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By F. W. Bradley

MY first Nevada City mining reminiscence is one of seeing Capt. Thomas Mein, over 52 years ago, in the old Wyoming mill on Deer Creek about a mile below the town of Nevada City. Captain Mein was then superintendent of the Wyoming mine, where the old fashioned Cornish pump was used, as well as hurdy-gurdy water wheels for power. This mill was one of the typical, up-to-date mills of that time and consisted of stamps, fed by Chinese hand feeders, who also cobbed the ore down to a small enough size to be fed into the mortars. Stamps at that time were of light weight and crushed about one ton to one and a half tons to the stamp, the pulp going over plates, then into sluices with self-raising gates. When a sluice became full the pulp was shut off and directed into the parallel sluice, also with a self-raising gate. The concentrate thus collected in the sluice was shoveled out and carried to Cornish buddles and there cleaned up, preparatory to being sent to a local custom chlorination works.

Jan 1, 1929

By Frederic P. Dewey

(New York Meeting, February, 1912.) By the old method of determining platinum in ores and bullion, the silver-alloy first obtained in the regular course of assay is parted in strong sulphuric acid and the residual metal weighed. This is re-alloyed with silver by a second cupellation and parted in nitric acid, the residual metal being again weighed. Any difference shown between the two weighings is assumed to be, and is called; platinum. Sometimes it is so, and if any considerable amount of platinum be present, there will be a decided difference between the two weighings; but a slight difference is no real evidence whatever of the presence of platinum. On the other hand, the second weight may equal or possibly exceed the first, even when traces of platinum are present. Again, other members of the platinum group may go into solution in nitric acid more or less. If present, these would be called platinum and escape detection. The method does not provide any direct tests whatever as to the presence or absence of platinum. It is often indecisive, and sometimes jives erroneous results. It is, therefore, quite unsatisfactory. Being called upon many times to determine platinum in a wide variety of materials, particularly when present in very small amounts, I have realized the disadvantages and defects of this old method. In an article on the solubility of gold in nitric acid, 1 I have briefly outlined a method of gathering a little gold out of a solution containing much silver, which furnishes the basis of

Apr 1, 1912

By Wm. A. Haven

ON the northern part of the globe, almost since the earliest days of mankind's history. ironmaking has been practiced in one form or another. Some investigators question the generally accepted belief that copper and bronze were in earlier general use than iron, explaining the greater age and abundance of copper relics by their greater resistance to natural oxidation. However, the occurrence of copper in its natural state and its greater ease of reduction from the simpler copper minerals is a strong argument that the making and use of copper came first. Nevertheless, good evidence exists that ironmaking was practiced in ancient India and China, as well as in ancient European countries. Some interesting vestiges of those early operations still survive and have a place, in the background at least, of a discussion of modern blast-furnace practice.

Jan 1, 1940

By Robert M. Grogan, James C. Bradbury

The Illinois-Kentucky mining district has, since 1880, accounted for 80 per cent of all U.S. production of fluorspar. The ore deposits are of two types: vein deposits formed by fissure fillings along faults and bedding-replacement deposits formed by the replacement of strata at certain favored stratigraphic positions along minor faults and fractures. Fluorite is the chief valuable mineral in the deposits. Sphalerite and galena commonly are present in small amounts but, in some ore bodies, may form a substantial part of the valuable constituents of the ore. Calcite is the chief gangue mineral; quartz and barite Exposed strata range from Devonian are present in various amounts. through Pennsylvanian in age. Igneous intrusive rocks occur as mafic dikes and sills and intrusive breccia dikes and plugs. Structurally, the district is situated on a generally northwest- trending arch that has been sliced into a series of long, narrow blocks by normal faults that trend northeastward. The structural The localization of the ore deposits by faults and fractures, the association of fluorite mineralization with intrusive breccias, and various lines of petrographic and geochemical evidence indicate that the fluorite-zinc-lead deposits were epigenetic and deposited by solutions emanating from a deep alkalic magma.

Jan 1, 1968

By Claiborne C. Van Zandt

THE heavy postwar demand for Portland Cement has created shortages that are gradually being overcome by increases in plant capacity. In the post-war period, the Lone Star Cement Corp. has expanded several of its existing 15 plants and has built 2 new plants, now in operation, with a third new plant under construction in Brazil, of design somewhat different from that of the two preceding ones. The new domestic plants are located at Lone Star, Va., near Roanoke, and at Maryneal, Tex., near Sweetwater, and went into operation during 1951. Each plant is equipped with two rotary kilns and has an initial capacity of 1,500,000 bbl per year, or 6,000,000 sacks. The total cost of each plant was about $10,500,000, and on this basis $7.00 in 1951 money are required per bbl of annual capacity; at 376 lb per bbl, this corresponds to $37.00 per ton of output. The investment corresponds to approximately $80,000 per hourly-wage earner employed. The purpose of this paper is to describe the most interesting design features of the two new and almost identical Lone Star plants. Why the Dry Process Was Chosen The two new domestic Lone Star mills employ the dry process because: 1-The raw materials at both properties are particularly suitable and can be dried very, readily. 2-The Maryneal, Tex., plant does not have water available for slurry. 3-Very substantial kiln fuel savings can be obtained. 4-Dry raw grinding reduces ball and liner wear and- general maintenance, without any sacrifice in power. Operating costs to date have more than justified the choice of the dry process for these two plants. Raw Materials The chemical composition of Portland Cement raw material after crushing, grinding, and mixing, but before burning, is about as follows: [ ] sometimes tailings from an iron ore concentrating plant. Certain objectionable materials occur in raw mix: magnesia, limited in cement to 5 pct, in excessive amounts; alkalies, as sodium and potassium; phosphorous; and sulphur, generally present in coal and oil. The Roanoke raw, materials are dense limestone and shale. The Maryneal materials are soft limestone and a hard brittle clay that can be handled much like shale. Sand and iron ore are required in small quantities. General Plant Layout and Construction The two plants are so similar that one joint description will cover both, with such exceptions as will be especially indicated. The crushing plant is located in the quarry, and raw material is conveyed by belt to the storage building, where all materials are stored and handled. Fig. 1 identifies the various structures of the Roanoke plant. The large storage building is used for the storing and handling of all materials, including limestone, shale, sand, iron ore, coal, clinker, and gypsum. Directly adjoining the storage building is a structure under a similar arched roof, containing the raw and clinker grinding departments and the electrical substation. The discharge ends of kilns and coolers, and coal or gas burning equipment are also placed at one end of the mill building. The 340ft long kilns extend away from the main buildings to form the long leg of an L, at the end of which is the feeding and kiln dust collecting equipment, and the raw blending silos are conveniently located adjacent to the feed end of the kilns. The machine shop, storeroom, electrical shop, foremen's office, service rooms, and meeting hall are combined in one structure in the center of the plant, and the office and laboratory are close by. The cement silos and packhouse do not have to be tied directly into the manufacturing process and are therefore located at a point convenient to the railroad tracks.

Jan 1, 1952

By J. J. Beeson

For the past fifty years or more, the structural features of the Cordil-leran mountain system of western United States have presented some most interesting problems. Any geologist or engineer living in this region, or even making occasional examinations of the mines, will lose much of interest and importance if he is not familiar with the literature. Some of the greatest works on geology have been the result of studies carried on in sections of this region. Among the more important of the earlier works are those of Dutton,l King,2 Gilbert3 and Powell;4 of the more recent Lindgren,5 Ransome,6 Spurr,7 Butler8 and others have contributed much. Many of the papers are largely of scientific interest but even these lay the foundation for the commercial application of the broader features of the geology. I have read many of these works with the keenest interest and pleasure; in fact, some have been read until some of the more important findings seem to be my own. In this paper, however, it is my aim to accept credit for little more than the labor of assembling some of the ideas of others. This is done with the hope that an interesting and valuable discussion will be the result. If some of the ideas presented should

Jan 1, 1927

By D. N. Hedges

This paper discusses the actual recovery and installation of a longwall in a bituminous coal mine in western Pennsylvania. The coal bed mined is in the Lower Freeport seam, which averaged 1.07 m (42 in.) in height locally. Drainage from the mine is about 13.25 ML/day (3.5 million gal per day) of water. This water deteriorates the mine's predominately fire clay bottom making it extremely difficult to move equipment. Support removal is accomplilshed by pulling the 5.44 t (6 st) shields out under their own hydraulic power and transporting them by track 8.05 km (5 miles) to the next longwall panel. This paper also discusses the changes that will be made to aid in the succeeding longwall recoveries and installations.

Jan 1, 1985

By W. B. Plank

I HAVE been asked by the Chairman of the Engineering Education Committee to outline what the engineering colleges would like the mining companies to do with the young engineer just, out of college. It has been suggested that, because my own personal experience has been almost entirely within the coal industry, I handle this subject from that view- point. Many thoughtful engineering educators are today wondering what effect the present employment policies of many industrial companies are going to have on the young man just starting out in his profession. Since before the World War large industrial concerns, such as those in the electrical and mechanical industries, have gone to the colleges to interview 'likely graduates until today there has developed in most of our engineering colleges, especially in the eastern part of the country, what appears to be a lively competition on the part of these companies in bidding for the young graduate engineer. The employers of mining engineers, with one or two exceptions, have not yet begun to enter this competition. It remains to be seen how serious this situation will become, how it will affect the training of other engineers, and what effect, if any, it will have on the mind of the young man about to enter college who may be inclined to take up mining engineering, but who gains the impression from this well advertised employment service just mentioned that there is no opportunity for him in the mineral industry as com- pared with the opportunities offered in say civil, mechanical, and electrical engineering.

Jan 1, 1929

By Clyde E. Williams

MUCH has been said recently concerning the depletion of the Lake Superior iron ore re- serves. Estimates given indicate a total life of the present known reserves of twenty to thirty years. Some argue that there is no need to concern ourselves about the possible depletion of the Lake Superior iron ore supply because foreign ores can be brought in to this country at a lower price than rich agglomerated ore can be produced from the lean domestic ores. Some fear, as a result of this, a displacement of the steel business from present districts to the Atlantic seaboard. Others show that foreign ores will be brought to interior points via the projected Great Lakes-St. Lawrence waterway. Others believe that the South, given better freight rates, will extend its iron and steel market into northern territory.

Jan 1, 1931

By L. Seigle, R. Resnick

An inert-marker movement experiment indicates that the ratio of the intrinsic diffusion coefficients DC:DTa = 80:l in TaC at 2500°C. Measurements of the diffmion coefficient of carbon in nonstoichiometric TaC at temperatures from 1700° to 2700°C reveal that Dc increases with decreasing carbon content, but much less than expected from the probable change in vacancy concentration with carbon content. A diffusion process involving two simultaneously operating mechanisms is postulated, and shown to be theoretically feasible. The average value of the carbon diffusion coefficient is given by DC = 0.18 exp[(-85,000 ± 3000)/RT] sq cm per sec over the composition range 46 to 49.5 at. pct C. BECAUSE of their high melting points and hardness, the carbides of the IV, V, and VI group transition metals, along with those of uranium, have attracted considerable interest for applications at high temperatures. In these applications the reactivity of the materials is important, and, since rates of diffusion within the compounds influence reactivity, a knowledge of diffusion kinetics and mechanisms is desirable. While many investigations of the mechanical and electrical properties of these compounds have been made, only two fundamental investigations of diffusion in the carbides are known. Chubb, Getz, and Townleyl measured the diffusivity of carbon and uranium in UC, and Gel'd and Liubimov2 measured the diffusivity of carbon and niobium in NbC. This paper describes an investigation of the diffusion of carbon in tantalum monocarbide and, in particular, the influence of carbon deficiency on this process. Tantalum carbide melts at approximately 3800°C, which makes it one of the highest melting materials known. The compound exists over a rather wide range of carbon Content.3-7 At the peritectic temperature, 3240°C, the phase extends from about 36 to 50 at. pct C. Although the compound can exist with a substantial carbon deficiency, the high carbon phase boundary remains near the stoichiometric composition over the entire temperature range; i.e., no carbon excess is observed. The structure of TaC is the NaCl type wherein carbon atoms normally occupy the octahedral sites in a somewhat expanded fcc lattice of tantalum. Decrease of the lattice parameter with decreasing carbon suggests that the removal of carbon introduces octahedral vacancies into the lattice. I) EXPERIMENTAL DETAILS AND RESULTS Inert-Marker Experiments. In a compound such as TaC the interstitial element would be expected to diffuse more rapidly than the metal. This was confirmed by an inert-marker experiment, following Srnigelskas and irkeendall.8 Ideally, the markers should be placed at the interface between a slab of low-carbon TaC and graphite, and their movement during subsequent inter-diffusion measured. Unfortunately, no solid could be found which is unreactive in contact with carbon at the high temperatures employed in these experiments. In order to circumvent this problem, a specimen was designed in which the markers consisted of several small canals running just below the surface of a tantalum slab. This specimen was prepared by machining grooves on the surface of the tantalum slab and then diffusion-bonding a thin plate of tantalum to the slab over the grooves. The surface of the plate was then ground down until the distance between the canals and surface was as small as possible (about 0.01 cm). Thus, the canals would lie entirely within the TaC phase after a short period of diffusion. The diffusion anneal consisted of immersing the metal sample in high-purity graphite powder and heating for approximately 10 hr at 2500°C under vacuum. At this temperature, the vapor pressure is sufficiently high and the transfer of carbon from graphite sufficiently rapid to allow the surface of the diffusion sample to attain the stoichiometric carbon concentration very quickly. Conclusions regarding the relative diffusion rates of carbon and tantalum in the compound layers (TaC and Ta2C) can be drawn from the location of the canals after the diffusion anneals. If the growth of the layers is governed mainly by the diffusion of carbon, as expected, the canals should remain close to the sample surface. If the diffusion of tantalum contributes appreciably to formation of the compound layers, the distance from the markers (canals) to the surface should increase. Fig. 1 shows, diagrammatically, the appearance of the specimens after diffusion, and Table I presents the depth below the surface at which the

Jan 1, 1967

Jan 1, 1961

By Johnson Crawford, Alan H. Hoagland

Zinc mining at Jefferson City began in 1854 with small scale production of oxidized ore from open pits. Significant production began in 1913 with the development of the Mascot Mine by the American Zinc Company. In 1965, four flotation mills were treating crude ore at the rate of about 12,000 tons per day and the Mascot-Jefferson City district currently is the largest zinc producing area in the United States. The producing mines, Mascot, Young, North Friends Station, New Market Zinc, Grasselli, Davis-Bible, Coy, and the Jefferson City, are 15 to 28 miles northeast of Knoxville in the Valley and Ridge physiographic province, an area of gentle relief lying between the more rugged Great Smoky Mountains and the Cumberland escarpment. The ore is strata bound, occurring essentially within a stratigraphic range of 200 feet in the Lower Kingsport and Upper Longview formations of Lower Ordovician age. In the lower strata of the mineralized section, the ore generally is found in coarsely crystalline elastic dolomite breccia containing silica and chert debris within a sequence of aphanitic limestones. The upper strata of the mineralized section are fine-grained primary dolomites that, in the ore zones, have been fragmented in mosaic patterns by solution collapse with the interfragmental space filled by white gangue dolomite and sphalerite. The mineralogy is unusually simple, sphalerite being the only important sulfide. Pyrite is very sparse. Dolomite gangue is abundant, silica was deposited in quite small amounts, calcite is minor, and fluorite and barite are very rare. The principal ore controlling structures are rubble breccia zones that were formed during the post-Lower Ordovician-pre-Middle Ordovician erosion interval by supergene solution as a phase of the development of a regional karst system of underground drainage that extended to' depths of at least 800 feet. The major Appalachian orogenic structures are post-ore and have been superimposed on the ore bodies. There is substantial evidence to support the current thinking of the writers that the ore deposits were formed at a depth not exc1~eding 800 feet.

Jan 1, 1968

By John G. Hall

The pumping operations at the Chief mine have been unique in the respect that for many years the entire flow of water into the mine has been disposed of by pumping into natural underground " caverns" or "sinks." Volumes up to 4000 gpm have been pumped into these caverns with no apparent tendency for the caverns to fill with water, and it has never been proven that any of the water returns to the mine workings. Major pumping operations have been carried on during two periods, the first from 1918 to 1927, and the second from 1942 to the present time.

Jan 1, 1949

By F. C. NINNIS

AT THE Belmont mill, the pregnant solution is de¬livered to a 30 by 10-ft. tank, from which it is pumped to three Merrill clarifying presses of the sluice-bar type, whence it flows through the meter to the precipitation supply tank. ?The solution for precipitation is pumped by a 10 by 10-in. Aldrich triplex pump and delivered through a 6-in. line to the forty-eight triangular frame Merrill presses at the head of the mill. Zinc dust is fed in at the pump suction and the solution precipitated to 0.01 to 0.02 oz. silver. The solution flowing from the presses is tested at 1-hr. intervals with sodium sulfide. All solution is precipitated to the same value; 4J tons of solution are precipitated for each ton of ore treated and the presses are cleaned every 15 days. The product from the presses' is dumped into steel cars having steam-jacketed bottoms, in which they are dried until the moisture content is between 15 and 17 per cent. when 8. per cent. of soda and .3 per cent. of borax are added and the contents thoroughly mixed. In the case of special clean-ups, the precipitate is tested and the flux is added to meet the requirements.

Jan 1, 1921

By Sidney Cornell

THE technical- advantages of adding oxygen to air and producer gas, or using it as a reactive agent, producing 400 B.t.u. gas instead of. the present 150 B.t.u., with higher flame temperatures and a reducing flame possible, with a smaller volume of gases passing through a furnace, will result in quicker melting, sharp working, and the production of a higher quality steel. Probably electric-furnace quality steel can be produced in an open-hearth furnace using oxygen. A modern, standard, 100-ton open-hearth furnace, with all equipment, costs from $350,000 to $500,000; there are about 1000 open-hearth furnaces in this country. When considering the use of oxygen in the open-hearth furnace, it is necessary to study: (1) The use of oxygen in the present furnaces, such that modification of existing furnaces and equipment cost the minimum, although the full advantages of oxygen are not thus obtainable. (2) The use of oxygen in a furnace designed for its use, producing quality and quantity steel at the lowest possible cost. This entails the junking of approximately one-half the value in existing equipment-writing off $250,000,000. The basis of such an estimate is the present cost of manufacturing open-hearth steel. Objection may be taken to some of the unit prices here given, but while some companies obtain their ores for much less, the prices quoted are -market price. They are used to show the maximum economy obtained by oxygen at that point.

Jan 11, 1924

By Mark C. Malamphy

AT present the Federal Government represents the only organization applying geophysical methods of prospecting in Brazil. The geophysical work of the National Department of Mineral Production, which will be described in the following pages, must be considered as a program of experimental work designed to demonstrate the applicability of the more or less "standard" methods of geophysical prospecting to various problems of economic interest in Brazil by means of practical examples of results obtained in certain typical areas. Our work is somewhat similar to that of the Imperial Geophysical Experimental Survey of Australia, but our task has been greatly simplified by the ever increasing number of technical publications relative to the theory of instruments and methods.

Jan 1, 1936

By O. W. Shimer, D. C. Helms, C. E. Brown

THE early history and progress of anthracite stripping, from the first known operation at Summit Hill in 1821 through 1917, was covered in 1917 in a paper by J. B. Warriner,1 then chief engineer, now president of the Lehigh Navigation Coal Co., and stripping methods between 1917 and 1931 were the subject of a paper in 1931 by H. H. Otto,2 of the Hudson Coal Company. The present paper is confined to methods used today on pitching beds in the western middle and southern anthracite fields. The anthracite industry, not unlike other large industries, had been affected for more than a decade by the adverse economic conditions of the country. High development and operating costs and the competition of other fuels caused some collieries to be closed temporarily, while others were permanently abandoned. In order to obtain a larger tonnage at a lower development cost, a larger stripping program was put into effect by many companies. In 1932, stripping operations accounted for 334 million tons, or 7 per cent of the total anthracite production of the year, and in the next 10 years this increased until more than double that amount, or over 14 per cent of the total production, was from stripping operations. These figures represent the total production of the entire anthracite region; unfortunately, the figures have not been separated from the different fields. There are some operations in the southern and middle western fields where the tonnage obtained from stripping amounts to more than 30 per cent of the total colliery production. Stripping operations on pitching beds present difficult problems. Owing to the various geological formations, a different situation is encountered in nearly every stripping pit; and because of the proximity of an overlying bed, it is very often necessary to load the entire overburden into trucks and haul it out of the pit to the dump area, although back filling and casting is done whenever possible. Beds in the areas described in this paper pitch from 20° to 90° and some are on the invert in, many sharp folds and faults. PLANNING The more successful strippings have had adequate engineering analysis. Some work is being done without much preliminary planning, but many strippings would have failed completely if close supervision by the engineering department had not been maintained. Locations of stripping areas are determined as follows: 1. By constructing cross sections over the areas and drilling sufficient diamond-drill or well drill holes to study the strata and to determine the location, thickness and pitch of the beds.

Jan 1, 1944

By A. W. Schlechten, R. F. Doelling

Parkes' process crusts were vacuum distilled using a shortened Pidgeon retort. Zinc was effectively removed below 800°C and recovered as a zinc sheet easily stripped from the furnace liner. Lead dasdistillationazinc required about 950°C and the resulting lead condensate tillationtended to stick to the thin metal liner. Final purity of residue is limited only by nonvolatile metals such as copper. THE successful commercial application of vacuum distillation for the removal of zinc from lead, as described by W. T. Isbell,' raises the question of whether or not a similar method can be used for other metal separations. Preliminary laboratory experiments on the vacuum distillation of Parkes' crusts by one of the authors' gave such encouraging results that it was decided to make a series of tests with large scale equipment to determine the results that might be expected in plant operation. The pilot-plant test results are reported in this paper. The great advantages of vacuum dezincing are its simplicity, the relatively low temperature of operation, and the fact that the zinc is recovered in the metallic state ready for use again in the desilveriza-tion of lead bullion. These same advantages and others would be realized from the vacuum distillation of the zinc-lead-silver crusts made in the Parkes' process. Zinc readily will distill over at temperatures of 800" to 900 °C as contrasted with the 1200°C or more used in the Faber du Faur furnace. Furthermore, the recovery of zinc as metal is practically perfect since there is no loss by oxidation or fuming. If the vacuum distillation is continued and hastened by raising the temperature to around 1000°C, the lead will distill over at an appreciable rate and deposit in a warmer zone of the condenser. This lead will contain a small amount of silver, but it can be returned to the desilverizing kettles and there is not the chance of loss that there is in disposing of the rich litharge from cupelling. The lower temperatures required will mean a saving of fuel and less wear on the equipment. One further point is that the vacuum distillation could be run on a small scale practically continuously, so as to avoid the accumulation of large amounts of silver-rich material and the need of assembling a large crew for special cupellation runs. It should be pointed out here that the final purity of the silver residue will depend on the copper or iron content of the crusts, as these and other metals with low vapor pressure will not be eliminated. The idea of treating the silver-zinc-lead crusts from the desilverization of lead bullion by vacuum distillation is not a new one, but such experiments have not been reported, as far as can be determined. In 1912, T. Turner presented a paper3 before the Institute of Metals on the vacuum distillation of brass, and a member of the audience suggested that he try his method on Parkes' crusts. In 1935, W. J. Kroll, noted for his discovery of debismuthiz-ing lead by calcium additions, published a paper' on vacuum distillation of metals and pointed out possible applications in the lead industry. Principles of Separation The successful separation of two or more metals by distillation depends upon an appreciable difference in the effective vapor pressures of the metals in the alloy to be treated. The vapor pressures of the common metals have been determined with considerable accuracy; for example, at 800°C the vapor pressures of the individual metals which are of particular interest in this paper are about .as follows: Zn, 241 mm; Pb, 0.0553 mm; and Ag, 0.0000276 mm. Unfortunately,, data are not available on the activities of the components in the ternary system Zn-Pb-Ag, but it can be estimated that on the basis of the vapor pressures of the individual metals a good separation can be made by distillation. The preliminary laboratory tests previously mentioned' supported this assumption. The pilot-plant size vacuum distilling furnace is shown in Fig. 1. It consisted of an abbreviated Pidgeon retort, 5 ft long with an ID of 8 in., heated by six silicon carbide elements placed symmetrically

Jan 1, 1952

[Separates of all the Technical Publications published in 1930 are available at Institute headquarters. All the papers are on file in public, university and technical libraries, and when so indicated in the list, may be found in the Transactions.] Metal Mining Technical Publi- Title Author Meeting Tran~. cation Volume No. and Page* 264-A.29 Quicksilver Industry in 1929. Im- L. H. Duschak San Francisco T30, 283, 319 provements in the Metallurgy of C. G. Maier and Oct., 1929 Quicksilver and Symposium on The others Present Status of the Quicksilver Industry (With Discussion) (37) 271-A.30 Observation on Ground Movement R. E. Palmer New York T30. 168 and Subsidences at Rio. Tinto Feb.. 1930 Mines, Spain (20) 274-A.31 Development and Installation of the C.L.Berrien New York T30, 139, 166 Hawkesworth Detachable Bit (29) Feb., 1930 276-A.32 Protective Measures . Against Gas 0. A. Glaeser New York T30, 129. 167 Hazards at United Verde Mine (11) Feb., 1930 287-A.33 Use and Cost of Compressed Air (12) R. S. Lewis New York Feb., 1930 314-A.34 Miami Copper Company Method of F. W. Maclcnnan New York T30, 39, YO Mining Low-grade Orebody (44) Feb., 1930 319-A.35 How Human Beings Respond to W. J. McConnell New York Changing Atmospheric Conditions Feb., 1930 (9) 324-A.36 Vertical and Incline Shaft Sinking at Arthur B. Foote San Francisco T30, 87 North Star Mine (21) Oct., 1929 32bA.37 Governmental Control of the Pro- W. E. Colby New York duction and Sale of Mineral Re- Feb.. 1930 sources (With Discussion) (16) 333-A.38 Some Recent Developments in Open- E. E. Hunner New York T30, 106, 117 pit Mining on the Mesabi Range Feb.. 1930 (25) 334-A.39 Mining Methods and Costs at Presi- V. D. Howbert El Paso dio Mine of American Metal Co. of R. Bosustow Oct., 1930 Texas (15) 339-A.40 Operation of Pressure Fans in Series W. 8. Weeks New York (8) V. 6. Grishkevich Feb., 1931 364-A.41 Top Slicing with Filling of Slices as H. Willey El Paso Used at the Charcas Unit of Com- Oct., 1930 pania Minera Asarco, S. A. (17) 373-A.42 Drill Sampling and Interpretation of H. T. Matson New York Sampling Results in the Copper G. A. Wallis Feb.. 1931 Fields of Northern Rhodesia (17)

Jan 1, 1930

By B. A. Kulp, R. R. Reeber

Lattice parameters for the wurtzite form of' CdS mere measured by powder X-ray diffraction techniques over the temperature range 26° to 1000 K'. A negative thermal -expansion coefficient was determined parallel and perpendicular to the c axis below 13.5°K. Near 808°K, the curves of the a, parameter, the differential thermal expansion, and the resistivitv vs absolute temperature exhibited a reversible discontinuity. j\. direct determination of the lattice parameters of CdS over an extended temperature range is of particular use in interpretation of the effects of high pressure on the band structure of semiconductor materials. For example, Langer' has studied the effects of pressure on the absorption edge of CdS from 77°K to room temperature. In order to properly interpret his results it is necessary to know the change in lattice constants as a function of temperature for the wurtzite, zincblende, and rocksalt2 modifications of this material. Thermal-expansion measurements for CdS, wurtzite phase, have previously been determined over a limited temperature range.s74'5 The zincblende phases, of other compounds with similar bonding, have been investigated by Novikova et a! .'' Previous thermal-expansion measurements for metals with hexagonal symmetry have for the most part used bulk sample techniques for low-temperature result. Most X-ray measurements at low temperature have been on materials with cubic symmetry.'jQ The use of X-ray powder-diffraction techniques offers a convenient and accurate method of measurement over a wide temperature range. The X-ray method, besides measuring unit cell size, also provides information about change in structure type and the nature of some of the stacking defects present. I) EXPERIMENTAL PROCEDURE The thermal expansion was measured by X-ray powder-diffraction techniques. Lattice parameters for the range 300" to 1000°K were determined in a 19-cm Unicam camera. From 26" to 300°K a 34-cm back-reflection camera with the Van Arkel" film arrangement was used. The sample was bonded to a copper cold finger below a helium, hydrogen, nitrogen, oxygen, dry ice, or ice brine bath in a metal cryistat. che inner bath was surrounded by another one for radiation shielding. Nitrogen was used in this outer bath for the very low-temperature runs while dry ice and acetone was used for the 195°K point. CuKa X-rays, filtered with a nickel foil, entered the cryostat through a 0.001-in.-thick aluminum window. During a typical 9-hr exposure the sample was continuously rotated through a 30-deg arc. Heat losses from the sample holder limited the minimum temperature attained to 26°K with helium in the inner dewar. Temperature calibration between 25" and 125°K was determined with an Allen Bradley 300-ohm carbon resistor. The resistor was attached to the back of the copper finger with a thin layer of silicone grease. Liquid He, HZ, N2, and O2 baths were used to calibrate the resistor. Temperature variation is estimated to be *2"K with a slightly higher uncertainty at room temperature and 264°K. The thermal expansion of high-purity germanium from 373" to 900°K was measured as a calibration for the Unicam camera. This value was compared with the known value1' for the thermal expansion. A discontinuity in the thermal-expansion coefficient of the CdS a, parameter was observed. Similar discontinuities in the resistivity and differential thermal analysis at the same absolute temperature indicate that the temperature error is *5°K in the temperature range above 500°K. Temperature errors in the Unicam camera below 500°K are appreciably higher due to large gradients in the resistance furnace. II) SAMPLE PREPARATION The CdS was Eagle Picher ultrapure grade. The crystallite size range of the as-received powder

Jan 1, 1965