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Jan 1, 1961

By J. B. Cohen

EARLY investigators1-4 reported that additions of beryllium to silver caused embrittlement. The in-termetallic phases which are now known to exist5,' were not known at the time. Solidification appeared to occur by a simple eutectic reation.4,7 (The primary beryllium-rich phase appeared globular, when the liquidus temperature was near the melting point of pure beryllium, and angular when the liquidus was much lower; in discussion of Sloman's work,4 it was suggested that this difference was due to an intermetallic compound which was not revealed by the polishing technique.) In the investigation reported here, it was found that if the compounds now known to exist were avoided, certain beryllium-silver alloys containing large amounts of the primary beryllium phase possessed sufficient ductility to be cold formed. Alloys containing 14 and 20 at. pct Ag were prepared from vacuum-cast beryllium containing 1.0 to 1.2 pct impurities and silver, 99.99+ pct pure. The elements were melted together by induction in beryllia or alumina crucibles under argon at less than 1 atm pressure. The cooling rate was adjusted by regulating the temperature of the melt and by reducing the power to zero without stopping the water flow in the induction coils, which were in contact with the crucible. Ingots were about 0.75 in. in diam with a grain size of 0.12 to 0.25 in. Microscopic investigation of transverse or longitudinal sections of an ingot cast from a temperature well above its melting point showed that, in general, the compounds did not form, presumably because of rapid cooling; the alloys consisted of beryllium-rich particles in a silver-rich matrix as shown in Fig. 1. A eutectic structure was not observed, probably .due to the low beryllium concentration of the eutectic composition and eutectic divorcement. Within a given grain, the small globules of the primary phase were all oriented in the same direction, as indicated by examination under polarized light; the orientation varied from grain to grain. This suggested that the globules were branches of the same dendrites. If cooling was too slow, a third constituent was observed in the microstructure; because it formed around the primary beryllium-rich globules it was Fig. 1—Ag-Be alloy, 18.6 at. pct Ag, as-cast. Bright field illumination. Etched with an aqueous solution of NH,OH and H2O2. X500. Reduced approximately 21 pct for reproduction. probably the 6 compound. A thin ring around an ingot often contained this constituent. When this compound was present in large quantities, or the silver segregated so that large regions occurred with the beryllium-rich globules in contact, sections from the ingot were brittle. When the compound was initially absent, it was possible to carry out reductions in thickness of 50 pct by cold rolling with only limited edge cracking; failure did not occur until reductions of 80 pct. A typical cross section after cold rolling is shown in Fig. 2. After simple bend tests, microcracks were found; these apparently were difficult to propagate in the two-phase structure, as the specimens continued to behave in a ductile manner after the cracks appeared. Similar cracks would probably be closed during rolling. It is apparent in Fig. 2 however, that the primary beryllium particles undergo extensive plastic deformation. Hardness values of the alloys indicated that some work-hardening occurred during cold working. Fig. 2—Ag-Be alloy, 18.6 at. pct Ag, reduced 83 pct in thickness by cold rolling. Bright field illumination. Etched with an aqueous solution of NH,OH and H2O2. X500. Reduced approximately 21 pct for reproduction.

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

By V. D. Perry

Mineralized breccia pipes, because of their widespread occurrence and close structural relations to some of the world's great ore bodies, are objects of unusual interest for mining engineers and geologists. The literature contains many references to them, but it is questionable whether their genetic significance and economic importance have been sufficiently emphasized. The purpose here is to stress these features, relating them to the field facts, for the particular benefit of younger generations of geologists who, confronted with and sometimes confused by the growing flood of geochemical, geophysical, and other specialized research approaches, may be reassured that mappable field relations remain a foremost guide to a better understanding of ore deposits. A mineralized breccia pipe is a pre-mineral, breccia structure which has controlled the circulation and deposition of subsequently introduced mineralization. It is composed of relatively rotated angular or rounded rock fragments, set in a mineralized matrix. A pipe in plan outline may be circular, oval or approach polygonal form, with a steep to vertical axis proportionately much greater than its horizontal dimensions. The pipe is a steeply plunging, chimneylike mass of brecciated rock cemented with later minerals. Rock breaks in a variety of ways and complete fragmentation often occurs without rotation of individual pieces. A finely broken rock mass may fit into a tight jig-saw pattern, each fragment having mutually concordant boundaries with its neighbors. The result is a stockwork of innumerable reticulating cracks that, once cemented by mineralization, forms a complicated intersecting network of individually insignificant but collectively important seams and veinlets. Stockwork fracturing among its many forms takes the shape of domes of subsidence, fracture pipes, and related peripheral zones around and over breccia columns, or a combination of any of these structures. The significance of the mineralized breccia pipe is that it represents the extreme or climactic expression of a structural type which has a variety of mutations including subsidence domes, fracture pipes, and other stockwork zones all with related ancestry and similar to dissimilar characteristics. These allied and associated structures hold an answer to the fundamental question of the origin of many important ore deposits. CANANEA-TYPE LOCALITY FOR BRECCIA PIPES The Cananea district is characterized by an unusual development of mineralized breccia pipes. It is an important copper producer located in Sonora, Mexico, a short distance southwest of Bisbee, Arizona, and at the southerly limit of the great porphyry copper belt of the southwestern U.S. Cananea's rocks consist of Paleozoic quartzite and limestone capped unconformably by a thick series of volcanics including andesitic flows, tuffs, and agglomerates. These rocks have been intruded by a deep-seated granite with related basic and acid differentiates including dikes and plugs of quartz mon-zonite porphyry. Mineralization coincides with a northwesterly trending belt of these intrusives which break upward into and through the sedimentary-volcanic rock sequence. The district has weakly defined tectonic alignments in a northwesterly direction with subordinate intersecting fracture elements, but lacks important faulting or fissuring to provide throughgoing avenues for the upward circulation of mineralizing fluids. Thus, as will be discussed in subsequent paragraphs, the alternate way in which late magmatic and hydro-thermal derivatives of the parent magma reached the near-surface zone was by excavating their own breccia pipe channelways. There are numerous stages of breccia pipe development, related both in time and space to magmatic activity. A compilation of similarities and differences in various pipes suggests that proximity or remoteness of a demonstrable or inferred magmatic source provides an orderly genetic basis for describing the following representative types. Cananea Duluth Type: There are no intrusive rocks within or close to the Cananea Duluth pipe; therefore, the existence of any deep-seated magma that may have been related to its formation must be inferred. The structure is an oval-shaped ring 1200 x 300 ft in plan dimensions, cutting steeply across low angle, bedded tuffs, and other volcanics; it has been developed by drill holes to a depth of 2000 ft below the surface. The ore follows the periphery of the pipe and is composed of intensely brecciated rock which is cemented by minor galena, sphalerite, chalcopyrite, quartz, carbonates, and adularia. There is a definite vertical zoning of sulfides with less galena, continuing sphalerite, and increasing chalcopyrite at deeper levels. Within the interior of the ore ring, the brecciation becomes progressively weaker and coarser, the whole indicating relatively gentle slumping with broken, thin tuff beds pre-

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. W. Goss, M. J. Coolbaugh

Most grouting has been done to stop water flaw in mines and for stabilizing foundations of various man-made structures, a survey of the U.S. literature reveals. Apparently Sun Manuel is one of the first mines in this country to use grout extensively underground for strengthening and stabilizing ground in drifts, shafts, and stations. A comparison with other procedures as well as details of the Sun Manuel program are covered. The employment of pressure grouting as a ground stabilizer at the San Manuel Copper Corp. mine reduces delays in both development and production, lowers costs, and makes possible safer working conditions. It specifically reduces delays in haulage operations and permits the maintenance of normal ventilation. In development work this grouting allows faster excavation by cementing together highly fractured or broken ground that otherwise would require extensive cribbing or spiling. In drift repair, it consolidates the loose or fractured rock over the timber or steel drift supports, thus decreasing the frequency of repair, lessening the hazards from falling rock, and curtailing delays due to blockage of drifts by muckpiles and repair operations. Pressure grouting is the process of pumping an accurately controlled mixture of cement and water into loose, fractured, or porous rock. The ratio of water to cement varies according to the nature of the rock encountered, from the thinnest mixture of 30 gal of water per sack of cement, used to fill very fine fissures, to very thick grout of 5 gal of water per sack of cement, used to fill large fissures or extensive areas of loose, broken rock. The pumping pressures at San Manuel vary from about 100 to 1000 psi, depending upon the compactness of the rock, while at other mines the pressures sometimes go as high as 5000 psi. In order to grout an area in which ground water is encountered, the pumping pressure of the grout must be increased by an amount equal to the pressure of the ground water. GROUTING IN DEVELOPMENT WORK The areas under development at San Manuel include many sections of loose, highly fractured rock. Prior to the advent of the grouting program, drifts, shafts, and stations in these areas could not be excavated without utilizing extensive support such as cribbing, spiling, and breast boarding. This slowed down the development work and increased the costs considerably over that required for excavating in more competent ground. Now, when a particularly bad area is contacted, the mining is temporarily stopped while the bad portion of drift or shaft is grouted. After the grouting is completed, the excavating is resumed with an approximate decrease of 50 pct in lost time and costs. Grouting in Drifts and Turnouts: The grouting procedures and patterns used in drifts and turnouts are very similar. The standard procedure for grouting such a turnout is shown in Fig. 1. After the ground is supported as well as possible with cribbing or lagging, the gaps between the back lagging and side lagging are plugged with empty cement sacks or additional timber, if necessary. The ground surrounding the proposed turnout is then grouted in two stages. In the first stage, the broken and caved rock is drilled and grouted to a depth of 5 to 10 ft, depending on the depth of the broken rock. This stage forms a grouted seal that allows higher pressures to be used at depths beyond 10 ft without developing excessive leaks at the face. After a grout hole is drilled, a 10-ft long pipe is wedged tightly into it with empty cement sacks. Grout is then pumped into the hole until the pressure reaches 200 to 300 psi, and the pipe is subsequently removed if it hasn't become cemented in. No more than one hole at a time is drilled and grouted because the grout has a tendency to go from one hole into another, plugging up the latter. Five or six holes are usually adequate for the first 10 ft of grouting. Experience has shown bentonite to be a useful admixture to the grout, particularly when it is indicated that the grout is being lost into large fissures or voids. Bentonite increases the plasticity of the grout enabling it to remain in place more easily until it has begun to set. In the second stage, the longer holes are drilled through the previously grouted rock, after which the

Jan 1, 1961

By C. E. Birchenall

DaVIES and Richardson1 have measured composition changes for Mn1-Owith variation in the equilibrium partial pressure of oxygen at 1500°, 1575°, and 1650°C, where 6 is the deviation from the simple stoichiometric ratio. No trend in this relationship with temperature was observed, so these remarks apply to the whole temperature range. The experimental values and their spread are shown by the bounded straight-line segments in the figure. Davies and Richardson assume that the stoichiometric oxide shows Frenkel disorder, given by the equation Mn2+Mn2+ + Mn" [1] where Mn2+ is a normal lattice ion which moves into an interstitial site (Mni2+) leaving a vacancy (Mn,"). The superscript dashes indicate that there is an excess charge on the anions surrounding the vacancy. Schottky disorder, in which a perfect crystal acquires equal numbers of cation and anion (Ov") vacancies according to leads to equations of exactly the same form in the analysis below. In view of the neutron diffraction results of Roth,2 which shows extensive Frenkel disorder in Fe1-o, Eq. [I] seems more appropriate. The deviations from stoichiometric composition, MnO, result from the addition of oxygen according to In effect Davies and Richardson ignore the variation of Mn3+in constructing equilibrium constants. This approximation might not appear to be very serious if the excess positive charges are really free posi- tive holes (P+) and if the intrinsic conductivity is high as a result of the reaction where e- is a conducting electron. However, the calculations of Buessem and Butler3 indicate that the partition functions of the free charges make a large contribution to the equilibrium constant, and this approximation would not be a desirable one. Furthermore, Morin4 shows that the positive holes are probably localized in MnO and therefore are described better by the mass action principle than by a degenerate gas model. Davies and Richardson's considerations require that activity corrections be applied beyond a 6 value of about 0.005. It is proposed to show here that the dissociation pressure curve can be calculated reasonably well over the whole composition range studied without activity corrections by choosing appropriate equilibrium constants for reactions 1 and 2. As stoichiometric composition The mass action constant, Ks, for reaction [I.] and the equilibrium constant, K,, for reaction [2] are given by where the concentrations which do not change significantly have been absorbed into the constants. The brackets denote concentrations. The deviation from stoichometric composition is given by gardless of [Mni2 ]. Substituting Eq. [7] in [6]

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 Benjamin Petkof

Production quarry blasts in three rock types were photographed with a high-speed camera. Analysis of the films showed that step increases sometimes occur in the horizontal velocity of the broken rock. These step velocity increases were observed only in the first foot or so of rock movement. This observation indicates that the gaseous products of the explosion do additional work on the rock after it is crushed and cracked by the initial compressive-stress pulse and the reflected tensile-stress pulse. The observed initial fly-rock velocity is compared with the calculated fly-rock velocity for reflection spalling. A mechanism possibly causing the velocity increases is discussed. INTRODUCTION When a small concentrated charge of explosive is detonated at the bottom of a drill hole near a free surface, two modes of rock failure have been observed; both are associated with the stress pulse generated in the rock by the detonating explosive. The first mode of failure is the crushing and radial tensile cracking associated with the initial passage of the compressive-stress pulse as it propagates outward from the explosion. This type of rock failure is usually confined to the immediate vicinity of the charge hole. The second mode of failure is the tangential and radial tensile cracking associated with the tensile-stress pulse that is reflected from the free surface. This mode of failure is commonly called scabbing or spalling and has been shown to be a primary cause of rock failure in crater formation at one free surface. (3).4

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 J. C. Bokros

At temperatures above 950°F, zirconium which has been strained a critical amount will experience critical recrystalli-zation. The large grain size thus formed can result in a reduction in the fatigue life by a factor of 2 to a factor of 9 at both high and low temperatures. The critical strains for zirconium vary from 15 pct at 900°F to about 2 pct at 1125°F, while those for zircaloy III vary from 15 pct at 1050°F to 5 pct at 1200°F. Zircaloy II ,experiences no critical recrystallization up to 1200°F. ZIRCONIUM has become increasingly important for nuclear applications and is being employed in reactors at temperatures where recrystallization can occur. Recent work' on the fatigue properties of zirconium has shown that coarse-grained structures developed in zirconium during recrystallization have much lower fatigue lives than fine-grained material. The development of these large grain sizes under such conditions is well known to be the result of critical recrystallization.2-4 Briefly, critical recrystallization occurs when a metal is strained a critical amount and annealed in the recrystallization range. The critical strain is defined as that minimum strain necessary to promote nucleation in the time unit and temperature considered. The maximum grain size occurs at the critical strain, since at this strain the fewest stable nuclei per unit volume grow into new grains. Recrystallization is not evident below this; strain since the nucleation rate is vanishingly lolw, and metal strained more than the critical amount has a higher nucleation rate per unit volume which results in a finer grained structure. This paper describes the critical recrystallization observed in reactor-grade zirconium, zircaloy 11, and zircaloy I11 as a function of annealing temperature and temperature of strain. EXPERIMENTAL The zirconium used was hafnium-free, double arc-melted sponge obtained from the Bureau of Mines. The ingots were forged and hot reduced to 0.08 to 0.10-in. sheet and subsequently cold reduced to 0.035-in. sheet with intermediate and final anneals at 1200 OF for 15 min. The zircaloy II and zircaloy III used were 0.035-in. sheets in the annealed condition. Compositions of these materials as tested are given in Table I. To determine the critical strain at a given temperature, tensile specimens having a0.065-in. taper in a 2-in. gage length were machined from the sheets parallel to the rolling direction. The specimens were polished, etched, and examined metallographically to ensure that all of them were strain-free, initially. Tukon indentations were made every half millimeter along the gage length of each specimen. These served as fiducial marks enabling the plastic strain to be measured with a microscope and micrometer stage. The specimens were pulled to failure at a rate of 0.002 in. per min in an Instron tensile-testing machine. Three temperatures were used for straining: room temperature, 500 ºF, and 900 ºF. The 500º and 900 ºF tests were run in an argon atmosphere. Since the rate of work hardening changes with temperature, a different critical strain was obtained for each temperature of strain. Specimens, prepared in the manner described, were annealed in vacuunl at various temperatures ranging from 900" to 1200 F for up to 1000 hr, after which they were examined metallographically. The critical strain and the recrystallized grain size as a function of strain were determined for each specimen. Results for the same temperature and time indicated that the critical strain measured was reproducible to within 5 pct of each other. RESULTS AND DISCUSSION Since increasing the time of anneal increases the probability of the nucleation of a new grain, the critical strain decreases with time at a decreasing

Jan 1, 1961

By P. C. Good

Tungsten metal in fused form and of high purity was prepared by reducing tungstic oxide with redistilled calcium metal in a heavy-walled sealed reactor. Alloys of tungsten with vanadium, molybdenum) chromium, columbium, and tantalum were prepared by coreduction of mixed metal oxides in the same manner. This work was undertaken by the Bureau of Mines to investigate new approaches for preparing tungsten and its alloys in high-purity form. The standard method of producing tungsten metal has been the reduction of tungstic oxides by hydrogen. The resulting metal powder is compacted, sintered, and fabricated by powder metallurgy methods. Long experience in this field has resulted in the development of a technology that (by careful control of the variables such as metal composition, particle size, and sinterng technique) is well adapted to producing wire and the small shapes usually prepared from tungsten metal.

Jan 1, 1961

By Joseph A. DeCarlo

This information circular presents data for 1960 on individual coke plants in the United States. All oven-coke plants in existence, whether active or idle at the close of the year, are listed in this report. With two exceptions, only beehive plants on which reports were submitted to the Bureau of Mines are included. Although the Bureau was unable to obtain reports from these two active plants in 1960, the number of ovens and annual coke capacity are estimates, based on previous reports filed with the Bureau of Mines. Accordingly, there were 73 oven-coke plants in existence at the end of 1960 of which 70 were active. Reports were received on 44 beehive plants of which only 13 were in operation at year end. Oven-coke plants are listed alphabetically by States in table 1 which shows the name and address of the company, location of plant, classification or type of ownership, number and type of ovens, annual coke capacity, and coal-chemical materials produced. The terms "furnace" and "merchant" plants used in this and all other reports of the Bureau of Mines designate the type of ownership. Furnace plants are those owned by iron and steel companies whose main business is production of coke for use in their own blast furnaces. Merchant plants are those associated with chemical companies, gas utilities, as well as those that produce for sale on the open market metallurgical, industrial, and residential-heating grades of coke and coal-chemical materials. The annual coke capacity shown for each plant in this table is based on the minimum coking time necessary to produce coke with qualities suitable for its intended use. Therefore, the annual capacity of a plant may change from year to year, depending on age and condition of ovens, the character and quality of coal carbonized, the grade of coke required, and other factors. For example, annual coke capacity of a coke plant primarily making foundry coke with longer coking cycles would be lower than one making blast-furnace coke. Also some ovens must be operated at slightly lower than normal flue temperature because of the condition of the refractories and maximum capacity would be somewhat lower than designed capacity. For this reason, the capacity reported to the Bureau of Mines may differ from the designed or rated capacity estimated by the coke-oven builders at the time of construction. For example, if the generally accepted standard coking rate of one inch per hour were used on all ovens to calculate total annual capacity, it would have been 80.4 million tons or 2 percent higher than the capacity reported to the Bureau. Because of the factors mentioned above, the annual coke capacity shown in this table is believed to be a reliable measure of the practical operating capacity of the industry.

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