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By H. R. Quina

Phosphate is one of the most important minerals in our world today. It contains the life-giving element of phosphorus, which is essential to the growth of every living cell in plant, animal, and man. This vital mineral is found in twenty-three states of the United States; however, for more than 70 years, Florida has led the nation in phosphate-production and now produces 70% of the requirements of this country. Since the early 1880% when rich phosphate deposits were accidentally discovered in a river-bed in Central Florida, the industry has developed into a multi-million-dollar operation. Phosphate mining began in Florida in 1887 with very crude methods and equipment. The original process was necessarily slow and tedious, resulting in total production of 3000 tons in 1888. Progress was made in improved mining operations, and by 1894. Florida had grabbed the lead as the nation?s largest phosphate-producing area, and is still in the top position.

Jan 1, 1962

By J. W. Town

This report summarizes the results of laboratory investigations made by the Bureau c! Mines on the recovery of mercury from caustic sulfide solutions by aluminum precipitation and by electrodeposition. Statistical methods were used to design the experiments and evaluate the resulting data. Precipitation studies demonstrated tint metallic mercury could be recovered from mercury sulfide-sodium sulfide solutions with aluminum. Other metals and their salts and aluminum, salts precipitated only black mercury sulfide. Over 95 percent of the mercury was precipitated from solutions prepared with reagent-grade chemicals and from cinnabar leach solutions. Two equivalents of aluminum were required to obtain 95 percent precipitation of the mercury. Under optimum conditions 1 gram of aluminum precipitated from 4 to 7 grams of mercury; the excess Aluminum was recovered for reuse. The effects of time and temperature on the precipitation of mercury were minor when compared with the effects of mercury concentration and aluminum equivalents. The particle size of aluminum had no significant effect over the ranges studied. When aluminum was used as a precipitant, the mercury concentration in solution was reduced to below 1.0 grams per liter. Adding arsenic and antimony sulfides to the mercury solution resulted in their coprecipitation with the mercury when the aluminum was added From 95 to 99 percent of both the arsenic and antimony were precipitated as metal, which amalgamated with the mercury.

Jan 1, 1962

By M. R. Geer

All the coal lands in Alaska are publicly owned, and the Federal Government is the principal consumer of coal. Therefore the Government has long been concerned with the wise utilization of the coal reserves of Alaska as well as with the availability of coals meeting the specifications for use in various Government installations. Coal preparation plays a key role in both of these areas of interest. The proper choice and operation of coal-washing equipment permits the mining of inferior deposits, minimizes waste of coal in preparation, and assures a prepared product of the best quality obtainable from the raw coal. Thus, from time to time, the Bureau of Mines has made washability examinations on most of the coals mined in Alaska. Generally, these examinations were made when new mines or new beds were opened, when construction of new preparation plants was being considered, or when the operation of existing plants could be improved by better knowledge of the raw coal. The purpose of this report is to bring together all the washability data available on the coals of the Matanuska Valley and Beluga River fields. The pattern of energy development for the rapidly growing Anchorage area is not clear at this time. Formerly coal was the only fuel available for large-scale space heating and power generation. More recently both oil and natural gas have entered the market, and several hydroelectric projects have been completed. Additional major hydroelectric projects are being considered. The role that will be played by coal in this competitive energy market is uncertain. However I if coal is the fuel used in future power plants or industrial installations, the information contained in this report will be useful in indicating the quality of the coals that can be supplied and in selecting proper preparation techniques.

Jan 1, 1962

By Judson G. Brown

In order to filter small amounts of fine slimy solids the reversible cake-filtration process was developed. The filterable solids contents lion in feeds can range from less than 1 ppm up to about 5%. The relative advantages of this process, are usually the greatest in the range of 0.05% to 1.0% filterable solids. Filterable solids that average in particle size about 20 microns& are non-compressible are very easy for this filtration process. Some feeds have been all sub-micron in particle size. A 1/8 inch thick cake is considered to be very thick. The usual cake is between 13/2 and 1/16 inch thick. A new line of injection molded plastic filter plates were developed for use with the reversible cake filtration process. The first commercial sized installation of this system was made 3 years ago in the Wakefield Y.M.C.A. swimming pool. Over 70 filters ranging in size from one plate to 63 plates have been produced. In addition to the process advantages there are the low cost and corrosion resistance advantages of the plastic plates.

Jan 1, 1962

By Leonard Obert

This report presents evidence indicating that when rock is stress-relieved during the course of mining or in drilling a core, it may be altered or damaged to the extent that the physical properties of the relieved specimen are not the same as those of the in situ rock. Furthermore, this type of damage may result from stress change other than that accompanying stress relief, such as the application of a relatively large compressive stress. In some instances the damage is microscopic, manifesting itself as incipient cracks or the failure of individual crystal bonds. However, if the sample is taken from a high-stress area, macroscopic damage may occur.

Jan 1, 1962

By E. V. Kleber, V. F. Novy, R. C. Vickery

The constitutional diagram for the gadolinium-cobalt system has been determined. Seven intermetallic compounds have been found at compositions corresponding to the follwing gadolinium-cobalt ratios: 3:1, 1:1, 2:3, 1:2, 1:3, 1:4, 1:5. The GdCor compound has a congruent melting point above 1600°C. whereas the remaining compounds melt incongruently. Eutectics exist at 16 wt pct Co and 84 wt pct Co, with melting points of 620° and 1260°C, respectively. PREVIOUS papers'" have recorded constitutional data for systems of gadolinium with iron and nickel. This paper presents data obtained on alloys of gadolinium with the remaining 3d transition element-cobalt. voge13 found that cerium forms, with cobalt, the intermetallic compounds; Ce3Co, CeCo, CeCo2, CeCo3, CeCo4, and CeCo5 Other workers4-' found the 1:2 compound in this series to exist in a C-15 (face-centered cubic) structure and the 1:5 compound to exist in a hexagonal crystal system. Comparison of earlier data with that now reported will be made subsequently. EXPERIMENTAL Methods of alloy preparation, annealing procedures, and experimental techniques have been previously reported.' The cobalt content of alloy specimens was determined volumetrically. RESULTS Microstructure—The alloy containing 10.5 wt pct Co corresponds closely to the composition of the first intermetallic compound Gd3CO. In Fig. 1 the microstructure is essentially single phase composed of Gd3Co which formed peritectically. The globular areas are remnants of the peritectic reaction which did not quite go to completion. A eutectic occurs between Gd3Co and the next higher compound GdCO, which is followed by a series of peritectic compounds. Fig. 2, an arc-cast alloy containing 20.2 wt pct Co, shows large primary crystals of GdCo etching either white or black (depending on crystallographic orientation), embedded in the eutectic. Similarly, in Fig. 3 at 31.2 wt pct Co, a compound, probably GdCo3, has separated from the melt. Subsequent peritectic reactions were almost completely by-passed as the alloy cooled, the residual liquid freezing as a fine eutectic. In the 47.5 wt pct Co alloy, Fig. 4, the high melting point compound, GdCO4, has solidified as massive, white-etching grains, which reacted with the liquid to form GdCo3 as the second phase. The microstructure of an arc-melted alloy containing 60.5 pct Co is complex, Fig. 5, and presents some difficulty in interpretation. The grey etching matrix is probably primary GdCO4. The dappled phase represents grains of GdCO5 which have separated from the melt on cooling. The discrete spots in this phase are eutectic liquid. Small light etching crystallites are probably GdCO5 formed by the incomplete high-temperature peritectic reaction. GdCO4 is retained in arc-melted specimens containing 70.5 wt pct Co, Fig. 6. White areas of this compound are held in a matrix of GdCO5 the appearance of which is mottled slightly by inclusions of the second eutectic in this system. The development of the spheroidized eutectic at high cobalt contents is depicted in Fig. 7 (80.3 wt pct Co) in which the white massive crystals are GdCO5 compound. Further development of this eutectic is seen in Fig. 8, the primary white phase here being pure cobalt. Thermal Studies—Differential thermal analyses and melting point determinations have yielded the data shown in Fig. 10. The high gadolinium eutectic, indicated by microscopy, was confirmed at about 16 wt pct Co, melting at 620°C . A eutectic also occurs at about 84 wt pct Co melting at about 1260°C. The thermal arrests at 8803 960°, 1060; and 1210°C,

Jan 1, 1962

By Adrian C. Dorenfeld

Laboratory data form the basis for the design of flotation circuits. These data, obtained from testing samples of the ore, should show the optimum con- ditions for concentrating the ore and the effects of change in process vari- ables. Among the more important variables commonly met in flotation practice are: Liberation Size-This is the particle size at which substantially all of the valuable minerals are detached from the gangue minerals. Reagent Additions- Experimental data will show the reagents used and their quantity, quality, and point of addition. Pulp Density-This is an important variable in the design of the flotation circuit because it is one of the factors determining the size and number of flotation cells. Flotation Time-The time necessary to make the separation into concentrate and tailing depends on such factors as particle size and reagents used and must be known for determination of the size and number of flotation cells in the plant. Temperature of Pulp-Temperature affects flotation reactions. Water at approximately room temperature is satisfactory for most flotation separations, but some minerals such as fluorspar are best floated in hot water. Type of Circuit-Many types of circuits can be designed, as discussed in detail later. The laboratory tests should provide data for design of the plant circuit best suited to the ore. Water-Knowledge of the quality of the future plant's raw water is important because water quality may drastically affect flotation results. If possible, flotation tests should be made using samples of the water to be used in the plant. Flotation results may vary with seasonal temperatures and with circulation of reclaimed water. Experimentation can show whether it will be necessary to provide for heating, cooling, treating, or reclaiming the water. Uniformity of Ore-The extent of variation of the ore in hardness, grind- ability, mineral content, and floatability should be investigated so that the designer can ascertain methods to overcome problems caused by ore variations. Settling and Filtration Data-To design the plant flotation circuits, settling and filtration rates and ultimate percentage solids of the various products must be determined. Corrosion and Erosion-Corrosion and erosion tests should be made on the flotation pulps, particularly if the pulps are acid or at an elevated temperature, so that suitable materials of construction can then be chosen.

Jan 1, 1962

By D. F. Smith

The thermodynamic data presented in the literature for zirconium compounds are incomplete. Among the compounds for which adequate data are Zacking are zirconium fluoride and sulfate. This paper reports experimental heat-content values determined by the Bureau of Mines for these two zirconium salts throughout the temperature range of 273° to 1,200° K. No crystalline transformations were found in the two compounds investigated, and neither of the compounds melted over the temperature range studied. MATERIALS TESTED The Oak Ridge National Laboratories, Oak Ridge, Tenn., supplied the two zirconium salts used in this investigation. The zirconium fluoride was high- purity reactor grade material. The zirconium sulfate contained between 0.01 and 0.10 percent hafnium and calcium, and other elements in concentrations below 0.01 percent, A spectrographic analysis of the two compounds is given in table 1. Before use the compounds were dried at 400° C. for several hours to removed adsorbed moisture.

Jan 1, 1962

By A. W. Henderson

The growing importance of halide metallurgy for preparing high-purity metals has stimulated research to extend halogenation reactions to the direct extraction of metals from low-grade sources. This Bureau of Mines investigation involves a pioneering study of chlorination reactions in the presence of a fluorine donor. Tin slags containing tantalum and columbium and a zircon concentrate containing a relatively high ratio of hafnium to zirconium were studied. Direct chlorination of these materials at 500° C. yields only a 5-percent conversion of tantalum and columbium or zirconium and hafnium to anhydrous chlorides. This investigation showed that small additions of calcium fluoride to the reaction increased the recovery of tantalum and columbium to 95 percent and the recovery of zirconium and hafnium to 27 percent. These results were achieved with ratios of calcium fluoride to mineral or slag of only 0.2. Silica, the major impurity in the materials studied, was found to be converted to silicon tetrafluoride during chlorination in direct proportion to the quantity calcium fluoride added to the charge. However, large additions of calcium fluoride decreased the volatility of the resulting halides of tantalum, zirconium, and hafnium. Smaller amounts of calcium fluoride also favored recovering minor metal constituents in the zircon concentrate (uranium, thorium, and rare earths).

Jan 1, 1962

By R. J. Wasilewski

THERMAL expansion of rhenium data have been reported by Agte et al.,&apos; and Medoff and cadoff,&apos; respectively, while the linear expansion coefficient was determined by Sims et Al.3 Denoting expansion coefficients parallel and at right angle to c axis by all and Al respectively, their weighted mean should be equal to dilatometric linear coefficient of a random polycrystalline specimen. The values reported for these coefficients are tabulated below: Since these values are in poor agreement, and because of anomalous expansion behavior observed in titanium 4 and chromium, a rede termination of the axial expansion was carried out. A Unicam 19-cm-diam high-temperature camera was used, with unfiltered CuK radiation. Camera calibration was carried out using at Pt wire standarde at temperatures up to 1100oC, the variation between indicated and true temperature being within the experimental error (estimated at <3oC) above 750o C. Rhenium Johnson Matthey spectrographic standard) was vacuum annealed at 1000 oC prior to X-ray diffraction experiments. Lattice parameters were obtained by least-squares solution using the reflec- tions (1232), (1015), (2024), and (3030) for all the patterns, and the additional reflection (2133) for higher temperature (400°C and above) patterns. The relative expansion data obtained are shown in Fig. 1, lengths of the vertical bars indicating the spread in the parameter values obtained by using various combinations of three spacings from the four or five measured. The data calculated from the equation of Ref. 2 are included for comparison purposes. Several specimens were used to obtain the above data, neither of them showing a significant parameter change after completion of the high temperature runs. Some parameter data and the corresponding expansion coefficients between 25 oC and the measurement temperature are tabulated below. The comparison of the present data with those previously reported shows reasonable agreement with the results of Medoff and cadoff2 within the temperature range covered by them (up to 1000 oC). The a values are appreciably higher throughout most of the investigated temperature range. The basal expansion is—in agreement with their findings—appreciably higher than that in the direction of hexagonal axis. The expansion coefficient, al, however, decreases rather more slowly with temperature than previously reported. The expansion along the c axis up to nearly 1000°C appears in excellent agreement. However, at higher temperatures there is a marked deviation towards higher expansion, reproducible between different specimens. Furthermore, there seems to be some irregularity in the variation of all with temperature, the apparent local minimum and maximum values at 510o and 1024o C, Table II, being well outside the experimental error limits. It must be stressed that the apparent discontinuity in the c parameter expansion is still insufficient to account for the expansion value reported by Agte et al.&apos; since a total expansion of close to 2 pct would

Jan 1, 1962

By John J. Mulligan

Lead-silver deposits in the Omilak area, on the western slopes of the Darby Mountains, Seward Peninsula, Alaska, were investigated by the Bureau of Mines, during the 1953 and 1954 field seasons, as a part of the U.S. Department of Interior&apos;s continuing program for the development of Alaska&apos;s resources. The Omilak area was the scene of early day prospecting and mining activity. The Omilak mine, which operated from 1881 to 1890, was the second producing lode mine in Alaska; the first was a small gold mine near Sitka. Several hundred tons of ore were produced at the Omilak mina; as an indication of grade, 41 tons shipped from Omilak in 1889 contained 75 percent lead and 142 ounces of silver per ton. A prominent, nearby occurrence of lead-silver minerals, found but not explored during this period, has since become known as the Foster prospect. Subsequent exploration of this prospect revealed an abundance of massive galena occurring on an outcrop and as float scattered through limestone talus. Evidence of lead deposition, together with the generally high silver content of lead ores previously shipped from the district, indicated that deposits might be found which would be commercially valuable even in this remote area. To investigate the possibility, the Bureau of Mines made a reconnaissance of the Omilak area and did bulldozer trenching, diamond core drilling, and sampling at the roster prospect. Data resulting from the investigation are presented in detail in this report and are summarized in the following paragraphs.

Jan 1, 1962

By Orvar Nyquist, Klaus W. K. Lange, John Chipman

Liquid Fe-C-Si alloys containing 0 to 12 pet Si and up to 4 pet C were equilibrated with carburizing gases at 1550°C. Two to 5 alloys simultaneously were held in close proximity for 5 to 7 hr to establish uniform carbon activity in the group. Analysis of the data gives the activity coefficient of carbon as a function of the mole fractions of carbon and silicon, Fig. 7. Values of the interaction coefficients at infinite dilution are

Jan 1, 1962

By W. H. Ode

An investigation of standard methods for determining ash in low-rank* coals showed that generally 60 to 95 percent of the total sulfur in the coal is retained in the ash as SO3. This large sulfur retention causes a positive error in the determined mount of ash of as much as 6 percentage points for the coals examined, although it usually is 2 to 3 percentage points for lignites and about 1 for subbituminous coals. Unless the sulfur content is low or unless a correction is made for the SO3 retained, the fixed carbon and oxygen have an equivalent negative error when determined by difference; also other inaccurate analytical values occur when the data are calculated on an ash- free bas is. No simple modification of the ashing procedure was found that would reduce the sulfur retention to a point where its effect on the ash determination would not be significant, Therefore, for accurate analytical work on law-rank coals, the SO3 should be deducted from the determined ash to obtain a "corrected" ash value.

Jan 1, 1962

By M. E. Tyrrell

To promote greater use of abundant domestic raw materials in the manufacture of synthetic mullite, the Bureau of Mines has undertaken a comprehensive investigation to determine the effects of the impurity oxides TiO2, Fe203, and alkali on physical properties of sintered mullite-forming mixtures. The first part of the report presents the results of work covering a major area within the mullite study; namely, the effect of impurity oxides on volume stability, one of the outstanding characteristics of mullite refractories. The volume stability of 20 compositions in each of 3 alumina- to-silica ratios, which blanket the range commonly found in purchase specifications, has been determined following procedures of Navy Specifications B-15606 A for Grade A high-alumina refractories. Results indicated that so long as 5 percent of impurities are combined approximtely in the proportions of 3 percent Ti02, 1 percent Fe203, and 1 percent alkali, sintered mullite-forming compositions in the almina to silica range tested will be volume stable. A permissible tolerance of one-half per- cent in each impurity oxide provides a range that includes values common in the natural minerals from which sintered mullite may be made. Within the total range of 5-percent impurity mixtures, a greater number of volume-stable compositions were obtained by increasing the alumina-silica ratio.

Jan 1, 1962

By G. W. Birge

Carbonizing properties of the principal coal beds of Perry County, Ky., are described in this Bureau of Mines report. Seven samples, representing the Hindman, Flag, Haddix, and Fire Clay beds, were carbonized by the Bureau of Mines-American Gas Association (BM-AGA) method, and yields of products and physical properties of cokes were determined. Carbonizing properties of blends of Flag and Fire Clay coals, with 20 and 30 percent Pocahontas No. 3 low-volatile coal from McDowell County, W. Va., also were determined. Expanding properties of the Flag and Fire Clay coals and their blends were determined in the Bureau of Mines sole-heated oven. The Perry County coals tested are high-volatile A bituminous in rank and, with the exception of the Hindman-bed sample, which contained excessive sulfur, were chemically suitable for metallurgical use. The three coals tested in the sole-heated oven contracted less than normal for Appalachian coals of similar rank, Blending the Fire Clay and Flag coals with 20 or 30 percent low-volatile coal increased coke strength appreciably but increased the expansion beyond normal limits for industrial blends.

Jan 1, 1962

This report is the 24th in a series summarizing research on coal and related investigations3 by the Bureau of Mines. The coal programs of the Bureau of Mines include a wide range of theoretical and applied studies--such as fundamental studies of coal structure and properties, the development and evaluation of new mining techniques, and work toward more effective processing and utilization of coal. The scope of these programs is indicated, in topical outline, by the table of contents. These investigations are integrated into a broad but coordinated effort to develop information on coal that will benefit the coal mining industry and the coal consumer while promoting the wise conservation and utilization of our national coal resources. Any attempt to summarize in one volume the progress in all of the program areas indicated must necessarily be limited to a brief review of developments, without detailed reporting of the data. However, while the brief discussion in each section will present only the highlights of the Bureau&apos;s work during the year, details of many of the operations or investigations described here can be found in the publications cited throughout the text. Other work, reported here for the first time, will be covered in greater detail in later publications.

Jan 1, 1962

By D. F. Boyd

On April 10, 1958 a new 7500 long ton/day iron ore beneficiation plant went on stream producing an average of 3000 long-tons of high quality concentrate a day. Plant operates on two, 12-hour shifts is six days per week, The new mill end crust ink plant were built adjacent to the company&apos;s open pit dining operate on at Bomi Hills, Liberia. The mall is essentially a gravity concentrator employing crushing, and grinding to liberate the mineral values, followed by concentration in Humphreys spirals. The cleaner spiral tailings are re-ground and tabled to recover additional iron values. Ire addition to. this mills the company operates a crushing and screening plant for the high grade direct shipping ores

Jan 1, 1962

By G. Asai

The purpose of this Bureau of Mines investigation was to determine the properties of arc-melted iron-chromium alloys ranging in chromium content from 12 to 50 wt.-pct. Alloys were prepared by consumable-electrode arc melting of electrodes composed of high-purity chromium and high-purity iron. Alloys were fabricated to rod and sheet, and the following data were obtained: Electrical resistivity, hardness, tensile strength, and impact strength at room temperature; and creep-rupture life at 650° C. (1,200° F.). As the chromium content of the annealed alloys varied from 12 to 50 pct., the properties varied as follows: The electrical resistivity increased proportionally from 41 to 53 microhm-cm,; the Rockwell hardness varied from A 38 to A 58; the tensile strength ranged from 52,000 to 96,000 p.s.i.; the impact strength of V-notched charpy specimens varied from 140 to 405 ft.-lb., and the 100-hour creep rupture life at 1,200° F. varied from 5,000 to 16,000 p.s.i.

Jan 1, 1962

By Nicholas J. Grant, Irmgard Rump, Bill C. Giessen

The system W-Hf was determined by use of metal -lographic and X-ray methods. The only interrnetal-lie phase W2Hf melts peritectically at 2650° ± 50°C. A eutectic between W2Hf and ß-Hf solid solution exists at 78 at. pct Hf arul 1930º ± 10°C. The addition of tungsten loulers the hafnium transfornzation; there is a eutectoid at 93 at. pct Hf and 1560°C. The solubility limits of the terminal solid solutions were determined. At the beginning of this investigation, the system had not been elaborated; only crystallographic work had been done to determine the structure of the occurring intermetallic compound W2Hf, and a certain analogy to the system W-Zr was to be expected. Special emphasis was placed in this program on the Hf-rich part of the diagram. Following the completion of our experiments, a phase diagram was suggested by Braun and RUdY.1 EXPERIMENTAL METHODS The investigation utilized tungsten powder supplied by the General Electric Co. with a purity of about 99.9 pct and hafnium crystal bar of about 97.7 pct purity, 2.3 pct Zr, supplied by Foote Mineral Co. Typical analyses are given in Table I. The procedures followed were identical with the ones described for the Re-Nb diagram.&apos; Tungsten powder was compacted at 16,000 psi and the necessary amount of hafnium was added in the form of small pieces cut from the crystal bar, with a reasonable excess of tungsten powder to make up for powder losses on melting. High hafnium or tungsten melts were prepared from premelted tungsten and hafnium or by employing master alloys. The melting was done in a Heraeus arc-furnace under argon. Melting and remelting up to 8 times resulted in fairly homogeneous alloys. No weight

Jan 1, 1962

By P. C. Badgley

The purpose of this paper is to demonstrate the usefulness of systematic analyses of weakness patterns. The term weakness here includes structural features such as fractures, foliation planes, lineaments and bedding. Many of these features are mapped by geologists in the field, but analysis of the field date is frequently overlooked. Examples are presented to show the value of such studies in petroleum and mineral exploration, in dam site selection, and in regional tectonic interpretations. Numerous theories have been presented to account for the mechanics and time of origin of fracturing. This is an extensive subject and cannot be reviewed in detail here. The reader may wish to refer to other papers.*"5 It is sufficient to say that most fracture patterns can be related to one or more of the following force mechanisms: compression, tension, torsion and fatigue (inheritance by upward propagation of pre-existing fractures). Fractures generally occur in sets in a district. The angular relationships and other characteristics of the individual sets frequently help in determining the force mechanism and movement history of the deformation. From a geometric point of view fractures are commonly referred to as longitudinal, cross, or diagonal (shear), depending upon their orientation relative to other major structural features such as anticlinal axes and so forth. These terms will be used from time to time and are illustrated schematically in Fig. 1. FIELD PROCEDURE AND TREATMENT OF DATA In fracture studies it is very important to collect adequate field data. Fig. 2 illustrates a notebook sheet for recording significant field observations in sedimentary rocks. Slight adaptations have to be made for igneous and metamorphic terrains. Fracture density and persistence are very important factors in petroleum exploration for fractured reservoirs and mineral exploration. The density for each joint set is recorded in terms of number of joints per linear yard. The total number of joints at any one

Jan 1, 1962