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By Robert N. Morris

Ladies and Gentlemen: It is a distinct pleasure and honor to appear before you representing the railway industry as I do, but there is a much closer personal relationship. I am a graduate Mining Engineer and worked in the coal industry for 15 years prior to becoming a railroader only 4 ½ years ago. I have been a member of AIME most of my adult working life and am currently active in the Washington, D. C. Section. While having been in the railway industry only a short time, I have become involved during the recent period of innovation and development of the new railroad technique known as unit train service. I have had the privilege of helping to work out a number of unit train movements to both electric utility companies and to a major steel concern, handling coal from mines on the Southern Railway to the consuming plants. On Southern, our unit trains are all of what I shall describe as shuttle train operations whereas within the railroad industry today several types of service are characterized as unit train service and many don't offer comparable efficiencies.

Jan 1, 1968

By Thomas E. Green

A solvent extraction procedure using 8-hydroxyquinoline and chloroform was investigated by the Bureau of Mines as a preconcentration technique for the determination of aluminum, calcium, cobalt, copper, iron, lead, magnesium, manganese, nickel, and zinc in large samples of high purity tungsten. X-ray spectrographic and atomic absorption methods were used to determine the trace metals after preconcentration. The presence of 10 grams of tungsten had a pronounced effect on the distribution of 8-hydroxyquinoline between the aqueous and chloroform phases. This change in the 8-hydroxyquinoline distribution in turn had an adverse effect on the extraction of the trace metals. Extraction efficiencies can also be adversely affected by an increase in the quantity of extractable metals present, as shown by radiotracer tests using 65Zn. Excess 8-hydroxyquinoline in the extracts did not interfere with the determination -of the serious interference in the combined ion exchange paper--X-ray spectrographic method. Although preconcentration by 8-hydroxyquinoline extraction was found to be partially successful, other preconcentrationn methods based on ion exchange and dithizone extraction were found to be superior.

Jan 1, 1968

By R. K. Koch

The vapor pressures of liquid columbium and liquid hafnium were deter-mined by the Langmuir free evaporation method as a part of the Bureau of Mines program on the study of transition metals. An electron-beam furnace with a water-cooled copper crucible was used for melting. Temperature was measured with a two-color ratio pyrometer. Least-squares analyses of the vapor pres-sure data gave the following equations: [Logp (atm) = 5 .429 -31,310 T] for liquid columbium in the range 2,740° - 3,140° K, and [Log p (atm) = 5,690 28 T] for liquid zirconium in the range 2,500° -2,810° K. Third-law evaluations of each data set gave mean heats of sublimation (298.15° K) of 175.1±3.2 kcal/mole and 148.3±1.2 kcal/mole for columbium and hafnium, respectively. Second-law standard heats of sublimation determined from sigma plots and from sigma-prime plots agreed fairly well with the third-law values. The sigma-prime plots gave standard entropies of sublimation of 30.96±0.84 eu and 33.S6±0.44 eu for columbium and hafnium, respectively.

Jan 1, 1968

By R. E. Hamilton

It is more than ten years since the first fully automated process using a computer started operation. Computer control has become common in a number of process industries, yet in spite of the tremendous incentives which ere present, there are only a few computer installations in the mining industry and none of these has announced successful control of a process. Recognizing that one of the reasons for this slow progress is the lack of adequate mathematical models of the various processes involved, the author's company started a project in the summer of 1966 to develop such models. It was early recognized that the existence of a major disturbance input, in the form of the mineral composition of the feed prevents most flotation plants from attaining a steady state condition. This makes the custom¬ary method of developing correlations from steady state plant data inapplicable and requires a more fundamental approach.

Jan 1, 1968

By G. R. St. Pierre, L. M. Adelsberg, R. Speiser

The rate of scale fot'~I~ti0n on tantalum held in H20-Hz-Ar gns mixtures at temperatures between 840" and 1250°C is related to gas composition and ternpevature. It is found that water vapor partial pressure determines the oxidation rate at a given temperature and that the oxygen potential as fixed by the water vapor to hydrogen ratio Ins no significant effect on the oxidation rate. The Ta205 scale formed during oxidation is composed of an inner lattice-dijf~ision barrier and an outer layer of- cracked/porous oxide 1 HE oxidation of tantalum at temperatures less than 800°C is characterized by solution of oxygen into the metal,'-' the formation and growth of suboxides into the metal,')2~10-15 and the delayed nucleation of the highest oxide, Above 800°C, Ta205 is found to nucleate rapidly10, 11, 15, 16 except at low oxygen pressures:15 however, there is uncertainty regarding which does not retard the oxidation process. For each gas con~position and temperature investigated, the oxidatioz rate becomes constant after a short adjustment period. It is shozm that a constant oxidation rate nzay pre~?ail even though the tlzickness of the inner lattice-dijjitsion layer of Ta205 is clanging. TFze initial czcrz!ature of the typical 'Paralinear" oxidation curve may result froprz causes other than an increasing thickness of tlze inner protective layer. the detailed mechanisms of the high-temperature oxidation. Peterson, Fassell, and wadsworth17 observed linear oxidation behavior for tantalum in oxygen at temperatures between 600" and 1000°C. They reported that equilibrium adsorption of 0, occurs on a surface prior to the rate-deter mining step of the reaction. Cowgill and stringer1' confirmed the observations of Peterson and his coworkers. They stated that the rate-determining step of the reaction could be either the incorporation of adsorbed oxygen into the anion lattice or the dissociation of 0, at the gas-oxide interface. The relative rates of the two surface reactions were proposed to be dependent upon the reaction temperature and the oxygen pressure. stringerlo subsequently reported that the reaction surface is located somewhere

Jan 1, 1968

By E. A. Gulbransen, A. Pebler

Pressure-composition isotherms have been determinedfor the systems ZrMo2 -H2 between 0" and 900°C at hydrogen pressures between 10-4 and 760 Torr. Tkese studies plus X-ray diffraction analyses of selected compositions show that these intermetallic compounds form a complete series of hydrogen solid solutions within this temperature and pressure range. The partial molar enthalpies and entropies of solution of hydrogen in the three intermetallic compounds were calculated. The solubility of hydrogen in these Laves phases can be related to their free electron concentration. ThE reaction of hydrogen with inter metallic compounds of zirconium with Laves phase-type structure has both theoretical and practical interest. The in-termetallic compounds have structures different from any of the pure metals. In addition the electron to atom ratio of the intermetallics varies appreciably. In the nuclear materials field, these materials are of interest since intermetallic compounds may exist as precipitates in commercial zirconium alloys with transition metals. From studies on the hydrogen reaction, one can establish the stability of the intermetallic compounds relative to the hydrides of the component metals. The intermetallic compounds may also be used as getters for hydrogen and as materials for hydrogen storage. This paper will present the results of equilibrium and structural investigations of the ZrCr2-H2, the ZrV2-H2, and the ZrMo2-H2 systems for the temperature range of 0" to 900°C and the pressure range of Torr to 1 atm. A complete thermochemical analysis will be made of the measurements. Some of the results have been referred to in a survey paper' covering the types of hydrogen behavior observed in zirconium alloys. LITERATURE ZrCr2 is the only intermetallic phase in the Zr-Cr system.' It exists in two allotropic modifications. Between 900" and 1000°C the hexagonal MgZa (C14) structure transforms into the cubic MgCu2 (C15) structure. Beck4 has previously shown that the intermetallic ZrCrz takes up hydrogen into solid solution up to a composition H/ZrCr2 = 1.14 at room temperature and 1 atm hydrogen. A ZrCr2 hydride was stated to have a fcc structure. The binary Zr-V system has been investigated by williams5 although Rostoker and Yamamoto 6 had given earlier a partial phase diagram. ZrV2 was the only intermediate phase found in the system. wallbaum7 reported earlier that the compound ZrV2 hp the MgZm (CJ4) type structure with a = 5.288A and c = 8.664A. This was not comfirmed by Elliot8 nor by Matthias, Compton, and corenzwit9 who reported that ZrV2 has a cubic MgCua LC15) type structure. The latter authors gave a = 7.429A. Also, several authors do not agree on the temperature of the peri-tectic horizontal. It appears that ZrV2 may exist in several modifications. A high capacity for occluding hydrogen was reported by Beck4 who found H/ZrV2 = 1.38 at room temperature and 1 atm of hydrogen. ZrMoz is the only intermetallic phase in the Zr-Mo system.10 ZrMoa is formed by a peritectic reaction of the melt with a molybdenum-rich solid solution. ZrMo2 has the C15-type structure with a = 7.59A. MATERIALS High-purity chromium, vanadium, and molybdenum were used together with grade 1 crystal bar zirconium to prepare the alloys. Table I lists the chemical analysis and the sources for the metals. Ten-gram alloy compacts were levitated and melted in an inert argon

Jan 1, 1968

By Donald L. Brothers

"OUT IN BRITISH COLUMBIA, we have a legendary creature called ""The Sasquatch,"" a large ape-like creature which, according to those who claim to have seen it, somewhat resembles the Abominable Snowman of the Himalayas. Through the years, the legend bas been perpetuated by hunters and prospectors who return from remote wilderness areas with fantastic tales about hairy creatures, twice the height of an average human being, who leave 2-ft-long footprints in the soft forest floor. However, the existence of this creature bas never been proven and the attitude in British Columbia circles is that the whole thing constitutes either a great discovery or a giant hoax, and is about equally unbelievable either way.The Sasquatch, however, is not the only giant in British Columbia. If you find the Sasquatch story un-believable, you'll fi nd it just as hard to believe what is happening in the mining industry out west. We have opened four new mines so far this year (1967), another mine is expected to be brought into production before the end of the year and any mining man will tell you it's just the start of a mining boom which will continue for many years if metal prices are maintained and the federal government sees fit to discard the taxation changes pro-posed in the Carter Royal Commission Report regarding mining."

Jan 1, 1968

By R. C. Himes, K. Zanio, J. B. Wagner, J. W. Moody, J. F. Miller, W. Johnson

The recent research with which this paper deals has been concerned with the preparation of pure PbTe crystals suitable for control of radiative processes and othe.v electronic applications. The research has been directed toward the developrnent of methods for the preparation of puve, homogeneous, loul-ca,wier-density PbTe crystals suitable for use in the fabrication of optically pumped and electrically pumped diode lasers. Steps in the preparation of the crystals include 1) purification of the starting materials, 2) synthesis and purification of the PbTe, 3) growoth of PbTe crystals, and 4) adjustt~zertt of composition of the crystals This Paper describes the general preparation procedure employed and discusses some investigntiotzs of purification processes. THE as-received lead and tellurium are nominally 99.999 to 99.9999 pct pure. Assays furnished by the suppliers, obtained by emission spectrographic analysis, show only the presence of about 2 ppm Mg in the tellurium. Such analyses are not very informative, however, since they give no information on the concentrations of normally gaseous impurity elements such as oxygen. Both the lead and the tellurium in the as-received state usually contain appreciable concentrations of oxygen—primarily in the form of oxides on the surfaces of the material. To reduce the oxygen content, the lead is held in the molten state in hydrogen at -700°C for several hours. For this treatment, the lead is contained in a graphite boat which is rf-heated, and the hydrogen is passed through a liquid-nitrogen trap prior to use. Tellurium is subjected to multiple distillation in hydrogen to remove oxygen and other foreign impurities. If, in conducting the distillation, approximately the last 10 pct of the charge at each "stage" is left as the discard cut, purification of the tellurium proceeds as indicated in Fig. 1.l Tellurium used in this work has been distilled two or three times to reduce carrier concentration to about 10" per cu cm. The PbTe is prepared from the purified elements by reacting them in the molten state in sealed, evacuated, or hydrogen-filled silica ampoules. The charge is usually held above the melting point of PbTe (923°C) at 1000 C for 24 hr to ensure that it has been homogenized. Two methods have been employed for the growth of the required single crystals of PbTe: growth from the melt, which will be discussed first, and growth from the vapor phase. Large single crystals of p-type PbTe can be grown readily from the melt by the Bridgman method. For this method of crystal growth, the PbTe is synthesized in situ from proper proportions of the purified elements. Growth (dropping) rates in the range 1.3 to 6.5 mm per hr are employed. Material near the maximum melting composition (about 50.012 at. pct Te) is utilized to avoid composition change on freezing, and thus to obtain crystals of nearly uniform composition. Crystals prepared by use of procedures described up to this point were sufficiently pure and perfect that they could be used for the preparation of laser crystals in studies at Lincoln Laboratory.2-5 ADJUSTMENT OF COMPOSITION Good n-type crystals of PbTe cannot readily be grown from the melt. Further, growth from the melt of crystals of any compositions (n or p type) other than those near the maximum melting composition is difficult because of the large composition changes that must occur on freezing.'" However, melt-grown crystals can rapidly be brought to other desired compositions by isothermal equilibration through the vapor phase with a two-phase Pb-Te stock material, essentially as described by Brebrick and Allgaier.1 The work to be discussed has been concerned with the preparation of n-type crystals; thus, the two-phase stock which was employed contained excess lead, and all ensuing discussion is of the preparation and properties of n-type crystals. The equilibration was designed to the shift composition to the lead-rich limit of stability at the selected temperature. Initial treatment of the crystals at high temperature was employed to minimize the total time required for the equilibration. Final adjustments of the composition and state of the crystals were made by use of low-temperature heat treatment at temperatures in the range 200" to

Jan 1, 1968

By D. Dever, E. S. Fisher

Measurements of the temperature dependence of the elastic moduli in single crystals of hep ruthenium, rhenium, cobalt, dysprosium, and erbium were carried out for various temperature ranges so as to investigate the correlation, suggested by prior work, between the shear anisotropy ratio, A = C44/C66, and the occurrence of the hcp — bee phase transformation. These measurements confirm the suggestion that A has a positive temperature dependence in that group of hcp metals that undergo thermally induced transfornzations to the bee structure and a negative or zero temperature dependence in the other hcp metals. It appears, from indirect evidence, that the hcp -fee transformation in cobalt is preceded by a highly negative temperature dependence of A. These results indicate that elastic anisotropy is an important factor in determining the temperatures at which martensitic phase transformations occur. Two possible roles for elastic anisotropy are proposed: 1) the shear-modulus ratio within the habit planes must be nearly similar for the two phases and 2) a large anisotropy decreases the stress necessary for the movement of the transfornzation dislocations. FUCHS' calculations of the elastic moduli in the alkali metals have shown that the high shear-anisotropy ratios, c/c', in certain bee metals and alloys are the result of large negative contributions to c' = (c11 - c12)/2 arising from the nearest-neighbor repulsive forces.' On this basis, and following Zener,2 the association between high c/c' ratios and the martensitic phase transformations that occur upon cooling certain bee metals is explained as a unique characteristic of the bee structure. Recent measurements of the elastic moduli in hcp titanium and zirconium show, however, that a high elastic anisotropy also exists in these hcp structures at the temperatures at which they transform to bee upon heating3. If there exists a direct and consistent correlation between the elastic anisotropy in close-packed structures and the occurrence of transformations to the bee phases then there is evidently a need to re-examine the conclusions of Zener theory. Elastic anisotropy may also be the result of the effects of temperature on the stability of the low-temperature close-packed structures or it may play an important role in the mech- anism of the martensitic transformations. The present measurements were aimed at establishing the phenomenological correlation between elastic shear anisotropy in hcp structures and the thermally induced hcp —bee transformations that occur in the majority of the twenty-three hcp metals, as shown in Table I. Prior to the present work the temperature dependence of the anisotropy ratio, A = c44/c66, was known at various temperatures for nine of the metals listed. The data showed a negative temperature dependence of A for cadmium, zinc, magnesium, and cobalt, which do not transform to bee, and a positive temperature dependence of A for thallium, zirconium, titanium, hafnium, and yttrium. The correlation was, however, ambiguous in that these two groups of metals are also separated with respect to the c/a ratios as noted in Table I. There remained the possibility that the temperature dependence of A is a function of c/a and not consistently associated with the transformation. The measurements of the elastic moduli in rhenium and ruthenium, in which hcp —bee transformations do not occur, were needed to help decide this question. The studies of dysprosium and erbium were undertaken to determine whether the correlation holds for the heavy rare earth metals.

Jan 1, 1968

By V. Lessels, D. J. Buckwalter, D. H. Rose

A cyanide leaching process developed at Michigan Technological University was tested in a 12 to 24 tpd pilot plant. Flowsheet layout and equipment are described. Cyclic operation of leaching, copper precipitation by acidification, and regeneration of the cyanide leaching solution are discussed. Copper extraction and reagent consumption were as predicted by laboratory tests, and the process was proven to be technically feasible. The White Pine Copper Co., a wholly-owned subsidiary of the Copper Range Co., produces copper in the Upper Peninsula of Michigan. Production in 1965 amounted to 138 million pounds of metal. An expansion program now under way will increase this by approximately one half. The highly mechanized room and pillar mine produces 18,000 tons of ore per day, which is treated in a flotation plant. The concentrate is smelted in a reverberatory furnace, the matte is blown in converters to blister copper, and the blister copper is further refined to a uniformly high-quality Lake copper, which is 100% conductive and has a silver content of 25 to 40 oz per ton. The run of the mine ore averages 22.5 lbs of copper per ton with the ore mineral occurring in the form of chalcocite. The nature of the mineralization is such that the sand tailings average a little over 4 lbs of copper per ton. Intensive research has improved copper recovery in the flotation operation to some extent, but at the scale of present operation about 12,000 tons of sands containing over 48,000 lbs of copper go to the tailings pond daily. When the plant expansion is completed, the loss of copper will be somewhat greater. In 1959, the White Pine Copper CO, initiated a study of the recovery of copper in the sand tailings. Inasmuch as the flotation operation was considered to be optimized, a logical approach seemed to be leaching. For various reasons ammonia, ferric chloride, acid, and biological leaching were ruled out as impracticable. This led to a consideration of cyanide leach-

Jan 1, 1968

By C. B. Kenahan

The Bureau of Mines is developing methods for reclaiming the metal and mineral values contained in municipal incinerator residues. This report describes the first phase of the research, in which reliable methods for sampling and analyzing municipal residues were established and the composition and characteristics of the residues were determined. Samples were obtained from a variety of grate-type furnaces and also from a rotary kiln furnace. The samples were processed on a batch basis and separated into their natural categories by a variety of methods including screening, magnetic separation, air separation techniques, and handpicking. The main components of the residues were determined to be metal and metal oxides, glass, and ash.

Jan 1, 1968

By Daniel R. Shawe

Large tabular beryllium deposits in waterlaid rhyolitic tuff at Spor Mountain, Utah, contain the world's largest known resources of beryllium (as bertrandite). The district also has produced fluorspar and uranium. The largest beryllium deposit is about 2.5 miles long, and known deposits contain many million tons of material with at least 0.5 per cent BeO. The beryllium-bearing tuff (Pliocene?) underlies topaz-bearing rhyolite ( Pliocene?) that contains unusually high amounts of beryllium, fluorine, and uranium, and overlies other volcanic rocks (Pliocene? or Micocene?) and marine carbonate and elastic rocks ( Paleozoic). The deposits occur in hydrothermally altered tuff only where it contains abundant carbonate pebbles eroded from the Paleozoic rocks and where the tuff was deposited as thick layers in now-buried paleovalleys. Basin and Range faults, thrust fa ults, and possibly strike-slip faults formed in this part of the Basin and Range province during the late Tertiary, and volcanic rocks were extruded. Beryllium mineralization probably occurred during this episode. Undoubtedly the beryllium deposits are related genetically to the topaz-bearing rhyolite, but the details of their genesis are not certain and probably are complex. Beryllium deposits are close to major faults, and locally the beryllium is concentrated at faults, indicating fault control of mineralization. Some elements in the deposits, such as lithium, however, are evenly distributed in certain Luff beds and perhaps were introduced prior to faulting. Still other elements, such as manganese and lead, were concentrated in the beryllium deposits and subsequently were leached along late fractures, indicating a period of metal redistribution following mineralization.

Jan 1, 1968

The ore treatment expansion programme at Mount Isa Mines required the erection of a new lead-zinc concentrator to be known as No. 2 Concentrator. This concentrator was designed by Western-Knapp Engineering Company in conjunction with staff of Mount Isa Mines Limited. Metallurgical design followed conventional wet milling practice, but the size of many plant units is larger than previously used at Mount Isa. The. total capacity of the new plant is 150,000 tons per four weekly period, and the plant is designed to operate in two equal parallel sections.Erection was contracted on a turnkey basis, and the plant was commissioned as a production unit on 23rd June 1966.The existing concentrator, No. I, was converted to treat all copper ore, and the total capacity of the two plants is now 390,000 tons per four weekly period.

Jan 1, 1968

By F. E. Brantley

Optimum autoclaving conditions were determined for separation of iron and manganese values from pregnant leach liquor produced in extracting manganese from low-grade umber are. The umber was leached with a synthetic anolyte similar to a recycle solution, used in manganese electrolysis cell operations, that had been renewed with ferrous sulfate and sulfuric acid. The equipment used and results obtained are presented for the several conditions employed. The kinetics of the separation were studied. Rate equations were derived for the formation of solid ammonium-manganese sulfate, (NH4)2 Mn2 (S04)3.

Jan 1, 1968

By A. J. Petrina

"At Craigmont Mines Limited, Merritt, B.C., tests were begun in March, 1965 to evaluate the use of shotcrete as a method of ground support m development headings; previously, ail drifts had. required support, which was accomplished mainly by timber and occasionally by the use of rockbolts. The tests demonstrated conclusively the effectiveness of shotcrete for supporting Craigmont's ground. Gradually, the use of timber for ground support was virtually eliminated in favour of shotcrete. This paper describes the equipment used, the operation of the equipment, pertinent cast data and opera ting details. Also discussed are other uses developed for the shot-creting equipment, the use of reinforcing bar rockbolts, and a method used at Craigmont for lining long vertical ore passes with steel plate and concrete as part of the raising cycle."

Jan 1, 1968

By Sunder S. Saluja

Man had to learn to break rocks as early as the Stone Age, when they formed his main source of raw material. He started with chipping and over the years has reached a stage where he can employ atomic blasts and break, with one blast, millions of tons of rock. In between these two extremes there have been several stages of development including firesetting, use of the expansion of water on freezing in chipped cracks in cold climates, the use of low or deflagrating explosive black powder in about the 17th century, the use of high explosives with the discovery of nitroglycerine in 1846 by Sobrero, followed by the monumental discoveries of the great Swedish scientist Alfred Nobel in the latter half of the nineteenth century. The attempts to develop a stronger and still stronger explosive force were accompanied by investigations to understand the mechanism of failure of rock so that the force could be used to the best advantage; the latter, of course, have lagged far behind the former. This is mainly due to the fact that the chemical reactions involving high explosives as well as the processes resulting in the breakage of rock take place at too great a rate to be studied with the equipment that has been only recently available. Moreover, the development of stronger explosive forces was prompted by military necessities in the past and competition, at present, among highly developed nations. With the development, however, of the new techniques such as micro- second photography, microsecond flash radiography, extremely high-speed movies, strain gage assemblies, electronic chronographs and other improved electronic techniques, the investigator has in the last decade or

Jan 1, 1968

By Rodney L. Stone

As part of an overall laboratory and plant test program to determine mixing and other techniques relating to the more economic use of bentonite as an iron ore pellet binder, a settling test was developed for measuring the bentonite content within a pellet or within a batch of pellets. Between pellet batches, each containing a different level of bentonite, the dry fracture load is directly proportional to the bentonite content between pellets of the same batch, however, the fracture load is inversely proportional to the bentonite level; this is explained by a negative correlation between a pellet's size and its bentonite content and the fact that larger pellets can withstand a higher fracture load than the smaller.

Jan 1, 1968

By Glenn C. Waterman, Scott Hazen

3.1-1. Purpose. Development drilling is directed towards determining the grade, volume, and three-dimensional outline of a mineralized zone previously located by exploration. It is distinguished from exploration or reconnaissance drilling, which has as an objective the discovery of new mineralized areas. A development drilling and bulk sampling program should furnish the following information: 1. Geology of the mineralized zone. 2. Quantitative data on grade and tons of material within pertinent cutoff limits. 3. Physical size and shape of the deposit. Areas underlain by waste as well as ore. 4. Mineralogica1 and metallurgical characteristics of the ore. 5. I1hysical characteristics of the ore. 6. Hulk samples for metallurgical testing and grade check. 7. Data on other factors that could affect mining operations, such as ground water, ground conditions, etc. 3.1-2. Procedures. There are numerous methods and techniques that are used to acquire pertinent data on a potential ore deposit. The total cost and accuracy of a development program depends on significant evaluation of the geology, proper selection of a drilling method, thorough analysis of sample data, and accurate evaluation of all the information. Knowledge of the geology of the mineral deposit is important in planning the development testing program and in evaluating the data obtained from such a program. Exploration work usually provides some significant information on the general size, shape, thickness, grade, and geology of the deposit. In some cases no further data are needed; in many cases geological complexities suggested by the preliminary work require further geological study. Of considerable importance may be the following:

Jan 1, 1968

By B. C. Allen

The solubility of chromium in liquid silver and that of molybdenum and tungsten in liquid tin have been determined by equilibrating Ike Liquid in a crucible of the solule metal. Generally the weight of solute in solulion was delermined both chemically and from crucible weight losses. The resulting weight percent solubilily of chromium in silver as a function of absolule temperature T is given by log w = -6660/T + 4.02 in the range 960° to 1445°C, and that of molybdenlttrl in tin by log w = —5050/T + 1. 79 in the range 1200° to 2200°C. The values appear unaffected by minor changes in solute composition. Calculations aye made of the parlial molar heal and excess entropy of mixing. The estimated solubility of tungsten in tin is 0.001 pct at 2000°C. Evidence is presented that molybdenwm dissolves in tin without compound for mation and that tungsten and tin form W10Sn. RECENT developments in coatings, heat transfer, and brazing require a knowledge of equilibrium solubilities in a variety of systems at elevated temperatures. Of particular interest are solid-liquid interactions in metal systems involving dilute solutions. This investigation was undertaken since little is known about the phase relations or solubility of chromium in liquid silver or of molybdenum and tungsten in liquid tin.1,2 EXPERIMENTAL WORK As indicated in Table I, high-purity metals or those of known impurity levels were used. Crucibles were machined from chromium, molybdenum, and tungsten bar stock 1.3 cm diam and 2.2 cm long. Chromium rod was prepared by arc melting and extruding iodide process crystals.3 The five chromium impurity alloys were in the form of 0.6-cm-diam swaged rod. A Cr-0.06N* alloy was prepared by exposure to NH3 at 1150°C in a closed quartz capsule for 24 hr. Because significant nitrogen was lost during annealing in argon at 1600°C,4 the estimated level was 0.01 pct N. Chromium and Mo,W crucibles were outgassed at 1200" and 1600°C, respectively, at 3 X 10-5 mm. The solvent was placed In crucibles of the solute metal- 6 g Ag in chromium, 0.4 g Ag in the five chromium impurity alloys, and 4 g Sn in Mo,W crucibles. The silver and tin series were outgassed at 900" and 110O°C, respectively, and held at the desired solution temperature in a tantalum resistance furnace under 1.05 atm 99.995 pct Ar. An equilibration time of 0.5 to 1 hr was chosen since 0.3-, I-, and 4-hr anneals at 1235°C for Cr-Ag yielded similar results. Temperatures were measured optically to +10°C under essentially black body conditions which were checked against the melting point of silver. The Cr-Ag and Mo-Sn,W-Sn series were respectively equilibrated at 990° to 1400°C and 1200" to 2000°C. Vaporization losses were generally held to <1 pct by the argon. In the 1800" and 2000°C anneals for 0.5 hr, the crucibles were placed in tightly sealed tantalum cans which kept tin losses to <5 pct. After the anneals, the specimens were furnace-cooled. One anneal was made on small Mo-0.02 C, Mo-0.5Ti-0.lZr, and tungsten crucibles containing tin at 2200°C. The metals were sealed in an electron-beam-welded tantalum can of minimum volume. After the anneal, tin was still present in each crucible, none of which was severely attacked. After equilibration, the saturated solvent metal was selectively removed from the crucible by acid leaching. Weight losses sustained by the crucibles were determined from the initial weight minus the final blank-corrected weight after acid leaching. Chemical analyses were performed on some of the samples. Hot 1:l HNO3-H2O removed silver from chromium with the blank running <0.1 mg or <0.002 pct on measured solubility. Tin was removed from molybdenum and tungsten by hot concentrated HC1 with the respective blanks amounting to -0.004 and -0.0004 pct in the presence of tin. The insoluble residues were weighed and checked for composition. The leaching solutions contained traces of the solute metals which were analyzed by colorimetric methods, Diphenyl Carbazide for chromium, Thiocyanate for molybdenum, and Dithiol for tungsten. The total of the two percentages found from the residue and leaching solution minus the blank gave the desired solubility values. On the basis of annealing empty molybdenum and tungsten crucibles, weight losses due to MoO3 or WO3 volatilization were found to be generally 10.4 mg and affect measured solubilities by <0.01pct. RESULTS AND DISCUSSION Chromium-Silver . Since no intermediate compounds are reported to form in the Cr-An system,&apos; crucible weight losses and chemical analysis of the entire melt should provide reliable measures of the chromium in solution. Values obtained by the two methods are in agreement as shown by the results for unalloyed chromium in Table II and plotted in Fig. 1. Furthermore, the results are consistent with those previously determined by melting equilibrated silver out of the crucible and analyzing calorimetrically for chromium.&apos; On the basis of limited thermal analysis data, the solubility of chromium in silver has been quoted as 8 pct at the monotectic temperature of -1445°C.1 This investigation indicates an extrapolated solubility of 1.38 pct which is believed to be more reliable. At the eu-

Jan 1, 1968

By J. C. Nigro

The potential use of prereduced pellets in the burden of the blast furnace continues to be a topic of interest. Several excellent papers have been written describing the theoretical and experimental rewards. (1) (2) (3) (4) (5) (6) (7) (8) (9) Significant increases in iron output and substantial savings in coke consumption are major advantages over conventional iron oxide pellets. The savings are especially important in areas where good coking coal is at a premium. Lower handling and transportation costs may also be factors favoring prereduction. When considering the overall cost of making and smelting prereduced materials the optimum metallization level becomes significant. An analysis by Agarwal and Pratt of the thermodynamic aspects of blast furnace operation with all prereduced pellets shows that the criteria controlling coke consumption depends upon the degree of reduction and upon the percentage of oxygen (present as FeO) removed by solution loss.(8) The authors state that although the chances of obtaining large fuel savings are greatly improved when metallization is high, reduction to the highest degree, which is costly, may not result in the lowest energy requirement per ton of hot metal; thus, over reduction could possibly result in wasted energy in the blast furnace.

Jan 1, 1968