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By W. S. Pellini, F. N. Rhines

IN many of the otherwise well established alloy phase diagrams the solidus curves (temperatures at which liquid first appears upon melting) have not been located accurately, chiefly because the experimental techniques that have been most popular for determining solidus temperatures have been both cumbersome and subject to large errors. C. E. Homer and H. Plummer1 have described a sensitive and at the same time a very simple technique for locating the solidus curves in a number of alloys of tin. Their method consists simply in noting the temperature at which a specimen of the alloy ruptures under the influence of a light bending force. Although this method is not new, it has been little used for this purpose in the past; nevertheless, it appears so attractive in its possibilities of speed, simplicity, and precision that the investigations presently to be described were undertaken to verify its merits. The redetermination of the solidus and eutectic temperatures of the lead-antimony system was employed as a medium 0f experimentation. New values obtained in this way are believed to be sufficiently precise to warrant a revision of the currently accepted lead-antimony phase diagram (Fig. I). Determinations of the solidus of the lead-rich lead-antimony alloy series have been published by R. S. Dean2 and by E. E. Schumacher and F. C. Nix.3 Their points are represented in Fig. I. In their work the solidus was not located at antimony concentrations greater than 2 per cent; the curve was presumed to meet the eutectic horizontal at an antimony concentration of about 2.5 per cent. In the present studies the solidus has been traced to 3.5 per cent, where the eutectic horizontal is intersected (Table I and Fig. I). Within the range investigated by Dean and by Schumacher and Nix the agreement with their values is good. H. Seltz and B. De Witt,4 on the basis of activity measurements, have calculated that the intersection of the solidus and the eutectic reaction horizontal should lie at 3.86 per cent of antimony. The following determinations of the eutectic temperature have been reported: Roland-Gosselin,5 228°C.; Ewen,6 228°C.; J. E. Stead,7 247°C.; Campbell,8 228°C.; W. Gontermann,9 245° to 252°C.; R. Loebe,10 245°C.; E. Heyn and 0. Bauer,11 245°C.; H. Endo,12 250°C.; R. S. Dean,2 249° to 258°C.; E. Abel, 0. Redlich, and J. Adler,13 245°C.; W. Broniewski and L. Sliwowski,14 250° to 252°C.; H. Seltz and B. De Witt,4 250°C. A temperature of 249°C- appears to have been generally accepted in recent years; it is the value most frequently obtained by the method of cooling curves. Values below 249°C. have usually been obtained by inferior cooling-curve techniques; those above 250°C., by the method of heating

Jan 1, 1942

By George B. Clark

Many basic engineering principles of all four phases of mining operations, namely, prospecting, exploration, development, and exploitation, can be analyzed better in terms of quantitative geology. Geological data from both field and laboratory will also complement scientific methods now being developed. THE geological data emphasized so successfully in prospecting for new deposits, that is, structural controls, strength of solutions, and type of mineralization, are basically those required for successful exploitation. In the mining of newly discovered deposits the most economical methods should be employed as early as possible to keep the overall cost per unit produced at a minimum and to permit maximum extraction of valuable minerals. A crucial question is: How can geological data be translated into useful quantitative results which will aid in achieving this end? H. E. McKinistry' has suggested that a solution may be reached in one of two ways: 1—the usual approach, use of judgment based on experience; or 2—mathematical calculations and tests on models, both subject to certain limitations. He also suggests that in addition to better use of geology more case data and theoretical data are needed on which to base sound judgment. Further research, therefore, is necessary. Perhaps in this field the emphasis should be on more specialization in mining methods and ground movement by men with thorough training in physics, engineering, geology, and underground mining. These specialists would be equipped to point out the most economical and scientific methods of exploitation. Selection of a stoping method is governed by the amount and type of support a deposit will require in the process of being mined, or by the possibility of employing the structure of the deposit to advantage in mining the ore by a caving method. In addition to these factors there are others which almost invariably influence the choice of an economical method of mining:' 1—strength of ore and wall rocks; 2—shape, horizontal area, volume, and regularity of the boundaries of the orebody, and thickness, dip and/or pitch of the deposit and individual ore shoots; 3—grade, distribution of minerals, and continuity of the ore within the boundaries of the deposit; 4—depth below surface and nature of the capping or overburden: and 5—position of the de- posit relative to surface improvements, drainage, and other mine openings. In the final analysis it is usually necessary to disregard the less important of these factors to satisfy the requirements of the more important. Because of the variation of geological conditions throughout and surrounding the deposit, no mining method will be everywhere ideally applicable to the conditions encountered in one ore deposit. The immediate problem is to interpret the above physical characteristics of deposits in terms of geological characteristics. Very few quantitative geological data are available on the factors related to a choice of mining methods. However, there are many descriptive data in mining and geological literature which collectively show how important an effect details of geology have upon all phases of mining operations. The following categories of basic mining methods were investigated to establish the geological factors that have affected their successful application: 1— open stopes with pillars; 2—sublevel stoping; 3— shrinkage stoping; 4—cut-and-fill stoping; 5— square-set mining; 6—top slicing and sublevel caving; and 7—block caving. It should be noted that the first five of these methods are listed in the order of increasing support requirements. Mines were selected as examples only where geological descriptions were complete enough to warrant their use. A study of the geological factors involved in mining operations led to a choice of the following classifications, employed in Table I: 1—structural type of orebody; 2—dimensions (geometry); 3— country rock (type); 4—faulting, folding, and fracturing; 5—alteration of ore and rock; 6—type of mineralization; and 7—geological factors determining mining method (summary). Of these factors only one yielded results that can be defined from available data in a quantitative manner, i.e., dimensions of the deposit. These are the most reliable guides that can be used in selection of suitable mining methods. They are, in general, the properties of geologic structure most difficult to evaluate by studies of models, pho-toelastic studies, and other laboratory methods, all of which are at present more limited in their applications than the geologic method. Application of geology has proved a reliable guide in other phases

Jan 1, 1955

By William A. Kapp

INTRODUCTION Coal is being mined from beneath residential areas, structures, bodies of water and other surface features in the coalfields to the north, south and west of Sydney. The particular problems faced by mine operators in these areas vary considerably due to differences in the overlying strata, the variation in the depths of cover and also depend on the number of seams being mined. Detailed subsidence work first commenced in the Southern Coalfield in 1965 and is now being carried out over areas of extraction at roost collieries. The analysis of the results of the early investigations and of the work which continues in other areas has shown that there is a consistent relationship between subsidence and mine geometry and has led to a reliable empirical method for the prediction of subsidence. In addition, particular aspects of each of the studies in the Southern Coalfield results in a clearer understanding of strata movements and of the resulting subsidence. The features of a subsidence trough apply generally to all areas but the magnitudes of specific features vary according to the stratigraphy of the particular coalfield. The aim of the subsidence work is to quantify the effects of subsidence for a range of mining geometries and mining conditions to enable the maximum safe recovery of coal from beneath surface features. The importance of local subsidence investigations is becoming more evident to mine operators and to authorities or organisations with surface interests. The subsidence work also provides important information on the stabilities of pillars of coal which remain unmined between panels of extracted coal. These pillars are not extracted either because of poor mining or geological conditions, or because pillar extraction is not part of the particular mining operation. Subsidence studies over these coal pillars clearly establish whether the pillars have remained stable or have failed to support the overlying strata. With subsidence studies continuing over several years, it is possible to assess the stabilities of these pillars on a long term basis. BACKGROUND TO THE STUDY OF SUBSIDENCE Geographical setting Most of the black coal production in Australia comes from the Sydney Basin. The coal seams extend for approximately 350 km along the coast of New South Wales and inland for distances up to 150 km. The City of Sydney is located near the centre of the coastal extent of the Basin where coal has been mined at a depth of 900 m. The Sydney Basin is part of the Main Coal Province of NSW and is divided into several coal- fields. The Southern Coalfield to the south of Sydney contained 15 operating mines and produced 12.7 million tonnes of raw coal during the 12 months to June 1981. The collieries discussed later are shown in Fig. 1. The prominent topographical feature of the area is the Illawarra Escarpment which rises to 400 m above sea level, or 300 m above the coastal strip along the South Pacific Ocean. The escarpment is mainly sand- stone and the weathering of the cliff line has resulted in a covering of talus material at its base. Several collieries are located near the seams which outcrop along the escarpment. The city of Wollongong is located in a scenically attractive area on the coastal plain. The suburbs of Wollongong extend north along the coastline, south to beyond Lake Illawarra and west to the lower slopes of the escarpment. The Illawarra Escarpment forms the eastern boundary of the Woronora Plateau. On a regional scale the surface dips gently to the west and thus forms a watershed for the rivers, most of which flow in a general north westerly direction, sometimes forming steep gorges in the sandstone. These rivers join the Nepean and Hawkesbury River system and flow into the Pacific Ocean north of Sydney. Seven dam have been constructed over the Southern Coalfield (Fig. 1) and with one large dam further to the west, their stored waters provide the needs of the Cities of Sydney and Wollongong and the surrounding districts. A large part of the area affected by mining is the undeveloped bushland of the associated catchment areas. In general no special precautions have been required with respect to subsidence with the exception of the dam structures and stored waters. With the increase in coal mining activities and the expanding residential development south of the City of Campbelltown in the outer Sydney Metropolitan area, subsidence is becoming an increasingly important area of research. Structures which have been affected or considered are townships and extensive residential areas, buildings of historical importance, major tollways, and a high pressure natural gas pipeline. The subsidence effects of mining beneath natural features within national parks is coming under study as mining approaches these areas. Geological setting The coal seams of the Southern Coalfield lie within the Illawarra Coal Measures. They contain high rank coking coal used in the local steel industry and for export. The Bulli Seam is mined extensively through- out the Southern Coalfield with the lower Wongawilli Seam being second in importance with regard to coal production. The top of the Bulli Seam is taken to be the marker horizon between the Permian Coal Measures

Jan 1, 1982

By H. M. Morse

Mississippi, during the year 1941, experienced the greatest diversity of oil activity since the beginning of oil interest in the state—core tests for exploration, core tests for sulphur, continued drilling at Tinsley for production, and wildcatting, which brought to light two new oil fields and two new salt domes. There were 45 wildcat wells drilled in 1941, which showed greater results and findings geologically than the 85 drilled in 1940. Tinsley Oil Field (Yazoo County).—The Tinsley oil field, with its boundaries fairly well defined now, is 8 miles long and 3 miles wide at its widest point. During the past year 213 producing wells were completed, which brought the total number of producers in the field by the end of 1941 to 325 wells. Seven producing sands have been logged, with a total average thickness of 30 ft. of oil sand. The producing formations are the Selma, Eutaw and Tuscaloosa. The average total depth of the wells is 5012 ft. The average gravity of the oil is 35.4°. Production for 1941 was approximately 15,500,000 bbl. of oil. Vaughan-Pickens Oil Field (Yazoo County).—At the end of 1941 only three wells were Producing in this field, the fourth having been abandoned. The total production for the field for the year was approximately 250,000 bbl. of oil. The producing sand is the Wilburn, in the Eutaw formation. Cary Field (Sharkey County).—The British American Oil Producing Co. completed, on Sept. I, 1941, its F. B. Houston No. A-I well, sec. 23, T. 11 N., R. 7 W. It is

Jan 1, 1942

By H. M. Morse

Mississippi, during the year 1941, experienced the greatest diversity of oil activity since the beginning of oil interest in the state—core tests for exploration, core tests for sulphur, continued drilling at Tinsley for production, and wildcatting, which brought to light two new oil fields and two new salt domes. There were 45 wildcat wells drilled in 1941, which showed greater results and findings geologically than the 85 drilled in 1940. Tinsley Oil Field (Yazoo County).—The Tinsley oil field, with its boundaries fairly well defined now, is 8 miles long and 3 miles wide at its widest point. During the past year 213 producing wells were completed, which brought the total number of producers in the field by the end of 1941 to 325 wells. Seven producing sands have been logged, with a total average thickness of 30 ft. of oil sand. The producing formations are the Selma, Eutaw and Tuscaloosa. The average total depth of the wells is 5012 ft. The average gravity of the oil is 35.4°. Production for 1941 was approximately 15,500,000 bbl. of oil. Vaughan-Pickens Oil Field (Yazoo County).—At the end of 1941 only three wells were Producing in this field, the fourth having been abandoned. The total production for the field for the year was approximately 250,000 bbl. of oil. The producing sand is the Wilburn, in the Eutaw formation. Cary Field (Sharkey County).—The British American Oil Producing Co. completed, on Sept. I, 1941, its F. B. Houston No. A-I well, sec. 23, T. 11 N., R. 7 W. It is

Jan 1, 1942

By C. E. McWhorter

IN underground mining recent trends toward mining large tonnages of low-grade ore have created, among other things, a need for cheaper and more flexible ore transport. A relatively new development has been the adaptation of shaker conveyors to meet this need. Although widely used in coal mining, only in the last few years have shaker conveyors been used in underground metal mining. The equipment consists of a driving engine, either electric or air powered, upon which is mounted a drive trough supported in ball-bearing frames. The trough line, or conveying medium, is made up of a number of sections, each section connected to another, usually with bolts. The length of each trough section is controlled by the length that can best be handled underground, but is usually from 9 to 13 ft over-all. The length of a complete conveyor line is determined by the character and weight of material to be handled as well as by the size of the ore body. Trough lines vary in lengths from 100 to 300 ft and the trough has a cross-section area of 127 sq in., and is 22 in. wide by 6 ½ in. deep.

Jan 1, 1948

By D. L., Hayes

THE concentration of zinc ore in Wisconsin is a comparatively simple process, although it presents problems that must be overcome in an efficient manner in such a way that installation and operating costs are low. As the ore deposits are small, the first cost of the concentrating plant must be low; while the low margin of profit makes it necessary to have the minimum operating costs. The original mills were copied from those of the Joplin district, as most of them were built and operated by Joplin millmen. These served the purpose well; they made a clean concentrate, which was the chief requirement at that time, as most 'of the mines were' considerably 'richer than the average at the present time, and wages and supplies were also considerably lower. ' The apparatus used at present has changed very little in principle. . The grizzly opening has gradually been increased to 12 in. and sometimes no grizzly 'is used. The crusher, gradually grew in size, the largest crusher has -an opening of about 24 by 13 in. and a 7/8-in. throw on the. eccentric shaft.

Jan 1, 1921

Richard Moldenke, New Pork, N. P. (communication to the Secretary*):—Iu following the discussion of the specifications for cast-iron and finished castings, I mas strongly impressed with two points which might be ventilated to advantage more fully from the view of the practical foundry-man. First, the reasons why only silicon and sulphur were specified and not phosphorus, manganese and carbon; and second, why but little was said concerning the presence of iron oxide in the material.

Jan 1, 1905

By Bai Shiwie, Li. Guangyu

This paper presents the study in situ on stress field of rock mass in a large dam site. By means of two different measure instruments and the method of stress relief, a lot of measure in situ has been done, including stress measurement of three dimensions at ten points and two deep-hole stress measurements in the perpendicular boreholes which are 59.4m and 53m deep seperately, and the basic accordant results corresponding two methods have been got. In the process of the deep-borehole stress measurement we got the stress value in critical state in which cylindrical core would become core-disking in the high stress area, which was first got in the world. The maximum principal stress was up to 650 kg/cm2. The stress value obtained by test and the thickness of rock disks all basically accord to the analysis by mechanical mechanism of core-disking The plane linear elastic finite element analysis has been completed. Results of inverse calculation all ac- cord to the measurement results in four different positions. The whole outline of the stress field of dam site was delineated clearly.

Jan 1, 1982

By H. J. Struth

The benefits of proration of oil production were perhaps more concretely realized in 1932 than at any time since the oil industry adopted nation-wide production control. Reduced output of crude petroleum, which brought the daily average of the United States down to approximately 2,000,000 bbl. from a peak in 1931 of more than 2,600,000, had a telling effect on the trend of oil prices. Mid-Continent crude was advanced in price from 776, for 36-gravity oil, to $1.04 a barrel. California crude, of 26-gravity at Signal Hill, moved forward from 736 to 976 a barrel. Pennsylvania crude, the only exception to the upward trend, rose in price from $1.82 per barrel to $2.02, only to react to $1.72. This was due to local conditions which necessitated an adjustment to overcome competition from other areas of the United States. East Texas continued to exert a far-reaching influence on the crude and gasoline market during 1932. Despite the fact that oil prices were advanced in most fields, large quantities of oil were produced in East Texas in violation of state proration orders, and sold in the market at prices considerably below official postings. This created competitive conditions in the gasoline market that were felt by all refining centers of the United States. The quantity of gasoline produced from cheap East Texas crude was not large, but the volume was sufficient to influence prices in practically all sections of the country. Thus, while the industry's' economic situation showed visible improvement statistically, the unreported and unseen statistics originating in East Texas proved to be an insurmountable obstacle to the economic betterment that was otherwise apparently justified. Somewhat surprising to many was the fact that gasoline consumption was maintained within 10 per cent of the preceding year. Domestic consumption showed only a net decline under 1931 of about 8.5 per cent; exports dropped in volume to the extent of about 23 per cent. As a matter of fact, domestic gasoline consumption was only about 1.4 per cent less than it was in the predepression year of 1929. Exports, however,

Jan 1, 1933

By J. H. Brophy, S. J. Michalik

A constitution diagram for the system Mo-Ir has been determined. The maximum solubility of iridium in molybdenum is 16 at. pct at 2110ºC and decreases to less than 5 at. pct at 1500°C. The solubility of molybdenum in iridium is 22 at. pct. Three intermediate phases appear in the system: 8 MoJr, having the p-tungsten structure; a phase, a cornplex tetragonal structure; and the hcp ? phase. Metallography, melting point determinations, X-ray diffraction and fluorescence, and electron micro-probe unalyses were employed in establishing the diagram. PREVIOUS to the present investigation, the intermediate phases in the Mo-Ir system were identified, but no detailed account of the phase diagram has been reported in the literature. Raub1 investigated alloys of Mo-Ir over an extensive range of composition between the temperatures of 800º and 1600°C. The in-termetallic compound MosIr was found to exist with nearly pure molybdenum, as the solubility of iridium in molybdenum was not detectable parametrically in this temperature range. MO3Ir was found to be iso-morphic with a ß-tungsten type structure, having a parameter of 4.959Å. An intermediate hcp phase, designated as the ? phase, ranged in composition from 52 to 78.5 at. pct at 800ºC, and from 41 to 78.5 at. pct Ir at 1200°C. Parameters noted for the ? phase were as follows: at 42.7 at. pct Ir, a = 2.771i0, c = 4.4366, c/a = 1.601; at 78.5 at. pct Ir, a = 2.736A, c = 4.378A, c/a = 1.600. Molybdenum was found to be soluble in iridium up to 16.5 at. pct Mo (83.5 at. pct Irj, with the parameter of iridium increasing to 3.845A at the solubility limit. Knapton,2 who investigated alloys between 15 and 85 at. pct Ir, essentially agreed with Raub's data, but, in addition, found a a phase in as-melted alloys near 25 at. pcto Ir. The oaphase lattice parameters were a = 9.64Å, c = 4.96Å, c/a = 0.515. The a phase was replaced by the 8 -tungsten phase on annealing at 1600°C. Knapton concluded that the a was stable only at elevated temperatures, and placed the composition of the a phase at approximately 30 at. pct Ir. The intermetallic compound Mo3Ir, with a lattice parameter of 4.965A, was included among the 8-tungsten structures reported by ~eller.' Matthias and Corenzwit,4 and Bucke15 studied the superconducting nature of MosIr, and reported a superconducting transition temperature of 8.$K. The present investigation describes the phase relationships in the Mo-Ir alloy system determined by melting point measurements, X-ray diffraction and fluorescence, and metallography. EXPERIMENTAL PROCEDURES Alloys for the determination of the phase diagram were prepared from powders. Commercial 99.9 pct Mo from Fansteel Metallurgical Corp. and 99.9 pct Ir powder from J. Bishop and Co. Platinum Works were used. The powders were weighed to nominal compositions, mixed, and then pressed, without binder, into compacts weighing 4 to 6 g. These were presintered in uacuo between 1200' and 1400°C for 1 hr, to reduce the degree of spattering during subsequent arc-melting. The compacts were arc-melted in a nonconsumable tungsten electrode furnace six times on alternate sides on a water-cooled copper hearth in an atmosphere of zirconium-getter ed argon at 500 mm of mercury pressure. In almost all cases, this procedure yielded buttons of satisfactory homogeneity. The composition of all melted buttons were confirmed by X-ray fluorescent analysis using the experimentally determined ratio of the iridium La1 line intensity to that of the molybdenum Ka1 line as a function of composition. In this determination four alloys analyzed by wet chemical methods were used as standards. An uncertainty range of ±1 at. pct has been attributed to all indicated compositions. All heat treatments and solidus measurements were carried out in tantalum resistance heating elements in vacuum conditions of 10-4 to 10-5 mm of mercury. A detailed account of this procedure has been reported by Schwarzkopf and Brophy.8 In the heat treatment and solidus measurements of iridium-rich alloys (50 at. pct Ir or greater), a tungsten lining was inserted into the tantalum resistance heating element because of a eutectic reaction which occurs between iridium and tantalum at 1948ºc.7 Heat treatments and solidus measurements carried out at compositions less than 40 at. pct Ir both with and without tungsten linings within the resistance

Jan 1, 1963

By Ross Blake

THE St. Joseph Lead Co. became interested in the Tri-State district in 1921 through acquisition of prospecting and development rights on approximately 20,000 acres of land extending northeastward from the Picher mining field, mostly in Kansas. Prospecting with churn drills was begun the same year and the first commercial ore body was found on the Jarrett tract at the then northern limit of the main Picher field. Operations at this mine began in 1923. Kansas Explorations, Inc., was organized in 1923 by the St. Joseph Lead Co. as a wholly-owned subsidiary to carry on its operations in the Tri-State District from an office at Joplin, Mo. As prospecting of the original acreage proved largely negative, attention was subsequently turned to other sections of the district. Numerous additional leases were acquired and prospected. The Company was successful in developing into operating properties the Jarrett, Isherwood, Robinson, Sullivan and Lotson tracts and, in more recent years, the Ritz, Snapp, Buckingham, Gibson and Jasper mines.

Jan 1, 1947

By Charles C. Fatino, Joel S. Hirschhorn

Loose compacts of strained and annealed stainless-steel powders were sintered at various temperatures and times to determine the effect of residual strains on the sintering behavior. The atomized powders were prepared by annealing, ball milling, and rean-nealing. The residual strains and domain size were determined by a Fourier analysis of X-ray diffvaction dala. The specimens were prepared by siwzultaneously sintering cylinders of both strained and unstrained powder. The evaluation of the sintered compacts included density measurements, metallographic examinations, and analyses of X- ray diffraction data. The results of these studies reveal a definite increase in sintered density and sintering rate for the strained powders. THE pressure compacting of metal powders causes deformation of the particles, mechanical interlocking, and increased contact area. After the deformation, severe residual strains remain in these particles. The subsequent contributions of these strains to the sintering process have been considered to be negligible, since the recovery and recrystallization temperatures usually occur prior to the temperature required for the sintering process. Sintering is con-sidered to be the process by which the powders are transformed into solid compacts at temperatures below their melting points. The sintering operation for stainless steel usually takes place in the range of 2050" to 2400°F (0.84 to 0.95 T,, where T, is the absolute melting point or liquidus temperature) while the temperature required for recovery is approximately 1800°F (0.75 T,). However, it has been shown for several metal powders that densification becomes significant in the range of 0.35 to 0.45 T,.' It is the purpose of this study to determine what effect residual strains have upon the sintering behavior of stainless-steel compacts. Loose compacts were selected for study in order to isolate the strain contributions and eliminate the variables inherent in sintering of pressure-formed compacts. Additional variables were minimized by using only one mesh size, one composition, one particle shape, and also by simultaneously sintering both types of powder. Very little work has been carried out previous to the present study to delineate the effect of strains on sintering behavior. Lenel et 01.2 observed that residual stresses in copper compacts caused shrinkage at comparatively low temperatures. Delisle3 loose-sintered ball-milled electrolytic iron and observed that bonding among particles began at a lower temperature as compared to the behavior of annealed powder. Increased densification of ball-milled oxide powders has also been noted.4'5 EXPERIMENTAL PROCEDURES Powder Preparation. The powder used for this study was a commercial-type 316L stainless steel made by the atomization process. A typical chemical analysis is: C- 0.025 pct Mo- 2.2 pct Cr-18.6 pct Ni-12.5 pct Fe—Balance The atomizing process is essentially the rapid freezing of liquid droplets. This nonequilibrium cooling causes coring to occur and two distinct phases are present within the solid particle, the austenitic phase and the ferritic phase. Due to the presence of this ferritic phase, the particles tended to fracture as well as become cold-worked during the subsequent ball-milling operation. (It was also found that this type of cooling produced a broadened and shifted

Jan 1, 1968

By T. D. Yensen, R. K. McGeary

While we have not been primarily interested in the determination of hydrogen in the alloys that we have been dealing with, we arc very glad to cooperate in this symposium on sampling and analysis for hydrogen, as we can never tell when we may find it desirable to perform such analyses. Vacuum-fusion Method Our primary interest has been oxygen and carbon, in the analysis of which we think we have become very proficient. Our oxygen-analyzing apparatus is of the vacuum-fusion type (Fig. I). This employs Dr. Derge's type of graphite cruciblc and slit sleeve, with graphite powder between, for heat insulation (Fig. 2) supported in a clear quartz bulb connected to the Pyrex glass system by means of a carefully made ground joint. The latter is kept cool by means of an air blast from a circular copper tube surrounding the joint. The crucible is heated by high-frequency induction and the 24 one-gram samples successively dropped in from the horizontal tube at the top by means of a magnet. The gases (H², CO, N2) are passed through the CuO catalyst held at 300°C. (converting CO to CO²I, H² to H²O) and the CO² and H2O frozen out in the main liquid air trap, while N2 is evacuated. At the end of the operation, shown by the termocouple vacuum gauge indicating a pressure of 10-4 mm. Hg, the analyzing system is isolated by means of the mercury cutoffs, and the CO² and H2oare determined by transferring first the CO2 and then the HzO to the small trap at the right. This is done by placing liquid air on the small trap, then removing the liquid air from the large trap for one minute, which is sufficient to evaporate the Co2 and transfer it to the small trap. The CO2 is then measured by closing the mercury cutoff at the extreme right, removing the liquid air from the small trap, warming it up to room temperature, adjusting the mercury level to one of the three marks on the glass tube (corresponding to three volumes calibrated so that I mm. Hg of CO² corresponds to 0.001, 0.002 and 0.010 mg., respectively, of oxygen) and finally reading the pressure. Liquid air is now replaced on the large trap, the mercury cutoff at the right opened, transferring the COz back to the large trap. The cutoff to the pumps is then opened, the liquid air removed for one minute, thus evacuating the CO², the pumps again cut off and the H2 O transferred to the small trap as before, except that it is now necessary to warm the large trap with a Bunsen burner in order to evaporate all the H2O. This requires about three minutes, as the inner tube must be heated to at least 100°C. In order to prevent H²O from being adsorbed on the glass walls, the glass tubing beyond the catalyst (i.e., to the right in Figs. I and 3) is kept heated to about 150°C. by means of Nichrome ribbon as shown in Fig. 3. For a I-gram sample the above amounts of oxygen (0.001, 0.002 and 0.010 mg.) 35

Jan 1, 1945

Executive SIDNEY J. JENNINGS, Chairman GEORGE D. BARRON J. E. JOHNSON, JR. EDWIN LUDLOW ROBERT M. RAYMOND Membership KARL EILERS, Chairman LEWIS W. FRANCIS J. E. JOHNSON, JR. LOUIS D. HUNTOON ARTHUR L. WALKER Finance GEORGE D. BARRON, Chairman CHARLES F. RAND BENJAMIN B. THAYER Library E. GYBBON SPILSBURY,1 Chairman ALEX C. HUMPHREYS2 GEORGE C. STONE2 J. H. JANEWAY4 BRADLEY STOUGHTON1

Jan 3, 1918

Executive SIDNEY J. JENNINGS, Chairman GEORGE D. BARRON J. E. JOHNSON, JR. EDWIN LUDLOW ROBERT M. RAYMOND Membership KARL FILERS, Chairman LEWIS W. FRANCIS J. E. JOHNSON, JR. LOUIS D. HUNTOON ARTHUR L. WALKER Finance GEORGE D. BARRON, Chairman CHARLES F. RAND BENJAMIN B. THAYER Library E. GYBBON SPILSBURY,1 Chairman ALEX C. HUMPHREYS3 GEORGE C. STONE 2 J. H. JANEWAY4 BRADLEY STOUGHTON

Jan 5, 1918

Organization Place Date 1919 American Chemical Society Philadelphia, Pa. Sept. 2-6 National Assn. of Stationary Engineers Huntington, W. Va. Sept. 8 American Peat Society Minneapolis, Minn. Sept. 22-24 American Iron, Steel Electrical Engineers St. Louis, Mo. Sept. 22-26 American Institute of Min. and Met. Engineers. Chicago, Ill. Sept. 22-27 American Steel Treaters' Society, First Annual Convention Chicago Ill. Sept. 22-27 National Exposition of Chemical Industries.... Chicago, Ill. Sept. 22-27 National Safety Council Cleveland, O. Sept. 29-Oct. 2

Jan 8, 1919

By A. B. Kinzel

SILICON, unfortunately, is not in the same category as some other metals with respect to the absolute value of the highest purity material prepared. Tucker, in England, and Becket, in this country have devel-oped procedures for the purification of silicon, and Becket's process has made industrially available silicon of a purity of 99.8 per cent or better. However, even the term "silicon metal" may be a paradox to some people, although not more so than the term "amorphous" as applied to silicon. These terms come from commerce, and "metal" is used to distinguish industrially high-purity silicon from ferrosilicon, silicon-aluminum, and other high-silicon alloys. Alloys of iron and silicon with 95 per cent Si or less are known as ferrosilicon, with a designation of silicon content where necessary, and the terns "silicon metal" is invariably applied to the grades containing 96 per cent Si and higher. The Becket method of purification was referred to in a monograph on the Alloys of Iron and Silicon, and the Tucker procedure was described in some detail in that publication.1 In order to get silicon of still higher purity, a sample, prepared by the Becket method, analyzing 99.84 per cent Si, 0.020 Fe, 0.016 Al, 0.005 Ca, 0.025 C, 0.033 per cent 02, 0.006 H2, 0.006 N2, and 0.001 per cent Mn, was crushed to pass a 100-mesh sieve said further purified by a modification of Tucker's procedure. This modification differs from Tucker's method in that after treatment the 100-mesh alloy was centrifuged to remove the last traces of acid. Our directly determined analysis of this purified sample shows: Si, 99.952 per cent; Fe, 0.009; Al, 0.012; Ca, 0.003; C, 0.006; or 99.982 per cent. Silicon by difference equals 99.97 per cent. The variation between silicon by difference and silicon as directly determined is important. Although Tucker mentions the amount of insoluble matter in commercial silicon both before and after his treat-ment, he does not mention the existence of carbon in the alloy; neverthe-less, lie reports silicon by difference. Any final figure as to purity obviously results from agreement between direct determination and

Jan 1, 1939

By AIME AIME

THE convention which met in Washington at the call of the Joint Conference Committee was called to order at ten o'clock on Thursday morning; June 3, by Richard L. Humphrey, temporary chairman, member of the American Society of Civil Engineers, who made a brief statement of the reason for the meeting. Lieut. Col. Charles W. Kutz, Corps of Engineers, U. S. A., and Engineer Commissioner of the District of Columbia, then welcomed .the engineers composing the convention on behalf of the District of Columbia and, the Washington engineers. Although an elaborate program had been prepared on which were many well-known speakers on interesting and important topics, , it was voted to intersperse this to fill in the usual and unavoidable hiatuses in the business program of such a convention[ Calvert Townley, president of the American Institute of Electrical Engineers, was elected permanent chairman, and J. C. Hoyt, of Washington, was elected secretary of the convention. The following committees were appointed: Consti¬tution and by-laws, Richard L. Humphrey, chairman; resolutions, Philip N. Moore, chairman; and program, F. H. Newell, chairman. Then, Gardner S. Williams, member of the, A. S. C. E. and the Grand Rapids Engineering Society of. Grand Rapids, Mich., and one-time member of the American Association of Engineers, offered the following resolutions:

Jan 1, 1920

Organization Place Date 1919 American Chemical Society :.... Philadelphia, Pa. Sept. 2-6 National Assn. of Stationary Engineers Huntington, W. Va. Sept. 8 American Peat Society Minneapolis, Minn. Sept. 22-24 American Iron, Steel Electrical Engineers St. Louis, Mo. Sept. 22-26 American Institute of Min. and Met. Engineers. Chicago, Ill. Sept. 22-27 American Steel Treaters' Society, First Annual Convention Chicago, Ill. Sept. 22-27 National Exposition of Chemical Industries.... Chicago, Ill. Sept. 22-27 National Safety Council Cleveland, 0. Sept. 29-Oct. 2

Jan 7, 1919