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By J. L. Eakin

The Bureau of Mines determined agents that are effective in foaming heavy brines and oil from gas wells in severe concentrations of sodium chloride, in severe concentrations of calcium chloride, or in moderate oil-brine mixtures. Dynamic foam tests were designed to select the more effective foaming agents. Numerous foaming agents were tested in concentrated simulated brines, in oilfield brines having varied concentrations of ions, in heavy natural brines, and in a commercial brine generally used as a reservoir pressure-balancing fluid. Several agents were detected that could perform efficiently in the field under the most severe saline conditions. Agents that promote foaming in oil-brine mixtures were also determined.

Jan 1, 1965

By W. H. McFarland

The mechanical properties have been determined for a large number of alloy-free martensitic steels with carbon contents ranging from 0.08 to 0.20 pct and with manganese contents of about 0.4 to 0.5 pet. These steels were tested 1) as water-quenched, 2) after quenching, temper rolling, and tinning, and 3) after tempering treatments which involved temperatures from 400o to 1300oF and times from 1 min to 8 hr. The majority of these tests represent steel from commercial-size coils, i.e., strip 32 in. wide, coil weights up to 20,000 16, and steel thicknesses from 0.0055 to 0.024 in. As a result of these treatments, it has been shown that as-quenched low-carbon alloy-free steels can be produced with tensile strengths ranging from 140,000 to 220,000 psi and tensile elongations from 3.0 to 4.0 pet in 2 in. The tensile strength of the as-quenched martensites can be represented by the equation, tensile strength (ksi) = 119 + 560 (wt pet C). The response to tempering of these steels is related to previous work by Muir, Averbach, and Cohen and by Grange and Baughman. Strain aging of low-carbon martensite has also been investigated. If low-carbon steels are defined as those steels with a maximum carbon content of 0.2 pet, it is found that the literature on low-carbon, alloy-free martensites contains little data on the mechanical properties of these steels. However, the following facts concerning low-carbon alloy-free martensites seem firmly established:'-' 1) The major factors in controlling the strength of the martensite appear to be a) fine structure, b) the internal strain resulting from the transformation, and, particularly, c) the amount of carbon in solid solution. 2) In low-carbon steels, the martensite is auto-tempered and is in the form of needles with only minor amounts of internal twinning, whereas the martensite in high-carbon steels forms as plates which are internally twinned on a fine scale. 3) Care must be taken in comparing the results of work that has been done on low-carbon steels with varying amounts of alloying elements to data on plain carbon steels. As has been noted by Irvine, Pickering, and Garstone,6 alloying elements generally lower the martensite start temperature and, thereby, decrease the amount of auto tempering obtained during the quench. This makes it difficult to

Jan 1, 1965

By Robert Parker

Measurements of the latent heat of transformation from a to 0 titanium were made using a pulse-heating technique. Rapid heating was accomplished electrically by discharging a low-inductance capci-tor hank through a thin-strip specimen. Both high-purity titanium and titanium containing 2700 ppm of 0 were studied. An electrical-resistivity technique and a plot of energy input us temperature rise were used to monitor the phase change. It was concluded that: 1) the latent heat of transformation is 800 i 48 cal per mole; 2) phase change occurred in less than 200 sec; and 3) the percentage phase change that occurs is linearly a function of the energy available for phase change. In addition, this experiment provides a simple and inexpensive method for determining specific heat of electrical conductors over large temperature ranges. The chief advantages of this technique over past pulse-heating experiments are: 1) static measurements of capacitor-bank voltage capacitance and specimen resistance can be made quickly and accurately to determine the energy supplied to the specimen; 2) the specimen is heated so rapidly (10 µ sec) that there is no appreciable heat loss during the heating. THE purpose of this paper is to illustrate the use of the capacitor bank as a tool for basic experimental investigations and to determine the rapid phase-change kinetics of titanium. The capacitor provides a number of unique properties: 1) rapid heating rates in the order of l09oC per sec can be obtained; heating rates as slow as l04oC per sec are available by merely adding a given amount of inductance to the circuit; 2) the energy input can be precisely determined and can be varied from several joules to millions of joules, depending on the bank capacitance and voltage; 3) the specimen can be heated uniformly through the thickness and length or non-uniformly, as desired; 4) the apparatus is simple and inexpensive and can be easily altered; 5) the form of the specimen can be wires, sheets, foils, rods, and cylinders; 6) there is great precision in the timing of events; 7) this technique may be readily used in conjunction with rapid cooling.

Jan 1, 1965

By W. D. Haentjens, A. P. Pipilen, M. Weintraub, A. A. Orning

W. D. Haentjens (Barrett, Haentjens and Co., Hazleton, Pa.) — The authors are to be complimented on undertaking a project which has little available experimental data. There are so many variables in the hydraulic transport of solid materials that it is difficult to correlate the experimental information from one series of tests into usable data involving other materials or even similar materials but of different size consists. The friction data is of particular interest to those involved in pipeline design. Most such pipelines, however, involve portions which are not level and the effect of sloping or vertical lines might also be considered in extensions of this test work. Pump manufacturers are concerned about criticism resulting from the stated amount of degradation occurring in a pump. The amount of degradation is affected somewhat by pump design and this should be taken into consideration. The pump which was loaned for this work was a modification of a standard medium duty slurry pump. This modification was for maximum particle size, however if minimum degradation is the object, then other design changes would be indicated. Although there is a tendency to be less concerned with degradation in industrial applications, it is nevertheless an important factor in many uses and further studies should be made. In particular, the amount of degradation could possibly be segregated into more classifications, rather than charge some losses to the pump which apparently are occurring in other handling. It seems difficult to evaluate the degradation which occurs in handling the coal into the pump sump and in removing it from the line into the tank. Each handling, of course, contributes some degradation, as does the screening operation itself. These are all charged to the pump, or to the pipe line and pump together; and, although they may be small, they could possibly be evaluated. It is interesting to note the verification of the old rule of thumb of maximum particle size equal to approximately one-third of the pipe size. Our experience has shown size distribution to have an effect on the flow characteristics and if this data is available for the tests which were run, it would be interesting supplementary information. A. P. Pipilen, M. Weintraub and A. A. Orning (Authors' Reply) — In this paper the authors have attempted to outline some of the major factors affecting a rational design for a solids-liquid transport system. They are grateful to Mr. Haentjens for pointing out several other equally important considerations. Pump manufacturers, in general, should be complimented on the strides that have been made in decreasing particle degradation within the pump. Considerable research and a great deal of mathematical analysis is required before pump design in this field can become a science rather than an art, for each system requires a different set of compromises. As Mr. Haentjens indicates, maximum-particle-size handling capability may be inconsistent with minimum degradation; even more important, the rotor profile for the most efficient transfer of energy to the fluid may have to be compromised to reduce particle breakage, for, whenever particle density differs from fluid density, the two phases will have different trajectories. Some evidence of this geometric factor is provided by a cursoy analysis in the Bureau of Mines Report of Investigations now in preparation, where it is indicated that, for the pump used, degradation decreased when the tangential velocity was decreased and when the radial velocity was increased. This relation, itself, is probably a function of particle size and concentration. Some data on particle size distribution, as requested by Mr. Haentjens, will be provided in the Report of Investigations referred to above in addition to that already presented in Table II of the original paper. However, in the limited number of tests it is difficult to distinguish between cause and effect, for not only did the particle size distribution alter the flow characteristics, but, through the medium of degradation, the operating conditions rapidly altered the particle size distribution.

Jan 1, 1965

By G. E. Rennick

A siphon-type laboratory airlift well was designed and operated by the Bureau of Mines to study the concurrent flow of air and oil in small-diameter pipes. Glass flowstrings ranging from to 1 inch in diameter and from L4 to 64 feet in length were equipped with various-sized air-entry jets. Liquid holdup volumes were used to correlate vertical-flow data, and empirical equations for computing gas requirements were derived. The effect of flowstring length on flow efficiency, oil- and gas-production rates, and gas-oil ratios was relatively minor at all flowing pressures. Air-jet sizes and flowstring diameters, however, had a marked effect on flow efficiency and oil- and gas-production rates. The small air-jet sizes increased maximum flow efficiency and its associated flowing pressures but decreased oil- and gas-production rates. An increase in flowstring diameter increased maximum flow efficiency with its associated flowing pressure and also increased the production rates of oil and gas.

Jan 1, 1965

By L. S. Darken, H. A. Wriedt

In a previous paper,1 an experimental study of nitrogen dissolved in a cold-rolled ad heat-treated, low-carbon steel at 300° to 450°C yielded the equilibrium solubility relations and the concentrations of the two types of deject sites involved. In this paper, the probable identities of the defects that absorb nitrogen are restricted from the available evidence to screw dislocatioms for B sites, and to either micro crack surfaces or edge In a previous paper.' we reported an experimental study of the excess nitrogen solubility in a low-carbon steel produced by a combination of plastic deformation and nonrecrystallizing heat treatment. The concentrations of the defect sites that absorb the excess nitrogen were measured in terms of their capacities for nitrogen. Also measured were the equilibria of nitrogen distribution among the sites. Several problems and questions arise from these measurements. We should like a physical identifi- dislocations for A sites. The concentrations of these defects in experimental steel specimens are estimated from the concentrations of defect sites. finally, the influence of chemical composition upon the nitrogen-trapping defects—the relative numbers generated in deformation, the relative numbers surviving as temperature is raised, the apparent numbers observed, and the distribution equilibria-is discussed. cation of the defects involved and of the two kinds of nitrogen-absorbing sites, called A and B types, upon those defects; the concentrations of the defects themselves could then be computed. We should also like to know how exclusively the findings apply to the "X steel" used in the experiments and to what extent they apply to cold-rolled steel given no subsequent treatment. By considering the data already given, together with results from a few specific tests which will be reported as they are invoked, we are able to eliminate some interpretations altogether and to secure an acceptable though limited interpretation from among the remaining possibilities.

Jan 1, 1965

By W. W. Agey

An inexpensive technique that laboratory studies indicated would significantly reduce seepage in irrigation canals was devised and tested through research sponsored by the Bureau of Reclamation and the Missouri River Basin Field Committee. Laboratory tests simulating optimum field conditions determined that easily applied sodium carbonate solutions made test beds of canal lining materials virtually impermeable for long periods. The study comprised alternative laboratory treatments of 3-inch-deep test beds of canal earths with 74 water-soluble chemicals in search of one 01' more that would effectively improve the water barrier characteristics of the component clays. Sodium carbonate, one of the least expensive, was among the most effective. The addition of 0,4 lb of reagent per sq yd greatly reduced the seepage from typical, highly permeable test beds. The reagent penetrated and sealed surface for about a 1.5-inch depth.

Jan 1, 1965

By H. E. Rudi

The advent of open nit mining permitted the development and processing of minerals never before thought possible. New equipment was needed; new techniques were devised; new methods were called for. This development and acquisition of new techniques, methods and equipment did not, however, stir the souls of our industry and educational leaders sufficiently to a recognition of the problem of people, especially the future development of the people needed in open-pit mining. The people problem has been and will be with us as long as there are two of them. The development of people will be required for the same reason. The problem of developing future personnel for open-pit mining is not what must be developed; that is known to all of us and can be briefly stated ashore and better of everything." As I see it, the real problem lies in determining (1) what personnel are really critical, (2) why are they critical and (3) how can we develop them.

Jan 1, 1965

By J. B. Conway

RECENT studies of first-stage creep data have led to a special least-squares procedure for use in calculating the Andrade creep-equation constants. This procedure is easy to apply, uses only experimental data, and yields results which do not vary with the individual making the analysis. Taking logarithms of the Andrade equation I = lo(1 +ßl1/3)ekt leads to In l = In lo + In(1 + ßl1/3) + kt A residual can then be defined as the difference between the logarithm of an experimental length value and the logarithm of a calculated length value. Following the usual least-squares approach differentiation with respect to 10 and k of the expression for the sum of the squares of the residuals leads to two equations which cannot be solved directly for the three constants involved. However, values of ß can be assumed and corresponding values of lo and k can then be calculated. Then the sum of the squares of the residuals can be calculated. For a certain value of ß this sum will exhibit a minimum value to identify the least-squares values for ß, lo, and k. An illustration of the application of the above least-squares approach is obtained by employing the creep data for lead originally presented by Andrade' in the development of the one-third creep law. A plot of the sum of the squares of the residuals as a function of ß is shown in Fig. 1 along with the corresponding lo and k values. The minimum is seen to occur at ß = 0.0143 from which lo = 39.149 and k = 7.27 x 10-5. Based on these results the Andrade equation for these lead data is 1 = 39.149(1 + 0.0143 t1/3)e7.27 x 10-5t compared to the equation I = 39.13(1 + 0.01457/l/3)e6.95 X 10-5t developed by Andrade (calculation procedure not given but was probably a graphical solution). Calculating length values using the above equations and comparing with the experimental length values, residuals corresponding to the difference between experimental and calculated length values can be obtained. The sum of the squares of the residuals can then be calculated. For the case of the least-squares approach a value for this sum was found to be 2.37 x 10-3 compared to a value of 3.47 x 10" for the equation originally proposed by Andrade. In other words, while the constants proposed by Andrade provide an excellent fit for the lead data, a still better representation is afforded by applying the least-squares approach discussed above. A similar result was obtained for the lead data at 162oc.l The least-squares approach led to 1 = 9.866(1 + 0.0497 t1/3)el.011 x 10-2t compared to the equation I = 9.94(1 + 0.0433 l1/3)e1.06 X 10-2t given by Andrade. In this case, too, the sum of the squares of the residuals is slightly smaller for the equation based on the least-squares approach. It should be pointed out that a double trial and er-

Jan 1, 1965

By P. J. Jorgensen, J. H. Westbrook

The anomalous indentation creep of nonmetallic solids is shown to be due to the presence of adsorbed water. Although a specific mechanism is not proposed, it is suggested that the water may be present in two chemically adsorbed states. DEPENDENCE of the indentation hardness of solids on the time of load application was first studied systematically by Hargreaves1 in a study of lead and certain low-melting alloys. This technique has become known as indentation creep and has been exploited particularly by underwood and by Mulhearn and Tabor3 as well as by others.4°7 For metals good correlations have been found between the time dependence of hardness over several orders of magnitude in the seconds range and creep parameters from conventional tests at the same temperature where creep strains were measured over hundreds or thousands of hours. However, Walker and Demer8 and Mitsche and Onitsch9 observed extensive indentation creep at room temperature (particularly for light loads) in certain minerals and in materials such as lithium fluoride and magnesium oxide for which conventional creep is ordinarily not observable unless the testing temperature is at a very much higher fraction of the melting point. Normal behavior was observed' for metals such as copper, i.e., negligible time-dependent flow during room-temperature indentation. Walker and Demer attempted to find some distinctive difference in the surface deformation markings about indentations in the anomalously behaving materials at short and very long indentation times. No significant differences were observed. Increased duration of loading was found, however, to result in an increase in the length of glide of edge-dislocation loops extending into the interior of the crystal. Jorgensen and Westbrook,10 in a recent study of

Jan 1, 1965

The purpose of this paper is to present the methods used in ground water control and the considerations that affected the development of these techniques. Production at Knob Lake is currently proceeding at depths which may be as much as 200 feet below the original standing water table. In order to produce a more saleable product and to improve operating and maintenance conditions, it is necessary to depress the water table below the mining level. Considerable success has been achieved by drilling deep wells in strategic locations and installing vertical tur-bine pumps at depths of up to 400 feet. This method is especially suitable for operation under severe winter conditions and has reduced the detrimental effects by a far greater extent than other methods of water control, Spring runoff is handled in open sumps, but all other water from four mines, with flows exceeding 16,000 g.p.m., is pumped all year 'round from about thirty-five wells. THE Knob Lake operation of the. Iron Ore Company of Canada is located on the Quebec-Labrador border, 320 miles north of Sept-lies, a seaport

Jan 1, 1965

By A. Heim, M. Gondouin

Invasion experiments were run on Berea sandstone cores to get laboratory measurements of resistivity and saturation profiles characteristic of water and oil sands invaded by mud filtrate. Injection rates were as low as 1.13 cm/D, and the cores were 30 to 36 in. long, cut parallel to the bedding planes. In the water-sand case, the resistivity profiles revealed the existence of an extensive transition zone between flushed and uncontaminated zones. In the linear geometry of the experiment, the width of the transition zone increased as the square root of the injected fluid volume. For the oil-sand case the core was prepared by displacing the formation water with kerosene to minimum water saturation. During the subsequent invasion experiment. oil saturation was measured directly by means of an oil-soluble radioactive tracer, and resistivity profiles along the core were taken at the same time. These data were interpreted in terms of an oil-water front, followed by a formation water bank, a zone of mixed waters, and finally, invaded mud filtrate near the borehole. Micro-fingering and capillarity seemed to affect considerably the resistivity profiles observed in the invaded oil-sand experiment. Beyond the regular conductive annulus or "low zone", it was found that a resistive "anti-annulus" could also be formed. As a result of these experiments, some simplified invasion profiles have been accepted and are being used in Grand Slam* interpretations. INTRODUCTION The importance of the mud filtrate-invaded zone in interpreting electrical logs has long been recognized.',* In trying to account for its effect, only very simple models of the resistivity profiles in the radial direction from the borehole have been used. In fact, most log interpretation charts have been based on resistivity models consisiting of two media of uniform resistivity (R, and R,) abruptly separated at the diameter of invasion. Such a clean separation of the media of different resistivities seems unrealistic, since flushing may not be perfect and may vary with radial distance into the formation.3** The nature of the transition zone, when it is within the radius of investigation of the surveying devices, may affect the log readings. Campbell and Martin' verified that a conductive annulus containing a high percentage of formation water may be formed when mud filtrate invades an oil-bearing sand. Interpretations which are to include the effect of such an annulus require the addition to the model of a conductive zone located at the outer rim of the invaded zone.' Using the Buckley-Leverett relations,6 aturation profiles may be derived, from which resistivity profiles can be calculated. Results of such computations by K. S. Kunz and J. H. Moran were given in a paper by Dumanoir. Tixier and Martin,7 and led to the construction of log interpretation charts which were based on a representation with three media of resistivities R, R0 and R1. Fig. 1 shows a schematic representation of a resistivity profile which includes an annulus. Campbell and Martin realized that, during the invasion of an oil sand, both capillarity and mixing would contribute to rounding of the profile shown in Fig. 1. Capillarity tends to draw some of the formation water from the annulus into the uncontaminated (Rt) zone, whereas mixing of the mud filtrate with formation water of the

Jan 1, 1965

By Norman G. Foster

The mass spectra of 14 previously unreported alkylthiophenes are pre-sented. Low ionization voltage data of selected compounds from these 14 and 23 previously reported alkylthiophenes are presented and discussed for their value in supporting fragmentation mechanisms analytical correlations. A comparison with and corroboration of earlier correlations is made. Additional correlations concerning detection of side chain branching and the detection of ethyl-alkyl and propyl-alkylthiophenes are made. A discussion of the possible fragmentation routes and mechanism of fragmentation is given. Speculative structures are inferred s out some of the ions and hence this work provides a basis for suggesting fation mechanisms for the alkylthiophenes according to modern theories ass spectrometry. Verification of these mechanisms must await the availability of isotopically labeled molecules which are labeled in specific lotions that permit the definition of the paths of frag-mentation. Some suggestions for further work to generalize on the correlations and studies made to this point are presented.

Jan 1, 1965

By A Turek

The Lake Cinch deposit occurs in the Tazin gneisses on the footwall side of the Black Bay fault. Ore is localized by two faults, the Main Ore fault and the Cracking-stone River fault, occurring in shoots along the former and on tension fractures between the two faults. Faulting leading to the localization of the deposit is analyzed in detail and tied into the regional pattern. Pitchblende, the chief radioactive mineral, is investigated by X-ray and found to be of very small particle size. The relation-ships of U, Fe and Mn in the ore are established quantitatively, and Fe is found to bear a catalytic relation to U. The deposit is classed as belonging to Lindgren's mesothermal class. Mineralization is attributed to carbonate solutions, and the uranium is believed to have been trans-ported in the hexavalent state as the uranyl tricarbonate ion; analogy is drawn to a recently developed hydro-metallurgical technique for the production of uranium dioxide. Introduction THE Lake Cinch deposit is located in the Beaver-lodge Camp, Saskatchewan. The property was staked in 1948 and went into production in 1957

Jan 1, 1965

By F. L. Wideman

SPURRED by demands of a buoyant economy for mineral products, output from mines in the United States established a new record. Removal of waste material, necessary for the extraction of economic minerals, kept pace with mine production. Earth moving by these two activities exceeded 3 billion tons, an increase of 5 percent over that of 1963. Crude materials from which metal or nonmetal products were derived accounted for 75 percent of the total. The remainder, mostly worthless, was classified as waste. Changes in the minerals industry result from many causes. Technological trends and labor productivity are among several significant and interrelated indexes that assist in the analysis of the changes. Therefore, a. study of productivity is helpful in measuring technological growth in mining. Concepts of productivity tend to vary with the purpose for which the term is used; frequently, productivity is expressed in terms of units of output per unit of labor, such as tons of ore per man-hour or man-shift. Comparisons of levels of productivity for a group of products are usually made using composites of output. Data for all metal and nonmetal mines except gold, silver, mercury, platinum metals group, and sand and grave were used to compile the composite for determining productivity for 1960-64. Copper ore, iron ore, and phosphate rock are mined mainly by surface methods, but characteristics of the deposits and differences in processing the crude material affect production of the commodities. Therefore, productivity data for these selected segments of the minerals industry reflect the influence of physical conditions on the exploitation of them.

Jan 1, 1965

By W. A. Backofen, D. H. Avery, W. F. Hosford

Sheets of the magnesium alloys AZ31B, HK31A, and ZE10A in several different tempers were tested in tension and determinations were made of the ratio of width-to-thickness strain. A marked increase in the ratio with tensile straining and a dependence upon alloy and test direction are rationalized in terms of a balance between the amounts of basal and prism-plane slip. All such variations are related, in turn, to the prevailing crystallographic texture. Fracture appearance is explained on the basis of anisotropy in plastic flow, and implications for developing texture -hardening effects in these alloys are discussed. ThE crystallographic texture or preferred orientation of a given material is determined by details of processing history. Such texture is known to influence many aspects of material behavior, in particular both the yielding and strain-hardening characteristics which are of special interest in the present work. Traditionally, the resulting plastic anisotropy has not been regarded as especially desirable. Earing in drawn sheet is perhaps the most common example of an unwanted effect of texture. However, it has also been recognized that suitable textures may be usefully employed to improve drawability,1,2 as a specific example, and generally to control yielding resistance under combined-stress loading.374 Texture would seem to be a detail of structure not yet exploited to nearly the fullest extent. A convenient basis for characterizing anisotropy in plastic behavior is the ratio of width-to-thickness strains obtained in a tension test;5&apos;6 the parameter is frequently labeled "R" and its value is revealing with respect to the nature of the prevailing texture. R gives a useful measure of a material&apos;s "thinning resistance". For an isotropic material, R = 1. With R > 1 the increased through-thickness strength in a sheet means greater resistance to yielding under biaxial tension, or "texture hardening";3&apos;4 if R < 1 the result may be a "texture softening" under the same loading conditions.4 Most R data relate to steel sheets for deep-drawing applications. Values for steel and other materials of cubic structures are not often much greater than 1 and nearly constant with strain in testing.1,2,7,8 To explore the implications of plastic anisotropy further, it was felt that experiments with much more strongly textured materials would be useful, and this led to the choice of magnesium alloys. The "ideal" sheet texture for magnesium contains the (0001) plane in the rolling plane, which ought to lead to R values approaching infinity. However, departures from the ideal texture, the possibility of slip in non-close-packed directions, and deformation by twinning would all be expected to introduce some range of R. Accordingly, studies on these materials were undertaken. EXPERIMENTAL Alloys in sheet form, Table I, were selected to obtain a variation in crystallographic texture, in the expectation that this would be reflected in differences in plastic anisotropy. Pole figures constructed by the Schulz surface-reflection technique9 were provided with the experimental materials by the Dow Metal Products Co. Profiles of pole density along great circles through the rolling (0 deg) and transverse (90 deg) directions were prepared from the pole figures and are collected in Figs. 1 and 2; considerable departure from the "ideal" (0001) alignment in the rolling plane is evident, with the largest angular spread in both directions being found in the ZEl0 alloy. Results of tensile tests on full-thickness specimens of 6-in. gage length by 1/2-in. width are given in Fig. 3 as engineering stress-strain curves* in rolling and transverse directions. All tests but one were made at a constant drive rate of 0.02 in. per min, and the final values of percent elongation at fracture, over the initial 6-in. gage length, are noted at the ends of the curves; one test on ZE10A-

Jan 1, 1965

By Clarence O. Babcock

ROCK BEHAVIOR has proved of national interest in a variety of fields. The behavior of rock consequent to a nuclear blast was used to detect such blasts, as criteria for the design of underground military defense installations that would resist nuclear blasts, and for judging the feasibility for peaceful uses of nuclear explosives. An obvious peaceful application of nuclear explosives would be for large-scale rock excavation, and plans were presented during the year to improve the present Panama Canal or create a new canal by this method. These plans were based largely on earlier crater tests that demonstrated rock behavior when subjected to a buried nuclear blast. A knowledge of rock behavior under impact was used to evaluate the materials of the moon by means of the geometric configurations visible in the close-up pictures of the moon surface taken by the U.S. rocket Ranger 7. The composition of the moon must be considered in devising methods for taking samples of the surface layers or in designing underground shelters as bases for future explorations of the moon.

Jan 1, 1965

By S. L. May

Tantalum and columbium can be extracted from several of their ores or concentrates by chlorination procedures. Direct chlorination of high-grade minerals in the presence of carbon at temperatures between 500° and 800° C will extract up to 99 percent of the tantalum and columbium. Metallurgical beneficiation of low-grade source materials by carbothermic reduction produces a ferroalloy that is amenable to chlorination at a temperature of 500° C. Over 90 percent of the tantalum and columbium can be recovered.

Jan 1, 1965

By C. D. Hall, F. E. Dollarhide

Conventional static tests of fluid-loss agents do not realistically simulate conditions in a fracturing treatment. The dynamic tests reported here show that fluid-loss volume is better represented as proportional to time, rather than as the square root of time. This leads to a different equation for fracture area. The leak-off rate increases with increasing shear rate at the fracture wall, but appears to approach a limiting value. Pressure effects are minor. Spurt loss ordinarily is not affected by the flow velocity in the fracture and is inversely proportional to concentration of agent. The filter cake, once it is well established, is resistant to damage by the flow of plain fracturing liquid (without fluid-loss agent). The latter two findings indicate that a treatment employing a high-concentration spearhead followed by plain fluid can offer a more economical treatment under suitable conditions. INTRODUCTION The successful design of hydraulic fracturing treatments depends on accurate knowledge of the fluid-loss properties of the fracturing fluid. Howard and Fast,&apos; in giving the basic equation relating fracture area to fluid and treating parameters, described three mechanisms which might control the rate of fluid leak-off from the fracture. One mechanism usually is dominant in a given well treatment. For each mechanism, the leak-off velocity is inversely proportional to the square root of time, and the proportionality constant is designated as the fracturing-fluid coefficient. For the wall-building type of fluid-loss agent, the coefficient is determined by a filtration test in a pressure cell, usually with a rock wafer or core as the filter medium. In these static tests, the cumulative volume generally is proportional to the square root of time, after an initial spurt volume. The static-fluid-loss test is not representative of the con,-&tions under which a fluid-loss agent performs in a fratturing treatment. The marked difference between the dynamic- and static-fluid-loss behavior of drilling fluids reported in the literature2,3 implies that dynamic testing is also needed with fracturing fluids. We have therefore undertaken a study of the dynamic-fluid-loss behavior of fracturing fluids. The testing apparatus has also afforded opportunity to evaluate the resistance of the filter cake to removal or damage by flowing fluid containing no fluid-loss agent, with and without sand. The results of these studies offer a means for more accurate evaluation of fluid-loss agent performance, and point the way to a "spearhead" fracturing technique which may offer more economical treatment for some wells. EXPERIMENTAL METHODS The dynamic-fluid-loss testing method is applicable to any type of wall-building fracturing fluid. The present study aimed first at finding what phenomena are involved, and therefore has been limited in the number of materials tested. All of the results specifically reported herein are for kerosene containing a commercial solid fluid-loss agent, which is commonly used at 50 lb/1,000 gal of oil. Another agent in liquid form, used usually at 20 ga1/1,000 gal oil, has shown all the same phenomena in dynamic tests, and generally the same level of fluid-loss control as the solid agent. The dynamic-fluid-loss core cell used in all tests is shown in Fig. 1. The fracture was simulated by the an-nulus between a 2.03 in. OD sandstone core and the surrounding pipe. Annulus widths of 0.234 and 0.117 in. were used, and the core was 3.5 in. long. The annular geometry provides a uniform fluid velocity and a well-defined shear rate over the entire filtering surface, and permits a large filter area (144 sq cm) in a reasonably compact cell. The leak-off fluid passed into a 0.5 in. diameter axial hole in the core. A hollow steel rod through this hole was threaded into a rounded "streamliner" upstream of the core, and into a mounting stud downstream. The streamliner and the stud had the same outside diameter as the core. In all tests except those where sand was circulated, the mounting stud had protruding rings which constricted the annulus, to minimize any tendency for channeling of the fluid to the side exit port. The ends of the core were sealed by Neoprene, steel and Teflon washers. The leak-off fluid was conducted from the hollow rod to an exit tube, through a metering valve (a fine-pitched needle valve) and a quick-opening toggle valve in series, and into graduated cylinders for volume measurement; Two separate circulating systems were used in the experimental program. The extensive initial testing was done at 50 to 150 Psi. The fluid was circulated by a variable speed Moyno pump, and the flow rate was read by a rota-meter flow meter. The filtration Pressure was supplied by holding a back-pressure with a throttling valve. The discharge streamcould be diverted into any of four sections

Jan 1, 1965

By David A. Thomas, David N. French

The lrnrdness of WC crystals has been measured with the Knoop indenter at loads of 100 and 500 g on the (0001) and (1070) planes. The hardness as tneasitred on the basal plane is 2400 kg per sq mm and shows little anisotropy. The hardness on the prism plane, however, shows a marked orientation dependence, with a low value of 1000 kg -per sq mm when the long axis of the Knoop indenter is oriented parallel to the c axis and a high value of 2400 kg per sq mm when the indenter is perpendicular to the c axis. Slip lines (Ire observed surrounding the microhardness indentations and they show slip on (1010) planes, probably in [0001] and (1120) directions. This slip behavior can be explained by the crystal structure of TVC, which is simple hexagonal with a c/a ralio of 0.976. The hardness anisotropy call be explained by [0001]{1010} and (1130) {10l0] slii) and the resolved shear-stress analysis of Daniels and Dunn. HARDNESS anisotropy is a well-known phenomenon and has been reported for many metals, with both cubic and hexagonal structure.1-6 For hexagonal tungsten carbide, WC, a wide range of hardness values is reported in the literature. For example, Schwarzkopf and Kieffer7 give a hardness of 2400 kg per sq mm and report a value of 2500 kg per sq mm by Hinnüber. Foster and coworkerss give the average Knoop microhardness as 1307 kg per sq mm with a maximum value of 2105 kg per sq mm. Although these values and the structure of WC suggest the likelihood of hardness anisotropy, no such measurements have been made. We first detected a large apparent hardness anisotropy in WC crystals about 75 p large, in over-sintered cemented tungsten carbide. Prominent slip lines also occurred around many indentations. This report presents further observations and interpretations of hardness anisotropy and slip in WC crystals obtained from Kennametal, Inc. Both Knoop and diamond pyramid indenters were used on a Wilson microhardness tester with loads of 100 and 500 g. EXPERIMENTAL RESULTS The carbide crystals tended to be triangular plates parallel to the (0001) basal plane of the hexagonal structure. The side faces were parallel to the ( 1010) prism planes. Specimens were mounted approximately parallel to these two types of faces and metallographically polished. Laue back-reflection X-ray patterns were used to orient the specimens, which werethen ground to within ±1 deg of the (0001) and (1010) planes. The Knoop hardness values measured on the basal plane are plotted in Fig. 1. There is only a small anisotropy, with a hardness range of 2240 to 2510 kg per sq mm. The additional points at angles from 52.5 to 67.5 deg confirm the sharp minimum hardness at 60-deg intervals, consistent with the sixfold hexagonal symmetry. The average hardness of all values obtained on the basal plane is 2400 kg per sq mm. While the basal plane shows only slight anisotropy, the (1010) plane exhibits marked hardness anisotropy, from 1000 to 2400 kg per sq mm. Fig. 2 shows the hardness as a function of the angle between the long axis of the indenter and the hexagonal c axis, the [0001] direction. The minimum and maximum occur when the indenter is oriented parallel and perpendicular to the [0001] direction, respectively. The anisotropy of the prism plane is contrary to that reported for hexagonal zinc and hard- However, the basal-plane anisotropy is similar to these two metals.1&apos;2 To check the accuracy and reproducibility of the measurements, a series of fifteen impressions was made at 100-g load in the same orientation in the same area of the specimen surface. The average for all was 2040 kg per sq mm, with a range of 1950 to 2130 kg per sq mm, giving an accuracy of about ± 5 pct. Thus the slight anisotropy on the basal plane is almost within experimental error. Fig. 3 shows slip lines around the Knoop indentations on the basal plane. The slip traces are in directions of the type (1130). The presence of slip steps on the basal plane indicates that the slip direction lies out of the (0001) plane. Because WC has a c/a ratio of 0.976,&apos; the shortest slip vector is [0001], which suggests slip systems of the type [0001] (1010). Fig. 4 shows slip lines around the Knoop intentations on the (1010) plane. These slip lines are inconsistent with [0001] slip but can be

Jan 1, 1965