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By B. K. Shibler

During a research program to develop improved methods for recovering elemental sulfur and useful sulfur compounds from secondary source materials, the technical literature was searched for pertinent articles on processing methods. This report summarizes results of the literature survey and describes the more important processes that have been used or suggested for recovering sulfur and sulfur compounds from all non-Frasch sources. The bibliography presented represents a survey of the available English language literature on the subject through 1958, with particular attention focused on the period 1950 through 1958. Engineering Index and Industrial Arts Index were the principal guides used in the survey of this period. Chemical Abstracts was used to a limited extent to identify a few key foreign articles and patents. The Sulfur Symposium (4)4 published in November 1950 by Industrial and Engineering Chemistry includes a broadly representative selection of the literature up to 1949. Therefore, this reference was used extensively to locate and list pertinent articles on processing methods reported in the period prior to 1950.

Jan 1, 1962

By Leonard P. Colvin

Like all successful American enterprises, the mining industry is constantly trying to increase production, lower costs and improve working conditions. Companies are, of course, intensely interested in new equipment to help them gain these important ends, and one recent development-the mechanical raise climber--contributes to all three goals. Properly used, it increases production, cuts costs and has a number of important safety aspects all of which are the subject of this article.

Jan 1, 1962

By John E. Wallace

A recent study by the New York Trap Rock Corporation has conclusively determined that the number of blasting complaints is directly related to the noise produced by the blast. In turn it has been known for some years that the noise produced by the blast is directly related to atmospheric structure of temperature, wind, and humidity in the vertical direction. Normally during daylight hours the temperature decreases with altitude at the rate of about five and one half degrees per thousand feet on a sunny day, and to somewhat lesser amounts on cloudy days. Consequently, sound travels slower with altitude because of the lower temperature, and the sound rays tend to bend skyward, and are soon dispersed in the atmosphere. Quite frequently, however, the temperature increases with altitude, and just the opposite effect is attained. That is sound rays are bent downward, and sometimes reach the ground with intensities approaching that at the source. When the temperature increases with altitude a temperature inversion is said to exist. Less frequently than these two atmospheric conditions a condition is observed where temperature remains constant with altitude. This is called an isothermal atmospheric condition, and sound passing through this type of atmosphere tends to travel in straight lines, neither bending upward nor downward. The sound will be greater than normal near the blast, but will dissipate rapidly with distance from the blast site with no zone or zones of silence.

Jan 1, 1962

By Scott W. Hazen

This report describes the design, analysis, and results of a special experimental mine-sampling project conducted as part of the Bureau of Mines continuing program on sample-methods research. The experimental project was conducted at the Bureau?s Denver Mining Research Center and at the Climax molybdenum mine within the framework of a cooperative research agreement between the Bureau and Climax Molybdenum Co., Division of American Metals-Climax, Inc. The primary objective of the project was to investigate the interrelation-ship between sample volume, number of samples, the standard deviation of an assay distribution, and the precision required for an estimate of grade of ore, and to develop this interrelationship into a relatively simple method of application for use in mine sampling.

Jan 1, 1962

By F. J. Chernosky

In the past, a number of papers have been written on the use of various reagents as coal flotation frothers. For the most part, these papers have attempted to correlate the intrinsic chemical and physical properties of the reagents or reagent groups to the floatability of various fine coals. Because of the type or nature of evaluations made, chemically pure reagents were normally used. Generally, these reagents are unavailable in commercial quantities. Therefore, the results obtained with these reagents were usually limited in usefulness to the plant operator or metallurgist. This paper presents the results of a study in which commercially available forms of various reagents were used as flotation frothers. Flotation procedures which would conform in general to those employed in a large number of commercial coal flotation plants were utilized. The objective of the test was to compare these reagents on yield-selectivity-cost basis, that is, (1) the yields obtained, (2) the ash levels obtained, and (3) the reagent cost relating to these results.

Jan 1, 1962

By S. R. B. Cooke, Y. S. Kim, I. Iwasaki

lron oxides or the gangue minerals of iron ores can be made to float, depending upon the choice of collector. The selectivity of the separation is controlled by the accompanying chemical and operating conditions. In this report the findings on the general flotation characteristics of magnetite are summarized and the results are compared with those obtained for other iron oxides. Depending upon the choice of collector, either the iron oxides or the gangue minerals of iron ores can be made to float, the selectivity of the separation being controlled by the accompanying chemical and operating conditions. The mechanism by which a collector exerts preferential affinity for either group of minerals has been a subject of extended discussion. Previous investigations on the electrokinetic properties and flotation characteristics of hematite,' goethite,2 and quartz3 have demonstrated the electrical nature of the interaction of the collector with these oxide surfaces; anionic collectors are effective on positively charged surfaces and cationic collectors on negatively charged surfaces. Thus, from the differences in the electrokinetic properties of the above-named oxides, a theoretical basis has been provided for their separation by some typical collectors. Examination of the results reported for hematite and goethite shows that their electrokinetic properties and flotation characteristics are remarkably similar. It is of considerable interest, therefore, to examine similar information for magnetite, another common iron oxide, in order to consolidate the flotation characteristics of the three principal minerals of oxide iron ores. Such information is practically significant in the up-grading of both natural and artificial mag- netite produced from taconite, and in the treatment of partially oxidized magnetite ores. Information on maghemite and lepidocrocite, polymorphs of hematite, and goethite, respectively, is also of some theoretical interest in ascertaining the effects of crystal structure and of hydration in the iron oxide group. This article reports the findings on the general flotation characttxistics of magnetite, and compares the results with those obtained for other iron oxides. Experimentally, tlhe surface properties of magnetite were investigated by electrophoresis, and by measurement of the aclsorption of some typical flotation collectors. Its flotation behavior was tested by contact angle measurements and by simple flotation tests using a modified Hallimond tube. The basic information thus gathered was shown to be directly applicable to the interpretation of the results of batch flotation tests made on an artificial mixture of magnetite and quartz. EXPERIMENTAL MATERIALS Magnetite: Magnetite concentrate from Port Henry, N. Y., was further purified by fine crushing and magnetic separaiion, and was used throughout this investigation. For flotation tests the 150/200 mesh fraction was iso1ated and was cleaned by leaching briefly with warn 0.1 N HC1 followed by repeated washing with demineralized water. The final sample analyzed 71.71 pct Fe, 22.37 pct Fe" and 0.47 pct insoluble, and was stored in demineralized water. For e1ectrophoresis and adsorption measurements, the —400 mesh fraction of the magnetite concentrate was ground dry in a pebble mill. The surface area of the ground sample, as determined by the gas permeability method, was 70,000 sq cm per g. Since artificial magnetite has been reported to possess somewhat different physical properties than those of natural magnetite, it also was briefly examined. Preliminary flotation tests on a sample of artificial magnelite, prepared by reducing Brazilian hematite in a C0/CO2 mixture and analyzing 71.94 pct Fe and 23.78 pct Fe'', gave, however, nearly identical results with those using natural magnetite. It was concluded that artificial magnetite behaves similarly to natural magnetite. Samples which had been magnetically separated showed a tendency to cluster together due to residual

Jan 1, 1962

By R. E. Lindstrom

Effective separation of rare-earth mixtures is obtained using hydrogen as a retaining ion at 200° F with ethylenediaminetetraacetic acid (EDTA) eluant. Results obtained in Bureau of Mines bench-scale apparatus and large columns with hydrogen as a retaining ion closely parallel those obtained with copper as a retaining ion. The use of hydrogen as a retaining ion permits EDTA and water, collected before rare-earth breakthrough, to be recovered in a form that allows the material to be recycled without extensive processing. With the exception of yttrium and dysprosium, separation of rare-earth mixtures is improved and throughput is increased by elevated temperatures. Separation with 1,2-diaminocyclohexanetetraacetic acid (DCTA) eluant increases markedly on increasing temperature from ambient to 250° F; however, on the basis of separation efficiency, DCTA does not compare favorably with EDTA.

Jan 1, 1962

By J. M. Morkowitr

A. Sawatzky (Atomic Energy of Canada, Ltd.)—The detailed criticism by Markowitz of my simple treatment of the thermal diffusion of hydrogen in Zircaloy-2 indicates that my paper was not as lucidly written as it could have been. I would therefore like to reiterate several of the main points of my proposed mechanism and describe in more detail some of the features only implied in the original paper. The distribution equation derived in my paper was stated to hold only for the case where the volume taken up by the hydride was small compared to the volume taken up by the solid solution phase, subsequent work, mentioned below, having shown it to be out by only a few percent up to a hydrogen concentration of about 3000 ppm. Of course, hydrogen in the two-phase region alone is not conserved in my treatment as pointed out by Markowitz. On the contrary, one of the important features of my proposed mechanism is that in the presence of a temperature gradient a two-phase region cannot exist over the whole specimen. For example, if the specimen is entirely a + 6 initially, then on application of a temperature gradient, a single phase (a) region at the hot surface develops from time t = 0 onwards. As mentioned in my original paper, the interface between the a and a+d regions moves toward the colder surface of the specimen with a discontinuity in hydrogen concen- tration developing at the interface and increasing with time. This interface moves at such a rate that hydrogen in the specimen as a whole is conserved. It must be pointed out that my distribution equation (Eq. [5] in Markowitz's paper) holds only for linear geometry. It is easy to show that for the cylindrical geometry of Markowitz the assumptions used in my treatment lead to

Jan 1, 1962

By M. R. Geer

Information on the performance of coal-cleaning equipment is necessary to provide a basis for evaluating the performance of existing plants and projecting that of new plants. Performance data can contribute greatly to the wise selection and effective use of coal-washing equipment. The Bureau of Mines has published information on the performance of several commercial plants, as well as of some laboratory-scale equipment, 5 (2-9, 11, 12, 17-12, 21-25) from time to time for a number of years. A more intensive program to provide such information for all the principal types of cleaning equipment is underway. The present evaluation of table performance is part of this program.

Jan 1, 1962

By R. G. Ward, John Henderson. R. G. Hudson, G. Derge

Densities of melts of the iron oxide-silica system in contact with solid iron have been measured by the maximum hubble pressure method in the composition range O to 37 wt pct SiOz and the temperature range 1255 to 1410C. The constitution of the melts is discussed and it is postulated that the structure changes from a dislribution of iron ions in an oxygen ion network at pure "FeO" to a distribution. of iron ions in a network of silicate tetrahedra at the orthosilicate composition. JOHN HENDERSON, Junior Member AIME, was formerly with the Metals Research Loborotory, Carnegie Institute of Technology, Pittsburgh, Pa., on leave from Broken Hill Proprietary Co., Ltd., Research Division, Shortland, Australia. R. G. HUDSON, formerly with Metals Research Laboratory, is now with the John Jay Hopkins Loborotory for Pure and Applied Science, General Atomic Division, General Dynamics Corp., LaJolla, Calif. R. G. WARD, was formerly with the Department of Metal lurgical Engineering, Carnegie lnstitute of Technology, while on leave from the Department of Metallurgy, University of Sheffield, England. G. DERGE, Member AIME, is Jones and Laughlin Professor of Metallurgical Engineering, Carnegie lnstitute of Technology. Manuscript submitted January 19, 1961. ISD The system iron oxide-silica is an important one metallurgically because it forms the basis of several complex slag systems in use for industrial smelting and refining processes. In recent years considerable work has been done on liquids of this system but there are still many points of difference among workers using different experimental techniques and theoretical approaches. Phase equilibria/"3 activity,4-6 electrical conductivity,' current efficiency,' transference number,8 viscosity,9 surface tension,'' and density" measurements have all contributed to an understanding of the problem. Measurement of density is one procedure which is directly indicative of liquid structure since any deviation from ideality must be a result of structural interactions. Liquids of the iron oxide-silica system are of special interest because this is one of the few metal oxide-silica systems on which measurements can be carried out conveniently over the entire composition range from pure oxide to silica saturation. This includes the range of high basicity which has received relatively little attention in other systems. Although one investigation of density in this system has previously been undertaken," the results seem of sufficient importance to warrant the independent redeter-mination reported here.

Jan 1, 1962

By Heinz Petry

In deep strip mines the job of moving overburden may be so much bigger, and more costly than the removal of coal or ore that the operation is often called dirt mining. Constant improvement in stripping machines and techniques of using them is needed to offset rising costs and to increase production in mines that are now operating, and to make it economically possible to work deeper or thinner deposits.

Jan 1, 1962

By F. W. Mueller

It seems to be a matter of general understnading that title extraction or use of ground water may not be used as the basis of a depletion deduction under the United States Revenue Code And indeed, I have been unable to find any precedent upon which to base such a deduction. It is for this reason that the Shurbet case, which is the subject of my discussion and is now before the Court, may well become a precedent as authority for the allowance or disallowance of a depletion deduction for income purposes. It is well known that the law recognized that capital is consumed in the process of extracting minerals, oil and has, other natural deposits, and timber (underscoring supplied). This exhaustion, or depletion, is likened to the using up of raw materials in manufacturing. The law, therefore, provides a deduction for depletion which is intended as compensation for the exhaustion of assets consumed in the production of income through severance of minerals, oil and gas, other natural deposits, and timber.

Jan 1, 1962

By Henry B. Estabrooks

As was the case with many other mining companies, the management of Tennessee Copper Company' viewed with some interest reports in various trade and technical journals of the successful use of ammonium nitrate-fuel oil mixtures as an explosive in coal stripping., construction, open pit mining and finally in underground salt mines. The apparently simple transition from the "interested" stage to a point where in excess of 80% of the ex¬plosives used is ammonium nitrate may be of interest. The Tennessee Copper Company operates five mines in the "Copper Basin" of Polk County which lies on the extreme southeast corner of Tennessee. The ore is a massive sulfide principally pyrrhotite and pyrite with some tough lime silicates as gangue while the walls are greywacke interbedded with schist. Average total production is 28,000 tons per 5-day week and an average of 422 feet of development per week. Development work consists of 8'x 8?, 6?x 7?, 5'x 7? and 4'x 6? drifts driven with drifter drills using 1-5/8" carbide detachable bits and 5'x 5' raises driven with stopers using 1-5/8" bits.

Jan 1, 1962

By C. N. Garman

Homestake-New Mexico Partners operate a 750-tpd carbonate leach uranium concentrate mill near Grants, N.M. The highly mineralized water available as process water leaves much to be desired. The 628 ppm as CaCO 3 makes the use of raw water very troublesome in pipes and on filter cloths. However, the residual sodium carbonate in the final filter cake going to tails makes an ideal softening agent. To take advantage of this fact, all makeup water used in the mill is first used as tailing slurry dilution water and comes to the mill from the tailings pond. The 5-acre tailings pond serves as a thickener and 100 to 150 gpm of nearly clear solution is decanted to a pump to be returned to the mill. Since this tailings water has small quantities of uranium in the solution an ion exchange scavenger unit was installed to remove as much uranium as possible. The ion exchange raffinate is then used as final filter wash ahead of the tailings slurrying step. In spite of the large settling area this return water is not clean enough for ion exchange feed. The solids present are very fine and composed of approximately 15 pct (by weight) burnable carbonaceous material common to the sandstone uranium ores in the area, 40 pct SiOz plus 45 pct CaC03. Laboratory work showed that this material responds very well to flotation. Before deciding to use flotation, various clarifying systems such as pressure leaf filters, sand filters, and continuous vacuum pre-coat filters, were considered. Each of these could have solved the problem but with much more operating labor, more reagents and greater installation costs than the flotation step. About 100 to 150 gpm of fouled water is fed to two 66-in. Fagergren cells, in series. Reagents used at the beginning were Arquad 2HT75 and Arquad C50, at the rate of about 1% lb per 8-hr shift, or about 0.0053 lb each per ton of ore. This did not completely remove the solids but does an acceptable job. Approximately 75 pct of the slimes are a size that can be caught on a 41-Whatman Paper are removed. Removal of these slimes also allows much better settling of the coarse nonfloatable material. Advantage is also taken of this fact in a small settling tank ahead of precipitation. Removal of this amount of the slimes makes the ion t:xchange feasible. PREGNANT SOLUTION CIRCUIT The carbonate? leach-caustic precipitation method of uranium concertration does not provide for any process purification step ahead of precipitation. Therefore, any fine solids getting into the pregnant solution through the filter cloth show up in the final concentrate. This, of course, lowers the grade, and, at times, the slimy nature of these very fine solids rendered final filtration of the concentrate difficult if not impossible At Homestake-New Mexico Partners a 75-ft thickener was available for gravity clarification of 100 to 120 gpm of this pregnant solution. However this did not sufficiently remove the slimes. Laboratory investigation of the whole range of flocculants that were suggested by literature, salesmen, and friends failed to turn up anything of consequence. A continuous vacuum pre-coat filter would do the job and was investigated. The capital cost and the operating labor and materials made this a last chance choice. Following work done in the metallurgical laboratory on the tailings return water, it was found that some changes in the reagent strengths and combinations made a very definite decrease in the solids in the pregnant solution. Concentrate grade improved about 5 pct anti the final product after drying had an appreciably greater bulk density. Compared to a cost of about 2.2e per ton for pre-coat filter opelation for cleaning just one circuit, flotation costs less than 1.0 per ton of ore for cleaning two circuits. While a pre-coat filter would do a more thorough job, the flotation does all that is required for either circuit. Gravity causes the froth produced to run back into the leach circuit. This does not appear to result in a build-up of objectionable slime. No extra manpower is required; the operators in the separate areas can observe the operation of the cells and mix the small quantities of reagents as needed. Normally the 66-in. Fagergren cell requires 15 hp per cell, but this very dilute slurry needs only 10 hp for both cells. Originally, a combination of the two Arquads mentioned previously served as frothers and promoters. As further testing

Jan 1, 1962

By M. D. Banghart

The Republic of South Africa is an outstanding example of the benefits to a new land by the application of individual enterprise, capital and know-how. While South Africa was colonized by European and Bantu people some 300 years ago, it was only 70 to 80 years agog when diamonds were discovered at Kimberley and gold on the Witswatersrand, that the mining, industrial and commercial potential of the country began to emerge. South Africa s national income rose from R1, 200 million in 1945 to over R4 billion in 1960 (1R = 10 shillings = $1.40 U. S.) The annual national income per head of population -- including all races -- is currently R254 (£127) This compares with £24 for India., £30 for Nigeria, and £50 for Ghana. Allowing for the increase in population, the increase in real income per head of population was about 40% during the past 15 years.

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 Edward P. Larsen

At our annual meeting in St, Louis, Mo. in February 1961, we presented a comprehensive paper (No. 61-B-22) on the subject of "Blending and Handling of Materials for Agglomeration". In that paper you will find a discussion on the difference between "blending" and "mixing". With regard to "blending" we brought out the facts of its usefulness for the preparation o materials in an agglomerated mass to attain controlled chemical and physical uniformity. "Mixing" was discredited as not being useful for the attainment of uniformity of any kind.

Jan 1, 1962

By Nathaniel Arbiter

The question of automation of concentrator operations with computer control is under increasing consideration. Some of the problems involved will be discussed from the viewpoint of the availability of the requisite, detailed knowledge of the unit operations. The justification for full-scale automation of a mill must ultimately be economic--an increase in profitability over and above the cost of instrumentation and development, Potential savings would be in three probable directions: decrease in operating labor costs by substitution of machine control; improved metallurgy through continuous effective control; and decreased operating costs by achieving higher unit capacities and process efficiencies.

Jan 1, 1962

By C. J. Thompson

In the course of the work currently conducted by the Bureau of Mines in cooperation with the American Petroleum Institute Research Project 48 on identifying sulfur compounds in petroleum, a micromethod was developed (12)5 for catalytically removing the sulfur atom from sulfur compounds. The product is the residual portion of the molecule; the structure otherwise was unaltered except for hydrogenation of any unsaturated bonds that were present in the original compound. Positive identification of sulfur compounds isolated from crude oils is a difficult problem. Direct comparison of properties of the unknown with those of reference compounds is often impossible because of the limited number of reference sulfur compounds available. However, a relatively large number of pure hydrocarbons is available, and the conversion of the sulfur compound to a hydrocarbon enhances the possibility of identification. The technique also can be used to prepare microquantities of scarce hydrocarbons by hydrogenating compounds that are readily available.

Jan 1, 1962

By E. H. Rennhack

Phase equilibria of the zinc-rich portion of the Zn-Fe-A1 system containing up to 20.0 wt pct Fe and Al have been investigated at 600°C (1112°F), 450°C (842°F), and room temperature by metallographic and X-ray diffraction techniques. The phase relationships were found to involve only those phases present in the three binary systems. THE presence of small quantities of aluminum (approx. 0.2 wt pct*) in zinc galvanizing baths is known to suppress the formation of Zn-Fe alloy layers within the coating.' As part of an extended investigation of this suppression effect and the alloy reactions involved, the zinc-rich corner of the Zn-Fe-A1 equilibrium system containing up to 20.0 pct Fe and Al was determined at 600°C (1112°F), 450° F (842° F), and room temperature. The present paper reports the findings of this study. The constitution of the Zn-Fe system has been reported by Raynor2 based mainly on the work of Schramm3-3 and Truesdale et a1.6 The solid solubility of iron in zinc is extremely small and lies between 0.0009 and 0.0028 pct in the range 150° to 400°C (302°to752°F). Within the temperature and composition range of interest, a eutectic reaction involving nearly pure zinc, liquid = Zn+FeZn13, is observed at about 419°C (786° F) and 0.018 pct Fe along with a peritectic reaction, FeZn7+ liquid e FeZn13, at 530°C (986° F) and 6.2 pct Fe. The latter reaction is sluggish due to the large proportipn of solid phase involved in the transformation. Halla et al.,7 identified the compound FeZn13 as monoclinic with a = 13.68, b = 7.63, c = 5.07, and B = 128°44'. The structure of FeZn7 was reported by Bablik, et al.,8 to be of hexagonal symmetry, belonging to either the C6v = C6/m mc or D46h = C6/mc space group. Divensions of the unit cell are a = 12.81A and c = 57.6a. The Zn-A1 diagram as composed by Raynor9 and later Gebhardt10 is characterized by a eutectic decomposition, liquid 382°C (720°F) and 95.0 pct Zn and a eutectoid decomposition, at 275° (527°F) and 78.0 pct Zn. The eutectoid reaction cannot be suppressed permanently by quenching. Above 275° (527° F), a and a' co-exist in a closed miscibility gap between 31.6 and 78.0 pct Zn. Both phases are fcc and have nearly the same lattice parameter. The maximum solubility of aluminum in zinc (B) is approximately 1.0 pct at the eutectic temperature. PROCEDURE Materials. The experimental alloys were prepared from both massive and powdered material. Cast alloys were composed from three zinc-base master alloys containing 8.0 pct Fe, 16.0 pct Fe, and 50.0 pct Al which were made from C.P. zinc, Armco iron, and

Jan 1, 1962