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By D. K. Deardorff, Earl T. Hayes

An improved technique is described for the accurate determination of melting points of metals in the temperature range 1500' to 2500°C. The improvements consist of gradient heating and refinements in cavity preparation to obtain true black-body conditions. The melting point of hafnium, as determined by this method, is set at 2222°±30°C. This is over 200°C higher than one of the values reported earlier. Discrepancies in the previously reported values for the melting point of hafnium are explained. The melting points of zirconium and titanium are found to be 1855O±15OC and 1668°±10°C, respectively. Reproducibility of results was ±3OC. PRIMARILY, this report is being made to correct a 1975o±25oC1 value for the melting point of hafnium, and to present an improved method for melting point determination. As a matter of interest, the technique was also applied to determining the melting point of zirconium and titanium. There is a wide difference in the melting point of hafnium as reported by competent investigators. DeBoer and Fast' reported a value of 2230°±500C, and later work of McPherson, as reported by Aden-stedt, placed the melting point at 1975o±25oC. Zwikker" calculated that the melting point was 2430°C. In resolving this discrepancy, improvements were made in the procedure for determining the melting points of refractory metals in the range 1500" to 2500°C. Special techniques are necessary to determine the melting point of these metals accurately. Since the metals oxidize in air above 900oC, the determinations must be carried out in an inert gas or vacuum. Also, every known refractory contaminates them to some extent. In addition, the attainment of true black-body conditions is always difficult. DeBoer and Fast actually determined the melting point of Hf-Zr as-deposited iodide process alloys and extrapolated to 100 pet Hf. McPherson employed a tungsten wire suspension similar to that described by Schramm, Gordon, and Kaufmann,1 and used hafnium metal produced by the iodide process. There was no apparent reason for the wide spread in melting points, since the quality of the metal was very good and the work was under the direction of highly competent investigators. Retracing some of this work revealed one understandable error in the case of hafnium, and led to development of an improved technique for determining melting points of reactive metals in the range 1500" to 2500°C. Material Crystal bar hafnium, zirconium, and titanium were used for this work, with analyses as shown in Table I. The hafnium was of the highest purity that has been prepared, though not as pure as the zirconium and titanium. At the instigation of the Pittsburgh Area Office of the AEC, a special lot of Hfo2 was purified, converted to the tetraflouride, and bomb-reduced with calcium, all at the Iowa State College Laboratories. This crude hafnium metal was then refined by the iodide process at the Foote Mineral Co. All specimens were cut with a Sic wheel, ground, pickled, and dried carefully before use. Procedure General Tungsten Suspension Method—In this method, a small specimen is suspended by a fine tungsten wire in a slender, induction-heated tungsten or tantalum cylinder, all under vacuum. The melting point is determined by heating the specimen slowly while observing it with an optical pyrometer focused upon a portion of the specimen that radiates as a black body. This means that there should be no reflected radiation, either from colder objects near the pyrometer or from hotter surfaces. The induction heater would be the only hotter object and, if it is slender enough, the specimen will attain the same temperature. Often a slender hole is drilled into the specimen as a source of black-body radiation. This was the general method used by McPherson in obtaining his value of 1975°C for the melting point of hafnium. In trying to repeat this work, it was found that the points of contact between the

Jan 1, 1957

Arthur Jarman, Sydney, New South Wales, Australia (communication to the Secretary*):—All designs for modern metallurgical and chemical laboratories should provide each student's desk with a hood or cupboard for the removal of fumes, but I doubt the advisability of placing air-baths and similar apparatus close to the hot plate. It seems to me that unless the draft be exceptionally strong the fumes from ordinary wet assay work will corrode the iron-work of the fittings, in which case the baths would have to be removed to a general desk in order to lighten the work of the laboratory attendant. Since the laboratory described by Mr. White has been in use for two years, I should like to ask if any inconvenience has resulted from this corrosion. If not, it is certainly an important improvement to have the air-baths and similar apparatus placed on the student's desk. The hoods described by Mr. White are supplied with a good draft by means of a fan, which gives them a great advantage

Jan 1, 1905

Among the recent bulletins are the following, which. may be obtained from the Superintendent of Documents, Government Printing Office, Washington, D. C. BULLETIN 127. Gold dredging in the United States, by Charles Janin. 1918. 224 pp;, 63 pls., 23 figs. 50 cents. BULLETIN 161. California mining statutes annotated, by J. W. Thompson. 01918. 312 pp. Paper cover 20 cents. BULLETIN 169. Illinois mining statutes annotated, by J. W. Thompson. 1918. 594 pp. Paper cover 35 cents. The. Potash Situation, by A. W. Stockett. 13 pp. Preparation of Crucible Graphite, by George D. Dub. 27 pp. National Importance of Allocating Low-ash Coke to the Manganese-alloy Furnaces, by P. H. Royster. 4 pp. Production of Ferromanganese in Blast Furnaces, by P. H. Royster. 31 pp. Production of Spiegeleisen in Blast Furnaces, by. P. H. Royster. 19 pp.

Jan 6, 1919

By G. H. LeFevre

THE Metal Sales Department, with offices in New York, is responsible for the sale of the Company's products, with the exception of gold and coal. At present the department handles the sales of lead, zinc, silver, antimonial lead, , cadmium, bismuth, arsenic trioxide, and tellurium; gold is shipped direct to the United States Mint and coal is marketed by United States Fuel Company's own sales organization. The department keeps in close touch with the metal markets and collects information on marketing conditions, which it makes available to other departments of the Company. The electrolytic lead produced at the U. S. S. Lead Refinery, Inc., is a high-uality product marketed as corroding grade under the "U. S. S.-ELECTRO" brand. It is largely sold to manufacturers of paints, pigments, lead oxides, and storage batteries.

Jan 1, 1948

By N. H. Emmons

(Canal Zone Meeting, November, 1910.) AN interesting development of copper blast-furnace construction has been brought about in adapting the blast-furnace to be a "burner" for sulphuric acid making. When the Tennessee Copper Co. first decided to construct an acid-plant, the standard type of brick-top furnace, supported by structural steel, was the only one in use at this plant. All the tests for temperature and strength of gas had been made on these furnaces, and had been satisfactory. When, however, the acid-plant was put on the flue, and the flue had to have a damper put in it to force the gas into that plant, troubles began. The furnaces were fairly tight, and for a few months the work was quite satisfactory., Fig. 1 shows the old type of furnace-top used at the start. It was soon found that this top would not stand the temperatures, particularly when dampered back, as was necessary to force the gas into the Glover towers. The structural steel, of which the furnace skeleton was constructed, warped and twisted so badly that it was not safe to use the furnaces. This effect is shown by Fig. 2, which is a photograph of old No. 4 furnace, after the brick-work had been removed. It became apparent that a new type of top was necessary and the engineering force was started oil the design of a new furnace-top, with the result that a low top, with brick-lined flues at each end below the feed-floor, leading to the main concrete dust-chamber, was constructed. This furnace, No. 7, is shown in Fig. 3. The charging-doors are made of cast-iron sections, three sections to a door, and three doors to a side. A door to the furnace was made of cast copper, but the heat was so great that the copper bent readily, due to the jarring of its * General Manager, Tennessee Copper Co.

Feb 1, 1911

Jan 1, 1907

By Ellsworth Daggett

Jan 1, 1879

Jan 1, 1968

By D. A. Elgillani, M. C. Fuerstenau

In this paper, oxidation potentials measured in the presence of various concentrations of cyanide, ferro-cyanide, and ferricyanide and ethyl xanthate at various values of pH are related to flotation response. Eh-pH diagrams are presented to show that the formation of surface ferric ferrocyanide is probably responsible for depression when cyanide is added. The influence of cyanide on the depression of pyrite with xanthates as collector has been the subject of a number of investigations,'-6 and several theories on the mechanism of depression have evolved from these studies. Wark and Cox7 and Gaudin8 have suggested that the depressing effect is due to a competition of cyanide ion with xanthate ion for the surface. Cook and his colleagues9-11 have explained this phenomenon in terms of competition between hydrocyanic acid and xanthic acid. Sutherland 12 has shown that although both of these theories accurately describe the relation between pH value and cyanide addition at constant collector addition, they fail to describe the relation between pH value and the amount of collector required to cause flotation. Taggart 13 suggested that depression in these systems is due to the formation of a reaction product between ferric ion at the pyrite surface and ferrocyanide ion derived from solution. Majumdar4,6 has attempted to prove this hypothesis by measuring the contact angles of pyrite in the presence of 25 mg per liter ethyl xanthate and different concentrations of potassium ferrocyanide and ferricyanide. In all cases the contact angles were quite high up to pH 10. These results indicate that pyrite should not be depressed by either potassium ferrocyanide or ferricyanide. In view of these facts, Majumdar has assumed that the compound Fe(CN)2 forms at the surface. Gründer and Bornl4 have stated that depression may be due to the formation of the compound K2Fe(II)Fe(CN)6 at the pyrite-solution interface. This compound is thought to be an interaction product between the K2Fe(CN)6-2 ion from solution and the Fe++ ion at the pyrite surface and, accordingly, K4Fe(CN)6 should depress pyrite at least as effectively as KCN. This was proven experimentally, but there was no simple relation between the depression of pyrite and the concentration of either KCN or K4Fe(CN)6 in solution. In view of the many mechanisms that have been proposed for pyrite depression by cyanide, it is apparent that a clear understanding of the phenomena occurring in these systems is lacking. One reason for this may be the fact that the species responsible for pyrite flotation in the presence of xanthate is not the xan-thate ion but rather dixanthogen.15 Since the oxidation of xanthate to dixanthogen is dependent on the oxidation potential of the solution, it would seem that knowledge of these potentials would be a requisite to understanding the pyrite-xanthate-cyanide system. It is the object of this paper to measure both the oxidation potential and pH of the pyrite systems in the presence of various concentrations of cyanide, ferrocyanide, and ferricyanide and xanthate and to relate these values to flotation response. EXPERIMENTAL MATERIALS AND 'TECHNIQUES In the experiments discussed here, pure potassium ethyl xanthate was used as collector, and reagent grade potassium cyanide, potassium ferrocyanide, and potassium ferricyanide were used as depressants. Reagent grade HC1 and KOH were added for pH adjustment. Conductivity water, made by passing distilled water through an ion exchange column, was used in all experimental work. Two natural samples of pyrite were used in the investigation. Sample preparation for flotation included dry grinding with a mortar and pestle and sizing the product to 100 x 200 mesh. Prior to flotation, a 0.75-gm sample of pyrite was added to a solution containing a known amount of depressant at the desired pH value, and the system was conditioned for 4 min. Following this, a known amount of collector was added and the system was conditioned for another 4 min. The pH — termed flotation pH - was measured; the pulp was transferred to a Hallimond cell, and flo-

Jan 1, 1969

By Morris J. Elsing

FOR MANY YEARS lead and zinc have had the so-called protection of a tariff and it is the purpose of the following brief discussion to show what' such protection actually accomplishes with a view to forecasting the possible results of the present copper tariff. In analyzing the subject, tabulations of the United States production, consumption, imports and exports, including ore and concentrates and all of the metallic products, of both lead and zinc have been made for each year since 1900. Of these data, the relationship of the imports and exports and the relative foreign and domestic prices are shown in Table 1. The conclusions drawn from these figures are listed below. 1. The United States is an exporter of zinc. 2. The United States is an importer of lead. 3. The average price of zinc at St. Louis for the last 32 years has been no higher than on the London market even though zinc and zinc ore have "enjoyed" a protective (?) tariff of varying amounts per pound for 22 years of this period. 4. The average price of lead on the New York market for 32 years has been 1.2c. per pound higher than on the London market, the tariff varying from 0.75 to 1.5c. per pound of lead in ore, and 1 to 2c. or more on manufactured lead.

Jan 1, 1932

By E. L. Jr. Spain

This study was undertaken primarily to determine the reasons for certain varia-tions in the soundness of gravel aggregate taken from a number of widely separated points on the Tennessee River. Under laboratory tests, concrete made with these various aggregates it some cases exhibited marked differences in specific gravity, crushing strength and durability. Gravel was studied in detail from Chattanooga to the mouth of the river and to a lesser extent from Chattanooga to Knoxville. The causes of variation were determined, and variational curves were constructed, which accurately predict the composition of aggregate at any point on the river and therefore its relative suitability for use in concrete. The aggregate at any point is suited for making sound concrete; the variance of suitability is due to varying percentages of sandstone and weathered material, which are less sound than other constituents.

Jan 1, 1937

By AIME AIME

THOUGH the Annual Meeting of the Institute-officially numbered 158 on the records was delayed a bit at the start by low steam pressure on the locomotives bringing members to New York, the crowd that finally arrived more than lived up to expectations, and the technical program had few difficulties because of absent authors or lack of competent discussers. The transportation difficulties were occasioned by the fact that Monday, Feb. 15, was the third coldest day in the 72 year history of the New York Weather Bureau, the official temperature being 8 below zero. The New York Central's premier train, the 20th Century, due at 9:30 a.m., arrived about 6:30 p.m., and the Commodore, another crack train from Chicago, was about equally late.

Jan 1, 1943

C. M. Bishop (Aircraft Div., A. V. Roe Cnnada Ltd., Toronto)—Reference is made to the coherency hardening of ß due to ß' and also to the hardening of ß due to a coherent precipitation of the a phase. What is meant by the term "ß'?" Would not the coherency hardening of ß during cooling be due to precipitation of a sub-microscopic dispersion of a, as is the case during reheating a ß-quenched alloy? I feel that these two phenomena are essentially the same mechanism, i.e., precipitation of a from unstable or supersaturated ß. From the text, it would appear that Tables III and IV are intended to show the effect of the martensite transformation on the properties of Ti-Mn alloys. Referring to Table 111, the ß-quenched alloys would contain a greater proportion of retained ß than would the equilibrated alloy. Could not the increase in properties be attributed to this, along with possible coherency hardening of the ß? In the same way, the structures referred to in Table IV contain ß from which they could derive their hardness. It would appear to be difficult, if not impossible, to assess the role of the martensite transformation from the data contained in these tables. F. C. Holden, H. R. Ogden, and R. I. Jaffee (authors' reply)—In reply to the first question raised by Mr. Bishop, the term "ß"' designates an apparent retained-p structure which is harder than it is after the most rapid cooling from the ß field. It is thought to be the result of a coherent precipitation of a. The mechanism by which hardening takes place is undoubtedly the same as that involved in the early stages of aging of a re-tained-p structure, and we are in agreement with Mr. Bishop on this point. The term "ß'" to designate the anomalously hard retained-ß structure was agreed upon at a symposium in 1953." The authors do not agree that the quantity of retained ß and/or ß' in the ß-quenched specimens of Table III is necessarily greater than that of the 600°C equilibrated specimens. The ß-quenched specimen has a structure which appears to be completely a' formed by the martensite reaction. It is recognized that there could be some retained ß (or ß') between the a plates if the M, temperature is below room temperature. This is unlikely for the 3.4 pct Mn alloy where the M, is known to be at about 640°C. Therefore, the increase in strength cannot be attributed to the presence of a greater quantity of coherency-hardened ß, but, rather, the increase in strength must be attributed to the transformation products formed, e.g., a' (martensiti-cally formed a). Concerning the data in Table IV, we agree that it is difficult to estimate the role of the martensite reaction, since the 6.4 pct Mn alloy was retained ß in the quenched condition.

Jan 1, 1955

By R. E. Hudrlik, G. W. Preckshot

The diffusion coefficients of silver from solid silver in molten lead were measured to within ± 0.8 pet in a columnar type diffusion cell ower, the temperature range of 326° to 530°C. Fick's law describes the process up to 530°C where the laminar mechanism appareltly breaks down. These is negligible resistance at the interface as shown by mathematical analyses. The diffusion coefficients are found concentration independent. IT would seem that diffusion in liquid metals would be free of such effects as molecular structure, dissociation. polarization. and compound formation. This view was taken by Gorman and preckshot in their study of diffusion of copper from solid copper into molten lead. They reported diffusion coefficients which were independent of the concentration over the range of 478° to 750°C. They found that the Stokes-Einstein equation with constant radius of the diffusing specie represented the diffusion data better than Eyring's rate theory equation and Sheibel's correlation. The radius of diffusion was found to be that of the doubly charged copper. There appeared to be no resistance across the solid-liquid boundary. In the present work the diffusion coefficients for silver in liquid lead were measured over a range of temperatures of 350° to 505°C. The solubility of silver in lead over the range of 303° to 630°C was also obtained. These results are compared with calculated or correlated values or with data in the literature. EXPERIMENTAL Procedure—The experimental equipment techniques and procedures were those reported in detail by Gorman and preckshot9 and will not be repeated here. Measured values of WT, Co, A. L were obtained for various diffusion times and the diffusion coefficient was computed for the case of no resistance at the interface9, 11 by: WT/CoAL = 1- 8/p2 n=1 1/(2n - 1)2 exp[-(2n - 1)2p2 Dt/4L2] [1] or where there was resistance at the interface by: WT = 1- ?n=1 2h2/ap2L [sxp [-Dan2t]/[(h2 + an2) L + h] The roots an are those of the transcendental equation3 tan (an L) = Iz/cun. The diffusion coefficient is that defined by Hartley and Crank.7 The total silver in the lead cylinder and equilibrium slug was determined by a cupellation technique' with proper correction for losses. Analysis of known samples showed that this method is surprisingly accurate. The amount of silver in the lead adhering to the silver cylinder was obtained in the same fashion as shown by Gorman and preckshot.9 The small errors involved in this determination are not critical since the silver in this adhering lead layer is only 3 to 15 pet of the total diffused. Materials—Electrolytic silver containing 99.9+ pet Ag obtained from General Refineries of Minneapolis, Minn. was used for all but runs 7 and 8. For the balance of the runs this silver was reduced with hydrogen at 1100°C and its oxygen content was found to be about 0.017 pet. For the runs. 7 and 8, phosphorous-reduced silver of the same purity was obtained from Handy and Harman Co. of Chicago, Ill. The densities of the phosphorus-reduced silver and the hydrogen-reduced electrolytic silver were 10.484 and 10.487 g per cm3, respectively. These values agree with those reported for pure silver. Silver which was reduced at 900 C had an average density of 9.998 g per cm3, indicating porosity. This silver was used for a number of runs which were not tabulated in Table I. These are indicated by crosses on Fig. 2. The 99.999 pet Pb was obtained from the National Lead Co. Research Laboratory of Brooklyn, New York. DISCUSSION OF RESULTS The diffusion and solubility results are reported in Table I for eleven runs using either phosphorus-reduced electrolytic silver or hydrogen-reduced silver at 1100° C. The solubility data shown in Fig. 1 show the excellent agreement with that reported by Heycock and Neville.8 The data of Friedrichs5 apparently are in error. The experimental solubility data of this work are reported to 0.3 pet. The experimental diffusion coefficients computed from Eq. [1] are reported within 1.2 pet of the mean and are plotted in Fig. 2. These are expressed within +0.8 pet of the experimental values over the entire temperature range by: D= 8.26 x 10 -5 e-1925/RT . [3] There appears to be little difference due to the

Jan 1, 1961

There were two official representatives of Foreign Governments as guests at the Chicago Meeting. One was Frederick Goransson, managing director of the Saudvikens Steel Works, who represented the Jernkonteret, the Iron and Steel In-stitute of Sweden, and who came to this country especially for our meeting. The other distinguished guest was Commander Toublet, who repre-sented the French Embassy. Commander Toublet delivered a most polished address at the Banquet, dealing with the felicitous relations existing between this country and France for the last 150 years. Com-mander Toublet was accompanied by Mrs. Toublet, who won the hearts of all the ladies present, whose guest she was.

Jan 11, 1919

Aase, Glenn D., (J'40) Jr. Met.. American Smelt. k Refin. Co., Selby, Calif. Abadie, Henry G., (J'43) Petr. Engr., Avenal, Calif. Abbott, Clarence E., (M'04) Civil Engr., V.P.. Tennessee Coal, Iron & R.R. Co., 1542 Brown Marx Bldg., Birmingham, Ala. Abel, Raymond L., (M'28) Chem. Engr., C.O., Pitts¬burgh Chem. Warfare Procurement Dist., American Bank Bldg., Pittsburgh. Pa. Abel, Walter D.. (M'32) Min. Engr., Supvr. Engr., R.F.C.Lee Angeles, Calif. Abele, Louis T., (M'31) Route No. 1, Adameville, Tenn. Abell, Leo M., (M'31) Mill Supt. & Met., Emperor Gold Min. Co. Ltd., Vatukoula, Fiji Is. Abernathy, G. E., (M'38) Geol., Kansas State Geol. Survey, Pittsburg, Kans. Abernathy, Jack H,, (M'40) Asst. Cenl. Supt. of Prod., Sunray Oil Co., 11th Floor, Philtower Bldg.. Tulsa 3. Okla. Abernethy, D. Carl, (M'44) Min. Engr. Rm. 3217, N. Int. Bldg., Washington, D. C.

Jan 1, 1944

By Barry K. McMahon

Following minor slope failures at the commencement of mining the west wall of the Kanmantoo Mine was redesigned from an overall slope between haul roads of 55° to 46°. This decision was based on a probabilistic analysis which indicated that 46° was the optimum economic slope.

Jan 1, 1983

By Joseph Jensen

CURTAILMENT of oil production in California began in 1922 and 1923 when certain of the major companies completely shut down some pumping properties. Efforts of this kind were generally carried on without coordination by individual companies until 1923. From May to August of 1923, oil production in the Los Angeles Basin was curtailed because of lack of pipe-line outlets. This work was handled by a small committee of executives and engineers of some of the pipeline companies without any established. Method such as obtains at present. Not all of the major companies participated in ibis curtailment and the effort was not well organized. The problem then was principally to move the oil. The crisis passed in September of 1923 from then on the major companies each on it own initiative, shut in additional production. At Domiuguez, in 1921, Shell, Union and Associated agreed to limit drilling to a 100-ft. zone for one Near. In the summer of 1925, operators at Ingde-wood agreed to limit developments to a 1300-ft. zone during the 1925 drilling campaign. In the summer of 1927, the Ventura operators cut back their production one-third and deft it thus for 90 day. Drilling in this field has always been at a slow and conservative rate.

Jan 1, 1932

By Tegner C. Johnson

Just a few years ago, my company was referred to as the Marion Steam Shovel Company. Though we still make shovels, both two and eight-crawler types, the eight-crawler stripping shovel appears to have been replaced by the walking dragline for overburden removal and in some cases for the mineral as well. The walking dragline appeared in the coal fields in the early 1930's. It is popular because it can cope with overburden depths in excess of 100 ft and with blasted sedimentary rock, all at an O & O (ownership and operational) cost of ±10[c] per bank cu yd (bcy).

Jan 10, 1974

By J. C. Bayles

Jan 1, 1886