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By L. A. Roe

The year 1867 marks the first year of commercial production of phosphate rock in the United States. South Carolina produced almost all of the domestic output of mineral phosphate until phosphate mining began in Florida in 1888. During the period 1868 to 1949 the total marketed production of domestic phosphate rock was about 186 million long tons of which 71.5 percent was produced in Florida, 18 percent in Tennessee and 7 percent in South Carolina (1). From 1949 through 1960, Florida phosphate rock production has ranged Prom 71 to 77 percent of the total domestic production. Since three-fourths of the domestic phosphate production is from the Florida field, and since most of the phosphate from the Tennessee and Western fields is not processed, but used directly as electric furnace burden, this paper will concern itself almost entirely with water requirements for mining and processing ore from Florida. Figure 1 summarizes phosphate rock production for Florida vs. total United States production over the period 1947-1960.

Jan 1, 1962

By Richard S. Watt

The Bureau of Mines is often called upon to analyze the demand for various minerals and fuels and to make projections of the future demand. Because minerals and fuels are raw materials and because the demand for raw materials [pends] on the demand for finished goods, these projections are usually [conned] with derived demand rather than final demand. In order to obtain quick [d] reasonably accurate analyses of the demand for mineral commodities, the [reau] developed a method and has used it successfully (31).4 To illustrate the [thod], this report presents a full analysis of the demand for a mineral commodity with enough general theory to permit application of the method to any mineral. Sodium chloride (common table salt) was chosen as the subject of the analysis because the demand for it is less complicated5 and permits a simple application and clear presentation of the method.

Jan 1, 1962

By D. W. Bridges

Solvent extraction has become important in recent years as a unit process in extractive metallurgy. The flexibility and simplicity of the technique have attracted widespread attention, and numerous papers describing actual and projected metallurgical applications have been published. However, differences in terminology, procedure, objectives, and standards, as reflected in reports by different operators and investigators, have sometimes made appraisals and comparisons difficult. Consequently, a need appeared for n series of basic reports on the subject. This Bureau of Mines Information Circular is the first of such a series. It deals with the status of solvent extraction in metallurgy, as well as with the rudiments and terminology of the unit operation. In analytical chemistry, extraction of molecular species from aqueous media by immiscible organic solvents has been used for many years to separate and determine chemical elements (61).4 Complex chlorides of iron and other metals are readily soluble in ethers and ketones, as are the nitrates of uranium and thorium. Most metals are extractable as complex salts of some organic reagent, such as dithizone, 8-hydroxyquinoline, or cupferron.

Jan 1, 1962

By A. C. Johnson

This circular is one of a series published by the Bureau of Mines describing mining and beneficiation methods and costs at various mining operations throughout the United States. Inclusion of the Abbott mine in this series is of particular interest, as the complex geology and the character of the deposits make their exploitation a unique operation. The mine operates on a high-cost, comparatively small-scale basis, and only the persistence of an aggressive management has enabled it to maintain its rank among the major mercury producers of California. Rising costs and decreasing metal prices, which continuously threaten the low profit margin, are reflected in increased efficiency of operation. This report summarizes past operations and describes, in detail, the geology and ore deposits; exploration and mining methods; and furnacing and condensing operations. It covers the entire operation from initial exploration to the actual production of mercury. Comparative production costs for 1944 and 1958 are of special interest.

Jan 1, 1962

By Hudson S. B

With a particular electrode configuration, and a particular combination of electrode voltage and roll speed, a relatively small increase in electrode voltage, or a relatively small decrease in roll speed, resultsin a marked improvement in the separation of zircon from ilmenite. In general, fine minerals can be separated using a higher roll speed, or a lower electrode voltage, than is required to separate coarse minerals. The ionizing electrode should be reasonably close to the point at which mineral is fed on to the roll, and nearer to the roll than the non-ionizing electrode. The optimum conditions for the separation of zircon from ilmenite may not apply for the separation of other non-conductors from other conductors.INTRODUCTIONAlthough the high tension separators used in the Australian beach sand industry are efficient, this efficiency has been gained very largely by a process of trial and error, and not by a systematic study of the effects of changes in the operating variables. The optimum roll speed for a particular electrode position and electrode voltage, and the optimum electrode voltage for a particular roll speed and electrode position, can both be determined quite readily. It is not so simple to determine the optimum electrode position for a particular electrode voltage and roll speed. The reason for this is that the electrode used in high tension separators consists of two parts-an ionizing and a non-ionizing electrode respectively. The angular and radial positions of these electrodes, relative to the feed roll and to each other, affect the behaviour of conductors and non-conductors to varying degrees.

Jan 1, 1962

By L. M. Burman

The phase-boundary pressure required to maintain a natural hydrocarbon fluid in a single phase must be considered in planning the recovery of reservoir liquids by miscible-phase processes. The change in the phase-boundary pressure at reservoir temperature that results when a light component or a mixture of light components is added to a reservoir fluid is an especially important consideration. The cricondenbar pressure (maximum phase-boundary pressure) and the critical pressure are unique correlated pressures that have been utilized to calculate the change in phase-boundary pressure that may result when the composition of a reservoir liquid is altered by an additive. In this study one reservoir oil and three gas-condensate fluids are used as examples. Correlations pertaining to the critical and cricondenbar states in chapters 4 and 5 of Bureau of Mines Monograph 10 (3)5 were used to demonstrate how butane and lighter components added to these reservoir fluids affect their phase-boundary pressures.

Jan 1, 1962

By L. H. Banning

This investigation was undertaken to obtain basic information necessary for the design and operation of a plant for recovering metallic values from nickeliferous laterite and serpentine of the Philippine Islands. It was divided into three parts: (1) Mineralogical studies and preliminary mineral dressing tests; (2) electric smelting of the ores, upgrading of ferronickel by blowing with oxygen, smelting laterite slag to produce crude iron, and the production of mild steel; and (3) nickel and cobalt recovery from upgraded ferronickel. Results of the investigation indicate that it should be feasible to recover nickel, iron, and possibly cobalt products from the laterite and ferro-nickel from the serpentine. Mineralogical studies were made on representative fractions of the laterite and serpentine tonnage samples and on five selected samples; mineral dressing tests were made only on laterite. The nickel occurs principally associated with hydrous iron oxides and chemically combined with serpentine; garnierite was the only discrete nickel mineral identified, and it was found in a highly decomposed serpentine. The bulk of the cobalt was found in wadlike manganese oxide material. Approximately twice as much chromite was found in the laterite as in the serpentine, By mineral dressing techniques, laterite was separated into two fractions: one fraction contained over 90 percent of the nickel and cobalt, and 83 percent of the iron; the other fraction contained 74 percent of the chromium. A cobalt concentrate (1.1 percent Co) was produced by a scrubbing and sizing procedure.

Jan 1, 1962

By C. R. Montgomery

Coal companies in order to supply their customers En the metallurgical market, both home and abroad, must be able to control their production in order to meet carbonization specifications over and above those of the proximate analyses which has been the prime consideration of purchases in the past. It is the purpose of this paper to review in brief some of the tests used and give data to show the application of such as it applies to the customers needs. It is now recognized that coal is not homogeneous in any of its properties and an amazing fact is that it has been used for so long a time as the principal raw material for the manufacturing of coke without more emphasis having been placed on the variation between coals; yes, even from coals in the same seam at different geographical locations, Recently Kuchta and Clendenin pointed this fact out In a study of the(1) carbonizing behavior as related to chemical and plastic properties of Alabama medium volatile coal.

Jan 1, 1962

By A. Gene Collins

Potassium, lithium, strontium, barium, and manganese are present in many oilfield brines, None of them except barium is determined routinely in brine analyses. Therefore, sensitive and accurate flame-spectrophotometric methods were developed. Potassium, lithium, and strontium were determined by a standard-addition technique in ethyl alcohol solutions. Barium and manganese were determined in ethyl alcohol and normal propyl solutions, respectively, after interfering substances were removed.

Jan 1, 1962

By R. R. Lowery

This project was proposed to provide information on the hazards associated with arc melting of thorium. A general air-sampling analysis was made to determine the separation, concentration, and distribution of thorium daughter (decay) products throughout arc melting, machining, and forging processes of a thorium handling facility. The value of well coordinated health physics program is stressed in connection with potential health hazards and personnel protection. Building, equipment, and exhaust ventilation requirements for such a facility are discussed. Special handling methods are described for thorium. INTRODUCTION The Bureau of Mines at the Albany Metallurgy Research Center has been involved in handling the naturally radioactive metals, uranium and thorium, for several years. Cooperative work for the Atomic Energy Commission has been carried out with thorium metal, and as a result the concerned laboratories of the Center have accumulated experience on the hazards associated with this metal. This report details the radioactive hazards arising from the arc melting, machining, and forging of thorium.

Jan 1, 1962

The Kingsgate molybdenite pipes are considered on petrochemical data and field occurrence to be, possibly, epi-magmatic plutonic offshoots grading into hydrothermal bodies. There is reason to believe that the ore is derived from a highly acid granite of type similar to that of the tin bearing areas of northern New England. The mineralogy, microtextures and paragenesis of the ore are discussed.INTRODUCTIONThe Kingsgate Mining Field is situated in steep, heavily timbered terrain 18 miles E.N.E. of Glen Innes and 430 miles north of Sydney. Bismuth and molybdenum ores were discovered at Kingsgate (Yarrow Creek) in 1877. Subsequently some 50 pipes were developed yielding tonnages which at the peak of operations, 1905 to 1920, rivalled production from the rich deposits of northern Queensland.Attempts to revive the field have been made periodically and small parcels of ore have been forthcoming.' During World War II demand for piezioelectric quartz again focussed attention on Kingsgate but twinning and other imperfections of the quartz prevented all but a minor exploitation of the otherwise noteworthy crystals of this locality.There is reason to believe that the ore at Kingsgate is not exhausted through exploration and mining costs would probably be high due to the capricious nature of the pipes and to the irregular distribution of rich ore shoots within them.

Jan 1, 1962

By W. H. Class

The embrittling effects of oxygen, ozone, nitrogen, air, and surface residues, on NaCl has been investigated. The embrittlement by ozone and oxygen was found to be associated with the formation of a NaClO3 surface compound. In these cases the initial crack that was responsible for fracture (in a bend test) always nucleated at the corners between the tension and side faces. The behavior of air was very erratic and on certain days did not produce enzbrittlement. During these periods, crystals that had become embrittled by the ozone treatment completely recovered their ductility after a short exposure to the ambient atmosphere, It was established many years ago1 that considerable ductility could be obtained in NaCl single-crystal specimens if the crystal surfaces were dissolved in water either during or immediately prior to the test. The original interpretation of this effect by Joffe attributed the enhanced ductility to the removal of surface microcracks by dissolution. Later investigations2'3 have suggested that the exclusion of air from the specimen surface is the criterion for extensive plastic flow prior to fracture. The air em-brittlement in this later work was attributed to the diffusion of gaseous atoms into the surface layers of the crystal, thereby impeding the movement of dislocations. This model satisfactorily accounts for the reembrittlement observed after further air exposure subsequent to the water dissolution treatment. However, the situation has recently become more complex by the observations in several laboratories4-t that under certain conditions air exposure does not impair the ductility of NaC1. It has also been recognized5 that improper drying operations after water dissolution can leave surface precipitates that lead to embrittlement. Cleavage defects on as-cleaved crystals can often be another source of embrittlement. In the present work the effect of the gaseous atmospheres nitrogen, argon, air, oxygen, and ozone, on the ductility of rock salt was studied extensively. The embrittlement resulting from oxygen and ozone exposures was found to be associated with the formation of a NaC1O3 surface film. It is suggested that certain atmospheres, one of which often can be ambient air, which inhibit the formation or favor the decomposition of this compound, can promote ductility. Thus one aspect of the Joffe effect is certainly related to the removal of surface compounds or complexes by water dissolution. The effect of surface precipitates that remain after drying operations and of cleavage defects were also studied. In neither of the latter cases was the embrittlement as severe as that found with a NaClO3 surface layer. PROCEDURE AND SPECIMEN PREPARATION The nature of the embrittlement produced by the agents mentioned above was studied by means of microscopy, mechanical testing, and X-ray diffraction. Specimens were cleaved from large crystals of optical quality sodium chloride obtained from the Harshaw Chemical Co., and, except for those tested in the as-cleaved condition, were given a 15- to 20-sec immersion in distilled water followed by a rinse in absolute methyl alcohol. The specimens were then blotted on a soft, absorbent paper, and dried by a few seconds exposure to a stream of warm, dry air. Such a procedure was found to give a control surface which was microscopically free of residues. (A few crystals were intentionally painted with a concentrated NaCl solution in order to investigate the effect of surface residues). All specimens were of 0.140 sq in. cross-section. Crystals prepared in the above manner were immediately placed in a gas train where they could be exposed to the desired gases for preselected periods of time. For the oxygen and nitrogen exposures, pure reagent-grade gases were employed. The ozone was provided in the form of an ozone-oxygen mixture (approximately 10 pct ozone) prepared by passing commercial grade oxygen over a strong ultraviolet light source. All gases were dried prior to their introduction into the train. Since argon was found to be completely inert in its behavior (i.e., residue-free specimens that were exposed to argon were not embrittled), it was periodically utilized to check the control specimen surfaces as well as the condition of the gas train used for aging the specimens. After exposure to the gaseous media in question, the crystals to be used for the measurement of the strain to fracture were transferred from the gas train to a protective oil bath (without further exposure to the atmosphere) where the tests were conducted in three-point bending. The apparatus was so adjusted that the load could be applied at a constant, continuous rate. Other Snecimens from the gas train were deformed

Jan 1, 1962

By W. M. Merritts

A joint investigation by the Bureau of Mines and the Christopher Coal Co. at the Humphrey No. 7 mine, operating in the Pittsburgh coalbed in northern West Virginia, was undertaken to gain more insight concerning the hazardous emission of methane gas in mining, This report describes the equipment, procedure, and results. Horizontal bleeder holes drilled in the faces drained large quantities of methane, eliminating downtime of mining equipment. Also, larger quantities of methane were removed by forcing 14 to 25 g.p.m. water at 25 to 200 p.s.i. 5 pressure into the bleeder holes, In one infusion test a fluorescein dye was added to the infusion water; in later mining operations, the infusion water was traced for a distance of 1,500 feet. With vacuum pump applied to the horizontal hole the gas-flow rate increased, and the methane content decreased.

Jan 1, 1962

By Lindsay D. Norman

Eleven major pyrometallurgical processes and operations suggested for recovering manganese from domestic resources are described. These include seven pyrometallurgical processes that usually yield a ferroalloy or a product from which ferromanganese can be produced in one operation. The remaining four involve pyrometallurgical operations whose products require either an additional two-stage process to produce ferromanganese or chemical processing to recover a high-quality manganese oxide product.

Jan 1, 1962

By Michael G. Zabetakis

Vaporization of a solvent into an airstream at temperatures above the flash point of the solvent is hazardous if vapor is liberated at a rate that is sufficient to produce a flammable mixture. In may operations, the formation of such a mixture is prevented by rapid diluton of the vapors with air. The minimum air requirements for the dilution process are determined by the composition of the lower limit mixture at the temperature and pressure of interest. Because limits of flammability cannot always be calculated with sufficient accuracy for a proposed operation, they .rust often be determined experimentally. The present Bureau of Mines investigation was prompted by an application in which the lower limits of flammability of a number of solvent mixtures were required over a range of temperatures at atmospheric pressure. These limits were to be used along with available solvent-vaporization-rate data to establish minimum airflow rates needed to prevent the formation of flammable mixtures in an industrial process. Lower limits of flammability were determined for a number of mixtures containing methyl ethyl ketone, tetrahydrofuran, toluene, ethyl alcohol, and ethyl acetate in dry air-at atmospheric pressure and temperatures between 16° and 200° C. The experimental values were found to be in good agreement at with those predicted by Le Chatelier's law; variations with temperature were in fair agreement with those predicted by a modified Burgess-Wheeler law.

Jan 1, 1962

By James R. Kerr

Although metallurgical benefits of processing metals in a vacuum or reduced atmosphere have been realized for a hundred years, the problem of creating a vacuum in the range from 10-0 to 10-4 mm. of mercury in a moderately sized furnace chamber has been difficult to solve. The demand for these and lower pressures, with the advent of World War II, for separating the fission-able uranium isotope from its stable twin by the electromagnetic process, gave impetus to developing pumps capable of delivering extremely low pressures. With the release of data by the Atomic Energy Commission on methods of securing high vacuum in large equipment, steel companies took the initiative, and the growth of the vacuum-melting industry was assured. Vacuum-induction melting of steel in the United States began on a small scale in early 1945 and in 10 years grew to 60,000 pounds per month or 720,000 pounds per year. The years following 1954 showed tremendous expansion, culminating in 1958 in a capacity of more than 36 million pounds.

Jan 1, 1962

By R. W. Kraft

A back- reflection precession-type X-yay camera for determining the crystallographic orientation of the crystallites of both phases in small areas of thick specimens of polyphase alloys is described ad the geometry, advantages, and limitations of the apparatus are discussed. Metallographic obseg-vations of interfacial angles (or habit planes or growth direction are made on the same specimen so that the crystallographic and metallographzc orientation data call be directly correlated. An example of the application of tile technique to a unidi-~~ectionally solidified CuA12-A1 eutectic specimen is presented. The interfacial planes ad growth directions of each phase were established, and the orientation relationship between the phases was observed and found to be approximately intermediate between two previously reported relationships. The crystallographic interfacial relationship between two solid phases is an important parameter in a variety of metallurgical phenomena because of the energy associated with the interface and because this energy is at least partly associated with the way in which the two space lattices are in contact along the interface. In order to describe the interfacial planes in the crystallites of both phases it is necessary to determine the crystallographic orientation of each phase in a specimen relative to each other, and to directly correlate these data with met-allographic measurements from which the interfacial planes can be determined on the same specimen. The back-reflection Laue technique is the easiest way to determine the orientation of thick single crystals or large grains and the method can be combined with metallographic techniques to provide the necessary data, provided the reflections from each phase can be distinguished from one another. However, if the crystallites are small or of varying orientation or if one or both phases has a unit cell with less than the maximum symmetry, many overlapping and complex Laue patterns are recorded simultaneously and it becomes impractical if not impossible to interpret the photographs. All of these complexities were present in a unidirectionally so- lidified A1-CuA12 eutectic alloy1 for which a crystallographic analysis was desired. Consequently the method described here was developed since no known X-ray or electron diffraction technique had all of the following attributes which were required. 1) Method should yield data from which the crys-tallographic orientation of every crystallite or diffracting unit in the irradiated area can be determined. 2) Method should be adaptable to the study of small areas. Depending upon the degree of preferred orientation in the specimens, it should be possible to obtain reliable data in a reasonable length of time on irradiated areas as small as 1.0 or even 0.1 mm in diam. 3) Method should permit direct correlation of crystallographic data with microscopic orientation data pertaining to crystallite axes, habit, morphology, and growth directions as determined by optical microscopy. 4) method should be such that selected areas of large specimens can be easily studied. Trepanning of a small specimen (such as an electron microscope specimen) from larger specimens was undesirable since it would greatly increase the problem of correlating the crystallographic and microscopic directional data. Requirements 3 and 4 dictated that an X-ray back-reflection pinhole technique should be used on large samples, such as metallographic specimens which had previously been examined and analyzed for their microscopic characteristics. Similarly, requirement 2 could be satisfied by choosing a collimator of appropriately small diameter. Exposure times would not be excessive provided the detector were close enough to the specimen. Because of space limitations film was chosen in preference to a Geiger counter. Requirement 1 was fulfilled by using monochromatic radiation and providing enough additional degrees of freedom in specimen rotation to compensate for Bragg law restrictions on diffracted beams. DESCRIPTION OF APPARATUS The apparatus shown in Fig. 1 consists of a pin-hole collimator, (a), projecting through a rotatable circular film in a holder, (b), which records X-ray reflections in the back-reflection region. The specimen, (c), is mounted on the end of a shaft, (d), which is provided with an adjustment, (e), so that the specimen surface can be placed accurately on

Jan 1, 1962

By William J. Campbell

Expansion measurements of platinum, added as an internal standard, are used for thermal calibration of X-ray cameras and diffractometers. Accuracy of the temperatures derived by this technique depends on the precision of expansion measurements and the reliability of reference expansion data. Temperature measurements to ± 1° C. require ?d or ?a to be determined within ± 0.001 percent. Selected expansion data are concluded to be reliable to 2° C., 5° C., and 25° C., over the temperature ranges 0° C. to 700° C., 700° C. to 1,000° C., and 1,000° C. to 1,700° C., respectively. Tabular expansion values from 25° C. to 1,700° C. in 2° C. intervals were calculated from the following equation; Expansion, percent = [8.91 + 1.28 x 10-3(t-25) + 0.04 x 10-6(t-25) ] [t-25.104 ] These tabular values facilitate future corrections of published temperatures as more reliable expansion-temperature data become available.

Jan 1, 1962

By Michael G. Zabetakis

The spillage of liquid diethyl ether in rooms at floor level and 3 feet above the floor resulted in flammable vapor-air mixtures in the immediate vicinity of the exposed liquido The liquid temperature was found to decrease by as much as 35° C., with a resultant decrease in vaporization rate. A search of the literature yielded numerous references to unstable peroxide (residue) formed by the autoxidation of ether. Such residues appear to constitute an explosion hazard in the condensed state.

Jan 1, 1962

By Walter C. Lorenz

In connection with its renewed study seeking solutions to problems created by release of acid water from bituminous coal mines, the Bureau of Mines recently surveyed reports already written on the subject. This publication is based on that search. The Problem Poor distribution of water is evident on an ordinary geographic map of the United States. The more abundant supplies of surface water appear to be centered in the northeast, the southeast, and the central humid areas of the country. It is in the midst of this abundant surface water, in the Ohio River Valley, that most of the bituminous coal is mined. Varied industry has located in the valley to use the coal and the river. The coal is a source of power and o raw material. The river provides transportation for raw and finished materials; equally important, it provides the water that is used for cooling and processing in manufacturing. It also serves as a vehicle for the disposal of waste.

Jan 1, 1962