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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 John B. Goodman

This report presents a study of a modification of the precision laboratory carbonization-assay apparatus that renders the unit capable of performance at low-, medium-, and high-temperature assay levels and permits, under controlled conditions, evaluation of the relationship between carbonization temperature and the yield of pyrolysis products. Second, the interest and value derived from the temperature study data directly apply to the particular semiplant carbonization processes and techniques currently being investigated in this laboratory. Data obtained with the assay apparatus enables the fuel technologist to predict the probable yields of carbonization products from pilot-plant operations under various carbonizing conditions. Data obtained with the assay apparatus has been used to predict the product yields of industrial carbonization plants at Kemmerer, Wyo., and Rockdale, Tex. The assay provides a useful tool in detecting, from the carbonized plant product, the degree of effectiveness of pilot-plant operation. Third, the residual volatile matter in some industrial carbons has broad significance. Evaluation of the volatile material remaining with or in the carbon may be assessed through the high-temperature-assay technique. The low-temperature carbonization assay devised by the writers has proved to be a versatile tool in predicting the probable product yields from pilot-scale carbonization processes. The apparatus described in previous publications has been modified to extend the range of testing above 500° C. without impairing the accuracy and reproducibility obtained in the low-temperature range. Results presented here include product yields from a typical Texas lignite and Wyoming subbituminous-B-rank coal over the temperature range 150° to 1,000° C.

Jan 1, 1958

By Albert E. Long

Diamond-bit performance and cost data accumulated in core-drilling sandstones reveal significant trends of economic interest. Large-size, AA-Grade drill bort suffered less diamond loss per foot drilled than any other size or grade of diamonds assessed. Detailed analyses of the factors that affect diamond-bit performances -diamond size, diamond quality, bit size, bit type, percentage of core recovered, and physical characteristics of bit matrices -are assessed in the tables, graphs, and discussion. INTRODUCTION Since 1945 the Bureau of Mines has been compiling detailed performance records on diamond bits used in core drilling throughout the United States and Alaska. Analytical reports covering bit performance in various rocks are issued as in-formation on a significant number of bits used in anyone type of rock is accumulated. The first three such reports analyzed bit performance in gneiss,2/ schist,3/ and lime-stone and dolomite.4/ This report evaluates diamond-bit performance in sandstone. Data obtained from 627 bits, which drilled 42,665 feet on 45 different projects, are presented. The geographical distribution of the projects is shown in figure 1.

Jan 1, 1958

By Michael J. Gallagher

Diamond-bit performance data accumulated by the Bureau of Mines in core-drilling limestone and dolomite show that the physical characteristics of the diamonds and the sizes and types of bits used are economically significant. An analysis of the data establishes one trend of particular significance to those engaged in core drilling: Bits set with small, low-quality drill bort are the most economical. Detailed analysis of the factors that affect diamond-bit performance, such as size and quality of diamonds, sizes and types of bits, percentage of core recovered, and physical characteristics of bit matrices are assessed in the tables, bar charts, and discussion.

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 M. M. Fine

In an experimental study by the Bureau of Mines, in cooperation with National Lead Co., the roast-flotation process was found to be an effective means of upgrading certain cobalt-nickel stockpiles. The research was undertaken to determine whether the process could yield an enriched feed, with a minimum cobalt content of 6.0 percent, for the company refinery. The stockpiles (products of the company Fredericktown, Mo., milling operations) were essentially complex sulfides of cobalt, nickel, copper, lead, and iron, 1 sample of which contained 2.84 percent Co and 3.57 percent Ni. After a controlled oxidizing roast at 400° C., laboratory flotation with conventional sulfhydric reagents yielded an enriched concentrate analyzing 9.22 percent Co and 11.43 percent Ni, with recoveries of 84.9 and 85.8 percent, respectively. These are typical laboratory data; other data indicated higher grades were possible but at reduced recoveries. A brief, continuous campaign verified the applicability of the process to the raw material in question but was not continued long enough to establish optimum conditions. As a consequence, the results of the large-scale tests did not equal those obtained in the laboratory but definitely confirm the beneficiation possible from the roast-flotation process.

Jan 1, 1958

By C. I. Pierce

Knowledge of the water content of oil-bearing formations is important in petroleum-reservoir evaluation work. Electric logging provides a means for making reliable estimates of water content if resistivity-saturation relationships representative of the formations are available. Relationships can be determined in the laboratory by a number of methods. This report describes and presents results of a laboratory investigation conducted at the Bureau of Mines Appalachian Experiment Station, Morgantown, W. Va. (1) to evaluate an evaporation method of attaining water saturations in sandstone samples when determining resistivity-saturation relationships and (2) to compare saturation exponents derived from data obtained, using different methods of achieving water saturations. A series of tests was conducted to determine the effect of evaporation on salinity distribution within the core specimen. Results of these tests show that a zone of high salinity was set up at the surface of a sample during evaporation and that long periods were required for the sample to reach resistance equilibrium after evaporation had ceased. Equilibrium time ranged from several minutes to several days, depending on the sample size and the technique used. The high-salinity zone was removed from the sample by using auxiliary porous material in capillary contact with the sample surface during evaporation. Salinity determinations and resistance measurements indicate that, at saturations greater than the minimum interstitial values, the mechanism of flow during evaporation was one of moisture migration mainly as a liquid from the interior of the test specimens to their exterior surfaces. The concentration of the contained brine remained essentially unchanged, except for a narrow zone near the evaporating surfaces.

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