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By A. M. Gaudin, D. W. Fuerstenau, M. M. Turkanis

SOLUBLE silver salts are effective activators for flotation of sphalerite with potassium ethyl xanthate as collector.' Since sphalerite takes up large quantities of silver ions rapidly," investigation of this system appeared fruitful for studying the mechanism of sphalerite activation and deactivation. Experimental data presented here comprise studies of the mechanism and rates of activation and deactivation of sphalerite with silver and cyanide ions. A 20-lb sample of sphalerite from Ottawa County, Oklahoma, was handpicked, crushed, screened, hydrosized to produce a 65/100-mesh fraction, and purified by electrostatic separation. The sphalerite was then leached with benzene and absolute ethyl alcohol to remove possible organic contaminants and with 0.1 M NaCN to remove any copper that might have been picked up during screening. The benzene had been specially purified by grinding with fine sphalerite for 12 hr to remove trace impurities that might have had a specific affinity for sphalerite. Finally, the mineral was washed, dried in flowing nitrogen, and stored in large ground-glass stoppered weighing bottles under a small nitrogen pressure.

Jan 1, 1957

By Allan J. Clark

It may be said that the history of gold in the Black Hills begins with one of South Dakota's most. interesting relics, the so-called Thoen Stone, now in the Adams Memorial Hall at Deadwood. This slab of reddish sandstone, about 14 in. square, was found in by Louis and Ivan Thoen, at the base of Lookout Mountain, near Spearfish, a town in the northern foothills of the Black Hills uplift. Both sides of the stone bear clearly legible inscriptions. One side reads: Came to these hills in 1833. Seven of us, De Lacompt, Ezra Kind, G. W. Wood, T. Brown, R. Kent, Wm. King, Indian Crow. All ded but me, Ezra Kind. Killed by Indians beyond the high hills. Got our gold June 1834. On the reverse side: Got all the gold we could carry. Our ponys all got by the Indians. I hav lost iny gun and nothing to eat, and Indians hunting me. Attempts were made to trace these men. Relatives of Brown were found in Missouri, and it was learned that he had left for the West in 1832, with one Kent. Kind's relatives were also found, and stated that he had started West the same year. None of them had been heard from since their departure. So Kind failed to get out with "all the gold we could carry"; 15 years later California became the center of the first great gold rush, and the Hills waited 40 years for their gold to be rediscovered. It is interesting to speculate on what might have been "the course of Empire" had this little group won through. The history of Dakota, of Montana, indeed, of all the Northwest, might have been very different. When, late in 1875, the goldseekers arrived, they passed quickly northward from the first discovery near Custer, and soon were established on Deadwood Creek, along which, as well as for short distances above the mouths of its tributary streams, Blacktail and Bobtail, placer operations went forward vigorously. These placers were near the northern outcrop of the Homestake ore-body. Their gold was partly derived from this, perhaps in greater quantity from the erosion of the conglomerate or cement deposits, of Potsdam time, themselves a "fossil placer" or beach deposit formed by

Jan 1, 1935

By Theodore Simons

The rapid and comparatively recent development of flotation has opened so fascinating a field for study and research that the older processes of gravity concentration no longer receive the attention they deserve. The early work of Munroel and Richards12 and the more recent contributions by Clevenger and Coe,3 Laist and Wiggin,4 Ammon,5 Bardwell,6 Crowfoot,' and Hayden8 (to mention only some which have appeared in our own Transactions) and by Schu1z,9 have furnished so much data that to offer something new seems a difficult task. It is still possible, however, to present known facts from a different point of view, and, with this in mind, the writer has undertaken to express basic principles of gravity concentration in terms of simple mathematics and mechanics; the conclusions thus reached will be found to correspond, in general, with those obtained by experimental methods. Rittinger, in his classic Aufbereitungskunde (1867)) reached analogous conclusions by way of intricate higher mathematics, for which reason his interesting investigations have remained a sealed book to most of us. The writer hopes that a more elementary treatment of the subject, based in part on Rittinger's metheds, may arouse new interest in the study of basic principles.

Jan 1, 1923

By Theodore Simons

The rapid and comparatively recent development of flotation has opened so fascinating a field for study and research that the older processes of gravity concentration no longer receive the attention they deserve. The early work of Munroel and Richards12 and the more recent contributions by Clevenger and Coe,3 Laist and Wiggin,4 Ammon,5 Bardwell,6 Crowfoot,' and Hayden8 (to mention only some which have appeared in our own Transactions) and by Schu1z,9 have furnished so much data that to offer something new seems a difficult task. It is still possible, however, to present known facts from a different point of view, and, with this in mind, the writer has undertaken to express basic principles of gravity concentration in terms of simple mathematics and mechanics; the conclusions thus reached will be found to correspond, in general, with those obtained by experimental methods. Rittinger, in his classic Aufbereitungskunde (1867)) reached analogous conclusions by way of intricate higher mathematics, for which reason his interesting investigations have remained a sealed book to most of us. The writer hopes that a more elementary treatment of the subject, based in part on Rittinger's metheds, may arouse new interest in the study of basic principles.

Jan 1, 1923

By AIME AIME

IN an address before the New York Section. A.I.M.E., Oct. 20, Alex L. ter Braake, speaking on the tin industry of the Netherlands East Indies, interjected a few remarks, at the chairman's request. on the mineral stock-piling project now before Congress in a bill sponsored by Senator Scrugham. The full text of Mr. ter Braake's paper was published in the Nov. 6 issue of the American Metal Market. Following mention of the buffer stock scheme as applied in the tin industry, Mr. ter Braake continued:

Jan 1, 1943

For convenience, we tabulate below the weight systems contained in the Probierbüchlein: [Pound and centner weights used by merchants for ore, lead, and copper I frother = 20 or 50 centners (depending on locality) I centner (Stolberg & Eisleben) = 112 pounds. I centner (Nuremberg) =100 pounds I pound =2 marks =32 lot =128 quintlein-512 pennyweights =1024 beller I mark -16 lot -.64 quintlein =256 pennyweights = 512 beller 1 lot= 4 quintlein= 16 pennyweights= 32 beller I quintlein = 4 pennyweights= 8 beller I pennyweight = 2 beller Netherlands mintmasters' weights for silver I mark =12 pennyweights=288 grains I pennyweight - 24 grains Assay weights for gold I mark= 24 carats 96 carat-grains. I carat = 4 carat-grains] The assayer's weights were miniature copies of the legal weights of his locality, intended, like the modern assay ton, to eliminate calculation. Each assayer made his own, not usually bothering about a given proportion between the true weights and the assay set, but maintaining the correct ratio between all the weights in any one set. The weights were quite small, to permit the use of less sample, but the exact size is nowhere stated in the Probierbüchlein. Even the legal pound varied considerably from place to place, depending on locality, and assayers would use different factors depending on the sensitivity of their balances, among other things. Agricola makes the assay centner equal to one actual drachma, by which term he means the German quintlein, or 1/12,800 of the full weight of the 100-pound centner. Schreittmann says that the 100-pound centner on the assay scale should be less than half a quintlein, i.e., the factor should be at least 25,600. Biringuccio says the assay centner might

Jan 1, 1949

By R. K. McGeary, B. Lustman

Orientation relationships and rates of annealing of 97 pct cold rolled zirconium have been studied by X-ray techniques, metallography, and by hardness measurements. The process of annealing occurring by the formation of domains, and their subsequent growth without recrystallization, is demonstrated. NUMEROUS investigators1-' have revealed sub-grain formation after annealing cold worked metal single crystals and have generally described the results in terms of a dislocation mechanism of polygonization.5,6 in heavily cold rolled polycrystal-line aluminum the first stages of heating cause an apparently spontaneous subdivision of regions of the deformed matrix into a great number of slightly disoriented domains followed or accompanied by rapid growth of certain domains to form a recrystallization texture.7,8 In the present investigation the isothermal rate of annealing of cold worked polycrystalline zirconium has been studied by X-ray techniques, metallography, and by hardness measurement. It will be shown that, rather than by the usual nucleation and growth mechanism,"12 the process of annealing can best be explained by the formation of domains early in the annealing treatment and the subsequent growth of these domains without recrystallization. Experimental Procedure All the experimental work was performed on an arc-melted ingot of high purity zirconium crystal bar made by Westinghouse in a production scale deBoer unit. The weight percentage of impurities in the zirconium were as follows: C, 0.04; Fe, 0.05; Hf, 0.014; W, 0.01; Ti, Ni, and Al, 0.003; Si and N, 0.002; Cr and Cu, 0.001. Metallographically the zirconium showed only a single phase. The 4 in. diarn ingot was forged at 760°C to a 1 1/2x3 in. plate and was then rolled at 760°C to 0.150 in. thickness and annealed at this temperature for 20 min to produce an equiaxed grain structure of about 0.1 mm average grain diameter. The hot rolled plate was roller-leveled, surface ground to 0.135 in., cold rolled 83 pct reduction in thickness on a two-high mill, and then to a total reduction of 97 pct on a Sendzimir mill. The 0.004 in. strip material so produced received no subsequent mechanical treatment. Specimens % in. square were sheared from the rolled strip and isothermally annealed at 104 mm Hg in an all glass vacuum system equipped with a Vycor furnace tube. The temperature data presented are the average temperatures during the runs and did not vary more than about k3"C. X-ray Diffraction Methods: When zirconium is drastically cold rolled, a high degree of preferred orientation results in which prism poles, {1010}, are perpendicular to the rolling direction. After fully annealing this material an entirely new texture develops which corresponds to a 20" or 40" rotation of the deformation texture about hexagonal axes of

Jan 1, 1954

By J. W. Spretnak, G. W. Cunningham

Grain growth across the bond region in Pressure bonded copper was found to be mainly dependent upon the presence or absence of microvoids, but it was also found that prior history, bonding pressure, bonding time, and bonding temperature are important variables. An increase in pressure, time, or temperature tends to promote grain growth in the interfacial region. Polygonization is observed after pressure bonding except for specimens previously annealed at temperatures on the order of 1800°F or higher. The dislocation density in bonded specimens was found to be greater in the bond region. THE bonding of metals by the application of gas pressure at elevated temperatures is a relatively new process, having been developed over the past 10 years. The technique, as described by Paprocki, Hodge, and Boyer,l is unique in that assemblies of many parts and complex shapes can be bonded with a negligible amount of deformation. The process thus differs metallurgically from pressure welding, cold welding, and recrystallization welding in that deformation occurs only in a microscopic region whereas, in general, the welding requires severe deformation and may extend the contact surface by a factor of 3 to 10 during the welding. From a practical standpoint, pressure welding is not amenable for bonding large surfaces. During the time in which Paprocki and coworkers were deve1oping the process, West2 established aproc-ess,for bonding aluminum to uranium, and Barnes and Maze? developed a gas-pressure-bonding technique for nickel and copper. Recently, Fugardi and Zambro4 have used equipment similar to that developed by Paprocki and coworkers to establish parameters for bonding stainless steel, aluminum, and zirconium. Most of the investigations on pressure bonding have been empirical in nature and, although methods have been developed for bonding such metals as molybdenum, columbium, titanium, zirconium, and stainless steel, the information concerning the mechanism of bonding is limited. Several workers5"7 have studied the pressure bonding of dissimilar metals in order to gain information on diffusion and formation of inter-metallic phases under application of pressure. Clapson and Robbins8 have shown by a series of annealing studies that voids in the interfacial boundary of roll-bonded copper can prevent movement of the boundary until the voids are spaced far enough apart to prevent pinning. They also indicated that recrystallization and grain growth can eliminate the voids. In this paper it is shown that voids are the major detriment to grain growth across pressure-bonded interfaces, but it is also shown that prior history, bonding pressure, bonding time, and bonding temperature are

Jan 1, 1962

By H. Cecil Spicer

THE results described in this article are based on field work conducted during the periods April-May, 1939, and May-July, 1940. The United States Potash Co. is mining potash on Government land under a permit from the Department of the Interior and the geophysical investigation was completed under a cooperative arrangement made between that company and the Conservation Branch of the Geological Survey. The writer, a member of the Section of Chemistry and Physics of the Geologic Branch, was assigned to this investigation. Four definite objectives were in mind for the geophysical work in the studies over the salt deposits. The first was to determine the measure of success that could be attained in this type of work with the resistivity methods that were to be employed. These methods had been introduced into the work of the Conservation Branch by Benjamin E. Jones for the investigation of dam sites, and have been used under his direction by the author for such work. If the method proved to be applicable, an effort was to be made to contour the top of the salt beds and also the other formation boundaries known to be present in this area. Salt-water aquifers were to be studied in an effort to determine their boundaries, and an attempt was to be made to delineate the potash-bearing beds. EARLIER STUDIES Others have made, and reported, resistivity studies over saliferous deposits in different areas. Friedel1 and Messrs. Schlumberger2 reported geophysical work performed in the discovery of the salt domes of Alsace; Carrette and Kelly3described the geology of the same area. Leonardon and Kelly4 published a resistivity curve obtained over the Hettenschlag dome, and a further discussion of this same area was given by the Messrs. Schlumberger5 in a communication. Messrs. Alty6 described studies on salt deposits in which the single-probe method was used. Sinerez7 mentions that electrical methods were tried over salt deposits in Spain. Geoffrey and Charrin8 show a resistivity curve obtained over marl, gypsiferous marl and salt which is similar to that obtained over the New Mexico salt deposits. Kelly9 reported resistivity work performed with the ground comparator of Zuschlag over the salt deposits near Syracuse, N. Y., where the Salina formation is at a depth of 700 to 8oo ft. Some structural studies on the potash basin of Alsace are described by Poldini.10 Another single-probe resistivity study, made over salt deposits in New Mexico, is briefly described by Heiland,11 through the courtesy of Harry Aurand, of the Midwest Refining Co.

Jan 1, 1941

By Joseph Fry, Ralph H. Espach

In the spring of 1943, when it was evident that the Tensleep bandstone in the Elk Basin Field, Wyoming and Montana, held a large reserve of petroleum, Bureau of Mines engineers obtained samples of oil from the bottom of nine wells and analyzed them for such physical characteristics as the volumes. of gas in solution. saturation pressures or bubble points, shrinkage in volume caused by the release of gas from solution, expansion of the oil with decrease in pressure, and other related properties. The composition of the gas in solution in the oil was studied. The pressures and temperatures existing in the reservoir and the productivity characteristics of the oil wells were determined. The data obtained indicate that the oil in the Tensleep Reservoir of the Elk Basin Field has unusually varying physiral characteristics, such as a saturation pressure of 1,250 psia and 490 cu ft of gas in solultion in a barrel of oil at the crest of the structure and a saturation pressure of 530 psia and 134 cu ft of gas in solution in a barrel of oil low on the flanks. The hydrogen sulfide content of the gas in solution in the oil varies from 18 per cent for oil on the crest to 5 per cent for oil low on the flanks of the structure. Of even greater significance is the fact that these and other variable characteristics of the reservoir oil are related to the position of the oil in the structure. Many geologists and petroleum engineers have considered that all the oil in a petroleum reservoir has rather uniform physical characteristics and that equilibrium conditions prevailed in all underground accumulations of oil and gas; that such is not always so is borne out by the results of the study by the writers. INTRODUCTION The Rocky Mountain region is one in which may be found striking examples of the unusual in oil and gas accumulations, as is evident from the following: The high helium content (7.6 per cent) of the gas in the Ouray-Leadville limestone sequence in the Rattlesnake Field, New Mexico, and gases of similar helium content in other fields; 50" to 55' API gravity distillate in solution in carbon dioxide gas and recoverable through retrograde condensation, in the North McCallum Field, Colorado; the occurrence of gas, oil, or both in closely related structures contrary to the usual concepts of gravimetric segregation: the accumulation of gas and/or oil in structures closely related to other structures that apparently are more favorable but do not contain oil or gas accumulations; the high hydrogen sulfide content (as high as 42 per cent) of the gas associated with oil in some fields in the Big Horn Basin, Wyoming; and the wide range of fluid chararteristics found in the Elk Basin reservoir. Elk Basin, an interesting old oil field that has been producing oil from the Frontier formation since 1915, is situated in a highly eroded basin resulting from the erosion of the crest of an anticline and some of the underlying softer shales. The field came back into national prominence during 1943 when it became known that it was the largest single reserve of new oil discovered in the United States that year. The Tensleep sandstone was found to contain oil in November. 1942, when a well drilled to a depth of 4,538 ft (44 ft into the Tensleep sandstone) flowed oil at the rate of 2,500 B/D. By the end of 1949, 137 oil-producing wells and five dry holes had been drilled, and approximately 32 million bbl of oil had been produced. Approximately 6,000 acres may be considered productive of oil in the Tensleep Reservoir, and estimates of the oil that will be produced average 200 million bbl. The Tensleep Reservoir has further interest because it ha-greater closure than any oil field in the Rocky Mountain region; the closure of the Elk Basin anticline is variously estimated at 5.000 to 10,000 ft. of which the top 2.00 ft of the structure contained oil. SUBSURFACE OIL SAMPLING Fig. 1 is a structural map of the Elk Basin Tensleep Reservoir, on which the nine wells used in this study and the numbers correvponding to the well designations hereafter referred to are shown. Wells 1. 2, 3, 4, and 8 were tested and sampled during October and November. 1943. and Wells 5, 6. 7, and 9 during June and July, 1944. An electromagnetic type sampler developed by the Bureau of Mines and described by Grandone and Cook' was used in obtaining the subsurface oil samples. As the wells were tubed nearly to bottom, the sampler was run as far as possible in the tubing hut never below the top perforations. The following procedure was used in testing and sampling the wells: A well was shut in for at least three days, after

Jan 1, 1951

By Joseph Fry, Ralph H. Espach

In the spring of 1943, when it was evident that the Tensleep bandstone in the Elk Basin Field, Wyoming and Montana, held a large reserve of petroleum, Bureau of Mines engineers obtained samples of oil from the bottom of nine wells and analyzed them for such physical characteristics as the volumes. of gas in solution. saturation pressures or bubble points, shrinkage in volume caused by the release of gas from solution, expansion of the oil with decrease in pressure, and other related properties. The composition of the gas in solution in the oil was studied. The pressures and temperatures existing in the reservoir and the productivity characteristics of the oil wells were determined. The data obtained indicate that the oil in the Tensleep Reservoir of the Elk Basin Field has unusually varying physiral characteristics, such as a saturation pressure of 1,250 psia and 490 cu ft of gas in solultion in a barrel of oil at the crest of the structure and a saturation pressure of 530 psia and 134 cu ft of gas in solution in a barrel of oil low on the flanks. The hydrogen sulfide content of the gas in solution in the oil varies from 18 per cent for oil on the crest to 5 per cent for oil low on the flanks of the structure. Of even greater significance is the fact that these and other variable characteristics of the reservoir oil are related to the position of the oil in the structure. Many geologists and petroleum engineers have considered that all the oil in a petroleum reservoir has rather uniform physical characteristics and that equilibrium conditions prevailed in all underground accumulations of oil and gas; that such is not always so is borne out by the results of the study by the writers. INTRODUCTION The Rocky Mountain region is one in which may be found striking examples of the unusual in oil and gas accumulations, as is evident from the following: The high helium content (7.6 per cent) of the gas in the Ouray-Leadville limestone sequence in the Rattlesnake Field, New Mexico, and gases of similar helium content in other fields; 50" to 55' API gravity distillate in solution in carbon dioxide gas and recoverable through retrograde condensation, in the North McCallum Field, Colorado; the occurrence of gas, oil, or both in closely related structures contrary to the usual concepts of gravimetric segregation: the accumulation of gas and/or oil in structures closely related to other structures that apparently are more favorable but do not contain oil or gas accumulations; the high hydrogen sulfide content (as high as 42 per cent) of the gas associated with oil in some fields in the Big Horn Basin, Wyoming; and the wide range of fluid chararteristics found in the Elk Basin reservoir. Elk Basin, an interesting old oil field that has been producing oil from the Frontier formation since 1915, is situated in a highly eroded basin resulting from the erosion of the crest of an anticline and some of the underlying softer shales. The field came back into national prominence during 1943 when it became known that it was the largest single reserve of new oil discovered in the United States that year. The Tensleep sandstone was found to contain oil in November. 1942, when a well drilled to a depth of 4,538 ft (44 ft into the Tensleep sandstone) flowed oil at the rate of 2,500 B/D. By the end of 1949, 137 oil-producing wells and five dry holes had been drilled, and approximately 32 million bbl of oil had been produced. Approximately 6,000 acres may be considered productive of oil in the Tensleep Reservoir, and estimates of the oil that will be produced average 200 million bbl. The Tensleep Reservoir has further interest because it ha-greater closure than any oil field in the Rocky Mountain region; the closure of the Elk Basin anticline is variously estimated at 5.000 to 10,000 ft. of which the top 2.00 ft of the structure contained oil. SUBSURFACE OIL SAMPLING Fig. 1 is a structural map of the Elk Basin Tensleep Reservoir, on which the nine wells used in this study and the numbers correvponding to the well designations hereafter referred to are shown. Wells 1. 2, 3, 4, and 8 were tested and sampled during October and November. 1943. and Wells 5, 6. 7, and 9 during June and July, 1944. An electromagnetic type sampler developed by the Bureau of Mines and described by Grandone and Cook' was used in obtaining the subsurface oil samples. As the wells were tubed nearly to bottom, the sampler was run as far as possible in the tubing hut never below the top perforations. The following procedure was used in testing and sampling the wells: A well was shut in for at least three days, after

Jan 1, 1951

By H. R. Banks

THE Sullivan concentrator has completed 20 years of operation. During this period a considerable amount of data has been accumulated concerning the characteristics of several types of flotation machines in their application to the problem of the differential separation of the lead sulphide, zinc sulphide and, in more recent times, iron sulphide, in the ore from the Sullivan mine. It is the author's intention to sketch briefly experiences encountered when the several types of flotation machines were introduced into the flow. ORIGINAL FLOTATION EQUIPMENT AND ORE The original flotation equipment consisted of four 18-cell lead-roughing machines, whose concentrate was cleaned in an 8-cell and recleaned in a similar 8-cell machine. Zinc concentration was carried out in four 18-cell machines. One 8-cell zinc re-treatment machine received the reground zinc middling. The 168 cells handled some 3000 tons of original daily feed. These cells were of the standard Minerals Separation type, equipped with 24-in. impellers. Spindles were driven through geared line shaft at a speed of 255 r.p.m. The impellers were the 45° type, except for the last three cells of the zinc-rougher machines, which were of sub-aeration type, with full bottom shroud and half shroud for the top side of the impellers. Four-pound air was introduced. This recognition of the benefit of intensified flotation operation for "gleaning" was an important phase in the early operation and will be discussed further on in this paper. Sullivan ore during this period is described as a finely disseminated mixture of four sulphides, totaling 90 per cent made up of 13.6 per cent galena, 14.4 per cent marmatite, 1 per cent pyrite and 61 per cent pyrrhotite. The specific gravity of the ore was approximately 4.4. There has been a gradual change in the ore content. The 10 per cent of nonsulphide constituents has increased to between 15 and 20 per cent and all three sulphides have dropped somewhat. Added equipment and changing technique have made possible the treatment of 8000 tons per day of mill feed instead of the 3000 originally handled. SPECIAL FEATURES OF FLOTATION AT SULLIVAN Sullivan flotation differs greatly from customary practice. The very heavy return of lead rougher middling and lead cleaner tailing, totaling at times 125 per cent of the new feed tonnage, has been the subject of much investigation. The practice is still employed.

Jan 1, 1944

By B. M. Loring, I. R. Krame, F. M. Walters

NO observations on the mechanical properties of man-manganese alloys have been published since pure manganese became readily available, either distilled manganese or electrolytic manganese. The purpose of this investigation was to determine whether iron-manganese alloys are essentially brittle, as reported by Hadfield,' or whether the lack of ductility observed was due to impurities in the alloys that he studied. Experimental Methods The alloys were melted in a roo-lb. high-frequency induction furnace with a magnesia crucible, using ingot iron and electrolytic manganese. The heats were split, the first giving six 18-lb, ingots and the second three. Each successive heat was higher in manganese and about 0.3 per cent silicon was added as ferrosilicon. The alloys forged without difficulty and were given a 9' per Published by permission of the Navy Department. Manuscript received at the office of the Institute June 28. 1941. Issued as T.P. 1369 in Metals Technology. September 1941. * Division of Physical Metallfirgy Naval Roscarch Laboratory. Anacostia Station Washington. D. C. 1 References are at the end of the paper. 4 cent reduction to ¾-in. rounds. The chemical analysis of the alloys is given in Table I. The forged rods were homogenized for 224 hr. at r150°C. (2100°F.) and air-cooled. The alloys were tested in two conditions of heat-treatment: (I) as normalized from 870°C. (1600°F.) and (2) normalized from 870°C. and tempered for I hr. at 540°C. (Iooo°F.) and air-cooled. The tensils specimens were 0.505 in. in diameter with a 2-in. gauge length, and the impact specimens were v-notch Charpy. The proportional limit and yield strength were taken from the stress-strain diagrams drawn by a Peters recorder. The data obtained from the tensile test and the hardness measurements are given in Table 2. Specimens that were normalized are designated by N; those that were normalized and tempered by T. Alloy G was tempered after forging (D).

Jan 1, 1942

By B. M. Loring, I. R. Krame, F. M. Walters

NO observations on the mechanical properties of man-manganese alloys have been published since pure manganese became readily available, either distilled manganese or electrolytic manganese. The purpose of this investigation was to determine whether iron-manganese alloys are essentially brittle, as reported by Hadfield,' or whether the lack of ductility observed was due to impurities in the alloys that he studied. Experimental Methods The alloys were melted in a roo-lb. high-frequency induction furnace with a magnesia crucible, using ingot iron and electrolytic manganese. The heats were split, the first giving six 18-lb, ingots and the second three. Each successive heat was higher in manganese and about 0.3 per cent silicon was added as ferrosilicon. The alloys forged without difficulty and were given a 9' per Published by permission of the Navy Department. Manuscript received at the office of the Institute June 28. 1941. Issued as T.P. 1369 in Metals Technology. September 1941. * Division of Physical Metallfirgy Naval Roscarch Laboratory. Anacostia Station Washington. D. C. 1 References are at the end of the paper. 4 cent reduction to ¾-in. rounds. The chemical analysis of the alloys is given in Table I. The forged rods were homogenized for 224 hr. at r150°C. (2100°F.) and air-cooled. The alloys were tested in two conditions of heat-treatment: (I) as normalized from 870°C. (1600°F.) and (2) normalized from 870°C. and tempered for I hr. at 540°C. (Iooo°F.) and air-cooled. The tensils specimens were 0.505 in. in diameter with a 2-in. gauge length, and the impact specimens were v-notch Charpy. The proportional limit and yield strength were taken from the stress-strain diagrams drawn by a Peters recorder. The data obtained from the tensile test and the hardness measurements are given in Table 2. Specimens that were normalized are designated by N; those that were normalized and tempered by T. Alloy G was tempered after forging (D).

Jan 1, 1942

By R. P. Agarwala, M. S. Anand

Using residual activity technique, the diffusion of palladium, silver, cadmium, indium, and tin in alunzinum has been studied in the temperature range of 400" to 630°C. The diffusivities (in units of square centimeters per second) have been expressed as: IMPURITY diffusion in aluminum,1-9 silverand lead5 for cases of low solid solubility of the impurity in the host metal has yielded frequency factors in the range of l0-6 to l0-9 sq cm per sec whereas the activation energy is practically half the self-diffusion activation energy value. From the observed values of frequency factor, activation energy, and entropy of activation, it has been suggested' that these solutes are not diffusing by vacancy or interstitial mechanisms but by a mechanism which should be consistent with such low values of the diffusion parameters (Do and Q). However in spite of extensive work on these types of systems, the mechanism of diffusion is still not well understood. The present investigation on the diffusion of palladium, silver, cadmium, indium, and tin in aluminum has been carried out to throw further light on the diffusion mechanism in systems, where the solid solubility is very low (except for the case of silver). The results are discussed on the basis of solid solubility and the structural changes involved owing to the presence of the solutes in aluminum solid solution. An attempt has also been made to apply the existing theories of charge5-8 and size8 difference between the solute and the solvent. EXPERIMENTAL PROCEDURE Specimens (1/2 in. diam by 3/8 in. high) were machined out of pure aluminum (99.995 wt pct) rod obtained from Johnson Mattheys. They were sealed under vacuum in quartz tubes and annealed at 620° C for several hours; the grains thus developed were sufficiently large to eliminate the possibility of diffusion along the grain boundaries. The flat ends were prepared carefully after polishing as described previously,10 Radioactive nitrates of cadmium, indium, and tin and chloride of palladium containing, respectively, cd115, 1n114, sn113, and pd103 were dissolved in distilled water and mixed with 30 pct acetone. By means of a micropipet a drop of this solution was placed on a smoothly polished and lightly etched surface of the specimen. Due care was taken to see that the solution spread uniformly on the surface of specimen without trickling down its sides. Radioactive silver was elec-trodeposited using a AgCN-KCN bath. The amount of sample deposited in all the cases was not more than 0.1 µ thick. The samples were then sealed in quartz tubes in vacuum. The cadmium samples were sealed in a purified argon atmosphere to avoid evaporation. The samples were then diffusion-annealed. The temperature of annealing varied between 400° and 630°C and was controlled to ±5°C. On heating to -400°C,the deposits of cadmium, indium, and tin, which were of the order of 0.1 p in thickness, were converted to their respective oxides. The contribution of oxygen present in the lattice of aluminum due to these oxides has been calculated and found to be less than 10 ppm in all cases. Oxide method has already been used by other workers11'12 in diffusion studies without any controversy on the issue. However, in some of these investigations, metallic deposition was also tried. The diffusivities calculated from these measurements were found to agree very well with the diffusivities obtained by using the oxide method. Thus it is assumed that the measured diffusivities represent true diffusion coefficients. Since palladous chloride decomposes at about 500°C, the deposited samples which were to be diffusion-annealed below 500°C were heated in vacuum for a very short time at 500°C to allow the decomposition of palladous chloride to palladium metal. Time taken in decomposition of nitrates to oxides and chloride to metal was negligibly small as compared to the period of the diffusion anneals. The residual activity technique13 was used to study the diffusion profiles where thin layers from the specimen surface were removed by grinding it parallel to a flat surface on a 600-grade carborundum paper. The specimen was washed, dried, and weighed, the differ -ence of the weight being the measure of the thickness of the layer removed. After each such abrasion and weighing, the total residual activity on the surface of the specimens was measured by counting 0.656, 0.94,

Jan 1, 1968

By D. C. Hilty, W. Crafts

The solubility of oxygen in iron containing aluminum has been determined at 1550°, 1600°, and 1650°C and found to be much higher than predicted from theoretical considerations, possibly due to equilibria with an iron-aluminum spinel phase rather than pure AI,O.. The presence of manganese greatly increased the deoxidizing power of aluminum. DEOXIDATION and inclusion formation in steel have proved to be elusive phenomena that are difficult to control in spite of much effort to understand and evaluate the reactions. Study of the problem indicated that more accurate data on the solubility of oxygen in iron containing deoxidizers were essential to further progress, and an empirical determination of oxygen solubilities has been initiated at the Union Carbide and Carbon Research Laboratories, Inc. The investigation has included the effects of aluminum, silicon, manganese, and combinations of these elements at 1550°, 1600°, and 1650°C. The equipment and experimental procedure as well as the results of a study of the effects of aluminum are described below. In general, it was found that the solubility of oxygen in iron containing aluminum is much higher than predicted, possibly because of the formation of complex nonmetallic phases, and that manganese greatly increases the deoxidizing power of aluminum. The generally accepted deoxidation curves for 1600°C are summarized in fig. 1, from "Basic Open Hearth Steelmaking"'. These curves are assumed to represent the solubility of oxygen in the presence of deoxidizers and should indicate the limits of mis-cibility gaps in the phase diagrams of the systems that control the formation and character of non-metallic inclusions as described by Benedicks and Lofquist'. They were derived mainly by application of the methods of thermodynamics to the available experimental observations, and by calculations based on the thermal constants of the pure substances when experimental data were lacking. Among the more notable researches contributing to the development of knowledge of oxygen solubilities are those of Korber and Oelsen8, 4, C. H. Herty, Jr. and associates5,6, Krings and Schackmann7, Went-rup and Hieber8 Schenck and Briiggeman9, Vacher and Hamilton'" and Chipman and co-authors 1,11,12,13 Practically, the deoxidation curves are of limited value in predicting oxygen content and rationalizing deoxidation practices. The reasons for this inadequacy appear to be error from inaccurate data, oversimplifying assumptions, interacting effects of combined deoxidizers, and possibly unknown extra-equilibrium and side reactions. Although inclusion formation is a very complex reaction it must be re-

Jan 1, 1951

By J. L. Huitt, IM. L. Slusser, E. E. Glenn, M. L. Slusser

This paper is concerned with: (1) an analysis and interpretation of the filtration characteristics of drilling muds on filter paper, and (2) an interpretation of early stage "filtration" on consolidated synthetic porous media, herein referred to as the "surge loss" period. It is shown that water-loss data can be plotted so as to disclose the existence of a surge period, a non-uni-form cake thickness period, and a constant pressure filtration period. The same periods occur during exposure of consolidated porous media to muds. The data on consolidated porous media indicate that: (1) mud particles bridge pores inside porous media during the surge period, and (2) "filter cake" build-up inside porous media occurs during subsequent filtration. The data also show that the surge loss increases with sample permeability and with pressure differential. INTRODUCTION The phenomenon of mud filtrate invasion into porous sands of a drilling well has been recognized for many years.1,2,3,4 Part of API Code 29 is concerned with the filtration testing of a drilling mud to yield data on this subject. In a number of investigations "plastering properties" of muds were studied,5,6,7,8 "plastering" apparently meaning cake forming properties. In such studies the characteristics (thickness, permeability, and toughness) of the cake and the rate at which the liquid phase of the mud was separated from the solids (filtration rate through the cake, commonly referred to as water loss) were measured or at least considered. From the standpoint of its effect on well productivity, filtrate invasion into "clean" water-wet pay sands (i.e., those containing no clay minerals) may not necessarily be a serious problem. An increase in water saturation in the zone immediately around the wellbore would cause loss of oil permeability. However, in such a system, much of this water may be removed by oil production. If filtration occurs into "dirty" sands (i.e., those containing appreciable clay minerals), clay swelling or other mechanisms may cause losses in oil permeability which cannot be overcome by oil production.'.' The phenomenon of mud particle invasion into the pay sand of a drilling well was considered to be a possible serious factor in the early days of rotary drilling. Opinions varied as to whether drilling fluids "mudded up" and "sealed" oil sands. In 1932 Rubel,9 Gill,10 and Parsons," in separate papers, presented differences of opinion together with some laboratory and field data concerning loss of oil production caused by drilling fluid invasion into pay zones. These papers, and the discussions, furnish a large background on this subject and indicate the very clear thinking of many men at a time when petroleum production technology was in its infancy. Jones and Babson,6 and Silent,' experimentally found that the depth to which mud particles invaded water-saturated sand packs was small (no greater than 1/16 in). Arn-quist12 in 1937 observed loss of water permeability due to invasion of mud particles into water-saturated, consolidated, sandstone samples. Williams and Cannon5 studied the filtra-tion properties of drilling muds and mentioned "sludge" which penetrated a short distance into the water-saturated filtering medium (sand pack). Byck5 concluded that formation permeability had no effect on the plas-

Jan 1, 1958

By Gerald Edmunds, M. L. Fuller

The development of "fiber" or preferred orientations, during the plastic deformation of metals, and the relation of such structures to the anisotropic characteristics of worked metals has become a subject of common knowledge among metallurgists. Very little has been published, however, relative to variations existent throughout the cross-sections of rolled strips,1 and the influence that such variations may have. This paper presents such a study on a rolled zinc alloy.2 The significance of small differences in surface structure is shown in relation to bending properties. Experience with zinc and its alloys has shown that the outer radius of the bend, which is subject to tensile deformation, is the common region of failure. In considering relations of structural characteristics to bending properties it will suffice, therefore, to consider the ease and possible extent of tensile deformation resulting from various orientations. It is necessary in this connection to assume that on the average the individual crystals of a polycrystalline material act substantially as if their movements were unobstructed by the surrounding grains. This assumption is not strictly valid, but the error involved is unlikely to affect seriously the qualitative conclusions derived from its use. The mechanism of the plastic deformation of zinc crystals has been described by Mark, Polanyi and Schmid3 and by Mathewson and Phillips14 and is regarded as being accomplished by block movements or * Investigator, Rolling Mill Section, Research Division, New Jersey Zinc Co. f Investigator, X-ray Laboratory, Research Division, New .Jersey Zinc Co. 1 Variations of structure throughout the cross-section of wire have been reported in the literature. 2 This alloy contained, in addition to zinc, 1.0 per cent copper and 0.01 per cent magnesium. Its crystal form is hexagonal close packed, the sarne as that of pure zinc. 3 H. Mark, M. Polanyi and E. Schmid: Vorgange bei der Dehrlung von Zink-kristallen. Zlsch. f. Phys. (1922) 12, 58. 4 C, H. Mathewson and A. J. Phillips: Plastic Deformation of Coarse-grained Zinc. Proc. Inst. Met. Div., A. I. M. E. (1927) 143. C. H. Mathewson: Twinning in Metals. Proc. Inst. Met. Div., A. I. M. E. (1928) 7. The results of a further study of plastic deformation of zinc as related to twin-

Jan 1, 1932

By H. Cecil Spicer

THE results described in this article are based on field work conducted during the periods April-May, 1939, and May-July, 1940. The United States Potash Co. is mining potash on Government land under a permit from the Department of the Interior and the geophysical investigation was completed under a cooperative arrangement made between that company and the Conservation Branch of the Geological Survey. The writer, a member of the Section of Chemistry and Physics of the Geologic Branch, was assigned to this investigation. Four definite objectives were in mind for the geophysical work in the studies over the salt deposits. The first was to determine the measure of success that could be attained in this type of work with the resistivity methods that were to be employed. These methods had been introduced into the work of the Conservation Branch by Benjamin E. Jones for the investigation of dam sites, and have been used under his direction by the author for such work. If the method proved to be applicable, an effort was to be made to contour the top of the salt beds and also the other formation boundaries known to be present in this area. Salt-water aquifers were to be studied in an effort to determine their boundaries, and an attempt was to be made to delineate the potash-bearing beds. EARLIER STUDIES Others have made, and reported, resistivity studies over saliferous deposits in different areas. Friede1 and Messrs. Schlumberger2 reported geophysical work performed in the discovery of the salt domes of Alsace; Carrette and Kelly3 described the geology of the same area. Leonardon and Kelly4 published a resistivity curve obtained over the Hettenschlag dome, and a further discussion of this same area was given by the Messrs. Schlumberger5 in a communication. Messrs. Alty6 described studies on salt deposits in which the single-probe method was used. Sinerez7 mentions that electrical methods were tried over salt deposits in Spain. Geoffrey and Charrin8 show a resistivity curve obtained over marl, gypsiferous marl and salt which is similar to that obtained over the New Mexico salt deposits. Kelly9 reported resistivity work performed with the ground comparator of Zuschlag over the salt deposits near Syracuse, N. Y., where the Salina formation is at a depth of 700 to B00 ft. Some structural studies on the potash basin of Alsace are described by Poldini.10 Another single-probe resistivity study, made over salt deposits in New Mexico, is briefly described by Heiland,11 through the courtesy of Harry Aurand, of the Midwest Refining Co.

Jan 1, 1941

By L. D. Clark, S. S. Saluja

A physical law, governing the rupture of rock by confined explosive charge correspondent to current expressions for determining weight of charge to rupture rock burden, W, was developed in the form Q = cVw3 by two early investigators performing unique experiments with ice. The coefficient C, is found by trial blast. Recent physical tests conducted with rock, synthetic materials and ice to establish the validity of the theory on which it and other related formulae are based indicated: (a) that failure under hydrodynamic impact pressure is by tension rather than shear as was assumed; (b) that the fundamental law of mechanics, enabling the determination of Q = cvw3, modified to the form P = R x Sa x Wb is valid when low velocity explosives are used; (c) that rock breakage under the action of low velocity explosives is entirely due to explosion gas pressure, as was believed; (d) that under the action of high velocity explosive it is due to the joint effects of scabbing and gas pressure; and that further possible modification could make the above equation also applicable to these joint mechanisms. shape could be easily frozen and because large loads would not be required. They found: (a) that the not unfamiliar shearing equation for metals was applicable to ice where P = load in lb; S = periphery of pressure surface, in.; W = burden, in.; K = modulus of rupture by shear in lb per in.2; and (b) that "the form of cavity produced by the application of gradual pressure is similar to that obtained by blasting in rock under similar conditions of free face and pressure surface!" This similarity in crater shapes leads to the conclusion that rock would rupture by shear, as did ice, and its behavior under the force of a blast could be governed by such a relationship as P = S x W x K. Three important interrelated empirical expressions were derived and rock, charging and spacing coefficients C,, C, and e were established and substantiated by trial blasts. In checking the accuracy of the main assumptions, duplication of the ice tests, substituting rock, suggested that K is not constant and that P = K x W x S, though valid for ice, does not necessarily hold for homogeneous limestone.' Conclusions from this later work raised questions making continued investigation desirable because such conclusions do not destroy the practical value of the empirical equations or theory. Further study for the establishment of the relationship between load, burden and periphery of the pressure surface and possible application of these to the mechanism of rock blasting was undertaken by the authors of this paper. MECHANICAL TESTING - EXPERIMENTAL PROCEDURE Certain inconsistencies in the results of the aforementioned tests repeated on three types of limestone suggested these inconsistencies be attributed to rock inhomogeneity. It was also suspected that the loading speed, which could not be held uniform, may have contributed. The earlier work with both rock and ice

Jan 1, 1964