Search Documents

By Paul D. Merica

One of the most useful, and at the same time least commonly used, methods of thermal analysis for the determination of transformations in metals and alloys consists in the recording of the time intervals required for successive increments of temperature change during heating or cooling, the temperature of the furnace containing the specimen being altered at a uniform rate. The curve obtained by plotting these time intervals as a function of the mean temperature of the specimen durnig the interval is called the inverse-rate curve. It is probably due to the fact that no simple and convenient method has apparently been available for the measurement of the successive time intervals that this method has not been so generally used as, for example, the differential method, for which several types of automatic or semi-automatic apparatus have been designed. Whenever this method has been used, the intervals have usually been measured with the use of a chronograph; its operation as practised at the Bureau of Standards1 is as follows: The temperature of the specimen is measured by a thermocouple and a dial potentiometer. The operator sets the potentiometer at successive values of the electromotive force differing by equal increments, usually 0.02 millivolt, and records the exact instant on the chronograph, by pressing a contact key, at which the galvanometer coil passes through its null position. Two-second intervals are also recorded on the chronograph record, and the number of seconds elapsing between successive signals is afterward counted from the record and plotted as a function of the electromotive force or of the temperature. This is an admirable method and by it most minute thermal arrests may be detected, but it requires a good chronograph, which is generally difficult to obtain, and the time of one operator during the recording and, subsequently, to read the intervals from the record; the latter operation often takes from one to two hours. There is here suggested a simple, convenient, and, it is believed, equally accurate method of recording the successive time intervals, by which the

Jan 1, 1921

By J. R. Hassemer, T. T. Chao, University of Georgia, K. C. Watts, R. F. Sanzolone

Secondary oxides of Fe-Mn have been used in mineral exploration from the time gossans were first recognized Since gossans are conspicuous features and are largely explored, it is necessary to look for more subtle indication of blind mineralization. Sampling materials used in these geochemical studies consist of secondary Fe-Mn oxide-rich products of hydrothermal mineralization, and "in situ" weathering found in fracture fillings-as selvages along joints and disseminations in host rock. These materials were selectively collected and studied in the Silver City mining region. Two independent sampling methods were compared. The difference in the sampling methods was mainly in the ways samples were obtained and processed. One method involved systematic sampling of fracture fillings and coatings from which secondary Fe and Mn oxides and associated trace elements were then selectively extracted by chemical methods. The second approach involved collection of composite stream sediments and physical extraction of Fe-Mn oxide materials by gold panning, bromoform concentration, and electromagnetic separation. The source of the Fe-Mn-rich materials in the stream sediments is considered to be fracture fillings and coatings that mechanically entered the drainage basins. Map distributions of the two-sample types were compared. Both methods showed generally supportive patterns of anomalous metal dispersion, although anomaly-to-background contrast seems better in joint coatings. Both were useful in distinguishing geochemical differences between mining districts in the region. For example, the Pinos Altos district may contain more hydrothermally-introduced iron than the Central district, whereas the Central district has lead and zinc enrichments that are less on the amount of iron enrichment than is the case in the Pinos Altos district. The methods were qualitatively compared relative to time, expense, and other advantages and disadvantages.

Jan 1, 1984

By J. E. Tiffany, S. S. Lubelsky

For blasting in coal mines the U. S. Bureau of Mines recommends that permissible explosives be used exclusively, that these shall be fired electrically, and that where feasible the working place shall be cut or sheared. These recommendations are made to promote safety and prevent mine explosions. Although permissible explosives are not flameless, their lower flame temperature and shorter duration of flanie make their use safer than that of nonpermissible explosives. Mixtures of air with both methane and bituminous coal dust, which are liable to occur in coal mines, may be ignited by coming in contact with any type of flame or spark of sufficient temperature and duration or by the firing of a blast. In a working place where a blast is to be fired, in addition to the use of permissible explosives, adequate ventilation for the dilution and removal of accumulations or outbursts of flammable gas should be provided. Bituminous coal mines should be rock-dusted as a means of rendering the coal dust harmless The efficient use of permissible explosives depends upon the proper preparation of the working place, standardized drilling, the strength characteristics of the explosive, and the use of a proper weight of charge. Experienced shotfirers should load, tamp and fire all holes. The major part of the information and data here presented is based on the results of efficiency tests made in large producing mines of Pennsylvania and Illinois. Bureau of Mines Report of Investigations, Serial No. 2697, describes how a standard method of blasting was worked out and put into operation in a mine in southern Illinois.' This paper contains a description of the methods worked out subsequently in another mine in that district. Descriptions of tests in two Pennsylvania mines are given in Bulletins 11 and 19 of the Carnegie Institute of Technology.2 These tests

Jan 1, 1928

By EDWARAD A. SIVEDENBORMG

REPORTS have been made at different times on the progress of water encroachment in the Frontier sands in the Salt. Creek oil field, Natrona county, Wyoming. All previous reports have, -however, been largely based on the position of water in the sands as determined by various physical tests. Subsequent information has been secured through a preliminary investigation of the porosity, grain size and degree of saturation of the Frontier sands. Also, a closer differentiation has been made between the waters encountered incident to the production of oil by means of chemical analysis. In view of the more recent developments there has been a need of a water encroachment map of the first Wall Creek based on a field survey and additional information acquired since the water encroachment map of the sand of 1926, by J. S. Ross and E. W. Henderson, petroleum engineers of the U. S. Geological Survey. The present report is confined to a study of the first Wall Creek sand and was written in connection with the preparation of the map, showing water encroachment in this sand. The first Wall Creek sand was the discovery sand in the field, the first well having been drilled in 1908. Its thickness averages 120 ft. and, varies between 90 and 160 ft. The sand is in the Colorado group of the Upper Cretaceous series and is further considered as a part of the Frontier formation found in other parts of Wyoming.

Jan 1, 1930

By U. C. Tainton

FOR the last 15 years lead has been the standard material for anodes in electrolytic zinc production and it has been generally accepted that this lead should be as free as possible from impurities. Laist1 says, "Next in importance to the purity of solution is the purity of the electrodes and tank lining material. The purest lead obtainable should be used for anodes." The same conclusion is expressed by Ingalls2 and by two German investigators who say that experiments have demonstrated that the purer the lead, the greater is its resistance to corrosion during electrolysis.3 Pure lead, however, while the best material hitherto available for anodes, is not entirely free from objection. The plain lead anode gradually disintegrates under electrolysis, so that the life of an anode, say ¼ in. thick, is frequently not more than two years. Part of the lead from the anode finds its way to the cathode, lowering the purity of the deposited zinc and decreasing the hydrogen overvoltage. The rest of the lead that comes from the disintegration of the anode goes into the manganese dioxide which is precipitated in the cells, rendering unsaleable what might otherwise be a valuable by-product. Yet a further disadvantage of plain lead anodes comes from their tendency to bend or buckle during electrolysis, as a result of intercrystalline oxidation. This makes it necessary to use a fairly wide spacing between anode and cathode to avoid short circuits, and thus leads to a higher power consumption than would otherwise be necessary. The power consumption is also affected by the high decomposition voltage at a lead peroxide surface.

Jan 1, 1929

By M. R. Geer, H. F. Yancey

With the exception of pneumatic processes and a few special beneficiation methods of comparatively limited application, all mechanical coal-cleaning and mineral-dressing processes involve the admixture of solid particles with a liquid, generally water. Upon completion of the beneficia-tion process the solids must be reclaimed from the water. With coarse particles separation of solids from water is accomplished readily by the simple expedient of screening, but recovery of fine solids presents a much more difficult problem. Thickening and dewatering are practiced so generally, both within the mineral industry and elsewhere, that they have been the subject of study through the years and a number of processes for making the solid-liquid separation have been developed. Dorr-type thickeners have been standard equipment lor many years, and more recently driers employing centrifugal force have gained in popularity.' A cyclone device employed to thicken the loess suspension is a novel feature of the loess heavy-medium coal-cleaning process developed by the Netherlands State Mines in the thirties. The cyclone thickener was first mentioned by Driessen2 in 1939 in a paper describing the loess process and has been the subject of two more recent reports by the same author.3 The cyclone does not differ greatly from cyclone dust collectors used in this country for years, except that it is operated wet rather than dry. Advantages of the cyclone over other thickening devices are its simplicity of construction, high capacity, and the fact that, having no moving parts, it is simple and inexpensive to operate. The Bureau of Mines became interested in the cyclone after one of the present authors observed it in operation in the Netherlands in 1945. The first experimental work with the cyclone conducted by the Bureau of Mines was an investigation of the unit functioning as a heavy-medium cleaner for fine coal—a use for the cyclone that was conceived long after it had been perfected as a thickener. The results of this investigation were published last year.4 The present investigation deals exclusively with operation of the cyclone as a thickener. Object and Scope of Investigation Although the cyclone thickener has been dealt with in three reports by Driessen, its use as a thickener was not the principal subject of any of these reports and therefore neither the cyclone itself nor its operation was described completely. The design of the cyclone was described only in a very general way, only limited operating results were given, and virtually nothing was disclosed about the influence of the various possible operating variables. Moreover, the Netherlanders apparently had employed the cyclone exclusively for thickening loess and had not employed it On coal 'lurries. One English colliery has used a cyclone to thicken coal slurry,5 and as it appeared that

Jan 1, 1949

By James Ruddy

THE medical program of the Climax Molybdenum Co. is under the supervision of the department of industrial medicine of the University of Colorado, of which James J. Waring, professor of medicine at the University Medical School, is director. Dr. Waring is consultant and direct supervisor of both the hospital and industrial medical department at Climax. At Climax the program is in charge of the medical director and the associate physician, Dr. Galen M. Hover. The hospital at Climax is completely equipped with all that is necessary for the practice of scientific medicine and surgery. Only graduate registered nurses with experience in industrial medicine are employed. Being only a few hundred yards from the portal of the mine. acci-

Jan 1, 1946

By Carl A. Zapffe, George A. Moore

IN a previous publication from this laboratory1 the conclusion was drawn that the embrittling effect of occluded hydrogen on iron and steel must result from the precipitation of the gas within small openings through the crystal structure. A review of the literature then published indicated the real existence of crystal sub- structures of the mosaic type and gave presumptive evidence that the "rift openings" associated with hydrogen occlusion are the same as the "disjunctions" of the mosaic theory. Inasmuch as no clear conception of the actual nature of the crystal fragments and openings inherent in these theories has been established, it was considered desirable to obtain direct micrographic evidence of their true configuration. In this direction the standard methods of metallographic attack have proved useless. Recourse was had, therefore, to the direct examination of the surfaces upon which failure by cleavage had resulted from the presence of hydrogen. It was expected that such a surface, un- affected by chemical attack and undistorted by polishing, would reveal the fine openings penetrated by the gas and thus indicate the real nature of the substructures. MATERIALS STUDIED In commercial steels, defects caused by hydrogen take various external forms ac- cording to such factors as structure and purity, and to the extent to which hydrogen either occludes or produces chemical changes. The present work relates only to the well-known transcrystalline hydrogen embrittlement-"pickling brittleness"-in which elemental hydrogen occluded within the grain develops cleavage characteristics. For example, hydrogen embrittlement resulting from hydrogen reaction products is excluded from detailed study. It was also desirable, as far as possible, to have the study uncomplicated by other elements which themselves cause brittleness. Three types of iron were used. These included ingot iron, decarburized free- machining steel, and a specially prepared, aluminum-killed, electrolytic iron. This , choice allowed a comprehensive selection of unavoidable minor impurities and inclusions, which could subsequently be shown to have no specific effects on the structures within the grains. Carbon, and any other impurities free to react with hydrogen, were first removed by a preliminary annealing treatment in hydrogen. Subsequent treatment in vacuo extracted much of this hydrogen and its gaseous reaction products. The resultant ductile iron was then embrittled either by a second anneal in hydrogen, followed by rapid cooling, or by cathodic electrolysis. Group I: Prepared from Armco Ingot Iron As shown in Table I, the principal impurity in this iron was oxygen, which survived the purifying treatment to a large extent. Two series were prepared. The first (Nos. SIO-24) was purified only one day in hydrogen and dehydrogenized one day in nitrogen. Containing both hydrogen and its

Jan 1, 1943

By R. S. Silo

A new process for leaching oxidized copper ore (CuO) is presented. Its principle advantage is that it requires low cost raw materials. For large operations the only materials used are sodium chloride (NaCl) and calcium carbonate (CaCO3). In those operations of medium size, sulfur, which is abundant in the North of Chile, is used. However the process may also be applied to small copper plants provided low cost sulfuric acid is available as a substitute for sulfur. That is, it may be applied to those small capacity plants where large additional installations for the regeneration of the leaching solution are not needed. The method is comprised of six stages, namely: Crushing, Leaching, Washing of the Solution, Precipitation, Regeneration of the Leaching Solution, and Fusion. A flow diagram for this process in a large or medium-sized plant is given. LEACHING This process requires hydrochloric acid as the leaching solution for treating copper ores. This is easily produced from sulfuric acid and sodium chloride as follows: A small excess of NaCl is advisable to avoid the presence of free sulfuric acid. The experiments reported here were performed with 36 grams of HC1 per liter of solution to obtain a free acidity equivalent to 50 gpl of H2SO4 (the usual leaching solution concentration). Hydrochloric acid leaching may be done by either of the usual methods; i.e. percolation or agitation. The method selected depends on the characteristics of the ore. No matter which method is chosen, low pressure air can be used either as an air lift for circulation of the solution, or for agitation of the pulp with "Pachuca" tanks. In either case, there are no problems with respect to oxidation. Leaching by agitation produces good recovery; but at times, the problem of high consumption of leaching solution or the overproduction of grinding slimes which interfere with contact between phases negates this advantage. The percolation method was used in this study. Percolation took place in four 15-liter containers, 11 1/2 in. diam. by 12 in. height, having hemispheric bottoms. Each container was fitted with a wooden bottom having 1/4 in- holes. The air lift was a 3/4 in. plastic tube 10 in. high. Air at 6 psi was supplied from a rotating laboratory compressor. 10 kg of ore were charged to the container and counter-current leaching was used. The leaching solutions were fed through the center pipe in order to use the ascending solutions to reject the air in the charge. The solution circulated through the air lift in order to facilitate the movement according to the increase in density produced by the reaction between the phases present. Specific observations made in this report cannot be generalized because the leaching characteristics are dependent on the nature of the ore used, the method of leaching, and the production of primary or secondary slimes while crushing or leaching.

Jan 1, 1967

By Robert Bell

The regions to which this paper refers include the whole of the Dominion of Canada east of the 130 Rocky Mountains and north of the water-shed of the St. Lawrence. Very little exploration for economic minerals has yet been done in this immense country; but that little has already served to indicate great wealth in some localities. Having been engaged for a number of years in conducting government geological explorations in these vast territories, I shall endeavor to give the members of the Institute an idea of the prospective mineral resources of almost half a continent, as far as they are yet discernible. I purpose confining my observations to the economic minerals, and will not attempt a description of the geology of these territories; hut it will be necessary to say a few words about the rocks in order the better to explain the distribution of such minerals. The Laurentian nucleus of the continent is the principal feature of the geological map of the Dominion. It stretches from Lake Superior to Baffin's Bay, and from Great Bear Lake to the Straits of Belle Isle. Hudson's Bay itself, which is half the size of the Mediterranean Sea of the old world, lies in the center of this area. Its shores are bordered in places with newer rocks. On the west side of James' Bay (its southern prololigation) these extend inland over 200 miles, and consist of fossiliferous Devonian and Silurian strata. On the western and northwestern side of Hudson's Bay proper, altered rocks are met with, some of which resemble the gold-bearing strata of Nora Scotia, some the Huronian of Lake Huron, some the older Huronian, and others the crystalline series of the neighborhood of Sherbrooke in the Province of Quebec. Along the east coast (called the Eastmain)and among the islands lying off it, there is an interesting set of volcanic and sedimentary rocks which appears to be identical with the Animikie and the Nipigon series of Lake Superior. The area which I have characterized in a general way as Laurentian, includes tracts and belts, more or less extensive, of the Huronian series. Such areas appear to be most common, and have been best explored, in the country between the Great Lakes and Hudson's Bay.

Jan 1, 1886

I have the honor to submit herewith the report of the Secretary for the year 1915 showing the principal activities of the Institute: Meetings.-The 110th Meeting, including the Annual Business Meeting, was held in New York City, Feb. 15 to 17, 1915. The full report of this meeting is given in Volume LI of the Transactions. The number of papers presented was 53, and the attendance was 357 members and guests. The 111th Meeting was held in San Francisco, Cal., Sept. 16 to 19, 1915. Sixty-eight technical papers were presented, and the attendance was over 400 members and guests. The full report of this meeting is given in the Bulletin for December, 1915. Local Section.-A new, strong Local Section of the Institute, with head-quarters in Arizona and known as the Arizona Section, was formed during 1915. Affiliated Student Societies.-Three new Affiliated ,Student Societies were recognized in 1915 consisting of the Pick and. Hammer Club of the University of Oklahoma, Mining and Metallurgical Club of the Univer-

Jan 2, 1916

By John Birkinbine

The experience of the past five years has furnished opportunities to study and to partially explain the operation and some of the causes of the short blast of Warwick Furnace at Pottstown, Pennsylvania, as described in the paper read at the Lake Superior Meeting, in August, 1880.* The many inquiries concerning the details of furnace operation which followed the publication of the paper, and the expressed desire of furnace managers to be informed as to future operations of this plant, have encouraged the preparation of the following data. To make the record continuous, and add to the value of both contributions, the present paper commences where the review of a short blast of Warwick Furnace ended, and includes the data of another short blast of two months, and a subsequent continuous campaign of nearly five years, which, by comparison, we shall designate as "the long blast." Frequent visits to the plant in the five years, during which its operation could be studied, and correspondence with the manager, Mr. Edgar S. Cook, have given a knowledge as to general features and details, and the courtesy of the officers of the Company which has given free access to the books of record permits the presentation of data which it is believed will be welcomed by furnace managers. Interest will undoubtedly be increased by the remarkable results which Mr. Cook has achieved chiefly with anthracite coal in a furnace whose details of construction will scarcely be generally admitted as embodying advanced ideas, its height being but 55 feet, with a bosh diameter of 15 feet 6 inches, its bosh-slope comparatively flat, its crucible smaller than the average, and the heat of the blast never reaching 1000' Fahrenheit. At present writing the credit of the best anthracite blast-furnace practice recorded in our Transactions is conceded to be that pursued by Mr. Fackenthal, at the Durham furnace, and Mr. Cook, at War-

Jan 1, 1886

By P. E. Demmler

The apparatus in which the process of bright annealing of copper wire was carried out consisted of a section of iron pipe, 6 ft. long and 3 ft. in diameter. The pipe was provided with flanges to which were bolted the end plates for sealing, also with inlet and outlet tubes to allow for the displacement of the air in the pipe by natural gas. After charging with copper wire, sealing and displacing the air, the pipe was heated to 350' C. (662" F.). It was expected that the natural gas would furnish a neutral atmosphere which would prevent oxidation and give a satisfactory bright-annealed product. It was found, however, that the outer layers of wire were discolored and not suited for the use for which they were mtended. To obtain an idea of what was taking place in the annealing furnace, skeins of the hard-drawn wire were placed in a glass tube so that all changes in appearance could be observed as they were heated to different temperatures and under varying conditions. The temperature in each case was determined by means of a thermocouple placed in the tube close to the wire. Following is a summary of the results of these experiments: 1. When the wire was heated for 1 hr. in a current of natural gas at a temperature of 350") 400") or 500" C. (662", 752", or 932" F., respectively), there was a marked darkening of the wire throughout the skein. 2. When heated for 1 hr. in natural gas at a temperature of 600" C. (1112' F.), there was no coloration, the wire remaining clean and bright. 3. When heated in natural gas to 350" C. until darkened and the treatment continued with the temperature raised to 600' C., the coloration disappeared and the wire became clean and bright.

Jan 1, 1923

By P. E. Demmler

The apparatus in which the process of bright annealing of copper wire was carried out consisted of a section of iron pipe, 6 ft. long and 3 ft. in diameter. The pipe was provided with flanges to which were bolted the end plates for sealing, also with inlet and outlet tubes to allow for the displacement of the air in the pipe by natural gas. After charging with copper wire, sealing and displacing the air, the pipe was heated to 350' C. (662" F.). It was expected that the natural gas would furnish a neutral atmosphere which would prevent oxidation and give a satisfactory bright-annealed product. It was found, however, that the outer layers of wire were discolored and not suited for the use for which they were mtended. To obtain an idea of what was taking place in the annealing furnace, skeins of the hard-drawn wire were placed in a glass tube so that all changes in appearance could be observed as they were heated to different temperatures and under varying conditions. The temperature in each case was determined by means of a thermocouple placed in the tube close to the wire. Following is a summary of the results of these experiments: 1. When the wire was heated for 1 hr. in a current of natural gas at a temperature of 350") 400") or 500" C. (662", 752", or 932" F., respectively), there was a marked darkening of the wire throughout the skein. 2. When heated for 1 hr. in natural gas at a temperature of 600" C. (1112' F.), there was no coloration, the wire remaining clean and bright. 3. When heated in natural gas to 350" C. until darkened and the treatment continued with the temperature raised to 600' C., the coloration disappeared and the wire became clean and bright.

Jan 1, 1923

By Donald J. Knight

HEAT Treatment at 1500' F of a mild steel containing 0.1 pct C, in an atmosphere which is oxidizing to both carbon and iron, results in the progressive oxidation of the metal surface with little or no change in the carbon content of the underlying metal. Further heat treatment of the scaled metal in either a neutral atmosphere or in a vacuum may or may not result in the decarburization of the metal depending upon the physical nature of the scale. It is apparent that if a continuous layer of oxide is present on the steel surface, the reaction OScale + Cmetal Cogas cannot progress since the SO formed gas would be unable to leave the oxide/metal interface. Thus, in order for the reaction to progress, the oxide must be cracked or porous. Vacuum heat treatment at 1500" F of samples with a thick continuous oxide scale showed no decarburization of the steel. However, when cracks were introduced mechanically into the scale prior to the vacuum heat treatment notable decarburization of the metal resulted and a structure as shown by Fig. 1 obtained, i.e., reduction of the crack walls to ferrite. With reference to the diagram of Fig. 2, it would appear that a mechanism of the following type takes place. Carbon atoms arriving at an oxide/metal/void interface, such as 'A', Fig. 2(a), can combine with oxygen atoms from the scale and leave the reaction site as Cogas thereby reducing the oxide to metal. On a greatly magnified scale, Fig. 2(b),this will appear as a ferrite projection along the crack wall. Carbon atoms entering this projection can react with oxygen atoms at point 'C', which is a new interface, and so on leading to a progressive growth of the ferrite along the crack wall and to the surface, Figs. 2 (c) and 1. It would appear that the only means by which thickening of the ferrite film can take place is by a diffusion of oxygen through the ferrite film to react with carbon at the newly formed ferrite/ void interface. Since the diffusion rate of carbon is reportedly much greater than that of oxygen, and since there is a low probability factor of oxygen and carbon atoms arriving simultaneously at the same site on the ferritehoid interface, there will be a tendency for more rapid lengthening than thickening of the ferrite layer, as is observed.

Jan 1, 1962

The materials used for pump construction vary according to the nature of the solution handled. The pump materials in use are the result of extended experiment and are all giving satisfactory results. Research is still in progress, particularly with stainless steel and rubber lining, both of which show considerable promise. Following are the materials used: For tank-room acid, carrying about 100 grams per liter free sulphuric acid, hard lead is used. Stainless steel is under investigation. Duriron is satisfactory, but requires very careful handling to prevent mechanical breakage. For pulps containing low acid (10 grams per liter), abrasive solids, ferric iron, copper, etc. pumps are made of hard lead. Stainless steel is satisfactory. For pulps containing no acid but carrying abrasive materials and copper, bronze is used. Pulps containing acid (10 grams per liter), copper, iron and nonabra-sive solids require lead pumps. Rubber linings are under investigation. Clear neutral solutions containing copper are handled in bronze pumps; neutral solutions free of copper, acid, abrasive material, etc., in iron or bronze. The hard lead used contains 13 per cent antimony. The stainless steel has the following analysis: Cr, 20.0 per cent; Ni, 7.0; C, 0.25; W, 4.0; Cu, 2.0.

Jan 1, 1937

By Douglas J. Harvey

The surface tension of lead-tellurium alloys (in the range 0 to 6.70 at. pct Te) ad lead-arsenic alloys (in the range 0 to 10.53 at. pct As) has been examined by the maximum bubble pressure method. The surface tension of high purity lead can be expressed over a range of temperatures (M.P. to 750°C) by the relationship = 512 — 0.133t. Arsenic and lellurium were both found to be surface active in lead. The surface excess concentration at 700°C was .found to be constant at 0.74 x 10-10 moles per sq cm for tellurium. The surface excess of arsenic at 700°C varied between 0.26 x 10-10 moles per sq cm at 0.16 at. pct to 1.5 x 10-10 moles per sq cm at 8.3 at. pet. The surface tension of lead has been investigated sporadically over the last 90 years. The first recorded study was made by Quincke1 who used a rather crude application of the drop-weight method. Hogness2 obtained the first reliable value for the surface tension of lead by measuring the pressure necessary to force the liquid metal from the end of a small capillary of known radius. Hogness gives the empirical formula: ?(surface tension)= 444 - 0.077 (l-327) which describes the relationship between surface tension and temperature ("C); This work was followed by that of Bircumshaw3 who applied the two-capillar maximum bubble pressure method of Sugden.4 The values published by Bircumshaw are in good agreement with those found by Hogness. Matuyama5 examined the surface tension of lead by the drop weight method. However, the values found are somewhat higher than those previously reported. More recent investigations by Greenaway6 and by Melford and oar' have resulted in data which are not in close agreement, but which are well within the expected range at most temperature levels. The study of the surface tension of lead alloys began with Drath and sauerwald8 who examined the lead-bismuth system. They found that the surface tension values of the alloys in this system deviated only slightly from the ideal mixture rule. Matuyarna5 examined the lead-antimony system. Bircumshaw the lead-tin, and the lead-indium system was studied by Hoar and Me1ford.10 The results of these investi- gations are summarized in Fig. 1. It may be seen that the data vary only slightly from the ideal mixture rule. As none of the metals studied and reported in the literature has a very interesting effect on the surface tension of lead,*the next logical step might be to examine the effect of metals of low solubility or nonmetals having some liquid solubility. Baes, and Kellogg11 have pointed out that the elements most likely to be surface active in liquid metals are ones of limited solubility in the liquid state and possessing weak intermolecular bonding forces in the solid state. Therefore, Group V, VI and VII nonmetals are most likely to be surface active. It was decided to examine the effect of a borderline metal, arsenic, and a nonmetal tellurium. Arsenic forms a eutectic with lead having a melting point of 290°C and a composition of 6.9 at. pct As.13 Pure arsenic sublimes when heated above 610°C. Even though alloying with lead lowers the vapor pressure, fumes containing arsenic are evolved at a very noticeable rate when lead-arsenic alloys are heated above 650°C. Tellurium raises the liquidus temperature of lead sharply to 904°C,14 the melting point of PbTe (lead-telluride). The solid solubility of tellurium in lead was determined by Greenwood and worner15 to be 0.0007 at. pct at room temperature. EXPERIMENTAL METHOD Surface Tension Measurement—The two capillary maximum bubble pressure method for measuring surface tension developed by Sugden,4 and used later

Jan 1, 1962

By R. W. Titshall

WHAT IS SAMPLING? We are all involved in sampling almost every day of our lives, by tasting, feeling, or smelling. Most raw materials, food products or manufactured items are sampled several times at various stages of the production process before a commodity of suitable quality can be produced. Data obtained from sampling is used in establishing price, quality control, allocating production costs, or overall process efficiency. The area of sampling outlined in this article is the collection of a small quantity of material from large continuous bulk flows of solids and slurries. The concern in obtaining the sample is that the material obtained is truly representative of the main flow in every respect. The methods and equipment outlined are for the collection of a manageable sample. The sample has to be analyzed in a laboratory to determine its characteristics and compliance to set standards. SELECTING A SAMPLING SYSTEM When selecting a sampling system, it is essential to define the requirements, as to what the actual sample obtained will be used for and what degree of precision is required. Determine whether or not the system has to comply with any set standards such as A.S.T.M. (American Society for Testing and Materials) which have established methods for collection of a gross sample of coal. Sampling which is done for in-plant or process control is not generally governed by set procedures, but similar care should be taken during the selection process so that when the equipment is put into service it will operate reliably and produce a sample which is truly representative of the total material lot or consignment.

Jan 1, 1982

By E. P. Klier, S. M. Grymko

The transformations in eutectoidal systems have been extensively studied as they occur in steels.&apos; As a consequence of these studies the martensite, bainite and pearlite reactions found for most steels are widely recognized. Further, because of the work of Smith and Lindlief2 and of Greninger and Troiano3 these reactions, except for the bainite reaction, are considered as typical for all eutectoidal systems. The primary alloy studied by Smith and Lindlief2 was a CuAl alloy of near eutectoid composition as was the alloy more recently studied by Mack.4 The transformations in these alloys were, for the most part, studied metallo-graphically, while an X ray analysis of structures was essentially wanting. It has appeared desirable, therefore, to investigate selected CuAl alloys at and slightly away from eutectoid composition. For this purpose three alloys were prepared containing 10.5,11.9 and 13.5 pct A1 respectively. The results of a metallographic and X ray analysis of structures obtained for isothermal transformation of the ß-phase are reported here for the 11.9 and 13.5 pct A1 alloys. Introduction The phase equilibria in the CuAl alloys of immediate concern are indicated in the equilibrium diagram section presented in Fig 1.5 The equilibrium and transition structures which have been reported in this system are as follows: a = copper rich terminal phase (f.c.c.) ß = high temperature eutectoidal phase (b.c.c.) r2 = aluminum-rich intermediate phase (r-brass structure) a&apos; = modified a-phase postulated by Bollenrath and Bungnrdt.26 ß1 = ordered ß (b.c.c.) ß&apos; = martensite structure: A1 < 13 pct (near h.c.p.) ß" = ß&apos; of Smith and Lindlief2 7&apos; = martensite structure: A1 > 13.5 pct (h.c.p.); ß2 of Bollenrath and Bungardt.26 The eutectoid transformation can be suppressed at sufficiently high cooling velocities. The ß-phase is then retained to about 500°C where ordering sets in. The ordering interval is not satisfactorily known but indirectly appears to be non-suppressible. Subsequent to the ordering reaction and consequently at lower temperatures, the ordered ß1 decomposes to a marten-sitic structure. The kinetics of these reactions and in particular those of the martensite reaction have an important bearing on the results obtained in this investigation. Since some confusion exists concerning certain reported aspects of these reactions, they will be considered in some detail. THE MARTENSITE REACTION The martensitic structure is formed on cooling through a critical range6

Jan 1, 1950

By J. F. Smith, J. E. Davison

The heat capacity of CaMg2 was measured over the temperature interval, 4.8° to 287°K, by the technique of low-temperature adiabatic calorimetry. Heat content measurements were performed with a drop calorimeter over the temperature interval, 273" to 673°K. From these data the thermodynamic functions, (FT - H0)/T, ST - So, and & - Ho, were evaluated. A third-Law calculation of the standard entropy of formation of CaMg2 yields a value of -0.25 * 0.06 cal per (°K g-atom) , and the free-energy function derived from this study when combined with existing equilibria data yields a value for the standard enthalpy of formation which is in agreement with direct calorimetric enthalpy measurements. The accompanying paper&apos; shows that the enthalpy of formation of CaMg2 has been determined with good precision by three different calorimetric techniques.&apos;-= TWO independent determinations of the Gibbs free energy of formation of CaMg2 have also been made; both determinations were based on vapor pressure measurements, being in one case hydrogen vapor pressures over ternary Ca-Mg-H alloys4 and in the other case magnesium vapor pressures over binary Ca-Mg alloys.5 The present determination of heat capacity of CaMg2 below room temperature and of the heat content of CaMg2 above room temperature was undertaken to provide supplementary data. These data are useful in their own right but can in addition be used to evaluate an entropy of formation for CaMg2 which, because of the interrelation of free energy, enthalpy, and entropy, can be used as a check of the self-consistency of the composite of the presently available information. LOW-TEMPERATURE HEAT CAPACITY The heat capacity of CaMg2 was measured over the temperature interval 4.87° to 286.64°K in an adiabatic calorimeter. The physical details of the calorimeter and the experimental procedure for measuring the heat capacity of a specimen have been adequately described by Gerstein et a1.6 The source and purity of the calcium and magnesium are described together with the methods of sample preparation and chemical analyses in the accompanying paper.&apos; Results of chemical analyses of the material which was used in the present investigation are shown in Table I. These analyses show that, on the basis of the published phase diagram,7 the heat capacity sample contained a slight excess of a calcium while the heat content sample contained a slight excess of magnesium. However, in both cases the excess was small, and X-ray diffraction patterns showed reflections which were without exception attributable to CaMg2. The sample which was used for heat capacity measurements weighed 69 g while the sample container and addenda weighed 132 g. The sample was in the form of annealed powder, 50 to 60 mesh, and was sealed into the sample container under 0.1 atm of helium. Copper fins inside the sample container facilitated thermal equilibrium of the powdered Sample. Time intervals of the order of 10 min were required for thermal equilibration, and such times are normal for this calorimeter regardless of the form of the sample. The observed heat capacities were corrected for the small excess of a calcium through use of the heat capacity values tabulated by Hultgren et a1.8 The corrected heat capacities are tabulated as a function of temperature in Table II. The free-energy function and the absolute entropy of CaMg2, which were calculated from the experimental heat capacity data, are listed in Table 111. A smooth curve was fitted to a plot of the experimental values of the heat capacity and in only two instances above 30°K did the plotted points deviate from the curve by more than 0.2 pct. Below 10°K the deviation of several of the points was as much as 50 pct. These large percentage deviations were attributed to the small value of the heat capacity and to the low sensitivity of the platinum resistance thermometer in this temperature range. The deviations in the region of 10°to 30°K were less than 5 pct. Although the percentage deviations of some of the low-temperature measurements are large, the actual value of these deviations is small since the magnitude of the heat capacity in that temperature range is small. The error in the value of the third-law entropy at 298.15°K was estimated to be less than 0.01 cal per (°K g-atom). A value of -0.25 ±0.06 cal per (°K g-atom) was obtained for the standard entropy of formation at 298.15°K from the relation:

Jan 1, 1969