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By E. J. Dulis, G. V. Smith

AS reported several years ago,' nitrogen may be taken up from the atmosphere by austenitic Cr-Ni steels during creep or creep-rupture tests. This was indicated by chemical analysis and by the appearance of a new microstructural phase, or phases, tentatively identified as chromium nitride (S), at the surface or at the intergranular cracks associated with fracture. The nitrogen pickup was observed to be dependent on time, temperature, and deformation. In a more recent investigation, a sample was obtained in which there was sufficient of the precipitate to suggest that it could be readily identified by X-ray diffraction. This sample had been taken from a 1/4 in. diam creep-rupture specimen of annealed, type 304L stainless steel of the following initial composition: C, 0.03 pct; Mn, 0.65; P, 0.010; S, 0.019; Si, 0.54; Cr, 19.50; Ni, 12.02; N, 0.031; and Al, 0.005. The specimen had ruptured after 10,470 hr at 1500°F (2000 psi). In this case nitrides were distributed across the whole section of the sample, Fig. 1. The precipitate occurred both at the grain boundaries and within the grains; the latter precipitate had in some cases the appearance of pearl-ite, and in others was distinctly Widmanstatten. Chemical analysis of the sample after test showed 0.64 pct "soluble" nitrogen (soluble in 1:1 hydrochloric acid: water) and 0.18 pct "insoluble7' nitrogen (insoluble in the hydrochloric acid solution but dissolved by fuming sulphuric acid). For identification of the precipitate by X-ray diffraction, the matrix in the surface layer of the specimen was dissolved by prolonged attack in an alcoholic solution of picric and hydrochloric acids. The appearance of the specimen surface after such etching is shown in Fig. 1c. The diffraction pattern of the surface-concentrated precipitate was obtained with a recording spectrometer in both the forward and back-reflection regions (the latter by adapting a special fixture to the conventional X-ray unit). The observed X-ray diffraction lines, Table I, show the presence of Cr,N and CrN; the agreement with interplanar spacings calculated from reported data2,3 is quite good. Since it has been suggested' that CrN dissolves only in concentrated sulphuric acid, whereas Cr2N dissolves in dilute hydrochloric or sulphuric acids, an effort was made to distinguish between the two nitrides. This proved possible, inasmuch as etching in a dilute solution of hydrochloric acid gave a sample in which microscopic examination showed that much of the Widmanstatten-pearlitic precipitate within the grains had been eaten out, leaving the grain boundary precipitate in relief, and which, when examined by X-ray diffrac-

Jan 1, 1953

By S. H. Ash

THE INVESTIGATION of barrier pillars in the Southern field is part of the comprehensive study of the mine water problem in the anthracite region of Pennsylvania by the Federal Bureau of Mines (1, 2, 5, 6, 7, 8, 9, 10, 11, 12, 15, 16, 18).4 Tim Southern field is in Carbon, Schuylkill, Dauphin, and Lebanon Counties, in eastern Pennsylvania; has an area of 200 square miles; is 70 miles long from Mauch Chunk on the east to the Susquehanna River on the west; and is 1 to 6 miles wide. In the Southern field are 37 underground water pools containing 37312 billion gallons of water (5). Most of these pools overflow to the surface because the barrier pillars controlling them are effective under existent, conditions. Abandonment of mines in the Southern field has resulted in the hooding of 34 percent of the field. The largest tonnage of reserves of anthracite lies in this field, where mining conditions are most difficult. Large reserves of anthra¬cite underlie the abandoned mine workings, and before a great part of these reserves can be developed and extracted, the abandoned workings must be unwatered and kept drained (5).

Jan 1, 1953

By Secretary of the Interior

"INTRODUCTION The Bureau of Mines Synthetic Liquid Fuels Program again forged ahead during 1952, and important technical advances led the way to improved methods of converting coal and oil shale into liquid fuels. Marking the eighth year of activities under this program, the past 12 months brought a new domestic industry nearer realization.The increasing demand for gasoline and oil and the rising cost of finding new petroleum, coupled with America's growing dependence on imports and the unsettled international situation, have continued emphasize the importance of the Bureau's Synthetic Liquid Fuels Program. Oil, the indispensable material of wartime, likewise has critical importance in peacetime, touching as it does the life of every individual. Supplementing petroleum with synthetic liquid fuels will not only conserve this Nation's petroleum reserves but also will bring into greater use its tremendous reserves of coal, as well as the vast deposits of oil shale for which no other practical use has yet been found.The Bureau of Mines Synthetic Liquid Fuels Program is one of the most important and far-reaching of the Government's research projects. Through development, of commercial synthetic liquid fuels, the United States can obtain oil products from its great inland reserves of coal and oil shale to supplement petroleum in any quantity that may be necessary, consistent with economic and other requirements, such as national defense. The use of raw materials from such deposits would be of highest importance in wartime, when shipping lanes are menaced by the enemy. The Synthetic Liquid Fuels Program of the Bureau of Mines and research efforts of industry have advanced American technology to the point where it is now possible to begin the design and construction of prototype plants. Certainly, significant improvements will be made as the program continues, but this prospect in no way alters the fact that the start of prototype plants should be encouraged. These plants, as the first step in the development of a synthetic fuels industry, would serve a threefold purpose:"

Jan 1, 1953

By E. H. Timmerman, A. F. van Everdingen, J. J. McMahon

The prevent paper contains a method which combines the material balance equation' with the water influx equation' to obtain reliable values for the active oil originally in place and a quantitative evaluation of the cumulative water influx. The method is illustrated by an application to a reservoir without original gas cap. In the absence of an original gas cap. results may be obtained using only field production and pressure data, PVT analyses. and a minimum of subsurface information. CHARACTERISTICS OF RESERVOIR AND RESERVOIR FLUIDS Production in the field under review is obtained from the top of the Wilcox formation of Eocene age, at a depth of approximately 8,100 ft subsea. The structural map, Fig. 1, shows that the accumulation, half elliptical in shape with the long axis in east-west direction, is trapped to the north and on the upthrown side of a normal fault. A number of east-west faults with additional minor faulting in random directions are found in the general area, and seismic information and production performance indicate in this particular case the existence of a second fault a short distance downdip, with a strike more or less parallel to the fault controlling the accumulation. It is estimated that 1,830 acres were originally underlain by oil and that the maximum thickness of the original oil column, about 37 ft, was only slightly greater than the maximum thickness of the oil-bearing sand. Maximum net sand thickness was estimated at approximately 26 ft. From logging and subsurface information the gross sand volume has been placed at 37.400 acre-ft. which reduces to about 27,500 acre-ft after probable non-productive intervals have been deducted. The following table presents laboratory analyse; data for the Wilcox sand cores. Average Average Samples Considered Permeability Porosity All Samples 236 md ..19.9percent Samples with k>l md 256 md 20.5 per cent Samples with k>8 md 275 md 20.9 per cent Interstitial water was estimated at 15 per cent. The initial gas-oil ratio was approximately 900 cu ft/bbl. and the initial shrinkage factor was determined by the laboratory to

Jan 1, 1953

The primary object of this paper is to describe the present metallurgical practice of the Emperor Combined Mill, wherein ores from the adjoining and Associated Mining Companies, Emperor Gold Mining Company Ltd., Loloma (Fiji) Gold Mines, N.L., and Dolphin Mines, Ltd., are treated for the recovery of gold and silver.The mining field is located in the foothills, five miles from the sea, on the northern side of Viti Levu, the largest and most important island of the Fiji group.The orebodies occur in basalt and associated ash beds overlain by andesite, tuffs and sediments. The basalt is a dark greenish-black rock and in much of the ore mined is weathered with alteration of the olivine to serpentine and iron oxides, of the augite to chlorite and of the minute included crystals of iron ore to other iron oxides. Into the basalt intrudes a considerable number of andesite dykes, and the lodes occur as veins in these dykes, as "flatmakes" along fissures or, ash beds extending horizontally from the dykes and at the contact of the basalt and the andesite dices.The Emperor orebody is the largest and most important, and consists essentially of massive, shattered, well altered and mineralized basalt.Little or no free gold occurs in the ore at present being milled, the most important host minerals for gold being the tellurides sylvanite and hessite, next in importance being the sulphides, pyrite, marcasite and arsenopyrite. Chalcopyrite is present in quantities large enough to be troublesome in the subsequent concentrate treatment section, while sphalerite, tetrahedrite, bornite, galena and native tellurium are present in small quantities.Unimportant occurrences of native copper have been observed in both Dolphin and Emperor orebodies.

Jan 1, 1953

By W. H. Triplett

Silver-lead-zinc replacement deposits occur in limestones of the anticlinal Caja range at Providencia, near Avalos, Zacatecas, Mexico. The description deals with intrusives, outcrops, preferred horizons, changes from bedding to fracture, control in depth, and variations in abundance and ratios of minerals throughout a vertical range of 500 m. THE purpose of this paper is to record a few field observations and accumulated office data concerning outcrops, relation of ore occurrences to intrusive and host rock, and mineral zoning. Reasons for some of the phenomena are not clear to the author so the facts are given with the hope that other investigators may be able to furnish the explanations. The Avalos unit of the Compania Minera de Penoles, S. A., operates the Alicante, Bonanza, Providencia, Albarradon, San Eligio, Nazareno, Leona, Salaverna, and Santiago mines situated between Avalos railroad station and Concepcion del Oro on the Coahuila and Zacatecas railroad in the State of Zacatecas, Mexico. Some of these mines are within Penoles property while others are on mining claims leased from the Compania Nazareno y Catasillas, S. A., Mazapil Copper Co., and the American Smelting and Refining Co. The main office and camp are at Providencia, about 170 km southwest of Monterrey, N. L., so the silver-lead-zinc mines of the district are usually referred to as the Providencia mines. The Aranzazu, Catarroyo, and Cabrestante copper-gold mines are situated a few kilometers to the southeast on the same mountain range near Con- cepcion del Oro, the name by which the camp is known. It is operated by the Mazapil Copper Co. The main theme in the following pages is a description of the silver-lead-zinc ore occurrences of the district. Rock Formations Sedimentary Rocks: Many competent geologists have contributed generously to an ample fund of information concerning the sedimentary columns of northern Mexico. Among them are Carlos Burck-hardt, E. Bose, L. B. Kellum, and R. W. Imlay. Carlos Burckhardt, who covered a number of extensive areas in many parts of the Mexican Republic, devoted years to mapping the geology of the Caja, Zuloaga, and Santa Rosa mountain ranges around Mazapil, Concepcion del Oro, and San Pedro de Ocampo, Zacatecas. He did most of the original mapping which has been used as a basis and amplified by others. C. E. Burbridge and, more recently, John

Jan 1, 1953

By F. W. C. Boswell, R. L. Cunningham, H. M. Weld

Chemical analysis shows the partition of the magnesium addition between the metal and the graphite is independent of whether the graphite is in the form of nodules or flakes. The bright central spot observed in nodular graphite polished sections is shown to be due to the structure of the nodules. DURING the past few years numerous papers have been published on the production1-7 and heat treatment" of nodular cast irons. However, very little information is available on the structure of the nodules and the reason for their formation. It would appear that an explanation of the phenomenon of nodulation must await a detailed knowledge of the nature of the nodule. Disagreement exists among various workers on such a fundamental point as to whether or not a nodule actually contains a microscopically visible, nongraphitic nucleus.9-11 Work was initiated with a view to obtaining definite information on this and other aspects of the problem. Chemical Separation and Analysis Microscopic appearance had indicated9-11 that a nongraphitic core might exist in nodules (Fig. 1). It appeared that a chemical comparison of separated nodules and flake graphite would be profitable, for if the core is nongraphitic a relatively large amount of certain elements would be found in the nodules as compared to the flake. This comparison could best be made by obtaining nodules and flake from the same melt of cast iron, part of which had been in-noculated with a suitable addition reagent for the formation of nodules. A 300 lb melt was produced. About half of this was innoculated in the ladle with an Fe-Si-Mg alloy to produce nodules and cast into keel blocks; the remaining half of the melt had silicon added in an effort to compensate for the silicon in the innoculant used in the other half of the melt and this was cast into similar keel blocks. The analyses of the resultant irons are given in Table I. Nodules and flake were chemically extracted from 2 kg samples of metal as described in the appendix. While this method dissolved the iron and chromium carbides, it did not dissolve the titanium, vanadium, and molybdenum carbides. These latter carbides could have been removed by nitric acid, but in other experiments it was found that it attacked pools of metallic iron entrapped in the nodules which had, until the nitric acid treatment, been protected from the attack of the sulphuric, hydrochloric, and hydrofluoric acids. It will be shown in the next section that entrapped iron exists in nodules but not in flake. On microscopic examination many tiny irregular particles were observed to accompany both the nodules and the flake. These were identified by tabling a sample of nodules from which a sufficient fraction was obtained for X-ray analysis. A good pattern of titanium carbide was obtained indicating that this was the predominant compound present. Since it was not possible to determine how completely the carbides could be removed mechanically and since their removal from flake is much more difficult, it was decided not to resort to any separation as this would render further comparisons more difficult. The samples were ashed in a combustion

Jan 1, 1953

By Alan Stanley

THE MacIntyre Development of National Lead Co. is located at Tahawus, N. Y., in the heart of the Adirondack Mountains. Operations involve the mining and concentrating of a titaniferous iron ore to produce ilmenite and magnetite concentrates. A general description of the operation and metallurgy has been given by Frank R. Milliken.' Pigment plant production demands that the MacIntyre mill produce a 44.7 pct TiO, ilmenite concentrate. To achieve the required ilmenite grade and tonnage it is important that the table concentrate grade be closely controlled. Unfortunately, however, the titaniferous orebody which feeds the MacIntyre mill is not uniform. Ore dressing characteristics vary from one end of the orebody to the other, and from • one level to the next. The changeable nature of the mill feed precludes a single adjustment of the equipment for long periods of time. Thus the operators must constantly watch the equipment to insure a uniform concentrate from the fine and coarse tables and Wetherills, or dry magnetic separators. Chemical assaying of mill products requires about 4 hr from the time the sample is taken until assay results are obtained, and this is available only on a two-shift basis. The ore may change rapidly, even several times during a shift, so that assay results lose most of their control value by the time they are reported to the mill operating crew. Members of the crew have therefore tried to evaluate the table and Wetherill concentrate by visual inspection, since through long experience the shift operators, under most circumstances, can gage closely the grade of the mill products. However, there are times when the physical nature of the ore is radically different from normal. Under these conditions visual inspection is of no value, and at such times final ilmenite as low as 43 pct TiO, has been produced and shipped before the assay results have been received. The specific gravity method of assaying for TiO, has been attempted to eliminate the shipping of ilmenite below normal grade as well as to help control day to day and hour to hour mill production. Table I shows the minerals found in the MacIntyre ore along with their average weight proportions and specific gravities. The first two products considered for the specific gravity method were fine and coarse table concentrates. It was reasoned that these products were essentially ilmenite with the higher specific gravity gangue minerals. Since they were always produced the same way, and the desired grade of TiO, was always constant, the specific gravity of these materials would increase or decrease as the amount of ilmenite increased or decreased. Thus for table concentrates which assayed 40 pct TiOz a constant gravity would invariably be obtained, and as the TiO, value changed the specific gravity would change in direct proportion. The third product considered was Wetherill ilmenite. It was assumed that a desired grade of 44.7 pct Ti02 would also always contain the same amount and type of gangue minerals along with the ilmenite, and thus would always have the same specific gravity. As the TiO, value of the ilmenite concentrate changed so would its specific gravity. Dr. Kenneth Vincent, chief metallurgist of the Baroid Division of National Lead Co. at Magnet Grove, Ark., ran specific gravity tests on 17 samples of the desired products. The lowest specific gravity reading assayed the lowest in TiO, and as the specific gravity increased the trend was for the TiO, assay to increase, see Fig. 1. Since these results warranted further investigation, a 500-g capacity Torsion balance and 250 ml Le Chatelier specific gravity bottles were obtained. Shift samples of fine table concentrate, coarse table concentrate, and final ilmenite were tested. Each sample was split and 85 g weighed on the Torsion balance. The Le Chatelier bottle was filled with water to a zero mark. To avoid wetting the neck of the bottle it was found necessary to do this

Jan 1, 1953

By J. H. Hild

The Shanton magnetite-ilmenite deposits lie on the east flank of the Laramie Mountains, 43 miles northeast of Laramie, Albany County, Wyo. (fig. 1). The Shanton and other similar deposits in the Laramie Mountains were examined by Bureau of Mines engineers during 1942, 1943, and 1945, and a report2/ describing the results of a dip-needle survey and surface sampling was published in 1946. The Shanton deposits occur in a relatively flat section of the range at altitudes varying from 7,500 to 1,650 feet (fig. la). Prevailing rocks in the Shanton area consist of anorthosite with intrusive dikes of gabbro differentiates and granite. Titaniferous magnetite outcrops in five masses, which are separated at the surface by overburden and anorthosite.

Jan 1, 1953

I have chosen this topic for my address with the intention of preserving a rather extraordinary record of recurrent additions of capital in the financing of one of the world's important silver-lead-zinc mines. The recitation of the trials and tribulations which fore-shadowed the rise of Mount Isa Mines to a position of relative prominence in the realm of non-ferrous mineral production may, I hope, be of assistance to some of the younger members of the Institute who may be called upon during their careers to meet similardevelopmental and financial problems.Mount Isa Mines Limited was incorporated in New South Wales in 1924 with an Authorised Capital of 40,000 shares of £20 each.In November 1925 the Company acquired the leases and water rights of the Mount Isa Proprietary Silver-Lead Limited for 6,250 fully paid £20 shares. Shortly thereafter, but in the same year, the £20 shares were split up into £1 shares, thus bringing the Authorised Capital to £800,000.The leases purchased consolidated and brought under one management the principal ore bodies of the Mount Isa area.Transportation facilities were indispensable to the economic future of the field, so the construction of a railway extending the Government line from Duchess, 54 ,miles to Mo.unt Isa, was assured by the passage of a bill in October 1925 by the Queensland Parliament. Under the provisions of the so-called Mount Isa Railway Act the Company was required to idemnify the Government against national loss on this branch line for a period of 10 years.

Jan 1, 1953

By G. G. Gunther, C. L. Boeke

(Any discussion resulting from presentation at the Los Angeles Extractive Metallurgy Division Meeting will appear in the November 1953 issue.) I. M. Symonds (Cia Minera de Penoles, Monterrey, N. L., Mexico)—This is a most interesting paper describing zinc deleading operations. Mr. Gunther was kind enough to show me his operation last fall. Outside of the excellent results, I was most impressed by the ease of control. I had expected a difficult operation requiring careful control and supervision, but found one requiring little attention. The only disappointing fact of the separation is the poor copper recovery in the concentrate of the deleading float. The final zinc concentrate still has about 3 pct chalcopyrite (assuming the copper is chalcopy-rite) which adversely affects the zinc grade. If the copper mineral is free, the poor recovery is probably due to the high cyanide concentration. Fortunately, about 75 pct of the copper is recovered before the pulp goes to the zinc circuit. Mr. Gunther's remarks about proper cyanide to zinc sulphate ratios cannot be overemphasized. Although our experience has been mostly confined to the conventional Pb-Zn separation, we have found these ratios most important, and more important in the mill than in the laboratory. The laboratory appears to give optimum results over a wider range of reagent control than the mill, especially in regard to the effect of cyanide. In the mill in handling relatively high grade ores, we usually find that ratios of cyanide to zinc sulphate of 1 to 10 or 20 or higher work best. Where there is a substantial amount of chalcopyrite present, it has been noted that cyanide in the range of 0.02 to 0.10 lb per ton of ore is often beneficial in zinc rejection and possibly in copper recovery in the lead concentrate, while larger amounts, say 0.20 to 0.25 lb per ton, will float more zinc and cause a serious rejection of chalcopyrite. On an ore with 15 to 20 pct Zn content, we have had to use 0.8 to 1.2 lb of zinc sulphate per ton of ore with the above cyanide to obtain optimum results. Sometime ago we made a laboratory study following Parral and Santa Barbara practice on an ore which never had a very satisfactory rejection of zinc in the lead concentrate. The results were not encouraging and a mill test was not run. Since then the study has been reopened using fresh zinc concentrate from the mill in the laboratory instead of one made in the laboratory. A reasonably clean lead float from the zinc concentrate was obtained. It has been checked several times and each time the zinc concentrate made in the mill responds and the one made in the laboratory does not. Although undoubtedly some reasonable explanations can be given, it is presented here only

Jan 1, 1953

By H. Wilton Clark

"IntroductionTHE CANADIAN use of short-period delay-action detonators in coal shooting has been carried on for about two years, mostly in British Columbia, and this is a preliminary report on progress to date. Entire coal faces are being shot successfully with one application of electric current.The electric blasting cap came into use about the beginning of the century. The low-tension electric cap, the type most commonly used, consists essentially of a metal tube containing an initiating explosive. Two wires lead into the end of the cap and are connected inside the cap with a short 'bridge wire .of very high resistance. This •bridge wire is buried in a match-head of a readily ignitable powder composition. When current goes through the lead wires, the bridge wire becomes extremely hot and sets• off the match-head which, in turn, ignites the powder just below it in the tube. This explosion sets off the main charge of explosive. Thus, by connecting a group of caps to a source of electric .current, a number of charges could be exploded simultaneously. This immediately became of great value to mine and quarry operators. Explosives could now be used to break up large masses of material at one time, as against the older, slow method .of blasting small amounts with single charges.The next step was to develop a delay detonator which would allow charges of explosive to fire one after the other, one or two seconds apart. Such detonators allowed first blasts to relieve some rock burden before the next charge fired, giving the second charge an easier task in forcing out more rock, and so on for the rest of the series of charges."

Jan 1, 1953

By N. H. Grace

"IntroductionDURING the past half century, the economy of Western Canada was largely centred on agriculture. However, the impact of World War II has led to an acceleration in the development of a variety of natural resources so that, today, Western Canada is experiencing great industrial development. Consequently, the availability •of low-cost energy assumes prime importance. In the final analysis, industrial growth and expansion are intimately linked to the energy resources.Coal ReservesHas Western Canada adequate coal reserves to meet the present accelerating demand for power in the days that lie ahead? This question must be answered before detailed consideration can be given to the probable patterns •by which various energy sources in Western Canada may be expected to meet the expanding demand. Figure 1 indicates the extent and distribution of the Canadian coal reserves, the data having been prepared by Dr. B. R. MacKay for the Royal Commission on Coal in 1946 (1). The amount of readily recoverable coal is listed as one-half the quantities shown on the chart. It is interesting-to note that upwards of 90 per cent •of the Canadian coal reserves .are located in the three most westerly Canadian provinces. It has been estimated that the coal reserves, at the present rate of mining, would be adequate for about 3,000 years. Consequently, it may be concluded that the coal •reserves in Western Canada •are indeed adequate to meet tremendous energy demands for many centuries. When the oil and natural gas have been exhausted, the great coal reserves will still be available."

Jan 1, 1953

By Joseph J. Wallace

1. From the standpoint of present production and recoverable reserves, there are two beds of major importance in Allegheny County -Pittsburgh and Upper Freeport -and one of lesser importance -Redstone. 2. Known measured and indicated reserves in all beds, based on a minimum thickness of 14 inches and 1,800 short tons per acre-foot of coal in place, are estimated at 832 million short tons as of January 1, 1953. Of this total, 768 million short tons is in beds 28 inches and more thick. Areas in some beds were omitted from the estimate because available data relative to the bed characteristics are too meager for making an estimate that conforms with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove reserves in these areas, such reserves should be added to the total estimated reserves.

Jan 1, 1953

By C. N. Schuette

THE producers of this liquid metal call it quicksilver, while the consumer generally refers to it as mercury. It is one of he seven metals that were known to the ancients. These seven were gold, silver, iron, copper, quicksilver, lead, and tin. Other metals were sometimes accidentally alloyed with some of these, but it was not until 1490 that antimony, for example, was discovered and identified as a separate metal. It is not surprising that quicksilver should have been known in ancient or even in prehistoric times, as globules of the native metal often occur in the outcrops of the ore. Furthermore, the first man to build a fire on an outcropping of quicksilver ore would probably have found globules of quicksilver in the cold ashes of his fire after it burned out. The inability to pick up the globules with the fingers would excite interest and an attempt to gather it in shells or gourds to be exhibited and traded. The ore of quicksilver is the red sulfide, cinnabar, which has been mined and used as the pigment vermilion since before the beginning of written history. In recorded history, quicksilver is first mentioned in documents by Aristotle, 384-322 B.C. Theophrastus, in 315 B.C., credited the Athenian, Callias, with the invention of methods to beneficiate cinnabar in 415 B.C. In China also there are records antedating Christ which mention both vermilion paint and the fluid metal. From these early records, it seems certain that not only was cinnabar used as a pigment in those days but also that the metal was reduced from the ore and was used for amalgamation, for gilding, and for medicinal purposes. Quicksilver mining and metal-

Jan 1, 1953

By Paul D. Merica, O. B. J. Fraser

PROBABLY the first metallic objects used by man were nickel alloys. In search for flints suitable for the fashioning of their rude tools, our paleolithic ancestors, some 25,000 years ago, quite likely may have come upon some of those heavy, metallic fragments that we now know as meteorites, which consist of an alloy of nickel and iron containing usually from 5 to 15 pct of nickel. Whether paleolithic man ever did discover and use meteoritic fragments, his sketchy records do not actually disclose. We do know, however, that such fragments have been found and used by peoples, particularly the North American Eskimos, for weapons and implements in just the same manner as stones, and prior to any knowledge by those peoples of the reduction of metals from ores. Meteoritic showers were recorded frequently in earliest times and the meteorites often were found and fashioned into useful objects. The ancient Arabic and other myths of "invincible swords fallen from heaven" seem thus to have had a very definite basis in fact, and such weapons, of meteoritic material, have actually been re- covered from archeological excavations. It thus seems probable that meteoric nickel-iron was found and used long before iron was recovered by smelting iron ores (perhaps about 1200 B.C.) and probably even before there was knowledge and use of bronze and gold. Although many centuries were to pass before nickel was first isolated, in 1751, from Swedish ores and recognized as an elemental

Jan 1, 1953

By Donald F. Taylor

TANTALUM and columbium are newcomers in the world of metals. Many of the metals described in this volume had been known and used for centuries before either tantalum or columbium was known to exist. The scarcity of the ores and the comparative difficulty of extraction delayed their technology until specialized methods of processing could be developed. HISTORY Early in the nineteenth century, 1801, Hatchett discovered a new oxide, which he called columbium oxide, and a year later, Ekeberg announced that he had found a new element, which he named tantalum. The preparation of the metal tantalum in impure form was first announced by Berzelius in 1824, but the actual production of ductile metal did not occur until 1903, when von Bolton, of Siemens and Halske, developed a process for the production of tantalum pure enough to be drawn into electric-lamp filament wire. The use of tantalum as a filament wire began to decline when ductile tungsten was introduced in 1909. In 1921, C. W. sake, of Fansteel Metallurgical Corporation, produced the first ingot of tantalum metal in America. The first ingot of columbium was produced in 1927 in the laboratory of the same company. There are several good reasons why tantalum and columbium are often mentioned together. They occur together in their important minerals, are similar in many of their properties, and are

Jan 1, 1953

By P. A. Laxen, H. R. Spedden

WHEN a mineral particle is fractured, bonds between the atoms are broken. The unsatisfied forces that appear at the newly formed surface are considered to be responsible for the adsorption of ions at the mineral surface. A knowledge of the mechanism and extent of ion sorption from solution onto a mineral surface is of interest in the development of the theory of flotation.'*' Study of the adsorption of sodium from an aqueous solution oftheon quartz offers a simple approach to this complicated problem. The availability of a radioisotope as a tracer element meant that accurate data could be obtained."." Three main factors which appeared likely to affect the adsorption of sodium are: l—concentration of sodium in the solution, 2—concentration of onotherof cations in the solution, and 3—anions present in the solution. Hydrogen and hydroxyl ions are always present in an aqueous solution. By controlling the pH, the concentration of these two ions was kept constant. The variation in thesethe amount of sodium adsorbed with variation in sodium concentration was then determined under conditions standardized in regard to hydrogen ion. The effect of concentration of hydrogen ions and of other cations was also measured. A few experiments were made to get a preliminary idea on the effect of anions. The active isotope of sodium was available as sodium nitrate. Standard sodium nitrate solutions were used throughout these experiments except when the effects of other anions were studied. It was found that sodium adsorption increased with sodium-ion concentration, but less rapidly than in proportion to it. Increasing hydrogen-ion concentration, or conversely decreasing hydroxyl-ion, brings about a comparatively slight decrease in sodium-ion adsorption. Increasing the concentration of cations other than hydrogen or sodium decreases somewhat the adsorption of sodium ion. It would appear as if the kind of anion is a secondary factor in guiding the amount of sodium ion that is adsorbed. Materials and Methods Quartz The quartz was prepared as in previous work in the Robert H. Richards Mineral Engineering Laboratory' except for the refinement of using de-ionized distilled water for the final washing of the sized quartz, prior to drying." To minimize the laborious preparation of quartz, experiments were made to determine .whether the sodium-covered quartz could be washed free of sodium and re-used. The experiments were successful as indicated by lack of Na" activity on the repurified material and by its characteristic sodium adsorption. Table I gives the spectrographic analyses of the quartz used. The quartz ranged from 16 to 40 microns in size, averaging about 23 microns (microscope measurement), and had a surface of 1850 sq cm per g (lot I), 2210 (lot 11) and 2000 (lot 111) as determined by the Bloecher method." Radioactive Sodium Method of Beta Counting for Adsorbed Sodium: Na22, the radioisotope of sodium, possesses convenient properties.' It has a half-life of 3 years, thus requiring no allowance for decay during an experiment. On decay it emits a 0.575 mev ß+ radiation and a 1.30 mev r radiation. The decay scheme is illustrated in the following equation: ß+ NaR-------'8'77NeZ2 3 years The /3 radiation is sufficiently strong to penetrate an end-window type of Geiger-Mueller counting tube. This, in turn, makes it possible to use external counting, a great advantage in technique. Furthermore, it permits the assaying of solids arranged in infinite thickness, while assaying evaporated liquors on standardized planchets. The equipment used was standard and similar to that employed by Chang.R The original active material was 1 ml of solution containing 1 millicurie of Na" as nitrate. This active solution was diluted to 1000 ml. Five milliliters of this diluted active solution was found to give a quartz sample a sufficiently high activity for accurate evaluation of the sodium partition in the adsorption measurements. Also, 1 ml of final solution gave a sufficiently high count for precision on the liquor analyses. The sodium concentration of the diluted active solution was 1.2 mg per liter, so that 6 mg of sodium for 60 ml of test solution and 12 g of quartz was the minimum amount used. The active solution was stored in a Saftepak bottle. Procedure for Adsorption Tests: The method consisted of agitating 12 g of quartz with 60 ml of solution of known sodium concentration for enough time to establish equilibrium between the solution and the quartz surface. The quartz was separated as completely as possible from the solution by filtering and centrifuging. The activity on the quartz and in the equilibrium solution was measured and the partition of the sodium was calculated from the resulting data. The detailed procedure for the adsorption test is set forth in a thesis by Laxen." In brief, it included the following steps: 1—Ascertainment of linearity between concentration of Na" and activity measured. 2—Evaluation of factor to translate activity on solid of infinite thickness in terms of activity on an evaporated active film of minute thickness, on the various shelves of the counter shield. 3—Taking precautions to avoid evaporation of water during centrifuging

Jan 1, 1953

By Alfred R. Powell

FOR the purposes of this discussion, the direct gasification of coal means the of hydrogen and carbon monoxide by the well-known water-gas reaction. Chemicals or other synthetic products may be made from these constituents of the gas and under such circumstances the gas is called synthesis gas. Or, if the same gas is used as a fuel, it is called blue gas or water gas. This type of gas has usually been made from coke, especially in this country, and has been used both for fuel purposes and for manufacture of chemicals. Recently, natural gas has gained the ascendancy as a source of synthesis gas for manufacture of chemicals because of its relative cheapness. As natural gas becomes less readily available and more expensive, coal will take its place as a raw material for the preparation of synthesis gas. This substitution will probably take the form of direct gasification of the coal rather than the present two-step procedure of carbonization of the coal followed by gasification of the coke. The chief reason for this probability is the intensive research now being carried on by several organizations to develop successful and economical processes for the direct gasification of coal, which is a considerably cheaper fuel than coke. In the following pages an attempt has been made to predict the chemicals that will result from this future production of synthesis gas by the direct gasification of coal. CHEMICAL REACTIONS OF SYNTHESIS GAS Given the proper conditions, there are many chemical reactions leading to production of useful products that can be carried out with this mixture of hydrogen and carbon monoxide. These many reactions may be grouped into three classes: (1) interaction of hydrogen and carbon monoxide, possibly with addition of other reactants; (2) reaction of hydrogen with various substances; (3) reaction of carbon monoxide with various substances. Thus sometimes hydrogen and carbon monoxide are utilized together in the same chemical reaction while in other instances only the hydrogen or only the carbon monoxide is required as a reactant. Fortunately, practical methods are available for securing either hydrogen or carbon monoxide from synthesis gas, some of which are also applicable for changing the ratio of these two constituents in the gas when that is desirable.

Jan 1, 1953

By W. Rostoker

LAVES and Wallbaum1 and more recently Duwez and Taylor' have reported on the occurrence of a family of intermediate phases having the composition Ti2X, where X may be Cu, Ni, Co, Fe, or Mn.

Jan 1, 1953