Search Documents

By A. C. Dorenfeld

CHANGES in circuits are often made in milling operations. At the same time that these changes are being evaluated the ores are changing. Even from the same mine, the ore is usually variable as to amount and type of mineral content, degree of association of valuable and gangue minerals, amount and types of soluble salts, hardness, etc. The question then arises whether any small differences in results, after changes have been made in the various circuits, are really due to these changes or whether the variability of the ore can account for those differences. Statistical evaluation provides one method of answering the question that arises so often in beneficiation studies: Did changed results come about because of changed process, or did ore variation cause the change? In this case, data were available for statistical analysis from an operating period of 42 months, representing treatment of approximately 1 million tons of ore. During this period there had been two flowsheet changes: 1) regrind of the zinc circuit middlings was introduced, and 2) alcohol- pine oil frother mixture was substituted for cresylic acid-pine oil frother mixture. Findings are in Table I.

Jan 10, 1954

By H. E. Mussey

When the American Institute of Mining Engineers visited the Birmingham district in May, 1888, the four Ensley furnaces (Fig. 1) then completed were referred to as monumental.' Their dimensions are givcn in Table 1. Mr. Gordon stated, with considerable satisfaction, that on the preceding day one furnace had produced 165 tons. The blast was

Jan 1, 1925

By R. E. Maringer, A. Schwope

IT has been recognized that oxygen in minute quantities is extremely detrimental to the room-temperature ductility of molybdenum. Early fracto-graphic studies' of the cast metal indicated that oxides are formed preferentially at the grain boundaries. Additional verification of this preferential segregation has been obtained from internal friction studies on poly crystalline molybdenum (average grain diameter varied from 0.039 to 0.065 mm) and from observations of the effect of oxygen on specimens of extremely large grain size. Specimens A, B, and C, of 0.040 in. diameter commercial molybdenum wire (Lot FW 13-40) were heat treated in the vacuum furnace described by Few and Manning according to the specifications given in Table I. Internal friction studies of these specimens were carried out using a low frequency (approximately 1 cycle per second) torsional pendulum completely enclosed in a vacuum tank. As the pressure of oxygen in the heat treating atmosphere changed, the portion of the internal friction vs temperature curves ascribed to grain boundary relaxation changed correspondingly, Fig. 1. The decrease in the damping capacity at high temperatures as the pressure of oxygen in the heat treating atmos-

Jan 1, 1955

By F. W. Aul, R. C. Glenn

EXTRACTION techniques are of particular importance in determining size, shape an: crystal structure of particles smaller than l000Å in steels and other alloys. However, artifacts that can arise during the preparation of extraction replicas may lead to erroneous conclusions. The purpose of this note is to illustrate some of these artifacts and the misinformation that can result from their presence. An alloy of iron with 0.8 pct Cu was investigated in the following conditions: 1) Solution treated 3 days at 925°C in dry hydrogen and quenched in water. Aged in steps to precipitate copper, as follows: heated to 700°C, held 1 day; then furnace cooled to 50O°C, held 3 days; then furnace cooled to room temperature. 2) Solution treated 3 days at 925OC in dry hydrogen and furnace cooled to room temperature. 3) Solution treated 3 days at 925OC or 17 hr at 1100°C in dry hydrogen to dissolve all copper, then quenched in water. A normal parlodion dry-extraction technique was employed after etching the specimens with super picralP or with 2 pct nital. A wet-extraction method

Jan 1, 1962

Bureau of Mineral and Topographic Survey, University of Kentucky, Lexington, Ky. Arthur C. McFarlan, State Geologist The Kentucky Geological Survey was abolished by a recent legislative act and the Bureau of Mineral and Topographic Survey at the University of Kentucky was created in its place Publications of the former Survey are distributed by the present Bureau Several series of papers and volumes have been issued but only those of Series 3, 4 and 6 are now to be had in whole or in part Of Series 4, (1912-18) only one group of papers is available Vol: 1, pt. 2, Miscellaneous papers on fire clays, limestones and coals of parts of the state (1913), $125. Of Series 3 (1904-1912), the following bulletins are pertinent and may be had. Bulletin 3, Coals, clays, etc., of Kentucky (1905), 50 cents, 14, Coals of the Pineville Gap region (1912), $1.25, 16, The Waverlain formation of east central Kentucky (1912), 50 cents, 17, Coals of the Tradewater region (1912), 50 cents, 18, Coals of Quicksand region (1912), 50 cents; 19, Geology and coals of the Central City, Madisonville, Calhoun, and Newberg Quadrangles (1912), 50 cents

Jan 1, 1933

By Charles R. Fettke

The permeability of an oil or gas sand is its capacity for transmitting fluids, either liquids or gases, under pressure. The permeability of a sand depends upon the size and shape of the openings in it and the extent to which these communicate with one another, as well as upon the ratio of their volume to the total volume of the sand. The apparatus employed and the method of procedure used by the authors in conducting the permeability tests have been described in a previous pub1ication.l For the tests described here 1/2-in. cubes were used. They were set in the lower end of a 1-in. union, inserted in a square hole cut in a hard rubber stopper which fitted into the lower end of the union. In the tests with air, volumes were measured with a wet American gas meter of 100 cu. ft. capacity. In those with water, distilled water at room temperature was employed, unless otherwise noted. DescRiption of Sands Tested The tests described in this paper were performed upon 18 samples representing typical oil and gas sands from 7 localities in northwestern Pennsylvania. For purposes of identification, the cores from which the samples came have been designated by capital letters, the sequence of the samples in the cores by numerals, and the individual cubes by small letters. All cubes from the same samples came from adjacent portions parallel to the bedding. Core A of the Bradford sand came from the north central part of the Bradford field, from an area where water-flooding operations have proved highly successful. Core B of the same sand was obtained from the southern part of the field. This core contained a so-called "loose streak," 7.5 ft. thick, in the middle portion of which B2 is a representative sample. The "loose streak" has given trouble in water-flooding but responded favorably to an air-drive, using a pressure of 300 lb. The natural production was increased approximately five times over a period of three years in which the air-drive was in operation. Core C, also of the Brad-

Jan 1, 1931

By C. G. Black

The purpose of this paper is to present data obtained from an investigation conducted on the grindability of coal by the American Society for Testing Materials Tentative Standard ball-mill method. This investigation has been conducted over a period of a year, during which time several hundred tests were run on a wide selection of different coals coming from Pennsylvania, Ohio, West Virginia and Kentucky. The data herewith presented tend to show that the tentative standard ball-mill method might give results that are misleading and that a volume measure might be more indicative of the true grindability of materials of varying specific gravity. A means whereby the time element might be reduced has been studied and other phases of this work such as preparation of samples, mechanical screening, reporting results and duplicating tests have been investigated. It is hoped that all criticism offered in this paper will be taken as constructive, with the purpose ill mind of perfecting the method now tentative to show the true conditions 2nd of making optional the manner in which certain parts of the test might be conducted to meet diversified laboratory conditions. Weight and Volume The results of grindability on extraneous material from the coal scam obtained with the present tentative standard ball mill method indicate easier grinding of these materials as compared to most coals. Varying amounts of these impurities in the coal therefore may cause a raising of the grindability index and may lead to the erroneous conclusion that coals containing large amounts of these foreign materials are easier to grind. For a true comparison of grindability, it would seem necessary to grind to the same particle weight. If material were sized in a commercial mill by means of an air current set at a velocity to remove 1.60 sp. gr. float coal ground to 80 per cent minus 200 mesh, any 1.60 sink particles would be left behind, and in order to remove this 1.60 sink material by the same current it would be necessary to grind finer and produce a

Jan 1, 1936

By C. G. Black

The purpose of this paper is to present data obtained from an investigation conducted on the grindability of coal by the American Society for Testing Materials Tentative Standard ball-mill method. This investigation has been conducted over a period of a year, during which time several hundred tests were run on a wide selection of different coals coming from Pennsylvania, Ohio, West Virginia and Kentucky. The data herewith presented tend to show that the tentative standard ball-mill method might give results that are misleading and that a volume measure might be more indicative of the true grindability of materials of varying specific gravity. A means whereby the time element might be reduced has been studied and other phases of this work such as preparation of samples, mechanical screening, reporting results and duplicating tests have been investigated. It is hoped that all criticism offered in this paper will be taken as constructive, with the purpose ill mind of perfecting the method now tentative to show the true conditions 2nd of making optional the manner in which certain parts of the test might be conducted to meet diversified laboratory conditions. Weight and Volume The results of grindability on extraneous material from the coal scam obtained with the present tentative standard ball mill method indicate easier grinding of these materials as compared to most coals. Varying amounts of these impurities in the coal therefore may cause a raising of the grindability index and may lead to the erroneous conclusion that coals containing large amounts of these foreign materials are easier to grind. For a true comparison of grindability, it would seem necessary to grind to the same particle weight. If material were sized in a commercial mill by means of an air current set at a velocity to remove 1.60 sp. gr. float coal ground to 80 per cent minus 200 mesh, any 1.60 sink particles would be left behind, and in order to remove this 1.60 sink material by the same current it would be necessary to grind finer and produce a

Jan 1, 1936

By John J. Croston

IN the closing months of 1936 the copper industry gave every evidence that it was at last on the threshold of an improved era. At the beginning of the year prices stood at 9 ¼ ¢, which in itself was a great improvement over prices prevailing for the three previous years. Industry generally was showing signs of moving forward in this country, and business was definitely good in certain foreign quarters. The threat of war and preparations for rearmament in Europe and Asia acted as a further stimulus to purchasing. By midsummer the situation had so improved and stocks had been so reduced that the cartel of foreign producers (including American producers with foreign mines) decided to increase the production quota to 75 per cent on Aug. 1. Large-scale buying gave continued strength to the price and by Oct. 1 the quota was increased to 80 per cent, and again on Oct. 15, to 85 per cent. Notwithstanding this the price of copper continued its advance and on Nov. 1, with stocks declining continuously, the cartel increased operations to 95 per cent, then to 105 per cent on Nov. 5. In the meantime the domestic producers, because of the great increase in home consumption, had increased their production by nearly one-half. At the close of the year copper sold at 12¢ per pound, and since the turn of the present year has reached 17¢. This rapid increase has not been wholly justified. Much of the increase was due to the legitimate demands of recovering industry, but rearmament orders plus accumulation of reserve stocks in case of war, purchases in anticipation of labor strikes and purely speculative activities on the London Metal Exchange accounted for the balance. Certainly in view of the state of industry and the general world price level, it appears unnecessarily high. Talk of a copper shortage is sheer nonsense, the recent condition in the market being created by overbuying, leaving but a small volume for speculative supplies. It takes some months for an increase in mine output to reach the market, but production is again overtaking apparent consumption, stocks have begun to increase, and this, together with the reopening of many small

Jan 1, 1937

By B. L. Dunic, Terkel Rosenqvist

rr has long been suspected that sulphur has a small but finite solid solubility in iron, but up to the present more accurate data have been lacking. The survey given by Hansen' illustrates the divergence of data and opinions. Solubilities between 0.01 and 1.5 pct have been suggested, and opinions vary regarding the effects of temperature and phase transformations in iron on the sulphur solubility. The extent of solid solution and its variation with temperature might be expected to be an important factor in the occurrence of hot shortness in steel. Therefore, the object of the present investigation was to study this problem more systematically. It was furthermore hoped that solubility data for sulphur might contribute to an understanding of the factors which determine solid solubilities in general. Experimental Procedure The present work was based on the measurement of the chemical activity of sulphur in the solid solution by means of equilibrium with a mixture of hydrogen and hydrogen sulphide. When the solid solubility limit is reached, the sulphur activity in the iron becomes equal to that in the coexisting sulphide phase. A gas mixture of a controlled H,S/H, ratio was passed over pure metallic iron heated to a temperature in the range 900" to 1500". The amount of sulphur absorbed by the iron was determined by analysis, and from a plot of percentage of sulphur vs. gas composition the sulphur activity and the solubility limit were determined. As the rate of diffusion of sulphur in solid iron is very small, often several days were needed to be sure that equilibrium conditions had been established. To produce a gas flow with less than 1 pct H,S of constant composition for several days, was in itself a problem. The most satisfactory arrangement was obtained by a continuous synthesis of hydrogen sulphide from the elements. This was done in the part of the apparatus shown to the left in Fig. 1. The hydrogen used was first purified in tank batches by passage through activated charcoal cooled in liquid nitrogen under a pressure of 150

Jan 1, 1953

By N. A. Zeigler, T. D. Yensen

Aging is a term that connotes a slow change in properties under ordinary operating conditions. It can be accelerated by increasing the temperature and by mechanical straining. The magnetic properties of iron and some of its alloys have for many years been known to be subject to such a change. But the cause of the change was not recognized until a few years ago after mechanical age-hardening in non-ferrous alloys of the "duralumin" type had been definitely shown, by means of solid solubility curves, changes in electrical resistance and microanalysis, to be caused by slow precipitation of one or more constituents from the solid solution. The similarity between the solid solubility curves of such alloys (Fig. 1) and those for iron-nitrogen (Fig. 2) and iron-carbon alloys (Fig. 3) below the A1 transformation point suggested at once that magnetic aging of iron might be caused by a similar process; namely, by the slow precipitation of carbon and nitrogen in the form of Fe4N and Fe3C at ordinary temperatures because of a cooling rate that had been too rapid to permit complete precipitation according to equilibrium conditions. This suggestion has since been amply confirmed, particularly by the comprehensive work of Köster1 on the effect of nitrogen and carbon. Typical curves are shown in Fig. 4 for the relationship between aging temperature and coercive force. Previous to the establishment of the precipitation-hardening theory it was thought that the effect of nonmetallic elements like C, N, O, etc., on the magnetic properties of iron was greatest when these elements were retained in solid solution, atomically dispersed throughout the interstitial spaces of the iron lattice2. Based on the theory that magnetic properties are intimately connected with the regularity of the lattice, it now follows quite logically that a greater effect on this regularity may be obtained when the above impurities are precipitated as very fine particles of Fe3C, Fe4N, FeO, etc., more or less uniformly dispersed within the grains. But if this is the case, it follows also that there must exist a relationship between the size

Jan 1, 1935

By N. A. Zeigler, T. D. Yensen

Aging is a term that connotes a slow change in properties under ordinary operating conditions. It can be accelerated by increasing the temperature and by mechanical straining. The magnetic properties of iron and some of its alloys have for many years been known to be subject to such a change. But the cause of the change was not recognized until a few years ago after mechanical age-hardening in non-ferrous alloys of the "duralumin" type had been definitely shown, by means of solid solubility curves, changes in electrical resistance and microanalysis, to be caused by slow precipitation of one or more constituents from the solid solution. The similarity between the solid solubility curves of such alloys (Fig. 1) and those for iron-nitrogen (Fig. 2) and iron-carbon alloys (Fig. 3) below the A1 transformation point suggested at once that magnetic aging of iron might be caused by a similar process; namely, by the slow precipitation of carbon and nitrogen in the form of Fe4N and Fe3C at ordinary temperatures because of a cooling rate that had been too rapid to permit complete precipitation according to equilibrium conditions. This suggestion has since been amply confirmed, particularly by the comprehensive work of Köster1 on the effect of nitrogen and carbon. Typical curves are shown in Fig. 4 for the relationship between aging temperature and coercive force. Previous to the establishment of the precipitation-hardening theory it was thought that the effect of nonmetallic elements like C, N, O, etc., on the magnetic properties of iron was greatest when these elements were retained in solid solution, atomically dispersed throughout the interstitial spaces of the iron lattice2. Based on the theory that magnetic properties are intimately connected with the regularity of the lattice, it now follows quite logically that a greater effect on this regularity may be obtained when the above impurities are precipitated as very fine particles of Fe3C, Fe4N, FeO, etc., more or less uniformly dispersed within the grains. But if this is the case, it follows also that there must exist a relationship between the size

Jan 1, 1935

By H. E. Doerr

THE writer has been unable to find much information relative to tests made to determine the effect of forging on the specific density of steel. The opinion, however, among men engaged in the business, seems to he that forging greatly compresses or consolidates the steel. While such is doubtless the case with spongy or porous steel, the following experiments indicate that there can be little or no change in the density with steel initially free from cavities: Ten ingots of basic open-hearth steel cast as shown in Fig. 1 were used in the experiments. All the specimens were 0.53 carbon with all other elements the same, the analysis being determined from drillings taken midway between the center and outside of the upper end, as shown in Fig. 2. The specimens were selected from over one thousand ingots so that the tests could be comparative for the work done in forging only, but no two of the ingots were cast in the same heat. Each ingot remained in the mold approximately 30 min., when it was removed and air-cooled. About 12 hr. later, when the temperature had been reduced to approximately that of the surrounding atmosphere, the head was discarded and the ingot heated in an oil furnace to approximately 2250° F. (1235° C). Approximately 1 min. was required to forge under the steam hammier to 1 ¼ in. (31.75 mm.), rough diameter, as shown by the dotted lines in Fig. 2. All ingots were allowed to air-cool after forging. Cylinders ½ in. (17.7 mm.) in diameter and ½ in. high were then turned from the forged and unforged parts of the ingots and numbered. The ten pairs of specimens were submitted to Louis E. Endsley, Professor of Railway Mechanical Engineering, University of Pittsburgh; A. N. Talbot, Professor of Applied Mechanics, University of Illinois; L. Z. Slater, chief chemist, Scullin Steel Co., St. Louis, Mo. No in-formation was furnished as to which specimens were forged or unforged and each laboratory used the same specimens, submitting the average of three independent determinations, a tabulation of which is shown in the accompanying table in which the laboratories are designated by

Jan 1, 1919

By William Sharp

Discovery of new ore in the Eureka district, Nevada, as a result of bold and persistent exploration based on a geologic interpretation of structure has recently aroused wide comment in mining circles. It may therefore be of interest to the profession to have a summary of the historical background and an account of the recent program of development. The mines of Eureka, discovered in the late 1860's, were the first important silver-lead mines in the United States. They have a production record of more than fifty-one million dollars.' After the ore bodies were apparently bottomed in the 1880's, repeated attempts to find new ore were unsuccessful until 1940, when a diamond-drill hole cut a 40-ft width of sulphide ore 1409 ft below the 841-ft level of the Locan shaft. The next hole cut 30 ft, of ore and three additional holes drilled in 1943 and 1944 showed the ore body to be continuous, Shaft sinking to reach and open up the ore body has been in progress since 1945. Geology Stratigraphy The ore in the Eureka district occurs in a series of Cambrian sediments which is exposed through a thickness of over 6000 ft. The stratigraphic column is as follows:2 Thickness. Ft Ordovician : Pogonip limestone (upper part). Thin bedded limestone with some chert. Upper Cambrian: Pogonip limestone (lower part). Thin-bedded limestone (with shaly limestone and chert).... 425 + Dunderberg shale. Shale (clay and calcareous shale) and thin-bedded limestone............. 34°+ Hamburg dolomite. Dolomite and limestone.................... 900+ Middle Cambrian: Secret Canyon shale. Shale and thin-bedded limestone........ 1,035 Geddes limestone. Carbonaceous, flaggy limestone with some shale partings................ 335 Middle (?) and LoweR Cambrian: Eldorado dolomite. Dolomite and limestone.................... 2,000 Lower Cambrian: Prospect Mountain quartzite. Quartzite with occasional intercalated conglomerate and shale 1,660+ The Prospect Mountain quartzite has been subdivided into two formations: Upper part, Pioche shale. Shale, quartzite with some intercalated limestone (Lower Cambrian fossils)-200 ft. Lower part, Prospect Mountain quartzite proper- 1,460Sft. Total thickness................ 6,695 + Much the most productive of these formations has been the Eldorado dolomite, which yielded more than $42,000,000 at Ruby Hill and an additional amount

Jan 1, 1949

By William Sharp

Discovery of new ore in the Eureka district, Nevada, as a result of bold and persistent exploration based on a geologic interpretation of structure has recently aroused wide comment in mining circles. It may therefore be of interest to the profession to have a summary of the historical background and an account of the recent program of development. The mines of Eureka, discovered in the late 1860's, were the first important silver-lead mines in the United States. They have a production record of more than fifty-one million dollars.' After the ore bodies were apparently bottomed in the 1880's, repeated attempts to find new ore were unsuccessful until 1940, when a diamond-drill hole cut a 40-ft width of sulphide ore 1409 ft below the 841-ft level of the Locan shaft. The next hole cut 30 ft, of ore and three additional holes drilled in 1943 and 1944 showed the ore body to be continuous, Shaft sinking to reach and open up the ore body has been in progress since 1945. Geology Stratigraphy The ore in the Eureka district occurs in a series of Cambrian sediments which is exposed through a thickness of over 6000 ft. The stratigraphic column is as follows:2 Thickness. Ft Ordovician : Pogonip limestone (upper part). Thin bedded limestone with some chert. Upper Cambrian: Pogonip limestone (lower part). Thin-bedded limestone (with shaly limestone and chert).... 425 + Dunderberg shale. Shale (clay and calcareous shale) and thin-bedded limestone............. 34°+ Hamburg dolomite. Dolomite and limestone.................... 900+ Middle Cambrian: Secret Canyon shale. Shale and thin-bedded limestone........ 1,035 Geddes limestone. Carbonaceous, flaggy limestone with some shale partings................ 335 Middle (?) and LoweR Cambrian: Eldorado dolomite. Dolomite and limestone.................... 2,000 Lower Cambrian: Prospect Mountain quartzite. Quartzite with occasional intercalated conglomerate and shale 1,660+ The Prospect Mountain quartzite has been subdivided into two formations: Upper part, Pioche shale. Shale, quartzite with some intercalated limestone (Lower Cambrian fossils)-200 ft. Lower part, Prospect Mountain quartzite proper- 1,460Sft. Total thickness................ 6,695 + Much the most productive of these formations has been the Eldorado dolomite, which yielded more than $42,000,000 at Ruby Hill and an additional amount

Jan 1, 1949

By Georges Caraghiaur

INTRODUCTION A small, independent mining enterprise (SIME) is an independently owned and operated business concern engaged primarily in mineral development, from the exploration to the production stage. By definition, a SIME is not dominant in its field and has no long-term financial backing. It is not a major producer of minerals, nor is it a petroleum company, a government organization or a subsidiary of such organizations. A SIME may or may not be listed on stock exchanges. The SIME is also called small miner, junior mining company, speculative mining company, and penny-stock mining company. The survival and growth of a SIME is most often controlled by an independently minded entrepreneur, who not only conceives and carries out new projects, but is materially affected by the success or failure of these projects. Usually, a SIME does not have a large or constant cash flow. Such a lack of long-term financial backing forces the SIME to meet the challenge of finding capital for its activities on a step-by-step basis. Its survival strategy is thus based on finding funds at the right time, of the right type and in the right quantities. The purpose of this paper is to show that the type of venture in which a SIME is involved affects the difficulty of raising new capital and the choice of possible sources of funds. The Small, Independent Mining Enterprise (SIME) The SIME is not a figment of the imagination of financial speculators. In Canada, there are more than 1,800 small mineral enterprises which spend on the average less than $1,000,000 per year on activity which is directed at bringing forth new mineral supply. In the United States, 64% of the non-fuel mining operations are conducted by nine or fewer men, and the coal industry is characterized by several thousand smaller independent producers, still predominantly family owned or controlled. In Chile, 80% of the mines can be classified as small mines. In the Philippines, approximately 60% of metal mining operations are classified as small mines. The SIME is actively engaged in mining all over the world, and very much so in the Pacific Rim. The Mineral Supply Process The whole process of bringing forth new mineral supply involves a dynamic sequence of activities, ranging from the initial exploration for a mineral occurrence to the production of a marketable product. A typical sequence is outlined in Figure 1. At the grass-roots exploration stage, a series of geological, geophysical and geochemical tests is aimed at locating a mineral occurrence. Especially in the early phases of such activities, the uncertainty (risk) surrounding a venture is high, since only general geological information exists on which to base a judgement of the economic viability of the venture. Such risk is attractive to few investors. As the information-gathering process continues, uncertainty diminishes. Once exploration efforts result in the discovery of a mineral occurrence, i.e. when indications of mineralization and mineable widths are obtained by drilling, there is still uncertainty concerning the extent of mineralization and the probability of having located an economic mineral deposit. The expected return on investment at such a stage may well be negative but the slight possibility of a very high positive return will make a number of financial sources available to an exploration company. At the development stage, much of the uncertainty

Jan 1, 1985

By Walter Kauenhowen

Germany's crude-oil production during 1937 totaled 3,174,157 bbl., an increase of 1.9 per cent over the 3,112,494 bbl. produced in 1936. According to official published data, and using a conversion factor of 1 metric ton = 7 bbl., the oil production of Germany in 1937 by fields was as follows:

Jan 1, 1938

By W. C. Winegard, E. L. Holmes

The effects of the solute elements lead and bismuth on grain growth in zone -refined tin have been investigated. At low temperatures, viz. below 160°C. or at high concentrations, viz. greater than 0.03 at. pct, the temperature dependence of grain growth was found to be constant. A correlation was found to exist between the rates of grain growth in the presence of solute impurities and the factor [C Ir - 1]2 , where C is the solute concentration, r is the radius of solvent atom, and r' is radius of solute atom. It is shown that the Liicke and Detert theory does not give a satisfactory explanation of the results obtained. INVESTIGATIONS of grain growth in zone-refined lead and tin and some effects of solute elements on grain growth in these metals have been reported by Bolling and winegardly2 and Holmes and winegard? The present investigation is an extension of the previous work, and was undertaken to provide additional results which might make it possible to discover the mechanism whereby the rate of grain growth is affected by the presence of foreign solute atoms. The experimental procedure was exactly the same as that described previously.3'4 Figs. 1 and 2 show the results obtained with lead and bismuth additions over the same temperature range, viz. 167" to 220°C, as that used for the investigation of grain growth in zone-refined tin.3 Fig. 3 shows the results obtained for zone-refined tin and for this tin with lead solute additions over an extended temperature range. DISCUSSION OF RESULTS As mentioned previously,3 the character of grain growth in the particular zone-refined tin used in these experiments appears to change as the temperature of annealing falls below about 160°C. The grain growth became somewhat irregular and was characterized by a jaggedness of many of the grain boundaries. The reason for this change is not known, but may be due either to residual impurity effects or possibly an oxide precipitation. It was obvious that normal grain growth only occurred in the zone-refined tin through the high-temperature range 167" to 220°C, and so the effects of solute atoms on grai11 growth over the two temperature ranges will be discussed separately. a) Effect of Impurity on Grain Growth in the Temperature :Range Above 167°C. It is apparent from Figs. 1 and 2 that, for low concentrations of solute, the rates of grain growth tend towards a common value as the melting temperature of tin is approached. As the concentration of lead is increased, the rate of grain growth close to the melting temperature is also reduced, and at high concentrations the temperature dependence of the rate of grain growth appears approximately constant. It should be noteil that the effect of bismuth is greater than that of the same concentration of lead, but both these solutes have a smaller effect on the rate of grain growth than silver, as seen from an earlier investigation of Holmes and Winegard. It should

Jan 1, 1962

By G. D. Hobson, I. Mrosovsky

Material balance relationships for expansion-type reservoirs above the bubble point have been discussed in recent years by H. N. Hall and M. F. Hawkins, Jr. The former drew attention to the effects of rock compressibility, and the latter to the effects of the compressibility of any interstitial water. Hawkins derived a general relationship which took note of oil, water and rock compressibilities, and then by assuming first, the absence of interstitial water and secondly, no effects due to interstitial water or rock compressibility, obtained relationships symbolically of the same form as those previously derived directly by Hall. Hawkins defined his terms clearly, and noted an approximation, due to the omission of a term involving the product of two compressibilities, made in reaching his final equation. There is, however, possible ambiguity with regard to Hall's written definition of the oil production term. One interpretation would mean that the produced oil and initial oil-in-place, if both required as stock tank barrels, would be obtained by using different formation volume factors in the conversion in order to satisfy the conditions implicit in Hall's formulae. The other would involve an approximation which, if used, was not stated. In both Hall's and Hawkins' studies the effect of the approximation or inconsistency is very slight. Nevertheless, it may be justifiable to give a somewhat more consistent derivation, since the complexity of the final relationships is not thereby greatly increased. Let the initial pore volume be Vi and the volume after a pressure drop of Ap, V. Then V = V, (1 - ?p . cr), where c, is the rock compressibility expressed as change in pore volume/unit pore volume/unit pressure change, and is defined with the initial pressure as base. Suppose that the interstitial water saturation under the initial conditions is Sw. The total volume of interstitial water under those conditions will be ViSw. If the volume of the water after dropping the pressure by ?p is V., this will be given by Vw = ViSw (1 + ?p.c,w), the compressibility of the water being c, which is ex- pressed using the volume at the initial pressure as base. If Boi is the reservoir volume factor of the crude oil for the initial reservoir conditions, and B. the equivalent factor when the pressure has dropped by ?p, with N the initial amount of oil expressed as stock tank barrels. N.Boi = Vi - V,Sw If n is the amount of oil produced (in terms of stock tank barrels) as a result of the pressure drop ?p, the remaining subsurface volume of oil at the lower pressure will be Bw, and Bc can be related to the compressibi:ity of oil and the pressure drop, and if c, is the compressibility factor based on the initial conditions, The relationship derived by Hawkins was case to a standard at the lower pressure, while a term (Ap) had been dropped, because of its smallness arising from its dependence on the products of two compressibility factors. When there is no interstitial water and rock compressibility can be ignored, Eq. 1 reduces to:

Jan 1, 1957

By Nicholas J. Grant, Italo S. Servi

SPECIAL polishing and etching techniques were developed during an investigation of the high temperature mechanical properties of high purity aluminum (99.995 pct Al).* Electrolytic polishing was done successfully in the following electrolyte: 5 ml perchloric acid (72 pct), and 95 ml glacial acetic acid. No special precautions need be taken during the preparation of the electrolyte since no appreciable heat of mixing is evolved. Although the electrolyte is not an explosive, it is recommended that Jacquet's safety rules' be followed during the polishing operation. A voltage of 25 to 60 v gives a good polish in about 2 min at room temperature after preparation on 3/0 metallographic paper. Most of the grain boundaries are visible under the microscope after polishing. Since the current is controlled essentially by the resistance of the bath, it is necessary to keep the anode-to-cathode distance as constant as possible. Accordingly, polishing of irregularly shaped pieces will be difficult. A cooling bath and a stirring system are advisable in order to keep the temperature of the bath uniform and constant. Coarse-grained samples can be macroetched in a few seconds by lowering the voltage below 10 v. This is done after electrolytic polishing, without removing the sample from the bath, Fig. 1. The specimen can be repolished in less than 1 min by raising the voltage above 25 v. The "galvanic etching" technique, which has been described elsewhere,' was found to be helpful not only for macroetching, but also for microetching coarse-grained specimens. In fact, the different orientations of adjacent grains provide good contrast at the grain boundaries, when the sample is observed under polarized light. If the specimen is only partially etched, Fig. 2a, the grain boundaries can be located without completely destroying the appearance of the surface of the specimen. The unetched surface appears black under polarized light. Excellent color contrast is obtained by using a "sensitive tint" plate in the optical system of the microscope. In this case, the unetched surface has a magenta color, while the etched part of the sample assumes different colors varying from green to brown, according to the orientation of the grains. Etch pits were produced on high purity aluminum by using the technique suggested by Lacombe and Beaujard." Good results also were obtained by substituting 70 pct nitric acid for the fuming nitric acid recommended. This gave an etching reagent of the following composition: 70 ml nitric acid (70 pct), 50 ml hydrochloric acid (37.5 pct), and 3 ml hydrofluoric acid (48 pct). An example of the results is shown in Fig- 2b. The outline of the etch pits is revealed sharply if the specimen is observed under polarized light, as shown in Fig. 2c. These metallographic techniques are not suitable for the examination of commercially pure (2s) aluminum. References 'P. A. Jacquet: Metal Finishing (Nov. 1949) 47, p. 62. 21. S. Servi: Metal Progress (1950) 58, p. 732. 3 P. Lacombe and L. Beaujard: Journal Inst. of Metals (1947) 74, p. 1._________________________

Jan 1, 1952