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By G. D. Jermain

The Bureau of Mines investigated the Gypsum-Camel deposit on Iyoukeen Cove Chichagof Island, Southeastern Alaska, from April 21 to August 26, 1948, as A part of the United States Department of the Interior program for developing an Alaskan construction industry. As gypsum is one of the components necessary for the manufacture of cement and one of the raw materials for plaster and plaster-board products, it is desirable to locate and develop a readily accessible deposit of gypsum in Alaska. In 1928, B. D. Stewart of the Territorial Department of Mines surveyed the gypsum deposits at Iyoukeen Cove, and during the summer of 1946 George M. Flint, Jr., and Edward H. Cobb of the Federal Geological Survey examined and mapped the old workings at Gypsum Creek and the prospect at Iyoukeen Cove. Both the Territorial Department of Mines and the Federal Geological Survey recommended the Gypsum-Camel prospect as warranting a diamond-drilling program by the Bureau of Mines. The Bureau of Mines project consisted of cleaning out and sampling, the old underground workings and diamond drilling from the surface to ascertain the lateral extensions of the deposit.

Jan 1, 1952

By W. A. Young

Vermiculite deposits on the. Platt ranch, 12 miles southeast of Encampment Carbon County, Wyo., were investigated by the Bureau of Mines early in 1949. Major activity was centered on property held under lease by the Mikolite Mining & Development Co. (figs. 1 and 2). Vermiculite occurs in masses and lenses of varying size and as disseminations in altered hornblende diorite. Alteration of the host rock probably resulted from the proximity of dikes and irregular masses of pegmatite. Investigation of the Mikolite property consisted of surface trenching, diamond drilling, and sampling. Four trenches totaling 5,401 linear feet were excavated with a bulldozer and Diesel power shovel. Three diamond-drill holes totaling 600 feet were drilled from the surface to determine the character of mineralization at depth. Eighty-one bulk samples were obtained from the trenches, and 130 sludge samples were collected from the drill holes. Samples were analyzed, and ore-dressing tests were made in the Bureau of Mines laboratories at Salt Lake City.

Jan 1, 1952

By F. A. Rutledge

The Batesville district in north central Arkansas is one of the important sources of manganese ore and ferruginous manganese ore in the United States, with a history of production dating back to 1849. From studies by the Federal Geological Survey, it was recognized that the district probably still contains substantial reserves of low-grade ore. It was natural, therefore, that the deposits in this area should be among the first investigated by the Bureau of Mines under the Strategic Materials Act of June 1939, by which the Bureau was authorized to explore domestic deposits of strategic minerals, at that time designated as those of antimony, chromium, manganese, mercury, nickel, tin, and tungsten. The field work of the Bureau of Mines in the Batesville district was done in two distinct phases. Under project 308, active from August 1940 to June 1941, carbonate-oxide ores were investigated at five separate areas in which 100 trenches, test pits, shafts, and edits aggregating 4,364 linear feet were excavated and 839 samples were taken and assayed. Under project 323, in progress from February 1941 to January 1942, wad deposits were explored at 10 separate areas by 408 prospect shafts, churn-drill holes, and bucket-drill holes aggregating 23,680 linear feet from which 285 samples were taken and assayed. Processes for beneficiating the wad ores were investigated at ore-testing laboratories of the Bureau of Mines.

Jan 1, 1952

By John H. Soule

The Torpedo Copper mine in the Organ Mining District, Dona Ana County, N. Mex., was discovered In 1899. Production was begun immediately and continued until 1907. Since 1907 very little ore has been produced, although Many individuals and companies have been interested in the property at one time or another. Approximately 6,621 feet of diamond-core had been completed on the property before 1949. The results from some of this drilling were unsatisfactory because of the poor core recovery. In addition to its investigation of the Torpedo ore deposits, attention was given by the Bureau of Mines to obtaining better core recovery through the use of special equipment and techniques. This project was begun October 3, 1949, and was completed April 30, 1950. Four diamond-drill holes totaling 2,140.5 feet, which includes 18.2 feet of overlap in a deflected hole, were drilled. All drilling was done with a Government-owned hydraulic-feed drill with some special rods and core barrels, in addition to the usual equipment. The over-all core recovery was 89.5 percent. Omitting the drilling in overburden where little or no core was desired, the recovery was 94.6 percent. Core recovery in the ore zones averaged 95.2 percent. This paper describes the location, the general features of the area, the geology, the Bureau of Mines procedures, and the results attained by these procedures.

Jan 1, 1952

By Jr. Sillers

To prove to .the satisfaction of all concerned that electrolytic manganese from our low-grade domestic ores could be substituted satisfactorily for ferro-manganese made from high-grade foreign fires, an extensive series of tests was conducted in cooperation with industry, in which electrolytic manganese pro-duced by, the Bureau of Mines at its Boulder City, Nev., Station was substituted for the ordinary ferro grades in the production of ferrous and nonferrous metals and alloys and welding-rod coatings. Over 1,200,000 pounds of manganese was given out for this purpose. The objectives of the tests were accomplished, and for some purposes electrolytic manganese was shown to be superior to other grades because of its high purity. The only serious objection that can be raised against electrolytic manganese is its price, which puts it out of reach for most purposes. Even if the price were to be lowered to a point where it would be in line with ferro grades, it is questionable whether electrolytic manganese from domestic ores could supply more than a small part of the needs of American industry because of the large volume of domestic ore that would have to be processed to supply a satisfactory feed for the electrolytic process. Thus, although electrolytic manganese is highly desirable from a metallurgical standpoint, it could not be expected to substitute for more than a fraction of our domestic manganese requirements.

Jan 1, 1952

By BUREAU OF MINES

This report is submitted in accordance with the provisions or une Synthetic Liquid Fuels Act of April 5, 1944 (30 U.S.C. 321-325, as amended), which require that: "The Secretary of the Interior shall render to Congress on or before the first day of January of each year a report on all operations under this Act." Owing to the broad scope of the content and the diversity of interests represented, the Annual Report for 1951 has been divided into two separate publications. Each has been published by the Bureau of Mines as a Report of Investigations, and the respective titles follow: Oil from Coal. R. I. 4865, Part I - R. I. 4866, Part II - Oil from Oil Shale. Identical in each report, the introduction summarizes research progress made in 1951 under the entire Synthetic Liquid Fuels program. A free copy of these publications may be obtained by a written request to the Bureau of Mines, Publications Distribution Section, 4800 Forbes Street, Pittsburgh 13, Pa. The R. I. number and title of the publication desired should be indicated.

Jul 1, 1952

By A. L. Engel

This report is a compilation of results of preliminary tests on scheelite (tungsten) ores and tailings. These investigations were made to assist in establishing satisfactory treatment methods for small-scale concentrator operations, or to indicate a. method for conserving previously lost mineral values in old tailings, if possible. A discussion of test procedures is included, as it was felt that this would add to understanding the results reported under the several projects. The treatment of scheelite ores has become more or less standardized. Important differences occur in textures of ores from various mining districts. However, and this must be considered when planning ore-dressing operations. In most of the present investigations, only a limited amount of work was done, usually just enough to answer a specific question in regard to a particular ore or concerning local conditions. Two methods of treatment included gravity concentration, magnetic separation, and flotation.

Jan 1, 1952

By G. L. Humphrey

Although thermodynamic data for ferrous oxide are among the most important in extractive metallurgy, adequate values have not been available until quite recently. The older data suffered not only from the usual experimental difficulties but especially from lack of the knowledge that ferrous oxide of stoichiometrical composition does not exist as a single, thermodynamically stable crystalline phase under any circumstances. This paper reports new experimental data on the heat of formation of ferrous oxide by two methods (combustion calorimetry and solution calorimetry), employing material of unequivocal composition. The results are compared with values obtained from data for the hydrogen reduction, carbon monoxide reduction, and disproportionation reactions of ferrous oxide, and a best value is selected. A table of heat and free energy of formation values of ferrous oxide to 2,000°K is given. These values are combined with available data for water, carbon monoxide, and carbon dioxide to obtain theoretical heats and free energies of reduction corresponding to the selected heat of formation. Hydrogen and carbon monoxide reduction equilibria are compared, and the differences in trend with temperature and the percentage utilization of the reductants are considered.

Jan 1, 1952

By Arnold B. Hubbard

This report describes a method of concentrating the insoluble organic material (kerogen) in a rich Colorado oil shale without any apparent alteration of its original chemical form. The method involved treating finely pulverized shale with dilute acetic acid at room temperature to remove the carbonates, which act as a cementing agent for the shale, and cause the shale particles to partly disintegrate into the organic and inorganic components. The acid-treated shale then was centrifuged in different liquid mediums ranging from 1.4 to 1.15 gravity to effect a mechanical separation. From a Colorado oil shale containing 48.0 percent ash, kerogen concentrates containing 43.3 to 8.7 percent ash were obtained. The carbon:hydrogen ratios of the kerogen in the original shale and the different concentrates were essentially the same. The oil:kerogen ratios calculated from Fischer assays of the above samples were essentially the same, regardless of the organic or inorganic contents. This was also true of the assay water:kerogen ratios of the same samples. These data indicate that no significant change occurred in the kerogen during the concentration process.

Jan 1, 1952

By W. E. Wells

This report describes experimental investigations made in the batchwise retorting of Colorado oil shale. Three heat-carrying mediums were used -hot shale gas, superheated steam, and hot flue gas. Using hot Shale gas for retorting, the several variables studied were retort-inlet-gas temperature, gas velocity through the shale bed, shale particle size, and grade of shale. In studying the effect of any one of these variables on oil yield, as and operability, the other variables were maintained essentially constant. Oil yields decreased with increasing in-let-gas temperature and increasing shale-particle size, and oil yield increased with increasing grade of Shale up to 50 gallons of oil per ton of shale, beyond which the process was inoperable because of swelling and caking of the shale during retorting. Changes in gas velocity had little effect on oil yield. Gas yield increased with increasing inlet-gas temperature, gas velocity, particle size, and shale grade. Oil yields of 100 percent of Fischer assay and from 1,600 to 1,800 cubic feet of 300-B.t.u. gas per ton of shale were obtained. Two runs only were made using superheated steam. Oil yields averaged 97 percent of Fischer assay, and gas yields averaged 4,00o cubic feet per ton of shale. Retorting with a hot flue gas produced from combustion in the shale bed, as in the N-T-U process, gave excellent yields using closely sized shale with recycling of flue gas. An excess of fine shale in the charge resulted in channeling and low oil yields. Using no recycle gas, good yields were obtained that tended to decrease with increasing air rate, and the retorting rate increased with increasing air rate over the range studied. Coking was not found serious with 30-gallon shale at the air rates used.

Jan 1, 1952

By John Nagy

To facilitate increase in the rate of coal production the Bureau of Mines conducted a study several years ago, on the basis of which the allowable charge limit for permissible explosives in single-hole blasting was raised from 1.5 to 3.0 pounds. Further demands for accelerated production led to consideration of multiple blasting in coal, a practice that is deemed hazardous and is not permitted by most States in this country. In multiple blasting, 10 to 20 pounds of explosive or more may be detonated in a coal face within a fraction of a second, which might result in blown-out or blown-through shots with possible ignition of gas or coal dust. As experimental evidence was lacking, in January 1949 an investigation was undertaken in the Experimental coal mine at Bruceton, Pa., principally to study and compare with single blasting the condi-tions under which simultaneous multiple blasting and particularly multiple short-delay blasting may be practiced without danger of igniting gas or coal dust in mines. The first report on this subject was presented at the last international conference of mine safety research. Since that time numerous additional experiments have been made; because of other pressing problems the work has been brought temporarily at least to a conclusion. This paper is the second report on the problem. It does not contain a detailed description of all test conditions and test arrangements, many of which were described 2 years ago in part 1 (now available as Report of Investigations 4868), but the conclusions are based on the entire study. A more complete review, which will incorporate data from the entire investigation, is being prepared as a Bureau of Mines bulletin. Up to the present time, short-delay blasting of coal in commercial mines has been introduced only experimentally in Washington and in a few mines elsewhere. If the system is adopted more generally, new problems may arise, and the study may have to be reopened.

Jan 1, 1952

By H. C. Fuller

This paper discusses 105 production runs at Boulder City, Nev., in which titanium metal was made in 200-pound batches. It describes the equipment and techniques used in preparing raw material, the reduction process, and the removal of the reaction mass from the reaction vessel. Also, some data on man-hour requirements are presented. The main emphasis was on producing ductile-grade titanium and developing a standard procedure for obtaining a consistently pure product. Some departures from techniques used before were found to be desirable. The most important of these was the use of a sealed room with a controlled dry atmosphere in which the reaction vessel was opened and the reaction mass removed. This minimized the moisture taken up by the magnesium chloride in the reaction mass, and it could be purified successfully by vacuum distillation. Using the dry room also made it possible to leave al-inch shell of the reaction material on the walls of the vessel, which lowered the iron contamination and eliminated the labor and time-consuming job of cleaning the vessel after each reduction. Another change was lowering of the temperature during reduction to 750° C. instead of 850° C. This was found to give good results more consistently. The first poke to break the crust during reduction was eliminated, as it was found to be unnecessary and only added more work and was another possible way of introducing air. A rotating feed arm was installed in the reaction vessel to distribute the titanium tetrachloride over a larger area and, thus, prevent local overheating. The process, conducted in a batchwise manner as described and followed by good purification and fusion, produces a metal adequate in quality for nearly all purposes.

Jan 1, 1952

By D. W. Frommer, M. M. Fine

"INTRODUCTION Laboratory mineral-dressing investigations covered by this report show that ores from Montgomery County, Ark., and Morgan County, Mo., are potential sources of barite and zinc. Fine grinding and froth flotation yielded drilling-grade barite from the former and chemical-grade barite and zinc concentrates from the latter.Samples from these deposits were subjected to a laboratory investigation to develop an economic and feasible treatment. The Arkansas ore, submitted by the Husky Refining Co., consisted of an intimate mixture of the economic mineral and quartz. Fine grinding and fatty acid flotation were utilized to effect a good recovery of a drilling-grade product. The other was a zinc-barite ore submitted by the Rocky Ford Mining Co., Stover, Mo. There was no problem in the recovery of zinc (most of which occurred as sphalerite), but the recovery of barite by flotation was complicated by the presence of gangue carbonates. Ultimately, an excellent recovery of barite was achieved with a relatively new type of flotation promoter, petroleum sulfonate.In recent years, barite has become one of the major industrial minerals as an essential ingredient in heavy drilling fluids, pigments, and chemicals. New sources of this important commodity are always interesting; thus, it is the purpose of this report to present information that may permit commercial exploitation of two deposits not in production."

May 1, 1952

By Claude W. Sill

In the usual volumetric determination of uranium, the solution containing uranium is reduced in a Jones reductor, yielding a mixture of trivalent and tetravalent uranium; the trivalent uranium is oxidized to the tetravalent state by bubbling a stream of air through the solution. The resulting solution of. Tetravalent uranium is titrated with a standard oxidant, generally sulfatoceric acid, dichromate, or permanganate; It seemed likely that the, same general procedure could be used in determining semimicro quantities of uranium if the conditions affecting the variables involved were understood more clearly than at present. In the method described below, the use of ferric sulfate to oxidize tetravalent uranium allows the titration to be made at room temperature in an essentially colorless solution with sulfatoceric acid. The latter oxidant its turn permits the use of the very stable indicator, ferroin, with its sharp color.., change and exactly reproducible blanks. Solutions of uranyl sulfate were prepared by diluting a stock solution that had been standardized gravimetrically according to the method of Lundell and Knowles (8).3/ Solutions of sulfatoceric acid were prepared according to the directions of G. F. Smith (12) and were standardized against arsenic trioxide in the presence of osmic acid according to the directions of Gleu. The cerium solutions were stored in 18-liter carboys fitted with siphon arrangements so that the bottles did not need to be opened and protected from light in a dark cupboard. Under these conditions, even the 0.01 N solution changed by less than 1 part per thousand over a period of about 6 months.

Jan 1, 1952

By Heber E. Peterson, Sill. Claude W.

"INTRODUCTION In the usual volumetric determination of uranium, the solution containing uranium is reduced in a Jones reductor, yielding a mixture of trivalent and tetravalent uranium; the trivalent uranium is oxidized to the tetravalent state by bubbling a stream of air through the solution. The resulting solution of tetravalent uranium is titrated with a standard oxidant, generally sulfatoceric acid, dichromate, or permanganate. It seemed likely that the same general procedure could be used in determining semimicro quantities pf uranium if the conditions affecting the variables involved were understood more clearly than at present. In the method described below, the use of ferric sulfate to oxidize tetravalent uranium allows the titration to be made at room temperature in an essentially colorless solution with sulfatoceric acid. The latter oxidant in turn permits the use of the very stable indicator, ferroin; with its sharp color change and exactly reproducible blanks.Solutions of uranyl sulfate were prepared by diluting a stock solution that had been standardized gravimetrically according to the method of Lundell and Knowles (8).3/ Solutions of sulfatoceric acid were prepared according to the directions of G. F. Smith (12) and were standardized against arsenic trioxide in the presence of osmic acid according to the directions of Glen (5). The cerium solutions were stored in 18-liter carboys fitted with siphon arrangements so that the bottles did not need to be opened and protected from light in a dark cupboard. Under these conditions, even the 0.01 N solution changed by less than 1 part per thousand over a period of about 6 months."

Jun 1, 1952

By Louis A. Panek

An improved centrifugal-testing apparatus has been designed and built in the Bureau of Mines laboratory at College Park, Md., which is unique in that it incorporates the use of resistance gages to measure directly the strains in a rotating model without testing it to failure. Owing to this feature, a more rapid testing method can be used; furthermore, model materials need not be restricted to those of the prototype. The behavior of any structure in which strains of significant magnitude are produced by its own weight may be studied in a small model subjected to simulated gravity loading. The model is rotated in a centrifuge to induce in it centrifugal forces, which, like the gravitational forces in the full-size structure, act on the volume elements and are proportional to the masses thereof. Centrifugal testing is, therefore, applicable to the design of mine openings and to the study of similar ground-control problems. It constitutes an experimental method for determining the state of strain in a structure for which analytical methods are excessively laborious or even impossible. In previous applications of centrifugal testing by other investigators, the models usually were tested to failure, and the analysis was made from-the type of break produced. The models were made of the same materials as the proto-type, and the test results were applied only to the particular prototype represented by the model. Beam deflections were measured from photographs of the rotating model, but no means was employed either to determine the actual distribution of stress in the model or to determine quantitatively the degree of restraint imposed on the ends of the loaded model beam, that is, to determine whether the loaded model behaved as a beam with rigidly fixed ends or as some other type of beam. With the apparatus described, it is possible to determine the state of strain, and thus the boundary conditions, in a rotating test model weighing up to 90 lb., which can be subjected to centrifugal forces up to about 2,600 times the force of gravity. The load-strain relationship, applicable directly to the prototype, can be determined from a Single model test. The test results can be presented as quantitative relations between the loads, strains, and dimensions and mechanical proper-ties of the structural members and can be applied to any prototype, whatever its component materials, that satisfies the similarity requirements.

Jan 1, 1952

By K. C. Vincent

In the course of, investigation of domestic manganese-mineral occurrences, examining engineers of the Bureau of Mines collected 2-ton lots of ore from properties in the Cleveland-district, Idaho. As only one of the ores was high enough in grade for direct marketing to-producers of ferromanganese, ore-dressing concentration methods were investigated to determine their amenability to treatment. High-grade ore. (38.7 percent Mn) from the Idaho Manganese Mining Co. was taken from a replacement deposit in limestone consisting of several horizontal beds 1 to 5 feet thick, about 1 mile northeast of Cleveland. The manganese minerals occur as an intimate intergrowth of manganese oxides, containing minor amounts of limonite, ?quartz, and calcite as rather fine inclusions. However, the major contaminants are claylike products of rock decomposition, which can be eliminated by thorough washing of the ore at relatively coarse sizes. The Hot Spot property is 1 mile south of Cleveland. The ore occurs as a replacement deposit of medium-grade- ore in limestone, .The sample taken by the Bureau of Mines assayed 26.0 percent Mn. The manganese minerals consist of nodules, principally pyrolusite with some psilomelane and manganite embedded in wad.' The low-grade wad, containing manganese and siliceous minerals in intimate association, was easily rejected by washing.

Jan 1, 1952

By A. G. Loomis

Although secondary-recovery methods have not been applied widely in California, it is apparent that increasing attention and effort must be given to this phase of recovery if the State is to maintain its high rank as a petroleum producer. Steadily increasing demands for petroleum products and decreasing rates of discovery of new oil fields and rapid depletion of existing reserves emphasize the prospect of an adverse situation of supply and demand in the not-far-distant future. If the trend of discoveries becomes more favorable or if more complete economic recovery of the oil in place can be obtained by secondary recovery, this situation can be averted. Not only are these reserves of economic importance to the petroleum industry to meet increasing market demands, but economic reclamation of such reserves is an important conservation measure, which will prolong the productive life of many fields" Accordingly, progressive operators in California are alert to the possibilities of secondary recovery and have done much to implement such operations wherever feasible. Most of the operations are of the pressure-maintenance type} in which the reservoir pressure is maintained or partly maintained by injecting natural gas to increase oil recovery. The possibilities of recovering additional oil from stripper fields by gas drive and water flooding (including water disposal) also are being tested in experimental field projects. Table 1 summarizes gas and water-injection projects in California.

Jan 1, 1952

By A. G. Loomis

Although secondary-recovery methods have not been applied widely in California, it is apparent that increasing attention and effort must be given to this phase of recovery if the State is to maintain its high rank as a petroleum producer. Steadily increasing demands for petroleum products and decreasing rates of discovery of new oil fields, with rapid depletion of existing reserves, emphasize the prospect of an adverse situation of supply and demand in the not-far-distant future. If the trend of discoveries becomes more favorable or if more complete economic recovery of the oil in place can be obtained by secondary recovery, this situation can be averted. Not only are these reserves of economic importance to the petroleum industry for meeting increasing market demands; but economic reclamation of such reserves is an important conservation measure, which will prolong the productive life of many fields. Accordingly, progressive operators in California are alert to the possibilities of secondary recovery and have done much to implement such operations wherever feasible. Most current operations are of the pressure-maintenance type, in which the reservoir pressure is maintained or partly maintained by injecting natural gas to in-crease oil recovery. The possibilities of recovering additional oil from stripper fields by gas drive and water flooding (including water disposal) also are being tested in experimental field projects. Table 1 summarizes current gas-and water-injection projects in California.

Jan 1, 1952

By G. L. Humphrey

Although silicon carbide has been an important manufacture refractory for many years, knowledge of its thermodynamic values has been seriously lacking. In fact, some of the very properties that make it a useful substance, particularly chemical inertness, obstruct determination of its heats of formation and reaction. This paper reports the results of new measurements of the heats of combustion and formation, low-temperature heat capacity, entropy at 298.16°K., and heat-content and entropy increments between 298° and l,800°K. Two varieties of silicon carbide were studied -the common, hexagonal (type II) and cubic. The data are combined to obtain heat and free-energy-of-formation functions, which are given in tabular form. It is shown that the cubic variety is the more stable at temperatures to at least 1,800°K but, because of the inherent difficulties and errors in the heat-of-formation determinations at 298°K, it was not found possible to specify the free-energy difference accurately. The mechanism of silicon carbide formation from silica and carbon is not known and is not ascertainable from thermodynamic data. It appears improbable, however, that it can be a single-step reaction. Some reactions involving silicon monoxide gas and metallic Silicon, as possible intermediates in silicon carbide formation, are considered and shown to be thermodynamically feasible.

Jan 1, 1952