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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 G. F. Fix

Oil and gas activity reached a higher peak in Indiana during 1940 than for any like period during the past decade. Major activity, as during 1939, was in the southwestern part of the state, the Indiana portion of the Eastern Interior Coal Basin, where most of the increase was due to field drilling in previously proven areas. The amount of wildcat drilling was about the same as for 1939. No new fields of any apparent consequence were discovered during the year, with the possible exception of the College pool, in southwest Posey County. Only one well had been completed in this area at the end of the year. About 10 ft. of saturated Aux Vases sandstone was drilled in this well and the initial production was I00 bbl. of oil a day. Other discoveries during the year 1940 include: St. Thomas, in southwestern Knox County, where four McClosky wells, ranging from I00 to 300 bbl. a day initially, were com-pleted; Buff kin, in central Posey County, with 11 oil wells and 5 gas wells completed; and new developments in two old areas —Randolph County (part of the old Trenton field) and Gentryville, northwestern Spencer County, where some oil was found many years ago. The St. Thomas field proved disappoint-ing, with very spotty production from the McClosky horizon of the St. Genevieve limestone at a depth of about 1875 ft. The discovery well flowed 362 bbl. a day ini-tially. At the end of the year the field was pretty well outlined by dry holes and some inside locations were dry. The Buffkin pool also proved spotty, with production from shallow Pennsylvanian sands and from the Basal Pennsylvanian Mansfield sandstone, the latter at a depth of approximately I175 ft., with small production from the Cypress sandstone of Chester age. Oil wells in this pool are small, ranging from 25 to 75 bbl. a day. The Randolph County area, on the east side of the Trenton gas field, showed some promise for a commercial gas field, with four completed gas wells having cumulative initial flows of about 1,200,ooo cu. ft. a day. The area appar-ently was not depleted during the Trenton boom at the turn of the century, since casing pressures are about as high as the virgin pressure in the old field. Elsewhere the pressure has dropped as low as 5 pounds. The Griffin field received most of the drilling during 1940, with 163 completed oil wells. This field now covers about 3200 acres on the Indiana side of the Wabash River and is not as yet completely delimited. It produced the major part of Indiana's oil during the year—a total of 3,594,000 bbl. At the end of 1940, there were 253 producing wells in Griffin. New Harmony had five completions for a total of 24. The Rockport field, in Spencer County, continued to be actively developed and had a total of 45 gas wells and 9 oil wells at the end of the year. Oil in commercial quantities had not been found in the field previous to 1940. Total gas production for the year was 394,470,000 cubic feet. In all, 521 wells were drilled in the state during 1940, as compared to 377 for 1939. Of this number 248 were oil wells, 77 were gas wells and 196 were dry. Divided into

Jan 1, 1941

By P. P. Gregory

The rate of drilling operations in the West Texas district during 1940 was approximately equal to that of 1939. The total number of wells dillled in the area during the year was 1834, of which 1716 were completed as oil producers, 12 were gas wells and 106 were dry holes. The number of wildcat wells drilled during the year was comparatively small. The drilling of inside locations in proven areas and the drilling of wells for the purpose of extending the productive limits in producing fields constituted the bulk of development during 1940. Gaines County led all other counties in the district in the total number of oil-well completions. The oil production totaled 83,345,381 bbl., the highest figure for any year since proration was begun. The 1940 oil production exceeded the 1939 production by approximately four million barrels. Discoveries While comparatively few new oil-producing areas were discovered during 1940, it appears that the oil production found in simpson lime in the Abell field, pecos County, was an outstanding discovery for the year. This was the second Ordovician discovery in Pecos County. Taubert, McKee & Siemoneit located its discovery well, V. W. Crockett No. 1, set. 4 1/2 H. & T. C. R.R, co, survey in the Imperial area of northwestern Pecos County. The top of pay was encountered at 5270 ft., and the well was bottomed at 5357 ft. in simpson lime, on act. 17, I940. The initial production was 928 bbl. of 43" gravity sweet oil in 11 hr. 23 min., flowing naturally through 2-in. tubing with gas-oil ratio of 783 cu. ft. per barrel. Following the completion of the discovery well, large blocks of land were leased in the area, and several locations were made toward the close of the year. There is every indication that the Abell field will become a major producing field in the West Texas district. There was no pipe-line outlet for the field at the end of the year. Shipley-Silurian field, discovered by the Gulf Oil Corporation, appears to be another major addition to the oil reserves in 1940. The discovery well, Wristen Brothers No. 5, is in sec. 18, block 5, H. & T. C. R.R. Co. survey in Ward County. The well was drilled to a total depth of 9187 ft. and was plugged back to 7075 ft. The Silurian lime section was acidized with 3000 gal., from 6993 to 7075 ft., and on Dec. 5, 1940, the well was completed for initial production of 3040 bbl- of 32.2" gravity oil in 24 hr., flowing through tubing. Todd Deep field, Crockett County, was discovered by the Continental Oil Co. et al. The discovery well, J. S. Todd No. 2, set. 29, block WX1 G.C. & S.F. R.R. Co. survey, was completed on April 3, 1940. The top of pay was encountered at 5623 ft., and the well was bottomed at 5691 ft. for initial production of 1613 bbl. of 40.6' gravity oil flowing naturally through 2-in. tubing. The pay section was found in Strawn lime of Pennsylvanian age. There were six producing wells in the field at the end of the year. This appears to be another major discovery in 1940. There was no pipe-line outlet in the field at the end of the

Jan 1, 1941

By P. P. Gregory

The rate of drilling operations in the West Texas district during 1940 was approximately equal to that of 1939. The total number of wells dillled in the area during the year was 1834, of which 1716 were completed as oil producers, 12 were gas wells and 106 were dry holes. The number of wildcat wells drilled during the year was comparatively small. The drilling of inside locations in proven areas and the drilling of wells for the purpose of extending the productive limits in producing fields constituted the bulk of development during 1940. Gaines County led all other counties in the district in the total number of oil-well completions. The oil production totaled 83,345,381 bbl., the highest figure for any year since proration was begun. The 1940 oil production exceeded the 1939 production by approximately four million barrels. Discoveries While comparatively few new oil-producing areas were discovered during 1940, it appears that the oil production found in simpson lime in the Abell field, pecos County, was an outstanding discovery for the year. This was the second Ordovician discovery in Pecos County. Taubert, McKee & Siemoneit located its discovery well, V. W. Crockett No. 1, set. 4 1/2 H. & T. C. R.R, co, survey in the Imperial area of northwestern Pecos County. The top of pay was encountered at 5270 ft., and the well was bottomed at 5357 ft. in simpson lime, on act. 17, I940. The initial production was 928 bbl. of 43" gravity sweet oil in 11 hr. 23 min., flowing naturally through 2-in. tubing with gas-oil ratio of 783 cu. ft. per barrel. Following the completion of the discovery well, large blocks of land were leased in the area, and several locations were made toward the close of the year. There is every indication that the Abell field will become a major producing field in the West Texas district. There was no pipe-line outlet for the field at the end of the year. Shipley-Silurian field, discovered by the Gulf Oil Corporation, appears to be another major addition to the oil reserves in 1940. The discovery well, Wristen Brothers No. 5, is in sec. 18, block 5, H. & T. C. R.R. Co. survey in Ward County. The well was drilled to a total depth of 9187 ft. and was plugged back to 7075 ft. The Silurian lime section was acidized with 3000 gal., from 6993 to 7075 ft., and on Dec. 5, 1940, the well was completed for initial production of 3040 bbl- of 32.2" gravity oil in 24 hr., flowing through tubing. Todd Deep field, Crockett County, was discovered by the Continental Oil Co. et al. The discovery well, J. S. Todd No. 2, set. 29, block WX1 G.C. & S.F. R.R. Co. survey, was completed on April 3, 1940. The top of pay was encountered at 5623 ft., and the well was bottomed at 5691 ft. for initial production of 1613 bbl. of 40.6' gravity oil flowing naturally through 2-in. tubing. The pay section was found in Strawn lime of Pennsylvanian age. There were six producing wells in the field at the end of the year. This appears to be another major discovery in 1940. There was no pipe-line outlet in the field at the end of the

Jan 1, 1941

By G. F. Fix

Oil and gas activity reached a higher peak in Indiana during 1940 than for any like period during the past decade. Major activity, as during 1939, was in the southwestern part of the state, the Indiana portion of the Eastern Interior Coal Basin, where most of the increase was due to field drilling in previously proven areas. The amount of wildcat drilling was about the same as for 1939. No new fields of any apparent consequence were discovered during the year, with the possible exception of the College pool, in southwest Posey County. Only one well had been completed in this area at the end of the year. About 10 ft. of saturated Aux Vases sandstone was drilled in this well and the initial production was I00 bbl. of oil a day. Other discoveries during the year 1940 include: St. Thomas, in southwestern Knox County, where four McClosky wells, ranging from I00 to 300 bbl. a day initially, were com-pleted; Buff kin, in central Posey County, with 11 oil wells and 5 gas wells completed; and new developments in two old areas —Randolph County (part of the old Trenton field) and Gentryville, northwestern Spencer County, where some oil was found many years ago. The St. Thomas field proved disappoint-ing, with very spotty production from the McClosky horizon of the St. Genevieve limestone at a depth of about 1875 ft. The discovery well flowed 362 bbl. a day ini-tially. At the end of the year the field was pretty well outlined by dry holes and some inside locations were dry. The Buffkin pool also proved spotty, with production from shallow Pennsylvanian sands and from the Basal Pennsylvanian Mansfield sandstone, the latter at a depth of approximately I175 ft., with small production from the Cypress sandstone of Chester age. Oil wells in this pool are small, ranging from 25 to 75 bbl. a day. The Randolph County area, on the east side of the Trenton gas field, showed some promise for a commercial gas field, with four completed gas wells having cumulative initial flows of about 1,200,ooo cu. ft. a day. The area appar-ently was not depleted during the Trenton boom at the turn of the century, since casing pressures are about as high as the virgin pressure in the old field. Elsewhere the pressure has dropped as low as 5 pounds. The Griffin field received most of the drilling during 1940, with 163 completed oil wells. This field now covers about 3200 acres on the Indiana side of the Wabash River and is not as yet completely delimited. It produced the major part of Indiana's oil during the year—a total of 3,594,000 bbl. At the end of 1940, there were 253 producing wells in Griffin. New Harmony had five completions for a total of 24. The Rockport field, in Spencer County, continued to be actively developed and had a total of 45 gas wells and 9 oil wells at the end of the year. Oil in commercial quantities had not been found in the field previous to 1940. Total gas production for the year was 394,470,000 cubic feet. In all, 521 wells were drilled in the state during 1940, as compared to 377 for 1939. Of this number 248 were oil wells, 77 were gas wells and 196 were dry. Divided into

Jan 1, 1941

By W. A. Bates, R. J. Miller

Although cresylic acids have been standard frothers in flotation for many years, there has been little discussion of their nature in the metallurgical literature. Aside from references in the patent literature, the paper by Landolt, Hill, and Lowyl in 1930, which resented a study of the frothing and collecting properties of some of the constituents of crude cresylic acids, represents the only contribution of this type. The close froth control required in the delicate selective separations of present-day flotation operations have required the flotation metallurgist to choose his frothers with care, and have caused him to require of the manufacturer a closely controlled, uniform product. A background of knowledge of the chemical composition and physical and chemical properties of the frothers, by which their action may be correlated, should aid in selecting frothers for particular flotation requirements. Further, the recent almost complete replacement in flotation of coal-tar cresylic acids by those derived from petroleum makes it especially desirable to review the flotation behavior of the acids from the old and the new sources. In view of these facts the Milling Methods Committee of the A.I.M.E. suggested to the Oronite Chemical Co. of San Francisco the preparation of a paper on the subject, and this paper has accordingly been prepared as a contribution by the California Research Corporation, the research affiliate of the Oronite Chemical Co. The discussion is from the following aspects: (I) constitution and properties; (2) sources; (3) comparison of coal-tar and petroleum cresylic acids; (4) characteristics as frothers, with particular reference to the effect of the substitution of petroleum acids for coal-tar acids. Constitution and Properties Cresylic acids are commonly regarded as mixtures of orthocresol, metacresol and paracresol. This was, indeed, the former meaning of the term, but in recent years it has been loosely applied to any mixture of alkyl phenols boiling above 190°C.; that is, excluding only phenol itself. This means that cresylic acids, as they are known today, may consist of mixtures, not only of the three isomeric cresols, but of six xylenols and of a variety of higher boiling homologues. Generically the constituents of cresylic acids are alkyl phenols, and they are often so designated in the literature to avoid the more indefinite term, "cresylic acids." They form an homologous series starting with phenol, which has the familiar benzene ring, with an hydroxyl group in place of one of the hydrogen atoms. The series of alkyl phenols is formed by the substitution of alkyl side chains, such as methyl, ethyl, propyl, butyl, etc., for hydrogen atoms of the benzene ring of phenol. Some

Jan 1, 1947

By R. J. Miller, W. A. Bates

ALTHOUGH cresylic acids have been standard frothers in flotation for many years, there has been little discussion of their nature in the metallurgical literature. Aside from references in the patent literature, the paper by Landolt, Hill, and Lowy1 in 1930, which presented a study of the frothing and collecting properties of some of the constituents of crude cresylic acids, represents the only contribution of this type. The close froth control required in the delicate selective separations of present-day flotation operations have required the flotation metallurgist to choose his frothers with care, and have caused him to require of the manufacturer a closely controlled, uniform product. A background of knowledge of the chemical composition and physical and chemical properties of the frothers, by which their action may be correlated, should aid in selecting frothers for particular flotation requirements. Further, the recent almost complete replacement in flotation of coal-tar cresylic acids by those derived from petroleum makes it especially desirable to review the flotation behavior of the acids from the old and the new sources. In view of these facts the Milling Methods Committee of the A.I.M.E. suggested to the Oronite Chemical Co. of San Francisco the preparation of a paper on the subject, and this paper has accordingly been prepared as a contribution by the California Research Corporation, the research affiliate of the Oronite Chemical Co. The discussion is from the following aspects: (I) constitution and properties; (2) sources; (3) comparison of coal-tar and petroleum cresylic acids ; (4) characteristics as frothers, with particular reference to the effect of the substitution of petroleum acids for coal-tar acids. CONSTITUTION AND PROPERTIES Cresylic acids are commonly regarded as mixtures of orthocresol, metacresol and paracresol. This was, indeed, the former meaning of the term, but in recent years it has been loosely applied to any mixture of alkyl phenols boiling above 190°C.; that is, excluding only phenol itself. This means that cresylic acids, as they are known today, may consist of mixtures, not only of the three isomeric cresols, but of six xylenols and of a variety of higher boiling homologues. Generically the constituents of cresylic acids are alkyl phenols, and they are often so designated in the literature to avoid the more indefinite term, "cresylic acids." They form an homologous series starting with phenol, which has the familiar benzene ring, with an hydroxyl group in place of one of the hydrogen atoms. The series of alkyl phenols is formed by the substitution of alkyl side chains, such as methyl, ethyl, propyl, butyl, etc., for hydrogen

Jan 1, 1946

By R. J. Miller, W. A. Bates

Although cresylic acids have been standard frothers in flotation for many years, there has been little discussion of their nature in the metallurgical literature. Aside from references in the patent literature, the paper by Landolt, Hill, and Lowyl in 1930, which resented a study of the frothing and collecting properties of some of the constituents of crude cresylic acids, represents the only contribution of this type. The close froth control required in the delicate selective separations of present-day flotation operations have required the flotation metallurgist to choose his frothers with care, and have caused him to require of the manufacturer a closely controlled, uniform product. A background of knowledge of the chemical composition and physical and chemical properties of the frothers, by which their action may be correlated, should aid in selecting frothers for particular flotation requirements. Further, the recent almost complete replacement in flotation of coal-tar cresylic acids by those derived from petroleum makes it especially desirable to review the flotation behavior of the acids from the old and the new sources. In view of these facts the Milling Methods Committee of the A.I.M.E. suggested to the Oronite Chemical Co. of San Francisco the preparation of a paper on the subject, and this paper has accordingly been prepared as a contribution by the California Research Corporation, the research affiliate of the Oronite Chemical Co. The discussion is from the following aspects: (I) constitution and properties; (2) sources; (3) comparison of coal-tar and petroleum cresylic acids; (4) characteristics as frothers, with particular reference to the effect of the substitution of petroleum acids for coal-tar acids. Constitution and Properties Cresylic acids are commonly regarded as mixtures of orthocresol, metacresol and paracresol. This was, indeed, the former meaning of the term, but in recent years it has been loosely applied to any mixture of alkyl phenols boiling above 190°C.; that is, excluding only phenol itself. This means that cresylic acids, as they are known today, may consist of mixtures, not only of the three isomeric cresols, but of six xylenols and of a variety of higher boiling homologues. Generically the constituents of cresylic acids are alkyl phenols, and they are often so designated in the literature to avoid the more indefinite term, "cresylic acids." They form an homologous series starting with phenol, which has the familiar benzene ring, with an hydroxyl group in place of one of the hydrogen atoms. The series of alkyl phenols is formed by the substitution of alkyl side chains, such as methyl, ethyl, propyl, butyl, etc., for hydrogen atoms of the benzene ring of phenol. Some

Jan 1, 1947

By G. S. Cole, G. F. Bolling

A series of Al-Cu alloys has been cast from constant superheat to solidify either with a hot top or with a free liquid/air interface. All the other variables which affect relative fluid motions were kept constant except the imposition of slow rotations m oscillations of the mold. Depending upon the exact circumstances, evi-dence could be found for the nucleation of equiaxed grains from dendrite bits detached from the columnar zone, or from the free surface, or from solid bits induced at pouring; a special experiment showed the solute buildup during ingot solidification and by inference the reality of constitutional supercooling. All methods of grain nucleation are thus supported. When solidification is arranged in a static mold the columnar- to-equiaxed transition occurs by one of these nucleation paths, subject to the natural decay of temperature gradients which promotes nucleation or the survival of nuclei. But when solidification is forced under special fluid flows it may display odd transitions. In one of these the equiaxed zone is synihesized from. dendrite bits detached from the solid/liquid interface. These survive under the concurrent lowering of temperature gradients and eventually cause transition by impeding columnar growth. GRAIN structure control is desired because real experience shows that specific properties are associated with specific cast grain structures. But since control is thus a matter of need and does not require understanding, much of casting remains art. For example, the manipulation of relative fluid motions in simple ingots provides a control of grain structure development,1-4 but theoretical insight is not required in order to broaden its potential applicability. Fortunately, however, once a variable like fluid flow is recognized it can also provide paths toward new insight. New observations using this variable have provided an insight which is curious. All the theories or descriptions of the columnar-to-equiaxed transition (CET) seem to be supported as long as the appropriate experiment is carried out. In order to develop this idea, let us ignore segregation, the chill zone (until a later section of this paper), and the origin and development of the columnar zone.= The details of questioning how equiaxed material forms in a casting may be divided in two. The first part is simply a questioning of the origin for equi-axed grains: are there fresh nuclei from heterogeneous nucleation, or dendrite bits broken off or melted from the columnar zone or elsewhere,6 or other solid bits surviving from the outset of freezing? The second is more complex, a questioning of the CET: does columnar growth slow down and allow the dominance of equiaxed grains, however they are formed, or do equi-axed grains take over and force columnar growth to stop? This "chicken-or-the-egg" second question can be quite useful, especially because it allows us to delineate the ordinary or NATURAL EQUIAXED ZONE and the induced or SYNTHETIC EQUIAXED ZONE. A natural equiaxed zone occurs if solidification proceeds in the absence of disturbances or extraneous forces such as ultrasonics, stirrings, and so forth. Both the CET theory proposed by Winegard and Chal-mers, 7requiring constitutional supercooling, and the CET theory suggested by Chalmers,8 requiring nuclea-tion only on pouring, pertain to the natural equiaxed zone. The best collating evidence to date for both these theories is contained in the work by Biloni and Chal-mers;9,10 the former theory7 is supported by special versions of the unidirectional growth experiment performed by Plaskett and winegardl1 and the latter theory' is supported in detail for the solidification of small ingots. An equiaxed zone can be synthesized when disturbances caused by forced fluid flows2-4 or other artificial means9,10 break off or melt off dendrite tips from an advancing solid/liquid interface,* if (and only if) temperature gradients in the melt are (forcibly) reduced enough to ensure the survival of these bits of dendrites, 2'3 Willful disturbances even so trivial as those produced by rapping a mold might be included here; as will be shown for example, this follows Southin's suggestion that the free liquid/air interface

Jan 1, 1970

By B. Lustman

IT has been known for a number of years that the addition of certain alkaline-earth and rare-earth metals to nickel-chromium base electric resistance alloys causes marked increase in their oxidation resistance as measured in an intermittent oxidation test similar to the ASTM—B 76-39 test. However, the mechanism whereby such additions confer protection is still unknown. On the basis of the experimental observation that the increase in life in intermittent tests of nickel-base alloys is proportional to the atomic radius of the added element, Hessen-bruchl has proposed that the added metal ions occupy holes in the oxide lattice which prevent diffusion of nickel ions in the oxide. Horn2 has postulated that the effect of such additions is to accelerate the rate of diffusion of chromium atoms in the metal and thus to favor the formation of Cr2O3 scales. Hickman and Gulbransen3 concluded from electron diffraction observation that the addition of the elements in question results in the formation of a barrier to the diffusion of nickel ions to the surface. In connection with some experiments conducted to develop a test for the resistance to oxidation of alloys in massive form under conditions of intermittent heating and cooling, some features of the oxidation of nickel-chromium base alloys were revealed which may serve to elucidate the mechanism of protection conferred by rare-earth and alkaline-earth elements. Specimens of cylindrical shape 0.360 in. diam x 0.37 in. long were placed in alumina thimbles and inserted into and withdrawn from a Globar-heated furnace operating at 2150°F at 7.5-min intervals. The weight of oxygen absorbed as well as the weight of oxide spalled were measured at intervals. With the particular experimental conditions used, the specimens in a 7.5-min cycle were at temperature for 2 min which corresponds to the heating time of the ASTM test. The weight changes of similar specimens under conditions of continuous heating in air at 2150°F were also measured. The specimens after oxidation were examined metal- lographically and samples of the spalled oxide collected for X-ray diffraction identification of the phases. The specimens used were from the same lot of material used by Hickman and Gulbransen3 and had the compositions shown in table 1. Included in table I are results of ASTM life tests on the materials in the form of wires. These materials, their composition and the ASTM life test data thereon were all supplied by F. E. Bash of the Driver-Harris Co. It may be noted that alloy 13246 of 80 pct nickel, 20 pct chromium nominal composition showed the shortest life in the ASTM test; alloy 12246 with the addition of small amounts of the elements zirconium, calcium, and aluminum, intermediate life; and alloy 12046 with the further addition of silicon, the longest life. In fig. 1 are shown the results of intermittent oxidation tests made on bulk specimens at 2150°F as well as continuous tests conducted at the same temperature. Duplicate tests were made on each specimen. The ordinate scale, inches of metal oxidized, was derived from the experimentally observed weight gain of oxygen by assuming the scale to be entirely Cr2O3. It may be noted that the metal-loss curves during intermittent oxidation show a constant or continuously increasing rate of weight

Jan 1, 1951

By AIME AIME

THE Wednesday morning session was devoted entirely to the consideration of the tentative code for coal mine ventilation. A. W. Hesse is chairman of this subcommittee. E. A. Holbrook presided at the session and assisted by A. W. Hesse and George S. Rice, gave the historical background of the movement for a ventilation code. They stressed the point that this was to be an engineer's code, and that it was hoped that it might serve as a valuable guide to operating companies in securing greater efficiency as well as safety in ventilation. The discussion was continued into the afternoon session, and by adjournment the entire' code had been covered.' Many sections were referred back to the Committee for further study and several new sections were suggested. The various opinions and new ideas brought out during the discussion proved very valuable and. contributed much to the progress being made in the preparation of this code.

Jan 1, 1929

By R. S. Shoemaker, F. W. McQuiston

RECOVERY METHODS AS RELATED TO PROPERTIES OF SILVER ORES The earliest metallurgical process for treating silver ores was amalgamation with mercury which was in use in the early 1500's. Closely following was the development of the Patio process for treating ores at Pachuca, Mexico. Silver often occurs as the native metal and in deposits associated with other metals such as gold, copper, lead and zinc. Principal silver minerals include compounds of sulfur, antimony, arsenic, and copper. Silver chloride, and argentiferous galena are also prime sources. Native silver and the chloride characterize the oxide zone of most deposits. Native silver can be concentrated, amalgamated, or cyanided. Silver chloride rapidly dissolves in cyanide without oxygen. Oxidized silver ores containing the higher oxides of manganese are generally refractory to metallurgical treatment. A refractory compound of manganese and silver is formed, probably a manganite , which is insoluble in cyanide solutions. Argentite is the predominant silver mineral. Other important economic minerals are native silver, argentiferous galena, cerargyrite, pyrargyrite and tetrahedrite. Argentite dissolves slowly, the reaction being reversible requires an excess of cyanide. Argentite with disseminated fine grained gold occurring in quartz veins with minor amounts of chalcopyrite and galena may be cyanided directly after grinding, with high silver and gold recoveries. The flowsheet adapted to this type of ore is the Minas de San Luis, Tayoltita cyanide plant, which treats a high grade argentite silver ore containing gold. It is a standard cyanidation circuit but employs long periods of agitation contact for the high silver sulfide content ore. Lead-zinc base metal semi-oxidized- complex ores in pipes and chimneys are replacement deposits in limestone at El Mochito Mine, Honduras. Mineralization comprises galena, cerussite, anglesite, sphalerite, calamine, and smithsonite. The silver content of about 16 ounces occurs as native silver globs, wire and the mineral argentite. After flotation of lead and zinc concentrates, the tailings are cyanided for gold and silver recovery. The great Huelva pyritic copper deposits of Spain carry a little gold and silver. At Cerro Colorado, these metals were concentrated above the chalcocite zone into the so-labeled Mgossanu. This material with a content of 0.08-0.09 oz Au and 1.50 oz Ag per ton is amenable to cyanidation. See Cerro Colorado flowsheet. In southern Hidalgo, about 60 miles north of Mexico City, are the great silver--gold veins of one of the foremost silver mining districts of the world. Real del Monte, Pachuca. The mineralized area consists of flow rocks and intrusives. The oxidized ores carry pyrites with oxides of iron and manganese and other minerals, silver and gold. The first zone contains

Jan 1, 1975

By Irving B. Cadoff, Ernest Levine

The fracture path in a Cu-4 pct Ag alloy wet with mercury was found to he dependent on the heat treatment used prior to tensile testing. Both quenched and slow-cooled alloys were embrittled by the mercury.. For quenched alloys, which were single -phase, the crack path was intergranular. Slowly cooled alloys, which contained precipitate platelets, exhibited transgranular fracture. By comparing stress-strain data for these alloys with similar data on mercury -embyittled solid-solution alloys, it was found that the role of the precipitate and that of the grain boundary in the fracture process were equivalent . THE fracture path which results when metals are strained in a liquid environment appears to be dependent upon the nature of the specific system. Mixed transgranular and intergranular cracking has been observed in the 2024 T4 aluminum alloy when wet with a Hg-Zn amalgam.' Transgranular fracture was induced in an A1-4 pct Cu alloy by masking off the grain boundaries from the liquid Hg-Zn amalgam.' The embrittlement of solid-solution alloys of copper in mercury results in intergranular fracture.' The effect of a precipitated phase on the fracture path in copper alloys is the subject of the present investigation. Cu-4 pct Ag was chosen so that its behavior could be compared with previous work on embrittlement of copper alloys. PROCEDURE High-purity copper (99.999 pct) was used as a base metal, along with 99.999 pct purity silver. Melting was carried out in graphite crucibles with manual agitation to get adequate mixing. The ingots were homogenized by means of vacuum annealing, chemically cleaned, and cold-rolled with intermediate vacuum anneals, to the desired thickness of 0.025 in. The rolled sheets were sheared to the final specimen size of 1 by 0.025 by 0.1 in. The specimens were then electropolished in phosphoric acid (concentrated) and heat-treated in an evacuated capsule at the solution temperature of 770°C. One batch was slow-cooled and the other quenched in water. The thermal etching which occurred during heat treatment was sufficient to permit grain boundary and precipitate delineation. Tensile tests were carried out in air and in mercury on a Table-Model Instron at a pulling speed of 0.2 in. per min. Wetting was accomplished by electro-polishing in phosphoric acid, rinsing in alcohol, and immersing in a pool of mercury. Once wet the coating was stable throughout the mechanical tests. In our studies it was found that wetting the surface or total immersion in mercury produced identical results. For convenience, the wetting technique was used for the experiments described. The crack pattern was observed directly on the surface by removing the mercury after testing. De-wetting was accomplished by flame heating the samples in a vacuum after testing and before observation of the surface. No etchant or polishing was used so as not to obscure the crack pattern on the surface. The mercury removal, however, resulted in a pitted surface but otherwise left the pertinent features visible. Photomicrographs were taken in this condition so as not to disturb the structure associated with the crack pattern. The average precipitate spacing was measured previous to coating the sample with mercury by use of an optical eyepiece micrometer. RESULTS The microstructure of the quenched specimens was single-phase while that of the slow-cooled specimens contained thin platelets of a second

Jan 1, 1964

By C. G. Bieber, J. R. Mihalisin, R. T. Grant

A growing demand for longer service life of gas turbines has placed increasingly rigorous requiret~rents upon superalloys employed for that application. Long-titne testing at high temperature has revealed that phase transformations occur in all superalloys. A common one of particular interest is o formation. Presented here are studies made to identify a and to characterize its formation and effect on properties in three cast nickel-base superalloys—IN 100 alloy, alloy 713C, and alloy 713LC. Methods are discussed by which o can be eliminated or inhibited in IN 100 alloy and alloy 713C. Evidence was obtained to indicate that some types of o may be more detrimental than others. Limitations in the electron vacancy approach to o prevention are pointed out, and it is shown how alternative approaches, such as reducing a complex superalloy matrix to the form of a pseudo-ternary system permitting equilibrium diagram treatment, lead to additional insights into the formation of in these alloys. AROUND 1960. Beiber1 developed IN 100 alloy, which still remains one of the strongest commercially available nickel-base superalloys. The principle used in the design of this alloy was to produce large quantities of y' phase in a y matrix through the use of copious amounts of aluminum and titanium. In 1963, ROSS' showed that when certain heats of this alloy were held for a long time at 1650°F they formed an acicular phase, subsequently identified as a.3 a is a hard and brittle phase first discovered in the Fe-Cr system by Bain and Griffiths.4 They termed it the "B" constituent. Subsequently this same phase was found in other systems, primarily those of the transition elements, and acquired the name "a" by which it is now known. The crystal structure of the a phase was first determined in the Fe-Cr system in 1950.5 It was shown to be tetragonal with a c/a ratio of about 0.52. as is the case with a found in other systems. This characteristic crystal structure is now the means by which a is identified. In superalloys, such as IN 100 alloy. large amounts of o impair the high-temperature creep strength and drastically reduce room-temperature tensile ductility. Discovery of o phase in some heats of IN 100 alloy quickly led to investigations of other superalloys for similar transformations. It was found that many of the stronger, more highly alloyed. super-alloys were indeed susceptible to o formation. This investigation has been concentrated on three commercial alloys: IN 100 alloy, alloy 713C, and alloy 713LC. J.R.MIHALISIN,MemberAIME, and C.G.BIEBER are with The International Nickel Co., Inc., Paul D. Merica Research Laboratory, Sterling Forest, Suffern, N. Y. R. T. GRANT, Member AIME, is with The International Nickel Co., Inc., Pittsburgh, Pa. Manuscript submitted May 22. 1968. IMD A detailed study has been made of the phase transformations and their relation to a formation along with a consideration of electron vacancy approaches for predicting a-forming propensity in these alloys. EXPERIMENTAL PROCEDURE Phase transformations were studied by light and electron microscopy, electron diffraction, microprobe investigations, and X-ray diffraction. Specimens for light micrographic examination were prepared by conventional grinding and polishing followed by etching with glyceregia (2:l HC1/HNO3 + 3 glycerine by volume). Photomicrographs of stress-rupture specimens were taken adjacent to the fracture unless otherwise noted in the text. Negative replicas for electron microscopy were taken from surfaces electropolished with a solution of 15 pct H2SO4 in methanol. For carbon extraction replication, a solution of 10 pct HC1 in methanol was used. A Siemens Elmiskop I was used for all electron microscopy. Selected-area diffraction studies were made at 80 kv using evaporated aluminum for standardizing the patterns. A nondispersive electron microprobe attachment was used to analyze the extracted precipitates chemically. The fluorescent X-rays were recorded using a flow counter containing P10 gas (90 pct Ar-10 pct methane) with a beryllium window and a single-channel pulse-height analyzer. The pulses from the analyzer were passed to a scaler-ratemeter and differential curves of counting rate vs pulse amplitude were obtained. The base line of the analyzer was driven with a synchronous motor at 0.5 v per min and a channel width of 0.5 v. The time for 105 counts was printed out for each 0.5-v increment. The microscope was operated at 80 kv with beam currents of 1 to 20 pa. This equipment detects elements from atomic number 13 to 40. X-ray diffraction studies were usually made on residues electrolytically extracted in 10 pct HC1 in H2O, although in one case a pattern was obtained from an etched surface of a metallographic specimen. A Siemens Crystalloflex IV was used with iron-filtered CoKa radiation. X-ray patterns were recorded using a goniometer speed of : deg per min. The scintillation counter and pulse-height analyzer operated at a channel height of 10 v and a channel width of 12 v. The equipment was calibrated with a powdered gold standard. The residues usually contained a number of phases. several of which could not be found in the ASTM card file. In addition, as is shown for the case of a phase in IN 100 alloy, other phases had a somewhat different lattice parameter from that reported in the ASTM card file, making it difficult to separate and identify constituents by comparison with ASTM d spacings. For these reasons, phases were identified on the basis of the lattice parameter obtained by indexing the ob-

Jan 1, 1969

By D. E. Etter, J. E. Selle

HIGH-PURITY cerium metals, supplied as 99.9 pct pure, by various suppliers, vary widely in melting points and in the shapes of the differential thermal-analysis curves obtained as the samples are heated. A definite correlation is noted between the melting point, amount of premelting, and the number of inclusions present in the material. Briefly, the DTA apparatus, previously de-

Jan 1, 1964

By FREDERICK W. BRADLEY

MINING is one of the world's oldest industries and has pioneered the civilization of all new lands. Today, mining is not only one of the essential and basic industries of the world, but it is constantly growing in magnitude and becoming more important. We think that the most of our mining is done in the western portion of this country, but in the old State of Pennsylvania mines and products derived from minerals account for about two-thirds of the entire productive wealth of the State. As our forests are denuded, mining furnishes substitutes for timber in the way of concrete, gypsum board, etc. ; and as civilization increases the wants of mankind, mining is producing metals and minerals of every kind in increasing quantities. For example: during the past ten years the per capita consumption of copper in the United States has increased 49 per cent, to 14.56 Ib.; that of lead has increased 35 per cent, to 12.24 lb.; and that of zinc has increased 70 per cent, to 9.57 Ib. The consumption in European countries is about one-half of this, and there are other countries with large populations where there is virtually no consumption; so when all other countries catch up in consumption with our country, you can see what an enormous demand there is going to be for the metals, even to the extent of having to find substitutes for copper, lead, and zinc.

Jan 1, 1929

By F. W. Willard

VIEWING with alarm is a preoccupation not exclusively the habit of the political spellbinder. In good faith many of our mineral technologists have been and are genuinely alarmed over the prodigal consumption of our mineral reserves. Most competent observers are cautiously pessimistic. There are sound technical reasons for such caution. It is the purpose of this paper to discuss some of those reasons without benefit of a gift of prophecy. Perhaps the outstanding reason for caution is ignorance of accessible but undiscovered mineral reserves. The petroleum technologists have an edge on their metallurgical brothers for they have better tools for exploration. This is not to say that the mining geologist has to depend on hunches or the divining rod. The outstanding work on orogenesis by Lindgren and others has provided the mining geologist with some sound scientific knowledge as to where accessible metallic minerals are most likely to be found, As Clinton H. Crane has recently observed, most of the accessible areas of the earth have been combed for easily identified outcrops, and those have been or are being actively exploited. To find ore bodies hidden below the surface is still a costly speculation.

Jan 1, 1946

By Wayne Loel

THE application of aerial photographs to all phases of geologic mapping is set forth, indicating the advantages to be gained in different types of country and under varying climatic conditions, Methods of field and office procedure are given from a geological point of view, as well as suggestions regarding the best methods of aerial mapping for different uses and under varying field conditions, including the study of submarine geology. Aerial photographs with accompanying geologic maps are shown to illus-trate the appearance from the air of different geologic features under varying climatic and topographic conditions.

Jan 1, 1938

By James C. M. Li, J. Weertman

James C. M. Li (United States Steel Covp.)—The author has discovered a single analytical relation between the minimum, or the steady-state, creep rate and the applied stress confirming a statement made earlier by orn" that such relation should exist and should reduce to the power law at low-stress levels and to the exponential law at high-stress levels. However, as pointed out by the author, all the available theories of creep are not adequate to explain such a single relation. Inspired by such a statement, I have made a suggestion concerning a possible explanation13 of the new relation. This is based on the concept that the rate-controlling step is the cooperative motion of a short dislocation segment. The nature of and the reason for the cooperation have been discussed13 as well as the reason why the motion of the dislocation could be controlled by the mobility of the short segments. A natural short segment has been proposed13 to be the node formed at the intersection of two dislocations. The reason why the node may contain only a few atoms has not been discussed and the application of the proposed model to all the metals and alloys reported in this paper has not been attempted. It seems appropriate to include these in this discussion. The model was partly inspired by the substructure recently observed in the electron microscope on creep specimens. One such example is shown in Fig. 48 in Darken's Campbell Memorial Lecture. The substructure is a collection of dislocation intersections and irregular networks. No pileups have ever been observed in such specimens. A closer look at the network indicates that one set of dislocations is more straight than the other set sug- gesting that the other set may be mobile in the plane of the net. Since, for the network to survive the creep deformation, some dislocation reaction has to take place at the intersection of the two sets of dislocations, the mobile dislocation, even if it can slip in the plane of the net, will have difficulty in moving at these intersections. To illustrate, an idealized network is shown in Fig. 9. The thin lines represent the set of dislocations which are mobile and can slip in the plane of the net except at the nodes which are formed at the intersection of the two sets of dislocations. The other set of dislocations, represented by the thick lines, may have a Burgers vector which is not parallel to the plane of the net, and therefore may be immobile. Because of this nonparallel Burgers vector, the Burgers vector of the node, which is avectorial sum of the Burgers vectors of the two sets of dislocations, will also be nonparallel to the plane of the net. Therefore, the node cannot slip in the plane of the net and the set of mobile dislocations will have to drag the node along as indicated in Fig. 9. Now the problem is how many atoms could be involved in the nodes. Exact calculation of the length of the node is a difficult task especially since the length should be a steady-state length and not an equilibrium length. An estimate of the equilibrium length can be made by balancing the line tension of all the dislocations. The results would be a small fraction of the length 1 between nodes as shown in Fig. 10. In some instances such a calculation shows that the node will not be formed. But, since the calculation is only approximate, it does not rule out the possibility of the formation of a short node. In other instances the equilibrium length of the node is an appreciable fraction of I. Such a node would

Jan 1, 1963

By M. Gell, G. R. Leveran

The high- and low-cycle fatigue properties of the nickel-base superalloy, Mar-MBOO, in columnar-grained and single-crystal forms were determined at room temperature. It was found that the fatigue lives of these materials were greatly affected by the size of preexisting cracks in MC-type carbides contained in the micro structure. Most of the data falls on two curves given by: (zN)'/A€= K, where Nf is the number of cycles to failure, Af is the total strain range, and K is a function of carbide size. No difference was observed in the fatigue behavior of the columnar-grained and single-crystal materials for the same MC carbide size. Matrix slip and crack initiation occurred at precracked MC carbides and, to a lesser extent, at micropores. Fatigue crack propagation was mainly in the Stage I mode, i.e., on cry stallo graPhic slip planes. The Stage I fracture in these materials was unusual in that distinct features were observed on the fracture surfaces. In high-cycle fatigue, these features resembled those commonly observed on the cleavage fracture surfaces of bcc and hcp materials. Yet, in this study, the cracks propagated slowly in a cyclic manner. In low-cycle fatigue, the Stage I facets contained equiaxed dimples, similar to those observed on the tensile fracture surfaces of ductile materials. These observations indicate that both local normal and shear stresses are involved in these Stage I fractures. A model is proposed to explain these results based on the weakening of the cohesive energy of the active slip planes by reversed shear deformation and the fracture of the bonds across the weakened planes by the local normal stress. RECENT developments in casting technology have produced cast nickel-base superalloys in columnar -grained and single-crystal forms.1'2 The tensile and creep properties of the nickel-base superalloy, Mar-M200, cast in these forms have been shown to be superior to the corresponding properties of the conventionally cast polycrystalline material.lp2 This improvement in properties results, in part, from the elimination of grain boundaries in the single crystals and the alignment of the grain boundaries parallel to the stress axis in the columnar-grained castings. As part of a program to evaluate the fatigue properties of nickel-base superalloys cast in single-crystal and columnar-grained forms, a study has been made of the cyclic deformation and fracture of Mar-M2OO at room temperature. M. fiFl I .hininr Mpmher AIMF ic ^pninr Rocoarrh Accn^iata anH I) EXPERIMENTAL PROCEDURE The composition range of Mar-Ma00 in weight percent is: 8 to 10 Cr, 9 to 11 Co, 11.5 to 13.5 W, 0.75 to 1.25 Cb, 1.75 to 2.25 Ti, 4.75 to 5.25 Al, 0.01 to 0.02 B, 0.03 to 0.08 Zr, 0.07 to 0.12 C, bal. Ni. All of the castings met the above specifications. The castings were solutionized for 1 to 4 hr at 2250°F followed by aging at 1600°F for 32 hr which resulted in a 0.2 pct offset yield stress of 150,000 psi at room temperature. The microstructure of the material consisted of cuboidal, coherent particles of ordered, fcc Ni3(A1,Ti) (commonly designated y'), approximately 0.3 p on edge, distributed in an fcc y solid-solution matrix. MC carbides together with shrinkage and gas micropores were also distributed throughout the materials. The MC carbides and micropores were located preferentially in the interdendritic interstices, as well as in the grain boundaries in the columnar-grained castings. The (100) direction of all the single crystals and the common (100) axis of the grains in the columnar materials were aligned within about 5 deg of the specimen axis. Fatigue testing was carried out in the high-cycle (HCF) and low-cycle (LCF) fatigue regions, with the major difference being gross yielding of the specimen occurred during the first cycle in the LCF region. This division also corresponded with the more usual one in which the life of a specimen in LCF is less than lo4 cycles and that in HCF is greater than lo4 cycles. The designs of the high-cycle fatigue and low-cycle fatigue specimens are shown in Figs. l(a) and (c), respectively. The gage sections of both HCF and LCF specimens were electropolished prior to testing. The HCF specimens were tested in an MTS, closed-loop, hydraulic fatigue machine at 10 cps in air. The specimens were cycled between a tensile stress of 5000 psi and a maximum tensile stress which ranged from 35,000 to 125,000 psi, Fig. l(b). The LCF specimens were cycled under strain control from zero to a maximum tensile strain, Fig. l(d), in a Wiedemann-Baldwin testing machine. The experimental procedure has been described elsewhere.3'4 Both HCF and LCF tests were interrupted periodically in order to replicate the development of slip and cracking at the specimen surface. This was accomplished by placing plastic replicating tape around the gage section of the specimen while the specimen was in the mahine. The size of the MC carbides for all specimens was measured on a polished longitudinal section through the gage section after fatigue testing. The method of measurement consisted of carefully scanning the entire polished section in order to locate the largest MC carbides. Photographs were then taken of the six longest carbides oriented approximately normal to the

Jan 1, 1969