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By H. M. Crankshaw

The early methods of mining anthracite in the steep pitching Mammoth bed consisted in driving breasts up the pitch from the gangways and airways driven in the bed along the strike (Plate 2, Fig. 1). Breasts are simply rooms driven up the pitch the full thickness of the bed (Plate 2, Fig. 2), having a width of from 18 to 30 ft., and a manway or traveling way on one or both sides. (For detail of breast method see Whildin, Trans., vol. 50, p. 704). Many difficulties were encountered, and the maintenance cost of the timbered gangways was so great as to be practically prohibitive. To reduce this expense, the gangways were driven in the thin Skidmore bed underlying the Mammoth, and the coal mined through rock holes. (Plate 2, Fig. 2, A.) It was found that after the breasts were driven up 80 to 100 ft., the coal almost invariably rushed or "ran away," making good ventilation almost impossible and the extraction of coal from the upper portion of the lift very difficult. The economic length of a lift is from 200 to 250 ft., and the percentage of extraction by the old method above mentioned was often under 50 per cent., while the coal recovered was so badly broken up as to reduce materially the percentage of large sizes. Principles of Present Mining Methods The present methods designed for the recovery of a maximum percentage of coal and a maximum yield of the prepared sizes depends largely on the following principles: First.—Formerly the practice in mining bituminous coal was to space rooms so that as much coal as possible could be extracted in first mining (Plate 3). The small pillars were often lost, and an improvement in total extraction was found in the system of driving narrow rooms with wide pillars, with a much larger final recovery (Plate 4). Second.—The early method of ventilation was to maintain a single

Jan 1, 1917

By D. D. Button, L. D. Jaffee

INTEREST in the use of graphite as a high-temperature engineering structural material has recently increased markedly. However, actual use of this material has been limited, in part because information about its high-temperature mechanical properties has been lacking. The information needed includes not only reliable values for the properties, but also how to control these properties. Malmstrom, Keen, and Greenl have reported on the tensile and creep properties of some graphites above 2700° F (1500°C). They observed measurable creep under tensile loading at 4000 OF (2200 °C) and higher, with elongations of about 7 pct at 4500°F. Their typical elongation-vs-time curve showed the normal three stages of creep found for many metals at elevated temperatures. The specimens used were heated by passing an electric current through them. This method of heating caused a significant difference between the surface and axis temperatures, and may have affected the results. More recent work by kattus, in which the specfinens were also heated by their own resistance, showed very little plastic deformation for either slow or fast tensile testing or for creep testing. Work at this Laboratory, already reported,3 showed that for temperatures above 4500 "F and under conditions of slow tensile loading some commercial graphites exhibited elongations up to 20 pct. The work reported here is the continuation of a study of the tensile creep behavior of some commercially available synthetic graphites at temperatures up to 5300°F, and is preliminary to a more systematic investigation of the variables governing the high-temperature mechanical properties of graphite. MATERIALS TESTED The tests were conducted on six blocks from four lots of synthetic graphite bearing four different commercial-grade designations. These blocks were selected because their tensile stress—strain properties had been determined in previous work.3 Table I pre- sents the available information, supplied by the producers, on the processing of these materials. Also included in this Table are the densities and the tensile strengths at room temperature and 4500°F determined by the authors. EXPERIMENTAL TECHNIQUE The furnace used to heat the specimens for testing is shown in Fig. 1. The heating element was a graphite tube, 3-in. OD by 2 1/2 in. ID by 24 in. length. A spiral was cut into the 6-in. center portion of this tube to provide a high-resistance sec-

Jan 1, 1961

By Erwin Zodrow

An elaborate model for the magnetite distribution and genesis in the Smallwood mine, Labrador, based on factor analysis with orthogonal and oblique rotation of the factors, was proposed in an earlier paper. However, it is implicit in that model that variances of one variable shared with all others (communality) are estimated. To avoid the problem of communality estimation in the present investigation, a different type of factor analysis is used which (1) emphasizes the shared variances, and (2) attempts to eliminate, as much as possible, errors associated with the estimation of communality and sampling (unique variance). The samples for the present analysis are not the commonly employed oxide percentage variables, but counts of mineral species in specified areas of thin sections from drill core in the Smallwood mine: quartz, magnetite, calcite, and specular-hematite minerals. The counting procedure for mineral species is similar to modal analysis differing from it principally in the aspect of texture recognition. The constant area in which mineral species are counted is dependent primarily on

Jan 1, 1975

By G. C. Trevorrow

STRIP mining during 1943 increased considerably with further extension of mechanical loading in mines already partly mechanized; with the considerable introduction of mechanical loading into hand-loading mines; and with improvements in the use of loading equipment. Extension of the use of machinery both in strip mining and underground is due to reduction in labor supply and increased cost of labor, together with the increased demand for coal during the period of labor shortage.

Jan 1, 1944

By Marcus Nadler

WAGES in the United States, in spite of the wage freeze, have increased materially. Overtime payments have become standard practice in almost all industries. Now efforts are being made to place wages on an annual basis, and if this is adopted, it will result in an increase in the cost of production. Organized labor today is more powerful than ever before; union membership is large and steadily increasing, and in many instances membership in the union is a prerequisite to employment. The treasuries of many unions are strong as a result of the large membership and full employment. The unions, therefore, today are in a much better position than ever before to carry on long strikes. Politically, too, the unions are more powerful today than they ever were. On the basis of their strength, one may expect that some of the demands that the labor unions will make in the not distant future will be granted. It is, therefore, quite evident that before long, particularly when the curtailment in war production reaches about 40 per cent, this country will be confronted with a serious labor problem.

Jan 1, 1945

By R. H. Johnson

The Manual of the Oil and Gas Industry, under the Revenue Act of 1918, published by the Treasury Department for the guidance of oil companies in preparing their estimates of future recoverable oil for the purpose of calculating depletion, gives the first large public collection of comparative decline curves for the whole country. It is a matter of both scientific and practical interest to so arrange these data that the pools can be readily compared. There are certain difficulties in such a comparison, however: (1) The economic limit varies from 50 to 2000 bbl. a year in different pools taken. (2) Because of this variation in economic limit, the range of data shown makes comparison possible only for wells of intermediate size. In order to be as inclusive as possible, I have taken as an expression of the rate of decline the amount of oil produced in the period during which a well drops from 3000 to 2000 bbl. a year. No period of smaller production could be used because of the high economic limit in California; and no period of larger production and yet include the small well areas of the Appalachian. As it is, the Lima-Indiana wells are excluded. In a few instances, curves were extrapolated to obtain the reading, where the curve seemed regular enough to warrant it. In general, the amount of oil, in barrels, produced while a well declined from 3000 bbl. to 2000 bbl. a year is shown in Table 1.

Jan 1, 1921

By R. M. Hays

Prior to use of this model siphon finisher, the only means of evaluating metallurgical performance of the siphon finisher was by pilot plant studies. These are costly and require large quantities of material. A model siphon finisher and a test procedure which permits the evaluation of siphon finisher metallurgical performance has been developed. Metallurgical results between the model siphon finisher and pilot plant or commercial units show fairly good correlation. The upgrading of magnetic taconite concentrates by hydraulic concentration has been practiced for several years. In the 1940's, Braund1 used a multistage upflow classifier to upgrade magnetized magnetic concentrates. In present taconite plants, the SiphonSizer, marketed by Dorr-Oliver, Inc., has been particularly suitable for upgrading magnetic concentrates. When the hydraulic SiphonSizer is used to upgrade the concentrates in the finishing portion of the overall flowscheme, the unit will be called a siphon finisher to distinguish this application from classification. Prior to this work the only means of evaluating the metallurgical performance of the siphon finisher was by pilot plant studies which are costly and require large quantities of material. Therefore, it was desirable to develop a model siphon finisher and a test procedure which would simulate siphon finisher performance and require only small samples of material. This model would permit the evaluation of small samples such as drill core samples and be useful in evaluation of commercial siphon finisher design and performance. THE SIPHON FINISHER The siphon finisher, as shown in Fig. 1, is a tank equipped with a system of water jets which distribute the hydraulic water uniformly across the bottom of the vessel with an energy release for agitation in the teeter bed. The feed to the siphon finisher is intre duced through a feed well in the center of the unit. The silica and middling particles overflow a peripheral weir into the overflow launder. The magnetite fraction is discharged by a siphon or a modulated discharge valve. The siphon or the discharge valve is usually operated automatically by a float assembly which is responsive to the depth of the teeter bed. Various interface sensing devices have also been

Jan 1, 1968

By John V. Beall

Since the U. S. Metals Refining Co. works was established, around the turn of the century, near the town which is now called Carteret, N. J., it has grown to be a major producer of refined copper and the main source of that special brand known as "oxygen-free high-conductivity copper." Owing to the complex metallurgical problems arising from handling a variety of raw materials such as copper concentrate from Matahambre, Cuba, copper and brass scrap from the New York area, and domestic blister copper, the organization is geared from top management down through its 2000 employes to maintain a high degree of flexibility in plant operation. The Company is a subsidiary of The American Metal Co. Charges for the smelter furnaces, one reverberatory furnace and one blast furnace, are made up in. bedding bins so that they may be tailored to the production of a constant grade of blister copper. The reverberatory furnace smelts the .sulphide charge, which may be a blend of ten different materials but principally the Cuban concentrate, and the matte from the process is poured into a converter. This reverberatory is 80 by 20 ft, silica lined with a slag bottom, fired by pulverized coal, and continuously side-charged from the top by bottom-dump cars which keep the side walls covered. It produces a 40 to 50 per cent copper matte. The fuel-charge ratio is 4.35 tons of solid charge per ton of coal. The furnace has a capacity of 10,000 tons of charge per month and produces from 5000 to 6000 tons of slag per month which must be disposed of. About 5000 tons of converter slag is produced monthly and returned molten to the reverberatory furnace. The converter gases go through a spray chamber to a Cottrell precipitator and thence to the flue system. Smoke from the

Jan 1, 1948

By Robert Baschwitz, John Chipman

The distribution of silicon between liquid silver and Fe-Si-C alloys has been studied at 1420oand 1530°C. The data are consistent with earlier studies. New data of Hager on the liquidus lines of the system Ag-Si and the distribution data are used to obtain the activity coefficient of silicon in both liquid phases. Data on the heat of mixing in iron permit accurate extension to 1600°C. Equilibrium data involving SiO2 and silicon in liquid iron together with revised data on the free energy of SiO2 are used to fix the activity of silicon in the infinitely dilute solution. The binary system exhibits strong negative deviation from ideality. At infinite dilution ? Si at 1600" is 1.25 x 10'3, and at concentrations up to NSi = 0.4 the slope d InySi/dNSi has a constant value of r; = 13. It is found that logysi in the ternary solutzon is approximately but not exactly the same function of Nsi + NC as of NSi in the binary. The results are consistent with currently available data on the free energy of Sic and its solubility in molten iron. LIQUID solutions of the system Fe-Si-C have acquired considerable importance as the laboratory prototypes of blast furnace hot metal. Equilibrium studies involving such solutions and slags approximating those of the blast furnace have yielded useful information concerning the thermodynamic properties of blast furnace slags. In studies of this kind great importance attaches to a knowledge of the thermodynamic activity of silicon in the solution as a function of temperature and composition. An attempt was made by Chipman, Fulton, Gokcen, and askey' to evaluate all of the pertinent data on this system and to deduce the desired relation between activity, composition, and temperature. These authors published data on the solubility of graphite and Sic in molten Fe-C-Si solutions and on the distribution of silicon between liquid iron and liquid silver. They showed further how the activity of silicon in very dilute solutions in liquid iron could be calculated from equilibrium data involving the molten alloy and solid SiO,. These calculations rested on the published thermodynamic properties of SiO, in- cluding its heat of formation which at that time was recorded as -209.8 kcal. This value has been under suspicion for some time and has recently been replaced by the concordant results from two independent laboratories2,3 which place the heat of formation of a-quartz at -217.6 kcal. This revision necessitates a re-evaluation not only of the activity of SiO2 in slag but also of silicon in molten iron. It is the purpose of this paper, therefore, to recalculate the activity of silicon, and in furtherance of this objective to present new data on its distribution between liquid Fe-Si-C alloys and liquid silver. HEAT OF SOLUTION OF SILICON IN IRON In order to determine the effect of temperature upon the activity coefficient it is necessary to know the heat of solution of silicon in iron as a function of composition. This is found in the data of Korber and Oelsen4 shown in Fig. 1. The curve corresponds to the following equation, which is of a form suggested by Wagner:5 Here AH is the heat absorbed in kilocalories in forming one gram atom of molten alloy from its molten elements and the N's are atom fractions. The relative partial molal enthalpies of the components, each referred to its pureliquid state and defined as zFe = aFe - PFe and zsi = HSi — -psi, are shown graphically. At low concentrations zSi = -28.5 kcal, in agreement with Kijrber and Oelsen's computation. This is in good agreement with the value of -29.3 kcal obtained by Chipman and Grant6 using an entirely different method. ACTIVITY AT INFINITE DILUTION From the known free energy of SiO, it is possible to obtain the activity of silicon in dilute solution in liquid iron from equilibrium studies. The heat of formation of a-quartz is —217.6 kcal and the heat capacity and entropy data are given by Kelley and ~ing.' The free energy of formation of ß-cristo-balite at temperatures above the melting point of silicon is expressed by the following equation: Si(Z) + O2(g) = SiO2 (crist); AF" =-226,500 + 47.50T [I] The value of the deoxidation product for silicon [%Si] x [%O]2 at 1600°C according to Gokcen and chipmans is 2.8 x 10"5, in agreement with results of Hilty and Crafts.9 More recent works of Matoba,

Jan 1, 1963

By P. D. Proctor, M. P. Nackowski

Quantification in recording geologic phenomena and application of well-known geologic principles to engineering works continued at an increasing rate during the year. Highway departments, water resources agencies, private firms and governmental agencies involved in tunnel excavations, dam site locations and construction, consultants and government experts in subsurface liquid-waste disposal, designers of underground storage facilities and city and regional planners all confirmed greater use of applied geology in their planning and implementation of plans. Applications of quantified geologic data to highway locations, slope control of cuts, raw material sources, water sources and water run- off showed a striking increase in number. Environmental geology and geologic hazards became part of the jargon of the geologic profession, and the American public began to realize more fully the significance of where they live, and on what and near what geologic phenomena which might effect their well-being. Tunnel work for water projects of almost dream-like magnitude kept geologic engineers busily engaged in predicting and testing local geologic conditions for construction projects. Disposal of industrial and radioactive liquid wastes continued as problems, but use of stratigraphic data, fluid flow rates and direction of flow helped solve some critical waste disposal problems. Unusual applications of seismic networks, remote sensing methods and X-ray techniques in geological engineering applications added other tools to this increasingly important profession.

Jan 2, 1968

By Chingyuan Y. Li, C. Y. Hsieh

Realizing that aluminum will have a great role to play in the coming industrialization of China, Chinese geologists have long been looking about for some aluminum deposits. The possible sources appear to be alunite, the alumina-rich shales, and the bauxite deposits. The locations of deposits are shown in Fig. I. Alunite Our attention was first directed to the alunite deposits along the southeastern coast of China. Table I summarizes the reserves now believed to exist in that region. Other alunite deposits have been found in Kiangpei, Szechuan province; Charming. Liuyang and Hsanshan, Hunnan province Tsingchow and Chowyuan, Shantung province. No reserve figures are available. High-alumina Shale Shale high enough in aluminum to serve as a source of that metal has been found in northeastern China(Tab1e 2). In Manchuria, the Manchuria Light Metals Co., at Antung and Fushun, operating under Japanese control, has been the only active producer of aluminum. It is not known, however, whether the company uses local raw materials or imports ore from elsewhere.* Shantung Bauxite Bauxite was first recognized in China at Paoshan, Shantung province. Although the reserve is reported to be large (estimated at 271 million tons), the high content of insoluble residue (SiO2) and mineral composition (diaspore) are dis-

Jan 1, 1948

By Chingyuan Y. Li, C. Y. Hsieh

Realizing that aluminum will have a great role to play in the coming industrialization of China, Chinese geologists have long been looking about for some aluminum deposits. The possible sources appear to be alunite, the alumina-rich shales, and the bauxite deposits. The locations of deposits are shown in Fig. I. Alunite Our attention was first directed to the alunite deposits along the southeastern coast of China. Table I summarizes the reserves now believed to exist in that region. Other alunite deposits have been found in Kiangpei, Szechuan province; Charming. Liuyang and Hsanshan, Hunnan province Tsingchow and Chowyuan, Shantung province. No reserve figures are available. High-alumina Shale Shale high enough in aluminum to serve as a source of that metal has been found in northeastern China(Tab1e 2). In Manchuria, the Manchuria Light Metals Co., at Antung and Fushun, operating under Japanese control, has been the only active producer of aluminum. It is not known, however, whether the company uses local raw materials or imports ore from elsewhere.* Shantung Bauxite Bauxite was first recognized in China at Paoshan, Shantung province. Although the reserve is reported to be large (estimated at 271 million tons), the high content of insoluble residue (SiO2) and mineral composition (diaspore) are dis-

Jan 1, 1948

By S. J. Im

Bupyung Silver Mines daily treats average 14 tons of concentrates containing 9,000 g Ag per ton. Bupyung Silver Refinery uses Merrill Crowe process to recover the silver from the leach solution containing 1.0 g/l Ag; Series of experiments were carried out to recover the silver from the solution by means of direct electrowinning in place of Merrill Crowe process. The recovery of the silver was 99% when the cell voltage and the retention time were 1.9 v and 3.0 hours, respectively. Power consumption was 3.2 Kwh/kg of Ag. It was found that impurity buildup was not significant during the recycling. The direct operating cost for the electrowinning was evaluated to be $ 0.35/kg of Ag.

Jan 1, 1984

By Philip B. Bucky

WITH the exhaustion of the sections of iron ore bodies amenable to opencut mining the iron ore miners raise the question: "How can we mine the extensions of these ore bodies in depth with the same costs as obtained in opencut work?" This question brings to the fore the relationship between mineral exploration and research on mining procedures. The iron miners must either find new de? posits amenable to their known methods of mining or develop new mining methods for deep deposits. It is understood that the oil companies will spend $30,000,000 next year in the search for new oil fields. How much the metal mining companies will spend in the search for new ore bodies is unknown, but without doubt the amount will run into several millions of dollars. If the mining companies that concern themselves with metals, nonmetallics, and fuels will set aside a substantial sum for fundamental and applied research in mining methods, they can not only lower their costs but increase their reserves thereby. Any increases in mining efficiency automatically result in increased ore reserves at no cost.

Jan 1, 1947

By William P. Blake

This camp is just now startled by the alarming suggestion that unless there shall speedily be an appreciation in the value of silver, and a decrease in the cost of salt, it will be prudent business policy to close the Alice mines and mills until the conditions of production are more favorable. Such an event would be a great blow to the prosperity of Butte. It would throw some hundreds of men out of employment, and it might lead to the adoption of the same policy by other companies, which, like the Alice, have not been able to pay dividends to their shareholders for a long time. The question arises, and becomes emphatic: If, under the present adverse conditions, the mines and mills cannot be made to pay a proper profit, why should they continue to be worked ? The owners mentally ask: Shall we go on exhausting our mines, pouring out a stream of silver for the maintenance of the community, and the support of the rail ways, or shall we husband our reserves, withdraw the miners from our slopes, and wait for more favorable conditions ? This is the impending question, and all concerned dread to meet and answer it. Let us briefly review the situation and forecast, if possible, what the solution of' the problem will be. It must be understood that the discussion does not include, or refer to, the immense copper-producing interests of the camp, which may or may not be upon a very much more satisfactory basis. It will be confined chiefly to the operations of the Alice company, sta tistics of which are at hand, without involving the other silver com panies in the conclusions beyond those inevitable from well-known facts, patent to all. There are at present in Butte and in its vicinity in the principal mills an aggregate of 290 stamps dropping upon silver-ores: Alice,...........80 stamps. Moulton,. .........40 " Lexington,...50 " Silver Bow,.........30 " Blue Bird,..........90 " The Alice mills at present, with their 80 stamps, devour, in round numbers, from 100 to 120 tons a day. The actual amount

Jan 1, 1888

By Charles Catlett

Probably no one has had occasion to examine an undeveloped coal property without hearing some hopeful or interested party insist that the bed will improve when opened some distance under cover. When the bed is already in good condition, the opinion is usually advanced that the same character may be expected, at least to the bounds of the hopeful individual's holdings. My attention has been called in this way to the extent to which a bed is affected by its outcrop at the surface ; and having had opportunity to examine a number of openings immediately at the surface, and also a short distance under cover, I submit some observations bearing on this question. Whatever may have been the original variations, we may assume that coal-basins presented in comparatively modern times approximately parallel beds interstratified with fire-clay, slate, sandstone, etc., as represented by Fig. 1. Under the effect of erosion, Fig. 2 would be formed. It is obvious that along the line A, B, C, in Fig. 1, the beds exist under conditions differing from those at A', B', C', or again at A", B", C", in Fig. 2, in their exposures to atmospheric agencies, pressure and erosion. The effect of the first is to decompose and soften many of the strata; of the second, when presented unequally, to cause the movement of such material as was at all plastic towards the point of least pressure ; and of the third, to remove the strata in whole or in part. It

Jan 1, 1901

By R. S. Dean

THE commercial production of electrolytic manganese on a small scale commenced in 1939. The writer made a short report on the progress of production and utilization in MINING AND METALLURGY for January 1941. Progress during the last two years, naturally, has been more rapid. In June 1940, Congressman (now Senator) Scrugham presented a proposal to Congress for an appropriation authorizing erection of a pilot plant for "the production of metallic manganese by electrolytic or other means." As a result of this, a pilot plant, having a capacity of a few hundred pounds per day was built at Boulder City, Nev. Subsequent appropriations permitted expansion of the plant to about a ton per day. Much has been learned in this plant about electrolytic manganese, and the product even in its small way has found war uses of considerable importance. Meanwhile, the Knoxville plant of the Electro Manganese Corporation, the sole commercial producer, was expanded to about 4 tons per day to supply needed material for the war program. Other proposals for commercial plants have not been favorably received by the War Production Board. The Bureau reported on one such proposal by the American Alloys and Chemical Corporation. PRACTICE AT BOULDER CITY The present practice, as carried out at Boulder City, which is being described in more detail in a current paper by the Bureau staff at Boulder City, starts with a manganese dioxide ore containing about 20 per cent manganese. Currently this ore comes from the Three Kids deposit near Las Vegas. The steps for the production of electrolytic manganese, in general, are as follows: I. The manganese in the ore is reduced to MnO. 2. The MnO is dissolved from the ore in spent electrolyte, which contains about 38 to 47 grams per liter of free sulphuric acid, 135 grams per liter of ammonium sulphate, and 10 to 12 grams per liter of Mn as sulphate. In the leaching step the manganese is built back up to 32 to 36 grams per liter of Mn as sulphate; the pH is adjusted to neutral by means of gaseous ammonia and passed through thickeners. 3. The electrolyte is purified by adding H2S, which precipitates the heavy metals. After filtering, ferrous sulphate is added to the solution and oxidized with air and the solution is filtered and clarified on a precoat filter. 4. The purified catholyte is electrolyzed in a diaphragm cell using stainless-steel cathodes and lead-silver anodes. The current density is about 45 amp. per sq. ft. Current efficiencies of 60 to 65 per cent are regularly obtained.

Jan 1, 1944

By John Greenawalt

IN view of the increasing importance of sintering in the beneficiation of iron ores preparatory to their reduction in the blast furnace, the writer believes the time is opportune for an up-to-date, though brief, discussion of the general principles of sintering, as well as a discussion of some of the recent improvements and mechanical developments that have been achieved in this industry, its present trend and future possibilities. Sintering may be defined as the agglomeration of fine mineral particles into a porous mass by incipient fusion caused by heat produced by com-bustion within the mass itself. Its first successful application, in connec-tion with the treatment of lead sulphide ores, was known as blast roasting. In this process the lead ore was given a preliminary roasting in a reverber-atory furnace, then the incandescent mass was placed in a pot with a grate and an updraft was applied. It was soon discovered that much better results were obtained by cooling the ore, moistening it, and placing it upon an incandescent layer of fuel previously placed upon a grate, and then applying the updraft blast of air until the charge was converted into a more or less agglomerated mass. The fuel was sulphur and the process one of desulphurization, which was the principal result desired. The application of downdraft to blast roasting brought about tremen-dous results; the principal one of which was that an air blast of high pressure could be passed through a layer of ore deposited on a grate, or on a grate covered by a layer of coarse porous material, without disturbing the particles of which the layer is composed. The air current is compelled to filter through the pores of the charge, whereas if the same pressure applied to the top surface of the charge with downdraft were applied to the bottom of the charge with updraft, the charge would be completely blown off the grate. Another result of reversing the draft was that a flame could readily be applied to the top surface of the charge for ignit-ing purposes.

Jan 1, 1938

There was such a large demand for copies of the speech of Herbert Hoover at the A. I. M. E. dinner given in his honor on Sept. 16, that a special edition has been run off; anyone desiring copies may obtain them by applying at the office of the Secretary.

Jan 12, 1919

By G. E. Keller, G. D. Coe

Several methods have been devised for rapid determination of sulfur in coal using a high-temperature combustion furnace. The fundamental principles of the various methods are similar but the techniques vary widely. The method described herein is no different in principle from some of its predecessors but varies considerably in technique. Originally devised to overcome the low-accuracy criticism leveled against the others, the tube-furnace method has proved successful for limited applications. Work is being done to widen the applicability of the technique. Subsequent to the work of A. Vita1 in 1920, a number of investigators have published data dealing with the rapid determination of sulfur in coal using a high-temperature combustion furnace.2-5 These, together with several unpublished methods, involve wide differences in technique although they are all similar in principle. Investigation of typical details of procedure showed that poor precision or accuracy could be attributed to one or more of the following: 1) inadequate quantity of sample to be representative, 2) a delivery tube temperature too low to confine condensation to a washable area of the tube, 3) no provision for back washing the delivery tube, 4) incomplete absorption of the sulfur compounds due to inadequate bubbler, and 5) the false assumption that all of the sulfur is evolved as sulfur dixoide. The method herein discussed is no different in principle from some of its predecessors; the differences are in technique. Although the method is rapid—a determination can be completed in 5 min— accuracy has riot been sacrificed in order to achieve speed. MATERIALS AND EXPERIMENTAL WORK Fig. 1 shows the arrangement of the equipment. A metered volume of oxygen is passed through calcium chloride for removal of moisture, then through Ascarite for removal of carbon dioxide, and thence through a glass tee to the feed end of the combustion tube. Connected to the side arm of the glass tee is a rubber tube that is closed with a pinch clamp during combustion of a sample. The products of combustion are expelled through a Vycor bubbler, the end of which is submerged 3 cm below the surface of a 1 pct hydrogen peroxide solution contained in a 300 ml high-form beaker. At the completion of the 4-min combustion period the contents of the beaker are titrated to a yellow end point, using a methyl red indicator, with 0.05 N sodium hydroxide (or sodium tetraborate). The pinch clamp on the tube leading from the tee in the oxygen line is then opened and mouth suction applied to draw the hydrogen peroxide up into the bubbler past the ell, almost to the rubber tube connecting the bubbler to the combustion tube. This washing of the bubbler is repeated until no further acid reaction with the indicator is obtained. The hydrogen peroxide-sul-furic acid solution is then titrated to the final yellow end point. Test work conducted at the Robena Laboratory disclosed the following critical conditions that had important bearing on the precision of the method: Weight of Sample: Several series of tests wherein the sample weight ranged from 0.1 to 0.5 g of -60 mesh coal showed that the lowest variance (standard deviation squared) resulted from the use of 0.5-g samples; the variance was slightly greater when 0.3-g samples were used, and with less than a 0.3-g sample weight the variance increased rapidly with decrease in weight. Although the use of a 0.5-g sample invariably resulted in a very slight explosion as soon as the sample entered the hot zone of the combustion tube, this did not detract from the precision of the method. Temperatures: Mott and Wilkinson5 found that a combination of low temperature (1250°C) and low oxygen flow rate (less than 700 ml per min) tended to give high results due to formation of oxides of nitrogen. Although the method herein employs a much higher oxygen rate than 700 ml per min, as an additional precaution to assure accurate results, 1315°C (2400° F) is recommended as the most desirable furnace temperature. The temperature of the elbow of the bubbler should be at least 75°C to minimize condensation

Jan 1, 1961