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By Erik Q. Dahl

The strength of green and sintered pellets during reduction under various conditions in a laboratory kiln has been investigated. Equipment and test methods are described, together with the results obtained. The strength of sintered pellets drops sharply when the reduction starts, and goes through a minimum at the 70 per cent oxidation level. At more advanced reduction, the strength increases with increasing metallization. Successful use of green pellets as kiln feed requires that more attention be paid to the pellet preparation than is necessary when producing pellets for separate sintering. In particular, the ores have to be ground to a greater fineness. The initial strength of green pellets is low. Below the 70 per cent oxidation level, however, the strength of these pellets is about the same as the strength of sintered ones. Additions of such materials as silica, limestone and anthracite coal; within reasonable limits, affect the strength only slightly.

Jan 1, 1966

By L. J. E. Hofer

THIS BULLETIN analyzes and summarizes research at the Bureau of Mines dealing with the preparation, properties, and reactions of iron carbides in the period 1948-60, part of which was sponsored by Wright Air Development Laboratories. The objective was to develop better catalysts for the synthesis of methane and higher hydrocarbons from hydrogen and carbon monoxide. The investigations resulted in the first adequate characterization of epsilon iron carbide, which later proved to be an important intermediate in the tempering of martensite in steel. At temperatures near 170° C, the carbon in carbon monoxide reacts nearly quantitatively with finely divided alpha iron to form an iron carbide in which the metal atoms occupy the positions of the close packed hexagonal arrangement with lattice parameters of ao=2.754 A and co=4.349 A. The carbide has a composition within 2 atomic percent of that required for the formula Fe2C, a Curie point of about 370° C, a specific magnetization of 160.4 ergs per gauss-gram Fe at 50° C, and a ferromagnetic moment of 1.70 Bohr magnetons. Epsilon iron carbide can be converted to chi iron carbide by thermal treatment at 343° C for about 70 hours. The chi iron carbide so formed has a Curie point of 247° C, a specific magnetization of 142.5 ergs per gauss-gram Fe at 50° C, a ferromagnetic moment of 1.72 Bohr magnetons per iron atom, and a paramagnetic moment of 5.5 Bohr rnagnetons per iron atom. Direct synthesis of this carbide from carbon monoxide at 240° C indicates a composition within 7 atomic percent of that required for Fe2C. Chi iron carbide can be converted to cementite at 550° C in about 315 minutes. The theta iron carbide so prepared has a Curie point of 210° C, a specific magnetization of 147.3 ergs per gauss gram Fe at 50° C, a ferromagnetic moment of 1.72 Bohr magnetons per iron atom, and a paramagnetic moment of 3.9 Bohr magnetons per iron atom. Pure chi iron carbide reacts to form theta iron carbide by the elimination of free carbon. In the presence of an excess of free iron in intimate contact with the carbide, chi iron carbide reacts with the free iron to form theta iron carbide. The second reaction proceeds at an appreciable rate at 320° C and can be used to snythesize finely divided theta iron carbide with no free-carbon impurity at low temperatures. The ease of the reaction in the presence of free iron suggests that chi iron carbide is an intermediate in the tempering of epsilon iron carbide to theta iron carbide as it proceeds in steels. Experiments on carbon steel show that the magnetic moment of the iron atoms in martensite is about 2.2 Bohr magnetons per atom, a value approximately the same as that of the iron atoms in alpha iron. The Curie points of epsilon iron carbide, chi iron carbide, and theta iron carbide were found -in various specimens of tempered steel to be 10° to 20° C lower than normal values. This shift is probably the result of manganese in solid solution. Preparations of various compositions of epsilon iron carbonitrides show many effects of extensive isomorphism between epsilon iron carbide and epsilon iron nitride. The action of carbon monoxide on finely divided alpha iron at 400° C results in free carbon deposits containing filaments about 0.1 micron in diameter and several times as long. The filaments are characterized by nuclei of dense material located midway from each end of the filament. Although carbiding to near completion at 240° C over periods of about 300 hours produces a preparation containing no appreciable percentage of epsilon iron carbide, very brief periods of carbiding of the order of a minute result in the formation of detectable epsilon iron carbide even at temperatures as high as 325° C. The data indicate that epsilon iron carbide is an intermediate in the formation of chi iron carbide during its formation from carbon monoxide in the gas phase. Attempts to convert cementite to chi iron carbide by cold work increased the Curie point but did not change the X-ray powder diffraction pattern.

Jan 1, 1966

By L. J. E. Hofer

The Bureau of Mines determined rates of adsorption and desorption of methane as a function of particle size and temperature, using coals from the Pocahontas No.3 seam (lvb) from the Bishop mine of western Virginia, and the Pittsburgh seam (hvab) from the Pursglove No. 15 mine of northern West Virginia. For a given coal sample and temperature, the rate curves for adsorption and desorption are essentially the same when expressed on a fractional approach to equilibrium basis. The rates of adsorption and desorption increased eightfold as the particle size was decreased from 6-8 to 270-325 mesh per inch. The adsorption process appears to be diffusion controlled. Rate of sorption processes increased with increasing temperature; however, the amount adsorbed at equilibrium decreased.

Jan 1, 1966

By H. W. Hughes

"The Wasamac Gold Mines mill, situated 10 miles from Rouyn-Noranda on highway 59, commenced milling April 1st 1965 at a rate of 700 tons per day. This has gradually increased to over 1200 tons per day in December. The mill has done up to 1400 tons on occasion.The ore was formed in the Wasa shear zone by means of replacement. The minerals which replaced the original rocks were carbonates, quartz, pyrite, chlorite, gold and silver. Work index varies from 9. 6 on the chlorite to 11. 6 on the quartz. The gold is very finely disseminated throughout the gangue and while associated with the pyrite is not included in the pyrite. Very seldom is gold found or seen in the free state.Test work showed a medium fine grind of 85 to 90 per cent was necessary to achieve a 95.00 per cent extraction. Straight cyanidation time of 30 to 36 hours was indicated. This has been borne out by subsequent mill performance with a grind around 87 per cent minus 200 mesh and extraction ranging from 95 to 96 per cent.When it was decided to bring the Wasamac property into production, the Bicroft Uranium Mines Ltd. crushing and grinding units together with one pebble mill and the pachuca tanks from Dyno Uranium Mines Ltd. were purchased.Wasamac crusher house and mill buildings are of laminated wood construction, covered with 5/ 8th inch plywood and corrugated iron sheeting."

Jan 1, 1966

By Robert S. Warfield

Eight samples of high-volatile bituminous coal, each large enough for a study of its coking properties by the Bureau of Mines, were obtained from a location along the Kukpowruk River, Arctic Northwestern Alaska. Bench scale and pilot plant carbonization studies with several patterns of coal blending were conducted. The data from these tests were compared to data from similar tests on a coking blend used by the Kaiser Steel Corporation at Fontana, Calif. The majority of the samples representing the 20-foot seam was found to have significant coking properties, and produced coke approaching metallurgical quality when blended with selected coking coals. Although oxidation effects were evident in the samples representing upper portions of the seam, it appears that the whole seam could be used.

Jan 1, 1966

By J. W. Town

The Bureau of Mines conducted petrographic classification and flotation studies to determine if acid-grade concentrates could be obtained from individual and composite samples from the Meade Peak member of the Phosphoria Formation, Idaho. The petrographic studies were made to determine the effect of compositional features on concentration of phosphates. The ore grade, ovule size, and clay content were the main features affecting grade and recovery of phosphate. Flotation results on roasted ore with a tall oil emulsion scheme showed that beds containing over 10 percent P2O5 could be beneficiated and composited with the two high-grade beds to produce a composite concentrate containing 31.9 percent 05 at 84.3 percent recovery. Treatment of these intermediate-grade phosphate beds by flotation increased ore reserves over 200 percent and increased the ore-to-waste ratio in the ore zone from 1:5.7 to 1:0.27.

Jan 1, 1966

By J. B. Mitchell

Many of the pre-production and plant startup problems that we regard as inevitable are actually caused by poor organizational methods. Traditional methods of organization can be modified to provide clear definitions of responsibility, continuity and depth of involvement of key personnel in order to overcome these problems.

Jan 1, 1966

By Paul M. Buttermore

As part of a national canvass of water use the Bureau of Mines compiled data on water requirements in the petroleum and natural gas industries for the calendar year 1962, specifically in well drilling, secondary-recovery operations, and natural gas processing plants. Total new water use in the petroleum industry of the United States, excluding refining, was 5.3 billion barrels. Secondary-recovery operations and natural gas processing plants required about 2.5 billion barrels of new water input; each of these requirements was about eight times greater than that for well drilling. Total use, including recirculated water, was 45.3 billion barrels of which 3.4 billion barrels was consumed. The greatest use of recirculated water was for natural gas processing, amounting to 38.2 billion barrels. Projections of total water use show that by 1975, 75.4 billion barrels will be used by the petroleum industry, of which 10.2 billion barrels will be new water. By 1985, the total use requirement will be 92.8 billion barrels, of which 13.1 billion barrels will be new water.

Jan 1, 1966

By Neil Campbell

"The gently-dipping Devonian dolomite beds south of Great Slave lake in northern Canada are nearly every-where concealed by a cover of glacial drift and muskeg. Nevertheless, in 1898 or earlier, four small outcropping areas of dolomite, richly mineralized with lead and zinc sulphides, were discovered. Exploration work performed here up to the end of 1930, included intensive trenching and drilling of the showings, together with mapping and wide-spaced drilling in the surrounding region. This work proved that the discoveries are isolated pockets of mineralization much too small to be commercially valuable by themselves. No evidence of orebodies elsewhere was reported.Meanwhile, mapping by the G.S.C. in the Shield far to the east disclosed major Precambrian faults, some of which can be projected southwesterly (under a cover of Paleozoic sediments) to the vicinity of Pine Point. During the period from 1940 to 1947, consideration was given, by The Consolidated Mining and Smelting Company Ltd., to evidence of a theoretical possibility that, although apparently dormant in Paleozoic times, these faults may have provided a structural control and a source of ore-bearing solutions in some post-Devonian period. From this, it was postulated that the breaks might have created, in the overlying dolomite, a linear array of orebodies concealed by overburden but lying in a belt of considerable length and in a position predictable within practical limits. A program of drilling designed to test and exploit this specific concept was conducted from 1948 to 1955.he drilling within the new, theoretically-defined search area resulted in the discovery of many lead-zinc ore-bodies, none of which was exposed at the surface. Some of these are large and (as indicated by 1965 production records) very rich. They are situated 1 to several miles distant from, and apparently not connected to, the earlier-known surface discoveries. The drilling also disclosed that the ore, which consists of disseminated sphalerite and galena replacements together with colloform sphalerite and coarse galena cavity fillings, occurs mainly at certain stratigraphic horizons within a large, coarsely-recrystallized dolomite barrier reef. Considerable fracturing and folding was found. It has been suggested that reef development was influenced by post-Precambrian tectonic movements associated with the old faults in the basement complex. The ore may have been deposited by solutions moving from distant sources to favourable structural and chemical environments in or related to the reef.In more recent exploration performed in the course of preparing for mining production, the rate of ore discovery within the same general geological context has been greatly accelerated by the use of new geophysical techniques and drilling equipment. Reserves of 21.5 million tons, averaging 4 per cent lead and 7.2 per cent zinc, were reported in 1965, and production from open pits at the rate of approximately 248,000 tons of concentrates per year is in progress"

Jan 1, 1966

By Zoltan F. Oszter

Feeding bulk solids from bins or bunkers sometimes poses a problem to the materials handling engineer. The paper describes, by practical examples, how material flow can be improved on existing installations, and how difficult-to-handle materials can be successfully drawn from storage and fed to fully automated process systems. The examples illustrated are based on actual experience with projects designed for the mining and metallurgical industry. Maintenance costs, where available, are also indicated.

Jan 1, 1966

By H. C. Fuller

A method was devised and developed by the Bureau of Mines for decomposing manganese sulfate at significantly lower temperature than that required by the conventional procedure of using heat alone. This technique, called the partial reduction method, effected decomposition at 700° to 800° C, as compared to 900° 1,000° C normally required. The process consisted of heating, in the absence of oxygen, a mixture of manganese sulfate and a controlled quantity of a reducing agent. The suitability of commercial-type equipment was tested in laboratory-size models of an externally heated rotary kiln, a r bbled muffle-hearth furnace, and a fluidized-bed reactor. The rabbled-hearth furnace gave the best results with the least operating difficulty produced a gas containing more than 80 percent SC and eliminated 96 percent of the sulfur when coal was used as the reductant. Sintering of the powdery decomposition product produced an agglomerate containing, in percent, 63.6 Mn and 0.4 S.

Jan 1, 1966

By Stephen D. Hill

The Bureau of Mines devised and constructed a modified Knudsen effusion apparatus, permitting a constant measure of the weight of effusing vapor, to determine the equilibrium vapor pressure of metal halides at temperatures up to 1,200° K and over the pressure range 10-5 to 10-2 torr. The reliability of the apparatus was established by determining the vapor pressure of potassium chloride. After correcting for partial dimerization of the vapor, data obtained on solid KCl between 750° and 950° K can be expressed by the following equation:

Jan 1, 1966

By Wallace W. Key

This report concerns types, quantities, specifications, and uses of non-metallic minerals as a basis for improving their supply, conservation, and utilization. Supply-demand details concerning mineral fillers, rooting granules, and roofing rock used in asphalt are incorporated in this report, along with highlights on production and sales of rooting, floor tile, and other related asphalt products of California. Comparable data for the United States are included. Although large quantities of commercially prepared mineral fillers are used in asphalt for paving and related applications in other States, addition of commercial fillers for these uses rarely is required in California because of the natural tines available. On the other hand, California manufacturers of asphalt products other than having utilize about 300,000 tons of asbestos, diatomite, limestone, mica, soapstone, and other nonmetallic minerals as filler, mainly for reeling and flooring. Also about 500,000 tons of roofing, granules is produced in California, most of which goes into roofing manufacture in California. In addition. A significantly large and growing tonnage of relatively coarse mineral aggregates Ire used on low-angle, built-up, asphalt roofs to produce in attractive surface and offer protection against the clements. Clearly ill minerals used in asphalt products manufactured in California come from local sources, except asbestos and mica--and there are indications that local deposits of those commodities could be utilized in some use categories.

Jan 1, 1966

By R. F. Abernethy

A modified Unterzaucher method was applied to the direct determination of oxygen in coal. Coal samples were pyrolyzed in a nitrogen atmosphere, and the gaseous oxygen compounds liberated were converted to carbon monoxide by a platinized-carbon catalyst at 9000 C. After passing over heated copper and through a tube containing soda-asbestos and magnesium perchlorate, the purified carbon monoxide was oxidized to carbon dioxide by iodine pentoxide--liberating an equivalent amount of iodine. The iodine was titrated with 0.02 ~ sodium thiosulfate; in a few tests the weight of carbon dioxide produced was determined. Direct oxygen determinations of coal included organic oxygen from the coal substance, plus a small quantity of inorganic oxygen derived principally from carbonate minerals and from combined water of silicates in the mineral matter. The influence of mineral matter on the direct oxygen determination was investigated by testing (1) untreated coal, (2) demineralized coal from which most of the mineral matter except pyrite was removed by treatment with hydrofluoric and hydrochloric acids, and (3) coal samples treated with dilute hydrochloric acid.

Jan 1, 1966

By Charles G. Zink

Anthracite is widely known as a domestic or space heating fuel. The prevailing market ratio of domestic to industrial consumption was about 80 to 20 up until 1950. Since then it has been shifting until now the ratio index is about 50/50, exclusive of overseas export. Despite a declining domestic space heating market, the demand for industrial anthracite remains good. However, as a result of stringent air pollution regulations, there is a renewed interest in this low sulphur coal which cannot smoke under any conditions. Anthracite serves other important industries such as power generating, metallurgical, cement, ceramic, chemical, water sewage and industrial wastes filtration. Anthracite is an excellent natural source of carbon and may be utilized in many processes.

Jan 1, 1966

By Kenneth R. Farley

The Bureau of Mines developed a rapid and accurate flame photometric procedure for determining cesium and rubidium in ores and in products associated with the extractive metallurgy of these elements. The effect of associated ions is neutralized by addition of buffer solution; alkali metal effects are neutralized by parallel analyses made on standard solutions similar in composition to the sample being studied. The overall accuracy of the method is within 2.5 pct of the amount of cesium or rubidium present; the range from 1 to 25 pct is the most accurate.

Jan 1, 1966

By Samuel S. Adams

The Permian Salado Formation of west Texas and southeastern New Mexico is composed of halite and subordinate amounts of anhydrite, clay and potassium and magnesium-bearing evaporite minerals. Aspects of the geochemistry of the Salado Formation have been investigated through studies of the stratigraphy, mineral assemblages, textures and minor element content of the salts. These studies provide information on the origin of the evaporites when combined with data on equilibria in saturated salt solutions. The principal potash ore zone in the district is composed essentially of halite (NaC1) and sylvite (KC1). Data on the color, bromide content, and proportions of halite and sylvite suggest that this simple assemblage is the product of a series of replacements rather than primary precipitation. The bromide content of the salts also indicates that the brine which precipitated the Salado Formation was derived from the dissolution of older evaporites rather than the simple evaporation of sea water.

Jan 1, 1966

By Guy T. Jr. McBride

World food production is not matching the exploding increase in world-population. Since arable land is limited, ways are being sought to increase yields by turning_ to fertilizer. Phosphate, an essential fertilizer ingredient, is undergoing a period of growth unparalleled in history. The United States is at once the world's largest producer of food and of phosphate rock. Both food and fertilizer output in the United States are being enlarged to meet the demands posed by the threatening world food crisis. New phosphate deposits are being developed in Florida and North Carolina to assure the United States' continued preeminence in this vital resource. Large fertilizer complexes are also being constructed with an eye to both domestic and foreign markets. The growth of the U. S. phosphate industry has been characterized by developing technology in the processing and distribution of phosphate raw materials. The trend from low analysis to high analysis materials accompanied by a change from a large number of small fertilizer plants oriented toward the marketplace to a fewer number of large plants located at the raw material source is illustrative. These changes in technology and distribution have also been important factors in the development of new mining areas in Florida, the Western States and North Carolina.

Jan 1, 1966

By J. Handin

Triaxial compression tests with independently applied external confining pressures and internal pore pressures show that the ultimate compressive strengths of representative oil well cements are nearly linear functions of effective pressure — the difference between external and internal pressures on the jacketed cylindrical specimens (to 15,000 psi). The strengths are little affected by the test temperature to 350F (not to be confused with the curing temperature). At an effective pressure of 15,000 psi, strengths are in the rage of 30,000 to 50,000 psi, comparable to those of sedimentary rocks under similar conditions. The cements become very ductile even under low effective pressures; permanent shortenings of 30 per cent or more are attainable without rupture. INTRODUCTION Since the pioneering work of Richart, Brandtzaeg and Brown1 on the failure of cement under combined compressive stresses, it has been recognized that ultimate compressive strength is greatly enhanced by the application of confining pressure. More recently, Mc Henry2 showed that the strength of concrete was a linear function of the effective pressure (the difference between the external confining pressure on a jacketed specimen and the internal fluid pore pressure), at least for a range of 0 to 1,500 psi. The effect of temperature had not been investigated, and no previous systematic triaxial compression testing of naterials used for oilwell cementing seems to have been done. The present work was suggested by the late J. hi. Bugbee3 who stated that "consideration of the common application of high-pressure hydraulic fracturing to the initial completion or recompletion of wells, and the large pressure drawdowns in some producing wells, particularly those in abnormally high-pressure gas-condensate reservoirs, raises the question of what is a suitable cement strength for various completions. The intuitive belief exists that cement strength need be no greater than formation strength. Tests should, however, be conducted at downhole conditions." The ultimate compressive strengths of rocks penetrated by the borehole must rise several fold with increasing depth.4 This marked enhancement of strength is due to the influence of the effective pressure, the total weight per unit area of the overburden less the hydrostatic pore pressure. (The effect of temperature due to the geothermal gradients is relatively small for depths to 30,000 ft.) .A significant comparison of the strengths of rocks and cements at downhole conditions requires knowledge of the confined compressive strengths of cements as well. EXPERIMENTAL PROCEDURES The theory and technique of triaxial compression testing are fully discussed in earlier reports.4-6 Briefly, cylindrical specimens 1-in. long and 0.5-in. in diameter are jacketed in thin copper tubes of negligible strength, placed in the test chamber and subjected to an external confining pressure of kerosene and loaded axially by the piston at a strain rate of 1 per cent per minute. Pore pressures of water (or kerosene) are applied independently through the hollow piston and are maintained constant during the shortening of the specimen, Tests at sensibly 0 pore pressure are arranged so that any free water in the cement can escape to the atmosphere. (If egress of water were denied, pore pressure would rapidly attain the value of the external confining pressure because of reduction of pore space.) The test chamber can be heated for high-temperature experiments. Unless otherwise noted, the cement samples were air dried for about a week. Recorded during a test are pore and confining pressures, shortening and axial differential force (total force less the product of the confining pressure and the area of the piston). True stress-strain curves are constructed by dividing the measured differential force by the actual cross-sectional area of the specimen at a given

Jan 1, 1966

By C. Ortuglio

The Bureau of Mines developed equations to determine the relationship of yields and products obtained from BM-AGA carbonization in 13-and l8-inch-diameter retorts. The developed equations indicate that results of carbonization in l8-inch-diameter retorts can be predicted from results obtained with l3-inch-diameter retorts.

Jan 1, 1966