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By C. O. Hawk

Distillable oils derived from coal were desulfurized and hydrogenated at 2,500 psig in a two-step vapor-phase catalytic operation to give a product rich in saturated cyclic hydrocarbons. The first step was mainly a desulfurization at 400 C, the second a saturation at 300 C. One of the oils used as feed stock was from low-temperature carbonization of a bituminous coal, the other was from the liquid-phase hydrogenation of coal in the Bureau's pilot plant. The product from the saturation step was distilled to remove the light ends and high-boiling residue and to recover a fraction having acceptable properties with respect to heating value, density, freezing point, viscosity, and boiling range according to specifications suggested by the Air Force for ultra-high-speed aircraft fuel. Quantities of the fuel fraction available were too small for the thermal stability test approved by the Air Force. The experiments, performed on laboratory scale, comprised mostly a study of the effect of varying the oil feed rate (at constant oil-to-hydrogen ratio) on the yield of the desired fuel fraction. The yield of the fuel fraction made from low-temperature carbonization oil was a little more than 1 percent of the weight of coal carbonized; that from coal-hydrogenation oil was about 12 percent of the weight of coal hydrogenated. A few attempts to do both desulfurization and saturation in one operation with sulfur resistant catalysts, developed for vapor-phase hydrogenation or hydroforming, were unsuccessful. By leaving the low-boiling ends in both feed stocks to desulfurization, another product was obtained: a low-sulfur aromatic cut boiling below 200 C. This material would be suitable as a solvent or a chemical raw material.

Jan 1, 1965

By J. G. Donaldson

Cobalt-tungsten binary deposits were formed in laboratory experiments by hydrogen reduction of the anhydrous mixed vapors of cobaltous chloride and tungsten hexachloride. The materials were sublimed in seperately heated zones of reaction tube and were transported in a stream of purified helium into the deposition section of the tube where the chloride gases were reduced to metal by a countercurrent flow of hydrogen. Heattreating of the near stoichiometric binary metallic deposits converted nearly all to the intermetallic compound Co3W, however, small quantities of both cobalt and tungsten remained. Mechanical tests showed that the tensile strength of heat-treated 75 percent cobalt-25 percent tungsten deposits was twice as high as that of similarly treated deposits of cobalt.

Jan 1, 1965

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The room-temperature Knoop hardness of single -crystal titanium diboride has been determined. Variations in microhardness have been correlated with orientation and structural imperfections in the crystals. Maximum differences in hardness values of 750 kg per sq mm with respect to orientation and 450 kg per sq mm with respect to substructure were found. The effects of etchants, load on indenter, and degvee of cracking of indentation were studied. The average hardness was determined as 2800 kg per sq mm on the as-grown crystals. Annealing increased the average hardness to 3375 kg per sq mm. ThE microhardness of polycrystalline titanium diboride approximating the stoichiometric composition TiB, has been studied by several investigators. The values for the Knoop hardness number range from 2710 kg per sq mm (Khn = 2710 kg per sq mm) to 3400 kg per sq mm.'-4 Samsonov et al.' reported a Vickers hardness number of 3400 kg per sq mm (Vhn = 3400 kg per sq mm) at 120-g loads for a 98 pct Ti + B material of 96 pct theoretical density. Recently Dunegan measured the Vickers hardness and obtained 2060 kg per sq mm with a 10-g load (Vhnlo = 2060 kg per sq mm), 1425 kg per sq mm for Vhnloo, and 1320 kg per sq mm for Vhnlooo. We have obtained a Khnloo = 3000 * 350 kg per sq mm for hot-pressed polycrystalline TiB2 that was 99.1 pct Ti + B and 96.6 pct of theoretical density. The present investigation has been made on single-crystal titanium diboride boules, and is believed to be the first such study on TiB, crystals of known orientation. EXPERIMENTAL The single crystals were prepared by a Verneuil-type process using an electric arc by the Linde Division of Union Carbide Corp. The largest specimens were 6 mm in diameter by 12 mm long. The crystals were of theoretical density (4.50 g per cm3) with a Ti + B content of 99.8 pct. The major impurities present were: 0.03 pct (by weight) 0, 0.06 pct C, 0.01 pct Si, 0.05 pct Fe, 0.01 pct Cr, and 0.01 pct Ni. The crystals were boron-rich, the average boron content being 31.S7 wt pct (stoichiometric value is 31.12 wt pct), and titanium-poor, the average titanium content being 68.2 wt pct (stoichiometric value is 68.88 wt pct). Titanium was determined gravimetrically by cupferron precipitation and boron by titration of H3B03 from a NaOH-fused specimen after removal of titanium with BaC03. The outer edge of the boule accounted for some of the excess boron. An electron-microprobe analysis showed that the titanium content increased from 60.0 wt pct at the edge to 68.5 wt pct at D, ~ 1000 p, where D, = distance from outer edge (see Fig. 5). X-ray measurements indicate that the boules are single crystals with considerable substructure. Upon etching this structure is seen in the form of a Widmanstatten-type rhombohedral line pattern in the basal (c) plane and a parallel "lines" pattern in the prism (a) planes. A typical WidmanstHtten-type pattern is seen in in Fig. 1. Electron microscopy reveals that the lines are less than 1 p across, which does not allow direct electron probe or microfocus X-ray determination of their composition. The identity of the second phase has not been established. It might be a higher boride or a nonstoichiometric TiB2. On annealing above 2200°C the precipitate is dispersed and dissolves in the matrix. The best etchants found were HF/HNO/HO, KF(CN)$NOH/HO (Murakami's Etch), and A large number of other etchants were previously Studied. The acidic etchant produced an acicular or "needles" pattern in the (a) planes which is an etchant effect on the "lines" pattern.

Jan 1, 1965

By Wallace W. Key

The California pesticide industry in 1962 consumed about 30,000 tons of clay, talc, limestone, diatomite, sulfur, and other minerals as fillers (carriers and diluents) in pesticide formulation. This was 10 percent of the U.S. filler requirement for pesticides. About two- thirds of the California total was supplied by a few local mineral producers; the remainder came mainly from Florida, Georgia, and Wyoming. The objectives of this report are to provide data on quantities, sources, specifications, and market conditions for minerals used as fillers by California pesticide formulators. The study disclosed that specifications for mineral fillers have become more rigid and formulators have become more numerous in recent years. During 1962 over 1,200 firms registered 16,000 pesticide products with the Bureau of Chemistry in California. Factors which will tend to diminish future need for mineral fillers include the trend toward greater use of organic sprays rather than dusts and further development of biological controls, such as the development of sterile insect strains.

Jan 1, 1965

The Red Lake greenstone belt is an irregular mass of lavas sedimentary rocks and intrusives which is approxiately 35 miles long 18 miles wide and 7 miles deep. Basaltic volcamcs are the oldest rocks w1thm the belt. They are believed to have been laid down on an ancient crust which is at least 3 billion (3 x 109) years old and was composed partly of sediments. The basaltic rocks are overlain by acid volcanics and sedimentary rocks which have been complexly folded and are preserved as a down-folded remnant of younger rocks within the older crust. The volcanics and sedimentary rocks of the greenstone belt have been cut by intrusives with a wide range of composition. The emplacement of the intrusives and the accompanying regional metamorph-ism which terminated the orogenic activity in this area are believed to have occurred approximately 2.4 billion years ago. The basalts and many of the basic and ultrabasic intrusives undoubtedly had their source in the sub-crust or mantle. At least some of the granitic intrusives are believed to have had

Jan 1, 1965

By R. C. Buehl

A pyrometallurgical process for recovering manganese from open-hearth furnace slags or low-grade manganiferous iron ores is described. The slag or ore is smelted in a blast furnace to produce spiegeleisen; the speigeleisen is then blown with air in a basic converter to give an oxide slag. This slag product contains 60 to 75 percent manganous oxide and may be considered a synthetic manganese ore. In the smelting operations coke rates for five test periods ranged from 3,255 to 4,130 lb per ton of spiegeleisen. The recovery of manganese in the spiegeleisen varied from 60 to 76 percent. Recovery increased to 83 percent when the open-hearth slag feed to the blast furnace was diluted with a high-? grade iron ore sinter to facilitate smelting. In blowing the spiegeleisen a cyclic procedure was developed that gave nearly 90 percent recovery of manganese in the slag product (synthetic ore) yet prevented excessive contamination of the slag by phosphorus and iron. The overall recovery of manganese was about 75 percent when iron ore sinter was used with the open-hearth slag in the smelting step. The metal remaining after oxidizing the manganese from the spiegeleisen contained approximately 3.5 percent phosphorus. It was refined in a basic converter by blowing with air in the presence of lime" A high--grade iron and a basic phosphate slag were produced.

Jan 1, 1965

By Richard F. Hewlett

This report describes how a limited number of preliminary exploration drill-hole assays from a mineral deposit can be used to design grid spacing that is both economic and efficient for subsequent evaluation drilling of that deposit. Relationships between desired precision of the estimate of grade of ore and drilling cost are used to determine the economic drill-hole spacing. The statistical concept of precision in estimating grade of ore is used to determine the efficient drill-hole spacing. Assay data from approximately 50 known copper deposits were studied, and the relationships of the statistical parameters of these deposits were computed. Drilling requirements for various precisions of the estimates of grade of ore were computed for some of these known deposits to serve as guides for drilling future copper deposits. The effect of various geologic factors on the trend in grade of ore and, therefore, on the drilling requirements is shown for certain deposits.

Jan 1, 1965

By Thomas A. Morgan

The distribution of stress adjacent to each of 25 mine openings was determined by the borehole stress-relief method in the FMC Corp. Westvaco trona mine at Westvaco, Wyo. The purpose of the stress determinations was twofold: First, to study the effect on these distributions of various factors such as opening shape, stress level, and loading history; and second, to estimate the distribution of stresses adjacent to extensive high-extraction (85 to 100 percent) areas. Stress distributions in areas of low average stress correspond closely to the theoretical distributions based on elastic theory. However, in areas of high average stress, the stress distributions are of a type associated with plastic failure. The stresses adjacent to a mined-out area supported by remnant pillars were significantly higher than the stresses adjacent to another area in which the remnant pillars were removed.

Jan 1, 1965

By R R. Wainwright

Friction-type hoists have been in operation at Geco Mines Limited since Septtember, 1957. At the end of the year 1963, the skip hoist had handled nearly ~ million tons of ore and waste. In March, 1962, with the deepening of the shaft, the hoisting de11th was increased from 1,450 to 2,450 feet. Operating experience with the hoists, hoist and balance ropes, rope treads and other related equipment is presented. The paper is intended to supplement an earlier one -"Heavy-Duty Friction Hoisting at Geco Mines," by W. M. Harvey (C.I.M. Transactions, Volume LXIII, 1960, pp. 193 -197). General G ECO Mine Limited is located at Manitouwadge, Ontario, approximately 160 miles east of Port Arthur and 190 mile northwest of Sault Ste. Marie. The Company was formed to exploit a copper-zinc-silver orebody, with current ore reserve (1963) of approximately 21 million tons. The production plant was designed to mine and treat 1.25 million tons per annum. The production and service hoists are mounted at-the top of a reinforced concrete tower above the shaft.

Jan 1, 1965

By Curt D. Edgerton

This study was made to determine trends in fresh water usage by California petroleum refineries, to forecast fresh water requirements to 1975, and to evaluate water conservation practices. Statistical data used in the study were obtained largely from published sources and from records of selected companies. An adequate sampling of the State's refining capacity was obtained, and the data were extrapolated to the total California refining capacity. A breakdown of the data was then made on the basis of the following refining regions: (1) the Los Angeles Basin and Southern Coastal region, (2) the Southern San Joaquin Valley, and (3) the San Francisco Bay area. An unpublished forecast of crude oil input to refineries by a major oil company operating on the West Coast was used as a basis for predicting fresh-water usage. The 1963 fresh water intake by California petroleum refineries was 84 million gallons per day. This is expected to increase to 128 million gallons per day by 1975. The fresh-water to crude-oil ratio is increasing in all regions except the Southern San Joaquin Valley. At present, the supply of fresh water available to almost all of the State's petroleum refineries, mostly from surface sources and company-owned wells, is adequate, although shortages may develop within the foreseeable future. Present conservation methods are centered around the following four objectives: (1) minimum intake of fresh water of the lowest possible quality commensurate with sound technologic practice; (2) optimum recirculation; (3) proper treatment before discharge; and (4) substitution of air cooling for water cooling.

Jan 1, 1965

By D. H. Baldwin, R. E. Reed-Hill

DURING the course of experiments involving oxygen equilibrations with a high-purity Pd-5 at. pct Rh alloy, the appearance of a subscale was noted. Most of the heat treatments in a pure oxygen atmosphere were performed at 900°C. The presence of the subscale was noted when the oxygen partial pressure was in excess of approximately 95 mm, up to 1 atm, the highest pressure used. According to available thermodynamic information' on the free energy of formation of Rh2O3 (the only reliably reported solid oxide of rhodium), this oxide should not be stable under these conditions, nor, of course, any oxide of palladium. Extraction of the subscale from the matrix was affected by treatment with aqua regia, and the resulting X-ray diffraction powder pattern is shown in Table I. This pattern is not that of Rh2O3, nor that of any known rhodium or palladium oxide. It can be indexed on a hexagonal lattice with a. = 5.22Å and co = 6.0Å. In addition to this unknown material, there was a weak Rh2O3 pattern. An X-ray fluorescence analysis of the powder gave 3214 palladium counts per sec and 5381 rhodium counts per sec, thus indicating the likelihood of a double oxide of palladium and rhodium. In view of the fact that the above result was obtained on a single sample, it is perhaps best not to insist upon the above ratio of about 0.6, but possibly to tentatively assume 0.5 or 1/1. The small amount of Rh2O3 in the X-ray pattern might have occurred on cooling, and it seems possible that the double oxide, below some temperature level, is not as stable as Rh2O3. To examine this point, some of the extracted double oxide was heated on a sheet of pure palladium in air at 900°C, and allowed to furnace-cool over a period of several hours. The X-ray diffraction pattern of the powder showed approximately the same intensity of Rh2O3 and the "hexagonal" oxide as before, but, in addition, a rather faint pattern of another crystalline species made its appearance. This finding again suggests partial transformation of the major (double) oxide to other oxides on cooling from 900°C. Application of the phase rule shows that only one equilibrium oxide (subscale) could have been present at temperature. Vacuum-fusion, oxygen analysis of the extracted subscale showed 7.7 ± 0.7 pct O. Combining this information with that of the X-ray fluorescence analysis suggests the formula PdRhO. This compound should have an oxygen content of 7.07 pct, which is within the range of error of the oxygen analysis. However, until a more careful stoichiometric study is made, it is suggested that the formula be written

Jan 1, 1965

By Martin J. Hughes

The Eagle Mountain Mine of the Kaiser Steel Corporation is located in the California portion of the Colorado Desert at a distance of about 60 miles east of Indio, California. At the present time, this mine is producing at the rate of 5,000,000 tons of concentrate per year. A total of 1,000,000 tons of ore per year is presently being sold on the Japanese market while the remainder is consumed by the Kaiser Steel Company blast furnaces at Fontana, California. A new Pellet Plant and Concentrator is presently under, construction with completion scheduled for May or June 1965. This plant will have a rated capacity of 2,200,000 tons of pellets per year and essentially all of this production will be sold to Japanese steel companies.

Jan 1, 1965

By Joseph A. Cavallaro

This report describes the timed release analysis technique that was developed to serve as a tool for assessing the froth flotation cleaning potentials of fine-size coals. Using this developed technique, 16 coals from 10 different coalbeds were tested. All of the coals included in this study were quite amenable to froth flotation with float coal yields ranging from 80.7 to 99.5 percentage points. Float-and-sink analyses of the coals tested are shown to be of limited value in predicting froth flotation cleaning potential. Generally the float-and-sink analyses indicated a better product could be obtained than froth flotation could provide; although, in four of the coals tested froth flotation results were superior to those expected from the gravimetric analysis. The fixed carbon content of the samples collected was found to correlate with the floatability of the coals. The higher rank coals were the most readily floatable coals while the lower rank coals did not respond quite as well to flotation.

Jan 1, 1965

By Wallace W. Key

The California pesticide industry in 1962 consumed about 30,000 tons of clay, talc, limestone, diatomite, sulfur, and other minerals as fillers (carriers and diluents) in pesticide formulation. This was 10 percent of the U.S. filler requirement for pesticides. About two-thirds of the California total was supplied by a few local mineral producers; the remainder came mainly from Florida, Georgia, and Wyoming. The objectives of this report are to provide data on quantities, sources, specifications, and market conditions for minerals used as fillers by California pesticide formulators. The study disclosed that specifications for mineral fillers have become more rigid and formulators have become more numerous in recent years. During 1962 over 1,200 firms registered 16,000 pesticide products with the Bureau of Chemistry in California. Factors which will tend to diminish future need for mineral fillers include the trend toward greater use of organic sprays rather than dusts and further development of biological controls, such as the development of sterile insect strains.

Jan 1, 1965

By Adrian C. Dorenfeld

The concentrator of Bonneville Ltd.* at Wendover, Utah, processes a feed obtained by, solar evaporation of a brine containing sodium and potassium chlorides with minor amounts of impurities. Salable potassium chloride concentrateis produced from this feed in two steps: flotation with amine reagents to concentrate the potassium chloride, and washing of the concentrate with fresh water to reach final grade. In the flotation step emphasis is placed on recovery, whereas the washing step has as its objective the production of salable grade (in excess of 60 percent K20 equivalent), with recovery being important but secondary Ideally, flotation should give maximum recovery at a concentrate grade which will permit washing to salable grade with a minimum recovery loss, thereby maximizing over-all recovery. Except for this relationship, flotation and washing are two separate and distinct operations.

Jan 1, 1965

By T E. Tibbetts

This paper deals with coal sampling in general and with mechanical coal sampling in particular. The necessity of obtaining representative samples is emphasized. Other sections of the paper are devoted to the design and selection of automatic samplers, with a consideration of the three main types, and the testing, operation and maintenance of these samplers. The cost of the installation of an automated sampling system must be related to the value of the material to be sampled, to the volume of coal involved, and to the savings in labour and economy which can be achieved. Introduction T HE Committee?:; on Coal Sampling of the Coal Study Subsection, Thermal Power Section (Eastern Zone), Canadian Electrical Association, was established in November, 1963, to "study the various problem areas of coal sampling." The first undertaking of the Committee was to at-tempt to survey the problem areas of coal sampling through an evaluation of coal sampling difficulties as experienced at both the plant design and operational levels within the electric utilities represented on the Committee. The results of this enquiry indicated that satisfactory answers to almost any conceivable

Jan 1, 1965

By R. E. Campbell

Uranium metal of improved purity was prepared by electrorefining commercial magnesium-reduced uranium in a molten sodium chloride-uranium trichloride electrolyte. The best operating conditions for the preparation of refined metal were established as follows: an electrolyte containing 8.7 to 13.3 weight-percent uranium; initial cathode current densities from 300 to 1,500 amp/sq ft; and a molten salt temperature of 860° C. Ingots produced from electrorefined uranium crystals prepared with these operating conditions were substantially free of metallic impurities. The only impurities in the refined and consolidated metal were present in low or undetectable amounts.

Jan 1, 1965

By T. A. Sullivan

High-purity vanadium metal was prepared by electrorefining commercial vanadium in a molten sodium bromide, potassium bromide, and vanadium dibromide electrolyte. Variables investigated were operating temperature, current densities, electrolyte composition, and condition of the anode. The purity of the refined metal was in the range of 99.95 percent vana-dium. Iron and oxygen in the 50- to 250-ppm range were the only major impurities. Metal with hardness numbers of 50 to 60 in the Rockwell F scale was prepared from feed material with a Rockwell B hardness of 90. The arc-melted metal was highly ductile and could be cold-worked into sheet or foil.

Jan 1, 1965

The 8 ft by 91/2 ft drive which joined No. 7 Shaft with Browne Shaft on the 1,480 ft level was extended from both ends and met at a point approximately 12,000 ft from No. 7 (2,000 ft from Browne).The surveying required for this 2 1/2 mile haulage drive called for greater accuracy than was obtainable from South Mine standard methods. Procedures and devices from published information were tried and modified as required to suit local conditions. Several new methods were applied and improved as the drive advanced. The control of angular, linear and level measurements was perhaps considerably in excess of the requirements, but this was offset by abnormally large discrepancies resulting from shaft plumbing. The accuracy of the final breakthrough, although not to the standard desired, was sufficient to complete the connection without inconvenience and added cost.INTRODUCTIONThe acquisition of the Browne Shaft leases in January 1962 presented the management of Broken Hill South Limited with the problem of transporting ore from these leases to its mill. It was eventually decided that diesel locomotivehaulage through a 2t mile drive on the 1,480 ft level between the two mines was the best solution. The drive was advanced from both ends after Browne Shaft was deepened by 80 ft to reach the 1,480 ft level horizon. Each end advancedabout 15 ft/day with the miners working three 7 hr shifts. Blasting was restricted to the end of the shift.The survey work involved five shaft plumbings and 78 theodolite stations in a traverse, underground and surface,of more than 5 miles. Because of the exceptional length of the drive, an unusually high degree of reliability was required.The aim was for a maximum error at breakthrough of 1 ft 1 in 30,000, and to secure this, precise methods of linear measurement were necessary. Shaft plumbing in particular posed special difficulties.

Jan 1, 1965

By Donald B. Evans, Robert D. Pehlke

The solubility of nilrogen in liquid binary alloys of iron with Litanium. zivconium, columbium, vanndiurn, and tantalum was measured for alloy composiLions up to the solalbility limils of lhe alloy nitrides. All five alloying agents were found to decrease markedly the activity coefficient of nitrogen in liquid ivon. The metal/nitvogen mole ralios in the alloy nitrides formed were generally .found to be slighlly greater than 1.0, but in no case greater than 1.5. From the experimental data, the standard free energies of fortmation of titanium and zir-conium nitrides have been calculated for the Lemperaluve range 1550° to 1750 C. The solublily Products for columbium, tantalum, and vanadium nitrides are also reported. A number of research investigations have examined the effect of refractory metals on the solubility of nitrogen in liquid iron. Although data on zirconium are not available, investigators are in agreement that titanium, vanadium, columbium, and tantalum markedly increase the solubility of nitrogen in liquid iron. This fact alone makes desirable the acquisition of thermodynamic data for these elements in liquid iron. Since refractory metals are known to be stable nitride formers, they have been suggested as steel denitrifying agents, and some of their nitrides have recently been considered as containment materials for liquid iron and iron alloys. Most available thermodynamic data for these metals relate to their dilute concentrations, but effective thermodynamic treatment of these applications requires data at concentrations near the solubility limit of the alloy nitride. Although some work has been done at relatively high alloy concentrations in liquid iron (particularly for vanadium 2,3 and titanium 2,4), the results have been somewhat contradictory. Disagreement may be partly attributed to the fact that the compositions of most refractory metal nitrides have been shown to be nonstoichiometric, and to vary 2,5-8 depending on the temperature and nitrogen gas pressure with which the solid nitride phase is in equilibrium. One purpose of this study consequently has been to determine the compositions of the refractory metal nitrides precipitated from a liquid iron solution. EXPERIMENTAL PROCEDURE Rao and Parlee2 and Evans and Pehlke 9 have discussed the technique for measuring the solubility product of an alloy nitride phase in liquid iron by finding the point of departure of the nitrogen solubility from Sieverts' law. The method consists of measuring the solubility of nitrogen in a melt of iron containing a known concentration of a second metal as a function of the nitrogen gas pressure over the melt. In this study the second metal was one of the refractory metals titanium, zirconium, columbium, vanadium, or tantalum. When the nitrogen pressure at which the refractory nitride forms is reached, a deviation of the measured solubility of nitrogen in the melt from Sieverts' law is observed in the form of a "pressure halt." The concentration of nitrogen in the melt associated with this breakpoint in the nitrogen-absorption curve is then used to calculate the nitride solubility. The Sieverts method was used to measure nitrogen solubility as a function of nitrogen pressure and temperature. The experimental equipment for this technique has been previously described in detail. 1,9 Charge materials used were vacuum-melted high-purity iron (Ferrovac-E) and the best commercial grades of the refractory metals obtainable (in all cases at least 99.8+ pct pure). Recrystallized alumina crucibles were used to hold all melts except those containing zirconium, for which zirconia crucibles were necessary. Temperatures were measured by a disappearing-filament type optical pyrometer sighted vertically downward on the melt surface through a 1/4-in.-diameter sight hole in the crucible lid. By means of a technique previously described, 9 in which the refractory-metal nitride was precipitated at one temperature then redis-solved by raising the temperature 50°C and precipitated again at a higher temperature, it was possible to obtain data over a temperature range of up to 200°C on a single melt. It was found that this technique could not be used with melts containing zir-

Jan 1, 1965