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Discussion of the paper of S. E. Bretherton, presented at the Butte meeting, August, 1913, and printed in Bulletin No. 80, August, 1913, pp. 1481 to 1487. S. E., BRETHERTON, San Francisco, Cal.:-Since preparing my paper, our chemist, F. L. Wilson, has been experimenting with Leadville, Colo., oxidized zinc ore and Leadville zinc sulphides containing lead, operating upon 40-1b. lots at a time. His results on Leadville sulphides are as follows: The raw ore contained a trace of gold, 5.04 oz. of silver, 19.1 per cent of zinc, and 7.24 per cent of lead. After roasting the ore contained a trace of gold, 5.72 oz. of silver, 0.75 per cent of copper, 21.7 per cent of zinc, and 8.29 per cent of lead. The loss in weight by leaching was 38.8 per cent. The extraction was 42.8 per cent of the copper, 80.6 per cent of the zinc, 7.1 per cent of the lead, 0.64 per cent of the silver, and no gold. The little .silver that is extracted would be thrown down with the copper when precipitating it from the zinc and both thrown hack into the residue to be smelted. There would be no trouble in smelting the residue with nearly all the sulphur eliminated and containing less than 7 per cent. of zinc. On zinc carbonates containing silicates the results are not satisfactory. H. O. HOFMAN, Boston, Mass. (communication to the Secretary*) :¬The paper by Mr. Bretherton upon the application of ammonia and carbonic acid to the recovery of zinc as oxide from roasted sulphide ore is of interest to me, as the first installation of the Schnabel process for the extraction of zinc from a mixture of zinc oxide, lead oxide (with some cupric oxide), and pellets of enriched lead, produced in steaming liquated zinc-silver-lead crust of the Parkes process, was made at Lautenthal, Harz mountains, where I was chemist. In that capacity I carried out numerous experiments on the Schnabel process, was active in the erecting of the plant, and later had charge of it. After the Lautenthal plant had been in operation for some time a similar one was built at Hoboken-les-Anvers, but both have been abandoned, as the wet process could not compete with the distillation of the liquated zinc-silver-lead crust, now used universally in the Parkes process.

Jan 11, 1913

By Clifford Wilson

SCREENED pipe is designed with the view of restraining the fine, free-running sands of the production zone from entering oil wells. Its successful use is dependent on a number of factors. The nature and effects of some of these factors can be determined through experiment and observation, but some of the elements that have a distinct bearing on the use of screened pipe can be evaluated only by estimate. The important subsurface conditions which affect the use of screened pipe are: 1. Depth of production zone. 2. Extent of production zone. 3. Reservoir pressure. 4. Character and relative quantity of oil and gas. 5. Character of sediments a. Consolidation of beds. b. Variation in beds. c. Grain-size gradation of sands. d. Free-running characteristics of sand from different levels. Aside from the use. of mechanical equipment and tools, the measures to be taken in the installation of screened pipe involve: 1. Size of liner. 2. Length of liner. 3. Design and mesh of screen. 4. Portion of liner to be screened. 5. Manner of setting liner. 6. Preparation of or washing of the well before or during the setting of the screen. 7. Manner of bringing in the well. 8. Manner of flowing the well. Values applicable to the actual subsurface conditions that exist at any well can only be approximated. The accuracy of the estimate will be measured by the amount and quality of the evidence at hand and the personal factor of ability to interpret the evidence fairly, whether

Jan 1, 1932

By C. Norman Cochran, James L. Brandt

ALTHOUGH gas in aluminum and its effect on aluminum products have been the subject of a number of papers, not many quantitative determinations of the hydrogen content of solid aluminum and its alloys have been recorded in the literature. For solid aluminum samples, four investigators have reported hydrogen contents which appear reasonable compared with the hydrogen solubility of 0.7 ml per 100 g, STP, in molten aluminum at 660°C established by Ransley and Neufeld' and verified by Opie and Grant' and Ransley and Talbot. Sloman," who used a vacuum fusion procedure, reported the hydrogen content of some high purity aluminum as 0.66 ml per 100 g, STP. Griffith and Mallett, employing the tin fusion method, reported the internal hydrogen content of six different aluminum alloys as ranging from less than 0.1 ml per 100 g, STP, for 1100 alloy to 0.7 ml per 100 g, STP, for 4043 alloy (previously 43S, a 5 pct Si alloy). Eborall and Ransley," using a solid extraction of the gases at 600°C, reported hydrogen contents ranging from 0.1 ml per 100 g, STP, to 1 ml per 100 g, STP. Ransley and Talbot reported that several thousand analyses on 99.2 pct and higher purity aluminum as well as Duralumin type alloys indicated hydrogen contents ranging from 0.1 ml per 100 g, STP, to 0.5 ml per 100 g, STP.

Jan 1, 1957

By J. K. Brooke, F. A. Renninger

During 1966, crushed stone production in the United States totaled just over 811 million tons valued at almost $1.2 billion. This represented in- creases of 4 % in tonnage and 5 % in value over that for 1965. Excluding the crushed stone used for agricultural and certain industrial purposes (cement, lime and flux), crushed stone mineral aggregate production totaled 616.3 million tons valued at almost $910 million, also up roughly 4% in tonnage and 5% in value over the 1965 figures. Limestone was by far the most widely used rock variety, followed by basalt, granite and sandstone in that order. Concrete aggregate and roadstone continued as the main uses for stone, accounting for 63% of all tonnage produced in 1966 and 60% of total stone value. Sand and gravel production in 1966 increased 3% over that for 1965. Total 1966 output was just in excess of 934 million tons valued at almost $985 million as compared with 908 million tons at $957 million for the previous year. Excluding the higher valued industrial sands, 903.2 million tons of sand and gravel valued at $891.6 million were used directly as mineral aggregates, representing a 2.9% increase in tonnage and a 2.4% increase in value over 1965.

Jan 2, 1968

By S. E. Bronisz, Dana L. Douglass

a Uranium was deformed by cold rolling, and the effects of this plustic deformation on the microstruc-ture of the metal were observed by the technique of transmission elecbon microscopy. The recrystalli-zation of selected cold-wmked samples was also studied by this method. The samples were prepared for examination by electrolytic thinning in a standard metallographic electrolyte which has not been previously reported as being used in producing thin foils of uranium. The microstructural changes observed in the a uranium were generally similar to those seen by optical microscopy. The changes in the microstructure of a uranium following cold work and recrystallization treatments have been the subjects of several studies employing optical and X-ray techniques.12-19 These studies indicated that twinning was the redominant mode of deformation at room temperature20 and that the regions of high energy associated with the deformation twins were preferred sites for the initiation of recrystallization.15,18, Recently several workers have prepared thin foils of uranium suitable for examination by transmission electron microscopy.'-lo The foils thus prepared have been used to study fission fragment damage; a particular dislocation reaction,' and gas precipitation." At this laboratory the microstructural changes occurring during the cold working and recrystallizing of a uranium samples have been studied by using transmission electron-microscopy techniques. The foils used in this work were electrolytically thinned in a polishing bath not reported previously in the literature as being used for this purpose. EXPERIMENTAL PROCEDURE The uranium used in this investigation was depleted a uranium sheet 4 mils thick. The results of a spectrochemical analysis of this material are shown in Table I. The as-received uranium was cut into strips, 1 in. wide by 5 in. long, and annealed in vacuo at 600°C for 2-1/2 hr. The resulting microstructure consisted of relatively uniform, equiaxed grains having diameters of 10 to 50 p. Cold Working. The cold-worked samples were prepared by rolling several of the annealed uranium strips to various thicknesses. The strips were reduced 3.5 ± 0.5, 6.0 ± 0.6, 10.0 ± 0.5, 19.5 ± 1.0, and 28.5 ± 2.0 pct in thickness. It was not possible to achieve these reductions with a single pass through the rolling mill, so the strips were turned end for end during the rolling procedure. The cold-rolled strips were stored in dry ice until samples from them could be thinned and examined (within 24 hr after rolling). Annealing. The samples used in studying the re-crystallization behavior of a uranium were obtained by annealing sections of the strips which had been reduced 10.0 and 28.5 pct. These samples were sealed in evacuated Pyrex capsules and were annealed in a tube furnace at temperatures from 200" to 600°C and for times from 1/2 to 2 hr, see Table l. Thinning: The samples from the rolling and heat treatments were prepared for examination in the electron microscope by electropolishing in a bath composed of 25 g chromic acid, 133 ml glacial acetic acid, and 25 ml water. This electrolyte has been used and recommended for preparing specimens for optical metallography It was necessary to mask the edges of the sample with a stop-off paint in order to prevent preferential attack in these areas. The paint used was made by dissolving polystyrene in benzene. The electrolytic cell consisted of a cylindrical stainless-steel cathode placed in a beaker containing the electrolyte, with the sample as the anode positioned at the cell axis. The temperature of the electrolyte was held below 15°C by cooling with liquid

Jan 1, 1963

By J. A. Snyder, W. L. Finlay

SEVERAL notable studies of the effects of sub- stitutional solutes have been reported. Outstanding among these for its elucidation of general principles, is the summarized work of Hume-Rothery and coworkers.1 For a systematic study of the effects of substitutional solutes on the mechanical properties of the solvent lattice, the work of Brick, Martin, and Angier² on copper; of Frye and coworkers³,4,5 on copper and silver; and of Lacy and Gensamer6 and of Austin7 on iron may be mentioned. Titanium is one of the few elements offering the possibility of a similar study of interstitial solutes since, unlike most metallic elements, it exhibits extended solid solubility for most of the interstitial solutes—hydrogen, boron, nitrogen, oxygen, and carbon. This paper reports a survey of the effects of dilute solutions of nitrogen, oxygen, and carbon on the mechanical properties of high-purity alpha titanium. Previous Work: Van Arkel and De Boer showed" that high purity titanium was quite ductile and De Boer, Burgers and Fast established".' that not only were oxygen and nitrogen very soluble in solid titanium but that, long before the limit of solid solubility of either had been reached, these interstitial solutes rendered the metal brittle. Their electrical resistance data as a function of

Jan 1, 1951

By J. B. Newsom

SAFER, cheaper, and faster sinking of mine openings seems to have been realized with the completion of a borehole 5 ½ ft. in diameter and 1208 ft. deep, in Minnesota, during 1938. Moreover, as the opening is to be used solely for ventilation, its circular cross section, smooth walls and freedom from fire hazard recommend it in comparison with the usual timbered shafts of rectilinear cross section. It should be pointed out that a drill hole sunk without the use of explosives frequently will stand open without support, whereas a shaft sunk by standard procedure using dynamite usually must be timbered because of the wall-shattering effect of explosives. The saving in maintenance resulting from the elimination of timber is obvious. The work was done by Pickands Mather & Co. at its Zenith mine, Ely, Minn. This company wanted a ventilation opening capable of delivering 50,000 cu. ft. of air per minute to the fourteenth level, 1200 ft. below the surface. While several general articles1-3 have described the method used, detailed time and performance records have not been presented before. Moreover, with a method as new as this, it is important to compare the results attained under widely varying conditions. Among the new conditions faced at Ely were some extremely hard rock, a series of vertical fractures, seepage water, and some long stretches of sound rock which, combined with excellent equipment, gave a chance to operate without unusual delays. Developments in boring large holes have generally taken the obvious course of increasing the size of the equipment, a line of attack that has resulted in putting down 3-ft. diameter holes at damsites for studying the foundations4 and in drilling ventilation openings between levels at Butte. 5 Such drills operate from the collar of the hole, and the power from the drill is transmitted to the cutting tool through drill rods or pipes. In order to keep down the volume of rock that must be ground to sludge, the cores in large-diameter drilling are made as large in diameter as possible. Their large diameter increases their weight per foot of length, which

Jan 1, 1939

By Y. C. Liu, H. Margolin

Investigation of martensite habit plane in water-quenched Ti-Mn alloys was carried out in the range of manganese contents between 4.35 and 5.25 pct. On the basis of 22 measurements, the poles were observed to fall into two groups, indicating the existence of two habit planes. The Miller indices of the poles close to these two groups were found to be <334>ß and <344>ß. TITANIUM has an allotropic transformation at 882.1° ± 0.5C1 by which the high temperature ß (body-centered cubic) phase changes to a (hexagonal close-packed) phase. It is well known, as in the case of low carbon steel, that the unalloyed high temperature ß phase cannot be retained no matter how rapid the cooling rate. However, the addition of alloying elements usually lowers the transformation temperature continuously and stabilizes the ß phase to a temperature much lower than the allotropic transformation temperature in pure titanium. A typical example of this behavior is found with manganese-alloying of titanium. Fig. 1 shows the titanium-rich Ti-Mn equilibrium diagram as established by Battelle Memorial Institute.&apos; The addition of manganese lowers the ß transus line and the eutectoid reaction takes place at 550°C, the eutectoid composition being 20 wt pct Mn. However, upon quenching to room temperature from the ß field, the ß phase can be completely retained with much less manganese, see Fig. 2. If the composition is less than that required to stabilize the ß phase completely, a plate-like structure, similar to that of martensite in other alloy systems, appears as shown in Fig. 3. Much lower alloying content merely intensifies the amounts of these transformed structures, as shown in Fig. 4. This paper presents the results of an investigation of the habit plane of these martensitic structures in Ti-Mn alloys. Experimental Procedure Investigation of the pole of a given platelet was made using the two-surface method of analysis." In order that a given martensite trace on two surfaces be readily recognized both at low and high magnifications, it is desirable that only a small amount of martensite be present. From a review of the data obtained at Battelle Memorial Institute4 on quench hardening in Ti-Mn alloys and the results of Duwez" on transformation in Ti-MO alloys, it was decided that the most appropriate Ti-Mn composition for this study would be about 6 pct Mn. A group of alloys containing from 3 to 10 pct Mn was made to bracket this composition. The choice of the 6 pct alloy was apparently proper, since it was later learned that approximately 5.5 to 6 pct Mn is required to stabilize the ß phase on water quenching.

Jan 1, 1954

By John A. Meech, J. G. Paterson

Activated carbon is a strong adsorbent for amyl xanthate, capable of removing from solution up to a quarter of its own weight in xanthate. In selective flotation system where depression is unstable, separation efficiency increases with activated carbon additions. The improvements observed are brought about by two mechanisms. First, by removing stripped and residual collector ions from solution, competition between depressant and xanthate is reduced and depression is stabilized. In addition, the texture of the froth phase at high pine oil concentrations is modified by activated carbon such that better drainage between the air bubbles takes place, alleviating the mechanical entrapment of depressed mineral particles. In treating a bulk copper/lead concentrate produced from GECO ore, selectively between galena and chalcopyrite is increased when activated carbon is used. Although the rate of flotation of galena is marginally lowered by activated carbon, a small extension in the duration of flotation allows the lead recovery to increase by 19% at the same recovery of copper. An addition rate of 0.75 kg/ton (1.5 lb/st) of bulk concentrate is suggested as optimum from this testwork. However, the actual level used in the mill is dependent upon the residual concentrations of collector and frother in the bulk concentrate pulp.

Jan 1, 1979

By Gary E. Parish

TABLE OF CONTENTS Contents I. Introduction II. Purpose of the Paper III. Historical Perspective A. Existing Sources B. New Sources (NSPS) C. Hazardous Pollutants (NESHAPS) D. Enforcement/Judicial Review 1. Title I Enforcement 2. Title III Enforcement 3. Information Gathering E. Summary IV. The Clean Air Act Amendments of 1977 (1977 Act) A. SIP-Related Provisions 1. Section 107(d) - Geographic Boundaries 2. Section 108 - Air Quality Criteria 3. Section 109 – NAAQS 4. Section 110 – SIPs 5. Section 122 and Sections 402 and 403 of P.L 95-95 – Unregulated Pollutants 6. Emission Offsets – Interpretive Ruling (I.R.) B. PSD Provisions - Part C. 1. Regulations Under the 1970 Act 2. The 1977 Act 3. Regulations Under the 1977 Act C. Visibility Protection - Part C, Subpart 2 D. Non-Attainment Provisions - Part D E. Monitoring and Modeling F. NSPS G. NESHAPS H. Enforcement/Judicial Review 1. Title I 2. Economic Enforcement 3. Title III Enforcement/Judicial Review (a) Section 304 (b) Section 307 4. Summary V. Special Problems and Opportunities for the Uranium Industry A. End Use B. Transportation C. Milling/Processing D. Extraction E. Exploration/Discovery F. General VI. Conclusions Appendix A Footnotes

Jan 1, 1979

By Thomas J. Crocker, Galen G. Waddell, Eugene H. Skinner

This paper describes a method of measuring initial and long-term deformations which occur in the medium surrounding mine accessways, and discusses the importance of this type of measurement in assessing support-problem areas. Delineated are (1) description of the rock-deformation monitoring equipment, (2) results of two field tests which monitored rock deformation around 4-foot-diameter raise bores, and (3) a numerical-analysis (finite-element) technique to correlate theoretical with experimental results. Instrumentation developed provided the sensitivity and resolution needed to measure rock deformation around a full-scale raise bore during excavation. Results of the tests conducted at the Lucky Friday mine, Mullan, Idaho, show the relationships between (a) de- formation vs. time, and (b) deformation vs. bit progress. Based on theoretical evaluation of the initial deformation, the medium appeared to behave elastically. Using an estimated field stress of 5,500 psi and Poisson&apos;s ratio of 0.20, the gross modulus of elasticity of the rock was calculated to range from 3.15 to 6.0 x 106 psi (with one outlier which was determined to be >12 x l06 psi).

Jan 1, 1971

By J. A. Church

I. Early Furnaces,......423 11. Experiments with the HIgh-Shaft FURnace,..... 426 III. ExperMents wIth the Wide FURnace,..429 IV. ExperEentS with Extreme BOSH,... 43.2 V. Survival of the 56 by 180 IN. Furnace,.434 VI. Recent ExpeEiments,.....436 VII. SUMMary,........438 I. Early Furnaces. Copper blast-furnace construction in America has long recognized a general standard in the rectangular water-jacketed shaft with separate forehearth. The details, however, and especially those relating to shaft dimensions, have had to meet a great variety of conditions, and show no uniformity whatever. Selecting a few of the present day Western plants, we find furnace lengths varying from 12.5 to 87 ft., widths at tuyere level from 42 to 84 in., and heights above tuyeres from 5 ft. 4 in. to 22 ft. 4 in.; and comparing present designs with those of the past, we meet contrasts no less striking. Unlike its transverse section, the length of a furnace has come to depend rather on the size of unit desired than on the requirements of smelting; and if the question of length be ignored, several of the various existing designs can be grouped together on the basis of a common transverse section. This section, having a width at tuyere level of 56 in. and a height above tuyeres of 18 ft., was developed at Great Falls, and the story of its development contains some interesting features. Ground was broken for the Great Falls works in the spring of 1891. About a year later, the concentrator was able to begin operation, followed within the next few months by the Brueckner, reverberatory, and converter departments, and in April, 1893, by the first blast fur-

Jan 1, 1914

By R. C. Dalzell, A. E. Wells

In 1866, Thomas Graham1 called attention to the volume of gases, three times the volume of the sample, evolved from a meteoric iron heated in an evacuated porcelain tube. From that time to this the occurrence and significance of gases in metals have been the subject of investigation by many workers, among whom Sieverts,2 Iwasé3 and 0. W. Ellis4 stand preeminent. Sieverts and Iwasé concerned themselves with the solubility of a number of gases in metals in the liquid and solid states. They determined the absorption coefficients of these gases, and in all cases found a sharp change in solubility at the melting point of the metals. Ellis analyzed the gases evolved by solidifying copper and those occluded by the solidified metal. Lobley and Jepson5 endeavored to determine the effects of hydrogen, carbon monoxide and nitrogen on the porosity of copper that was allowed to solidify in the presence of each gas after 30 min. exposure to it in the

Jan 1, 1930

Discussion of the paper of W. A. Forbes, presented at the New York Meeting, October, 1913, and printed in Bulletin No. 82, October, 1913, pp. 2477 to 2514.. SAMUEL K. VARNES,* Steelton, Pa.:-We have a gas-cleaning plant consisting of a, centrifugal dry dust catcher, and two rain-type wet scrubbing towers, 25 by 60 ft. each, for rough cleaning of blast-furnace gas. This plant was put in early in 1910, with the intention of cleaning gas for use in hot blast stoves and under boilers, and was so used for several months. Soon after it went into service, the blast-furnace men complained that they could not get as high blast temperatures as they had obtained when using dirty gas. It was decided to run a series of careful tests to determine if this were true and to what degree the apparent results might be affected by other conditions. About 60 tests were run, covering a period of five months, and at the end we came to the conclusion that it did not pay us to scrub the gas for stoves and boilers. The tests were all run upon a single stove, no boiler tests being made, but the conclusions of the stove tests being applied to the boilers. The furnace burden was practically the same for all the tests and averaged: Per Cent. Daquari and other hard ores 57 Nodules 13 Raw Mayari ore 25 Mill cinder and scale 5

Jan 12, 1913

By L. R. Weisberg, E. A. Miller

Single-crystalline films of silicon of good quality were vacuum-deposited on sapphire. The improved crystallinity was achieved by the strict exclusion of oxygen from the evaporation system, including the use of a "oxygen-free" silicon source. To minimize possible contamination of the source, the silicon was sublimed from the solid at about 1390° C. using a simple electron bombardment system to heat the silicon. This resulted in deposition rates of about 5 to 7 µ per hr and film thicknesses of 4 to 20 µ. The vacuum during deposition was ordinarily about 5x 10-8 Torr, DESPITE the success achieved in the chemical vapor deposition of silicon on sapphire using Silane,1-4 vacuum deposition has not provided comparable properties. For example, Chu et a1.5 vacuum-deposited silicon on single-crystalline substrates of A12O3, Sic, ThO2, and other compounds, and, although some epi- but the use of ultrahigh vacuum (about 1 to 3 x10-9 Torr) during deposition did not significantly improve the results in the oxygen-free system. The crystalline quality of films deposited on (0001) sapphire was found to be considerably superior to (1102) sapphire surfaces. Using (0001) sapphire, single-crystalline films were deposited at temperatures as low as 780° C and as high as 1075°C, with the best crystalline quality obtained at about 1000°C. At this temperature, hole mobilities over 250 sq cm per v-sec were achieved. taxy was indicated, single-crystalline films were not produced. More recently, Salama, Tucker, and young6 evaporated silicon on single-crystalline sapphire, but only poor crystallinity was observed, and low carrier mobilities were measured. In the present experiments, good-quality single-crystalline films of silicon on sapphire have been achieved by specifically excluding oxygen from the evaporation. This included not only the use of a "clean" vacuum system but, of special importance, the use of an oxygen-free silicon source. This has also been shown to provide a dramatic improvement in silicon homoepi-taxy.7 As a result, silicon-on-sapphire films with hole mobilities over 250 sq cm per v-set were achieved, and single-crystal films were grown as low as 780°C and as

Jan 1, 1969

By R. C. Schmidt, B. E. Kennedy

The Mont Klahoyo magnetite deposit is located about 600 km (373 miles) northwest of Abidjan, Ivory Coast. During an exploration period ending in 1977 an international joint venture group investigated the deposit and proved reserves of 670 Mt (739 million short tons) grading 36% iron. The deposit occurs at the northeast end of the Baoubly-Kiriao chain of Precambrian iron formations with associated amphibolites, pyroxenites, and gneisses of the Liberian Shield. The ore body is represented by a highly metamorphosed banded quartz-magnetite iron formation with alternating beds of iron silicates and quartz-magnetite. Amphibolite-pyroxenites and sillimanite-cordierite-garnet gneisses form hanging and footwall rocks. The iron formation has been folded into an elongated, overturned 2-shaped major drag fold with axes trending and plunging approximately northeast. Beds are vertical or dip steeply to the southeast. The ore zone has an average thickness of 130 m (427 ft) and outcrops intermittently over a distance of approximately 5.5 km (3.4 miles). Based upon detailed studies of drill cores and the results of ore dressing test work, eight stratigraphic units, identified as K- 1 to K-8, are recognizable in the iron formation. Four interbedded units are low grade silicate zones (silicate facies) while the remaining quartz-magnetite units are oxide facies, representing the important Mont Klahoyo deposit ores. Ore-bearing "K" units are subdivided further into 11 ore types, based upon their specific lithologies, iron content, and concentration characteristics. Identification of these ore types proved particularly useful to mine planning and flowsheet design. A cap of oxidized material overlies the primary quartz- magnetite iron formation, but no enrichment has occurred. It is thought that the Mont Klahoyo iron formations were deposited chemically in a volcanic environment as a siliceous iron formation with volcanism the primary source of iron and silica. Metamorphism converted the siliceous iron formation to a coarse-grained, quartz-magnetite-silicate iron formation.

Jan 1, 1983

By Robert C. Linares

Cubic zinc sulfide has been grown from molten salt solutions substantially below the hexagonal-cubic phase transition of 1020°C. Crystals free of birefringence have been grown from molten lead chloride at temperatures from 500° to 800°C. Factors affecting the optical transmission and the birefringence are discussed. CUBIC zinc sulfide is of interest for electrooptic devices and as an optical coating material. However, it cannot readily be produced as large crystals which are free of birefringence. The birefringence arises from the fact that the cubic ZnS is usually grown as the high-temperature hexagonal phase and is transformed to the lower cubic phase by annealing.&apos; This results in stacking faults, stress, and birefringence. A requirement for the growth of cubic ZnS is that it be grown below the phase transition of 1020°C.2 Crystals of cubic ZnS have been grown below 1020°C by the hydrothermal,3 flux,4 and vapor transport5 techniques. However, these all appear to have limitations in size or quality of material produced. It was felt that a new flux method might have a good chance of overcoming some of the previous problems. Mita6 reported the growth of hexagonal ZnS from molten NaCl and wilke7 reported the growth of iron sulfides from molten lead chloride solution, indicating that molten chlorides make good solvents for sulfides. An investigation of a number of possible molten chlorides as solvents showed that molten PbCl2 has an appreciable solubility for zinc sulfide and that crystals can be grown at temperatures from 500° to 800°C. EXPERIMENTAL Crystal growth was performed in open or sealed Vycor or fused silica tubes, in an argon atmosphere or vacuum. There were no deleterious effects due to using vacuum; however, a sealed essentially isothermal system must be used to prevent vapor transport mechanisms from dominating. This will be discussed later in detail. Noble metal containers were not usable as they were severely attacked by these melts. The materials used were: reagent-grade PbC12, reagent-grade ZnS, optical-coating-grade ZnS, and Irtran 2 (ZnS). Crystal growth was accomplished by both slow cooling techniques and gradient growth techniques. In the slow cooling techniques, 15 g of ZnS and 100 g of PbCl2 were used. The components were placed in the silica tube, heated at 800°C for 2 hr, and then slowly cooled (l° to 10° C per hr) to 500°C. The furnace was constructed so that the tube could be inverted, thus allowing the liquid to drain off the crystals at the end of the run. The gradient runs were made by placing the above mixtures in a silica tube at 550° to 600°c, Fig. 1. A temperature gradient was maintained such that the floating mass of undissolved sulfide was 10° to 50°C warmer than the bottom of the tube. Growth occurred on spontaneously nucleated sites at the cooler bottom. RESULTS When using high cooling rates (5° to 10°C per hr), crystals form in thin sheets perpendicular to the {111} face. Crystals 5 by 5 by 1.2 mm, Fig. 2, have been ob-

Jan 1, 1969

By Nicholas J. Grant, William H. Ferguson, Bill C. Giessen

Ta-lr alloys have been examined over the complete range of compositions using metallographic and X-ray techniques. The terminal solid-solubility limits, solidus temperatures, and intermediate phases were determined. There are four inter-mediate phases: o, tetragonal, analogous to a (Fe-Cr); 0,. orthorhombic; az, tetragonal; and a TaZr,, cubic, AuCu, structure. Of these, o and a, melt peritecticaLly, a, decomposes peritectoidally, and a TaIrs has a congruent melting point. Three peri-tectic and one eutectic reactions occur. 1 HE Ta-Ir phase diagram has not been treated in the literature. Intermetallic phases and terminal solid solubilities have been described and estimated.&apos;-4 The previous findings have been confirmed in this work. A complete diagram with additional phases and solidus curves is presented. EXPERIMENTAL METHODS Starting materials were tantalum powder of 99.8 pct purity, supplied by the National Research Corp., Cambridge, Mass., and iridium powder of 99.9 pct purity, supplied by the Bishop Co., Malvern, Pa. Both powders were -200 mesh. Table I lists the analyses as given by the suppliers. A standard procedure was employed in making the alloy buttons, which was described in detail in Refs. 5 and 6, and which included repeated arc-melting of powder compacts and determination of the composition by the weight-balance method. This is especially justifiable due to the similar vapor pressures of tantalum and iridium. In the critical parts of the diagram, a spacing of 1/2 at. pct was used, based on premelted master alloy material. The observed structures and X-ray spectra were consistent with the composition sequence of the alloys. Table II lists the final alloy atomic percentages with the calculated percent error of composition. Cross sections representative in grain size and composition were selected for the study, as described in Ref. 5. Based on prior experience, no contamination from the tungsten electrode was considered. Temperature measurements were obtained using a Leeds and Northrup optical pyrometer and have been described extensively in Refs. 5 and 6. All heat treatments were made in the high-vacuum tantalum tube furnace mentioned in Ref. 5. Samples annealed in tantalum containers cooled from 1800" to 1000"~ in 5 sec; those annealed in ceramic crucibles cooled over the same range in 15 to 30 sec. The thermal treatments are listed in Table 111. All specimens were homogenized at 1735°C for 24 hr. Tantalum-rich compositions were treated in tantalum buckets. Iridium-rich compositions were annealed in tantalum buckets below the eutectic temperature of 1950°C; up to 2200°C, tungsten-lined tantalum baskets were used; and above 2200°C thoria crucibles were used. It was found that refractory oxides (in early stages of the investigation alumina crucibles were used up to 1800°C and thoria crucibles were used to 2400"~) give off minute amounts of oxygen and thereby influence the microstructure considerably, or react directly with the alloys.

Jan 1, 1963

By R. M. Sellwood

The No. 4 I.S.F. Smelter Complex at the Avonmouth Works of Imperial Smelting Corporation (N.S.C.) Limited commenced operation at the beginning of 1968. The furnace rating is 120,000 tons zinc and 40,000 tons lead per annum. Zinc and lead concentrates are unloaded onto a 1,000 tons per hour capacity conveyor belt and automatically weighed and sampled before receipt into a 48,000 ton capacity raw material store. Distribution is by a reversible boom stacker into 16 x 3,000 ton bays and recovery is by a front end loader. Materials are fed to 16 proportioning bins for feeding via continuous weigh feeders to a 132 square metre effective updraught area sinter machine with a material flow rate of 240 tons per hour over the machine. The required quantity of output lump sinter at up to 800ºC is fed to 2 x 600 ton storage bins on the I.S.F. plant. By-product SO2 rich gas is fed to a conventional wet gas single stream acid plant rated at 600 tons per day utilizing a dry N.T.P. gas volume of 100,000 cubic metres per hour. The hot sinter and preheated coke (800ºC) are automatically neighed and charged to a 27.3m2 shaft area I.S.F. fitted with 2 x 5.5 m. wide lead splash condensers. Grade 4 zinc is tapped and transferred to the zinc refinery. Conventional type lead bullion and slag are tapped from the bottom of the furnace through a separation forehearth. The refinery consists of 6 lead and 3 cadmium columns to produce some 52,000 tons per annum of S.H.G. metal. S.H.G. metal and Grade 4 metal is cast into various shapes as required.

Jan 1, 1970

By H. F. A. Hergt, K. L. Sutherland, J. Rogers

In 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group — SO4- or — SO3- are excellent collectors for cassiterite and promise to be selective. The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000-gram Denver cell. Experimental Methods Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously de- scribed.5,10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these the determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver SUbmachines,—Melboume tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947