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By James M. Nishi, Lloyd Carpenter

Sixteen elements were determined spectrochemically in the general range of 3 to 1,000 ppm in high - purity columbium . Samples were converted thermally to Cb2 O , mixed with graphite and Ge02 , and excited for 15 seconds using a 15 - ampere dc arc . For the molybdenum determination , the oxidized samples were mixed with NaCl and Geo₂ and excited for 30 seconds . Spectra were recorded on photographic plates , and spectral line transmittance values were measured photometrically . Relative - intensity ratios of selected analytical and internal standard spectral lines were plotted against concentrations of standards to form curves from which concentrations of impurities were read . Average precision of the method was 11.2 percent relative standard deviation .

Jan 1, 1964

By A. Gene Collins, Cynthia A. Pearson, Cathy J. Waters

The chemistry of selenium and tellurium is discussed , along with a method of preparing a synthetic oilfield brine , an oilfield brine sampling method , and methods for determining selenium and tellurium in complex oilfield brines . Selenium either can be reduced to the elemental form with sulfur dioxide and determined semiquantitatively by color comparison of the red amorphous form or can be converted to selenite and determined quantitatively by reacting it with 3,3 ' - diaminobenzidine and obtaining its spectral absorbance at 420 mu . Tellurium can be reduced to the elemental form with hypophosphorous acid , and the spectral absorbance of its red hydrosol can be measured at 400 mu . Less than 0.05 mg / 1 of selenium and 0.1 mg / 1 of tellurium can be determined by the described methods .

Jan 1, 1964

By V. E. Edlund

This report presents the results obtained in a study of the technical feasibility of recovering a usable pig iron by pyrometallurgical treatment of typical copper reverberatory slags . The iron in the slag was readily reduced with carbon , but the copper and sulfur content of the metal was best controlled by a three - stage procedure comprising ( 1 ) melting the slag with pyrite to remove copper as a low- grade matte , ( 2 ) smelting the partly decopperized slag with fluxes and carbon to reduce the iron , and ( 3 ) refining the impure iron alloy from step 2 with a flush slag to remove sulfur and residual copper . Laboratory - scale tests demonstrated that washing with 8 wt pct of pyrite lowered the copper content of a typical reverberatory slag from 0.58 to 0.12 Subsequent smelting of a mixture composed of 70 pct decopperized slag , 25 pct lime , and 5 pct coke reduced 84 pct of the iron to metal containing 2.27 pct sulfur . This metal then was successfully desulfurized by treatment with a basic flush slag to produce a finished metal that contained , in percent , 93.5 Fe , 0.02 S , 0.26 Cu , and 4.9 C. Overall recovery of iron under the conditions of trial was about 80 pct . This could be increased if higher tolerances for copper could be accepted . Commercial processing would be accomplished in three furnaces with molten materials passing from one to another . Currently produced smelter slag could be treated fairly inexpensively , because the molten product would require only a little additional heat to produce an iron byproduct that undoubtedly would be attractive to local foundries .

Jan 1, 1964

By Oliver C. Fursman, Lloyd H. Banning

This research was undertaken to determine the feasibility of producing steel from hydrogen - reduced , pyrophoric iron powder . Before steelmaking tests were begun , investigations were made to develop procedures for handling the pyrophoric powder safely , and melting tests were made in a single - phase , electric - arc furnace to determine inert gas requirements for preventing powder oxidation . Steelmaking tests were conducted in a conventional electric - arc furnace , usually by a two - slag basic procedure . Results of the research indicated that ( 1 ) pyrophoric powder can be handled safely and can be prevented from oxidizing excessively during charging and melting in electric - arc steelmaking furnaces ; ( 2 ) little , if any , more electrical energy is required for melting Cerro Bolivar iron powder per unit of contained iron than is required for melting heavy melting scrap ; ( 3 ) high - quality steel can be produced readily from high- grade iron powder , having recoveries up to 95 percent of the total iron ; ( 4 ) steel can be produced from simulated titaniferous , chromiferous , and manganiferous iron powders ; and ( 5 ) the electrical energy required for melting increases with increase in the proportion of slag - forming constituents in the furnace charge .

Jan 1, 1964

By H. R. Babitzke, H. Kato, M. D. Carver

A number of columbium and tantalum alloys were investigated to determine their suitability for use at elevated temperatures . Columbium-vanadium , tantalum-vanadium , and tantalum-hafnium alloys , and also columbium- 10 wt pct titanium alloys modified with additions of 0.1 to 2 mole pct ZrO2 , TiO2 , ZrB₂ , TiB , ZrC, or TiC were prepared and examined . Workability , tensile properties , and oxidation resistance were tested . Of the columbium alloys studied , the columbium- 12 at . pct vanadium exhibited the best properties ; it compared closely with the columbium- 10 at . pct vanadium alloy studied in a previous investigation.

Jan 1, 1964

By Albert W. Deurbrouck

This report describes the preparation characteristics of the Pittsburgh and Upper Freeport coalbeds in Hancock , Brooke , Ohio , and Marshall Counties , W. Va . Over 4.5 million tons of coal was produced in these four counties in 1962. Most of this production came from the Pittsburgh coalbed . Twelve coal samples were collected for this study , 11 from the Pittsburgh bed and 1 from the Lower Freeport bed . Two of these samples could be upgraded to produce metallurgical - grade coal . The sulfur content of the Pittsburgh- bed coals was generally excessive --as high as 4.9 percent in the raw coal and 3.19 percent in the float 1.30 specific gravity fraction . The rank of the coals in this area ranges from high-volatile A to high-volatile B bituminous .

Jan 1, 1964

By Oliver Q. Leone

Three electrorefining cells were designed to investigate various factors associated with the electrorefining of reject - grade titanium sponge . Operation of the cells provided information on cell design as well as on how design and operating variables affected the quality of the titanium product . A sodium chloride - titanium chloride electrolyte was used , and the electrolyte chambers had capacities ranging from 400 to 3,500 pounds of molten salt . Major factors investigated were electrolyte composition , temperature and useful life , effect of various cathode shapes and materials of construction , methods for removing cathode deposits , effect of current density and cell potential , and the mechanics of deposit growth and crystal morphology . One of the cells was in intermittent operation over a 4 - year period and produced 2 tons of refined titanium . A product with a hardness of 80 or less Bhn (Brinell hardness number ) was consistently and easily obtained . Some metal with a hardness of less than 60 Bhn was produced . In one of the cells in which the electrolyte was held at operating temperature with an internal heater an ac input of 25 kw maintained 3,500 pounds of electrolyte at 850 ° C , but with an external heater 35 kw was required to maintain 400 pounds at 850° C.

Jan 1, 1964

By F. E. Block, Robert R. Brown, A. W. Henderson

The chlorination of Cr₂ 03 (chromic oxide ) in the presence of carbon with CC14 (carbon tetrachloride ) and COCl2 (phosgene ) chlorinating agents was investigated by employing the radioactive tracer carbon By tagging carbon mixed with Cr₂ 0з , the chlorination reaction was evaluated in terms of the competitive reaction of the elemental carbon and the carbon contained by the chlorinating agent . A unique gas - analysis train was used to separate the chlorination product gases ; CO , CO₂ , and COC12 . The C¹ activity of the gases was determined and used to calculate the reactivity of each source of carbon . Reactivities were determined for the temperature range from 600 ° to 900 ° C. The results of the investigation show that each source of carbon reacts significantly with the Cr2 03 and that the reactivity of each form of carbon depends on the reaction temperature , and each form is independent of the other . Radioisotope and gas - analysis techniques are discussed and a description of the experimental apparatus is given .

Jan 1, 1964

By Robert M. Becker

This report (the second in a series of five) presents the mathematical development in extending the theory of sample reliability from a sample consisting of a fixed number of items to a sample consisting of a fixed amount of items. Examples of a fixed amount of items per sample are samples consisting of a fixed weight or a fixed volume of unequal size particles. The probability distribution functions (those here called the compound binomial and compound multinomial functions) are developed from fundamentals. Their distributions are generalized to include some measured characteristic of the items. Infinite population moments are derived from moment-generating functions, while finite population moments are developed from corresponding infinite population moments using the finite probability operator defined in part 1 of this series.

Jan 1, 1964

By H. R. Babitzke, H. Kato, R. E. Siemens, G. Asai

The purpose of this investigation was to develop a wide variety of columbium and tantalum alloys and to determine their suitability for use at elevated temperatures . Sixty - nine columbium and tantalum alloys were investigated . For this study , columbium was alloyed with two or more of the following : nium, tungsten , vanadium , titanium, and zirconium . Tantalum was alloyed with vanadium or hafnium, or hafnium and carbon . The fabricability was determined by an arbitrary procedure . Hardness measurements , elevated - temperature tensile properties , and oxidation- resistance studies were made . Of the alloys studied , Cb - 15 Hf - 5W, Cb - 15Hf - 5W- 10Ti , Cb - 15Hf - 10W- 10Ti , Cb - 10V - 5W, Ta - 30V , and Ta - 20 to 33Hf exhibited excellent high - temperature properties . These alloys were not only easy to fabricate , but they also had good oxidation resistance and excellent high- temperature strength .

Jan 1, 1964

By D. J. Stoops, H. Kato, M. D. Carver

The effects of impurity elements silicon , aluminum, copper , nitrogen , and manganese , at 50 to 300 ppm, on properties of the zirconium alloy Zircaloy 2 were investigated . Variations in microstructure , mechanical properties , and corrosion behavior in some inorganic acid and salt solutions were observed with variations in level of impurity element . Corrodents were solutions of sulfuric acid , phosphoric acid , copper chloride , and iron chloride . Silicon was found to modify annealed microstructures by spheroidizing and dispersion of secondphase material throughout grains . Silicon or manganese improved ultimate and yield strength of the alloy without loss in ductility . All five elements affected corrosion rates of the alloy , the effect being generally different for each element .

Jan 1, 1964

By W. P. Haynes, A. J. Youngblood, J. J. Demeter

Synthesis of high - Btu gas , using the Fischer - Tropsch reaction was investigated in a tube - wall reactor of 2 - inch steel . The catalyst was carbonexpanded iron ( CEI ) , formed on the walls of a steel reactor by exposing the reactor to 1H₂ + 100 synthesis gas under certain conditions . Advantages to be gained from successful development of the CEI - coated tube- wall reactor are elimination of catalyst plant and catalyst handling and charging operations , high- temperature operation , and a relatively low- cost , reactor -heat recovery system . In one test ( TW- 8 ) in which the reactor was filled with CEI , the reactor was operated for 1,910 hours before the test was stopped because of excessive pressure drop caused by carbon deposition . The pressure drop was satisfactory for 1,000 hours of operation at an hourly space velocity of 300 , but it increased rapidly at space velocities of 600 and 1,000 . When operated at a space velocity of 300 , with a ratio of 1 to 1 recycle at 534 ° C , a conversion of 72 percent of the 3H + 100 synthesis gas was achieved . The product gas had a heating value of about 610 Btu per cubic foot and could be suitably upgraded to 900 - Btu gas by subsequent use of a nickel catalyst . CEI did not operate effectively as a film catalyst under conditions of generation tried in this study . Generally , operation of the 2 - inch reactor with CEI catalyst was unsatisfactory because of poor reproducibility of the activation step and poor temperature control resulting in high- operating temperatures and eventual plugging of the reactor . Tests using CEI in fixed , packed beds suggest that the most likely application for CEI in producing high - Btu gas would be a moving - bed reactor , where sufficient bed movement and heat removal are provided to prevent plugging .

Jan 1, 1964

By R. J. Leary, W. M. Mahan, F. X. Tartaron

A new type of apparatus for prerefining molten blast furnace iron and to reduce the cost of subsequent steelmaking consists of a funnel - shaped device lined with firebrick into which a horizontal stream of molten pig iron is directed tangentially at the top . The rotary motion thus induced causes the stream to flatten itself upon the wall and flow in a spiral path to the outlet ; thus , the device was termed " vortex cone .' Oxygen and other refining agents are impinged upon the flowing metal in the cone where reaction is facilitated by the large metal surface exposed and the turbulent flow pattern . Experiments with water in 1 - foot - diameter funnels provided an idealization of the flow patterns to be expected with molten iron . A brick - lined reactor 3 feet in diameter was built for desiliconizing molten pig iron in lots of 1 to 2 tons . At flow rates of 0.3 to 0.5 ton min - 1 (430 to 720 tons per day ) this apparatus was 64- to 90 - pct effective in desiliconization with oxygen efficiencies of 19 to 41 pct . Detailed experiments to develop basic engineering data are underway , and adaptation of this principle to other reactions and reactants is planned .

Jan 1, 1964

By Charles J. Stehlik

This report deals with the changing behavior of mine roof bolt and roof rock as a result of repetitious production blasting . Observations were made in the upper shale production headings at the White Pine Copper Co. room and pillar mine , White Pine , Mich . Roof bolt compression pads and a stratascope were used in the investigations , which were carried out in three separate test sites in which nearly identical procedure produced comparative , repetitive , and anomalous observations . Results indicate roof bolt tension change and roof quality deterioration anomalies were coincident with blasting . The hypothesized cause of the anomalies is a seismic shock generated by the blasts .

Jan 1, 1964

By Sabri Ergun, Robert W. Smith, Victor H. Tiensuu

Factual geometries are considered for X- ray scattering studies of weakly absorbing materials by both reflection and transmission methods . These studies are usually made on slab specimens to obtain adequate scattered intensities ; however , the intensities are appreciably influenced by absorption of the X-rays in passing through the specimens . Conventional equations derived to account for this absorption are based on idealized geometries , but for polycrystalline carbons the use of idealized geometries leads to several percent error in the corrections to be made . Use of factual geometries substantially reduces this error .

Jan 1, 1964

By Robert K. Koch, Henry E. Blake

Laboratory tests were made to determine if aluminum fluoride of commercial grade could be synthesized by reacting alumina hydrate with dilute ( 25 to 75 grams per liter of fluorine ) aqueous fluoride solutions . • Products containing up to 90 percent aluminum fluoride ( A1F ) were synthesized by reaction of alumina trihydrate ( A120 3H2O) with either dilute hydrofluoric acid ( HF ) or ammonium fluoride ( NHF) solutions , the ammonium fluoride solution resulting from ammonia ( NH ) desilication of a hydrofluoricfluosilicic acid ( HF - H₂ SiF ) solution . Fluorine recoveries of over 80 percent were obtained with either type of solution . The hydrated precipitates of AlF, and ( NH4 ) , A1F ( ammonium aluminum fluoride ) obtained by reacting hydrated alumina with these solutions were subsequently converted to anhydrous AlF, by controlled heating .

Jan 1, 1964

By James S. Browning, W. H. Eddy

Laboratory batch and small - scale continuous flotation tests were conducted on a ferruginous barite - fluorspar ore from near Sweetwater , Tenn . , to determine the feasibility of producing commercial - grade fluorspar and barite concentrates . The lignin sulfonate - sodium fluoride - fatty acid method of floating fluorspar produced acid - grade concentrates . Flotation of the barite from the fluorspar tailing using petroleum sulfonate yielded concentrates suitable for use as a weighting agent in oil -well drilling muds . The continuous flotation tests , treating about 150 pounds of ore per hour , yielded fluorspar concentrates that assayed 98.3 percent CaF2 and barite concentrates that assayed 91.2 percent BaSO4 . The recovery of the two minerals was 91.2 and 85.2 percent , respectively .

Jan 1, 1964

By H. R. Babitzke, H. Kato, R. E. Siemens

An investigation was made to provide further information for evaluating columbium- hafnium alloys for use as high - temperature structural materials . The columbium- hafnium system was investigated between 700 ° and 2,400 ° C by melting point , thermal analysis , X - ray diffraction , electrical resistivity , and metallographic techniques . The equilibrium diagram is the beta isomorphous type , with columbium tending to stabilize the beta phase . Addition of 60 atomic percent columbium stabilizes the beta phase at 700 ° C. The allotropic transformation temperature of hafnium is 1,750 ° ± 20 ° C. A minimum melting point occurs near 75 atomic percent hafnium .

Jan 1, 1964

By G. W. Birge, D. E. Wolfson, J. H. Lynch

Fourteen coal samples representing the Flag , Fire Clay , Whitesburg , Amburgy , Upper Elkhorn No. 3 , Upper Elkhorn No. 2 , Upper Elkhorn No. 1 , and Lower Elkhorn beds in Letcher County , Ky . , were carbonized by the Bureau of Mines - American Gas Association ( BM- AGA ) method , and yields of products and physical properties of cokes were determined . The samples tested were high- volatile A bituminous in rank , with dry , mineral - matter- free fixed - carbon contents ranging from 55.3 to 62.2 percent . Five of the samples , as received , were chemically unsuitable for metallurgical use because of excessive ash and/ or sulfur content . Generally , strength indexes of the cokes were low and all of the coals would require blending with higher rank coal to obtain satisfactory blast furnace fuel .

Jan 1, 1964

By Joe L. Castagno, Kenneth H. Johnston

Several hundred membrane - filter tests were made as part of a program to develop equipment and procedures to evaluate the quality of waters and to determine the quality of water suitable to efficiently flood oil sands of known permeability . Results indicated that neither the color of the water nor that of the precipitate on a membrane filter is a criterion for determining the quality of injection water . Reasons for poor water quality include poor operation of filtering systems , dirty filtering aggregates , excessive amounts of oil in injection water , commingling of incompatible waters , and excessive use of chemicals . A good water is required to efficiently flood sands of low permeability , but fair results may be obtained in flooding more permeable sands with poorer quality water .

Jan 1, 1964