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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 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

By E. H. Mulligan

THE ERRINGTON B-I mine is located on the Errington orebody of Steep Rock Iron Mines, Limited, at Steep Rock Lake, Ontario. In 1946, this orebody entered the shipping lists of the Lake Superior iron ranges as an open-pit operation. During the period 1946 through 1953, the mine produced a total of 9,000,000 tons of iron ?ore. In 1950, as the mine approached the economic limits for open-pit operations, ground was broken for an underground development to exploit the deposit at depth. The mine is designed for an ultimate production of 1,500,000 tons per year by the block-caving system of mining. The initial shaft is 1,200 feet deep and will produce or-e from the 700 and the 900 levels. The 1,100 level will be used as a drainage level and as a haulageway for waste rock, which is hoisted to surface by skip. Ore from the two production levels moves by a system of ?ore passes to a crushing plant located below the 900 horizon and is hoisted from this point to surface by conveyor belt. At the present time, all material handling on the levels is by tramming, but as tram distances increase conveyor haulage will probably be installed. The initial stage of the Errington B-1 development is expected to produce 6,000,000 tons of ore over a period of four years. The second stage will require deepening of the shaft and development of lowe1? production levels. The conveyor hoisting plant will be extended to serve these new levels. We visualize the mining of this orebcdy down to 2,500 feet by these methods.

Jan 1, 1956

By H. A. Watson

This circular, which is a revision and combination of two previous publications,3 4/ presents information on the different types of equipment that may be used to analyze mine atmospheres, with particular reference to the application and limitations of each type. Such information is frequently requested by mining companies, State mining departments, and other agencies concerned with safety in mining who wish advice regarding methods of analysis of mine atmospheres and the equipment necessary for establishing laboratories for that purpose. Since the Haldane-type apparatus is particularly applicable to the accurate determination of carbon dioxide, oxygen, and combustible gases such as methane in mine atmospheres, that apparatus and the method of operation are described in detail. The circular presents results of a critical study of the accuracy attainable with the Haldane-type apparatus in the determination of methane in concentrations of the order of 0.25 percent, by volume. Analytical procedures involved in the other methods discussed are presented in publications referenced in this circular. Information is given also on the various accessory equipment needed in a laboratory for the analysis of mine atmospheres, and suggestions on laboratory design are included. INTRODUCTION 'The analysis of mine atmospheres plays an important part in promoting safety and maintaining safe conditions in mining operations, particularly in coal mining, where the flammable gas methane presents a continuous hazard in Nome mines and may be encountered unexpectedly in others.5/ Methane has been encountered also, often unexpectedly and with disastrous results, in noncoal mines and in tunnels under

Jan 1, 1956

By G. K. Manning, W. E. Few

WORK on the effect of vacuum heat treatment of 0.040 in. diam sintered and wrought molybdenum wires has been sponsored by the Office of Naval Research at Battelle for the past several years. An electrical resistance furnace' capable of maintaining a vacuum of less than 0.1 micron of mercury at temperatures as high as 4000 °F was used for heat treating the wires. Early in the work, it was found that the introduction of a few microns pressure of oxygen into the furnace resulted in a rapid increase in the oxygen content of the wire specimens and the appearance of a discrete oxide phase. Subsequent elimination of the oxygen atmosphere caused the disappearance of the oxide phase. This was used to determine the solid solubility of oxygen in molybdenum over the temperature range of 2000" to 3000°F.2 It was observed that, with the disappearance of the oxide phase, the wires regained some ductility. Single-phased wires possessed from 5 to as much as 40 pct elongation in 2 in. Later, attention became centered on determining the cause of this wide range in ductility. Wires containing less than 0.002 pct C, less than 0.0007 pct 0, less than 0.0005 pct N, and less than 0.00003 pct H exhibited the erratic ductility noted above. These percentages represent approximately the limit of accuracy of presently available methods of analysis and thus it became apparent that chemical analysis would be of little help in the study. A number of possible explanations for the wide range in ductility were suggested during the course of the work. It was first suspected that variations in the grain size of the recrystallized wire specimens might be responsible. Wire from several lots of material was available. One of these lots tended to develop very large grains when recrystallized, the others all developed an ASTM grain size of 3 to 4 when heated above 2700°F. No correlation between grain size and ductility could be found. It was thought that back diffusion of oil from the diffusion pump might cause contamination of the wire, principally with carbon, but when wires were treated without cooling the cold trap in the pumping system,

Jan 1, 1956

By C. L. Brown

Coal has been transported by belt conveyors in mines for many years; however, only since the beginning of the general mechanization period have complete transportation system of this type been employed. Aside from my complete belt-conveyor transportation systems, belt conveyors are frequently used in conjunction with other transportation. Many early installations, for the most part, were made without standards as a guide. As a result, some States have outlined certain requirements based more or less on experience following mine fires. Correlation of these regulations should result in more uniformity in connection with standardization of regulations. The National Electrical manufacturers Association has published standards for mining-belt-conveyor installations2/ that should be helpful to the coal-mining industry generally. Bureau of Mines Schedule 2F3/ requires certain controls for permissible-belt- conveyor drives, and similar requirements are listed in Bureau of Mines bulletin 514.4/ Committees of the American Mining Congress have prepared much valuable information concerning operation of belt conveyors, and a subcommittee on fire-resistant belting has been active. 5/

Jan 1, 1956

By F. W. Luerssen, J. F. Elliott

F LUSHING the early slag from a stationary open Fhearth having a high percentage of hot metal in its charge is necessary in order to remove silica from the system. The flush slag is strongly oxidizing and is somewhat acidic. It has, however, considerable capacity to extract phosphorus from the bath and it also removes considerable manganese. It seems probable that factors which control the distribution of phosphorus and manganese between slag and metal in the refining period also should be dominant in the flush and postflush periods. Several studies, as summarized elsewhere,1,2 support the viewpoint that conditions closely approaching equilibrium for these elements are rather readily established during the refining period. Over the years these studies have repeatedly demonstrated that 1—high slag v01ume, 2—low bath and slag temperature, 3—basic slag, and 4—strongly oxidizing slag favor rapid elimination of phosphorus from the bath to the slag. They also show that the following conditions favor retention of manganese in the bath: 1—low slag volume, 2—high bath and slag temperature, 3— basic slag, and 4—minimum oxidizing power of slag. When it is considered that the flush slag often carries as high as 75 pct of the manganese charged and only 25 to 60 pct of the phosphorus charged, it is evident that in removing silica much manganese is sacrificed but phosphorus removal is far from conplete. Because of overriding circumstances, this is accepted in most operations and actually it is considered to be inevitable. This may account for the fact that little attention has been paid to conditions affecting the elimination of phosphorus and manganese in the flush slag. A recent study of the behavior of various charge oxides has developed considerable information on the flush and postflush periods. Because the data are felt to be of general interest, they have been brought together and Presented in this paper. The object is to show the various factors in the flush and postflush periods which influence elimination of phosphorus and manganese. Physical Conditions During and After Flushing Physical conditions existing during the flush vary from plant to plant, from shop to shop, from furnace to furnace, and even from heat to heat. They are strongly influenced by the physical and chemical character of the charge oxide which is ordinarily necessary to provide sufficient oxidizing power early in the heat. Invariably the period is characterized by a vigorous reaction between the principal re-actants: the hot metal being added and the charge oxide. During the flush, it is probable that the slag acts to some extent as an oxidizer; but, because of the critical influence of the behavior of the charge oxid'e on flushing action, it seems apparent that the oxide itself is the dominant oxidizer. Fig. 1 shows the course of two heats which were selected as being typical of the group studied. Heat A was charged with 55 pet hot metal, based on the total metallics charged, and heat B had 57 pct hot metal. As indicated in Table I and Fig. 1, the melt-down slag, which is not usually voluminous and which is principally FeO, expands greatly in volume and will show rather high levels of SiO2, MnO, and P2O5 very soon after the beginning of the hot metal addition. Simultaneously, large volumes of CO are liberated which cause violent mixing of slag and metal. It is of interest to note that the time required to bring carbon down to a low level is very much longer than that required for the removal of silicon, manganese, or phosphorus. At the end of flush, carbon in the bath is still approximately 2 pct. When strongly reducing hot metal is brought into contact with strongly oxidizing conditions within the furnace! it is probable that the rate of mass transfer to the slag (and atmosphere) of silicon, manganese, phosphorus, and carbon initially depends principally on the rates at which the two participating phases are brought into contact That is, it depends on the nature of the various reactions. Later in the flush period, when the scrap is virtually all dissolved and the action of the bath has settled down to a steady and somewhat gentle boil, it is likely that other factors, such as the transfer of oxygen across the slag-metal interface, become dominant. The temperature of the slag-metal system is far from uniform. Heat is being driven by the flame down through the slag. Bubbling and surging of the metal also frequently brings portions of the bath in contact with the flame. At areas of contact between the ore and liquid metal, or slag and liquid metal, the oxidizing reactions generate much heat. On the other hand, scrap is being melted which tends to absorb large quantities of heat. Because the liquid bath is high in carbon, the steel scrap is brought into solution rapidly. This can proceed at a rather low temperature; and until much of the scrap has been taken into solution, the bath temperature would not be expected to increase appreciably. Consideration of these factors leads to the conclusion that during the flush period the slag should be rather hot and the bath relatively cold. Both observation and temperature measurements bear this out. Experimental Data The extended program of charge oxide evaluation permitted study of the widely varying conditions existing during the flushing period. Slag and metal analyses and bath temperatures reported herein (Tables I and 11) were obtained toward the latter portion of the work. Four different types of charge oxide, sinter, two types of hydraulic cement-bonded soft ores, and a pyrobonded agglomerate were used in the study. Although the heats reported were from only one 205 ton furnace, they show variations in flush slag analyses all the way from 25 pct FeO, which is typical with the use of a hard natural charge ore, to 45 pct FeO which resulted when a very poorly agglomerated fine ore was used. The physical behavior of the flushes showed a correspondingly wide variation from well controlled reactions to violent surges following periods of inac-

Jan 1, 1956

By T. E. Howard

The western phosphate field, comprising parts of Idaho, Montana, Wyoming, and Utah, contains one of the world's largest known reserves of phosphate rock. Although phosphate-rock deposits of good-grade have been known since before the turn of the century and production has been recorded since 1906, real development of this important field did not begin until immediately after World War II. Since then fertilizer-manufacturing facilities using western phosphate rock have been expanded, and three electric-furnace plants for producing elemental phosphorus have been installed, resulting in a rise in mine production from 323,955 long tons2/ in 1945 to 1,653,916 long tons3/ in 1953. Interest in the field is increasing, and it is reasonable to expect that the western phosphate industry will continue to expand. Before 1945 all western production was from underground mines. In that year the first strip mine in the field was started near Montpelier, Idaho,~ and in sub-sequent years a number of other open-pit mines were opened in southeast Idaho and western Wyoming. At present the major part of the production comes from surface mines. Underground mining has continued, and new underground mines have been opened in the field, but recent exploration by operating companies has been aimed primarily at developing additional deposits suitable for low-cost surface mining. Preliminary reserve estimates by the Federal Geological Survey5/ indicate that only a very small part of the total resource may be recovered by surface methods and that the industry eventually must depend largely on underground mining. Because one function of the Bureau of Mines is promoting the conservation and development of the Nation's mineral resources, it is appropriate that research be conducted to develop low-cost maximum-recovery underground mining methods applicable to western phosphate-rock deposits.

Jan 1, 1956

By P. N. Summerfield

This report describes the first phase of a general investigation designed to ascertain whether an electronic roof-testing device can be developed that will improve the ability to detect "loose" or "drummy" roof rock over that possible by striking the roof with a sounding bar and noting the character of the air vibrations with the unaided ear or the rock vibrations with the fingers. The amplitude, frequency content, and duration of the vibrations produced by striking solid and drummy roof rock with a hammer or sounding bar have been measured. Results disclosed that there is a significant difference between the characteristics of the vibrations produced in solid and drummy roof. This difference is such that the design of an electronic device to indicate quantitatively the condition of the roof rock appears possible. INTRODUCTION The conventional method of roof testing consists of striking the roof with a bar2/ and judging its soundness from the character of the air vibrations heard with the ear and/or the rock vibrations felt with the fingers -a procedure that depends upon the experience and the sensory abilities of the observer. Impact testing of a solid roof rock usually produces a sharp ping or click, whereas impact testing of a drummy roof rock produces a dull thud or drummy sound. This method of roof testing is, at most, only a qualitative test, and many roof rocks are difficult to classify as drummy or solid.

Jan 1, 1956

By Robert E. Hershey

1. Estimates of reserves were made for three coal beds in Hamilton County the - Lantana, Sewanee, and Richland. Nine coal beds have been mined at one time or another in the county, but not enough information was available to estimate reserves in any beds other than the three given. 2. Known measured and indicated reserves for all beds, based on a minimum thickness of 14 inches and on 1,800 short tons per acre-foot of coal in place, are estimated to be 53 million tons as of January 1, 1954. Of this total 35 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 were insufficient for making an estimate conforming with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove re-serves in these areas, such reserves should be added to the total estimated reserves determined by this investigation.

Jan 1, 1956

By Milton Glicken

THE airborne geophysicist is a busy man these days. In his plane he may have the airborne magnetometer, the airborne scintillation counter, and the airborne electromagnetic surveying system. Each of these is an independent tool, but all require additional auxiliary equipment for locating the aircraft in space: recording altimeters and Shoran or aerial cameras. Now there is still another piece of equipment, the airborne magnetic gradiometer, an accessory to the magnetometer. To understand its uses, consider the function of the magnetometer itself. Aside from detecting magnetic ore, the airborne magnetometer finds greatest use in spotting intrusions of igneous material. Where there is enough contrast in magnetic susceptibility of igneous rock and adjacent formations, it outlines the intrusion. Certain minerals also influence the magnetometer directly, but with the exception of magnetite and possibly one or two others, their effect is weak and can be detected only when there is sufficient ore and the magnetometer flight passes very close to it. An igneous intrusion of infinite depth with vertical sides is represented on a magnetometer record by an anomaly, as in Fig. 1. Amplitude of the high depends on susceptibility contrast of the igneous rock. Generally speaking, the edge of the intrusion lies below the point of inflection of the curve, and this point, where the curvature changes from positive to negative on the magnetometer profile, would be near A in Fig. 1, with a counterpart, of course, on the other side. Location of the contact is one of the principal objects of the survey, but finding the precise point is not always easy, as inspection of the curve near A will show. Mineralization is often found at the contact zones, as at B. Magnetic effects, if detected, may be small, as in B', and when superimposed on the anomaly due to the instrusion they are very difficult to discern and analyze. Furthermore, if these small fluctuations are to be perceived by the magnetometer the vertical scale should be large. This increases the slopes of the anomaly and makes detection of small deviations and inflection points even more difficult. The airborne magnetic gradiometer was designed to help overcome these difficulties. What it presents is the first derivative of the magnetometer record with respect to time, that is to say, the slope at any point. Fig. 2 represents an actual magnetometer record (solid line) with the corresponding gradiometer record (dashed line) superimposed. Both records read from right to left. Vertical lines on the original magnetometer record are automatic steps designed to keep the pen from going off scale. The slope of any curve is greatest at the point of inflection or point where the curvature changes sign, and this point is a maximum (or minimum) on the gradi- ometer. The chief advantage of the gradiometer is that maxima or minima are much easier to see and to locate precisely; hence an accurate location for the point of inflection can easily be found. Note that points C and D are more sharply defined than C and D'. Similarly the small fluctuations of the original record, so important to the interpreter, are far more clearly shown at E, F, and G, than on the original record at E', F', and G'. Though not necessarily highs and lows on the gradiometer, they do show up clearly what would take a painstaking analysis to detect on the original magnetometer record. Will the gradiometer have a particular configuration which indicates an orebody? Not necessarily. The total intensity curve, or original magnetometer record, can display an orebody in various ways, depending on dimensions, orientation, latitude, and composition, as well as on direction, flight height, and instrumental sensitivity of the traverse. Where the total intensity can take on so many different shapes the gradiometer must vary too. It is generally recognized that interpretation of total intensity magnetometer records requires an expert analysis; the gradiometer can be of considerable assistance to the expert but it does not replace him. Mechanism of the gradiometer is simple. A Leeds & Northrup recorder in the aircraft records the magnetic gradient simultaneously with the total intensity, which is on another recorder. Fiducial marks are put on both records simultaneously and the speed of the paper through the recorders is kept the same on both. This makes it possible to place one record over the other for direct comparison. In the laboratory the flights are positioned on a map. Maximum and minimum points on the gradiometer, which can then be posted on the map at their proper locations, may be expected to fall along a trend crossing the direction of flight. Trends should indicate the edge of an intrusion, or some other important features, and when superimposed on the total intensity contour map help greatly to locate the points of inflection, or line of zero curvature.

Jan 1, 1956

By W. Hodge, A. F. Haskins, R. M. Evans

Refractory boron compounds are shown to resist corrosion by molten zinc. Coatings were made from ferroboron and manganese boron by several methods: welding, hard facing, and pack diffusion; and techniques of coatings are very important. Mechanical failure of the diffusion coatings can be partially eliminated by applying them to type 416 chromium steels rather than carbon steels. Welded coatings made with a tungsten arc are better than those made by other welding methods. Sintered compacts of mixtures of iron and chromium borides developed strengths of about 30,000 psi. They resisted corrosion of zinc at 600°C and oxidation at higher temperatures. MOLTEN zinc rapidly attacks common metals of construction. The rate of attack is greatly amplified at temperatures over 500°C. However, there are many applications where it is necessary, or at least advantageous, to use metal construction, such as for galvanizing pots and zinc smelter equipment. Condensers and agitator linings used in continuous zinc smelting processes are eroded and corroded by violently agitated molten zinc. Pumps, tubing, and other parts to permit transfer of molten zinc would be desirable in many zinc handling operations. The development of metallic materials which are resistant to molten zinc also might permit its use as a heat-transfer medium in modern high efficiency power plants. In reviewing previous work on zinc-resistant metals, it was evident that most of the available data refer to corrosion at temperatures just above the melting point. Tungsten and high Mo-Fe alloys containing more than 80 pct Mo resist corrosion by molten zinc.', ' Imhoff states that because chromium is not attacked by zinc, chromium plating improves galvanizing pot life." Nitrided cast iron has been used in die-casting machines' where the molten alloy is 96 pct Zn and 4 pct Al. Other metals that have been suggested as of possible value for zinc resistance are columbium, tantalum, and titanium.V he corrosion of steel by zinc has been discussed by many authors,z, "2 None of these materials resisted corrosion by molten zinc at the temperatures used in this investigation, i.e., 600" to 700°C. I. Exploratory and Resistant-Coating Tests To make a study of zinc-resistant metals, exploratory tests were conducted to sort out roughly those materials which seemed most worthy of further development. This preliminary study included both solid metals and surface coatings. Exploratory Corrosion Tests in Molten Zinc—In initiating a study of this problem, numerous samples of metals and alloys were evaluated by dynamic corrosion tests made at 440 °C. Each metal was tested in its most readily available form, which, because of shape and size, was often unsuited for standard corrosion testing. The equipment used for dynamic corrosion testing of all materials, except in a few initial experiments, is shown in Fig. 1. Samples were tied to tungsten rods with tungsten wire, immersed in the zinc, and revolved at 12 rpm about the circumference of a 4 in. diam circle. Speed of travel was about 12.5 fpm. The molten zinc was protected from oxidation by an atmosphere of carbon monoxide, or, at a later period in the program, by a 9:1 mixture of nitrogen and hydrogen. When the effect of both molten metal and atmosphere was desired, the zinc level was lowered. Special high grade zinc was used in all of the corrosion tests. Corrosion losses for materials tested are shown in Tables I and 11. Whenever the materials were available in suitable form, the losses are reported in mils per year. It was recognized that weight losses on irregularly shaped specimens did not show the corrosion rate but the important consideration—poor resistance to corrosion—could be determined readily.

Jan 1, 1956

By M. M. Fine

A preliminary mineral-dressing study of five samples of East Texas limonitic brown iron ores was conducted as part of the Bureau of Mines program to develop and extend domestic resources of iron ore. The samples were considered to be typical of ore currently being mined and beneficiated by the Lone Star Steel Co. and Sheffield Steel Co. The objective of the research was to investigate those mineral-dressing unit operations that might recover some of the fine iron lost in current industrial wastes or perhaps improve the recoveries when applied to the ores as well. Since current industrial beneficiation practice yields a washed limonite analyzing 41 to 45 percent iron, higher grade concentrates were not sought in this laboratory study. Laboratory investigation included washing and sizing, reduction roasting, and subsequent magnetic separation of the finely ground roasted materials. The results showed that laboratory recoveries of over 80 percent of the iron were possible, for the ores investigated, at concentrate grades comparable to those expected from cur-rent industrial beneficiation practice. ACKNOWLEDGMENTS Acknowledgment is made to the Lone Star Steel Co. and Sheffield Steel Co. for supplying the brown iron-ore samples on which this research was conducted.

Jan 1, 1956

By R. L. Grant

At the Eighth International Conference of the Directors of Safety in Mines Research, Sartorius and Thouzea5/ presented and discussed data obtained in explosives tests made under varying conditions of humidity. These tests showed that there was less probability of explosives failure when the humidity of the testing gallery atmosphere was high. As it is to be expected that the relative humidity of mine atmospheres where permissible explosives are used will not be identical with that of the test-gallery atmospheres, the influence of atmospheric moisture upon the incendivity of permissible explosives is of the utmost importance if decreasing humidity reduces the relative safety of an explosive. Because of this and because the question has recurred frequently in discussions of gallery testing at Bruceton, Pa., it was decided to investigate the effect of humidity and ambient temperature on the ignition of firedamp by explosives, applying the small-scale gallery methods developed at the Bureau of Mines and used earlier to study the fundamental causes of such ignitions.6 7 8/

Jan 1, 1956

By F. E. Block

The reaction between calcined dolomite and ferrosilicon has been studies with the aim of developing a continuous process for magnesium production. Small-scale tests were made in vacuum retorts similar to those used in the vacuum retort process as developed by Pidgeon (1)2/ and operated during the period of World War II in several Government-owned plants. Factors investigated with respect to the silicon efficiency were the reaction temperature, reaction time, amount of excess dolomite in the charge, and effect of adding sodium silicate to the charge to serve as a binder. Additional laboratory tests were made to study the reaction at elevated temperature but at atmospheric pressure. Silicon efficiencies exceeding 80 percent were found to result when operating in the temperature range from 1,750° to 1,800° C. for periods of 20 to 30 minutes.

Jan 1, 1956

By H. D. Kline

Manganese ores have been mined in the Batesville district since 1849. Although not continuous over the intervening years, production had totaled approximately 432,000 tons of manganese ore and ferruginous manganese ore to the end of 1953. The ores occur in deposits, essentially low in manganese content, distributed over an east-west belt 24 miles long and 4 to 8 miles wide, the core of which is about 6 miles north of Batesville, Independence County. Although the reserves of high-grade ores in the district are comparatively small, the large deposits of subgrade ores and low-grade manganiferous material comprise potential sources of supply of manganese that may have increasing future importance. The manganese occurs as primary oxide and carbonate minerals in relatively flat-lying limestone and shale formations in which they were originally deposited and as oxides in residual clays resulting from decomposition of the shale and lime-stone. Most of the deposits underlie from a few to over a hundred feet of sedimentary chert, but many occur in the residual clays on exposed slopes of chert-covered hills.

Jan 1, 1956

By J. M. Provost

1. Estimates have been made for eight coal beds in Marion County, but only the Pittsburgh is important from a production standpoint at this time. The Pittsburgh bed has the largest recoverable reserve, and the Sewickley is second in importance. 2. Known measured and indicated reserves thickness of 14 inches and on 1,800 short tons estimated at 3,141 million tons, as of January lion tons is in beds 28 inches and more thick in all beds, based on a minimum per acre-foot of coal in place, are 1, 1955. Of this total, 2,983 mil-Areas in each bed were omitted from the estimate because available data relative to the bed characteristics were 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 Floyd G. Anderson

Owing to the rapid growth of the perlite industry in recent years, the Bureau of Mines has received numerous requests for information relative to the possible harmful effects of breathing dust resulting from the processing and use of perlite. As published information on the composition of perlite is rather meager, consisting chiefly of conventional chemical analyses, samples of crude and expanded perlite from 9 deposits in 6 Western States were studied. Crude perlite ores were examined petrographically and analyzed by chemical, spectrographic, and X-ray-diffraction methods. Sized crude and expanded perlites were analyzed chemically for total free and combined silica content.

Jan 1, 1956

By Leendert de Witte, Fred J. Radd

In many areas caring failures can be directly related to electrical currents observed in the casings. It is the thesis of this paper that the observed casing currents are mainly due to electrochemical potentials of the type in evidence on spontaneous potential curves of electrical logs. The general nature of these potentials are discussed and an equivalent circuit is given for current and potential distributions around open holes. The casing forms a short circuit to these potentials and tends to average the effects of local cells. The case of casing corrosion opposite the Dakota water sands in the salt-mud area of Kansas is discussed anil used us a qualitative, illustration of the relation between SP's and casing currents. A method of quantitative derivation of casing current distribution frorn electric log SP curves, using linear transform theory, is described and results are compared with a measured current profile. The effects of hydrogen over-potentials at the cathodic portions of the pipe are considered and some laboratory data are given in support of conclusions regarding the over-1.01tuge.s. INTRODUCTION To date an appreciable amount of work has been done on the measurement of oil well casing currents and on the correlation of the anodic portions of the current profiles with corrosive casing failures. Speculations on the origin of the casing currents have, however, remained rather vague; and although almost every plausible cause has been mentioned, there is to the writers' knowledge no clear-cut expose' on the details of the causes of the corrosive currents in the literature. A study of current surveys and casing failures in the N.W. Burnett field, Ellis County. Kan.. indicated the probability that concentration cell emf's between the Wellington salt section and the relatively fresh waters in the Dakota sands were a major cause of the corrosion currents. A more general concept evolved upon analysis of the severe corrosive conditions in the Pleistocene sands in the Ventura Avenue and San Miguelito fields in California. In this area no major variations in the salt content of the formation waters occur and yet large casing currents are observed. An explanation is found in the fact that the local spontaneous potentials which are set up due to concentration contrast between the drilling fluid and the connate water are short circuited when casing is set. The very conductive path through the casing increases the magnitude of the currents and has the tendency to average local sources over fairly large intervals. Current will flow between the sections that are predominently shaly and the sections that are mostly sandy. At the places where the current leaves the pipe, corrosive attack will occur. This same phenomenon will be present wherever unprotected pipe is set through sections that show large SP kicks on the electric logs over reasonably thick interval~. GENERAL- NATURE OF THE SPONTANEOUS POTENTIALS When a sequence of sedimentary rocks is penetrated by a drill hole filled with a mud which has a different salt concentration from that in the formation waters, various types of electrochemical potentials are established between the formations and different parts of the mud column. Opposite clean sand sections. a simple liquid-liquid junction potential will be observed; while opposite argillaccous formations, a membrane potential, often referred to as shale potential, will be established. The first quantitative analysis of these emf's in terms of liquid junction and membrane potentials is due to Wyllie.1

Jan 1, 1956

By J. J. Gilman

Examination showed that characteristic cleavage step patterns are observed on the cleavage surfaces of undeformed, slipped, bent, twinned, compressed, and indented zinc crystals; and the effect of temperature is discussed. Dimples were seen to produce cleavage steps in a treelike pattern in otherwise undeformed crystals. The steps seem to originate when cracks intersect screw dislocations. IT has been known for a long time that the path of fracture in polycrystals may be discontinuous (see Jaffe, Reed, and Mannl for review). Recently, Kies, Sullivan, and Irwin2 have proposed, and given evidence, that crack propagation is discontinuous within individual crystals as well. Other evidence has been given by Low.' When discontinuous cracks within a crystal join together to make a macrocrack, the lamellae between each set of two cracks are torn somewhere, forming small cliffs. These cliffs appear as lines when the cleavage surface is observed microscopically.4,5 The lines have been called vein, tree, and riverlike markings by various authors, and they have sometimes been mistaken for fissures. The descriptive term cleavage steps is used in this paper. Cleavage steps vary in height over a wide range of values, from molecular dimensionsG to lor. and larger. Kies, Sullivan, and Irwin,2 as well as George,' have shown that the gross cleavage step patterns for plastics, polycrystalline metals, and for mono-crystals are sometimes similar. Thus, they depend mostly on the mechanical variables that prevail during cleavage and are relatively insensitive to the structure of the material. For example, parabolic markings2,7,8 sometimes result when cracks open up ahead of, and not coplanar with, the main crack front. If the advance crack has the same velocity as the main crack, their intersection line is a parabola, otherwise it is a hyperbola or an ellipse. The patterns are strongly affected by differences in crack velocities. This results in chevron patterns which point to the place of origin of the main crack. It is the purpose of this paper to demonstrate the existence of a mechanism of cleavage step formation which is a continuous rather than a discontinuous process. Also, certain characteristic step patterns are described, and the strong effect of temperature is shown. The specimens were zinc monocrystals (grown from 99.999+ pct pure metal). These were cleaved at room temperature and at — 196°C. Results and Discussion Cleavage step patterns are highly variable from point to point on a given specimen, as well as from one specimen to another. Although the patterns shown in the photographs are typical, they have been selected for graphic illustration. Figs. la and lb compare undeformed crystals that were cleaved at —196 °C and room temperature, respectively. Cleavage at room temperature (Fig. lb) resulted in a higher density of high steps (dark black lines) and enhanced the visibility of the fine background markings. Deformation by simple slip caused no marked change in the step patterns until the glide strain reached about 1.0. But, as Fig. lc shows, the density of high cleavage steps was greatly increased by large glide strains. Corrugations lying perpendicular to the slip direction may also be seen in Fig. lc. These are caused by deformation bands. The cleavage resistance of the crystal of Fig. lc was very high compared to undeformed crystals (estimated by the force on a needle required for cleavage). Striking and varied cleavage step patterns were observed on bent crystals. Two characteristic patterns that were observed on crystals bent at 25°C, and cleaved by reverse bending at —196°C, are shown in Figs. 2a and 2b. The first, Fig. 2a, consists of V-shaped lines similar to the parabolas of other materials2,7 Fig. 2b shows a pattern that is the equivalent of Fig. la, consisting of faint background lines with a few higher step markings. Cleavage of bent crystals at room temperature resulted in Figs. 2c and 2d. Now, the cleavage step lines show a strong tendency to follow one of two perpendicular paths. In Fig. 2c (bent once), many of the cleavage step components that lie parallel to the bend axis are assembled into irregular lines. In Fig. 2d (bent twice), the cleavage steps again tend to consist of two perpendicular components, but neither of the components is assembled into lines. Also, the step density is higher.

Jan 1, 1956