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By Irving Hartmann

Modern mechanized mining with high-speed machines, multiple-entry systems, multiple blasting, high-velocity air currents, and rapid haulage has brought many economic benefits and has on the whole enhanced safety in the coal-mining industry. It has, however, also introduced some added hazards, the control of which requires concerted effort and ingenuity. Mechanized mining has greatly increased the production and dissemination of fine coal seam or in mine entries. Use of high-speed machines has increased the probability of formation of incendive sparks, which are produced by frictional contact between moving metals and certain mineral substances in the coal seam or in the adjoining rock strata. In gassy seams rapid extraction of coal has increased the rate of gas evolution. These facts have made more urgent the need of preventing the ignition of coal dust and the development of widespread mine explosions. The ignition hazard can be controlled best by eliminating all potential igniting sources and by careful attention to ventilation designed to prevent accumulation of gas capable of triggering a coal-dust explosion. Frictional spark ignition by mining machines and suggested safeguards are discussed in a recent publication. Extensive research and long experience have shown conclusively that the propagation of coal-dust flames can be arrested and the development of widespread explosions prevented by properly applied, generalized rock dusting.

Jan 1, 1956

By Donald M. Hausen

Diamond-bit performance and cost data accumulated by the Bureau of Mines in core-drilling schists reveal significant trends of economic interest. Low-quality, small-size drill bort were the most economical. The percentage of core recovery, type and size of bit, and bit matrix are also correlated with bit performance and costs. Detailed analyses of the factors affecting diamond-bit performances and costs are assessed in the tables, graphs, and discussion.

Jan 1, 1956

By R. G. Travis

1. Reserve estimates have been made for eight coal beds in Monongalia County, W. Va., but only the Pittsburgh, Sewickley, and Upper Freeport beds are important at this time. The Pittsburgh, Sewickley, Waynesburg, and Upper Freeport beds contain the largest recoverable reserves. 2. Known measured and indicated reserves in all beds, based on a minimum thickness of 14 inches and 1,800 short tons per acre-foot of coal in place, are estimated at 3,526 million tons as of January 1, 1954. Of this total, 3,294 mil-lion tons is in beds 28 inches and more thick. Areas in each bed except the Pittsburgh were omitted from the estimate because available data relative to the bed characteristics are too meager for making an estimate that conforms with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove reserves in these areas, such reserves should be added to the total estimated reserves.

Jan 1, 1956

By L. D. Jaffe

From the limited experimental data in the literature, preliminary values were derived for the thermal diffusivity of titanium alloys and for the quenching severity of various mediums used in heat treating them. The thermal diffusivity, under quenching conditions, was found to be approximately 0.006 sq in. per sec. The quenching severity H for brine is approximately 8, for water 4, for oil 0.9, for air 0.08, and for argon 0.02 in. -' The quenching severity of the Jominy-Boegehold end quench water jet against titanium alloys appeared effectively infinite. Using these results, graphs were prepared showing ideal round sizes and Jominy positions having cooled conditions equivalent to those at the center and surface of titanium alloy rounds, plates, and sheets quenched in various media. THE importance of proper quenching of steel parts has long been recognized, and much quantitative work has been done on the subject. Recently, it has become evident that for titanium alloys, too, the rate of cooling from high temperature is important in obtaining high strength and hardness. Maximum hardness and strength may not be attained in the as-quenched condition but rather after a subsequent tempering or aging treatment. Nevertheless, if cooling from temperatures near the ß transus is too slow, for the hardenability of the alloy used, a soft a-ß structure will be produced which will not harden on subsequent aging.'-" The quenching of parts of practical interest can usually be approximated by simple shapes, such as cylinders (rounds) and plates (or sheets) of various thickness and combinations of these. A standard that has been used extensively for comparison purposes is the center of an ideal round: a cylinder quenched in a medium that instantly cools its surface to room temperature." For steel, considerable practical use has been made of the Jominy-Boegehold end quench hardenability specimen,".' and its value for titanium alloys is becoming evident. It therefore appeared worthwhile to attempt comparison of cooling conditions in titanium alloy rounds and plates of various sizes quenched in various media with cooling conditions in ideal round and Jominy quenches. These comparisons are based upon measurements reported in the literature. Quenching Severity of Jominy Water Jet and of Brine As one starting point, there were available the data of Phillips and Tobin8 for positions on a Jominy specimen having the same hardness as the centers of round bars of various size quenched in 5 pct NaOH brine, shown in Table I. The Jominy speci- men is a round bar, normally 1 in. diam and 4 in. long, quenched by a water jet at one end and air cooled on the other surfaces.' After quenching, hardness is measured vs distance from the quenched end on longitudinal flats ground 0.015 to 0.10 in. deep. The data of Table I were based on a subsized specimen of 3/4 in. diam. Since the positions tested are close to the jet quenched end, cooling there may be taken as due solely to the jet, and air cooling can be neglected. These positions are then equivalent to various locations near one surface of an 8 in. plate jet quenched on both sides. Assuming that the thermal diffusivity is constant and that Newton's law of cooling holds, temperature vs time curves at corresponding positions in Jominy specimen and round bar then may be calculated for various assumed quenching severities of the water jet and of the brine. Cooling curves are generally taken to be metallurgically equivalent when they show the same time to reach a temperature halfway between the initial (heat treating) temperature and the final (quenching medium) temperature.5 On this basis, using Russell's tables,9 upplemented by heat flow tables derived in similar fashion by the author for positions near the surface of severely quenched plates, it was found that the experimentally observed equivalence, Table I, was best matched if the quenching severity H of the Jominy water jet was taken as infinite (H = co). This means that the jet quenched surface should be considered as instantly cooled to the temperature of the water

Jan 1, 1956

By R. L. Thorne

The Snettisham Peninsula, 30 miles southeast of Juneau, Alaska, was studied by the Bureau of Hines to obtain basic information about the size, grade, and metallurgical characteristics of a large basic intrusive containing titaniferous magnetite. The investigation, which was part of a continuing program to determine the potential reserves of iron and titanium ores in Alaska, included transit and magnetometer surveys, followed by diamond core drilling and metallurgical testing. The magnetic attraction of a part of the Snettisharn Peninsula is noted on early navigational charts prepared by the Coast and Geodetic Survey. Reconnaissance examinations by the Geological Survey and a preliminary dip needle survey by the Territorial Department of Mines indicated the general nature of the basic intrusive, but little was known as to the grade and extent of the magnetite mineralization. The detailed survey by the Bureau of Mines proved an area of approximately 390 acres in which generally high magnetic anomalies with exceptionally high localized anomalies occur. Subsequent drilling across B representative section of the deposit yielded core samples, which assayed from 11 percent to over 45 percent total iron. A large sample of core composited to represent the drilled portion of the de-posit assayed 18.9 percent Fe, 2.6 percent Ti02, and 0.29 percent S, 0.32 percent P, and 0.05 percent v.

Jan 1, 1956

By J. C. Barrett

Bureau of Mines research on the arc welding characteristics of titanium was initiated in 1948. Little was known about the art except that the easily contaminated metal required more protection from the atmosphere during welding than most other metals. Chambers were designed and built within which titanium could be welded with adequate inert gas protection. Welds were made and their properties studied, and prototype items were made successfully. This report, presenting a resume of the titanium arc-welding experiments undertaken by the Bureau of Mines, demonstrates that the process is successful if conducted under proper conditions and describes the welding of prototypes. INTRODUCTION The Bureau of Mines' first report on methods of joining titanium covered the subject of spot welding,4/ outlining the conditions necessary for producing spot welds in ductile titanium consolidated by powder metallurgy methods and describing the characteristics of such welds. This report embraces the field of fusion weld-ing of titanium and traces the development of suitable methods and equipment for producing such welds.

Jan 1, 1956

By Lloyd Williams

1. The investigation shows that the Coal Creek has been the most productive, bed in Campbell County and contains the largest recoverable reserves of coal. The Pewee, Red Ash, and Jullico have been relatively productive beds and contain appreciable recoverable reserves of coal. The Blue Gem also has been productive in the past, but available information indicates that most of the remaining coal is Less than 28 inches thick. The Big Mary has relatively large reserves over 28 inches thick, but the coal is high in ash and sulfur. Thick partings in the Windrock bed have discouraged mining in that bed. The Poplar Creek and Rex beds generally are below drainage, and large areas have been excluded from the reserve estimate, Reserves in the Walnut Mountain bed will be difficult to mine due to the irregu¬lar thickness and lack of continuity of the bed. Estimated coal reserves are- small in the remaining five beds. 2. Known measured and indicated reserves of coal, based on a minimum bed thickness of 14 inches and on 1,800 short tons per acre-Foot of coal in place, are estimated to be 398 million tons as of January 1, 1953, o? this total, 267 million tons is in beds 28 inches and more thick. Areas in each bed were omitted from the estimate because available data relative to the bed characteristics are too meager to make an estimate that conforms with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove reserves in these areas, these should be added to the total estimated reserves.

Jan 1, 1956

By Oliver Bowles

From remote antiquity stone has been employed for structural, ornamental, and memorial purposes. It was, and still is, so used because of its availability in innumerable localities and its architectural adaptability, dignity, substantiality, and durability. The principal varieties of stone used are granite, marble, limestone, sandstone, and slate. This report deals with granite. OCCURRENCE AND CHARACTER OF GRANITE Granites usually have been classed as igneous rocks derived from molten masses or magmas, but there is wide evidence that the origin of some granites may be attributed to regional metamorphism of preexisting rocks, rearrangement and recrystallization taking place without a liquid or molten stage. In any event granitization is a slow, deep-seated process.

Jan 1, 1956

By W. F. Stowasser

downdraft traveling grate process to agglomerate pelletized iron ore concentrates has been successfully demonstrated in a pilot plant at Carrollville, Wis. Work there followed several years of development in the Allis-Chalmers Mfg. Co. laboratories, and the pilot plant phase was carried out in cooperation with Arthur G. McKee & Co., consultants and engineers to the iron and steel industry. End result of the process is conversion of iron ore concentrates into a form which can easily be transported and smelted in the blast furnace. Process Description The first of two process steps incorporates the art of balling and prepares the concentrates for burning. The second step consists of burning the green balls on the grate machine to the hardness required for shipping and handling purposes and for reduction in blast furnaces, see Fig. 1. Facilities are provided at the pilot plant to receive carload quantities of concentrate. The concentrates are loaded into a 50-ton bin direct from railroad cars. Because of the variable moisture content of the concentrates after shipment in an open railroad car it is necessary to repulp and refilter the concentrates to maintain a uniform and proper moisture content for the balling operation. Concentrates are conveyed to slurry tanks, and the slurry, at 50 to 60 pct solids, is pumped to a 4x4-ft drum filter. The filter provides feed of uniform moisture to the plant. Magnetite concentrates are normally filtered to produce a cake containing about 10 pct moisture, a necessary requirement for the following balling operation. The filtered concentrate is conveyed to a rotary bin table feeder which acts as a surge bin for the filter cake and delivers a steady flow of concentrates to the balling drum. It is often desirable to make additions to the concentrates as they are fed to the balling drum. These additives, such as bentonite, increase the strength of the finished green pellet and improve ballability of the concentrate. A vibrating feeder supplies additive to the feed belt, and the additive is mixed with the concentrate in the balling drum. The balling drum, shown in Fig. 3, is 8x3-ft diam. An oscillating cutting bar maintains the lining in the drum by trimming off the buildup of excess concentrate as it forms. The drum is operated in closed circuit with a lx4-ft rod-deck vibrating screen. Undersize pellets or seed pellets from the screen are returned to the balling drum until they grow to the desired size. Size of pellets is controlled by the opening in the screen deck. The formation of pellets in the balling drum is affected by many variables. Some of these are: the size distribution of the feed, the particle shape of the concentrate, the feed rate to the drum, the moisture in the concentrate, the speed of rotation of the drum, the slope of the drum, and the type of trimming obtained with the cutting bar. In this process, attempts are made to control the pellet size within the limits of % to 5/8 in. diam. The screened oversize pellets are conveyed under a coal feeder where sufficient powdered coal is added to the belt to produce desired results in the burning process. The top size of the coal successfully used has been 20 mesh, and anthracite was used in the test program. Fig. 4 illustrates the vibrating screen and the coal feeder. The pellets and free coal are conveyed together to the 5x3-ft diam- reroll drum that rolls the coal onto the surface of the pellets. This drum is also equipped with a cutting bar. The prepared pellets, containing bentonite, water, and surface coal, are elevated to the traveling grate, which consists of a continuous strand of 37 pallets. Each pallet, with a grate bar area 2 ft wide by 1 1/2 ft long, has 14-in. high side plates, Fig. 5. Feeding and distribution of the green balls to the grate is handled by a short conveyor which oscillates back and forth across the 2-ft width of the grate. An adjustable vertical plate located several inches in front of the head pulley of the oscillating conveyor controls the height of the bed and levels the moving bed of pellets. This method of feeding prevents segregation of various size pellets as well as fines and produces a uniform, permeable bed. The pallet train moves under the furnace and across four windboxes, located beneath the pallet frames, see Fig. 2. As the green pellets are deposited on the grate, partial drying of the pellets begins over a 2-ft long updraft windbox. The low temperature air reduces the moisture in the pellets in the lower level of the bed and this operation is essential to prevent sagging of the bed during later stages of the Process. The air used for this drying is recuperated from cooling the pellets on the grate, and supplemental heat, required for starting the Process, is obtained from an auxiliary burner. The pellets are then moved by the grate into the furnace and over an 8-ft windbox, designated as the downdraft waste windbox. Products of combustion are exhausted from this windbox to atmosphere. The furnace, shown in Fig. 6, is constructed with three chambers to provide downdraft drying, preheating, and ignition, respectively, to the pellet bed as it passes through. Overall length of the furnace is 5.57 ft; however, the exterior wall ends may be moved to reduce the length and also adjusted to Obtain the bed height desired, The drying, preheating, and ignition sections of the furnace are supplied with medium temperature

Jan 1, 1956

By A. J. Barry

To determine the torque-load relationship for SIB-inch (nominal)-diameter roof bolts, the Bureau of Mines tested 5 makes of expansion shells and 2 types of bolts (regular and high-strength) in 2 sandstone and 2 shale mine roofs. Unused flat-steel bearing plates in as-received condition were used in these tests. The relationship between torque and load was found to be approximately 50 pounds of load per foot-pound of torque for both the regular and high-strength bolts. This relationship is valid up to 130 foot-pounds for the regular bolts and up to 175 foot-pounds for the high-strength bolts. A torque of 130 foot-pounds on a regular bolt will produce a load of 6,150 ± 1,910 pounds 90 percent of the time, and a torque of 175 foot-pounds on a high-strength bolt will produce 8,050 ± 2,750 pounds 90 percent of the time. Above these values, the torque-load relationship tends to be erratic due to binding between the bolt and plug threads. Binding causes excessive torque to be expended in producing torsion in the bolt rather than tension. This torsion adversely affects the yield load of the bolt. Therefore, the installed torques should not exceed the 130-and l75-foot-pound values. A statistical analysis of the data showed that the torque-load relationship was not significantly affected by the type of bolt or expansion shell unit but might have been affected by the type of rock.

Jan 1, 1956

By A. O. Dufresne

WITHOUT transportation, mining would be quite impossible. Any person familiar with the operation of a mine knows full well that from the minute ore is blasted, it is kept moving until it reaches the treatment plant. In the mill, by means of conveyors and elevators, the ore is brought from receiving bins to one machine after another until finally its valuable mineral is separated from the gangue. The finished product must then be shipped -either by boat, rail, or motor trucks to industrial centres, where it undergoes further treatment and transformation into finished commercial goods. Everybody appreciates that the winning of an or-e includes, amongst various operations, the moving of large quantities of material of generally low value. Transportation, therefore, must be considered One of the most important factors in the economics of mining. My assignment, this afternoon, is not to treat of that phase of transportation as it directly affects mining operations, but rather to consider some of the aspects of overland transportation and its influence in bringing about the development of mining camps in Canada. I shall take the liberty of rapidly surveying conditions facing prospectors, mine developers and operators from the time a region is still in a pre-pioneering stage until such time as a mine starts shipping its concentrates.

Jan 1, 1956

By Ralph V. Higgins

The present methods of appraising the long-range performance of oil reservoirs are based upon physical properties of the crude oil and the permeability of the reservoir rock. By means of these methods the performance of a reservoir may be estimated throughout its entire life. Before these methods were used, the future performance was estimated mostly by extrapolating pressure-decline curves -a method that is satisfactory for extrapolating only for a short period into the future. One factor that affects satisfactory long-range prediction of reservoir performance is the extent to which small changes in the physical properties of the oil and differences in the choices of relative permeability influence the calculated oil recovery. Selection of the physical properties of the samples to represent those of the oil and rock for the entire reservoir is difficult. This report is concerned with the error in calculated recoveries that may result from these inherent difficulties.

Jan 1, 1956

By R. R. McLellan

The Brown Derby pegmatites are in Gunnison County, Colo., about 18 miles east of Gunnison. Approximately 860 tons of lepidolite concentrates, with smaller amounts of microlite and beryl, was produced from 3 dikes of the Brown Derby group from 1943 through 1947. No mining was done from 1948 until December 1950, when production of lepidolite and beryl was resumed by the Poston Mining & Milling Co. Mining was intermittent during 1951 and 1952. The dikes were mapped and studied by the Federal Geological Survey during the field seasons of 1942 to 1944, and in May 1950 the Bureau of Mines initiated a diamond-drilling project to test the three dikes for lepidolite and beryl. After being recessed twice, the project was terminated indefinitely July 1951. Seven drill holes were completed for a total of 1,841.6 feet of drilling.

Jan 1, 1956

By Manuel Gomez

A lignite from Milam County, Tex., has been oxidized by air at temperatures from about 27° to 300° C. for varying lengths of time. The oxidized coal was carbonized at 500° C. in a laboratory assay unit, and the products of carbonization were measured and analyzed. The data presented suggest that, as lignite is progressively oxidized, tar yields are decreased and gas yields are increased in a ratio approximating 1:1. It is surmised that tar-yielding structures in the nonoxidized coal produce gas, principally, when the coal is oxidized. Char-yielding structures of the nonoxidized coal give rise to additional water of decomposition after oxidation and pyrolysis. As lignite is subjected to greater oxidation, the gaseous product evolved on pyrolysis becomes almost entirely carbon dioxide. Tar yields decrease with an increased degree of oxidation, so that the reduction in tar yield may be used as a qualitative measure of oxidation. Pilot-plant drying and carbonization, where air is used as the transport gas and where some air is included in the drying and carbonizing gases, induces some oxidation of the coal particle. The short residence time in a fluidized system with reference to the oxidation environment limits the oxidation.

Jan 1, 1956

By E. G. Erspamer

Laboratory investigations were made by the Bureau of Mines on ore containing the sulfides of both mercury and antimony to develop a method or methods for the economic recovery of mercury metal and the concurrent recovery of antimony as metal or salts,. If standard mercury-recovery techniques are applied to such ores, the antimony content interferes with the effective production of mercury metal; further-more, the antimony is lost. This report presents the results of tests on a sample of cinnabar-stibnite ore from the Red Devil mine near Sleitmute, Alaska. Red Devil ore was chosen for the investigation because it is purported to be typical of ores of the Kuskokwim River area, which, in their aggregate, constitute large potential reserves of mercury and antimony. Studies included petrographic, spectrographic, and chemical analyses, gravity-separation tests, bulk flotation of mercury and antimony sulfides, differential flotation, leaching, and furnacing of crude ore and of flotation concentrate.

Jan 1, 1956

By E. W. Stewart, G. P. Conard, J. F. Libsch

The effects of several additives upon the reduction characteristics of hydrogen-reduced ferrous formate are described. The various additives inhibit sintering of the reduced iron particles by apparently different mechanisms. The magnetic properties of the low density compacts produced from the resulting ultra-fine iron powders were improved markedly. THE permanent magnetic characteristics of ultra-fine iron powder prepared by various means have been a subject of considerable interest and experimentation in the past few years. When such particles are small enough to show single domain behavior, they possess' 1—permanent saturation magnetization, and 2—high coercive force. In the absence of domain boundaries, the only magnetization changes in a particle occur through spin rotation which is opposed by relatively large anisotropy forces. With decreasing particle size, the coercive force tends to increase to a maximum and then decrease because of the instability in magnetization associated with thermal fluctuations. Kittel' has calculated the critical diameter at which a spherical particle of iron can no longer sustain domain boundaries or walls to be approximately 1.5x10-' cm. Stoner and Wohlfarthr in England and Neel4,6 in France have shown from purely theoretical calculations that the high coercive force expected from single domain particles is dependent upon crystal anisotropy, shape anisotropy, or strain anisotropy contributions. Further work by Weil, Bertaut,' and many others has contributed much to the understanding of fine particle theory. Neel and Meikeljohn" have demonstrated that a decrease in particle size below a critical value of approximately 160A leads to a quite rapid decrease in coercive force because of the prevention of stable magnetization by thermal agitation. Lih1, working with powders prepared by the reduction of formate and oxalate salts of iron, has shown the marked influence of powder purity upon magnetic properties. Maximum coercive force was obtained in powders of approximately 65 pct metallic iron content while the maximum energy product, (BxH) occurred in powders of 85 pct metallic iron content. Careful consideration of the preceding theoretical considerations and experimental results has led to the manufacture of permanent magnets from ultra-fine ferromagnetic powders by powder metallurgy techniques. Such work has been done by Dean and Davis," the Ugine Co. of France, and Kopelman." The aforementioned work of Kopelman and the Ugine Co. was concerned somewhat with the effect of various additives upon the properties of hydrogen-reduced ferrous formate. Virtually no work, however, has been published on the effects of additives on the reduction rates of metal formates, although unpublished work by Ananthanarayanan16 howed promise of improved energy product in ultra-fine iron compacts prepared by the hydrogen reduction of a coprecipitated mixture of magnesium and ferrous formate. After consideration of the preceding information, it was hoped that a better balance between the metallic iron content and particle size of the reduced iron powder could be accomplished by a prevention of the attendant sintering of the partially reduced iron powder during the reduction reaction. It appeared possible that magnesium oxide might interpose a mechanical barrier between adjacent iron particles and prevent their sintering together, while metallic cadmium and metallic tin would interpose a liquid barrier which might accomplish the same purpose. The degree to which these materials were effective in accomplishing the foregoing objective and the experimental details associated with the work are reported in the following sections of this paper. Experimental Procedure Preparation of Formate and Oxide Mixtures: To obtain ferrous formate of reproducible reduction characteristics, a slight modification' was made in the technique of Fraioli and Rhoda." A supersaturated solution of ferrous formate was mixed with an equal volume of 95 pct ethyl alcohol and the formate crystals precipitated by stirring and screened to —325 mesh. These crystals were in the shape of elongated hexagons, approximately 4x10 micron in dimension. Various preparations of such ferrous formate, designated as lot 111, were reduced for 2 hr, yielding ultra-fine iron particles of exceedingly reproducible size, metallic iron content, and magnetic properties. The magnesium and cadmium formates were prepared by the reaction of dilute formic acid with their respective carbonates, while the tin formate was prepared by the reaction of dilute formic acid with stannous hydroxide. To evaluate the effect of metallic formate additives in intimate mixture with the ferrous formate, varying amounts of magnesium, cadmium, and tin formates were coprecipitated with the latter. The designations of these materials and their chemical compositions are given in Table I. Due to the differing solubilities of the various formates in aqueous media,

Jan 1, 1956

By R. L. Smith, I. G. Greenfield

The binary system Ga-Sb has been investigated by thermal, X-ray, and metallo-graphic methods. 'The intermetallic compound GaSb melts at 705.9OC and forms a eutectic with antimony at 11.8 atomic pct Ga. This eutectic melts at 589.8OC. A eutectic appears to be formed at 29.8°C but is too close to the composition of pure gallium to be detected. IN the course of an investigation of the semiconducting properties of the intermetallic compound, GaSb, the phase equilibrium between gallium and antimony has been investigated. Recently, the phase diagram of similar systems, such as In-Sb,' In-AS,' and Bi-As3 have been determined. These diagrams have the same general appearance in that an intermetallic compound is formed at 50 atomic pct and a eutectic is formed on both sides of the intermetallic compound. Jenny,& who has been investigating the semiconducting properties of intermetallic compounds, has concluded from thermal data of several alloys that the phase diagram of the Ga-Sb system resembles those mentioned previously. This paper represents a more detailed study of the Ga-Sb equilibrium. Experimental Procedure The gallium that was used to prepare the alloys was obtained from A. D. Mackay Inc. and the Aluminum Co. of America; the latter reported the purity as 99.95 pct. The antimony was obtained from Bradley Mining Corp. who specified a purity of 99.997 pct. Since the intermetallic compound of GaSb was prepared primarily to be used for further studies of the semiconducting properties, additional purification by a standard zone-melting technique under an atmosphere of hydrogen was performed. Hall-effect measurements on this material indicated an impurity content of less than 3 ppm.5 The antimony also was purified by zone melting and used in conjunction with the compound GaSb to make the necessary alloys for the determinations of the antimony-rich side of the phase diagram. The antimony-rich alloys were chill cast in Vycor tubes which were evacuated to a pressure of less than one micron. Since these alloys expand on freezing, precautions were taken to prevent oxidation of the ingot in the event the tube fractured. To insure homogeneity, the brittle alloys were ground and then placed in the furnace for the thermal-arrest determinations. Since the cost of gallium is high, the experimental procedure was complicated somewhat because of the necessarily limited sizes of the melts. In order to economize, the gallium-rich side of the diagram was determined by using a 35 g ingot of pure gallium initially and adding increasing amounts of antimony in order to obtain additional alloys. The furnace used in the determination of the cooling curves is illustrated in Fig. 1. A 2¼ in. quartz tube, sealed at one end, was fitted with a brass flange which was attached with DeKhotinsky cement. The brass collar was water cooled to prevent the cement from softening. An "0" ring was used to provide a seal between the brass collar and the furnace cover. Nichrome ribbon was wound around a 2 ½ in. asbestos-covered copper core which was used to reduce the thermal gradient in the furnace. The insulation consisted of alternate layers of asbestos and aluminum foil surrounded by sil-o-cel refractory and

Jan 1, 1956

By W. A. Griffith

Fractional replication of factorial design, a general method for planning experimentation and for analysis of data obtained, is described as applied to a flotation investigation. This method leads to determination of optimum process conditions with minimum experimental effort. Its advantages over simple factorial design are demonstrated. A METHOD for planning experimentation and for analyzing the data secured will be demonstrated. This method, termed fractional replication of factorial design, employs a relatively small number of individual experiments to determine which of a large number of process variables are controlling, to determine which combination of levels of these variables is most likely to produce optimum results, and also to predict what results will be obtained with a particular combination of conditions not already tested. Although the general method is not new, having been developed by Finney in 1945,' the extent to which it can improve the effectiveness of applied research generally has not been recognized by metallurgists. The fractional replication procedure is particularly useful in flotation experimentation and an example from such an investigation will be used in the paper. However, it has equal value in any investigation in which similar experimental difficulties are encountered. In developing a flotation process for a particular mineral separation, the investigator is inevitably confronted with the following difficulties: 1—There are a large number of potentially important process variables. 2—Results of individual experiments are not highly reproducible, due in part to the difficulty in precisely controlling all the variables. 3—Considerable effort is expended in conducting individual experiments. 4—There are practical limits on the number of individual experiments which can be made. In situations of just such a type, modern statistical methods of planning experimentation and analyzing data have their greatest value. Applications of one such technique, called factorial design, to problems of this type have been described by Dorenfeld and others.'-' The simple factorial design is an efficient procedure when the investigator hopes to provide a comprehensive understanding of the effects and interrelationships of a small number of variables over a limited range. In applied research, this is seldom the main objective. Rather, the investigator usually wishes to determine which of the many potentially important variables are in fact controlling, which levels of the controlling variables will provide opti- mum metallurgical results, and what these results will be at optimum conditions. Interest in detailed trends is limited to the controlling variables and to levels in the region of optimum conditions. Simple factorial design has serious deficiencies for such objectives and is not the most efficient method of experimental design. Deficiencies of Factorial Design In a simple factorial design, an experiment must be made at every possible combination of each level of every variable, once these have been chosen and the levels of each to be included have been decided upon. As the number of variables or levels of each increases, the experimental program quickly reaches prohibitive size. For example, an investigation of only four variables, each at four levels, requires 256 individual experiments. Often upon completion of such an extensive program, it is found that one or more of the variables has metallurgically unimportant effects or that a poor estimate has been made as to the appropriate range of levels to be investigated. The result is that only a small proportion of the data obtained falls in the range of real metallurgical interest. Indeed, it frequently can be anticipated that certain combinations of levels of variables will not produce results of interest, but they still must be included so that the essential balance, or orthogonality, of the design will be retained. It may be true that factorial design will provide the greatest amount of information from a given number of experiments, but it does not necessarily follow that it will lead to the desired information with a minimum number of experiments. Much of the information provided may be of little value. Advantages of Fractional Replication The disadvantages of simple factorial design are overcome to a great extent by a modification known as fractional replication. This is a technique for sampling systematically the potential data of a full factorial experiment, that is, the data which would have been obtained if the complete factorially designed program had been completed. Only a fraction of the total array of experiments is made, but the experiments are chosen in such a way that the important advantages of factorial design and the accompanying analysis of variance are retained. The data obtained from the first group of experiments are used to determine which of several variables are controlling and which levels of these variables are most likely to produce the desired result. Unimportant variables and levels of variables then may be

Jan 1, 1956

By W. F. Stowasser

Robert E. Hagen (Oliver Iron Mining Div., U. S. Steel Corp.)—Mr. Stowasser and his associates are to be congratulated on their achievements in developing the design of a pilot agglomerating plant, based on information obtained from experiments made in a laboratory sinter pot, and subsequently constructing and successfully operating this plant. In his Transactions article, May 1955 (vol. 201) Mr. Stowasser stated that the output of his heat treating strand was about 2 Lt per sq ft of grate area per day and that the fuel consumption was 0.7 to 0.8 million Btu per Lt of product. If it is assumed that the burning zone extends from the back of the ignition furnace to the beginning of the recuperation windbox, only about 1/3 of the grate area over the windboxes is utilized for burning pellets, and the actual rate at which partially dried pellets are burned is about 6 Lt per sq ft of grate area per day. It may be interesting to compare the above operating data with that obtained at the Extaca plant, where taconite concentrate is treated on a conventional sin- tering machine using limestone or hydrated lime additives with no recuperation of heat. The entire windbox area is used for burning, and a production rate of 2.5 Lt per sq ft of windbox area per day has been attained at a fuel consumption of 1.8 to 2.0 million Btu per Lt of product, the latter being considerably in excess of that reported by Mr. Stowasser, partly because a circulating load of returns amounting to 28 to 30 pct of the machine feed is used and because no attempt is made to recuperate heat from the waste gases. With the high capital and labor costs prevailing today, it seems that future development of the downdraft grate pelletizing process should be directed toward taking advantage of the high burning rate of predried pellets and increasing capacity, perhaps at the expense of fuel economy, by decreasing the proportion of grate area utilized by ancillary functions. For example, eliminating the cooling zone and using this area for burning would increase the proportion of grate area available for burning from 33 to 50 pct of the total windbox area, and a proportionate increase in capacity would result.

Jan 1, 1956

By R. B. Rosene, G. L. Foster, A. R. Hendrickson

he properties of some of the common fracturing oils, such as sand-falling rate, fluid loss and viscasity, are a function of the three major constituents of the oil. These are: asphaltic material, parafin waxes and a base oil. The base oil can be either high or low viscosity. Asphaltic material increases viscosity by thickening the oil, decreasing the rate of fall of sand through the oil. at temperatures up to 200" F. When large arnorrnts of parafin wax are present, much of the wax i.s not dissolved, but is present in the form of rnicroscopic crystals. 7'his, of course is limited to temperatures below the melting points of waxe.s. As a result, parafin waxes clo not function primarily as thickener.7, but rother as bullting materials. The functiori of wax, without asphaltic material, in a low viscosity base oil is uniquely unlike that of wax with asphalt coexistent in the oil. The resulting difierence in wax crystal size governs the sand-falling rate to a large extent. An ideal type of fracturing oil is one containing neither asphalt nor waxes. In such cases, the viscosity and resulting low sand-falling rate are apparently due to soluble resin- ous hydrocarbons, which are compatible with formation oils. INTRODUCTION Since the introduction of hydraulic fracturing as a method of stimulating production from oil and gas wells, a variety of fluids have been employed to open the fractures and carry the propping agent. Such fluids include gels, emulsions, and oils. In the latter category, the use of refined oils has increased tremendously, and it is probably safe to assume that such oils represent more than one-half of the total fluid used in fracturing. The general acceptance of refined oils for fracturing can be accounted for on the basis of their relatively low cost and general applicability. To minimize transportation costs, such refined oils are generally obtained within the local areas of operation. As a result there are several kinds of oil used in different areas, with a wide variation in the basic composition. These types may vary from a fair grade of lubricating stock to a highly viscous cut-back asphalt. or road oil. Originally, little attention was paid to the composition of the oils used for fracturing, and any oil which would carry sand was considered satisfactory. Recently, however, service companies and well operators have become more concerned with the type of oils used for fracturing. With this in mind, the present work was undertaken to evaluate and compare many widely used fracturing oils to determine which constituents were most desirable for fracturing purposes. Some of the important properties of fracturing fluids are sand-falling rate, viscosity, and fluid loss. Other properties, that are actually of no less importance, include flash point, pour point, emulsifying tendencies with formation brines, and compatability with the formation oils. This discussion has been limited, however, to the first mentioned properties in order to give some idea of the general composition of the refined oils, how they function, and why. PROPERTIES OF FRACTURING OILS The properties of fracturing oils are a function of the three major constituents of the oil. These may be designated as: (1) asphaltic material, (2) paraffin waxes and (3) a base oil, which may be of either high or low viscosity. The asphaltic material clas-

Jan 1, 1956