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Mr. Joseph P. GAZZAM,Germiston, Transvaal, So. Africa (communication to the Secretary*) :—About fourteen years ago, in southeastern Missouri,I used a method for the wet determination of lead which closely resembles the modified sulphate-chromate method described by Mr.. Guess. The principal difference, however, is, that after dissolving the lead chromate in hydrochloric acid, the chromic acid is determined by means of a standard solution of ferrous sulphate. The method, which I believe is still in use in southeastern Missouri, was found to be convenient and accurate for the determination of lead in the ores and various products of the mills and furnaces in that district, but it was never used for complex ores. A number of determinations of lead in mill-tailings were made in the year 1891; a few of these results are given in Table I. Table I.—Determinations of Lead in MilL-Tailings by Wet Assay.

Jan 1, 1905

By Eleanor Haslem, Carl A. Zapffe

THE present investigation has three principal purposes: I. To develop a method for measuring hydrogen embrittlement that avoids certain errors complicating previously used methods. 2. To explore in a preliminary way some of the fundamental factors controlling embrittlement. 3. To apply the measurements specifically to stainless grades of steel, whose sensitivity or insensitivity to hydrogen embrittlement has never been clearly defined. SELECTING A TEST METHOD Hydrogen embrittlement is a condition of low ductility resulting from excessive absorption of hydrogen by the steel at some period in its history, and may be revealed by almost any test involving cold deformation. Tensile tests, impact tests, and bend tests are commonly used for detecting hydrogen embrittlement; although numerous other tests, such as cold-upsetting or extrusion, could be used. The simplicity of using a wire specimen for cathodic and acid pickling tests, and the especial adaptability of the bend test to wire specimens, led to selection of the bend test for the present research. Bend tests usually have been of three general types: (I) fatigue, (2) reversed bend, and (3) single bend. The first two types, though widely used, are inaccurate because their measurements are counteracted by an aging effect; and the third type has not been developed to its fullest utility. The effect of cold-working in removing hydrogen is well known. During a bend test hydrogen can be observed escaping from the convex side simply by coating the specimen with oil; and any technique employing flexing or reverse bending may therefore have its measurements masked because the mechanical action reduces the embrittlement during the test. This factor is so important that even elastic flexing of a hydrogen-charged wire specimen should be avoided before testing if accurate measurements are desired. DEVELOPING A MACHINE FOR MEASURING HYDROGEN EMBRITTLEMENT As for the single-bend test, its theory is good, and recovery caused by mechanical work is kept to a minimum. With a given degree of hydrogen embrittlement, a specimen will break at a given angle if the bending is applied unidirectionally and uniformly. The radius of the bend must be kept constant; and the rate of bending should be a constant, slow enough to allow reading of the breaking angle, and yet rapid enough to prevent significant recovery from the escape of hydrogen during bending. A simple apparatus (Fig. I) was constructed using a type H Foxboro drive unit A, which is a synchronous motor with a gear-reduction ratio of 600 to I. A cord, fixed at one end to a wooden pulley B on the drive shaft of the motor, follows the pe-

Jan 1, 1946

By Sidney A. Swensrud

The writer has been interested for some time in trying to appraise our industry's prospects for gasoline consumption over the next half dozen years or so. Anyone who has even approached the problem knows the intimate relationship to it of the number of automobiles in use— by automobiles I mean both passenger cars and trucks. Probably at least 90 per cent of our gasoline is used in automotive vehicles. Some recent estimates secured from the Department of Commerce show the following breakdown: Per Cent Passenger cars............................................ 60.0 Trucks................................................... 27.4 Busses................................................... 2.9 Taxicabs................................................. 2.2 Subtotal............................................... 92.5 Aviation, motor boats and railroads......................... 0.5 Agricultural: farm tractors, etc.............................. 3.3 Balance (manufacturing, government use, construction, etc.)... 3.7 100.0 Up to the beginning of the depression there was, of course, a constant annual increase in the number of automobiles in use, for each year the industry added to the total inventory or ''population" more new units than were being scrapped, as may be seen in Fig. 1. Few of us in the oil industry needed to give much attention to the detailed figures, although the automobile industry seemed to interest itself in all sorts of calculations of replacement demand vs. new car demand, the average life of the car, the number scrapped, and the like. Probably many people in the oil industry, as well as outside it, were surprised at the way in which automobile registrations and gasoline consumption held up during the early years of the depression. Nor were they greatly perturbed when, as in the last two years, both registrations and consumption began to fall somewhat. That was natural enough; it

Jan 1, 1933

Discussion of the paper of DAVID COLE, presented at the New York meeting, February, 1915, and printed in Bulletin No. 9S, February, 191.5, pp. 431 to 444. R. H. RICHARDS, Boston, Mass.-The Butchart riffle seems to violate, according to our preconceived notions, some of the very essential principles of the Wilfley riffle, and therefore ought not to succeed, but it does. On this account it must conform to other very important principles, or it would not succeed. It would beinteresting to know what these principles are which enable it to succeed. E. P. MATHEWSON, Butte, Mont.-I cannot, explain the principles on which this riffle acts, because I have not given it personal attention. All I can say is that I first saw the riffle in operation several years ago at the Steptoe Valley mill in Nevada, and I was told that a man had been around there guaranteeing that these riffles would make the table do twice as much work and do it better than with the ordinary Wilfley riffles. I heard nothing further about it for a long time. I heard about a year ago, from David Cole, the author of this paper, that the riffles were a success, and that he was using them at Morenci, and if, we were interested he would send the inventor to show us how they worked. As we knew of David Cole's reputation, we invited Mr. Butchart to come up and show us how his riffles worked. We did not have sufficient confidence in the invention to guarantee Mr. Butchart his traveling expenses, but lie came up entirely at his own expense and put in a set of the riffles on one table. It was known as a roughing table in our No.

Jan 5, 1915

By D. Van Winkle, C. Zener, H. Nielsen

THe internal friction of metals has been studied frequently at elevated temperatures.1-4 In most cases it rises rapidly with increasing temperature. The notable exceptions are ferromagnetic materials, and lead.2 This paper describes an investigation of the general features of the high-temperature internal friction of 70-30 alpha brass. Experimental Method The internal friction of a metal is a measure of the rate at which it dissipates energy of vibration. The measure adopted here, I/Q, is (I/2p) times the specific damping capacity, a measure commonly used by engineers. In the measurements of this investigation, the stress level was kept so low that the observations were independent of the stress, The general method of making such measurements, and of observing temperature of a specimen during a measurement, has been described.5.6 The driver and detector coils were wound with wire insulated with glass thread, in order to withstand the high temperatures used. In previous work electrical eddy currents in the specimen served as the coupling between the mechanical vibration of the specimen and the electrical circuits of the driver and detector. The high values of the internal friction in the present investigation rendered this coupling insufficient. In order to increase this coupling, pole pieces cut from ordinary telephone diaphragms were attached to the specimen. A mixture of French chalk and water glass proved a satisfactory cement. All measurements were made at the fundamental frequency for transverse vibration, which lay between 600 and goo cycles per second. Specimens The measurements described herein were made upon a single cylindrical rod of brass, kindly furnished by Dr. Cyril Stanley Smith, of the American Brass Co. This rod was the specimen E of the set of alpha-brass rods described in an earlier paper.6 Successively larger grain sizes were obtained by annealing at .successively higher temperatures. A slice was cut off one end after each set of measurements. Grain counts were made on each slice by W. E. Lindlief, of the American Brass Co. Nine fields were viewed on each piece, located as shown in Fig. I. Results are given in Table I. The grain size is defined in the usual way; namely, Grain size = I/n1/2 where n is the mean number of grains per square millimeter. Experimental Results This paper is concerned exclusively with the part of the internal friction that be. comes dominant at high temperatures. It is thus desirable to separate this part of the internal friction from the part that is

Jan 1, 1942

By C. Zener, H. Nielsen, D. Van Winkle

THe internal friction of metals has been studied frequently at elevated temperatures.1-4 In most cases it rises rapidly with increasing temperature. The notable exceptions are ferromagnetic materials, and lead.2 This paper describes an investigation of the general features of the high-temperature internal friction of 70-30 alpha brass. Experimental Method The internal friction of a metal is a measure of the rate at which it dissipates energy of vibration. The measure adopted here, I/Q, is (I/2p) times the specific damping capacity, a measure commonly used by engineers. In the measurements of this investigation, the stress level was kept so low that the observations were independent of the stress, The general method of making such measurements, and of observing temperature of a specimen during a measurement, has been described.5.6 The driver and detector coils were wound with wire insulated with glass thread, in order to withstand the high temperatures used. In previous work electrical eddy currents in the specimen served as the coupling between the mechanical vibration of the specimen and the electrical circuits of the driver and detector. The high values of the internal friction in the present investigation rendered this coupling insufficient. In order to increase this coupling, pole pieces cut from ordinary telephone diaphragms were attached to the specimen. A mixture of French chalk and water glass proved a satisfactory cement. All measurements were made at the fundamental frequency for transverse vibration, which lay between 600 and goo cycles per second. Specimens The measurements described herein were made upon a single cylindrical rod of brass, kindly furnished by Dr. Cyril Stanley Smith, of the American Brass Co. This rod was the specimen E of the set of alpha-brass rods described in an earlier paper.6 Successively larger grain sizes were obtained by annealing at .successively higher temperatures. A slice was cut off one end after each set of measurements. Grain counts were made on each slice by W. E. Lindlief, of the American Brass Co. Nine fields were viewed on each piece, located as shown in Fig. I. Results are given in Table I. The grain size is defined in the usual way; namely, Grain size = I/n1/2 where n is the mean number of grains per square millimeter. Experimental Results This paper is concerned exclusively with the part of the internal friction that be. comes dominant at high temperatures. It is thus desirable to separate this part of the internal friction from the part that is

Jan 1, 1942

The income of the Institute is derived mainly from dues, advertising in MINING AND METALLURGY and sale of publications. These sources fortunately are supplemented by the interest from invested funds now amounting to over $500,000, a considerable portion constituting endowments for special purposes. Aside from the medal funds the principal endowments are the James Douglas Fund for support of the Library, the Charles Hayden Memorial Fund, designated to further the education of Student Associates, the Rocky Mountain Fund, and the Seeley W. Mudd Memorial Fund. The income from the two last named is available for the support of research and a variety of other purposes. It is allocated by the Board of Directors upon recommendation of standing committees in each case. An active effort is being made to increase the endowment funds of the Institute through a standing, committee, of which H. T. Hamilton is chairman, and of which the other members are: W. H. Aldridge, George D. Barron, Cleveland E. Dodge, Henry Krumb and J. V. W. Reynders. This committee feels that there exists a tremendous opportunity for the Institute to be of ever-growing service to the public, to the mineral industries, and to the profession. It welcomes suggestions as to names of men of means who are vitally interested in the mineral industries, and to whom the opportunity to make a contribution or bequest might appeal favorably if presented in the proper light by the committee.

Jan 1, 1940

By W. H. Bassett

W H. BASSETT was elected first vice-president at . the executive session of the new Board on Tues- day afternoon. Karl Eilers, H. Foster Bain, Thomas T. Read, and H. A. Maloney were respectively re-elected as treasurer, secretary, assistant secretary and assistant treasurer. The new Executive Committee will consist of W. H. Bassett, Chairman, and Richard Peters, Jr., H. C. Bellinger, E. De Golyer, Edgar Rickard. The Finance Committee will be J. V. W. Reynders, Chair- man, Henry Krumb and H. G. Moulton. George D. Barron was reappointed Chairman of the Admissions Committee, and F. Julius Fohs put in charge of the Papers and Publications Committee.

Jan 1, 1929

By Edward Saibel

The various theories that have been advanced to explain or predict the conditions under which a metal fractures may be divided into two categories: First, there are the macroscopic theories generally used in engineering practice. These are empirical in nature and limited in application. For example, the maximum normal stress criterion, which is quite satisfactory for a mild steel in simple tension at atmospheric pressure,' no longer suffices when this steel is pulled under hydrostatic pressure.2 In all of these empirical theories, the critical condition characteristic of the material and of the loading conditions must be obtained experimentally. Secondly, there are the theories based on interatomic forces,3'4 or on the energy required to form new surfaces.5,6 These have all dealt with the theoretical evaluation of the tensile stress necessary to bring about rupture in a purely brittle manner; that is, without plastic flow preceding fracture. All of these attempts have led to values of the tensile strength of crystals or of polycrystalline bodies that are 100 to 1000 times higher than observed values. On this account, it has been thought necessary by some investigators to conceive of a microcrack structure or distribution of flaws throughout the specimen such that the resulting stress concentrations provide the factor necessary to bring about agree- ment between calculation and experiment. It has been pointed out by several observers' that this point of view is highly unrealistic, in that the weakening effect of these flaws or microstructures must be very uniform from specimen to specimen, since the fracture stresses found for various specimens of the same material tested under similar conditions are so nearly constant. Furthermore, since calculations based on atomic forces or atomic energy are for purely brittle fracture, a condition probably never satisfied in tests, agreement is hardly to be expected. Thermodynamic Theory of Fürth In order to resolve this apparent discrepancy between the theoretical cohesive strengths and the observed fracture strengths, Fürth8 advanced a thermodynamic theory of the tensile strength of isotropic bodies based on work of Born relating to the melting of crystals. Assuming an isotropic material free from imperfections and flaws, behaving elastically up to the breaking point, and assuming a connection between rupture and the melting phenomenon, Fürth obtains an expression for the rupture stress a, in the form where Q is the melting energy per unit mass, p is the density, and is Poisson's ratio. Furth compares fracture stresses computed from Eq I with the fracture stresses of metals as given in the Landolt-Bernstein Tables (1927) and in the Hand-

Jan 1, 1947

By Edward Saibel

The various theories that have been advanced to explain or predict the conditions under which a metal fractures may be divided into two categories: First, there are the macroscopic theories generally used in engineering practice. These are empirical in nature and limited in application. For example, the maximum normal stress criterion, which is quite satisfactory for a mild steel in simple tension at atmospheric pressure,' no longer suffices when this steel is pulled under hydrostatic pressure.2 In all of these empirical theories, the critical condition characteristic of the material and of the loading conditions must be obtained experimentally. Secondly, there are the theories based on interatomic forces,3'4 or on the energy required to form new surfaces.5,6 These have all dealt with the theoretical evaluation of the tensile stress necessary to bring about rupture in a purely brittle manner; that is, without plastic flow preceding fracture. All of these attempts have led to values of the tensile strength of crystals or of polycrystalline bodies that are 100 to 1000 times higher than observed values. On this account, it has been thought necessary by some investigators to conceive of a microcrack structure or distribution of flaws throughout the specimen such that the resulting stress concentrations provide the factor necessary to bring about agree- ment between calculation and experiment. It has been pointed out by several observers' that this point of view is highly unrealistic, in that the weakening effect of these flaws or microstructures must be very uniform from specimen to specimen, since the fracture stresses found for various specimens of the same material tested under similar conditions are so nearly constant. Furthermore, since calculations based on atomic forces or atomic energy are for purely brittle fracture, a condition probably never satisfied in tests, agreement is hardly to be expected. Thermodynamic Theory of Fürth In order to resolve this apparent discrepancy between the theoretical cohesive strengths and the observed fracture strengths, Fürth8 advanced a thermodynamic theory of the tensile strength of isotropic bodies based on work of Born relating to the melting of crystals. Assuming an isotropic material free from imperfections and flaws, behaving elastically up to the breaking point, and assuming a connection between rupture and the melting phenomenon, Fürth obtains an expression for the rupture stress a, in the form where Q is the melting energy per unit mass, p is the density, and is Poisson's ratio. Furth compares fracture stresses computed from Eq I with the fracture stresses of metals as given in the Landolt-Bernstein Tables (1927) and in the Hand-

Jan 1, 1947

By T. Sterry Hunt

AT the meeting of the Institute in Easton, October, 1873, I made a communication on the Ore Knob copper mine, in Ashe County, North Carolina (Transactions, vol. ii, p. 123), in which I called attention to the chemical decomposition alike of the pyritous lode and the inclosing gneiss rock to a depth of 60 feet, by which the feldspar of the latter had been converted into clay, and the whole rock very much softened. Such a decomposition is well known to be almost universal in the crystalline rocks of the Appalachians south of the Potomac ; and if it is only seen in rare and exceptional cases farther to the northward, this, as I have elsewhere pointed out, is due to the fact that the decomposition began and ended in the ages anterior to the drift period, and that the decayed portions which still remained were at that time removed from the surface, except in some localities which were protected from the eroding agency. I have lately had an opportunity of studying a remarkable instance of this kind in an examination made last month for the corporators of the Hoosac Tunnel.* The locality is at the western base of Hoosac Mountain, the western slope of which rises rapidly 1300 feet above the town of North Adams, in Berkshire County, Massachusetts, itself 700 feet above the sea level. Through this mountain, as is well known, a tunnel for the Troy and Boston Railroad has lately been opened, a distance of 25,081 feet from east to west. The rock of the mountain consists of mica schist and micaceous gneiss, including in its western half a great mass of harder feldspathic and quartzose strata in part a granitoid gneiss, the strata for the most part dipping to the eastward with variable angles, but with occasional western dips, apparently due to inversion. The crystalline strata of the mountain crest and sides are in many places exposed, and present rounded surfaces, often deeply grooved and striated, but with no appearance of decay. At the western base of the mountain, however, the gneissic rock is in a state of complete decomposition, which was well displayed in opening the tunnel, which, for a distance of several hundred feet, was driven through highly inclined strata so much decomposed that they were excavated with pick and shovel, and without the aid of blast- * See, for a detailed account of this examination, Dr. Hunt's report, published by the General Court of Massachusetts in House Document No. 9, 1875.

Jan 1, 1875

By J. S. Pascover, J. K. Abraham

The influence of the early stages of precipitation on the kinetics and structure of martensite formation in Fe-27Ni and Fe-29.5Ni alloys containing from 0 to 10 pct Ti was examined with X-ray and electron microscopy techniques. The formation of a coherent, ordered preprecipitate had a profound stabilizing effect on the austenite. The Ms was decreased by increased titanium content and aging time up to a critical time. When the critical aging time was exceeded, the Ms was observed to increase markedly. The formation of the clusters was insuppressible and the volume fraction of clusters formed during the quench was a function of the titanium content. Martensite resulting from transformation of the clustered austenite is tetragonal with the c/a ratio increasing with titanium content. A model for the tetragonality is suggested. The morphology and substructure of the m artensite is inter-preted in terms of the above information and the cur-rent models of twinned martensite. ThE ramifications of precipitation in austenite to the properties of austenite have been the subject of numerous investigations. The current research is concerned with the influence of precipitation in austenite on the kinetics and structure of subsequent marten-site formation. In a previous investigation, Abraham et al.1 followed the aging reaction in an Fe-29.5Ni-4.2Ti* (at. pct) alloy using an X-ray diffraction technique. This technique, employing a Guinier camera, provided kinetic measurements through observation of the side band position as a function of aging time. The salient results of this work were: 1) The initiation of precipitation was not suppressed by quenching, i.e., there was a finite cluster zone size at zero aging time; and 2) The hardness of the aged austenite correlated extremely well with the zone size. During the previous work it was noted that the mar-tensite formed after aging was tetragonal, substanti-ating an earlier observation.2 Systematic investiga-tion revealed that the martensite was tetragonal in both the solution-treated then quenched, and the solu-tion-treated, aged, and quenched condition, and, furthermore, that a marked stabilization of the austenite occurred as a function of aging time. The present work is concerned with documenting the tetragonality and the stabilization phenomena as well as the ob- served microstruction with a suggested rationale for the behavior noted. EXPERIMENTAL PROCEDURE The compositions of the alloys are listed in Table I. The analyses were performed after the solution treatment of the strip material. Nickel was determined using the standard dimethy1-glyoxime procedure whereas titanium was determined colorimetrically with hydrogen peroxide and volumetrically by titrating with ferric iron. The materials were melted in a 5-lb vacuum induction furnace, cast into 2-in.-diam ingots, and forged in a temperature range of 950. to 1200°C to 1/2-in. slabs. The three higher titanium containing materials cracked during forging; therefore, to get the alloys into strip form, slices 1/8 in. thick were cut from the slab, homogenized 4 hr at 1150°C, then cold-rolled to a 0.04-in. thickness. The remaining slabs were hot-rolled, homogenized 4 hr at 1065"C, then cold-rolled to a final thickness of 0.03 in. All of the heat treatments were performed under a protective atmosphere of argon. The Ms temperature for most of the alloys is below room temperature; therefore, it was possible to solution treat, quench to room temperature, polish, and then observe the transformation optically on a cold-stage microscope. To determine the effect of aus-tenitizing temperature on Ms, eight of the alloys were treated at two temperatures, 1025" and 1120°C. No measurable variations in Ms were noticed. The remaining alloys were treated at 1025°C. The specimens, : by 5/16 by 0.03 in., were austeni-tized in a vertical tube furnace under a dynamic argon atmosphere. The bottom of the tube was submerged in water for quenching purposes. The question of stabilization that may be operating at room temperature was investigated and found to be negligible. Many of the specimens were held at room

Jan 1, 1970

E. L. BLOSSOM, New. York, N. Y.-That this paper deals with a real problem is illustrated by a statement made to the speaker a few months ago by the manager of a silver-lead property: "Our ore contains 60 per cent. silica on which the smelters are penalizing us heavily, and they are not able to take all our stuff even then. We have simply got to find some method other than smelting for getting the silver and lead out of our ores. We have had experts down here and have investigated flotation, leaching and volatilization, of which processes the latter is by far the most promising. We are continuing investigation." I was somewhat concerned in certain chloride volatilization experiments which we carried on in Denver in 1903, working on a carload of ore from Butte. Now being connected with the Cottrell process, by which method the fumes will undoubtedly he recovered if they solve the volatilization problem, I have looked into the matter again, and believe it can be developed into a commercial process. On a laboratory scale, working With silver-lead ores, experimenters have obtained a volatilization of over 90 per cent. of the total values in 30 to 60 min, on quantities of 1 to 5 lb., using a roasting dish and a muffle. That looks very good, and would be entirely commercial. On attempting to duplicate these results in a reverberatory furnace, they found that it is more likely to take 8 hr. firing to yield 75 per cent. extraction, which is not commercial at all, as it requires too much time, labor, and fuel, and the whole process is too slow. Of course it can be done, because we have done it in the laboratory.

Jan 1, 1918

By John V. Beall

Dear J. B.: The recent cable I sent you for a transfer of $200,000 was the outcome of the diligence and perspicacity of our group which, as you know, is laboring under severe hardships here in Rondônia. I only mention the latter difficulties in passing because no reply has been received to our urgent appeal for money. As much as I detest appearing to plead for more attention than you feel called upon to pay to our forgotten mission, I can assure you that it would be in the best interest of the company for you to do so. The fact is, we have been able to outmaneuver the competition and have succeeded in securing pesquizas on some of the most promising cassiterite gravels. We have not been able, up to now, to do much bulk sampling (for lack of funds) but our preliminary panning shows great promise as you can see from the enclosed assay sheets.

Jan 1, 1971

EDWARD HART*, Easton, Pa. (written discussion?) .-In 1895 I visited the chemical plant of the Messrs. Chance at Oldbury, England, under the guidance of Mr. France, the manager. In the stock house I saw a pile of coal brasses with adhering coal and said to Mr. France, "I should think you would get dark acid." "Yes," he replied, "our acid has always been rather black. and our customers have grown used to it. Some time ago we ran out of brasses and could get only Spanish pyrite. Our product became white and the customers began to complain, so I put a little sugar in each carboy." E. A. HOLBROOK,* Pittsburgh, Pa. (written discussion?).-Mr. Davis says, "A very large tonnage of pyrite is annually being thrown in the waste in the coal mines of this country." This quantity is much larger than is generally realized by people not intimately associated with coal mining. At the beginning of the war this country seemed threatened with a short-age of pyrite. The U. S. Bureau of Mines conducted a general investiga-tion of the pyrite resources of the country in order to ascertain what material was commercially available. The general pyrite investigation was in charge of H. A. Buehler, with the subsection on coal pyrite in charge of E. A. Holbrook.

Jan 10, 1919

By E. H. Bunce, H. M. Haslam

The "direct process" for the manufacture of pigment zinc oxide produces the oxide directly from ore. This is accomplished by reducing the zinc by means of carbonaceous fuels and immediately burning the evolved zinc vapor to zinc oxide. For many years this was done by smelting a loose charge of ore and fuel on perforated grates. Since this process was developed in America and was extensively used here, it has become known as the "American process." Alternative methods of producing pigment zinc oxide are the "indirect process " and the "wet process." In the indirect process the raw material is metallic zinc, which is volatilized and burned to the oxide. For a long time this has been done in externally fired horizontal refractory retorts. This process has become known as the "French process," from the country of its origin. The wet process precipitates the carbonate or hydrate from zinc-bearing liquors and then calcines the precipitate. This method has been but sparingly used for producing commercial quantities of zinc oxide. It appears to be advisable to restrict the use of the terms "American process" and "French process" to the methods of the earlier periods and to consider the terms "direct process" and "indirect process" as generic terms to designate, first, all methods of producing pigment zinc oxide directly from ores, and, second, to include all those methods of producing zinc oxide from metallic zinc and metallic zinc-bearing substances. American Process In 1796 John Atkinson was granted British Patent No. 2094/1796 entitled, "Manufacture of White Paint." This patent describes a method of producing zinc oxide in which roasted zinc blende or calcined calamine is mixed with charcoal, and the mixture heated in a muffle to liberate zinc vapor, which is then burned to obtain zinc oxide fume. About 1850 The New Jersey Zinc Co., at its plant in Newark, N. J., attempted to make zinc oxide by smelting, in a reverberatory furnace, a mixture of coal and ore from its Franklin mine. A considerable amount

Jan 1, 1937

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

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

Jan 1, 1962

By L. G. Huntley

I. HISTORY OF OIL DEVELOPMENT IN MEXICO THE occurrence of oil or "tar" in Mexico was mentioned as early as the seventeenth century by Friar Sagahun, who gives the Indian name "chapopote," by which these asphalt seepages are still called. This asphalt was apparently used, as it has been used by primitive people in many parts of the world, in religious ceremonies and for medicinal purposes. Travellers also report that the ruins in Yucatan and the pyramids in southern Mexico show traces of the use of "chapopote" as a building cement.1 DeGolyer says that the first attempt to exploit oil or gas in Mexico in a commercial way is shown by the records of the Memoria de Fomento of 1865, when permission was granted to a Senor Ildefonso Lopez to exploit the deposits of petroliferous substances in the San Jose de Ias Rusias area in the State of Tamaulipas. Other concessions follow, and probably refer to surface seepages which occur in that district. This was several years after the discovery of oil in Pennsylvania. In 1868, a well 125 ft. deep was drilled by a company organized in Mexico City, in what is now known as the Furbero district, and a little oil was refined there. In 1873, residents of Tampico denounced seepages along the Tamesi River, and asphalt was mined near Tempoal in the Canton of Tantoyuca. No drilling was attempted. But between 1880 and 1883 several shallow wells were drilled for oil in Mexico, two of them being near the present Potrero de Llano field west of Tuxpam. The wells were drilled by a Boston company with Canadian rigs, and are said too have reached a depth of about 400 ft., while one is reported to have flowed. Several other abortive attempts were made to drill for oil between 1885 and the beginning of the present century, about which time the Mexican, Petroleum & Liquid Fuel Co., Ltd., in which Cecil Rhodes was interested drilled 24 wells unsuccessfully, several of them as deep as 1,500 ft., in the State -

Jan 9, 1915

By C. J. Rosa, W. C. Hagel

An attempt is made to determine the diffusion coefficients of oxygen ions in hypostoichiometric zirconium oxide. A phenomenological theory is developed for three-phase, unidirectional volume diffusion of a gaseous species from a planar source. Knowledge about oxygen diffusion in a and ß zirconium and experimentally measured rates of movements of interfaces permit the evaluation of oxygen ion diffusivi-ties in ZrO2-x. The results conform to the relationship: sq cm per sec, for the temperature range of 875" to 1050° C. DIFFUSION coefficients of oxygen ions in stoichio-metric oxides have been studied by many investigators. The obtained results not only supplement the knowledge about the lattice-defect structures of oxides and conduction mechanisms but also provide information of technological importance. Rate processes such as oxide sintering, high-temperature creep deformation, and oxidation of metals and their alloys are directly dependent on diffusion phenomena. Unfortunately, diffusion coefficients obtained from studies on stoichio-metric oxides cannot be treated without restraints when applied to oxidation kinetics, if precise evaluations of oxidation rates are desired. Oxides formed on metals are usually nonstoichiometric and exhibit nonuniform distribution of either cation or anion vacancies across their thicknesses. Debuigne and Lehr1 extended Danckwerts'2 mathematical analyses and furnished a semitheoretical treatment for evaluating oxygen diffusion coefficients in zirconium oxide in terms of weight gain measurements during oxidation of zirconium in the temperature range 400° to 850°C. Their calculations are based on theoretical partitioning3 of the total amount of oxygen between a zirconium and its oxide phase. An inherent discrepancy appears to continue throughout their calculations. The amount of oxygen confined to the oxide phase should be corrected by multiplying the calculated oxide thickness by the inverse of Pilling-Bedworth ratio, if expansion of zirconium dioxide is taken into account. The purpose of the present investigation is to provide a new semitheoretical treatment for evaluating diffusion coefficients of moving species in hypostoichiometric oxide. The analyses are relevant to unidirectional volume diffusion. Although the presented method is quite general, its applicability will be discussed in terms of kinetic measurements from oxidation of zirconium at temperatures above the a/ß transition, for reasons stated in the later part of this paper. EXPERIMENTAL Pure, 99.93 wt pct, zirconium samples of approximately 2 by 1 by 0.35 cm were exposed to oxygen for various times at four temperature levels: 875°, 950°, 1000°, and 1050°C. High-purity, better than 99.9 vol pct oxygen was passed through a cold trap and columns containing anhydrous CaSO4 to remove residual water vapor. Before exposing to oxygen at a pressure of 500 Torr, specimens were subjected to wet abrasion on 200- through 600-grit Sic papers and polished with 1—p diamond dust. Prior to oxidizing, all zirconium samples were vacuum-annealed at 10-6 mm Hg for about 15 min at the test temperature. The temperature variation across the uniform heat zone was ±2°C from the preset value. Final polishing, for phase thicknesses measurements, was performed by using 8- and 1-p diamond dust and followed by vibrator polishing with 0.05-µ ? Al2O3 solution. Measurements of phase thicknesses were made by projection on a metallographic viewing screen. Conventional powder X-ray analyses for the oxide were employed. RESULTS Fig. 1 is an example of the cross section of oxidized zirconium. Designations of phases given below this figure are the same as those used in the three-phase diffusion system represented by Fig. 5 in the following section. Zirconium oxidized for longer exposure times showed two types of oxides: white oxide at the surface and an underlaying layer of gray oxide. X-ray powder patterns of these oxides at room tern-

Jan 1, 1969

By Howard Scott

Invar is the preeminent low-expansion metal by virtue of the fact that it can be prepared with a zero coefficient of expansion at atmospheric temperature. This fact suggests that there is little room for improvement in the expansion properties of the low-expansion nickel steels. The inference is true, however, only so far as the expansion at and near atmospheric temperature is concerned, because the expansivity of invar starts to increase rapidly on heating above 100" C. and soon reaches the value of copper. Guillaumel met this situation by increasing the nickel content above that of invar. By that expedient, alloys having low expansivity under higher temperatures were obtained, but not without a large increase in minimum expansivity. The increase in minimum expansivity with increasing nickel content severely limits the technical applications of these alloys at high temperatures. Prospects of improving the expansion characteristics of the nickel steels is offered by alloying. Search for an advantageous alloying addition by analogy with other alloy systems, however, is not productive because the low-expansion characteristic is unique with that system. The rule of mixtures usually gives a fair value of the expansivity of other solid-solution alloys, but in the iron-nickel systems gives a value of 18 X 10-6 per deg. C. whereas the actual value is 1 X 10-6 per deg. C. Apparently suitable additions are not to be deduced from such ingenuous considerations. Recognition of the fact that the temperature range of low expansivity in nickel steels is terminated with loss of magnetism affords a more promising basis for the selection of an advantageous element. One may expect from that fact that additions of nonmagnetic elements to the iron-nickel alloys are detrimental to the low-expansion characteristic. Indeed, carbon, manganese, silicon, copper and chromium are detrimental to the expansion properties and no nonmagnetic element is reported to be beneficial. From the same viewpoint, the addition of a magnetic metal offers prospects of improvement. As two of the three ferromagnetic elements are already present in the

Jan 1, 1930