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By C. H. Fisher

[Many methods of analyzing tar oils for their tar acid and base content have bun employed in connection with both academic and. industrial investigations. Most of these analytical procedures are based on the diminution in volume caused by extraction with alkali and mineral acids (contraction method), although other methods haves been employed.4/ In many instances the adoption of an analytical method was not preceded by adequate study, and, as a consequence, the literature, on this subject is conspicuous for its contradictory claims and recommendations. It has bin shown in the, case of certain synthetic solutions5/ that large errors may result if the analysis is carried out by simple extraction with alkali and mineral acids.]

Jan 1, 1936

By J. S. Gomer

The U.S. Bureau of Mines conducted Cu exchange tests for six common clays under simulated in situ leaching conditions. Regression equations were obtained from the data expressing the Cu exchange capacity as a function of Cu concentration, pH, and temperature. Using these equations, an analysis was made of the impact each clay could have on overall Cu recovery. The results suggest that Ca and Na montmorillonite clays could have a major impact on Cu recovery and that attapulgite and illite clays could have a smaller, but still significant, impact. Kaolinite and ripidolite clays pose little threat to loss of Cu from in situ leaching solutions.

Jan 1, 2010

By J. H. Field

Results of studies by the Federal Bureau of Mines on a pilot-plant scale for removing hydrogen sulfide and carbonyl sulfide from gas mixtures by the hot carbonate system are given in this publication. Gases containing up to 10 pet. hydrogen sulfide and 48 grains carbonyl sulfide per 100 cu.ft. were treated. In most tests carbon dioxide also was present and was removed simultaneously with the sulfur compounds. Because the rate of absorption of hydrogen sulfide is much more rapid than that of carbon dioxide over a wide temperature range, selective removal of hydrogen sulfide occurred in the bottom section of the absorber near the point of gas entry. Hydrogen sulfide was removed to pipeline specifications with carbonate solutions by using split-stream flows in the absorber and regenerator.

Jan 1, 1960

By William K. Tolley

The U.S. Bureau of Mines (USBM) is investigating hydrometallurgical processing techniques to recycle metals from semiconductors and other advanced materials. Cadmium and tellurium were recovered from mixed CdTe/CdS scrap produced in the manufacture of thin-film photovoltaic devices. Selective cadmium dissolution was achieved using oxygen-pressure leaching in dilute sulfuric acid. Leaching the scrap for 90 min at 110° C in 2.2NH2S04 under 400 psig 02 yielded 97% Cd extraction; however, cadmium content of the residue ranged between 4% and 7%. Soluble iron was added to the lixiviant to catalyze oxidation of the CdS component. Tellurium and sulfur remained in the leach residue primarily in the elemental form. The iron and tellurium were removed from the cadmium-rich leach liquor by adjusting the pH to 5.3. The cadmium was recovered as cadmium sulfate crystals by evaporating the solution. Alternative leaching and purification schemes are discussed.

Jan 1, 2010

By Theodore L. Turner, Joseph H. Swift

A study on a small laboratory scale was made of the use of ammoniacalammonium carbonate for batch leaching Mn from low- grade manganiferous materials ( 6 to 16 pct Mn) obtained from deposits in the southern district of Aroostook County , Maine . These materials were partially reduced at 500 ° to 700 ° C with H₂ or CO and then leached with solutions of NH and CO₂ dissolved in water . Extraction of 80 to 90 pct of the Mn was obtained from some sample materials , but 10 to 34 pct of the iron was also extracted . Material from the Littleton Ridge deposit contained manganese intimately associated with Fe , a condition which contributed to difficulties in obtaining a commercially acceptable product . Extensive investigations of the leach and reduction processes with various mixtures of H₂ and water vapor , and CO and CO₂ , failed to disclose a set of conditions for selectively leaching the manganese . Finely divided metallic Fe was probably produced during the reduction steps so that Fe was leached with the Mn in the subsequent extractions .

Jan 1, 1964

By John S. Ball

Aniline points have been used to some extent for more than 20 years. to indicate the types of structures in hydrocarbons and thus to analyze mixtures of hydrocarbons . This type of analysis has been applied - principally to the low -boiling hydrocarbons found in the gasoline range . Although there is some disagreement as to their merits , both aniline point and diesel index (aniline point in degrees Fahrenheit times A.P.I. gravity at 60 ° F. divided by 100) are used rather extensively for evaluating ignition qualities of diesel fuels . In recent years aniline points have been employed in the study of lubricating - oil fractions . They also have been used to predict : the tendency of different oils to cause swelling of synthetic rubbers.5/ Recent standardization of the aniline - point determination by the American Society for Testing Materials has encouraged wider use of this test . Considerable data concerning , aniline points and critical solution temperatures in aniline have been accumulated in the course of a study of related subjects . Thesc data , together with some original results , are presented here in the hope that they will prove useful to other worker's in this field ...

Oct 1, 1943

By V. M. Benson

A simplified, routine method for determining lithium in lithium-bearing rock is presented. The sample is decomposed by repeated treatments with nitric, hydrofluoric, and perchloric acids. Since this procedure does not appreciably dissolve beryl, interference by beryllium (the principal interfering cation) is minimized for most samples. The salts are brought into solution with water and enough citric acid-ammonium citrate buffer is added to make the final volumetric dilution 0.20 M with respect to citrate. The addition of citrate greatly reduces anion interference in the hydrogen-oxygen flame, slightly increases the intensity of the lithium 671 millimicron emission line, and reduces the effect of most of the interfering cations to the extent that analytical separations are not necessary. The accuracy of results of single determinations of lithium in a pegmatite containing spodumene, lithium-bearing mica, and beryl are approximately equal to that obtained by other flame methods, INTRODUCTION This investigation was undertaken in Bureau of Mines laboratories to develop a reliable, rapid, routine analytical method for determining lithium in lithium-bearing minerals. The requirements of the procedure were that the method should be applicable to the analysis of a variety of lithium-bearing ores and test products, and the results would be reasonably accurate for materials containing 0.05 to 8 percent Li20.

Jan 1, 1961

By R. E. Head, Virgil Miller

"Under existing conditions in the treatment of oxidized lead ores containing small quantities of molybdenum no provision is made for the recovery of the molybdenum. Considerable quantities of this important element are lost in the slags of the lead smelters and constitute an economic waste. There is little or no probability that slag dumps containing molybdenum in small quantities could be economically treated for the recovery of the element, and steps for the prevention of waste in this respect must be taken prior to smelter treatment.Wulfenite, lead molybdate (PbMo04), and molybdite, molybdic ocher (Mo03), are the molybdenum minerals most abundantly found in deposits of oxidized lead ores. Wulfenite contains 39.3 per cent molybdenum trioxide and 60.7 per cent lead oxide; molybdite contains 66.7 per cent molybdenum and 33.3 per cent oxygen. Plumbojarosite, argentojarosite, cerussite, and occasionally anglesite are commonly associated with wulfenite ores, and the oxidized iron content is usually fairly high.The recent discovery and development of a body of wulfenite ore in the Star district near Milford led to a cursory microscopic examination of samples of the ore, followed by a few preliminary tests which had for their object the separation and recovery of the lead and molybdenum in separate products.The microscopic examination showed that the samples used in the work were composed of wulfenite, plumbojarosite, and a small quantity of cerussite, and indicated that the iron content was quite high. The ore was porous and yellowish-brown; crystals of wulfenite appeared to be quite uniformly distributed through it, and this mineral and plumbojarosite (Pb0.3Fe203.4S03.6H20) apparently accounted for the major part of the lead content, although lead"

Sep 1, 1928

By H. H. Dewing

The Bureau of Mines constructed a process research unit (PRU) to demonstrate new technology for extracting zinc from sphalerite concentrates. Up to 9 kg/hr of sphalerite (ZnS) concentrate was reacted at ambient pressure in the PRU with 80 pct sulfuric acid at 160° to 180° C to produce zinc sulfate and elemental sulfur. The PRU consisted of a three-stage glass reactor system: a 4-liter premix stage in which feed was slurried with 78 to 82 pct H2S04, a 40-liter stirred reactor, and a ISO-liter settling stage in which high reaction conversions were effected and excess H2S04 for recycle was separated from insoluble ZnS04 and sulfur. Evolution of sulfur-containing gases was minimized by sub-surface addition of acid feed slurry to the stirred reactor and by exclusion of air from the reactor to prevent the oxidation of elemental sulfur. Conversion of zinc to zinc sulfate averaged over 99 pct at the optimum acid concentration of 80 pct. Total sulfur losses (primarily S02) were less than 2 pct of the sulfur in the sphalerite. Elemental sulfur remained in the insoluble portion of the settled reactor product after leaching with simulated spent zinc electrolyte containing sulfuric acid. The sulfur residue contained 75 to 89 pct sulfur. Neutral zinc sulfate, required for zinc electrowinning processes, was separated from the sulfuric acid leach solution by crystallization at -15° C as zinc sulfate heptahydrate (ZnS04?7H20). The crystallization operation simultaneously effected a partial concentration of the recycled electrolyte solution by removing water.

Jan 1, 1982

By G. R. Palmer

Using a fluidized, countercurrent multiple-compartment ion-exchange (MCIX) column previously developed by the Bureau of Mines, Bureau researchers have successfully extracted uranium from a simulated acidic in situ leach liquor that contained 150 ppm U30s? This successful demonstration of the MCIX system is reported, and the effects of varying the operating conditions on the performance of the system are also examined. Operating the MCIX system with a flow rate of 15 gpm/ft2 and an aqueous-to-resin flow ratio of 200:1, more than 90 percent of the uranium Has extracted, and a resin containing approximately 28 grams U308 per liter was produced. The absorption column used to investigate the operating variables was approximately 18 feet long with a 2-inch ID and was divided into compartments that were 1 foot long.

Jan 1, 1980

By C. H. Fisher

[Mxny methnhs of ,analyzing tpr oils fnr thoir tar acid ~nd base cnntent hava boon employL~d in connection mith both ac~d,.mic and. industrial investigs- tions. Mnst of thznu nnalyticel proc?durn~s aro bpsed nn th; diminution in volums caused by extract lon sit5 alkali 5 minL+ra,l acids (cantrsction rn,>thod) , although othrr mr~thrids havu &apos;sL<on ?q~lnglt 8 . In many instmccs th-: donti ti on of RT~ m~lytic~l m ithod was not ;r.:c ~d~d by ~d.jqunt9 study, and, ns 3 cone+ qucnce, tha lit .,ratur ? on thls sub,jr:.ct is consoScuous for its cnntr~dictnry . claims and rocnmmondatinna.. 1.t tiR.s b9~n shoyn in th;, cnsn of c.lrtn.in synth?tic solut innsfi/ thnt larg~ jr-orn sny rcsult if th2 ,mnlysis is c~rri~d out by sim~la extraction wi.th alidi r.nd min 3rd ncids.]

Jan 1, 1937

By H. J. Heinen

The Bureau of Mines, investigated a cyanidation-carbon adsorption technique for extracting gold from arsenopyrite concentrates. Agitation leach experiments were conducted on 85-pct-minus-35-mesh gravity concentrates containing 21.8 oz gold and 6.4 oz silver per ton. Results obtained in leaching the concentrates showed that 96.9 pct gold and 90.7 pct silver extraction could be achieved in 96 hours of agitation. Gold and silver were recovered from the resulting pregnant solution by exposure to granular activated carbon in a countercurrent system. Carbon loadings of 2,556 oz of gold and 502 oz of silver per ton were achieved. These loadings are significantly higher than heretofore thought practical.

Jan 1, 1980

Reduce the time, complexity and expense of dissolving metal and mineral samples in solution in preparation for chemical analysis. Approach In earlier research, the Bureau of Mines developed a rapid and inexpensive method for the dissolution of mineral and metal samples in plastic pressure bottles heated in a boiling water bath. Using this technique, samples could be prepared for chemical analysis in less than one hour compared with several hours by traditional dissolution methods (see Technology News No. 85, December 1980 for further details). By heating in a microwave oven, sample dissolution time can be reduced to approximately 5 minutes.

Jan 1, 1983

By M. Clair Smith

This report is one of a series describing exploration, development, mining methods, and costs at United States open-pit mines; the Bureau of Mines prepares and publishes them in cooperation with the mining companies. Their purpose is to promote development and conservation of our mineral resources by disseminating technologic information on mining methods and practices at various United States mines. The exploration, development, equipment, and mining of a large, oxidized-copper ore deposit by open-pit methods, the leaching of the ore with sulfuric acid solution, and the recovery of the copper as cement copper are described herein.

Jan 1, 1958

By D. J. Bauer

A pure scandium solution was concentrated from 10-4 mole per liter to 0.5 mole per liter by continuous foam fractionation in a spaced, packed column. Recovery in the foam was 77 percent using a spaced, packed draining column with sodium n-methyl-n-"coconut oil acid" taurate as the surfactant. The technique was first studied batchwise in a small unpacked column to determine the more important variables. Optimum surfactant concentration was found to depend on scandium concentration. Extraction and, in general, enrichment ratios were highest in the 2.5 to 3.5 pH range at temperatures ranging from 50° to 70° C. An airflow rate of 136 ml./min. was satisfactory in the equipment used.

Jan 1, 1962

The Bureau of Mines has reviewed those portions of the "Tariff Schedules of the United States Annotated 1963" that are of interest to the minerals industry. This study shows to what extent rates of duty were altered (increased or decreased), and provides a bridge where possible from the old Schedule A classification sys tem to the new TSUS system of statistical reporting of import data. In general the new tariff has corrected previous classification defects and inconsistencies, but the rates of duties have not been materially changed.

Jan 1, 1965

By Alvin Schallis

The. problem of supplying enough magnesia for the American war effort has become highly important. Before hostilities began, only about two-thirds of our, require vents came from domestic sources; now they must supply almost all the magnesia we need. A further burden is placed upon our own supply by the fact that more and more magnesia is being required, not alone to pace the war tempo of general industrial activity, but also to replace chrome ore in refractories and to make magnesium metal. The domestic magnesite and brucite industry is equipping itself to satisfy much of this greater demand for magnesia, but the remainder must be obtained elsewhere. The principal sources of magnesia are magnesite, brucite, dolomite or high-magnesium limestone, natural brines, sea water, salt-works bitterns, magnesium silicates, and magnesium salts. Although dolomite is tae subject of this paper, it should be considered in perspective with all these highly competitive sources of magnesia.

Jan 1, 1943

By Bernard S. Covino

The Bureau of Mines is conducting a study of methods to improve the efficiency of the process used to pickle stainless steels. A review of the literature on pickling of stainless steels showed that the chemistry of several process operations involved in the pickling of stainless steels is not fully understood, and that further research could improve the pickling efficiency. The benefits of this research would be a reduction in the annual loss of several thousands of tons of critical minerals such as nickel and chromium, and a reduction in the amount of solids and spent acid solution that are currently discarded. The conclusion from this review is that further research is needed in four operations that either directly or indirectly influence the pickling process: hot working, annealing, conditioning, and the actual operation of pickling, Laboratory studies of the pickling operation are presently in progress.

Jan 1, 1984

By Allen D. Look, Stanley M. Walker, Van Fleet. Leonard A.

"INTRODUCTION The hazards to be encountered in temporarily or permanently abandoned underground mines, quarries, and open pits are numerous, and hardly a year goes by without several reported cases of fatal or serious injuries occurring to unwary people who enter these old mines. Persons visiting mining areas for the first time, tourists, and young people, especially, proceeding in the spirit of adventure common to youth or to the venturesome have suffered many such accidents during exploration trips. The possibility of salvaging salable or usable equipment prompts men and boys to go into old mines, some through ignorance of the attendant hazards, but some jeopardize their lives hopeful of gain (in some cases pitifully small), thinking the hazards are not dangerous and that they can ""get away with it.""Persons fall into unprotected holes, some seek shelter from storms under high banks, and quarries and open pits are often chosen as places for recreation, picnics, swimming, etc; all such uses of these places are likely to be hazardous and to lead to accidents, frequently fatal.These hazards are known to men in the mining profession, and the danger to the public is realized by most of them. A solution to the problem has been sought at many mining meetings, and it is recognized that complete prevention of entry into old mine workings and surface mining areas is the ideal solution, but this, unfortunately, is not always practical; better education of the public, particularly children, should help to reduce the number of such accidents and will be effective in direct proportion to the extent and vividness of such education."

Aug 1, 1948

By Marvin L. Whisman

Several parameters controlling the reproducibility of tritium determina¬tion in organic compounds by liquid scintillation counting were evaluated by the Federal Bureau of Mines. These included optimum volume of scintillator solution for maximum counting efficiency, reproducibility of counting a sealed commercial standard and comparison with duplicate counts on laboratory-prepared samples. The error introduced by using microliter pipets, optical differences in counting vials, reproducibility of counting organic samples where quenching is a factor, reproducibility of counting laboratory-prepared samples with an added internal standard, optimum ratio of internal standard activity to sample activity, effect of sample volume upon counting efficiency, count rate at which coincidence losses become apparent, and reproducibility of organic compound radioassay by the standard addition technique are outlined. From the evaluation of these parameters, a technique that can be applied routinely to organic compounds containing tritium has been established, and details are included in this report.

Jan 1, 1961