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By M. H. Stanczyk

The Bureau of Mines made bench-scale laboratory tests on a sample of typical Florida phosphate slime to determine alumina and phosphate extractions obtainable by agitation leaching, by baking and curing, and by a leach-electrolysis scheme. Recovery of mineral values from leached slime pulps by resin-in-pulp ion exchange contact and the reaction of the leached pulps to filtration, flocculation, and settling were also investigated. The best extractions of alumina and phosphate were obtained by (l) agitation leaching with sulfuric, hydrochloric, or nitric acid at an elevated temperature or (2) curing or baking the slime with sulfuric acid. Alumina extractions ranged from 80.8 to 90.0 percent and phosphate extractions ranged from 93.3 to 98.4 percent when the slime was leached at 90° C with sulfuric, hydrochloric, or nitric acids. Baking the slime with sulfuric acid at 200° C for 4 hours yielded an alumina extraction of 92.3 percent and a phosphate extraction of 97.0 percent, whereas curing with sulfuric acid at 100° C for 24 hours gave slightly higher alumina and phosphate extractions. Flocculation and settling properties of the slime were virtually unaffected in all cases. Filter area requirements, although somewhat improved as compared to untreated slime, remained relatively high. The lowest filter area requirement obtained was 44 square feet per ton of dry solids treated per day. Contacting leached slime pulps with ion exchange resins depleted the leach pulps of solubilized values; however, the filtration and settling properties of the barren pulps were unaffected. A leach-electrolysis scheme resulted in some concentration of solubilized phosphorus, but the method showed little promise of being commercially feasible.

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

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 A. W. Deurbrouck

The Bureau of Mines reviewed available data on the effect of crushing high-sulfur coals for the liberation of impurities in the light of increasingly stringent air pollution regulations. The survey, which provided information on Appalachian region coals only, indicated that such important coal- beds as the Upper and Lower Freeport and the Upper Kittanning show significant sulfur reductions when crushed to 14-mesh top size. For many other coalbeds amenability to sulfur liberation by crushing was indicated, although too few samples were available to draw firm conclusions,

Jan 1, 1966

By K. P. Wang

SIGNIFICANT general developments took place in the Far East during 1964, with far-reaching repercussions on the mineral and industrial economies of individual countries and the region as a whole. Japan, during this, "the Year of the Open Door," ushered in the era of industrial maturity, greater independence in economic policy, and expanded technical assistance to less developed countries. Symbolic of its dynamic economic growth is the fact that Japan out-produced the Federal Republic of Germany in steel during 1964 to take over a third-ranking world position. Mainland China, recovering from the "Leap Forward" debacle, made significant gains in industrial output. Mainland Chinese trade with Japan was on the upswing, and discussions were held between the Chinese and the Soviets for possibly resuming Soviet aid in industrial and mineral development. Meanwhile, United States aid to Taiwan was being phased out because of progress achieved. Rapprochement between South Korea and Japan was imminent late in 1964, a factor which may well affect South Korean mineral development. The Indonesian-Malaysian confrontation created economic difficulties in both countries. The war in Viet-Nam seriously disrupted industrial activities, particularly in the south.

Jan 1, 1966

By D. J. Weintritt, R. G. Hughes

Statistics show arz increase in the average depth of wells drilled in recent years. As a corollary to this trend, drilling fluids have been improved in an effort to meet the problems inherent at temperatures approaching 500°F. Of importance are (1) deterioration of mud components and (2) the effect of solids on filtration and rheological properties. High-temperature, stable water-base and oil-bare muds are discussed. Those areas in which differences exist are pointed out. Results are based on data taken from the Fann consistotneter, rheometer and shear-strength measurements, static and dynamic filtration tests, methy-lene blue test for bentonite solids and specific heat measLrrenlents of muds. INTRODUCTION Higher well temperatures go along with the fact that the average depth of wells continues to increase. Recent data by Gardner' lists 137 completions deeper than 15,000 ft for the first half of 1964 with a record second-half total of 167 wells drilling or proposed. In addition, there has been an increase in drilling for steam for power production or mineral recovery. In this application the depths are modest, but the mud may approach the critical pressure and temperature of water. Scearce and Magnon' report drilling mud used at temperatures of about 700°F in the Salton Sea area of California. Most deep wells have been drilled with water-base muds. In recent years, however, there has been a substantial increase in the use of oil-base muds because of technological advances in effective additives. The significance of this development was dealt with in considerable detail by Simpson and his co-workers.3 Additiona1 field data have now been obtained to indicate that oil muds are competitive in control, performance and cost with the best types of water muds for use at high temperaturc. This parallel offer of two very different fluid systems, each offering a similar variability in performance, cost and convenience, has created the need to evaluate the merits of these fluids under specified conditions so that the advantages and disadvantages of each can be weighed in relation to the over-all drilling program. This paper is not intended as a review of all the factors. Rather, it attempts to emphasize: (1) important condltions and facts peculiar to high-temperature drilling muds, (2) that more than one imposed test condition or testing method is necessary to describe the quality of a mud at high temperature and (3) that elaborate experimental precautions are necessary whenever laboratory data are used in selection of a mud for field use. WHAT IS A HIGH-TEMPERATURE DRILLING FLUID? For the purpose of this discussion, a high-temperature drilling fluid is any system so formulated or treated to economically minimize the effects of temperature on the properties of the fluid. Our experience in drilling fluids suggests that these effects become obvious for many mud materials at temperatures of 300F or higher. It is understood that hydrolysis of starches, depoly-merization of certain organic thinners, or irreversible chemical reactions (such as that of clay and lime) can affect filtration, viscosity and shear strength at less than 300F. However, the temperature level is not a serious point and in no way affects the precautions and techniques used in this study. An up-to-date review of the literature on high-temperature drilling fluids and the many variations was treated by Rogers'in 1963. EXPERIMENTAL REQUIREMENTS TESTING EQUIPMENT AND PROCEDURES With the advent of deeper drilling and increased demand for temperature-stable drilling fluids, new testing equipment and laboratory techniques were devised for the evaluation of drilling fluids subjected to elevated temperature and pressure. While the equipment has not been standardized, it is in widespread use. Milligan et al. Qescribe a filtration cell for determining the filtration properties of drilling fluids at temperatures in excess of 300F. They showed the effect of variations in temperature and pressure on oil and water muds filtered in the 300 to 400F range. The dynamic filtration apparatus described by Simpson6 permits the study of the filtration properties to temperatures of 350F for drilling fluids circulated over sandstone cores. Watkins et al.' describe the use of pressure bombs for studying the effect of prolonged periods of elevated temperature upon the gelation or solidification of drilling fluids. Chisholm et a1.' describe the use of a modified cement consistometer adapted for use in drilling fluid evaluations. A similar consistometer is used in this study, although the application and data-recording method have been changed. The consistency of a mud sample is measured by timing the movement of a soft iron bob which is magnetically moved up and down in the sample container.* Changer in the time of travel and the temperature of the mud at that moment are plotted with a two-point Brown Elec-tronik Recorder. A 10-in. chart with a speed of 4-in./hr is used. Fia.- 1 is a generalized internretation of the data ob-

Jan 1, 1966

By C. Bernier

This paper deals with three major problems associated with mining operations during the winter. These are the maintenance of the cooling systems of diesel engines, the high incidence of hydraulic dump failures on packaging machines, and the build-up of frozen fines on wet-ore conveyor belts.

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

Jan 1, 1966

By M. E. Hawkins

This Bureau of Mines report provides information on all of the 329 proved salt domes in the Gulf Coastal States and offshore area of the United States. It includes specific data related to location, depth to the cap rock and to the salt, storage facilities for LPG, and production of salt, sulfur, petroleum, and rock related to or associated with the dome structure in the subject area. Also included is a brief history of the salt, sulfur, and petroleum industries as related to the salt domes. Gulf Coast salt domes were the scene of the first discovery of a large deposit of rock salt in North America, the birthplace of the Frasch sulfur industry, and the location of the first large oil gushers that ushered in the modern liquid fuel age.

Jan 1, 1966

By Eliot J. White

The Bureau of Mines tested cores from 35 wells from 14 oil-producing zones in southern Illinois, southern Indiana, and western Kentucky to determine why rates of water injection were apparently low in some zones. Since these zones contain only minor amounts of clay minerals, it is concluded that permeability reduction results from movement of dislodged silica particles and other material, including the clays, that lines the pores. Both single-phase and two-phase permeability measurements, however, indicated that most samples had only low to moderate water sensitivity, so that permeability reduction due to such particle movement should usually not be of practical significance. The effective permeability to water was considerably lower than the effective permeability to oil during two-phase flow measurements, as is typical of most reservoir rocks. It can be concluded, therefore, that relatively high injection pressures will be required in waterflooding thin zones or zones having low permeabilities.

Jan 1, 1966

By John P. Capp

In recent years limited markets have been developed for fly ash, the dust removed from coal-burning powerplant stacks, but most of it is still dumped in spoils areas at a cost ranging from 20 cents to $1.75 per ton. Aside from this cost, the creation of huge spoils areas can present a considerable aesthetic problem. Since the present annual fly ash output of about 20 million tons will probably reach 30 million by 1970, and because satisfactory disposal areas are becoming more limited, markets for much larger quantities of the waste are needed to keep disposal costs from becoming a significant economic factor in coal-burning powerplant operation. Current stress on air-pollution control and beautification, plus the vital need for good powerplant economy, makes it imperative, therefore, that coal producers and consumers expand markets and develop new applications for fly ash. Markets for established uses can be increased by making a greater effort to sell fly ash. New large tonnage markets for fly ash should be sought via more intensive, coordinated research. The economics of fly ash utilization underscores the vital role that must be played by research. To be competitive with other products, processes for the conversion of fly ash into marketable materials face difficulty in regard to two important economic factors--transportation cost and product utility--the other economic factors are favorable. Raw material costs of fly ash, for example, are quite attractive, and supply is no problem because there are many coal-burning powerplants in operation and many more are planned. Demand for products made from fly ash will grow if their utility is established and a good sales program is initiated. The major problems then are transporta¬tion costs and development of useful products.

Jan 1, 1966

The distribution of tin and iron between slag and metal phases at about 1150°C was studied in pot scale experiments. The distribution coefficient k = (Sn/Fe) In metal X (Fe/Sn) in slag was found to vary from about 300 for metal corresponding to nearly pure tin, to about 100 for metal of about miscibility gap composition (17' 4 per cent Fe). Results conformed reasonably well to a straight line relationship between log k and (l-2NFe), as expected on theoretical grounds, and are consistent with thermodynamic data for the Fe-Sn phase diagram and the reaction Fe + SnO = FeO + Sn.Calculations are presented indicating the feasibility of smelting low-grade tin concentrates in a two-stage counter-current reduction process.

Jan 1, 1966

Jan 1, 1966

By John A. Hansuld

Geochemical dispersion of metals under various environmental conditions is discussed within the frame-work of Eh (oxidation potential) and pH (acidity). In general, two aspects are considered -(1) the oxidation of certain primary sulphides in the outcrop or sub-outcrop environment, and (2) the movement of metals in different dispersion media. Practical applications of each are illustrated by means of exploration case histories representing environmental conditions in the Canadian Shield, the southwestern United States and the Caribbean.

Jan 1, 1966

By C. R. Johnson, R. A. Greenkorn, R. E. Haring

Three confined five-spot miscible displacements at unity, favorable, and unfavorable mobility ratios were conducted in a shallow, water-saturated sandstone of Pennsylvan-ian age near Chandler, Okla. These studies, plus associated laboratory experiments, were designed to measure miscible displacement performance in a controlled natural system, using known scaling criteria to develop an approach to modeling the heterogeneous field system. We have concluded from these studies that: (I) displacement efficiency in the field is a pronounced function of mobility ratio, indicating that miscible fingering observed in simple laboratory models occurs in the field: (2) field displacements can be quantitatively predicted by scaled laboratory models if the degree and location of field permeability variations are preserved in the models: and (3) arbitrary simplifications of heterogeneity will not necessarily predict observed displacement efficiency, and the simpler the model, the more optimistic the prediction. INTRODUCTION Many processes to achieve miscible displacement of reservoir oil by injected fluids have been conceived and field tested by the oil industry. Among the better known are high-pressure gas, enriched gas, and LPG banks. The simplest form of miscible displacement—one fluid miscibly displacing another fluid of different viscosity but the same density—has been studied extensively in homogeneous laboratory models. Observations of unstable fingering have been made which explain the significant decrease in displacement efficiency as the mobility ratio (ratio of displacing fluid mobility to displaced fluid mobility) increases. General industry experience with field tests of miscible displacement projects, mostly LPG banks, has been premature solvent breakthrough and lower than predicted production rate increases. These results have been attributed to either unstable fingering, unusual or unexpected permeability stratification, or both. Miscible displacement data in a controlled natural system have never been reported, however. Also, it has not been shown that properly designed and constructed laboratory models quantitatively predict field-scale behavior. The purpose of the combined field and laboratory ex- periments reported in this paper is twofold. The first was to measure miscible displacement performance at different mobility ratios in natural rock approaching field size under precise, controlled conditions. The second purpose was to utilize known scaling criteria plus several approaches to heterogeneity to model the field. Comparison of model and actual field results should then determine whether or not the laboratory phenomena (manifested by miscible displacement efficiency) are exhibited in large, natural rock systems. We carried out our program by first locating a shallow, water-saturated reservoir whose rock properties were representative of oil-bearing reservoirs. Detailed reservoir description by core analysis and interference testing showed the field site to be heterogeneous. A sequence of controlled, aqueous-phase miscible displacements was conducted at unity, favorable and unfavorable mobility ratios. A central, confined pattern was used to obtain the displacement data. A laboratory program using sand-packed models was conducted to determine the modeling criteria necessary to simulate field behavior of miscible displacement in a heterogeneous system. SCALING THEORY The detailed derivations and descriptions of the scaling laws that apply to laboratory models of reservoirs are adequately described elsewhere, so the following discussion will be restricted to facets of importance in this study. For a displacement in which one liquid miscibly displaces another, the following dimensionless groups are required to have the same numerical value in the model as in the field: The model also must be geometrically similar to the field, be spatially oriented the same as the field (same dip angle), and have the same initial and boundary conditions as the field (same initial fluid saturations and same injection-production well arrangement). When these conditions are satisfied, the theory predicts that at dny dimensionless time (pore volumes of produced fluids) the dimen-sionless flow potential and dimensionless fluid concentrations will be identical at all dimensionless spatial locations within the model and the field. If this prediction is correct, then the local dimensionless velocities must be identical, thus the instantaneous fraction of displaced fluid produced and the cumulative recovery expressed as fraction of original fluids in place must be identical at all dimensionless times. The theory outlined above has been obtained by either dimensional analysis or inspectional analysis of differential

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