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By Clarence F. Zeuch

Mr. Shaw's work showed the dodecyl mercaptan as a very good collector compared with other collectors on Cu-Mo ores, Mo ores, and for Au and Au-Ag ores plus Pt ores. However, as one who has had extensive experience on Cu-Mo ores, the work is not complete in making only a rougher concentrate with a collector; the work must be carried on in making a Cu-Mo separation. Did Mr. Shaw do any of this work? Before trying the dodecyl mercaptan as a Cu-Mo collector for the Cu-Mo ore it would be well to have any new work conducted knowing how the reagent acts on the Mo. Will it allow a good separation? The use of the collector at Palabora was also mentioned. From some earlier literature I thought that the reagent has been used as an oxide Cu collector after the sulfide mineral was floated out. I thought the pH at this point was about 1.5-3.0. I would like to have this point clarified.

Jan 1, 1982

By S. H. Williston

IT not often that bore hole surveys can be checked by actual. civil engineering methods. A recent Arizona survey was checked by normal surveying methods and the comparison of the results should be of value to both oil and mining men. During the summer of 1948 the Phelps-Dodge Corporation, at its Copper Queen property near Bis-bee, Ariz., drilled a 1245 ft, 8 in. diarn, churn drillhole in a mineralized area and cased part of it, intending to use it to transfer mill tailings for stope fill. The hole, as frequently occurs, was not straight, and, in endeavoring to locate the bottom in the underground workings, they found no evidence of the hole at the underground coordinates directly below the surface location. The noise of the drilling tools was reasonably clear, but the direction of sound was uncertain. Preliminary tests with available equipment were not successful in locating the bottom of the hole. Because of the mineralized character of the area and the fact there was some casing in the hole, any magnetic method of well surveying would give results of doubtful value. Sperry-Sun gyroscopic well-surveying instruments were finally used to locate the bottom of the hole. These instruments consist of a gyroscope to determine azimuth and either a pendulum or bubble inclino-meter. A multiple shot camera photographs both instruments on a single film and superimposes the photograph of a watch. Coordination of depth with time at the surface makes it possible to select the corresponding picture for any depth. After making several runs of the empty instrument housing from the top of the hole to the bottom to make sure there were no obstructions in the hole, three surveys on wire line were completed during the afternoon. The three surveys, in which readings were taken at different points in the hole on each survey, were computed and gave the following locations of the bottom of the hole in relation to the surface collar: survey No. 1—24.92 N, 30.30 W; survey No. 2—24.24 N, 31.11 W; survey No. 3—26.54 N, 27.72 W. Then the data from the three surveys were combined into a single set of calculations which gave a location for the bottom of the hole: combined surveys—24.27 N, 30.16 W. (Fig. 1.) Immediately upon the determination of the coordinates at the bottom of the hole, a drift on the 1300 ft level was started toward the indicated loca- tion some 38 ft northwest of the coordinates of the surface location, The bottom of the hole was located within the drift round in which it was expected, and the transit survey run to the actual location of the hole indicated N 27.18, W 29.71. This shows a discrepancy between the well survey and the transit survey of 0.45 ft in the westerly direction and 2.91 ft in the northerly direction. All surveys, both gyroscopic and transit, fell well within the width of an ordinary drift. While this is satisfactory for almost any and all mining requirements, a theoretical examination was made as to reasons for the discrepancy. A study of the course of the hole indicates that considerable right turn or spiral existed, and in all probability the surveying instrument was pulled out of alignment while traversing the turn by approximately 0.05 ft at the top and another 0.05 ft in the opposite direction at the bottom of the instrument. If such an allowance were to be made, the survey calculations would almost exactly correspond with those determined by transit. This sort of discrepancy would be minimized by the use of stabilizing guides. It is unfortunate that physical laws probably effectively prevent the use of gyroscopic instruments in EX and AX diamond drill holes. The directive power of a gyroscope falls off inversely at some rate between the third power and the sixth power of the diameter. Present instruments can be run in casing 53/4 in. ID or over and might be adapted to somewhat smaller diameters, but the difficulty of reducing these diameters to 11/4 in. or 2 in. is almost insurmountable at the present time. Acknowledgment The author wishes to express his appreciation to the Phelps-Dodge Corporation for permission to publish this article, and to the Operating and Engineering Departments for their cooperation on the survey; also to Donald Hering, of the Sperry-Sun Well Surveying Co., who actually made the survey and calculated the results.

Jan 1, 1951

By S. H. Williston

IT not often that bore hole surveys can be checked by actual. civil engineering methods. A recent Arizona survey was checked by normal surveying methods and the comparison of the results should be of value to both oil and mining men. During the summer of 1948 the Phelps-Dodge Corporation, at its Copper Queen property near Bis-bee, Ariz., drilled a 1245 ft, 8 in. diarn, churn drillhole in a mineralized area and cased part of it, intending to use it to transfer mill tailings for stope fill. The hole, as frequently occurs, was not straight, and, in endeavoring to locate the bottom in the underground workings, they found no evidence of the hole at the underground coordinates directly below the surface location. The noise of the drilling tools was reasonably clear, but the direction of sound was uncertain. Preliminary tests with available equipment were not successful in locating the bottom of the hole. Because of the mineralized character of the area and the fact there was some casing in the hole, any magnetic method of well surveying would give results of doubtful value. Sperry-Sun gyroscopic well-surveying instruments were finally used to locate the bottom of the hole. These instruments consist of a gyroscope to determine azimuth and either a pendulum or bubble inclino-meter. A multiple shot camera photographs both instruments on a single film and superimposes the photograph of a watch. Coordination of depth with time at the surface makes it possible to select the corresponding picture for any depth. After making several runs of the empty instrument housing from the top of the hole to the bottom to make sure there were no obstructions in the hole, three surveys on wire line were completed during the afternoon. The three surveys, in which readings were taken at different points in the hole on each survey, were computed and gave the following locations of the bottom of the hole in relation to the surface collar: survey No. 1—24.92 N, 30.30 W; survey No. 2—24.24 N, 31.11 W; survey No. 3—26.54 N, 27.72 W. Then the data from the three surveys were combined into a single set of calculations which gave a location for the bottom of the hole: combined surveys—24.27 N, 30.16 W. (Fig. 1.) Immediately upon the determination of the coordinates at the bottom of the hole, a drift on the 1300 ft level was started toward the indicated loca- tion some 38 ft northwest of the coordinates of the surface location, The bottom of the hole was located within the drift round in which it was expected, and the transit survey run to the actual location of the hole indicated N 27.18, W 29.71. This shows a discrepancy between the well survey and the transit survey of 0.45 ft in the westerly direction and 2.91 ft in the northerly direction. All surveys, both gyroscopic and transit, fell well within the width of an ordinary drift. While this is satisfactory for almost any and all mining requirements, a theoretical examination was made as to reasons for the discrepancy. A study of the course of the hole indicates that considerable right turn or spiral existed, and in all probability the surveying instrument was pulled out of alignment while traversing the turn by approximately 0.05 ft at the top and another 0.05 ft in the opposite direction at the bottom of the instrument. If such an allowance were to be made, the survey calculations would almost exactly correspond with those determined by transit. This sort of discrepancy would be minimized by the use of stabilizing guides. It is unfortunate that physical laws probably effectively prevent the use of gyroscopic instruments in EX and AX diamond drill holes. The directive power of a gyroscope falls off inversely at some rate between the third power and the sixth power of the diameter. Present instruments can be run in casing 53/4 in. ID or over and might be adapted to somewhat smaller diameters, but the difficulty of reducing these diameters to 11/4 in. or 2 in. is almost insurmountable at the present time. Acknowledgment The author wishes to express his appreciation to the Phelps-Dodge Corporation for permission to publish this article, and to the Operating and Engineering Departments for their cooperation on the survey; also to Donald Hering, of the Sperry-Sun Well Surveying Co., who actually made the survey and calculated the results.

Jan 1, 1951

By M. S. Azun

M.S. Azun I have many objections to the content of the author's paper. Before discussing it, however, I would like to repeat the property of semivariogram function. Second order stationary properties of regionalized variables (ReV's) such as semivariogram function ?(h) are perfectly known in geostatistics. Also, the kriging equations in the language of mathematical statistics using second order stationary properties are well understood. However, the way to use the sample (estimated) semivariogram function in any one of the kriging procedures is vague. The sample semivariogram function is given as follows: [1 N-hy*(h) = 2(N h) i21 {Xi-Xi+h}Z, h=0, 1, N-1] where N is the total number of samples, Xi is the sample value at the i - th location, X i+h is the sample value at the i +h - th location, and h is the distance among the samples. An estimation variance of sample semivariogram function of first lag is smaller than that of higher order lag. The theoretical semivariogram function reaches the variance of samples asymptotically. But this is not easily observable because of the larger variation involved in the estimate of semivariogram function. In general, an estimation procedure is done for h = 0, 1, 2,…., up to the greatest integer less than N/2, even though sample semivariogram function can be computable through N-1. After estimating semivariogram function, the critical question of how to model sample semivariogram function arises. As seen in the above equation, sample semivariogram function is discrete and can be smoothed by the model being selected. Therefore, modeling of sample semivariogram function is the most important step in geostatistics. It not only smoothes a discrete function but also affects the results of the kriging procedure. When the only aim is to model the semivariogram function, which is the basic point of the author's paper, one can employ any fitting techniques, such as curve fitting, or any ar¬bitrary functions, which are called submodels in the paper. The term "arbitrary function" is used rather than "submodel" because there is no basic understanding of developing them. The author suggests that the sum of those submodels can also be used for the modeling of sample semivariogram function. The combination of any arbitrary functions brings many problems instead of giving an insight of the domain structure considered. The author used two arbitrary functions and the nugget effect in response to sample semivariogram function (Fig. 10). For the same example, he stated that the parameters involved in the mixed arbitrary function model can be accepted when the discrepancy between sample semivariogram function and the model is small visually. For verifying the fitting behavior of any selected model, one should not be contented with the visual satisfactory. Some statistical measure such as goodness of fit has to be used. The author's practice is no more than an exercise in curve fitting without any fundamental understanding or conceptualization of the underlying physical mechanism. Furthermore, the selection of any model is not an easy task if the purpose is the search for the "best" response to the observed second order properties of ReV's. I suggest that the Markovian model (Azun, 1983), on the basis of a theoretical understanding of underlying mechanism, which gives more information about the occurrence of regionalized variables, is used to respond all properties of ReV's. There are a lot of problems for modeling of onedimensional sample semivariogram function. Thus, it is not appropriate to go to higher order dimensional sample semivariogram function modeling. In the meantime, I would recommend that one can connect the values of standardized sample semivariogram function rather than simple values of semivariogram function in the two-dimensional estimation. The standardized values can be computed in dividing the semivariogram function value by the number of sample pairs involved in each lag regardless of the directions. In conclusion, geostatistics is an interdisciplinary area in mining that uses the principles of mathematical statistics. Thus, it should not violate any probabilistic and statistical rules. When Matheron was developing the theory of geostatistical study in the early years of geostatistics, many mining people had a reservation accepting the geostatistical tools. However, this does not mean that we, the geostatisticians, might try to convince those people using some "strange" tools or rules as some authors implied (Baafi and Kim, 1984). Instead, we have to develop and explain the geostatistical tools staying only in the framework of statistical concepts and properties. ? References Azun, M.S., 1983, "Stochastic Process Modeling of Spatially Distributed Geostatistical Data," Columbia University, Ph.D. Thesis. Baafi, E.Y., and Kim, Y.C., 1984, "Discussion - Comparison of Different Ore Reserve Estimation Methods Using Conditional Simulation," Mining Engineering, Vol. 36, No. 3, p. 280. Reply by J.M. Rendu The interactive method proposed by Rendu allows practitioners to develop semivariogram models that take into account not only the numerical information obtained by sampling, but also highly significant additional information that often cannot be quantified. The geology of the deposit - including hypotheses concerning its genesis, sampling methods, assaying methods, and mathematical methods used to calculate the semivariograms - all have an influence on the numerical results obtained and on how these results should be interpreted. If all the information concerning the spatial distribution of values in a mineral deposit was contained in the sample values, it could be argued that statistical techniques alone would produce optimum models. However, this is rarely, if ever, the case. Methods that allow the user to take into account his experience and his geologic understanding of the deposit should not be rejected for the sake of theoretical statistical purity. ?

Jan 1, 1986

By Thomas R. Stauffer

The principle that conventional schemes for taxing petroleum or mineral resources are "inefficient" is illustrated using simulation calculations tested against an "ideal" system. Inefficiency is defined as the relative success in maximizing expected government revenues from the resources. Most systems fail because: 1) they leave oil in limbo, i.e. unproduced because of excessive fiscal burden; or 2) they unnecessarily increase the variance in the explorationist'c, rate of return by undertaxing large fields and overtaxing smaller but infra-marginal fields. This increases his discount rate and reduces taxable surplus. An "ideal" tax system is specified which maximizes government revenues while minimizing risk to the operator. Two criteria are developed: 1) the tax falls to zero on fields which yield only the minimum necessary rate of return ("marginal" fields); and 2) the after-tax present value of all fields is the same for all fields above a threshhold size. In particular, marginal fields, while contrib- uting little to expected values, do contribute to reducing variance and hence risk praemia by distributing the exploration costs over a higher probability of successful outcomes.

Jan 1, 1982

By H. H. Hausner, O. V. Roman, F. V. Lenel, G. S. Ansell

The radial shrinkage during sintering of cylindrical compacts and loose aggregates of copper powder was measured. It was found to be nonuni-form from top to bottom of the samples and to depend upon the method of supporting them. The non-uniformity is due to the effect of gravity forces during sintering. Since gravity has an effect in sintering without externally applied stresses, no sharp dividing line can be drawn between conventional sintering and hot pressing. RECENT investigations of the sintering behavior of compacts1 and of loose powder aggregates2 have indicated that forces, other than those arising from surface tension effects, may play a role in shrinkage. In compacts it was shown that residual stresses from the pressing operation influence shrinkage behavior. In loose powder aggregates gravity forces due to the weight of the powder affect the ratio of shrinkage in the vertical and the horizontal direction. The main effort in the work reported here was to show that gravity plays a role also in the sintering of compacts. A few additional experiments were made confirming the effect of gravity in the sintering of loose powder aggregates. EXPERIMENTAL PROCEDURE Compacts and loose powder aggregates were prepared from irregularly shaped, electrolytic copper powder. Prior to use the powders were reduced 30 min at 400°C in dry hydrogen to remove surface oxides. Then the -325 mesh size fraction was separated from the -100 + 325 mesh fraction. The compacts were pressed at a pressure of 10,000 psi from 50 g of powder in a hardened steel die, 1 in. in diam. The height of the compacts was 0.725 i 0.005 in. An effort was made to get as uniform a green density distribution in the compacts as possible. The walls of the die were lubricated with a suspension of 3 pct of zinc stearate in acetone and the compacts were pressed using double action by first pressing the powder at 1200 psi with the die barrel supported, then removing the sup- ports and pressing to final pressure of 10,000 psi with the die barrel floating. The pressure was maintained for 10 sec. The compacts were sintered at a temperature of 925°C, generally for 1 hr. In order to maintain uniform temperature they were sintered in boats made from cylindrical copper blocks. The blocks were 2 in. in diam, either 2 or 2 1/2 in. long and, split to form the body of the boat and a lid. The body of the boat contained a cavity 1 3/8 in. wide, 1 in. deep and either 2 1/8 or 1 3/8 in. long. The longer cavity accomodated two samples, the shorter one only one sample. The uniformity of temperature distribution within the boats was checked with thermocouples welded to the top and bottom of the samples. The maximum variation between top and bottom temperatures was i 1/2°C. The actual sintering temperature was held constant within ±2°C. In order to determine the effect of gravity forces, i.e., the weight of the compacts, upon shrinkage, they were supported in the following ways during sintering: a) Full Bottom Support. The compacts rested either on a flat alundum disk or on alundum powders. b) Partial Bottom Support. The compacts rested on a graphite cylinder, 0.3 in. in diam which formed a projection on a larger graphite disk. It is difficult to balance the compact on the small projection. To avoid having the compact tip, a small hole was drilled through the compact and through the graphite disk and its projection. The graphite disk was then suspended from the lid of the boat by a thin iron wire which passed through the holes in the disk and the compact. c) Top Support, first type. A hole 3/32 in. in diam was drilled diametrically through the green compact 3/16 in. from the top of the compact. The compact was sintered suspended from an alundum rod (thermocouple protection sleeve) inserted into the hole. d) Top Support, second type. A hole was drilled axially through the center of the compact. The upper part of the hole from the top surface of the compact one fourth of the way down was 1/16 in. in diam; the lower part of the hole from the bottom surface three fourth of the way up was 3/32 in. in diam. The compact was suspended from the lid of the boat by an iron wire passing through the upper part of the hole and then tied into a knot. The loose powder aggregates were made by filling l in. deep, l in. diam cylindrical graphite molds with -325 mesh powder. To achieve uniform density in all the loose powder aggregates, the powders were settled in the molds by placing the

Jan 1, 1963

By Alwyn Birchmore Cox, Ian William Wark

Different parts of the world in which mineral separation by flotation is practiced experience vastly different natural temperatures, and in some districts there is a big difference between summer and winter temperatures. It will be shown in this paper that the temperature is of considerable importance where it is desired to separate pyrite or arsenopyrite from other minerals. It is probable that some of the differences obtained in the flotation of these minerals at plants working under otherwise similar conditions are due to temperature variations. The influence of temperature on the flotation of galena, chalcopyrite and sphalerite by xanthates is less marked than its influence on pyrite flotation. Experimental Method The methods used have been described previously.l-4 In each test the clean mineral specimen was immersed in a solution prepared by adding the reagents in the following order: (1) sodium carbonate and hydrochloric acid as necessary to buffer the solution and to give approximately the pH value desired, (2) sodium cyanide, (3) copper sulphate, (4) ethyl xanthate, followed by (5) a final adjustment of pH value. After ½ hr. the mineral was tested for a xanthate film by bringing a bubble of air into apparent contact with the submerged polished surface. If true contact (spreading) was not obtained within ½ min. and after cleaning the surface by wiping with a small linen pad, it was concluded that the adsorption of a xanthate film had been prevented. Following the method already described (ref. 2), curves have been constructed such that for a solution composition corresponding to any point below the curve, contact between mineral and air is possible, whereas for a solution composition corresponding to any point above the curve, contact is impossible.

Jan 1, 1939

By William Ian Wark, Alwyn Birchmore Cox

DIFFERENT parts of the world in which mineral separation by flotation is practiced experience vastly different natural temperatures, and in some districts there is a big difference between summer and winter temperatures. It will be shown in this paper that the temperature is of considerable importance where it is desired to separate pyrite or arsenopyrite from other minerals. It is probable that some of the differences obtained in the flotation of these minerals at plants working under otherwise similar conditions are due to temperature variations. The influence of temperature on the flotation of galena, chalcopyrite and sphalerite by xanthates is less marked than its influence on pyrite flotation. EXPERIMENTAL METHOD The methods used have been described previously.1-4 In each test the clean mineral specimen was immersed in a solution prepared by adding the reagents in the following order: (1) sodium carbonate and hydrochloric acid as necessary to buffer the solution and to give approximately the pH value desired, (2) sodium cyanide, (3) copper sulphate, (4) ethyl xanthate, followed by (5) a final adjustment of pH value. After ½ hr. the mineral was tested for a xanthate film by bringing a bubble of air into apparent contact with the submerged polished surface. If true contact (spreading) was not obtained within ½ min. and after cleaning the surface by wiping with a small linen pad, it was concluded that the adsorption of a xanthate film had been prevented. Following the method already described (ref. 2), curves have been constructed such that for a solution ' composition corresponding to any point below the curve, contact between mineral and air is possible, whereas for a solution composition corresponding to any point above the curve, contact is impossible.

Jan 1, 1938

By Ian William Wark, Alwyn Birchmore Cox

Different parts of the world in which mineral separation by flotation is practiced experience vastly different natural temperatures, and in some districts there is a big difference between summer and winter temperatures. It will be shown in this paper that the temperature is of considerable importance where it is desired to separate pyrite or arsenopyrite from other minerals. It is probable that some of the differences obtained in the flotation of these minerals at plants working under otherwise similar conditions are due to temperature variations. The influence of temperature on the flotation of galena, chalcopyrite and sphalerite by xanthates is less marked than its influence on pyrite flotation. Experimental Method The methods used have been described previously.l-4 In each test the clean mineral specimen was immersed in a solution prepared by adding the reagents in the following order: (1) sodium carbonate and hydrochloric acid as necessary to buffer the solution and to give approximately the pH value desired, (2) sodium cyanide, (3) copper sulphate, (4) ethyl xanthate, followed by (5) a final adjustment of pH value. After ½ hr. the mineral was tested for a xanthate film by bringing a bubble of air into apparent contact with the submerged polished surface. If true contact (spreading) was not obtained within ½ min. and after cleaning the surface by wiping with a small linen pad, it was concluded that the adsorption of a xanthate film had been prevented. Following the method already described (ref. 2), curves have been constructed such that for a solution composition corresponding to any point below the curve, contact between mineral and air is possible, whereas for a solution composition corresponding to any point above the curve, contact is impossible.

Jan 1, 1939

By Arthur S. Dwight

From the latest and best literature on lead-smelting, little can be learned concerning the present state of the art of mechanical feeding in the United States. H. O. Hofman, in his Metallurgy of Lead (5th ed., 1899), briefly describes the main features of the system in use at Pueblo, Colo., and later (p. 235) says " the only successful mechanical feeding, as far as the writer is aware, is that found at the works of the Pueblo Smelting and Refining Co." H. F. Collins, in his Metallurgy of Lead and Silver (London, 1899), covers American practice pretty thoroughly; but as to mechanical charging, he says: "The German plan of taking off the gases by means of a small iron pipe suspended in the center, and the plan of charging by means of cup and cone, as in iron blast-furnaces, have both been tried, but have not found favor, chiefly on account of the difficulty of obtaining free access to the furnace-shaft for barring, etc., with such devices."' . H. W. Hixon, in his Notes on Lead and Copper Smelting (3d ed., New York, 1900), gives a description and drawing of the Hixon feeding device, as originally installed at East Helena. Evidence that this system of feeding has passed its experimental stage, and deserves more serious consideration than it has heretofore received, is furnished by two large plants—the Pueblo and the East Helena—of the American Smelting and Refining Co., where mechanical feeding has been in continuous and successful operation for a considerable period; one new plant now erecting at Salt Lake City, Utah, and one old one belonging to the same company, the El Paso works, now being rebuilt after a disastrous fire, in both of which mechanical feeding is to be a prominent feature ; one new plant of an independent concern at Torreon, Mexico, which will adopt mechanical feeding; and a number of other smaller plants, among

Jan 1, 1902

By G. D. Cremer, J. J. Cordiano

ALUMINUM powder is a well-known article of commerce and in various forms has been marketed widely for use in paint, for pyrotechnic purposes and for exothermic mixtures. For a number of reasons, how- ever, aluminum powder has not been employed extensively in powder metallurgy, although a great many proposals along this line have been offered. Aluminum and aluminum-alloy powders oxidize readily upon exposure to air and the thin film of oxide (or hydroxide) thus formed is highly refractory, in that ordinary gaseous reducing agents such as hydrogen or carbon monoxide do not reduce the oxide to metal at temperatures below the melting point of aluminum. It has been thought that the presence of these films of oxide on aluminum particles would interfere markedly in powder metallurgical work and a number of suggestions have been made, either for preventing the formation of the film through the production of the powders in inert or reducing atmospheres, or for the removal of the oxide by means of powerful reducing agents, including "nascent" or atomic hydrogen released from metal hydrides. 4 second and more serious difficulty in the use of aluminum and aluminum-alloy powders in powder metallurgy resides in the fact that during compression such powders tend to adhere or cold-weld to the die walls, thus interfering with the formation and ejection of a compact. A third difficulty, which has been encountered only with aluminum-alloy powders, is their hardness when compared with elemental aluminum. Certain of these powders are susceptible to age- hardening, which further hinders the formation of strong green compacts. These conditions are particularly true of atomized aluminum-alloy powders. Even in the annealed condition, plastic deformation of alloy powders under pressure is low when compared with unalloyed powders. This fact, coupled with the lower corrosion resistance of the alloy powders, is probably the significant factor in our failure to obtain strong sintered pieces. METHODS OF PRODUCING THE POWER Many methods have been proposed for manufacture of aluminum powder, only a few of which are used commercially. Several of the more important processes include: (I) atomization of the molten metal; (2) mechanical pulverization and other types of comminution; and (3) graining, in which molten aluminum is stirred during freezing. For pigment and certain pyrotechnic uses aluminum flake powder is desirable, because of its greater proportion of surface to volume; and large quantities of such material are made by a procedure that involves stamping or ball milling. In making flake intended for use as pigment,

Jan 1, 1943

By S. A. LoPilato, J. T. Smith

SEVERAL techniques have been evaluated for cooling the throat area of rocket-nozzle inserts to prevent erosion or fracture of the inserts during exposure to high operating temperatures and pressures. Self-cooled composites, such as infiltrated tungsten, have shown considerable promise for these applications. These composites can be fabricated by infiltrating the refractory matrix with a lower-melting metal or non-metal which is insoluable in tungsten. During firing, the lower-melting substance undergoes a series of continuous endothermic phase changes which absorb sufficient heat to maintain the nozzle matrix material at or below a safe operating temperature. At present, the state-of-the-art has reached a point where the refractory matrix density and microstruc-ture have been established as the critical parameters to be controlled for optimum self-cooled performance.'" Nondestructive testing has been utilized to ensure that porous tungsten billets were of uniform density and free from cracks or other defects prior to fabrication into rocket nozzle inserts. Ultrasonic-velocity techniques have been employed because of their reliability and reproducibility. The purpose of this note is to present and interpret the test data developed for porous tungsten matrices. For evaluation purposes, tungsten powders with Fisher subsieve sizes of approximately 4 and 18 p have been obtained for study from four commercial sources: the General Electric Co., Wah Chang Corp., Fansteel Metallurgical Corp., and Kennametal, Inc. Porous tungsten matrices were fabricated from the powders by hot pressing in induction-heated graphite die assemblies. Typical billets ranged from 3 in. diam, 2 in, high to 5 in. diam, 5 in. high. The ultrasonic-velocity measurement technique employed was through transmission, pulse echo at a frequency of 1.0 mc using matched barium titanate crystal transducers. The testing equipment included a pulsed ultrasonic generator, an amplifier, a specimen holder, and an oscilloscope, as shown in Fig. 1. The porous tungsten thickness was measured to i 0.0005 in, with precision micrometers while the oscilloscope achieved 0.02 psec time measurement accuracy. The time for a sound wave to pass through the billet, the bulk wave velocity, was calculated to 0.5 pct using Eq. [l]: V-} where V = bulk wave velocity, in. per psec, T = specimen thickness, in., and / = time, psec. To develop inspection standards, the bulk density of a porous tungsten billet was determined by the ASTM water-immersion technique.3 The ultrasonic-velocity measurements were completed at seventeen positions for each billet and averaged to develop a characteristic standard velocity for a particular tungsten powder at several density levels. A plot of ultrasonic velocity vs density is presented in Fig. 2 for six different tungsten powders. This graph has been established as

Jan 1, 1967

By C. M. Moncrief, B C. Craft

A bentonite-clay drilling mud when treated with tetrasodium pyroarsenate underwent substantially the same reduction in viscosity and water loss as when treated with the complex phosphates. The complex arsenate showed a slightly higher reversion after heating; the other arsenates showed poor viscosity-reducing properties. Introduction During the past 10 years the chemical control of drilling mud has become of major importance in affecting the successful drilling and working over of wells. The desired properties of drilling mud have been well established, and in obtaining these characteristics there has developed a large market for viscosity-reducing chemicals. Viscosity reduction produced by humic acid, tannic acid, sodium silicate, sodium tannate, Calgon, and the complex phosphates has been described by Loomis, Ford, and Fidiam.l The effects Of treatment with complex phosphates and ammonium PolyPhosPhates on the rheological properties of muds were investigated by Fancher2 and the alkali vanadates have been described by Williams.3 Laboratory Investigations It is the purpose of this paper to point out the effects of arsenates in controlling the viscosity and gelling characteristics of a drilling mud. Viscosities and gel strengths were measured at room temperatures with a Stormer viscosimeter calibrated in centipoises and operated at 600 r.p.m. Water loss was determined at 80°F. with the Baroid low-pressure wall-building tester at a pressure of I00 lb. per sq. in. for 30 min. The hydrogen-ion concentration was measured with a glass electrode. The bentonite-clay suspensions were prepared in the laboratory and allowed to age several days before testing. Members of the Arsenic Group in the periodic Table include arsenic, antimony and bismuth, but this investigation was limited to arsenic. Phosphorus also occurs in Group V of the Periodic system and phosphorus and arsenic form many closely related compounds such as pH3 and AsH3, P2O5 and As2O5, H3PO4 and H3AS04 Samples of tetrasodium pyroarsenate were prepared by fusing c.p. disodium arsenate (Na2HA5O4.7H2O). According to Friend,' this re-forms the ortho-arsenate on dissolution in water. Sodium trihydrodiorthoarsenate was prepared as described by Mellor,5 from arsenic pen-toxide as follows: As2O5 + 3H20 -> 2H3AsO4 2H3AS04 + 3NaOH Na3H3(AsO4)2 .3H20 Sodium dihydrogen orthoarsenateWaHz-As04) was obtained by fusing together equivalent quantities of arsenious Oxide and sodium nitrate, dissolving the residue in water and allowing it to crystallize.

Jan 1, 1946

By C. M. Moncrief

A bentonite-clay drilling mud when treated with tetrasodium pyroarsenate underwent substantially the same reduction in viscosity and water loss as when treated with the complex phosphates. The complex arsenate showed a slightly higher reversion after heating; the other arsenates showed poor viscosity-reducing properties. Introduction During the past 10 years the chemical control of drilling mud has become of major importance in affecting the successful drilling and working over of wells. The desired properties of drilling mud have been well established, and in obtaining these characteristics there has developed a large market for viscosity-reducing chemicals. Viscosity reduction produced by humic acid, tannic acid, sodium silicate, sodium tannate, Calgon, and the complex phosphates has been described by Loomis, Ford, and Fidiam.l The effects Of treatment with complex phosphates and ammonium PolyPhosPhates on the rheological properties of muds were investigated by Fancher2 and the alkali vanadates have been described by Williams.3 Laboratory Investigations It is the purpose of this paper to point out the effects of arsenates in controlling the viscosity and gelling characteristics of a drilling mud. Viscosities and gel strengths were measured at room temperatures with a Stormer viscosimeter calibrated in centipoises and operated at 600 r.p.m. Water loss was determined at 80°F. with the Baroid low-pressure wall-building tester at a pressure of I00 lb. per sq. in. for 30 min. The hydrogen-ion concentration was measured with a glass electrode. The bentonite-clay suspensions were prepared in the laboratory and allowed to age several days before testing. Members of the Arsenic Group in the periodic Table include arsenic, antimony and bismuth, but this investigation was limited to arsenic. Phosphorus also occurs in Group V of the Periodic system and phosphorus and arsenic form many closely related compounds such as pH3 and AsH3, P2O5 and As2O5, H3PO4 and H3AS04 Samples of tetrasodium pyroarsenate were prepared by fusing c.p. disodium arsenate (Na2HA5O4.7H2O). According to Friend,' this re-forms the ortho-arsenate on dissolution in water. Sodium trihydrodiorthoarsenate was prepared as described by Mellor,5 from arsenic pen-toxide as follows: As2O5 + 3H20 -> 2H3AsO4 2H3AS04 + 3NaOH Na3H3(AsO4)2 .3H20 Sodium dihydrogen orthoarsenateWaHz-As04) was obtained by fusing together equivalent quantities of arsenious Oxide and sodium nitrate, dissolving the residue in water and allowing it to crystallize.

Jan 1, 1946

H. H. Campbell, Steelton, Pa. (communication to the Secretary) : I wish to thank Mr. Webster for the copious quotations he has made from my writings, as he has given nearly all the arguments I wish to advance. It is necessary to note, however, his statement that most of his experiments were made on universal-mill plates, and that these were not subject to my condemnation of irregularity. I think this is a mistake. It is well known that universal-mill plates are finished under very different conditions of temperature, with the express purpose of regulating the tensile strength. This is a perfectly legitimate practice; but it renders almost worthless any calculations on the relations of the chemical and physical equations when the influence of such finishing is omitted. Another important point Mr. Webster has not answered at all. I have shown by an excerpt from his own table that two entirely different formulæ may be constructed; and it is undeniable that one is as valid as the other, since Mr. Webster started with no premise at all save an assumption that the effect of carbon was constant. This was an assumption pure and simple, and hence has no special virtue. The whole result of Mr. Webster's investigation is not that the effect of carbon is a constant, and that those of phosphorus and manganese are variables. On the contrary, there are two answers, with nothing to show which is right. We learn that if carbon is a constant, then phosphorus and manganese are variables; but that if phosphorus and manganese are constants, then carbon is a variable. This is a distinct advance over complete ignorance, but it is not final and satisfactory from either a mathematical or metallurgical standpoint. Regarding my own formulæ, I would say that they are used regularly in the testing-laboratories of the Pennsylvania Steel Company. The tensile strength of every heat is calculated

Jan 1, 1899

By Richard T. Newcomb

Federal and utility industry research has largely ignored coal beneficiation techniques in the implementation of SOx control. This paper accepts the hypothesis that beneficiation cum scrubbing is the cheapest way for the vast majority of seams in the eastern coal provinces to comply with standards. Comparisons are based on point estimates of average beneficiation costs from a model of coal preparation (COBET) designed to simulate four levels of cleaning. The paper describes how economic theory can be applied to derive econometric supply functions from actual data on the geology of minable seams, washability and technical constraints. West Virginia is taken as an example of a producing region. Spatial supply functions are derived empirically from the engineering model simulations.

Jan 1, 1977

By H. l. Burghoff, J. S. Porter

THIS paper presents the results of an investigation of the effect of cold-working and annealing treatments upon the occurrence of preferred orientation in annealed brass wire. The subject has received less consideration than has the same phenomenon in annealed brass sheet or strip, and perhaps very properly so in view of the obvious and undesired results obtained in the forming or drawing of strip having preferred orientation, which results are in contrast with the lack of any spectacular visual evidence in wire. The factors of cold-working and annealing that control preferredness in strip are naturally expected to function similarly in wire. Indeed, one might expect the condition to be commoner in annealed wire, because the severity of the cold-working between anneals in commercial practice is usually much greater for wire than for strip. For example, a wire that is to be finished in the annealed condition on a diameter of 0.040 in. is commonly subjected to a final reduction of 96 per cent between the last two anneals, the large reduction being accomplished in the successive drafts of a multiple-die machine. Wire for rivets, for instance, on 0.125-in. diameter, although given a slight reduction of about 10 per cent after the final anneal, may have been given a prior reduction of 75 to 80 per cent. Barrett1 states the fiber axis of annealed 70-30 brass wire to be [111] with some indication of [100] as a secondary fiber axis. Croft and Sachs2 have reported briefly on some differences in brass wire with random and with preferred orientations. They showed statistical plots of the twin-band angles with respect to the wire axis or direction of drawing as observed on an axial plane. They also pointed out that the resistance of the wire to corrosion-cracking when externally stressed and exposed to a mercurous nitrate solution decreased as the degree of the preferred orientation increased. MATERIAL AND PROCEDURE All the wire for the investigation was processed from one. portion as cut for extrusion from a cast billet of the following analysis: 70.13 per cent copper; 0.01 lead; 0.01 iron; 0.02 nickel; 29.83 zinc (by difference). The billet section, 8 in. in diameter, was extruded hot to 3/4 -in. diameter, after which it was processed by alternate cold-drawing and annealing treatments as indicated in Fig. I. The earliest anneals in process were at about 1100°F. and the next to the last reductions by drawing were 58 per cent. The diameter of the finally annealed wire was 0.132 in. Semifinal anneals were at 800°F., 950°F. and 1100°F. and reductions of 47.5, 74, 83.5 and 89.5 per cent were employed in drawing to 0.132 in. The final anneals were at 875°F., 1050°F. and 1250°F. and were

Jan 1, 1944

By R. I. Jaffee, E. S. Bartlett, D. N. Williams

The oxidation resistance and fabricability of molybdenum powder-metallurgy alloys containing up to 20 wt pct nickel in the form of a fine dispersion were studied. The effects of dispersion distribution and of amount and type (pure nickel or nickel compounds) of additive were considered. A definite improvement in oxidation resistance was observed, but the amount of improvement fell far short of requirements for an oxidation-resistant alloy. Fabricability by hot-rolling was limited. INVESTIGATIONS at Ohio State university1 and Battelle Memorial institute2 have indicated that the attainment of a truly oxidation-resistant molybdenum-base alloy for high-temperature service, with the coincident retention of high-temperature strength and toughness, will be a difficult, if not impossible, feat. Among the most promising alloy systems studied was the molybdenum-nickel system shown in Fig. 1. Alloys in this system show good oxidation resistance at temperatures well above the normal melting point of molybdenum trioxide because of the regenerative formation of protective nickel-molyb-date (NiMoO4) on the surface of the alloy during exposure at high temperatures. Unfortunately, the required alloy content to obtain oxidation resistant molybdenum-nickel alloys far exceeds the limits of the narrow terminal solid-solution boundary, and closely approaches the peri-tectic composition involving the brittle intermetal-lic compound, MoNi. Because of the peritectic reaction, fusion alloys are characteristically brittle, since the MoNi phase, being the last to form, tends to occur as a continuous grain-boundary network around each molybdenum grain. An added problem with this system is that the protective nickel-molybdate layer formed at high temperatures is unstable, undergoing one or more allotropic modifications upon cooling. The volume changes associated with this modification during cooling are such as to cause violent expulsion of the protective molybdate coating from the surface of the piece. This is, of course, quite detrimental in material exposed to cyclic temperature during service. The research reported here resulted from an attempt to overcome the aforementioned problems associated with the molybdenum-nickel alloys primarily by controlling the amount, size, and location of the MoNi phase. By using powder-metallurgy techniques of alloy preparation and sintering the blended molybdenum-nickel powder mixtures at a temperature below the peritectic reaction temperature, molybdenum-nickel alloys with a randomly dispersed MoNi phase were produced. MATERIALS The molybdenum powder used in the preparation of alloys for this study was commercial hydrogen reduced, minus 325-mesh (Tyler) material. Master alloys, by which nickel was added, consisted of elemental carbonyl nickel powder (12 average particle size), an alloy of 50 wt pct Ni-50 wt pct Cr, and compounds of MoNi, Ni,Si, and Ni2B. The nickel-chromium powder was prepared by filing a vacuum-arc-melted ingot, separating impurities magnetically, and screening to minus 200-mesh. The MoNi powder was prepared by pulverizing a hydrogen-sintered powder-metallurgy compact to minus 325-mesh material. Further sizing of this powder for study of effects of dispersion distribution was accomplished by air classification of the minus 325-mesh powder. The Ni2Si and Ni2B powders were prepared by crushing vacuum-sintered powder-metallurgy compacts to minus 200-mesh material. EXPERIMENTAL PROCEDURE Specimen Preparation—The general procedure followed in the preparation of alloys for testing is described as follows: 1) Blending. Either hand-blending of the powders in a ceramic mortar and pestle for X 1/2 or mechanical blending was used. Hand-blending seemed preferable for optimum homogeneity. 2) Compacting. Most of the blended powders were pressed to green compacts at pressures of 15 tons per sq in. in a single-action die, although some were pressed at 80 tons per sq in. A 1 X 11/4 X 1/4-in. green compact was the standard size for oxidation test material, and 7 X 1/2 X 1/4-in. compacts were used for fabricability test specimens. 3) Sintering. All green compacts were sinteredat

Jan 1, 1959

By G. D. Cremer, J. J. Cordiano

Aluminum powder is a well-known article of commerce and in various forms has been marketed widely for use in paint, for pyrotechnic purposes and for exothermic mixtures. For a number of reasons, however, aluminum powder has not been employed extensively in powder metallurgy, although a great many proposals along this line have been offered. Aluminum and alumiuum-alloy powders oxidize readily upon exposure to air and the thin film of oxide (or hydroxide) thus formed is highly refractory, in that ordinary gaseous reducing agents such as hydrogen or carbon monoxide do not reduce the oxide to metal at temperatures below the melting point of aluminum. It has been thought that the presence of these films of oxide on aluminum particles would interfere markedly in powder metallurgical work and a number of suggestions have been made, either for preventing the formation of the film through the production of the powders in inert or reducing atmospheres, or for the removal of the oxide by means of powerful reducing agents, including "nascent" or atomic hydrogen released from metal hydrides. A second and more serious difficulty in the use of aluminum and aluminum-alloy powders in powder metallurgy resides in the fact that during compression such powders tend to adhere or cold-weld to the die walls, thus interfering with the formation and ejection of a compact. A third difficulty, which has been encountered only with aluminum-alloy powders, is their hardness when compared with elemental aluminum. Certain of these powders are susceptible to age-hardening, which further hinders the formation of strong green compacts. These conditions are particularly true of atomized aluminum-alloy powders. Even in the annealed condition, plastic deformation of alloy powders under pressure is low when compared with unalloyed powders. This fact, coupled with the lower corrosion resistance of the alloy powders. is probably the significant factor in our failure to obtain strong sintered pieces. Methods of Puoducing the Powder Many methods have been proposed for manufacture of aluminum powder, only a few of which are used commercially. Several of the more important processes include: (I) atomization of the molten metal; (2) mechanical pulverization and other types of comminution; and (3) graining, in which molten aluminum is stirred during freezing. For pigment and certain pyrotechnic uses aluminum flake powder is desirable, because of its greater proportion of surface to volume; and large quantities of such material are made by a procedure that involves stamping or ball milling. In making flake intended for use as pigment,

Jan 1, 1943

By G. D. Cremer, J. J. Cordiano

Aluminum powder is a well-known article of commerce and in various forms has been marketed widely for use in paint, for pyrotechnic purposes and for exothermic mixtures. For a number of reasons, however, aluminum powder has not been employed extensively in powder metallurgy, although a great many proposals along this line have been offered. Aluminum and alumiuum-alloy powders oxidize readily upon exposure to air and the thin film of oxide (or hydroxide) thus formed is highly refractory, in that ordinary gaseous reducing agents such as hydrogen or carbon monoxide do not reduce the oxide to metal at temperatures below the melting point of aluminum. It has been thought that the presence of these films of oxide on aluminum particles would interfere markedly in powder metallurgical work and a number of suggestions have been made, either for preventing the formation of the film through the production of the powders in inert or reducing atmospheres, or for the removal of the oxide by means of powerful reducing agents, including "nascent" or atomic hydrogen released from metal hydrides. A second and more serious difficulty in the use of aluminum and aluminum-alloy powders in powder metallurgy resides in the fact that during compression such powders tend to adhere or cold-weld to the die walls, thus interfering with the formation and ejection of a compact. A third difficulty, which has been encountered only with aluminum-alloy powders, is their hardness when compared with elemental aluminum. Certain of these powders are susceptible to age-hardening, which further hinders the formation of strong green compacts. These conditions are particularly true of atomized aluminum-alloy powders. Even in the annealed condition, plastic deformation of alloy powders under pressure is low when compared with unalloyed powders. This fact, coupled with the lower corrosion resistance of the alloy powders. is probably the significant factor in our failure to obtain strong sintered pieces. Methods of Puoducing the Powder Many methods have been proposed for manufacture of aluminum powder, only a few of which are used commercially. Several of the more important processes include: (I) atomization of the molten metal; (2) mechanical pulverization and other types of comminution; and (3) graining, in which molten aluminum is stirred during freezing. For pigment and certain pyrotechnic uses aluminum flake powder is desirable, because of its greater proportion of surface to volume; and large quantities of such material are made by a procedure that involves stamping or ball milling. In making flake intended for use as pigment,

Jan 1, 1943