals and metals. 2d. The greater safety and welfare of those employed in these industries. In European countries, where the arts of mining and metallurgy have long been the subject of the most careful study, no means have been found so effectual in attaining the end above proposed as the free interchange of experience among those actually engaged in these industries, and this object has been accomplished, mainly, through the medium of institutes, associations or societies, composed of those engaged in these occupations, and by the periodical publication of essays or papers, communicated to such societies by their members. I t must be evident to all practical men that the interchange of the varied experience of those engaged in such occupation in this country could not fail to advance very materially the desired objects; it is, therefore, proposed to establish an American Institute of Mining Engineers, which will hold its meetings periodically in the great mining and metallurgical centers, where works of interest, such as mines, machine shops, furnaces, and other metallurgical works, can be inspected, and the members exchange their views, and consult for mutual advantage upon the difficulties encountered by each; these transactions or proceedings, when published, would form a most valuable and greatly-needed addition to our professional literature. I t is proposed that a meeting of those sympathizing with the object above mentioned shall be called for the purpose of organizing such an association, the place and time of meeting being Wilkes-Barre, Pa., and the month of April or May. Communications indicating the opinion and wishes of all, both as to these points, and also as to the organization and objects of the Institute, will be gladly received by any of the undersigned, and a notice of the date of meeting, which will be arranged to suit the greater number, will be duly communicated. Any

By John Gross

THE method of measurement of surface on quartz particles was given in a previous paper.1 With such a method the relation of surface produced in crushing quartz can be compared to the work in crushing without recourse to sieve sizing or microscopic measurement. In crushing, the work input must be known with a fair degree of accuracy. With crushers, rolls, ball mills, and similar apparatus the measurement of the work in crushing is subject to possible errors, due to friction in .the transmission as well as in the machine itself. Moreover, relatively large quantities of material must be crushed to get an average figure. In the selection of a method of crushing, simplicity in design and operation was desired and this was most readily obtained by the use of a free-falling body. A description of the apparatus embodying this principle is given herewith. THE CRUSHING DEVICE The apparatus used is shown in Fig. 1 and in cross-section in Fig. 2. The material to be crushed is placed in the crushing chamber C in the steel mortar M. The mortar is 3 in. dia. by 3 in. high. Two mortars are used, one having a crushing chamber 1-in. dia. by 1/2 in. deep, with a capacity of 4 g. of quartz, the other having a crushing chamber 1 ½ in. dia. by 3/4 in. deep, with a capacity of 12 g. of quartz. The position of the mortar is adjusted by means of three centering screws A. The steel plunger P, which fits neatly into the chamber, is placed on top of the material to be crushed. Plungers of different lengths were tried and as they were found to give practically identical results the length adopted was equal to the depth of the chamber.

Jan 1, 1928

By P. K. Currie, J. V. Walters

Solution mining of magnesium salts (Carnallite and Bischofite) is taking place near Veendam, in the northeast Netherlands. The magnesium salts are used for the production of magnesia sinter, used as a base material for the manufacture of refractory bricks for furnaces. This paper gives, first, an introduction to the operational procedure followed in Veendam, with the emphasis on some of the unique aspects, and then discusses rock-mechanical aspects of the cavity behaviour. The creep behaviour of magnesium salts is described, and Finite Element calculations on cavity stability and potential surface subsidence are discussed.

Jan 1, 1985

By Henry Sturgis Drinker, Rossiter W. Raymond

Jan 1, 1914

By Bauer. Larry G.

The vast coal reserves in the Wyoming, Montana, North and South Dakota region are sufficient to supply the total energy needs of the United States for several hundred years. Not only is there an abundance of this sub-bituminous and lignite coal available, but it is easily obtainable by strip-mining . The overburden varies from several feet to several hundred feet. This western coal has yet another asset, namely, a low sulfur content. Whereas eastern and midwestern coal has a sulfur content of 2.5%, the upper Great Plains coal contains sulfur in the 0.5% range. The importance of the sulfur content of the coal is a direct result of federal government emission standards for sulfur dioxide (SO2). Hand (1) points out that "sub-bituminous coals and lignites have a propensity for retaining this sulfur in the ash under certain conditions which is not evident in higher rank coals." This would tend to reduce further the SO2 concentration in the combustion gases of boilers. Western coal is no panacea, however, in that it is far removed from most population and industrial centers. Furthermore, the moisture content of the coal varies from 20 to 40%. This moisture is almost exclusively inherent, that is, it is chemically and physically bound to the organic matter of the coal. It is believed that the water forms a part of the coal structure perhaps as water of hydration of organic salts or organic acids, perhaps by hydrogen bonding, or perhaps by simple adsorption (2). The primary market for this coal is the electric power industry. Lesser markets will be as coke for the steel industry and possible as a raw material for coal gasification and coal liquefaction plants.

Jan 1, 1983

Robert Carl Sticht, member of the Institute since 1886, an American metallurgist of world-wide reputation, died in St. Margaret's Hospital, Launceston, Tasmania, on April 30, 1922, after an illness of eleven months, against which he fought with the highest courage and characteristic fortitude. The news of his passing came as a great shock to a host of his friends and former associates here, but on account of his long absence from the United States, exact biographical details have been heretofore lacking. Throughout Tasmania, the expressions of public sorrow were many and impressive, and the flags were flown at half-mast in Queenstown, Zeehan, and the entire Mt. Lyell district, in honor of the man who had won his place in the community as a great captain of industry and a man universally admired and loved. Sticht had been connected with the Mt. Lyell Mining & Railway Co. in Tasmania throughout its entire productive period. He had originally been induced to go to Tasmania through the good offices of the late Dr. E. D. Peters, then professor of metallurgy at Harvard University, who after personally examining the undeveloped Mt. Lyell properties, recommended Sticht as the best possible man to work out the complex metallurgical problem which that great orebody presented. Sticht had already made himself the leading authority on pyritic smelting, having taken up the idea as suggested and partly worked out by Lawrence Austin and carried it through to a certain degree of perfection in the case of limited tonnages of special ores. After studying the situation at Mt. Lyell, Sticht found the conditions there to be almost ideal for pyritic smelting, and he had the courage to adopt as the basis for a permanent, and eventually successful, solution of the metallurgical problem, a process that was then little more than a theoretically interesting possibility. The thorough studies and remarkable results attained at Mt. Lyell were published as chapters in Doctor Peters' various publications on the metallurgy of copper, Doctor Peters giving full credit to Sticht for their authorship. These chapters by Sticht practically constitute the: best literature of the art of pyritic smelting. The accuracy of observation,

Jan 1, 1923

Robert Carl Sticht, member of the Institute since 1886, an American metallurgist of world-wide reputation, died in St. Margaret's Hospital, Launceston, Tasmania, on April 30, 1922, after an illness of eleven months, against which he fought with the highest courage and characteristic fortitude. The news of his passing came as a great shock to a host of his friends and former associates here, but on account of his long absence from the United States, exact biographical details have been heretofore lacking. Throughout Tasmania, the expressions of public sorrow were many and impressive, and the flags were flown at half-mast in Queenstown, Zeehan, and the entire Mt. Lyell district, in honor of the man who had won his place in the community as a great captain of industry and a man universally admired and loved. Sticht had been connected with the Mt. Lyell Mining & Railway Co. in Tasmania throughout its entire productive period. He had originally been induced to go to Tasmania through the good offices of the late Dr. E. D. Peters, then professor of metallurgy at Harvard University, who after personally examining the undeveloped Mt. Lyell properties, recommended Sticht as the best possible man to work out the complex metallurgical problem which that great orebody presented. Sticht had already made himself the leading authority on pyritic smelting, having taken up the idea as suggested and partly worked out by Lawrence Austin and carried it through to a certain degree of perfection in the case of limited tonnages of special ores. After studying the situation at Mt. Lyell, Sticht found the conditions there to be almost ideal for pyritic smelting, and he had the courage to adopt as the basis for a permanent, and eventually successful, solution of the metallurgical problem, a process that was then little more than a theoretically interesting possibility. The thorough studies and remarkable results attained at Mt. Lyell were published as chapters in Doctor Peters' various publications on the metallurgy of copper, Doctor Peters giving full credit to Sticht for their authorship. These chapters by Sticht practically constitute the: best literature of the art of pyritic smelting. The accuracy of observation,

Jan 1, 1923

By C. L. Berrier, Wm. B. Daly

Jan 1, 1923

By Wm. B. Daly, C. L. Berrier

Jan 1, 1923

By O. W. Ellis

The writer has dealt with the effect of various methods of melting copper upon the gas content of the metal.' The copper referred to in his earlier paper was melted in the foundry both in the oil furnace and the electric furnace. As the metal did not measure up to conductivity standard, the term "casting copper" was applied to the material in the title of the paper. It was thought that some information in regard to the gases in a sample of overpoled copper might also be of interest, and through the courtesy of C. R. Stevens, superintendent of the copper mill of the West-inghouse Elec. & Mfg. Co., such a sample was obtained. The metal was chill-cast in the form of an ingot about 7 in. long, 2 1/2 in. deep (from the base to the raised surface of the ingot) and from 1 3/8 to 1 7/8 in. wide. A photograph of part of the ingot is shown in Fig. 1. The effect of over-poling on the surface of the metal is here quite clearly shown.

Jan 1, 1929

By O. W. Ellis

The writer has dealt with the effect of various methods of melting copper upon the gas content of the metal.' The copper referred to in his earlier paper was melted in the foundry both in the oil furnace and the electric furnace. As the metal did not measure up to conductivity standard, the term "casting copper" was applied to the material in the title of the paper. It was thought that some information in regard to the gases in a sample of overpoled copper might also be of interest, and through the courtesy of C. R. Stevens, superintendent of the copper mill of the West-inghouse Elec. & Mfg. Co., such a sample was obtained. The metal was chill-cast in the form of an ingot about 7 in. long, 2 1/2 in. deep (from the base to the raised surface of the ingot) and from 1 3/8 to 1 7/8 in. wide. A photograph of part of the ingot is shown in Fig. 1. The effect of over-poling on the surface of the metal is here quite clearly shown.

Jan 1, 1929

By C. Law McCabe, R. G. Hudson

The Knudsen cell has been employed to determine the free energy of formation of Mn7Cs in the temperature range 800" to 950°C. A value of 66,440 cal was found for hH°o for a-manganese. Measurements of the pressure of manganese over a mixed carbide, (Fe,Mn),C, points to a power relationship between aun7cs and N.4,. RECENTLY Kuo and Perssonl have reported that the carbide of manganese which is in equilibrium with graphite at temperatures up to 1100° C is Mn7Ca. There are no published data on the thermo-dynamic properties of this compound. In order to determine the stability of Mn7Ca, it appeared that, by obtaining the pressure of manganese above 8-manganese and also above Mn,C, in equilibrium with graphite, the free energy of formation of Mn7Ca from 8-manganese and graphite could be obtained. In addition, the vapor pressure of manganese, reported by Kelley From data of Bauer and Brunner,' is subject to some uncertainty and further determinations of the vapor pressure of manganese seemed warranted. In this investigation of the pressure of manganese vapor above pure manganese and also above the carbide of manganese in equilibrium with graphite the apparatus used is the Knudsen orifice cell. The same apparatus, experimental procedure, and method of calculating the pressure was used in this investigation as in one previously reported.~ Care was taken to insure that the cells were at constant weight before using them in a run. The manganese charged in the cell was CP grade powder, carbon free, obtained from the Fisher Scientific Co. A spectroscopic analysis of the manganese after appreciable amounts of it had vaporized from the Knudsen cell showed that no element was present in sufficient quantities to contribute to a weighable weight loss or to decrease the vapor pressure of manganese to any appreciable extent. The spectro-graphic analysis was 0.002 pct Cu, 0.05 pct Fe, 0.002 pct Pb, and 0.002 pct Ni. 8-manganesea is the allo-tropic form of manganese which was present in the cell at temperatures used in this investigation. The manganese carbide, Mn,Ca, was made in the following way: In a closed graphite cell manganese powder was added to graphite powder, which was made from graphite rods for spectrographic use. The manganese powder was the same as that described previously; 5 pct excess graphite was added over that required for the formation of Mn7C,. The mixture was heated in a closed graphite cell for approximately 20 hr at 1350°K under vacuum. X-ray analysis revealed that there was no manganese present after this treatment, but that the lines due to Mn,C, were present. In order to prove that there was no volatile carbide of manganese which was effusing out of the cell, the following experiment was performed: A graphite effusion cell containing graphite power, in excess of that to form Mn,C, of a desired amount, was brought to constant weight on heating at 1228°K. The required amount of manganese was accurately weighed and then added to the graphite effusion cell. The cell was placed in a vacuum at 1228°K for one week, which was the time calculated for the manganese to have effused completely, assuming instantaneous formation of Mn,C8. The cell was then weighed again. This experiment was carried out on two different occasions and both times the weight loss of the cell came within 1 pct of the weight of manganese originally charged minus the weight of manganese left in the cell, as determined by chemical analysis. These data are summarized in Table I. This agreement is considered to be within experimental error and is taken as proof that no carbide of manganese is volatile in this temperature range. It was established, by X-ray analysis, that Mn,C, formed before appreciable amounts of manganese vaporized from the metal powder which was charged. The identification of the carbide of manganese which was present in the Knudsen cell in equilibrium with graphite and manganese vapor was carried out by Kehsin Kuo at the University of Uppsala. He established that the authors' sample, which was submitted to him for analysis, contained the phase

Jan 1, 1958

By Arthur Knapp

NEARLY every technical man is called upon at some time in his life to deliver a paper before a technical audience or to write a technical paper for publication. It is not necessary to be an accomplished public speaker to deliver a technical paper successfully; it is only necessary to bear in mind a few obvious points. Poorly presented papers are nearly always the result of a few errors of deportment, but they are vital and at the same time so obvious that they are often overlooked. Experience is a good teacher but a little study and careful preparation will moderate the suffering of both an amateur speaker and his audience. An author's paper suffers, through poor delivery, in direct proportion to the suffering of his audience. The best test of a paper is to have it read aloud to the author. This will bring out faults not apparent when read silently by the author. Some of the things which will probably need correcting are improper phrasing, noneuphonic sequences, and long or involved sentences. Frequently authors write their papers in short crisp sentences for oral presentation, then rewrite them for publication.

Jan 1, 1942

By R. W. Raymond

THE situation in 1872, from the standpoint of the prospector, the locator, the possessory claimant, and the patentee of mineral land under Federal statutes, cannot be understood without a knowledge of the situation prior to 1866, and between 1866 and 1872. The Situation before 1866 The western public domain acquired by the United States through treaties, as the result of conquest or purchase, was invaded after Marshall's re-discovery of gold in California, by an overwhelming multitude of prospectors and miners from all parts of the world. The mineral lands of the whole Pacific slope were practically unsurveyed. Congress, disgusted with the experiment of leasing mineral lands; which it had tried for 40 years, and abandoned in 1847, enacted no laws for the management of these public mineral lands, and the pioneers made their own laws governing mining titles. These local regulations applied at first to gulch-mining in the auriferous river-beds only; and they constituted a simple and practical system, adapted to the needs and means of primitive communities-significantly called "camps." They had the means of measuring distances, but not angles; they knew no -property except personal property in the form of pickaxes, pans, supplies, camp-equipage, horses or mules, and mining rights. The earliest codes which they developed expressed what might be called the law of the lariat. With the lariat they measured the distance assigned to each miner along the gold-bearing gulch-a double portion to the discoverer, and a single portion to his successors, in the order of their coming. With the lariat, they hung, after such due process of law as was available, the rascal who stole a horse, or a bag of gold-dust, or a; mining claim, or killed another man without giving him fair notice and a chance to defend himself. In these pioneer codes, adopted in mass-meetings and enforced by the same authority, two features concern us most:

Jan 4, 1914

By D. Harker, E. Epremian

The constitution of the nickel-tungsten system has been studied by a number of investigators, the most recent of which are Ellinger and Sykes.1 On the basis of metallography, electrical resistivity and hardness measurements and some X ray diffraction work, they constructed a consitution diagram (Fig 1). Ellinger and Sykes report a0 for the alpha face-centered cubic phase (nickel saturated with tungsten) as 3.66?.‡ The gamma phase (tungsten saturated with nickel) is given as body-centered cubic, but no value of a. is recorded. At 43 pct tungsten by weight (approximately 20 at. pct) a beta phase is reported, but structure and lattice parameter are not known. Primarily on the basis of metallographic evidence, they conclude that beta is a new phase and rule out the possibility of formation of a superlattice since they- observe a new phase in the microstructure. Grube and Schlecht2 report an ordering reaction in a system similar to the Ni-W (Ni-Mo) and Harker3 has shown that NirMo forms a superlattice upon the pre-existing face-centered cubic lattice of the alpha phase. Elliniger arid Sykes observed a change in the diffraction pattern of a 4.3 pct W alloy upon aging and attributed it to the formation of a new phase. Thus, there appears to be some question as to the character of the beta phase reported by Ellinger and Sykes. The purpose of the present work is to determine precisely the structure and nature of the beta phase in the Ni-w system of X ray diffraction methods. Experimental Procedure One inch diameter ingots of 43.66 pct, 40.15 pct and 34.06 pct .tungsten by weight (19.8, 17.6 and 14.1 at. pct respectively) were melted and cast under vacuum from electrolytic nickel and pure wire filament grade tungsten. The ingots were soaked for 16 hr at 1300°C in a hydrogen atmosphere furnace, then swaged at this temperature and finally drawn to 0.020 in. diam wire. Some of the bar stock was retained in 1/2 in. diam rod for hardness and metallographic studies. Wire samples for diffraction work were sealed in evacuated quartz tubes and subjected to the various solution and aging heat treatments in a hydrogen furnace. X ray photograms were taken in a Debeye-Slierrer camera using copper K radiation filtered by nickel foil. Results X RAY DIFFRACTION The lattice parameters of the alpha and gamma phases at saturation were determined by an X ray photogram of the 19.8 at. pct W alloy after solution heat treatment at a temperature well within the alpha-gamma range above the peritectoid temperature (17 hr at 1150°C—oil quenched). The alpha phase was found to be face-centeted cubic with a. of 3.594 ± 0.001?, while the gamma phase was determined as body-centered cubic with a. of 3.158 ± 0.001?. Exactly the same phases and parameters were ohtained with the 17.6 at. pct W alloy for the same solution heat treatment. Thorough analysis was made of an X ray photogram of a 19.8 at. pct alloy sample in the quenched and aged condition (solution treated 1T hr at

Jan 1, 1950

By C. J. Delisio

The basic concept of tunnel boring has not changed since the late 1800's. R. Stanley of Great Britain obtained a Canadian patent as early as December 1891. Mr. Stanley's machine was a device that consisted of a rotating wheel equipped with drag-type teeth; it had a means of thrusting the cutterhead against the face or heading; it had a means of clamping or gripping the machine in its bore; it had a means of collecting and depositing the cuttings into a screw-type conveyor located near the invert of the tunnel. It even had a means of varying the speed of the forward motion of the machine to suit different hardnesses of rock encountered. This description essentially fits the latest tunnel-boring machines being built today. In short, there has been no significant advance in the basic concept in 70 to 80 years. It may well be that no significant change can be expected for some time into the future. Today's machines, while still basic in concept, offer many advances aimed at faster tunneling. Among these are 1 ) improved cutters, 2) guidance and steering devices, 3) dust-control devices, and 4) mechanisms to aid in installing tunnel supports. CUTTERS The most important part of a hard-rock tunnel borer is the cutter. If the cutter can cut the rock, it is a boring machine. If the cutter cannot cut the rock, no other part of the machine can. When Jarva, Inc. decided to build a machine, the first problem was to find a good cutter. In our search, we looked at most of the cutters on the market. We selected Reed Drilling Tools' cutter because the design of their cutter was aimed at hard-rock tunneling. We feel that they build the best cutter available and provide the best possible service to their customers. As tunnel-boring machine design advanced, the transition from drag bits to roller bits was natural because harder formations required a roller bit, and it is the goal of all mole users to bore harder formations. Roller bits

Jan 1, 1970

By Charles Waidner

IN response to many urgent requests for a concrete realization of a series of standard temperatures that would be available to any one anywhere for the standardization of pyrometers and the reproduction of the standard scale of temperature for use in laboratories and industrial works, the Bureau, in 1916, made arrangements with several manufacturers to prepare a series of- pure metals that could best serve this purpose. After the necessary preliminary work of chemical analysis, as a check on the purity, together with exact determinations of melting or freezing points, the Bureau began, in 1917, the issuing of melting -point standards of tin, zinc, aluminum, and copper. At the outset, it was decided to secure metals of the highest purity and of American manufacture, and this was accomplished in a more satisfactory manner than anticipated. In the preparation of these temperature standards, the Bureau has had the hearty cooperation of several American companies, which have succeeded in producing metals highly satisfactory for the purpose and of as high a state of purity as could have been obtained anywhere. Each company that undertook the responsibility of furnishing a metal for this series of standards exercised most painstaking care to produce the best possible product as to purity and uniformity. A representative of the Bureau witnessed the actual preparation of each metal. The 300 and 400-lb. (136 and 181-kg.) samples making up the first series were all used up, with the exception of the aluminum, early in 1919. The Bureau has taken steps to replenish its stocks of metals serving as pyrometric standards and to the list has been added lead. The copper and lead are being ordered this time in 1-ton lots and the zinc and tin in 300-lb. (136 kg.) lots as before. The wide dissemination of these samples will be appreciated when it is noted that the metals are distributed by the Bureau inn quantities of 50 cu. cm. each, at $2 a sample and accompanied by a certificate which gives the melting point as determined by samples from the same lot. The manufacture and detailed description of chemical analyses, physical measurements, and precautions in use of these pyrometric standards, are described in detail in the Bureau Circulcar No., 66.

Jan 8, 1919

By R. F. Dickerson, D. A. Vaughan, A. F. Gerds

ALTHOUGH the metallurgy of uranium has been under intensive study since the early 1940's, no systematic effort has been made to identify the non-metallic inclusions in uranium. Uranium carbide (UC), which is probably the most common inclusion found in graphite-melted metal, has been tentatively identified by previous investigators, but the other nonmetallic inclusions have received little attention. Since metallography is a valuable tool in metallurgical studies, the metallographic identification of the nonmetallic inclusions in uranium is important. Such an investigation has been completed and the identification of slag-type inclusions and of uranium monocarbide, uranium hydride, uranium dioxide, uranium monoxide, and uranium mononitride is described. Metallographic Preporation It is often possible to prepare specimens for metal-lographic examination equally well by several methods. The specimens which were examined in this work were prepared by one of two acceptable methods. For the convenience of the reader, both methods will be discussed in detail and will be referred to simply as Method I or Method II in the subsequent sections. For both Methods I and 11, specimens for microscopic examination usually were mounted either in bakelite or in Paraplex room temperature mounting plastic. Method I—Specimens were ground in a spray of water on a revolving disk covered successively with 120-, 240-, and 600-grit silicon carbide papers. It was necessary to perform the final grinding operation carefully on worn 600-grit paper to keep the scratches as fine as possible. After washing and drying, the specimens were polished for 3 to 4 min on a slow speed wheel (250 rpm) covered with a medium nap cloth. Diamet Hyprez Blue diamond polishing paste, Grade 00, 0 to 2 µ, was used as abrasive with kerosene as lubricant on the wheel. Specimens were washed thoroughly in alcohol and final polished electrolytically in an electrolyte composed of 1 part stock solution (118 g CrO, dissolved in 100 cm3 H2O) with 4 parts of glacial acetic acid. A stainless steel cathode was used. At an open circuit potential of 40 v dc, a polishing time of 2 sec retained inclusions well with the bath at room temperature. If additional etching was required to sharpen the interface between the metal and the inclusions, an electrolyte composed of 1 part stock solution (100 g CrO3 and 100 cm8 H20) and 18 parts glacial acetic acid was used at room temperature. Best results were obtained by etching for from 10 to 15 sec at 20 v dc in the open circuit. Surfaces obtained by this method are suitable for microscopic examination. However, if desired, they may be etched further with other chemicals. Method 11—Rough grinding was done on a wet 180- or 240-grit continuous grinding belt. The specimen was then ground by hand successively on 240-, 400-, and 600-grit silicon carbide papers in a stream of water. Final polishing was accomplished on a 4 in. high speed wheel (3400 rpm) covered with Forstmann's cloth. Linde B levigated alumina, suspended in a 1 volume pet chromic acid solution, was the abrasive. Specimens usually were polished in 5 min or less by this technique. Often the inclusions present in the metal were identified in the mechanically polished condition. When etching was required to outline inclusions more sharply, one of the two following methods was used. In the first method, the specimen is etched lightly while electropolishing in the chromic-acetic acid solution described above (1 part of stock solution to 4 parts of acetic acid). The electrolyte was refrigerated in a dry ice-ethyl alcohol bath and specimens were etched at 60 v dc on the open circuit for 2 or 3 cycles of 3 to 4 sec each. The second technique utilizes electrolytical etching at about 10 v dc (open circuit) in a 10 pet citric acid solution at room temperature. X-Ray Diffraction Technique The major problem in the identification of inclusions in metals by X-ray diffraction techniques is the extraction of a sufficient amount of each type of inclusion to obtain an X-ray diffraction pattern. In the present study, X-ray diffraction patterns were obtained from individual inclusions of the order of 10 µ diam. The polished and etched samples shown in the micrographs were examined at a magnification of X54 or XI00 with a binocular microscope. This allowed sufficient working distance to extract the inclusions with a needle probe for powder X-ray diffraction analysis. Friable inclusions such as MgF2, CaF2, UO2, and UH3 could be freed from the metal by probing the as-polished and etched surface. The fine particles then were picked up on the end of a Vistanex-coated glass rod (0.002 in. diam) which was held in a brass adapter made to fit the powder X-ray diffraction camera. The end of the glass rod was centered in the path of the X-ray beam. In the case of the UC, UO, and UN inclusions which are smaller in size, more metallic in appearance, and less friable than the other inclusions, it was necessary to etch the inclusion in relief before extraction. UN inclusions etched sufficiently in relief in the electrolytic polishing solution described in Methods I and II by increasing the polishing time. UN inclusions were relief etched by extending the

Jan 1, 1957