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By Isaac A. Zlochower, Michael J. Sapko, Ronald S. Conti

The Bureau of Mines has developed a system using a high-speed electropneumatic mechanism for the rapid (grab) sampling of dusts and gases during an explosion. The sampling system consists of an aluminum housing that incorporates two 30-cm3 preevacuated glass vials with rubber septums. Upon actuation, the sampling probe needle is driven through the septum with a pressurized air pulse, filling the tube with gas and dust from the mine explosion. After a predetermined time, the sampling probe needle is retracted by a second high-pressure air pulse to its normal (quiescent) state, allowing the sampling tube to reseal. The onset and the duration of sampling are independently variable and controlled by a time-delay relay package. This technique enables the monitoring of pyrolysis-charring in coal particles and the generation and combustion of the pyrolysis vapors in both large- and small- scale explosions. The following results were obtained from full-scale dust explosion tests at the Bureau of Mines Lake Lynn Laboratory: (1) Gas sampling of the leading edge of the flame front shows the large concentration changes, characteristic of the flame front; (2) gas samples taken entirely in the flame zone consist of pyrolysis and combustion products with very low residual oxygen; and (3) the particles collected in the flame zone show signs of extensive pyrolysis and charring.

Jan 1, 1988

By Alla D. Mah

No experimental heat-of-formation value has been reported in the literature for cerium sesquioxide. The heat of formation of bismuth sesquioxide has not been determined in recent years, and the older value was subject to large uncertainty. Accordingly, the heats of combustion of cerium sesquioxide and bismuth metal were measured by the Federal Bureau of Mines. The heats of formation were: ?H°298.15 = -427.01 ± 0.70 kcal. /mole for cerium sesquioxide and ?H°298.15 = -137.16 ± 0.30 kcal./mole for bismuth sesquioxide. The free energy of formation was estimated for cerium sesquioxide and accurately calculated for bismuth sesquioxide. The data were compared with values in the literature.

Jan 1, 1961

By L. F. Christianson

The presence of salt in crude petroleum has been known for many years, but recently the percentage of chloride salts of calcium, magnesium, and sodium produced with some crude oils has increased to such an extent that the removal of the salty compounds is imperative for some refiners and their presence causes considerable apprehension for others. The exact reason for this increase of salts is not known definitely, but in all probability a combination of factors contributes to the condition. The most important are acidizing of wells, development of new fields producing crude oils of greater salt content, and the depletion of old fields with an attending increase in the production of emulsified brine. Due to handling

Jan 1, 1938

By R. S. Dean

In the early days, most smelters were erected in nonarable land and at some distance from settled communities. The movement of population, which resulted in many instances from employment at the smelters, has brought to most smelterman in the United States the problem of preventing damage to plant and animal life in the territory adjacent to the smelters by sulphur dioxide gas (S02). This problem has been met, broadly, in two ways: (1) By diluting and removing the S02 by means of air currents and (2) by converting the S02 to a liquid or solid compound of sulphur and disposing of the compound.

Jan 1, 1937

By R. S. Dean

In the early days, most smelters were erected in nonarable land and at some distance from settled communities. The movement of population, which resulted in many instances from employment at the smelters, has brought to most smelterman in the United States the problem of preventing damage to plant and animal life in the territory adjacent to the smelters by sulphur dioxide gas (S02). This problem has been met, broadly, in two ways: (1) By diluting and removing the S02 by means of air currents and (2) by converting the S02 to a liquid or solid compound of sulphur and disposing of the compound.

Jan 1, 1937

By James J. Dowd

The investigation to evaluate the reserves of coking coal is being made by the Bureau of Mines in three parts: (1) To estimate known (measured plus indicated) recoverable reserves of all coking coal, (2) to upgrade marginal coals through effective preparation, and (3) to study the carbonizing properties of coal and coal blends not now widely used for metallurgical coke making. This is the seventh of a series of reports giving the results of studies by counties under part (1) of the investigation. (See appendix.) This report covers Floyd County, KY., which comprises parts of the Paintsville, Prestonsburg, Harold, Hindman, and Pikeville quadrangles. (See fig. 1.) A base map for each bed in each quadrangle was made to the scale of 1 inch equals 1,200 feet. Maps of mines, locations of drill holes, bed and total coal thicknesses, and the outcrop of the bed were plotted on the maps. With all avail-able data plotted, isopach lines were drawn to limit areas of known unmined reserves in beds up to 14 inches thick, 14 to 28 inches thick, 28 to 42 inches thick, and over 42 inches thick. These areas of coal reserves also were divided into "measured" and "indicated" categories. All areas in each thickness range and in each category, mined-out areas, areas excluded from the estimate but which may contain reserves based only on geologic inference, and areas outside of the outcrop were measured by planimeter on the base maps. Estimates of total reserves 14 inches and more thick and maps for individual beds were prepared from these data.

Jan 1, 1951

By David H. Yee

Because of environmental concerns, the Bureau of Mines investigated an anhydrous chlorination process for the recovery of copper from chalcopyrite, Pelletized concentrate was reacted continuously with chlorine in a vertical shaft reactor at 550° to 750° C to extract copper-iron chlorides and elemental sulfur. The resulting molten metal chlorides drained from the reactor and collected in a receiver while sulfur distilled from the top and condensed in a separate unit. The tests were conducted in a 10-cm-diam reactor constructed of glass and in l5-cm-diam reactors constructed from various refractory materials. A high-alumina ramming mix exhibited the best resistance to molten metal chlorides and elemental sulfur in chlorine atmospheres. A reactor made with this high-alumina refractory was operated for 55 hr under actual chlorinating conditions without suffering any deterioration. Tests results show that more than 96 pct of the chalcopyrite was converted to copper-iron chlorides and elemental sulfur. Good separation of the metal chloride and sulfur products was achieved. After filtration, elemental sulfur of greater than 99 pct purity was obtained.

Jan 1, 1977

By L. F. Christianson

The presence of salt in crude petroleum has been known for many years, but recently the percentage of chloride salts of calcium, magnesium, and sodium produced with some crude oils has increased to such an extent that the removal of the salty compounds is imperative for some refiners and their presence causes considerable apprehension for others. The exact reason for this increase of salts is not known definitely, but in all probability a combination of factors contributes to the condition. The most important are acidizing of wells, development of new fields producing crude oils of greater salt content, and the depletion of old fields with an attending increase in the production of emulsified brine. Due to handling

Jan 1, 1938

By C. M. Flynn

The Bureau of Mines prepared and investigated xanthated sawdust adsorbents to determine their effectiveness in removing heavy metal ions from dilute aqueous solutions, mine-drainage waters, and brines. Stripping of the metal values from the metal-laden adsorbent was also investigated. The treated sawdusts had an adsorption capacity of 0.3 to 0.4 meg/g dry adsorbent for Mn, Co, Ni, Cu, Ag, Zn, Cd, Hg, or Pb from feed solutions with pH 5 to 6. The feed solutions tested included mine-drainage waters and geothermal brine. Effluent metal concentrations as low as 0.05 to 0.1 mg/l were obtained at effluent pH values of 6 to 9. The order of affinity of metals for the sawdust adsorbent is Na«Ca~Mg~Mn<Zn<Ni<Cd<Pb~Cu. The presence of Ca, Mg, or Na in concentrations as high as 2 g/l does not seriously impair the heavy-metal adsorption. Metals were desorbed from the metal-laden adsorbent by elution with dilute mineral acids, sodium cyanide, or salts of ethylenediaminetetra-acetic acid.

Jan 1, 1979

By Henry E. Perlee

In a Bureau of Mines study two-dimensional mathematical equations were solved that describe the transient thermal response of a rock dust particle in a cloud of similar particles in a gas flame&apos;s preheat zone subject to a radiant field from the approaching flame. The description includes both radiant energy absorbed and emitted by the particle and thermal conduction inside the particle and into the surrounding gas environment moving relative to the particle. Two situations were studied; in one the radiant energy incident on the particle is converted to thermal energy at the particle surface, and in the other the radiant energy is converted to thermal energy uniformly over the volume of the particle. The result of the study showed that for a 10-µm-radius particle, a 200-mg 1-1 loading density, and a flame approach velocity of 30 m sec-1, the particle temperature rise was twice that previously calculated by Singer and Cook based on the model of Essenhigh and Csaba. It was further established that under the conditions examined a rock dust particle temperature never increases more than about 200 K before crossing the flame front.

Jan 1, 1976

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 R. V. Lundquist, H. Leitch

The solubility characteristics of three calcium aluminates , 12Ca0 · 7A120½ 3Ca0 A1203 , and 4Ca0 A12 03 Fe2O3 , were determined in water and in solutions of NaOH and Na₂ CO₂ to more clearly define their role in relation to the recovery of aluminum by the lime sinter and the lime - soda sinter processes . The calcium aluminates were prepared by sintering stoichiometric mixtures of CaCO3 , Al2O3 3H20, and Fe 0 at 1,375 ° C. The rates and extent of aluminum extractions were determined . The aluminum extractions from the aluminates were dependent on the presence of carbonate ions in the leach solutions , temperature , time , leach solution composition , and solid - liquid ratio of the slurry . The aluminum extracted from the calcium aluminates in water and in NaOH solutions varied from 4.6 to 22.9 percent . Virtually , complete extraction could generally be obtained for 12Ca0.7A120 and 4Ca0.A12 03 • Fe₂ 03 ; in one instance it was obtained for 3Ca0.A1203 , when an excess of carbonate ions was present over that required for the conversion of all of the calcium in the aluminates into CaCO3 . In some cases of poor aluminum recoveries , extractions could be improved by regrinding and releaching the solid residues .

Jan 1, 1964

By A. Gene Collins

The Bureau of Mines undertook research to determine the bromide and iodide content of Mississippi and Alabama oilfield waters of the Tertiary and Cretaceous Period to determine genetic relationships of the ions, to determine their origin, and to determine their genetic relation to petroleum. The 280 samples were analyzed after a pretreatment to remove interferences. The iodide was oxidized to iodate and was titrated with thiosulfate. The bromide was oxidized to bromate and was determined iodometrically. A computer was used to calculate the correlation coefficients of iodide to bromide and to other ions. The other ions are sodium plus potassium, calcium, magnesium, chloride, bicarbonate, and sulfate. The mineral content of the samples ranged from 52 to 1,760 mg/l for bromide and from 2 to 65 mg/l for iodide. The mean bromide-to-chloride and iodide-to-chloride ratios were 0.0065 and 0.0002. The correlation coefficient matrix and linear plots indicated a definite bromide-to-calcium relationship for the brines investigated.

Jan 1, 1967

By W. E. Cooper

The International Intercalibration and Intercomparison Program (HIP), consisting of several selected laboratories from four countries, held a radon progeny intercomparison measurement at the U.S. Bureau of Mines experimental Twilight Mine on September 12-14, 1988. Grab samples were taken at four different conditions of low and high radon progeny and condensation nuclei concentrations, respectively. The results showed good agreement among all seven participants. The coefficient of variation of all measurements was 4.7%; after minor corrections for flows and some systematic biases, it was reduced to 3.2%.

Jan 1, 1990

By J. L. Eakin

A method was developed by the Bureau of Mines in the laboratory and in the field to relieve capillary waterblocks in gas wells. Impaired gas permeability was improved by this inexpensive chemical treatment which lowers the surface tension of the water held in the capillaries of the formation. Effectiveness of the alcohol-surfactant treatment was tested with a variety of chemicals and with sandstone cores cut from rocks having relatively low permeability. Field tests on 20 gas-producing and storage wells demonstrated the effectiveness and limitations of the method. The productive capacity of some wells was doubled by the treatment. The final test was evaluated by the neutron logging technique for measuring changes in apparent liquid saturation. Maximum apparent liquid saturation was reduced by 52 percent; gas production rate increased from 2.3 to 3.5 MMcfd (million cubic feet per day).

Jan 1, 1965

By W. R. McDonald

Part of the U.S. Bureau of Mines mission is to supply the U.S. mineral industries with information that is useful in planning to meet the Nation&apos;s critical and strategic mineral needs if a national emergency occurs. The Bureau conducted laboratory research including operating a nominal 100 lblh pilot plant to demonstrate the recovery and concentration of chromite by gravity and flotation operations from three northern California mineral deposits. Gravity beneficiation test results show that concentrates contained as much as 52 pet chromic oxide (CrZ03) with recoveries of about 80 pet. Results from the bench-scale unit operations of mineral liberation, tabling, vanning, spiraling, pinch sluice, work index, and thickener area determination tests are presented in this report.

Jan 1, 1990

By M. S. Seehra, R. S. Pandurangi

"The interaction of amorphous silica particles with several hydrogen bonding agents (H2O,, C2H,OH, C,H,NO) was investigated by monitoring the changes in the bulk and surface IR vibrational modes of silica using photoacoustic spectroscopy, It is argued that the intensity of the silanol band at 3747 cm-1 provides (an inverse) quantitative measure of the interaction of surface groups, along with the shift in the broad hydroxyl band, the interaction following the order C,H,NO > C2H2OH > H2O.The use of IR spectroscopy to study the adsorption on solid surfaces is well documented in the literature,"" For example, hydroxylation of a clean silica surface results in the formation of the free silanol group Si-OH, with a sharp IR band near 3747 cm-1. Further hydroxylation produces a broad band near 3500 cm-1, which is believed to result from various hydrogen-bonded silanol bands leading to a multilayered surface structure of few nm.3-6 Earlier studies had indicated a relationship between the surface silanol band and various chemical activities of silica such as cytotoxicity,7-9 catalysis,10-12 and others.13 Recent studies from our group14-in which the intensity of the silanol band and cytotoxicity of silica, heat-treated at various temperatures up to 1095°C, were investigated-have provided a strong correlation between cytotoxicity and intensity of the silanol band.Coating of silica by PVPNO (polyvinyl-2-pyridine N-oxide with the empirical formula C7H8N0), a strong hydrogen bonding agent, is known to reduce the cytotoxicity of silica, presumably by chemically blocking the silanol groups from phospholipids.15 This interaction of the hydrogen bonding agents with the silica can be studied by IR spectroscopy, and Knozinger16 and Rouxlet and Semples17 have used transmission IR spectroscopy to study the effect of various chemicals on the surface IR modes of silica. However, one of the major disadvantages of transmission IR spectroscopy is that the sample preparation (grinding and mixing with KBr and pelletizing) usually distorts the surface modes (see, e.g., Ref. 14) and there is always a doubt about the effect of the sample preparation on the measured properties, In recent years, photoacoustic (PA) spectroscopy has become the technique of choice for studying the IR spectra of samples in their natural state, since no sample preparation is necessary.18,19 Moreover, according to a recent paper,20 the relative intensity of the surface modes in PA spectroscopy of silica particles is much higher than that in transmission FT-IR spectroscopy. Consequently PA spectroscopy is ideal for studying the surface chemistry, In this work, we have used PA spectroscopy to investigate the interaction of three hydrogen bonding agents (C7H8NO, C2H5OH, and H20) with the silica surface by monitoring changes in the surface IR modes, Our results show that the surface IR modes get perturbed to a larger extent than the bulk IR modes in interaction with the hydrogen bonding agents, Moreover, whereas in the earlier studies, the shift of the broad silanol band near 3500 cm-1 was used as a measure of the interaction with hydrogen bonding agents,16,17 here we show that the relative decrease in the intensity of the sharp silanol band near 3747 cm-1 also serves as a quantitative parameter for the relative surface coverage and surface modification, Details of this work are given below,The Cab-O-Sil samples of silica used here were obtained from the Cabot Corporation of Tuscola, IL, In our earlier studies,14,20 we have shown these particles to be amorphous and about 0.05 am in size, For coverage of these particles with H20 and C2H50H, the following procedure was employed. About 5 mg of silica was mixed with 50 mL of the liquid (H2O or C2H5OH) and refluxed for one hour, The remaining liquid was allowed to evap¬orate to dryness and 1 mg of the treated sample was used to collect the PA spectra. In the case of PVPNO, the amount that binds to Cab-O-Sil is taken from the data on quar"

Mar 1, 1992

By Albert J. Rambosek

The objective was to obtain qualitative information on (1 ) the stress field in a core stub at the bottom, or face , of a cored borehole and (2 ) whether , and at what distance , in terms of core diameters from the face of the borehole , relief of stresses in the core is complete . The photoelastic and brittle lacquer techniques of stress analysis were used to determine the pattern of stresses in two- dimensional models , simulating the bottom of a borehole with a projecting stub of core . The core was stress- free at 1-1 /2 core diameters or more from the face of the simulated borehole . The analyses of the isoclinic and isochromatic patterns in the core near the face of the borehole reveal why core occasionally breaks into thin plates , when core or stress - relief drilling is attempted in highly stressed rock masses , such as heavily loaded mine pillars . stub broke away from the bottom in a hydrostatically loaded artificial rock specimen in a manner indicating that core " wafering" can result from tensile stresses developed in the core when a coring bit penetrates the highly stressed rock mass .

Jan 1, 1964

By Howard E. Rollman

South Central United States, an area including Arkansas, Kansas, Louisiana, Mississippi, Missouri, Oklahoma, and Texas, is a net exporter of refractories. Nearly $45 million of these materials was shipped in 1954 from plants in the area, compared with area consumption of $18.5 million. About 88 percent of all refractories production is concentrated in Missouri. The prevalent consumption pattern, however, is one of localized shortages. For example, although Texas uses more than half of the refractories consumed in the South Central United States, production of refractories in Texas is relatively small. Also, the apparent self-sufficiency of the area is in terms of value produced rather than in terms of products consumed. Nearly all of the $6,425,000 nonclay refractories consumed in the area were shipped from other States. Local resources possibly could be developed for making refractories to serve markets that currently are being supplied from outside the area. Since other industries are growing rapidly in the area, the market for refractories is expected to continue to grow--more rapidly than the national market. The Missouri refractories industry is economically important nationally. Nearly one-fourth of the clay refractories produced in the United States are made in Missouri. Moreover, Missouri produces most of the higher grade clay refractories, about 62 percent of the high-alumina refractories, and 85 percent of the superduty refractories. The competitive position of the Missouri refractories industry is strong. The national market for clay refractories and the market in the South Central United States are expected to continue to grow. The ratio of net income to the value of refractories shipped in Missouri is larger than the national average.

Jan 1, 1960

By Cleo Griffith Rall, D. B. Taliaferro

The method for determining oil and water saturations described herein has been used successfully for several years in the core laboratories of the Bureau of Mines. The apparatus constructed according to the original specifications has proved very satisfactory; in fact, it has been widely adopted by core laboratories throughout the petroleum industry. The writers have found that the method gives reproducible results, the degree of accuracy depending largely on the attention to details given by the operator. The relative importance of these details of procedure and the design of the apparatus are discussed in this report. In September 1940, the Bureau of Mines published a report describing a method used in its laboratories for the determination of the water content of oil-field cores. The procedure was essentially the same as that adopted by the American Society for Testing Materials for the determination of the water content of petroleum products, although the apparatus and technique were altered slightly to increase the precision of the method and to adapt it to the characteristics of the material to be tested. The report also contained a description of the method used at that time in the Bureau’s core laboratories for measuring the oil content of a core, utilizing the sample on which the water-saturation determination had been made. The procedure involved the transfer of the weighed sample, from which the water had been distilled and measured, to a Soxhlet extractor and the removal of the remaining oil by means of a suitable solvent. Soon after the report was published, the water-determination apparatus described therein was modified so that both the oil and water contents of a core sample could be determined simultaneously. This method, which has been described by Yuster, is now widely used throughout the industry.

Dec 1, 1946