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By G. L. Neumann

In October 1949 the College Park Branch of the Mining Division instituted a survey of the New England pegmatites. Many of the New England pegmatite deposits were superficially examined, and the Bumpus quarry in Albany, Oxford County, Maine (see fig. 1), was selected for a diamond-drill exploratory-development project to supply information for developing more economical mining methods and no increasing production of beryl and other scarce minerals associated with pegmatitic intrusives. The Bumpus quarry has been mined intermittently by three operators since it was opened in 1927. At the time of drilling, the vein or dike (see figs. 2 and 3) had been mined to a depth of 60 feet for a strike length of 280 feet. The dike averages 40 feet in thickness and dips 50 degrees southeast. The Bureau of Mines drilled seven diamond-drill holes between September 27 and November 27, 1950. These holes showed that the dike persists for at least 350 feet to the east and probably 200 foot to the west of the present excavation. The drilling also indicated that the dip, as exposed at the surface, continued unchanged at 500 to a depth of at least 50 foot below the pit. The dike was not delineated, although it fingered out as pegmatite interbanded with Granite, diorite, and gneiss in diamond-drill hole B-4, approximately 250 feet west of the pit. Further drilling will be necessary to find the extent of this pegmatite dike and to determine the safest and most economic mining system.

Jan 1, 1952

By L. H. Kalenowski

The metal lithium, its alloys, and its salts are becoming Increasingly important as industrial materials. Lithium metal, because of its great affinity for elements, such as nitrogen, hydrogen, oxygen, sulfur, phosphorus, carbon, and silicon, has become important for a wide variety of uses, ranging from purifying helium gas by removing the nitrogen to scavenging molten metals of undesirable impurities. The excellent fluxing properties of lithium salts have found increasing use in such applications as fluxes for welding aluminum and in lower melting ceramic glazes and coatings. Lithium chloride is one of the most hygroscopic salts known and is widely used as a dehumidifying agent. .About 17 lithium minerals are known. Four of these have commercial importance: Amblygonite, lepidolite, zinnwaldite, and spodumene. Spodumene is the most important source of lithium and lithium salts at present, but sizable deposits of amblygonite occur in the pegmatite area of the Black Hills of South Dakota. The size and nature of these deposits preclude the, possibility of, any assurance of an adequate supply of amblygonite for an operation processing only this mineral. Frequently spodumene and amblygonite occur associated in pegmatite minerals. Preliminary investigations indicate that a simultaneous recovery of spodumene and amblygonite can be made by froth flotation. A single process for treating spodumene and amblygonite or mixtures of thorn, would make possible more use of amblygonite as a source of lithium and obviate the separation of spodumene and amblygonite when they occur together.

Jan 1, 1952

By Fred D. Wright

A drill unit designed by Bureau of Mines engineers for testing various types of rotary bits has been in use since April 1950 at the experimental oil-shale mine near Rifle, Colo. The unit has a hydraulic drill and feed system, which provides the wide range of operating conditions necessary for adequate testing of drill bits and for obtaining data needed for the design of production scale equipment. Through the use of this unit, it has been proved that rotary drilling of vertical holes for mining the benches of the oil-shale mine is much cheaper than percussion drilling, and it is believed that in the near future the rotary drilling of horizontal blast holes in the top heading of the mine will prove equally economical.

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 Irving Hartmann

In recent years various modifications in the methods of blasting have been tried as a means of increasing the production of cod and of reducing mining costs. Following an investigation by the Bureau or Mines, authorization was granted to increase the charger limit for permissible explosives par shot hole from 1.5 to 3 pounds under contain conditions; this greatly facilitates the blasting of coal in some cool fields the practice has gradually evolved of simultaneously charging several shot holes in a face and then firing the charges singly without inspecting for gas after each blast. This practice is disapproved by the Bureau of Mines. In other coal mines the explosive chews in several adjacent shot holes are fired simultaneously. This form of shooting is claimed to increase the rate of production, generate smaller volumes of noxious gases, promote the health and safety of workers by eliminating the need of inspection of the face after each charge is fired, produce less float dust, and require less explosive than single shooting. However, simultaneous blasting may have a more harmful effect on the immediate roof strata; in some instances it leads to wedging of the broken coal, thereby making the coal more difficult to load out; it makes misfired shots more difficult to detect and possibly increases the chances of misfires. This lacy be duo to variations in the characteristics of detonators, because of more stringent requirements for adequate firing current, to the need for better electrical connections in the shot-firing circuit, and partly to the inadequacy of present permissible multiple blasting devices.

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 G. B. Shea

In the search for possible future sources of petroleum products, the recovery and utilization of bitumens from the large outcropping deposits of bituminous sandstones in the United States have been under study by the Bureau of Mines for the past several years. The results of laboratory research in the adaptation of the hot-water separation process to recovery of bitumen from bituminous sandstones were reported in an earlier publication, on the Edna deposits near San Luis Obispo, Calif. This publication included analytical data on the cracked products and asphalts obtained from the extracted bitumen and on the cracking and distillation of the bitumen. Comparable hot-water separation tests have been run in the San Francisco, Calif., laboratory of the Bureau of Mines on quarry samples from the large deposits of bituminous sandstones near Vernal and Sunnyside, Utah. The bitumens were isolated from the extracts of the separation plant and analyzed at the Petroleum and Oil-Shale Experiment Station of the Bureau of Mines, Laramie, Wyo. Part I of this report summarizes the general characteristics of the Vernal and Sunnyside deposits and discusses the hot-water separation process as applied to those bituminous sandstones and the results obtained. The separation tests showed that these bituminous sandstones also respond to treatment by the hotwater method of separation. The bitumen in the Vernal sandstone was extracted more readily by the action of hot water than was the Edna bitumen, which greatly simplified plant operation. The Vernal sandstone contains no water-soluble iron compounds, such as were found in the Edna sandstone, and, therefore, required no preliminary water washing. Recovery of bitumen from the Vernal sandstone was about 96 percent.

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 Irving Hartmann

When permissible explosives are used in coal mines according to the procedure recommended by the Bureau of Mines they are relatively safe, and no mine explosions are known to have resulted from this type of blasting. However, unsafe blasting practices - the use of nonpermissible explosives or the improper use of permissible explosives - have caused many serious disasters. In fact, such unsafe practices constitute the third most important cause (exceeded only by electricity and the use of open lights and smoking) of coal-mine explosions in the United States. During 1929-1947, inclusive, 81 explosions, resulting in 475 fatalities, were ascribed to unsafe blasting. The hazards of black powder, dynamite, and other nonpermissible explosives in coal mines have been recognized for many years, and attention has been called to this in numerous Bureau of Mines publications. Not only can these explosives ignite namable gas-air mixtures readily, but they can also ignite coal dust, as has been illustrated repeatedly in tests and at educational public demonstrations at Bruceton and elsewhere.

Jan 1, 1952

By Irving Hartmann, F. P. Christofel, John Nagy, E. B. McGibbeny

"INTRODUCTION When permissible explosives are used in c procedure recommended by the Bureau of Mines 5/ they are relatively safe, and, no mine explosions are known to have resulted from this type of blasting. However, unsafe blasting practices - the use of nonpermissible explosives or the improper use of permissible explosives - have caused many serious disasters. In fact, such unsafe practices constitute the third most important cause (exceeded only by electricity and the use of open lights and smoking) of coal-mine explosions in the United States. During 1929-1947, inclusive, 81 explosions, resulting in 475 fatalities, were ascribed to unsafe blasting. 6/The hazards of black powder, dynamite, and other nonpermissible explosives in coal mines have been recognized for many years, and attention has been called to this in numerous Bureau of Mines publications. Not only can these explosives ignite flammable gas-air mixtures readily, but they can also ignite coal dust, as has been illustrated repeatedly in tests and at educational public demonstrations at Bruceton and elsewhere. 7/Research in the Experimental coal mine 8/ of the Bureau of Mines at Bruceton, Pa., and unfortunate experience in commercial mines have proved beyond doubt that improper use of explosives that have passed the official permissibility tests can cause as explosions. In limited tests with a fey American permissibles at Bruceton, and in more, extensive tests with permitted explosives at the Polish experiment station, 9/ explosive charges were fired from steel cannon and freely suspended in coal-dust clouds. In these experiments coal dust was ignited under some conditions. However, it has never been definitely established whether permissible explosives can initiate coal-dust explosions when fired in a coal seam. It is true that a few mine explosions were strongly suspected to have resulted from ignition of coal dust by misuse of permissibles, but in each case other complicating factors introduced some doubt in the minds of the investigators. Full knowledge of the problem is important, because coal dust is present in most blasting operations in coal."

Apr 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. Kenworthy

The objective of this research was to develop methods and determine conditions under which metallic sulfides with lower boiling points than sphalerite may be removed from zinc sulfide concentrates by volatilization. A higher percentage of extraction of lead, cadmium, and germanium than is common in current practice was sought. The investigation, conducted by the Metallurgical Branch of the Minerals Technology Division, Region VI, showed that, under proper conditions, it is possible to remove over 90 percent of the lead, cadmium and germanium as an enriched sublimate. The uses of lead, and cadmium to a lesser extent, are well-known. Although germanium was discovered in 1886 by C. Winkler, commercial use has been achieved only in recent years. The amount consumed per manufacturer unit is so small that the price of germanium may still be quoted by the gram. The electronic industries have been the chief consumer of this semiconductor. Germanium is sold largely to the fabricator as a dioxide for reduction to metal and subsequent processing into wafers for use in diode and triode electronic tubes. Extensive research at Purdue University during World War II led to the first practical use of germanium.

Jan 1, 1952

By G. W. Jones

From evidence made available during the investigation, it was concluded that the first of a series of explosions occurred at 1:15 to 1:20 p.m. September 21, 1951, in an underground vault that housed pressure regulators on the gas-distribution lines that served Brighten. This explosion damaged the pressure regulators and permitted high-pressure gas to enter the distributing mains and individual-service lines. As a part of the gas-distribution system was not provided with means for protection against such excessive pressures, gas gained access to the interiors of many residences in this area and caused a series of disastrous explosions and fires, which took place during a period of approximately 2 hours after the initial explosion in the pressure-regulator vault. Two persons were killed in the first explosion in a residence, and a third person died of a heart attack attributed to the excitement that prevailed during the explosions and fires, Twenty-three persons were listed as injured. Forty-one residences were either destroyed or damaged - 11 by explosion and the remainder by fires, which developed as a result of gas leakage into residences. Fifteen residences were listed as "completely down" or "gutted." Unofficial estimates of property damage ranged from $1,000,000 to $1,500,000. In view of observations made and information obtained during the investigation, recommendations are presented in this report relative to the natural-gas distribution system in Brighton, which may be helpful in the prevention of similar accidents in this and other communities.

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