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By R. B. Booth, W. F. Linke

The continuous interest of the American Cyanamid Company in producing superior polymeric flocculants and dispersants for the mining industry has resulted in a broad, general study of the physical chemistry of mineral-polymer systems. The aim of this program has been to establish a sound theoretical basis on which practical problems could be analyzed, and which would lead to the development of new and improved flocculating and dispersing agents. This study has required the cooperative effort of physical, analytical, and polymer chemists, as well as engineers familiar with mining problems. This report summarizes the results of some of our investigations over the past two years. Further studies along these and other lines are in progress and will be reported in the near future. MEASURING FLOCCULATION IN THE LABORATORY The foremost problem in studying flocculation in the laboratory has been to establish reproducible methods of comparing and evaluating the effectiveness of various reagents. Previous workers have measured settling -rates 1,8 filtration rates2 , and sediment volumes3 . Direct observations of the floc size, or the clarity of the supernatant liquid, can also be used. AIthough these parameters are all interrelated, they do not always measure the same physical properties of the suspensions, and hence are not equally useful or reliable. Whatever the method of comparison selected. the testing procedure must be carefully defined and standardized. The results must be satisfactorily reproducible, and for practical purposes must accurately reflect the results obtained in mill use. In order to compare the data obtained in these various types of test, the physical nature of the flocculated system must be examined in some detail. In an unflocculated system, only the larger or denser particles (the "sands") settle at a useful rate. The sediment can be observed to build up from the bottom of the cylinder, while the fines remain in suspension for a long period of time. If the system is not disturbed, even the microscopic fines can be seen to classify themselves as they fall over a period of days. When a high molecular weight polymer is added to the system, the colloidal particles are tied together randomly in flocs, and the sands and fines settle together. The line of demarkation between solid and liquid phases moves downward from the top of the cylinder. The settling rate of the flocs depends on their size and on their effective density. For a given mineral sample, the larger the flocs, the faster the settling. Since the large flocs cannot pack as closely as small ones, they produce a sediment with more pore spaces, and hence of larger volume, which is easier to pump and to agitate. Although it is nearly impossible to measure individual floc sizes, it is relatively easy to determine settling rates and sediment volumes. Of these two, the settling rate is simpIer to measure, and hence generally more practical. Reproducible sediment volumes can only be obtained by allowing the solids to pack for a rather long period of time (e.g., hours to days), and although the volumes thus observed are directly related to the degree of flocculation (average floc size), it is often impractical to wait so long for the results.

Jan 1, 1961

By M. D. Carver

This investigation was undertaken by the Bureau of Nines to determine the effects of impurity levels on the mechanical properties of columbium at low temperatures. High-purity, electron-bombardment-melted columbium was purchased and used as a basis material. Variations in impurity levels were obtained by arc-melting charges containing definite amounts of added impurities. Tensile tests were conducted at low temperatures. Results showed the almost pure basis metal to be ductile at minus 194° C., the lower limit of the range used, Ductility of less pure columbium appeared to depend on interstitial element content. The ductile-to-brittle transition temperature appeared to be raised by increasing carbon content in the range of 50 to 730 parts per million, nitrogen content in the range of 50 to 200 parts per million, or total interstitial element content in the range of 240 to 1,380 parts per million. Some evidence was obtained indicating that decreasing cold work also raised the transition temperature, but recrystallization appeared to have no effect on it. Variations in interstitial element levels appeared to have little or no effect on ultimate strength of columbim in the range of room temperature to minus 194° C, Physical metallurgy studies of massive arc-melted and electron-bombardment- melted columbium were included in the columbium-tantalum research work assigned to the Albany Metallurgy Research Center in fiscal year 1959.

Jan 1, 1961

Jan 1, 1961

By John P. Capp

The feasibility of simultaneously burning several paths through a coalbed to develop a multiple path underground gasification system was investigated by the Bureau of Mines during two experiments, Boreholes were drilled through the overburden and into the coal and arranged in a circle approximately 50 feet from a central borehole. In the first experiment, in an area which had previously been hydraulically fractured,5 air was injected at the center borehole. The coal was ignited at the other boreholes and the fire fronts traveled toward the center, counter to the flow of air, to backward burn paths through the coalbed. Two paths were linked during the first 5 days of operation. The outlets of these two paths were throttled and air pressure was increased to maintain the flow of air, but no other linkages were made. Fourteen days after the two linkages these two paths were opened and gasification was carried on for 10 days, but with only moderate success. In an effort to overcome operating difficulties air was injected at the peripheral boreholes, and the gases were drawn off at the center borehole. Reversed flow operations continued for 12 days and two more paths linked. The heating value of the gas generally was higher than 100 British thermal units per standard cubic foot (B.t.u. per std. c.f.). Because only four of seven paths linked, however, the entire system could not be evaluated with respect to product-gas output and recovery of energy.

Jan 1, 1961

By J. M. Hemstock, H. L. Ames

THESE forums have been held annually since they were introduced by Mr. L. E. Djingheuzian in 1957. The response of millmen to questionnaires such as the one this year is ample evidence of the interest these create. This year's topic is unlike those of past years since it is an attempt to understand a new concept of grinding rather than to improve the old. Before, we were thinking in terms of 2-5 cents improvement in grinding costs, now we will be discussing savings of 15-2 5 cents. As a background for this forum we will begin by summarizing the major controversial issues relating to grinding with steel, many of which will undoubtedly apply to pebble milling. Our •task to-day is to learn what has already been done in pebble milling and obtain a fair overall view of this method of grinding.

Jan 1, 1961

By J. W. Davis

The storage stability characteristics of a diesel type fuel were determined to evaluate the effect of the polar compounds in the fuel. These compounds, comprising most of the nitrogen and oxygen containing compounds and many sulfur containing compounds, were separated from the fuel with a chromatographic column. This fraction was further separated into three polar extracts by graded elution through the column. Each extract was characterized. A storage program using the depolarized fuel, the fuel as received, and blends of the extracts with both fuels, was conducted. Results showed that the removal of the more polar components stabilized the fuel. Blending the polar extracts with the original fuel and with the depolarized fuel in the same ratio as they existed originally and at two and three times the original ratio increased the amount of gum present before storage, but had little effect on the formation of additional gum during storage. Distillate fuels produced by commercial refining of petroleum contain traces of organic nitrogen, sulfur, and oxygen compounds that are more polar4 than the remainder of the fuel. Recent laboratory studies by the Federal Bureau of Mines (1),6 in which these compounds were removed from a fuel, have shown that they influence its storage stability. The objective of this work was to determine the amount of these compounds present in a fuel and their effect upon its stability in storage. To evaluate the role of these polar compounds, it is necessary to remove them from the distillate fuel. Many can be removed by chemical treatment (2), but such treatment precludes reblending the polar components to approximate the original fuel composition. Solvent extraction is free of some of the criticism of chemical treatment, but it is more difficult because of the complex mixture from which compounds must be removed.

Jan 1, 1961

Jan 1, 1961

By E. C. Perkins

The purpose of the research described in this report was to develop techniques for using ilmenite from domestic deposits for the production of titanium tetrachloride. The research was done by the Federal Bureau of Mines in cooperation with the General Services Administration under contract DMP-116, Utilization of Domestic Ilmenite. Bench-scale continuous chlorination of an Idaho ilmenite containing 27.9 percent titanium and 35.6 percent iron yielded a crude titanium tetrachloride suitable for purification and for the production of titanium metal and pigment. A summary of the results of 380 hours of operation showed that 82.4 percent of the titanium was chlorinated, with 92.5 percent utilization of chlorine. The construction- of a. quartz tube chlorinator 4-inches in diameter and 24 inches long is described with the necessary details of operation.

Jan 1, 1961

Cessation of mining on the Bendigo goldfield makes it evident that, as the older generation fades away, knowledge of the famous Bendigo saddle reefs will be limited in the future by their written records. It is important therefore that the summarised account by D. E. Thomas (1953) in the Geology of Australian Ore Deposits should not be misleading. Fig. 6 in this article is stated to portray a cross section and longitudinal section through a series of gold shoots in the Garden Gully 300 ft. reef. The gold shoot along the capof the saddle reef is represented as extending down the east leg in a series of prongs, with the tips of the prongs about 50 ft. apart. It is the purpose of this note to indicate that this illustration can be suspected to be a diagram of the old stopes instead of a diagram of the distribution of gold in the quartz.The original sketches of Figs. 6 and 7 in Thomas' account were extracted, I believe, from the field note books of H. S. Whitelaw, years after his death in the late twenties. Whitelaw was stationed in the Bendigo office of the Geological Survey of Victoria, carrying out geological surveys of the Bendigo mines. He was there for many years before the Gold Research committee started its investigations in 1916 and he was acutely aware of the problem attached to the distribution of gold in the reefs. He had felt concern that manyauriferous reefs were being mined without adequate study and record and he decided, as he expressed it to me, to pick up what he could as he went along. There can be little doubt that the diagrams of Figs. 6 and 7 are products of this resolve.Opportunities to investigate gold occurrences at Bendigo were limited before 1916 because the field was operated by Manuscript received at The Institute 18th November, 1960.

Jan 1, 1961

By A. D. Hahn

The Federal Bureau of Mines examined ilmenite-bearing sands in southern Texas as part of a program to discover sources of supply for the domestic titanium industry. Deposits were examined from May 1956 through January 1959 in the outcrops of sandstone beds in the Jackson group of Eocene formations in Lee, Burleson, Fayette, and Starr Counties on the Gulf Coastal Plain; in alluvial valley fill in Brewster County in southwest Texas; in the sand beaches of Matagorda Peninsula and the Galveston, Padre, and Brazos Islands--part of the offshore chain of barrier islands along the Texas coast; and in unconsolidated sediments in Willacy County on the Rio Grande delta in the southeast Texas.

Jan 1, 1961

The oxidation of sulphide minerals in aqueous suspension is discussed from several viewpoints. Limitations of our present knowledge are pointed out, and several points where further information would be of special interest are mentioned.Firstly, some properties of minerals and their effect on oxidation are discussed. Properties of different species, such as crystal structure, lattice bonding, and "metallic" properties are mentioned, and then the effect of variation within a given species is discussed. The effect of physical factors, especially particle size, is also considered. Other variables discussed include the importance of solution composition, and its effect on the nature and rate of reaction, and the use of various oxidising agents. Some factors concerned with the whole system, such as temperature, pulp density and stirring rate are then considered.Finally, the nature of various oxidation products is discussed with reference to the kinetics of reaction and the nature of the rate limiting step. It is suggested that more attention should be paid to electrochemical explanations of the reaction mechanism.INTRODUCTIONKnowledge of the factors governing the rate of oxidation of sulphide minerals in aqueous suspension is a prerequisite for the effective control of many ore treatment operations. Rapid oxidation of sulphides is usually desired during the leaching of sulphide ores and concentrates, but in the cyanidation of gold ores, or in the leaching of uranium ores, any oxidation of sulphides may be regarded as an undesirable side reaction. Knowledge of many of the factors involved is also of interest in connection with the oxidation of sulphides in flotation circuits and in natural ore forming processes.Systems for which some reasonably quantitative data have been published are listed in Table 1. Qualitative...

Jan 1, 1961

By J. L. Konchesky

In gasifying pulverized coal with steam and oxygen, the particle size of the coal fed to a gasifier should be as small as economically possible. A potential way to achieve this advantage is to reduce the particle size of the coal by passing the coal-steam mixture at high velocity through a heated tube coil before the mixture enters the gasifier. To evaluate this method the Federal Bureau of Mines flashed coal-water slurries in externally heated metallic tube coils to determine the extent of size reduction. The first of two different laboratory-scale apparatus reduced the average particle diameter of subbituminous C coal from 190 to 110 microns at an outlet velocity of 330 feet per second (f.p.s.). At the same outlet velocity, a second apparatus reduced the average particle diameter from 250 to 140 microns. An increase in velocity produced more finely divided coal, but variation in temperature and pressure had no effect except as they affected velocity. Virtually the same size reduction was noted for five ranks of coal at equal velocities. The rate of increase in particle-size reduction with increase in velocity decreased with a decrease in particle size. The pulverizing mechanism was concluded to be abrasion of the particles with each other and with the tube wall.

Jan 1, 1961

By Eugene T. Sheridan

The Bureau of Mines annually canvasses the peat producers in the United states and publishes economic data on the peat industry, based upon reports submitted by producers. This publication lists all producers that reported commercial production to the Bureau for 1960 and presents data on individual plants. The companies named herein represent virtually all commercial producers, although a few small companies may not have been canvassed as the industry has many small operations that operate intermittently. Output of the various companies listed ranged from a few tons to more than 50,000 tons. Peat is included in the Bureau's annual surveys of the mineral industries because peat is classified as a mineral fuel. Although none is used for fuel in the United States, peat is a potential source of energy and ranks as one of our large mineral resources. The domestic peat industry sells peat, chiefly, for use as a soil amendment for general soil-improvement purposes. During the past decade the industry has expanded rapidly with operations increasing from 45 in 1947-494/ to 115 in 1960. Output during this period has more than tripled, increasing from 131,782 short tons to 470,889 short tons.

Jan 1, 1961

By Ronald M. Lewis

Quadratic functions, Q(hkl), are given to six places in increments of 0.01° for 2? from 00 to 90° for FeKa and from 25° to 180° for FeKa1. The wavelengths used for Fe in the computation are those agreed upon by the Editorial Commission of the International Tables for X-ray Crystallography (1950): FeKa1 1.93597 A.; Feka2 1.93991 A. INTRODUCTION At the Federal Bureau of Mines laboratory, Norris, Tenn. X-ray diffraction crystallography using tubes with iron targets revealed a need for a handy reference for the quadratic functions of iron radiation. The tables presented here were prepared to satisfy that need. The quadratic form Q(hkl) may be expressed in terms of the Bragg diffraction angle 2? and of the wavelength ? as

Jan 1, 1961

By P. M. Sullivan

The principles and application of amalgam electrolysis to the recovery of zinc and tin from secondary products were studied; this Bureau of Mines project was one phase of investigating the development of more efficient methods for processing iron-bearing zinc and tin to produce both base metals of high purity. Zinc of 99-99-percent purity was recovered from galvanizer's dross with recovery efficiency of 98 percent. Tin of 99.9-to 99.99-percent purity was recovered from hardhead with recovery efficiency of 81 percent. Both materials were treated by the same method in separate systems. Mercury was used to leach zinc from dross and tin from hardhead to form amalgams of each metal, both of which were subsequently refined electrolytically to produce high-purity metal. Impurities that were contained in both secondary products behaved as theoretically predicted; impurities that were insoluble in mercury remained as sludge in the leaching column. Except for lead, the readily amalgamated impurities were prevented from fouling the electrolyte by the blocking action of the amalgam electrode. Lead impurity in the tin-refining system dissolved and immediately precipitated as the sulfate. The primary advantage of the amalgam refining method lies in direct recovery of the extremely pure base metal from highly contaminated secondary material.

Jan 1, 1961

[Appalachian Petroleum Section: James M. Kimbrough, chairman; John H. Adair, first vice-chairman; Walter L. Diddle, second vice-chairman; Byron M. Finch, secretary-treasurer. Balcones Section: Robert V. West, chairman; Frank W. Jessen, first vice-chairman; Zane V. Morgan, second vice-chairman; Brantley G. Myers, secretary-treasurer. Meets 4th Wed., Petroleum Club (San Antonio) or Terrace Dining Room (Austin) Billings Petroleum Section: Charles B. Evans, chairman; L. M. Lyon, first vice-chairman; Gordon E. Lansford, second vice-chairman; Fred. A. Haddenhorst, secretary-treasurer. Meets 3rd Tues., Billings Petroleum Club. California Coastal Section: Robert L. Richardson, chairman; David K. Hayward, first vice-chairman; W. Jackson Bransford, secretary; William N. Harwell, treasurer. Meets 3rd Thurs., Pierport Inn, Ventura. Caracas Petroleum Section: Edwin A. Moo re, chairman;. Jose Cirigliano, vice-chairman; Frank B. Davis, secretary; Robert N. Powers, treasurer. Meets 2nd Tues., Caracas Theater Club.]

Jan 1, 1961

By Mah Alla D.

Previously existing heat-of-formation values for the oxides of vanadium were rudimentary. They were subject to uncertainties of 1 to 5 kilocalories per gram-atom of contained oxygen. This fact has been the only adverse influence on the accuracy of thermodynamic calculations involving these substances, as the requisite entropy and high-temperature heat-content data are known with reasonable accuracy. This report presents new heat-of-formation data for four oxides of vanadium (VO, V203, V02, and V205), obtained by combustion calorimetry. It is believed that the uncertainties have been reduced to 0.1 to 0.3 kilocalorie per gram-atom of contained oxygen. The new heat-of-formation data were combined with existing entropy and high-temperature heat-content values to obtain free energies of formation of the four oxides at temperatures up to 2,000° K.

Jan 1, 1961

By E. R. Palowitch

This report stems from a study by the Bureau of Mines of the possibility of reducing coal filter-cake moisture by applying radiant heat directly to the filter cake while under vacuum during the drying phase of the filter cycle. One disk of a 4-foot-diameter vacuum filter was equipped with gas-fired radiant-heat generators and the effect of radiant heating on the moisture content of a variety of filter cakes was studied. The results of this investigation show that this process can best be described as a filter aid capable of increasing the effectiveness of conventional filtration approximately 6 percentage points of moisture. The operating cost of removing water by this method is somewhat lower than the average operating cost of thermal drying and is considerably cheaper when the total cost is considered. Removal of water from coal that has been wet-cleaned is an important part of the overall coal preparation process. Water is a contaminant, and it is foolish to wash coal to reduce its ash content and add inert water in the process. In some instances the removal of water is actually more important than the removal of ash-forming minerals; its weight adds to the cost of transportation, and its evaporation during burning or carbonizing absorbs useful heat. Fine coal that contains more than about 10 percent moisture is notoriously difficult to handle. A problem thus exists for which there are sound practical and economic reasons to seek a solution.

Jan 1, 1961

By T. Koulomzine, R P. Jaeggin

The claims now held by Mount Wright Iron Mines Co. Limited were acquired by staking in 1956, 1957 and 1958, i.e., some time after the major deposits of the Quebec Cartier Mining and Normanvi!le Mining Co. (formerly Quebec Cobalt & Exploration Ltd.) were already discovered and partly outlined. The choice of the location of the Mount Wright hold-ings was governed simply by the -availability of ground still open to staking and by its proximity to properties held by major iron companies. Mount Wright Iron Mines had no previous knowledge of the geology and no aeromagnetic results were available to it to guide the choice of areas to be staked. In order to explore the newly ac-quired claims it was decided to make a grid of widely spaced magnetic profiles on the ground rather than use aeromagnetics. This afforded the possibility of making some geological observations simultaneously with the geophysical measurements.

Jan 1, 1961

By R. W. Stahl

Employees and dollars are necessary to all enterprises and any force, such as fire, which destroys either, can bring very serious consequences, including business failure. Since everyone acknowledges the necessity of conserving human life, we will devote most of our paper to the economic factors involved. A coal-mine fire is considerably more difficult to combat than a fire in a surface building because of the combustible surroundings in the mine, the explosive gases emitted from the coal, the suspension of explosive dust when mine timbers burn and the unsupported roof falls, the limited space in which approach to the fire can be made, and the limited avenues of escape. A survey of coal-mine-fire protection indicated that a rather low value was being placed on property and equipment. This prompted comparison with other industries. The comments made in this comparison are not intended as an indictment of the coal industry, since we do have mines that are well protected against fire, but the comments on conditions at the mines visited are factual and may help others to improve similar conditions. SURVEY PROCEDURES Plants of the steel, aluminum, rubber, chemical, and petroleum industries were surveyed, and all facets of the fire-protection scheme were covered. The industrial plant invariably had four times as much water readily available for instant use than the mine. In many mines where water is available, no equipment for applying it is provided, such as hose, nozzles, and adapters, so that time is lost in collecting this equipment. (See Table I.) EXTINGUISHERS Many more and generally larger portable extinpishers are available at the plant as compared to the mine. The extinguishers are generally placed nearer to sources of danger. In addition, respiratory protective equipment is always available at strategic points in plants but only in a few mines. (See Figs. 1 and Table 11) INSPECTING AND TESTING EQUIPMENT Plant water facilities are checked weekly and flushed at 6-month intervals, and hose is pressure-tested at least yearly; some mines check water yearly, but hose is not tested unless used. Fire extinguishers are inspected weekly in plants and completely overhauled yearly; one mine had monthly checks and overhauls only after use. FIRE BRIGADES AND TRAINING Every plant had designated fire-fighters and some complete full-time brigades; at one mine a chief mechanic was designated as being in charge of fires, and other depended entirely upon officials who might not be familiar with the equipment. COST OF FIRES AND PERCENTAGE OF CAPITAL INVESTMENT IN FIRE PROTECTION The direct cost of recent mine fires ranged from $128,000 to $240,000; indirect costs, such as lost tonnage, idled equipment, lost orders, and the like might run the cost to over $500,000. (See Figs. 2 and 3).

Jan 1, 1961