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Established as a Division February 16, 1948 H Rush Spedden, Chairman Neil Plummer, Associate Chairman Stephen E Erickson, First Regional Vice-Chairman D A Dahlstrom, Second Regional Vice-Chairman Win T Marston, Secretary-Treasurer Dorr-Oliver, Inc 77 Havermeyer Lane Stamford, Connecticut

Jan 1, 1960

By R. S. Archibald

The subject of this paper is particularly appropriate, since Daniel C. Jackling was active in early exploitation of taconites on the Mesabi Range and contributed greatly to their later economic development. After his success in developing the low grade porphyries in the West he looked for more worlds to conquer, and so undertook the concentration of low grade taconites, from which he hoped to produce commercial ore. Mesabi Iron Co., organized in 1919, actually did produce merchantable sinter from taconites in 1922. The enterprise did not prove commercial at the time, as cost of production was high and the surplus of iron ore in the Lake Superior District already contributed to a low market price, but this same property has since been developed by Reserve Mining Co. The work done by Jackling had much to do with the success of this later venture. Iron ore was first discovered on the Marquette Range in Michigan in 1845. The first ore from this range came from the old Jackson mine in Negaunee in 1848. During these early years this property and others on the Marquette produced limited tonnages for transportation to Lower Lakes and for consumption by charcoal furnaces in the area, where a plentiful supply of hardwoods furnished the charcoal for iron smelting. The Marquette and other ranges tributary to Lake Superior did not produce much ore for transportation to Lower Lakes until the locks at Sault Ste. Marie were constructed, but from the time the first lock at the "Soo" was completed in 1855 these ores were transported through the locks to consumer centers in the East. The Marquette Range has a history of continuous production from 1848 to the present day. In 1877 the Menominee Range was discovered at the location of the old Penn Mines near Vulcan, Mich. There were further discoveries of ore on the old Menominee Range and at Florence, Wis., in 1880 and at Iron River and Crystal Falls, Mich., in 1882. Penn Mines continued in operation from the date of their discovery until they were finally exhausted by Pickands-Mather in 1945, but operations still continue on the Menominee in the Crystal Falls and Iron River districts. Ore is shipped to a lake port at Escanaba, Mich.

Jan 1, 1960

By O. E. Brown

The measurement principle of the Coulter Counter for particle size analyses is described. The application of the Coulter Counter to cement particle content and size analysis and to the size distribution of clinker from standard grindability tests are described. Methods of calibration, sample preparation and data reduction are presented. The results of the analyses obtained are compared with characteristics associated with performance showing both concordance and non-concordance of test data., Future uses of the Coulter Counter for particle size analysis in research and plant control adaptations are indicated.

Jan 1, 1960

By G. F. Round

In order to obtain values of angle of shearing resistance and initial resistance for McMurray oil sand for use in general design calculations, the shear strength of this oil sand was measured in a controlled strain type tester, modified so that the rate of deformation could be varied between 0.01725 and 0.1869 inches per minute. Effect of temperature was investigated by adapting the equipment to operate at both 71 ° and 185 °F. The data are reported in terms of angle of shearing resistance and initial resistance for varying rates of deformation, composition and temperature. While the main sets of results reported here were obtained at a bulk density range of 108.7- 109.5 lb. / cu. ft., some results were obtained at a bulk density range of 101-102 lb. / cu. ft. Analysis of varance tables have been drawn up from the results obtained from least squares correlations and significance tests applied. It was concluded that oil content and temperature were significant variables for the degree of shear strength developed by the oil sand; increase of oil content and decrease of temperature each cause an increase in shear strength. The bulk density range 108.7 to 109.5 lb./cu. ft. gave angles of shearing resistance from 30° to 40° and initial resistance values of 0.37 p.s.i. to 0.85 p.s.i. For the bulk density range 101 to 102 lb. / cu. ft., lower values of shear strength were obtained, indicating that compaction density was also of importance

Jan 1, 1960

By A. N. May

"This paper describes the present approach of the Mines Branch to the problem of measuring the stress condition in the interior of rocks surrounding underground openings. An instrument, which will be referred to as a stressmeter, has been developed at the Mines Branch to measure un-directional stress changes in absolute units. There are two modes of operation of this stressmeter. It can be regarded as a fixed instrument, in which case it is installed at the end of a diamond drill hole and left in position to record any subsequent stress changes taking place. Alternatively, three of the stressmeters can be used in conjunction with a trepanning opera-tion to allow the existing stress condition to be determined. The initial laboratory work and subsequent experiences in the field with the stressmeter are described. All the field development work on the stressmeter was made possible through the co-operation of Canadian Refractories Limited, Kilmar, Quebec."

Jan 1, 1960

By R. W. Coburn

The results of field experiments on wells which required stimulation indicated that engineered well-completions will cause an increase in ultimate recovery at reduced costs. Techniques and tools have been developed which can be used to establish well conditions most conducive to successful stimulation. Cementing, perforating and treating are bound together so completely that the success of one phase is completely dependent on the .effectiveness of the preceding phase. A method of determining the efficiency or effectiveness of any given well-stimulation treatment has been derived. Pressure behaviour during a treatment can be analyzed to yield the total percentage of the formation which has been treated.

Jan 1, 1960

Volumetric measures [ ]

Jan 1, 1960

By J. Croeni

The search for new alloys for application in the atomic energy field had prompted investigation of zirconium-rare earth metal alloys by the Federal Bureau of Mines. In this instance the zirconium-dysprosium system was investigated by melting point, thermal analysis, resistivity, X-ray and metallographic methods. Results indicate a single eutectic system with a peritectoid reaction occurring at 890° C. The eutectic isotherm extends from 30 to 95-percent dysprosium at 1,280° C. Eutectic composition is located at approximately 70 percent dysprosium. Solid solubility of dysprosium in both alpha and beta zirconium is extensive. The extent of solid solubility of zirconium in dysprosium has not been determined. Although zirconium rich alloys exhibit a significant increase in hardness, they can be cold worked extensively. These alloys also appear adaptable to solution heat treatment. Additional investigations concerning corrosion resistance and other mechanical properties are necessary for satisfactory evaluation of these alloys. The superior corrosion resistance of zirconium and the nuclear cross-section characteristics of the rare earth metals have stimulated alloy investigations using zirconium as a base metal. Alloys combining these characteristics present a possible substitute for hafnium as a control rod material. In this particular study dysprosium was chosen as the alloying element, and several series of alloys were used to establish the equilibrium diagram.

Jan 1, 1960

By A. Bartkowiak

The lower flammability limit of methane at 0 p.s.i.g. and ambient temperatures is 5.6 volume percent in chlorine, 5.2 in oxygen, and 5.0 in air. The corresponding upper limit values are 70, 60.5, and 15 volume percent, respectively, so that the range of flammable mixtures is greater in chlorine than in oxygen or air. The lower flammability limit of ethane at 0 p.s.i.g. and ambient temperatures is 6.1 volume percent in chlorine, 3.0 in oxygen, and 2.9 in air. The corresponding upper limits are 58, 66, and 12.5 volume percent, respectively. In this instance the range of flammable mixtures is greater in oxygen than in chlorine or air. Generally, the limits of flammability for both methane-chlorine mixtures and ethane-chlorine mixtures widen with increases in temperature and pressure.

Jan 1, 1960

By John B. Riddell

"AN EXCELLENT review of the status of applied geochemistry was given by Warren (1959) at last year's General Meeting of the C.I.M. The purpose of this paper is to present recent developments and trends. Several important books were announced during 1958: Ginzburg, I. I. Principles of geo-chemical prospecting. (In process of translation from the Russian by V. Sokoloff).Vinogradov, A. P. The geochemistry of rare and zvidely scattered chemical elements in soils. Consultants Bureau, N.Y. Korzhinskii, D. S. Physicochemical basis of the analysis of the paragenesis of minerals. Consultants Bureau, N.Y.In addition to these translations Mason's Geochemistry' has been revised, and Hawkes and Webb (personal communication) are publishing a book on geochemical exploration. A Symposium on Geochemistry was head in Paris in July, 1957, in conjunction with the XVIth International Congress of Pure and Al-lied Geochemistry. The abstracts of the papers presented at this Symposium were published in Geochimica et Cosmocl1imica Acta, 1958, Vol. 14, pp. 150-167."

Jan 1, 1960

By H. K. Birnbaum

The effect of 1ow-temperature stabilization anneals on the structure of the 0 phase Au-Cd alloys and on the diffusionless transformations observed in these alloys was examined by X-yay diffraction techniques. A phase separation in the ß-phase region was proposed to account for the experimenta1 results. The effects of quenching from elevated temperatures on the transformation behavior of these alloys were shown to be consistent with the proposed mechanism. IT has been shown that the high-temperature ß phase (CsCl structure) of the Au-Cd alloy system transforms to a phase having an orthorhombic (D2) ß&apos; structurel1-3 for compositions near 47.5 at. pct Cd and a tetragonal (4/m, m, m) ß" structure* in the vicinity of 50.0 at. pct Cd. Both transformations are diffusionless, crystallographically reversible, and occur on cooling at about 60° and 30°C respectively. The temperature interval from the beginning to the end of the transformation is of the order of 5°C in each case. Although the transformations are normally athermal, some of them have been reported to occur isothermally.= wechsler6,7 has shown that the effects of quenching a 49.0 at. pct Cd alloy from elevated temperatures are consistent with the retention of a nonequilibrium number of lattice vacancies. Annealing of these quench effects results in a broadening of the X-ray reflections.8 After a suitable quench, the 47.5 at. pct Cd alloy transforms to a phase having not the p&apos; orthorhombic structure but another structure which has properties similar to that of the ß" tetragonal structure.5.9 This change in the type of transformation has also been obtained after long anneals in the ß-phase region at about 70oC10 The present investigation was primarily concerned with the structural changes accompanying the above transformation phenomena. The change in transformation product and accompanying physical changes during an anneal in the ß phase have been termed stabilization effects. Experimental Procedure —The results reported in this investigation were obtained with the use of a Norelco diffractometer fitted with a temperature-controlled cryostat. The specimen temperature was controlled to better than ± 0.l°C during the measurements. CrKa radiation monochromated electronically with the use of a scintillation counter and pulse height analyzer was utilized. Specimens containing 47.5 and 50.0 at. pct Cd were prepared by sintering filings obtained from homogenized ingots of the proper alloy composition. (Gold of 99.999 pct purity and cadmium of 99.98 pct purity were used). All heat treatments were carried out with the specimens capsulated in vacuum ( < 10 % mm Hg) or in a He-H gas mixture. The quenching technique used in these experiments was to drop the pyrex capsule which contained the specimen from the annealing furnace into water, the temperature of which was controlled. The pyrex capsule shattered on contacting the water resulting in a relatively rapid quench. After the heat treatment, the specimens were mounted in the diffractometer and were left undisturbed in the diffractometer specimen holder during each sequence of measurements. EXPERIMENTAL RESULTS A) Low-Temperature Annealing—The transformations which were considered "normal" for these alloys were those obtained athermally during furnace cooling at approximately 50°C per hr after an elevated temperature anneal. Under these experimental conditions, the specimens were observed to transform to phases having structures whose diffraction patterns could be indexed as the ß&apos; orthorhombic structure for the 47.5 at. pct Cd and as the 0" tetragonal structure for the 50.0 at. pct Cd alloys. The transformation temperatures on cooling were approximately 60" and 30°C, respectively. Under the "normal" conditions both transformations were observed to go to completion, i.e., the entire volume of the ß phase was transformed to the product phase. In some specimens an extremely weak ß 110 reflection was observed at 20°C indicating that a small amount of retained ß was present. The effect of low-temperature annealing on the nature of the diffusionless transformations was examined for the 47.5 and 50.0 at, pct Cd alloy. The specimens were annealed in evacuated capsules at temperatures in the vicinity of 600°C (as specified in Table I) for 24 hr and were then cooled to 100°C at a rate of 50°C per hr. The specimens were then removed from the capsules and mounted in the diffractometer without allowing the specimen temperature to drop below 80°C. Annealing at the low temperatures was accomplished in the diffractometer by means of the cryostat which was mounted around the specimen. During the low-temperature anneals the lattice parameter, integral breadth of the reflections, and ratios of the integrated intensities of the fundamental and super lattice reflections for the 0 cubic phase were periodically determined. After annealing for the required time, the specimens were slowly cooled in the diffractometer and the diffraction patterns were recorded as a function of temperature. The specimens were cooled until the phase transformations were completed, following which the specimens were heated and diffraction

Jan 1, 1960

By M. Smutz, C. J. Baroch, E. H. Olson

IN 1949 an orebody containing some 10 billion lb of recoverable rare earth metals was discovered in the Mountain Pass district of San Bernardino County, California.&apos; The following year Molybdenum Corp. of America purchased a number of claims at the deposit and a mill on the property which had been constructed to process the district&apos;s gold ores. Average composition of ore from the San Bernardino deposit is less than 0.1 pct Tho2, 25 to 35 pct calcite, 10 pct rare earth oxides, 15 to 20 pct silica, and 30 to 40 pct barite.&apos; Rare earth content of the ore analyzes 50.7 pct CeO2, 4.2 pct Pr6O11, 11.7 pct Nd2O3;, 1.3 pct Sm2O3,, and 34.3 pct La2O3 and others.&apos; By floating the barite and depressing the bastna-site, Molybdenum Corp. of America produced a concentrate that contained 60 to 70 pct rare earth oxides. More than 25 pct of the rare earths, however, was lost in flotation. It seemed likely that a more economical method could be found. At the present time most of the rare earths in the concentrates are converted to rare earth chlorides, which are either fed to ion exchange columns for separation of the individual rare earths or reduced to misch metal. Current investigation shows that solvent extraction may achieve this separation more economically than ion exchange. The study reported here was undertaken to develop an economical method of preparing a pure rare earth nitrate mixture from California bastnasite ore. Results indicated that more than 98 pct of the rare earths could be recovered. Several possibilities were considered for processing bastnasite ore, but only the method outlined in Fig. 1 was investigated. This involved leaching the calcined ore with nitric acid. The nitric acid process is discussed under the following headings: 1) calcination of the ore, 2) leaching of calcine, 3) filtration studies, 4) solvent extraction, and 5) nitric acid recovery. Calcination: Since California bastnasite ore contains 25 to 35 pct calcite and about 10 pct bastnasite, calcination was needed to reduce the violence of reaction with nitric acid. Weight losses of 26 to 30 pct were obtained by calcining the ore at 900°C for I hr or at 800°C for 4 hr. Longer periods resulted in no further weight loss. Leaching the Calcine: When the bastnasite calcine was leached with 30 pct nitric acid for 8 to 10 days, rare earth recoveries of only 45 to 50 pct were

Jan 1, 1960

By J. P. McGee

As part of a joint U.S. Atomic Energy Commission-Federal Bureau of Mines program for using nuclear energy to supply process heat, a simulated nuclear loop has been constructed to test components. This loop has been operated for more than 1,800 hours at 100 p.s.i.g. Of this period, 23 hours were at 2,500° F. and higher; 540 at 2,000° to 2,500° F.; 840 at 1,500° to 2,000° F.; 200 at 1,000° to 1,500° F.; and 260 below 1,000° F. Leakage at flanges and welds was not a serious problem. A helium-recycle system with gas temperatures of 2,300° to 2,500° F. and a static pressure of 250 p.s.i.g. appears feasible. Difficulties were encountered with the recycle compressor due to thermal distortion of the impeller and shaft. The use of sealed bearings limits compressor operation to the life of the bearings.

Jan 1, 1960

By R. Didchenko

THERE are many methods described in the older literature which claim to produce anhydrous rare-earth chlorides in general. and cerium chloiide in

Jan 1, 1960

By W. M. Nabors

As part of a program to promote conservation and efficient utilization of petroleum resources, Bureau of Mines engineers at the Morgantown (W. Va.) Petroleum Research Laboratory are studying secondary oil-recovery projects in the Appalachian region. The increasing demand for petroleum and its products and the increasing cost of exploratory drilling tend to emphasize the importance of improving the recovery of oil from known petroleum reserves. Published reports setting forth the pertinent facts of these operations may help others to profit by the experience. This report presents the results of a study of secondary-recovery methods used in West Virginia by the Piedmont Oil and Gas Co., the Ryan Oil Co., and Water floods , Inc., on their Roane County leases in the Walton and Clover Rush Run pools. The principal oil-producing horizon underlying the area studied is the Big Injun sand, at approximately 2,000 feet. The sand is often referred to as blanket sand because it underlies much of the State and is oil-productive in many localities. Most of the pools in the area were discovered during 1907 to 1910 and were similarly developed and operated.

Jan 1, 1960

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 Charles T. Baroch

RESEARCH strengthened the position of cesium as the preferred material (commonly but erroneously called "fuel") for ionic propulsion engines. Its use as an element of the plasma thermocouple for generating electricity also seemed more likely. Domestic Production.-No domestic ore of cesium and rubidium was produced. San Antonio Chemicals, Inc., San Antonio, Tex., and Maywood Chemical Works, Maywood, N.J., continued to produce cesium and rubidium compounds including carbonate, chromate, hydroxide, nitrate, sulfate, and all four halides. Rocky Mountain Research, Inc., Denver, Colo., began producing various cesium and rubidium salts. American Potash & Chemical Corp., Los Angeles, Calif., offered cesium and rubidium for sale.

Jan 1, 1960

By N. P. Titkov

This paper presents the results of laboratory and pilot plant investigations for the development of efficient methods of beneficiating hematite ores from the Krivoi Rog, Kursk Magnetic Anomoly, Olenogorsk, and other localities. The tests included gravity, magnetic (in a high intensity field), flota¬tion, and magnetizing roasting methods. It was possible to develop efficient beneficiation methods depending on the mineral composition of the ore and degree of dissemination of ore and gangue minerals. The paper shows the relationship between the iron silicate and quartz content of the ore and the technologic indices of the various beneficiation methods. Some of the conclusions based on these investigations and the technical and economic computations related to the cost of one ton of pig iron produced from concentrates obtained by the various beneficiation methods are: 1. If the hematite ore is not disseminated uniformly, it is expedient to use a combined gravity and flotation process. Ore particles up to 50 am. in size are beneficiated by gravity (heavy suspension, jigging, and others) and yield a lump concentrate. The middlings from this process are recrushed and floated; 2. Finely disseminated hematite ores, containing small quantities (less than 5 percent) of iron silicates, are most effectively beneficiated by flotation. Anionic (sulphate soap, tall oil emulsion with various foam depressors) as well as cationic collectors may be used. Depending on the mineral and chemical composition of the ore, it is possible to obtain concentrates containing up to 65 percent iron with an extraction up to 94 percent; 3. Finely disseminated, mixed hematite-magnetite ores may be beneficiated by flotation or a magnetic separation-flotation process; 4. Finely disseminated hematite ores, containing large quantities of iron silicates and earthy hematite ores are most efficiently beneficiated by the magnetizing roasting method. This method will yield concentrates containing up to 68 percent iron with extractions up to 90 percent. Although beneficiation by the magnetizing roasting process is costly, it will nonetheless, when employed on this type of ore, yield the least expensive pig iron.

Jan 1, 1960

By G. L. Coleman, D. S. Hutton, W. C. Leslie

The occurrence of twins in a iron, generated during cooling through the ?-a transformation, is well established,1-8 but this phenomenon has been nearly ignored during the past 20 years. It is the purpose of this note to call attention to the prevalence of such twins and to illustrate their appearance. The work of paxton7 and Kelly8 has demonstrated beyond reasonable doubt that for Neumann bands (mechanical twins) in a iron the twinning plane is (112) and the twinning direction <III>. The agreement with McKeehan&apos;s earlier work4 on transformation twins indicates that both types of twins in ferrite follow the same twinning law. There is little doubt of this conclusion, but it could be strengthened by a microbeam X-ray determination of the orientation relationship between a single ferrite grain and a transformation twin within that grain, as in the technique used by Kelly8 on Neumann bands. RESULTS AND DISCUSSION Transformation twins, identified by their appearance on a polished and etched section, were found in

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