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By W. R. Ingalls

ThE following chronology presents the history of lead-mining in the United States in a brief form and is a useful reference in connection with the statistics of production: 1621.. Lead was mined and smelted near Falling Creek, Va., to supply the local demand for bullets and shot. This was the first mining and .smelting of lead in what is now the United States. 1632. In a report made on the minerals of New England, lead-ore is mentioned. (Bishop, I., 470.) 1650. Supposed beginning of mining by Jesuits in Pima county, Ariz. 1651. Grant of lead-mine at Middletown, Conn., to Gov. John Winthrop. 1682. Lead-ore supposed to have been discovered in Wisconsin by Nicholas Perrot. (K. D. Irving, Mineral Resources of Wisconsin, Trans., viii., 498.) 1700 Discovery of lead in Missouri by Penicaut, one of Le Sueur's party. Tile same expedition discovered lead near the southern boundary of Wisconsin in August of the same year. 1712. Grant by Louis XIV. of the Crozat patents, with special privileges respecting the discovery and operation of mines in the then territory of Louisiana. Little or no mining was done under this patent until about 1720. 1717. Transfer of Crozat patents to the Mississippi Co., promoted by John Law, which prepared for active mining. 1719. First attempt to mine and smelt lead in Missouri, made by Sieur de Lochon, in behalf of the Mississippi Co., near Meramec river. Results unsuccessful.

Jan 1, 1908

By H. F. Yancey

PHYSICAL properties have been used for a long time in characterizing different kinds of coal, and physical properties, such as friability and slacking, have been included with chemical properties in grouping coals according to the widely used system of classification adopted by the U. S. Geological Survey. Nevertheless, the usefulness of physical properties for classifying the different ranks or kinds of coal has been limited because it has not been possible to express these properties in definite form as numerical values. Because of the present wide interest in the formulation and adoption of a satisfactory system of coal classification, the Northwest Experiment Station of the U. S. Bureau of Mines, in cooperation with the College of Mines of the University of Washington, has recently completed a study of the physical and chemical properties of approximately 100 different coals ranging from lignite to, anthracite. PURPOSE AND SCOPE For this investigation samples were collected in approximately 45 mines and prospects in Washington and 23 mines in other states. The following studies, in addition to proximate and ultimate analyses, were made of the samples: Determination of (1) friability, (2) slacking or weathering characteristics, (3) yield of products by low-temperature carbonization in a laboratory retort, and (4) agglutinating value. Most of the coals examined were subjected to each of the tests enumerated, but with coal of some ranks this was unnecessary in some instances, and in others it was not feasible to do the work involved.

Jan 1, 1932

By William Fink

THIS paper is the nineteenth of a series from the Aluminum Research Laboratories, presenting the results of the investigations of equilibrium relations in aluminum-base alloys made from electrolytically refined aluminum. In previous papers equilibrium) relations have been deter-mined and correlated for 12 binary systems. Equilibrium relations have also been determined for portions of the aluminum corners of three ternary systems (aluminum-iron-silicon, aluminum-magnesium-silicon and alu-minum-copper-magnesium). The object of the present paper and those to follow is to increase our knowledge of the aluminum corner of the more important ternary systems. In 1926 Dix and Keith? suggested a new method for designating the phases encountered in alloy systems. The system has been used to a very limited extent 1,2,3. The system has since been slightly modified and will be used in this and future papers. In the system as modified, a phase is designated by placing in parentheses the chemical symbols of the elements essential to the formation of that phase. The symbols in the parentheses are separated by dashes in order to clearly distinguish them from a chemical formula. Elements that are not necessary to the formation of the phase in question, but which may be present in solid solution, are not indicated in the designation. If two or more phases would have the same designation according to these rules, they are dis-tinguished by prefixing Greek letters, and are definitely identified by X-ray diffraction patterns.

Jan 1, 1936

By W. F. Dietrich

Mineral fillers are relatively inert chemically under the conditions of use but have physical properties* that modify those of the materials • The properties. uses, and other data on 15 classes of important *The pro listed in the second edition of Industrial Minerals and Rocks.l A third edition of this reference is in preparation. in which they are incorporated. The mineral fillers considered in this article are asbestos, barite, clays, diatomite, crushed limestone, limestone whiting and lime, mica, silica, talc and soapstone, and pyrophyllite. Slate and stone, other than limestone and its derivatives, are excluded because, even though used in large quantities, they are exceptionally low-cost materials generally produced close to the area where they are used. Carbon black is excluded because it is manufactured from natural gas and more than 90 pct of the output is used in rubber; hence the factors for estimating requirements are easily evaluated. OVERALL GROWTH FACTORS Table I gives the population, retail sales, and value added by manufactures in the U. S. and in the eleven western states in 1954. These data are rough guides to the proportionate part of total U. S. markets for products containing mineral fillers that may be expected in a given area. For example, the population of the eight Mountain states in 1954 was 3.6 pct, and retail sales in these states were 3.8 pct of the U. S. total, but the value added by manufactures was only 1.3 pct of the U. S. total. On the other hand, the three Pacific Coast states, with 10.3 pct of the total population, had 12.0 pct of the retail sales and produced 9.6 pct of the value added by manufactures. On an industry-by-industry basis the correlation between the three guideposts will not be as close as shown in the 1954 data for the Pacific Coast states, but in the long-term view the continuing rapid population growth in the western states is certain to result in expanded industrial production at an even more accelerated pace, which will shorten the gap between local consumption and production in most major groups of manufactured consumer goods. Of course, there will always remain favorable areas for production of specific products. Such special situations must be individually analyzed. Fig. 1 compares the population trends in the U. S., the western states, and California with Real Gross National Product from 1910 to 1957, with forecasts to 1970. It is estimated' that the U. S. Real Gross National Product, as measured by the value of goods and

Jan 1, 1960

By C. W. Hamilton

In the production of crude petroleum for the year 1930 Venezuela again maintained its world rank of second only to the United States. During the latter months of the year Russia forged ahead of Venezuela in daily rate of production, and from the present outlook will probably rank second among the oil-producing countries of the world in 1931. It is now believed Venezuelan production has passed its peak. The producing fields of the Bolivar coastal district, along the east side of Lake Maracaibo, continue to be the principal source of supply. Such fields as Lagunillas, Mene Grande and La Pas were not produced to capacity throughout 1930. During the year, three new fields entered into commercial development: The Rio Tarra field in the District of Colon, State of Zulia; the El Mene de Salto field in the District of Acosta, State of Falcon and the Quiriquire field, District of Piar, State of Monagas. For 1930 the total crude production of Venezuela was approximately 137,424,000 bbl. as compared to 137,739,000 bbl. during 1929, or a decrease of 315,000 bbl. During the past year exports of crude from Venezuela amounted to 137,8.50,000 bbl. as against 130,044,000 bbl. exported during 1929. Crude oil in field storage decreased from 14,138,-000 bbl. at the beginning of 1930 to 9,600,000 bbl. as of Jan. 1, 1931— present crude stocks fill about one half the field tankage available. Drilling operations in the producing fields declined sharply but throughout the year there was maintained a satisfactory potential reserve in the shape of proven territory and closed-in producers. Of the 2555 wells which have been completed in Venezuela, 1571 wells were in production on Jan. 1, 1931. The status of these present producing wells may be classified as follows: flowing 652, pumping 170, gas-air lift 193 and closed-in 556. The ratio of closed-in wells to producing wells declined in 1930, while the number of wells produced by artificial means increased materially. In the Bolivar coastal fields there is now observed a marked decline in gas volume and well-head pressure. Lago Petroleum Corpn. and Venezuela Gulf Oil Co. each have under construction electric plants designed to generate power for pumping wells by electricity. The first units of these plants will be placed in conlmission in the early spring of 1931. Venezuela Oil Concessions, Ltd. has installed a number of stenrn-

Jan 1, 1931

By Albert H. Chester

During the summer of 1875 I visited some of the iron mines of Houghton County, Mich., and was quite interested to observe the progress made there within a few years. Working in open pits is gradually giving place to underground work in most of the mines where this system is practicable. In some cases, as in the Lake Superior Mine, the body of ore is so irregular, and the deposit so liable at any time to be pinched out, or nearly so, that it. has been found impractical, if not impossible, to lay out any plan for systematic underground work. But in many other mines the deposit is so regular in character, that the work can be laid out in shafts at regular intervals, and a series of 60 feet levels. The Michigammi Mine, opened in 1872, and first worked in 1873, is arranged on this plan, though some quarrying is still done. But the men are being put at overhead stoping as fast as it can be got ready for them, and before long it will all be worked in this way. The New York Mine is undergoing a similar change to the pillar system, and several others have either been changed, or it is about to be done. My principal object in visiting this region was to obtain samples from some of the important mines, so as to be able to answer the question: "What is the average percentage of iron in the Lake Superior ores?" Most iron furnaces work on mixtures of ore, so that it is impossible to tell, from their records, just the percentage in each one.

By Charles Albert Ashburner

Natural gas has been known to exist for many years in the St. Lawrence Valley, between Quebec and Montreal, and more partirularly in the vicinity of Louisville and Three Rivers, 74 and 94 miles respectively northeast of Montreal, and 98 and 78 miles respectively southwest of Quebec; the distance from Montreal to Quebec along the St. Lawreuce River being about 175 miles. It was not until 1880 that any practical explorations were begun with the hope of finding gas in sufficient quantities for commercial uses. In this year Messrs. Piret and Genest, of Three Rivers, sank a well near St. Maurice to a depth of 50 feet, where solid rock was encountered. A similar well was drilled through the glacial and allavial drift, in the same district, in 1883, by the Messrs. Renaud Freres and Dubois, to a depth of 70 feet before solid rock was encountered. In this latter well a strong flow of gas was obtained. The gas was an outflow from a very limited reservoir in the porous glacial gravel, which had been filled from the gas resulting from the decomposition of vegetable remains, which had been buried in the gravel at the time of its deposition. Subsequently, other wells were sunk in the same way, with the hope of getting gas in commercial quantities from similar reservoirs. Commercial Gas.—By gas in commercial quantities I mean gas in such quantity that, if utilized with proper care and economy, it would generate steam at a cost below the cost at which the same duty could be obtained from the use of coal or wood at current prices, and that

Jan 1, 1890

By J. J. Oberly

WHILE examining lineage boundaries in germanium single crystals as described by Vogel et al.,&apos; patterns of conical etch pits were noted which reveal interesting properties of dislocations. The crystals were grown by pulling in the <100> direction, and (100) surfaces perpendicular to the growth direction were etched 4 min in a mixture of 6 cu cm HF, 10 cu cm HNO3, 6 cu cm acetic acid, 3 drops Br,. Lineage boundaries extended in any direction, but favored the <110> direction. The patterns which were noted first were composed of two or three etch pits arranged symmetrically about the lineage boundary, so that the doublets were spaced equally on either side of the boundary line and the triplets had their center pit on the boundary line. The triplets occurred less often than did the doublets; occasionally combinations were found. Two such combination patterns are shown in Figs. 1 and 2. The orientation of the patterns was determined approximately by subsequently etching the same surfaces in a mixture of 5 cu cm HF, 5 cu cm super-0x01, and 20 cu cm distilled water which produced nearby random square etch pits having edges in the <110> direction. In all cases, the axis of symmetry was <110>, being parallel to the etch-pit edges. Several successive lapping and etching operations showed that the patterns tended to continue through the crystal in the <100> direction, but eventually changed or vanished. It can be seen in both photographs that the pits in the patterns are much further apart than the pits in the adjacent section of the lineage boundary. In Fig. 1, the 10 pits of the pat-

Jan 1, 1955

By Theron Wasson

The discovery of eight new oil fields, two of which may be of major importance, was the outstanding record in Michigan this year. These new fields have helped to support the declining production from old areas and place the total of 18,559,000 bbl. in line with the past six or seven years. Thus, it appears that Michigan is doing its part in maintaining the production of the country in the third year of the war. The new fields are in the central basin area where oil was first discovered in Michigan, thus tending to focus attention on the deeper part of the lower peninsula of the state. Through 1944 the state of Michigan has produced a total of 222,-641,580 bbl. of crude oil from 100 pools, many of which arc relatively small. Among the previous1y discovered fields Reed City is still the outstanding producer, with Fork, Headquarters, and Adams following in the order named. The Reed City pool produced a little over 5,000,00 bbl., which was more than one third of the state&apos;s total for the year. Almost two thirds of the year&apos;s total oil production came from fields discovered in the past five years. Maps A map of the oil and gas fields of Michigan in 1943, published in the A.I.M.E. report for 1944,* shows the main producing areas and should be referred to if information in regard to their location is desired. The producing zones are shown in the columnar section in the same publi- cation." The data in Tables I and 2 have been carefully &apos; checked and every effort has been made to show as complcte information as possible. New Discoveries and New Developments Eight new producing areas were discovered during 1944 which, in order of importance, are: Deep River Field.—The discovery well in the Deep River field was drilled by Don Rayburn and others, and should be listed as a chance discovery, as, from a geological standpoint, it was not considered favorable until oil was found at a depth of 2838 ft. in a dolomitic layer in the top of the Dundee limestone. The first well was completed in January 1944, with an initial production of 2500 bbl. By the end of the year 15 wells had been completed, proying an area 2 1/2 miles long and 1/2 mile wide. Coldttater Field.-The Coldwater field was discovered in August 1944, by the Sohio Oil Co. Production is from secondary dolomite at the top of the Dundee at a depth of 3703 ft. To the end of 1944 nine wells had been drilled on 40-acre spacing. Essexville Field.—Essexville field was discovered by United Drillers and Producers, Inc. Eight wells had been completed to the Dundee lime by the end of 1944, and prospects were good for further development during 1945. Hilliards Field.—Hilliards field was discovered by Cook and Fortney. Production is from the Traverse lime at an average depth of 1588 feet,

Jan 1, 1945

By C. S. Matthews, W. R. Strickler, M. Prats

To gain an insight into the deviations from normal behavior caused by dip. a mathematical study has been made of single-fluid five-spot floods in dipping reservoirs for flooding techniques likely to be employed in such cases. Streamline patterns and sweep eficiencies are computed for a number of different cases, and the results, where possible, are presented in graphical form. An increase in sweep efficiency can be obtained by moving the central injection well updip, and the opti~num position is found for several cases. The applicnhility of the results is discussed. INTRODUCTION Because of the growing importance of water flooding in California and in other locations where large angles of dip are quite common, it is important to know at least some of the effects of dip on the performance characteristics of water floods in such instances. In the past, only reservoirs having relatively mild dips have been wateflooded. Consequently, little is known today as to the effect of dip on the performance characteristics of a flooding operation from the point of view of field experience; and because of the complexity of the problem, little, if anything, has been done on the problem from the point of view of theory. There are two distinct aspects of the role played by gravity in a flooding operation. The first is that of the preferential segregation of the reservoir fluids at the time when the flood is to commence. The second is the role that it may play in affecting the performance of the reservoir during the course of the flooding operation. In this paper the reservoir is assumed to be filled with only one fluid, so that there is no preferential segregation of reservoir fluids at the commencement of the flood. Moreover, the injected and in-place fluids are assumed to have the same characteristics, so that in effect we consider only a single-fluid problem. Single-fluid results have been used as a guide in the past for predicting and interpreting the behavior of regular five-spot floods in horizontal reservoirs. It is thought that single-fluid results might likewise be used for five-spot patterns in dipping reservoirs as a norm to which the effects of the multifluid problems might he referred.* In confining our attention to the single-fluid case, we therefore do not consider the preferential segregation of injected water in the oil bank, or of the oil bank in the unflooded zone. Instead we consider the deviation from the behavior of a horizontal five-spot which is caused by use of flooding techniques (i.e., the flow potential pattern at injection and production wells) likely to be employed during flooding operations in dipping reservoirs. In other words, we consider effects which are caused by the pattern of injection and production well pressures which we choose to apply. Performance characteristics are given for the five-spot spacing pattern as a function of two parameters; one is the ratio of gravity head to potential difference bctwccn the high updip injection well and the low downdip producer of the same five-spot, denoted by Rg; the second is the orientation of the five-spot pat-

Jan 1, 1956

By Theron Wasson

The discovery of two new fields—the Reed City area of Osceola County and the Headquarters field, of Roscommon County —and the important development in Winterfield township, Clare County, again demonstrate the fact that it is the unknown and unexpected that enter very definitely into the oil-producing history of Michigan. This is particularly true in the area of thick glacial drift in the north central part of the state, where the new prolific fields have been discovered this year. This shifts the interest from the southwestern part of the lower peninsula, where a number of pools were rapidly developed during 1939 and 1940, back into the Central Basin area. As a result of strict proration in the new areas, the production for the state of Michigan for the year has not been as great as in 1940 or 1939. In 1941 the total production was 16,300,000 bbl., in 1940 it was 19,551,000 bbl., and in 1939, which was the peak year, it was 23,300,000 bbl. However, the discovery of the new fields this year nearly doubles the estimated reserves for Michigan reported at the end of 1940 In 1941 about 12,000,000 bbl. of oil was produced from the older fields, in which the individual well productions were so small that proration was not an important factor. The total production for the state from the discovery of oil in 1925 through 1941 now stands at 161,205,000 barrels. ActIVe Oil Fields Reed City Field.—In the Reed City field, Lincoln township, Osceola County, only small oil wells were completed during 1939 and 1940. The discovery of much larger production in wells drilled somewhat deeper, by The Pure Oil Co. and the Weber Oil Co., in the early part of 1941, led to the rapid development in this area. Some wells have had initial productions as high as 10,000 bbl. By the end of the year III producing wells were completed, with an average depth of 3600 ft., from the Detroit River formation of Devonian age. The entire development of the field to the end of 1941 was on 20-acre spacing. Headquarters Field.—The Headquarters field, which lies along the line between Clare and Roscommon Counties, was one of the most important discoveries of 1941 and will be the scene of vigorous development during 1942. Production so far has been from the Traverse lime at about 3400 it., and development has indicated that this is probably one of the most productive Traverse pools yet discovered. One well had been given a potential of 10,000 bbl. per day. Dry holes well located in relation to big producers indicate that it is a typical Traverse development. Winterfield Field.-This field, in Winter-field township, Clare County, was discovered late in 1940. By December 1941, 14 Dundee and 5 Traverse producers had been completed. The Dundee lime is found at a depth of 3750 it. and the Traverse lime at 3070 it. Producing conditions in the Dundee seem to be erratic because of varying porosity in the dolomit-ized limestone. Kawkawlin Field.—The Kawkawlin field, which was discovered by the Gulf Refining Co. in 1938, is in Monitor and Kawkawlin townships, Bay County. Small production

Jan 1, 1942

By Theron Wasson

The discovery of two new fields—the Reed City area of Osceola County and the Headquarters field, of Roscommon County —and the important development in Winterfield township, Clare County, again demonstrate the fact that it is the unknown and unexpected that enter very definitely into the oil-producing history of Michigan. This is particularly true in the area of thick glacial drift in the north central part of the state, where the new prolific fields have been discovered this year. This shifts the interest from the southwestern part of the lower peninsula, where a number of pools were rapidly developed during 1939 and 1940, back into the Central Basin area. As a result of strict proration in the new areas, the production for the state of Michigan for the year has not been as great as in 1940 or 1939. In 1941 the total production was 16,300,000 bbl., in 1940 it was 19,551,000 bbl., and in 1939, which was the peak year, it was 23,300,000 bbl. However, the discovery of the new fields this year nearly doubles the estimated reserves for Michigan reported at the end of 1940 In 1941 about 12,000,000 bbl. of oil was produced from the older fields, in which the individual well productions were so small that proration was not an important factor. The total production for the state from the discovery of oil in 1925 through 1941 now stands at 161,205,000 barrels. ActIVe Oil Fields Reed City Field.—In the Reed City field, Lincoln township, Osceola County, only small oil wells were completed during 1939 and 1940. The discovery of much larger production in wells drilled somewhat deeper, by The Pure Oil Co. and the Weber Oil Co., in the early part of 1941, led to the rapid development in this area. Some wells have had initial productions as high as 10,000 bbl. By the end of the year III producing wells were completed, with an average depth of 3600 ft., from the Detroit River formation of Devonian age. The entire development of the field to the end of 1941 was on 20-acre spacing. Headquarters Field.—The Headquarters field, which lies along the line between Clare and Roscommon Counties, was one of the most important discoveries of 1941 and will be the scene of vigorous development during 1942. Production so far has been from the Traverse lime at about 3400 it., and development has indicated that this is probably one of the most productive Traverse pools yet discovered. One well had been given a potential of 10,000 bbl. per day. Dry holes well located in relation to big producers indicate that it is a typical Traverse development. Winterfield Field.-This field, in Winter-field township, Clare County, was discovered late in 1940. By December 1941, 14 Dundee and 5 Traverse producers had been completed. The Dundee lime is found at a depth of 3750 it. and the Traverse lime at 3070 it. Producing conditions in the Dundee seem to be erratic because of varying porosity in the dolomit-ized limestone. Kawkawlin Field.—The Kawkawlin field, which was discovered by the Gulf Refining Co. in 1938, is in Monitor and Kawkawlin townships, Bay County. Small production

Jan 1, 1942

By Margaret V. Doyle, R. W. Powers

INTERNAL friction measurements, carried out as functions of temperature, have been used extensively to obtain data on the mobility of interstitial impurities in the Group V metals, vanadium, colum-bium, and tantalum. For a given frequency of vibration, the internal friction peaks at a temperature which depends principally on the particular metal and interstitial impurity. Relaxation times and corresponding activation energies are determined from a knowledge of such peak temperatures for various vibration frequencies. These experimentally determined relaxation times are related to the average jump frequencies of the interstitial impurity atoms using the model of Snoek1 and can be related to macroscopic diffusion coefficients as shown by Polder.2 In these Group V elements, the impurity whose diffusion rate has been the hardest to pin down by the internal friction technique has been carbon. The experimental difficulties associated with carbon in these metals were not evident in the earliest investigation carried out by Ke on tantalum.3 The carbon peak was thought to occur near 140°C at 1 cps on the basis of the enhancement of the height of this peak measured on specimens which had been coated with colloidal carbon and heated in vacuo at 1200°C. Presumably on the basis of similar evidence, Wert identified a peak also near 140°C at 1 cps in columbium with the diffusion of carbon in that element." Later, the difficulties of admitting carbon into these metals without simultaneously introducing oxygen were pointed out by Ang and Wert- nd by Marx, Baker, and Sivertsen.6 The latter suggested that the peaks attributed to carbon in tantalum and columbium might arise from the presence of traces of oxygen, adventitiously absorbed during the carburization. Such suspicion was confirmed, at least in tantalum, when it was found possible to prepare C-Ta specimens without contamination by oxygen. Specimens sci prepared, aitnough high in carbon content, gave no evidence of a damping peak near 140°C.7 Recently, the authors were able to Show that carbon diffuses in tantalum at a rate only slightly slower than that for nitrogen.8 At 1 cps, the carbon peak lies at 34g °C, only a few degrees above the nitrogen peak at 341 °C. However, the two could be distinguished by a different stability with respect to aging at 400 °C and by a different dependence of peak height on solute concentration. On the basis of this experience with tantalum, it appeared worthwhile to search also for a carbon peak in columbium in the vicinity of the nitrogen peak." In this report, the location of the carbon peak in columbium is made known and its position relative to the nitrogen peak is compared with the authors&apos; previous findings in tantalum. In addition, a second source of internal friction seen only in specimens of very high purity is discussed. Columbium was obtained from the Fansteel Metallurgical Corp. as either 30 or 40 mil diam stock. The manufacturer gives the following analysis as typical of this material: 99.4 pct minimum Cb, 0.10 pct maximum C, 0.5 pct Ta, 0.04 pct Ti, 0.02 pct maximum Si, and 0.01 pct maximum Fe. Wires 13 in. long were degassed near 2200°C for 4 to 16 hr in an ultimate vacuum better than 2.10" mm Hg in an apparatus described previously.8 This treatment reduced the oxygen and nitrogen damping peaks observed in the as-received material to less than 0.0001 in Q-1 above background. The latter value varied somewhat from specimen to specimen in the range 0.0004 to 0.0008, depending chiefly on the wire diameter and the frequency of vibration. The high temperature evacuation left the specimen in a rather soft condition, the Vhn being reduced to 40 from a value near 121 in the as-received conGi~iur~. The gram size was about the diameter of the specimen. After outgassing, specimens were loaded with carbon by absorption of such hydracarbons as methane or ethylene. Carbon was also added to a few speclrnens by heating them at

Jan 1, 1958

By Paul Rhedey

Various commercial pelroleum cokes were heat-1,reated at temperatures between 500° and 1500°C, in a nitrogen atmosphere, in laboratovy induction furnaces. The rate of tenlperature rise was varied betzveen 10" and 300°C per min, or the green cokes were flash-calcined, orv a combination of heating rates was used. Changes in the rate of heating had only negligible effects on the degree of&apos; calcination as characterized by mean crystallite thickness and the chemical properties of the calcined coke. The physical structure of the cake was however significantly affected when rate of heating during calcination exceeded 50°C per min over the temperature range of 600° to 900°C. Surface-accessible porosily increased with the .rate of temperature rise, and this was accompanied by a change in pore size distribution. Source and properties of the green coke also had an influence on the structure of the calcined coke. The evidence presented suggests a similar mechanism of porosity development in petroleuiiz coke during calcination in industvial equiplnenl, such as rotary kilns. An increase in surface accessible povosity incveased the pitch binder requirement when the coke was used as aggregate in Soderberg paste. A correlation was established between calcined coke porosity and paste binder requiremenl. ManY results have been published on the changes of properties of petroleum coke during calcination, such as chemical composition, real density, electrical resistivity, crystallite and pore structure. The correlation of these properties with temperature of calcination and time at maximum temperature has been rather well established in both laboratory and pilot plant experiments. Surprisingly little attention has been given however to the effect of calcination conditions, such as rate of temperature rise or furnace atmosphere, on the chemical and structural properties of the calcined coke. It has been observed that petroleum coke, when calcined in industrial equipment, acquires higher porosity and lower real density than those attainable in laboratory furnaces at apparently identical calcina- tion temperature and soaking time. This paper describes a study of the effect of rate of heating during calcination on calcined coke properties using green petroleum cokes of different volatile matter, hydrogen, and sulfur content. An attempt was made to correlate the changes in coke structure with the flowability of anode paste of the type normally used in aluminum reduction cells. EXPERIMENTAL Petroleum Cokes Used. In the study of release of volatile matter and sulfur during calcination and the effect of rate of heating on calcined coke properties two delayed cokes of different sulfur contents were used. The results of analysis of the green cokes are given in Table I. In the study of the effect of flash calcination thirty-six commercial petroleum cokes from twelve different refineries were used with a range of properties shown in Table 11. Calcination Conditions. Calcination experiments were carried out in a laboratory induction furnace. In each run a 200-g sample of dry green coke sized to 10 by 65 Tyler mesh was calcined in a graphite crucible. The crucible containing the sample was placed in the middle of a stack of eight others filled with metallurgical coke to reduce temperature gradients within the sample. Temperature was measured by two Pt, Pt-10 pct Rh thermocouples and controlled by a Celectray instrument. The two couples generally agreed within 5°C. In the study of volatile matter and sulfur release the samples were heated to temperatures in the range of 500" to 1500°C at a rate of 10°C per min in a nitrogen atmosphere and held at the final temperatures for 30 min. In the study of the effect of heating rate on calcined coke properties the desired rates between 10&apos; and 300°C per min were obtained by manually adjusting the power input. Flash calcination was carried out by dropping 100 g of the green coke into the graphite dish preheated to the calcination temperature. Because of the small heat capacity of the furnace the coke was introduced in 20-g portions at a time. For this purpose a 2-in.-long nipple between two 1-in. gate valves installed on the top flange of the furnace served to provide a gas seal while feeding coke to the furnace. It was estimated that the temperature of the coke reached that of the furnace at a rate of approximately 1000°C per min. Holding time at final temperature was also 30 min. Calcined Coke Proper- Determined. Porosity was determined on 20 by 35 Tyler mesh samples using an Aminco-Winslow mercury pressure porosimeter with an operating range of 1.8 to 3000 psi absolute pressure (100 to 0.05 p pore diameter range).&apos; Apparent density was obtained by the mercury poro-simeter. It represents a particle density of the 20 by

Jan 1, 1968

By H. P. Rassbach, E. R. Saunders

MUCH progress has been made in recent years in the theory and practice of making stainless steel. By effective utilization of oxygen for decar-burization and more suitable alloying agents, it has been possible to attain consistent production of very low-carbon stainless steel. In order to facilitate economical production of stainless steels, the Electro Metallurgical Co. has carried out an extended experimental program that has clarified some of the complex interrelations of temperature and composition under decarburizing and reducing conditions. These results&apos;-:&apos; have been founded in large part on small experimental heats, and in order to confirm their validity and significance under commercial conditions, a survey of stainless steel melting practice has been made with the cooperation of stainless steel producers. Conditions required for decarburization and associated oxidation of chromium, manganese, and iron have been fairly well established in relation to the beneficial effect of the highest practicable temperature. The recovery of chromium and manganese from highly oxidized slags by reduction with silicon has been indicated with somewhat less precision and this study has shown significant deviation in large commercial heats from the small experimental heats. In spite of an unsatisfactory degree of accuracy in estimating the conditions affecting reduction of metallic values, it has been possible to calculate a slag weight in reasonably good agreement with the results observed in large heats. While there still is much to be learned about both the qualitative and quantitative aspects of stainless steel melting, this survey has indicated the manner by which the efficiency of the production process may be measured. Oxidation Period In order to establish practices for the recovery of chromium and manganese from the slag the amounts of these metals oxidized should be known. Moreover, since reduction of oxidized chromium and manganese must necessarily be accompanied by similar reduction of iron, knowledge of the total quantity of metallics oxidized is essential. The relations between carbon, chromium, and temperature under oxidizing conditions were developed by Hilty in 1948.&apos; While it had been realized previously that retention of chromium in the metal during carbon oxidation is favored by high temperatures, the Hilty relation provided quantitative information useful for evaluating melting procedures. For example, it was shown that decarburization to moderate carbon levels can be achieved while retaining substantial amounts of chromium. However, in decarburizing to the low-carbon level necessary for producing 0.03 pct maximum carbon stainless steel, very little chromium remains in the bath at the temperatures generally employed. For this reason, Hilty, Healy, and Crafts&apos; later projected an extension of the chromium-carbon relation to the low-chromium region. Although this chromium-carbon-temperature relation defined the composition of a chromium steel bath at the end of the oxidizing period, it did not provide a direct means for estimating the total amount of metallic oxidation occurring during decarburization of a stainless steel heat. This subject was investigated by Crafts and Rassbach³ and, later, by Hilty, Healy, and Crafts" who demonstrated that metallic oxidation is a function of the chromium content of the initial furnace charge, the minimum carbon content attained, and the temperature. It was further demonstrated from data on 1-ton heats that an empirical relationship exists between the ratio of chromium plus manganese to iron in the slag (S) to the corresponding ratio of these components present in the metal bath. The following expression was derived to permit the calculation of the amount of metallics oxidized during decarburization of a given charge: W-2000 (Cr1 + Mn1)-(Cr2 + Mn2) 1 100s/s+1-(Cr3 + Mn2) where W is the pounds of chromium, manganese, and iron oxidized per ton of charge; Cr1, the percentage of chromium in the charge; Mn1, the percentage of manganese in the charge; Cr2, the percentage of chromium in the bath after oxidation; Mn2, the percentage of manganese in the bath after % Cr + % Mn oxidation; and S =%cr+ % Mn/%Fe in the slag after %Fe oxidation. In order to establish whether the slag ratios of commercial heats are consistent with those found in the experimental heats, the slag and metal analyses shown in Table I were evaluated. These data represent samples taken after the oxidation of two 1-ton and seven 15 to 25-ton heats of types 303, 304, and 304L stainless steel made in chromite, acid, and basic hearths. Fig. 1 illustrates that the results for the commercial heats correlate reasonably well with the relationship originally established for experimental 1-ton heats. It will be noted that in the range of metal composition of these heats, the slag values generally lie above the line. As was suggested by

Jan 1, 1954

By E. C. Wright

FOR many years the cost of making pig iron and steel in the Birmingham district has been about the lowest in the United States. The close proximity of the important raw materials such as coal, iron ore, limestone, and the large available scrap supply made it possible to assemble all of the important ingredients necessary for steel-making with only nominal costs for transportation. Both iron ore and coal were being mined in this district at one time for about $1 per ton from underground operations. At that time mining wages were low everywhere and the labor rate in the South was considerably below that of other mining districts. This situation persisted until the emergence of labor unions as an economic and political force, emigation of southern labor to northern plants, and continued growth of industry in the South in the years following the depression of 1932. Since that time union organizing of miners and steel workers throughout the nation has increased labor costs in mining and steelmaking. This influence has been felt particularly in underground mining operations since the proportion of labor cost to total cost is still high. The previous advantage in basic labor rate in the South has been almost entirely eliminated by the equalization of labor rates in basic industries by national unions.

Jan 12, 1950

By Carl S. Westerberg

1,. C. McCABE*-—An increased derliand for coal in the west is to be expected because of the growth in population and industry during the past ten years. The author calls attention to the increased mechanical cleaning of Utah coal between 1938, when no cleaning was being done, and 194.7, when more than 24 pct of the production was cleaned. This is essentially the Period of most rapid growth of the Pacific Coast. area altliough the growth and, no doubt, the general trends in coal production and cleaning continued at a less accelerated rate during 1948. The Pacific southwest increased 37 pct in population between 1940 and 191.7 while the United States showed only a 7 pct increase in the same period. it has been estimated that there will be an additional 15 pct increase in population between 1947 and 1950. The conclusion that more coal and more mechanicak cleaning capacity will be required appears to be well founded. Mr. Westerberg discusses the cco- nomic advantages of coal cleaning reflected in freight savings, in lower cost per million Btu, and lowered ash and sulphur content. In view of the limited occurrence of coking coals in the west it would be interesting to know whether significant beneficiation in coking strength can be expected from mechanical cleaning of Utah coals. This has been demonstrated for some eastern and midwestern coals. One can readily agree to the desirability of recovering the fine coal that has heretofore been lost in washery slurry. The very cheapness of coal has Iridered

Jan 1, 1950

By H. A. Davies

DURING a current program of research on the structure and properties of liquid sodium alloys, the need arose for information on the solubilities as a function of temperature of several B subgroup metals in liquid sodium. In the absence of reliable information in the literature for several of these systems, par- ticularly at temperatures in the range 100° to 300°C, an apparatus was constructed to determine solubilities by a direct melt-sampling technique, followed by wet-chemical analysis for both sodium and the solute metal. The details of the technique have been described previously.&apos; The solubility of indium in liquid sodium was determined at eight temperatures in the range 100° to 270°C. The solubility as a function of temperature is shown on Fig. 1; this represents the liquidus line over this composition range. A cooling curve was plotted after the completion of the sampling and an arrest was observed at 94.9°C which must be interpreted as being the result of a eutectic reaction. By extrapolation of the liquidus to this temperature, the eutectic composition was estimated to be about 0.25 at. pct In. The present estimate of the eutectic temperature and composition are in good agreement with the values of 96.0° to 96.2°C and between 0.28 and 0.45 at. pct In, respectively, which were reported by Heycock and Neville.2 However, no further information on the liquidus of this system at the sodium-rich end could be found in the literature for comparison. One compound: NaIn, has been reported in this sys-

Jan 1, 1968

By N. N. Breyer

A specially built "hard" tensile machine with characteristics permitting the precise detertnination of the drop of the load at the yield point has been used to study the magnitude of the yield-point phenotnenon in prestrained martensitic 4340 steel. A new phenonzenon, the appearance of a secondary yield point, has been observed by holding the specimen at constant strain in the plastic region. Furthermore, it has been found that a series of yield-point drops could be introduced by successive constant strain holds in the plastic region. The isothermal kinetics of the development of the secondary yielding point lave been studied at four temperatures: 24° 0° -18°, and -79°C. From the results of the kinetic investigation, equations for the In a previous investigation1 it was shown that, contrary to generally held opinion, steels of medium carbon content, such as 4340, 4140, and 86B30, in the as-quenched martensitic condition, can be cold-drawn through a die with reductions in area of up to 10 pct without cracking. Tensile specimens of 4340 machined from bars quenched and prestrained in this manner exhibited tensile strengths of about 400,000 psi coupled with 30 pct reductions in area. In addition, it was found that each sample of such steels exhibited a yield point in the quenched, cold-drawn condition. Since these studies were conducted on a commercial hydraulic testing machine of a type which is not well-suited to detailed study of yield-point behavior, it was decided to study this phenomenon more thoroughly on a rigid straining machine. In this new investigation, use of such a "hard" machine not only allowed study of the magnitude of the yield-point drop but also revealed a new phenomenon—secondary yielding of the martensite introduced by stopping crosshead motion after plastic deformation of the sample had begun. The present paper is a report of these findings. MATERIALS AND PROCESSING The material used was a commercial 4340 steel of the composition shown below: 0.41 0.80 0.013 0.019 0.31 0.85 1.76 0.28 1 0.42 0.77 0.015 0.024 0.30 0.84 1.69 0.28 0.08 2 1 = Ladle analysis. 2 = Laboratory analysis. Bars of this steel were processed in the following way: 1) machined to predetermined diameters; 2) austenitized at 870°C for 1 1/2 hr; 3) oil-quenched; 4) cooled to -115°C for 1/2 hr; onset and increase in magnitude of the secondary yielding in this temperature region have been found to fit the relationship ?Ys = Atn where ?Ys is the magnitude of the secondary yield Point in psi, t is the time in seconds, and A and n are parameter characteris-tics of the material. Although the occurrence of the primary and secondary yield points could be rationalized qualitatively on the basis of stress-induced ordering of carbon atoms in the stress fields of dislocations, as postulated in an earlier paper, the kinetics of the secondary-yield-point development were interpreted to indicate that the ordering involves more than just single jumps of carbon atoms from high-energy to neighboring low-energy sites. 5) pickled and lime-coated; 6) drawn through a carbide die. The predetermined diameters were chosen so that drawing through the same die gave the various reductions desired. Tensile specimens of 0.252 in. diam with a 1 1/4 in. gage length were then prepared from the drawn bars and tested. In order to study the stress-strain behavior at the yield point in detail, a rigid tensile machine with a high spring constant was constructed. Columns of large cross section (relative to the specimen cross section) constituted the machine frame. A dc motor was used to drive a screw via a gear reducing train and a "crane" thrust bearing. In this relatively simple device small deformations could be observed un-blurred by the slow response and lower spring constant inherent in hydraulic machines.&apos; A strain-gage dynamometer permitted load changes as small as 8 lb to be read. RESULTS Tensile test samples machined from bars in the as-quenched condition with no subsequent drawing and samples from bars with 3.8 pct reduction after quenching gave stress-strain curves typified by those shown in Figs. I and 2. The time lapse between predrawing and tensile testing varied but usually ranged between 3 to 6 days at room temperature. The strain rate during testing was 0.003 in. per in. per min. The as-quenched curve is seen to have a broad serrated maximum whereas the stress on the specimen prestrained 3.8 pct rose linearly to point A, Fig. 2, fell abruptly to B, and then gradually to C. The abrupt drop to B was accompanied by evidence of incipient necking. The drop of the stress at the yield point in the prestrained samples (A to B in Fig. 2) changed with the percent prestrain, as illustrated on Fig. 3. Although the tensile strength increased continuously with the amount of previous cold drawing, the magnitude of the yield point drop first increased—up to about 6 pct prior reduction—and then decreased. Specimens from bars predrawn more than 8 pct broke in a brittle fashion in the elastic portion of the stress-strain curve.

Jan 1, 1967

By Lars Thomassen, Ernest Kirkendall, Clair Upthegrove

THE amount of research done in the last few years on the subject of diffusion in solid metals is significant of the importance of this problem. To review the literature dealing with diffusion is unnecessary here. Desch1 in 1912 reviewed the work that had been done on diffusion in solids and gave a bibliography of the literature published before that time. Mehl&apos;s paper in 19362 is an excellent review of diffusion in metals and contains a large bibliography. Of importance also for its review and bibliography is an article by A. I. Krynitsky.3 While considerable material has appeared in the literature on diffusion in brass, the amount of information is not great compared to that pertaining to some of the other alloys. Most of the information published is of a qualitative nature; that which is quantitative varies considerably. Thus the quantitative determination of the rates of diffusion of copper and zinc in alpha brass by a new method appeared worth while. In the present investigation the rate of diffusion of zinc in approximately the same composition alpha brass has been determined at three temperatures. PROCEDURE The method used consisted of plating copper on a beta brass, heating it to allow diffusion to take place, and measuring the concentration of copper by determining the lattice constant of the alloy. This method is unique in that it uses a beta brass of such a composition that at the temperature at which diffusion takes place the beta brass is saturated with copper. Thus, while the beta brass supplies the zinc, no diffusion takes

Jan 1, 1938