Search Documents

CONTENTS PAGE THOENEN, J. R.-Limestone Production as a Mining Problem. Discussed by Oliver Bowles, J. T. Singewald, S. R. Russell 1 GRIGGS, C. C.-Engineering in Limestone Production. Discussed by W. C. Phalen, John Rice, Samuel M. Shallcross, Oliver Bowles, Nathan C. Rockwood, George Milliron 2 WILDER, FRANK A.-Rotary Calciners for Gypsum. Discussed by L. K. Arm-strong 9 PORTER, JOHN J.-Manufacturing Problems of Cement Industry. Discussed by Samuel M. Shallcross 9 KIRKHAM, VIRGIL R. D.-Phosphate Deposits of Idaho and Their Relation to the World Supply. Discussed by F. A. Wilder, S. L. Willis, G. R. Mansfield, R. W. Stone, L. K. Armstrong 9 Limestone Production as a Mining Problem Discussion of the paper of J. R. THOENEN, presented at the New York Meeting, February, 1925, and issued, as Paper 1417-H, with MINING AND METALLURGY, February, 1925. OLIVER BOWLES, New Brunswick, N. J.-I am so thoroughly convinced of the growing importance of underground work in the production of limestone that I had the author make a detailed study of limestone mining for the Bureau of Mines and prepare a report on the principles of limestone mining. Many limestone operators, long accustomed to open¬pit work, are being forced to mining. About 6 months ago I thought there were twenty-five or thirty underground limestone operations in the United States but the author has been finding new ones until his list now runs nearer sixty. Some of these are very extensive; one at least has 4 ½ miles of underground workings. There is an ever-expanding field for the engineer in the operation of limestone mines and quarries. Some of the larger companies realize the need of skilled engineering advice, but many of the companies regard the engineer as an unnecessary expense. Although almost every metal mine, even those handling only a few hundred tons of ore per month, employs a mining engineer, many limestone operations ten times as large employ no mining engineers. Few mining engineers are at all familiar

Jan 6, 1925

By Edward W. Parker

At the Cleveland meeting of the Institute, October, 1912, I had occasion to call attention to the general though erroneous impression that the principal mining activities of the United States lie west of the 100th meridian of longitude. Few, I believe, realize that the States east of the Mississippi river, which comprise only 28.8 per cent. of the total area of the United States, exclusive of Alaska, contribute about two-thirds of the total mineral production, computing by values. In 1910 the percentage of the production credited to the Eastern States was 67; in 1911 it was 65. When I have, with becoming modesty, ventured to speak of these comparisons, I have usually been met with the rejoinder, " But you include coal." I surely do, for whereas coal (m petroleum, as natural gas, as limestone) is not in the strictly technical definition of the word, a " mineral," it is legally mineral, is certainly a mineral substance, and contributes by far the largest tonnage and approximately one-third of the total value of all mineral products. The production of coal-mines in 1911 weighed approximately 500,000,000 tons. In 1912 it exceeded that record by nearly, if not quite, 50,000,000 tons. According to H. D. McCaskey, of the U. S. Geological Survey, the total weight of all the metallic ores mined in the United States in 1911 was 105,000,000 tons (a little more than one-fifth that of coal). In 1910 Mr. Lindgren estimated the total weight of all metallic ores at 120,000,000 tons. The products of the quarries, clay-pits, oil-wells, phosphate-mines, and other non-metallic products, taken all together, did not in 1911 weigh in excess of 300,000,000 tons, so that the output of coal exceeds by 25 per cent. the combined tonnage of all other mineral products. The coal-mines give to

Jan 1, 1914

By E. M. Rogers

In hoisting from shafts of considerable depth, the dead weightdue to the accumulating length of cable is an important element, and has

Jan 1, 1889

By L. P. Bayvel

The method of spectral transparency was investigated. A device for measuring particle sizes based on this method was developed, tested and applied. The device affords measurements of particle size distribution in the range from 0.1 to 4 µm. It proved possible to measure sizes not only of spherical particles but also of non- spherical ones. The spectral range in which it is necessary to determine transparency for particle size measurements was found.

Jan 1, 1980

By AIME AIME

UNQUESTIONABLY the Coal Division has never had a meeting in which so many outstanding technical papers were presented of immediate practical application to problems of personnel, mining, safety, preparation, combustion, and carbonization. Should there have been those present with the lingering idea that all that was needed for success in the coal industry was a strong back and a weak mind they must have had a rude awakening.

Jan 1, 1942

By E. C. Rudolphy, M. E. Potter, J. R. Mitchell

The effects of 0.006 to 0.20 pet Sn ml the hot workability and the annealed mechanical properties were investigated for Types 302, 410, and 430 stainless steel. The hot workability of these steels was not significantly affected by their tin content within the range studied, although some effects on mechanical properties were noted. Apart from the effect of tin, optimum hot-working temperatures and V-notch Charpy impact transition temperatures for these grades were determined. HIGH tin residuals in some heats of stainless steel have been blamed for the poor hot workability, particularly during secondary mill rolling. However, very little quantitative information has been available. Previous work1"6 with carbon steels indicates that tin increases tensile strength and hardness but de- creases tensile and impact ductility. Halley,7 in reviewing the sources and effects of residual elements in carbon and alloy steels, concluded that much of the surface checking (hot shortness) encountered in rolling was caused by copper, and that tin, arsenic, and antimony combined with copper to form low-melting constituents which further increase the steel's sensitivity to hot shortness. These elements had little effect in the absence of copper. A more recent paper by Langenberg and Johnson8 concluded that tin reduces hot workability but that researchers disagree concerning the amounts which will cause trouble. They state that laboratory investigations with small ingots seem to indicate a higher tolerable level of tin than do statistical studies of mill data, and also that statistical analysis of mill data indicate that small amounts of residual tin are detrimental to the surface quality of stainless sheet. The accumulative increase in the general level of tin and other tramp elements in steelmaking materials will present greater problems to steelmakers in the future. The purpose of the present study was to obtain quantitative information on the specific effects of tin on the hot workability and mechanical properties of such common stainless steels as Types 302, 410, and 430.

Jan 1, 1962

By John C. Smock

While I was engaged in the preparation of a catalogue or list of mineral localities of the United States, east of the one hundredth meridian, for the U. S. Geological Survey, the thought occurred to me that an arrangement or classification of the iron-ore districts of the eastern part of our country according to their geological horizons would be an interesting topic for a paper, and would furnish a basis upon which to arrange many facts brought out by the constant development of our iron-mining districts. Our text-books of mineralogy, geology, and ore-deposits describe the iron-ores and the

Jan 1, 1884

By Lester Strauss

The fact that the loss of silver in the slag of the smeltingprocess increases with the amount of silica in the furnacecharge, was probably the ground of a general opinion that the silver is present in the slag as a silicate. Dr. Iles, in his inter-

Jan 1, 1901

The D'Arcy Exploration Company Ltd. has been granted prospecting licenses in Great Britain to explore four different types of prospect. In the south of England (Dorset, Hampshire and Sussex) the objective lies in Jurassic and Lower Cretaceous beds. In an area of approximately 4470 sq. miles, covering parts of Nottinghamshire, Lincolnshire and Yorkshire, the search is directed to testing Carboniferous rocks. In northeastern Yorkshire a single license covers structures in which the Permian limestone will be explored. In Scotland, southeast of Edinburgh, the company holds another single license where Lower Carboniferous horizons are the objective. Southern England Among the more important "indications" that led D'Arcy Explora-tion Company Ltd. to undertake a testing program in southern England was the discovery of sands in the Wealden (Lower Cretaceous) series of Dorset, impregnated with oil residues. Traces of oil and bitumen were also found in limestones of the Portland and Purbeck beds of the same area. In addition, traces of petroleum had been recorded from Upper and Lower Jurassic beds in borings, more especially those drilled in the course of coal exploration in Kent and Sussex, and an outcropping oil sand was known to occur in Wealden beds near Pevensey in Sussex. Besides these tangible proofs that at least some oil has been generated in this area, _the Jurassic beds, as developed at outcrop in Dorset and elsewhere, include considerable thicknesses of strata that may well be considered as possible source rocks of petroleum. A regional view suggested that these possible source rocks extended, without great thinning, beneath at least the southerly parts of the Weald of Sussex, the South Downs and still farther south beneath the English Channel. It appeared, and still appears, a reasonable conclusion that, where suitable structural conditions occur in this tract of country, an oil accumulation of commercial value may be found. Of the several possible anticlinal structures, those at Portsdown (Hampshire) and between Henfield and Steyning (Sussex) were selected as sites for the first test wells. The groups of strata which at outcrop sug-

Jan 1, 1937

By G. T. Murray

The aging behavior of a Cu-Ti (3.2 at. pct Ti) alloy has been followed by electrical resistivity, hardness, and metallographic changes. The resistivity data indicate two principal processes, the first causing a sharp decrease in resistivity, and the second, which occurs over a long period of time, a much smaller rate of decrease. Lamellar nodules, Widmanstätten platelets, and homogeneous continuous precipitation was observed. The Widmanstätten platelets grow at the expense of the latter. When this study was initiated, little information was available on the aging behavior of copper-base titanium alloys. Several articles'-3 that appeared in the early 1930's showed that these alloys could be strengthened by precipitation, but a detailed study was not made. Within the past year, however, two other more comprehensive studies4'5 have been reported in the literature, one consisting primarily of an investigation of mechanical properties, the other

Jan 1, 1961

By O. N. Carlson, K. E. Solie

The brittle-ductile transition temperatures of single and poly crystalline chromium metal were studied as a function of nitrogen concentration and chromium nitride distribution. It was observed that In recent years there has been an increasing interest in chromium-base alloys for high-temperature applications. The principal disadvantages, however, have been the difficulties of fabrication and the design problems associated with a material of such limited ductility. Various studies have been the effects noted in the poly crystalline material are essentially reversed in the single crystals. These observations are discussed in terms of existing theories for the brittleness of chromium. conducted recently directed toward a determination of the cause of this brittleness and to find ways for minimizing its effects. Allen et al.,' Wain Abrahamson and rant,' and weaver4 have carried out studies on the effects of interstitial impurities on the brittle-ductile transition of chromium metal of various degrees of purity. These investigations have shown that oxygen has little or no effect on the transition temperature of chromium in all conditions studied but that carbon increases the transition temperature under all conditions tested. Nitrogen was found to increase the transition temperature in the wrought condition and in the quenched or cast conditionS but reportedly has no effect in the furnace-cooled condition.

Jan 1, 1964

By O. L. Kowalke

THE measurement and control of temperatures have assumed positions of great importance in many industries. The manufacturers of byproduct coke and carbureted water gas find that proper temperature control helps to produce a better product and economizes in the use of raw materials. In the manufacture of glass, enameled ware, brass, and high-temperature refractories, temperature control is now regarded as being coordinate in importance with the control of materials used. To control such processes as malleablizing cast iron, and hardening, tempering, and annealing of steel in a manner to meet exacting market requirements has, within recent years, involved the installation of large and expensive pyrometer equipments. In many of these installations, it was necessary not merely to measure but also to record the temperatures over a period of time and thus obtain a record of the entire heat treatment and an effective check on the workmen in charge. In view of the importance of temperature measurement and control in such a wide variety of industries and the necessity for proper supervision of the installation and operation of the outfits, the following questions may be pertinent: What instruction is offered by the engineering colleges and what departments in the colleges are responsible therefor? The latest available catalogs of ten prominent engineering colleges east of the Mississippi River showed courses in high-temperature measurements given by the departments of physics. These courses, in general, were described as comprising classroom and laboratory instruction in the theory of high-temperature measurements, together with exercises in the calibration of the various devices used. In some cases it was stated that consideration would be given, in the courses, to the practical applications in the industries. In only one. college was the course required of all engineering students; in most colleges it was optional; in a few colleges, it was required only of certain groups. In colleges offering a course in metallurgical engineering, instruction in pyrometry was always given in connection with metallurgical laboratory work. The students in ceramic,

Jan 8, 1919

By T. F. Witherbee

In the sections, Figures 1, 2, and 3, are shown three crucibles that have been applied to substantially the same furnace, all the conditions having been the same except a variation of one foot of bosh, and a slight variation in the angle of the same. The bosh of No. 3 was originally the same as No. 2, the additional foot in diameter being the result of three months' cutting. Beginning with No. 1, which mas 5 feet 6 inches diameter, with tuyeres 5 feet 4 inches high, and cinder-tap four feet from bottom, great trouble was found in holding iron a proper length of time, four hours being the outside limit when working well, and two hours or less if working badly. "Break-outs" through the iron

Jan 1, 1880

By J. F. Kemp

PAGE Introduction,............170 I. The Competence oF the Igneous Rocks to Supply the Materi als oF Veins,...........171 The Demonstrated Presence of the Metals in the Igneous Rocks,. . 171 The Presence of the Metals in the Sedimentary and Metamorphic Rocks, 173 Conclusions,...........175 The Abundance in Igneous Racks of Vapors or Dissociated Gases which will Yield Water on Emission and Cooling,. 175 The Sequence of Eruptions,. .. . 1 . • .. 78 The Sequence of Vein-Formations,.......1 79 Contact-Metamorphism,.........180 Pegmatites,............181 Frequency of Pneumatolitic Minerals in Veins,.. 183 Surface-Flows of Igneous Rock Unfavorable to Vein-Formation,. . 183

Jan 1, 1902

By Carle Hayward

THE effect of copper on steel has been studied by numerous investigators. Before modern testing methods had been developed, blacksmiths noted red shortness in iron, the cause for which was ascribed to the presence of copper. Numerous papers have been published on the corrosion of steels containing various amounts of copper, and a few writers have discussed the effect of copper on the mechanical properties of steel. The purpose of the investigation described in the following paper was to obtain additional data on the mechanical properties of medium-carbon steel containing small quantities of copper. Among those who have published results of mechanical tests on copper steels are Ball,1 who states that copper increases the tensile strength and 'hardness but lowers the elongation. Stead2 states that copper steels closely resemble nickel steels containing equivalent percentages of nickel,, as regards tensile strength, resistance to shock, corrosion and hardness. Wigham 5 found that copper in small amounts had no injurious effect on steel. Breuil4 found that with 1 per cent. carbon, copper lessened the brittleness of steel and in low-carbon steel it increased the tensile strength and lowered the ductility slightly. H. H. Campbell 5 states that copper up to 0.25 per cent. slightly raises the elastic limit, elongation and reduction of area.

Jan 1, 1918

By W. P. Sykes

In an earlier paper1 the composition-temperature limits of the gamma iron phase in the iron-tungsten system were reported as approximated by thermal analyses. At that time no attempt was made to develop metallographic evidence of the coexistence of two phases in the iron-rich solid solution at temperatures between 900" C. and 1400" C.

Jan 1, 1931

By Arnulf Muan, D. P. Masse

PHASE relations in the system CoO-SiO2 have been determined as a basis for further investigations of thermodynamic properties of olivine solid solutions involving Co2SiO4 as a component. Previous data on the system CoO-SiO2 are incomplete or uncertain. Biltz and Lemke1 determined the melting point of cobalt orthosilicate as 1345°C , but Asanti and Kohlmeyer2 have later found a considerably higher temperature, 1420°C. The latter authors also studied melting relations of one mixture on the CO side and two mixtures on the SiO2 side of the orthosilicate composition and sketched a tentative phase diagram for a limited composition range of the system. However, no phase identification was carried out, and the authors left unanswered the question of the possible existence of a stable meta-silicate phase. Greig3 showed that a 90 wt pct SiO2-10 wt pct Co mixture at 1725°C consists of two immiscible liquid phases. The quenching technique was used in the present investigation. Mixtures of high-purity cobalt oxide ("Fisher Certified") and dehydrated silicic acid ("Baker Analyzed") were equilibrated in air atmosphere. The samples were then quenched to room temperature and the phases present were identified by microscopic and X-ray examination. The samples were kept in small envelopes made from thin (0.0004 in.) platinum foil. Thermodynamic data which have become available recently for Pt-Co alloys4 were used to check that the losses of COO from the oxide samples by alloying of cobalt with platinum in the present investigation were too small to change significantly the compositions of the oxide material during the equilibration. A vertical tube furnace with an 80 pct Pt 20 pct Rh resistance winding was used in runs up to 1510°C. Temperatures in these runs were measured with a Pt vs 90 pct Pt 10 pct Rh thermocouple calibrated against the melting point of diopside (CaMgSi2O6, 1391.5?C). The given temperatures as measured by this technique are estimated to be accurate to *5°C. Quench runs at temperatures above 1650°C were made with a modified Roberts and Morey5 strip furnace, using strip resistors composed of a 60 pct Pt-40 pct Rh alloy. Temperatures were measured with an optical pyrometer which was calibrated against the liquidus temperature of a mixture composed of 10 wt pct CaO, 90 wt pct SiO2 (1707°C). The temperatures measured with this technique have an estimated accuracy of +15°C. The results are shown graphically in Fig. 1. Only one intermediate phase, the orthosilicate Co2SiO4 with olivine-type structure, is stable in addition to the end members cobalt oxide and silica. The melting point of the orthosilicate was found to be 1415" ± 5°C. The metastilicate CoSiO3 is not stable at the temperatures of the present investigation. The two eutectic points in the system CoO-SiO2 where COO plus olivine, and olivine plus silica, coexist with liquid were found to be 72 wt pct COO and 1407°C and 63 wt pct COO and 1381°C, respectively. The melting point of cobalt oxide in air was taken as 1745?C, based on the previous data of Aukrust and Muan.6 Within limits of error (+ 5?C), identical eutectic temperatures to those determined in air were found when two representative mixtures were equilibrated at 1 atm O2 pressure and in an atmosphere of 84 vol pct CO2, 16 vol pct H2. This suggests that changes in oxidation state of cobalt in the condensed phases are not significant as far as their effect on the phase relations are concerned. This inference was substantiated by failure to detect7 any "excess oxygen" (i.e., oxygen in excess of that contained in Co2SiO4) in a sample of orthosilicate composition equilibrated in air 10°C above the liquidus temperature and subsequently quenched to room temperature. This work was carried out as part of a research program sponsored by the U.S. Atomic Energy Commission under Contract No. AT(30-1)-2781.

Jan 1, 1965

By L. S. Darken

It has been known for sometime that in an ionic lattice, such as that of Ag,S or FeO, the migration velocity of the anion may differ markedly from that of the cation, the cation being usually the more mobile. It has been shown, for example, that during the formation of silver sulphide tarnish on silver, the tarnish layer grows principally by the motion of silver cations through an essentially stationary silver sulphide lattice. Similarly, the growth of wüstite scale on iron proceeds principally by motion of iron ions, this being accomplished with the aid of vacant iron lattice sites into which the iron may readily move. Likewise investigations of solid solutions of various salts show that there is usually considerable difference in the mobility of the different cations. Measurements of the mobility of various metals in liquid mercury indicate that the various metals move at different rates relative to the mercury. In view of the foregoing it seems reasonable to suppose that when any single phase solution is acted upon by a field, the atoms of different elements respond in different ways; in particular, that the force arising from a particular concentration gradient in a binary alloy would cause the atoms of one component to move with a drift velocity which is in general different from that of the atoms of the other component. The recent experiments of Smigelskas and Kirkendall' support this viewpoint, since they found, in essence, that during diffusion in alpha brass zinc moves appreciably faster than copper. This was evidenced by the relative motion of inert molybdenum wires. Such a phenomenon is incompatible with the place interchange theory of diffdsion proposed by several authors, most recently by Bir-chenall and Mehl.2 This theory has, however, also been questioned3v4 for other reasons, principally because of the high energy required for direct atomic interchange. The rather large difference between self-diffusivity, as determined by tracer technique, and mutual diffusivity, as determined with the aid of another element at low concentration, might also be interpreted as favoring the above idea; however. Birchenall and Mehl have pointed out that there is another possible interpretation of this difference; this is discussed later. A rather interesting and pertinent observation was made by Schwartz, who noticed that tungsten lamp filaments, heated by direct current, commonly fail by necking down in the region at the temperature gradient near the positive end, with a concomitant swelling at the corresponding position near the negative end. He introduces considerable auxiliary evidence to show that this phenomenon is occasioned by the motion of tungsten cations which migrate in the high temperature region from the positive end toward the negative end. The mechanism of this migration is not clearly understood. If, however, this experimental evidence be accepted, we are forced to conclude that alloying elements in the tungsten may migrate by the same or a Similar mechanism, whatever it may be, at a greater Or lesser rate, thus giving rise

Jan 1, 1949

By L. S. Darken

It has been known for sometime that in an ionic lattice, such as that of Ag,S or FeO, the migration velocity of the anion may differ markedly from that of the cation, the cation being usually the more mobile. It has been shown, for example, that during the formation of silver sulphide tarnish on silver, the tarnish layer grows principally by the motion of silver cations through an essentially stationary silver sulphide lattice. Similarly, the growth of wüstite scale on iron proceeds principally by motion of iron ions, this being accomplished with the aid of vacant iron lattice sites into which the iron may readily move. Likewise investigations of solid solutions of various salts show that there is usually considerable difference in the mobility of the different cations. Measurements of the mobility of various metals in liquid mercury indicate that the various metals move at different rates relative to the mercury. In view of the foregoing it seems reasonable to suppose that when any single phase solution is acted upon by a field, the atoms of different elements respond in different ways; in particular, that the force arising from a particular concentration gradient in a binary alloy would cause the atoms of one component to move with a drift velocity which is in general different from that of the atoms of the other component. The recent experiments of Smigelskas and Kirkendall' support this viewpoint, since they found, in essence, that during diffusion in alpha brass zinc moves appreciably faster than copper. This was evidenced by the relative motion of inert molybdenum wires. Such a phenomenon is incompatible with the place interchange theory of diffdsion proposed by several authors, most recently by Bir-chenall and Mehl.2 This theory has, however, also been questioned3v4 for other reasons, principally because of the high energy required for direct atomic interchange. The rather large difference between self-diffusivity, as determined by tracer technique, and mutual diffusivity, as determined with the aid of another element at low concentration, might also be interpreted as favoring the above idea; however. Birchenall and Mehl have pointed out that there is another possible interpretation of this difference; this is discussed later. A rather interesting and pertinent observation was made by Schwartz, who noticed that tungsten lamp filaments, heated by direct current, commonly fail by necking down in the region at the temperature gradient near the positive end, with a concomitant swelling at the corresponding position near the negative end. He introduces considerable auxiliary evidence to show that this phenomenon is occasioned by the motion of tungsten cations which migrate in the high temperature region from the positive end toward the negative end. The mechanism of this migration is not clearly understood. If, however, this experimental evidence be accepted, we are forced to conclude that alloying elements in the tungsten may migrate by the same or a Similar mechanism, whatever it may be, at a greater Or lesser rate, thus giving rise

Jan 1, 1949

By E. J. Rapperport, J. P. Pemsler

The thermodynamic activities of zinc in six solid solution Cu-Zn alloys ranging from 5 to 35 at. pct Zn were determined experimentally in the temperature range 400° to 600°C. This low temperature investigation was canducted in order to evaluate techniques developed to utilize the inherently high sensitivity of atomic absorption flocesses in the measurement of thermodynamic activities. Analytical expressions ,for the activity and actizlity coeflcient are given for the six alloys in the temperature ranges investigated. RELATIVELY few experimental methods are available for investigation of thermodynamic activities of alloys, especially in the solid state. The techniques most frequently used have been the electrochemical potential and the effusion methods, both of which have severe limitations in many instances. It is therefore desirable to expand the ability to perform such measurements in order to obtain new information as well as to provide an additional independent verification capability. In this work, we present a significant improvement in the spectrophotometric method for sensing small vapor pressures in static absorption cells. Similar techniques have been used previously;1"5 however, applications had been limited to relatively high pressures, often greater than 1 torr. Prior investigators have, for the most part, used broad spectral sources such as xenon or mercury lamps, and high intensity arcs. Hollow cathode sources were first suggested in 1956 6 and were used soon afterwards.4'5 These sources offer significant improvements in sensitivity and freedom from interfering spectral lines.'-' EXPERIMENTAL High purity zinc was obtained from Cominco Products, Inc., and copper from American Smelting and Refining Co. Both elements were of 99.999 pct purity. Copper-zinc alloys were vacuum melted in a high fired carbon crucible with each alloy pulled from the melt as a 4 -in. diam bar. The bars were swaged to -1/4 in. rods and vacuum annealed for 160 hr at 800° + 1°C. Samples for gross chemical analysis were taken at intervals along the length of the rods to ascertain the axial zinc gradient. Electron microprobe analysis of homogenized specimens indicated that the alloys had uniform compositions over their cross sections on a macro (200 p) and micro (1 u) scale to better than *1 pct (20) of the gross composition. This tolerance was determined by counting statistics, rather than assured composition fluctuations. All SiO 2 windows were high-ultraviolet-transmission grade to minimize intensity losses. Silica absorption cells were scrupulously cleaned consecutively in organic solvents, dilute HF, and distilled water before use. The empty cells were then flamed while under a dynamic vacuum, cooled, and removed to an argon-filled glove bag. Alloy pieces were cut and filed in the glove bag to produce fresh surfaces, and then loaded into the cells. The loaded cells were temporarily sealed, removed from the glove bag, reevacuated to 10-5 torr or better, and permanently sealed. The instrument used is schematically shown in Fig. 1. The spectral emission from a commercially made hollow cathode lamp (A) of a selected element is focused through an absorption cell (B) inside a well-controlled furnace (C). The intensity of the transmitted beam is measured using the spectrometer* (D) 'Techtron model AA4 atomic absorption spectrometer. which contains a grating (E) that disperses the light prior to impingement on the photomultiplier (F). The monochromator grating is adjusted so that only the wavelength of interest is measured. The power supply delivered an interrupted voltage to the lamp, causing a chopped radiation output to be transmitted. The detector read only the intermittent component of radiation incident upon it, so that all continuous noise signals (furnace radiation, and so forth) were eliminated. Three recording thermocouples contained in the muffle furnace were positioned along the length of the absorption cell: one at each end and one at the center. An effort was made to keep the ends of the cell several degrees hotter than the center to avoid window condensate. Appropriate thermal corrections were then necessary to relate cell pressure to radiation attenuation. Water-cooled heat shields, as shown in Fig. 1, were found to aid signal stability by protecting the hollow cathode and the photomultiplier from furnace radiation. The furnace had a 2-in. diam muffle, Kan-thal wound, with SiO 2 windows at its ends to minimize convective effects. The hollow cathode radiation was masked and focused to form a conic beam that was a maximum of { in. diam within the furnace. Thus, the 1.5 in. diam absorption cell easily contained the entire beam. The furnace was mounted on ball-bearing slides with positive positioning detents. This arrangement allowed the removal of the entire furnace assembly from the radiation path, position [I], Fig. 1, so that frequent sampling of the unattenuated beam intensity could be obtained. In all cases the beam intensity was kept constant to 0.1 pct as judged by readings taken immediately before and immediately after data collection. Only data for absorptions of less than 80 pct were utilized, as systematic deviations from linearity were found for greater absorptions.

Jan 1, 1970