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By W. Tempelaar Lietz

The Ten Section oil field is located in the San Joaquin Valley in Kern County, California. about 12 miles southwest of Bakersfield in Township 30 South, Ranges 25 and 26 East. The accumulation is in a low relief anticlinal dome and has a productive area of approximately 2,200 acres. Discovered in 1936 as a result of seismic work, it was the first field on the floor of the Valley to obtain production. It had a small primary gas cap, and since its inception has been produced by depletion with controlled withdrawal from the gas cap to minimize blowthrough. STRUCTURE AND STRATIGRAPHY The Ten Section structure is an elongated anticlinal dome with flank dips of only about 7 degrees. A map of the field, now fully developed, and a composite log are shown in Figs. 1 and 2. Contours shown on the map are on the top of the first zone, or Marker XA as indicated on the composite log. As shown, the field has a productive closure of only some 350 feet, and there apparently is no faulting in the reservoir. The productive measures in Ten Section are of Upper Miocene age and are known as the Stevens sand. They contain thin, irregular shale or siltstone streaks which vary considerably in stratigraphic position and thickness and apparently are rather discontinuous. As a result, individual sands and shales cannot be correlated over any appreciable area, which makes it difficult to subdivide the sand body into separate zones which are distinct throughout the field. However, there are two fairly persistent siltstone bodies that at the time of development were considered to divide the productive measures into three - zones. The first, or uppermost zone is productive over the entire field and has an average thickness of 180 feet, of which some 65 per cent is sand. It had a primary. gas cap in the crestal area with an areal extent of 930 acres. The second zone has a productive area somewhat smaller than the first zone, but it did not have any original gas cap. It has an average thickness of about 360 feet, of which 55 per cent is sand. The third zone has a very limited areal extent and a maximum productive thickness of 100 feet, of which 80 per cent is sand. Recently, a deeper oil accumulation, termed the "53" sand, was discovered, but it is not discussed in this analysis. In the first and second zones the water table was at 7,980 feet subsea, while in the third zone it was at 8,080 feet subsea. RESERVOIR CHARACTERISTICS Sand Characteristics The Stevens sand in Ten Section is hard and well consolidated, and numerous wells were cored for core analysis. Core data on four representative wells are shown, plotted beside the electric logs in Figs. 3 to 6. The average porosity is 20 per cent, with porosities ranging from 15 to 30 per cent. It is estimated, from cores taken with oil base muds, that the interstitial water content is about 40 per cent. The average weighted permeability is approximately 140, with measured permeabilities ranging from 10 to 3,000 md. As might be expected with practically no correlation of individual sand

Jan 1, 1949

By William Kent

In the paper by Mr. Fernom, on Red Charcoal, read at the first session of this meeting, it was suggested that this fuel might be used in the blast furnace with greater economy than ordinary or black charcoal. In the discussion which followed the paper, it was stated that the charcoal furnaces of the Lake Superior District have used imperfectly burned charcoal with success, and that these furnaces have given the best results in fuel economy on record. On consulting some of our well-known metallurgical authorities the writer finds that the question of the use of red charcoal, or other imperfectly burned charcoal, or charred wood, is not at all new. In Percy's late work on Fuel, pages 409-414, are given a few facts, which are here condensed, as follows:

Jan 1, 1879

By R. Gibson, F. S. Turneaure

The tin deposit of Monserrat, Bolivia, consists of one major vein 1600 m in length. The ore is unusual because of the notable quantity of teallite, even though cassiterite is the principal tin mineral. The deposit, formed at shallow depth under a wide range in temperature, may be classed as xenothermal. Polished sections reveal a complex history of replacement, with low-temperature minerals deposited before high-temperature minerals. THE Monserrat mine1'2 of the Compania Minera Monserrat is located 11 km east of Callipampa, a station on the Antofagasta and Bolivia Railway some 55 km south of Oruro. The mine lies in a group of low hills on the east slope of a broad valley of northerly trend. The valley is separated from the altiplano to the west by a prominent ridge that rises several hundred meters above the surrounding country (fig. 1). Callipampa is situated a short distance west of the ridge, near the east margin of the altiplano. The elevation at Callipampa is 3700 m and at the mine 4100 m. Monserrat is near the northeast limit of what may be called the Poopo-Pazna district, an area of northwesterly trend about 25 km in length and 15 km in width. The district includes the tin-silver prospects of Poopo to the north, the zinc-tin deposits of Salvador to the southwest, and the tin-tourmaline veins of Avicaya to the south. Along the prominent ridge already mentioned, which forms the western limit of the district, there are several tin and antimony prospects including the Trinacria mine, which is famous for its fine specimens of cylindrite. Although the principal ore mineral is cassiterite, the tin deposit of Monserrat contains an unusual amount of teallite. Cassiterite occurs in part as a finely granular mixture with sulphides of iron and zinc and in part as needle tin of late hypogene age. The regional structure is dominated by broad folds typical of the Andes of Central Bolivia and similar to those of the Llallagua district. The area adjacent to the Monserrat mine is underlain by thin-bedded shale somewhat variable in color but predominantly dark grey to black. The beds strike northwest and dip at low angles southwest, forming part of the northeast limb of a major syncline. A resistant sandstone formation, which underlies the black shale, crops out along a ridge east of the mine and also accounts for the high ridge to the west that was previously mentioned. No igneous rock of any kind is found at Monserrat. The nearest intrusive bodies known are the irregular dikes and masses of quartz porphyry at Avicaya about 10 km to the south. Mine Workings The Monserrat property includes one main vein, which can be followed on the surface for 1600 m, and two or three branch veins of distinctly minor importance. The principal haulage tunnel, referred to as the San Carlos adit or level III, extends northeasterly for 1700 m, following the main vein throughout most of this distance. Above the adit, there are

Jan 1, 1951

By F. S. Turneaure, R. Gibson

The tin deposit of Monserrat, Bolivia, consists of one major vein 1600 m in length. The ore is unusual because of the notable quantity of teallite, even though cassiterite is the principal tin mineral. The deposit, formed at shallow depth under a wide range in temperature, may be classed as xenothermal. Polished sections reveal a complex history of replacement, with low-temperature minerals deposited before high-temperature minerals. THE Monserrat mine1'2 of the Compania Minera Monserrat is located 11 km east of Callipampa, a station on the Antofagasta and Bolivia Railway some 55 km south of Oruro. The mine lies in a group of low hills on the east slope of a broad valley of northerly trend. The valley is separated from the altiplano to the west by a prominent ridge that rises several hundred meters above the surrounding country (fig. 1). Callipampa is situated a short distance west of the ridge, near the east margin of the altiplano. The elevation at Callipampa is 3700 m and at the mine 4100 m. Monserrat is near the northeast limit of what may be called the Poopo-Pazna district, an area of northwesterly trend about 25 km in length and 15 km in width. The district includes the tin-silver prospects of Poopo to the north, the zinc-tin deposits of Salvador to the southwest, and the tin-tourmaline veins of Avicaya to the south. Along the prominent ridge already mentioned, which forms the western limit of the district, there are several tin and antimony prospects including the Trinacria mine, which is famous for its fine specimens of cylindrite. Although the principal ore mineral is cassiterite, the tin deposit of Monserrat contains an unusual amount of teallite. Cassiterite occurs in part as a finely granular mixture with sulphides of iron and zinc and in part as needle tin of late hypogene age. The regional structure is dominated by broad folds typical of the Andes of Central Bolivia and similar to those of the Llallagua district. The area adjacent to the Monserrat mine is underlain by thin-bedded shale somewhat variable in color but predominantly dark grey to black. The beds strike northwest and dip at low angles southwest, forming part of the northeast limb of a major syncline. A resistant sandstone formation, which underlies the black shale, crops out along a ridge east of the mine and also accounts for the high ridge to the west that was previously mentioned. No igneous rock of any kind is found at Monserrat. The nearest intrusive bodies known are the irregular dikes and masses of quartz porphyry at Avicaya about 10 km to the south. Mine Workings The Monserrat property includes one main vein, which can be followed on the surface for 1600 m, and two or three branch veins of distinctly minor importance. The principal haulage tunnel, referred to as the San Carlos adit or level III, extends northeasterly for 1700 m, following the main vein throughout most of this distance. Above the adit, there are

Jan 1, 1951

By John V. Beall

Probably it won't happen to us again in a thousand years, but it was very embarassing at the time. It is only because of certain matters that have come up this month that we tell you at all about it. At the beginning of our trip to Peru and Chile last summer, we were flying with Bill Haddon from Lima to Tacna aboard Fawcett. Being an old hand at foreign travel, particularly in South America, we felt obliged to explain some of the special features of travel in Latin America and the niceties of etiquette in particular and were so engaged when the plane landed at the airport. We led the way briskly into the terminal, expecting at any moment to have a representative of Southern Peru Copper pop up and present himself. However, this didn't happen so we repaired to the baggage arrival station to wait. All the bags were quickly picked up, but ours were no where to be seen. Bill was slightly agitated because the plane was being buttoned up for take off. However, rising to the emergency with our usual aplomb, we took charge of the situation. Brandishing the claim checks under the nose of the porter who pointed to them and said, "si, Tacna," we nodded briskly and in our serviceable Spanish said "si se[n]or, vayase viejo, rapido." He was off and back with our suitcases quickly enough.

Jan 1, 1970

BURKE BAKER, Philadelphia, Pa. (written discussion*).-The small briquetting plant of the American Briquet Co., at 25th Street and Washington Ave., Philadelphia, was built primarily as a demonstration plant. Its output per hour is 4 tons of 2-oz. briquets, which have been retailed in the, vicinity during the year the plant has been in operation. They have proved very acceptable for use in ranges, heaters and grates in-home, and in steam heating plants in apartment houses and hotels. They have not been sold for power purposes, although satisfactory tests have been made in. this field. Anthracite silt is used and is shipped direct from breaker or washery, the only preparation it receives being the removal f excess moisture by means of a Ruggles-Coles rotary dryer. Care is taken, however, to purchase silt containing less than 18 per cent. ash. The method is covered by U. S. Patent No. 941454, issued to Chas. E. Hite, and is known as the "emulsion process." The binder, which is the, basis of the patent, is composed. of 0.5 per cent. cornstarch or wheat flour; 1 per cent. asphaltum or hydrolene, and 6.5 per cent. water, on the weight of coal dust. It is prepared in a tank equipped with paddle agitators and heated by steam jets. The starch and water are first made into a paste by being brought to the boiling point with live steam; the melted asphaltum is then introduced and thoroughly beaten into the paste by the agitators. This rapid stirring breaks. the hot asphaltum into minute particles which are distributed through the paste, producing a smooth chemical emulsion. This emulsion, when dried, is not soluble in water. The binder is mixed with the dry coal dust in a horizontal paddle mixer, 8 per cent. binder to the weight of coal being used. The resultant plastic mass is then discharged into the press, which is of the simple roll type. Since the binder is a liquid and is not sticky or gummy until

Jan 3, 1918

By L. W. Casteel

St. Joseph Lead Company's Southeast Missouri mines have been successfully converted to the use of ammonium nitrate and fuel oil as a blasting agent. This is significant to the company because it means a savings of a quarter of a million dollars per year. It is significant to the mining industry because of the unusual conditions involved and the methods and materials used to overcome them. St. Joe has been mining the low grade lead deposits of southeast Missouri since 1864. This ore occurs as disseminated galena in widely scattered pockets within the Bonneterre dolomite. The daily production of 20,000 tons is obtained from several hundred small, room and pillar stopes covering an area 10 miles long and five miles wide. Distribution of explosives and other materials is a real problem. Drilling in the stopes is done with air legs, column- mounted machines or jumbos, depending on the size and location of the stope. Drill hole sizes vary from 1 3/8-in. diam down to 1 1/8-in. Each driller charges his own holes and shoots them at the end of the shift. Numerous shafts provide natural ventilation which is supplemented in isolated areas by churn drill holes equipped with blowers. Water, in most stopes, is not a serious problem, although the mines do produce about 20,000 gpm.

Jan 5, 1962

By R. S. Rickard, M. C. Fuerstenau

Anodic polarization curves for iron dissolution and cathodic polarization curves for copper deposition and ferric and hydrogen ion reduction were studied. These results were used to predict the relative rates of the reactions: The rates of the first two reactions were found to be first order with respect to the reacting ion, and the rale-controlling step was diffusion of the ions to the callzode surface. The rate of hydrogen ion reduction in an oxygen-free solution is dependent on the reciprocal of the square root of the hydrogen ion activity. In solutions containing oxygen, the rate of hydrogen reduction becomes dependent on the square root of the partial pressure of oxygen. At equal concentrations copper precipitation occurs about twice as fast as ferric ion reduction. In an air-saturated solution containing 0.01 M cupric ion at pH 2, the rate of hydrogen ion reduction zs about 10 times slower than that of copper precipitation. At pH values below 3, the rate of hydrogen reduction in oxygen-free solutions is very slozu. COPPER cementation has been utilized industrially for many years as a means of recovering copper from aqueous solutions. There are many different types of cementation plants, but all simply provide a means of contacting iron with relatively dilute copper solutions. In the past little or no attention has been paid to rates or mechanisms of the reactions involved. As a result, this and other studies'-3 have been undertaken recently to establish the important parameters in this system. The reactions involved in copper cementation by iron are: Since transfer of charge is involved in every case, these reactions should be considered from an electrochemical point of view. In any electrochemical system involving electrolytic conduction, passage of electrons necessitates ion transfer to the respective electrodes according to Faraday's law. The current in the system will be proportional to the rate of ion transfer, and, therefore, when the current in the galvanic cell is known, the rates of the reactions involved can be determined. Galvanostatic electrode measurements5" are applicable for these electrochemical studies, in that with this technique polarization curves (current density vs electrode potential) are established by impressing a constant current through an electrode and measuring the electrode potential. Once the current density, electrode potential, and reacting area are known for each reaction in this cementation system, the rates of the iron-consuming reactions can be determined. EXPERIMENTAL MATERIALS Several metal electrodes were used in this investigation; they are shown in Table I. Solutions were made with reagent-grade salts and conductivity water. Air, nitrogen, and oxygen were employed. All of these gases were saturated with water and degreased prior to use. EXPERIMENTAL PROCEDURE The experimental work was divided into two general areas. The first area involved galvanostatic measurements, which were used to determine the rates of reactions as a function of various parameters. The second area comprised actual cementation experiments to check the rates predicted from the electrode measurements. Galvanostatic Electrode Experiments. Polarization curves were obtained using a standard galvanostatic technique5'= with the apparatus shown in Fig. 1. The various electrode polarization experiments were run the same way except for changes in solution composition, polarity, and type of measured electrode. The general procedure involved the following steps: 1) a solution was made 0.5 M in sulfate ion and to the desired cation concentrations; this solution was placed in a constant-temperature bath and saturated with the desired gas; 2) the electrodes were cleaned and placed in the electrode holder; 3) the previously cleaned apparatus was assembled and immersed in a constant-temperature water bath (temperature controlled to ± 0.05"C); 4) the electrode was then positioned; the solutions were introduced, and the polarization meas-

Jan 1, 1969

By William Kent

(Read at the Philadelphia Meeting, February, 1878.) IN the paper by Mr. Fernow, on Red Charcoal, read at the first session of this meeting, it was suggested that this fuel might be used in the blast furnace with greater economy than ordinary or black charcoal. In the discussion which followed the paper, it was stated that the charcoal furnaces of the Lake Superior District have used imperfectly burned charcoal with success, and that these furnaces have given the best results in fuel economy on record. On consulting some of our well-known metallurgical authorities the writer finds that the question of the use of red charcoal, or other imperfectly burned charcoal, or charred wood, is not at all new. In Percy's late work on Fuel, pages 409-414, are given a few facts, which are here condensed, as follows:

Jan 1, 1878

By H. W. Fox, M. R. Achter

IN a previous study of the effect of atmosphere on creep-rupture properties,' it was shown that the relative strength of nickel in air and in vacuum may be reversed by a change in either stress or temperature, Fig. 1. At low stresses and high temperatures the metal is stronger in air but stronger in vacuum at high stresses and low temperatures. A mechanism to explain this reversal was proposed involving two competing processes; oxidation strengthens the metal while adsorption of gas lowers the surface energy, relative to that in vacuum, and reduces the work required to propagate a crack. The process which controls is determined by stress and temperature. In a number of private communications, however, the objection has been made that even in the vacuum of objection mm of Hg used in this study, the surface of a

Jan 1, 1960

By T. J. Woods

Tars paper deals with the origin, definition and prevention of scabs an semifinished rolled-steel product. Mold coatings, which are considered essential in scab prevention, were found to be effective only in relation to the ingot surface of semikilled and killed steels and not necessary for the rolled product. That is to say, the scabs on ingots caused by having been cast in uncoated molds are eliminated in the soaking and rolling operations, therefore are not present on the rolled product. This fact, which is contrary to the average opinion, was established after extensive and thorough experiments had proved the ordinary conception of the origin of scabs to be incorrect. This subject may be of little or no concern to steel plants producing small ingots for the manufacture of small billets and bars, except as it may be of interest in showing why their surface troubles with scabs do not exist on the product of heats with normal pouring practice. But to the producer of large ingots to be rolled into slabs for large plates used in shipbuilding, it is a very important subject. DEFINITION OF A SCAB The generally accepted opinion is that the individual scabs present on rolled products (as shown by Fig. I) are considered to have been individual splashes on the ingot surface. This opinion was found to be incorrect. Experiments showed that there were no individual scabs on the product that had appeared as individuals on the ingot surface. The single scabs seen are either pieces of a shell that is present near the bottom of all top-cast ingots, or a veneer that may be present on any part of an ingot improperly poured, as when the stream strikes the mold wall. This definition is based on a detailed study of scabs and their characteristics in which the following have been found true: Location.- On the product of heats poured without trouble, scabs, if present, are always on the product that corresponds to the bottom end of the ingot, and usually occur in clusters, This is true whether molds are coated or not. Shape.-There is no regularity as to shape, size or thickness. It is sometimes possible to separate a few pieces and place them together, like pieces of a jigsaw puzzle, indicating that at one time they had been united as one piece. If individual splashes were the origin of scabs, the foregoing would not be true. Instead, the splashes, which occur throughout the pouring of the ingots, would be present uniformly over the entire product and there would be considerable similarity in the shape and thickness of the scabs. EXPERIMENTAL WORK Our experimental work was conducted on 200-ton heats of semikilled plate steel tapped into an oval ladle 15 ft. high. All ingots were top-cast direct into 24 by 54 by 82-in. molds, straight-sided, set on fat stools. Two separate studies were made about one year apart, each study extending

Jan 1, 1943

By W. C. Wright

A PRACTICAL program of education for workers of the mining industries is being formulated by the Federal Board for Vocational. Education in cooperation with the States in which this industry is a dominant one. The Federal Government last year passed a law, known as the Federal Vocational Education Act, that provides for the promotion of vocational' education and for cooperation with the States in the promotion of such education in agriculture and trades and industries and in the preparation of teachers of vocational subjects. More than 1,000,000 men in the continental United States are employed in mines and quarries. The following table, from the-1910 Census Report, shows the relative importance of mining and manufacturing pursuits: Manufactures Mines and Quarries Employees 7,405,313 1,109,410. Capital $18,428,269,706 $3,380,525,841 Value of product $20,672,051,870 $1,238,410,322 Of the more than 1,000,000 men employed in mining, almost three-fourths are engaged in the, production of bituminous and anthracite coal; one-fifth, in the production of copper, iron, lead, zinc, and other metals; and the remainder in getting out structural and miscellaneous materials from quarries. The meeting of the needs of the coal-mining industry, therefore, is the problem of greatest importance in the point of numbers to be served. Moreover, the dangers in coal mining are greater than in metal mining. Practically all States have set up educational and technical standards , for the position of foreman, boss, superintendent, etc., and every applicant for these positions must have a certificate of competency. The qualifications, too, are becoming increasingly difficult in the field of technical information. In some States, every miner must have a certificate, which is issued by the mine examining board. only after an oral examination.

Jan 1, 1919

GEORGE F. COMSTOCK (author's reply to discussion*).-Mr. Thum's description of the effects of butt welding and spot welding on the micro-structure of steel are interesting and timely. The speed with which the changes noted by Mr. Thum must take place is indeed remarkable, but the writer has noted a similar very rapid diffusion of carbide in annealing a t a rather high temperature certain samples of soft sheet steel containing massive cementite segregated on a small scale. The massive cementite in such steel can be dissolved and distributed very quickly if the proper temperature is attained. Mr. Thum's explanation of the structure he found in the spot welds seems entirely reasonable, but the mystery of the decarburized material in the butt weld is one that might well be the subject of further research. The possibility of decarburization by air ,might perhaps be worthy of a little more consideration than he gives it, for the oxides formed would be gaseous on account of the presence of carbon, and hence not visible in the microscope, and the effect of the pressure might be to squeeze the carbon oxides, which would normally form blow-holes, out of the metal or possibly into such small volumes as not to be noticed The removal of carbon by liquation and squeezing into the fin would be an effect similar to the "bleeding" of a steel ingot that is rolled while the center is still liquid, giving a soft low-carbon interior in the finished section while the segregate was removed in cropping the pipe. This effect in Mr. Thum's butt welds could, however, only be obtained if the weld was heated to near the melting point of the steel, and if the carbon was considerably segregated in the bars at the start, for the first effect of the high temperature would be to promote diffusion rather than the contrary segregation and Equation. It is gratifying to learn from Dr. Ruder's remarks that his researches have resulted in no disagreement with the few points brought out by the writer's experiments. In addition to the three forms in which nitrogen may occur in iron that he mentions, it would seem that a fourth form is often found; This is apparently a eutectoid, like pearlite, and sometimes almost as coarse as the massive cementite seen in soft steel sheets that have been annealed for a long time. One of the things needed in the metallographic study of steel is an etching reagent that will distinguish definitely between nitride in this form and the more common pearlite or cementite.

Jan 6, 1919

By A. A. Smith, J. S. Smart, A. J. Phillips

The preparation of a sufficient quantity of high-purity copper for extensive laboratory use in the study of impurity effects has been an integral part of a research program in progress at the Central Research Laboratory of the American Smelting and Refining Co. for the past several years. Initially the degree of purity desired was that necessary to meet two essential requirements for experimental accuracy: (I) no impurity was to be present in the copper in an amount capable of producing a detectable effect on the properties to be studied, (2) even the minor changes in propertties caused by the addition of extremely small amounts of individual elements were to be measured without significant interference from contaminants. In the course of the investigation, evidence has accumulated to justify the conclusion that this copper is of exceptional purity; in fact, no impurity can be detected by any chemical method or spectrographic technique known to the authors. The present paper describes the method of production of the copper and presents some of its properties. Preparation oF High-purity Copper The elimination of impurities from commercial electrolytic copper is accomplished by a three-step purification process. The first operation consists of an electrolysis through a purified CuSO4-H2SO4 electrolyte using bagged anodes, low current density (5 amp. per sq. ft.) and low tem- perature (25°C max.). The electrolyte is prepared from commercial Cu2SO4 and is purified by heating the solution and adding I gram Fe as Fe2(SO4)3 to each 100 grams dissolved copper; sufficient hydrated oxide of copper, prepared from Cu2SO4 and NaOH, is supplied to precipitate Fe(OH)3, which carries down arsenic, antimony, tin, selenium, tellurium and other minor constituents. Silver and remaining traces of lead are removed by addition of Na2S to the acidified filtrate, which is then reatered after standing hot overnight. The cold solution is made up to 30 grams per liter Cu and 150 grams per liter H2SO4 and introduced without addition agents into the electrolytic system, which consists of a double row of hard-rubber battery boxes with the inside webbing and partitions removed, arranged in seven steps of ascending height. Electrolyte is uniformly supplied to the two highest cells by glass siphons operating from a constant-level reservoir, and flows by gravity through the bank of seven cells, entering each at the bottom and leaving at the top. Glass air lifts continuously supply the returning liquid to the constant-level reservoir for recirculation. Each cell contains three 4 3/4 by 4 3/8 by 1-in anodes cast from high-quality electrolytic wirebar copper, various lots of which have been used with equal success. The anodes are pinned to sheet copper hangars shaped to prevent crawl of the electrolyte to the multiple-wired bus bars—which would result in fouling of the contacts—-and hang inside wool flannel bags stretched over open wood frames. The deposit

Jan 1, 1941

By A. J. Phillips, A. A. Smith, J. S. Smart

The preparation of a sufficient quantity of high-purity copper for extensive laboratory use in the study of impurity effects has been an integral part of a research program in progress at the Central Research Laboratory of the American Smelting and Refining Co. for the past several years. Initially the degree of purity desired was that necessary to meet two essential requirements for experimental accuracy: (I) no impurity was to be present in the copper in an amount capable of producing a detectable effect on the properties to be studied, (2) even the minor changes in propertties caused by the addition of extremely small amounts of individual elements were to be measured without significant interference from contaminants. In the course of the investigation, evidence has accumulated to justify the conclusion that this copper is of exceptional purity; in fact, no impurity can be detected by any chemical method or spectrographic technique known to the authors. The present paper describes the method of production of the copper and presents some of its properties. Preparation oF High-purity Copper The elimination of impurities from commercial electrolytic copper is accomplished by a three-step purification process. The first operation consists of an electrolysis through a purified CuSO4-H2SO4 electrolyte using bagged anodes, low current density (5 amp. per sq. ft.) and low tem- perature (25°C max.). The electrolyte is prepared from commercial Cu2SO4 and is purified by heating the solution and adding I gram Fe as Fe2(SO4)3 to each 100 grams dissolved copper; sufficient hydrated oxide of copper, prepared from Cu2SO4 and NaOH, is supplied to precipitate Fe(OH)3, which carries down arsenic, antimony, tin, selenium, tellurium and other minor constituents. Silver and remaining traces of lead are removed by addition of Na2S to the acidified filtrate, which is then reatered after standing hot overnight. The cold solution is made up to 30 grams per liter Cu and 150 grams per liter H2SO4 and introduced without addition agents into the electrolytic system, which consists of a double row of hard-rubber battery boxes with the inside webbing and partitions removed, arranged in seven steps of ascending height. Electrolyte is uniformly supplied to the two highest cells by glass siphons operating from a constant-level reservoir, and flows by gravity through the bank of seven cells, entering each at the bottom and leaving at the top. Glass air lifts continuously supply the returning liquid to the constant-level reservoir for recirculation. Each cell contains three 4 3/4 by 4 3/8 by 1-in anodes cast from high-quality electrolytic wirebar copper, various lots of which have been used with equal success. The anodes are pinned to sheet copper hangars shaped to prevent crawl of the electrolyte to the multiple-wired bus bars—which would result in fouling of the contacts—-and hang inside wool flannel bags stretched over open wood frames. The deposit

Jan 1, 1941

By R. I. Jaffee, C. M. Craighead, G. A. Lenning

Hydrogen forms a beta-stabilized system with titanium, with a beta eutectoid at about 300°C and 44 atomic pct H2. 'The solid solubility of hydrogen in alpha decreases from about 8 to about 0.1 atomic pct from 300°C to room temperature. Hydrogen has little effect on tensile properties, but decreases notch-bar toughness to a large degree. This latter effect appears to be the result of increased notch sensitivity. PRIOR to this investigation, only a small amount of information was available on the effect of hydrogen on the mechanical properties of titanium. The effects of the other interstitially soluble elements, carbon, oxygen, and nitrogen, had received detailed study. Jaffee and Campbell1 indicated that hydrogen up to 1 atomic pct did not affect tensile properties deleteriously. Pitler' indicated that 1 atomic pct H, in titanium reduced the impact strength appreciably, but his alloys contained appreciable amounts of oxygen, and it was difficult to attribute the embrittlement entirely to hydrogen. The high temperature portion of the equilibrium diagram for the Ti-H system was established by McQuillan," and his data generally corresponded with the results of Kirschfeld and Sieverts," Gibb and Kruschwitz," Bevington, Martin, and Mathews," and other investigators. The lower concentration limit of the hydride phase varied considerably among investigators, and Gibb and Kruschwitz9 ad shown that small amounts of contaminants in either titanium or hydrogen caused considerable variation in this lower limit. In view of this pronounced effect of contaminants, the extrapolated value of McQuillan's, about 48 atomic pct at the 325°C eutectoid, appeared the most reasonable. McQuillan's lowest experimental value was 54 atomic pct at a temperature of 450 °C. The density of titanium had been shown to decrease with increasing hydrogen content, but discrepancies were noted among the various investigations. The best values indicated that the density was decreased from 4.56 grams per cc at 0.27 atomic pctl to 3.84 grams per cc at 61.3 atomic pct? This investigation was conducted to determine the effects of hydrogen on a titanium, both in high purity and commercially pure metals, and on high purity a titanium alloys. Material and Fabrication The literature indicated that impurities in either the hydrogen or the titanium must be kept to a minimum. For this reason, the initial studies were made with high purity iodide-refined titanium. The vendor's analysis of the iodide titanium and the hydrogen content of the as-fabricated Y4 in. diameter rods are shown in Table I. Two 1 lb ingots were prepared by arc melting under argon in a water-cooled crucible, using a water,cooled tungsten electrode. This equipment has been described.' As-cast Brine11 hardness numbers of 88 and 58 for these ingots were low enough to insure that the high purity of the metal was maintained during arc melting. The ingots were hot forged to % in. diameter rods at 800°C, cleaned by grit blasting, and then cold swaged to Yz in. diameter rods. The rod was then air annealed at 725 "C, ground to remove scale, and cold swaged to Y4 in. diameter (75 pct reduction in area). The material was then annealed for 1 hr in argon at 800°C to develop an equiaxed a grain size of about 0.05 mm. Micro tensile specimens and microimpact specimens were machined from this rod prior to treatment in the Sieverts-type absorption apparatus. Two lots of commercially pure RC-55 titanium were also used in this investigation to determine the effects of hydrogen and the normal impurities on mechanical properties. The commercially pure RC-55 alloy was obtained in the form of % in. diameter rod. The analysis of this material is also given in Table I. The % in. diameter rods were hot swaged

Jan 1, 1955

By I. S. Servi, N. W. Marr

TIN markedly increases the softening temperature of pure copper with only a moderate effect on conductivity. Smart and smith' indicated a substantial increase in softening temperature upon addition of different levels of tin up to 0.05 pct in oxygen-free copper. However, after finding no effect of tin in copper containing about 0.025 pct O, they concluded that "the presence of oxygen completely nullifies these changes in properties by precipitation of SnO2.'' Since preliminary tests on Cu-Sn-0 alloys indicated that this conclusion is not valid outside the extremely limited tin range investigated by Smart and Smith, research was primarily directed toward the partition of tin between the copper-base matrix and the oxide phases. Experimental. Material was prepared by sealing an 80 to 100-g charge consisting of oxygen-free copper, tin, and copper oxide into a y-in.-ID quartz capsule which was evacuated and back-filled with tank-grade argon to 3 atm. The sealed vials were heated to 1125ºC, kept at temperature for 30 min, occasionally agitated, and then allowed to air-cool outside the furnace ("as-cast"). The castings were cold-swaged to 0.370 in., annealed 1 hr at 600°C ("as-annealed"), and cold-swaged 16.5 pct ("as-swaged"). Cross sectional wafers were annealed for 1 hr at various temperatures and Rockwell F hardness measured. The "softening temperature" was defined as the interpolated temperature at which the hardness was 50 Rockwell F. Electrical resistance was measured by an ac poten-tiometric method on 0.040-in.-diam wires after a 1 hr anneal at 600°C. Relative accuracy was of the order of 1 pct. Chemical analyses for tin were performed by two methods, identified as "Acid flux" and "HN03 dissolution". The first consisted of fusing the sample with potassium pyrosulfate and leaching the resulting melt with 10 pct sulfuric acid. The spectrophotometric procedure which followed is described in Ref. 2. Oxygen analyses were performed by the vacuum-fusion method with a bath temperature of 1650°C. Tin content of oxides and copper phases was measured with the X-ray microprobe, using a calibration curve based on a series of oxygen-free Cu-Sn alloys. Results. In Fig. 1, the nominal tin composition for alloys containing nominally 400 ppm O was plotted vs the analyzed or the computed tin content—the latter derived from one of the following: 1) "acid flux" chemical analysis; 2) "HN03 dissolution" chemical analysis; 3) X-ray microprobe analysis of the copper matrix; 4) equivalent tin content, based on the measured increase in electrical resistivity (an increase in resistivity of 1.6 microhm-cm is approximately equivalent to 1 wt pct of sn1,3). It is evident from Fig. 1 that the results of the acid flux analysis are consistent with the nominal composition while the HNO3 dissolution method generally yields lower values, consistent with those obtained from electrical resistivity measurements and somewhat higher than those obtained by microprobe analysis. Microprobe and resistivity values are affected only by the tin in solid solution; hence the HN03 method

Jan 1, 1970

By Pedro Bolsaitis, Paul M. Sullivan

The activities of zinc in liquid Zn-A1 alloys in the temperature range of 1000' to 1160°K were determined by means of the isopiestic technique. The results are in reasonable agreement with the previous values determined by the radioactive tracer dew point method. Slightly negative excess entropies of mixing were found. The measured activities suggest that the a function for these alloys is not a constant, as has frequently been assumed, but is better represented by two straight line segments of different slopes. THE thermodynamic data of Al-Z alloys have been the subject of investigation by many authors. However, in the recent compilation of such data by Hult-gren et al.,5 the conclusion is reached that none of the previous measurements are reliable or consistent with each other. Since then two new sets of measurements have been reported,2, 8 both laying claim to good accuracies, yet showing very significant disagreement in the measured activity coefficients of zinc in Zn-A1 alloys and in the magnitude and sign of the excess entropies of mixing. Information on the thermodynamics of the system is of particular interest for interpreting results of the Bureau of Mines research on refining of zinc by distillation of die cast scrap. The present study was undertaken as an independent check on the recent values obtained from dew point measurements 8 and electromotive force measurements.' The isopiestic method, first introduced by Herasy-menko,' was chosen because it is one of the few thermodynamic techniques which, in principle at least, is carried out under perfect equilibrium conditions. The disadvantage of the method is that data are obtained at various random compositions and temperatures, which makes the interpretation somewhat cumbersome. The random errors arising from temperature gradients and fluctuations appear to be comparable to those of other techniques, as evidenced by the magnitude of the estimated uncertainties in the calculated integral thermodynamic quantities. An advantage of the method is that each run provides a relatively large amount of data; thus, it is less time consuming than those methods where samples of each composition must be measured individually. EXPERIMENTAL PROCEDURE The activities of zinc in liquid Zn-A1 alloys were measured by the isopiestic method which uses the principle of the tendency toward equilibrium of a series of samples at various temperatures under an imposed vapor pressure of the more volatile component (i.e., zinc, in this case). The basic apparatus is shown in Fig. 1. The small graphite crucibles that contained the metal samples were 15 mm ID and 13 mm deep with approximately 3 mm wall thickness. Each crucible was notched at the top and bottom to allow easy passage of vapor from one to another. At the beginning of an experiment each crucible was weighed on an analytical balance. Zinc and aluminum of spectrographic purity (99.999 pct) were then weighed into the crucibles. The amounts of each metal added were such that initial compositions varied above and below equilibrium values. One crucible contained only pure zinc. After weighing, the crucibles were stacked with the pure zinc on the bottom (corresponding to the lowest temperature in the furnace) and richest aluminum alloys at the top. The entire stack of crucibles was then placed in the silica glass container "E" which was then sealed under vacuum. Sixteen to twenty calibrated Chromel-Alumel thermocouples were attached by wire along the length of the silica tube, one or more adjacent to each sample.

Jan 1, 1970

By F. M. Lewis, J. F. Myers

W. I. Garms-—The authors state that when they added 11 tons of balls to the 45 pct volume ball load, the power needle did not budge. The question arises as to whether any increase in capacity accompanied the 11-ton addition. It is hardly conceivable that all of the balls making up the 11-ton addition were sterile. However, as the work done in the ball mill is not by kilo-watthours per se or balls per se but by kilowatthour-balls, it is possible that the kilowatthourballs in the mill before the 11-ton addition had a different amperage, voltage or robustage than those in the mill after the addition and that the overall outcome was that equal work was done before and after the addition. The authors can keep the efficiency that they got with the 45 pct volume 1-in. ball charge and get additional capacity by putting more kilowatthourballs to work in the form of the addition of 11 tons of 2-in. balls to the present ball charge, and subsequent makeup additions by weight of 20 pct 2-in. balls and 80 pct 1-in. balls. J. F. Myers (authors' reply)-—Mr. Garms points his finger at the 11 tons of "sterile" balls added to the Tri-cone mill. A fact so interesting to us that we felt it should be reported. Clearly, ball slippage at the existing mill speed prevented any further transfer of power from the shell to the ball mass. We agree that the kilowatthourballs would increase, were we charging rough 2-in. balls as suggested by Mr. Garms. The assumption is, of course, that we would get a corresponding increase in work done. Our reported data (CIME meeting, Vancouver, 1946) shows a gain of work accomplished of 7.6 pct as we decreased the ball size from 2 in. to 11/2 in. and a further gain of work accomplished of 2.1 pct when we went from 11/2 in. to 1 in. The small ball results reported by H. R. Banks at Chapman Camp are also very convincing. In the case of 2-in. balls they would take the conventional ball path and start cascading. They would thus destroy the classifying pool over the "foot" of the

Jan 1, 1951

By J. F. Myers, F. M. Lewis

W. I. Garms-—The authors state that when they added 11 tons of balls to the 45 pct volume ball load, the power needle did not budge. The question arises as to whether any increase in capacity accompanied the 11-ton addition. It is hardly conceivable that all of the balls making up the 11-ton addition were sterile. However, as the work done in the ball mill is not by kilo-watthours per se or balls per se but by kilowatthour-balls, it is possible that the kilowatthourballs in the mill before the 11-ton addition had a different amperage, voltage or robustage than those in the mill after the addition and that the overall outcome was that equal work was done before and after the addition. The authors can keep the efficiency that they got with the 45 pct volume 1-in. ball charge and get additional capacity by putting more kilowatthourballs to work in the form of the addition of 11 tons of 2-in. balls to the present ball charge, and subsequent makeup additions by weight of 20 pct 2-in. balls and 80 pct 1-in. balls. J. F. Myers (authors' reply)-—Mr. Garms points his finger at the 11 tons of "sterile" balls added to the Tri-cone mill. A fact so interesting to us that we felt it should be reported. Clearly, ball slippage at the existing mill speed prevented any further transfer of power from the shell to the ball mass. We agree that the kilowatthourballs would increase, were we charging rough 2-in. balls as suggested by Mr. Garms. The assumption is, of course, that we would get a corresponding increase in work done. Our reported data (CIME meeting, Vancouver, 1946) shows a gain of work accomplished of 7.6 pct as we decreased the ball size from 2 in. to 11/2 in. and a further gain of work accomplished of 2.1 pct when we went from 11/2 in. to 1 in. The small ball results reported by H. R. Banks at Chapman Camp are also very convincing. In the case of 2-in. balls they would take the conventional ball path and start cascading. They would thus destroy the classifying pool over the "foot" of the

Jan 1, 1951