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By J. B. Zink

The Bureau of Mines developed a spectrochemical method to determine six constituents in coal ash in the following concentration ranges: silica 9 to 63 percent, alumina 7.5 to 35 percent, ferric oxide 2 to 30 percent, calcium oxide 1 to 29 percent, magnesium oxide 0.5 to 6 percent, and titanium oxide 0.5 to 4 percent. Samples of coal ash are fused with a mixture of lithium tetraborate and vanadium pentoxide. The resulting beads are crushed, mixed with powdered graphite, and briquetted. The pellets are analyzed spectrographically, using controlled high-voltage spark excitation. Vanadium serves as the internal standard. Effects due to matrix variations are minimized by fusion with lithium tetraborate. Intensity ratios of selected analytical lines are determined photometrically, Concentrations are read from analytical curves, prepared from synthetic standards, relating log intensity ratios to log concentration. A combustion procedure is used to determine sulfur tri-oxide. The method is most useful when large numbers of coal ashes must be analyzed but a high degree of accuracy is not essential.

Jan 1, 1967

By Jeffrey M. Listak

The Respiratory Hazards Control Branch of NIOSH routinely conducts laboratory and mine-site evaluations of dust control technologies. Gravimetric and instantaneous dust sampling instruments are used in these evaluations to measure and document dust levels to determine worker exposure. The Thermo personal DataRam (pDR) is an instantaneous sampler that uses light-scattering technology to provide relative measures of airborne respirable dust. The pDR can be used in active and passive modes to measure respirable dust levels. Tests were conducted to evaluate the sampling performance of active and passive pDR operation relative to each other and. against a gravimetric sampler (the accepted standard for respirable dust measurement). The purpose of the test was to determine if the pDR can be used effectively in the passive mode in higher velocity airflows (up to 5.1 m/s (1000 fpm)). Studies of the pDRs in both modes of operation were conducted in a controlled laboratory environment and in field situations. Dust measurements using pDR units in both modes of operation were recorded in ve¬locities ranging from 1.0 to 5.1 m/s (200 to 1000 fpm). Tests were conducted in ambi¬ent air and in air with the addition of moisture. Results show that, although the units measure different concentrations in their respective modes of operation as compared to a gravimetric sample, the relative readings can be corrected to yield accurate dust measurements.

Jan 1, 2007

By D. P. Schlick

As of June 30, 1970, Federal regulations required the operator of each underground coal mine to maintain the average concentration of respirable dust below legislative standards. As of March 1, 1971, over 152,000 respirable dust samples have been processed by the Bureau of Mines. Approximately 75 percent of underground working sections are being sampled in accordance with Federal regulations. Results indicate that 72 percent of the sections which have completed at least one basic sampling cycle are below 3.0 mg/m3, the standard in effect under the Federal Coal Mine Health and Safety Act of 1969 (P.L. 91-173). Notices of Violation were issued on 1,670 underground mines for failure to begin a sampling program; Withdrawal Orders were issued in 64 of these instances. Notices of Violation were issued on 1,121 sections where applicable dust levels were exceeded; Withdrawal Orders were issued in seven of these instances. There are 381 mining sections currently operating on permit; from the interim Compliance Panel.

Jan 1, 1971

By P. A. Bloom

Bureau of Mines research was conducted to develop effective separation methods that might be used in exploiting substantial tonnages of complex barite-fluorspar ores in Arizona. The exploitable reserves now may be increased as recent batch and continuous flotation tests demonstrated that a complex barite?-fluorspar ore from the Red Chief deposit, Yuma County, Ariz., could be selectively treated to concurrently produce (1) fluorspar and (2) a barite byproduct of marketable grade. The sample contained 24.8 percent CaF2 and 24.3 percent BaS04. Processing comprised production of a fluorspar product containing 97 percent CaF2 with an 82 percent recovery, using a sodium fluoride-lignin sulfonate-fatty acid reagent combination. Concurrent retreatment of the fluorspar tailing, using sodium cetyl sulfate as a collector, yielded a barite product of 94 percent BaS04 grade with a 71-percent recovery. The products met specifications for acid-grade fluorspar and drilling mud-type barite.

Jan 1, 1963

Unfortunate occurrences resulting in injuries, loss of life, and destruction of property by explosion, fire, and other mishaps during shaft sinking in the past few years have focused the attention of the Bureau of Mines on the need for safety standards for such operations. Several States have some rules and regulations applicable to local conditions, and several Bureau publications (including some now out of print) cover the hazards that may be encountered in shaft sinking. Certain requirements of the Federal Mine Safety Code and Federal Coal Mine Safety Act may be applied, but there are no definite, uniform standards that will guide those desiring to sink a shaft safely and bring about uniform safety inspections.

Jan 1, 1957

By B. W. Madsen

The Bureau of Mines conducted a large-scale (6.4 t), long-term (2,165 days) test to gain a better understanding of the leaching characteristics of chalcopyritic ores. An ore sample containing 0.77 pct Cu was leached in a fiberglass column by downward percolation of acidified ferric sulfate solutions. Three sets of leaching conditions were investigated: (1) ambient temperature leaching, (2) elevated temperature (50° to 60° C) leaching, and (3) elevated temperature leaching after inoculation with thermophilic bacteria. Leaching at ambient temperature resulted in a copper extraction rate of 0.44 pct per 100 days. Increasing the temperature to 50° to 60° C resulted in decreased activity of natural mesophilic bacteria, and the leaching rate decreased to 0.22 pct per 100 days. The pH was lowered from 2.0 to 1.6, and nutrient solutions that contained thermophilic bacteria were added. This procedure resulted in an increase in the ferric-to-ferrous iron ratio and an increase in the copper leaching rate. However, the increased leaching rate was not sustained, and 120 days after inoculation the bacterial activity declined, the ferrous iron content increased, and the copper leaching rate decreased.

Jan 1, 1983

By A. C. Rice

Aminopolyacetic acid chelating agents were added to separatory-funnel-scale solvent-extraction systems to determine the effect on separating rare-earth elements. Average values for separation factors between adjacent elements obtained with Primene JM-T2 increase 36 percent when EDTA is added to the aqueous phase. Adding HEDTA or DCTA also improves separation factors for certain rare-earth elements. Percentage of extraction and the separation factors exhibit marked sensitivity to concentrations of amine, chelating agent, and hydrogen ion. The chelating agents improved separation in Primene JM-T, BHDA, and Primene 81-R extraction systems.

Jan 1, 1963

By E. M. Tignor

As a part of the program of promoting the conservation and efficient utilization of petroleum, studies are being made by engineers of the Bureau of Mines on secondary oil-recovery projects throughout the United States. In furthering that aim, engineering data concerning the reservoirs, methods of stimulating the production of oil, and other pertinent facts are collected, studied, and subsequently published so that others may profit by the experience gained. This report presents the results of a study made by engineers of the Franklin, Pa., office of the Bureau of Mines of secondary oil-recovery operations in the Boggs field, Spencer district, Roane County, W. Va., whore natural gas is injected into the reservoir to stimulate the production of oil from a so-called stripper field. The Boggs field, like most others in the Appalachian region, is one in which the major part of the natural energy that caused oil to flow through the reservoir to the producing wells during the primary stage of oil production has been dissipated. For all practical purposes, most of the oil produced in the Appalachian region at the present time can be considered to be from stripper fields. Consequently, secondary recovery methods are being used extensively in the oil-producing areas of New York, Pennsylvania, West Virginia, Ohio, and Kentucky for recovering some of the oil that was not produced by primary production methods.

Jan 1, 1949

By R. L. Hopkins, H. T. Rall, H. J. Coleman, C. J. Thompson

Two methods were tested for separating sulfur compounds in certain petroleum fractions into types . Such separation is preliminary to identifying the compounds . Each method involved extraction of sulfides from petroleum sulfur concentrates . In the first method , the sulfur concentrate was reacted with methyl - ptoluenesulfonate to form sulfonium compounds from which unreacted portions of the sample were removed by washing with solvent . The sulfides then were recovered by heating the sulfonium compounds with anhydrous triethanolamine . The second method consisted of passing anhydrous hydrogen iodide into a n-butane solution of the sample cooled in dry ice , whereupon the hydrogen iodide adducted with the sulfides to form sulfonium compounds . These adducts separated as crystalline solids or , more frequently , as glassy viscous liquids . The sulfide was regenerated by adding water to the filtered sulfonium compound and was recovered by steam distillation or by extraction with pentane . These methods have been evaluated , using individual pure sulfur compounds and blends of sulfur compounds . They also have been applied successfully to separating sulfides from sulfur concentrates derived from petroleum fractions .

Jan 1, 1964

By W. E. Robinson

Samples of raw oil shale and kerogen concentrates were oxidized by alkaline potassium permanganate, air, nitric acid, oxygen, and ozone to obtain information about the chemical structure of organic kerogen in oil shale. In one test, oil shale and oil-shale products were oxidized exhaustively with alkaline potassium permanganate, and the distribution of the organic carbon in the final oxidation products was determined. Comparing results of this oxidation with those obtained from other carbonaceous materials and known compounds gave information about the structure of kerogen. Alkaline potassium permanganate oxidation also was used partly to degrade kerogen into soluble products for characterization purposes. Structures present in these degradation products were indicative of type structures originally present in the kerogen. Nitric acid, oxygen, and ozone were used also for partly degrading kerogen to soluble oxidation products. Carbon-balance oxidation tests using alkaline potassium permanganate showed that Colorado oil-shale kerogen differs from many other carbonaceous materials such as coal and kerogens from other areas. Composition of the degradation products indicated that Colorado oil-shale kerogen is predominantly cycloparaffinic and saturated heterocyclic structures with some long-chain paraffinic and aromatic structures present. The ring systems may be connected through short carbon chains or bridges containing oxygen, nitrogen, and sulfur.

Jan 1, 1963

By H. R. Shell, John L. Miller, M. V. Denny

In the mica research program conducted by the Bureau of Mines at Norris , Tenn . , many micas other than silicon fluorphlogopite have been synthesized . It has been well established since the initiation of the program that synthetic micas are important materials useful for their superior or unique properties as well as substitutes for natural micas . The possibility of controlling the physical properties of synthetic mica by isomorphic substitution of other ions in the fluorphlogopite lattice further emphasizes the importance of these materials . Accurate measurement and reporting of their properties constitute an essential part of the research program . The study of germanium fluorphlogopite is in keeping with the requirements of a comprehensive study on isomorphic substitution , specifically to identify precisely the material -- chemically , structurally , and optically . The X- ray measurements , including indexed powder and single crystal data , with a description of the methods used to obtain these data , are provided . 5 Earlier work on germanium mica by R. A. Hatch et al . (5) gave an estimate of the cell parameters from X - ray powder data , but no attempt was made to index the diffraction pattern or to determine the space group symmetry . Later work by E. A. Schatz and J. C. Withers (9) listed X- ray and optical measurements , but no attempt was made to index the mica or determine its symmetry . Roth (7) found that germanium dioxide having the a - quartz structure , when heated with equimolar percentages of MgO , CaO , Sr0 , or Ba0 at 1,235 ° C , formed ABO3 -type compounds , e.g. MgGe03 isostructural with enstatite (MgSiO3 ) . Geo₂ also has a rutile - type polymorph with Ge ++ ions in octahedral coordination . Germanium was substituted for silicon in the serpentine structure by Roy and Roy (8 ) using hydrothermal techniques . These authors wrote as follows : "The substitution of Ge + for Si + yielded a magnesia - germania serpentine , formed easily in euhedral hexagonal plates which in some instances were visible in the light microscope . Electron micrographs and the sharp X - ray diffraction patterns confirm a plate - like rather than tubular habit . " It has been shown in this investigation that substitution of germanium for silicon in the mica structure is readily accomplished without radically changing the characteristics of the mica . Substitutions in the mica structure take place in three locations : Tetrahedral , octahedral , and interlayer positions . The tetrahedral positions are normally occupied by Sit or by a combination of Sit with Al +3 the most common combination being 2A1 +3 and 6Si +4 · , The octahedral position , which has six - fold coordination in phlogopite , contains a larger cation such as magnesium . In muscovite it contains only 2A1 ions ; therefore , this mica is considered a dioctahedral mica , whereas phlogopite is considered trioctahedral . +3 The interlayer position has twelve - fold coordination with six oxygen ions from each of two adjacent tetrahedral silica layers . This is the cleavage plane of the mica and commonly contains the largest cation in the mica structure (e.g. potassium) .

Jan 1, 1964

By Z. Zhiqun, V. A. Marple, B. Y. H. Liu

"IntroductionIt is commonly understood that aerosol particles may be injurious to human health if they are of a size that enables them to enter the respiratory tract. Coal Workers' Pneumoconiosis (CWP) is one disease known to be caused by coal mining related particles.The location in the respiratory tract where the particles are deposited is primarily a function of the equivalent aerodynamic diameter (EAD) of the particle. The equivalent aerodynamic diameter is the diameter of a spherical particle with a density of 1.0 gm/cm3 with the same falling speed as the particle in question. For a spherical particle the calculation is rather simple in that the equivalent aerodynamic diameter is simply the diameter of the particle in question multiplied by the square root of the density of the particle. For irregularly shaped particles, such as coal particles, there is no simple way to make the EAD calculation. For example, Figure 1 is only one of an infinite variety of particle shapes that can be found in practice and the aerodynamic size of this particle and, therefore, its deposition location in the respiratory tract would be nearly impos-sible to estimate accurately.The normal method for determining the aerodynamic diameter of particles has been to experimentally measure the size of the particles in a settling chamber or with an inertial classifier such as an impactor, cyclone or a centrifuge, since inertial classifiers have the property of classifying the particles according to their aerodynamic diameters."") However, these devices can only give limited information on the EAD of a single particle with a specific shape. Impactors and cyclones, for example, collect particles in size ranges and not at a specific size, so the determination of the EAD of a specific particle is not possible. A centrifuge, on the other hand, can measure the EAD of a specific particle but the equipment is costly and procedure laborious, and it may not be possible to disperse a particle of a specific shape into the centrifuge. The centrifuge can be used to determine the EAD of clusters of spheres in various arrays, but introducing particles of a specific irregular shape may not be feasible. Furthermore, the EAD is a function of the orientation of an irregularly shaped particle and the orientation of a particle in an inertial classifier is unknown. The orientation may also vary as the particle passes through the classifier.Because of the difficulty in determining the EAD of an irregularly shaped particle, we have undertaken a program to apply theoretical numerical methods to calculate the EAD of any shape particle. In our laboratory we have, for some time, been using numerical methods to determine the flow field of air within instruments such as impactors, (2) inlets, (3) and virtual impactors (4) Recently, this technique has been expanded into the three-dimensional regime, and the flow fields and particle motion characteristics within cyclones (5) and glove boxes have been studied. We have now begun to use these numerical three-dimensional flow programs to study the flow field around irregularly shaped particles to determine their drag coefficients, falling speed, and thus, their EAD."

Mar 1, 1989

By N. S. Dalal, Xiaoya Sun, Xianglin Shi

"The in vivo toxicity of vanadium(V) has been found to correlate with the depletion of cellular glutathione and related non-protein thiols. With a view to understanding the mechanism for this observation, we have investigated the oxidation of glutathione, cysteine N·acetylcystcinc and pcnicil· lamine by vanadium(V), using electron spin resonance (ESR) and ESR spin trapping methodology. The spin trap used was 5,5-dimethyl-l-pyrroline I-oxide (DMPO). It is found that the oxidation of these thiols by vanadium(V) generates the corresponding thiyl radicals and vanadilim- (IV) complexes. The results suggest that free radical reactions play a significant role in the depletion of cellular thiols by vanadium(V) and hence in vanadium(V) toxicity. 1. INTRODUCTIONThis communication reports on the identification of thiyl radicals formed as intermediates in the reaction of vanadium(V) with glutathione (GSH) and related nonprotein thiols. This study was undertaken because the biochemical mechanism of vanadium toxicity is still not fully understood,. despite being a topic of current research activity [1-20). As to possible clues, it is known that vanadium is most toxic when administered in its pentavaient state [21), and that vanadium(V) administration into laboratory mice reduces cellular levels of NAD(P)H and GSH [22). While the oxidation of NAD(P)H by vanadium has been studied extensively [16-20), that of glutathione and related non-protein thiols has been paid less attention. On the other hand, GSH and related thiols are important cellular antioxidants [23). Their functions include decomposing lipid peroxides and protecting cell membranes [23-25). Thus any reduction in the cellular contents of such nonprotein thiols after vanadium exposure may result in the accumulation of lipid peroxides which might ultimately lead to tissue injury. With a view of finding the mechanism for this thiol depletion process, we have investigated reactions of non-protein thiols with vanadium(V). Particular attention has been paid to the detection of thiyl radicals, since it has been postulated [l] (but not experimentally proven) that the glutathionyl radical (GS·) might be an intermediate in the reaction between vanadium(V), NADH and GSH. We have used electron spin resonance (ESR) and ESR spin trapping methodology for investigating the reactions of GSH, cysteine, N-acetylcysteine and penicillamine with vanadium(V). The results show that the corresponding thiyl radicals are indeed formed in the one-electron reduction of vanadium(V) by all of the above mentioned thiols."

Jan 1, 1990

By M. J. Spendlove

A progress report is presented on a research program in which an attempt was made to develop a practical sulfide-volatilization process for recovering tin from low-grade Bolivian ores. Shaft-furnace designs and operating techniques were studied in a series of experiments in which the objective was to sulfidize cassiterite to stannous sulfide, remove the stannous sulfide by volatilization, reconvert the stannous sulfide to stannous oxide, and collect the resulting fume. A shaft furnace was developed and operated in a final test in which many of the previous difficulties were surmounted. Since the supporting funds were exhausted at this point, the project was discontinued; recommendations for further improvements in furnace design and operation were made on the basis of interpretation of experimental results obtained in shaft-furnace experiments and other related studies.

Jan 1, 1955

By Richard D. Miller

This publication contains routine analyses and related source data for 434 gas samples from 16 States. These samples were collected during calendar year 1961 as part of the continuous survey for the occurrence of helium in natural gas conducted by the Helium Activity of the Bureau of Mines. The analyses herein were made by mass spectrometer and Frost helium apparatus. The most important helium resource discovery made during 1961 was the Table Mesa field in San Juan County, N. Mex. This field, Which has an estimated recoverable helium reserve of 850 million cubic feet, is now supplying gas containing approximately 5.4 percent helium to the Bureau of Mines Navajo Helium Plant at Shiprock, N. Mex.

Jan 1, 1964

By Richard D. Miller

This publication contains routine analyses and related source data for 434 gas samples from 16 States. These samples were collected during calendar year 1961 as part of the continuous survey for the occurrence of helium in natural gas conducted by the Helium Activity of the Bureau of Mines. The analyses herein were made by mass spectrometer and Frost helium apparatus. The most important helium resource discovery made during 1961 was the Table Mesa field in San Juan County, N. Mex. This field, Which has an estimated recoverable helium reserve of 850 million cubic feet, is now supplying gas containing approximately 5.4 percent helium to the Bureau of Mines Navajo Helium Plant at Shiprock, N. Mex.

Jan 1, 1964

By F. K. McIntosh, A. F. Robertson, T. J. Ballard

"INTRODUCTION Molybdenum deposits occur in Halifax County, N. C., near the eastern border of the Piedmont province. The deposits are associated with a small granite body about 2 miles long and half a mile wide. Molybdenite is the principal ore mineral and is found as disseminations or thin stringers in quartz veins and occasionally in the enclosing granite or schist wall rock.The deposits were investigated by Almon F. Robertson and Charles J. Cohen, engineers of the Bureau of Mines, in 1942 and 1943, who recommended that the deposits be explored to supplement reserves of critical war minerals.The Bureau made the initial exploration of the deposits in July 1943 and continued its work to January 1944. Drilling was resumed from July to December 1946 to test the deposits at &eater depth than had been attempted during the previous exploration."

Dec 1, 1947

By Roy J. Greenfield

The overall purpose of this research was to improve the understanding of how the post disaster seismic location system works, what determines the signal size, what is the character of the seismic noise, how well the system can detect blows from a trapped miner, and how well the source of the blows can be located. Based on an improved understanding of the system, improvements were suggested in the seismic subarray configuration, and in the system deployment procedures. An important part of this research was to become familiar with the seismic system operation and to work with the Westinghouse Electric Corporation and MSHA personnel to modify and improve the system. To accomplish this we participated in the planning, execution, and data analysis for a number of seismic field tests. Several in-mine field tests were conducted. From these tests the capabilities of an in-mine seismic system were analyzed and specifications were made for designing an operational in-mine system. Several portions of the work done on this grant were covered in previous reports. In particular the capabilities or the presently operational surface based seismic location system has been thoroughly documented by Durkin and Greenfield (1981). Portions of the location procedures and effects of mine openings on seismic signals have also previously been published. These portions or the work will only be summarized in this final report.

Jan 1, 1982

By STUART R. BRINKLEY, Ruth F. Brinkley

This same phonomonon of diffraction may be transposed into the X-ray domain. All that is necessary is to reduco, in the samo proportion, the wavo length of the light and the diameter of the particlo; thus, with radi- ations whose wave length is of the ordog of angstroms, the dimensions of the active particles go from 10 to 100 A that 18, the dimensions of col- loidal particlos. The evidence of this fact is shown by the following experimental schomo (fig. 1a): A narrow beam of X-rays passes through a thin layer of a modium containing micelles; the photographic film is placed a few centimeters behind the sample, and a small absorbing screen stops the direct beam in order to prevent its fogging the film. The intersect of the direct beam is surrounded by a narrow spot whose blackness decreases with the distance from the center. We will call this the spot of central diffusion (fig. 1b). The phenomenon, in spite of its relatively reat intensity, has been observed only by a few authors, who have simply given a qualitative description without attempting any quantitative de- ductions. This is due to the fact that observation of this phenonenon is not possible with the apparatus generally used to obtain X-ray diagrams, because the parasite foggings in the vicinity of the incident beam are sufficiently important to hide those produced by the sample. With the monochromator, however, used by us to obtain Debye-Sherer diagrams, this parasitic diffusion can be totally suppressed. In this way our attention was again directed to the spot of central diffraction, and we were led to make a detailed quaititative study of it.. then several papers have been published on this subject. Hosemann, using methods of calculation outlined by us, has extended them to the special case of fibrous substances, Kratky, on the other hand, starts from an entirely different theoretical point of view; ho examines the case, not of scattered particles, but of closely packed particles. 6ince We will now describe the experimental methods, summarize the calcu- lations needed in the elaboration of diagrams, and finally review the first results obtained in the vast domain of these new physical-chomical studies.

Dec 1, 1946

By P. M. Sullivan

At its College Park Metallurgy Research Center in Maryland, the Bureau of Mines has installed and is operating a 5-ton-per-hour pilot plant for continuous mechanical separation of values contained in raw urban refuse. The entire sys tern was assembled using commercially available equipment. The process relies on multistage processing including shredding, air classification, screening, gravity concentration, and electrostatic separation. Compactor trucks deliver raw refuse collected along typical routes in metropolitan Washington, D.C., to the pilot plant. The loads are separated into concentrates of (1) light-gage iron, (2) massive metals, (3) glass, (4) putrescibles and waste combustibles, (5) paper, and (6) plastics. While some refinements remain to be made in the processing system flow-sheet, the data obtained to date have been highly encouraging, indicating favorable economics for commercial-size plants.

Jan 1, 1973