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NEW MEMBERS The following list comprises the names of those persons who became members during the period May 10 to June 10, 1914. Members ABE, ASAKA, Chief Min. Engr., Yamagano Gold Mine, Satsuma-Gori, Satsuma, Japan. ANDERSON, FRANK M., Geol Cartagena Refining Co., Cartagena, Colombia, S. A. BACON, MAURICE W., Genl. Mgr Stewart Mining Co. Butte, Mont. BACON, RAYMOND F., Chem Director, Mellon Institute, Pittsburg, Pa. BAKER, HAMILTON WALLACE, Min. Engr Fernley, Nev. VON BAYER, AUGUST HECTOR, Supt Kentucky Solvay, Coke Co., Ashland, Ky. BISHOP, WHEELER SCOTT, Research Chem Care Braden Copper Co., Rancagua, Chile, S. A. BOWEN, CHARLES GILMAN, Timekeeper 208 School St., Grass Valley, Cal. BOYER, SAMUEL L., Mine Operator, Mgr., Mike. Horse Min. Co., W. 2808 Boone Ave., Spokane. Wash.

Jan 7, 1914

By C. P. Lawhon, J. P. Simpson, W. M. Evans

Recent efforts to design drilling fluids for increased drifting rates have confirmed some laboratory results of other investigators, but have also produced additional data that should be considered. These data were obtained under controlled test conditions using a microbit drilling machine. Clays and some polymers have previously been reported to cause reduction in drilling rate. Recent data have shown that under laboratory conditions, suspensions of a single day or polymer have sometimes given faster drilling rates than when water was used. Measurements have been made of clay suspensions and polymer suspensions comparing filtration (I) under API conditions, (2) while drilling with temperature of 150F and differential pressure of 1,000 psi and (3) under dynamic conditions after drilling. Some correlation between instanraneous filtration (white drilling) and drilling rate has been observed. INTRODUCTION Several papers have been presented that related drilling fluids to penetration rate. Generally, it was found that a decrease in the solids concentration resulted in significant increases in the drilling rate. Of course, this change also resulted in a decrease in the viscosity of the drilling fluid.' Conclusions from investigations by this laboratory are in agreement. Data have shown that of the simple mud measurements commonly made at the drilling rig (density, plastic viscosity. yield point, API filtrate and total solids), only the density and total solids have a significant relationship to the drilling rate in Berea sandstone when attempting to correlate a single mud property individually.' More recent drilling rate experiments have been designed to study (1) effects of individual clays and polymers on drilling rates in Berea sandstone and Lueders limestone, (2) the relationship between drilling rate and dynamic filtration as measured after drilling and (3) the relationship between drilling rate and dynamic filtration as measured during drilling. Data show that drilling rates are dependent upon type and concentration of particles, type of formation and filtration of the individual fluids while drilling. Mud pressure: pressure of drilling fluid as measured after leaving the drilling chamber (Fig. 1). This is taken to be approximately the mud pressure just past the bit and at the face of the formation. Terrastatic pressure: pressure representing weight of overburden. Formation pressure: pressure of formation fluid as measured at outlet of drilling chamber (Fig. 1). This is taken to be approximately the pressure of fluid in the interstices of the formation. Differential pressure: difference between the mud pressure and formation pressure. LABORATORY EQUIPMENT AND TESTING PROCEDURE The drilling equipment was described in two previous publications."' Main components are a drilling chamber, filter-heater, rotary drive and variable-speed circulating pump. Auxiliary pumps supply pressure boosts for the mud, terrastatic and formation pressures. All equipment is designed for 15,000 psi and 500F. Capacity of the circulating system is approximately 7 gal. The mechanical design was facilitated by moving the rock down onto the bit. Data collected with this design should not differ from that obtained by a normal design where the bit moves into the rock. Drilling fluid is pumped through 50 ft of ID pipe coiled in an oil bath, enters the rotary shaft at a right angle and is pumped through the jets on the bit (Fig. 1). Most of the drilled solids are extracted by a screen mounted in the circulating system on the suction side of the pump. Data reported in this paper were obtained by controlling these parameters: mud pressure, 5,000 psi; formation pressure, 4,000 psi; terrastatic pressure, 5,000 psi; force on bit, 1,000 Ib; formation, Berea sandstone and Lueders limestone; flow rate, 7 gal/rnin; bit, 11/4-in. diameter with two 0.078-in jets; mud temperature. 150F; and rotary speed, 60 rpm. Mud pressure was controlled at 5,000 psi, thus giving a differential pressure of 1,000 psi even though the fluid densities varied. Cores of 3%;-in. diameter and 8 in. long were selected from quarry blocks to provide some control of grain size distribution, permeability and porosity. A 2-in. section was cut off each core and a I -in. diameter plug was taken from this section. Permeability to 5 percent by weight sodium chloride solution was determined and the large cores were

By Frederic Dewey

HAVING shown1 the difficulty of assaying so-called cyanide bullion and the extreme variations often found in the results, an investigation was undertaken to discover if possible the causes of these variations by a series of tests upon the specific action of various metals during cupellation. Zinc.-In order to test the effect of zinc, 48 assays were made in sets of 6, 2 rows of 3. The charge for the middle cupels consisted of 500+ mg. Au, 1,125 mg. Ag, 10 mg. Cu. To the end cupels 50, 75, 100 and 125 mg. Zn were added, and a set of each proportion was cupelled with 4 and 8 grants Pb. The cupels were assayed and showed the following gold contents in milligrams, the figures being arranged as the cupels stood in the muffle: TABLE 1 50 Mg. Zn 75 Dig. Zn 100 Mg. Zn 125 Mg. Zn 4 grams, Pb 0.2S 0.25 0.2S 0:29 0.27 0.34 0.33 0.28 0.41 0.31 0:30 0.36 0.30 0.33 0.34 0.31 0.31 0.29 0.35 0.37 0.42 0.41' 0.34 0.38 8 grams, Pb 0.40 0.43 0.42 0.38 0.36 0.43 0.35 0.34 0.41 0.33 0.37 0.37 0.54 0.17 0.59 0.44 0.43 0.43 0.38 0.39 0.41 0.57 0.38 0.46 _ In many instances the zinc does not appear to affect the cupel gold, but various exceptions are apparent, generally in the cupels in the back row. With 100 and 125 mg. Zn, in some cases the Zn burned with its characteristic flame before it could alloy with the other metals. Also, less fusible oxidized lumps were observed during the cupellation and some cupels showed a scum. In order to lessen the premature burning out of the Zn, an alloy of 2 parts Ag to 1 part. Zn was used. A uniform charge of 500,+ mg. Au,

Jan 7, 1917

By William R. Webster

This is a subject which our Institute has made peculiarly its own. In the first volume of its Transactions the analysis of steel received attention, and every subsequent volume has borne witness to the acuteness and industry of our members in the investigation of this subject. The keynote mas struck, in this as in so many other lines of progress, by A. L. Holley, in his paper on " Tests of Steel," read at the Easton meeting of October, 1873 (Trans., ii., 116)—an essay which may rank as a classic by reason of .its elegant form, logical force, and clear prevision of all the bearings of its theme, Taken together with the brief report of the discussion which followed it (in which Dr. Drown emphasized the effects of heat-treatment and mechanical handling, and Dr. Sterry Hunt the importance of minute variations in chemical composition, and of possible isomeric and allotropic conditions), it constitutes, after the lapse of twenty-five years, an admirable and adequate introduction to the long list of technical papers which have succeeded it. Three years later came the epoch-making papers of Dr. C. B. Dudley on the relation between the chemical composition and physical properties of steel rails, which, with the voluminous discussion they evoked, constitute a special volume, published by the Institute, and full of useful suggestions. If Dr. Dudley could be induced to resume this investigation, he would doubtless be able to solve many points still uncertain or disputed. But I cannot undertake to review the history of this subject, as represented in our Transactions—still less to restate all the contributions to it which have been made in books or in papers before other technical societies, since the initiative was taken by the Institute. My more modest purpose is to indi-

Jan 1, 1899

By Carl Gatlin, S. Srini-Vasan

It is shown thar k k ratios cornputed on the as.sutnption that the average sandstone reservoir has a pore-size distribution characrerized by a linear 1/P saturatioN plo are in good agreewient with correspotlding k,,/k,, ratios obfairzed by Wahl, Mul-/ins and Elfrink by correlatiotz of field measurements. Methods of calculating relative permeability data have recently been reviewed and extended.' It was shown that for sandstone reservoirs where ' is approximately a linear function of effective saturation (as suggested first by Corey') it is possible to express relative permeabilities in very simple terms. For systems wetted by connate water and producing oil and gas (gas saturation growing at the expense of oil) the expression for the The accuracy of Eq. I has been frequently confirmed in our laboratories; because of its simplicity we make routine use of it in the analytical solution of proble~ns in reservoir engineering. Nevertheless, comparisons of the k,,,/k,, ratios yielded by Eq. 1 with appropriate reservoir data have been few. The publica- tion by Wahl, Mullins and ElfrinkV of an empirical equation for k,,/k,, ratios is thus of interest since this equation is specificalljl stated to be Vased on the correlation of field measurements made on sandstone reservoirs. Not surprisingly these authors found that it was necessary to

By Oscar E. Harder, H. A. Grove

It is now just a quarter of a century since Fred W. Taylor§(23) pub-lished his classical paper On the Art of Cutting Metals, describing his researches in which he, in cooperation with Maunsel White, had developed what is essentially the modern method of heat-treatring high-speed steels. Regarding this research, Dr. Sauveur,(22) in his address on Steel Wizards, Past and Present, at the annual banquet of the American Society for Steel Treating in Philadelphia in 1920 said, "The discovery of high-speed steel, or if you prefer, of the treatment imparting high-speed properties to certain steels by Taylor and Maunsel White I am inclined to consider as our one epoch-making contribution to the metallurgy of steel." It was at about that same time (1900) that Taylor exhibited high-speed steels, heat-treated by the improved process, at the World's Exposition in Paris and attracted much attention by showing that the steels would operate at such feeds and speeds that the tips of the tools were visibly red hot. This observation must have started metallurgists to wondering regarding the relative hardness of the various steels at red-heat temperatures. Considerable work has indeed been done in an effort to measure the hardness of high-speed steels and related materials in the red-heat range, using various methods. The result's, however, have been only partly satisfactory, owing to experimental difficulties. The present investigation had as it's immediate inception an address by J. V. Emmons, of the Cleveland Twist Drill Co., to the Columbus Chapter of the American Society for Steel Treating in 1931, in which he deplored the fact that comparatively little was known with regard to the hardness of high-speed steels at elevated temperatures, in spite

Jan 1, 1933

By John Blatchford, William T. Hall

The product obtained by roasting stibnite is likely to contain some unoxidized antimony trisulphide and a mixture of antimony trioxide and antimony tetroxide. It was desired to determine, as accurately as possible, the condition of the antimony as well as the total quantity present. Attempts were made to separate the trisulphide and the two oxides by methods based upon their varying solubilities in different solvents, but no satisfactory results were obtained in this way. It was found, however, that by determining the total antimony content, the antimony present as trioxide, and the antimony present as trisulphide, a good idea of the chemical composition of the roasted product could be obtained. The total antimony was determined by dissolving the sample in concentrated hydrochloric acid, reducing the antimony entirely to the trivalent condition by means of hydriodic acid and eventually titrating the antimony back to the pentavalent condition by means of iodine in the presence of sodium bicarbonate1* The details of the procedure are as follows: Weigh out 0.25 gram of the roasted product into a trapped flask (Fig. I), add 4 grams of powdered tartaric acid, 2 grams of potassium iodide and 40 c.c. of concentrated hydrochloric acid. Boil the solution gently f;r 5 min. and then cool to room temperature by shaking the flask while holding it under running water. Then, very carefully discharge the iodine color by the cautious addition of 0.05-normal sodium thiosulphate solution, adding a little starch toward the last. Nearly neutralize the acid with ammonia solution, but leave the solution distinctly acid. Pour the slightly acid solution into 200 c. c. of water containing an excess of sodium bicarbonate and titrate to a permanent blue color with standard 0.1-normal iodine solution.

Jan 1, 1916

By William Lodding

Muscovite was the crystalline material used in the experiments discussed in this paper. It was both wet and dry ground for various periods of time. The effects (physical and chemical changes) produced in grinding are analyzed by use of thermal analysis. That grinding may change a crystalline material both in a physical and in a chemical sense has been shown by a number of authors in recent years. Mackenziel and Bartha2 reported the effects of careful grinding on muscovite, quartz, gypsum, dolomite, etc. Increase in specific surface produced by grinding implies increase in total energy of a system. Newly produced surfaces are chemically more reactive; dislocations may be introduced during grinding and, on the other hand, existing strain may be released by the same process, as shown by Holt, et a1.3 All these changes are easily detected by thermal analysis, but it is not easy to separate the multiplicity of effects registered and to arrive at quantitative interpretations. This paper is an attempt to analyze, by the use of thermal analysis, some effects produced in grinding. In differential thermal analysis (DTA) one measures the sum of all thermal changes occurring in a substance during heating or cooling; e.g., chemical changes, such as decompositions, synthesis, oxidation, reduction, etc., and physical changes such as phase transformations, changes in specific surface and thermal conductivity, strain release, etc. By thermogravimetric analysis (TGA), on the other hand, only chemical changes involving weight loss or gain are recorded. Similarly, gas evolution analysis (GEA) will register only reactions involving gas evolution. By performing two or all three of these methods of thermal analysis simultaneously and on the same specimen, one can separate the different effects registered and, by difference, evaluate their magnitude. The results of TGA are usually plotted as percent weight against furnace temp. When one differentiates weight against furnace temp, a rate of weight-change curve is obtained, and the resulting differential thermogravimetric (DTG) plots are similar in appearance to DTA thermograms for the same reaction. While the integrated area under a DTA peak represents enthalpy and can be expressed in calories per gram the area under the corresponding DTG peak represents the weight change which took place during a reaction. The similarity of DTA and DTG thermograms obtained from one material can be seen in Figs. 1 and 2. EXPERIMENTAL A Fisher mortar grinder and a porcelain mill with burundum balls were used for both dry and wet grinding. Muscovite was first carefully hand-filed and screened on 20 and 100 mesh. The middle fraction was considered essentially unaltered muscovite.

Jan 1, 1968

By Donald D. Carr, Lawrence F. Rooney

Perhaps no other mineral commodity in this volume has as many uses as limestone and dolomite. These carbonate rocks are the basic building blocks of the construction industry, the material from which aggregate, cement, lime, and building stone are made. Carbonate rocks, and their derived products, are used as fluxes, glass raw material, refractories, fillers, abrasives, soil conditioners, ingredients in a host of chemical processes, and much more. Although the use of limestone and dolomite goes back before recorded history, new uses and products are continually being found. Carbonate rocks form about 15% of the earth's sedimentary crust and are widely available for exploitation. Found extensively on all continents, they are quarried and mined from formations that range in age from Precambrian to Recent. Reserves of carbonate rock are large and will last indefinitely, although high-purity deposits may be absent or have limited availability in certain areas. Limestone and dolomite are so useful and so abundant that in 1981 about 644 million tons were produced in the United States. In fact, about 75% of all stone quarried or mined in the United States was carbonate rock. Sand and gravel was the only mineral commodity produced in greater quantity. In this chapter we have sought to provide the general reader an overview of carbonate rocks, their composition, distribution, production, and uses, with emphasis on developments since 1960. In doing so we borrowed extensively from our report on the applied geology of limestone and dolomite (Rooney and Carr, 1971). The literature on the limestone and dolomite resources of the United States and Canada is so vast and diverse that one can easily become mired down in print. We tried to list those references that are easily accessible and that provide the economic geologist with a starting point for more intensive study. The table listing selected references on limestone and dolomite resources in Canada and the United States reflects our attempt to be selective rather than exhaustive and to direct the reader to the best sources of detailed information. Geology Mineralogy The principal carbonate rocks used by industry are limestone and dolomite. Limestones are sedimentary rocks composed mostly of the mineral calcite (CaCO3) and dolomites are sedimentary rocks composed mostly of the mineral dolomite (CaCO3 • MgCO3). Aragonite (CaCO3), which has the same chemical composition as calcite but a different crystal structure, is economically important only in modern deposits, such as oyster shells and oolites. Aragonite is metastable and alters to calcite in time. Some other carbonate minerals, notably siderite (FeCO3), ankerite (Ca2MgFe (CO3)4), and magnesite (MgCO3), are commonly found associated with limestones and dolomites but generally in minor amounts. Because of their similar physical properties, the carbonate minerals are not easily distinguished one from the other. Specific gravity,

Jan 1, 1983

By Oswald J. Heinrich

THE origin of spontaneous combustion in collieries is, of course, chiefly due to bad system in laying out the pits, unclean workings, insufficient ventilation, and neglect in damming off works after they are exhausted of the main coal. This is particularly indispensable in the Richmond field, because it is difficult and dangerous here, on account of the inferior roof, to remove the last vestiges of coal ; and we are compelled also to retain all the slates and bands, as far as possible, in the pit, to help fill up, although such material is liable to fire. This, however, can be prevented to a great extent, as mentioned below. I am satisfied that the only system of working this thick coal is by cross-cutting (Querbau, ouvrage & travers) or working in benches, as practiced in France (Creusot, Rive de Gier, St. Etienne), in Silesia (Kiinigsgrube), which I have used as far as it is practicable in an old pit, almost torn to pieces by former workings. Modifications may, of course, be needed, even in the same pit, on account of irregularities in the seam. I am also satisfied for economical reasons (on account of the heavy cost for timbering) that pits here ought to be worked upwards, even if it requires a longer period of time to win the coal, and a greater outlay of capital to commence with. The various saddle-shaped " troubles " making natural minor basins in the main basin aid in the execution of this plan. A pit worked once ought to be worked out clean, given up, and dammed off forever. If sections of proper height are assumed, according to the required amount of production for a certain period of time, they ought to be worked out and filled in as much as possible, dammed off, and ultimately allowed to fill up with water, in order to protect the upper works in future from fire in the gob below. This I consider indispensable, because we may not be able profitably to fill in all the ground. To do so we have to use the waste of the mine, although it is liable to fire in time. In using this stuff, it ought to be surrounded by walls of rock not liable to take fire, laid firmly in clay, the gob being in the middle, and firmly covered and packed with clay on top. In

By Oswald J. Heinrich

(with figures on plate V.) THE origin of spontaneous combustion in collieries is, of course, chiefly due to bad system in laying out the pits, unclean workings, insufficient ventilation, and neglect in damming off works after they are exhausted of the main coal. This is particularly indispensable in the Richmond field, because it is difficult and dangerous here, on account of the inferior roof, to remove the last vestiges of coal ; and we are compelled also to retain all the slates and bands, as far as possible, in the pit, to help fill up, although such material is liable to fire. This, however, can be prevented to a great extent, as men¬tioned below. I am satisfied that the only system of working this thick coal is by cross-cutting ( Querbau, ouvrage à travers) or working in benches, as practiced in France (Creusot, Rive de Gier, St. Etienne), in Sile¬sia (Königsgrube), which I have used as far as it is practicable in an old pit, almost torn to pieces by former workings. Modifications may, of course, be needed, even in the same pit, on account of irregu¬larities in the seam. I am also satisfied for economical reasons (on account of the heavy cost for timbering) that pits here ought to be worked upwards, even if it requires a longer period of time to win the coal, and a greater outlay of capital to commence with. The various saddle-shaped "troubles" making natural minor basins in the main basin aid in the execution of this plan. A pit worked once ought to be worked out clean, given up, and dammed off forever. If sections of proper height are assumed, according to the required amount of production for a certain period of time, they ought to be worked out and filled in as much as possible, dammed off, and ulti¬mately allowed to fill up with water, in order to protect the tipper works in future from fire in the gob below. This I consider indispen¬sable, because we may not be able profitably to fill in all the ground. To do so we have to use the waste of the mine, although it is liable to fire in time. In using this stuff, it ought to be surrounded by walls of rock not liable to take fire, laid firmly in clay, the gob being in the middle, and firmly covered and packed with clay on top. In

Jan 1, 1873

By J. Burns Read

IT IS the purpose of this paper to summarize, as far as possible, the metallurgical information and experience gained by the Ordnance Department, during the War, in the manufacture of artillery cartridge cases, to describe the tests to which artillery cartridge cases were put, and to summarize the knowledge and experience gained in this testing. The authors wish to acknowledge the aid given by manufacturers, army officers, and civilian employees of the Ordnance Department in obtaining these data. Artillery cartridge cases are cold drawn from circular disks punched from strips of rolled brass. The manufacture involves from 25 to 30 main operations, which are done almost entirely on a punch press. Descriptions of the operations have appeared in various periodicals and, therefore, will not be given here. After each cupping, or drawing, operation, except the last, the cases are annealed at from 540° to 650° C. (1000° to 1200°F.), to remove all the hardening stresses set up in the metal and to allow complete recrystallization. After each annealing, the cases are pickled in niter cake or sulfuric-acid solution and then washed in water to remove all traces of acid. In some instances, the cases are then immersed in a cyanide-salt solution, and afterwards rinsed in water, to remove the thin layer of copper that forms on the surface of the cases during the acid pickle. The last cold-drawing operation is followed, by the heading operation which, by flattening the head of the case on the outside, causes the metal to flow on the inside to approximately the proper finished dimensions. The mouth, or open end, is then annealed at 430° to 480° C. (800° to 900° F.) by immersion in a salt bath or by gas flames. After being washed, the cases are tapered, when they are ready for machining, inspection, and testing.

Jan 4, 1922

By H. S. Bell

It seems unnecessary to dwell upon the advantages of the modern pipe still as compared with the older type of distillation equipment used by oil refiners. The relatively low installation cost, coupled with remark-able operating efficiencies of pipe stills, precludes the consideration of other types except in rare instances where some peculiarity of product or plant may have an influence. The question of the actual heat required to distil petroleum is quite involved. We have extensive data on the latent heats of the various hydrocarbons under different conditions of pressure. We also have information regarding the specific heats of various oils and the effect of temperature thereon. Because of the complexity of petroleum and of each fraction, it seems impossible to analyze theoretically the partisl-pressure effect of the great number of hydrocarbons upon one another during distillation. If a distillation curve and percentage analysis of any crude or product are available, it is possible to construct a curve with ordinates representing per cent. distilled and B. t. u. per pound or per gallon, or other desired unit. To do so the crude is split into fractions, of 5 or 10 per cent. The boiling point and gravity of each fraction being determined, it is possible to evaluate the heat required. As each fraction is removed, the residue must be raised to a higher temperature and latent heat supplied for the successive fraction. As the calculations progress, the latent heats decrease while the specific heats increase. Such a curve is illustrated by Fig. 1 for a typical 39.9° Be. North Texas crude. The chart is illustrative of batch distillation. Theoretically, if the oil were heated by a single flash in a pipe still, the partial-pressure effect of the light products would result in the removal of the same amount of vapors at a lower temperature. Practically, we find that because of the necessarily extensive fractionating equipment required when separating many products all in vapor phase, the oil has to enter the separator at temperatures corresponding to or even above those required in the batch still. Furthermore, in single-flash distillation the vapors evolved in the heater must be superheated to the outlet temperature. Very little is

Jan 1, 1928

By Frank C. Kelton

It is perhaps not widely realized that extraction and saturation processes carried out on oil well core samples alter the properties of these samples to varying degrees. On the other hand it is felt by some that quick-freezing of core samples increases their permeability and porosity significantly. Accordingly, laboratory tests were carried out on 49 pairs of horizontally adjacent samples in order to differentiate between the effect of quick-freezing per se on permeability and porosity of the samples, as distinguished from the effect of the identical saturation treatment on permeability and porosity of the companion samples. Also, additional field data were obtained on comparison of frozen vs unfrozen companion samples. LABORATORY INVESTIGATION OF FREEZING us SATURATION EFFECTS Procedure The samples used in these tests were two-cm cubes cut in horizontally adjacent pairs from cores from eight Gulf Coast and Mid-Continent wells, which cores had not previously been frozen. These samples were extracted with carbon tetrachloride, dried, and air permeabilities run in the conventional manner. They were then evacuated and saturated with brine of 25,000 ppm sodium chloride content, and porosities determined by gain in weight. The samples were partially desaturated by evaporation down to an average brine saturation of 68 per cent. One sample from each pair was quick-frozen by covering with dry ice after wrapping in a single layer of paper, and allowed to remain frozen for about two hours; the companion sample from each pair was not frozen. After thawing the frozen sample, all samples were immersed in tap water overnight in order to leach out most of the brine. Air permeabilities were re-run, and the samples were again saturated with brine to determine a second porosity value. For purposes of averaging of data, the samples were grouped according to four permeability ranges, from 0 to 10, 10 to 100, 100 to 1,000, and 1,000 to 3,840 md. Average permeability and porosity changes for the frozen vs the unfrozen adjacent samples are shown in Table 1. Discussion As may be seen from Table 1, the averages of the per cent permeability increases for the quick-frozen samples ranged from 3.8 to 12.9 per cent among the four permeability groups. The average changes among the four groups of unfrozen companion samples ranged from a decrease of 0.2 per cent to an increase of 9.3 per cent. There was no particular correlation of these changes with magnitude of permeability; however, the increase for each group of frozen samples paralleled the increase for the corresponding unfrozen samples. The differences between the two sets of values are believed to be a valid indication of the effect of the quick-freezing in itself, since the treatment of the two samples in each pair was identical except for freezing. The permeability changes which are strictly the result of the quick-freezing are shown in the sixth column of Table 1. These range from a decrease of 0.9 per cent to an increase of 4.0 per cent; the overall weighted average is 1.2 per cent, as compared to an average increase of 6.8 per cent caused by the saturation treatment of the samples not frozen. The average porosity changes are in general smaller than the changes in permeability, and range from a decrease of 2.3 per cent to an increase of 3.3 per cent. The overall weighted average change ascribed to the quick-freezing is 1.0 per cent of porosity. Many factors can contribute to the changes in permeability and porosity observed when subjecting cores to the simple processes used in these tests. Such are: hydration and swelling of clay, adsorption of ions, changes in surface structure and wettability, expansion and compression effects due to ice formation, shrinking and cracking, leaching of salts and colloids, displacement of particles resulting in either blocking or enlarging of pore openings. Whatever particular mechanisms are involved. however, it is apparent not only from this study but also from other investigations in the literature' not directly concerned with quick-freezing, that the effects produced by commonly used extraction, saturation and drying techniques may be of considerable magnitude The results of this study indicate that for the particular samples and techniques used, such effects are of the order of five to six times the effect of quick-freezing. insofar as changes in permeability are concerned. It may be argued that these samples might not include extremely shaly material where the effect of freezing upon permeability may be much greater. However, had such material been available for these tests, it would undoubtedly have been very susceptible also to alteration by the extraction and saturation treatment used. To investigate this point further, the individual sample data were re-grouped according to the magnitude of the average per cent permeability increases for the pairs of samples, irrespective of permeability. The results

Jan 1, 1953

By D. Turnbull, R. E. Cech

FISHER, Hollomon, and Turnbull have developed a theory for the nucleation of martensite. They first tested the theory on Fe-C alloys and low alloy steels. The major factor influencing nucleation of martensite was considered to be statistical composition fluctuations occurring in small regions at high temperature and frozen-in on quenching. These local regions of varying size and composition serve as nucleation centers. They become supercritical, one by one, as temperature is progressively lowered, resulting in temperature-dependent or athermal transformation. Fisher next applied nucleation theory to substi-tutional solid solution alloys. Detailed predictions were made for Fe-Ni alloys because of the availability of free energy data on this system. It was shown that composition fluctuations that were significant energy-wise did not occur, and nucleation frequencies could be calculated from average properties of the system. Nucleation was predicted to occur as time-dependent and having the functional relationship to give a C curve of nucleation frequency vs temperature. The analysis further predicted that the nucleation frequency was extremely sensitive to composition. Experimentally, it would be found that the transformation in some compositions is so slow that measurable amounts will not form in a reasonable length of time. With other compositions, only slightly different, the nucleation frequency becomes so great that the material becomes transformed while still distant in temperature from the maximum nucleation frequency. On quenching an alloy of such composition, the observed transformation kinetics would be similar to those found in Fe-C alloys. Cech and Hollomon repeated experiments of Kurdjumov n which the kinetics of transformation were similar to those predicted by Fisher for Fe-Ni alloys. The alloy studied in this investigation contained 73.3 pct Fe, 23.0 pct Ni, and 3.7 pct Mn. Fisher,' using an idealized model for the extent of transformation as a function of the number of martensite crystals per grain of parent phase, derived nucleation frequencies from the transformation curves of Cech and Hollomon. Complicating influences such as coupling effects between grains in the polycrystalline specimens were neglected. Nevertheless, excellent agreement was found between the theoretically and experimentally derived nucleation frequencies. These experiments, however, could not provide a critical test of the theory. Experimental nucleation frequencies could vary widely from those calculated, depending upon the extent of deviation from ideal partitioning and the extent of coupling effects. Further, since the compositions of material theoretically analyzed and experimentally determined were different, the free energy changes involved in the experimental work could only be estimated. Also, the effect of heterogeneities on the transformation kinetics was not considered. For these reasons, it was decided that experiments designed to test the validity of the Fisher analysis must be conducted on binary Fe-Ni alloys, which were the ones considered theoretically by Fisher. The martensite transformation in Fe-Ni alloys has been the subject of considerable study. Machlin and Cohen have shown that transformation proceeds in a manner quite unlike that in any other ferrous alloy system. They found that single crystals would transform to a large extent in a single burst. In large grain polycrystalline specimens, frequently more than one grain and sometimes the whole specimen would transform at the same instant in this manner. Results on filings indicated that different particles would undergo the burst transformation at widely different temperatures. These results support the conclusion that the transformation behavior could not be described by a single nucleation frequency as would be the case if the nucleation were homogeneous. It appeared that further work was necessary to define the factors responsible for burst-type transformation, so that the conditions could be altered to favor homogeneous nucleation of martensite if such could be accomplished. This report summarizes the results of some experiments conducted with powdered Fe-Ni alloys for this purpose and the re-

Jan 1, 1957

By G. A. Swanquist, E. M. Morales

INTRODUCTION The idea of water management and control at the Church Rock Mill operations began to take shape in February 1979. At that time, we were already investigating the feasibility of decreasing the fresh water requirements so that the solids would become the limiting factor in tailings impoundment utilization. The area for solution evaporation could be kept at a fraction of the normal requirements under the standard process of full water usage. The Church Rock Mill is an acid leach circuit followed by solids/liquid separation with thickeners in counter current decantation, and solvent extraction. Following the normal design of acid leach circuits, reuse of tailings solution was not incorporated in the original mill process design. INITIAL WATER CONTROL INVESTIGATIONS The investigations to decrease the fresh water requirements centered around modifying the grinding circuit from the present semi-autogenous grinding (SAG) mill in closed circuit with hydrocyclones, to open circuit grinding with a rod mill. The open circuit grinding with the SAG mill and rod mill in series had the potential of decreasing the water requirements for grinding and leach dilution by approximately 50% or 1.4 m3/min (300 gpm). The grinding pulp density would be maintained at 70 to 72% solids, and the leach dilution to 50% solids would be accomplished with acid tailings liquor recycle. In such a grinding circuit arrangement, the SAG mill would provide the primary or coarse grind, and the rod mill would be used for the fine grind. By the SAG mill and rod mill series grinding method of water control and other secondary water controls in various places downstream from the grinding circuit, the required necessary evaporation area was estimated at 120 acres of liquid surface. A second method of water control at grinding was investigated. A two-stage cyclone classification circuit appeared to have a good potential of achieving the same water reduction at a much lower capital and operating cost. However, in retrospect, this would not have been a viable method since a high slime recycle load would have been established hindering classification. The use of reagents to neutralize the acid tailings solution was not considered seriously at that time, since it would have materially increased operating costs, although it would have also allowed more tailings solution recycle and consequently, less fresh water usage. However, with the tailings solution deposition area available at that time, it was not then necessary to incur the high cost of neutralization. The control expected by the series grinding of semiautogenous and rod mills would have been sufficient to maintain a water consumption/evaporation equilibrium well in line with the available land area. IMPLEMENTATION OF NEUTRALIZATION OPERATIONS During the summer of 1979, the UNC Church Rock Mill experienced a tailings dam breach which resulted in a prolonged mill shutdown. Upon resumption of operations at the end of October 1979, tailings deposition was restricted to a small portion of the tailings impoundment area. Figure 1 shows the general tailings area and the limits of the present deposition area in the central part including the borrow pits. These borrow pits had been excavated to provide materials for tailings dam construction. Immediately after resumption of operations, it became evident that it would be necessary to control the quantity of liquid to be evaporated because of the small confined area available for tailings solution deposition and to maximize the deposition time in the tailings area. The water control required had to be exercised on a large scale, and to be in operation as quickly as possible. An obvious solution was to reuse the tailings liquor in mill process. Immediate steps were taken to install the necessary equipment for tailings neutralization on an interim basis. Anhydrous ammonia was selected as the primary neutralization reagent since it was the quickest system that could be placed in operation. Previous laboratory tests indicated fair results with ammonia neutralization. Such a system required a minimum of installed equipment and handling. INITIAL NEUTRALIZATION OPERATIONS Actual neutralization operations began on November 26, 1979. The raffinate solution which normally would have been discarded was pumped to a 3.7 m (12ft) diam by 4.3 m (14ft) tank for reagent contact, see Figure 2. At this tank, anhydrous ammonia was added directly from the tanker trailers and controlled at pH 7.0 nominally. Agitation was provided by air sparging. The neutralized product formed a highly viscous slurry in the grinding circuit which resulted in pumping and cyclone classification problems.

Jan 1, 1982

By Nathaniel Arbiter

THE separation of minerals by flotation can be regarded as a rate process, with the extraction of any one mineral determined by its flotation rate, and the grade of concentrate by the relative rates for all the minerals. So regarded, the significant variables for the process are those that control the rates. These variables are of two types, the first describing the ore and its physical and chemical treatment prior to flotation and the second characterizing the separation process in the cells. This paper will examine the variation in rates for a group of separations, will show that a simple rate law appears to govern, and will consider the relation of the control variables to the rates. The use of rate constants for evaluation of performance and efficiency will be discussed. Flotation involves the selective levitation of mineral and its transfer from cell to launder. The flotation rate is the rate of this transfer. It may be defined by the slope of a recovery-time curve for any cell in a bank, or at any time in batch operation. The objective in flotation rate study is an equation expressing the rate in terms of some measurable property of the pulp. This can be either the concentration of floatable mineral in weight per unit volume1,2 or a relative concentration, which will be a function of the recovery." A rate equation for an actual flotation pulp will contain at least two constants, both to be determined from the data. One of these, the initial concentration or proportion of floatable mineral, is not necessarily equal to the feed assay because of nonfloatable oversize or locked particles." The other, a rate constant, is a measure of proportionality between the rate and the pulp property on which the rate depends. The value of the rate constant will be determined by the values of all variables which control the process and will be changed by significant changes in any of them. It is, therefore, a direct measure of performance. Where recovery or grade change continuously with flotation time, the rate constant will be independent of time and will characterize the entire course of the separation. Development of Rate Equations Rate equations can be developed either by analysis of the mechanism of the process or by direct fitting of equations to recovery-time data. Sutherland's attempt by the first method' suggests that the effect of particle size variation on the rate complicates the derivation of a simple equation applicable to an ore pulp. A further problem with an ore is the concentrate grade requirement, which usually involves a variable rate of froth removal. Thus the final rate for any cell may depend on the froth character and froth height, as well as on the pulp composition. This does not imply that each cell cannot reach a steady state2 in which the rate will depend ultimately on pulp composition. The second method is the fitting of rate equations consistent with the necessary boundary conditions* to experimental recovery-time curves. On the assumption that under constant operating conditions the flotation rate is proportional to the actual or relative concentration of floatable mineral in the pulp, a generalized rate equation may be expressed as follows: Rate = Kcn [I] where K is the rate constant, c is some measure of the quantity of floatable mineral in the pulp at time t, and n is a positive number. In previous rate studies, the value of n has been taken as 1, either by direct assumption," or as a result of the hypothesis that bubble-particle collision is rate determining.' A first order equation results, which after integration in terms of cumulative recovery R, leads to Loge A/A-R = Kt [2] The quantity A is the maximum possible recovery with prolonged time under the conditions used. No conclusive proof for the validity of this equation in flotation has been advanced. The evidence cited in its support consists entirely in the demonstration that it appears to apply to a limited number of recovery-time curves."' It will be shown subsequently that this procedure is not sufficient to establish the order of a flotation rate equation. The possibility that the equation may be of higher order therefore requires examination. If, in particular, the exponent in eq 1 is assumed to be 2, then after integration there results R = A2Kt/1 + AKt [3] with K again a rate constant and A the maximum proportion of recoverable mineral. Eq 3 may be

Jan 1, 1952

By A. R. Troiano, W. J. Barnett

The existence of a grain size stabilization effect on martensitic type reactions as shown by Scheill in an iron-29 pct nickel alloy and by Troiano and Tokich2 in cobalt prompted a review of other martensitic reactions to determine if this stabilization effect is characteristic of all martensite type reactions. Preliminary work has shown this effect to be present both in the gamma —+ epsilon transformation in an iron-20 pct manganese alloy and the martensite transformation of SAE 4140 and 3 pct Cr-O.40 pct steels. No appreciable effect was found in an SAE 2340 steel. The M, temperature for the gamma —+ epsilon transformation was lowered from 380°F to about room temperature by varying the annealing treatment following cold work as shown in Table I. The effect of austenitic grain size on the M, of three steels is shown in Table 2. M, was deter- mined by the conventional quench-temper method of Greninger and Troiano. In a single crystal the change in external shape concomitant with the homogeneous shear mechanism of the martensite transformation can take place unhindered. In a polycrystalline specimen a restraint of these changes must occur at the grain boundaries. Therefore, the smaller the grain size the greater the shear strain energy necessary for the formation of a martensite crystal. The degree of lowering of M, due to the reduction of grain size is much greater when the change in crystal structure involves only a small energy change, such as face-centered cubic —+ close packed hexagonal (that is, CO and Fe-20 pct manganese alloy). The maximum lowering of M, observed in the steels investigated was 50°F with a change in the ASTM austenitic grain size of 1-2 to 8-9. In comparison, the crystal structure change face-centered cubic —+ body-centered tetragonal involves a considerable energy change. There is little doubt that with much finer grain sizes the increased grain boundary restraint would greatly enhance this stabilization effect. The implications of this phenomenon are multifold. Undoubtedly. under certain conditions it offers a method of stabilizing high temperature phases for room temperature

Jan 1, 1949

By Hiram Brown

The problem of stress corrosion has been discussed a great deal recently, but many factors have as yet not been clarified. There are many interpretations of the definition of the word, different corrosive media are used, and numerous methods of stressing are utilized. Some quarters believe that the inherent strength of the material under test is the determining factor of its resistance to stress corrosion, while others think that the natural corrosion resistance of the material is the determining factor. This paper is intended merely to set forth the limited experience we have had and to discuss some of the other stress-corrosion tests which have been made with light alloys.

Jan 1, 1945

Jan 1, 1887