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By P. L. Weston

The Bureau of Mines used high-temperature reduction roasting, magnetic separation, acid-leaching, and autoclave precipitation processes to recover iron and manganese from brown Cuyana range ores of Minnesota. Wet magnetic separation concentrated over 90 percent of the iron in 3 of 4 ores as high grade products analyzing 74 to 85 percent iron, 2.5 to 6 percent manganese, and 3 to 10 percent SiO2. The nonmagnetic fractions were leached with dilute sulfuric acid extracting 83 to 93 percent of the contained manganese and small amounts of iron. The leach solutions contained Mn-to-Fe and Mn-to-SiO2 ratios favorable enough for possible consumption in metallurgical mane operations. Exceptionally pure Mn solutions were achieved by pressure precipitation of the remaining iron in an autoclave followed by lime precipitation of silica and alumina.

Jan 1, 1966

By Jean-Paul Drolet

"This paper charts, briefly, the :salient facts of international trade in minerals and their products and Canada's place in it. It also reviews inter-national agreements, economic groupings and national measures to channel and regulate production and trade in minerals. Canada's mineral industry now produces raw materials worth $3.7 billion per year, making this country a giant among mineral producers. Two-thirds of this production is exported, chiefly to the United States, accounting for about 30 per cent of Canada's merchandise exports and topping all other classes.However, several other nations are also pressing the development of their mineral resources and markets. The Soviet Bloc, China and principally Australia and Africa are becoming important suppliers of basic raw materials to some traditional markets of Canada in Europe and Japan.The outlook for Canadian mineral exports to the countries of the Common Market, Great Britain and Japan is good, although some tariff barriers remain troublesome.Concerning the United States, our most important market, Canada is seeking to have that country lift import quotas on lead and zinc, and re-cent statements by U.S. authorities give hope that this may be achieved soon. Moreover, Canada wishes to obtain easier access to the American market for several of its metals and minerals.Canada is now participating in the Kennedy Round of tariff talks under the auspices of the General Agreement on Tariffs and Trade (GATT), and is seeking to open wider doors for its exports of products.In summary, Canada has done reasonably well in some mineral commodities on world markets, but has lost ground in others. Any slackening of Canada's efforts in the development and marketing of mineral resources would soon lead to the decline of its role in the world miueral economy."

Jan 1, 1966

By D. M. Waldorf

Steam permeability measurements have been made in the laboratory on several samples of natural reservoir materials. The steam temperatures and pressures were selected to simulate conditions which might exist in a reservoir during the injection of steam. For each sample tested, the experimental permeability to superheated steam was comparable to that measured with air and no evidence of plugging was detected. Some samples were exposed to water at various temperatures and plugging was found to occur in materials which contained significant quantities of monmorillonite clay. Temperature had little effect on the degree of plug-ning between 75 and 325 F. The measured pemeabilities tended to increase slightly with temperature, but the changes were small compared with the initial loss of per~neability on wetting. Sequential pemzeability measurements were made on two samples using air, water, steam, water and air, in that order. Both samples were water-sensitive and plugged extensively after the initial injection of water. Upon exposure to superheated steatm the samples dehydrated and their permenbilities to superheated steam were comparable to those initially measured with air. The remaining measuretnetzts with water and air confirmed that the water plugging was reversible and that the samples were not seriorrsly damaged during the tests. INTRODUCTION The swelling of water-sensitive clays during water floods has long been recognized as a potential source of reservoir damage. The recent extensive application of steam injection and stimulation has compounded this problem since both hot water and steam (as well as fresh water at reservoir temperatures) are, at sume time, in contact with the producing zone adjacent to the bore of a steam injection well. The purpose of this paper is to present data which compare the sensitivity of some natural sedimentary rock samples to water at various temperatures, and to super-heated steam. Some properties of montmorillonite clay are briefly reviewed, and comparisons are drawn between empirical data and the predicted behavior of the montmorillonite known to be present in the samples. PROPERTIES OF MONTMORILLONIT E CLAY Water initially adsorbs on dry N a -montmorillonite clay in discrete layers in the interlaminar space between clal platelets. The platelet spacing, which is 9.6 A (angstroms) for a dehydrated clay, has been observed to expand in discrete steps to 12.4, 15.5, 18.4 and 21.4 A spacings, indicating the formation of four discrete layers of regularly oriented water molecules.' The first two layers are easily formed by hydrating a dry sample to equilibrium in an atmosphere with carefully controlled humidity. The formation of the higher layers is more difficult. The usual X-ray diffraction patterns of the more highly hydrated samples indicate a gradual increase in the average spacing betwcen 15.5 and 19.2 A, followed by a discontinuous expansion to 31 A when the weight ratio of water to dry clay is between 0.5 and 1.2.' Platelet expansion above 31 A proceeds monotonically as the moisture is increased and no regular arrangement of the platelets ib observed. Water-sensitivity in sedimentary rocks is usually associated with Na-montmorillonite clay when it is in the noncrystal-line state. Mering3 found that the average lattice spacing of sodium montmorillonite hydrated at 68 F and 70 per cent relative humidity was 15.5 A, and that the spacing, at 92 per cent humidity was 16.5 A. The water adsorbed at the higher humidity has the same free energy as liquid water at 65.6 F. Kolaian and Low' used a tensiometer to measure the thermodynamic properties of water in diffuse suspensions of montmorillonite clays relative to pure water. They observed that water in suspensions as dilute as 6 per cent clay became partially oriented when left undisturbed. The bonding associated with this orientation was not extensive because the free energy difference between the water in suspension and pure water was only a few millicalories per mole. They also found that the measured free energy difference decreased rapidly with temperature and became negligible above 100 F. This evidence indicates that montmorillonites contained in sedimentary rocks would dehydrate to a crystalline structure when exposed to superheated steam, and that the rock permeability measured with steam would be equivalent to that measured with air. The effect of elevated temperatures on the swelline of montmorillonite clays in aqueous suspensions has not been investigated. The Gouy-Chapman diffuse-ion-layer theory has been used to predict the swelling pressure of clay suspensions in dilute salt solutions at room temperature with reasonable success. theory also correctly predicts the direction of the thermal response of Na-mont-morillonite swelling pressures in dilute salt suspensions, 9 Over the temperature range of 33 to 68 F, an increase in

Jan 1, 1966

By V. E. Homme

Low- and high-temperature reduction techniques were employed by the Bureau of Mines in study of conditions favorable to the formation of massive titanium crystals. '1,1,2 low-temperature method, feeding molten sodium to solidified titanium lower chloride-sodium chloride, produced higher quality and high quantity crystalline metal. The percentage of crystalline titanium was increased with increasing reactor diameter, melt depth, and titanium dichloride concentration. The high-temperature technique, feed molten sodium to melts above 8000 C, producing needle-type crystals of lower quality and with less consistent results than the low-temperature method. Layers of titanium foil, sponge, fine needles, wool, and crusts of sin-tered granules were formed during the earl, -art of the low-temperature reduction, and massive crystals were produced beneath this barrier in the latter part of the reduction. Crystalline titanium having an average hardness of Bhn 76 and representing 58 percent of the total titanium was obtained. Lamellar crystals up to 1 1/2 inches long with a hardness as low as Bhn 54 were also produced. A second-stage reduction for reclaiming titanium from offgrade sponge is described. Titanium produced by this method was comparable in quality to that from sodium reduction of titanium tetrachloride.

Jan 1, 1966

By J. M. Belland

This paper deals with the geology of the Smallwood mine in relation to its influence on mining and milling operations. Structure within the orebody, and variations in ore grade and material types, will be described and associated with the various drilling, blasting and milling operations. The orientation of planes of weakness, either bedding or jointing planes, and contacts between extremes in material types influence the size of the broken material. Generally speaking, variations in grinding rates and recovery can be associated with stratigraphic sequence and metamorphism.

Jan 1, 1966

By Heinz C. Dittmar

The phenomenon of radioactivity has been known since the turn of the last century. Scientists of many nations, intrigued by the strange effects of radioactivity, have engaged in research to probe the heretofore presumed, but largely unknown world of atomic structures and subatomic- particles. A theory evolved of splitting the atom, thus providing insight into the structure of matter and opening the way to possibly create new materials. Many years of effort culminated in the first chain reaction in 1942. The beginning of the atomic age was drastically demonstrated by the flash of the large scale chain reaction of the first atom bomb. It was actual proof of the incredible energies contained in matter.

Jan 1, 1966

By R. L. Hopkins

The work described was performed to determine whether sulfur compounds of the thienothiophene class occur in crude oil. The presence or absence of various classes of sulfur compounds in crude oils is of interest and value to petroleum science. The Bureau of Mines, for the first time, identified hydro-carbon products of desulfurization that point directly to the identity of two individual thienothiophenes, namely 3-methylthieno[2,3-b]thiophene and 2-meth-ylthieno[3,2-b]thiophene, in Wasson, Texas, crude oil. These identifications, described in detail, were accomplished using microdesulfurization, mass spectrometry, and gas-liquid chromatography.

Jan 1, 1966

By C. L. Emery

The geology and early history of the discovery of potash in Saskatchewan as described by Heber Cole (1) and R. V. Thompkins (2) has dealt with the distribution of the salt beds and their potash content. From the many bore holes through the Prairie Evaporites the outlines and contours of the series have been well established. The thickest section of the salt beds lies to the north of the "barren" area and forms a belt running easterly to a point west of Yorkton. The "barren" area is a region where the salt has been redissolved and the strata have slumped down, to fill the voids. This area is of interest from the standpoint of rock mechanics. The potash-rich beds extend both east and west of the region. mentioned and the top of the Prairie Evaporite is at a depth below 3200 feet from the surface near Saskatoon and dips southerly at an average rate of about five feet to ten feet per mile.

Jan 1, 1966

By L. A. Wasselle

The Israel Mining Industries Institute for Research and Development has developed, during recent years, a number of new processes for fertilizer materials. Their phosphoric acid processes, however, are capable of producing an acid of far higher quality than that normally associated with fertilizer grade acid. This paper will discuss two of these processes showing the quality attainable and the capital and operating costs for, U. S. conditions. The Standard IMI Process is based on the acidulation of phosphate rock with hydrochloric acid and involves solvent extraction for the separation of high quality, phosphoric acid from the resulting solution. The IMI Purification Process applies the same solvent extraction technique to the purification of a wet process phosphoric acid from sulfuric acidulated rock. IMI has built and operated a semi-works scale demonstration plant for the standard process. The first commercial plant was started up in; Japan in 1962. This small seven metric ton per day plant is currently producing a furnace quality acid. A larger 50 metric ton per day plant is nearing completion in Brazil. Another 50 metric ton per day plant is under design while a large plant with a capacity in excess of 150 metric ton per day is in the planning stage. Both of the latter facilities are for Israel.

Jan 1, 1966

"THE Canadian Advisory Committee on Coal Research, which is commonly known as CACCR, has been in existence for the past five years and has held annual meetings during that period. This Committee is comprised of representatives from: the Mines Branch, Fuels and Mining Practice Division, Ottawa; the Geological Survey of Canada; the Dominion Coal Board; and the Provincial Research Councils and Foundations. It embraces all coal research in Canada that is sponsored, for the most part, by Government funds.To bring the country's coal research activities to the notice of the Canadian coal industry, the Coal Research Committee of the Coal Division, C.I.M., passed a resolution at the 1964 business meeting in favour of recommending the publication of an annual research report prepared by the CACCR. The first such report was published in the September, 1964, issue of the C.I.M. Bulletin; the second appeared in the November, 1965, issue of the same publication."

Jan 1, 1966

By Paul L. Bearden

The accumulation, handling, and utilization of sludges formed from wet process phosphoric acid is one of the major problems in the industry. The purpose of this paper is to explain some of the considerations and techniques that can be employed to provide some measure of control over the problem. An acid made from a Central Florida phosphate rock is used to illustrate the effects of one process design approach used to provide one type of control. Other approaches or techniques are discussed on a general basis. In every case, the discussion is purposely limited to conventional dihydrate processing in which phosphoric acid is produced from the filter at a strength of approximately 30% P205 and is subsequently concentrated to higher strengths such as 44 and 54% P205.

Jan 1, 1966

By A. Mykytiuk, I. E. Puddington, W. D. Macleod, F. W. Meadus

"A laboratory-scale continuous procedure for the up-grading of naturally occurring tin ores, based on the principle of spherical agglomeration, is described. High recoveries are indicated. A proposed second stage suggests useful fractionation steps.IntroductionA LABORATORY-SCALE batch process for the upgrading of a tin ore using the principles of spherical agglomeration has already been described (1). This procedure consisted of milling, for about an hour, a precrushed ore with at least 200 per cent water, 0.2 per cent of a reagent such as tall oil (to render the de-sired ore particles hydrophobic) and about 3 per cent of a viscous petroleum oil. The feed material passed an 8-mesh Tyler sieve, and the percentages of re-agents are based on the dry weight of the feed. Du-ring the grinding, the hydrophobic particles transfer into the oil phase to produce coherent semi-solid bodies while the gangue stays preferentially in the aqueous phase. The concentrate can be separated from the gangue easily by a mechanical operation. Using an ore containing about 0.3 -0.5 per cent tin, grades of from 1.5 to 7.0 per cent were obtained by varying the pH of the system. Recoveries fell from about 80 per cent to as low as 50 per cent as the grade in-creased."

Jan 1, 1966

By Larmon J. Heath

The Bureau of Mines explored the use of air or natural gas for recovering additional oil from natural water-drive reservoirs with little or no original gas saturation. Engineering and production data for a field in the Mid-Continent area, results of limited laboratory experiments, and data shown in the literature were considered. Injecting air into a water-coned well could seriously damage the well. Injecting natural gas into the watered-out zone could improve the producing water-oil ratio. In the reservoir studied, oil recovery can be increased by injecting natural gas to decrease water-oil ratios. Laboratory tests on a core from the field show an increase in oil recovery of 7.6 percent of the original oil in place as a result of increasing the free gas saturation. This recovery could amount to as much as an additional 6 million barrels of oil from this field.

Jan 1, 1966

By E. K. Kleespies

The Bureau of Mines demonstrated a technique for electrowinning titanium from titanium nitride and titanium dioxide. Titanium-nickel-copper metal solutions containing 26 to 61 weight-percent titanium were prepared by electrolyzing titanium nitride in molten mixtures of potassium fluotitanate) and sodium chloride or barium chloride and depositing titanium on nickel-copper cathodes. A titanium-nickel alloy was prepared by electrolyzing titanium dioxide in an electrolyte of potassium fluotitanate) sodium fluoride) and calcium fluoride and depositing titanium on solid nickel cathodes. This alloy contained 21 weight-percent titanium and had a combined oxygen-carbon content of less than 0.1 weight-percent. A compartmented cell confined the oxide feed near the anode and inhibited oxygen contamination of the metal.

Jan 1, 1966

By Merwin H. Howes

In constructing the NORAD Combat Operations Center, controlled blasting techniques were employed to achieve smooth walls and to avoid shattering the rock beyond excavation lines. Extraordinary measures were taken to stabilize the rock to permanently preserve the openings. Rock stabilization was accomplished by means of reinforced concrete and gunite linings, rock boltings, installation of chain-link fabric, and epoxy resin and cement grouting. A particular zone of weakness at B vital location was supported by exceptionally thick reinforced concrete lining, rock bolts, and cement grout.

Jan 1, 1966

By B. J. Moore

This publication contains routine analyses and related source data for 528 natural gas samples from 21 States collected during calendar year 1965 as part of a continuous survey of the United States for occurrences of helium in natural gas. This survey has been conducted by the' Bureau of Mines since 1917. The analysis published herein were made by mass spectrometer and a special helium analysis apparatus, which are described in Bureau of Mines Bulletins 4863 and 576.4

Jan 1, 1966

The 1965 Lignite Symposium, the Louth in a series and the third sponsored by the University of North Dakota and the Bureau of Mines, was held at Bismarck, N. Dak., on April 29-30, 1963. These symposia provide a forum for those interested in the technology and utilization of solid fuels, especially lignitic coals. As part of the meeting, a 200-mile field trip was taken including; inspection of (1) the 200-megawatt, pulverized lignit-fired Leland Olds plant of Basin Electric Power Cooperative, under construction near Stanton, N. Dak.; (2) the site of the Glunharold mine of the Truax-Traer Coal Co., Division of Consolidation Coal Co., where a wheel excavator was being assembled; (3) the operating Beulah mine of Knife River Coal Mining Co., subsidiary of Montana-Dakota Utilities Co., near Beulah, N. Dak.; and (4) the 400-megawatt, hydroelectric Garrison Dam powerplant, near Garrison, N. Dak.

Jan 1, 1966

A symposium on pneumatic transportation of solids was held at Morgantown, W. Va., October 19-20, 196'), under the cosponsorship of the Institute ref Gas Technology. Chicago, Ill., and the Bureau of Mines. Objective of the symposium was to present information on developments and projected programs in the technology of feeding, transporting, recompressing, and utilizing gas-solids mixtures Dr. Henry R. Linden, Director, Institute of Gas Technology and Harry Perry, Director of Coal Research, Bureau of Mines, in the initial addresses at the symposium welcomed more than 140 representatives of industry, educational institutions, and government from 16 states, Canada, Great Britain, etc.

Jan 1, 1966

By C. M. Harrer

The location, features, qualities, and extent of iron occurrences and the associated resources--limestone and dolomite, bentonite, coal-lignite, petroleum and natural gas, power, and water--are evaluated. The results of pioneer beneficiation tests on South Dakota taconite are discussed. In addition, pertinent features of taconite development, cost factors, the Western and Central United States trade area and markets are reported. The State's production of iron ores until 1963 has been small and for purposes other than the manufacture of iron. This investigation disclosed the probability of large resources of taconite in Pennington and Lawrence Counties. The average iron content is 29 percent, and a 65-percent or better iron concentrate might be produced. Ample resources are available for mining and processing taconite. An investment of at least $26 million would be required for a plant capable of turning out 1 million tons of agglomerated iron concentrate per year. The feasibility of such an enterprise is indicated, but intensive investigation and research must be completed to justify such an investment.

Jan 1, 1966

By C. M. Harrer

The location, features, qualities, and extent of iron occurrences and the associated resources--limestone and dolomite, bentonite, coal-lignite, petroleum and natural gas, power, and water--are evaluated. The results of pioneer beneficiation tests on South Dakota taconite are discussed. In addition, pertinent features of taconite development, cost factors, the Western and Central United States trade area and markets are reported. The State's production of iron ores until 1963 has been small and for purposes other than the manufacture of iron. This investigation disclosed the probability of large resources of taconite in Pennington and Lawrence Counties. The average iron content is 29 percent, and a 65-percent or better iron concentrate might be produced. Ample resources are available for mining and processing taconite. An investment of at least $26 million would be required for a plant capable of turning out 1 million tons of agglomerated iron concentrate per year. The feasibility of such an enterprise is indicated, but intensive investigation and research must be completed to justify such an investment,

Jan 1, 1966