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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 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

By F. Dubuc

"The Adams Mine of Jones & Laughlin Steel Corporation is situated on the Boston Township iron range near Kirkland Lake, Ontario. Eight different orebodies have been outlined, with a total open-pit crude tonnage of. about 100,000,000 tons or the equivalent of 30,000,000 tons of concentrate. The ore consists of fine-grained, well-bedded Early Precambrian iron-formation composed essentially of alternating layers of chert and magnetite. Grade averages about 22 per cent magnetic Fe.The iron range varies in width from 3,000 to 4,000 feet and is made up of several horizons of iron-formation, cherty ""quartzite"" and volcanic rocks. The latter consist mostly of basic lava flows and minor amounts of tuff. Dips are rarely Jess than 50 degrees, and the range is believed to represent an overturned limb of a major synclinal structure. Dykes of syenite and lam prophyre, along with local younger diabase, intrude the rocks of the iron range."

Jan 1, 1966

By R. H. Schutz

TO ASSIST users in the selection of reliable and satisfactory respiratory protective devices, the Bureau of Mines bas established five schedules of minimum performance requirements for the approval of respirators. The current revisions of these schedules3 include 13D for self-contained breathing apparatus, 141F for gas masks, 19B and the amendments to 19B for supplied- air respirators, 21B for dust, fume, and mist respirators, and 23B for chemical cartridge respirators. Copies of these schedules may be obtained from the Bureau of Mines, Publications Distribution Section, 4800 Forbes Avenue, Pittsburgh, Pa., 15213. Approval tests on respirators are performed only at the request of the manufacturer4 of the respirator and at his expense. If the device meets the approval requirements, a certificate of approval is granted on the complete respirator. This certificate states that as long as the respirator is manufactured as originally approved, or in accordance with any changes covered by an extension of the original approval, the manufacturer may advertise and sell his respirator as being approved by the Bureau of Mines. Many industries and regulatory agencies require that respirators approved by the Bureau of Mines he used where respiratory protection is needed. The Bureau of Mines, however, has no regulatory power over the use of the respirators that it approves. It acts as an impartial testing agency to insure the availability of suitable and safe respirators.

Jan 1, 1966

By Gerald W. Elger

This report describes development of the fusion-leach crystallization precipitation process for producing a hafnium content feed material for hafnium-zirconium separation plants. Mixtures of zircon, potassium silicofluoride, and potassium carbonate (or potassium chloride) were fused to prepare soluble potassium zirconium hexafluoride-potassium hafnium hexafluoride salts. High extraction of these salts was obtained by countercurrent leaching the fused material in dilute hydrofluoric acid. About one-half of the hafnium was recovered in hafnium-enriched mother liquor by cooling clarified lead: liquor to crystallize most of the zirconium salt. Additional hafnium was recovered from the primary crystals in a multiple dissolution-recrystallization step. Hafnium-enriched oxides having a hafnium-zirconium ratio of more than three times that of zircon were precipitated from the combined mother liquors. The hafnium and zirconium recoveries in the precipitate were 83 and 24 percent, respectively. About 71 percent of the zirconium and the remainder of the hafnium were recovered in potassium zirconium hexafluoride crystals of low-hafnium content.

Jan 1, 1966

By K. P. Fournier

This report describes work on the problem of predicting oil recovery from a reservoir into which water is injected at a temperature higher than the reservoir temperature, taking into account effects of vis cosity-ratio reduction, heat loss and thermal expansion. It includes the derivation of the equations involved, the finite difference equations used to solve the partial differential equation which models the system, and the results obtained using the IBM 1620 and 7090-1401 computers. Figures and tables show present results of this study of recovery as a function of reservoir thickness and injection rate. For a possible reservoir hot water flood in which 1,000 BWPD at 250F are injected, an additional 5 per cent recovery of oil in place in a swept 1,000-ft-radius reservoir is predicted after injection of one pore volume of water. INTRODUCTION The problem of predicting oil recovery from the injection of hot water has been discussed by several researchers. l-6,19 In no case has the problem of predicting heat losses been rigorously incorporated into the recovery and displacement calculation problem. Willman et al. describe an approximate method of such treatment. 1 The calculation of heat losses in a reservoir and the corresponding temperature distribution while injecting a hot fluid has been attempted by several authors.7'8 In this report a method is presented to numerically predict the oil displacement by hot water in a radial system, taking into account the heat losses to adjacent strata, changes in viscosity ratio with temperature and the thermal-expansion effect for both oil and water. DERIVATION OF BASIC EQUATIONS We start with the familiar Buckley-Leverettg equation for a radial system:* This is sometimes referred to as the Lagrangian form of the displacement equation. If the injection water is at some temperature Ti which is above reservoir temperature TR, then lw, the flowing fraction which is water, is a function of both water saturation and fluid temperature at any given time and position in the reservoir. The temperature dependence of lw results from the temperature dependence of the viscosity ratio µo/µm of which lw is a function. Thus:

Jan 1, 1966

By Kenneth H. Johnston

This publication describes a thermal-recovery project and two waterflood projects in Carter, Garvin, and Stephens Counties, Okla., that will be visited during the 1966 annual tour by the Bureau of Mines in cooperation with the Kansas-Oklahoma Waterflood Association. Among the unique features of the projects arc (1) the movement of heavy (15° to 28° API gravity) crude oil through the reservoir and into the well bore with energy furnished by burning a portion of the crude oil therein; (2) the use of an inverted nine-spot pattern with dually completed injection wells, to produce oil from deep (8,200 to 10,200 feet) reservoirs; and (3) the flooding of five sand lenses separately by using controlled water injections through multizone completed injection wells. Discussion of the individual projects includes information on their early history, method of completing and operating wells, source and treatment of injection fluids, oil production decline curves, and the results obtained from the development.

Jan 1, 1966

By Lars Osen

The Bureau of Mines investigated (1) the effect of torsion on yield and ultimate strengths of bolts when the torsion is applied first and tensile load is applied independently of torsion and (2) various methods of increasing the tension-torque ratio and/or narrowing the data spread of the tension-torque relationship. A special torsional attachment was fabricated to attach to a universal testing machine to independently subject rock bolts to combined tensile and torsional loads. It was found that initially installed torsion is nullified during tensile loading and the tensile yield and ultimate strengths are not significantly reduced. Lubricating various components of a bolt assembly or using hardened washers will improve the tension-torque relationship during conventional installation; however, the torsional load is not nullified during this type of loading. Hence, a bolt is subjected to a combined stress throughout the loading cycle; the yield point will thus be lowered compared with the pure tensile yield if care is not taken during installation to stay below the torsional yield.

Jan 1, 1966

By E. S. Shedd

The Bureau of Mines investigated electrowinning and tapping lanthanum metal from lanthanum oxide in a fluoride bath. The electrolyte was composed of LaF3, BaF2, and LiF. Metal containing 0.2 percent impurities was produced at a rate of over 2 pounds per hour. Principal impurities were carbon, aluminum, and silicon. Low-carbon metal was produced by continually discharging the carbon oxide gases and maintaining 0.1-atmosphere pressure. Anode reactions and cell design were found to be important factors in cell operation. Both frozen electrolyte skulls and tungsten metal crucibles proved satisfactory for collecting the metal and did not react with the molten lanthanum.

Jan 1, 1966

By William E. Young

There are many large rhodunite-bearing veins containing manganese in the Eureka-Animas Forks area of the San Juan Mountains in Colorado. The Sunnyside vein is the largest known vein in the area. As observed on the surface, the vein is mineralized over 8,000 feet and attains a maximum width of 200 feet. The average width of the vein and its branches and ramifications is 58 feet in the area that was mapped in detail. The weighted-average analysis of surface and underground samples from the northeastern extension of the Sunnyside vein is 8 percent manganese. Most other known veins in the area have a similar manganese content. The Hidden Treasure vein lies southeast of the Sunnyside-No Name-Mastadon vein. The weighted average of the analyses of surface and underground samples from this vein is 13 percent manganese. Exposures of the Scotia-Silver Chord vein are visible over a strike length of 4,000 feet on Treasure Mountain. Diamond-drill holes show that the vein contains 10 percent or more manganese to a depth of 400 feet. The vein has an average width of 28 feet. The Independence vein is exposed on the surface for a distance of 600 feet and has an average width of 6 feet. Three cut samples taken across the vein had an average content of 20.7 percent manganese. Sampling of the outcrops of eight veins in the Placer Gulch area also indicates manganese. Numerous other veins cropping out in the surrounding area are similar to the outcrop of the. Sunnyside vein system mineralogically and are worth investigating.

Jan 1, 1966

By Albert W. Deurbrouck

The preparation characteristics of the coals of Buchanan County, Va., are described in this Bureau of Mines report. Twenty-one samples ,,,ere collected from 9 coalbeds in the county. Of these samples 13 were of metallurgical quality as received, and 8 required some upgrading to provide acceptable products. In general, the coals were of low to medium ash and sulfur content, and ranked as medium-to high-volatile bituminous. In 1963, production in the county was in excess of 13 million tons, of which 2.2 million tons were mechanically cleaned.

Jan 1, 1966

By W. L. Acherman

Molybdenum, tungsten, and vanadium were found by the Bureau of Mines to possess generally superior chemical and galvanic corrosion properties in many aqueous corrosive media at temperatures up to the boiling point. The corrosion resistance of vanadium in certain solutions was further improved by alloying it with such metals as columbium, tantalum, and titanium. was susceptible to a type of crevice corrosion in mercuric chloride solutions, but no other instances of crevice corrosion were encountered. With few exceptions, molybdenum, tungsten, and vanadium were not adversely affected when coupled with dissimilar metals in galvanic corrosion experiments; in some cases one or both members of a couple were protected by contact. When exposed to aqueous ammonia spray at 60° C, all three metals were attacked, but they were moderately resistant in spray environments of substitute ocean water and ammonium dihydrogen phosphate.

Jan 1, 1966

By J. van Lookeren

In the case of a reservoir where the oil underlies a large gas cap and overlies bottom water, production can be inzproved considerably if wells are perforated below the water-oil contact rather than opposite the oil-bearing section. The theoretical arguments for this improvement, which in some cases may be tenfold, are supported by experimental evidence. INTRODUCTION Reservoirs frequently consist of one sand body containing an oil layer underlying a thick, gas-bearing section and overlying bottom water (Fig. 1). Wells in such reservoirs are customarily opened up opposite the oil-bearing interval or, rather, opposite the lower part of this interval (Fig. 2). More often than not, it is inefficient or prohibited to blow off large quantities of gas with the oil. This im-psses a severe limitation on the drawdown, which results in low oil-production rates. Because of the small difference in specific gravity between oil and water, the latter will easily cone upwards, so that the production of water together with the oil is not prevented by this completion method. In such a situation wells should be opened deeper, in the originally water-bearing zone. The gas can be shut off by not perforating over the upper part of the interval (Fig. 3) or by a tubing hung close to the bottom of the interval (Fig. 4). Initially much water will be produced, but when steady-state conditions have been established (as depicted in Figs. 3 and 4) larger drawdowns are permissible than in a conventionally completed well, and correspondingly higher oil-production rates will result. Water cuts are only slightly higher because of the small effect of gravity on the water-oil flow distribution. CALCULATIONS The ratio of improvement has been estimated by means of approximate calculations. The completion depicted in Fig. 4 is the most convenient basis for these calculations. By postulating that vertical flow gradients can be disregarded, the Appendix shows that the well-known Dupuit formula can be obtained except for some complication due to the presence of two fluids rather than one. The Appendix makes the reasonable assumption that, for suitable boundary conditions, the oil layer occupies a constant fraction of the total fluid height throughout the reservoir. The oil- and water-production rates can thus be related to the liquid levels in the borehole as follows:

Jan 1, 1966

By C. W. Schultz

The vapor pressure of manganese in equilibrium with a series of liquid iron-manganese alloys was determined by the carrier gas method over a broad range of alloy composition. From these data the activities of manganese in the iron-manganese system were calculated. The system appears to be ideal.

Jan 1, 1966

By Foster Fraas

A separator for minerals of low magnetic susceptibility and fine particle size in a water suspension is described. A ring-shaped matrix of ferromagnetic fragments rotating so as to pass successively through magnetic-field and field-free regions provides for the separation. Application is illustrated in the separation of hematite and ilmenite from quartz.

Jan 1, 1966

By Jr. Koch

Statistical methods applied at the Bureau of Mines Denver Mining Research Center to data from metallic ore bodies were used to evaluate lignite reserves from core data and to predict the extent of lignite horizons in some Texas lignite beds. Six lignite seam units were studied using data from 361 drill holes. The data indicate a total of 214.2 million tons of lignite in the area examined, and probable reserves of 113 million tons in an area 2,000 feet beyond the limits established by the drill holes. It was demonstrated that lignite reserves present in lenticular beds could be reliably determined by statistical techniques, and that core drilling could be optimized to maximum information with minimum drill holes. The technique described is applicable to other coal beds.

Jan 1, 1966

By Jr. Jacobson

Thermal reactions of l-methylpyrrole, l-butylpyrrole, and l-isopropyl-pyrrole were investigated by a flow method in the temperature range of 4500 to 5750 C. Those of I-butylpyrrole and l-isopropylpyrrole were also investigated in the 3400 to 4000 C range in a static system. The I-substituted pyrroles isomerize by an irreversible reaction to 2-substituted pyrroles. A reversible isomerization reaction shifted the alkyl group from the 2-to the 3-position on the pyrrole ring. All of the isomerization reactions are homogeneous, unimolecular, nonchain, first-order reactions having similar mechanisms and transition states. There is decomposition and cleavage of the longer alkyl side chain when it is in either the 2-or 3-position giving, as products, pyrrole, 2-and 3-methylpyrrole, 2-and 3-ethylpyrrole, pyridines, and hydrocarbons. The decomposition reactions appear to be by free-radical mechanisms. Pyridine homologs are formed by the expansion of the alkylpyrrole: butylpyrrole produces pyridine, and isopropylpyrrole produces 3-methylpyridine. Approximate Arrhenius equations are given for the formation of the decomposition products.

Jan 1, 1966

By Albert F. Baker

Techniques were developed and circuitry was assembled for measuring the total and volume resistances to the flow of electric current through solid specimens of anthracite. The two-, three-, and four-terminal test methods demonstrated the extreme sensitivity of resistivity to differences in anthracite characteristics and showed response to changes resulting from variations in structure, temperature, and moisture content.

Jan 1, 1966

By Jr. Sharkey

The Bureau of Mines investigated gases from flash and laser irradiation of Pittsburgh seam (hvab) coal to determine the action of high temperatures on coal. Temperatures in excess of l,000° C were reached with both types of irradiation. Craters about 300 microns in diameter were produced in the coal with millisecond pulses from the laser unit rated at 1.7 joules' output. Gaseous products from laser and flash irradiations in vacuum contained 21 and 8 percent acetylene, respectively. Diacetylene, vinylacetylene, and other products to molecular weight 130 were indicated in the mass spectrum of the gas from the laser study. Single experiments were also conducted in which the laser energy, particle size of the coal, and atmosphere were varied. The results indicated that the distributions of products obtained from the flash and laser irradiations of coal were different from that produced in high-temperature carbonization.

Jan 1, 1966