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By A. B. Kinzel

Since the exposition of the behavior of certain iron alloys by Sykesl involving the existence of an austenite loop and the discovery of such a loop in the chrome-iron system by Bain,2 there has been much conjecture both on his part and on the part of metallurgists in general as to the exact shape and location of this loop. In previous work commercial steel has been used and the microscope has been employed to locate the critical points so that the position of the loop has been quite approximate. Numerous attempts have been made to measure the critical points of the carbon-free alloys but all of these for one reason or another have failed. A satisfactory method for studying these phenomena is presented here. MateRial The first difficulty in this study was to obtain pure chromium-iron alloys. This has been overcome by melting in a vacuum electrolytic iron and chromium analyzing 99.84 Cr, Fe and C. A pure magnesite crucible was used and the melt allowed to solidify in the crucible. A typical analysis is chromium, 10.10 per cent., carbon, 0.006 per cent., silicon and manganese nil. To overcome the problem presented by segregation, ingots were made into wire 0.04 in. in diameter. This was accomplished by hand-forging the ingots into rods, using an oxyhydrogen flame for heating, in order to avoid carbon. Subsequently the rods were swaged to wire, the heating being carried out in hydrogen. Thus local segregation was eliminated although differences in analysis between portions 50 ft. apart were noted. An electric-resistance method was first tried to determine the critical points, but due to the physical defects in the wire this failed. Bain had previously shown the presence or absence of critical points in a qualitative way by observing the sag in a catenary. The author has devised the following method which gives an accurate determination of the critical points from expansion-temperature curves of suspended wire, a special telescopic dilatometer being used for the purpose.

By Mark C. Malamphy

During colonial times, Brazil was famous for the richness of her alluvial gold deposits. Paul Ferrand has estimated that the gold produced during the period from 1700 to 1820 was the equivalent of some 64 million pounds sterling. Since that time, most of the more prolific alluvial deposits have been exhausted. A few gold mines are still functioning, notably the Morro Velho mine, which is one of the deepest mines in the world. Today, the gold production of Brazil is insignificant when compared with world figures, but there are still many gold-bearing regions and it is probable that in at least some of them profitable returns would result from an exploitation program taking advantage of all the most modern innovations in gold mining and ore treatment on a large scale. In order to demonstrate the value of some of these abandoned prospects and stir up interest in increasing the national gold production, the government has stimulated research. Experimental plants have been and are being established in various places, and tests on large quantities of ores are being carried out on a semicommercial basis. The Geological Survey of the State of Minas Geraes is very active in this line and the Federal Institution is also showing an increased interest in the matter. One of the lesser known gold-bearing regions of Brazil is in the vicinity of Lavras, in the State of Rio Grande do Sul. Gold was first reported from this region in the early part of the nineteenth century. In 1811, D. João VI sent an experienced prospector from Minas Geraes to investigate the validity of the reports. According to the reports of Baron Eschwege, he succeeded in extracting some 30,000 Oitavos (about 105 kg.) during the first few years, but the production costs exceeded the value of the gold obtained.

Jan 1, 1934

By Henry D. Hibbard

A noted ordnance engineer once said to a friend, in speaking of the production of great steel guns, " How is it ? We design our guns with a factor of safety of eight, and the guns burst." The vague way in which internal stresses and strains in iron and steel are often considered and spoken of makes it worth while to examine them, as to their nature, their causes and results, how they may, for useful purposes, be advantageously dealt with, and how, when detrimental or dangerous, they may be reduced or kept within harmless proportions. Rankine defines " strain " as a change of form or dimensions of a solid or liquid mass produced by a stress. This definition seems intended not to cover strains due to internal stresses, and it will help us in the present inquiry to consider strain as a tendency to change as well as an actual change of form. Internal strains in iron and steel are the result of stresses within the mass of the piece, some parts pulling and others pushing in resistance to them; or, in other words, some parts are in tension and some in compression, each part striving to relieve itself from strain and make the piece assume a form in which all parts are at rest. Subdivision, so that each part could relieve its strain by motion relative to the other parts, would, if carried out far enough, practically obliterate strain. The internal strains we are now to consider are not those due to the stresses of the service which the piece is rendering, either alone or as a part of a structure, which may be termed service-strains, but those which originate or at least are contained in the piece itself. Internal stresses in a piece of metal are, like action and reaction, always equal and in opposite directions. The stresses

Jan 1, 1907

By Alexander L. Field

This paper contains an account of experimental results obtained in an extensive investigation of steels containing zirconium. There recently appeared' an announcement by F. M. Becket, at whose suggestion and under whose general direction this investigation was made, a statement of the outstanding features of the work and a brief explanation of the factors that led to its inception. It is not possible, in a paper of this character, to record all of the operating and test data collected, which includes the production of more than 350 heats of steel. The difficulty of a complete presentation is increased by the fact that several lines of experimentation are too incomplete to warrant publication of the results at the present time. In addition to the methods of manufacture and test employed in the work, there is described experimental evidence on which are based certain definite conclusions regarding the remarkable effects brought about by the presence in steel of relatively small percentages of zirconium. When added to a molten steel bath, zirconium combines chemically with dissolved oxygen, nitrogen, and sulfur, in the order named, and is capable of neutralizing the embrittling effect of phosphorus in whole or in part; although in the case of phosphorus there is no evidence so far of actual chemical combination. These effects arc not in the nature of suppositions supported by theory, nor is their existence deduced merely on the basis of analytical evidence. In each phase of its relation to or reaction with the four impurities mentioned, zirconium affects beneficiauy the mechanical properties of the steel to which it is added, in a manner which it is one of the purposes of this paper to explain in terms of a tentative working theory.

Jan 1, 1923

By Alexander L. Field

This paper contains an account of experimental results obtained in an extensive investigation of steels containing zirconium. There recently appeared' an announcement by F. M. Becket, at whose suggestion and under whose general direction this investigation was made, a statement of the outstanding features of the work and a brief explanation of the factors that led to its inception. It is not possible, in a paper of this character, to record all of the operating and test data collected, which includes the production of more than 350 heats of steel. The difficulty of a complete presentation is increased by the fact that several lines of experimentation are too incomplete to warrant publication of the results at the present time. In addition to the methods of manufacture and test employed in the work, there is described experimental evidence on which are based certain definite conclusions regarding the remarkable effects brought about by the presence in steel of relatively small percentages of zirconium. When added to a molten steel bath, zirconium combines chemically with dissolved oxygen, nitrogen, and sulfur, in the order named, and is capable of neutralizing the embrittling effect of phosphorus in whole or in part; although in the case of phosphorus there is no evidence so far of actual chemical combination. These effects arc not in the nature of suppositions supported by theory, nor is their existence deduced merely on the basis of analytical evidence. In each phase of its relation to or reaction with the four impurities mentioned, zirconium affects beneficiauy the mechanical properties of the steel to which it is added, in a manner which it is one of the purposes of this paper to explain in terms of a tentative working theory.

Jan 1, 1923

Lieut. Maxwell E. Erdory, now with the Army of Occupation in France, writes as follows: "The 602d Engrs., many of whose officers are members of the Institute, started its active service in France at Avocourt, where we built a road across `No Man's Land.' This road from Avocourt to Montfaucon started us on a career of road building which lasted from Sept. 26 to Nov. 9. The engineer in war has no working hours. Our first job meant 50 hr. continuous work, a layoff of 4 hr. and 18 hr. more. That was our initiation in this war game. "Back in the States we practised building trenches, dugouts, and underground shelters of all sorts. In France we were unfortunate enough to come upon the scene when the so-called open warfare started. That made all the above unnecessary. Roads was the cry and our job was to see that all the artillery got their roads and got over them. "I might mention here that the roads of France, which were in excellent condition except for numerous shell holes, w re one of the leading factors in the rapid termination of the war. "We built a narrow-gage railroad from Romagne to Landre St. George which cost us a few men. At Stenay we did our first bridge building. We built nine bridges across the Meuse, capable of carrying tanks, in 18 hr. The next day the American army crossed these bridges on their way to Virton, Belgium, and the Rhine. " Our course from Virton, Belgium, took us through Longwy, Musson, and Athus, in which towns I inspected the steel plants. In Musson as well as Longwy the Germans had destroyed most of the blast furnaces. This destruction began in August, 1917. In Athus the furnaces were in good condition, the Germans having removed all motors land electrical apparatus, rendering the plant inoperative. I have taken several photos of interest of these plants. "It is but fitting that I say that the engineer in this war has contributed much toward its success but the "Doughboy" is its hero and we engineers one and all say "All hail the Doughboy."

Jan 2, 1919

By Howard S. Bryant

The state of Kansas in 1931 continued to hold fourth place on the list of oil-producing states, despite the fact that low prices for crude oil curtailed drilling to just one-half the amount done in 1930, which itself was the lowest in the preceding 10 years. The estimated crude oil production for 1931, according to sources available to the writer, will approximate 37,037,000 bbl., the lowest since 1925. Thus Kansas produced one-eighth less oil this year than it did last year when it produced 42,729,085 barrels. This year's development was characterized by a very small amount of wildcat drilling; however, large new areas were semiproven for oil production, and several thousands of acres were added to the actually proved areas in western Kansas, so that the state now has larger proven areas of oil reserves than at any time in its history since the heyday of the famous El Dorado pool. The general prospects for oil production in the near future are indeed promising for central western Kansas, where drilling costs are moderate and depths are relatively shallow compared to the remaining unexplored parts of the northern Mid-Continent area. Probably the greatest singular achievement in the state for 1931 was the development of its natural gas reserves. This development took place principally in two spots, McPherson County in central Kansas, and Stevens and Morton counties in southwestern Kansas, and it is a matter of record that more than one and one-half billion cubic feet of open-flow capacity per day were added to reserves, nearly twice the amount developed in 1930, previously the largest amount in the history of gas development in Kansas. Gas pipe lines already built and now building are in position to deliver natural gas by one system to Chicago, Ill., by another to Indianapolis, Ind., from whence lines already lead practically to the Atlantic seaboard, and to other cities large and small located west, northwest, north and northeast of Kansas. Table 2 shows all well completions for 1931 in a form to compare with the results of previous years.

Jan 1, 1932

By B. L. Dunic, Terkel Rosenqvist

rr has long been suspected that sulphur has a small but finite solid solubility in iron, but up to the present more accurate data have been lacking. The survey given by Hansen' illustrates the divergence of data and opinions. Solubilities between 0.01 and 1.5 pct have been suggested, and opinions vary regarding the effects of temperature and phase transformations in iron on the sulphur solubility. The extent of solid solution and its variation with temperature might be expected to be an important factor in the occurrence of hot shortness in steel. Therefore, the object of the present investigation was to study this problem more systematically. It was furthermore hoped that solubility data for sulphur might contribute to an understanding of the factors which determine solid solubilities in general. Experimental Procedure The present work was based on the measurement of the chemical activity of sulphur in the solid solution by means of equilibrium with a mixture of hydrogen and hydrogen sulphide. When the solid solubility limit is reached, the sulphur activity in the iron becomes equal to that in the coexisting sulphide phase. A gas mixture of a controlled H,S/H, ratio was passed over pure metallic iron heated to a temperature in the range 900" to 1500". The amount of sulphur absorbed by the iron was determined by analysis, and from a plot of percentage of sulphur vs. gas composition the sulphur activity and the solubility limit were determined. As the rate of diffusion of sulphur in solid iron is very small, often several days were needed to be sure that equilibrium conditions had been established. To produce a gas flow with less than 1 pct H,S of constant composition for several days, was in itself a problem. The most satisfactory arrangement was obtained by a continuous synthesis of hydrogen sulphide from the elements. This was done in the part of the apparatus shown to the left in Fig. 1. The hydrogen used was first purified in tank batches by passage through activated charcoal cooled in liquid nitrogen under a pressure of 150

Jan 1, 1953

By Alfred H. Bell

The year 1937 has been outstanding in the history of the Illinois oil industry. During the course of the year the state's daily production has been trebled, increasing from 12,000 bbl. per day at the beginning to 37,000 bbl. per day at the end, and the year's total, 7,426,000 bbl. is 66 per cent above the previous year's production of 4,475,000 bbl. The production in January was 368,000 bbl.; in December it was 1,085,000. Production from the old fields increased slightly. Most of the new production is from fields in the central part of the Illinois Basin, an area that for many years was considered unfavorable to the occurrence of oil and gas. The principal producing horizon of the new fields is the McClosky "sand," an oolitic limestone in the Ste. Genevieve formation of lower Mississippian age. Although development has not yet gone far enough to permit accurate estimates of oil reserves in the new fields, it is believed that they are of the order of 100,000,000 barrels. The following are the oil fields discovered in 1937 listed in order of amount of daily production at the end of the year; Noble (Richland County), Clay City, including Southeast Clay City (Clay and Wayne counties), Patoka (Marion County), New Centralia (Clinton County), Olney (Richland County), Cisne (Wayne County),.Beecher City (Fayette County), and Rinard (Wayne County). One gas field, the Russellville, in Lawrence County, was discovered in 1937. For locations of the new fields see Fig. 1. A generalized geologic column for Illinois, showing producing horizons in the new fields, is given in Fig. 2. The total productive area of the new fields at the end of 1937 was 1712 acres, in which 230 wells were producing. Thisrty-five dry holes were drilled within 1/4 mile of producing wells. At the end of the year there were 19 drilling wells, 28 rigs standing, 18 rigging up and 4 new locations in these fields. In the whole state 447 wells were completed, of which 284 were oil producers and three gas producers. Total initial daily production of

Jan 1, 1938

By G. F. Fix, R. E. Esarey

During 1939, Indiana experienced a grcat increase in prospecting and drilling for oil and gas. Major activity, as during the preceding year, was in the southwestern part of the state, the Indiana portion of the Eastern Interior Coal Basin. An increasing interest was evident during the year, however, in the entire state, chiefly in northern Indiana (on the south flanks of the Michigan Basin) and in the old Trenton field of east central Indiana. In the latter area several tests to deeper horizons in the Trenton and to the underlying St. Peter sandstone were completed. Results in this area have been discouraging, however, since these deeper horizons are very erratic. The regional structure in the Indiana portion of the Michigan Basin is generally favorable to oil accumulation, but the picture is complicated by a uniform mantle of glacial drift and a lack of subsurface information. Several wells were started during the last half of 1939 to test the Devonian and Trenton formations in this area. Production from these formations was found at several localities many years ago, hut, no sustained effort has been made to locate pools in this area, which covers perhaps 20 counties. There were 377 wells completed in Indiana during 1939, and 77 others were in various stages of drilling at the close of the year. Of the 377 completed, 255 were classed as field locations and 122 as wildcats. The field wells were divided as follows: 156 oil wells, 39 gas wells, and 60 dry holes; the wildcats: 98 dry holes, 19 oil wells and 5 gas wells (wildcat oil and gas wells include deeper production in oil fields and field extensions as well as new field discoveries). During the year 218 more wells were completed than during 1938. Outstanding developments for 1939 include the discovery of several new oil and gas fields. In the Griffin field, which was discovered during the closing days of the previous year, 103 wells were drilled, including field extensions. Of these, 97 were productive oil wells. This field now covers more than 2000 acres of productive area and has not as yet been defined. There are five producing horizons in the field, including the Waltersburg, Tar Springs, Elwren, and Aux Vases sandstones of Chester age and the McClosky horizon of the Ste. Genevieve limestone. Produe-

Jan 1, 1940

By G. F. Fix, R. E. Esarey

During 1939, Indiana experienced a grcat increase in prospecting and drilling for oil and gas. Major activity, as during the preceding year, was in the southwestern part of the state, the Indiana portion of the Eastern Interior Coal Basin. An increasing interest was evident during the year, however, in the entire state, chiefly in northern Indiana (on the south flanks of the Michigan Basin) and in the old Trenton field of east central Indiana. In the latter area several tests to deeper horizons in the Trenton and to the underlying St. Peter sandstone were completed. Results in this area have been discouraging, however, since these deeper horizons are very erratic. The regional structure in the Indiana portion of the Michigan Basin is generally favorable to oil accumulation, but the picture is complicated by a uniform mantle of glacial drift and a lack of subsurface information. Several wells were started during the last half of 1939 to test the Devonian and Trenton formations in this area. Production from these formations was found at several localities many years ago, hut, no sustained effort has been made to locate pools in this area, which covers perhaps 20 counties. There were 377 wells completed in Indiana during 1939, and 77 others were in various stages of drilling at the close of the year. Of the 377 completed, 255 were classed as field locations and 122 as wildcats. The field wells were divided as follows: 156 oil wells, 39 gas wells, and 60 dry holes; the wildcats: 98 dry holes, 19 oil wells and 5 gas wells (wildcat oil and gas wells include deeper production in oil fields and field extensions as well as new field discoveries). During the year 218 more wells were completed than during 1938. Outstanding developments for 1939 include the discovery of several new oil and gas fields. In the Griffin field, which was discovered during the closing days of the previous year, 103 wells were drilled, including field extensions. Of these, 97 were productive oil wells. This field now covers more than 2000 acres of productive area and has not as yet been defined. There are five producing horizons in the field, including the Waltersburg, Tar Springs, Elwren, and Aux Vases sandstones of Chester age and the McClosky horizon of the Ste. Genevieve limestone. Produe-

Jan 1, 1940

By Glenn A. Marsh, George Bernard

It is often assumed that aerated oil field brines which are to be injected underground contain dissolved oxygen in amounts which will cause appreciable corrosion. Through the use of a new portable dissolved oxygen meter, accurate determinations were made at three brine conditioning plants. At two older plants, dissolved oxygen concentration in the final treated brine was found to he almost zero In spite of aeration during the conditioning process. At a new plant, dissolved oxygen was initially present but disappeared soon after the brine was "inoculated" with oxygen-free brine from one of the other plants. Corrosion tests at the two older plants have substantiated predictions that the brines would lint be corrosive. These results show that mechanical deaeration may not always be required in brine treating plants. INTRODUCTION The present work was undertaken to add to our knowledge of aeration and deaeration of oil field brines in brine conditioning plants. It is commonly assumed that brines which are exposed to the air soon become more or less saturated with dissolved oxygen. Since oxygen-containing brines are known to be corrosive, precautions are often taken to keep air out of brine through the use of closed systems or mechanical deaeration. The study of oxygen in brine has been seriously hampered in the past because of the lack of a suitable analytical tool. The standard Winkler method for the determination of dis-solved oxygen is satisfactory for use in fresh water, but not in many oil field brines. Corrections have to be made for a number of reducing substances such as ferrous iron and hydrogen sulfide which are commonly present in natural brines. Very often the correction factors are much greater in magnitude than the amounts of oxygen which are to be determined, and consequently erroneous results are obtained. Also. erratic Winkler data are obtained when appreciable concentrations of calcium and magnesium salts are present. The first step in carrying out a systematic study involved designing a portable dissolved oxygen apparatus which would operate in natural brines. Subsequently, this apparatus was used in three brine conditioning plants. Dissolved oxygen data obtained here, and certain corrosion rate data, illustrate the interesting behavior of oxygen in these oil field brines. APPARATUS A portable dissolved oxygen meter described in detail elsewhere,' was developed specifically for use with oil field brines. It is a polarographic apparatus employing a small rotating platinum electrode (cathode) and calomel reference electrode (anode). A potential of 0.7 volts is applied across the electrodes while they are immersed in the brine to be tested. 4References given at end of paper.

Jan 1, 1952

By W. R. Bendy

GRINDING is a large and costly part of Portland cement manufacture. Prior to clinkering in the rotary kiln, raw materials are ground to a fineness of 80 to 90 pct passing 200 mesh. Then, after burning and cooling, the resulting clinker is ground to about 92 pct passing 325 mesh. In the cement industry the most favored method of grinding has always been by impact and attrition of a ball charge in a rotating mill. Other types of mills, in which materials are ground between die rings and rollers, or between die rings and large balls, are sometimes used for single-stage grinding and often for preliminary grinding followed by grinding in ball-type mills. Their efficiency is usually high, but maintenance and repair costs are high also, and the ball-type mill continues to be the most widely used. Together with 4 pct gypsum to retard setting time, the kiln run clinker—consisting of hard, semi-fused lumps that may have been crushed to — 1/2 in.—is ground to a Blaine surface area of 3000 sq cm per gram and about 92 pct passing 325 mesh. Approximately 32 kw-hr per ton, or 6 kw-hr per 376-1b barrel, are consumed in the grinding mills alone, not counting auxiliaries. Open Circuit Clinker Grinding: Many early clinker grinding plants employed two-stage, open circuit grinding. Comparatively short mills of large diameter, loaded with balls 4 in. and smaller, first reduced the clinker to 95 pct passing 14 mesh. Tube mills of smaller diameter and greater length, loaded with balls 11/4 in. and smaller, carried out the fine grinding operation. An early development was to assemble two or more stages of grinding in a single mill having two, three, or four compartments separated by division heads. There were difficulties in balancing the compartments, but compartment mills were popular in the 1920's because the layout was simple and there were no elevators and conveyors. Oversize Particles: Open circuit mills, whether separate ball and tube mills or compartment mills, always encountered the problem of tramp oversize in the product. A small percentage of clinker survived passage through the first grinding stage as particles—perhaps 1/16 in. diam—that were too large for the smaller balls in the following stages to reduce to —200 mesh. When the feed rate was lowered to reduce tramp oversize, there were serious losses in grinding efficiency. Many ingenious designs were perfected to incorporate perforated screen plates or wire mesh screens in the ball mills or in the first compartments of compartment mills. Their purpose was to prevent mate: rial passing out of the first stage until it was small

Jan 1, 1958

By R. H. Winn

In this paper a heterogeneous carbonate reservoir is considered as a succession of layers of formations of radically different porosities, permeabilities, water saturations, and rock matrix types; i.e., the heterogeneity is vertical rather than radial to the wellbore. Presumably each layer is more or less homogeneous. To determine the "net oil in place" in this reservoir it is desirable to know the porosity and water saturation of each layer. In addition, the section must be subdivided into that which will produce oil, that which will produce water, and that which will produce little or nothing. In numerous wells drilled in these reservoirs radioactivity surveys, guard electrode surveys, and caliper surveys have been made. These logs have been compared with core analysis data, when available, and the analysis of the surveys compared with production data. This study, still in progress, is intended to provide improved analytical techniques if such are possible. This paper is a progress report on the work. DETERMINATION OF POROSITY The neutron-gamma log has long been recognized as a measure of hydrogen concentration.1,2,3 In reservoirs that are free of clay, shale, or other hydrogen containing matrices, it has been accepted as a measure of porosity.4,5 Empirical methods to relate relative neu-tron-gamma intensity to porosity are often employed." To provide a more precise determination of porosity from the neutron-gamma log each instrument is calibrated immediately prior to each survey by a method which refers all tools to a hydrogenous cylinder. To insure stability a calibration check is made after each survey. These calibration records are printed as an integral part of the log that is recorded in standard counts per second. A detailed description of the calibration procedure is available in the literature.' The procedure employed insures that each Survey is numerically reproducible within the limits of statistical variation. To relate the standard neutron counts per second to porosity and hole size, records were made in test wells constructed of blocks of limestone. The porosities of the blocks were accurately measured and the blocks completely saturated with fresh water. Fig. 1 presents some of the results obtained in these test wells.' The lines shown in Fig. 1 were obtained by deriving an empirical equation relating the 11 points shown so that the relationship may be projected to larger and smaller hole sizes. A detailed description of the tool is available in the literature.' Field tests indicate that the tool is adjacent to the wall of the hole most of the time when the surveys are made in uncased holes drilled with saline muds. In this circumstance porosity may be calculated from Fig. 1 if the hole size is known. When fresh muds that form thick mud cakes are employed, the centralizing effect of the mud cake must be considered and the porosity determination is less reliable. In cased holes the combined effect of variations in hole diameter and the unknown eccentricity of the casing in the hole may make porosity determinations extremely unreliable. In any event, an accurate knowledge of hole size is essen-

Jan 1, 1958

By W. Crafts, J. L. Lamont

Electrolytic extraction of carbides from quenched and tempered steel and their examination under the electron microscope were found to be helpful in understanding the mechanism of secondary hardening in alloy steels1 and the same technique has been applied to isothermally transformed steels. A preliminary survey of the utility of the method has indicated that it has promising possibilities for investigating the characteristics of pearlite and bainite. The examination of a few carbon and chromium steels has suggested that pearlite is formed with carbides of two varieties representing the lamellar and nonlamellar forms and that bainite appears to form with a structure analogous to, but significantly different from, martensite. Procedure The method used for examining the carbides was similar to that described previously.1 The chromium steels used in the investigation were made from an Armco iron base in an induction furnace and were not treated with grain-refining deoxidizers. The composition of the steels is given in Table 1. Three-inch square ingots were forged and rolled to 1/8-in. thick sheet for use in the isothermal studies. After rolling, the sheets were sandblasted to remove the rolling scale. Specimens approximately 3/4-in. wide and l1/2-in. long were prepared from the 1/8-in. sheet. They were heated in a salt "bath at 2100°F (1150°C) for 1/2 hour, transferred to other salt baths at 1300°F (704°C), 1000°F (538°C), 800°F (426°C), or 600°F (315°C), held for various periods up to 100 hr and finally quenched in water. After quenching, the specimens were cut in half, one half being submitted to microscopic examination and the other half being used for the electrolytic extraction. The isothermally transformed specimens were submitted to examination under the light microscope to determine the degree of transformation and type of structure and were photographed at 2000 X. Carbide residues were obtained by electrolyzing in 10 pet hydrochloric acid and collecting the residue in glycerine to minimize attack by the acid. As pointed out in the earlier paper, the carbides are attacked to some degree during electrolysis. This attack is relatively minor on the coarser carbides but may be quite severe on the fine bainitic carbides. The residues were washed free of the glycerine with water and alcohol. The alcohol was removed by repeated washings of amyl acetate, and the amyl acetate suspensions were transferred to stoppered vials. Debye-Sherrer X ray diffraction patterns of the residues were prepared using a chromium target. A selection based on the microstructure and X ray data was then made of samples considered most illustrative of the progress of transformation. Electrolytically extracted residues from these samples were submitted to examination by W. D. Forgeng and A. C. Jenkins on the electron microscope at the Research Laboratories of The Linde Air Products Co. and electron micrographs were made at X 5000 and enlarged to 25,000 X. The micrographs obtained with both the light and the electron microscopes are mounted side by side in the accompanying figures. Although no effort was made to establish the T-T-T diagram for the chromium steels, the times for holding in the salt bath were adjusted with the intention of making the samples represent different stages in the transformation at temperatures of 600, 800, 1000, and 1300°F. The degrees of transformation and results of X ray examination are shown in Tables 2—4. The carbide designations refer to orthorhombic or trigonal carbide types and are not meant to imply that the compositions are exactly as indicated. X ray Diffraction Data The occurrence of Fe3C and Cr7C3 in these steels was found to be consistent with published data on comparable chromium steels. Steels A and B with relatively low ratios of carbon to chromium contained Cr7C3 in the pearlitic structures and FeuC in the

Jan 1, 1950

By R. C. Edwards, Will Mitchell, T. G. Kirkland

THREE years ago, when the Process Research Laboratory at Allis-Chalmers Manufacturing Co. sought a remedy for the increasing cost of disposing of great quantities of spent sands from foundries, R. C. Edwards developed a continuous inclined paddle scrubber which removed a substantial amount of the charred coatings from the grains with a surprisingly small amount of degradation of the sand itself.1 The satisfactory results obtained on foundry sand, using this piece of equipment in conjunction with classification, suggested that a similar procedure could probably be applied to the cleaning of other sands, such as those required by the glass and chemical industries. This paper describes the flowsheet and the results of tests performed on impure natural sands. The four materials tested were silica sands obtained from widely separated geographical areas. Three of the sands tested contained various amounts of iron oxide and the fourth an excessive amount of calcareous bonding material. The iron oxide was present predominantly in the form of grain coatings, which were scuffed by the paddle scrubber, and in all cases a product was manufactured which would meet one of the sets of specifications imposed by the glass industry' The Edwards paddle scrubber used in these tests consists of a rubber-lined steel cylinder 18 in. in diam and 48 in. long, mounted on a frame so that its slope can be varied 5 ° to 35º from horizontal. This variable slope permits controlled flow of material through the machine. Rubber paddles rotate inside the cylinder and are secured to a center shaft 2 in. square, which extends through the entire length and is turned at both ends so that it can be supported by sleeve bearings centrally fixed in the end plates of the shell. At the upper or feed end it extends through the bearing on the end plate into a sheave, to which the motor drive is connected by means of Texrope transmission. The four sets of paddles mounted on the shaft, two in each set, are made of rubber belting, 1/4 in. thick, 9 in. wide, and 16 in. long. The two paddles in each set are secured on opposite sides of the square shaft, but in the same longitudinal position along the shaft axis. In other words, the two paddles in the set operate 180° apart. Each successive set is mounted 90º from the preceding one. One end of each paddle is bolted to the square shaft and the other weighted by a steel bar, 1x1 ½ x9 in. long, which is attached about 1/ 2 in. from the outer tip of the paddle. By centrifugal force at proper shaft speed, these weights force the paddle surface to rub smoothly against the rubber lining of the cylinder. During operation, the sand forces its way between the paddle face and the surface of the cylinder, providing the necessary abrading action as the pulp flows by gravity down the length of the cylinder. The capacity of the machine is limited by the amount and the hardness of the coating material and by the quality of product desired. The degree of scrubbing is governed by the retention time in the scrubber, which in turn may be changed by varying the feed rate, water content of the feed, and

Jan 1, 1952

By C. L. Sollenberger, Will Mitchell, Ford F. Miskell

Heat treatment of ore prior to comminution reduces power requirements for grinding, reduces grinding media wear, and improves recovery of iron values from a typical Minnesota magnetic taconite. Test data demonstrating this, as well as an analysis of the economics of commercial application of the technique, are presented. THE taconites in general are hard, tough ores, difficult to grind. Liberation of iron mineral constituents usually is accomplished by grinding the ore through at least 100 mesh, and often it has been found necessary to grind substantially through 325 mesh to achieve satisfactory recovery and grade in the concentration process. Because of the fineness of grind required and the enormous tonnages of material contemplated for treatment in the future, costs resulting from grinding media wear and power consumption, together with capital investment required for comminution, approach astronomical figures. Economy in any one of these elements per ton of material ground could very well reflect a considerable saving to the ferrous industry in yearly costs. With this in mind, the Research Laboratories of Allis-Chalmers Manufacturing Co. have launched a program to discover means of effecting this economy. The initial phase of the work as described here deals with a heat treatment of crushed raw ore, followed by thermal shock in cooling, for the preparation of rod mill feed. Several investigators1-" ave noted an improvement in the grindabilities of ores treated in this manner. One investigator2 subjected low grade iron ores to heat treatment in an electric furnace. Basing his conclusions on screen analyses of crushed products, he observed that treated ore was more easily crushed than the untreated. He reported that observation of the treated and untreated ore through a microscope revealed cracks following the grain boundaries in treated ore, whereas no cracks were present in untreated ore. However, few if any have quantified the improvement in terms of total hp hours saved, reduction of wear of grinding media, or reduction of capital costs of grinding equipment involved. By means of Bond rod mill and ball mill grindabilitiesh nd by comparative wear tests, the conditions maintained during this investigation have been definitely evaluated. Heat treatment experiments have been made on a batch scale in a muffle furnace, followed by continuous scale experiments in a rotary kiln under various conditions of temperature, atmosphere, retention time, and quenching to determine the combination that would give the greatest improvement in the grindability of a taconite without affecting adversely the magnetic susceptibility of the magnetite. From these data, relative costs have been calculated for grinding both untreated and heat- treated ore on a basis of plant capacity of 120 tons per hour. Heat requirements for a rotary kiln, as well as the kiln capacity required for the treatment, have been estimated. For these tests 50 tons of ore were obtained from the Aurora mine of the Erie Mining Co., Hibbing, Minn. The ore was reported7 to have been selected from the magnetic portion of the lower chert horizons. An average chemical analysis of' this portion is shown in Table I and an approximate mineralogi-cal analysis is shown in Table 11. No attempt was made to differentiate between the various silicates because the compositions vary widely on the different horizons and depend on the degree of oxidation. Minnesotite, however, is the predominant silicate. The siderite grains were dispersed throughout the ore but were essentially associated with the rock-forming minerals. In a series of preliminary tests in which batches of —6 mesh ore were heat-treated in a muffle fur-

Jan 1, 1953

By Will Mitchell, Ford F. Miskell, C. L. Sollenberger

Heat treatment of ore prior to comminution reduces power requirements for grinding, reduces grinding media wear, and improves recovery of iron values from a typical Minnesota magnetic taconite. Test data demonstrating this, as well as an analysis of the economics of commercial application of the technique, are presented. THE taconites in general are hard, tough ores, difficult to grind. Liberation of iron mineral constituents usually is accomplished by grinding the ore through at least 100 mesh, and often it has been found necessary to grind substantially through 325 mesh to achieve satisfactory recovery and grade in the concentration process. Because of the fineness of grind required and the enormous tonnages of material contemplated for treatment in the future, costs resulting from grinding media wear and power consumption, together with capital investment required for comminution, approach astronomical figures. Economy in any one of these elements per ton of material ground could very well reflect a considerable saving to the ferrous industry in yearly costs. With this in mind, the Research Laboratories of Allis-Chalmers Manufacturing Co. have launched a program to discover means of effecting this economy. The initial phase of the work as described here deals with a heat treatment of crushed raw ore, followed by thermal shock in cooling, for the preparation of rod mill feed. Several investigators1-" ave noted an improvement in the grindabilities of ores treated in this manner. One investigator2 subjected low grade iron ores to heat treatment in an electric furnace. Basing his conclusions on screen analyses of crushed products, he observed that treated ore was more easily crushed than the untreated. He reported that observation of the treated and untreated ore through a microscope revealed cracks following the grain boundaries in treated ore, whereas no cracks were present in untreated ore. However, few if any have quantified the improvement in terms of total hp hours saved, reduction of wear of grinding media, or reduction of capital costs of grinding equipment involved. By means of Bond rod mill and ball mill grindabilitiesh nd by comparative wear tests, the conditions maintained during this investigation have been definitely evaluated. Heat treatment experiments have been made on a batch scale in a muffle furnace, followed by continuous scale experiments in a rotary kiln under various conditions of temperature, atmosphere, retention time, and quenching to determine the combination that would give the greatest improvement in the grindability of a taconite without affecting adversely the magnetic susceptibility of the magnetite. From these data, relative costs have been calculated for grinding both untreated and heat- treated ore on a basis of plant capacity of 120 tons per hour. Heat requirements for a rotary kiln, as well as the kiln capacity required for the treatment, have been estimated. For these tests 50 tons of ore were obtained from the Aurora mine of the Erie Mining Co., Hibbing, Minn. The ore was reported7 to have been selected from the magnetic portion of the lower chert horizons. An average chemical analysis of' this portion is shown in Table I and an approximate mineralogi-cal analysis is shown in Table 11. No attempt was made to differentiate between the various silicates because the compositions vary widely on the different horizons and depend on the degree of oxidation. Minnesotite, however, is the predominant silicate. The siderite grains were dispersed throughout the ore but were essentially associated with the rock-forming minerals. In a series of preliminary tests in which batches of —6 mesh ore were heat-treated in a muffle fur-

Jan 1, 1953

By D. R. Mash

A strong yield point with attendant enhanced mechanical properties was found in commercially pure beryllium under certain conditions of heat treatment. Beryllium specimens also responded to both quench and strain aging treatments. Based on these results, a possible means of obtaining increased normal temperature mechanical properties is suggested. COMMERCIALLY pure beryllium has been found to exhibit the yield point phenomenon and several other aging manifestations under certain conditions of heat treatment. This behavior is not surprising in view of the present accumulation of experience regarding such effects in numerous metals; but in addition to extending this experience to include beryllium, the present study is of interest because aging effects are generally associated with the presence of small amounts of solute elements. The well known lack of tensile ductility in beryllium at normal temperatures is also considered to be due to impurities in some way. In the present investigation, the view was taken that beryllium of commercial purity (greater than 98 pct) should be considered as a dilute alloy and that precipitation phenomena may well exist which could lead to enhanced mechanical properties. In connection with this possibility, published data on the variation of mechanical properties with temperature are of interest. For example, Fig. 1 illustrates the variation of ductility (percentage of elongation) and ultimate strength as a function of temperature for beryllium of various histories.* Although these curves are somewhat schematic in nature, they clearly indicate the possibility that precipitation of an unstable phase and/or aging effects occur during tests in the region 400" to 700°C. The existence of such behavior should be recognized as affecting the properties of the commercial material and perhaps can be employed advantageously. Experimental Method All testing was done at room temperature using a Baldwin universal testing machine. A microformer extensometer was used in conjunction with a micro-former-type stress-strain recorder. All tests were conducted at constant loading rate, the slowest rates being used. This corresponded to 120 lb per min in the 1200 lb full scale range and 300 lb per min in the 6000 lb full scale range. After the rate of loading was set in the elastic range of the material during the early part of the test, no further adjustments were made, allowing the test to proceed at that setting. In the plastic region of the curve above the yield region, strain rates of from 0.002 to 0.006 in. per min were regularly obtained. All experimentation was carried out on specimens machined from the same lot of beryllium, lot No. Y5036BP. Table I shows the chemical analysis as furnished by the supplier, Brush Beryllium Co., as well as the standard specifications to which commercial beryllium is produced. Both 1/4 in. thick hot pressed plate and ½ in. round hot pressed and warm extruded rods were obtained. The history of the material is reported to be as follows: 1—Beryllium metal plates, produced from a standard hot pressed QMV beryllium metal block 4x15x40 in., were cut off and finished machined to 1/4x6x12 in. flat plates. The original hot pressed block was made by hot pressing —200 mesh vacuum cast attri-tioned powder at about 1050°C under vacuum. 2—Beryllium rod was hot pressed and warm extruded. Extrusion billets were machined from the regular hot pressed blocks followed by extrusion at 425°C. The extrusion was done without jacketing, and graphite was used as a lubricant. The rods were then straightened at 720 °C, after which they were annealed at 800°C for 15 min. Both flat tensile specimens and round tensile specimens were tested. The former were machined from the plate stock into standard specimens according to specifications shown in ASTM E8-52T. The nominal cross-section was 0.25x0.500 in. and the gage length was 2 in. The round specimens were

Jan 1, 1956

By L. M. Pidgeon, K. T. Aust

There has been considerable interest in the possible use of titanium in magnesium alloys.' Zirconium has shown some promise in this connection2 and its general similarity with titanium suggests that the latter might act in a similar manner. A literature survey revealed that quantitative data on the Mg-Ti system was unavailable. Several patents3 have claimed that titanium additions from 0.2 to 4 pct to magnesium alloys were possible, but no mention was made as to the form in which the titanium existed in the alloy. Kro114 succeeded in introducing only traces of titanium into magnesium by bubbling TiCl4 through the metal under argon or by reacting it with sodium titanium fluoride. The application of theoretical data given by Carapella5 based on Hume-Rothery's principles, involving atomic size factor, crystal structure, valency and the electro-chemical factor, suggests that a Mg-Ti alloy is a favorable case, and the system appeared to warrant experimental examination. Experimental Procedure and Results THERMAL ANALYSIS If titanium is appreciably soluble in magnesium, a change in the melting point of the magnesium might be detectable using standard cooling curve methods. Magnesium was melted in graphite crucibles under an argon atmosphere, the assembly being enclosed in a silica tube. Graphite thermocouple protection tubes served also to stir the melts. The apparatus was very similar to Fig 1, with the addition of a refractory and baffle system to prevent undue heat losses from the top of the crucible. Chromel-alumel thermocouples were calibrated using Al of 99.97 pct purity. Dominion Magnesium Limited sup- plied redistilled high purity magnesium of the analysis given above. Titanium was added in three different forms: 1. Titanium powder —100 mesh, from the Titanium Alloy Manufacturing Co., Niagara Falls, N. Y. 2. Sheet titanium from the U.S. Bureau of Mines, produced by Mg reduction of TiCl4. 3. Magnesium —50 pct titanium master alloy from Metal Hydrides Inc., Beverly, Mass. The melting point of the high purity magnesium used was measured experimentally as 651.0°C. More than a dozen tests were conducted using titanium from the three sources referred to above, in calculated additions up to 20 pct titanium, at temperatures between the melting point and 1000°C and holding periods up to 6 hr. In no case was evidence obtained of solubility of titanium in magnesium, using inverse-rate and time-temperature curves. The melting point of the magnesium was unchanged within the accuracy of measurement, namely -+0.5°C; and no other thermal arrests were detected. Metallographic investigation of the thermal analysis billets indicated that the titanium additions were apparently mechanically entrapped in the magnesium in segregated areas. Consequently, these samples were not analyzed for titanium. The master alloy proved to be a mechanical mixture of titanium particles in a magne- sium matrix. These results indicated that the titanium solubility, if such existed, could not be obtained by the usual thermal methods. X RAY DIFFRACTION INVESTIGATION In an effort to detect solubility of titanium in magnesium, samples were investigated using both the Debye-Scherrer and the Focusing Back-Reflection methods. Filings from samples of the thermal analysis billets and from pure magnesium were annealed in argon one hour at 350°C to relieve mechanical strain. Measurements made of the interplanar spacings showed no difference between the Mg-Ti samples and pure magnesium. The interplanar spacings could be measured to within 0.0002A, and the greatest variation found was 0.0004A, in the back-reflection method. The diffraction lines for magnesium were not shifted by the titanium additions indicating that the solid solubility of titanium in magnesium is of a very low order—less than 0.5 pct. From both diffraction methods, a d or interplanar spacing of 0.817A was obtained for the redistilled high purity magnesium. This latter value is not given in the standard X ray diffraction cards for magnesium metal or vacuum distilled magnesium. Theoretical calculations for a close-packed hexagonal space lattice for magnesium indicate that the planes {2134) should give a line which was found. The relative intensity for this reflection at 0.817A is slightly less than that at 0.870k for magnesium. SOLUBILITY OF TITANIUM IN LIQUID MAGNESIUM The Mg-Mn system was examined by Grogan and Haughton6 who were

Jan 1, 1950