Search Documents

By Tugba Basargan Çagatay Morall, Gülhayat Nasun-Saygili

"The aim of this study is to prepare the apatitic material using colemanite mineral (2CaO.3B2O3.5H2O) which was obtained from Eastern Anatolia, Turkey. For this purpose, colemanite mineral was reacted with different phosphate sources, namely, dipotassiumhydrogen phosphate, ammoniumhydrogen phosphate and ortophosphoric acid at various temperatures and time periods. Experiments were run in batch system. The apatitic material was prepared by a wet method and followed by heat treatment at various temperatures. Structure of the samples was analyzed by XRD, FTIR, XRF and SEM. The particle size analysis was also made for the result product. The experiments showed that reaction temperature, contact time and heating temperature are important parameters to transform the colemanite into apatitic structure. Reaction of colemanite with dipotassiumhydrogen phosphate and ammoniumhydrogen phosphate results in amorphous, non-stoichiometric hydroxyapatite type structure, while acid based phosphate source gives brushite and monetite type product before and after heat treatment, respectively.IntroductionBoron which has properties intermediate between metals and non-metals is a member of semiconductor group of elements. Its atom is very small and has three valence electrons. Boron exists in Earth's crust (from 5 mg/kg in basalts to 100 mg/kg in shale) and in the oceans (4.5 mg/l) [1]. Turkey has 60% of world's boron reserves which is mostly in the form of colemanite (2Ca0.3B203.5H20). Colemanite is the most important calcium containing commercial borate mineral with 5 mol of crystal water [2].Calcium phosphate cements are very useful for bone repair applications because of its chemical structure. They are injectable, easy to shape and can be maintained locally. Because of those reasons calcium phosphate cements are very effective to fill bone defects with an irregular shape [3]. Hydroxyapatite (Ca10(PO)6(OHh) is the major component of the bone (70 wt%). However, hydroxyapatite stoichiometry, composition and crystallinity differ in human skeleton system [4, 5].The main objective of the present work was to study the transformation of colemanite to apatitic material using different phosphate solutions at several time spans and temperatures. The experiments were run in a batch system, change in pH and also weight loss were measured after the experiments. Several analysis methods were used to investigate the chemical and structural changes."

Jan 1, 2012

By P. L. Menaul, P. P. Spafford

This paper discusses the most dangerous form of corrosion encountered in condensate-well oil production, the discovery of the agent causing this corrosion and the remedial chemical treatment proved effective by field use. The injection of ammonium hydroxide, even as little as one quart per day, has proved effective in preventing gas-condensate well corrosion. The injection of "Bone oil" is applied to wells producing brines containing calcium and magnesium salts. Introduction The severe corrosion of equipment in high pressure gas condensate wells has been a problem for several years and numerous papers have been presented on the subject. The term "gas condensate" or "distillate well" is applied to a distinct variety of hydrocarbon producing well, the characteristics of these wells being high bottom-hole (formation) pressures and temperatures and high gas production. These wells usually produce about 40 gal of water per million cubic feet of gas and the gas contains from 0.1 pct to 2 pct carbon dioxide. In the operation of this type of well, the operators soon noted severe internal corrosion of the pipe carrying the production. In some instances the dl tubing has been found to be corroded to perforation in eight months. The high well head pressures of 2500 to 8000 psi makes any weakening of the well equipment by corrosion extremely hazardous. Bursting of the well equipment results in very expensive repair operations and may result in the loss of valuable production, loss of the costly well, or even loss of life. In November 1944, a gas-condensate well in a Gulf Coast field producing from 9500 ft showed a tubing leak. The well was "killed" by filling it with mud through the tubing, and then the tubing was pulled. Corrosion was found to have caused several perforations in the tubing, Fig I. While the mud was being circulated to kill the well, a high pressure jet from the corroded hole in the tubing perforated the casing and damaged the well to the extent that the cost of repairs amounted to $75,000. In November 1944, another gas-con-densate well in a Gulf Coast field producing from 11,400 ft showed tubing failure. This well had been producing an average of 2,500,000 cu ft of gas daily for two years. In the workover of this well, it was found that a hole one inch in diameter had corroded through the tubing and that corrosion had reduced the wall of the tubing to less than half the standard thickness over large areas of the interior of the tubing. It was found that corrosion had also caused two leaks in the casing. After four months spent in an attempted workover failed to make the well safe for further production, the well was plugged and abandoned at a total loss of $300,000,00.

Jan 1, 1948

By P. L. Menaul, P. P. Spafford

This paper discusses the most dangerous form of corrosion encountered in condensate-well oil production, the discovery of the agent causing this corrosion and the remedial chemical treatment proved effective by field use. The injection of ammonium hydroxide, even as little as one quart per day, has proved effective in preventing gas-condensate well corrosion. The injection of "Bone oil" is applied to wells producing brines containing calcium and magnesium salts. Introduction The severe corrosion of equipment in high pressure gas condensate wells has been a problem for several years and numerous papers have been presented on the subject. The term "gas condensate" or "distillate well" is applied to a distinct variety of hydrocarbon producing well, the characteristics of these wells being high bottom-hole (formation) pressures and temperatures and high gas production. These wells usually produce about 40 gal of water per million cubic feet of gas and the gas contains from 0.1 pct to 2 pct carbon dioxide. In the operation of this type of well, the operators soon noted severe internal corrosion of the pipe carrying the production. In some instances the dl tubing has been found to be corroded to perforation in eight months. The high well head pressures of 2500 to 8000 psi makes any weakening of the well equipment by corrosion extremely hazardous. Bursting of the well equipment results in very expensive repair operations and may result in the loss of valuable production, loss of the costly well, or even loss of life. In November 1944, a gas-condensate well in a Gulf Coast field producing from 9500 ft showed a tubing leak. The well was "killed" by filling it with mud through the tubing, and then the tubing was pulled. Corrosion was found to have caused several perforations in the tubing, Fig I. While the mud was being circulated to kill the well, a high pressure jet from the corroded hole in the tubing perforated the casing and damaged the well to the extent that the cost of repairs amounted to $75,000. In November 1944, another gas-con-densate well in a Gulf Coast field producing from 11,400 ft showed tubing failure. This well had been producing an average of 2,500,000 cu ft of gas daily for two years. In the workover of this well, it was found that a hole one inch in diameter had corroded through the tubing and that corrosion had reduced the wall of the tubing to less than half the standard thickness over large areas of the interior of the tubing. It was found that corrosion had also caused two leaks in the casing. After four months spent in an attempted workover failed to make the well safe for further production, the well was plugged and abandoned at a total loss of $300,000,00.

Jan 1, 1948

By G. Biles

The Eskay Creek Mine, a high-grade gold and silver underground mine in northwestern British Columbia started operations in late 1994. For the first three years of operation, ore was crushed to minus 2 inch; blended to satisfy smelter terms and direct shipped to smelters in Japan and Canada. Before commencing the above operations, preliminary evaluations had indicated that an extremely complex metallurgical facility, requiring a large capital investment, would be required to recover the precious and other economic metals. Subsequently markets for raw ore were identified and underground mining and ore transportation operations, at a nominal production rate of 300 tonnes per day, were commenced. Exploration diamond drilling in 1995 and 1996 discovered additional lower grade mineralized zones, which are less economic or uneconomic as direct shipping ore. Testwork demonstrated that these lower grade zones could be upgraded to marketable concentrates in a simple flotation mill. The mill was built in 1997 and has been in operation since late 1997. The mining rate now has increased to 400 tonnes per day including 250 tonnes per day of the direct shipping ore and ISO tonnes per day of the mill ore. Prime Resources Group Inc. wholly owns the Eskay Creek Mine. Homestake Canada Inc. owns 50.6% of Prime's shares and manages and operates the mine on Prime's behalf. This paper discusses the mining and milling operations as well as ore shipment and smelter contracts' administration.

Jan 1, 1999

By Ren G. Dong, Jay Kim, Daniel E. Welcome, Won Joon Song, Charles Hayden

Prolonged, extensive exposure to hand-transmitted vibration could cause a series of vibration-induced disorders in the vascular, sensorineural, and musculoskeletal structures of the human hand-arm system, which have been collectively called hand-arm vibration syndrome (HAVS).1 To assess the risk of HAVS the international standard ISO 5349-1 (2001)1 recommends using the root-mean-square (rms) acceleration of the measured vibration with a frequency weighting. While a few epidemiological studies have reported results consistent with the predictions made according to the recommendation, many other studies have reported results with large discrepancies.2 This may be partially attributed to the time-averaging effect involved in calculation of the frequency components, especially for impact type tools. Because the spectral characteristics of impact tools change dramatically with time, a time-frequency (T-F) analysis can provide better characterizations of such highly transient vibrations. The analytic wavelet transform (AWT) is an ideal T-F analysis tool because it possesses the advantages of both the Fourier transform and the wavelet transform.3 The objective of this study was to explore the application of the AWT method for characterizing the impact tool vibrations and assessing their exposure risk. Methods Five tools (two chipping hammers, two riveting hammers, and one concrete cutting saw) were used in this study. The saw vibration was measured when it was used to cut a section of road pavement during a repair. The vibrations on the other tools were measured by the procedure specified in ISO 8662-2 (1992).4 A sampling rate of 16,386 Hz was used in the measurement. The AWT and Fourier analysis were applied to these signals and to identify their characteristics. Results Figure 1 compares the T-F characteristics of the accelerations measured from the relatively steady concrete saw and a riveting hammer. The frequency weighting specified in ISO 5349-11 was applied in the calculations. The comparison clearly shows that the two tools have completely different T-F characteristics.

Jan 6, 2006

By L. Donovan Clark

The term "powder factor" is almost universally accepted as the measure of the efficiency of a blasting program. It represents the economics of blasting since it designates quantity of explosive (thereby providing quality control in rock fragmentation) in terms of the associated volume broken. It is the wide use of this concept that explains the interest shown in an approach to rock blasting preferred by A. W. and Z. W. Daw* in a treatise on 3 blasting (1) substantiating its use in the form, Q = CVW3 for single shot hole, where Q = quantity of explosive lb Cv = blasting coefficient W3 = unit volume of rock It is obvious that the term Cv could also be called the apparent powder factor should the equation be written in the form, Cv = Q/W3 (lb per cubic unit). However, while the approach was ingenious** and the practical applications straightforward, their original, rather limited experimental work, along with certain assumptions, was questioned.

Jan 1, 1970

By J. A. Procarione, M. K. McCarter, Bradley C. Paul

A numerical technique is described which can be used to model the quantity and distribution of air flow through broken rock. The method can also describe gas concentration and temperature distribution. A computer code implementing the numerical approach was developed to assist in determining the feasibility of a proposed modified in-situ leaching method for extracting copper from sulfide porphyry deposits. This mining method requires air to be forced through cells of rubblized ore. The flow serves to supply oxygen for the leaching reactions and to dissipate heat that would other-wise build due to the exothermic reactions. The method substitutes the Carman equation into the Laplace equation. The solution of the resulting non-linear formulation is done on a finite difference grid using SOR with iteration improvement of coefficients. This procedure yields the required air flow pattern and pressure drop. An equation for advection with absorption is then solved over the same grid using explicit schemes to yield oxygen concentration. Finally, a similar technique is applied to the convective heat transfer formula to yield the temperature profile. The model is potentially applicable to such mining problems as the prediction of leakage through caved ground, the prediction of methane concentration in gobbed ground, and the prediction of heat build-up in caved workings.

Jan 1, 1989

Erwin S. SperRy, Bridgeport, Conn.: The analysis of refined copper is a subject of great importance, and has not received the attention it deserves. Copper metallurgists, therefore, will welcome the paper of Mr. Heath with satisfaction. The state of the art of the chemical analysis of copper has been such that consumers, if they could not afford to run any risk, have been obliged to buy copper from the smelter having the best reputation, and a specification for copper to meet certain requirements could not be drawn up by the mere giving of the chemical constituents. Mr. Heath has brought the analysis of the copper to such a state that when a specification calls for copper " equal to Lake copper " one will know immediately what percentage of the pure metal to expect. It seems to be a pretty well established fact that the copper of Lake Superior is practically free from antimony and bitmuth ; and, with the exception of arsenic, the other elements are easily separated from copper by electro-deposition in an acid solution. The authorities differ in regard to the question whether antimony is deposited with the copper in an acid solution. Classen* recommends the employment of a solution containing 10 per cent. of free nitric acid, sp.gr.1.21, and the strength of the current from 0.3 to 0.4 ampere, in order to prevent the other metals from being deposited with the copper; and for this reason, I presume, the method has been generally used. I, myself, have been accustomed to use such a solution for the analysis of copper-alloys, but have found that for such alloys only a small quantity of nitric acid is necessary, if sulphuric acid is present in sufficient amount to give the solution the required conductivity.

Jan 1, 1898

By Jean M. Bouvet, Pierre M. Vuillaume

There is not just one ANFO: ANFO explosive behaviour depends significantly on the blasting conditions and on its physico-chemical characteristics. For instance, ANFO effficiency increases whereas AN porosity is higher and consequently loading density of the explosive is less. This can be argued against generally admitted ideas. Therefore, the efficiency of industrial explosives related to ANFO (for example "relative weight strength" or "relative bulk strength") is a tool that must be used with caution.

Jan 1, 1993

By William K. Tolley

The U.S. Bureau of Mines (USBM) is investigating hydrometallurgical processing techniques to recycle metals from semiconductors and other advanced materials. Cadmium and tellurium were recovered from mixed CdTe/CdS scrap produced in the manufacture of thin-film photovoltaic devices. Cadmium and tellurium dissolution was achieved using hydrogen peroxide in dilute sulfuric acid. Leaching the scrap in 2.2 N H2SO4 yielded 99% Cd extraction and 98% Te extraction. Sulfur remained in the leach residue primarily in the elemental form. Elemental tellurium was precipitated from the leach liquor by adding Na2S2O5. Cadmium sulfate was recovered by evaporation. A preliminary process evaluation suggests that the process may have economic potential. Alternative recovery schemes are discussed.

Jan 1, 1995

By V. O. Murray

Gentlemen: I'm glad to see the crowd that's here this morning, glad to renew acquaintances with many old friends, and if you'll look at the program you'll see a heading there which states that as President I have the honor and pleasure to be here to address the membership of this meeting of the Rocky Mountain Coal Mining Institute, this being the 49th regular meeting. The tentative schedule of this gathering lists on the program the "President's Address," and I want to assure you that this will not be an address or a lengthy speech. It's said that a good speaker is one who arises to the occasion and then promptly sits clown, so please be at ease for I intend to sit clown very soon. There are other men here who have spent time writing and preparing papers on subjects that are to come up for discussion at this meeting, which will be, I'm sure, more interesting than what I have to say this morning; so again I'll say, we'll get this part of the program under way promptly.

Jan 1, 1953

By Frank F. Rahne

Butler Taconite, operated by the Hanna Mining Company, is an Iron ore pelletizing operation that is located on the Western end of the Mesabi Iron Range in Northeastern Minnesota. The operation mines low-grade taconite ore and through primary crushing, two stage grinding, magnetic separation, agglomerating and indurating, produces 2.6 million annual tons of high quality, 66% iron pellets. Mining and stripping is done with 13 - M100 trucks and 5 - 12 cu. yd. shovels. The operating processes in the concentrator and pellet plant are primarily con¬trolled through a centralized control room and monitored by a PDP l140 computer. During 1969 and 1970, a re-organization of the Company took place. Through this re-organization, each mine unit was analyzed and studied to determine the proper staffing of the internal departments. At this time, it was decided to continue with further detailed studies of the Maintenance Department with the intent to reduce maintenance costs. Maintenance costs at the time of the re-organization were 38.6% of the total mine operating cost. The preliminary study indicated that the Maintenance Department had a system of maintenance, as a matter of fact, it had a separate system in each sub-maintenance division and in some of the sub-divisions each foreman had a system of his own. Therefore, from the data collected, it was decided to develop one system of maintenance that could be utilized throughout the entire operation. To determine the type of system suitable to all phases of the operation, detailed time and method studies were conducted. All types of maintenance tasks performed at the operation were studied. The data collected was analyzed and the recommended improved methods were reviewed with the Maintenance Superintendent and his staff. The new improved methods that were accepted as feasible, were introduced into the system immediately.

Jan 1, 1975

By Rodney T. Jones

DC arc furnaces were first used industrially for the reductive smelting of chromite fines to produce ferrochromium thirty years ago. Since then, they have been used for a variety of applications, including the smelting of ilmenite to produce titania slag and pig iron, the recovery of cobalt from non-ferrous smelter slags, and the smelting of nickel laterite ores to produce ferronickel. The power of these furnaces has increased from 12 MW to 72 MW for ferrochromium, and to 80 MW for ferronickel. The largest of these furnaces requires two electrodes to carry sufficient current to generate this much power. A review is presented of various DC arc furnaces in use, along with a discussion of the likely ways in which furnace power might be increased further in the future.

Jan 1, 2014

By M. J. Allan, D. J. Barratt

This paper reviews current testing methods for sizing autogenom and semiautogenom mills in the North American context with comments on the necessity for test work and requirements for different circuits and equipment selection. The economics of testing and the value received are discussed.

Jan 1, 1987

By A. B. Hooker, Iilsley. L. C.

"Flame safety lamps have been used for about one hundred years in coal mines where a dangerous accumulation of explosive mine gas (methane) might occur and thus render the use of ordinary unprotected flame lamps dangerous. Flame safety lamps are not only used for illumination, but also for detecting the presence of dangerous percentages of methane mixed in the air of the mine.The safety of the lamp depends chiefly upon the cooling qualities ofThe safety of the lamp depends chiefly upon the cooling qualities of the wire gauze used to permit free circulation of the air through the lamp. If one enters a part of the mine where methane is present in the air, the methane enters the lamp and coming in contact with the wick flame is ignited and continues to burn within the gauze without igniting the methane surrounding the lamp. If the air within the mine is traveling at a velocity of several hundred feet per minute the burning gases may be driven through the gauze by the air current. If the gauzes are properly designed and of the proper material, these burning gases will be so cooled as they pass through the gauze that they will not cause an ignition of the gas surrounding the lamp. In order to test the effectiveness of a given safety lamp, tests are made in moving explosive mixtures of gas and air arranged to simulate mine conditions.The Bureau of Mines investigated many features relative to the safety of flame lamps and in 1915 established an official schedule known as Schedule 7 whereby flame lamps having certain prescribed qualifications would be approved as permissible for use in gaseous mines."

May 1, 1920

By Greenleaf W. Pickard

The Parral mining district is located in the southern part of the state of Chihuahua in north-central Mexico, in the border area of the physiographic provinces of the Mesa Central and the Sierra Madre Occidental, at an average elevation of 1700 meters. This is one of the most highly productive lead-zinc districts of Mexico. The principal operating units are the Prieta, Santa Barbara and San Francisco mines. The Santa Barbara-San Francisco del Oro area is located 25 kilometers to the southwest of the Prieta mine. It has a system of generally narrow veins in fault zones, entirely in the shale series. The Santa Barbara veins follow long, persistent fractures, while the San Francisco del Oro veins are in relatively short fractures. The Veta Colorada structure, located 5 kilometers to the northwest of the Prieta mine, was a major producer of high grade silver ore with low lead-zinc content during the eary 1900's. It follows a major north-south fault zone in andesite and is noteworthy for a number of wide oreshoots of limited vertical extension along its 10 kilometer length. The Palmilla and Esmeralda mines are on the south end of the Veta Colorada structure. Numerous smaller mines are operating in the Parral area. During the last 45 years the Prieta mine has produced approximately 15,000,000 tons of complex sulfide ore, principally from one single vein. Extensive stoping has

Jan 1, 1970

By Kenneth N. Weaver

Introduction and Historical Background State Geological Surveys have been deeply involved in industrial minerals from their inception beginning in the first half of the 19th Century. To Massachusetts belongs the credit of having carried out the first Geological survey under state auspices on the Western Hemisphere. One of the causes leading up to this survey was. Governor Lincoln's message to the legislature of May 29, 1830, from which I quote in part: "Much knowledge of the natural history of the country would thus be gained (from a geological survey), and especially the presence of valuable ores, with the localities and extent of quarries and of coal and lime formations, objects of inquiry so essential to internal improvements and the advancement of domestic prosperity, would be discovered.". Similar phraseology is present in practically all of the initial organic acts creating the first State Surveys. High on the list of priorities for these embryo surveys was an inventory of the mineral resources of the State with particular emphasis on the industrial minerals. Prom these early beginnings, the state surveys have developed a great wealth of geological data either directly or indirectly relating to the development of mineral resources. One can gain some conception of the effort that state surveys today place on industrial minerals studies by noting the projects in which they are engaged as reported in the State Geologists Journal. In 1970, for example, approximately

Jan 1, 1972

By J Benn, V Kuznetsov, G Timms, A Spain

Earthen covers are now widely used in the mining industry to control the generation rate and/or release rate of low quality drainage from piles of sulfidic minewastes. Covers are usually designed to reduce the water infiltration rate and in some cases may also reduce the oxygen flux to the underlying sulfides. Engineered covers have only been used since the 1980s, however, and there is very little field data on their performance in the longer term. This lack of information has implications for the degree of confidence that can be placed on the predictions of the environmental impacts of sulfidic minewastes, for the acceptance of close-out criteria by regulatory authorities and for the financial liability of the mining industry. Covers were placed on sulfidic waste rock dumps at the abandoned Rum Jungle uranium mine during 1984 - 1985. These covers were designed to reduce the water infiltration to less than five per cent of incident rainfall by both water shedding and storage-release mechanisms. Regular monitoring by the Australian Nuclear Science and Technology Organisation (ANSTO) demonstrated that the covers performed better than the design criterion for around ten years, but infiltration rates have subsequently increased. There is a 66 per cent probability that the infiltration rate now exceeds five per cent of incident rainfall. The cover on the largest pile, WhiteÆs heap, was sampled in pits dug at eight locations. Sampling was carried out at the end of the monsoonal wet season and again at the end of the ædryÆ season. This, together with laboratory testing, enabled cover performance to be assessed against five criteria: design, construction, cover material characteristics, physico-chemical characteristics and biological characteristics. We are of the opinion that the design of the cover was suitable to achieve the objectives of stability, water shedding, storage-release, and provision of a substrate for vegetation growth. Over most of the surface of the heap, the construction of the covers, drains and erosion prevention structures was in accordance with design specifications. However, several small and localised bare patches on the upper surface of WhiteÆs heap coincide with a reduced cover thickness, which is likely to have been due to poor construction in those patches. The construction of covers on minewastes is dependent on an adequate source of material meeting design specifications. From our limited examination, it appears that there was shortage of material for each of the three zones û a lower impervious clay layer, the moisture storage-release layer and the upper erosion-resistant layer for vegetative growth. An indication of this was that the upper layers in some areas were observed to be thinner than specified. We are of the opinion that this shortage of suitable material has been responsible for some of the changes observed ten years after emplacement. Physical and geotechnical testing indicated that the cover materials no longer meet the original specifications. In particular, the permeability at the 8 locations was found to be greater than specified, by up to several orders of magnitude. The higher permeability may explain the higher observed rainfall infiltration and moisture content of the waste rock. This increased permeability appears to be due to a combination of biological and physical processes û galleries formed by termites and ants and an extensive system of shrinkage/desiccation cracks formed by the development of a polygonal blocky structure involving the entire lower clay layer. The desiccation cracks may fill with coarser illuviated materials and form a conduit through which roots access the underlying waste rock. Measurements were made of oxygen flux into the heap as cover layers were excavated in the pits. They indicated that the full cover currently reduces the oxygen flux to 20 - 23 per cent of that into bare waste and that this reduction seems to be proportional to the cover thickness. It was also found that the oxygen flux into the cover is about four times higher at the end of the dry season than at the end of the wet season and that the difference is due primarily to the difference in moisture content of the cover. Recommendations are made for the design and construction of covers.

Jan 1, 2003

By M. Allan Holtz

The shipment of coal, ores, and minerals in bulk form during the winter months presents a difficult problem in emptying rail cars. U. S. Steel Research in cooperation with U. S. Steel Coal Operations bas laboratory tested and field monitored the effectiveness of using freeze conditioning agents (FCA) to minimize the frozen coal problem. This report examines, in an overview manner, our experience after four seasons of treatment using different FCA agents on raw and preparation plant products. Our observations indicate that if an FCA is applied correctly it is effective mineral to mineral. Freezing problems still occur at the interface between the coal and the metal of the car sides and bottoms. Leading chemical suppliers have made positive improvements in their FCA formulations with second and third generation products. Further advances are needed to make chemical treatment for the prevention of frozen coal a real full-proof method.

Jan 1, 1980

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