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The production of sulphuric acid at Port Pirie by the contact process began in March 1924 with the commissioning of the Electrolytic Zinc Co.'s roasting and acid plant. This plant, operated by B.H.A.S. Pty. Ltd. on behalf of the E.Z. Co., continued to produce sulphuric acid from the gases evolved when roasting Broken Hill zinc concentrate in mechanically rabbled furnaces until September 1954, when the plant was closed down.In this peri9d of approximately 30 years some 600,000 mono tons of 98·5 per cent sulphuric acid was produced, most of which was used for fertilizer production at Wallaroo and Port Adelaide. During World War II 14,400 mono tons of the above was produced in the form of 20 per cent Oleum and railed to the Salisbury Munitions Factory for use in the production of nitro-glycerine, gun-cotton and T.N.T.In the early post-war period various ways of converting at least some of the sulphur in the gases' discharged to atmosphere from the lead sintering plant were considered until, in 1949, it was decided to erect a modern contact acid plant. Much work remained to be done on the roasting plant to produce a gas of suitable grade for the contact process and also on the design of a purification section suitable for the treatment of D.L. gases.The acid section itself, however, was largely of conventional design and it was therefore decided that this would be erected first. To it was then attached a sulphur-burning section to allow it to operate as a "hot gas" brimstone acid plant until the roasting and gas purification plants had been designed and erected. In this way the urgent need for sulphuric acid in the fertilizer industry would be relieved, to some extent at least, as soon as, possible.

Jan 1, 1956

By N. E. Hanna

Originally developed for use in coal mines where on-shift blasting with explosives was prohibited, compressed-air blasting has been used for the past 15 years as a substitute for fixed explosives. With the current commercially available compressed-air systems -Airdox and Armstrong -coal is dislodged by a high-pressure discharge of air from a pressurized shell placed in the coal borehole. In the original systems stationary compressors were mounted on the surface or in the underground ventilated areas. These proved so successful that a mobile compressor unit was developed for use at the working face. Because of the possibility that such a unit might operate in a gassy atmosphere, the Bureau of Mines has investigated the hazards associated with operation under conditions where firedamp could accumulate in explosive concentrations. ACKNOWLEDGMENTS Grateful acknowledgment is made of cooperation of C. E. Carter, H. R. Hiller, R. E. Kennedy, H. Kohn, H. D. Metzinger, J. Mahoney, J. Nickovich, G. So Scott and I. Spolan in the experimental work.

Jan 1, 1956

By H. Krueger, H. N. Hersh

USE of autoradiography in diffusion studies offers the advantage that no repeated sectioning is necessary and that the analyses are performed in a simple manner over the continuous range of penetration depths. As part of a program of solid-state physics, it was desired to develop the autoradio-graphic method' quantitatively for use in diffusion studies. Results are reported here for the self-diffusion of silver. Silver was chosen because the existing data are good enough to evaluate the technique." The silver used in this investigation was obtained in the form of ¼ in. diam rods of polycrystalline material, 99.99 pct purity. The radioactive silver, Ag110 (ß, y), was obtained as the nitrate and converted to the chloride for use in a standard cyanide plating bath. The diffusion specimens were 1/2 in. lengths of the rod. They were mounted in bake-lite and the exposed circular face carefully ground and polished. Prior to electrodepositing radioactive

Jan 1, 1956

By Lloyd Williams

1. The investigation shows that the Poplar Creek and Big Mary beds contain the largest known recoverable reserves of coal in Morgan County, Tenn. The Poplar Creek bed has been the most productive. 2. Known measured and indicated reserves of coal, based on a minimum bed thickness of 14 inches and on 1,800 short tons per acre-foot of coal in place, are estimated to be 96 million tons, as of January 1, 1954. Of this total, 59 million tons is in beds 28 inches and more thick. Areas in each bed were omitted from the estimate because available data relative to the bed characteristics were too meager to make 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, 1956

By A. T. Coumbe

During 1953-55, 31,105 miles of pipe for transporting crude petroleum and refined products was laid in the United States, a total slightly below that of the prior 3-year period, according to data compiled by the Bureau of Mines, United States Department of the Interior. The added mileage consisted of 22,571 miles of new pipe, representing about 2,163,807 tons of steel, plus 8,534 miles of secondhand pipe, equivalent to about 419,849 additional tons of steel. During the 3-year period, 13,069 miles of pipe was taken up. By January 1, 1956, the Nation had 188,540 miles of pipeline, an 11-percent gain over the 1952 total of 170,504 miles. The greater use of larger diameter pipelines indicated in recent surveys has continued, as the mileage for sizes 12 inches and over increased from 13 percent of the total mileage at the close of 1952 to 16 percent 3 years later. Crude-oil trunklines 12 inches and over in diameter gained 24 percent during 1953-55, and these larger lines represented 30 percent of the total mileage compared with 25 percent at the close of 1952. Furthermore, the mileage for crude-oil lines less than 12 inches in diameter declined 2 percent and made up only 70 percent of the 1955 total against 75 percent n the previous survey. Product Lines 8 inches and over increased 43 percent from 1952 through 1955 and composed 70 percent of the total mileage compared with 66 percent in 1952.

Jan 1, 1956

The completion of the Hot Strip Mill at the Port Kembla works of Australian Iron & Steel Ltd., makes possible the production of steel plates and wide strip of a quality and in quantities not possible previously in Australia, and will also enable the production of tinplate to be undertaken in this country.The site chosen for the mill was a mud fiat underlain by a hard stone bottom at 5, to 801 feet below the surface; and a total area of one hundred acres was reclaimed to a level of 20 feet above the original surface.Three adjoining buildings were constructed to house the slab receiving yard, mill equipment and electric drive, together with the plate finishing line.After slabs have been heated to 2250°F at a rate of 90 tons per hour, they are transferred to the vertical scale breaker which is the first stand in the hot roughing mill. Here the primary furnace scale is first cracked and then blasted off by high velocity water descaling sprays.The next stand is the horizontal scale l;Jreaker, where any remaining primary scale is broken and then blasted off. After descaling, the slabs pass to the broadside mill, where short slabs are turned and rolled on broad side for wide plate.The next step is a slab squeezer which squares up the edges after broadsiding ready for the reversing mill. This is the finishing stand for plate and the last roughing stand for strip, which then passes to the finishing mill.The hot strip finishing mill consists of six stands with a maximum finishing speed of 2,230 feet per minute. Strip is cooled for coiling by water sprays on a hot run table and then coiled on a mandrel type downcoiler, from whence coils of hot strip are weighed and transferred by conveyor to the coil storage building.Plates are transferred from the reversing mill to the plate finishing line where operations consist of levelling, inspection, branding, cutting to width and length:INTRODUCTIONDue'to the increasing production of cars, refrigerators, washing machines and similar consumer goods in Australia, together with the increased requirements of galvanised iron...

Jan 1, 1956

By Oliver Bowles

Limestone, including dolomite, is the most widely used of all rocks - nearly 300 million tons annually in the United States alone. It occurs in some form in every State and is produced in thousands of localities. Because of its attractiveness, substantiality, and durability it is employed extensively as a building stone. In crushed and broken form it is used for concrete aggregate and railroad ballast and in highway construction, metallurgy, agriculture, and a host of chemical and industrial processes. This paper proposes to furnish general information on the origin and occurrence of limestone and dolomite, chief production centers, major uses, and methods of quarrying and preparing stone for market. Footnote references will guide the reader to sources of more complete information.

Jan 1, 1956

The sulphides can be arranged in a series determined by the relative amounts of ionic and covalent bonding present. This series is similar to the paragenetic series common to most sulphide ore deposits. Investigation of the surface tensions of the corresponding heavy metal iodides by the maximum bubble pressure method throws some light upon this relationship. It is shown that the surface tension of molten iodides decreases as the chemical bonding within them becomes more covalent. These results are interpreted in terms of the constitution of the melts, and are extended to cover the case of sulphides in solution in a silicate melt. It is concluded that sulphides tend to lower the surface tension of silicate melts and that this tendency becomes greater as the bonding within the dissolved sulphide groups becomes more covalent. A possible relationship between this conclusion and the origin of paragenesis in sulphide ore deposits is indicated.INTRODUCTIONIt is well known that the order of deposition, or paragenesis of sulphide minerals is remarkably similar in hypogene ore deposits throughout the world. This widespread similarity points towards the operation of some fundamental process which must be intimately connected with -the genesis of these ores. A correct interpretation and understanding of the causes of paragenesis in sulphide ore deposits would shed much light on the origin of these deposits.In Table 1 a simplified paragenetic series for sulphide minerals is presented. In most cases, only the most important sulphide of any particular element has been included. The object of this procedure is to simplify the following discussion. Furthermore, it should be realized that this series is only a generalization and that exceptions and reversals of position are quite common. Especially does this...

Jan 1, 1956

By A. L. Simpson, J. M. Edwards

The application of the Scintillometer to radioactivrty surveys in boreholes of oil wells has made it possible to determine bed thickness with a high degree of accuracy. This fact, combined with known relation of logging variables, makes thin bed porosity determination practical. With the use of the Scintillometer a method hot been derived whereby the apparent level of radiactivity, as recorded on radiation logs, may be converted to the true level. The true level of radioactivity is that level to which the recording pen would have traveled had the detector remained at a given depth for on infinitely long period of time. This factor is: radioactivity level, Ra, is the apparent radioactivity level, T is the bed thickness, D is drag, and L is the length of the detecting system. This method depends entirely on accurate measurements of bed thickness and drag. A thorough discussion of the concept of time constant and logging speed as related to drag is undertaken. INTRODUCTION Neutron curve interpretation has become one of the accepted methods for porosity determination in oil field practices. A great deal of literature has been published about neutron derived porosities, but this has been concerned with thick beds, or possibly even averaging of a series of thin beds as a single unit. There has been a lack of written information on methods whereby porosity can be evaluated for beds less than 10 ft in thickness. In certain areas, production is derived from relatively thin formations. The importance of thin bed evaluation, the fact that the Scintillometer is an adequate tool for this application, and the general lack of published information concerning neutron porosity for thin beds are the fundamental reasons for presenting this method of porosity determination. This concept is not put forth with the idea of discounting existing methods, but is merely suggested as a modification of other accepted methods of porosity determination which makes no allowance for quantitative evaluation of thin beds. The effects on the neutron log of counting statistics, statistical variation in the porosity of earth materials, and hole size must be taken into account to obtain neutron derived porosities. Since these effects have been described in past literature, the authors have not made an attempt to go into the subject in detail. With the use of statistical and repeated sections on the log, it may be determined which responses on the log actually correspond with lithologic changes. EFFECT OF DRAG AND ITS RELATIONSHIP TO TIME CONSTANT AND LOGGING SPEED Before entering into a discussion of porosity determination of thin beds, there should be a thorough

Jan 1, 1956

By R. H. Sheaphim

THE RECENT and continuing activity in the Boundary district, British Columbia, makes the publication of this paper timely. The following description and discussions are based on two years' experience in the district as Field Manager and Geologist for Attwood Copper Mines, Limited. The Attwood project was organized by Dr. D. F. Kidd to re-examine the Boundary mining camp. Thanks are due to Dr. Kidd, both for his intelligent guidance during the project and for his permission to publish this paper. Much of the data and many of the interpretations presented are credited to the work of, and to discussion with, Dr. W. H. White, Consultant Geologist, who worked for two field seasons on the project. However, the author assumes the responsibility for this presentation. Dr. C. D. A. Dahlstrom worked with the author during the latter stages of the project. His assistance and advice are gratefully acknowledged.

Jan 1, 1956

By W. B. Agocs

IN August 1954 a low altitude test geophysical survey was made in the Green Pond area of Morris County, New Jersey, with a Gulf Research and Development Co. Model II total magnetic field variation magnetometer mounted in a Sikorsky S-55 helicopter. The test was made in this area to compare the results of a high precision, very low altitude magnetometer survey with an existing ground magnetic survey in this area having known magnetite concentrations, so that the method could be used in areas of difficult access for the detailing of airborne magnetometer anomalies of interest in place of ground surveys. The load capacity of the Sikorsky S-55 permitted installation of a recording scintillation counter so that a radioactivity survey would be made simultaneously with the magnetometer survey. The area surveyed is located at approximately 41°00'N and 74o28'W, just south and east of the town of Green Pond, N. J. The outstanding topographic feature of the region is Copperas Mountain, a well defined ridge, maximum elevation 1222 ft, which runs the entire length of the survey. The lowest point in the survey, 810 ft, is in the extreme eastern corner. Topography of the area is shown in Fig. 1. The three major rock units outcropping in the area are all metamorphic: the Pochuck gneiss, which has been divided into two metamorphic facies; the Byram gneiss; and the Green Pond conglomerate. The relative ages of the Pochuck and Byram formations, both pre-Cambrian, are in doubt, but it is believed that the Pochuck is the older of the two.' The Green Pond conglomerate is Silurian.' Distribution of the outcrops and mine locations is shown in Fig. 1. Two facies of the Pochuck gneiss can be distinguished locally—the Copperas Mountain and Kitchell members. The Copperas Mountain member is a hornblende gneiss, and all the mines and prospects in the area are in this unit. The Kitchell is a quartz-plagioclase feldspar gneiss. The Byram gneiss is a relatively nonresistant valley formation which is high in the potash feldspar. The Green Pond conglomerate is a well indurated quartzite-conglomerate which forms the Copperas Mountain and the Green Pond Mountain's ridge to the north. It overlies the gneisses with a strong angular discordance that may be a fault. The geologic structure of the Green Pond area is relatively uncomplicated. The foliation planes of the gneisses dip steeply to the southeast, and the Green Pond conglomerate dips steeply to the northwest. Additional faulting in the area is indicated at the contact between the Kitchell member of the Pochuck and the Byram along the base of the topographic spur extending to the southeast from Copperas Mountain. The magnetite mines of Pardee, Winter, Davenport, Green Pond, Copperas, and the Bancroft shaft are described by Bayleyl and Stampe2.' The ore is in the Copperas Mountain member of the Pochuck gneiss. The magnetite veins are 10 to 50 ft wide and up to 300 ft long, dipping to the southeast at angles ranging from 40" to 75". The locations of these mines are shown in Fig. 1. Dip Needle Survey: The dip needle survey shown in Fig. 2 was taken from a U. S. Bureau of Mines Report of Investigations." The figure numbers below the local, individual map area outlines refer to the figures in the aforementioned reports which were not contoured. The area of the dip needle survey was confined almost exclusively to the outcrops of the Pochuck gneiss. The separation between survey profiles was 100 ft and the distance between stations on the profiles was 25 ft in highly anomalous zones to 100 ft in magnetically flat areas. A total of 16 1/2 miles of traverse was surveyed over an area of approximately 1/2 sq mile with 2050 stations. The magnitude of the magnetic anomalies is difficult to determine due to the lack of information concerning the type of dip needle used and the procedure followed in making the dip needle survey. This latter would include the method of "zeroing" the dip needle and the procedure of reading at the stations, whether on the swing or statically. Calibrations made of the Gurley dip needle, Lake Superior type, show a static sensitivity of 385 gamma per degree in the range from —25" to +35o, corresponding to a variation in the total field of —9600 gamma to +13500 gamma in a total field of 57000 gamma, inclination 72". The sensitivity increases to 16 gamma per degree from a deflection of 60" to 76", and from 76" to 172" the sensitivity decreases continuously to a low of 260 gamma per degree. From the above it may be seen that it is difficult to assign an arbitrary sensitivity for the dip needle used on this survey. However, an estimated value of 100 gamma per degree may be assigned. On this basis, the majority of the magnetic anomalies, whose deviation is +20°, would be 2000 gamma. Locally, west and northwest of the Pardee mine the magnetic anomaly is +50°, or 5000 gamma; in the Green Pond mine area deviations of +75" are observed that would correspond to anomalies of 7500 gamma. The areal extent and width of the dip needle magnetic anomalies is comparable to profile and station spacing. Hence it is concluded that part of the detail may be due to control, and the probable cause of the magnetic anomalies is at or near surface exposures of magnetite concentrations in the form of veinlets and disseminations whose locations correspond to the local magnetic anomalies. On the basis of the magnetics, none of the magnetite concentra-

Jan 1, 1956

By L. D. Jaffe

From data found in the literature, a method has been derived for calculating hardenability of titanium alloys from their composition. A single graph gives the contributions of each alloying element. These are simply added to a base hardenability for unalloyed titanium. Results agree satisfactorily with measured harden-abilities. RECENTLY the importance of hardenability of titanium alloys in permitting attainment of high strength and hardness has become apparent. If a titanium-base alloy has adequate hardenability for the section size and quenching practice used, it can generally be heat treated to high strength and hardness either by simple quenching or cooling from temperatures near the ß transus, by quenching and tempering (aging), or perhaps by direct isothermal transformation of ß1,2 If the hardenability is inadequate, high strength cannot be attained. Preliminary charts translating hardenability requirements for shapes quenched in various media into terms of Jominy end quenched hardenability specimens or ideal round sizes are now available for titanium alloys." The method proposed in 1942 by M. A. Grossmann for calculating hardenability of steels from composition has proved to be of great practical value.' It appeared worthwhile to see whether, using information available in the literature, a corresponding method for calculating hardenability of titanium-base alloys could be derived. Data No systematic experimental study of the hardenability of titanium-base alloys has yet been made. There is available, however, a considerable quantity of scattered data bearing on hardenability. Some investigators determined Jominy curves on one or several alloys. Others reported as-quenched hardness for specimens of a few alloys cooled at various rates or in various media. Still others gave the as-quenched hardness for systematically varied composition, using one or several cooling mediums. The measurements utilized in this work were limited to hardness. Strength measurements were not used because a low strength may reflect high hardness combined with brittleness. Since, in general, the hardness of titanium alloys goes through a peak as the cooling rate is varied from extremely fast to extremely slow, the cooling conditions at which peak hardness was found were taken as the measure of hardenability.1,2 When as-quenched hardness was found to drop as the content of an alloying element (believed to increase hardenability) was raised, this was taken as an indication that the cooling rate was faster than that giving peak hardness; otherwise, the hardness should go up because of solid solution hardening. Also, if the hardness increased on tempering at low temperatures, this was again taken to indicate that the cooling rate had been faster than that giving peak hardness. Many of the data did not indicate precisely the cooling conditions for peak hardness but merely set a maximum or a minimum bound, or a bracket. Since the sizes of specimens quenched and the location of the hardness readings were not always given, it was occasionally necessary to estimate reasonable limits for them. Only the nominal compositions were available in some cases. As quenching from below the ß transus is equivalent to starting with a mixture of a and ß phases, whose individual composition would differ from the overall composition of the alloy, only measurements after quenches from above the ß transus were used. Hardness measurements on samples heated during metal-lographic mounting were also discarded. Because of their bulk, the data used will not be reproduced. They have been or will be published elsewhere.5-22 Approach All data were first translated into terms of ideal round size. For conversion from Jominy or quenched round or sheet, the author's graphs were used." For a few furnace cools or helium quenches where cooling rates were given, conversion was made on the basis of equal cooling coefficient.23 Plots of ideal round size for peak hardness against percentage of alloying element were next made for

Jan 1, 1956

By J. R. Ruark

Because of the importance of oil-shale reserves the Bureau or Mines resumed research investigations in this field beginning in 1944. The Bureau early decided to build a Large-scale demonstration plant to accomplish the dual purpose of obtaining design data and to produce crude shale oil for refining studies. Two 40-ton-Capacity batch N-T-U (Nevada-Texas-Utah) retorts were completed for this purpose in 1947. After a preliminary operation, the plant was used to investigate process variables of air rate, recycle gas rate, and shale particle size and crude. Correlations obtained from these variables are presented in this report. Researchers concluded that recycle gas was not necessary for efficient operation of the process. Short comings of the batch method of processing the oil shale are pointed out in the report. Several periods of prolonged production operations were carried out. During these periods, the retorts were operated to produce as much crude oil per day as possible. The lifetime operation of the N-T-U retorts was divides into three periods, namely, preliminary operation, process variable study, and production operation. During the preliminary operation, 187 runs were made with a total of 7,596 tons of raw shale used to produce 3,688 barrels of crude shale oil. During the process variable study, 179 runs were made with a consumption of 7,494 tons of raw shale and a production of 4,218 barrels of crude shale oil. The production operation consisted of 554 runs in which 22,457 tons of raw shale was used to produce 12,359 barrels of crude shale ail. The overall total for the lifetime operation of the retorts consisted of 920 runs with a total consumption of 37,547 tons of raw shale and a production if 20,265 barrels of crude shale oil.

Jan 1, 1956

By J. L. Weeks, K. F. Smith

IN order to determine the magnitude of thermal conductivity changes resulting from alloying vanadium with titanium and a few other elements, several sam~les were PrePared and measured. The thermal conductivity -values reported herein in Table I were determined with an apparatus previously described.' As in recently reported2 determinations on uranium and uranium alloys, whose thermal conductivities are in the same range as vanadium," the accuracy of the values was checked by using synthetic sapphire." The error in the measurement is estimated to be '-3 pct or 0.003 cal sec-1 cm-l "C-1, whichever is larger. The vanadium used in preparing the samples was the calcium-reduced type and was supplied by the Electro Metallurgical Co. as 99.6+ pct pure. All alloying elements used in the preparations were 99+ pct pure. A nonconsumable tungsten electrode arc furnace was used for melting the alloys and, without opening the furnace, each ingot was re-melted a number of times to insure homogeneity. The samples as prepared by the Armour Research Foundation were machined from as forged material without annealing. Acknowledgment The note is based on work performed under the auspices of the AEC. References 'J. L. Weeks and R. L. Seifert: Apparatus for the Measurement of the Thermal Conductivity of Solids. Review of Scientific Instruments (1953) 24, pp. 1054-1057. 2 J. L. Weeks: Thermal Conductivity of Uranium and Several Uranium Alloys. Trans. AIME (1955) 203, p. 192; Journal of Metals (January 1955). 3C. A. Hampel: Rare Metals Handbook. (1954) p. 593. New York. Reinhold Publishing Corp. Thermal conductivity of vanadium is given as 0.074 cal sec-1 cm- '°C-1 at 100°C. 4 J. L. Weeks and R. L. Seifert: Note Regarding the Thermal Conductivity of Synthetic Sapphire. Journal Amer. Ceramic Soc. (1952) 35, p. 15. At 70°C, K = 0.071 cal sec-l cm-l °C-1.

Jan 1, 1956

By J. P. Powell

Records show that systematic water flooding was begun as early as 1935 in Greenwood County and in 1937 in Butler County. Water flooding on some earlier projects in Greenwood County were described in a Bureau of Mines Report of Investigation.2/ This report presents a discussion of 4 projects -2 in Butler County, 1 in Greenwood County, and 1 in Butler and Greenwood Counties. The location of these projects is shown in figure 1. The projects have been in operation 6 to 12 years and have recovered about 6.6 million barrels of additional oil from the injection of 84.7 million barrels of water. Three of the projects take advantage of the elevation of the nearby hilly terrain, and water from the treating ponds flows by gravity through the filters into the clear-water tanks. By utilizing gravity flow, fewer pumps and less electrical energy is required, resulting in more economical operation.

Jan 1, 1956

By Reuben B. Ellestad, Fremont F. Clarke

Lithium chemical plant extraction methods are discussed with reference to 1) base exchange with alkali sulphates; 2) processing based on roasting with lime; 3) miscellaneous methods; and 4) application of the Lithium Corp. process to extraction of lithium from run-of-mine, low grade spodumene ore, or concentrates. IN the early days of the lithium industry most of the production was from lepidolite, zinnwaldite, and amblygonite. Nearly all the early extraction processes described in the literature involve heating the finely ground mineral with sulphuric or hydrochloric acid. On subsequent water leaching most of the bases present in the mineral (especially aluminum) are dissolved as sulphates. As a result, the leach solution required extensive chemical purification before the lithium could be precipitated as carbonate. Following the remarkable growth of the lithium industry to its present size, zinnwaldite and amblygonite ores must be considered of minor importance only. Attention is now focused on spodumene, abundant enough in North America to be a major source of supply, and there are important supplies of lepidolite and petalite in Africa. The extraction processes described below all apply to spodumene, although several will also operate on other lithium minerals, such as petalite. Base Exchange with Alkali Sulphates: A distinct advance was made with the disclosures of Wadman and von Girsewalt. In these methods the finely ground silicate ore (spodumene or lepidolite) is intimately mixed with an excess of alkali sulphate (usually K2SO4) in at least a 1 to 1 proportion, and the mixture was heated to a relatively high temperature. Base exchange results, with the formation of lithium sulphate. A water leach dissolves the lithium sulphate, together with the excess potassium sulphate. Successful operation of this type of process requires very thorough grinding and mixing, as well as careful temperature control. The use of K2SO4 is objectionable from cost considerations since purification of lithium carbonate requires the use of potassium carbonate, if the K2SO4 is to be recovered and recycled. The lower solubility of K2SO4 as compared with Na2S04 is also objectionable, since it limits the concentration of the Li2SO4 solution to be precipitated by K2SO4. Early laboratory-scale investigation of this process by Lithium Corp. was not encouraging. Other related base exchange processes are those of Lindblad, Wallden, and Sivander3 and Sivander, Gard, Villestad, and Wallen4. The former covers the reaction of lithium silicate minerals with a sodium sulphate solution, at 100" to 300°C (under pressure), while the latter involves the extraction of silicate minerals with molten sodium sulphate. Both these processes would seem to be difficult and expensive to operate.

Jan 1, 1956

By Reynold Q. Shotts

CHEMICAL methods, based on the relative rates of oxidation of fusain, bright coal, and dull coal by nitric acid, have been devised to determine these coal components.1-4 Results obtained by oxidation methods for fusain have been checked against results obtained from microscopic methods5, 6on duplicate samples of the same coals, but to the author's knowledge this has not been done for bright and dull coal components. For this reason it is not certain that the two methods of analysis identify essentially the same chemical or physical units. It would be highly desirable to see results of the application of both methods to duplicate samples, but in the absence of any such data the author has attacked the problem indirectly. From the U. S. Bureau of Mines samples were obtained of three Alabama coals which the USBM had analyzed optically and reported on over the past 30 years. These samples were subjected to analyses by oxidation rate methods. Results of this work, and comparisons with the USBM analyses, have been published." This was the first indirect approach to the problem. The present report attempts a second indirect approach by way of internal validation. By nitric oxidation samples of two whole coals were carefully analyzed for fusain, bright coal, and dull coal. One coal was analyzed in duplicate. Duplicate portions of each of the coals were divided into three density fractions by means of heavy liquids. A duplicate portion of one of the coals was divided by sieving into three size fractions. Each fraction was analyzed by oxidation and its percentage composition calculated in terms of fusain, bright coal, and dull coal. Because the weight percent of each fraction was known, a material balance calculation for the whole coal was also made. The resulting reconstituted analysis of the whole coal could be compared to that determined by direct analysis. In addition, specific reaction rate constants were determined for each component and for each whole coal or fraction. Arbitrary reactivity indexes were calculated by dividing by 100 the sum of the products of the percent of each component in the coal and its specific reaction rate constant. The resulting figure was an average reactivity index for each coal or fraction. Weighting the reactivity indexes for each fraction by the percent of the fraction in the coal gave a reactivity index for each whole coal which could be compared to that calculated directly from the whole coal analysis. If oxidation analyses really delineate definite physical entities within the coal, or even definite groups of similar entities, reconstituted analyses calculated from fraction analyses should check closely those made of the whole coal. It probably is true that optical methods identify and describe a greater variety of components than do chemical methods and that variations are wide in the appearance and quantity of those components identified optically. Chemical methods based upon differences in oxidation reaction rates would of necessity be less discriminating, as between similar components, than would optical methods. The procedures followed for oxidizing the samples, analyzing the residues, plotting and calculating the percentage of each component, and calculating its specific reaction rate constant have been fully described.'-' In brief the method originally proposed by Fuchs et al.1 for the determination of fusain consists of the oxidation of small samples of coal in boiling 8N nitric acid in a condenser-fitted flask. After boiling for periods of 1/2 to 4 hr, the unoxidized residue is filtered and washed. The washed residue is treated with normal sodium hydroxide, diluted, and allowed to stand for several hours. The resulting brown liquor is removed, and the filtered residue dried, weighed, ignited, and weighed again. The ash-free residue is expressed as a percent of original dry, ash-free coal. The percent residue is plotted against time, and the extrapolation of this line to zero time gives the percentage of dry ash-free fusain present in the original sample. The shape of the resulting time plots has been explained' by the assumption that they are the result of two different types of reaction, the first part representing a first order reaction with rate a func-

Jan 1, 1956

By R. A. Beall

Homogeneous zirconium-alloy ingots have been cast on a production basis by the consumable-electrode arc-melting process at the Northwest Electrodevelopment Experiment Station, Bureau of Mines, Albany, Oreg. This paper describes the various methods used to introduce alloying materials into the ingot and evaluates 1 each method by the degree of homogeneity of resulting ingots, as determined in tests on sections cut from the ingots. As many as 30 or more ingots, each 6 to 10 inches in diameter and weighing 300 to 500 pounds, were melted, using each method; and, as most of them subsequently were fabricated to strip 0.1 inch thick, the test results are considered to be representative of production practice. Ingot homogeneity has been considered more difficult to achieve in arc-melting practice than by methods where the molten metal is poured into molds and the addition can be stirred into the total mass of metal before casting. Owing to the unique requirements of consumable-electrode arc melting the addition can be made only to that part of the total mass of the ingot that is molten at one time. Observation of the flowlines in 500-pound ingots produced at Albany indicates that the molten pool has a maximum depth about equal to the ingot diameter. The weight of metal molten at one time is, therefore, not over 100 pounds. Characteristically, the arc-melting process is conducive to segregation, which can be overcome, at least partly, by adding the alloy constituents almost continuously during casting.

Jan 1, 1956

By Williams K. C

This paper presents a brief account of the plant which has been developed at Port Pirie to recover, by vacuum distillation, the greater part of the zinc content of desilverized lead. The present plant is an experimental unit, which is run in conjunction with the normal refinery practice, but can be cut out of the circuit. It will shortly be dismantled and duplicate units will be built on the sites chosen for the final plant installation.The unit described here has treated flows of 16 to 37 tons per hour of desilverized lead, to recover 90 to 95 per cent of the zinc contained in it. It is not intended here to detail all aspects of the vacuum dezincing operation, nor the developments which precededthe adoption of this design. The essential features of the present plant will be described and, where these are peculiar to the present experimental location, the intended alteration for the final plant will also be mentioned. OUTLINE OF PLANT AND PROCESSLead issues from the continuous desilverizing kettle at about 350° C. containing about 0·57 per cent Zn. It is conveyed by a tiled launder to the preheater, where it is heated to 580-620° C.Hot lead from the preheater enters the vacuum vessel via a barometric leg. From a reservoir holding about 19 tons of lead it falls by gravity in a thin film exposed to high vacuum (20-50 microns)3 and leaves the vessel via a barometric leg, entering the lead pot. The lead leaves this pot at 540-560° C., containing 0·03 to 0·06 per cent Zn, which is removed, together with residual antimony of 0.02 to 0·06 per cent, by a separate final refining process.

Jan 1, 1956

By P. Gordon

An isothermal jacket microcalorimeter, supplemented by metallographic, microhardness, and X-ray measurements has been used to study the isothermal annealing of high purity copper after room temperature tensile deformation. The amount of stored energy released during annealing has been measured as a function of deformation in the range 10.8 to 39.5 pct elongation. The data have shown the major heat effect to be associated with recrystallization and have allowed an analysis of the recrystal-lization kinetics and the calculation of activation energies of recrystallization. WHEN a metal is deformed plastically, some of the energy expended is dissipated as heat during the working process, while the remainder is stored within the metal in the form of lattice distortions and imperfections. During subsequent heating of the metal, the distortions and imperfections can be largely annealed out and the associated stored energy released as heat. It is apparent that measurements of the evolution of stored energy during such annealing may produce important information concerning the nature of the annealing mechanisms and the imperfections involved. Some excellent studies of this type have been made in the past, notably those of Taylor and Quinney,' Suzuki,2 Bever and Ticknor,3 Borelius, Berglund, and Sjöberg,4 and Clarebrough et al.5,6 None of this work, however, employed isothermal techniques, with the exception of the Borelius studies' in which only the early annealing stages were investigated. Since isothermal measurements, as compared with heating or cooling curve, have the merits that 1—they reveal the kinetics of a process more clearly, 2—the results obtained are more easily applied to theory, and 3—most fundamental investigations of annealing using techniques other than calorimetry have been carried out isothermally, it was considered important to apply calorimetry to the study of the isothermal annealing of metals. Accordingly, an isothermal jacket calorimeter of the Borelius type,' supplemented by metallographic, hardness, and X-ray measurements, has been used to study the annealing of high purity copper after room temperature tensile deformation. Experimental The microcalorimeter has been described fully elsewhere." Briefly, the specimen to be studied is placed in a constant temperature environment of virtually infinite heat capacity achieved, as shown in the drawing of Fig. 1, by means of a vapor thermostat. A high thermal resistance is provided between the sample and the environment and a sensitive differential thermopile (see Figs. 2 and 3) arranged with half its junctions in contact with, and thus at the constant temperature of, the environment, and the other half in contact with the sample. A reaction in the sample develops a small difference in temperature, AT, across the thermopile, which is followed by a recorder-galvanometer set-up as a function of time, t, and is converted to reaction heat per unit time, P, by the use of the equation AT P=a?T + b AT dt The constants, a and b, in Eq. 1 are determined by a simple calibration, making use of the Peltier heat developed by a small current run through the junction of a thermocouple located in an axial hole in the specimen (Fig. 2). In its present form, the limit of sensitivity of the calorimeter is a heat flow of 0.003 cal per hr. The copper used was the spectroscopically pure metal supplied by the American Smelting and Refining Co. in the form of 3/8 in. diam continuously cast rod, reported to be 99.999+ pct Cu. A small amount of the copper was available at the start of this work and is referred to hereafter as lot A. A second batch, lot B, was obtained later, most of the results described subsequently being for this lot. As will be seen, there is some indication that lot A was somewhat purer than lot B, but it is not known whether this difference was present in the as-received metal or arose during subsequent handling. The two lots of copper were remelted and cast into two 1½ in. diam ingots in vacuo, using high purity graphite crucibles and molds. The ingots were upset several times to break up the large cast grains, and then rolled and swaged to rods 0.391 in. in diameter, using several intermediate anneals with about 40 pct reduction in area between anneals. The penultimate anneal was 2 hr at 350°C. X-ray examination showed no marked general preferred orientation in the resulting rods. The grain structure typical of the two rods is shown in the micrograph of Fig. 4." It was found to be virtually im- possible to get an unambiguous measure of the absolute grain size in the two annealed rods because of the profusion of annealing twins and the lack of regularity of the grain boundaries. However, counts of the number of boundaries intersected per unit length along a random line on a polished section, making a correction for the proportion of boundaries (about half) estimated to be twin boundaries, gave a figure of about 0.015 mm for the average grain diameter. The grain size of the rod from lot A was about 5 pct smaller than that from lot B. The rods were cut into 1 ft long bars and these deformed in tension at room temperature to various total elongations in the range 10.8 to 39.5 pct. A strain rate of 1 pct per min was used. The deformed bars were then stored in a dry ice chest until such time as samples were to be cut from them. Five bars deformed as indicated in Table I were used for the subsequent tests. In all cases, all the calorimeter.

Jan 1, 1956