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By W. S. Landers

In contrast to the large fund of information available on the carbonizing properties of Eastern U.S. coals, the experimental data available for most Western U.S. and foreign coals are meager. To supply some self-consistent data, the Bureau of Mines conducted 220 low-temperature carbonization assay tests at 500° C. in a laboratory-scale carbonization apparatus. The results are included in this report. The U.S. coals tested are from Alaska, Arizona, Colorado, Illinois, Montana, New Mexico, North Dakota, Pennsylvania, Ohio, Texas, Utah, and Wyoming. Assays were also made on coals from Canada, Ecuador, France, Greece, India, Mexico, the Philippine Islands, Thailand, and Yugoslavia. In addition, one assay of pine sawdust and one assay of a peat from Ireland are reported. Prediction equations were developed relating the yield of products of carbonization obtained at 500° C. in the assay unit to the proximate and ultimate analyses of the coals. The equations for predicting the yields of tar plus light oil, char, and gas, and the heating value of the gas, are considered good, each equation having a multiple correlation coefficient of 0.90 or higher. The equation predicting volume of gas obtained upon carbonization is considered as fair, with a multiple correlation coefficient of 0.84. A reproducibility study of the assay made on 10 replicate samples of a subbituminous coal indicated that the standard deviation of the individual products was 0.31 percent or less.

Jan 1, 1961

By J. B. Gayle

Numerous investigators have studied the addition of inert4 substances to coking blends. Generally, the results have yielded trends applicable only to the particular coals and inerts studied. Recently, somewhat more general results were obtained for cokes produced from blends containing added inerts, using the sole-heated oven. The present investigation represents an extension of this work to include a wider range of inerts and to determine the applicability of the various conclusions to cokes produced with the Tuscaloosa oven. The results indicated that an increase in dry-coal charge density of 1 pound per cubic foot (p.c.f.) caused a corresponding change in the hardness (1/4-inch tumbler index) of Tuscaloosa oven cokes of 0.9 percentage points. This value compares favorably with the value of 0.7 determined previously for the sole-heated oven and Bureau of Mines-American Gas Association (BM-AGA) retort.

Jan 1, 1961

By Paul Meadows

This Bureau of Mines report presents operating practices and results of pressure maintenance and secondary recovery by water injection or by water injection supplemented by gas injection. Particular emphasis is placed on the results of water injection, which is the principal oil-recovery method employed in projects covered by this report. No attempt is made to study gas-injection projects or operations that are considered water-disposal projects. Also, this report does not include water-injection projects that have not been in operation long enough to evaluate results. Figure 1 is a map of north Louisiana showing the geographical locations of the projects included in this report. Most of the data used in this study were supplied by unit operators, operating companies, and the Louisiana Department of Conservation. Reservoir information and recovery data are generally those supplied by the operators, but include revisions where deemed necessary.

Jan 1, 1962

By L. M. Burman

The phase-boundary pressure required to maintain a natural hydrocarbon fluid in a single phase must be considered in planning the recovery of reservoir liquids by miscible-phase processes. The change in the phase-boundary pressure at reservoir temperature that results when a light component or a mixture of light components is added to a reservoir fluid is an especially important consideration. The cricondenbar pressure (maximum phase-boundary pressure) and the critical pressure are unique correlated pressures that have been utilized to calculate the change in phase-boundary pressure that may result when the composition of a reservoir liquid is altered by an additive. In this study one reservoir oil and three gas-condensate fluids are used as examples. Correlations pertaining to the critical and cricondenbar states in chapters 4 and 5 of Bureau of Mines Monograph 10 (3)5 were used to demonstrate how butane and lighter components added to these reservoir fluids affect their phase-boundary pressures.

Jan 1, 1962

By Wesley Holmes

Concentrating, nodulizing, and smelting studies were conducted at the Albany Metallurgy Research Center of the Bureau of Mines to determine whether (1) western iron ores of the type found in the Carter Greek deposit near Dillon, Mont., could be utilized; (2) concentrates of acceptable grade with good iron recovery could be attained by wet-magnetic beneficiation; (3) nodulized concentrates could be smelted with reductants readily available in Montana; (4) iron concentrates could be smelted without prior agglomeration; and (5) high-purity iron could be produced directly from high-grade concentrates, Three small samples and two tonnage samples from the Carter Creek deposit were uniform in chemical composition, and their iron content averaged about 31 percent. They were found to be banded gneisses, and magnetite was the principal iron-bearing mineral.

Jan 1, 1962

By A. C. Rice

Investigation of a variety of mines to determine efficiency for rare- earth extraction has resulted in a solvent extraction technique wherein Primene 81-R,4 N-benzylheptadeeylamine (BHDA), and Primene JM-T give favorable extraction from sulfate solutions. Extraction from chloride, nitrate, and perchlorate solutions is negligible. Distribution coefficients for 10 rare-earth elements with Primene 81-R establish an extraction sequence beginning with lanthanum and proceeding through lutetium according to atomic number. Yttrium and ytterbium are exceptions in the extract ion sequence.

Jan 1, 1962

By A. F. Colombo

Laboratory-scale tests were conducted by the Bureau of Mines on an argillaceous Michigan copper ore and mill tailing to determine the feasibility of leaching with acidified ferric sulfate solutions. The ore and tailings, containing 1.24 and 0.24 percent copper, respectively, were from the White Pine Copper Co., Ontonagon County, Mich. The investigation showed that ferric sulfate leaching of the ore and tailings followed a predictable pattern. Thus, with 4 hours of leaching, up to 58 percent of the copper in the ore was extracted, but prolonged leaching (2 to 3 weeks) was required to dissolve more than 90 percent of the copper. Similarly, about 50 percent of the copper in the mill tailings sample was dissolved in a few hours, but 8 days or more were required for extractions of over 90 percent.

Jan 1, 1962

By M. I. Copeland

The investigation of the iron-gadolinium phase diagram is part of a project undertaken by the Bureau of Mines and sponsored by the Atomic Energy Commission to investigate rare-earth alloys. Data from the investigation of the iron-gadolinium phase diagram revealed a single eutectic system with very limited terminal solubility and three intermediate phases. The eutectic point occurs at about 85 percent gadolinium, and the eutectic isotherm, which occurs at 850° C., extends from the compound Fe2Gd to 99-plus percent gadolinium. Very little solubility of the solid phases in each other was observed. The three intermediate phases, FegGd, Fe3Gd, and FeaGd, melt incongruently at peritectic isotherms at 1,320°, 1,150°, and 1,080° C., respectively. The crystalline systems of the three phases were determined as follows: FegGd, hexagonal; Fe3Gd, hexagonal or rhombohedral; and FeaGd, face-centered cubic. No lowering or raising of the alpha-gamma iron transformation at 910° C., the gamma-delta iron transformation at 1,388° C., or the gadolinium transformation at 1,262° C. was observed. The principal methods used in determining the iron-gadolinium phase diagram were melting-point determinations, thermal analyses, metallographic examination, and X-ray diffraction analyses. Melting, heat treating, and thermal analyses were conducted in a vacuum or under a helium atmosphere because of the avidity with which oxygen combines with gadolinium at elevated temperatures. A few hardness values were determined, but they had no part in the derivation of the phase diagram. No other mechanical properties were determined.

Jan 1, 1962

By G. W. Birge

Carbonizing properties of the principal coal beds of Perry County, Ky., are described in this Bureau of Mines report. Seven samples, representing the Hindman, Flag, Haddix, and Fire Clay beds, were carbonized by the Bureau of Mines-American Gas Association (BM-AGA) method, and yields of products and physical properties of cokes were determined. Carbonizing properties of blends of Flag and Fire Clay coals, with 20 and 30 percent Pocahontas No. 3 low-volatile coal from McDowell County, W. Va., also were determined. Expanding properties of the Flag and Fire Clay coals and their blends were determined in the Bureau of Mines sole-heated oven. The Perry County coals tested are high-volatile A bituminous in rank and, with the exception of the Hindman-bed sample, which contained excessive sulfur, were chemically suitable for metallurgical use. The three coals tested in the sole-heated oven contracted less than normal for Appalachian coals of similar rank, Blending the Fire Clay and Flag coals with 20 or 30 percent low-volatile coal increased coke strength appreciably but increased the expansion beyond normal limits for industrial blends.

Jan 1, 1962

By G. W. Birge

Carbonizing properties of the principal coal beds of Butler County, Pa., are described in this report by the Bureau of Mines. Eight samples, representing the Upper Freeport, Lower Freeport, Upper Kittanning, Middle Kittanning, Lower Kittanning, Clarion, and Brookville beds, were carbonized at 900° C. by the Bureau of Mines-American Gas Association (BM-AGA) method. Butler County coals rank as high-volatile A bituminous and are generally characterized by high sulfur content compared with Appalachian coals used for industrial coking. If cleaned, the Brookville and one sample of Upper Freeport coal would be acceptable as the major component of metallurgical coking blends. The other Butler County coals tested would be unsuitable for this purpose because of either excessive sulfur or poor coking properties.

Jan 1, 1962

By C. S. Tout

While investigating methods for determining the best temperatures for hot-working experimental stainless steels, the Bureau of Mines Albany Metallurgy Research Center developed a machine in which hot-twist tests could be made in a few minutes. This machine is similar to some used previously except that specimens are heated by induction instead of by radiation, and their temperature is measured by a calibrated radiation-detection unit instead of by a thermocouple. In. developing the technique for using the new machine, tests were made on specimens of medium-carbon steel, mild steel, and AISI (American Iron and Steel Institute) type 304 stainless steel. Tests also were made on as-cast specimens and preworked specimens of experimental AISI type 202, low austenitic stainless steel, and as-cast specimens of AISI type 301 experimental stainless steel. The optimum hot-working temperatures were determined for all types of steel tested. Also, data were gathered on the effects of test speed and temperature on torsional strength and the effect of twisting on tensile stress in the specimen.

Jan 1, 1962

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 D. W. Scott

Thermodynamics is a powerful tool for investigating rotational isomerism in substituted ethanes and related molecules. Accurate calorimetric data can be interpreted to give information, not only about the energy difference between conformations, but also about the shape of the potential barrier hindering rotation from one conformation to another. However, a deterrent to this use of thermodynamics is the labor required to calculate the contributions to the thermodynamic functions for assumed potential functions. Tables of thermo-dynamic contributions for appropriate potential functions can eliminate that labor and greatly facilitate the thermodynamic study of rotational isomerism. In this research, tables of contributions to the thermodynamic functions were compiled for two potential functions typical of some commonly encountered examples of rotational isomerism. TYPES OF POTENTIAL FUNCTIONS Potential function 1, illustrated in figure 1, A, has two equal minima higher than the third. It has the general shape of the barrier to internal rotation in n-butane, for example. The trans conformation of n-butane has the lowest energy, and the two skew or gauche conformations have equal but higher energy. Potential function2, illustrated in figure 1, B, has two equal minima lower than the third. It has the general shape of the barrier in 2-methylbutane, for example. The two C1 conformations of 2-methylbutane have equal energy much lower than the assumed Cs conformation, which has not been observed spectroscopically.

Jan 1, 1962

By W. H. Ode

An investigation of standard methods for determining ash in low-rank* coals showed that generally 60 to 95 percent of the total sulfur in the coal is retained in the ash as SO3. This large sulfur retention causes a positive error in the determined mount of ash of as much as 6 percentage points for the coals examined, although it usually is 2 to 3 percentage points for lignites and about 1 for subbituminous coals. Unless the sulfur content is low or unless a correction is made for the SO3 retained, the fixed carbon and oxygen have an equivalent negative error when determined by difference; also other inaccurate analytical values occur when the data are calculated on an ash- free bas is. No simple modification of the ashing procedure was found that would reduce the sulfur retention to a point where its effect on the ash determination would not be significant, Therefore, for accurate analytical work on law-rank coals, the SO3 should be deducted from the determined ash to obtain a "corrected" ash value.

Jan 1, 1962

By John Ward Smith

The potential economic value of oil shale depends on the products from thermal degradation of the rock, because no other practical method for producing valuable material from oil shale has been found. Detailed study of thermal degradation behavior can aid in characterizing oil shales and their deposits and in evaluating oil-shale processing methods, Numerous publications describe various pyrolysis properties of oil shales (see surveys 3, 9, 11 and articles 1, 2, 4-8, 10, 12),4 but they do not describe a generally applicable analytical procedure for detailed evaluation of thermal degradation products. The analytical method presented here for such evaluations is designed to provide for: 1. Control of retorting conditions--temperature, heating, rate, reaction atmosphere--plus some control over retort pressure and carrier-gas flow, 2. Precise direct gravimetric measurement of the thermal degradation products--oil, water, gas, and spent charge (residue after thermal treatment of the charge). 3. Samples of all products. 4. Determination of the identities and amounts of gaseous compounds produced. 5. Elemental analysis and gross heating value of all products. 6. Determination of the distribution in the retorting products of the elements present in the original samples.

Jan 1, 1962

By Gerald W. Elger

This report compares the quality of zirconium metal prepared by batch reduction of zirconium tetrachloride by (1) sodium, (2) magnesium, and (3) mixtures of sodium and magnesium. Criteria for quality are based on chemical analyses and hardness testing of zirconium arc-melted from sponge. The best quality zirconium with respect to low oxygen content and hardness numbers was prepared by reaction of zirconium tetrachloride with a mixture of sodium and magnesium. It was found that this reaction could be successfully carried out by two methods: (1) addition of sodium and magnesium before the initial reaction and (2) periodic injection of sodium during reaction of zirconium tetrachloride with magnesium. The largest quantity of metal was found to be recovered from experiments in which a mixture of sodium and magnesium was used. Magnesium appeared to be a better reductant than sodium because magnesium-reduced zirconium contained less oxygen and exhibited lower hardness numbers than sodium-reduced metal.

Jan 1, 1962

By Gerald V. Gibbs

As a part of the Bureau of Mines long-range program in asbestos, synthetic asbestiform compounds and minerals were prepared and described. Fundamental structural data on two such compounds are given in this report. Crystallographic data are provided for the synthetic isotypic compounds potassium-lead silicate, K2.Pb4 -Si8021 (I), and lead-aluminum silicate, Pb2. Pb4 .Al2Si6O21 (II). The space group symmetry 14/mmm was assigned provisionally to I and II on evidence of single crystal and piezoelectric measurements. A statistical evalua¬tion of indexed powder diffraction data revealed the cell edtes of I to be a 11.816 and c 7.932A and those of II to be a 11.723 and c 8.044A. The phases are uniaxial with observed refractive indices eD 1.790, an ?D,699 and eD 1.884, cusp 1,807, respectively. The atomic structure of I and II may be based on a complex of chains of silicon-oxygen tetrahedra lying along the c cell edge similar to the type of chain structure postulated by Pauling for scapolite. K2.Pb4.Si8021 and Pb2.Pb4 Al2Si6021 were first described by Geller and Bunting (5, 6)4 as fibrous compounds similar in crystal habit to asbestos. These authors gave powder diffraction data, although no attempt was made to find the cell edges or to index the powder diffraction patterns. Later, Shell and others (9) conducted a crystallochemical study of these fibrous silicates in search of a substitute for strategic asbestos. Their single crystal data revealed K2.Pb4 -Si8021 to be tetragonal body-centered with cell edges a 11.66, c 7.95 A. Pb2.Pb4 Al2Si6021 was concluded to be isotypic with K2.Pb4 -Si8021 on the basis of similar powder diffraction patterns, chemistry, and physical properties. No attempt was made, however, to index the powder diffraction record nor to determine the appropriate space group of either compound.

Jan 1, 1962

By G. Asai

The purpose of this Bureau of Mines investigation was to determine the properties of arc-melted iron-chromium alloys ranging in chromium content from 12 to 50 wt.-pct. Alloys were prepared by consumable-electrode arc melting of electrodes composed of high-purity chromium and high-purity iron. Alloys were fabricated to rod and sheet, and the following data were obtained: Electrical resistivity, hardness, tensile strength, and impact strength at room temperature; and creep-rupture life at 650° C. (1,200° F.). As the chromium content of the annealed alloys varied from 12 to 50 pct., the properties varied as follows: The electrical resistivity increased proportionally from 41 to 53 microhm-cm,; the Rockwell hardness varied from A 38 to A 58; the tensile strength ranged from 52,000 to 96,000 p.s.i.; the impact strength of V-notched charpy specimens varied from 140 to 405 ft.-lb., and the 100-hour creep rupture life at 1,200° F. varied from 5,000 to 16,000 p.s.i.

Jan 1, 1962

By C. J. Chindgren

Upgrading of commercial red cake and recovery of vanadium oxide from uranium-vanadium mill solutions were investigated by the Bureau of Mines. Alternative procedures potentially useful for manufacture of high-quality vanadium oxide at the mill site were explored and developed. The simplest and best procedure for converting commercial red cake containing about 10 percent combined sodium and potassium oxides (Na20) (K20) into a 98- to 99-percent vanadium pentoxide (V205 product appeared to be a metathesis in an ammoniacal solution of ammonium sulfate. Molybdenum, as well as the alkali metal oxides, was removed from the red cake by this procedure at a modest expenditure of labor and reagents. When preparing vanadium oxide of higher grade, it was necessary to dissolve the red cake and reprecipitate the vanadium as ammonium metavanadate. Calcination at 450° C, decomposed the metavanadate and yielded oxide of about 99.5 percent V205. By recyrstallizing the metavanadate before decomposition, an oxide product approaching 99.9-percent purity was obtained.

Jan 1, 1962

By E. L. Singleton

This Bureau of Mines investigation was initiated to study and establish some of the chemical and physical characteristics of the condensed Mno-Si02 system. To prevent oxidation of the manganous ion, I atmosphere of purified helium was used in the furnaces. Solidus-liquidus curves and invariant points were established from melting-point determinations and were supplemented from data obtained by the static-quenching method. Experimental findings and data are for the intermediate compounds of tephroite and rhodonite with their respective eutectics represented at 25.5 and 37.2 weight-percent silica. Tephroite melts congruently at 1,347° C., and rhodonite melts incongruently at 1,286° 8.. A metastable transformation was determined to exist at the 1,347° C. isotherm, the congruent melting point of tephroite. A composite X-ray-diffraction pattern was formulated for synthetic rhodonite. This investigation contributes fundamental data leading toward a better understanding of the more complex slag systems.

Jan 1, 1962