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By M. L. Leonardi

THE Searles Lake orebody is located in the north- west corner of San Bernardlno County. It is a dry lake bed with an exposed salt surface covering an area of 12 square miles. Recoverable mineral values are contained in the mother liquor below the surface of the lake. Stratification in the lake bed has separated the brine into two bodies which dlffer in composition. Although liquor is processed from both bodies, this paper will discuss only the upper structure brine. Fig. 1 illustrates a typical cross-section of the two commercial orebodies. The orebody is composed of a porous salt deposit 70 to 90 ft deep. The upper structure is separated from the lower orebody by a 12 to 16-ft thick impervious mud seam, as shown in Fig. 1. These salt structures are composed of 55 pct solid-phase salts and 45 pct voids which are filled with the original mother liquor. The brine wells are drilled to the separating mud seam and cased to wlthin 10 ft of the bottom. This is done to draw the brine horizontally from the bottom of the structure. It is pumped with multistage centrifugal pumps Into the plant at the rate of 3 milllon gal per day. The first process that was successful was developed by Charles P. Grimwood for the recovery of potash. The first evaporator unit was built in 1916. In the early twenties, Dr. Morse worked out a process for the recovery of borax. This made the cycle more efficient, as the end liquor could be sent back to the evaporators rather than being sewered. In 1926 the American Potash & Chemical Corp. was formed as a new company, and the entire plant was remodeled. The plant at that time produced only potash, borax, and boric acid. Since then the American Potash & Chemical Corp. has added processes for the production of USP boric acid, refined potash, sulphate of potash, soda ash, salt cake, lithium concentrates, Pyrobor (Na2B4O7) bromine, phosphoric acid, and lithium carbonate. The main plant cycle may be depicted as a closed cycle, see Fig. 2. The raw material, brine, enters the cycle to be mixed with the end liquor, known as ML2, from the pentahydrate borax crystallizers. The mixture of these two forms evaporator feed. Evaporator feed is pumped to the evaporators where it is concentrated, with respect to potash and borax. In the same operation water vapor, sodium chloride, salt trap salt, and clarifier salt are removed from the cycle, see Fig. 3 for potash plant product. The evaporators produce a concentrated liquor which contains approximately 19.5 pct KCI. This liquor is diluted as it enters the potash plant to keep all salts, except potash (KCI, 97.0 pct) in solution. Here the moist potash leaves the cycle at 100°F. The end liquor, known as ML1, is pumped to the borax pentahydrate crystallizers, where crude borax pentahydrate is crystallized and removed as solid phase. The ML2 is sent back to pan feed to be reconcen-trated, see page 207. Note that the only water to leave the cycle is in the form of vapor and moisture in the solid phase products crystallized. Thus there is a constantly cycling volume of liquor to which brine is added. Since the volume of liquor cycled does not increase, the brine is, in effect, evaporated to dryness. This would be true if there were no liquor losses. But, as in all processes, there are always unavoidable and accidental losses which reduce the volume of cycling liquors. The losses must be made up with brine. The concentration process is the beginning and the end of the cycling liquors. In this process there are three evaporator units of the triple effect counter-current type, that is, there are three pans in each unit and the heat flows in one direction while the liquor flows the other way through the evaporator pans, see Fig. 4. During the evaporation process a great deal of sodium chloride, burkeite, some sodium carbonate monohydrate, and a little lithium-sodium phosphate are crystallized. The volume of these salts is so great that they must be removed as they are formed or the process would come to a standstill. Brine and recycled mother liquor No. 2 enter the third effect evaporator pan from the evaporator feed storage tanks, see Fig. 5. A steady flow of liquor is removed from the bottom of the No. 3 pan and is pumped through the No. 3 cone of the salt trap, a clear liquor being returned to the NO. 3 pan. A portion of this clear liquor is pumped to the second effect pan. This process is repeated in each pan. The liquor from the No. 2 pan is pumped through the No. 2 salt trap cone and returned to the No. 2 pan.

Jan 1, 1955

By N. K. Chen, R. Maddin

Single crystals of molybdenum were extended at temperatures from 1300° to 2500°C. It was found that with increasing temperatures, the yield becomes more pronounced and the number of slip bands for equal amounts of elongation decreases. Slip at high temperatures fragments the structure. OTHER than the investigations on sodium and potassium by Andrade and Tsien,&apos; the researches of Steijn and Brick&apos; on a iron single crystals at low temperatures are about the only studies of the influence of temperature on glide of body-centered cubic single crystals. The effect of test temperature on glide has been rather widely investigated with hexagonal crystals" and less widely with face-centered cubic crystals. ~~ a result of these studies it can be said that, in general, the onset of plastic flow as measured by the initial rate of strain hardening becomes more abrupt with increasing temperature, and the value of the yield decreases with increasing temperature. Strain hardening, however, is markedly affected by changes in temperature except at very low and very high temperatures where the strain hardening rate becames constant. In the present investigation it is shown that temperature affects the glide of molybdenum single crystals in much the same manner as crystals of other classes, it., for comparable strains the number of slip bands decreases with increasing temperature; shear along the slip bands increases with increasing temperature; the yield becomes more pronounced with increasing temperature of test; and the strain hardening approaches a constant at very high temperatures. In addition, it is shown that, in agreement with the work of Tsien and Chow, Qlip occurs on (110) planes in <Ill> directions. It is further shown that slip at high temperatures fragments the structure into either irregular sized cells or bent atomic planes which are roughly aligned in crystallographic directions. Experimental Procedure Single crystals 3 mm in diameter by about 25 mm long were prepared using the technique previously described.&apos; The furnace in which the crystals were grown served as the extension apparatus for the tension tests. It consisted of a 4 in. water-cooled brass tube 20 in. long which was continuously evacuated at the bottom. Two water-cooled copper electrodes held the specimen by means of spherical collets secured in place in the electrodes by set screws. These electrodes served also to transmit power and stress to the specimen. The lower electrode was clamped to a stand, while the upper electrode was fastened to one side of a lever arm flexibly supported at the top through a slightly offset pinion. A metal bellows operating elastically was attached to the upper electrode to affect a vacuum seal and allow freedom of motion. The level of the arm was adjusted by rotating a graduated nut. Rotation of the electrode was prevented by a key fitted into a groove. After the specimen was mounted and the vacuum secured, the lever arm was adjusted so that the bellows was at its relaxed position. This insured that the total weight of the specimen, the upper electrode, and the downpull of the vacuum were balanced by the horizontal beam. Since the specimen was heated by its own resistance, expansion of the specimen proceeded freely by this arrangement. During the time of heating the specimen, the beam was maintained in a horizontal position by turning the nut at the top. By graduating the lever arm and using a known dead weight on the lever arm to supply a tensile stress, the graduated nut could be read to 0.0001 in. extension. Since

Jan 1, 1955

United Engineering Trustees, Inc C E Reistle, Jr (to Oct &apos;55), A B Kinzel, &apos;56, Andrew Fletcher, &apos;57, Philip Kraft (from Oct &apos;55 to &apos;59) The Engineering Foundation W M Peirce, &apos;56, A M Gaudin, &apos;58 Engineering Societies Library Board Frank T Sisco, &apos;58, C H Behre, Jr Engineering Societies Personnel Service Board of Directors E J Kennedy, Jr, E H Robie Advisory Committee, Milwaukee F T Agthe Special Survey Committee C M Cooley American Standards Association Mining Standards Board E R Borcherdt, &apos;55, Otto Herres, &apos;55, J K Richardson, &apos;56, E W Bullard, &apos;56, Alternate

Jan 1, 1955

By P. Pietrokowsky

lntermediate phases in the binary metal alloy systems Ti-Zn, Ti-Hg, Zr-Zn, Zr-Cd, and Zr-Hg have been investigated by X-ray powder diffraction methods. Gamma-TiBHg and Zr3Hg have a beta tungsten structure; TiHg and ZrHg are analogous to ordered AuCu (L l0 type); delta-TixHg and ZrHg, are isomorphous with ordered AuCu,, (L l2 type); ZrZnz is face-centered cubic (C 15 type); TiZna crystallizes in a C 14 type structure; and Zrll-, occurs in cubic and tetragonal modifications in which a random distribution of atoms exists. Additional information for the intermediate phase TiZn, is presented. THE physical metallurgy of titanium and zir-conium when alloyed with elements in subgroup 11-B of the periodic table has received comparatively little attention in the literature. Laves and Wallbaum&apos; reported the existence of several intermediate phases in the system Ti-Zn. They identified TiZn as a CsCl (B 2) structure and described TiZn, as an ordered Cu,Au (L 1, type) crystal structure. Gebhardt&apos; investigated very limited zinc-rich regions in the systems Ti-Zn and Zr-Zn. Phase relationships in these partial constitution diagrams were deduced from the results of thermal analysis and metallography, X-ray results being inconclusive. The first zinc-rich intermediate phase in either system was not identified. More recently, Anderson, Boyle, and Ramsey" have had occasion to refer to a partial Ti-Zn phase diagram (unpublished data) covering the region 0 to 10 atomic pct Ti, wherein two intermediate phases corresponding approximately to TiZn,, and TiZn,, were indicated. The metals used in this investigation and typical analyses as determined by the suppliers are given in Table I. The iodide-process zirconium which was used was not hafnium free. Experimental Methods Alloy Preparation: The relative ease with which titanium and zirconium combine with other elements places extensive restrictions on the methods by which alloying can be achieved. The direct current electric arc melting procedure was found to be unsatisfactory for preparing these binary alloys and for this reason solid state diffusion methods were utilized. The iodide process titanium and zirconium rods were filed by hand. Fines were subjected to a magnetic separation and classified as to size as either finer than 200 mesh or coarser than 200 but finer than 80 mesh. Powder mixtures of various binary combinations of titanium and zirconium with zinc and cadmium were compacted in a 12 mm diameter die and then placed in Vycor or quartz vials which were evacuated and sealed. The mercury alloys were prepared in a similar manner; the proper weight of liquid mercury being placed in a vial with minus 200 mesh titanium or zirconium. These ampoules were then heat treated at various temperatures and times depending on the characteristics of the particular alloy system. Upon completion of the heat treatment the ampoules were cooled rapidly and the specimens weighed. The loss in weight varied from 1 to 3 pct (except as noted in the text) and for this reason the calculated compositions were accepted as a fair measure of the actual alloy compositions. X-Ray Dif raction Techniques: Powder diffraction experiments were conducted at room temperature with a 143.2 mm Debye-Scherrer X-ray camera in which the film was placed in the Straumanis arrangement. When copper radiation was used, a nickel filter was employed, and for the cobalt target a filter of iron oxide was used. In both cases, the /i? filter was placed between the X-ray target and the powder specimen which was mounted on a glass fiber. The lack of information based on optical metallography placed reliance on the results obtained from the X-ray experiments for determination of

Jan 1, 1955

By J. E. Shelton

This presentation covers the results of laboratory studies conducted by the Bureau of Mines Mineral Dressing Section, Northwest Electrodevelopment Laboratory, Albany, Oreg., on alluvial sands from Dismal Swamp, Bear Valley, and Cascade, Idaho. The search for radioactive minerals has led to the reexamination of alluvial deposits; in the process of this reappraisal the frequent presence of minerals bearing columbium and/or tantalum was toted. Because of increased demand for these metals by the defense industries and because these industries depend upon foreign sources for their supply the domestic alluvial black sands are being considered, as a possible domestic source. However, utilization of these alluvial deposits depends upon development of methods of concentrating these valuable minerals. The primary objective of the test work was the study of the effect of attrition scrubbing, sizing, magnetic, electrostatic, and gravity separa¬tion as methods for concentrating and recovering the columbium and tantalum-bearing minerals, samarskite, euxenite, ilmenorutile, and columbite.

Jan 1, 1955

By P. R. Perry

This publication is a compilation of tested methods for the analyses of titanium tetrachloride, titanium sponge, and various intermediate materials and products. They are presented in concise form without the detail usually found in publication of new methods because many of them are modifications of well known procedures. The Electrometallurgical Experiment Station, Boulder City, Nev., has been developing titanium production methods since 1945. Most of this development was on a modified Kroll Process but also included work on sodium reduction and electrolytic methods. During these years a large variety of samples were analyzed. Most of the analytical problems were solved using published methods or modifications of the same. At the start, there were no published procedures for analyzing titanium sponge using spectrochemical methods. A great deal of study was given to testing several of the well known techniques, and some of them, such as direct sparking of the metal, proved to be completely unsatisfactory. Solution-spark techniques were finally tried, and satisfactory procedures were developed for some of the more common impurities. These spectrochemical methods were then put into routine use for several months before their publication.2/ Some new modifications have been made, and techniques have been developed to determine other impurities found in titanium sponge and tetrachloride. All spectrochemical methods used in 1954 are included in this publication.

Jan 1, 1955

By T. M. Allen, W. H. White

THE Greenwood-Grand Forks area of southern central British Columbia, known as the Boundary District, has a long history of mining exploration and production. At the turn of the century this was the premier copper mining camp in the British Empire, its total production amounting to some 20 million tons. Most of this ore came from the great Granby mines at Phoenix, but the Motherlode mine at Deadwood camp, 6 miles to the west, and several mines in Summit camp, 5 miles north of Phoenix, made important contributions. The large deposits were exhausted in 1918 and the district since has seen only desultory exploration and salvage operations. The orebodies are mineralized skarn zones in limestone members of a thick series of Upper Paleozoic sedimentary and volcanic strata. Chalcopyrite is the primary ore-mineral. Copper carbonates and silicates occur sparingly in outcrops, but the oxidized zone generally is very shallow. Much of the surface is mantled by glacial drift which in most places ranges in thickness from 2 to 15 ft. In some of the hanging valleys, however, the glacial drift may be as much as 100 ft thick and may assume drumlin-like forms. In 1951 an ambitious program aimed at the discovery of new orebodies and important extensions of abandoned deposits was launched by Attwood Copper Mines, Ltd. In this district so thoroughly searched by an earlier generation of prospectors, any orebody which had remained undiscovered must have little or no surface indication. Consequently, in addition to the basic detailed geological work, the program of exploration included magnetometer and self-potential surveys. Geological bets and geophysical anomalies were tested further, prior to diamond drilling, by a study of copper distribution in tree twigs and/or in the soil. The soil sampling and analytical methods used and some of the results seem of sufficient importance to warrant this paper. The authors had done some plant sampling in this and other districts, using the dithizone neutral-color-end-point method (Warren and Delavault, 1948, 1949; White, 1950),1-3 but they were unfamiliar with its soil application. Finally, after much experimenting in the field, they adopted the methods described here. These methods are not entirely original or defensible on theoretical grounds, but under field conditions of rapid sampling and analysis the results are reliable enough to be of use. Fig. 1, which shows the results of duplicate analyses of duplicate soil samples taken at 50-ft intervals across an anomalous zone, indicates the relative dependability both of the sampling and analytical methods. Sampling and Analytical Equipment A 2-ft piece of 1-in. solid drill steel, one end sharpened to a broad, conical point. The steel is marked at 1 ft from the point. A 2-ft piece of ½-in. black iron pipe, one end filed to a bevelled cutting edge. The pipe is marked at 1 ft 3 in. from the cutting end. A 3-lb hammer. A plastic or rubberized sheet about 18 in. square. Moisture-proof assay pulp envelopes. A 10-mesh seive made from window screen with the paint burnt off. A small assay spatula. A pan balance sensitive to 10 mg. Two ignition trays about 4 in. square, made of sheet iron turned up along the edges. A Coleman two-burner gasoline stove. An asbestos board about 5x8 in., used as a hot plate on the gasoline stove. A circular aluminum rack to hold 8 test tubes while refluxing (design of Almond and Morris). Pyrex Glassware Large refluxing test tubes, 25x200 mm, marked at 40 ml volume. Breakers, 20 ml. Pipettes, 1, 5, and 10-ml capacity. Graduate, 50 ml. Shaking cylinders, 100 ml, glass stoppers. Burette, 25 or 50-ml capacity, with holder. Chemical Supplies 1 N sulphuric acid. Hydroxylamine hydrochloride, solid crystals. Fisher Alkacid test paper. Copper standard solution. Dithizone standard solution 60 mg per liter. Water reasonably free of metals. Soil Sampling Method: The problem of how to take a soil sample is extremely crucial. The method outlined below, adopted after a number of tests, has the advantages of uniform pattern, uniform depth, and uniform size of sample. The area to be tested was marked off by chain and compass lines 100 ft apart, normal to the strike of possible ore deposits. Numbered stakes were set at 50-ft intervals along these lines and a soil sample was taken at each stake in the following manner. The drill steel was driven into the ground normal to the slope of the surface to the marked depth of 1 ft, moved slightly from side to side, then carefully withdrawn. The iron pipe was inserted to the bottom of this hole, tapped down to the marked depth of 1 ft 3 in. and withdrawn; the 3-in. soil plug in the

Jan 1, 1955

Jan 1, 1955

By E. S. Machlin

THE function of this paper is to present certain results based on the fact that the strain energy arising from the solution of out-of-size solute atoms into the solid matrix is free energy and not internal energy, and that this strain energy is almost wholly shear strain energy as Zener1 pointed out. One natural consequence of this fact is an expression for the excess entropy of mixing due to the strain energy. Also, a derivation of the integral molar free energy of mixing partitioned to strain energy will be made using the model of Lawson2 and thermodynamics. This derivation has the advantage of showing in a simple way the assumptions involved in Lawson&apos;s treatment. The excess entropy of mixing partitioned to strain energy can be derived in two ways. The first way makes use of the fact that the strain energy is almost wholly in the form of shear strain energy. In this case, as Zener1 pointed out, the change in entropy due to the addition of shear strain energy is to a first approximation given by ?S/?? p,T = - ?lnµ/?T p,? Hence, the excess entropy of mixing partitioned to strain energy will be given by Sx ? = ?S/?? p,T Gx ? = - ?lnµ/?T p,? Gx ? where, Gx ? is the relative integral molar free en- ergy partitioned to strain energy; S is the entropy; is the shear strain energy; µ is the shear modulus; T is the absolute temperature; p is the pressure; and ? is the shear strain. Zener,1 as well as others, has pointed out that the shear strain energy stored in a compressible isotropic solid due to the insertion of an off-size incompres-sible sphere into a spherical hole in the solid, is approximately given by 2/3 µ/O (O°I - O)2 where a is the volume of spherical hole and no , is the volume of sphere. If we now consider the introduction of one mol of such spheres into an infinite volume of solid, then the relative partial molar free energy excess due to strain energy alone is GM ? = 2/3 µ/v (v ° 1 - v)2 where v is the molar volume of solvent and v°1, is the molar volume of pure solute type 1. Let us consider that these spheres are the two types of atoms in a binary solution, then there will be a similar relation for solute 2. The total relative integral molar free energy excess due to strain is then, to the approximations stated above GM ? = GM ? x1 + GM2 ? x2 = 2/3 µ/v [(v ° 1 - v)2 x1 + (v ° 1 - v)2 x2]. Lawson&apos;s relation for the strain energy can be de-

Jan 1, 1955

By F. J. Radd, R. L. McGlasson

The mechanisms of corrosion and corrosion fatigue damages to sucker rods are examined from a fundamental electrochemical viewpoint, and the relationships of sucker rod microstructures to these damaging effects are defined. The common corrosive agents in crude oil production and storage are discussed as to types of attacks that they cause. The variations of fatigue strength with alloy content, surface preparation, and stress ranges are analyzed. Finally, conclusions are drawn as to how microstructures largely influence and control sucker rod performance. INTRODUCTION Greater than 90 per cent of the crude oil produced by artificial lift methods is produced through sucker rod pumping systems. In the USA each year more than $14 million is spent for sucker rods in new and old pumping installations. It is important to make this investment a wise one. Essentially, the sucker rod system is a long series of steel rods, operating under alternating stress loadings and under mechanical vibrations, which connect the surface power source with the subsurface pump. These rods often operate in a variety of corrosive media, including water, brines, carbon dioxide, hydrogen sul-fide, and air. Basically, this paper is concerned with the problem of the behavior of certain steels in various corrosive media under high and dynamic stress patterns. The main objective of this paper is to show how, once the stress effects and the corrosive environments are defined, one can still realize structural control and beneficial influence upon corrosion and corrosion fatigue. FUNDAMENTAL DEFINITIONS AND ANALYSIS In the corrosion and stress behavior of this solid state mixture of iron and iron carbide called steel, one must analyze upon what major factors does its service life depend and of what, exactly, is steel composed. The former question can be referred to two external factors and two internal factors. The two major external factors are: 1. the nature of the stress patterns — size and range of stresses present 2. the nature of the corrosion — erosion environment — the corrodent and/or wear involved The two fundamental internal factors that govern the strength and useful life of a steel both in normal duty and in heavy-duty corrosion service are: 1. the nature of the steel volume properties 2. the nature of the steel surface properties For the latter question normal steel is defined as a solid mixture of iron and iron carbide particles, generally with certain accidental and intentional elements present. (The amount of iron carbide present is determined by the carbon content of the steel.) These additional elements generally dissolve into either the iron (ferrite) or the iron carbide (cementite) components.

Jan 1, 1955

By J. H. Bilbrey

A recording thermobalance ,vas used to determine the rates of oxidation of mol-ten tin over the temperature range 550°-900° C. Oxidation rates were found to vary widely for a given temperature, as previously reported by other investigators. 1 X-ray diffraction data indicated that the probable cause of these variations was the development of preferred orientations in the crystals forming the oxide film. No reasons for the differences in degree of preferred orientation were discovered. For relating the weight of the oxide formed (w) to the time of oxidation (t) an equation of the form wn = kt was found to best represent the experimental data. INTRODUCTION In the course of conducting investigations on the feasibility of using selective oxidation techniques for the purification of various metals in the molten state it was soon discovered that data on the oxidation of molten metals and alloys were very scarce. In contrast to the many hundreds of publications on the oxidation of metals in the solid state there are relatively few articles on the rates of molten-metal oxidation. In view of this scarcity of data, it was decided to institute a series of investigations into the oxidation processes of molten nonferrous metals and alloys with the expectation that the information derived could be put to practical use in developing and improving refining processes based on selective oxidation. This report is the first of a series in which oxidation data for molten nonferrous metals and alloys are presented.

Jan 1, 1955

By Roscoe C. Clark, Henry F. Coffer, J. J. Reynolds

A cement slurry lightweight additive has been adapted in the Conoco laboratories for use in oil well cements. This additive makes possible the use of air to lighten oil well cement slurries. Specifically, the additive consists of small clay bubbles of air having sufficient strength to resist crushing by bottom hole pressures. Clay bubble cement slurry weights can be safely reduced to 10 Ibs/gal. In addition, the clay bubbles tend to act as lost circulation materials and to provide a cement texture which should produce good perforating characteristics. Clay bubble cement is relatively impermeable. INTRODUCTION In many areas in Oklahoma, Texas, Wyoming, and California, difficulties are experienced during casing cementing operations with lost returns caused by the high density of the cement slurries. Wells in these areas are ordinarily drilled with 9 to 11 lbs/gal. drilling mud while neat cement slurries may range in densities from 14.5 to 17 lbs/gal. In these areas, cement slurry weights are at present being successfully reduced to around 12 lbs/gal. (under bottom-hole conditions) by the use of additives in the cement. Since the use of additives will decrease the strength which the cement will develop, the amount of additives which can be used must be based on the minimum cement strength which is acceptable; and thus the maximum slurry weight can be reduced. At present, the minimum tensile strength generally acceptable is 50 lbs/sq in. cured for 24 hours under bottom-hole temperature. This figure is based on laboratory tests1 and on a large number of cement jobs which have been conducted using cement which will not develop more than 50 psi tensile strength in 24 hours under bottom-hole conditions. Two additives are now in use for decreasing cement slurry weights. These are expanded perlite and/or bentonite. The density of both of these materials is greater than that of the cement slurry; however, large quantities of water may be added with these materials without producing a slurry which will settle out of suspension. It is these large quantities of water which contribute to the reduction in the slurry weight. The minimum slurry weight at present obtainable with expanded perlite and/or bentonite is approximately 12 lbs/gal. using a standard Portland cement slurry. In many areas, this weight reduction is insufficient; and returns are still lost during casing cementing operations. In many cases, the pay formation itself is fractured; and a considerable quantity of this cement is lost to the pay zone. It is therefore believed that if cement slurry weights can be reduced to as low as 10 lbs/gal., two advantages will accrue: 1. The lighter densities (10 to 12 lbs/gal.) should mitigate or eliminate lost returns during casing cementing operations. 2. Cement slurries above 12 Ibs/gal. (the present minimum limit ) should develop considerably more strength than is now being obtained. A tensile strength of 100 psi is desirable.&apos; It is the object of this paper to describe a cement slurry having a weight of 10 lbs/gal. and capable of

Jan 1, 1955

Executive Committee, Board of Directors H D Smith, Chairman, C E Reistle, Jr, Vice-Chairman, T B Counselman, J S Smart, Jr, L F Remartz Finance Committee, Board of Directors A B Kinzel, Chairman, Philip Kraft, P D Wilson Investments Erle V Daveler, &apos;57, Chairman, Henry Krumb, &apos;56, Andrew Fletcher, &apos;58, G F Moulton, ex officio as Treasurer, A B KInzel, ex officio as chairman of the Finance Committee Endowment W W Mein, Jr, Chairman, D H McLaughlin, J V N Dorr, J B Haffner, J R Suman, Henry Krumb, E V Daveler, D C Jackling, Wilfred Sykes, N G Alford, W J Coulter, C E Weed, 0 H Johnson, L F Reinartz, J B Morrow, R McMillan Endowment Fund "X" G F Moulton, Chairman (RIME Treasurer), Erle V Daveler, &apos;58, G I Brigden, &apos;57, Philip Kraft, &apos;56

Jan 1, 1955

By C. J. Rodgers

The present day success of gravel packs to prevent or retard the migration of unconsolidated sands into the well bore is due to: (I) the use of a saline or non-aqueous, nonsolids drill fluid, (2) proper preparation of the well bore prior to gravel packing, and (3) pressure placement of the gravel. The experience gained from the "pressure pack" method of gravel packing indicates that sand-free fluid production can be maintained for a length of time sufficient to make the operation economically attractive. Data pertaining to the first 15 wells so completed by Gulf indicate that for each dollar spent to effect the completion, there will be a return of more than $2.92. The pressure pack technique of gravel packing is essentially the placing of gravel in and adjacent to the producing formations. This is done with fluid pressure and by the use of a drill fluid that will permit partial or complete loss of returns to the formation during placement. This technique was first intentionally used by Gulf in May, 1950, and since that time has been applied in more than 90 wells. Other advantages claimed for this type of completion are that the pressure placement of the gravel has a scouring effect on the casing perforations, that additional drainage channels to the well bore are created, and that the possibility of shifting of the formations adjacent to the casing is minimized and possibly prevented. During the past few years, the use of gravel to prevent or retard the migration of unconsolidated sands into the well bore has met with a favorable degree of success. Numerous methods and techniques of "gravel packing" have been used, each having its own relative merits, and with varying results. M. L. Cashion1 in 1939 ably reviewed the history of gravel packing to that time. As stated in his paper, ". .. the idea of gravel packing wells is not new." During the period 1939 to 1949, very little if any progress or change in technique in this type of completion was made. However, it was noted in some cases that during the placement of gravel, if there was a loss of drill fluid to the formation, there was a corresponding loss of gravel to the formation. Also, it was noted that in those gravel-packed completions (opposite casing perforations) that "sanded up," there was found to be an absence of gravel in the annular space between the liner and casing, although gravel had previously been placed in this space and no gravel had been removed from the well at the surface. These findings resulted in the placement of gravel with fluid pressure and by the use of a drill fluid that would permit partial or complete loss of returns to the formation during placement. Pressure placement of gravel became an accepted practice in late 1949 and early 1950. Another fact brought to light that has contributed to the current success of gravel pack completions is that drilling fluids containing solids will to some extent cause plugging of the screening medium or blocking of the producing section. The removal of these solids by chemical action, mechanical action, or a combination of the

Jan 1, 1955

By Lloyd Williams

1. The investigation shows that the Sewanee bed is the only bed of major importance in Marion County, 97 percent of the coal mined in the county having come from this bed. There are coal reserves in minor quantity in the Battle Creek bed, and production from this bed depends on a few small truck mines. The Richland bed, or Lower Sewanee, has been mined in the past, but no coal has been produced from it in late years. There are no production records of any other beds in the county, although same coal has been produced from them. 2. Known measured and indicated reserves in all beds, based on a minimum thickness of 14 inches and on 1,800 tons per acre-foot of coal in place, are estimated to be 61 million short tons as of January 1, 1953. Of this total, 55 million short tons is in beds 28 inches and more thick. Areas in each bed were omitted from the estimate where available data relative to the bed characteristics are too meager to permit 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, 1955

By P. G. Shewmon, F. N. Rhines

THE determination of the self-diffusion coefficient of magnesium has been made possible recently by discovery1-1 of a radioactive isotope, Mg28 having a half-life of 21.3 hr,1 and subject to manufacture in useful quantity. In the present research this material was condensed from the vapor phase upon a surface of high purity magnesium. The progress of diffusion of the tracer atoms into polycrystalline magnesium was followed by machining layers and measuring the change in the intensity of radiation as a function of the distance of each layer from the surface. The self-diffusion coefficient was found to be 2.1 X 10-8 sq cm per sec at 627°C, 3.6 X 10-9 sq cm per sec at 551°C, and 4.4 X 10-10sq cm per sec at 468°C; the activation energy is about 32,000 cal per mol. Experimental Procedure Since there was no other published measurement of a diffusion velocity in any magnesium-base material, is was necessary to employ a number of new experimental techniques. The short half-life of Mg28 made it necessary to complete the entire experimental procedure within three or four days. This meant that the work had to be done where a cyclotron was readily accessible and that all operations, prior to the diffusion heat treatment, had to be so designed as to minimize their time requirements. Unusual problems were imposed also by the chemical reactivity of magnesium, its high vapor pressure, and the fact that no satisfactory method for elec-trodepositing magnesium on magnesium is presently available. Finally, the machining and handling of the easily air-borne radioactive-magnesium chips involved certain health hazards, resulting in the need for further experimental restrictions. Preparation of Mg28 The Mg28 was produced in the Carnegie Institute of Technology syncrocyclotron by the neutron spallation of chlorine.5 his involved bombarding a 2 gram crystal of high purity NaCl with a beam of 350 mev protons for a period of 2 hr, after which the crystal was dissolved in warm water and the Mg28 was concentrated and purified by chemical means (see Appendix). About 50 microcuries of Mg28 thus were obtained in the form of magnesium oxinate (8 hydroxyquin-olatc?), which was ignited in air to produce MgO. This in turn was reduced to magnesium metal vapor, by the method of Russell, Taylor, and Cooper," in the vacuum apparatus shown schematically in Fig. 1. Here the essential part is a tantalum ribbon, slightly dished to receive the MgO. The ribbon, pre- viously outgassed at high temperature, is heated to about 1700°C by passing an electric current through it, whereupon tantalum oxide is formed, magnesium vapor is released almost instantaneously, and condensed partly upon the diffusion sample. Diffusion-Sample Preparation: Hot-extruded magnesium rod, 21/32 in. round was used in making the diffusion specimens. The magnesium analyzed as follows: 0.004 pct Al, 0.027 pct Fe, 0.040 pct Mn, 0.0004 pct Cu, 0.0002 pct Ni, and less than 0.01 pct Ca, 0.0004 pct Pb, 0.0011 pct Si, 0.001 pct Sn, and 0.001 pct Zn. A brief study of the crystal texture of this material revealed a sharp fiber texture with the (001) plane roughly parallel to the extrusion axis. Cylindrical samples 1/2 in. long by 5/8 in. were machined from this rod, the end faces dressed on 3/0 emery, and lightly etched with 20 pct HC1 in water. These samples then were annealed for at least twice the intended time of diffusion, at the intended diffusion temperature, in order to stabilize the grain structure at about 1 mm average diameter. The annealing treatments were conducted in argon in the same apparatus and in the same manner as the subsequent diffusion treatments, which will be described presently. Thus, a strain-free plane surface was produced, but there remained a layer of MgO which had largely to be removed before the layer of Mg28 was deposited. Most of this layer was taken off by two light passes over 3/0 emery paper. The balance of the oxide and a thin layer of metal were then removed by etching 5 to 10 min in 4 pct nital (4 pct HNO3 and 96 pct ethyl alcohol) made with absolute alcohol. There followed immediately three quick rinses in: 1-49 1/2 pct methanol, 49 1/2 pct acetone, and 1 pct formic acid, 2-50 pct methanol and 50 pct acetone, and 3-pure benzene. This procedure is essentially that of Sturkey.7 The resulting surface, which was of almost elec-tropolished brightness, remained plane and was free of cold work. It could be kept clean by storing under benzene, or in a desiccator; short exposure

Jan 1, 1955

By N. J. Grant, C. C. Wang

The Ti-Cr-O ternary system has been studied in detail near the titanium-rich corner within the limits of 10 wt pct 0, and 20 wt pct Cr. Studies were extended, but not in detail, to the region beyond 25 wt pct 0, (50 atomic pct) and 62 wt pct Cr (60 atomic pct). Four isothermal sections at 1400°, 1200°, 1000°, and 800°C are presented as well as two vertical sections at 1 and 2 wt pct 02. DURING the last decade much interest has been shown in the development of high strength titanium alloys for high temperature and corrosion resistant applications. Extensive research is being carried out at present, as the current literature indicates, in order to study the properties of titanium and to develop improved alloys. Two of the important alloying elements in commercial titanium alloys are chromium and oxygen and it would be desirable to know their combined influence upon titanium. For this purpose the present work was carried out to investigate the titanium-rich corner of the ternary system TiICr-0. The binary systems Ti-Cr and Ti-0 have been published recently. The Ti-Cr system was studied by several investigators " and their results are in close agreement. The eutectoid decomposition of the B phase has been shown to be extremely sluggish. TiCr, was the only intermetallic compound found in this binary system and was formed at 1350°C by a transformation from the p phase. TiCr? was established as the cubic C 15 (MgCu,) type of structure with 24 atoms per unit cell and was designated as the y phase. This terminology will be adopted in the present work. There was disagreement about the actual composition of this compound among the several investigators, although it is evident from their data that the compound probably has a solubility range of about 2 to 3 pct and is in the vicinity of 65 pct Cr. It has been indicated recently that a high temperature modification of this y phase (TiCr,) existed at a temperature above 1300°C." &apos; This high temperature modification was identified as a hexagonal C 14 (MgZn,) type of structure with 12 atoms per unit cell. The exact transformation temperature from the high temperature phase to the low temperature phase has not been established. A considerable hysteresis was observed and, due to the sluggishness of this transformation, the high temperature phase often co-existed with the low temperature phase at temperatures below 1300°C. A preliminary study of several Ti-0 compounds and the Ti-0 system had been carried out by Ehr-1ich."-"&apos; The most complete binary Ti-0 system was the one reported recently by Bumps, Kessler, and Hansen." The first intermediate phase found in the system was the 8 phase which formed by a peritec-toid reaction of the phases a and Ti0 at temperatures below 925 °C. This reaction is extremely sluggish. The structure of this 8 phase was tentatively identified by these authors as being tetragonal and the lattice constants were found as c,, - 6.645A, a,, = 5.333A and c/a = 1.246A. Experimental Procedure The raw materials used for this investigation were TiO,, electrolytic chromium, iodide titanium, and sponge titanium. The TiO, was in the form of powder of chemically pure grade (99.8 pct pure). The chemical analysis of the electrolytic chromium was: 0, 0.50 pct; Fe, 0.07; Cu, N, and C, 0.01; and Pb, 0.001. The oxygen in the chromium was calculated as part of the final oxygen content of the alloys. The alloys were prepared by the cold crucible method using a tungsten arc. The entire system was evacuated and flushed with purified helium three times and then filled with helium. Each alloy was melted, turned over, and remelted at least four times to insure homogeneity. The total melting time was generally from 6 to 10 min. A master alloy of 25 pct 0,-75 pct Ti was prepared to facilitate alloying by melting compacts of TiOl powder with either iodide or sponge titanium, yielding the compound TiO. It was found necessary to bake the TiO, powder compact at about 150°C to remove adsorbed moisture. This was done to prevent the disintegration and spattering of the compact when the arc was struck. TiO, powder dissolved quite readily into the melt and no other trouble was encountered.

Jan 1, 1955

By Blake M. Caldwell, Harrold D. Owen

The continued use of permanent-type, we11 completion Iras pointed LIP the need for more powerful through-tubing perforating equipment. A new expendable shaped charge perforator has been developed in which the charges are run through the tubing in a vertical position and then opened out to a horizontal position when at the desired shooting zone. The performance of this new tool is comparable to that of conventional casing type perforators. This paper describes the new tool and its applications. Performance data in targets rind under various actual well conditions are presented. INTRODUCTION The general acceptance and increasing use of pernianent-type well completion by the oil industry has indicated the need for through-tubing perforating equipment with performance comparable to that of conventional casing type perforators.&apos;.&apos; To achieve the performance desired, a new, expendable, shaped charge perforator has been developed with adequate power for effectively perforating both 51/2-in. and 7-in. casing below tubing. This has been accomplished without resulting severe damage to the casing and can he obtained under extremes of pressure and temperature. The design of this new tool is a radical departure from previous concepts of tubing guns since it was felt that the two major limitations imposed by previous designs severely handicapped performance. The first of these limitations was the restriction imposed upon the length of the charges by the necessary small inside diameter of the carrier. This resulted from the necessity for compromises in designing a hermetically sealed gun small enough to allow free passage through 2-in. tubing, yet with sufficient wall thickness to withstand some minimum pressure. In an effort to overcome this limitation, the charges were in some cases placed at an angle with the axis of the well with resulting loss in effective depth of penetration. The second limitation concerned the extreme distance of the charges from the casing when the gun was fired. An example of the latter situation is demonstrated by the fact that a conventional 13/4-in. tubing gun centralized in 51/2-in., 17-lb casing has a clearance of more than 1-9/16-in. on all sides. This means that a considerable portion of the force from each charge must be expended in penetrating this 1-9/16-in. of well fluid before it even reaches the casing. With the gun centered in 7-in., 23-lb casing, the amount of fluid penetration required of each jet is in excess of 21/4-in. In a situation where the 13/4-in. gun is touching one side of the 51/2-in., 17-lb casing, the jets from the charges on the opposite side have more than 3%-in. of fluid to penetrate. A similar situation in 7-in., 23-lb casing necessitates the penetration of more than 4-9/16-in. of fluid. The penetrating effect of the charges is severely impaired in passing through so much fluid. Under such conditions, there is usually insufficient force left to penetrate the casing. Previous studies have shown the decided disadvantage of having to shoot through such an excessive quantity of well fluid.&apos;.&apos; The problem. then, was how to position large powerful charges close to the casing prior to firing and still manage free passage through 2-in, tubing. The solution appeared to be in some method of folding sealed charge units in an open type, expendable. 13/4-in. carrier for travel through the tubing, and unfolding them upon their arrival at the shooting zone in the casing. It was desired to control the mechanism electrically from the surface through the regular shooting cable, making the release of the charges independent of the physical characteristics of the well, yet with a provision to prevent the gun from firing until the

Jan 1, 1955

By R. E. Powers, E. H. Kinelski, H. A. Morrissey

A group of 17 American blast-furnace sinters, an American open-hearth sinter, an American iron ore, and a Swedish sinter were used to evaluate testing methods adapted to appraise sinter properties. Statistical calculations were performed on the data to determine correlation coefficients for several sets of sinter properties. Properties of strength and dusting were related to total porosity, slag ratio, and total slag. Reducibility was related to the degree of oxidation of the sinters. THIS report to the American iron and steel industry marks the completion of a 1949 survey of blast-furnace sinter practice sponsored by the Subcommittee on Agglomeration of Fines of the American Iron & Steel Institute. The use of sinter in blast furnaces, sinter properties, raw materials, and sinter plant operation have been reported recently.1,2 After preliminary research and study," test procedures were adapted to appraise the physical and chemical properties of sinter to determine what constitutes a good sinter. During the 1949 to 1950 plant survey each plant submitted a 400-lb grab sample to research personnel at Mellon Institute, Pittsburgh, Pa. A 400-lb sample was also submitted from Sweden. In addition, 2 tons of group 3 fines iron ore were obtained from a Pittsburgh steel plant. The following tests were performed on the iron ore sample and on the 19 sinter samples: chemical analysis; impact test for strength and dusting; reducibility test; surface area measurements, B.E.T. nitrogen adsorption method; S.K. porosity test; Davis tube magnetic analysis; X-ray diffraction analysis for magnetite and hematite; and microstructure. Results of these evaluations are discussed in this paper and supply a critical look at testing procedures used to determine sinter quality. Sinter Tests and Results Each 400-lb grab sample of sinter was secured at a time when it was believed to represent normal production practice at each plant. It was not possible to use the same sampling procedures throughout the survey; consequently samples were taken from blast-furnace bins, cooling tables, and railroad cars. These were very useful for evaluation of test methods, since they were obtained from plants with widely divergent operations. With the exception of Swedish sinter and sinter sample N, which were produced on the Greenawalt type of pans, all survey sinters were produced on the Dwight-Lloyd type of sintering machines. Sinters submitted for test were prepared in identical manner by crushing in a roll crusher (set at 1 in.), mixing, and quartering. To secure specific size fractions for tests, one quarter of the sample was crushed in a jaw crusher and hammer mill to obtain a —10 mesh size. The remainder was screened to obtain specific size fractions. The group 3 fines iron ore was dried and screened and samples were taken from selected screen sizes to be used for various tests. Prior to testing, each ore sample except the —100 mesh fraction was washed with water to remove all fine material and was then dried. This iron ore, a hematitic ore from the Lake Superior region, was used as a base line for comparing results of tests on sinters. The iron ore did not lend itself to impact testing, since it was compacted rather than crushed in the test, and no impact tests are reported. However, the iron ore was subjected to all remaining physical tests to be described. Chemical Analysis: Table I presents chemical analyses performed on the survey sinter samples. Included in this table are data obtained from determination of FeO and the slag relationships: CaO + MgO and total slag (CaO + MgO + SiO, SiO2 + Al2o3 + TiO2). The percentage of FeO was used as an indication of the percentage of magnetite in the sinter. It was believed that slag relationships could be correlated with sinter properties. During initial determination of FeO great disagreement arose among various laboratories, both as to the results and the methods of determining values. Table I lists the values of FeO resulting from the U. S. Steel Corp. method of chemical analysis,&apos; which reports the total FeO soluble in hydrochloric and hydrofluoric acids (metallic iron not removed) with dry ice used to produce the protective atmosphere during digestion. Use of dry ice was a modification required to obtain reproducible results. In this method, the iron silicates and metallic iron are believed to go into solution and are therefore reported as FeO. This is important, for in the study of the microstructure of sinters, glassy constituents suspected of containing FeO as well as crystallized phases of undetermined identity which may also contain FeO have been observed. Strength Test by Impact: In evaluating sinter quality, one of the properties stressed most by blastfurnace operators is strength. This strength may be described as the resistance to breakage during handling of sinter between the sinter plant and the blast-furnace bins. It is also the strength necessary to withstand the burden in the blast-furnace. After

Jan 1, 1955

Jan 1, 1955