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By V. A. Nieberlein

This paper presents the results of research undertaken to recover titanium and columbium by low-temperature chlorination of low-grade columbium-bearing ilmenite concentrates, and to simultaneously remove chlorinated impurities from the volatile chlorides without resort to distillation. Coke-reduced ilmenite was chlorinated at 400° to 500° C., and the resulting TiC14 was free of most impurities before condensation. A heated purification column was used wherein various packing materials reacted chemically or physically with the impurities which passed through them in the vapor phase. A nearly water-white TiC14 product was obtained directly. The principal impurities in the titanium tetrachloride were: 0.02 percent Fe, 0.01 percent V, 0.05 percent A1, 0.04 percent Si, and 0.07 percent Cb. This is a less pure product than commercial TiC14. Most of the columbium was recovered as crude CbC15, requiring further refining.

Jan 1, 1960

By Henry P. Chandler

Tripoli is the general name for a number of fine-grained, lightweight, friable, minutely porous, forms of decomposed siliceous rock, probably derived from siliceous limestones or calcareous cherts. Tripoli is often confused, both in the trade and technical literature, with tripolite, a diatomaceous earth (diatomite), found in Tripoli, North Africa. A material found near Seneca, Mo., resembling tripolite was incorrectly termed "tripoli." This name has persisted and now has a definite physical and trade meaning. However, tripoli contains no diatoms, is of an entirely different origin, and has chemical and physical properties different from those of tripolite. There are two distinct types of tripoli in the United States; that from the Missouri-Oklahoma field and that from the Southern Illinois field. Commercially the term "tripoli" is applied to the material from the Missouri-Oklahoma field, while the material from the Southern Illinois area is often referred to as "amorphous" or "soft" silica. Material similar to the Missouri-Oklahoma tripoli, but finer grained, occurs in northwestern Arkansas. In its Minerals Yearbook the Federal Bureau of Mines groups statistically under "natural silica abrasives," tripoli from these producing areas and rottenstone from Pennsylvania. The justification for this grouping is the similarity of use. Composition and Physical Properties Commercial tripoli contains 97 to 99 pet SiO2. The remainder is mostly alumina, iron, lime, soda, and potash, some of which may impart desirable physical properties to the material. Variations in the chemical composition of tripoli are not as important as its physical characteristics. The color of tripoli varies from white to cream, brown, rose, and red, the variations from white being the result of iron deposited from percolating surface waters. The commercial varieties of tripoli mined in the Missouri-Oklahoma area are designated as cream and rose. Other physical properties of the tripoli from this area are: Free quartz, less than 0.5 pct; oil absorption, 50.71 to 53.14 pct; water absorption of the crude tripoli, about 38 pct, and of prepared material, about 52 pct; fracture, uneven to conchoidal; specific gravity, 2.15 to 2.62; weight per cubic foot crude, 35 lb, ground, 55 lb; fusion point, 3,225° to 3,300°F; and refractive index, 1.54. Tripoli occupies about 1 cu yd to the short ton in place and about 1.5 cu yd when broken. Packed for shipment, the powdered material occupies about 33 cu ft to the ton. Its value and usefulness depend primarily on a low content of crystalline silica, size of the natural particles, absorption, and color. Some beds in the Missouri-Oklahoma area are of sufficiently compact material that large, fairly strong blocks may be removed. These find a market as filter blocks and have been used for building material. In the Southern Illinois field the color of the material is the important physical property; pure white is preferred. The rottenstone mined in Pennsylvania is of higher density and lower in silica content than the various types of tripoli. Its composition approximates 60 pct silica, 18 pct alumina, 9 pct iron oxide, 8 pct alkalies, with small amounts of lime and magnesia. The material apparently is a ferruginous and siliceous shale, having properties rendering it suitable as an abrasive or as a filter for paint, rubber, and plastics.

Jan 1, 1960

By Alla D. Mah

THERMODYNAMIC data for manganese and its inorganic compounds have not been critically surveyed since the work of Maier (31) 3 in 1934. At that time data were lacking or inadequate for many of the important metallurgical compounds. Experimental work, conducted during the intervening years, has supplied so many new thermodynamic values that it is again desirable to examine the available data and compile them into a single publication for handy reference. This paper consists of three main sections. The first summarizes the basic metallurgical thermodynamic data for manganese and its compounds, including heat capacities, entropies, heat contents, temperatures and heats of phase changes, vapor pressures, and heats and free energies of formation. All data available to May 1959 have been considered. The second section contains heats, free energies, equilibrium pressures, and equilibrium constants of reactions of manganese compounds, with special emphasis on metallurgical reactions. The third section supplies basic thermodynamic data for other elements and compounds encountered in metallurgical reactions of manganese, thus making it possible for the reader to conduct thermodynamic calculations without recourse to other literature.

Jan 1, 1960

By C. A. Frenzel

Extensive spectroscopic data are needed in making reliable vibrational assignments for use in calculating thermodynamic functions of polyatomic molecules. The fundamental vibrations of organic molecules may be observed at any wavelength from 2.5 to 200 microns (micron = µ = 10-4 centimeters), but most often in the region from 3µ to 50µ. Raman spectra generally cover the range in which fundamental vibrations occur, but equally important infrared spectra usually are not measured at wavelengths longer than 25µ. This limitation results because most infrared spectra are determined for analytical purposes, which seldom require information outside the region 2µ to 25µ. Measurements of infrared spectra in the range 15µ to 35µ recently were begun by the Bureau of Mines to obtain data needed in making vibrational assignments. This report presents the spectra of the following thirteen compounds: Tetrahydrofuran, 1-methylpyrrole, piperidine, 2-methylpyridine, 3-miuthylpyridine, 2-propanethiol, cyclopentanethiol, 2-methyl-2-butanethiol, 3,3-dimethyl-2-thiabutane, cyclohexanethiol, cyclopentyl-l-thiaethane, 2,4-dimethyl-3-thiapentane, and hexamethyldisiloxane.

Jan 1, 1960

By T. E. Gray

This report describes preparation characteristics of the significant coalbeds in Marion County, W. Va., as determined by the Bureau of Mines. It is one in a series telling what coals are suitable for producing metallurgical coke, either as mined or after beneficiation. Over 9.4 million tons of coal was produced in Marion County, W. Va., in 1958, of which almost 6 million tons was cleaned mechanically in nine cleaning plants. All of the coal mechanically cleaned came from the Pittsburgh bed. The Bureau of Mines estimated that 1,578 million tons of recoverable coal remained in the county in beds 28 inches or more thick as of January 1, 1955.

Jan 1, 1960

By D. Geiselman, A. G. Guy

Single cvystals were grown from high-purity magnesium containing known amounts of nitvogen in the range 0.0008 to 0.0048 wt pet. Crystals of known ovientation were tested in tension in an Instron ma chine to determine the yield strength and to obsevue wheather a yield point occurred. Slowly cooled crystals or those given a solution heat treatment did not show a yield point. However, crystals that were aged following a solution treatment showed a yield point for all of the nitrogen contents studied. It was concluded that nitrogen caused the yield point by the Cottrell mechanism. NITROGEN has been shown to produce sharp yield points in single crystals of cadmium, zinc,2'3 ß-brass,4 and iron,5,6 as well as in polycrystalline iron7 and molybdenum.8,9 Since magnesium has a structure similar to zinc and cadmium, it seemed reasonable that magnesium should also exhibit a sharp yield point provided it contained sufficient nitrogen. Bobalek and Shrader10 reported a total nitrogen content of 0.002 to 0.0065 wt pct in com- mercial magnesium alloys, an amount well in excess of that required by theory. However. magnesium differs from cadmium and zinc in that it forms a stable nitride, Mg3N2, which has a standard free energy of formation of -95,480 cal per mole at 25" c." If rather than being in solid solution, the nitrogen were predominantly combined as the nitride, it could not act to produce a yield point. This type of behavior is the basis for the elimination of strain aging and a yield point in steel by the addition of strong nitride formers such as titanium,12 columbium,13 aluminum,14 vanadium,15 and boron.16,17 Thus, there appeared to be factors both favorable and unfavorable to the production by nitrogen of a sharp yield point in magnesium, and the purpose of this investigation was to determine the actual behavior of magnesium crystals containing known amounts of nitrogen.

Jan 1, 1960

By W. R. Hardwick

This information circular describes mining methods and practices at New Cornelia Branch, Phelps Dodge Corp., Ajo, Ariz. It is one of a series being prepared by the Bureau of Mines on mining methods, practices, and costs in various mining districts of the United States. The New Cornelia mine (fig. 1) is at Ajo, a town in southwestern Arizona (fig. 2) on Arizona State Highway 85 in the western part of Pima County. The [oncentrator] and smelter are near the mine (fig. 3). Copper ore is mined, crushed, ground, and concentrated, and the concentrates are smelted. Copper is cast in anode form and sent to the Phelps Dodge Corp. refinery in El Paso, Tex.

Jan 1, 1960

By C. S. Gibson

"MOST of the mines in the Province of Ontario in Canada are multi-level operations in steeply dipping veins; yet there is an appreciable number whose de-posits are relatively flat-lying, ranging up to 45° inclination.The veins vary in width up to several hundred feet and may or may not be branching systems. The depths of mines range from a few hundred to 8,000 feet, approximately. The primary products of the underground group are asbestos, gold, silver, cobalt, copper, nickel, iron, uranium, talc, fluorspar, gyp-sum and salt.There are a few open-pit mines. The majority are temporary in type because, as the outcrops are removed, mining is continued be-low surface. Primary products of the open pits are copper, nickel, iron, magnesium and nepheline syenite.The industry as a whole employs about 50,000 persons, approximately 60 per •cent of whom have dust-exposure occupations. The definition of a dust-exposure occupation and the requirements for •dealing with same are set forth in The Mining Act of Ontario.Results of extensive and continuing studies on the incidence and progression of silicosis have been reported periodically for years past, in annual reports of the Mines Accident Prevention Association of Ontario and in papers presented at Conferences sponsored by Mcintyre Research Foundation of Toronto, all of which have been published. The information provided therein proves the effectiveness of the means being used to prevent silicosis and allied disorders."

Jan 1, 1960

By Bernadette C. Michalski

Mineral raw materials, labor, capital, and technology form the basis of industrial production. The augmentation of one or all of the elements--labor, capital, and technology--will result in industrial growth. Thus, an increase in the labor force would increase output. A similar result would be achieved by expanding capital investment and supplying labor with more equipment. Finally, industrial growth can be achieved by introducing more productive methods and techniques born of technological advancement. The Soviet Union has employed these elements in many patterns to catapult from an agricultural to an industrial economy in four decades. The early history of the Soviet Union was marked by limited capital and borrowed technology, forcing the Soviets to concentrate on an abundant labor reserve to support the industrial program. The source of this reserve was the rural population. In [1928], 80 percent of the working population was employed in agriculture. This figure dropped to 43 percent by 1956, whereas industrial employment in the same period increased from 8 to 31 percent.3/

Jan 1, 1960

By W. A. Stickney

As part of a Bureau of Mines program to investigate recovery of manganese (Mn) from low-grade materials, laboratory studies were made of four samples of mill rejects: Three from Montana and one from Peru. These studies demonstrated that certain mill-waste products can be a potential source of manganese. Both manganese oxide and carbonate minerals were recovered by flotation in an acid circuit with a fuel oil-tall oil emulsion as collector. Sintering) required to prepare a physically acceptable product, also was used as a method of beneficiation. In addition to being low-grade, some of the samples presented problems of intimate mineral association and complex textures.

Jan 1, 1960

By George R. Mitchell

It is a common observation that objects having, different; temperatures exchange energy by radiative transfer. The quantity of radiant energy emitted by an object is a definite function of its temperature. Therefore, a measurement of emitted radiation, by means of a calibrated radiometric instrument, provides a temperature measurement without contacting the emitting object. The physical laws describing radiant energy transfer and their application to remote temperature measurement form the substance of this paper. The energy radiated by bodies having temperatures up to 4000°C is largely in the infrared spectral region. The infrared spectral region is that part of the electro-magnetic spectrum having wavelengths longer than visible light and extending to the microwave region. The wave-lengths range from 0.7 micron (1 micron = 10-4 cm) to 1000 microns. In general, infrared radiometry deals, with the methods of measuring energy flux in the 1 to 15 micron region of the infrared spectrum.

Jan 1, 1960

By A. U. Seybolt

Since the time this topic was originally treated in 1954, more recent French3,1 work has been published making it advisable to repeat the earlier oxygen solubility experiments, but using iron of a higher purity. Upon repeating oxygen saturation experiments with zone-refined iron, it was found that the oxygen solid solubility was at least an order of magnitude less than previously observed. SINCE the publication of an earlier paper1 (1954) on this subject by the present author, several contributions on this topic have appeared. Meijering2 in 1955 attempted to reconcile recent conflicting solubility data, without reaching any definite conclusion. sifferlen3 (1955) found that iron of high purity appeared to absorb a quantity of oxygen (0.005 to 0.025 pct) approximately proportional to the structural imperfections present, such as polygonization and grain boundary area. However, he also indicated that purity itself was a significant factor. He concluded that very pure iron nearly free of lattice imperfections would have essentially zero oxygen solubility. His second paper4 (1957) supported this contention since a zone-melted iron containing initially 0.0007 pct O analyzed only 0.0006 pct 0 after prolonged soaking at 850°C with an FeO layer on the surface. Because of the discrepancy between the results of Ref. 1 and those of Sifferlen, it seemed desirable to attempt to resolve this disagreement. EXPERIMENTAL PROCEDURE AND MATERIALS The experimental method used by sifferlen3,1 was essentially the same as that of Ref. 1. In this technique thin iron strip with a surface layer of FeO is soaked for prolonged periods at an elevated temperature in order to saturate the iron with oxygen. After two days at temperatures near 800° to 900° C, one would expect that the iron would be in equilibrium with the surface FeO. In the work reported in Ref. 1 there was evidence that two days holding at 8000to 900°C was more than sufficiently long for saturation. Sifferlen used 48 hr at 850°C. Because of the evidence presented by Sifferlen that the apparent oxygen solubility is a function of iron purity, three grades of iron were used as indicated in Table 1. The Bureau of Standards wire was used only for resistivity tests, while the other two irons were used for saturation-analysis tests of the type described above.

Jan 1, 1960

"Qatar, crude petroleum, production, annualdata MY 1949-51Quality mine, Ark., coal, carbonizing properties TP 667washabilty study RI 496N. Dak., lignite, grindabilty as function ofmoisture, tests, results RI 5167"

Jan 1, 1960

By K. A. Clark

"The repacked mineral aggregates of good grade oil sands have permeabilities ranging between 15 darcys to 350 millidarcys. The variation is due to the silt contents of the aggregates. Few good grade oil sands contain as much as 30 per cent •silt, most of them contain less than 20 per cent, and a large proportion have less than 10 per cent.The permeabilities of repacked good grade oil sands (oil included) depend on the degree of liquid saturation. When saturation with oil plus water reaches between 80-90 per cent, permeability is reduced to zero. As total saturation decreases below 80 per cent, permeability increases ranidly. Permeabilities of between one and two darcys were observed for total saturations between 60-70 per cent.The mean value for 18 measurements of the permeabilities of ""undisturbed"" core samples of good grade oil sands was 50 millidarcys. This value is •probably too high. The mean value for 20 measurements on core samples of interbedded oil sand and shale was 100 millidarcys. The mean value for 11 measurements on shale was 10 millidarcys."

Jan 1, 1960

By T. E. Gray

This report describes the preparation characteristics of the more significant coalbeds in Monongalia County, W. Va. It is one of a Bureau of Mines series planned to determine coals suitable for producing metallurgical coke, either as mined or after beneficiation. Over 9.5 million tons of coal was produced in Monongalia County in 1957, of which more than 7 million tons was cleaned mechanically in 8 cleaning plants. On January I, 1954 the Bureau of Mines estimated that 1,576 million tons of recoverable coal remained in the county in beds 28 inches or more thick.

Jan 1, 1960

By G. H. Martindill

Complex chemical and physical changes occurring during carbonization result in a heterogeneous system composed of gaseous, liquid, and solid phases, whose relative proportions and chemical compositions change constantly as temperature increases. Studies in which the participating variables are isolated and controlled should be useful in formulating the mechanism of coal carbonization. The most characteristic property of a coking coal is its ability to form a plastic mass at a certain stage of the carbonization process. During this period it is believed that fluidity of the coal influences the properties of the resultant coke. This report gives results of an investigation by the Federal Bureau of Mines of the influence of the maximum fluidity attained by the charge on the physical quality of the coke or char produced. As a first approach to the problem, researchers investigated high-melting-point pitches, which are relatively simple carbonaceous materials. The plastic properties of these pitches, prepared specially for this work, varied greatly; their fluidities, as measured by the Gieseler plastometer, covered most of the fluidity range characteristic of coking coals. Blending these pitches with increasing pro-portions of fine coke progressively reduced their fluidities. Coal-pitch and coal-coke blends also were treated; their fluidities were varied by changing their blending ratios. The various blends were carbonized in a small-scale carbonizer and the resistance of the carbonized residue (char) to abrasion was determined in a small-scale tumbler test, using the Roga drum.

Jan 1, 1960

By Gordon W. Parsons, Ross E. Sampson

"THIS PAPER will trace the work done in bringing the Munro underground ""A"" •Orebody into production to replace the open pit, which was scheduled to be completed early in 1959. Included will be an outline of the exploration work and early planning, and of the final decisions on mining methods. Some of the more detailed work will be described and reasons will be given for the decisions made regarding development work, mine ventilation, ground support, and equipment. Brief mention will be made of open pit operations, as these have had some influence on underground development. Also, some of the main geological features of the ore occurrence will be de-scri0bed, as these had to be taken into consideration when making decisions on ore development and mining methods.LOCATION AND HISTORYhe Munro mine of Canadian Johns-Manville is in Ontario, approximately 50 miles east of Timmins and 40 miles west of the Que-bec-Ontari-0 boundary. The producing orebody is in the southwestern part of Munro township. Property controlled by the Company extends nortl1westerly about 2¥2 miles into Beatty township, on which two other interesting asbestos-bearing zones have been partially expl-0red. Active exploration work on the property was started in March, 194.9, and continued until the summer of 1950."

Jan 1, 1960

By F. C. Frischknecht

Most early development and application of electromagnetic prospecting methods took place in Scandinavia, where geological conditions favor their use. In other parts of the world these methods have aroused cycles of interest, but in Scandinavia they have been used continuously and successfully since the 1920's. Electromagnetic methods may be classified into two general groups. One group includes methods in which the source of the electromagnetic field remains stationary while the receivers are moved about to explore the area. The other includes procedures in which the energizing and receiving systems are moved together. Other classifications could be based on the size of the energizing source, the particular components of the electromagnetic field which are measured, or the mode of transporting the equipment. The difference between fixed-source and moving-source methods, however, is of such great fundamental importance that it will be emphasized in this discussion. FIXED-SOURCE METHODS Essentially, a fixed-source method consists of the measurement of electromagnetic fields about the source. The mutual coupling between the source and the earth is constant, but the mutual coupling between the receiver and the earth (unless the earth is homogeneous) and also between the source and the receiver changes at each station. The results are usually normalized by relating the field data to the calculated free space or primary field. Turam and Radio Reference Signal Methods: The turam or two-frame* (see Fig. 1A) is probably * Turam means two-coil. the most common fixed-source method. The energizing source is an insulated cable grounded at both ends or formed into a large rectangular loop. Measurements are taken along a traverse at 5 to 50-meter intervals using two small receiving coils, the lagging coil being placed at the position previously occupied by the leading coil. The complex ratio (i.e., inphase and out-of-phase ratios) of the voltages induced in the two coils is measured. Operating frequency range is about 100 to 800 cps. In a typical turam survey a straight, grounded cable several kilometers long is laid out parallel to the probable strike of the ore deposits or conducting strata being sought. An area extending 1 or 2 km on each side of the cable, and within 1 or 2 km of the ends of the cable, is surveyed. Measurements are made at stations 5 to 25 m apart along traverses perpendicular to the cable. Measurements may be made along lines parallel to the cable to serve as base lines for the traverses or for other special purposes. Commonly the receiving coils are oriented with their planes horizontal so that only the vertical component of the field is measured. If additional information is required, one of the hori- zontal components may also be measured by orienting the coils with their planes vertical. In a modified turam technique developed recently for both ground and airborne measurements (Fig. 1B) the amplitude of the complex voltage induced in a single receiving coil is measured and its phase compared with that of a reference signal transmitted from the energizing system by a radio frequency carrier. Thus the un-normalized field is obtained directly, whereas with the turam method it is obtained by calculation from the ratios. The turam method and its modifications have a greater working depth than the other electromagnetic procedures used in ore prospecting. Under favorable conditions conductors have been located at depths of 200 to 300 m. A modified turam method with one of the electrodes grounded in the upper end of a plunging orebody was used to follow the extension of this body to a depth of 200 m beneath a layer of conducting schists. Straight grounded cables are usually preferred to insulated loops because they are easier to lay out and because they often make the method more sensitive. The greater sensitivity of a grounded cable is a result of ground return currents which may flow in the orebodies in addition to the eddy currents caused by induction from the current in the cable. Anomalies in the vertical field due to eddy currents are characterized by a correspondence between high values for the inphase component and positive out-of-phase components and/or low values for the inphase component and negative out-of-phase components. Also the inphase component may approach zero, but it does not become negative. In very long continuous conductors that are parallel to a grounded cable the effect of ground return currents may far exceed the effect of eddy currents. These ground return currents cause a lack of correspondence between the inphase and out-of-phase components and may cause negative inphase or anti-phase components. It becomes difficult to carry out the measurements and often difficult to interpret the results. Such results immediately suggest the presence of graphitic strata, however, since ore deposits are rarely extensive enough to accumulate sufficient ground return current to cause these results. A cable laid out perpendicular to the strike or an insulated loop is sometimes used in areas where graphitic schists and slates are present. Anomalies are then completely or almost entirely due to eddy currents and are easier to interpret. The measured voltage ratios are normalized by either subtracting or dividing by normal field ratios calculated from free space considerations. The normalized ratios are then plotted as individual profiles. When significant anomalies occur in the ratio measurements, the actual normalized fields are calculated by beginning with a measured or an assumed value for the field at a point near the cable and successively multiplying this value by the normalized ratios. There is a similarity between this process and a numerical integration of the ratio curve. Conversely, in many respects the ratio curve is similar to the first derivative of the field curve.

Jan 1, 1960

By J. Gordon Parr, D. A. Whitaker, G. A. Yorko

High purity alloys of zinc with 25 per cent to 50 per cent aluminum, have been prepared. Mechanical properties of the as-cast and heat-treated alloys have been related to constitution, determined by x-ray diffraction and microscopic methods. Investigations include the effects of aging and of small nickel additions on the properties of the alloys.

Jan 1, 1960

By The Staff

"THE Wabana iron ore mines, owned and operated by the Dominion Steel and Coal Corporation, Limited, .are on Bell Island in Conception bay, on the east coast of Newfoundland. Mining began on surface in 1895 and, although open-pit work is still done on a small scale, the entire output may be considered to•be derived from extensive submarine workings. In 1958 the average daily production of hematite ore was close to 12,000 tons, almost all of which was concentrated in a heavy-media plant. SUMMARYThe character, occurrence, and extent of the submarine bedded deposits enabled early operators to meet prevailing market demands with the minimum attention paid to exploration. Mechanization of the mine and the pressure for sustained high tonnages since 1955 have emphasized the importance of an expanded exploration and development programme.A serious handicap has been the impossibility of utilizing normal diamond drilling methods to explore ore conditions in advance of mining faces. Drilling between tl1e bedded zones has been done but the major difficulty has been to delineate ore reserves in the lower bed, which has the greatest ore potential of the three mineable seams."

Jan 1, 1960