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By Martin H. Stanczyk

The direct dissolution of a typical zinc sulfide flotation concentrate by elevated temperature and pressure leaching was investigated. The concentrate assayed about 55 percent Zn, 32 percent S, 6 percent Fe, and 1 percent Pb and contained minor quantities of copper and precious metals. The influence of various factors on the dissolution of the zinc in acidic and ammoniacal pulps when using oxygen as the oxidant was determined. The tests revealed that the sphalerite was difficult to oxidize. Complete dissolution of the mineral required vigorous and intimate nixing of the gaseous, liquid, and sold phases. The addition of pyrite or sulfuric acid to water slurries of the concentrate was required to obtain a high zinc extraction when leaching under acidic conditions. The quantity of pyrite and acid used was about 0.125 and 0.25 pound, respectively, per pound of zinc sulfide contained in the leach charge. In tests with acid, about 96 percent of the zinc was extracted from the concentrate in 1 hour at 200° C. when the oxygen partial pressure was 75 pounds per square inch gage or higher. Leaching with a continuous flow of air as the oxidant gave results that were almost as good as those obtained when oxygen was used, In tests with air fed through the autoclave at 320 liters per hour, 95 percent of the zinc was dissolved in 1 hour, Acid leach solutions assaying approximately 58 grams Zn per liter and containing Fe, Ni, Cr, and Cu impurities were produced in the better tests. The leached residue consisted essentially of red iron oxide together with substantially all of the lead and precious metals.

Jan 1, 1961

By R. Greenwood

The advent of the space age and its promise of interplanetary flight has prompted new ideas for propulsion systems that will allow maximum energy with minimum fuel weight. The use of cesium as the source of energy for such rocket flights has been found desirable. Theoretical efficiency of a rocket fuel is measured in terms of specific impulse, defined as the number of pounds of thrust per pound of propellant consumed per second. Specific impulse is usually expressed in seconds (the number of seconds for which one pound of fuel would produce one pound of thrust) although it is really a measure of total energy, not of power. The most sophisticated chemical fuels have a specific impulse of 300 to 400 sec; liquid hydrogen heated by nuclear reactor has a specific impulse of 1000 to 1200 sec. Specific impulses as high as 20,000 sec, however, are theoretically attainable with the ion rocket, in which free cesium ions are accelerated across a voltage drop and ejected at high velocity.' Characteristics of the system have been sketched by Boden.2 The desirable properties of an ion propellant are: 1) low ionization potential, 2) low boiling point, and 3) high atomic weight. Alkali metals best fulfill these requirements, and Table I indicates the superiority of cesium. The use of heavy complex ions such as UCl3 is ruled out by their instability and other disadvantages.' Despite its enormous superiority in specific impulse, the ion rocket is inherently low-powered, capable of very small acceleration. Application of ion propulsion will be limited to large rockets and spaceships on missions requiring powered flight for weeks or months and employing a separate chemical propulsion system for escape from the earth's atmosphere where power requirements are large but of brief duration. For example, Kraemer and Larson3 considered the case of an unmanned 25,000-lb pay-load placed in a 300-mile orbit by chemical rockets, proceeding thence by ion propulsion to the vicinity of Mars, where it would go into orbit once again. Calculations provide for 8500 lb of cesium for such a voyage. The question of whether such quantities of cesium will be readily available to the space program does not appear to have been considered by geologists and mining engineers. Present Production and Uses Literature on industrial applications of cesium is scanty. The metal is used in scintillation counters, photocells, infra-red detection devices, and as a "getter" in low-voltage vacuum tubes. Production is sporadic and total figures are not published, but the annual consumption is measured in pounds rather than in tons. The few pollucite deposits known, small as they are, can easily supply the present limited demand for gram or pound lots of cesium. Until recently the price of cesium was $2 to $4 per gram, but according to Chemical Engineering, cesium salts are now available at $13 to $27.50 per lb. Geochemical Distribution As a large alkali ion, the cesium ion accompanies potassium in geological processes and tends to be concentrated in the latest crystallizing fractions of potassium minerals in much the same manner as rubidium. Most of the cesium in igneous rocks, therefore, is in the micas and potash feldspars of granites, and especially in granitic pegmatites. The cesium content rises markedly in the micas of the late by-drothermal replacement stage in complex pegmatite~.' Typically, cesium is only 0.5 to 0.01 times as abundant as rubidium in potassium minerals. Rb', with a radius of 1.47 A, is close enough in size to K' (1.33 A) so that rubidium forms no minerals of its own. Cs+ is so large (1.67 A) that only small concentrations can be taken up in potassium minerals; when cesium is present in solution in larger concentration it forms the mineral pollucite, Cs3-Na2A17Si17O48.3H2O, which is known only in pegmatites. In the weathering of igneous rocks, cesium is dissolved, carried to the ocean, and apparently in-

Jan 1, 1961

[NORTH AMERICA UNITED STATES ALABAMA AUBURN Sturm & O'Brien, Consult. Engrs. °Sturm, Rolland G. BESSEMER Granger, W. C. BIRMINGHAM Air Reduction Sales Crockett, John M. Amer. Cast Iron Pipe Co. Carter, Sam F., Jr. Donoho, C. K. Anderson Elec. Corp. Davis, Moss V. J. B. Clow & Sons Neptune, Maurice D. Connors Steel Div. °Sandelin, Robert W. Hayes Aircraft Corp. Ricketts, W. E., Jr. Willhelm, A. Clyde, Jr. McWaine Cast Iron King, O. H. Worthington, B. W. Shook & Fletcher Sup. Co. Gearhart, Thomas A. Southern Res. Inst. Dismukes, Edward B., Wheelahan, Edmund J. Thomas Foys Miller, Ralph M. Union Carbide Metals, Co. Brandler, Edgar A. U. S. Pipe & Fdry. Co. Clay, Donald H. Unaffiliated Berg, H. A. Caldwell, H. A. Gilmer, H. U. Harris, Thomas H. Templeton, J. B.]

Jan 1, 1961

By A. D. Hahn

This report describes reconnaissance by the Federal Bureau of Mines of titanium-bearing sandstone in Kemper County, Miss. The purpose was to determine the ilmenite, rutile, and associated heavy-mineral content of black-sand-bearing Eocene deltaic formations" The investigation was part of a survey of titanium resources of the United States. Ilmenite (FeTi03), an iron-titanium oxide, is the major titanium-bearing mineral consumed in the titanium pigment industry. Rutile (Ti02), titanium oxide, is used mainly in producing welding-rod coatings and titanium metal. The fieldwork was conducted during the first half of November 1959. Seven holes, totaling 304 feet of bore, from which 64 samples of cuttings were taken, were drilled in the north-central part of the county; and two holes, totaling 172 feet of bore, from which 34 samples of cuttings were taken, were drilled in the southeastern part.

Jan 1, 1961

By A. Gene Collins

Rapid, sensitive, and precise methods of determing major, minor and trace constituents of oilfield brines are needed. Several methods have been developed or adapted by the Federal Bureau of Mines at the Petroleum Research Center, Bartlesville, Okla. The following methods are described in this report: Spectrophotometric and volumetric for iodides and bromides; potentiometric for pH, alkalinity, acidity, borate boron, total boron, and organic boron; gravimetric for potassium; disodium ethylenediaminetetraacetate (EDTA) volumetric for total hardness, calcium, and magnesium; spectrophotometric for fluorides; and color comparison .for arsenic. Adequate sensitivity, precision, and accuracy were obtained for each method. The Bureau of Mines pioneered in research on the analysis of oilfield waters (2, 46, 47).6 However, several of these early procedures were quite time consuming. Also, they did not include methods for determining trace and minor constituents of brines.

Jan 1, 1961

By K. E. Tame

A resume of the history and state of the art of physical beneficiation of uranium ores is presented along with a detailed description of research on concentration of uranium ores by attrition grinding. The information on flotation, gravity concentration, electronic sorting, and selective grinding was gathered to complement the study of attrition grinding methods. Both dry and wet grinding procedures were investigated as potential methods of upgrading a variety of ore types, ranging in grade from 0.02 to 0.42 percent U308. A Mardun4 disintegrator that employs high-speed rotating paddles in a cylindrical shell lined with interrupter bars was used in most of the dry grinding studies. Attrition scrubbing devices, which impart a violent mixing or attritioning action to ore pulps, and cylindrical mills, employing rods or punchings as grinding media, were used in the wet grinding tests.

Jan 1, 1961

By Dorothy M. Richardson

The Bureau of Mines has participated in the American Petroleum Institute Research Project 48A (API-RP48A) program on the Separation and Identification of Sulfur Compounds in Crude Petroleum. The lack of reference compounds or infrared spectral data has made difficult the identification of individual sulfur compounds boiling above 140° C. The recent acquisition of 24 alkylthiophnnes has made possible a limited study of this important class of sulfur compounds. The infrared spectra of 2-monoalkylthiophenes and 2,5-dialkylthiophenes for the 2 to 15p range are reported. Correlations for determining the 2-alkyl and 2,5-dialkyl substituted thiophenes are derived from this information. The 2-alkylthiophenes show a unique pattern in the 5.50 to 6.54 region, while the 2,5-dialkylthiophenes show a distinctive pattern in the 5.6µ to 6.7µ region. A skeletal vibration occurs in the 9.5 to 10.0µ region for all of the thiophenes investigated. These data will aid the infrared spectroscopist in the identification of compounds of the type reported.

Jan 1, 1961

By J. J. Demeter

Experiments were conducted in 2- and 4-inch-diameter standpipes to evaluate the effectiveness of standpipes as pressure seals. During the experiments, these standpipes conveyed Alan-Wood magnetite (60 to 230 U.S. standard sieve mesh) by gravity flow from one vessel to another of relatively higher pressure. The information obtained has been helpful in a Federal Bureau of Mines investigation of how to make either synthesis gas or hydrogen by a modified steam-iron process employing a continuous recycling stream of granular iron-iron oxide at temperatures of 600° to 900° C. In this process the mixture of granular material flows by gravity from a reduction vessel at low pressures to an oxidation vessel at higher pressures. Data from the 2- and 4-inch-diameter standpipes indicate that it would be practical to use a standpipe as a pressure seal between the reductor and oxidizer. Investigators found that, by gravity flow, the standpipe could convey the Alan-Wood magnetite against pressure gradients up to 1.07 pounds per square inch per foot of column height.

Jan 1, 1961

The first session of the Rocky Mountain Coal Mining Institute was called to order by John T. Maulsby, Superintendent of Maintenance and Planning, Columbia-Geneva Steel Division, U. S. Steel Corporation, Dragerton, Utah, representing the past-president. W. K. Dennison, Jr., Superintendent. Koehler line. Kaiser Steel Corporation. Raton, New Mexico, who was unable to attend. Mr. Maulsby welcomed the members and guests, and introduced the President, A. Z. Dimitroff, Mining Electrical Engineer, Health and Safety, District 1-L, U. S. Bureau of Mines. Denver. Colorado. The text of President Dimitroff's address of welcome is as follows: The President's Remarks Guests and Members of the Rocky Mountain Coal Mining Institute: The distinct honor and privilege of officially welcoming you to this, the fifty-seventh regular meeting of the Institute, is indeed a pleasure. Your officers and committees have tried to provide a varied program which I am sure should have something of interest to all of us. The theme of this meeting, "Where Do We Go From here'?", appeared rather fitting for the In¬stitute this year because, as most of you know, until only two weeks ago we thought that this is the last time we will be able to meet at the Colorado Hotel, which has been the favorite spot of most members. Your officers and many of you were literally asking just that question.

Jan 1, 1961

By John E. Shelton

Flotation tests were conducted on two samples of copper-nickel-bearing ore from the Harriman area near Rockport, Maine. The samples were taken by Roland F. Beers, Inc., for tests in cooperation with the Federal Bureau of Mines. One sample, analyzing 0.38 percent copper and 0.71 percent nickel, was essentially a disseminated pyrrhotite in hypersthene. Pentlandite, chalcopyrite, pyrite, and millerite were intimately associated with the pyrrhotite. Locked series flotation tests on this sample showed that 87.4 and 73.4 percent of the copper and nickel, respectively, could be recovered in a bulk concentrate that analyzed 3.47 percent copper and 5.34 percent nickel. The copper-and nickel-bearing minerals were collected with sulfhydric collectors in an alkaline circuit. Cleaning the concentrate three times with the addition of pH regulators was sufficient to attain the previously stated grades. The second sample had analyses of 0.31 percent copper and 0.85 percent nickel; talc and hypersthene were the main gangue minerals. Bulk sulfide flotation, made while depressing the talc, resulted in a concentrate that analyzed 2.33 percent copper and 4.70 percent nickel at recoveries of 70.0 and 54.4 percent, respectively. Flotation of the talc followed by bulk sulfide flotation resulted in a nickel content greater than 5 percent. A locked-series test showed that 60.7 percent of the copper and 73.7 percent of the nickel could be recovered at grades of 1.29 and 4.85 percent, respectively.

Jan 1, 1961

By W. Gibson Jaworek

Of increasing importance to the student of fuels economics has been the extent to which different primary energy sources can substitute for each other in the various energy markets of the nation. Knowledge of the nature and extent of fuel interchangeability can aid the fuels economist in projecting trends of energy utilization, as well as giving him a better understanding of the past and present conditions of fuel markets. It is also important to the consumer to know just how much flexibility he can maintain in his energy consuming operations. And, finally, various governmental bodies show keen interest in the degree of energy substitutability in determining public policies concerning the fuels industries. The presence of excess fuel production capacity in the United States during the early 1960's indicates that fuel interchangeability should become more prevalent in the increasingly competitive energy markets of the nation. Discussion of fuel intercompetition is almost always restricted to qualitative terms-because of the lack of comparable statistical data, between the different energy sources in geographic or "type-of-use" fuel, markets. There are exceptions, of course, such as, the excellent fuel consumption data which are available on steam electric generating plants throughout the nation. In other sectors, statistics are at best incomplete.' Inmost instances, indirect fuel consumption indicators, such as sales of fuel burning equipment, are extensively used to measure market shares of a particular fuel; however, these indicators are hard to evaluate precisely without prior knowledge of the total competitive market.

Jan 1, 1961

By W. W. Fowkes

The Federal Bureau of Mines examined a low-temperature tar obtained from a small-scale commercial unit for carbonizing North Dakota lignite for products that might be important to the economic processing of the tar. Tie tar may be divided into three distinct parts: (1) Tar acids, 45 volume-percent; (2) tar bases, 1 volume percent; and (3) neutral compounds, 54 volume-percent. It has a boiling range of approximately 150° to 380° C. (the decomposition temperature) and yields 18 weight-percent as hard pitch. The tar distillate up to 365° C. may be separated as: (1) Tar acids, 48 volume-percent; (2) tar bases, 1 volume-percent; and (3) hydrocarbons, 51 volume-percent. The tar-acid distillate, boiling to approximately 265° C., was characterized in some detail; the neutral fractions and the tar bases were less thoroughly examined. In general, as might be expected of a primary low-temperature tar, the lower boiling fractions are less in quantity compared with the usual high-temperature tar. The homologous series of each major class appears to be rather complete, although some components are present in very small amounts. The tar is quite unstable thermally, and might be more conveniently processed by extraction methods rather than by distillation procedures. The neutral fraction of the tar is highly aromatic, and might be considered as base stock for the production of liquid fuels.

Jan 1, 1961

By Orville D. Mussey

During, 1956 the water used in mining iron ore in the United States amounted to about 2 billion gallons and the water used in producing iron concentrates-amounted to about 166 billion gallons. By 1980 an increase of about 65 percent is anticipated in the amount of water used for mining and beneficiating iron ore. Except for boiler-feed makeup water the quality requirements for water, for mining and beneficiating iron ores are not stringent. Adequate supplies. of water for development should be available at reasonable cost with the possible exception of some in arid regions.

Jan 1, 1961

By A. S. Moore

The Bureau of Mines is doing research and development work on removing acid-gas impurities from synthesis gas made directly from coal. Since conventional gas scrubbers, packed towers and bubble-cap columns, are expensive to construct and difficult to operate with viscous solutions, one aspect of the work was developing a compact, agitated, gas-liquid contactor for use with concentrated absorbents. The efficacy of the agitated contactor for absorbing carbon dioxide in diethanolamine increased with increasing solution rate, turbine speed, diethanolamine concentration, and carbon dioxide concentration in feed gas, and with decreasing liquid-gas ratio. It was unaffected by pressure between 200 and 300 p.s.i.g. and little affected by temperature between 115 and 190° F.

Jan 1, 1961

By J. D. Meakin, H. G. F. Wilsdorf

Using a combined decoration and etching technique the dislocation structure of annealed and deformed a brass has been studied. Annealed crystals revealed a low density forest and well-developed subboundaries; lightly deformed crystals contained discrete groups of dislocations. The dislocation density and the number of dislocations in a group were obtained from the micrographs. Using slip-line data, the mean path of a dislocation and the configuration of groups along an active slip plane have been deduced. Observations on secondary and cross-slip are reported. It has been the aim of many investigations to obtain detailed knowledge of the dislocation patterns which are present in metals before and after their deformation. The "decoration" of dislocations with impurity atoms has been considered as one of the promising experimental approaches, and much work has been done to develop this technique for revealing dislocation sites in metals. Following the early work by Castaing,' Castaing and Guinier,' and Lacombe and Berghezan~ on aluminum-rich aluminum-copper alloys, dislocations in this material have been studied extensively by others.+' In these alloys the dislocation sites act as nuclei for the precipitation of the second phase. The main results of the investigations on aluminum with copper are: i) the confirmation of the earlier contention that subboundaries consist of dislocation walls, ii) that many more dislocations are found in slip bands than in regions where less glide had taken place, iii) the observation of individual dislocations, lying nearly parallel to the surface investigated, and iv) that parts of dislocation loops, apparently emitted from a dislocation source, could be made visible. Recently, Jacquet, Weill, and Calvert have succeeded in revealing nearly concentric dislocation loops in quenched A1-4 pct Cu and thus indicated directly the existence of dislocation sources in a fcc metal specimen of normal dimensions. Another decoration method developed by Dash10'11 and applied to silicon crystals makes use of diffusing copper to the dislocations from a surface deposition. The dislocation pattern can then be observed by an infrared technique. His results include evidence for symmetrical and spiral Frank-Read sources, and for arrays of dislocation loops which follow simple crys-tallographic directions. Recently Low and Guard" have studied the dislocation structure of silicon-iron using carbon for the

Jan 1, 1961

By E. G. King

Difficulty has been encountered in making thermodynamic calculations of metallurgical reactions involving interoxidic compounds of the ferroalloy elements because of the serious lack of most thermodynamic data for these substances. This Bureau of Mines report (the first of a planned series dealing with entropies of vanadates, tungstates, and molybdates) presents low-temperature heat-capacity data and entropy values at 298.15° K. for three crystalline sodium vanadates--metavanadate (NaV03), orthovanadate (Na3VO4), and pyro-vanadate (Na4V2O7). The results are combined with data for the constituent oxides and elements to obtain entropies of formation of the vanadates. Previous to this report only one vanadate had been studied Similarly, ammonium metavanadate.4/

Jan 1, 1961

By W. A. Roliff

The renewed interest of the past few years in the Appalachian and Michigan oil provinces has not, as yet, created any marked increase in activity in Southwestern Ontario. During 1960 development drilling in-creased somewhat over 1959, but exploratory drilling decreased slightly. More attention was devoted to the deeper horizons, but lake drilling de-creased considerably. Oil production reached a new peak and gas production increased slightly. During 1960 an interesting oil and gas discovery was made in the Cambrian and gas discoveries six miles off-shore in the eastern part of Lake Erie were made in the Clinton-Cataract zone of the Silurian. This paper reviews activities during 1960, summarizes the discoveries made to-date and the pertinent exploration data relating to the prospects of the region and discusses some of the economic aspects of exploration and development. D URING the last few years there has •been a marked renewal of interest in the old petroleum

Jan 1, 1961

By McKenzie A. M

The Corridor ore body is so named because it occurs in an east-west zone or corridor of schist bounded on the north by the siliceous conglomerates of Mount Lyell, and on the south by similar conglomerates of the Tharsis ridge (Fig. 1). It was discovered after the geophysical prospecting methods described below had defined a target zone for diamond drilling.Since the proving of copper mineralisation by drilling, the corridor orebody has served the vital function of a convenient known target body for the orientation of more recently developed geophysical methods. Traversing of the orebody by these new methods has provided experience for the evaluation of anomalies elsewhere.Some of the methods applied had not been used in Australia before, and were introduced to the west coast of Tasmania through the undertaking there of modern regional exploration programmes. The authors feel that the information gained could be of assistance to others engaged in geophysical prospecting.HISTORY OF DISCOVERYProspecting in the Mount Lyell district has been more or less continuous since 1881. The first geological report was published by Thureau (1886).In 1934, Blazey and Douglas (1934-38) commenced geophysical surveys at Mt. Lyell using the equipotential method.They obtained anomalous indications in several discrete zones and actually detected the south-east half of the corridor orebody but their work never became the basis for...

Jan 1, 1961

By L. R. Fisher

The purpose of this investigation was twofold: (1) To devise a rapid method for determining quantitatively the porphyrin-carboxylic acid content of a particular crude-oil porphyrin aggregate, and (2) to isolate porphyrins in the crystalline state from crude-oil porphyrin aggregates. The first purpose was accomplished by applying adsorption chromatography. In fulfillment of the second aim three different crystalline porphyries were isolated by methods which involved both adsorption chromatography and fractionation of benzene solutions with hydrochloric acid of varying strength. The three porphyrins had etio, rhodo-, and phyllo-type absorption spectra, respectively. INTRODUCTION Many samples of petroleum have, as interesting minor constituents, chemical compounds known as metalloporphyrins. Their presence in crude oil and other bituminous materials was first discovered by Treibs a quarter century ago. Much experimental work has been done on metalloporphyrins because of their importance to the petroleum industry. They have a deleterious effect on refining catalysts. The ash resulting from the burning of heavy fuel oil is very reactive, We to the presence of metallic constituents, particularly vanadium. In oil-fired gas turbines, the ash may build up on the blades, causing imbalance of the rotors and, in addition, severe corrosion. In industrial boilers, the ash residue is responsible for severe damage to boiler tubes and to the refractory brickwork (15).4 Through study of the chemical constitution of the various metalloporphyrins found in petroleum, much can be learned concerning the origin, migration, and history of crude oils.

Jan 1, 1961

By Floyd G. Anderson

The increasing trend toward use of continuous-type mining machines created a significant dust problem in coal mining, which resolved itself into three categories: Visibility at face, deposition on return airways, and the potential health hazard. The control measures applicable to these conditions and studied or developed from 1955 through 1957 are summarized and reviewed in this report. Other important problems brought into focus during the same period were radiation exposure in uranium mining and high temperature and humidity. Although temperature and atmospheric pressure alone may not be contributing factors in the incidence of silicosis, the few mining companies who operate under the extremes of these conditions are dust conscious and keep dust-control engineers on their operating staffs.

Jan 1, 1961