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By Benjamin C. Craft, Frank Perkins

The wall-building properties of salt-water muds can be maintained at high temperatures by additions of gum karaya, gum ghatti, gelatinized starch, or commercially prepared starch. A germicide should be used to prevent fermentation. Introduction The behavior of drilling mud has received special attention from the petroleum industry within the past few years in numerous research projects dealing with such subjects as chemical treatment, gelation, and filtration characteristics. The importance and control of filtration, or water loss, is readily apparent* It affects the analysis of side-wall cores and interpretation of electric logs; it controls to a large extent the work of primary cementing, reduces the amount of expensive fishing, and permits the running of long strings of casing. It has been found that among the many factors that have an adverse effect on filtration, the presence of electrolytes, in general, and of salt, in particular, is outstanding. The effect is one of flocculation of the colloids due to neutralization of the negative charges on the clay particles. This reaction is further increased on the Gulf Coast because high temperatures reduce dispersion, to a minimum, causing increased flocculation in both fresh-water and saltwater muds. The problem of reducing water loss in salt-water muds by the addition of gums and starch at atmospheric temperature has been investigated,' and many successful field tests in West Texas indicate its solution. From the work of Byck2 it is concluded that no existing method will permit an approximate determination of the filtration rate at high temperatures from data taken at room temperatures. Filtration should be measured at the ternperature actually anticipated in the well, or at least at a number of lower temperatures and extrapolated over a small range. A laboratory study has been made of the chemicals available for the filtration characteristics of salt-water muds at high temperatures, and the use of germicides to prevent fermentation. Laboratory Investigations Procedure Since the purpose of this investigation was to compare several different gums and starches at elevated temperatures, mud from the same source was used for all the tests. Viscosity was measured in a Stormer viscosimeter at 600 r.p.m. and water loss was determined with a Baroid High-pressure and High-temperature Wall-building Tester3 at temperatures from 80' to 250°F. and at a pressure of 500 lb. per sq. in. for 30 minutes. The samples tested consisted of 150 grams of commercial Louisiana mud, 50

Jan 1, 1943

By Benjamin C. Craft, Frank Perkins

The wall-building properties of salt-water muds can be maintained at high temperatures by additions of gum karaya, gum ghatti, gelatinized starch, or commercially prepared starch. A germicide should be used to prevent fermentation. Introduction The behavior of drilling mud has received special attention from the petroleum industry within the past few years in numerous research projects dealing with such subjects as chemical treatment, gelation, and filtration characteristics. The importance and control of filtration, or water loss, is readily apparent* It affects the analysis of side-wall cores and interpretation of electric logs; it controls to a large extent the work of primary cementing, reduces the amount of expensive fishing, and permits the running of long strings of casing. It has been found that among the many factors that have an adverse effect on filtration, the presence of electrolytes, in general, and of salt, in particular, is outstanding. The effect is one of flocculation of the colloids due to neutralization of the negative charges on the clay particles. This reaction is further increased on the Gulf Coast because high temperatures reduce dispersion, to a minimum, causing increased flocculation in both fresh-water and saltwater muds. The problem of reducing water loss in salt-water muds by the addition of gums and starch at atmospheric temperature has been investigated,' and many successful field tests in West Texas indicate its solution. From the work of Byck2 it is concluded that no existing method will permit an approximate determination of the filtration rate at high temperatures from data taken at room temperatures. Filtration should be measured at the ternperature actually anticipated in the well, or at least at a number of lower temperatures and extrapolated over a small range. A laboratory study has been made of the chemicals available for the filtration characteristics of salt-water muds at high temperatures, and the use of germicides to prevent fermentation. Laboratory Investigations Procedure Since the purpose of this investigation was to compare several different gums and starches at elevated temperatures, mud from the same source was used for all the tests. Viscosity was measured in a Stormer viscosimeter at 600 r.p.m. and water loss was determined with a Baroid High-pressure and High-temperature Wall-building Tester3 at temperatures from 80' to 250°F. and at a pressure of 500 lb. per sq. in. for 30 minutes. The samples tested consisted of 150 grams of commercial Louisiana mud, 50

Jan 1, 1943

By T. L. CONDRON

DURING the past fourteen months, this committee has had under consideration and study the subject of the licensing or registration of engineers. The fifteen members of the committee as appointed by Council, were selected from thirteen states, viz., Connecticut, New York, Pennsylvania, Ohio, Georgia, Louisiana, Illinois, Missouri, Iowa, Minnesota, Colorado, California and Washington, and therefore represent practically all sections* of the United States, as well as mechanical, electrical, mining, hydraulic, municipal, sanitary, railway and' structural engineering, and also colleges of engineering. The first work of the committee was to investigate the general subject and to collect, so far as possible, avail¬able material bearing upon the subject in hand,. in-' eluding opinions from many engineers as to the need or desirability of legislation, as well as copies of all state laws passed and proposed, having to do with licensing or registration of engineers, architects and surveyor, This preliminary investigation disclosed that very pronounced views were held by engineers throughout the country, both for and against state licensing or registration. The general sentiment one year ago was more opposed to such measures than it is today. The older members of the profession did not as a rule favor licensing nor did they feel there was need for state regulation of engineering practice, while among the younger men there was a feeling that licensing or registration by the states would add prestige to professional engineers and in many ways benefit -the profession, as well as individual engineers.

Jan 1, 1920

By J. V. W. REYNDERS

FIRST of all let me express my affectionate gratitude for the cordiality and good will of your reception. On the part of the men I venture to interpret the character of your greeting, not only as a recognition of the position to which you have been good enough to elect me, but also as an expression of your friendly attitude. However, I cannot pass over the tribute of the ladies so casually: Nor does it seem possible to do justice to my sentiments in addressing them collectively. I would feel more equal to the task if I could have the opportunity to talk to them singly, in doing which I know I may count upon their good sportsmanship not to compare notes. There has been some discussion between Mr. Kelly and myself as to our respective duties on this occasion: The precedents are not clear as to whether the retiring or the incoming president is expected to speak at length. Mr. Kelly's argument was that as the incoming president confines himself to promises for the future his field is a broad one and his opportunities for extending his remarks correspondingly unlimited.

Jan 1, 1925

By C. E. Birchenall, R. H. Condit, M. J. Brabers

In the oxidation of pure iron above 700°C the overall rate is determined mainly by the rapid growth of wiistite, through which iron ions can diffuse rapidly.' Nickel added to the iron progressively decreases the stable range of composition of wustite.' When enough nickel is added to eliminate wiistite as a stable phase, the spinel is the fast growing phase. This investigation was undertaken to test the hypothesis that nickel substituting for iron in magnetite might decrease the rate of spinel growth by reducing the iron mobility. Nickel ferrite boules grown by the flame fusion process were purchased from the Linde Co. Chemical analysis gave an atomic ratio of iron to nickel of 2.88 and showed no other cations. They were cut into discs and ground to give flat, parallel faces. The experimental procedure employed was like that of Eisen and Birchenall in which the distribution of radioactivity diffused in from a vapor deposited surface layer was determined by counting the residual activity through a series of ground faces. The diffusivities were calculated in a manner consistent with the requirements discussed by Condit and BirchenallP The details will be given in connection with a more extensive spinel diffusion study now in progress. The results of the measurements are shown in the figure in comparison with earlier data on magnetite1 and zinc ferrite. The uncertainties arising from scatter in the activity vs distance relationship and uncertainties in the temperatures are shown by flags. Despite the scatter it is clear that substitution of a considerable part of the iron in magnetite by nickel, in this case about one third decreases the iron mobility substantially. sachs' determination of the distribution of iron and nickel in scales on iron-nickel alloys appears to show that nickel is less mobile than iron in the spinel layer. It is evident, therefore, that nickel plays several roles in reducing the oxidation rate of iron-nickel alloys. 1) It reduces progressively the stability range of wiistite. ' 2) It reduces progressively the stability range of the iron-nickel spinel phase in terms of the variation in cation to anion ratio.' 3) As shown in this investigation, it reduces the cation mobility in the spinel phase which is the faster growing phase in the absence of wiistite. The fe was obtained from the Oak Ridge National Laboratory. The research was supported by the Air Force Office of Scientific Research (ARDC) under contract number AF 18(600)-967.

Jan 1, 1961

THE translators wish to record their appreciation of the help given by many individuals with whom they have discussed various details of the work. They are particularly indebted to Mrs. Anne Noble McKeachie, who initiated their collaboration; to Miss Cora Adamson, who spent many hours in making an accurate copy of a much-mutilated &st draft of the translation; and to the Yale University Library which gave access to its excellent collection of books on all aspects of the history of the sciences. The reader will share with the translators their obvious indebtedness to Mr. Carl P. Rollins, Mr. James W. Boyden, and the staff of the Printing-Office of the Yale University Press. The publication of this translation by the American Institute of Mining and Metallurgical Engineers has been made possible by a grant from the Seeley W. Mudd Memorial Fund, administered by a committee composed of Harvey S. Mudd, H. DeWitt Smith, and George Otis Smith. The translators are gratified that their work has been judged to fall within the scope of this Fund, which was established for the advancement of the sciences of mining and metallurgy by the encouragement of research and the dissemination of knowledge, and especially for the furtherance of such activities as might benefit the younger members of the profession. While Biringuccio's book would scarcely serve as a dependable text for the young mining student or metallurgist, it can give him a sense of his membership in a long-standing and honorable profession and enable him better to see his own work in true perspective. It is hoped that this English edition of a sixteenth-century Italian work will be read by the practicing metallurgist as well as by those who have already found pleasure in exploring the past of their profession. A man always feels more at home in a foreign country with men of his own craft than in his birthplace with those of different interests: As in space, so in time, and the modem metallurgist who may be unmoved by the literary and artistic Renaissance will quickly appreciate the spirit of that exciting period as he talks shop with Biringuccio on a visit to mine, smelter, forge, and foundry; as he sees in different forms the very furnaces and machines whose operation and response he knows so well; and as he discusses with this engineer of four centuries ago such topics as the best kinds of fuel or refractory for a given operation, and the importance of adequate supplies of power and material.

Jan 1, 1942

By B. N. Das, H. E. LaBelle, G. A. Wolf

ZnxHg1-xTe and GUPxAS1-x crystals have been grown from solution by a traveling heater method (THM). In a floating zone type fashion a solution zone sandwich of liquidus composition is made to migrate through feed material of solidus composition by a slow-speed movement of <0.25 mm per hr of the total charge through a stationary radiation or rf heater. ZnxHg1-xTe of composition 0 < x < 0.3 and GUPxAS1-x of composition 0.5 < x < 0.7 have thus been grown from their solution in liquid tellurium and gallium, respectively. A simplified analysis of heat and material transport is given. In this method, Proper adjustment of the temperature distribution along the liquid solution zone axis eliminates instability of the crystal growth front and constitutional supercooling. 1) ZnxHg1—xTe: The solid-solution telluride was grown in sealed quartz tubes at a temperature of 500 to 650°C. For first Preparations mechanical mixtures SINGLE crystals of solid solutions of III-V and II-VI compounds have been grown by various techniques from the melt, from the gaseous phase, or from solutions in of ZnTe and HgTe were used. X-ray determinations showed the resulting crystals to be homogeneous throughout their entire length, except for the end sections. The homogeneity is greatly improved by reusing the ingots obtained from first Preparations as feed material in subsequent crystal growth runs. Ingots of up to 4.5 cm have thus been obtained. 2) GaPxAs1-x: Crystals were grown in a EN crucible at a temperature of 1050°C. For first Preparation a mechanical mixture of Gap and GaAs was cemented together by a minimum amount of liquid gallium through "wet" grinding of Gap and GaAs crystals in the liquid metal and subsequent exuding of excess gallium by compacting of the charge in the EN crucible. Electron microprobe measurements using P-Ka and As-Ka radiation showed uniformity over a length of 0.4 cm. Properties of the various Preparations are described. liquid metals.&apos;-&apos; Their growth from the melt by passing a liquid zone of pseudobinary liquidus composition through a solid rod of solidus composition is generally a convenient method of growth of single crystals of solid solutions of homogeneous composition. This method loses much of its usefulness, however, if the melting point or the vapor pressure of the solid solution is high. In the case of a compound having a high melting

Jan 1, 1969

By A. U. Seybolt

RECENTLY, cases of coexisting ordered and disordered phase equilibria have been reported among face-centered cubic metals,1"3 but not on body-centered cubic systems.4 McQueen and Kuczynski5 showed a single line as the boundary between ordered solid solution of Fe3Al type and corresponding disordered solution in the Fe-A1 phase diagram based mainly on dilatometric and magnetic measurements. Such a single line would indicate a second or higher order transition. or an absence of coexisting order and disorder. The writer found previously a two-phase equilibrium region at 800°C consisting of ordered and disordered solid solutions of Fe3Si in a matrix of approximately 1-6 wt pct Si (Fe3Si is of 14.3 wt pct Si). A similar two-phase region of ordered and disordered Fe3Al solid solutions might be expected if the similarity between Fe3Si and Fe3Si structures hold true. In the present investigation, a wire of 22 at. pct Al, balance Fe and 0.0513 cm in diameter was subjected to electrical resistivity measurement in vacuum as a function of temperature between 300 and 800°C, see Fig. 1. There was excellent agreement between data taken on heating and on cooling: no hysteresis was observed. The Curie temperature was determined to be 640 °C which agrees with the finding by McQueen and Kuczynski.5 But in addition, there were two transitional points in the resistance-temperature plot at 510oC and 400 "C. The former is thought to be a connection with the transition from disordered state to a coexisting order and disordered equilibrium state; while the latter, from such coexisting state to ordered state. Fig. 2 shows a phase diagram where the suggested two-phase region lies between dotted lines. The solid lines are those of McQueen and Kuczynski.5 Since these authors found only a single-phase boundary between ordered and disordered Fe3 Al, it would seem likely that the dilatometric method used by these authors was not sufficiently sensitive to resolve the ordering reaction into the two-phase boundaries. In addition, their phase diagram conflicts with the statement they make on P. 1 of their paper: "The sharpness of the peaks indicates that ordering to Fe3A1 is a first order reaction." The suggestion of coexisting order plus disorder in Fe3A1 must be considered tentative until confirmed by high-temperature X-ray examination. If

Jan 1, 1961

Discussion of the paper of L. A. DELANO, presented at the St. Louis meeting, October, 1917, and printed in Bulletin No. 129, September, 1917, pp. 1267 to 1286. L. A. DELANO.-Since this paper was written, our daily mill tonnage has increased, from 2100 tons to 2700 tons a clay. We now use 11,000 lb. of chrome-steel balls of 2 ½ -in. maximum diameter, for an average crushing capacity of 275 tons per 24 hr., this giving a much higher crushing efficiency. I wish to call attention to two typographical errors in my paper as published. On page 1271, Table 1, the screen analysis of ore at the Bonne Terre mill should be stated in inches instead of mesh. - On page 1272, "the rolls average 185 tons per 24 hr., and have shown by test that 250 tons per hour can be maintained" should, of course, read "250 tons per 24 hours." THE CHAIRMAN (0. M. BILHARZ, Miami, Okla.).-Is the increased mill capacity due to improvement in the re-crushing of middlings or to keeping middlings out of circulation and treating them separately? L. A. DELANO.-AS was shown in Mr. Rabling&apos;s paper (Bulletin No. 128, p. 1161) the tonnage was raised by about 400 tons by simply changing the arrangement of screen openings in the jig bed and using punched plate instead of woven-wire screen. Then, by adding a ball-mill, we are taking from the jigs a much larger tonnage of middlings than before or as much as the ball-mill will crush. By sending the ball-mill product to tables and flotation, the jig capacity for original ore is increased. CHAIRMAN BILHARZ.-In your opinion, the satisfactory operation of a Hancock jig on a given ore requires adjustment of the length of the different screens and careful selection of screen openings? L. A. DELANO.-I think it does. In order to decide what screen openings to use on the jigs, we did a great deal of experimental work, making screen analyses of the various hutch products, and then hand-sorting the galena, middlings and chat from each size screen to determine the percentage of galena in each. Then adjusting our jig screens, we gradually worked the process up to a very efficient basis. ERNEST GAYFORD, Salt Lake City, Utah.-I would like too ask Mr. Delano whether the work of the Allen cone has been quite as satisfactory as the manufacturers claim for it.

Jan 1, 1918

By C. E. Birchenall

DaVIES and Richardson1 have measured composition changes for Mn1-Owith variation in the equilibrium partial pressure of oxygen at 1500°, 1575°, and 1650°C, where 6 is the deviation from the simple stoichiometric ratio. No trend in this relationship with temperature was observed, so these remarks apply to the whole temperature range. The experimental values and their spread are shown by the bounded straight-line segments in the figure. Davies and Richardson assume that the stoichiometric oxide shows Frenkel disorder, given by the equation Mn2+Mn2+ + Mn" [1] where Mn2+ is a normal lattice ion which moves into an interstitial site (Mni2+) leaving a vacancy (Mn,"). The superscript dashes indicate that there is an excess charge on the anions surrounding the vacancy. Schottky disorder, in which a perfect crystal acquires equal numbers of cation and anion (Ov") vacancies according to leads to equations of exactly the same form in the analysis below. In view of the neutron diffraction results of Roth,2 which shows extensive Frenkel disorder in Fe1-o, Eq. [I] seems more appropriate. The deviations from stoichiometric composition, MnO, result from the addition of oxygen according to In effect Davies and Richardson ignore the variation of Mn3+in constructing equilibrium constants. This approximation might not appear to be very serious if the excess positive charges are really free posi- tive holes (P+) and if the intrinsic conductivity is high as a result of the reaction where e- is a conducting electron. However, the calculations of Buessem and Butler3 indicate that the partition functions of the free charges make a large contribution to the equilibrium constant, and this approximation would not be a desirable one. Furthermore, Morin4 shows that the positive holes are probably localized in MnO and therefore are described better by the mass action principle than by a degenerate gas model. Davies and Richardson&apos;s considerations require that activity corrections be applied beyond a 6 value of about 0.005. It is proposed to show here that the dissociation pressure curve can be calculated reasonably well over the whole composition range studied without activity corrections by choosing appropriate equilibrium constants for reactions 1 and 2. As stoichiometric composition The mass action constant, Ks, for reaction [I.] and the equilibrium constant, K,, for reaction [2] are given by where the concentrations which do not change significantly have been absorbed into the constants. The brackets denote concentrations. The deviation from stoichometric composition is given by gardless of [Mni2 ]. Substituting Eq. [7] in [6]

Jan 1, 1961

By G. H. Enzian

W. C. Ellis—The intergranular fracture observed by these authors in brass seems to be characteristic of metals when tested under similar conditions. It has been observed by us in room temperature tests on lead alloys subjected to constant stress when the stress has been low enough to afford a small strain rate. If, however, the test be carried out at a high stress and therefore at a large strain rate, a characteristic, tapered, transcrystalline fracture is obtained. The same change of fracture has been observed by others with decrease of strain rate and increase of temperature for other metals—for example aluminum—and may be presumed, as the authors point out, to be general for metals. These findings suggest a plastic flow mechanism under conditions of small strain rate and high corresponding temperature differing from classical block slip. The required conditions point to a process fundamentally diffusive in nature—a less organized process than block slip. Nabarro18 has shown that plastic flow can occur by stress induced diffusion of vacant sites— a process of self-diffusion. Movements of a pseudo-viscous nature at grain boundaries are suggested in the work of Ke.15 Deformation near to a grain boundary by other than a slip mechanism appears necessary to Boas and Hargreaves.19 Wood and Rachinger20 report a cellular structure in slowly deformed alumi- num—the cell size is larger, the higher the temperature and the slower the strain rate. Presumably in the latter case diffusive movements occurred in the cell boundaries. In any case the nonslip mechanism seems somewhat obscure and further work is indicated. Such studies will undoubtedly clarify the nature and behavior of lattice imperfections—the very core of the strength and plastic properties of metals. F. H. Wilson and E. W. Palmer (authors&apos; reply)—It is certain that the metallic behavior which has been termed "creep" includes many interdependent phenomena of which a nonslip type of plastic flow may well be one. The reports to which Mr. Ellis refers are illustrative of the many different observations that must be correlated for a complete understanding of creep. The list could be extended considerably. For example, we ourselves have been impressed by the sensitivity of creep phenomena to the presence of minor impurities and feel that this aspect of the problem warrants more thorough study than it has yet received. References 18 F. R. N. Nabarro: Report of Bristol Conference on Strength of Solids. P. 75, (1948) London. 19 Boas and Hargreaves: Proceedings Royal Society. (1948) 193. 89. 20 wood and Rachinger: Journal Institute of Metals. (1949) 17, 237.

Jan 1, 1951

By C. Zener, H. Nielsen, D. Van Winkle

THE internal friction of metals has been studied frequently at elevated temperatures.1-4 In most cases it rises rapidly with increasing temperature. The notable exceptions are ferromagnetic materials, and lead.2 This paper describes an investigation of the general features of the high-temperature internal friction of 70-30 alpha brass. EXPERIMENTAL METHOD The internal friction of a metal is a measure of the rate at which it dissipates energy of vibration. The measure adopted here, I/Q, is (I/2p) times the specific damping capacity, a measure commonly used by engineers. In the measurements of this investigation, the stress level was kept so low that the observations were independent of the stress. The general method of making such measurements, and of observing the temperature of the specimen during a measurement, has been described elsewhere.5,6 The driver and detector coils were wound with wire insulated with glass thread, in order to withstand the high temperatures used. In previous work electrical eddy currents in the specimen served as the coupling between the mechanical vibration of the specimen and the electrical circuits of the driver and detector. The high values of the internal friction in the present investigation rendered this coupling insufficient. In order to increase this coupling, pole pieces cut from ordinary telephone diaphragms were attached to the specimen. A mixture of French chalk and water glass proved a satisfactory cement. All measurements were made at the fundamental frequency for transverse vibration, which lay between 600 and 900 cycles per second. SPECIMENS The measurements described herein were made upon a single cylindrical rod of brass, kindly furnished by Dr. Cyril Stanley Smith, of the American Brass Co. This rod was the specimen E of the set of alphabrass rods described in an earlier paper.6 Successively larger grain sizes were obtained by annealing at successively higher temperatures. A slice was cut off one end after each set of measurements. Grain counts were made on each slice by W. E. Lindlief, of the American Brass Co. Nine fields were viewed on each piece, located as shown in Fig. I. Results are given in Table I. The grain size is defined in the usual way; namely, Grain size = I/n ½ where n is the mean number of grains per square millimeter. EXPERIMENTAL RESULTS This paper is concerned exclusively with the part of the internal friction that becomes dominant at high temperatures. It is thus desirable to separate this part of the internal friction from the part that is

Jan 1, 1942

By F. V. Lenel

R. P. Seelig.*—Dr. Lenel is to be congratulated on his presentation of a particularly interesting paper describing the use of the powder metallurgy process for the production of magnetic pole pieces. The only thing that might be added is that we have been successful in producing pole . pieces with a narrow hysteresis curve by the use of considerably lower sintering temperatures than the ones used by Dr. Lenel. It is quite possible that this use of lowe- temperatures has considerably widened the field of commercial application for pole pieces made from metal powders. Development work is currently being done on an a.c. application of a sintered iron part. However, I am in full agreement with Dr. Lenel that if eddy currents are an important factor in the application, we cannot substitute sintered material for laminated sheet-metal structures. Mr. Peters&apos; remarks concerning the limitations of machine parts were well taken. The emphasis of the limitations makes it easier to define clearly what we can do and-what the advantages are of machine parts made of metal powders. When I mention metal-powder machine parts, I mean those of relatively high density, although complete elimination of porosity is not possible at this time. The limitations of the field for this type of parts are largely economical. I believe that Mr. Langhammer has made that point very clear. The following questions are very often asked: How large a part can you make? How close can you hold the dimensions ? How fast can a part be produced? In a majority of the cases, it depends on the cost at which the part can be produced. A large variety of shapes and sizes of a number of materials can be formed. However, the main requirement in this field of endeavor is whether this can be done more economically by powder metallurgy than by other manufacturing methods. As a general indication, it may be stated that densities up to 95 per cent of that of rolled material can now be produced commercially in simpler parts. Tolerances of plus or minus 0.001 in. are common, but where special conditions justify, closer tolerances can be held; we are producing a part of which one dimension is held to 0.0003 inch. Finally, as far as maximum size is concerned, technically this would depend on the capacity of the press and furnace equipment available. Actually, we find that the economical limit of powder-metallurgy machine parts is approximately one pound. From there on, each individual case must he studied on its own merits.

Jan 1, 1945

By William A. Mitchell

AN X-ray diffraction pattern for "calcined cold precipitated ferric oxide" is reproduced dia-grammatically along with data for other iron oxides by R. C. Mackenzie.1&apos; This pattern, which shows spacings higher than those for any other form of iron oxide, was obtained from material prepared and photographed at several different times over a period of weeks, but later attempts to reproduce the results were unsuccessful, the pattern of hematite being obtained every time.2 In an attempt to solve this problem, the original photographs showing the strange diffraction pattern were examined and a marked similarity to the hematite pattern was noticed, suggesting that the pattern was in fact due to hematite but corresponded to a shorter wavelength of X-rays than the Cu Ka which was assumed to have .been used. The eight strongest lines were provisionally identified with the strongest hematite lines and, by means of the corresponding hematite spacings, the X-ray wavelength was calculated for each line. This gave an almost constant value, with the exception of the innermost line which was somewhat diffuse, and confirmed the presence of hematite. The value obtained, 0.703 ± 0.015Å, corresponds to the molybdenum Ka wavelength. The X-ray tube used was a four-filament demountable tube with a copper target. Other photographs, mostly of soil clays, taken during the same period gave normal patterns of Cu Ka radiation with one exception. This was a calcined soil clay with a high iron content and also showed Mo Ka lines of the hematite structure. The explanation is almost certainly that the copper target was contaminated with molybdenum, but it is not known how this occurred. Specimens of alumino-silicates gave their normal Cu Ka pattern, but as the K absorption edge of iron is a little longer than the Cu Ka wavelength, specimens with a high iron content greatly reduced the intensity of the Cu Ka diffraction lines relative to that of the lines due to the shorter Mo Ka wavelength. The formation of hematite on calcining cold precipitated hydrated ferric oxide3 is thus confirmed. References R. C. Mackenzie: Investigations on Cold-precipi-tated Hydrated Ferric Oxide and its Origin in Clays. Problems of Clay and Laterite Genesis, p. 69, Fig. 4, F. AIME Symposium, St. Louis, Mo. Feb. 19-22, 1951. Published 1952. &apos;R. C. Mackenzie: Ref. 1. Note added on proof. V. C. Hansen and L. T. Brownmiller: Equilibrium Studies on Alumina and Ferric Oxide and on Combinations of These with Magnesia and Calcium Oxide. American Journal of Science (1928) 5, No. 15, pp. 225-242.

Jan 1, 1954

By Michael Perch, Charles C. Russell

Nearly 75 per cent of the total coke production in the United States in 1940 was consumed in blast furnaces. In 1939 the percentage was 69.9, and in 1938 it was 61.3. To produce a net ton of pig iron 1757 lb. of coke was required in 1940 and 1760 lb. in 1939. These figures indicate how dependent the production of pig iron is upon the production of coke. The rate of iron production is in some measure influenced by the physical and chemical characteristics of the coke. Blast-furnace operators believe that the physical properties of coke profoundly influence the operation of the furnace. Although it is true that coke of a wide variety of physical properties is used in American blast furnaces, the periodic fluctuation of these properties is one of the causes of irregularity of blast-furnace operation. The purpose of this paper is to present a broad picture of the physical properties of by-product coke that are generally considered to be important by coke-oven and blast-furnace operators. Effects of the kind of coal used, the preparation of the coal, the rate of coking, and other factors will be considered. Of all these variables, the kind of coal used is by far the most important. In this discussion use will be made of the method of coal classification by rank1 standardized by the American Society for Testing Materials. Although this method of classification has been an American standard for several years, it has not been given the attention it deserves, especially in connection with the selection of coal for production of coke. Despite the fact that many producers of blast-furnace coke are limited to some particular source or sources of coal, a good understanding of the principles involved in setting up the standard method of classification may lead to a better appreciation of the causes of changes in coke characteristics. Furthermore, where it is necessary to select new coals as a substitute for the original supply, this method of classification can be of great assistance. The data presented have been gathered from many sources, but no attempt has been made to cover the vast literature. Instead, some of the more important data have been selected to show how coals and their carbonization affect some of the physical properties of coke. It must be emphasized that generalizations concerning the behavior of coking coals are presented and that individual coals may vary widely from the specific behavior depicted. Nevertheless, it is believed that the data illustrate certain typical behaviors. Neither was it possible to cover completely all the factors involved; for example, the macroscopic constituents of coal are believed to have important effects on the physical properties of coke, but since there is little information available for such study, and since vitrain, clarain, and durain are neither

Jan 1, 1942

By J. D. Hanawalt, C. E. Nelson, J. A. Peloubet

The subject of the salt-water corrosion resistance of magnesium alloys is somewhat like that of the pitting of stainless steels, in that it involves a relatively small. percentage of the applications but receives a much greater proportion of the publicity. Actually magnesium alloys are in use in many exterior applications as well as interior, with no trouble from corrosion. Magnesium and its alloys have a striking stability against atmospheric attack, being far superior to iron. Specimens exposed unprotected to atmospheric weathering for Io Years show only a superficial surface-film formation. The basic nature of magnesium and of its important alloys is that they are also resistant to the attack of salt water even in an unprotected state, giving substantially no loss in weight after one year of alternate immersion in 3 per cent NaCl solution (Fig. 1). This basic behavior is often masked because of the extreme sensitivity of these alloys to certain impurities and combinations of impurities. It is known, and the subject of increasing emphasis, that higher purity leads generally to greater stability for many materials, non-metallic as well as metallic. However, a review of the literature on the corrosion factors in magnesium alloys shows that almost all researchers worked with base metal in which metallic impurities varied in uncontrolled amounts. The major factor, that of metallic impurities, Probably greatly overshadowed the effects of minor ones such as flux inclusions, nonmetallic impurities, porosity, metallographic state, which these researchers presumed to study. In the present investigation the first observation of interest is that whereas magnesium of commercial purity (99.9 per cent pure) has a corrosion rate in alternate immersion in 3 per cent NaCl solution at room temperature of anywhere from 5 to Ioo mg. per sq. cm. per day, the corrosion rate of high.purity magnesium is 0.15 ± 0.05 mg, per sq. cm. per day. The principle followed in the experiments was to add to such base magnesium other elements, singly and in inin in controlled and known amounts and to observe the corrosion behavior of the resulting alloy. These experiments show the existence of what may be called tolerance limits" of magnesium and some of its alloys for certain impurities. The extremely small percentages of impurities involved and the sharpness of the corrosion discontinuities appear to be quite unpredictable, In order to carry on this work, it was necessary to develop an analysis technique suitable to the problem. In some cases it was necessary quantitatively to analyze impurities to less than 0,001 per cent. The experimental data to be presented are based on observation of about 5000 alloy specimens and on more than 50,000 quantitative analyses. while the primary purpose of this paper is to present the experimentally obtained data on corrosion rates as a function of composition, and particularly to demon-

Jan 1, 1942

By J. D. Hanawalt, C. E. Nelson, J. A. Peloubet

The subject of the salt-water corrosion resistance of magnesium alloys is somewhat like that of the pitting of stainless steels, in that it involves a relatively small. percentage of the applications but receives a much greater proportion of the publicity. Actually magnesium alloys are in use in many exterior applications as well as interior, with no trouble from corrosion. Magnesium and its alloys have a striking stability against atmospheric attack, being far superior to iron. Specimens exposed unprotected to atmospheric weathering for Io Years show only a superficial surface-film formation. The basic nature of magnesium and of its important alloys is that they are also resistant to the attack of salt water even in an unprotected state, giving substantially no loss in weight after one year of alternate immersion in 3 per cent NaCl solution (Fig. 1). This basic behavior is often masked because of the extreme sensitivity of these alloys to certain impurities and combinations of impurities. It is known, and the subject of increasing emphasis, that higher purity leads generally to greater stability for many materials, non-metallic as well as metallic. However, a review of the literature on the corrosion factors in magnesium alloys shows that almost all researchers worked with base metal in which metallic impurities varied in uncontrolled amounts. The major factor, that of metallic impurities, Probably greatly overshadowed the effects of minor ones such as flux inclusions, nonmetallic impurities, porosity, metallographic state, which these researchers presumed to study. In the present investigation the first observation of interest is that whereas magnesium of commercial purity (99.9 per cent pure) has a corrosion rate in alternate immersion in 3 per cent NaCl solution at room temperature of anywhere from 5 to Ioo mg. per sq. cm. per day, the corrosion rate of high.purity magnesium is 0.15 ± 0.05 mg, per sq. cm. per day. The principle followed in the experiments was to add to such base magnesium other elements, singly and in inin in controlled and known amounts and to observe the corrosion behavior of the resulting alloy. These experiments show the existence of what may be called tolerance limits" of magnesium and some of its alloys for certain impurities. The extremely small percentages of impurities involved and the sharpness of the corrosion discontinuities appear to be quite unpredictable, In order to carry on this work, it was necessary to develop an analysis technique suitable to the problem. In some cases it was necessary quantitatively to analyze impurities to less than 0,001 per cent. The experimental data to be presented are based on observation of about 5000 alloy specimens and on more than 50,000 quantitative analyses. while the primary purpose of this paper is to present the experimentally obtained data on corrosion rates as a function of composition, and particularly to demon-

Jan 1, 1942

By Norris Johnston, Carrol M. Beeson

The gravimetric-vacuum distillation method was developed to permit rapid and accurate determinations of the oil-water ratios of small samples or sands containing little oil. In addition, the samples usually are so well cleaned and so little altered by the distillation at reduced pressure that rapid estimations of other physical properties may be made with the evacuated cores. Requiring only elementary glass-blowing technique, the distilling tubes and traps used in determining oil-water ratios were easily fashioned from the usual glassware. A sketch and description are given of the necessary apparatus, including the cylindrical electrical heaters. The procedure, requiring about 40 min., consists in raising the temperature and maintaining it between 675&apos; and 725°F. for at least 10 min. while the pressure is held between I and 2 mm. Hg. The fluids condensed in the trap (cooled by a mixture of kerosine and solid carbon dioxide) are separated in a centrifuge and the volume of water is recorded. Determination of changes in weight with an analytical balance of all parts of the apparatus permits computation of weight of oil distilled and total weight of oil recovered. Introduction In determining the oil-water ratios of core samples, distillation at atmospheric pressurel-5 has proved to be sufficiently reliable for samples containing moderate quantities of oil. Since small samples and sands with little oil are encountered, how- ever, it appeared advisable to develop a method that would be applicable under these circumstances. Thegravimetric-extraction procedure1,6-9 undoubtedly is very reliable and could be used in all tests, but the time consumed in the determination would often delay field operations. This would be especially true when dealing with tight sands or viscous oils, both of which retard the extraction process. Accordingly, the gravimetric-vacuum distillation method was developed in order to combine the good features of both of the older methods; that is, accuracy and speed. By reducing the pressure, it was found possible to perform the distillation at a temperature that permits the use of glass apparatus, all parts of which can be weighed on an analytical balance. Thus, the fluids may be removed quickly from the core, the water is readily trapped and measured, and the loss in weight of the core is easily determined. In addition, the total weight of material condensed in the distilling tube and in the trap provides a method of determining the oil-water ratio that is practically independent of the one involving the loss in weight of the sample. The use of vacuum not only permits as much accuracy as does the gravimetric-extraction process, but it actually allows an increase in speed over the atmospheric-distillation method, because of the time required to cool the metal pots from about 1200°F. between runs. More important yet, the innovation makes possible the almost immediate reporting of permeability, and saturation, which is impossible

Jan 1, 1946

By Norris Johnston, Carrol M. Beeson

The gravimetric-vacuum distillation method was developed to permit rapid and accurate determinations of the oil-water ratios of small samples or sands containing little oil. In addition, the samples usually are so well cleaned and so little altered by the distillation at reduced pressure that rapid estimations of other physical properties may be made with the evacuated cores. Requiring only elementary glass-blowing technique, the distilling tubes and traps used in determining oil-water ratios were easily fashioned from the usual glassware. A sketch and description are given of the necessary apparatus, including the cylindrical electrical heaters. The procedure, requiring about 40 min., consists in raising the temperature and maintaining it between 675&apos; and 725°F. for at least 10 min. while the pressure is held between I and 2 mm. Hg. The fluids condensed in the trap (cooled by a mixture of kerosine and solid carbon dioxide) are separated in a centrifuge and the volume of water is recorded. Determination of changes in weight with an analytical balance of all parts of the apparatus permits computation of weight of oil distilled and total weight of oil recovered. Introduction In determining the oil-water ratios of core samples, distillation at atmospheric pressurel-5 has proved to be sufficiently reliable for samples containing moderate quantities of oil. Since small samples and sands with little oil are encountered, how- ever, it appeared advisable to develop a method that would be applicable under these circumstances. Thegravimetric-extraction procedure1,6-9 undoubtedly is very reliable and could be used in all tests, but the time consumed in the determination would often delay field operations. This would be especially true when dealing with tight sands or viscous oils, both of which retard the extraction process. Accordingly, the gravimetric-vacuum distillation method was developed in order to combine the good features of both of the older methods; that is, accuracy and speed. By reducing the pressure, it was found possible to perform the distillation at a temperature that permits the use of glass apparatus, all parts of which can be weighed on an analytical balance. Thus, the fluids may be removed quickly from the core, the water is readily trapped and measured, and the loss in weight of the core is easily determined. In addition, the total weight of material condensed in the distilling tube and in the trap provides a method of determining the oil-water ratio that is practically independent of the one involving the loss in weight of the sample. The use of vacuum not only permits as much accuracy as does the gravimetric-extraction process, but it actually allows an increase in speed over the atmospheric-distillation method, because of the time required to cool the metal pots from about 1200°F. between runs. More important yet, the innovation makes possible the almost immediate reporting of permeability, and saturation, which is impossible

Jan 1, 1946

By Ward C. Smith

The industry of producing and processing boron compounds is called the borax industry because the chief product is borax, the decahydrate of disodium tetraborate. For the same reason, it is common to speak of borax mining. Reference to borate mining also is common, and while appropriate where it emphasizes the diversity of borate minerals that are mined in various countries, it is rather unsatisfactory where used in a general sense, because it seems to exclude the important production of borax from brine at Searles Lake, California, and of boric acid from steam vents in Tuscany, Italy. The terms "boron industry" and "boron mining" might seem more comprehensive, but are little used, and this is fortunate because they would be misleading-the element boron is manufactured only in small amounts for special uses, and it is not found free in nature. In most occurrences, boron is combined with oxygen and is in a borate or borosilicate material. The history of the modem borax industry starts with the introduction into Europe of borax from Tibet in the 13th century, about the time of Marco Polo, if not actually by him. The discovery that borax has unique value as a flux in metal soldering and ceramic glazing must have been made at some unknown time much earlier. As a rule, any mineral that has been used so long that its early history is lost must occur in deposits that are easily recognized and worked, and this is undoubtedly true of borax in Tibet. According to meager accounts,9 the borax occurs there in arid mountain basins as surficial crusts that coat the ground about thermal springs and seeps of mineralized water, and as coarser crystals in the bottom muds of shallow pools and lakes. Much the same essential features of surface exposures and minerals easy to recognize and recover characterize most of the deposits later found and worked elsewhere. The borax industry at the present time is faced with rising demands for its products, and consequently is increasing its productive capacity and appraising its borate resources.18 The areas that contain the known borate deposits are most likely to yield additional production, hence their distribution in the world is of interest, and is summarized later in this chapter. Mineralogy The mineral raw materials used by the borax industry include various borates mined in several countries, borax extracted from brines at Searles Lake in California, and boric acid extracted from the steam of vents in Tuscany in Italy. The hydrated borates[$] of chief commercial importance are listed in Table 1, which also shows their chemical composition. The properties of only the four most important borates are summarized here, but detailed descriptions of the borates and the minerals commonly found with them can be found in mineralogy textbooks.41 Ulexite generally forms clusters of silky fibers rather than large individual crystals. A

Jan 1, 1960