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By R. B. Rosene, G. L. Foster, A. R. Hendrickson

he properties of some of the common fracturing oils, such as sand-falling rate, fluid loss and viscasity, are a function of the three major constituents of the oil. These are: asphaltic material, parafin waxes and a base oil. The base oil can be either high or low viscosity. Asphaltic material increases viscosity by thickening the oil, decreasing the rate of fall of sand through the oil. at temperatures up to 200" F. When large arnorrnts of parafin wax are present, much of the wax i.s not dissolved, but is present in the form of rnicroscopic crystals. 7'his, of course is limited to temperatures below the melting points of waxe.s. As a result, parafin waxes clo not function primarily as thickener.7, but rother as bullting materials. The functiori of wax, without asphaltic material, in a low viscosity base oil is uniquely unlike that of wax with asphalt coexistent in the oil. The resulting difierence in wax crystal size governs the sand-falling rate to a large extent. An ideal type of fracturing oil is one containing neither asphalt nor waxes. In such cases, the viscosity and resulting low sand-falling rate are apparently due to soluble resin- ous hydrocarbons, which are compatible with formation oils. INTRODUCTION Since the introduction of hydraulic fracturing as a method of stimulating production from oil and gas wells, a variety of fluids have been employed to open the fractures and carry the propping agent. Such fluids include gels, emulsions, and oils. In the latter category, the use of refined oils has increased tremendously, and it is probably safe to assume that such oils represent more than one-half of the total fluid used in fracturing. The general acceptance of refined oils for fracturing can be accounted for on the basis of their relatively low cost and general applicability. To minimize transportation costs, such refined oils are generally obtained within the local areas of operation. As a result there are several kinds of oil used in different areas, with a wide variation in the basic composition. These types may vary from a fair grade of lubricating stock to a highly viscous cut-back asphalt. or road oil. Originally, little attention was paid to the composition of the oils used for fracturing, and any oil which would carry sand was considered satisfactory. Recently, however, service companies and well operators have become more concerned with the type of oils used for fracturing. With this in mind, the present work was undertaken to evaluate and compare many widely used fracturing oils to determine which constituents were most desirable for fracturing purposes. Some of the important properties of fracturing fluids are sand-falling rate, viscosity, and fluid loss. Other properties, that are actually of no less importance, include flash point, pour point, emulsifying tendencies with formation brines, and compatability with the formation oils. This discussion has been limited, however, to the first mentioned properties in order to give some idea of the general composition of the refined oils, how they function, and why. PROPERTIES OF FRACTURING OILS The properties of fracturing oils are a function of the three major constituents of the oil. These may be designated as: (1) asphaltic material, (2) paraffin waxes and (3) a base oil, which may be of either high or low viscosity. The asphaltic material clas-

Jan 1, 1956

By R. Stefanko

The use of strain gauges and compression pads for an underground bolt installation in a central Pennsylvania coal mine revealed that satisfactory anchorage could not be maintained in the shale stratum that constituted the immediate roof. Comprehensive laboratory tests resulted in a new shell designed with an increased area of contact and smaller surface serrations. Retightening of the bolt was also found to be beneficial for maintenance of high load values. Roof bolting in coal mines has progressed very rapidly in the last decade, and today this method of support is in general use. There are many theories concerning the functions of roof bolts, but the importance of beam building is indisputable. Proper tension in the bolts minimizes shearing along bedding planes and creates a thick, competent beam from individually weak layers. Bolting must be accomplished immediately upon exposure of the roof, and bolt tension must be maintained if roof failure is to be prevented. Seams are being mined today with roof bolt support where conventional timbering was not effective.' The widespread use of continuous mining equipment was made possible by roof bolts which permit long supported spans free of obstructions. Since adequate anchorage is the key to successful bolting, better methods for determining the efficiency of anchorage are continually being sought. Attempts have been made to measure bolt loads, thus assessing anchorage efficiency by employing sensing devices between the bolt head and roof. 3-s None of the techniques appears to be very accurate, and all have at least one serious deficiency. The greatest efforts are being directed toward the standardization of the pull test.6" Nevertheless, the author believes that the pull test is only one criterion for establishing the efficiency of anchorage and not necessarily the most important one. The conventional pull test involves the short-term application of forces, whereas the success of roof bolt installations is dependent upon the ability of anchorage to sustain relatively long-term forces. Therefore, it would appear that the time-dependent function of the anchor is the single most important parameter for the success of roof bolting in many types of rocks. UNDERGROUND TESTS Strain gauges and compression pads were employed to measure bolt loads in a central Pennsylvania coal mine.8 Bolting had been employed only sporadically in the shale top since dubious benefits were obtained with this type of support. Table I shows some typical results from this investigation. Anchorage losses were extremely variable among the bolts, but all showed a considerable degree of bleed-off. The tests indicated that anchorage efficiency was extremely low in this type of shale. The results confirmed that bolting under these conditions was practically worthless, and thus a waste of material and labor. Probably even more important, bolting constituted a hazard when reliance was placed upon it for support. Certainly the complete lack of confidence in roof bolting, which was apparent in the mine personnel, was justifiable since the bolts did not accomplish their purpose. PRELIMINARY LABORATORY BOLT TESTS The extreme losses in bolt tension that were detected in underground installations prompted a comprehensive study to assess the causes. However, preliminary studies were first made to determine the combined stresses in a roof bolt and to prove conclusively that the observed bleed-off phenomena were due to anchorage: slippage and not to some other physical manifestation. In all of the ensuing tests

Jan 1, 1962

By W. A. Backofen

THE texture of cold-drawn copper wire has been described most often as a composite of [Ill] and [loo] directions aligned parallel to the wire axis.' Hibbard2 suggested that sufficient reduction will result in a single [111] texture and reported that after a reduction in area of 96.4 pct, such a texture was nearly obtained. Other work3-4 has shown that recrystallization within the temperature range of 300" to 1000°C does not alter the texture established by cold-drawing. In general, however, the texture of cold-drawn end annealed copper wire is not as well defined as the deformation texture. In the work reported here it was found that the double-fiber, deformation texture persists even after a reduction in area of 97.3 pct, and after recrystallization the texture is practically all [l00]. The wire used in this work was prepared in the following way. A 3/4-in. diam length of annealed OFHC copper was cold-drawn to a diameter of 1/8 in., a reduction in area of 97.3 pct. Each step in the drawing operation brought about a reduction in area that varied from 6 to 10 pct. Short lengths of this wire were etched in a 50-pct solution of nitric acid to a diameter of approximately 0.01 in. The texture of the cold-drawn specimens was determined with the conventional X-ray transmission diffraction technique using filtered copper radiation. The X-ray beam was directed perpendicularly to the wire axis and the diffraction rings were recorded on a flat film. Fig. la is typical of the photo-grams obtained and reveals that the cold-drawing schedule described above introduces a distinct, double-fiber texture with both [Ill] and [l00] directions aligned parallel to the wire axis. Supplementary measurements with a Geiger-Mueller counter of the intensity of reflection from (111) planes showed that the [111] component was much more predominant than the [l00]. Additional specimens of the drawn and etched wire were annealed in a salt bath at temperatures from 300" to 450°C. The texture of the recrystal-lized wire was studied with the same technique applied to the cold-drawn wire. Fig. lb is an X-ray photogram of a specimen annealed for 1 ½ at 300°C and is typical of those obtained from re-crystallized specimens. The photogram shows that recrystallization of this material is accompanied by the almost complete elimination of the [111] component of the deformation texture. A pronounced strengthening of the [100] component was evident from intensity measurements with a Geiger-Mueller counter. In summary, the deformation texture of cold-drawn OFHC copper wire, after a reduction in area of 97.3 pct, may still be described as a composite of [Ill] and [loo] directions aligned parallel to the wire axis. Recrystallization of such wire at temperatures from 300" to 450°C introduces a texture which consists almost entirely of a [loo] alignment. Acknowledgment Sidney Rolle of the Scomet Engineering Co. generously supplied the OFHC copper used in this work. References 'C. S. Barrett: Structure of Metals. p. 382 (1943) New York. McGraw-Hill Book Co. 2 W. R. Hibbard, Jr.: Trans. AIME (1949) -185, p. 598; Journal of Metals (Sept. 1949) TN 19E. 3 P. 422 of ref. 1. 'E. Schmid and G. Wasserman: Ztsch. Physik (1926) 40, p. 451.

Jan 1, 1952

By W. P. Evans, R. W. Buenneke

Warren and Averbach's multiple order, Fourier method was applied to solid specimens of SAE 1045 steel. The material was hardened to three hardness levels and specimens of each hardness were shot peened to three intensities. Particle size, root-mem-square strain, mean strain, md macro residual stress were determined for each. Microstrains caused by either hardening or peening varied markedly over microregions. In general, increasing the hardness or peening intensity increased the rms strain and decreased the particle size. Similar effects were observed by varying hardness and peening intensity independently. At a Rockwell hardness of C 50, peening had little effect on line broadening, but both mean strain and macro residual stress increased. Mean strain was independent of column length. Induced macro residual stress by peening was affected most by initial hardness, but not by specific peening intensity. The purpose of this work is to establish the state of residual strain and particle size by X-ray diffraction in hardened and cold-worked plain carbon steel and attempt to relate these X-ray measured parameters to fatigue performance. X-ray line broadening (and its micro implications), along with X-ray residual stress (and its macro implications), may be basic indicators of the inherent fatigue resistance of the material. X-ray line broadening is caused by variable lattice strains and small particle size. Both are a result of plastic deformation which accompanies hardening or cold working processes. Therefore, X-ray line broadening is a good measure of both. warren1 has recently reviewed the Warren and Averbach2,3 Fourier analysis of line broadening. Strain and particle size effects can be separated because broadening due to particle size is independent of order of the diffraction peaks, while broadening due to strain is not. Microstrain is obtained as a root-mean-square strain averaged over discrete distances within the crystals causing diffraction. These distances are quite small, varying from 10 to 10081, and may be interpreted as the gage length over which the strains are averaged. Because of their variable nature, the X-ray line is broadened. The plot of rms strain vs distance (or column length) within the specimen gives a measure of their variability. Small particles also cause X-ray line broadening as already mentioned. A particle is interpreted as a region within a crystal or grain which diffracts X-rays coherently. This region is one of given orientation and may be bounded by a small angle grain boundary, dislocations, a twin boundary, or a stacking fault. The present work covers measurement of X-ray line broadening and macro residual stress on an SAE 1045 steel, quenched and tempered to various hardnesses. Various amounts of cold working were produced by shot peening the surfaces to various Almen intensities. Particle size, root-mean-square strain, and mean strain were calculated from the Fourier coefficients of the X-ray diffraction profiles in a direction normal to the peened surface. No effort was made to separate the various causes of particle size broadening. Macro residual stresses were reported in directions parallel to the peened surface. I) X-RAY METHOD The Fourier coefficients were determined for the 110 and 220 X-ray profiles. They were corrected for instrumental broadening by the method of Stokes,4 using an annealed reference specimen of similar geometry presumed to be free from broadening due to small particles and distortions. The nth Fourier cosine coefficient, A,, is related to a particle size coefficient, Ap, and a distortional coefficient, ADn, by the equation:

Jan 1, 1963

By H. C. Rogers

It has been shown previously'- 3 that when a mild steel or iron is charged with hydrogen, the normally observed yield point is eliminated or considerably

Jan 1, 1960

By Adam L. Wesner, A. C. Richardson

DURING World War II the demand for electrode carbon was greater than could be met by the supply of petroleum coke available for this use. It was believed that coke made from an extremely low-ash coal might be a suitable substitute for petroleum coke. Requirements for electrode carbon to be used for the production of aluminum are that the silicon plus iron content shall be not more than 0.14 pct of the coke. However, during the period when petroleum coke was in short supply, it appeared that relaxations of the specifications might be allowed to permit 0.4 pet iron plus silicon in the coke. For this work, the specifications were that the coal should contain less than 1 pet of ash, and the combined iron and silicon content of the coal should not exceed 0.28 pct. Heavy-liquid separations made on a number of coals showed that if certain size fractions of some coals were separated at low specific gravities the resulting float products would meet the required specifications. The objective of this work was to develop a continuous, commercially feasible process for producing low-ash coal. After consideration of various processes, the method chosen was a float-and-sink separation using a solution of calcium chloride as the separating medium. Eagle Seam coal was used for the experiments. The -10 +35 mesh fraction was found to be the most promising feed for producing the low-ash [ ] content coal. A batch of 30 tons of -3/8-in. coal was screened at 10 and 35 mesh; the yield of -10 +35 mesh was 20 pct of the feed. This fraction comprised the feed for the separation tests. In spite of the fact that this portion was screened a second time at 35 mesh, the coal still contained 16 pct that was finer than 35 mesh. Three-fourths of the undersize was in the -35 +48 mesh range. A representative portion of the -10 +35 mesh fraction was subjected to batch float-and-sink separations to determine the best gravity to be used in the continuous tests to obtain a high recovery of low-ash content coal. The heavy liquid used was a mixture of carbon tetrachloride and benzene which assured complete wetting of all of the particles. As usual in batch separations, adequate time was allowed for each separation so that even the near gravity particles had ample time to separate. The separations were made at increments of 0.01 sp gr from 1.25 to 1.28 and also at 1.32 and 1.59. Each specific-gravity increment was assayed for ash content. From these data it was concluded that 1.27 sp gr was best for the continuous separation of the coal. The products from the batch separation were composited into float 1.27 and sink 1.27 sp-gr fractions; these were assayed for ash, iron, and silicon. Table I shows the results of the batch separations. The composite float 1.27 fraction contained 66.04 pct of the total weight, and had an analysis of 0.79 pet ash, 0.073 pct iron, and 0.112 pct silicon, or 0.185 pct iron and silicon combined. These data are indicative of the results possible if a perfect separation is made at 1.27 sp gr under static conditions. Inasmuch as the method under investigation is a dynamic system these results could not be obtained. It remained to be determined, however, just how close to the theoretical results the actual continuous separation would be.

Jan 1, 1952

By F. von Gemmingen, E. J. Fasiska, L. Zwell

EARLIER studies of the dependence of creep on structure1 and of the dependence of creep rupture on creep behavior2 did not include detailed discussion of the phases present in the specimens under examination. It is of interest to determine the nature and amounts of such phases present since it is well known that these are dependent on composition, heat treatment and creep conditions.3 This investigation has therefore been undertaken to identify these constituents and to determine their relative amounts. This report presents the results of this investigation and describes an improved "extraction replica" technique developed in the course of the work. The composition of the Type 316 austenitic stainless steels studied in this investigation is given in Table I. The specimens were solution treated at 2000°F for 1/2 hr and water quenched. Those specimens subjected to prestrain at room temperature Methods for extracting precipitate particles from materials for electron and X-ray diffraction analysis have been described by Fisher,4 Smith and Nutting: and Booker and coworkers.6'7 Electrolytic extraction methods have been described by Andrews and Hughes.8 The first two methods have been used at this Laboratory, but have not proved satisfactory for many problems requiring X-ray diffraction analysis. It has been difficult to remove the replicas or to avoid tearing them during removal. These difficulties are overcome by backing the replica with a water-soluble plastic such as Dupont 51-05 Elvanol (polyvinyl alcohol). The backing increases the thickness of the replica so that it can be mechanically stripped from unloosened particles without folding or tearing. This procedure eliminates the stripping of wet replicas, which usually have a low tear strength. By stripping replicas after drying, it is possible to extract partially loosened particles which otherwise would remain imbedded in the metal. The modified method is as follows: after the specimen is polished, it is etched for 60 min in modified glyceregia consisting of 30 ml glycerol, 7 ml nitric acid, and 4 ml of hydrochloric acid. The sample is then washed, air dried, and coated with a 20 pct Baker and Adamson 1611 collodion (85 pct amyl acetate by volume) film. After the collodion film is dry (about 15 min), the sample is again etched in the modified glyceregia for 50 min, washed with isopropyl alcohol (to prevent dissolving the collodion) and air dried. A very thick coat of polyvinyl alcohol (about 50 pct solution "Elvanol Dupont 51-05" in water) is poured over the sample and is permitted to dry for about 24 hr. The composite film containing the precipitates is then stripped from the specimen and floated, polyvinyl alcohol side down, in water (at about 50°C) until the polyvinyl alcohol dissolves. This usually takes about 15 min. Should any of the polyvinyl alcohol remain on the replica, it does not give a crystalline diffraction pattern and therefore does not hinder identification of the precipitates. The extraction replica, floating in water, is picked up on a glass fiber and mounted in the Debye-Scherrer camera for X-ray diffraction analysis. Concentration of the etchant, and also etching time, had to be increased for several of the samples. Fig. 1 shows two extraction replicas taken from different areas of spec. M74-37; X-ray analysis showed a strong diffraction pattern of M23C6 and a medium one of u phase. A

Jan 1, 1962

By R. J. Jackson, D. E. Williams, W. L. Larsen

The phase diagram of the Ta-Zr system is presented with a discussion of the methods used in its determination. The solidus contains a minimum at 1820°C near 25 wt pet Ta. A complete solid solution exists at elevated temperatures between tantalum and ß zirconium. This solid solution decomposes monotectoidally at 800°C and 12 wt pet Ta. The maximum solubility of tantalum in a zirconium is slightly less than 2 wt pet, and decreases with decreasing temperature. The solubility of zirconium in tantalum is 5 wt pet at the monotectoid temperature and about 2 wt pet at room temperature. THIS investigation was part of a program of research on refractory metal alloy systems having potential application in nuclear reactor technology. Preliminary prop-ess has been reported in the Ames Laboratory annual research reports.l Most of the previously reported work on the Ta-Zr alloy system consisted of partial phase diagram investigations and the determination of the mechanical properties of the zirconium-rich alloys. Anderson eta1.2 studied alloys containing up to 30 wt pet Ta as part of an investigation of several zirconium alloy systems. These investigators also determined some of the mechanical properties of the alloys at room temperature and 650°C. In a discussion of Anderson's work, Pfei13 suggested that the bright phase in the microstructures of the intermediate alloys is a tantalum-rich solid solution or an intermediate phase in a matrix of ß zirconium solid solution. Litton,4 Keeler,5 and Chubb6 determined the mechanical properties of zirconium-rich alloys at ambient and elevated temperatures. Van Thyne and McPherson7 reported the tensile properties

Jan 1, 1962

By E. L. Kamen, H. D. Kessler, M. Hansen, D. J. McPherson

The highly reactive Ti-Mo and Ti-Cb alloys were prepared and heat treated under protective conditions. Phase diagrams were established based on micrographic and X-ray diffraction analysis and detection of incipient melting. ß titanium forms a continuous series of solid solutions with both molybdenum and columbium, whereas these metals are only slightly soluble in the a titanium modification. PREVIOUS work on the Ti-Mo and Ti-Cb systems was very limited and is discussed in succeeding sections of this paper relating to the respective phase diagrams. The diagrams in the present work were determined principally by micrographic analysis, because other methods such as thermal analysis and dilatometry are not suitable, due to the low diffusion rates of these alloys in the transformation range. X-ray analysis was believed less useful than micrographic analysis because: 1—On quenching certain high titanium alloys from above their transformation range, the body-centered cubic ß phase decomposes into acicular a (hexagonal close-packed) which room temperature X-ray diffraction techniques cannot differentiate from isothermal a. 2— High temperature X-ray techniques might be used, but are difficult to apply and are subject to error because of the high reactivity of titanium with gases such as oxygen and nitrogen. Although metallo-graphic study was the basic method used, X-ray diffraction analysis was applied to a limited extent, to further substantiate the findings. The transformation ranges on the titanium side of the Ti-Cb and Ti-Mo systems were studied both with DuPont Process A (magnesium-reduced) titanium alloys and with iodide titanium alloys. The Process A metal was used chiefly to bracket the transformation range in order to reduce the number of alloys given a particular treatment for the more accurate final study with iodide titanium alloys. Experimental Procedure The analyses of the metals used in the preparation of alloys for this study are presented in Table I. Melting Practice: Early in the work, a consumable electrode, arc melting furnace was used in the preparation of the Process A Ti-base Mo and Cb alloys. This type of furnace has been described by other investigators.', ' One of the major difficulties of the consumable electrode melting process was the prep- aration of homogeneous electrodes (with the mixture of coarse titanium sponge and fine powder alloying addition) which would give homogeneous ingots. Composition gradients encountered may have been due to a tendency for powdered alloying metals to drop away from the electrode in handling. This difficulty in the preparation of homogeneous alloys was overcome by the use of a nonconsumable electrode furnace for later work. This furnace is similar to the one used by Mc-Pherson and Fontana a Ohio State University. A diagram of the nonconsumable electrode arc furnace is given elsewhere.' The source of power was a 400 amp dc welding generator. Electrode tips of tungsten (% in. in diam) were used for all columbium melts and for a limited number of molybdenum melts. Molybdenum tips were used for the majority of molybdenum alloy melts. Columbium tipped electrodes were tried, but disintegrated rapidly at currents above 300 amp. In the Process A titanium melting practice the metals were charged into the water-cooled spun copper crucible in the following forms: l—titanium: sponge (—4 + 16 mesh); 2—molybdenum: sections of 0.003 in. sheet (approximately ½ in. sq); and 3— columbium: powder compacts (? in. lumps broken from large section). After alternately evacuating and purging the furnace several times with argon or helium, the arc was struck against the metal charge,

Jan 1, 1952

By H. R. Stahl

The ore of the Southeast Missouri lead district consists essentially of galena in dolomitic limestone. The galena usually is in a very finely disseminated condition. The experience of recent years in the concentrating plants of the St. Joseph Lead Co. has shown that dry crushing carried to a point where about 90 per cent of the ore passes a 14-mesh screen liberates the larger portion of the galena, and minimizes further necessary reduction in rod or ball mills. Concentration practice has attempted to carry size reduction to a point where economic unlocking of the galena is obtained, without causing undue sliming of the very friable galena. While 60 per cent of the tonnage of the district is treated by the flotation process, only 40 per cent of the total concentrates is produced by that means, as efforts have always been made to keep the grade and tonnage of flotation feed as low as possible. The milling practice of the district for some years has recognized the generally accepted idea of better selective grinding in rod mills as compared with ball mills, with the attendant decrease in production of fines. The function of rod and ball mills in the various concentrating plants is the grinding of table middlings and coarse tailings that carry lead values too high to be discarded. The simplified flowsheet in Fig. I illustrates the place of grinding mills in the circuit. The arrangement of classi- fiers, tables and mills constitutes a closed circuit within somewhat flexible limits. In 1937 experiments were conducted in replacing the ball charge in a 6 by 4-ft. ball mill with rods 2 in. in diameter and 51 in. long. This step was taken with some hesitancy, as it was easy to picture a mass of tangled and crossed rods. However, no difficulties developed, and after a short trial period, six more ball mills were converted to rod mills. These mills are of the spur gear and pinion, belt-driven type, using in most cases a 75-hp. motor and having a 9½-in. open trunnion discharge. As ball mills, they carried a charge of 16,000 to 20,000 lb. of balls, 2 in. in original size. The feed to the mills was dewatered by dewatering wheels and introduced at 70 to 75 per cent solids, with a single scoop feeder. One change in mill design was found advisable when rods were introduced. The existing end liners had an outward flare of 3½ in. in 12 in. These were replaced by linings having vertical interior faces, in order to prevent undue end travel of the rods. This change gave an effective working length of 52¾ in. inside the mill. No alterations were made in the shell liners, which are of the smooth type, made of manganese steel 2 in. in original thickness. The rods at present in use are 51 in. long and 1¾ in. in diameter. The composition has been varied at times; at present they contain 0.70 per cent carbon and 0.70 per cent manganese. Some breakage and etching occurs as the rods become small, but this is considered preferable to using softer rods, which may kink and cause tangling of the charge. The mill charges

Jan 1, 1947

By H. R. Stahl

The ore of the Southeast Missouri lead district consists essentially of galena in dolomitic limestone. The galena usually is in a very finely disseminated condition. The experience of recent years in the concentrating plants of the St. Joseph Lead Co. has shown that dry crushing carried to a point where about 90 per cent of the ore passes a 14-mesh screen liberates the larger portion of the galena, and minimizes further necessary reduction in rod or ball mills. Concentration practice has attempted to carry size reduction to a point where economic unlocking of the galena is obtained, without causing undue sliming of the very friable galena. While 60 per cent of the tonnage of the district is treated by the flotation process, only 40 per cent of the total concentrates is produced by that means, as efforts have always been made to keep the grade and tonnage of flotation feed as low as possible. The milling practice of the district for some years has recognized the generally accepted idea of better selective grinding in rod mills as compared with ball mills, with the attendant decrease in production of fines. The function of rod and ball mills in the various concentrating plants is the grinding of table middlings and coarse tailings that carry lead values too high to be discarded. The simplified flowsheet in Fig. I illustrates the place of grinding mills in the circuit. The arrangement of classi- fiers, tables and mills constitutes a closed circuit within somewhat flexible limits. In 1937 experiments were conducted in replacing the ball charge in a 6 by 4-ft. ball mill with rods 2 in. in diameter and 51 in. long. This step was taken with some hesitancy, as it was easy to picture a mass of tangled and crossed rods. However, no difficulties developed, and after a short trial period, six more ball mills were converted to rod mills. These mills are of the spur gear and pinion, belt-driven type, using in most cases a 75-hp. motor and having a 9½-in. open trunnion discharge. As ball mills, they carried a charge of 16,000 to 20,000 lb. of balls, 2 in. in original size. The feed to the mills was dewatered by dewatering wheels and introduced at 70 to 75 per cent solids, with a single scoop feeder. One change in mill design was found advisable when rods were introduced. The existing end liners had an outward flare of 3½ in. in 12 in. These were replaced by linings having vertical interior faces, in order to prevent undue end travel of the rods. This change gave an effective working length of 52¾ in. inside the mill. No alterations were made in the shell liners, which are of the smooth type, made of manganese steel 2 in. in original thickness. The rods at present in use are 51 in. long and 1¾ in. in diameter. The composition has been varied at times; at present they contain 0.70 per cent carbon and 0.70 per cent manganese. Some breakage and etching occurs as the rods become small, but this is considered preferable to using softer rods, which may kink and cause tangling of the charge. The mill charges

Jan 1, 1947

By Strathmore R. B. Cooke, Iwao Iwasaki

RECENTLY spectrophotometry has been reported to provide a convenient technique for the rapid and reproducible determination of xanthate concentration in pulp solutions,12 and for a kinetic study of xanthate decomposition in acid solutions." Since the application of this analytical technique is feasible for those compounds showing pronounced light absorption maxima in the near ultraviolet region, it was deemed advisable to investigate the absorption spectra of some of the organic compounds that are used in flotation. It is known empirically that certain groups of atoms in an organic compound cause characteristic light absorption in the ultraviolet and near ultraviolet range, and the wavelengths and intensities of the corresponding absorption maxima are relatively independent of the nature of the remainder of the compound. The characteristic values of such groups, which are known as chromophores, are given in the literature.4,5 According to this information, many of the sulphydryl compounds are expected to show absorption maxima in the near or long wavelength ultraviolet region, whereas the saturated fatty acids and the saturated alkylamines do not. This article reports the absorption spectra of the six following types of sulphydryl compounds; mono-, di-(xanthate), and trithiocarbonates, dithiocarba-mate, dithiophosphate (aerofloat), and mercaptan. A Beckman DU quartz spectrophotometer was used to investigate the spectra in the wavelength region of 215 to 350mp. Materials: All the mono-, di-, and trithiocarbonates used in this investigation were prepared in the usual manner" from appropriate compounds obtained from Eastman Distillation Product Industries. The dithiocarbonates included the normal alkyl compounds from methyl to octyl inclusive, as well as the isopropyl, isobutyl, and isoamyl xanthates. Iodo-metric titration gave 99.7 and 99.5 pct purity for

Jan 1, 1958

W. H. Blauvelt, New York, N. Y.—One thought lias been running through my mind during the wholc of this meeting and that is that the scientific and the practical men must recognize very clearly their interdependence. The value of scientific classification of coal is going to be of the very greatest importance to the users, the practical men. Is not the scientific investigation and the great amount of work that is being done in a measure at least lost to the world? Therefore the scientific investigations and the practical needs of the users should bo brought as close together, and the work should be done as closely together, as possible; that is, the scientific man should know what the practical man needs, and the practical man should not feel that the scientific man is merely a theorist. Scientific investigation is going to have a great effeet and be of great valuc to the practical man who is trying to solve his problems. In the subject which I discussed' for instance, we must look to the scientific man to tell us why coal cokes in one way and not In another and why certain coals will do certain things and others, which appear on the surfacc to be generally similar, do not act in the same way. Need or Physical Data on Coal H. J. Rose, Pittsburgh, Pa.—There is a subject which is a sort of hobby of mine; that is, the need for what might be called critical tables of constants for coal. The chemist has big volumes giving constants, such as the density, solubility, specific heat, thermal conductivity and all other physical and chemical data that have been determined for chemical compounds. Data arc also available on many common materials, for example, the density, hardness, modulus of rupture or maximum crushing strength of swamp white oak as compared with some other wood. In fact, physical data for practically cvery hype of wood commercially produced in the world can he found. In the same way the metallurgical man has handbooks giving the properties of alloys, etc., but we havc very little tabulated information about coal. Our principal reference works are the volumes published by the U. S. Bureau of Mines on the proximatc and ultimate analysis and calorific values of coals of the United States. That is 3 pioncer work of enormous value, but we have reached the point where we need more diversified information. Mr. Fulweiler raised the question of the relative strength of the different coals and cokes. Dr. Campbell and Dr. Ashley wanted to have some information on the resistance of coal to air slacking. It was brought out in the discussion that we want to know something about the coking properties of coal. There are any number of physical tests that we need, such as the thermal conductivity of certain coals, the coefficient of expansion, or the coefficient of friction; or other constants. A smattering of such information is scattered through the literature; for instance, a research worker in Wales will report a coefficient of expansion on Wclsh coals and one in South Africa will report something else for one or two kinds of African coals, hut it is difficult to find the information that is needed on our own coals. Would it not be worth while to consider collecting reliable critical

Jan 1, 1930

By James A. McGurty, Walter J. Koshuba, Samuel G. Gordon, Gilbert E. Klein

ONE of the problems encountered in working with metals at elevated temperatures is the instability resulting from solid-solid diffusion at a -common interface. A determination of the nature and magnitude of this phenomenon is important as related to structural properties of materials potentially useful in high temperature applications. This paper is concerned with the solid state reaction between metallic molybdenum and beryllium at elevated temperatures. In the older literature,' there were no known inter-metallic compounds in the system Be-Mo, and the list of beryllium intermetallics was rather small. New compilations have been made by Smithells' and by Taylor," listing all the then known beryllium binary intermetallic compounds. In addition to these, some new phases have just been reported' in the system Zr-Be and some further compounds of the type MBe,3 have been currently described. The new compound MoBe,, which is reported upon in this paper differs considerably from the above mentioned MBe13 group, and will be discussed in detail. Diffusion Study The nature of the solid diffusion at a Mo-Be interface was determined by sealing a beryllium rod inside a molybdenum capsule and heating at a temperature of 2000°F' (1100°C) for 100 hr. The molybdenum capsule was fabricated from % in. swaged molybdenum rod obtained from the Fansteel Metallurgical Corp. The beryllium metal was obtained from Brush Beryllium Corp. as % in. cold-drawn rod. This material assayed 99.05 pct Be and contained as impurities 0.84 pct Be0 and 0.19 pct Be2C. The molybdenum capsule was % in. in OD x 2 in. long. To prepare it, a concentric hole 0.250 in. + 0.001 in. — 0.000 in. in diam was drilled and reamed in one end of a rod to a depth of 1 '/2 in. A 1 in. long beryllium rod 0.250 in. + 0.000 in. — 0.001 in. in diam was pressed into the molybdenum capsule. A molybdenum plug 0.250 in. & 0.001 in. in diam x 9/16 in. long was then used to seal the beryllium in place. The capsules were placed in a molybdenum resistance furnace and heated at 2000°F (1100°C) for 100 hr. On cooling, the specimens were cut and examined metallographically. Fig. 1 is a micrograph at X250 of a portion of the interface from a transverse section. Four phases are clearly visible, with sharp boundaries between them. Phase A is a section of the molybdenum capsule; phase B is the molybdenum-rich intermetallic composition MoBe,; phase C is the beryllium-rich compound MoBe13; phase D is a section of the beryllium rod. All phases were readily polished to a high metallic luster. The molybdenum-rich phase has a pronounced purple tinge. The beryllium-rich phase (C) is only slightly darker than the pure beryllium. In polarized reflected light, however, it shows striking birefringence between crossed Nicols. The black areas represent flaws or pores in the material. A small representative amount of powdered material from each of the phases was carefully removed under the microscope with a diamond tool. With this material, powder X-ray diffraction patterns were made for the identification of each phase. Table I lists the X-ray diffraction spacings and corresponding indexes characteristic of these intermetallic compounds. Synthesis To establish the formula of the new intermetallic compound, X-ray diffraction patterns were made from powders obtained from solidified melts of known composition. The syntheses were made by

Jan 1, 1952

By H. D. Kessler, M. Hansen, R. J. Van Thyne

The phase diagram of the titanium-rich portion of the system Ti-Cr-Fe to 70 pct Ti was established by means of isothermal sections at 900°, 800°, 750°, 700°, 650°, 600°, and 550°C, using arc-cast alloys. An isotherm at 800°C was determined for the section bounded by Ti, TiFe2, and TiCr2. Micrographic analysis was employed as the principal method of investigation, supplemented by X-ray diffraction and incipient melting studies. A ternary eutectoid, ß ? a+ TiCr2 + TiFe, occurs at approximately 8 wt pct Cr, 13 wt pct Fe, and about 540°C. AMONG the first titanium-base alloys in commercial production were the Ti-Cr-Fe alloys. For this reason, the Materials Laboratory, Wright Air Development Center, sponsored an investigation of the system. No information on the constitution of the titanium-rich corner was available. Vogel and Wenderott studied titanium-poor ternary alloys.' As part of this program, the binary systems Ti-Cr and Ti-Fe have been determined previously by the authors.' Other investigators have also studied the binary systems Ti-Cr,3-7' Ti-Fe.³,8-10 Both of the binary systems are characterized by the eutectoid decomposition of the ß phase. Most of the effort of the present work has been concentrated on the titanium-rich corner with compositions of less than 30 pct total chromium and iron content. The determination of isothermal sections was the experimental approach used to obtain the ternary phase diagram. Vertical sections were used to check the consistency of the isothermal sections. While this investigation was in progress, a study of the Ti-Mo-Cr system at Armour Research Foundation disclosed the existence of a high temperature modification of TiCr2 above 1300 °C.11 This allotrope has a hexagonal structure of the MgZn2 type, iso-morphous with TiFe2, whereas the low temperature modification of TiCr2 is cubic," of the MgCu2 type. The existence of allotropy in TiCr2 of course means a more complicated set of phase relationships in this general region than if the phase were monomorphic, as was first assumed. Additional studies were made late in the investigation in order to clarify the part that the hexagonal TiCr2 phase plays in the ternary phase relationships. These will be discussed in a separate section. Because they are of greatest practical significance, the phase relationships in the titanium-rich corner will be presented first, omitting the equilibria involving the hexagonal modification of TiCr2 in an effort to simplify the presentation somewhat. Experimental Procedure Materials: The titanium used in the preparation of the alloys was iodide crystal bar (99.9 pct pure) produced by the New Jersey Zinc Co. High purity chromium and iron were obtained from the National Research Corp. Table I gives the analyses of these materials. Melting Practice: Over 100 alloy ingots weighing 10 to 20 g were melted in a nonconsumable electrode arc-melting furnace. As the techniques are identical to those reported previously,12,13 they will not be detailed here. The ingots were melted in the cavity of a copper melting block insert under a slight positive pressure of helium. No measurable hardness

Jan 1, 1954

By H. B. Aaron

DIFFRACTION micrography provides a useful tool for studying complex strain fields. Newkirk1 observed an X-ray diffraction effect due to strain interactions at the intersection of slip lines in LiF and attributed this effect to a reduction of primary extinction due to strain-gradients. It is the object of the current study to correlate the observations and rationalize the appearance of the strain fields around intersecting slip planes in x-ray extinction contrast studies by a semiempirical method. Fig. 1 shows typical strain patterns observed by Newkirk on (200) reflections in LiF using chromium radiation and a variation of the Berg-Barrett (B-B) technique. In other reflections (e.g., {220}) the strain patterns are absent. If one defines a vector 3 along the striations from the more to the less dense portion, and a vector v in the direction of the X-ray beam parallel to the reflecting plane, such that both 3 and v lie in the reflecting plane of the crystal, Fig. 1, then the positions of the striations on (200) reflections appear to be confined such that where is the angle between v and 3, Fig. 1. It will be seen later that 3 is the projection of Sb on the reflecting planes. In some instances the strain effects are observed only above the slip plane, Fig. l(C), in others only below, Fig. l(D). Where the strains appear to be both above and below the slip line, Fig. l(E), one sees that there are actually two slip lines present, Fig. 1(F) and (G). Furthermore, the strain patterns are observed in the vicinity of the intersection of emergent edge dislocations (diagonal lines on the micrograph) with emergent screw dislocations (horizontal lines on the micrograph), e.g., Fig. l(HJ) and (MN), but not in the vicinity of the intersection of two emergent edge dislocation arrays, Fig. l(HJ) and (KL). However, in the latter case the contrast of the dislocation array itself is reduced along (KL) and increased along (HJ). Line (AB) in Fig. 1 is the edge of the crystal, and the material to the left of (AB) is the side of the sample. Any empirical correlation will have to include most, if not all of the aforementioned observations. Lang2 and Newkirk1 determined that the condition for contrast is given by g-b#0 [2] where b is the Burgers' vector and g the diffraction vector (normal to the reflecting planes). If one assumes that the direction of the observed strain fields is given by the vector sum of the slip vectors (Sb1) of the intersecting slip planes, then Eq. [2] may be generalized to g-S#0 [3]

Jan 1, 1963

By B. B. Bucky

THIS investigation was carried on by means of models and the applica-tion of the principles of similitude to determine the effects of props, props and cribs and sand filling in longwall mining. The geologic structure and rate of face retreat were kept constant and the only change introduced was in the method of support. It is not felt necessary to repeat a description of apparatus, or to explain the fact that a scalar model made in all parts of the same material as the prototype will behave similarly to the prototype when rotated at speeds such that the centrifugal force is as many times the gravitational force as the prototype dimension is a similar linear model dimensions. The reader is referred to earlier papers1,2 for further information regarding these statements. All models were made of sandstone and were as in Fig. 6. They are composed of a 3/16-in. ore body bed A, overlain by a 3/16-in- bed B, a 3/8-in, bed C and two 1/8 -in. beds D and E. The model was rotated at ±2350 r.p.m. equivalent to a model ratio of 1268. It was worked back 1/4 in. at a time before being replaced in the centrifuge and again rotated. Table 1 gives model and prototype dimensions occurring in this discussion, the prototype dimensions being 1268 times the model dimensions. Figs. 1, 2, 3 and 4 were taken while the model was rotating at 2350 r.p.m. One was taken for each face retreat of 26.4 ft., but for obvious ,reasons all are not presented. Fig. 1 (A-E) shows the behavior of this type of structure with face retreats of 26.4 ft, and no artificial support. Fig. 2(A-E) shows the behavior of this type of structure where breaker and face props were used. The props were exceptionally strong, being of steel 1/8 in. square in cross section, and capped with 1/16 in. ± of soft wood and paper, to allow for roof deflection. The face props were

Jan 1, 1939

By A. Long, A. Silverman, J. L. Kulp

Garth Crosby has written an excellent geologic description of the deposits surrounding the Gem stocks in the Coeur d'Alene district. The ore deposits in the area of the Gem stocks may hold the key to the age and mineralization history of the entire Coeur d'Alene district. A recent isotopic study10 of the Coeur d'Alene district in this laboratory illustrates that a classical geologic interpretation of these deposits, with its implications for the whole district, may lead to erroneous conclusions. For this reason it seems pertinent to submit a summary of these results and an interpretation of the mineralizing history of the Coeur d'Alene districts. Pitchblende from the Sunshine mine has been dated as 1100-1200 million years (m.y.) by Kerr and Kulp,11 and Eckelmann and Kulp.12 This pitchblende is known to predate the major sulphide introduction in the Sunshine mine, but it clearly follows the metamorphism and folding of the Belt Series. Recently, Goldich (personal communication) dated sericite from the Belt rocks as 1200 m.y. by the potassium-argon method. This date establishes a minimum Belt age if the sericite is of metamorphic origin and a maximum age if detrital. The Belt Series, therefore, is not latest Precambrian. Lead isotope ratios of galenas have been measured and model ages calculated by Bate, et all3 for the Sunshine mine, Farquhar and Cummingl4 or the Bunker Hill and Sullivan mine, and Cannonl6,18 for a few other deposits in the district. Galenas from similar deposits in Southern British Columbia have been measured by Bate, et al,23 Farquhar and Gumming,11 and Wanless and Leech." The new work in this laboratory includes leads from ten widely scattered mines north and south of the Osburn fault, and through a vertical distance of over 5000 ft (Star mine). Included in this group are the Hercules, Sunset, and Mountain Goat mines, which are adjacent to the Gem stocks. In addition, galenas from stringers which cut the Gem stocks in the Success and Sunrise mines and the Hercules hanging wall dike in the lower western portion of the Hercules mine, were included in the study. All of the above leads, except one, give model ages of 1300-1400 m.y. for the time of segregation from the parent material. The concordance of the common lead and U-Pb ages, the great horizontal and vertical uniformity of the lead ratios, the sulphur ratios of two Sunshine mine galenas and three galenas from the Edith, Page, and Hercules mines indicating average crustal sulphur, and the U23/Pb204 ratio inferred for the original lead environment, indicate that the entire mineralization of the Coeur d'Alene-British Columbia base metal belt was derived from a deep source and emplaced in the Precambrian. One sample of galena from sulphide stringers cutting the North Gem stock at the Sunrise Prospect mine gave a modern (i.e., Tertiary) lead ratio. This mine is located at the northern tip of the stock. The presence of modern lead suggests mobilization of some rock lead during the intrusion of the Gem stocks and their outliers. Larsen et al.l8 have dated the Gem stocks as Tertiary by the lead alpha method. If Coeur d'Alene mineralization was genetically related to Tertiary magma formation and intrusion

Jan 1, 1961

By I. N. Knapp

Introduction.—The spccial object of these notes is to describe the mixing, testing, and use of mud-ladened water for rotary drilling in such a way as to make them helpful to the driller, the operator, or the engineer in solving his own special drilling problems. The structures, apparatus and tools used are indicated in a general way. No attempt is made to describe the art of rotary drilling; only such descriptions as are necessary to make plain the use of mud are given. The information is the result of actual experience in drilling in Coastal Plain formations. The materials encountered in the wells drilled were unconsolidated sands, gravels, and clays, in which thin layers of sandstones, shell conglomerates, and shales began to appear at about 1,200 ft, in depth, although one well was drilled to 3,018 ft. without encountering any cemented or indurated materials. Unusual Conditions.—-The general surface of the ground where the drilling was done being hardly a foot above mean tide, and the daily tidal variation being about 15 in., it was found necessary to plank over the sod surface with 3-in. plank to work from. A 30 by 30 ft. planked area was sufficient to carry the derrick with equipment and 2,500 ft. of 4-in. drill pipe stacked in it. The derrick was set up 3 ft. on cribbed blocking arranged to spread the load over the planking. The engine, bailers, and pipe yard were also carried on 3-in. planking. Drilling 0utfit.—This consisted of a derrick, 20 by 20 ft. and 84 ft. high, two 35-h.p., "oil country" boilers, one double 8 1/4 by 10 in. reversible engine, two 10 by 6 by 12 in. duplex mud pumps, one 15-in. rotary, "hoisting works" with chain drive, hoisting block with line, crown block with pulleys, rotary jetting swivels, hose, complement of tools, pipes and connections, and a mud mixer, with engine. Hydraulic Rotary Drilling Method.—This method of drilling is an adaptation of Fauvelle'sl invention made in France in 1833 for drilling

Jan 1, 1915

By L. Bombardieri, H. F. Mills

Iron King mine, producing gold-silver-lead-zinc-ore, is 10 miles east of Prescott, Ariz. At present the 1806 level is being developed. The echelon pat tern of ore deposit continues at depth but is less pronounced, and the orebody is now more or less continuous over 2600 ft of strike length, with widths 5 ft to as high as 26 ft where overlapping of lenses occurs in one section of the mine. Better continuity of ore at depth has encouraged systematic mining and improved plant facilities to offset higher operating costs. With favorable persistence of ore at depth, the three-compartment No. 6 hoisting shaft appeared inadequate to handle increased tonnage from greater depths, and in 1952, a four-compartment steel and concrete shaft was started. This is now at a depth of 1906 ft, and shaft pockets and loading cartridges are being installed on the 1806 level. Ore from the new shaft, hoisted in 5 ½ -ton Jeto bottom dump skips, is dumped into a 500-ton shaft bin, from which it is fed to a 16x30-in. gyratory crusher and conveyed 415 ft through an undersurface concrete gallery to the secondary crusher and conveying system supplying the 900-ton mill. Lead, zinc, and pyrite concentrates are floated, and the flotation tailings are cyanided after desliming. Waste from the new shaft is dumped into a 250-ton surge bin, fed from this bin to a 24-in. conveyor, and discharged into the glory hole above the block cave. The new shaft is served by a double-drum 400-hp hoist used for ore and waste; the No. 6 shaft conveys men and material.

Jul 1, 1956