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By E. Stansfield, J. W. Sutherland

It is well known that the ash left when coal is burned is not the same either in chemical composition or in weight as the mineral matter originally present in the coal. This mineral matter has been referred to as "mineral impurity," "ash-forming constituents" and "corrected ash." The authors prefer the simple name used in the title and throughout this paper. The mineral matter in a sample of coal cannot be isolated unchanged and then weighed; but if the relation between the weight of mineral matter in the coal and the weight of ash remaining when the coal is burned can be ascertained, the weight of mineral matter in the sample can be calculated from the determined weight of ash. When the weight of mineral matter in the sample is known, the weight of pure coal can be found by subtraction. This pure coal must be the basis of accurate coal classification. W. F. Wheeler,l,3 W. Brinsmaid,2 S. W. Parr, and many subsequent workers have studied the relation between mineral matter and ash. Wheeler and Parr and others have deduced formulas for calculating this ratio, and used heavy-solution separations for checking the accuracy of their formulas. Brinsmaid hand-picked and analyzed two separate samples (and mixtures of these) and based thereon a graphical method of deducing the ratio. In the Fuel Testing Laboratories of the Scientific and Industrial Research Council of Alberta, a graphical method, based on heavy-solution fractionation of coal samples, has been used with marked success for the past 7¼ years for determining the mineral matter-ash ratio. This method resembles that employed by Brinsmaid in 1907.

Jan 1, 1930

By Robert L. Haffner

When mining operations of The Eagle-Picher Co. began in the Illinois-Wisconsin zinc mining field in 1949, all underground loading of broken ore and waste was by caterpillar-tracked machines. Beginning in 1956 rubber-tired end-loaders were brought in; ultimately they completely supplanted the tracked units. End-loaders proved to have the mobility needed for the mining conditions and additional merit in auxiliary capacities. Eagle-Picher operates five mines in this area; two are entered by shafts and three by inclined adits. Several ore zones, some of which are attenuated over a considerable distance, are worked from the same entry. Consequently underground haulage roads connecting or following these orebodies have attained great length. In addition, working places are often widely separated because of the character of the mining operations which include pillar recovery and extending haulage connections into old workings. At one mine, the haulage distance is 5000 ft on either side of the shaft, at another the maximum one-way distance is 8400 ft, and at another the present road system of 6800 ft is expected to reach 10,000 to 12,000 ft.

Jan 6, 1962

By Herbert Clark Hoover, Lou Henry Hoover

QUALITIES which the perfect miner should possess and the arguments which are urged for and against the arts of mining and metallurgy, as well as the people occupied in the industry, I have sufficiently discussed in the first Book. Now I have determined to give more ample information concerning the miners. In the first place, it is indispensable that they should worship God with reverence, and that they understand the matters of which I am going to speak, and that they take good care that each individual performs his duties efficiently and diligently. It is decreed by Divine Providence that those who know what they ought to do and then take care to do it properly, for the most part meet with good fortune in all they undertake; on the other hand, misfortune overtakes the indolent and those who are careless in their work. No person indeed can, without peat and sustained effort and labour, store in his mind the knowledge of every portion of the metallic arts which are involved in operating mines. If. a man has the means of paying the necessary expense, he hires as many men as he needs, and sends them to the various works. Thus formerly Sosias, the Thracian, sent into the silver mines a thousand slaves whom he had hired from the Athenian Nicias, the son of Niceratus1. But if a man cannot afford the expenditure he chooses of the various kinds of mining that work which he himself can most easily and efficiently do. Of these kinds, the two most important are the making prospect trenches and the washing of the sands of rivers, for out of these sands are often collected gold dust, or certain black stones from which tin is smelted, or even gems are sometimes found in them ; the trenching occasionally lays bare at the grass-roots veins which are found rich in metals. If therefore by skill or by luck, such sands or veins shall fall into his hands, he will be able to establish his fortune without expenditure, and from poverty rise to wealth. If on the contrary, his hopes are not realised, then he can desist from washing or digging. When anyone, in an endeavour to increase his fortune, meets the expenditure of a mine alone, it is of great importance that he should attend to his works and personally superintend everything that he has ordered to be done. For this reason, he should either have his dwelling at the mine,

Jan 1, 1950

By S. S. Clarke

Late in 1942, the increasing demand for zinc, coupled with the growing shortage of miners and the knowledge that some abandoned mines would have to be reopened for prospecting and development, led to considerable thought as to the possibilities of further mechanization in order to conserve man power. The ore bodies, locally termed "sheet ground," are an important ore bed in some mines and are in the lower part of Boone formation of the Mississippian Series. Some mines contain interbedded layers of nearly pure galena and sphalerite in horizontal sheets ranging in thickness from a thin seam to several inches and is persistent over large areas. This type of ore body offered the best opportunity for study and experiments. The use of Jumbo drill carriers was advanced but some doubt was expressed as to the adaptability of Jumbos as then in use to mine headings as compared to post and arm mounting (Fig I). Another consideration was the introduction of truck haulage when several mines were trackless. A drill frame, built to carry 2 4-in. drifters, was mounted on a truck chassis. This design proved a failure as it was not rigid and the resiliency of the tires and springs allowed too much play. Long screw jacks were then used to hold the truck firmly in place, but placing the jacks and securing the truck required more effort and time than setting up post drills, so the truck carrier was abandoned. The use of a bull dozer underground had been under consideration for some time to be used in "brunoing" the broken dirt from behind pillars and other inaccessable places so the slusher drags could load without double dragging the dirt. A dozer with hydraulic blade lift was purchased and R. I. Tuthill, Superintendent of Section 30 Mines, suggested that a long drill arm be substituted for the blade, and the drills mounted on the cross member. The hydraulic lift would permit drilling holes at any required spacing. The "cat" was very mobile and answered the problem of a trackless mine. The initial tests showed that the "cat" would make a good carrier, but the hydraulic controls were not positive enough to keep the drills in alignment while drilling. The next step was to build a small hoist. This hoist was attached to the power take-off on the "cat" and by means of sheaves and a double line of 3/8-in. hoist cable, a positive control for raising and lowering the boom was obtained. To avoid serious injuries to the drillers should the cable break, a safety chain was fastened to the drill boom and hooked into a slot in the back of the "cat" frame. A different power unit was obtained for the "cat," as a state law prohibited the use of internal combustion engines in mines. A custom machine shop had just placed on the market a small hoist powered by a Model A Ford engine that had been very ingeniously converted to a slide valve engine using compressed air. To use this unit on a "cat," our master mechanic de-

Jan 1, 1949

By J. Rogers, H. F. A. Hergt, K. L. Sutherland

IN 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group -SO4- or _S03- are excellent collectors for cassiterite and promise to be selective.1 The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000gram Denver cell. EXPERIMENTAL METHODS Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously described.5-10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these tests determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver Submachines.--Melbourne tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By J. F. Sepulveda, J. D. Miller

Tar sand deposits in the state of Utah contain more than 25 billion bbl of in-place bitumen. Although 30 times smaller than the well-known Athabasca tar sands, Utah tar sands do represent a significant domestic energy resource comparable to the national crude oil reserves (31.3 billion bbl). Based upon a detailed analysis of the physical and chemical properties of both the bitumen and the sand, a hot-water separation process for Utah tar sands is currently being developed in our laboratories at the University of Utah. This process involves intense agitation of the tar sand in a hot caustic solution and subsequent separation of the bitumen by a modified froth flotation technique. Experimental results with an Asphalt Ridge, Utah, tar sand sample indicated that percent solids and caustic concentration were the two most important variables controlling the performance of the digestion stage. These variables were identified by means of an experimental factorial design, in which coefficients of separation greater than 0.90 were realized. Although preliminary in nature, the experimental evidence gathered in this investigation seems to indicate that a hot-water separation process for Utah tar sands would allow for the efficient utilization of this important energy resource.

Jan 9, 1978

By B. A. Rogers, K. O. Stamm

BECAUSE it is the basis of the economically important operation of hardening steel by quenching, the A3 transformation in iron has been the subject of numerous investigations. Although the contributions to this subject are interesting, no general review will be given here. Readers who care to follow the matter further are referred to the comprehensive summary by Cleaves and Thompson,1 which covers the literature to about 1935. Their references to 53 papers on the subject suggest that further investigation is hardly justifiable. However, considerable interest has developed recently concerning the reversibility of the transformation. From thermodynamic considerations, the transition ought to occur at the same point on heating or cooling, if the change of temperature is sufficiently slow. Yet all of the earlier investigators found a difference of several degrees. Burgess and Crowe,2 who used thermal methods, obtained average temperatures of 912° for Ac3 and 900°C. for Ar3 on electrolytic iron. Their data indicate a considerable range of temperature over which the change occurs, both on heating and on cooling. Terry3 measured the susceptibility in the critical range and estimated from the steepest parts of his curves that Ac3 came at 9180 and Ar3 at 903°C. Ishiwara4 was one of the first investigators to report a shorter interval between the temperature of the change in the two directions. He measured the change of susceptibility of kaolin-coated samples of steel, in a hydrogen atmosphere, at rates of heating and cooling so low that about 3 or 4 hr. were required for the transformation to complete itself. His results show some variability between samples, but indicate that the difference between Ac3 and Ar3 is in the vicinity of 6°C. Roberts and Davey5 measured the space lattice in pure iron in the vicinity of 900°°C. and concluded that a change occurs reversibly between 907° ± 3° and 9100 ± 3°C., probably between 907° and 910°C. Wells, Ackley, and Mehl6 made dilatometric determinations of the Ac3 and Ar3 points in samples of hydrogen-treated carbonyl iron maintained under a vacuum. They used three rates of heating and cooling: 2°, '1/2°, and 1/8°C. per min. and found the spread between the two points decreased with low rates. At the slowest rate, the Ac3 transition occurred at 909° to 909.5°C. and the Ar3 change at 907°C. in three of the samples believed to contain the lowest percentages of alien elements. They concluded that if the rate of temperature change and the content of alien elements were low enough, the A3 transformation would be completely reversible at 909.5° ± I°C. The question of reversibility is an interesting one and when some iron with especially small percentages of alien elements became available the opportunity to conduct an investigation was welcomed. This iron was prepared by the Division of

Jan 1, 1941

By G. F. Loughlin

MORE than 20 years have passed since the publication of Lindgren and Ransome's report on the Cripple Creek District,1 which was made when the district was much more active and prosperous than in recent years. They concluded that the output of the district, which had reached its maximum of about $18,200,000 in 1900, would gradually decline, and their conclusion has been confirmed by records of subsequent production. Between 1905 and 1915 annual declines were partly compensated by encouraging increases, especially in 1908, 1914, and 1915; but a rapid continuous decline followed, due largely to the war and its after effects, until in 1922 the value of output was only slightly more than $4,000,000. It rose to nearly $5,000,000 in 1924, but declined again in 1925 and in 1926, when it was about $4,400,000, and represented ores mainly from deep levels in the Cresson and Portland mines. The profitable operations of these two mines were the principal factors leading to a study of ore at deep levels in the district by the U. S. Geological Survey in coopera-tion with the Colorado Metal Mining Fund. The principal reasons for Lindgren and Ransome's conclusion were three: (1) the greater cost and difficulty of deep exploration; (2) the decrease in the number of veins with increasing depth, and (3) the probability that the telluride ore, believed to have formed at comparatively low temperature, would not persist indefinitely -in depth. Operations since they made these statements have verified the first two, but call for some modification of the third. Rich telluride, ore is being mined at a profit in the Portland mine 3000 ft. below the present surface, or 5000 ft. below the original surface of the Cripple Creek volcano, as interpreted by Lindgren and Ransome. The question arises, therefore, as to the number and extent of such deep deposits, and the answer, so far as it can now be given, must be based mainly on structural data, supplemented by data on the processes of ore deposition. Presentation of these data based on a study of deep mines in the southeast quarter of the district, the only

Jan 1, 1927

By Rollin E. Hook, Attwell M. Adair

The yield and fracture behavior of recrystallized chromiztm have been studied in order to gain an understanding of the recrystallization embrittlement-rheotropic recovery phenomenon. The duc tile-brittle tensile transition temperature of recrystallized chromium was found to vary from 225 ° to -80°C as the ratio of specimen diameter/mean planar grain size decreased. The applicability of this observation to other bcc metals is briefly discussed. Brittle fracture in recrystallized chromium was found to be initiated predominately from intercrystalline rupture nuclei. Single crystals exhibit a high degree of ductility at 23 "C. The experimental data indicate that grain boundaries play a significant part in the yield and fracture behavim. Pres training significantly reduces the transition temperature, and high temperature aging does not result in re-embrittle-ment until complete recovery or re crystallization occurs. SEVERAL theories have been used to explain the recrystallization embrittlement-rheotropic recovery phenomenon in chromium. Wain, Henderson, and ohnstone' propose a Cottrell dislocation locking mechanism due to nitrogen, and Weaver and Gross and weaver 3 propose a strain-induced precipitation mechanism involving a chromium nitride precipitate. The researches of many investigators seem to leave little doubt that brittleness in chromium is promoted by interstitial impurities. Smith and seybolt4 have shown that the ductile-brittle transition temperature is lowered as the interstitial content is reduced. weaver3 provides evidence for a 150°C reduction in the tensile transition temperature as the nitrogen content is reduced from 20 to 5 ppm. Maykuth and affee' have suggested that the amount and orientation of grain boundary impurities may be responsible for the brittle nature of recrystallized chromium. This suggestion was based on their findings that wrought iodide chromium possessing a fiberous grain structure is ductile in tension at room temperature while a recrystallized grain structure is completely brittle. Previous investigations have not studied this phenomenon sufficiently to determine its cause. Perhaps this has been largely due to previous experimental findings that brittle fracture observed in chromium has been almost entirely transgranular.' In addition McNeil and imb,' who investigated coarse-grained as-cast chromium, describe the point of initiation of fracture as cleavage, close to the (100) plane, near or at grain bound-daries, or at included particles or voids. However, Hook, Adair, and ipsitt found that fracture in coarse-grained recrystallized chromium is initiated by intergranular rupture and then propagates nearly entirely by cleavage. This result, together with their finding that room temperature ductility in bending is observed for single crystals and coarse-grained polycrystalline specimens for which the number of grains through the specimen diameter is small, suggests that grain boundaries may play an important role in the brittle behavior of chromium. The recrystallization embrittlement problem can be resolved into two questions. These are, whether the controlling mechanism is predominately one of crack initiation or crack propagation, and whether brittle fracture is initiated predominately by slip or twin induced intergranular rupture or by cleavage. The following research was designed to study the role of grain boundaries on the brittle fracture of chromium in an effort to resolve these questions. EXPERIMENTAL PROCEDURES, RESULTS, AND DISCUSSION General Procedure. All tensile specimens (except 0.04 in. diam wires) were prepared from 1/4 in. diam swaged rod fabricated from one ingot. Details of fabrication are given elewhere. The results of impurity analysis for the swaged rod and for the

Jan 1, 1963

By T. S. Lundy, R. E. Pawel, F. R. Winslow, C. J. McHargue

The volume-diffusion coefficients of Nb-95 and Ta-182 in niobium have been measured over the temperature range 878° to 2400°C. High-temperature specimens (T 21500°C) were sectioned by conventional lathe and grinding techniques while low-temperature specimens were sectioned by an anodizing and stripping technique previously described. Over a range of more than ten orders of magnitude in diffusivity, the self-diffusion data is well-represented by the equation: D = (1.1+ 0.2) exp [- (96,000 * 900)/RT ] cm2/sec Upward deviations from this line are explained by short-circuit diffusion in combination with the loss of resolution of the sectioning techniques. Oxygen contamination within the range 100 to 450 ppm was found to have little or no effect on the self-diffusivitj 01 niobium. In a limited number of measurements, the diffusivity of Ta-182 in niobium was found to be about half that of Nb-95 in niobium. These data may be described by D = (I.0+0.90.5)exp [- (99,300 * 2400) /RT ] PREVIOUSLY reported studies of self-diffusion in niobium were by Resnick and Castleman1 and Peart, Graham, and Tomlin.2 The data of Resnick and Castleman over a temperature range 1585" to 2120°C show considerable scatter but. can be represented by D = (12.4 *0.8) exp [-(105,000+3OOO)/RT] cm2/sec The limited data of Peart, Graham, and Tomlin follow the equation D = 1.3 exp (-95,00O/RT) cm2/sec In view of recent diffusion data for ß zirconium3 and 0 titanium4 in which Arrhenius-type plots do not yield straight lines and of the potential high- temperature uses of niobium and its alloys, we thought it important to investigate the diffusion behavior of this bcc refractory metal over a large temperature range. This has recently been done for molybdenum,5 chromium,6 vanadium,"" and tantalum.9 Niobium was a particularly suitable material for this study largely because of the development of an anodizing and stripping sectioning technique which enables diffusivities as small as l0-19' sq cm per sec to be determined accurately.10 In addition to self-diffusion data, data were obtained for the diffusion of Ta-182 in niobium and for the effect of varying oxygen content on self-diffusion. I) EXPERIMENTAL PROCEDURE Materials. The niobium was obtained from three sources: 1) melting stock from Shieldalloy Corp., 2) electron-beam melted single crystals, 1/2 in. diameter, from Semi-Elements, Inc., and 3) oxygen-doped, electron-beam melted single crystals from Materials Research Corp. The melting stock was electron-beam melted and specimens 5/8 in. diameter by 1/2 in. long were machined from the center of the bar. The analysis supplied by the vendor and an interstitial analysis of one of the specimens are given in Table I. The single crystals (type 2 above) were cut with a jeweler's saw to specimens about 3/8 in. long. The interstitial analysis of this material is given in Table 11. This material was used

Jan 1, 1965

By D. B. McWhorter, J. D. Nelson

Conventional analyses of seepage through saturated media do not apply when tailings impoundments are located above a partially saturated zone. Three stages of seepage are identified and methods for estimating the seepage rates and duration of each stage, based upon flow in partially saturated and saturated porous media, are demonstrated. The effectiveness of earthen liners is discussed and procedures for estimating the required properties of the porous media are provided.

Jan 1, 1981

By W. A. Tiller, J. P. McHugh

HE majority of liquidus and solidus surfaces in phase diagrams have been determined by the conventional cooling- and heating-curve techniques.' These techniques have two main shortcomings: 1) the solidus may be in considerable error due to the difficulty involved in completely homogenizing the solid and 2) the determination of liquidus and solidus in more than a two-component system does not enable one to determine tie-lines connecting the specific equilibrium solid and liquid compositions. However, in a recent paper by one of the authors,' a method was suggested whereby the liquidus and solidus surfaces plus tie-lines in an n-component system may be determined. This method utilizes a controlled solidification technique and assumes that interface equilibrium exists during freezing. The present work was undertaken with a twofold purpose; first, to determine the liquidus and solidus lines in the pseudo-binary system Bi2Te3-Bi2Se3 by heating- and cooling-curve techniques and, second, to determine the partition coefficients of Te and Se in the BizTe3-,Sex system by controlled solidifica- tion techniques. The two sets of results can be compared to test the accuracy of the controlled solidification method. EXPERIMENTAL I—The starting materials for this study were 997999 pct Bi, Te, and Se, obtained from the American Smelting and Refining Co. The compounds BizTe, and Bi2Se3 were each prepared by melting together stoichiometric amounts of the elements, followed by twelve zone-refining passes. This produced homogeneous bars of the compounds for use in the phase-diagram studies. The apparatus used to obtain heating and cooling curves is illustrated schematically in Fig. 1. The alloy samples were located in a graphite crucible placed in a stainless steel canister. The canister was supported in a heavily lagged pit furnace by a device which oscillated the canister about its vertical axis at a frequency of about 3 cycles per sec during heating and cooling-curve runs. The graphite crucible was designed to minimize the thermal coupling of the sample to the furnace. A thin graphite sleeve separated the alloy sample from the stainless steel tube that housed the thermo-

Jan 1, 1960

Jan 1, 1928

Frank Clemes Smith, Deadwood, 8. D. (communication to the Secretary): The reading of Mr. Chance's interesting paper suggests a few ideas relative to his discussion of certain Black Hills gold-ores. Mr. Chance refers to his examination, in 1897, of " the (Carboniferous) limestone plateau-country which encircles the central area of the Black Hills," and says that " it had been generally assumed that the mineralization of this formation was confined to the northern area;" further, that he "found, however, a general mineralization, extending in zones or belts throughout the region," and that the ores, being more or less specially

Jan 1, 1900

By Susan B. Leiter

That oxygen in copper has been a source of trouble is well known and that that trouble has been real in the commercial world has been shown by Fuller.' Moore and Beckinsale's paper2 at the annual meeting of the Institute of Metals in London, 1921, called forth considerable discussion. Prof. T. Turner expressed the opinion that it was not necessary to have cuprous oxide present in sufficiently large quantities to form either globules or seams in order to produce a bad effect if the copper were gassed. This brought up the question of the solubility of oxygen in copper and the authors desired to know whether there were any evidence of such solubility, because their experience was that whenever there was any oxygen in copper it was present in the form of free cuprous oxide, which was practically always in the form of globules. Later Hanson, Marryat, and Ford3 stated that 'for all practical purposes cuprous oxide may be regarded as insoluble in copper. However, they found particles of the eutectic to coalesce to form much larger particles. They suggested that cuprous oxide was actually slightly soluble in copper, for it was difficult otherwise to understand the mechanism by which such coalescence could take place. W. E. Ruder, in discussing that paper, said that his experiments had led him to conclude that a slight solubility must exist to allow for the ready coalescence of oxide particles, but conductivity tests convinced him that that solubility was very small. Nevertheless, there appeared to be a state of admixture of oxide with copper that closely resembled a colloidal mixture which at first was mistaken for a true solution and which usually existed at the grain boundaries. The purpose of this paper is to give the results of some investigations, begun in September, 1921, which would seem to show that although cuprous oxide may be only slightly soluble: (1) this solubility is sufficient

Jan 1, 1926

By R. C. Gould, A. M. Skov, L. F. Elkins

Comparison of long term decline in oil production during cyclic waterflooding or pressure pulsing of part of the Driver Unit with steady injection-imbibition flooding in the Tex Harvey area led to large expansion of flood in the Driver Unit on the steady injection basis. While the flood has been successful, the major problem has been attainment of satisfactory oil production rates in most of the wells. Large volume fracture treatments of low capacity wells were unsuccessful in achieving sustained increases in production. A two-section area in the Driver Unit has already recovered 620 bbl of oil per acre by waterflood but other areas have not performed so well. Sun Andres water containing 300 to 500 ppm H,S is sweetened to 0.5 to 1 ppm H,S by extraction with oxygen-free flue gas. This prevents contamination of gas produced in the area and apparently it has reduced corrosion in minimum investment, thin-wall, cement-lined water dktribution systems. Cement-lined tubing in injection wells has mitigated corrosion as effectively as thick polyvinyl chloride films have, and at less cost. Introduction As reported in the literature the Spraberry field of West Texas has presented unusual problems for both primary production and waterflood ing. Earlier information from the Spraberry Driver Unit included conception and evaluation of cyclic waterflooding or pressure pulsing in a nine-section pilot test as an aid to extraction of oil from the tight matrix rock and as a boost to normal capillary imbibition forces An additional 5 years' operation in that area, and performance of expanded steady injection water-flood, now covering a total of 68 sq miles, are reported herein. In addition, since the Driver Unit is one of the largest waterfloods in areal extent in the U. S., many operating experiences are presented for the benefit of engineers concerned with operation of other Spraberry floods or with other waterfloods where this reservoir technology and/or water handling technology may be adaptable in part. These include: (1) attempts to improve producing well capacity through large volume fracture treatments, (2) long-term performance of water treating plants utilizing oxygen-free flue gas to extract H,S from sour San Andres water, (3) performance of thin-wall cement-lined pipe in water distribution systems including comparison between those sections carrying raw San Andres water and those carrying treated water, and (4) comparison of performance of various lining materials and subsurface equipment in water supply and water injection wells. These experiences are reported without regard to whether results are good, bad or indifferent. Since the operations reported are limited to the techniques, materials, and equipment actually used in the Driver Unit, no comparison is possible with results of other approaches used in other Spraberry floods or in waterfloods generally under different conditions. However, an attempt is made to quantify these experiences as much as possible in the space available to permit other engineers to select those parts applicable to eheir problems. Background The Spraberry, discovered in Feb., 1949, is a 1,000-ft section of sandstones, shales and limestones with two main oil productive members—a 10- to 15-ft sand near the top and a 10- to 15-ft sand near the base, having permeabilities of 1 md or less and porosities of 8 to 15 percent. Extensive interconnected vertical fractures permitted recovery of oil on 160-acre spacing from this fractional-millidarcy sandstone, but they made capillary end effects dominant. Primary recovery by solution gas drive is less than 10 percent of oil in place, with most wells declining to oil production of a few barrels per day when reservoir pressures are still in the range of 400 to 1,000 psi. Partial closing of the fractures with declining reservoir pressure is believed to be the cause of such low production rates at these relatively high reservoir pressures. In 1952 Brownscombe and Dyes proposed that displacement of oil by capillary imbibition of water from the fractures into the matrix rock might significantly increase oil recovery from the Spraberry, overcoming otherwise serious channelling of water through the fractures." A pilot test conducted by the Atlantic Refining Co. during 1952 through 1955 indicated technical feasibility of the process; but low oil production rates averaging I5 to 20 bbl/well/D failed to create significant interest in large-scale waterflooding at that time." Humble Oil & Refining Co. conducted a highly successful 80-acre pilot test during 1955 through 1958 with

Jan 1, 1969

By J. A. Elias, A. J. Heckler

A simplified method is described for the prepauatior~ of comnposite samples for determination of one quadrant of an X-ray pole figure of a sheet material by the Schulz reflection method. Other special conzposite sampling methods were used to investigate specific areas of the pole figures. Plotting nets for these sampling plans were drawn by a computer. Step-scanning techniques were used to obtain detailed information about specific regions of a pole figure. Satisfactory pole figures were obtained for large-grained (0.5 to 1 in. diam) sheet materials. COMPOSITE sampling techniques for preparing one quadrant of an X-ray pole figure have been reported by a number of authors.'-5 All of these methods are similar in that they use a composite sample prepared by stacking and holding together coupons cut from a sheet material. The schulze reflection technique is applicable to the composite sample so that only minor corrections are needed for defocusing and absorption effects. Also, a relatively large area of a sheet is sampled through the use of multiple cross sectional pieces. In general, sampling methods necessary to obtain a composite-type specimen have been formidable enough to discourage their use in routine pole figure determinations. This paper presents a versatile sampling technique which is simpler than those previously described along with an accurate method for obtaining stereographic plotting nets for any orientation of a composite specimen surface. A step-scanning technique is used to obtain more quantitative determinations of specific regions in pole figures, and the composite technique is satisfactorily applied to determine pole figures of very large grained sheet materials. REVIEW OF PREVIOUS TECHNIQUES Mueller and ~nott' first proposed a technique for obtaining one complete quadrant of an X-ray pole figure by using a sheet sample and six different composite samples in which the individual coupons were aligned and held together by two types of jigs. Data from the seven different samples were overlapped to obtain a single quadrant. ~eieran~ and Lopata and ~ula~ obtained a complete quadrant of a pole figure from a single sample prepared by forming a cube from coupons cut from a sheet. These coupons were bonded together using an epoxy cement, and a cut was made at 54.7 deg to the normal, transverse, and rolling directions of the sheet, Fig. I. The normal direction of the cut face projects into one quadrant of a stereographic projection at equal angles to the three principal orthogonal reference directions mentioned above. X-ray reflection data obtained along a spiral path in physical space could then be plotted on a stereographic net offset 54.7 deg from the normal, as shown in Fig. 2. A rotation about an axis representing the surface normal is designated as a, and a rotation about an axis lying in the plane of the surface is 4. From Fig. 2 it is apparent that a tilting angle of no more than 55 deg @ is necessary to obtain the complete quadrant. ~eber~ devised an improved sampling technique by cutting coupons 45 deg to the rolling direction of a sheet, stacking and bonding these with an epoxy cement at an angle of 54.7 deg to a reference plane, and finally grinding and lapping a flat specimen surface parallel to this plane. An important consideration of this technique and that of Lopata and ~ula~ is variation in the diffracting power of the specimen surface due to the bonding medium. While any composite-type sample will have some such variation due to boundaries between coupons, the problem can be minimized by elimination of the bonding medium and by avoiding prolonged etching times which could lead to significant inter lame llar attack of the coupon faces. EXPERIMENTAL TECHNIQUE We were working concurrently though independently on a technique similar to ~eber's,' but which does not

Jan 1, 1968

By John Campbell

An approximate theoretical model is proposed to quantitatively predict freezing ranges Tf and hydrostatic tensions P developed within solidifying binary alloys, allowing for a certain amount of diffusion of solute in the solid during solidification. The maxima in ATf and AP as functions of composition are shorn to occur at smaller solute concentrations than would be expected from the equilibrium diagram, and are found to correspond closely to experimentally observed maxima in microporosity. THE freezing range of simple binary alloys appears to have been little studied, except for certain indirect observations on the defects, particularly microporosity and hot tearing, arising in long freezing range materials. Two theories relating to the freezing range of alloys and its effect upon porosity are reasonably well established, and appear to have been held in isolation from each other: a) From purely equilibrium considerations early researchers expected that an increase in solute content of an alloy should increase the freezing range (defined here as the equilibrium freezing range ?Tf = Tl-Ts where TL and Ts are the liquidus and solidus temperatures, respectively) and thereby increase the width of the pasty zone for a given set of conditions. This in turn should increase the difficulty of feeding the residual liquid through the dendrite mesh to compensate for the contraction on solidification, and consequently tend to increase the observed amount of porosity. From qualitative observations on steels Czikel1 reports an increase in porosity with increasing carbon content up to 0.46 pct C. More careful measurements by Whittenberger and Rhines2 on fourteen different alloy systems showed an approximately linear relation between ?Tf and pct porosity (although unfortunately the precise experimental data is not given). b) Conversely however, other authors3"5 propose that porosity is reduced by the presence of increased amounts of eutectic present at the final solidification temperature. Lees7 and Bochvar6 claim that the hot tearing of alloys is similarly reduced. Scheuer8 has put forward a theory to explain this effect, Fig. 1. The argument is basically that solidification progresses on a plane front through a relatively open dendrite network and is thus (the argument is not developed more explicitly) easier to feed. One would expect effect a) to operate at low solute contents, and b) to be important at higher solute contents, so that at some critical composition a max-

Jan 1, 1970

By F. Paredes, W. R. Holman, R. W. Crawford

The diffusion coefficient for hydrogen in the ß titanium alloy containing 13 pct V, 11 pct CY, and 3 pct A1 was measured over the temperature range 20° to 500°C. Results fit the expression: D= 1.58 x lgs exp-------==-----) cm2,sec THE diffusion coefficient for hydrogen in the metastable ß-phase titanium alloy containing 13 pct V, 11 pct Cr, and 3 pct A1 was measured as part of an investigation of the effects of hydrogen on the mechanical properties of titanium alloys. Several theories on the mechanisms of hydrogen embrittle-ment include diffusion of hydrogen at ambient temperature as an important step in the embrittling process.'-5 In hydrogen-contaminated a-ß titanium alloys, it has been postulated that the rate-controlling step may be the rate at which hydrogen diffuses from the ß phase to stress- or strain-nucleated brittle hydride platelets at the a-ß interface.' However, embrittlement of the all-ß alloy investigated in this work may proceed by a different mechanism, since this alloy can be embrittled without the formation of detectable hydride platelets.6 Troiano has suggested that in this case the mechanism of delayed failure or embrittlement is similar to that proposed for high-strength steel, i.e., repeated crack initiation caused by a decrease in bonding energy as hydrogen diffuses to points of high tri-axial stress at the root of a notch. In both types of alloy the rate of embrittlement is believed to be controlled by diffusion of hydrogen in the ß phase. Accurate hydrogen-diffusion data in the vicinity of room temperature should therefore be of some assistance in understanding the mechanisms of embrittlement in these two classes of titanium alloys. Diffusion of hydrogen in pure titanium has been studied by Wasilewski and Kehl7 at temperatures above 500°C. Their measurements on diffusion in the ß phase were extended below the ß-a transformation temperature (882°C) to approximately 600°C. This was possible because of the 8 stabilizing effect of hydrogen. No results at lower temperatures have been published and there are no data in the literature on hydrogen diffusion in the ß -phase alloy used in this program. Hydrogen diffusion in metals is generally investigated by measuring the rate of transport of hydrogen past a solid-gas interface, i.e., by absorption, permeation, or degassing-rate measurements. These methods produce accurate diffusion data when bulk diffusion is the rate-determining step in the over-all process. However, at the lower temperatures of interest in hydrogen-embrittlement studies or under conditions where surface films are present, the measured rates may be surface-controlled and the calculated diffusion coefficients will be in error. Surface effects were eliminated in the present work by using a modification of the common welded-couple technique m which two bars with uniform but different compositions are joined before the diffusion anneal." The same type of step change in the initial concentration vs distance curve was produced by electrolytically hydrogenating thin-strip specimens which had been electrically insulated over half of their length. Concentration vs distance curves were determined, after appropriate diffusion-annealing treatments, by vacuum-extraction analyses of transverse samples sheared from the strips. Diffusion coefficients were calculated by the methods of Grube.M This technique was feasible because of the large concentrations of hydrogen which can be charged into p -phase alloys without the formation of hydrides15'16 and because of the extremely low degassing rates observed when hydrogenated titanium alloys are heated in air. EXPERIMENTAL WORK The diffusion couples were cut from a 0.022-in.-thick mi ll-annealed sheet.* Strips 8 in. long by 1/2

Jan 1, 1965

By F. J. Schuh

The drilling industry long has been plagued by failures in the bottom few joints of surface and intermediate casing strings. This paper presents an analysis of the various possible causes of failure and concludes that failures are caused by short-lived, high-energy torque impulses delivered from the drill string through the bit while drilling out the cementing plugs, cement and floating equipment. The magnitude of these torque impulses is shown to be a function of the rotational momentum of the drill string, and a method is derived to calculate the magnitude of these impulses. The available methods of strengthening the bottom joints are reviewed. It is concluded that, while present methods are ineffective, a combination of improved procedures for strengthening and minor restrictions on drillout practices will prevent failures. Introduction In most cases, failure in the bottom few joints of casing strings is not discovered until electric logs record that the bottom one, two or three joints have parted from the casing string and slipped down the hole. However, in some cases the parted section of casing uncovers a high-pressure or lost circulation zone, or shifts laterally restricting the passage of drilling equipment. In these instances extensive remedial work is required to realign the parted pieces and seal the exposed formations. Several methods used to strengthen the bottom joints of casing strings include locking set screws in the couplings, putting wedges in special collars, welding straps across the couplings, welding the couplings and, most recently, using epoxy resin-based, thread-locking compounds. Since none of these techniques has eliminated the problem, this study was initiated to find the cause of failures and to evaluate the available methods of prevention. Mechanics of Casing Failures An analysis of the various possible causes of failure indicates that the casing is unscrewed rather than broken and that therefore failure must occur before the shoe is drilled. Since there is no general agreement as to the causes of casing failure, some possible mechanisms were ATLANTIC RICHFIELD CO. DALLAS, TEX. considered in this analysis. Failure of the bottom joints of casing can occur by only one of three types of stress: tension, torsion or bending. The possible mechanisms of failure were evaluated by determining the forces required to cause casing failure by each of the stresses; and, where applicable, the possibility of failure by fatigue was considered. For casing to part under tension requires a downward load of more than the tensile strength of the casing. The lightest API weight H-40 grade casing requires a bit load on the bottom of the casing of 27,000 to 34,000 Ib per inch of bit diameter (Table 1). Since maximum drill collar weights seldom exceed 10,000 Ib per inch of bit diameter, it is apparent that casing strings cannot be parted by the downward load of the drill string. The second mechanism considered was failure by bending. This mechanism requires that the lowermost casing joints be free to be deflected laterally until the bending stress exceeds the strength of the pipe. To fail, the casing (at a height L above the shoe) requires a force and deflection' at the shoe of To deflect the casing shoe with the drill string obviously requires a dog-leg at the casing shoe. This dog-leg must have a rate of change equal to or greater than the change in curvature of the deflected casing, which is given by

Jan 1, 1969