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By D. A. Reynolds

The Bureau of Mines-American Gas Association survey of the carbonizing properties of American coals was begun in 1929, and has been continued almost without interruption since that time. Upwards of 100 coals have been carbonized at low, medium, and high temperatures in this survey, and about 200 additional coals have been carbonized at high temperatures only. All survey coals were blended with coal of different rank for carbonization at one high temperature (900° C,). During the past few years, 12-high-volatile A coals were blended with Pocahontas No 3 coal from Kimball, McDowell County, W. Va., and in this report the physical properties of the cokes from these high-volatile coals and their blends are compared.

Jan 1, 1949

By Russell R. Trengove

In order to extend or delimit the known ore reserves adjacent to the Comet Coalition property on the western slope of the Highland Peak Range about 8 airline miles west of Pioche, Nev., the Bureau of Mines undertook an exploration project of diamond drilling. Production figures from this property, formerly known as the Schodde, are not available, but it has been reported that small amounts of rich silver and gold ore were Shipped by wagon to a smelter in the Salt Lake valley during 1900-1910. Small shipments were reported for the period 1915-1927, also. A study of the Pioche District by the Federal Geological Survey in 1942 and 1943 was the basis for the exploration program of the Bureau of Mines in 1947 This program consisted of diamond-drilling three holes. The total footage was 2,967 feet. No. 1 hole was drilled 1,260 feet, a record depth for diamond drilling in the Pioche District. Silver-bearing lead-zinc sulfide ores are found in the Combined Metals limestone, known locally as the C.M. bed, These deposits have been formed by replacement of the limestone that is inclosed in the Pioche shale.

Jan 1, 1949

By W. A. Lang

Introduction Under our present civilization, industrial developments will be greatest in those areas in which energy .can be most economically produced and efficiently used, where labour is in adequate supply, and where markets for the products of industry are available. A knowledge of fuels- the present major sources of energy- and of their utilization is therefore of vital importance. With that in mind, the aim in this paper will be to outline the known reserves of fuels in Alberta, to give their characteristics, to indicate the markets served by each, and to offer some suggestions for the future development of the coal industry. The paper should be regarded as a compilation of published data rather than as an original treatise. Alberta is richly blessed by having large reserves of mineral fuels. The estimated reserves of coal are 46,562 million tons. Alberta is the oil and gas province of Canada. The world's largest deposit of bituminous sand occurs along the Athabaska river in Alberta. In addition, there are large areas of forested land in the northern and western sections of the Province, and the rivers serve for the development of hydro-power.

Jan 1, 1949

By Cleo Griffith Rall

The method for determining the effective porosity, of oil- and gas- bearing sand described in this report is a development of an earlier method devised by Bureau of Mines. The apparatus has been improved and made more convenient to use, but the procedure has been in use for many years without essential changes. A tabulation at the end of the report gives the results of more than 2,000 porosity determinations for oil sands in the fields of 13 states. A selected bibliography of articles containing descriptions and evaluations of various methods of determining porosity Is a. part of this report. The method was devised and developed at the Petroleum Experiment Station at Bartlesville, Okla., as part of the Bureau's research on fluid-energy relationships and ,on methods of improving the recovery of crude oil from underground reservoirs.

Jan 1, 1949

By R. W. Geehan

The Yellow Pine zinc-lead mine, situated about 3-1/2 miles northwest of Goodsprings, Clark County, Nev., was explored by core drilling during the fall of 1942 and the summer and fall of 1944 by the Bureau of Mines in cooperation with the Federal Geological Survey. The Yellow Pine district was located in 1855. The original claims covering the Yellow Pine mine were located in the following years: Rover, 1892; Hilo, 1897; Bybee, 1900; Radio and Como, 1906. The mine was operated by the Yellow Pine Mining Co. from 1906 to 1929. This company was dissolved in 1935. At a later date, S. E. Yount and the Security First National Bank of Los Angeles, Calif., acquired ownership of the mine. Since 1939, the mine has been operated in a small way by leasers. Production has been at least 175,000 tons averaging about 10 percent lead and 25 percent zinc, with a gross yield of $5,785,174. Virtually all ore produced by this mine consisted chiefly of oxidized zinc and lead minerals and came from long, pipelike shoots in the 100-foot thick Yellow Pine limestone. Ore shoots are sharply defined; elsewhere, the limestone is nearly barren. Numerous faults cut the mine into blocks. Ore is now mined in an open stope, but in the past, large tonnages wore mined in stopes by square-set methods. Ore produced recently was shipped direct to smelters unprocessed; in the past, it was milled by gravity and produced separate lead and zinc concentrates.

Jan 1, 1949

By Paul Hammond

Abstract The Allard Lake ilmenite deposits, which are currently being developed on a large scale, occur as a series of dykes or lenticular, flat-lying bodies within the northeastern part of a large, oval shaped anorthosire mass of Precarnbrian age which lies with its long axis paralleling the gulf of St. Lawrence. The Lac Tio deposit, discovered by Kennco Explorations, Limited, in 1946, is the largest body of titanium ore of its type now known in the world. It contains upwards of 112,000,000 short tons of ilmenite ore averaging 32 per cent TiO2 and 36 per cent Fe. The ore is an aggregate of ilmenite with oriented microscopic blades of hematite. The deposits appear to be high temperature, late magmatic injections containing only a small amount of volatiles, and bear a genetic relationship to the anorthosite rocks in which they occur. * * * Introduction Recent developments on the ilmenite deposits in the Allard Lake district of Quebec indicate the probability of a major industry, and one which may make Canada the world's greatest producer of titanium pigments and, ultimately, of titanium metal. The presence of ilmenite in this district was first reported by the Quebec Department of Mines following a reconnaissance shore-line geological survey in the year 1941. The ensuing report by Retty describes the occurrence of a number of small ilmenite lenses about the shore of Allard lake and' along two smaller lakes in the vicinity. These showings were later staked by Toronto and Montreal interests who carried out a certain amount of development work, and were described in more detail by Longley for the Quebec Department of Mines. The claim groups were later optioned by Kennco Explorations, Limited, Canadian subsidiary of Kennecott Copper. None of the deposits in themselves constituted a sufficiently large body of ore to warrant the major construction expenditures necessary for their exploitation on a profitable basis. The surrounding anorthosite areas, however, were considered favourable for the possible occurrence of other ilmenite deposits

Jan 1, 1949

By T. W. Guy

The increased moisture due to water-spraying for coal dust control is of interest even for mines from which the coal is to be wet-washed before screening, because in many cases wet coal dust materially de- 20-mesh X 0 sizes as pct ROM average ............................... 6.3 pct Range 2.3 to 9.5 pct 20-mesh X 0 sizes as pct 3/8 X 0 sizes average........'...................... 18.9 pct Range 12.7. to 23.9 pct creases the loading efficiency of men and equipment at the faces. It also causes a serious increase in the normal wear and deterioration of all equipment with which it comes in contact. It is important to the consumer if it increases his as-received moisture. No attempt will be made in this paper to cover the entire subject of water-spraying of coal for dust control. It will be confined to discussion and data on (I) percentages of dust in bituminous coals, (2) moisture increases due to spraying for dust control in mines or plants by methods which have proved satisfactory for periods of one to five or more years, and (3) a few suggestions for research. Size and Percentage or Coal Dust The U. S. Bureau of Mines1 classifies as coal dust all bituminous coal passing a 20-mesh sieve (0.0328 in. square opening). The percentage of such dust to be found in ROM coal, of course, varies widely with the characteristics of the seam, and with the methods used in the mining and in the preparation of the coal. ROM screen analyses of 12 U. S. coals selected at random from personal files given in Table I show: A few other screen analyses examined indicating 40 pct or more of 20-mesh X 0 dust in 3/8 in. X 0 sizes were not included because of uncertainty that they were representative. The number of results in Table I is not sufficient to give a reliable estimate of the average, or of the range to be expected, but it indicates that in every case the coal dust is a relatively large percentage of the total ROM coal, and, of course, a progressively larger percentage of resultants as the larger sizes are separated for marketing.

Jan 1, 1949

By F. S. Wartman

This paper gives an account of the production of ductile-grade titanium powder in 100-pound batches by reduction of purified titanic Chloride with magnesium, grinding, leaching, and magnetic-separation of the reaction product. Apparatus, technique, and methods of controlling product quality are described and some data on operating costs are given.

Jan 1, 1949

By W. J. Blackstock

Introduction To The great majority of people, the term 'strip coal' has little or no meaning, or if it has any significance it is thought to refer to a poor grade of coal that had to be accepted during the war because no other fuel was available. Few people in the Province of Alberta realize the magnitude of our coal stripping industry, and fewer realize that strip coal has been available to domestic consumers for at least forty years. Among the first in the field of strip coal mining in Alberta were the Tofield Coal Company, Ltd., and Sterling Collieries Company Ltd. It was not until the advent of World War II, with its huge drain on industrial and domestic coal sup? plies produced by the underground mines, that some other source of coal was seriously sought. The tremendous shortage of manpower du ring this period of National emergency made it imperative that any increase in the coal production must be procured on a high tonnage per man-hour basis. It was therefore natural that the highly mechanized strip mine should be eagerly encouraged and subsidized by the Governmental agency - the Emergency Coal Production Board - under the very able direction of Mr. G. A. Vissac.

Jan 1, 1949

By L. E. Djingheuzian

Introduction Cylindrical grinding mills have been used for a long time, but during many years of testing no methods were established that gave consistent results. The work by both scientific investigators and operators led very often to contradictory conclusions, and each millman was very much 'on his own' when trying to find the limits for working of his ball-mills. Fred C. Bond, in the introduction to his paper on Wear and Size Distribution of Grinding Balls, freely states that the mathematical immaturity of the grinding process "is the cause of many inefficient designs and installations as well as of much poorly oriented experimental work", and evidently he sees the solution of all our grinding problems in the discovery of the fundamental laws "which can change the empirical art into a mathematically exact science". While the writer is in complete agreement with Mr. Bond that grinding is governed by fundamental laws which can be expressed by mathematical formulae, there are so many variables in grinding, all interwoven with each other and mutually influencing each other, that the coalescing and merging of all these variables into a harmonious mathematical whole appears to be a homeric job. However, a light appeared on the horizon when it was proposed that power be used as an index of the grinding operation. It is pertinent to quote Gow, Guggenheim, Campbell, and Coghill from their paper on Ball Milling, in which they say: "Much of the past literature devoted to the subject has been concerned with the Kick-Rittinger dispute over evaluating grinding, or with dissertations on ball paths and the closely allied impact versus attrition hypotheses or with the exclusive consideration of certain specific variables, such as mill speed or circulating load, irrespectve of the other factors in operation. Such subjects may be dismissed with but little discussion in what may be called, by comparison a new philosophy in the stud of ball milling. Briefly this 'new philosophy' consists ' of using power as an index of the mill operation, and investigating grinding from the standpoint of set and induced variables with emphasis on the latter". But it is safe to assume that it was the work by E.W. Davis, H. E. T. Haultain, F. C. Dyer, A: M. Gaudin, J. Gross, S. R. Zimmerley, and others, that cleared the path for the authors of Ball Milling and induced them and A. W. Fahrenwald to look farther afield and thus to establish a far-reaching relationship between the power and capacity and the diameter of the ball-mills.

Jan 1, 1949

THE book covers principally the assaying of silver and gold and the determination of these values in ores, sweepings, and base metal. It seems to have been written more for the goldsmith and jeweler than for the primary producer of metals. There were approximately sixty different substances needed in the operations described and not over a dozen different types of raw material (ore, matte, crude or alloyed metal) are mentioned. The methods of separation used were essentially simple and reasonably reliable, though the processes were not sufficiently understood to permit the selection of the simplest effective ingredients, and there was a great tendency to employ complicated fluxes, with unnecessary repetition of long-continued heatings indicative of a leisurely pace of life. Practically all the processes described are based on a few chemical facts: the inability of gold to combine with sulphur, while silver and the base metals form easily fusible sulphides; the ready oxidation of base metals; and the ii- solubility of gold in nitric acid. Fluxes serve to make earthy impurities fusible, and to carry oxidizing or sulphurizing ingredients. Many of the processes of assaying had changed little up to the beginning of the present century. Even as late as 1924, when the writer took a University course in fire assaying, the crucibles, cupels, scorifiers, molds, and tongs were identical with those of the sixteenth century, though the wind furnace had a stack on it and the muffle for cupelling was gas-fired.* The fluxes were purer, but of the same essential composition. That this branch- or twig-of metallurgy had not advanced in any funda-

Jan 1, 1949

By Laurence A. Dahners

As part of the strategic minerals program, the Bureau of Mines conducted a diamond-drilling project on three barite properties in eastern Tennessee and western North Carolina during the summer and fall of 1944. These properties, the Moccasin Gap prospect and the Krebs property in Cocke County, Tenn., and the Sandy Bottom mine of the Stackhouse group in Madison County, N. C. (fig. 1), are known to have produced some barite. The Bureau of' Mines project was planned to prospect for extensions of the ore bodies. A total of 3,169 feet of diamond drilling was done in 15 holes on the three properties. Tabulations of sample analyses and drill-hole logs are presented in this report. Two other mines of interest in the area are the McCoy and the Williams in Cocke County, Tenn. The Williams adjoins the Krebs. No drilling was done by the bureau in either of these properties.

Jan 1, 1949

By Reynold Q. Shotts

The small domestic underfeed stoker as now designed is unusually sensitive to the coking and plastic properties of coals, and when the attempt is made to burn the high rank coking and caking coals of the Appalachian fields, serious trouble may occur. Part of the trouble may be caused by the ash content and clinkering characteristics of the particular coal in use, but more often it is the result of an excessive ac-in of coke in the form of ''trees,, or masses in the fuel bed. Often the zone of burning becomes so restricted that the fire goes out, and in extreme cases the fire may be lifted completely out of the fuel bed and away from the air ports. Even if the fire is preserved, excessive coking may cause response to subsequent heat demand to be slow and irregular. Coke trees seem to grow most readily during periods of hold-fire operation, so that in order to preserve the fire in mild weather it is often necessary to set the timer for such a long operating period each hour that much unneeded and unwanted heat is developed, causing discomfort. During demand periods the fire may pick up so slowly that the intense burning which develops just before stoker cut-off causes a serious overshooting of the thermostat. Stoker coal performance tests which have been made in a number of labora- tories1,2,3,4,5 are one method of approach to the problem Of selecting stoker coals- As yet these tests have not been standardized and they are expensive and time-consuming. The value of the results probably increases with the length of the test. Sherman and co-workers at Battelle Memorial Institute believe that even a one-week test is not too reliable a trial2 and it is quite likely that Others will agree. A great advantage of such tests is that characteristics of coals, other than the tendency to form coke masses, may be evaluated from them. The selection of stoker coals would be greatly facilitated if there existed some simp1e measure Of the tendency Of a a to form coke in a fuel bed. Although possessing all Of the disadvantages Of any small-scale laboratory test, the test for the free-swelling index of coal has been found useful for evaluating the probable effects Of swelling properties upon combustion.7 Ostborg, Limbacherand Sherman, have shown that the test can Predict, roughly, the tendency Of coke to accumulate in the fuel bed Of a domestic stoker. They also gave instances of its value in predicting combustion behavior in some large installations. The use of the test for free-swelling index has become well established and has been adopted as a standard by the American Society for Testing Materials.8 When domestic stoker coal investigations began at the State Mine Experiment Station in the summer of 1944, it was decided

Jan 1, 1949

By William C. Martin

"Consolidated Sudbury Basin Mines Limited owns two mines, 4 miles apart, near the southwest end of Sudbury Basin. The Errington mine lies close to the north boundary of Creighton Township and about 18 miles by car from Sudbury. The Vermilion Lake mine is in Fairbank Township, on the south side of Vermilion Lake.The first discovery of base-metal mineralization within Sudbury basin was made by James Stobie in 1897 at Stobie Falls on the Vermilion River, half a mile west of the Errington mine. A few years later Alphonse Oilier made a discovery of massive pyrite with base-metal sulphides near the west end of the present Errington workings.No work of consequence was done on these discoveries until 1924, when Joseph Errington acquired options on a large acreage of ground which was later taken over by the Treadwell Yukon Company Limited. After considerable diamond drilling this company sank No. 1 shaft in 1926. In the next three years, a large amount of underground development was done, a pilot mill was constructed and operated for two years. All operations ceased in 1931 with the fall in metal prices. While in operation the pilot mill treated 186,172 tons of ore the average grade of which was 1·07 per cent copper; 1 10 per cent lead; 4·60 per cent zinc; 0·03 ounces gold; and 1 70 ounces silver.Up to the time of closing in 193 l there had been completed at the mine 26, 790 feet of lateral work and 75,500 feet of surface and underground diamond drilling. The company records, however, showed no figures on ore reserves, except broken ore in stopes amounting to about 60,000 tons. A study of the plans, prior to reopening the mine in 1952, showed 1,450 lineal feet of ore (at 1952 prices) opened up by drifting on the 300-foot and 500- foot levels. It is clear that no comprehensive picture of the structure was had at this time. The orebodies were considered to be very irregular pods scattered through masses of quartzite-carbonate in a sheared zone about 800 feet wide. In some way the ore was believed to be related to the tuff-slate contact zone. With this picture it was impossible to make a reasonable ore estimate or even gauge the tonnage potentialities with any feeling of reliability."

Jan 1, 1949

By C. R. Sandberg, T. A. Pollard, E. B. Elfrink

This paper presents an evaluation of compressibility factor data and a discussion of their application to the estimation of gas reserves. A correlation is presented which provides compressibility factors for use in both two-phase and single-phase hydrocarbon systems. Accuracies comparable to those obtained previously for single-phase systems only can be expected. A simple means of predicting the presence or absence of a liquid phase in a condensate system of known composition is illustrated. The correlation is based on 1,030 compressibility determinations from 21 hydrocarbon samples taken from eight oil fields. Of the data used, 75 per cent were from California, 15 per cent were from the Mid-Continent area, and 10 per cent were from South America. The average numerical deviation of the experimental data from this compressibility chart is 1.22 per cent. Charts and tables are included and discussed which illustrate the errors involved through the misuse or nonuse of compressibility factors in estimates of gas-in-place. INTRODUCTION The compressibility factor is a coefficient which expresses the deviation of a gas of given composition from the Perfect Gas Laws. A factor such as this is necessary in any calculation involving volumes of gaseous mixtures, and finds extensive application in the estimation of natural gas and condensate reserves. It is used in the decline curve, the volumetric, and the material balance methods of gas reserves estimation. The behavior of gases at high pressures has been investigated extensively in recent years and considerable data have been assembled on the compressibility characteristics of a number of gases. Notable among the investigators of high pressure gas relationships are Kvalnes and Caddya, Kay" Sage and Laceys, and Brown, Standing" and Katz4. Other contributors are Smith and Watson, Roland and Kaveler', and Stevens and Vance". The data on compressibility factors assembled by these investigators have been presented and correlated in numerous ways; particularly noteworthy is the method first presented by Kay5 which relates compressibility factor "Z" to pseudo-reduced temperature and Pseudo-reduced pressure. Other investigators have used this empirical relationship successfully and numerous charts covering a large number of gases have been constructed on this basis. It is the purpose of this paper to evaluate compressibility factor data and to illustrate the importance of their proper use in the estimation of gas-in-place for both gas and condensate reservoirs. EVALUATION OF COMPRESSIBILITY FACTOR DATA The compressibility chart presented by Standing, Katz, Brown and Holcomb in 1941 is probably the most recent and reliable chart for natural gases. The reliability of the Katz chart has been investigated by the writers for a fairly large number of gases (single-phase) in the pressure range from 500 to 10,000 psia and temperature range from 80 to 400°F. A summary of this comparison is presented in Table I. The numerical average deviation of the chart compressibility factors from the experimental compressibility factors is 1.05 per cent, and the algebraic deviation is -0.28 per cent. The Katz correlation appears to be quite accurate for single-phase hydrocarbon systems. It was based on single-phase systems and does not necessarily provide a means of accurately predicting the behavior of two-phase systems which might be encountered in condensate work. Data published recently by Sage and Oldsl' have enlarged the knowledge of phase behavior in condensate systems by covering extensively the Compressibilities of systems in the two-phase as well as single-phase regions for a wide range of temperatures, pressures and gas-oil ratios. An evaluation of these data indicates that conditions can arise, especially in condensate systems having fairly low gas-oil ratios, in which two phases occur and the usual gaseous compressibility factors do not accurately apply. The measured PVT data of Sage and Olds covering two-phase systems have been correlated with additional such data from the Mid-Continent area and South America; these are presented in Fig. 1. This chart is the result of 1,030 compressibility* determinations from 21 hydrocarbon samples taken from eight oil and condensate fields. Of the data used, 74.75 per cent were from California, 15.45 per cent were from the Mid-Continent area, and 9.80 per cent were from South America. The chart construction is based on the original

Jan 1, 1949

By Robert J. Hundhausen

This report describes Bureau of Mines investigations of a low-grade scheelite-bearing granodiorite intrusive situated on Henderson Creek, Granite County, Mont. The intrusive is in a narrow, V-shaped valley at the head of extensive placer workings. Since May 1943 the H. & R. Mines Co. of Portland, Oreg., has recovered scheelite sand and gold from the placer workings. A modified Yuba, 4?cubic foot bucket dredge was used in the operation. By February 1947 this operation had recovered and marketed over 215,000 pounds of scheelite concentrates containing 63 percent WO3. The scheelite in the placer was found to be derived principally from erosion of the granodiorite intrusive. The intrusive is one of a series of four similar, dikelike masses of granodiorite whose outcrops are aligned along a 10-mile zone of weakness trending N. 60° E. The intrusive has a triangular outcrop exposed over an area of 57 acres. Trenching and sampling by the Bureau of Mines demonstrated that scheelite is sparsely distributed throughout the granodiorite. This work delimited the outcrop of the intrusive and indicated a large submarginal reserve of low-grade tungsten mineralization. The deposit is ideally suited for exploitation by large-scale, open-pit mining operations; it would be easily available in a national emergency. Additional exploration would be necessary, however, before large-scale production plans could be made efficiently or accurately.

Jan 1, 1949

By H. W. St. Clair

Sampling of heterogeneous mixtures of fused metals or solidified melts is subject to errors not met in sampling finely ground ores or granular materials. These errors arise largely because of the segregation of constituent metals that usually takes place during solidification. It is seldom that a random sample of a lot of metal will represent the composition of the entire lot. The problem becomes especially difficult when it is necessary to make accurate analyses for a segregated impurity present in very small amounts. This paper discusses some of the pertinent experimental observations made in selecting a method for sampling melts of aluminum and zinc containing small amounts of iron and silicon as impurities. Although this experimental study dealt only with sampling this specific combination of metals, many aspects of the study apply generally to any mixture of mol ten metals containing minor constituents that segregate rapidly during freezing of the melt.

Jan 1, 1949

By Robert S. Sanford

In April 1948, the Bureau of Mines was requested to evaluate the graphite deposit' known as the Benjamin Franklin and Just mines in Chester County, Pa. After preliminary investigation, it was recommended that the Bureau core-drill, trench, and sample the deposit and make beneficiation tests on the ore. During the first and second World Wars, flake graphite was in short supply, and a number of deposits in the United States were exploited. In 1942, the Defense Plant Corporation, through its lessee, the Benjamin Franklin Graphite Co., purchased 70.263 acres of graphite-bearing land and built a complete mining and milling plant with a capacity of 300 tons of crude ore per 24-hour day at a cost of $426,250 (Plancor No. 1254).

Jan 1, 1949

By B. W. Gandrud

This is the first report published by the Bureau of Mines on washability characteristics of coal from beds in Tennessee. It is based principally upon screen-sizing and float-and-sink tests of raw coal from a bed on the Cumberland Plateau. Stripping operations were undertaken recently on this bed by the Cumberland Collieries, Inc., near Chalybeate,Van Buren County, Tenn. The bed has not been definitely correlated, but it may be an extension of the Sewanee bed, which has been mined extensively in the Tracy City district to the south-vest and at points near Dunlap and Pikeville to the southeast and east. It was spoken of by officials of the Cumberland Collieries as the Sewanee bed at the time of sampling for this study. In a letter dated October 16, 1948, W. D. Hardeman, geologist of the Department of Conservation, Nashville, Tenn., states: "The stripping operations of the Cumberland Collieries near the old postoffice at Chalybeate are, I am fairly certain, in the upper part of the Whitwell shale, which carries the Sewanee coal. This coal may be a stray seam, but it probably can be correlated with the Sewanee coal, which is mined farther east. "There are no detailed geologic maps or reports covering the area, and this opinion is based on what was observed in visiting the strip mines in that general vicinity." The laboratory work upon which this report is based was done at the Southern Experiment Station of the Bureau of Mines, United States Department of the Interior, in cooperation with the University of Alabama and the Cumberland Collieries, Inc.

Jan 1, 1949

By C. E. Sims, G. A. Moore

In previous publications of the writers4-7 it has been shown that vacuum extraction of steel can be carried as close to quantitative completion as desired provided the steel is in the austenitic state and sufficiellt time is allowed. For precise work, the method claims preference because the equipmelit for holding and heating the sample can be made simple, and because crucibles, boats, and other unnecessary materials can be eliminated and the blanks thus made very small. It is well known that the evolution rate of hydrogen is smaller just above the trans. formation than immediately below, as would be expected from the increase in solubility when passing into the gamma state. Many attempts have been made to obtain analyses by extraction just below the transition, using times of approxi. mately 2 hr. while it is true that the rate of evolution drops nearly to zero under these conditions, it has repeatedly been shown that the process is incomplete since on raising the temperature into the austenitic range, evolution will be resumed, usually after a, considerable induction period. The low-temperature evolution process appears to be useful in some cases for comparative tests where the residual crror may be more or less constant between samples, For general use, however, there is no guarantee that the error caused by incomplete extraction is constant; hence, the more laborious but more reliable high-temPe'atu'e Process must be used. At high temperature, an original flash evolution, similar to that at lower temperature, is first observed. After not more than an hour, the flash subsides and cvolution settles down to a regular first-order reaction rate for which the half-life* is usually of the order of a few hours for the 5/8-in. diam cylinder at 1050°C. The regular evolution may be followed for whatever period appears justified, after which the residual gas may be estimated as equal to that which was evolved in the last observed half-life period. Tests have shown that the composition of the evolved gas does not vary greatly during the progress of evolution; therefore the residual gas may safely be taken to have the same composition as the portion col-

Jan 1, 1949