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By A. E. Powers

YEARS of experience and research have shown that molybdenum, tungsten, and vanadium are among the most useful and effective elements in augmenting the high-temperature strength of heat-treatable, ferritic steels. Grün, for example, in conducting an early survey of the strengthening effects of various elements in annealed, low-carbon steel at 750° and 930°F (400° and 500°C), found molybdenum and vanadium to be the most effective.' Holtmann comprehensively studied the strengthening effects of molybdenum and vanadium in quenched and tempered steels at 930°F as a function of microstructure and carbon content.' He found creep strength to be related to the saturation of the austenite at the austenitizing temperature, such that strength is increased by alloying until the y loop is reached—the terminus of complete austenitization. Beyond this degree of alloying, the inability to heat treat will result in lower strength, at least for low and moderate creep temperatures. Tungsten, owing to higher cost than molybdenum, has been little used in ferritic high-temperature steels. As a result, very few investigations have been made of its high-temperature strengthening ability, and reliable data on its effectiveness are not available. Grün rated tungsten far less effective than molybdenum at 930°F (500°C) on a weight-percentage basis.' However, Tammann has found that tungsten is as effective as molybdenum in raising the recrystallization temperature of iron. For this reason Smith, in a review of the subject, has advocated a re-examination of the influence of tungsten on the high-temperature strength of steel.' In any study of the effects of alloying additions on high-temperature properties, recognition must be made of the many variables involved, some of which can be controlled but have been ignored in innumerable investigations of the past, and some of which are difficult or even impossible to control. One cannot, for example, assign a definite strengthening index to any one alloying element, for this will be dependent upon the microstructure (heat treatment and mechanical treatment), testing con- ditions (temperature, time, and stress), and the complete composition of the steel (accompanying alloying elements, impurities, etc.). One ever-appear ing variable, hardness or tensile strength at room temperature, may be eliminated by heat treating all of the alloys to a single hardness level. An attempt may be made to control the variable of primary quenched structure by oil or water quenching the test specimen. The control of such variables may not be possible in cases of widely varying compositions, but at least such deviations should be recognized. Material and Procedure The alloys, made as 30-lb ingots in an induction furnace, all had the same base composition of about 0.18 pct C, 0.85 pct Mn, and 0.48 pct Si. They were grouped as follows: Mo Group—Containing up to 5.2 pct Mo. W Group-Containing up to 6.0 pct W. V Group—Containing up to 3.3 pct V. Mo-V Group—Containing up to 2.7 pct Mo and up to 1.4 pct V. Mo-W Group—Containing up to 2.5 pct Mo and up to 2.5 pct W. The steels, listed in Table I, were forged to ¾ in. sq bars and the material for the high-temperature, rupture-test specimens was further swaged to %-in. round bars.

Jan 1, 1957

By M. R. Geer

The widespread adoption during the past decade of the dense-medium process for cleaning coal increases the need for technologic studies of the process. Such studies provide information that will insure maximum usefulness of this process in its present form and may well lead to substantial improvements in design and opera¬tion. The Bureau of Mines has published the results of cleaning trials on a wide variety of coals in two dense-medium pilot plants5/ and reported the recovery of coal from waste by dense-medium treatment.6./ The present report deals with the viscosity of magnetite dense medium, an important subject about which virtually nothing has been published. Specifically, the report concerns methods for measuring viscosity, the influence of various medium contaminants on viscosity, the effect of viscosity on cleaning results, and the influence of viscosity on consumption of medium. Cleaning trials on four coals of varied density composition in a pilot plant, using mediums of different viscosities, showed a steady reduction in cleaning efficiency with increasing viscosity in every instance. However, the behavior of each coal in a viscous medium was distinctly individual. With one, an increase of only 1 centipoise in viscosity caused a reduction in recovery efficiency of 7.7 percent, whereas the same increase in viscosity with another reduced recovery efficiency only 2.7 percent.

Jan 1, 1957

The first metal-mine accident-prevention course was prepared and published in 1942-45 as a series of seven miners' circulars (Nos. 51-57). The scope of the course has been broadened, revised, and brought up to date and is being published as a similar series of seven miners' circulars (Nos. 51-57, revised) on accident prevention in metal and nonmetallic mines. These circulars are: Accident Statistics (Miners' Circular 51), dealing with general statistics on accidents and injuries at metal and nonmetallic mines, including causes, costs, and the use of investigations and reports of all accidents.

Jan 1, 1957

By G. G. Eichholz

SUMMARY RADIOACTIVE dynamite has been prepared by introducing a small amount of antimony-124 into the explosive. Test work is described on the effectiveness of this tracer, on radiation levels in its neighbourhood, and on different methods of .application. Factors determining the choice of isotope, amount of activity, and overall cost of this process are discussed. INTRODUCTION Instances are known in which dynamite remains unexploded in drill holes in mining operations. Usually such 'bootlegs' are easily located by inspection of the face and the powder is removed before subsequent drilling is started. Occasionally, however, serious accidents occur because workmen drill into an undetected piece of dynamite. In order to avoid such accidents it was suggested that a different method of location might be tied, such as that afforded by the use of radioactive tracers. This paper describes some experiments that were carried out under the auspices of the Department of Mines and Technical Surveys, with the active co-operation of Canadian Industries Ltd. and Canadian Refractories Ltd., to test the feasibility of such a scheme.

Jan 1, 1957

By F. R. Cattoir

Analytical methods are presented in this paper for determining soluble titanium, total titanium, indicated titanium, and average effective valence in titanium chloride - sodium chloride mixtures. In addition, data are given showing the effects of coarse and fine grinding on the degree of oxidation and average effective valence of such samples. INTRODUCTION The Electrometallurgical Experiment Station at Boulder City, Nev., as part of the Bureau of Mines program to obtain more efficient utilization of our natural resources, has been developing and improving titanium extractive metallurgical methods and techniques since 1945. Numerous reports have been published describing development of the Kroll process,4/ the electrorefining technique,5/ and methods of analyzing titanium sponge.6/

Jan 1, 1957

By R. A. Hatch

This report summarizes the results of nearly 8 years research on and production of synthetic mica at the Electrotechnical Experiment Station of the Federal Bureau of Mines, Norris, Tenn. This program was undertaken at the request of the United States Department of the Navy and was financed mostly by the Army Signal Corps and the Navy Bureau of Ships through a contract with the Office of Naval Research, The original objectives included fundamental studies of fluor-phlogupite and other fluorine-micas and production of synthetic mica sheets on a pilot-plant scale. The first 3 years of this project were devoted mainly to a search for practical solutions of the many problems involved in designing and constructing a pilot plant for crystallizing fluor-phlogopite mica. The first and most urgent need was a suitable container for the corrosive mica melt. After extensive study, it was concluded that platinum, graphite, high-silica fire clay, and silicon carbide were the most promising refractories for crucibles; but none was perfect. Silicon car¬bide seemed to have the better combination of qualities, combining good corrosion resistance with oxidation resistance.

Jan 1, 1957

By F. N. Bender

Percolation leaching of wad-type manganese ores was investigated, using a novel system of alternate upward passage of sulfur dioxide gas through moistened ore and downward percolation of wash solutions to extract solubilized manganese. Bench and large-scale tests designed to simulate vat and heap leaching were made on four wad ores from Arizona and Nevada and on a pailomelane ore from Arizona. Three of the wad ores required prebaking at 500° to 600° C. to produce a permeable agglomerate that would not slake during percolation washing. The hard-type ore and one of the wad ores that contained a large amount of granular gangue did not require prior roasting. The deportment of the different ores toward leaching and percolation was studied with particular reference to the influence of the sulfur dioxide - oxygen ratio and the effect of gas dilution on the rate of manganese dissolution, dithionate formation, and acid production. Crushed charges of the ores, as coarse as 1 inch and as fine as 1/4 inch, were treated for periods of 5 to 11 days. Percolation of the gas and leach solutions through the charges was achieved without difficulty. The manganese extractions varied between 78 and 97 percent and depended upon the size and type of ore leached. The average quantity of sulfur dioxide required in the larger scale tests was about 2.6 pounds per pound of manganese recovered. The dithionate formation varied from 0.35 to 0.9 pound per pound of manganese extracted depending upon the strength of leaching gas.

Jan 1, 1957

By C. H. Schack

Although viscosity is known to be important in processing and handling finely ground urea, its effect has never been fully quantified. This report describes the methods used and the results obtained in the initial phases of a broad investigation of the influence of viscosity of water suspensions of minerals in flotation, thickening, filtering, and other mineral-dressing unit operations. Several types of vis-cosimeters were tested before reliable and reproducible results could be obtained on mineral suspensions. After the viscosimeter used in the research was calibrated and standardized, tests were made on six pure minerals to study the relationship of pulp density, particle size, crystallinity, and cleavage on viscosity. An orifice-type viscosimeter equipped with a mechanical stirrer gave as good results as other types and was more flexible, faster, and simpler to operate. The orifice-type viscosimeter, when calibrated and standardized with glycerin and water mixtures, proved satisfactory over a wide range of viscosities. The accuracy and reproducibility were reasonably constant between 1 centipoise and 200 centipoises, the anticipated range in common mineral-dressing unit operations.

Jan 1, 1957

By David B. Burrows, Francis R. Conley

INTRODUCTION A prerequisite to the evaluation and management of oil properties is accurate information derived from the analysis of core samples; but reliable data, such as porosity and permeability, can result only if all oil and water have been removed from the core samples analyzed. The most common method of core cleaning used to date has been Soxhlet extraction—a somewhat static technique, which depends upon the slow diffusion of hot solvent through the core sample. Soxhlet extraction performs satisfactorily only with highly permeable samples and at best requires long cleaning periods. The centrifuge method was developed in 1951 by Continental Oil Co. to overcome the inefficiencies inherent in the Soxhlet method. The new method is basically an operation in which hot solvents are caused to flow through the samples under the influence of centrifugal force. The centrifuge unit has proved so successful that samples which formerly required days for partial extraction can now be completely cleaned in approximately one hour. The original idea was conceived in 1950 by Elmer S. Messer, whose early experiments consisted of flowing solvent over sandstone samples suspended in a revolving basket and driven by a vertically mounted vacuum cleaner motor. Results were so outstanding that more permanent units were constructed. A modified model using this basic design was recently built by Core Laboratories, Inc., and is now used regularly in their operations. DESIGN Fig. 1 shows a photograph of the two extractors routinely used to clean small core plugs in the Production Research Div. of Continental Oil Co.'s Ponca City laboratories. For illustrative purposes, the basket from one of the units has been removed, and because both extrac- tors are of identical design only one is described in the following discussion. Each extractor unit consists of a centrifuge and a solvent still. The core basket of the centrifuge is made of mild cold rolled steel 7 1/2 in. in diameter and 1 1/8 in. deep. The basket holds 18 1-in. samples (cubical or cylindrical) and is attached directly to a cone fitted to the shaft of the motor. Both the outer rim and the hollow hub of the basket contain perforations for the passage of solvent and extract. The solvent is delivered to the perforations by means of a copper tube inserted into the hollow hub. The motor is a vertical tool post grinder motor; (115 v, 5.6 amp, 0-60 cycles, AC-DC, rated at 1/3 hp). It has a rated speed of 10,000 rpm under full load and 15,000 rpm with no load. Variation of speed is obtained by the use of a variable transformer. The solvent still was constructed from one end of a stainless steel oxygen bottle by inserting a heating element, sight glass, and piping as shown on the schematic diagram, Fig. 2. The heater used was a three-position, 1,000 w, 115-v, immersion type. Intermittent flow of solvent to the centrifuge is obtained by means of a siphon bottle inserted between the condenser and the centrifuge.

Jan 1, 1957

By Alla D. Mah

Titanium forms several compounds with oxygen and also is able to dissolve interstitially about 33 atomic percent of oxygen. Starting with titanium dioxide, reduction becomes increasingly difficult as oxygen is removed; and the final step, be reduction of the titanium-oxygen interstitial solutions, is by far the most difficult. The possibility of reducing titanium oxide, or of purifying titanium containing oxygen, by treatment with certain more volatile metals has been a subject of considerable interest. Theoretical appraisal of the limitations of this possibility, however, has been hampered by lack of adequate information on the thermodynamic properties of the titanium-oxygen solutions. The purpose of the present work was to remedy this difficulty by expanding the thermodynamic knowledge regarding these solutions. The experimental work involved three types of calorimetry and furnished the following information: (1) Heats of formation of 11 titanium-oxygen solutions, in the range of 0 to 10 wt.-percent oxygen, were determined at 298.15° K. As a byproduct, an improved value of the heat of formation of rutile was obtained, which, in turn, led to improved values of the heats of formation of the lower titanium-oxygen compounds. (2) Low-temperature heat-capacity data and entropies at 298.15°K in were determined for 2 representative titanium-oxygen interstitial solutions. (3) High-temperature heat-content data were obtained for 2 titanium-oxygen interstitial solutions to about 1,600° K.

Jan 1, 1957

By Herty, C. H.

No attempt will be made here to review the previous work done by investigators on the general subject of inclusions, because it was discussed sufficiently in an early cooperative bulletin of this series (No. 36, 1928), and reference was then made to general bibliographies. The work described in this present bulletin deals directly with the study of the mechanism of deoxidation of steel with aluminum and the formation of inclusions containing alumina. Unquestion- ably, such inclusions are encountered in most steel-making practices and little has been done to determine their characteristics. Aluminum is used to ensure rapid deoxidation during the solidification stages of the steel. For this reason the possibilities of inclusion elimination are slight and alumina-containing particles will undoubtedly be present in the ingot. Besides this common practice, aluminum is often used in the ladle with other deoxidizing agents such as silicon and manganese. Ladle additions of aluminum are made to rimming steels to obtain the correct partial deoxidation desired in this type of steel. In killed steels the aluminum is added to ensure soundness, as far as blowholes are concerned, in the ingot. In either rimmed or killed steels, alumina or alumina-containing inclusions are found therein, the amount and type depending on the oxidation of the metal, the amount of aluminum added, and the addition of other deoxidizers.

Jan 1, 1957

The first metal-mine accident-prevention course was prepared and published in 1942--45 as a series of seven miners' circulars (Nos. 51-57). The scope of the course has been broadened, revised, and brought up to date, and it is being published as a similar series of seven miners' Circulars (Nos. 51-57, revised) on accident prevention in metal and nonmetallic mines. These circulars are: Accident Statistics (Miners' Circular 51), dealing with general statistics on accidents and injuries at metal and nonmetallic mines, including causes, costs, and the uses of investigations and reports of all accidents.

Jan 1, 1957

By G. Reinberg, C. D. Clarke

MOST underground mining operations are dependent on pumping installations to keep the mine unwatered. The reliability of such installations is obviously of paramount importance. The volume of water to be handled is often considerable, and the total head is relatively high. In these cases, both capital cost and operating expense of the pumping installations will become significant factors in overall mining costs. To insure reliability and to keep efficiencies, and hence operating cosl;s, within acceptable limits it goes without saying that mechanical maintenance of a mine pumping installation must receive scrupulous attention at all times. Large mine pumping installations today almost invariably use multistage centrifugal pumps, since positive-displacement units would not be economically competitive except under very unusual conditions of small volume combined with extremely high heads. Centrifugal pump maintenance, under ideal circumstances, would be confined to parts subject to normal running water, i.e., bearing surfaces, stuffing box packing, and shaft sleeves. Under adverse conditions, however, metal may be lost from the wetted surfaces of a pump by erosive or corrosive action of the pumped fluid, and maintenance costs can easily attain enormous proportions. The following definitions are those most generally used for the phenomena encountered. Erosion is a general term meaning mechanical removal of material from a surface. As applied to pumps, it may be the result of simple abrasion, such as that produced by suspended solid matter in the liquid being pumped. In common with other hy-

Jan 1, 1957

By H. N. Dunning

A comprehensive production research program, now in progress at the Petroleum Experiment Station of the Bureau of Mines at Bartlesville, Okla., includes studies of the displacement of petroleum from sand by detergent solutions. An earlier report (12)2/ presented the results of an extensive research program to determine the value of detergents as floodwater additives. This report presents later results of the detergent-testing program (13, 17). Although water-flooding methods and controls are constantly being improved to increase the production of oil from secondary-recovery operations, considerable crude oil commonly remains.in place after a water flood has been terminated. Therefore, the possibility of improving the efficiency of a waterflood by the use of detergents is of increasing interest. The effects of many substances on the efficiency of water flooding have been investigated in laboratory studies (5, 11, 13, 17, 19, 24). Of the various sub-stances tested, only surface-active agents were consistently effective in removing oil from sand. Results of laboratory studies presented in earlier reports (9, 11, 12, 13) show that many detergent solutions effectively displace petroleum from sand surfaces under varying conditions encountered in centrifuging, manual and mechanical agitation, ultrasonic vibration, and imbibition.

Jan 1, 1957

By W. Dan Walker

In recent years the Federal Bureau of Mines tested and approved four new types of self-contained breathing apparatus and a facepiece designed for use with the McCaa 2-hour self-contained oxygen breathing apparatus. The Bureau also developed and perfected a battery-powered lifeline telephone for use in mine rescue and recovery operations. Some of this equipment is described in Bureau of Mines Information Circular 7413.4/ This publication is a revision of information Circular 7413 and presents pertinent information on more recently developed mine rescue equipment. The breathing apparatus described herein are 1/2- and 3/4-hour sell-contained types of much simpler design than the conventional 2-hour self-contained oxygen breathing apparatus ordinarily used by mine rescue crews; however, it is just as important to select rescue crews carefully and to train them properly in the use, care, and limitations of the newer types of apparatus as well as the older, established types, if the newer types are to be used safely. The Bureau of Mines recommends that 1/2- and 3/4-hour self-contained breathing apparatus be used only as auxiliary equipment in mine rescue and recovery work and that the capabilities and limitations of the apparatus should be well understood by those who wear the equipment.

Jan 1, 1957

By J. B. Rosenbaum

This report presents new findings and consolidates previously published data to provide a single reference containing a concise and comprehensive description of the Bureau's work on electrolytic chromium. Two separate systems for electrolytic-chromium recovery were developed, one designated as the oxidized system the other as the reduced system. The electrowinning of chromium metal follows the dissolution of chromium from the ore or from ferrochrome and its separation from gangue and metallic impurities. Chromite was first solubilized by pressure digestion at slightly elevated temperatures in an oxidized acid solution using Na2Cr2O7 as an oxidizing agent. Later it was found that a sodium-free electrolyte was preferable, using return-cell anolyte containing H2SO4 and Cr03 as the oxidizing agent. Gangue materials were separated from the soluble metallics by filtration; and, after the Cr+3 had been stabilized, the metallic impurities were separated as crystalline ammonium salts by vacuum crystallization.

Jan 1, 1957

By F. L. Wideman

This paper lists resources of sulfur in Wyoming, Colorado, Utah, New Mexico, and Arizons, an area comprising approximately 522,600 square miles, Sources of sulfur occuring within the region are sulfur are, pyrite and pyritic ores, and natural gases and petroleum. Data concerning these sources are presented on a statewide basis. Some of the known deposits of sulfur ore are surficial and of fumerole origin; other deposits have resulted from oxidation of pyrite or sulfide ores of copper, lead, and zinc. The deposits are small and the sulfur is distributed erratically in them. There is a small production from some of the deposits, and the material produced is used as soil conditioner.

Jan 1, 1957

By Clyde L. Brown

Recent developments in portable communication equipment for use in emergency recovery work following mine fires and explosions have wade possible a convenient and dependable means of directing rescue teams working under hazardous conditions. INTRODUCTION Mine rescue and recovery operations following; fires and explosions are frequently conducted under adverse conditions that require the use of oxygen breathing apparatus by members of a 5- or 6-man team. Conventional apparatus used for this purpose for many years was equipped with an oxygen supply adequate for at least 2 hours. The design of the apparatus is such that the nose passages are closed with a clamp, and breathing is accomplished through a mouthpiece connected to the apparatus by tubes and arranged to prevent inhaling air or gases from outside sources. The use of the mouthpiece has presented difficulties in the development of telephone communication because of the wearer's inability to speak while wearing the mouthpiece. The method of conducting operations of rescue teams requires a person to direct operations at a fresh-air base as close to the rescue team as possible. At least one standby rescue team and 2 or 3 other persons assigned to various tasks are stationed at the fresh-air base. An efficient and reliable means of communication between the director of operations and the rescue team is necessary for reasonably safe and efficient work in hazardous areas.

Jan 1, 1957

By L. J. Kane

While analyzing synthesis gas produced from coal, the Bureau of Mines found that conventional procedures for naphthalene determination were difficult and time consuming. The Bureau developed a rapid and sensitive turbidimetric procedure, which requires only simple instruments and hence can be used in plant-control laboratories. The gas is passed through a saturated aqueous solution of picric acid at 3° to 4° C. whose turbidity is then measured at room temperature. A dispersing agent is added to prevent coagulation of the suspension on warming. Only about 1 mg. (0.015 grain) of naphthalene need be absorbed, and precision and sensitivity are a few ten-thousandths of a grain, or a few hundredths of a grain per 100 cubic feet. The determination can be completed less than 10 minutes after absorption. INTRODUCTION One of the functions of the Branch of Coal Gasification, Bureau of Mines, Morgantown, W. Va., is to develop economical methods for manufacturing, from coal, a mixture of hydrogen and carbon monoxide for producing hydrogen, methane, and other gaseous fuels. This raw gas may contain many impurities, including naphthalene. This impurity is usually determined by first forming naphthalene picrate in a water solution of picric acid, separating the picrate, and titrating the unreacted picric acid or the picrate itself.

Jan 1, 1957

By A. D. K. Laird, C. A. Johnson

Drag coefficients for a cylinder being towed through water at constant velocity and also at constant linear acceleration were measured. Drag coefficients for constant velocity towing showed reasonable agreement with previous results. The drag coefficients found for constant acceleration showed little correlation with either the magnitude of the acceleration or the value of the modulus AD/V2 and tended to be slightly lower than those for constant velocity. INTRODUCTION For the design of offshore structures, wave forces acting on immersed cylinders are of importance. Several investigations have been made of these forces and of how they can be predicted from wave theories. A paper by Crooke' summarizes much of the work already done. More recent research by the Wave Research Laboratory at the University of California, Berkeley, has added much to the body of data collected under ocean wave conditions, but has not found a reliable method of force prediction from basic theories of wave motion. The present investigation is part of a long-range program to collect data with which to test current and future theories and correlations. The immediate objective was to measure drag forces on a circular cylinder subjected to linear accelerations over the range of Reynolds numbers between l04 and 105 where the drag coefficient was a constant for constant velocities. In particular, the effect of constant acceleration from rest and from uniform motion was to be investigated. The effect of acceleration may be evaluated in terms of drag coefficients. A useful resistance coefficient, C, is defined by the equation for total drag force, D, exerted by the fluid on the cylinder. DT =CSp V2/2.........(1) The coefficient C may be plotted as a function of the parameter AD/V2. Here D is the diameter and S is the projected area of the cylinder. The acceleration and velocity are A and V. The mass density of the fluid is p. An alternate drag coefficient, C, corresponds to the total force of the fluid opposing the motion minus the virtual mass force. This drag coefficient, arising from the velocity of the fluid, may be compared with that for the same cylinder in uniform motion. The similarities and differences between this coefficient as calculated for accelerated and for steady motion are of interest in the inverse process of predicting drag forces on cylinders under arbitrary conditions. One serious difficulty in this method is the specification of the virtual mass which depends also on the flow picture about the cylinder.1 EXPERIMENTAL EQUIPMENT The experiment was performed in the combination wave and towing tank at the Engineering Field Station of the University of California. The tank is 200 ft long, 8 ft wide, and 6 ft deep. The tow carriage is externally propelled by a cable, and the velocity of the carriage is maintained essentially constant by means of an am-plidyne. For the purpose of the present investigation, the speed control of the amplidyne was modified by inserting a linear speed control rheostat, which was rotated at a constant speed by a small d-c motor equipped with a slip-clutch. Accelerations which were constant over a reasonable length of time were thus produced. The magnitude of the acceleration depended upon the speed of the d-c motor and the limiting speed of the carriage. Data were obtained for a range of accelerations of 2 to 10 ft/sec,2 and a range of velocities of 2 to 15 ft/sec. An accelerometer (Statham Type C-2-350) with a range of ±2g was attached to the carriage and connected to a Brush analyzer and penmotor. A continuous coil of wire with 10 turns/ft wound around a fixed wooden form extending for a distance of 40 ft along the length of the tank was connected by an electrical contact mounted on the carriage to a Brush analyzer and penmotor, to give the time-position history for each run. The test cylinder was machined from solid aluminum alloy, 17-ST. to a diameter of 1.250 in., and could be

Jan 1, 1957