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By W. J. Kroll

The production of beryllium metal and its alloys is one of the most difficult tasks in metallurgy. In this report we shall examine the progress made in this work- in the last 15 years; taking into account the outstanding publications, including; those of the patent literature, and the information obtained during our 20 years? experience with this metal. The difficulties experienced' in producing elementary beryllium derive from the physical nature as well as from the chemical behavior of the metal and its compounds. Its oxygen affinity is about the same as that of calcium and a little higher than that of magnesium. Its chlorine affinity is much lower than that of magnesium, about equal that, of manganese, and little higher than that of aluminum. The sulfur and nitrogen affinity is probably almost the same as that of calcium for these elements, and beryllium carbide is probably more stable than aluminum carbide, A14C3. The intermetallic affinity of beryllium may be given in descending order, as follows: Nickel - copper - iron. It forms eutectics with -aluminum and silicon as well as with silver. It does not alloy with magnesium and only partly with calcium. Its oxide melts at 2,570° C., but CaO and BaO form readily fusible eutectics with BeO(65).3/ No igneous solvents are known for BeO, which behaves id this regard like Mgo. The beryllium silicate is a strong compound, the aluminete much less so; however, CaO easily displaces Be in the heated mixtures. The Anhydrous chloride hydrolyzes, and it cannot be made from aqueous liquors. It sublimes at 488° C, and melts at 405° C., The fluoride, which, is very Soluble in water, hydrolyzes also, but a kind of oxyfluoride of the approximate formula 2 BeO?5 BeF2 can be made from solutions by dessication. The fluoride melts at 800° C, and boils above 1,100° C. It forms very stable double fluorides with alkalifluorides, which have very low melting points and are fairly soluble in water. They are more stable than the analogous fluosilicates and the sodium fluoaluminate cryolite.

Jan 1, 1945

By E. R. Cole

One objective of Bureau of Mines recycling research is to devise technology that enables recovery of metals and minerals from wastes. From October 1982 through September 1985, researchers at the Bureau and at the University of Missouri Rolla (contract H0222002) investigated the use of nonferrous flue dust with varying Zn contents (11 to 66 pct) as a source of Zn for electrogalvanizing steel wire. The waste dusts used were from a secondary Cu smelter, a brass smelter, a Pb smelter, and a water treatment plant. The dusts were leached in H2S04, and the leach solutions were treated to make electrolyte for electrogalvanizing steel wire using soluble Zn anodes. Cyclic voltammetry was used in an inno-vative method to evaluate the quality of the electrolytes used for elec-rogalvanizing. After electrogalvanizing, the wire was drawn on a labo-ratory draw bench to simulate industrial practice. Corrosion resistance was measured by a number of electrochemical techniques and by the stan-dard ASTM salt-spray tests. After successful bench-scale tests, the process was demonstrated in an industrial pilot plant. Results indicate that nonferrous flue dusts can be used as a source of Zn for electro-galvanizing if certain impurities are either partially or completely removed from the starting electrolyte.

Jan 1, 1987

By R. Wiebe

During a recent investigation the authors were interested in determining: (1.) How many points were necessary to locate the deviation curve for copper-constantan thermocouples within an accuracy of about 0.05° C., used in connection with the "standard" thermocouple of L. H. Adams. (2.) Whether copper-constantan thermocouples showing considerable deviations from the "standard' were consistent throughout their calibration. (3.) How reliable the extrapolated portion is - that is, the interval between -183 and -220° C. of the "standard" thermocouple. It seems that a calibration between 0 and -193° C. can be made within the stated accuracy by determining experimentally the e.m.f. of the particular couple at -78.50°, the normal sublimation point of carbon dioxide, and at -182.97°, the normal boiling point of oxygen. Substituting the values found for the two fixed points in the simple quadratic. Equation

Jan 1, 1931

By Roy E. Peterson

The Bureau of Mines has been developing and evaluating methods for beneficiating the large deposits of nonmagnetic (oxidized) taconite located on the western Mesabi Range. In this segment of the research, a sample representing about 0.5 billion tons of nonmagnetic taconite from near Grand Rapids, Minn., was beneficiated using a reduction roasting, magnetic separation, flotation process. The sample contained 32.1 pct iron and 49.1 pct silica. Tests were conducted both on a bench scale and with a 1,000-lb/h pilot plant. In the bench-scale research a con-centrate containing 69.0 pct iron and 4.5 pct silica was produced with an iron recovery of 82.1 pct. In the pilot plant, reduction roasting was conducted in a 35-ft kiln using lignite as the reductant and major source of fuel. Dust from the kiln exhaust was pelletized and recycled to the kiln. The roasted taconite was beneficiated by magnetic sep-aration and flotation to produce a product containing 67.9 pct iron, 5.5 pct silica, and 69.7 pct of the iron in the kiln feed. The cyclone separation in the grinding circuit was sharpened by demagnetizing the cyclone feed in a 400-Hz, 1,000-Oe magnetic field.

Jan 1, 1983

By W. G. Messner

Pipelines for transporting crude oil and refined products in the United States totaled 189,982 miles on January 1, 1959. This mileage was less than a 1-percent increase from the 1956 total of 188,540 miles. During the three-year period (January 1956 - January 199), 14,886 miles of new pipe and 10,649 miles of secondhand pipe was laid. Pipe taken up in the same period was 24,093 miles. The facts regarding pipeline mileage were obtained by the Bureau of Mines from pipeline companies and information provided by the Interstate Commerce Commission. Crude-oil gathering lines, as of January 1959, were 40 percent of the United States pipeline mileage and totaled 75,182 miles, an increase of 1,656 miles during the three-year period. Crude-oil trunklines totaled 70,317 miles or 37 percent of the United States pipeline mileage, a decline of 8,277 miles from the 1956 total. Some of this loss is attributed to the converting of crude lines to refined products. Refined product lines in January 1959, totaled 44,483 or 23 percent of the United States mileage, an increase of 8,063 miles during the three-year period.

Jan 1, 1959

By S. H. Ash

The Pennsylvania anthracite-mining region is the only one in the world of major magnitude. As the deposits of anthracite in the United States are limited virt113.lly to Pennsylvania, the difficulties of this industry have been commonly considered a State rather than a national problem. However, there is also national interest in the conservation and wise utilization of all fuel resources and in the control of interstate waterways. The anthracite industry is confronted with the very se:;-ious :problem of accumu.lation of water in many of the mines. This problem must be solved soon if progressively higr-er mi~ing costs are to be avoided. The water proble~ cannot be solved by the operating compa,nies without State or Federal aid, or both, owing to the magnitude of the work requir~d, diversity of interests of the coal ana surfa.ce ovmerships, hazard to the whole mining community, and interests affec~ed outside the mining region. The cost of abati~ the ever-increasing_surface seepage to mine workings and of handling this seepage once it }3s occurred is beyond the economic resources of most ope~ating ma.'18.gements. The data in this paper giving the high lights of the water problem and indicating what appears to be a step in the right direction are based upon observations made during the past year that the industry desires and believes it is to the npublic interesttr to keep mine workings free of flood end surface waters.

May 1, 1941

By C. G. Storm

Permissible explosives are those that have passed the tests pre- scribed by the Bureau of Mines for explosives intended for use in coal mines, and are therefore recommended by the bureau as suitable for this class of work when used under the prescribed conditions. The tests for permissible explosives and the conditions prescribed for their use are described in Miners' Circular 6 of the Bureau of Mines. Up to June 1, 1915, 168 explosives had been classed as per- missible explosives; 133 of them were then on the bureau's "per- missible list" and 35 had been withdrawn by the manufacturers. In addition to the required physical tests, each explosive is sub- jected to a complete chemical examination in order that its exact composition may be known and also that the composition of future samples of the same explosive collected in the field may be compared with that of the sample which originally passed the bureau's tests, for by such comparison it may be possible to ascertain whether or not the explosive as supplied to the miner is still "permissible." This bulletin is published primarily for the purpose of informing manufacturers of such explosives as to the methods used by the Bureau of Mines in the analysis of samples received for tests to determine their permissibility. Such information may be of value in cases of possible controversy over the results obtained in the analysis of a field sample as compared with those obtained in ana- lyzing the sample originally tested by the bureau. Also, a descrip- tion of the methods used by the Bureau of Mines in the analysis of explosives should be of assistance to the many chemists engaged in similar analytical work.

Jan 1, 1916

By Homer J. Ballinger

The Alma, Degraff and other mines controlled by the Mon-Ark Mining Co. comprise one of the more important groups of zinc-lead mines in Christian County, Mo. The mines were first operated in .1857 and produced more than 5 million pounds of lead from rich, shallow ore deposits. Recent exploration and development led to the discovery of zinc sulfide ore at a depth of 165 to 214 feet in the northern part of the Alma mine. After examination of these mines in September 1942 by Bureau of Mines engineers, investigation of the extension -of the Alma mine and of the depth of mineralization at the other mines appeared justified in order to encourage the production of additional zinc and lead for war purposes. Twenty-nine churn-drill holes totaling 6.463 feet of bore were completed by the. Bureau from September 1943 to January 1944.

Jan 1, 1948

By Jr. Reistle

The tests reported in this paper were made in the East Texas field in the summer and fall of 1932 as a part of the Bureau of Mines study of the operation of flowing wells and reservoir performance; and to determine, if possible, the minimum reservoir pressure necessary to produce the wells in this field by natural flow through different sizes of flow strings. The minimum reservoir pressure that would be required to Maintain natural flow through 2 1/2-inch tubing was determined experimentally for the existing energy conditions in the East Texas field. With the present available data, however, it is impossible to predict accurately or to determine by calculation the necessary energy requirements for maintaining the vertical flow of oil and gas mixtures under all conditions. Although some valuable data were obtained which seem to have application to the solution of problems involving vertical flow, this important research of the petroleum industry is so involved that more study of the complicating factors influencing the flow of oil-gas mixtures through vertical pipes is required.

Jan 1, 1933

By E. S. Longfellow, S. H. Katz

Poisonous hydrocyanic acid gas (HCN) is sometimes evolved in dangerous quantities from cyanides used in metallurgical and chemical operations. This gas is much used for fumigating buildings, ships, greenhouses, and such commodities as grain and cotton to destroy rats, mice and insect pests. Wherever cyanide fumes are evolved, thorough ventilation is necessary in order to render the sur- rounding air safe to breathe. Many persons have been killed by entering tanks and fumigated places too soon, and a simple test for this gas would promote safety. In view of the need for an easy method for quantitatively determining HCN in air, the three color reactions used originally for testing HCN in solution tions *** were modified and adapted. The reactions employ (1) picric acid (CH(NO2)3OH) which is yellow but combines with hydrogen cyanide to form a red- purple dye, isopurpuric acid****; (2) phenolphthalin (CH1604), which is a reduc- tian product of the phenolphthalein (CH4) used for acid indicator, this colorless substance is oxidized***** by presence of HCN to pink colored phenolph- thalin; and (3) guaiacum which oxidized from colorless to blue******. Phenolph- thalin and guaiacum require the presence of copper compounds which catalize the color formation by reduction of cupric cyanide. The chemical processes involved *Associate physical organic chemist, Bureau of Mines, Department of the Interior. **Assistant gas chemist, Bureau of Mines, Department of the Interior. 2014 20 *** Kohn-Abrest, E., Notice toxicologique sur les gas: Arnales des Falsifica- tions, vol. 8, 1915, pp. 215-35. (Tested air with picric acid and guaiacum papers). **** Élasiwietz, H., Ueber eine neue Zersetzungsweise der Trinitrophenylsaure: Anal. der Chemie, vol. 110, 1859, pp. 289-303. ***** Weehuizen, F., Phenolphthalin as reagent for HCN: Pharmaceutrisch weekblad, Utrecht, vol. 42, 1905, pp. 271-2. Abstract, Jour. Chem. Soc., vol. 88, part 2, 1905, p. 489. ****** Schonbein, C. F., Ueber den thatigen Zustand der Helfte des in dem Kupfer- oxydenthaltenen Sauerstoffs und ein darauf beruhendes hochst empfindliches Reagens auf die Blausaure und die loslichen Cyanmetalle: Jour. fur. Praktische Chemie, vol. 106, 1869, pp. 263-70.

Jun 1, 1923

By K. L. Rubow

"IntroductionAir sampling for airborne contaminants requires a system for moving air, a collection method, and a procedure to determine the quantity of contaminant collected. Because occupational exposure limits and air quality standards frequently are expressed in terms of concentrations, a method of determining the volume of air sampled is also needed. The four principal components in a sampling train are shown in Figure 12-1. The inlet admits the air sample into the train; the collector(s) separates the gas, vapor, or particles from the air; the flowmeter measures the rate or total quantity of air sampled; and the pump (air mover) provides the suction required to draw an air sample through the train. Inlet sampling considerations are discussed in Chapter 21. Various types of collectors are described in subsequent chapters. Flowmeters are discussed in Chapter 7.This chapter will describe the air mover portion of the sampling train and air sampling systems that contain three or four components in a convenient package. The chapter consists of two parts. The first part contains a brief description of the different types of air movers and air sampling systems. The second part consists of tables and figures showing detailed information on a wide variety of commercially available air movers and sampling systems. ient size is filled with a liquid in which the suspected contaminant is insoluble. When the liquid is allowed to escape from the vessel, it is replaced by air from the atmosphere to be sampled. Such an air sample is an integrated sample rather than an instantaneous sample because the mass of fluid requires a finite time to empty. In fact, by employing a large vessel with controlled drainage, this method can be used to move air at low flow rates through a sample collector for extended intervals. Additional discussion of this method can be found in Chapter 17."

Dec 1, 1996

A knowledge of the mechanics of wave propagation through the earth is essential if reliable communication systems are to be designed for coal mine environments. To obtain a reliable basis from which accurate propagation predictions could be drawn, a series of theoretical studies have been prepared for the US Bureau of Mines by Mr. Ramsay Decker of Spectra Associates, Inc. through a subcontract with Collins Radio Group. These reports formulate the analytical techniques from which we may derive frequencies and antenna configurations that yield the optimum signal-to-noise ratios over the greatest distances in mine environments. The reports of sections 2 and 4 deal with analytical techniques for determining the signal-to- noise ratio within a mine environment for loop-to-loop and line source-to-loop antenna con- figurations. The analytical results of these reports were then implemented into computer programs to obtain predictions concerning through-the-earth signal propagation. These preliminary predictions are based on noise data compiled by Bensema, Maxwell and Stone, and WVU prior to the extensive research conducted by the National Bureau of Standards (NBS). These initial measurements indicated a 20- to 30-dB lower noise level than that measured recently by NBS. The recent NBS data is that used by Collins in the final predictions. The following outline indicates the order and subject matter treated in the subsequent sections: Section 2 - Signal-to-Noise Analysis for Loop-to-Loop Mine Communications Section 3 - The Horizontal Electric Dipole Section 4 - Signal-to-Noise Analysis for Down-Link Line Source Mine Communications Section 5 - LF Communication Section 6 - The Application of Recent NBS Noise Data to Mine Communications Section 7 - Analysis of Mine Communication Propagation Programs

Nov 15, 1974

By C. J. Wilhelm, John M. Devine

"Hydrogen aulphide associated with natural as was noted as early as at Point Albino, Canada. 4 The presence of this impurity was recognized also in other of the earlier oil and gas fields, although the occurrence ma by no means common. However, in recent years, with the development of the producing zones of west Texas and the Texas Panhandle the production of ""sour"" crude has increased greatly and hydrogen sulphide has proved a generally troublesome factor-frequently a major problem—in the drilling and operation of any wells in those areas.The problems arising from the drilling and producing of oil or gas wells in hydrogen-sulphide areas, fall under two general divisions: safety problems and corrosion problems. Mention is made of a third division which is closely related to the other two, that of treating--or the development of processes for the removal of hydrogen sulphide. From the standpoint of safety and health hazards, hydrogen sulphide in the petroleum industry has been discussed in a number of publications. 5 Likewise, the problem of hydrogen-sulphide corrosion of production equipment has been given considerable attention in the literature.6"

Sep 1, 1931

By C. M. Mason

The methods currently used by the Bureau of Mines to evaluate the sensitivity, strength, incendivity, gaseous products, and physical properties of explosives and hazardous chemicals are described. Included are the tests used to evaluate explosives which arc certified as permissible for use in underground coal mines.

Jan 1, 1972

By R. W. Huber, R. C. Wiley, V. C. Petersen

"Three arc- melted ingots, two of a t itanium-7 percent manganese all oy and the third of unalloyed titanium, were forged and rolled into 3/ 4-inch plate; comparative data were obtained on these processes. The finished plate, part of which was used by the Naval Bureau of Ordnance, was tested for mechanical and other properties.These properties were correlated with sponge purity, forging technique, rolling temperature, and cooling rate from the rolling temperature. For the alloy material, transformation data were obtained, and their age-hardening characteristics were studied. The temperature-impact relationship was established for rolled sections from all three ingots.INTRODUCTIONArc -melted ingots of unalloyed titanium and a titanium-manganese alloy were fabricated into plate under closely controlled conditions by personnel of the Metals and Alloys Section, Physical Metallurgy Branch, Bureau of Mines, College Perk, Md. This program was cosponsored by the Naval Bureau of Ordnance. Bureau of Mines interest lay in correlating the processing procedures with the mechanical properties of the finished plate.Considerable data have been published recently on constitution diagrams and properties of titanium-manganese alloys in genera1. 3/ 4/5/6/ However, little if any correlation between processing schedules and end results has been published, particularly with respect to the present commercial production of the proprietary titanium manganese alloys . Several factors in the production of titanium and titanium alloys have a pronounced influence on the physical and mechanical properties of the finished product: (1) The degree and nature of impurities in the base materials, ( 2) the amount of impurities introduced during the melting cycle and their distribution, (3) the homogeneity of the alloy, (4) forging, (5) rolling, and ( 6) final heat-treating cycles. All of these item£ are important from a metallurgical standpoint in producing the desired end properties in the metal."

Mar 1, 1955

By Tilman M. M.

The effects of substituting cobalt for nickel on the acid corrosion resistance of two types of austenitic stainless steel were determined. Cobalt substitutions to a maximum 2.2 weight-percent were made in types 302 and 309 stainless steels. Total immersion corrosion tests were made in 10 volume-percent hydrochloric acid, and boiling-acid tests were conducted in 65 weight-percent nitric acid and in undiluted glacial acetic acid. For modified type 309 in acetic acid, corrosion rates decreased for additions greater than 0.57 weight-percent cobalt. Corrosion rates increased as cobalt was increased up to about 1 weight percent for modified type 302 in nitric and hydrochloric acids and for modified type 309 in nitric acid, but these rates decreased with a further increase in cobalt content. A gradual increase in corrosion rates with increasing cobalt content was shown for type 302 in acetic acid and for type 309 in hydrochloric acid. Cobalt substitutions in larger amounts (above a ratio of 8 Ni to 1 Co) may increase the corrosion resistance of the austenitic stainless steels.

Jan 1, 1965

By Roy T. Sorensen

The Bureau of Mines has investigated the recovery of cell-grade alu-mina by RCI leaching of calcined kaolin in the alumina miniplant at its Boulder City (NV) Engineering Laboratory. Classification and thickening were used for separating aluminum chloride leach liquor from the siliceous residue generated in the acid leaching step of the clay-HCI process. Coarse solids were classified from fines at 115 mesh and countercurrently washed in three additional spiral classifiers. Fines were treated in a conventional five-thickener, countercurrent decantation circuit. When this method was applied to the solids-liquid separation of slurry from RCI leaching of minus lO-mesh calcined kaolin, 75 pct of the residue reported as classifier sands and 25 pct as thickener underflow. Predicted individual classifier and thickener area requirements were 6 and 25 ft2/tpd, respectively. Total thickener circuit flocculant requirement was 2.4 lb/ton solids. Aluminum chloride pregnant liquor was produced that analyzed 8.4 pct A1203 and contained more than 97 pct of the alumina in the liquid phase of the slurry. Bench-scale settling tests were used to correlate fines content of leach residue to thickener area and flocculant requirements.

Jan 1, 1983

By R. F. Abernethy

A chemical method of determining microgram quantities of arsenic in coal was investigated by the Bureau of Mines to supplement a semiquantitative spectrographic method of determining arsenic in coal ash. In accordance with a method recommended by the International Organization for Standardization, 1-gram samples of coal are decomposed by wet oxidation with boiling sulfuric acid (H2S04) and nitric acid (HN03) to remove the organic matter. After heating to fumes of SO3 to remove HN03, the arsenic is separated as arsine by the action of zinc in H2S04 solution. The arsine is absorbed in dilute iodine solution in which the arsenic is determined colorimetrically by the molybdenum-blue reaction. Two modifications of the method for obtaining the arsenic in solution, in addition to the wet oxidation method, give satisfactory results. The modifications are (1) furnace ashing with MgO added to the coal, followed by treatment with H2S04, and (2) extraction of arsenic from the coal by dilute HNO3 without ashing. Float-and sink-tests show that arsenic is associated mainly with mineral matter in the three coals examined. High-temperature ashing tests show that very little arsenic is volatilized from coal ash below 1,000° C, but it is virtually all removed from the ash at 1,300° C.

Jan 1, 1968

By D. S. Burgess

A commercially available Halon 1301 extinguisher has been evaluated as part of an explosion-suppression system for use in coal mines. Studies were made both of the dispersion pattern of the Halon 1301 at an initial pressure of 280 psig, and of the efficacy of this suppressant against 9.5 percent methane-air flames. These flames were quenched successfully only when the suppressant was applied before the fireball diameter exceeded 18 inches.

Jan 1, 1971

By William J. Campbell

This study was a part of two programs: The first, to develop and evaluate high-temperature refractories; the second, to investigate reaction-rate kinetics and phase equilibria in the sinter step of the lime-soda process for the recovery of alumina. High-temperature X-ray diffractometer techniques are to be used extensively in both programs. This paper summarizes developments in the field of high-temperature X-ray diffractometers through 1959, evaluates various furnace designs, and describes briefly the X-ray diffraction facilities of the Federal Bureau of Mines. A more detailed description of the equipment and its calibration is planned in a future paper on thermal expansion and phase inversion of rare-earth oxides.

Jan 1, 1961