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By W. L. Anderson

Standard tellurium analytical procedures were modified to obtain the greater sensitivity needed to support a survey of tellurium resources by the Bureau of Mines. Resulting volumetric and spectrophotometric methods for determining tellurium in all types of tellurium-containing materials are described. Sample decomposition and preliminary separations of interfering selenium, gold, and silver are the same in both procedures. The volumetric method is applicable to samples containing a minimum of 10 parts per million of tellurium, In this method the tellurium is reduced to elemental form, and the colloidal suspension is titrated with 0.01 normal iodine solution. The weight of sample for analysis, from 0.25 to 10 grams, should be selected so that the sample contains 0.1 to 5 milligrams of tellurium. To insure accuracy, duplicate samples should be run and the results averaged, particularly on samples of low tellurium content: The limit of determination is 0,001 percent tellurium, which is equivalent to 0.1 milligram of tellurium when using a 10-gram sample. The spectrophotometric method is particularly applicable to low-tenor materials containing from 0.5 to 50 parts per million of tellurium. Up to 10 gram samples are required for making accurate determinations in the low-concentration range. The sample used should contain between 5 and 100 micrograms of tellurium. The turbidity of a colloidal suspension of tellurium prepared from such a sample is determined in a spectrophotometer .t at a. wave-length of 440 millimicrons, and this value is compared with those of standard samples containing known amounts of tellurium.

Jan 1, 1963

By R. Barany

The heats of formation of goethite, ferrous vanadate, and manganese molybdate at 298.15° K were determined by solution calorimetry. For formation from the elements, the heat values were -133.7 ±0.3 kcal/mole for goethite, -453.8 ±0.5 kcal/mole for ferrous vanadate, and -284.8 ±0.2 kcal/mole for manganese molybdate. For formation from the oxides, the heat values were -0.9 ±0.1 kca1/mole for goethite, -19.4 ±0.3 kca1/mole for ferrous vanadate, and -14.6 ±O.l kcal/mole for manganese molybdate.

Jan 1, 1965

By [F. P. ] Stambaugh

Results of research on the hydrothermal precipitation of zirconium oxide from the Bureau of Mines' zirconyl chloride-sulfate strip liquors indicate that nuclear grade material can be prepared by this process. Greater than 99% of the zirconium value can be precipitated at 250-260°C in short (5-10 minutes) reaction time without consumption of acid value of the liquor. Thus, precipitation of zirconium dioxide on a continuous basis, i.e., the zirconium dioxide is precipitated in a continuous mode of operation by pumping the strip liquor through a heated pressurized reactor and recycle of the acidic (spent) liquor to the process stage are favored. The results of accompanying studies of liquod/solid separation, product washing and dewatering, product purity, and chlorination of the product are presented and discussed.

Jan 1, 1980

By T. E. Green, E. F. Spano, W. J. Campbell

A combined ion exchange X- ray spectrographic method was evaluated for the determination of 11 metallic elements in high - purity tungsten : Aluminum , calcium , chromium , cobalt , copper , iron , magnesium , manganese , nickel , titanium , and zinc . Copper , nickel , and manganese in the 5- to 100 - microgram range ( 1 to 20 parts per million based on 5 - gram samples of tungsten ) , calcium in the 10- to 100 - microgram range , and cobalt in the 5- to 20 - microgram range can be determined within an accuracy of ± 10 percent of the amount present . Limits of detection of these elements are 0.05 to 0.14 microgram . The overall method was unsatisfactory for the determination of aluminum , chromium , iron , magnesium , titanium and zinc in tungsten .

Jan 1, 1964

By A. A. Berk

The Bureau of Mines devised a test nipple for the field study of corrosion in the condensate-return lines of Federal heating plants. Corrosion surveys, made with this device, showed that the deterioration of the piping was caused principally by carbonic acid in the steam condensate. Corrosion problems were brought under control when the carbonic acid concentration in the condensate was decreased. In many instances, this was effected by decreasing the total carbon dioxide content of the feedwater; in others, the condensate acidity was neutralized with volatile, alkaline chemicals. Filming treatment with octadecylamine, reported successful in controlling return-line corrosion in industry, was much less effective in Federal area-heating plants. Laboratory study by the Bureau disclosed that octadecylamine is unstable in heating systems. Analytical methods were developed for this chemical and its degradation products in heating-plant condensate. Field surveys, in using these methods, confirmed the instability of the filming material. Laboratory tests showed that the degradation products are not useful film formers. Since filming treatment has little effect on condensate corrosivity, the piping was corroded where it was not coated by the treatment chemical.

Jan 1, 1962

By R. H. Nielsen

A new, cheaper precipitation scheme has been developed to produce purified zirconium oxide, Technical-grade sulfuric acid is used to precipitate a basic zirconium sulfate from a hot dilute hydrochloric acid solution. With close control of temperature, pH, and zirconium - sulfate ratio, excellent purification and complete zirconium recovery can be attained. The process has been successfully applied for 3 months and has proved to be a more satisfactory procedure than the ammonium phthalate process used previously. INTRODUCTION The Northwest Electrodevelopment Laboratory of the Federal Bureau of Mines has developed and improved the Kroll process for the production of pure ductile zirconium and hafnium. metal. Since 1946 over 1 million pounds of zirconium sponge metal has been produced, mostly high-purity material for the Atomic Energy Commission

Jan 1, 1956

By A. E. Sands

The Bureau of Mines, S. Department of the Interior) at, its Morgantown., W. Va., station, operating under a cooperative agreement with West Virginia University, is conducting research and development work on the problem of producing synthesis gas from coal. An important part of this work is the study of the gas purification necessary to meet the rigorous standards required to render the gas suitable for use in the Fischer-Tropsch synthesis of liquid fuels. One of the most detrimental impurities is sulfur in all forms, the maximum amount that can be tolerated being one-tenth of a grain per hundred cubic feet. Concentrations as low as this require the use of precise analytical methods to evaluate the performance of processes used for removing sulfur. At the same time the analytical methods should be rapid in order to reveal the failure of purification before damage to the expensive synthesis catalyst results. Although sulfur in unpurified gas is generally present as hydrogen sulfide and as organic sulfur compounds, the latter may be converted to hydrogen sulfide for analytical purposes. Thus a suitable method for the determination of traces of hydrogen sulfide may also be used for the determination of organic sulfur.

Jan 1, 1949

By K. O. Bennington

The thermodynamic properties of hedenbergite, of composition [(Ca0,9516) (Mg0,0583Fe2+0.7134 Fe3+0.0934 Mn0,1366) (Si206)], were experimentally determined at the Bureau of Mines. The standard enthalpy of formation determined by hydrofluoric acid solution calorimetry is AHf298 = -680.96±0.855 kcal/mol. The standard enthalpy of formation from the oxides is AR-96 = -24.55±0.485 kcal/mol. Low-temperature heat capacities were determined by adiabatic calorimetry from 12.3 to 300.1 K. The derived standard entropy is S-98 - 41.218±0.148 cal/mol-K. High-temperature heat capacities were measured with a differential scanning calorim¬eter from 397 to 1,147 K. These experimentally determined data were combined with data from the literature to calculate the Gibbs energies of formation and equilibrium constants of formation over the temperature range of measurements. Standard enthalpies of formation are given as a function of temperature. The standard Gibbs energy of formation at 298.15 K is AGf298 = -641.90±0.86 kcal/mol.

Jan 1, 1984

By C. A. Alien

The increasing activity in oil shale has had a tendency to direct the attention of the industry to any substance from which gasoline or other oils can be secured . Cannel coal for many years has been known, as a source of oil and formerly it was the only substance from which kerosene was obtained . The name of coal oil was given to kerosene because it was derived from cannel coal before any flowing wells were brought in in the United States . In an isolated region in Southern Utah there is an unusually thick and clean bed of cannel coal which laboratory experiments indicate can be made to yield about seventy gallons of oil to the ton . This coal was first described in Bulletin 341 of the United States Geological Survey under the title of Colob coal field . This field lies at the western and southern base of the Colcb plateau and extends from the town of Cedar City southward to Kanarra and then southeastward to the town of Mount Carmel . Cedar City is 35 miles south of east from Lund on the Los Angeles and Salt Lake Railroad which is the nearest railroad point . Mount Carmel is about 90 miles south of Marysvale , on the Denver and Rio Grande Railroad , which is the nearest railroad point from the eastern end of the field . The Colob coal occurs in Lower Cretaceous rocks and a number of wagon mines have been opened on the seam in the vicinity of Cedar City , Kanarra , and Mt. Carmel , but between these places the field has been very little prospected . The cannel coal , so far as known at present , is limited to a small area on the head waters of the north fork of the Virgin River in Township 39 and 40 South , Range 9 East . In this region it occurs as a bed 5-1 /2 feet thick over which lies a layer of bituminous coal 2 feet and 5 inches thick .

Feb 1, 1921

By John J. Henn

As part of the U.S. Department of the Interior programs on rutile, authorized by the Office of Emergency Preparedness in June 1967 under provisions of the Defense Production Act, the Bureau of Mines reviewed available literature on major proposed processes for producing rutile substitutes. The processes are grouped according to the major processing step, and important operating features are described. Sixty-one references are cited.

Jan 1, 1970

By Ralph V. Higgins

The present methods of appraising the long-range performance of oil reservoirs are based upon physical properties of the crude oil and the permeability of the reservoir rock. By means of these methods the performance of a reservoir may be estimated throughout its entire life. Before these methods were used, the future performance was estimated mostly by extrapolating pressure-decline curves -a method that is satisfactory for extrapolating only for a short period into the future. One factor that affects satisfactory long-range prediction of reservoir performance is the extent to which small changes in the physical properties of the oil and differences in the choices of relative permeability influence the calculated oil recovery. Selection of the physical properties of the samples to represent those of the oil and rock for the entire reservoir is difficult. This report is concerned with the error in calculated recoveries that may result from these inherent difficulties.

Jan 1, 1956

By W. W. Simpson

The Bureau of Mines conducted research to determine the effects of potassium trithiocarbonate (KTTC), a degradation product of potassium ethylxanthate (KEX), on flotation of chalcopyrite and molybdenite. Small amounts of KTTC were identified in fresh and aged solutions of KEX using thin-layer chromotography. Hallimond tube flotation tests on pure minerals showed that KTTC acts as a weak collector for chalcopyrite. Both KEX and KTTC tend to depress molybdenite, but the depression effect is easily overcome by addition of a small quantity of fuel oil. The results of the Hallimond tube tests were confirmed in batch flotation tests using a porphyry copper ore.

Jan 1, 1983

I do not regard the criticism by Rankin of my work as valid or even meaningful. I strongly reject the assertion by Rankin that my results are invalid. As stated in my paper, the equation to solve (in e. m.u. ) is: [ ] where n2 =4 ps? . This may be rewritten as three scalar equations in Cartesian coordinates, one of which is [ ] The equation to be solved is the diffusion equation, and it is not appropriate to consider waves in this context. In the method a point-wise solution to the problem is approximated. As discussed in my paper the approach taken at discontinuities in conductivity is to choose the normal component of [E] at the discontinuity as the average of the normal components on either side of the discontinuity. This is similar to the well-known assumption made in obtaining Fourier series representations for piecewise continuous functions (Pipes, 1958; p. 51). In the geophysical problem this means that the discontinuity is approximated by a transition zone, which is a very good approximation for such cases. By using this approach, both the values of the function and its derivatives give a good estimate for those associated with the physical situation. It is not apparent and Rankin has not shown that "all the field components and the derivatives are grossly distorted in the region about the boundary" for geophysically realistic situations. He has given no evidence to support his assertation that the results are "invalid". Although Rankin declares that one cannot calculate the electric components from the magnetic, in his discussion he has not stated why this is so. After once calculating the magnetic components the electric components may be calculated, but one must insure that the initial solution is accurate enough to prevent significant round-off errors.

Jan 1, 1973

By Thomas C. Mowatt

Chemical and petrographic studies were carried out on selected tin-bearing rock samples of contact-metasomatic origin from the Cassiterite Creek and Brooks Mountain areas, Seward Peninsula, Alaska. The tin content of rocks ranged from 0.39 to 8.9 pct. Leaching with a 20 pct hydrochloric acid solution released from 19.3 to 67.9 pct of the tin. Cassiterite was not observed in the rock samples. These results are significant with regard to tin recovery and reserve delineation in these and similar occurrences. Part of this leachable tin may be associated with metasomatic borate minerals.

Jan 1, 2011

By R. R. Hornor

Due mainly to conditions brought about by the war , the metal mining industry in this country is now passing through one of the most critical stages in its history , and is confronted by new problems upon the solution and adjustment of which depends , in a large measure , its future welfare and prosperity . The chief factors contributing to the cost of production are the cost of labor and supplies . It is conceded by our leading mine operators , managers , and engineers that any material reduction in the cost of labor or supplies , within possibly the next two or three years , cannot be anticipated , anl it is not thought likely that pre - war prices will ever again prevail . This being true , the mine operator must look in some cther direction to effect economies that will lower production costs . If this cannot be accomplished it will mean , in many instances , that mines and metallurgical works will have to be closed and abandoned , which will tend to disorganize the entire industry . How to lower production costs and still maintain the present high standard of wage , is the problem that is engaging the serious attention of mine operators and managers over the entire country . In As a solution to this problem it is thought that the most promising field of investigation lies in the direction of systematizing and standardizing mining practice , so as to effect economies in the use of both labor and materials . other words , to eliminate , in so far as possible , unproductive effort and waste and thereby secure a maximum of productive results , It is not the idea to speed up work or to demand a greater effort on the part of the workman , but rather so to systematize and standardize the various under ground operations that his energy will be directed into more useful and productive channels ,

Dec 1, 1919

By Lloyd H. Banning

Crucible-smelting tests at the Northwest. Electrodevelopment Laboratory and a pilot-plant test on electric smelting of western phosphate rock for the Westvaco Chlorine Products by the Tennessee Valley Authority indicated that the small vanadium content of the rock is concentrated in the ferrophosphorus by-product of Phosphorus smelting. This research is concerned' mainly with recovering vanadium and phosphorus froth the ferrophosphorus produced from western phosphate rock. Exploratory tests were made of several methods of treating vanadiferous ferrophosphorus. Attempts to separate vanadium as a carbide dross by saturating molten ferrophosphorus with carbon were unsuccessful. Volatilization of phosphorus from ferrophosphorus was accomplished to some extent, both with and without addition of sulfur in several forms, but elimination of phosphorus was not complete. Brief testing in a small experimental converter on oxidation of vanadium and phosphorus; into a slag by blowing with air showed promise. A method that comprised fusing vanadiferous ferrophosphorus mixed with soda ash under oxidizing conditions gave encouraging results and was tested beyond the preliminary stage. A slag product of the fusion contained most of the phosphorus and vanadium as water-soluble sodium phosphate and. virtually water-insoluble sodium vanadate. After leaching the sodium phosphate froth the slag, the leach residue was reroasted with soda ash and salt. This roasted product was leached again with water to extract the vanadium.

Jan 1, 1951

By Thomas E. Green

A combined solvent extract ion-spectrophotometric method for the determination of as little as 1 ppm of copper in tungsten metal or tungstic oxide has been developed and evaluated. Metallic samples are converted to tungstic oxide by treatment with hydrofluoric and nitric acids. The oxide is then dissolved in sodium hydroxide, and the copper is extracted as the colored neocuproine complex. Total elapsed time for the analysis is approximately 1-1/2 days; however, actual working time for a group of six or eight determinations is less than 4 hours. Precision at the 2-ppm level is better than 0.1 ppm.

Jan 1, 1963

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 J. Roth

The purpose of the present study is to increase the safety of explosive storage. This was accomplished by: a) review of the histories of recent and past magazine explosions to define causes and trends; b) observation of present-day explosive storage conditions and practices at active mines; c) examination of existing Federal regulations on explosive storage to determine whether they address all conceivable safety problems, whether they contain redundant or obsolete standards, and whether their intent is clearly stated; d) recommendation, for safety improvements and for revision and clarification (if necessity) of governmental regulations. Magazine explosions are rare. A recent increase in magazine explosion frequency must be attributed to a large increase in deliberate (criminal or malicious mischief) explosions. Fires of various origins account for the remaining explosions of the past decade. During 1884-1926 several lightning-generated explosions occurred in non-metal magazines, but none recently. It appears that the contents of a well-constructed, metal magazine are immune to direct lightning strikes, regardless of whether the magazine is grounded or not grounded. Grounding a metal magazine cannot be harmful, but it may well be superfluous. Magazines were observed at 34 widely separated mines and storage problems were discussed with personnel at these mines. In general, storage conditions and practices were found to be satisfactory. Usually, only small quantities of explosives are stored on mine property since most explosives are brought in by suppliers when needed. MSHA and BATF standards on explosive storage appear to cover safety aspects adequately. However, certain revisions are recommended to clarify some of these standards and to reduce inconsistencies in their enforcement.

Jan 1, 1983

By Donald W. Mitchell, John Nagy, Edwin M. Murphy

"Investigations in the Federal Bureau of Mines Experimental coal mine near Pittsburgh, Pa., have shown that high-expansion foam containing at least 0.2 ounce of water per cubic foot of volume is effective in controlling exper-imental underground coal, oil, or wood fires. Some of the fires were extinguished, but more of the coal and wood fires were brought under enough control to permit direct attack with water or other extinguishing agent or loading the hot material into cars. The largest controlled experimental fire, which burned about 5 hours before attack, was in a coalbed 5 feet wide, 10 inches thick, and 100 feet long. The greatest distance foam was transported to control a fire was 1,010 feet.An incipient fire should be attacked promptly with water, rock dust, or other approved and readily available extinguishing agents. Where heat, roof falls, and smoke prevent direct approach, the more involved procedure of using foam may be advantageous. The effectiveness of the foam in controlling a deep coated fire of considerable extent H,vet to be proved by actual trials in aSome hydrogen, carbon monoxide, and methane gases are generated when a fire is attacked with foam. Calculations showed that in experimental fire tests an explosive mixture could form; however, this would occur only within a narrow range of combustible gas-air mixtures not likely to be found in practice. The principal explosion hazards are due to generation of gases by the foam, localized build-up of normally liberated methane, and volatiles liberated by the coal during heating. The quantity of combustible gases generated by the action of the foam on the fire is about the same as that when an equivalent amount of water is applied."

Mar 1, 1960