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By D. E. Wolfson

As part of its overall program of coal carbonization, the Bureau of Mines is studying the coking properties of coals that may be used for metallurgical purposes. The objectives of this study were given in detail in a previous report.2/ The suitability of coal for metallurgical use depends primarily on (1) chemical composition, (2) preparation characteristics, and (3) carbonization behavior. The first two factors, as well as the available reserves, are considered in selecting coals for carbonization tests. According to the estimate of reserves by Dowd,3/ the recoverable coal in Raleigh County in beds 28 inches or more thick, in thousand tons, is: [ ]

Jan 1, 1957

By V. C. Petersen

The titanium-rich end of the titanium-germanium system was investigated by x-ray and metallographic methods and verified by resistivity and dilatometer measurements. A constitution diagram is proposed. The titanium-rich portion of the phase diagram is characterized by eutectic and peritectic reactions. The eutectic composition is 19 percent germanium, and the eutectic temperature 1,360° C. The peritectic reaction occurs at 905° C. and 4 percent germanium. Germanium is soluble in alpha titanium to a maximum of 4 percent at 905° C. and in beta titanium to a maximum of 12.5 percent at 1,360° C. Both limits of solubility decrease with decreasing temperatures. Although substantial quantities of germanium are soluble in beta titanium, beta is not retained on quenching. The beta phase probably transforms to alpha by a martensitic reaction.

Jan 1, 1957

By James L. Elder

Field-scale experiments were conducted at Gorgas, Ala., from 1951 to 1954. Three reaction paths were formed by electrolinking-carbonization, using electrode spacings of 150, 152, and 155 feet. The coal along these reaction paths was gasified, using air, oxygen, and steam separately or in various combinations. At the conclusion of operation, a drilling survey was conducted to determine the location and approximate area of the reaction zones. During the applications of the electrolinking-carbonization technique the maximum limitation on electrode spacing was not determined. Initial tests were conducted at 60-foot spacing. Successful path-preparation tests were made at 150-, 152-, and 155-foot spacings, and the indications were that much longer spacings were possible. The potential requirements appear to be constant, regardless of path length, while the gross power required probably will increase with path length. During the carbonization phase gas was produced that is similar in quality to coke-oven gas produced at low to intermediate temperatures.

Jan 1, 1957

By L. J. Kane

While analyzing synthesis gas produced from coal, the Bureau of Mines found that conventional procedures for naphthalene determination were difficult and time consuming. The Bureau developed a rapid and sensitive turbidimetric procedure, which requires only simple instruments and hence can be used in plant-control laboratories. The gas is passed through a saturated aqueous solution of picric acid at 3° to 4° C. whose turbidity is then measured at room temperature. A dispersing agent is added to prevent coagulation of the suspension on warming. Only about 1 mg. (0.015 grain) of naphthalene need be absorbed, and precision and sensitivity are a few ten-thousandths of a grain, or a few hundredths of a grain per 100 cubic feet. The determination can be completed less than 10 minutes after absorption. INTRODUCTION One of the functions of the Branch of Coal Gasification, Bureau of Mines, Morgantown, W. Va., is to develop economical methods for manufacturing, from coal, a mixture of hydrogen and carbon monoxide for producing hydrogen, methane, and other gaseous fuels. This raw gas may contain many impurities, including naphthalene. This impurity is usually determined by first forming naphthalene picrate in a water solution of picric acid, separating the picrate, and titrating the unreacted picric acid or the picrate itself.

Jan 1, 1957

By Richard N. Appling

This compilation presents information obtained through investigation of manganese deposits and a reconnaissance of potential manganese-bearing areas of southwestern Oregon and Del Norte County, Calif., from October 1952 to September 1955. The report includes maps, assays, and preliminary examination data on 39 manganese deposits distributed throughout Curry, Coos, Douglas, Josephine, and Jackson Counties, Oreg., and 1 deposit in Del Norte County, Calif. On the basis of mineral content the deposits can be divided into three groups: 1 Manganese silicate deposits, manganese oxide deposits, and manganiferous iron de-posits. Generally the oxides occur along the coast in the Curry-Coos County area, the manganiferous iron deposits are in the Josephine-Douglas area, and the manganese silicates are found in both the Josephine-Douglas and Jackson County areas. The deposits are characteristically irregular in form and usually small. Most silicate and manganiferous iron deposits are in metasediments of Triassic (?) age; oxide deposits are in sediments varying in age from Jurassic to Eocene.

Jan 1, 1957

By John W. Moore

The discovery of porphyries in petroleum by Treibs (17-19) is one of the most significant achievements relating to the origin of petroleum. The presence of these remnants of chlorophyll and hematin in petroleum has immediate practical interest in several aspects of the petroleum industry. Because of their interfacial activities and film-forming tendencies, the metal-porphyrin complexes may be expected to affect the wettability of petroleum-reservoir rock surfaces and influence the flow of fluids in these reservoirs. Also, studies of the relationship of trace elements and porphyrins in petroleum may be expected to yield valuable information on source beds and petroleum migration. Finally, the extreme stability of several metal-porphyrin complexes complicates removal of these metals from some petroleum stocks where they exert deleterious effects on processing and utilization. Metal-porphyrin complexes are commonly associated with the asphaltic residues of crude oils in which they occur (8, 9, 15). However, investigations in this and another laboratory (15) show that small amounts of these complexes often remain in partly refined petroleum products, such as thermally cracked distillates and deasphalted stocks.

Jan 1, 1957

By F. R. Cattoir

Analytical methods are presented in this paper for determining soluble titanium, total titanium, indicated titanium, and average effective valence in titanium chloride - sodium chloride mixtures. In addition, data are given showing the effects of coarse and fine grinding on the degree of oxidation and average effective valence of such samples. INTRODUCTION The Electrometallurgical Experiment Station at Boulder City, Nev., as part of the Bureau of Mines program to obtain more efficient utilization of our natural resources, has been developing and improving titanium extractive metallurgical methods and techniques since 1945. Numerous reports have been published describing development of the Kroll process,4/ the electrorefining technique,5/ and methods of analyzing titanium sponge.6/

Jan 1, 1957

By Bruce I. Thomas

As a part of the United States Department of the Interior program for developing natural resources in Alaska, the Bureau of Mines studied the tin-bearing gold-placer deposits in the Tofty area of the Hot Springs district in central Alaska. The principal objective of the Bureau's work was to obtain facts about the extent and character of the placer deposits (including tailing) to indicate the economic or strategic tin-production potential of the Tofty "tin belt." A secondary objective was to determine (if possible) the bedrock Source of the cassiterite and other minerals found in the placer deposits. The placer phase of the work was begun in July 1954 and was continued during the 1955 and 1956 field seasons. Extensions to, and connections between, known placer channels were sought by 82 churn-drill holes. The Bureau drilling did not expand the placer deposits beyond the limits established by drift-mining operations and by previous drilling done by private concerns.

Jan 1, 1957

By G. W. Birge

As a part of its overall program of coal carbonization, the Bureau of Mines is studying the coking properties of coals that may be used for metallurgical purposes. The objectives of this study were given in detail in a previous report.2/ The inherent suitability of coal for metallurgical use depends primarily on (1) chemical composition, (2) preparation characteristics, and (3) carbonization behavior. The first two factors, as well as the available reserves, are considered in selecting coals for carbonization tests. The selection of coal beds in Westmoreland County for coking tests was based, in part, on estimates of the coal reserves by Dowd,3/ who estimated the recoverable reserves in beds 28 inches or more thick, in thousands of tons, as follows: [ ]

Jan 1, 1957

By Scott W. Hazen

METHODS of determining the grade and tonnage in a mineral deposit have not kept pace with scientific developments in certain other fields. The most commonly used methods of computing ore reserves and grade based on diamond-core-drill sampling are the cross section, the polygon, and the triangle. Tonnage and grade may be determined by these methods with acceptable accuracy, providing a sufficient number of samples is obtained; however, there is no means of determining when an adequate number has been taken or conversely if the deposit has been sampled excessively. It is demonstrated that, by using the techniques of statistical analysis, a mining engineer will be able to determine when a sufficient number of samples has been taken to determine the grade of a mineral deposit within a specified degree of confidence. Using statistical analysis to compute the estimated average grade of the ore makes it possible to compute a fiducial interval, when a distribution of the sample means is normally distributed, so that there is 95-percent confidence in the statement that the true average grade of the deposit is covered by the interval. This report utilizes data obtained from the Maggie Canyon manganese deposit, Artillery Mountains region, Mohave County, Ariz. Four separate exploration projects were conducted at Maggie Canyon between 1936 and 1950. Present economic conditions have made it desirable to determine the amount of 5-percent manganese ore developed by these projects.

Jan 1, 1957

By C. M. McKinney

This report contains Bureau of Mines routine analyses of 492 samples of crude petroleum from 470 United States oilfields, each of which produced 2,500 barrels a day or more during at least 1 of the years 1946-56. The fields are listed alphabetically by State and field names in table 1, with information on the geographical and geological sources of the samples. Table 2 summarizes the general characteristics of the crude oils and analytical and computed data determined from the analyses. A previous report 4 contains similar analyses of 283 important United States oilfields; some of them are repeated in this report. Many fields for which analyses previously were published are represented by new analyses, which include data not previously reported. Refractive index nu and specific dispersion, ng minus nD divided by the density, for some of the distillate fractions are included in the analyses of 316 of the crude-oil samples. This is the first Bureau of Mines report on analysis of crude oils to contain such data, and their use in calculating hydrocarbon-type composition of the fractions is explained.

Jan 1, 1957

By R. R. Wells

As a part of the strategic minerals program of the Bureau of Mines, nine chromite-ore samples were obtained during the period 1949-56 from mines in the vicinity of Red Mountain, near Seldovia, Kenai Peninsula, Alaska. This report summarizes the results of beneficiation studies of the samples at the Bureau's Juneau, Alaska, and Albany, Oreg., laboratories. In general, the ores were found amenable to concentration by gravity methods for producing concentrates that assayed over 48 percent chromic oxide. Intimate association of chromite and gangue minerals, however, necessitated fine grinding and limited the amount of chromite recoverable. Recovery of chromium in concentrate that assayed 48 percent chromic oxide or higher ranged from approximately 20 percent for low-grade ores (10 to 12 percent Cr203) to more than 95 percent for 1 high-grade sample (42 percent Cr203). The iron content of the chrome-bearing mineral -hence, the chrome/iron ratio of finished concentrate -appears to vary with the grade of the ore. Concentrates made from high-grade ores had chrome/iron ratios as high as 3.1:1; the concentrates from low-grade ores, however, had chrome/iron ratios as low as 1.8:1.

Jan 1, 1957

By Farrel W. Lytle

An X-ray emission spectrographic method of analysis is presented for determining rare-earth elements in fractions obtained from bastnaesite ore. The method includes determination of yttrium, thorium, lanthanum, and the rare-earth elements in various complex mixtures. The analysis technique is based upon comparing the samples with synthetic standards approximating the composition of the samples. Working curves are plotted on an absolute-intensity basis, with no correction for back-ground. Examples of working curves and the analyses of typical rare-earth concentrates are included. The selection of spectral lines for the various sample matrices is discussed. A special technique is used for samples in which rapid hydration and carbonation occurred. By analyzing synthetic samples of known composition, the accuracy of the method was determined. The average error of analysis was about 3 percent of the amount present in the range from 5 to 100 percent and about 7 percent in the 0.2-to 5-percent range. A maximum of about 40 samples per day may be analyzed for 7 elements each.

Jan 1, 1957

By E. M. Tignor

A research program to aid development of improved methods for increased production of petroleum from partly depleted reservoirs is a vital part of the Bureau of Mines effort to effect true conservation of that mineral resource. This report presents results of an investigation to identify the clay minerals within some Appalachian petroleum-reservoir sands, the effect of clay content on the fluid-flow behavior of those sands, and the use of brines in water-flooding operations. Permeability measurements using kerosine, calcium chloride brine, simulated oilfield brine, potassium chloride brine, sodium chloride brine, and distilled water were made on reservoir-rock cores. Clay fractions were separated from sand grains of disaggregated portions of each core sample, and the clay minerals were identified by the differential thermal analysis method. Relations of the permeability to various fluids were developed.

Jan 1, 1957

By John W. Buch

Upon review of German World War II mining practices and equipment for planning coal, the Federal Bureau of Mines initiated research leading to the development of a pneumatic planer for anthracite. The results of tests are reported in this manuscript. It was demonstrated (1) that hard anthracite can be planed and (2) that the design and operating requirements are within the limits of present-day engineering and technology. For hard anthracite, the depth of cut indicated is 4 to 6 inches; with a chain pull of 20 to 40 tons and the speed of planer travel of 18 to 20 feet per minute, a 40-hp. motor will be required for the planer hoist. Compressed-air requirements for the planer will be 250 to 300 c, f, m, at 60 to 70 p. s, i. It was learned that the length of the 4 individual sections of the planer should not exceed that of the individual troughs of the armored chain conveyor (5 feet in this instance); otherwise, bottom coal will be left in synclines, and the planer will override the conveyor at anticlines. Pneumatic pushers should be operated from a separate compressed-air line fitted with a pressure regulator. Results indicate that additional development work is warranted.

Jan 1, 1957

By Milton B. Hall

This report discusses in detail laboratory and pilot-plant tests conducted from January 1951 until January 1955 at the Northwest Electrodevelopment Experiment Station of the Bureau of Mines, Albany, Oreg., on defluorination and recovery of evolved fluorine from phosphate rock. Results of use tests of defluorinated phosphate rock by cooperating agricultural colleges and the United States Department of Agriculture are also included. In 1954 the consumption of fluorspar, the only domestic fluorine-bearing mineral of commercial importance, was approximately 478,000 short tons; 245,000 tons was from domestic mines. The production of marketable phosphate rock in the same period was about 13,800,000 long tons. Of this total amount, approximately 15 percent was produced in the West. From the viewpoint of conservation and utilization of fluorine as a natural resource, it is interesting to note that the total estimated quantity of fluorine in domestically produced phosphate rock is more than double that present in domestically mined fluorspar.

Jan 1, 1958

By W. H. Oppelt

Converting small-particle lignite to a stable, storable fuel of relatively high heating value was investigated. The fuel was prepared by thermal pretreatment of the lignite in an 8-inch i. d. rotary-drum retort, then the pretreated material was pelletized in an experimental 15-inch-i. d. rotary-drum pelletizer. Pelletizing tests were made with both starch and bituminous binders. During the first phase of the project, the quantity, composition, and heating value of products from the thermal processing of Kincaid lignite from Burke County, N. Dak., in an B-inch i. d. rotary-drum retort were investigated at a series of temperatures from 250° to 950° F. to establish optimum conditions for preparing feed material for pelletizing. To determine the response to thermal treatment of different lignites, 5 other lignites from Divide, McLean, Mercer, and Stark Counties, N. Dak., and 1 lignite from Saskatchewan, Canada, were processed at 700° F.

Jan 1, 1958

By Roy F. Abernethy

All samples tested showed some loss of heating value for the 5-month period under all 4 storage conditions. The losses increased as the time of storage increased, with the pan-storage samples showing somewhat greater losses than those in cans. The individual daily analyses for the first 2 weeks and the analyses every other day for the third and fourth weeks of storage vary within the approximate tolerance of the test for heating value. During the first 2 months of storage the changes in heating values were not Significant for the samples from Pennsylvania, Indiana, and Colorado. The Ohio coal indicated some loss by the end of I month, which increased to a value measurable with certainty by the end of 2 months. These data show that (1) small changes may occur even to samples in closed cans and (2) the laboratory sample should be handled as expeditiously as is practical until the analysis is completed. The statement by the ASTM that "If the B.t.u. determination is an important consideration in the sale of coal, the time elapsed between sampling and analysis shall not exceed 30 days,"3/ is quite adequate for 3 of the 4 coals tested. The change in the Ohio coal stored for 30 days is merely indicated and could not be determined with certainty by the techniques normally employed. The data on free-swelling indexes determined on can samples, after 30° C. air drying, show that only the Indiana coal lost more than one unit in free-swelling index number in 120 days. No significant changes were observed with the samples from Pennsylvania, Ohio, and Colorado in the 5-month period.

Jan 1, 1958

By William M. Nabors

As a part of a program to promote conservation and efficient utilization of petroleum resources, Bureau of Mines engineers are studying secondary oil-recovery projects in the United States. Published reports that set forth the pertinent facts of these operations help others to profit by the experience gained. This report presents the results of a study of secondary-recovery methods used in Kentucky by the Cumberland Petroleum Co. on its L. C. Bailey lease, Oil Springs pool, Magoffin County, Ky. This is believed to be the first water-flooding project in eastern Kentucky (fig. 1).

Jan 1, 1958

By LaMar G. Evans

The rapid determination of uranium in ores by radiometric means was investigated by the Bureau of Mines. Among the various procedures and schemes tested, two showed most promise. They were the ratio scheme developed in the Bureau's Tucson, Ariz., laboratory and the equilibrium method developed by the Canadian Department of Mines and Technical Surveys. The ratio method is a simple, empirical procedure for classifying the state of equilibrium in ores by measuring their radioactivity by means of a Geiger-Muller counter under three different conditions, using filters. The principal merit of the method is in providing a clue as to the reliability of equivalent uranium determinations.

Jan 1, 1958