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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 Alla D. Mah

The heat of combustion of aluminum carbide (Al, C3 ) , obtained directly by combustion calorimetry , was AH298.15 -1,029.6 ± 1.9 kcal / mole . == The heat of formation of aluminum carbide corresponding to this value was AH298.15 = -53.4 ± 2.0 kcal /mole .

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 J. A. Ruppert, P. M. Sullivan

A process was developed on a laboratory scale in which iron contained in galvanizers ' zinc dross and aluminum contained in scrap zinc die - cast alloy were removed simultaneously . Melting both types of scrap together in the proper proportions resulted in formation of solid intermetallic Fe₂ Alg , which was readily removed from the melt by filtration and centrifugation . Recovery was 87 to 92 percent of the available zinc . Refined filtrate contained 0.02 percent iron and 0.20 percent aluminum. Aluminum content was further reduced to less than 0.01 percent by fluxing with zinc chloride . Low temperatures employed and inexpensive equipment requirements make the process commercially attractive .

Jan 1, 1964

By Gilbert M. Farrior

Tests of resistance to molten metals , to oxidation at elevated temperatures , and to various chemical reagents were made for a series of compositions in the TiB₂ - CrB₂ subsystem . In reaction with molten metals , there was no noticeable difference in reaction of the various compositions in the ( Ti , Cr ) B₂ series . The oxidation tests were ( 1 ) a rising - temperature test in which the specimen temperature was increased 4° per minute to 1,200 ° C and ( 2 ) a constanttemperature test in which the specimen temperature was held constant at 1,000 ° C. Compositions near Tio.6 Cro.4 B2 had the best oxidation resistance . Ti。.6 The chromium- rich alloys showed marked superiority to the titanium- rich alloys in resistance to corrosion by the chemical agents investigated . The chemical reagents used were sulfuric , nitric , and hydrochloric acids and sodium hydroxide of different concentrations .

Jan 1, 1964

By A. E. Schwaneke

Plans and specifications are given for constructing a quartz composite oscillator designed to measure internal friction in metals and alloys . The characteristics of the system are listed , and detailed procedures for its operation are explained . Typical measurements on manganese - copper alloy , on single - crystal magnesium , and on polycrystalline magnesium are shown to illustrate applications of the system .

Jan 1, 1964

By L. G. Trudell, J. W. Smith, K. E. Stanfield

Oil- yield data are presented for 40 sets of core samples and 83 sets of drill cuttings collected in 1952-62 from drilling operations in the Uinta basin of eastern Utah . This accumulated information on the location , extent , and richness of oil shales of the Green River formation is used to appraise the deposits as a source of oil and related products . Core samples used in the study were obtained specifically for evaluating oil shale , and they were satisfactory for this purpose , except they did not completely penetrate the formation . The drill- cutting samples were inferior to the core samples and yielded more erratic results . Consequently, oil yields based on cuttings should be regarded as indicative , rather than definite , until substantiated by other means . In general , the oil- yield data indicate Green River oil shale in Uinta basin is not as thick or as uniform as that in the Piceance Creek basin of western Colorado . However , it is an important potential source of oil . Estimates that beds 15 feet or more thick that average 25 gallons of oil per ton represent at least 120 billion barrels of oil in place are supported by the recent oil- yield data .

Jan 1, 1964

By L. C. George, J. W. Jensen

A new system for precisely counterbalancing and measuring vapor pressure operates by servomechanical principles . It was developed with the objective of determining the vapor - pressure equations of metal halides . The system is isolated from the vapor - pressure bulb by a diaphragm transducer that signals a pressure regulator to null any pressure difference that is detected . Pressure measurement and readout are continuously performed by a servomanometer , accurate to ±0.003 cm Hg for the range of 0.1 to 200 cm Hg . High response rate and sensitivity are obtained . Methods of use are described , and results for CdC1 and PbC1 , in agreement with data of other investigators , are given as examples .

Jan 1, 1964

By C. A. Pearson, W. D. Dietzman, M. E. Hawkins

Results of chemical analyses and electrical resistivity measurements of 422 samples of oilfield brines from 120 east Texas fields in Railroad Commission of Texas Districts 5 and 6 are presented in tabular form . These samples represent water from all of the major petroleum- productive formations in the area . Water analyses and electrical resistivity data , when fully utilized by proper study techniques , are useful tools in the solution of many engineering problems such as detection of well leaks , identification of water sources , and interpretation of electrical well logs . In the area included in this study , these representative data should facilitate the solution of problems in which water analysis and water resistivity are factors .

Jan 1, 1964

By Joseph A. Sutton, John D. Corrick

The chemistry involved in the microbial dissolution of iron and copper from such sulfide minerals as pyrite, chalcopyrite, chalcocite, cove11ite, and bornite is described. The chemical criteria used to evaluate the activity of microorganisms on these minerals were changes in pH, ferric iron produced, and oxygen consumption. In a series of experiments in which a ferrous sulfate nutrient solution was percolated over small portions of the above-mentioned copper sulfide minerals for 56 days, the iron-oxidizing bacteria Ferrobaci11us ferrooxidans and Thiobaci11us ferrooxidans were capable of bringing about the dissolution of 23.7 percent of the copper from chalcocite, 56.3 percent of the copper from cove11ite, and 29.8 percent of the copper from bornite by the microbial production of ferric sulfate which reacted with these minerals. Laboratory tests have demonstrated that pure strains of the iron-oxidizing bacteria act as catalysts to the ferrous iron being oxidized by the Oxygen of a system containing pyrite and chalcopyrite. In a series of experiments during which nutrient solution was percolated over pyrite for 70 days, the ferric iron produced by the iron-oxidizing bacteria was 112 to 120 times greater than that produced atmospherically.

Jan 1, 1964

By Raymond W. Hiteshue, Sam Friedman, Paul Dobransky, Robert Madden

A hvab coal was carbonized in a closed system at 600 ° C and 40 to 1 , 200 psig to produce a high- Btu gas and char . By retaining the volatiles within the system, it was possible to virtually eliminate production of tars and oils . Depending on pressure and residence time , yields of combustible gases (72 to 92 percent methane ) amounted to 4,000 to 6,000 cubic feet per ton of maf coal and gross heating values of these gases varied from 830 to 960 Btu per cubic foot . Yields of char (maf ) were about 1,600 pounds per ton of maf coal . Increased residence time favored production of gases but reduced their heating values , whereas increase in pressure resulted in somewhat higher heating values and lower production . Similar effects were observed from the carbonization of a low- temperature tar . If these results could be translated to an economical carbonization process for producing high- Btu gas from coal , the demand for coal could be expanded by 40 to 50 million tons per year . Because of large yields of char , a process of this type would obviously have to be integrated with coal - fired power plants . Fortunately , operations could be conducted at essentially atmospheric pressure as product gas under this condition can be obtained in satisfactory yields and with good quality .

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 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

By M. M. Tilman

The purpose of this investigation was to determine the effects of small amounts of cobalt in nickel on the tensile properties and hardness of representative types of austenitic stainless steels . Cobalt substitutions for nickel up to 2 weight - percent were made in types 302 and 309 stainless steels . Data were obtained at room temperature for tensile strength , yield strength , percentage elongation , percentage reduction in area , and hardness . In type 302 steels , tensile strength and hardness increased with increased percentages of cobalt , percentage elongation and reduction in area decreased , and yield strength showed little change . Property changes were largely due to the reduction of nickel content rather than to the addition of cobalt . In type 309 steels , only minor variations were observed for the properties investigated ; the effects of the relatively snall cobalt substitutions and nickel reductions were somewhat reduced by the higher total alloy content .

Jan 1, 1964

By Sarkis G. Ampian

Published optical microscopic and X- ray diffraction characteristics of the following compounds are critically evaluated and compared with Bureau of Mines data : Tricalcium aluminate , calcium monoa luminate , dodecacalcium heptaluminate , dicalcium silicate , tricalcium silicate , and sodium aluminate . A recommended set of definitive optical and X- ray diffraction characteristics is presented . These values are used to identify products of the lime soda sinter process for production of alumina . Polymorphism of gamma- , beta- , and alpha prime - dicalcium silicate is reexamined , and new data are presented on polymorphism of tricalcium silicate and sodium aluminate by high- temperature X- ray diffractometry . Polymorphism is not observed for tricalcium aluminate , calcium monoaluminate , and dodecacalcium heptaluminate . Bureau of Mines data indicating a stoichiometry of 12Ca0.7A10 for the phase 5Ca0.3A1 0₂ are discussed . A critical review of the literature concerning calcium dia luminate and sodium undecaluminate ( 8 -A10 ) is also included .

Jan 1, 1964

By Vernom F. Swanson, George E. Fish

A study was made during 1959-60 of reported nelsonite occurrences in Nelson and Amherst Counties, Va. The investigation was limited to core drill- ing on one deposit and beneficiation studies on three deposits. Three diamond-drill holes totaling 562 feet were drilled on the E. M. Hughes property to determine subsurface continuity. Although outcrops as much as 30 feet wide were present on this property, the only nelsonite intersected in the holes ranged from 4 to 18 inches thick. The ilmenite content of the core ranged from 50 to 75 percent. These nelsonite deposits are of secondary importance as a source of titanium, being small, rarely exceeding 1,500 feet in length and 30 feet in width, but they are high grade. Due to the proximity of some of the bodies it might be possible to mine several of them as one operation feeding one mill. Electromagnetic separation on composited samples recovered 83.0 percent of the Tio as an ilmenite concentrate in 68.5 percent of the weight. Two flotation procedures were developed. The first method, using oleic acid as a collector and fluo silicic acid as an apatite depressant on deslimed feed, produced an overall recovery of 59.3 percent in batch tests. The second procedure eliminated desliming. Laurylamine hydrochloride removed silicates in an acid pulp followed by an alkaline apatite flotation with oleic acid as the collector and dextrine as the ilmenite depressant. The ilmenite-rich tailing represented a 66.2-percent recovery of Tio in the batch tests.

Jan 1, 1964

By Edward Cogan

Equilibrium phase diagram studies of zirconium- rare earth metal alloys by the Bureau of Mines at its Albany Metallurgy Research Center prompted the development of a rapid gravimetric method for determining rare earths in zirconium in which the rare earths are absorbed from sulfuric acid solution of the alloy on a cation exchange resin . The sample in 10 percent H2SO4 is introduced into the column , the zirconium is eluted with 10 percent H2SO4 , and the rare earths are eluted with (NH4 )2SO4 solution and precipitated with NH4OH . A tracer technique was employed to determine the efficiency of the procedure . Y203 and europium 154 - 152 (Oak Ridge ) were added to 10 g of zirconium and taken through the entire procedure . Recovery averaged 97.6 percent on 0.002 μg europium in the rare earth fraction . Rare earths were determined in the range 0.10 to 90 percent .

Jan 1, 1964

By Paul W. Johnson, Ralph C. Kirby, Frank A. Peters

Alumina can be recovered from clay , using 30 percent nitric acid for digestion . Calcined clay is crushed and then digested at 325 ° F and 85 psig pressure with less than stoichiometric nitric acid required to form normal aluminum nitrate . In this way , a solution containing both normal aluminum nitrate , Al ( NO3 ) 3 , and basic aluminum nitrate , assumed to be Al ( OH ) ( NO3 ) 2 , is formed , and in which iron is virtually insoluble . The solution is filtered and then concentrated in vacuum evaporators to crystallize normal aluminum nonahydrate . The crystals are washed with 50 percent nitric acid and then decomposed to alumina and nitrogen oxides . The design that has been developed for this process is based on published work . For a plant producing 1,000 tons of alumina a day , the estimated operating cost is $60.69 per ton of alumina , and the estimated fixed capital cost is $ 76 million using a Marshall and Stevens chemical equipment index basis of 240.0 . This process is not competitive under current economic conditions with the production of alumina from bauxite via the Bayer process . For lowering costs , future research should include study of leaching at lower temperatures under atmospheric pressure and alternate aluminum nitrate decomposition methods .

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 B. H. Eccleston, R. F. Kendall, D. E. Hirsch, Norman G. Foster

The mass spectra of 23 alkylthiophenes are presented , including 21 that have not been previously reported . Correlations between mass spectra and the structure of the thiophene homologs are discussed . Comparisons with , and corroboration of , earlier workers ' correlations and predictions are made . Several additional correlations are reported to enable the spectroscopist to identify the substituents on alkyl - substituted thiophenes , and the relationship of the mono - substituted and 2,5 - disubstituted alkylthiophenes is discussed in detail .

Jan 1, 1964