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By L. F. Reinartz

ANOTHER year has rolled by. We are twelve months further away from the start of the depression and. therefore that much nearer to recovery. The accumulated needs and wants 'of our lame, virile population are ready to burst their bonds as soon as confidence returns and credit is stabilized. The steel industry has been harassed by uncertainty of the Government's attitude toward organized labor's de¬mands, and irregularity in volume of production. Steel labor, if left to its own devices, would in most instances, march shoulder to shoulder with the management of steel plants in their effort to pull the industry nut of the ?red.? Cooperation between management and men has improved considerably during; the year.

Jan 1, 1935

By AIME AIME

AMONG the recent mining and metallurgical developments in England great interest has been shown in the development of an iron-ore field covering 26,0.00 acres in Northamptonshire, containing 500,¬000,000 long tons of ore; and the erection at Corby, by Stewarts & Lloyds, of a modern basic bessemer steel plant and tube works. The entire project was planned to cost about £3,300,000. Many improvements have been made in the varied equipment that is being installed, some of which has set mew records for massiveness. There is, for instance, a new roll crusher, which has been manufactured by Hadfields, Limited, of Sheffield, the largest ever built in England, and weighing 130 tons. This machine, shown in Fig. 1, as erected at the Hadfields shops, is primarily designed to take blocks of iron ore as they come from the steam shovel. The maximum size is 54 by 48 by 36 in., hut occasional pieces slightly larger than this may be accommodated. The capacity is upwards of 500 tons per hour, the product passing to a secon-

Jan 1, 1934

By E. S. Moore

THE Kolar gold field has been for a long time the most important gold-producing area of India. It is situated in the State of Mysore, southern India, and not far from the City of Bangalore. The productive field is about 3 miles long and in it a gold-bearing quartz vein varying in width from 1 in. to over 10 ft. is worked. The vein carries high values to great depths and many of the mines have paid large dividends. GEOLOGICAL FORMATIONS IN THE MOLAR REGION The rocks of the Molar region are pre-Cambrian in age and bear a close resemblance to some of the pre-Cambrian formations of America. The oldest rocks seen are basic lavas, now mostly altered to hornblende-schists, with which is associated some banded iron-formation; these rocks are similar to the Keewatin schists and iron-formation in the Lake Superior region. The schist is cut by the gold-bearing quartz vein. In certain parts of the area there is also a conglomerate containing pebbles of granite, jasper,, and schist. The matrix resembles a horn-blende-schist and is intruded by small granite dikes, which in some cases have been pinched off by squeezing of the rock. This has led Dr. W. H. Smeeth, Chief Inspector of Mines of Mysore, to whom the writer is greatly indebted for information regarding this area and for his hospi-tality while visiting the field, to regard this conglomerate as a breccia due to crushing of granite dikes in the schist. Dr. J. W. Evans has regarded the conglomerate as probably a squeezed glacial boulder clay. From analogy with pre-Cambrian conglomerates in America, the writer regards it as a metamorphosed rock similar to our basal Huronian conglomerate. However, the main bearing which it has upon the problem under discussion is the apparent fact that it is younger than the schist

Jan 3, 1918

By H. R. Cooper, T. S. Mika

T. S. Mika (Department of Mineral Technology, University of California, Berkeley, Calif.) - Dr. Cooper's attempt to establish a correlation between process behavior and operational variables on the basis of a statistical analysis after imposing a reasonable process model is a very commendable improvement on the use of standard regression techniques. However, it must be recognized that the imposition of a model has the potential of yielding a poorer representation if its basic assumptions or mathematical formulation are invalid. It appears that at least two aspects of his treatment require some comment. First, the limitations on the kinetic law where xta represents a hypothetical terminal floatable solids concentration (cf. Bushell1), should be mentioned. Most current investigations2-9 appear to utilize the concept of a distribution of rate constants rather than a single unique value, k, to describe flotation kinetics. A distributed rate constant is certainly a more physically meaningful concept than that of a terminal concentration. The study of Jowett and safvi10 strongly indicates that xta is merely an empirical parameter, whose actual behavior does not correspond to that expected from a true terminal concentration. Rather than being a strictly mineralogical variable, as Dr. Cooper's treatment implies, it apparently represents the hydromechanical nature of the test cell as well as the flotation chemistry. The extension of batch cell kinetic results to full-scale continuous cell operation is a suspect procedure if the effect of such nonmineralogical influences on x,, remain unevaluated. There is evidence that introduction of a terminal concentration is necessitated by the inherent errors which arise in batch testing and are eliminated by continuous testing methods.' Possible lack of validity of the author's use of Eq. 1 is indicated by two unexpected results of the statistical analysis of his batch data. The first is the apparent corroboration of the assumption that the rate constant, k, is independent of particle size, i.e., of changes in the size distribution of floatable material. This assumption directly contradicts numerous results 2,4,11-l8 for cases where first order kinetics prevailed and ignores the phenomenological basis for the analysis of flotation in terms of a distribution of k's. It must be recognized that, if the rate constant is size dependent, the lumped over-all k would be time dependent; Eq. 1 would then no longer be valid. Cooper's x,, is determined by batch flotation of a distribution of sizes for an arbitrary period of time. If the size dependence of k is artificially suppressed, x,, will become a function of the experimental flotation time used in its determination. Upon reviewing the rather extensive literature concerning batch flotation kinetics, there appear to be few instances where constant k and x,, adequately adsorb variations in floatability due to particle size. The second surprising result is the low values of the distribution modulus, n, determined. Contrary to Cooper's assertion, most batch grinding (ball or rod mill) products yield values of n > 0.6, which increase as the material becomes harder.'' It is likely that the values of n = 0.25 and n = 0.42 for Trials 1 and 2, respectively, are completely unreasonable, and even the value n = 0.54 obtained for Trial 3 is unexpectedly low. Possibly, this indicates inherent flaws in the three trial models considered, in particular the assumed particle size independence of the rate constant, k. The above does not necessitate that Eq. 1 (and the terminal concentration concept) is invalid; it could constitute a good first approximation. However, the qualitative arguments used by Dr. Cooper in its justification are somewhat frail and require verification, particularly since much of the flotation kinetics literature is in opposition. Apparently, no effort was made to test these hypotheses on the actual data; in fact, since they pertain to a single batch test time, his data cannot be utilized to evaluate the kinetics of flotation. To evolve a control algorithm on the basis of this infirm foundation seems a questionable procedure. Another difficulty in his analysis arises in consideration of the froth concentrating process. As Bushel1 ' notes, for Eq. 1 to be valid it is necessary that the rate of recycle from the froth be directly proportional (independent of particle size) to the rate of flotation transport from the pulp to the froth, a restrictive condition." Harris suggests that it is more realistic to assume that depletion occurs in proportion to the amount of floatable material in the pertinent froth phase volume (treating that volume as perfectly mixed).12,21,22 The physical implications of

Jan 1, 1968

By Earle E. Schumacher, Alexander G. Souden

IN the field of physical metallurgy it is becoming increasingly difficult to keep abreast of the recent develop¬ments since the diversity of investigations is so great and the literature so voluminous. The purpose of this review is to present the more important advances in the nonferrous field during the past few years, the topics discussed being classified broadly as fundamental and practical. The former includes those studies that have done most toward developing the basic science of metals and alloys, and the latter includes technical developments and applications. With the rapid growth of the metal

Jan 1, 1938

By S. W. Ihle, L. J. Warren

A sample of garnet from the scheelite ore body on King Island, Tasmania, Australia, was upgraded and ground to produce an ultrafine portion suitable for micro-electrophoresis. X-ray and chemical analysis identified the garnet as andradite with some admixed grossular. At neutral pH the garnet particles were negatively charged, their zeta potential becoming rapidly more negative with increasing pH. An iso-electric point was found at pH 3.5. The effects on the zeta-potential of various electrolytes, hydrolyzable metal ions, and flotation collectors were also studied.

Jan 1, 1976

By C. N. J. Wagner, E. N. Aqua

The bee alloys of the terminal solid solution of rhenium in niobium were investigated by X-ray diffraclion methods. The analysis of the broadening of the powder pattern peaks from the niobium-rich alloys, cold-worked by filing, showed evidence for faulting on (211) planes. The alloys with larger rhenium concentrations were brittle, and fractured when filed. The analysis of the shapes of the diffraction profiles from powders produced by hammering with steel plates) of these brittle alloys indicated that the broadening was due predominantly to platelets bounded by clibe planes. This result was consistent with the Laue patterns from single-cleazlage facets which showed evidence for clearage fracture on {100} planes. The influence of faulting on the mechanical properties of face-centered cubic (fcc) metals and alloys, i.e., how faulting affects the various dislocation configurations in fcc metals, is well-known.' The important question is whether or not faulting occurs in body-centered cubic (bcc) metals and alloys, and, furthermore, if faulting does occur, to what extent it affects the mechanical properties. Theoretical calculations indicate that the stacking-fault energy is rather high in most bcc metals.2 The results of sev-eral studies using transmission electron microscopy have indicated that faults are present in well-annealed and lightly deformed bcc metals and alloys, such as tungsten,3 vanadium,4 and Mo-Re alloys.5,6 These faults, as have been observed, may be stabilized by the presence of interstitial (C,N,O) atom segregation to the extended dislocations. In addition, there is considerable X-ray diffraction evidence for faulting in bee metals,7-8 using the same techniques that were successful for the study of faulting in fee metals and alloys.7 This X-ray diffraction method is currently the only technique applicable for the investigation of faulting in metals with high stacking fault energies, i.e., when severe amounts of deformation are required to produce sufficient amounts of faulting to be detectable by X-rays. The thinned films of heavily deformed metals will become opaque in the electron microscope due to the high dislocation densities present. In a previous investigation of faulting8 in bee metals of group Vb and VIb, the authors observed that niobium was ductile when filed at room temperature, and showed the highest density of faults on the (112) family of planes. A niobium-base alloy system was therefore chosen to study the effect of alloying on the occurrence of faults in a bcc alloy. There is a large range of terminal solid solubility of rhenium in the alloys of the bee refractory metals. All of the Group VIb-rhenium alloys, i.e., Cr-Re, Mo-Re, and W-Re, exhibit solid solution hardening without loss of ductility.9 In fact, the ductility reaches a maximum for alloys with compositions near to the limits of solubility. This enhanced ductility has been attributed to the lowering of the stacking-fault energy in the alloy; i.e., the increased amounts of twinning provide an additional mode of deformation, resulting in the observed high ductility.' Because of this demonstrated effect of rhenium in bee alloys, it was decided to study a series of alloys of Nb-Re. Using the same X-ray diffraction methods as described in the previous investigation,' one is able to identify the possible causes of broadening of the powder pattern peaks, e.q., particle size, microstrains, stacking faults, and/or twin faults. The separation of these various contributions to the measured peak shape is accomplished by the Warren-Averbach analysis.7 I) EXPERIMENTAL PROCEDURE A series of seven bee solid solution alloys containing from 2.5 to 21.5 at. pct Re (remainder niobium) were prepared at the General Electric Research Laboratory. Buttons, weighing 25 g, were alloyed from electron-beam-melted niobium chips and random rhenium sheet by arc melting in a water-cooled copper crucible, under an argon atmosphere. The buttons were inverted and completely remelted to promote homogenization. The nominal alloy compositions are listed in Table I. Samples of the cold-worked alloys were obtained by filing to produce a powder for the X-ray study. Alloys too brittle to be filed were hammered with steel plates. The resultant filings or brittle impactings were screened through 150-mesh classifiers and compacted to the required shape for the diffractometer holder. The X-ray diffraction peaks were automatically recorded by fixed time counting at uniform 28 intervals, or by continuous registration with a ratemeter. In all cases, the (110)-(220) and (200)-(400) pairs of peaks and the (211), (310), (222), and (321) reflections were measured on a GE-XRD5 diffractometer using CuKa radiation with nickel filter or MoKct radiation and a LiF monochromator in the diffracted beam. The first part of the data reduction, completed with the aid of a series of programmed computations,10 was the analytical resolution of the Kol component of the diffraction profile. Subsequent computations were then made with reference only to the resolved Kol peak shape. These included the measurement of the

Jan 1, 1967

By F. Keller, A. H. Geisler

Some of the important changes that take place in the structure of aluminum alloys are largely submicroscopic in character. This is especially true of the changes that accompany age-hardening and recrystallization. Although improved metallographic practices have been helpful in indicating some of these changes indirectly, results are limited by the resolving power of optical microscope lenses. The electron microscope, however, provides a new and important means for investigating the fine structure of metals in a range not possible heretofore. It is anticipated that this microscope will yield new and useful information to metallurgists when suitable techniques are developed to utilize its very high resolving power. Several unique methods have been devised to permit the examination of the structure of opaque samples by the electron microscope. These are all based on the principle of producing a very thin film that represents the prepared surface of the opaque metal sample, which can be examined in the transmission microscope; however, the available methods fall into three categories, depending on the manner in which the film is obtained. With the oxide-film method developed by Mahl3-17 a very thin surface layer of the metallographic sample is converted into oxide by a thermal, chemical or anodic treatment. After removal from the metal sample by one of the special techniques described by Evans,19 this oxide film is examined in the electron microscope, and is found to portray the structure of the original metal surface. Films formed on aluminum,8,17 nickel,7 iron 3,8,9 and a nickel-beryllium alloy" by heating; films formed on iron 8.9 by chemical action; and films formed on aluminum3-16 by anodic oxidation, have been examined. The other two are more recent methods developed principally in this country; they consist in making the thin film in the form of a mold or replica of the surface contour of an etched sample. With the negative replica method the thin film is made directly on the sample; with the positive replica method it is made on a negative reproduction of the sample. With both methods, variations in the contour of the metal sample, caused mainly by etching, produce variations in the thickness of the surface replica. Because of the direct dependence of the amount of scattering of the illuminating electrons upon the thickness of the film penetrated, only the variations in thickness of the replica are responsible for tones in the electron image. Negative replicas are made by forming a thin film of some suitable material directly on the polished and etched metal sample, and derive their name from the fact that after removal from the sample they have the high and low points in the sample reversed, as shown in Fig. I. Nega-

Jan 1, 1944

By Michael Hoch, Walter C. Wyder

The isothermul section of the Nb-Ti-Zr-O system at 1500°C was investigated using X-ray dzffraction and metallographic techniques. UP to 66.7 at. pct 0, the system contains nine four-phase regions. Tsopleths at 10, 20, 30, 40, 50, and 55 at. pct 0 weye constructed. The purpose of this investigation was to determine the general shape of the quaternary equilibrium phase diagram of niobium, titanium, zirconium, and oxygen at 1500°C. The system was truncated at 66.7 at. pct. O., PREVIOUS INVESTIGATIONS The Ti-Zr-O system was investigated in this laboratory.' The binary systems of interest have been compiled and discussed by anssen2 and Levin, McMurdie, and Ha11. Elliott4 has determined the Nb-O system by metallographic and X-ray diffraction techniques. He shows the existence of three oxides, namely NbO, NbO2, and Nb2O5. At 1500°C the solubility of oxygen in niobium is about 4 at. pct. No solid solubility region is shown for either NbO or NbO2. EQUIPMENT The same equipment as that for the study of the Ti-Zr-O system was used. The X-ray diffraction patterns were analyzed with the help of the ASTM card set5 and NBS circulars.6 MATERIALS The niobium powder (99 pct pure), the titanium powder (99.6 pct pure), the niobium pentoxide, and the zirconium dioxide used in this study were purchased from the Fairmount Chemical Co., Newark, N.J. The zirconium powder (99.4 pct pure) was obtained from the Charles Hardy Co., Inc., N.Y. Reagent-grade titanium dioxide was purchased from the Matheson Co., Inc., Norwood, Ohio. The oxides were dried in air at 700°C for 24 hr before use. Though the materials used were not "hyper-pure," the impurities present do not affect the results (lattice parameters, phase boundaries), within the experimental accuracy. PROCEDURE Samples of the desired compositions were made up, in mole pct, from the materials listed above. In some cases the intermediate binary compounds, such as NbO and TiZrO4 were prepared beforehand and used in the preparation of the samples. This technique enabled equilibrium to be reached from two sides. The components of each sample were mechanically mixed in a mortar and pestle and pressed into 3/16-in. diam pellets. The pressures used in compacting were of the order of 50 to 100 x 103 psi. Sintering was accomplished by heating the samples in a tungsten crucible (3/4-in. high, %-in. diam, 1/8-in. wall, lid with XB-in. hole). The pellets were separated from each other and from the crucible by means of small spiral coils of tungsten wire placed between the stacked pellets and on the bottom of the crucible. The sintering time was from 4 to 12 hr at 1500°C under a vacuum of 6 x 101-5 to 1 x 10-6 mm of Hg. All samples were reground after the first or second heating repressed, and reheated. In most cases: equilibrium was obtained after the first heating, as the X-ray diffraction pictures after each heating remained unchanged. Quenching of the samples from 1500°C was at first only possible by allowing the crucible and its contents to lose heat by radiation. The temperature dropped from 1500° to 900°c in approximately 1 1/2 min, which was considered adequate when compared to the times used by other investigators to reach equilibrium in the temperature range of 1000°c and lower. Later, a new technique for faster quenching of the samples was cleveloped. This technique involved the removal of the samples from the crucible, whereupon they were quenched by coming in contact with the water-cooled copper base of the furnace. This manipulation was performed without breaking the vacuum. The sample pellets were placed on a tungsten wire rack inside the crucible. The wire rack passed through the hole in the crucible lid, where it was connected to a small nonmagnetic chain. The chain was fed to the side of the furnace by means of a brass rack which fitted between the body and lid of the furnace. Suspended at the end of the chain, near the furnace wall, were three magnetic washers. With the use of a strong

Jan 1, 1962

By George R. Cowan

A number of studies hare been reported of the effects produced in metals subjected to deformation by shock waves with maximum pressures ranging from tens to hundreds of kilobars. On the basis of the equations for the flow of mass, momentum, and energy through a stationary shock front, the macroscopic stress-strain curve for the resulting shock deformation can be calculated within narrow limits from the experimentally determined Hugoniol curve. In relatively weak shocks which are preceded by an elastic wave, the stress rises above the clastic limit only as plastic deformation proceeds cold thus the shock has a long toe. In strong shocks that override the elastic wave a high stress is applied without prior plastic deformation. A more important effect of increasing the shock pressure is the generation of shear stresses, called supercrilical shear stresses, that exceed the strength of the perfect lattice. A change in the mechanism of deformation is expected to result from the onset of supercritical shear. The shock disordering of ordered Cu3Au in strong shocks appears to be an example of such a change. It is suggested that the formation of fine twins in copper and nickel and the formation of structures which enable visible twins to be formed in the rarefaction ware, observed in copper and presumably in disordered Cu3 Au, are related to the occurrence of supercritical shear in shock dcformation. In recent years several studies1,2 have been made of the changes in structural and mechanical properties of metals produced by the passage through the metals of strong shock-compression waves ranging from about 50 to 800 kbar pressure. Recent work involving dynamic measurements of the shock compression "Hugoniot" curves 3-8 of many metals has developed techniques and provided data required to obtain the shock pressure and the (transient! plastic deformation produced in the shock-conlpression experirnents.9 Shock deformation has been found to be much more effective than slow deformation in changing the mechanical properties of metals, when the two are compared on the basis of equal plasti strain, Holtzman and Cowan9 made quantitative estimates of the shearing stress occurring in a shock front in a metal by assuming that the shearing stress is similar to that occurring in a shock front in a viscous, heat-conducting fluid, with the addition of a yield stress. Taylor's solution9 for a weak shock was used to estimate pairs of values of shearing stress and thickness of the shock front obtained by assumed choices of the ratio of effective kinetic viscosity to thermal diffusivity. It was noted from these values that. unless the shock front is extremely thin. heat conduction has slight effect, and the shearing stress is nearly independent of the mechanism of deformation. This mechanism does, however, determine the thickness of the shock front and the rate of strain. Furthermore, since the maximum possible shearing stress occurring in shocks of moderate strength does not greatly exceed the shear stress occurring in conventional slow deformation, the mechanism of deformation is not expected to be qualitatively different. The greater effectiveness of shock deformation in changing the mechanical properties of metals can be attributed partly to the fact that dislocations, when driven by near-conventional stresses, cannot keep up with the shock front, thus necessitating a higher dislocation density than required for an equivalent slow strain. The fast uni-axial strain occurring in the thin shock front would also be expected to cause a larger number of dislocation intersections to occur. In the upper range of shock pressures that have been studied the estimated values of the shearing stress exceeded the estimated shear strength of a perfect crystal. Under these circumstances it is reasonable to expect that the mechanism of deformation might be considerably different from that involved in slow deformation. Except for the observation by smith1 of twins in shocked copper, the effects of shock waves on metals did not show any obvious or large changes in properties that would indicate the onset of a change in the mechanism of deformation. The recent investigation of the effect of shock waves on ordered and disordered specimens of Cu3Au by Beardmore, Holtzman, and ever" showed a spectacular decrease in the amount of long-range order retained by initially ordered Cu3Au when the shock pressure was raised from 290 to 370 kbar. Since Dr. Holtzman and I suspected that this behavior probably was due to the onset of a shearing stress in the shock front in Cu3Au which exceeded the limiting shear strength of the perfect crystal. it was considered appropriate to examine directly the shock-front equations for a solid. and to obtain a sound estimate of the shearing stress occurring in the front using equation of state data obtained from shock studies. In this paper an estimate is made of the

Jan 1, 1965

By Lucius W. Mayer

WHILE the mind of the financier does not normally run along channels similar to those of his technical adviser, engineers, because of their exactness, are ever more called upon to manage affairs where financial matters are involved. It is, true, not a relatively large number have thus far functioned in this capacity. It is also true that the essentially financial mind could not serve in a responsible engineering position; for to be a successful engineer one requires precise thinking, making due allowance for factors of safety. To be a financier seems to require less aptitude for exact thinking than of enthusiasm and confidence in capitalizing prospective possibilities. Both require imagination, the engineer being, more conscious of the limitations of natural conditions. It is to be regretted that the engineer' stands so far aloof from financial matters. Many consider them- selves successful, as did Steinmetz, as long as their reward is the consciousness that they are giving supreme service to mankind. They are 'generally happy in their work and, like our honored brothers who are teachers, gain their greatest satisfaction, not in the amount of their remuneration so much as in the service rendered society and in the excellence of results achieved. Indeed, these sentiments bespeak character and command respect.

Jan 1, 1924

By R. J. Teitel

The Pb-U system has been investigated by X-ray, thermal, and microscopic analyses. Two pyrophoric intermetallic compounds were found; UPb3 and UPb. The crystallographic structure of UPb3 is reported. A phase diagram was drawn for the system showing three eutectic and one syntectic reaction. AS a result of the interest in uranium metallurgy, the Pb-U system has been investigated. Practically no quantitative data appears in the literature concerning this system. Chips were machined from bars of high-purity uranium obtained from Ames Laboratory and the lead was 99.9 pct high-purity grade from Bel-mont Smelting & Refining Co. The chips were pickled in a dilute solution of nitric acid, washed in water and then alcohol, and dried prior to use for alloy preparation. The lead was simply sheared from the pig with no chemical treatment. Lead and uranium were placed in graphite crucibles and loaded into an induction furnace. In order to insure good alloy formation, the lead was loaded above the uranium to wash the uranium chips into the melt. After the charge was held at the desired preparation temperature for 15 to 30 min, it was allowed to cool in the crucible. The entire melting operation was accomplished in an atmosphere of helium (double charcoal refined grade with no further treatment). The procedure was to outgas the furnace by first evacuating it to 10-% m Hg, admitting helium to 8 psi gage and sealing the furnace off. An optical pyrometer focused on the charge through a hole in the crucible cover was employed for thermal measurements. Usually a 50° to 70°C correction had to be added to the instrument value. The most suitable alloy preparation temperature range was found between 1220° and 1280°C. The reason for this is explained by the phase diagram, Fig. 7. Above this temperature range two liquids separate preventing alloy formation upon cooling at a reasonable rate. On the other hand, below this range the uranium was coated with a layer of both compounds and the rate of reaction was diminished by diffusion processes. The fastest reaction rate occurred in this narrow range of temperature because only UPb coats the uranium and it evidently does not protect the uranium as well as UPb,. Apparatus and Procedures The development of apparatus and techniques was determined by the peculiar properties of the alloys. All the alloys were pyrophoric, and, consequently, the alloys had to be protected from oxidation by handling them in a dry box or inert atmosphere furnaces. Other operations performed outside of this equipment had to be done as quickly as possible. Thermal analyses were conducted in a furnace and arrangement similar to that described by the author.' Graphite crucibles having a thermocouple well in the bottom were used to contain the prepared alloy, while a helium atmosphere protected the melt from oxidation. The furnace was outgassed by pumping a 10-3 mm Hg vacuum until the furnace had been heated to 400°C. Then helium was admitted and the furnace sealed under 8 psi gage pressure. Chromel-alumel thermocouples were used for thermal analysis and the accuracy of thermal measurements was judged to be k 5°C. At first, an attempt was made to use platinum-platinum-rhodium thermocouples, but evidently lead vapors attack it at high temperatures forming low melting alloys. These lead vapors had direct access to the thermocouple because the graphite crucible was porous. A differential temperature control was used to regulate thermal analyses. The thermal gradient across an alundum tube placed between the windings and the crucible was maintained constant by a controller.

Jan 1, 1953

By James Barr

Geology and Mineralogy1 TENNESSEE phosphates are commercially divided into three varieties: Brown, blue and white. The first two only are now of commercial importance. The white phosphates of Perry county are not being mined at present owing to their pockety occurrence. The white phosphate is Fig. I.-DEPOSITS OF 75 PER CENT. BROWN PLATE ROCK UNDERLAIN BY SAND. the highest grade of the three varieties, running often more than 90 per cent. tricalcium phosphate. The brown rock is found in three varieties, grading from the dense almost vitreous gray rock, 76 to 82 per cent. tricalcium phosphate, down

Jan 9, 1914

By H. M. Fisher, R. E. Snow, S. C. Sun

SEVERAL constructive and fundamental studies have been made in the analysis of data obtained from experiments carried on with batch ball and rod mills. The operating characteristics of ball milling in small continuous circuits have also been appraised. It is from these analyses that some of the theories of comminution have been developed. Relatively few studies of continuous rod milling have added significantly to the fundamental concepts, because seldom have they yielded sufficiently consistent results. Perhaps they have been too limited in their scope. Careful control of the variables in batch grinding is simple compared with that encountered in a continuous operation. This factor alone has discouraged many investigators. Occasionally results of systematic changes made in industrial rod mill circuits have been published, but usually the data are sketchy and are restricted because of the unwieldiness of the equipment used. The work, in general, has not been comprehensive; nevertheless it has provided empirical relationships that have bridged the gap between postulate and practice so that by proper manipulation of formulae, a mill designer can anticipate mill size and power requirements.14 Although operating variables of a small continuous mill are not so easy to control as with the batch mill, with present day devices, and with careful experimental work, consistent results can be obtained. Nearly four years ago, in the Process Laboratory, Allis-Chalmers Mfg. Co. began a systematic study of the effects of several variables upon the performance of the pilot rod mill. A mill was built in the laboratory to provide the versatility required for the proposed study. It was constructed in sections so that it could be operated, with a few modifications, as a rod mill 30 in. x 8 ft or 30 in. x 4 ft. The discharge end of the shell was flanged so that either an end peripheral discharge or an overflow discharge could be installed. Thus the performance of at least four types of mills could be studied merely by changing the type of discharge or the length of the mill shell. The grinding experiments were designed so that a study could be made of the way in which the mill speed, feed rate, and pulp density influenced the performance of both overflow and end peripheral discharge rod mills. Four sets of experimental data were collected from the four mill arrangements. The mill in each set of experiments was fed at four rates of feed depending on the length of the mill, at four pulp densities, and at five percentages of critical speed. Electrical and mechanical controls were in- stalled to regulate all these independent variables, and auxiliary devices were used to verify the precision of the controls at each point. The dependent variables used to quantify the experiments were the reduction ratio and the hew surface area produced as calculated from sieve analyses. These were incorporated with the energy factor by the calculation of both the new surface produced per unit of energy and the Bond work index.' Rod wear, as a dependent variable, was not studied because of the short period of operation for each run. Exclusive of repeat runs, each set of experiments yielded 80 products, and the total study at least 320 products, all of which were quantified. With the operating information collected, these data presented a bewildering accumulation. Statistical analysis has been invaluable in unraveling the confusion and in presenting a means of establishing the nature and the magnitude of the significant variables. Data presented in this paper are those from the 30 in. x 4 ft end peripheral discharge rod mill, Fig. 1, when limestone was ground at feed rates of 1000, 2000, 4000, and 5000 lb per hr, at pulp densities of 50, 60, 70, and 80 pct solids, and at mill speeds of 50, 60, 70, 80, and 90 pct of the critical speed. These 80 tests have all been run at least twice, and occasionally a third time, to prove that the data obtained were reproducible. The techniques of operation and the methods of quantification of results are described in the following pages and the results analyzed statistically to show the significant variables. The variables are plotted to show the relationships that exist. A massive dolomitic limestone from Waukesha Lime and Stone Co. was used for feed during these experiments because of its availability and its tex-tural uniformity. This limestone analyzed 28.7 pct CaO, 21.0 pct MgO, 6.0 pct SiO2, 0.4 pct A1²O³, and 0.3 pct Fe²O³ and had a loss on ignition of 44.1 pct. It had a rod mill grindability at 14 mesh of 9.6 grams per revolution from which a work index of 13.9 was calculated. The ball mill grindability at

Jan 1, 1955

[VOL. XXXVI. Page. Line. 155 29 For "Joachimstahl," read "Joachimsthal." 215 Foot-note 2. For " May, 1892," read " May, 1902." 216 21 For " ack-screw," read " jack-screw." VOL. XXXVII. 31 3 For "quantity of tons," read "quantity of slimes." 35 10 Expunge "recorded in Table VII." 37 24 Expunge "to." 38 33 For "page 89," read "page 9." 44 40 For "page 86," read "page 6." 47 In table, third line under heading "Excavators and Conveyors," expunge "per 40 ft. of."]

Jan 1, 1918

By M. V. Nevitt

In the systems Ti-Mn-O, Ti-Fe-O, Ti-Co-O, and Ti-Ni-O the bounda.r-ies of the Ti2Ni-type phases were determined at one or more temperatures and the variation of the lattice parameter with oxygen content was determined. Densities were calculated from the lattice parameters and compared with measured density values. The: results indicate that the occurrence of the phase in these systesms can be correlated qualitatively with valency electron concentration, and that the role of oxygen is that of an electron acceptor. The lower limit of oxygen solubility appears to be determined by the valencies of Mn, Fe, Co, and Ni, while the maximum oxygen concentration coincides with the filling of the 16 (c) positions of the O 7h - Fd 3m space group. THE suggestion has been made by several investigators'" that the phases having the cubic E9,-type structure, and known as 17-carbide-type, double-carbide-type and Ti,Ni-type, are members of a family of electron compounds. This concept has been given additional support by recent work8 in which new isostructural phases involving second and third long period combinations were found, and which provided further evidence of the regularity of occurrence of the phase in terms of periodic table relationships. In this laboratory attention has been focused on the isomorphs containing titanium, zirconium, or hafnium, and the role that oxygen plays in their occurrence. In some binary systems Ti,Nitype* phases occur having the formula A,B where A is the titanium group element. Based on previous workq and the present investigation, oxygen is known to be soluble in two of these binary phases, Ti,Co and Ti2Ni. It is probable that oxygen is also soluble in the other phases of this kind. In other binary systems the Ti,Ni-type phase does not occur, but does occur in the corresponding ternary systems with oxygen .3-5 The experiments described here were performed to determine whether the occurrence and composition of certain of the Ti,Ni-type phases could be related to an electronic effect and whether oxygen's stabilizing role is exerted through an influence on the electron: atom ratio. The ternary systems Ti-Mn-O, Ti-Fe-O, n-Co-O, and Ti-Ni-O were selected for study for two reasons: First, several schemes have been proposed for first long period elements which, although not in quantitative agreement, show a generally consistent trend for the variation of valency with atomic number. Although for a transition metal the term valency is difficult to define and is generally not a constant number which can be applied to all alloys, it is usually assumed to be an index of the number of electrons per atom involved in metallic cohesion. Second, the determination of the Ti2Ni-type phase boundaries was facilitated by the fact that the phase relations in several of these ternary systems have been investigated by other workers."' EXPERIMENTAL PROCEDURE___________________ The alloys were prepared by arc melting crystal-bar titanium, reagent grade TiO, and electrolytic manganese, iron, cobalt, and nickel. Each button was remelted at least three times. The metals had a minimum purity of 99.9 pct except the nickel whose purity was 99.4 pct, the major impurity in this instance being cobalt. The preparation of the manganese alloys was attended by the customary difficulties associated with the vaporization of manganese. The technique used in this case was to add approximately 10 pct extra manganese to the original charge and to continue remelting the button until the final weight was in agreement with its intended weight. At least three alloys in each system were analyzed chemically and the results, even for the manganese alloys, were in good agreement with the intended compositions. A few additional alloys in the Ti-Mn-O system were prepared by the sintering of mixed powders in evacuated quartz tubes followed in some cases by arc melting. For annealing, the alloys were wrapped in molybdenum foil and placed in fused silica tubes containing zirconium chips. The fused silica tubes were evacuated at room temperature to a pressure of 1 x l0-6 mm of Hg and sealed. These capsules were then annealed for 72 hr at an external pressure of 5 x 10-5 mm of Hg in a vacuum furnace whose temperature could be controlled to + 1°C. The success of this procedure in avoiding significant oxygen or nitrogen pickup was indicated by the bright, ductile condition of the molybdenum foil and by the complete absence of a microscopic reaction layer on the specimens. This method did not permit rapid quenching of the specimens but in no case did metal-lographic examination indicate that a solid-state transformation had occurred on cooling. Metallo-

Jan 1, 1961

By R. R. French

Investigations were conducted by the lndiana Geological Survey for some dry methods of bene-ficiating low-grade gypsum ore. Seventy-two batch and continuous flow tests were performed with a roller mill, rod mill, pebble mill, electronic color sorter, electrostatic separator, and an air separator. Approximately 650 size analyses and 550 chemical analyses were performed during the investigation. Batch samples were tested by the Survey, and most of the continuous flow tests were handled by com-mercial laboratories. INTRODUCTION Although many companies producing gypsum have been interested in dry beneficiation, very little information has been published in the past. One of the most comprehensive investigations was reported by the Canadian Department of Mines.5 Other reports of interest have been published by the Canadian Department of Mines,' the South Australian Department of Mines,2 and the U.S. Bureau of Mines.3 Some beneficiating practices, such as hand picking, selective mining, crushing and screening, milling, and air classifying, were already in use in the Canadian industry prior to MacPherson's investigations.5 MacPherson examined the effect of tabling, air separation, screening, flotation, electrostatic separation, calcining, washing, and various types of milling, in his efforts to eliminate dolomite, limestone, and small amounts of silica and clay from the gypsum ore. RAW MATERIAL Gypsum and anhydrite occur within the lower part of the St. Louis Limestone (Mississippian) in southwestern Indiana. Gypsum in single beds 10 or more ft thick occur at Shoals, Martin County; near Freedom, Owen County; near Bloomfield, Greene County; and in the Devonian strata of LaPorte County. Only the Shoals deposit has been exploited commercially. The western edge of the Shoals deposit is contaminated by a continuous bed of shale, about 1 1/2 to 2 ft thick, near the top of the evaporite and by thin continuous strata or irregular masses of carbonate rock. The low-grade material used in these investigations was obtained from the waste pile of the National Gypsum Co.'s plant at Shoals. The waste ore averaged about 67.4% gypsum and was contaminated by various amounts of shale, dolomite, and limestone. All the material had been previously crushed and screened to minus 1 1/4 to plus 3/8 in. X-ray analyses of powdered, sedimentated, gly-colated, and heat-treated samples of the shale showed that it was composed of slightly structurally disordered illite, Fe-rich chlorite, and very finegrained disseminated silt. The clays and silt were partly cemented with carbonate material. Light-gray argillaceous limestone and gray or brown porous dolomite made up most of the carbonate rock contamination. Crushing Characteristics: The rate unweathered gypsum, carbonate rock, and shale reduce in size was determined by crushing handpicked samples in a rod mill and screening at minus 100 mesh (.0059 in.). Fig. 1 graphically represents the data. These data indicate that carbonate rock should be relatively easy to separate from gypsum, but that shale should be difficult to separate from gypsum by differential crushing. Controlled Samples: Eight rod mill tests of hand-picked samples of mixed gypsum and shale and mixed gypsum and carbonate rock were made. Sample weight and crushing weight were standardized, but the scalping screen size was varied from 3 to 10 mesh (.265 to .0787 in.) in order to obtain the optimum purity and recovery. The data obtained from the tests (see Table I) illustrate that the relatively hard carbonate rock allows appreciable beneficiation (13.6 to 18%), but the low strength gypsum and shale allows only minimal separation (3.1 to 7.5%).* Semi control led Samples: During the investigation considerable slaking of the shale was noted when the ore was subjected to alternate wetting and drying. As demonstrated in laboratory tests, as much as 76% shale can be removed by two cycles of wetting and drying in a 48-hour period with subsequent screening at .265 in. Five ore samples, stockpiled and weathered, were screened, rod-mill crushed and rescreened at .157 or .187 in. with excellent results (Table 11).

Jan 1, 1967

By A. F. Witt, A. M. Gaudin, A. K. Biswas

Finite contact angles in the rutile-water-organic liquid system are traceable to contamination or are due to addition of a surface-active agent. Finite contact angles are invariably accompanied by hysteresis.1-7 Besides surfactant concentration and pH, the nature of the organic liquid is found to be a factor influencing the magnitude of contact angle hysteresis. In a recent paper the authors have reviewed principles and applications of measurement methods for contact angles and their hysteresis.22 In this paper, these methods are applied to a system consisting of rutile, an organic liquid (benzene, decane, or dode-cane) and water. Surfactant (dodecylamine hydro-chloride) was used at various concentrations and various pH values. MATERIALS A synthetic rutile crystal supplied by the Linde Co. was used. It is a cylinder 1/2 in. diam, with faces cut perpendicular to the c-axis. The crystal is stated to be alumina-free and to be 99.9% pure. Rutile is a high surface energy solid, its calculated average field strength being 2.7 x 105 e.s.u.,9 its dielectric constant10 is 114. The zero point of charge of rutile was measured11 and found to be at pH 6.0. The atomic distances and bond angles of the tetragonal crystal of rutile have been precisely determined.l2 The organic liquids were specially purified. Reagent grade benzene was repeatedly shaken with concentrated sulfuric acid to remove thiophene, then neutralized with sodium hydroxide solution, rinsed with distilled water, dried overnight over anhydrous calcium chloride and filtered. The refractive index of this chemically purified benzene was 1.4977 (at 25°C) - very close to that of pure benzene (n25 1.4979).13 Both n-decane and n-dodecane were washed with aqueous sodium hydroxide, concentrated sulfuric acid (repeatedly, until the acid layer was colorless) and again with alkali, to free the organic hydrocarbon from fatty acids and unsaturated hydrocarbons. The organic phases were subsequently washed with distilled water and dried over anhydrous sodium sulfate. The filtered hydrocarbons were then distilled under vacuum (9-10 mm pressure). Decane, thus purified, showed traces of unsaturated and of carboxylic compounds. On gas chromatographic analysis the purified n-dodecane showed the presence of two impurities. However, the relative retention times of these components did not change substantially when measured on a polar or a nonpolar column. This indicates that the compounds were probably in the same polarity class, i.e. the components were nonpolar like dodecane. Conductivity water has always been one of the liquids. Conductivity of the water used was 10-6 ohm-' cm". Dodecyl ammonium chloride was prepared from pure amine (supplied by Armour and Co., Chicago), by Li in the MIT Mineral Engineering Laboratory.14 The critical micelle concentration at 25°C is known, 0.0138 mol per liter15 or 3.06 gpl. All our experiments have been done at concentrations lower than the critical micelle concentration. The glass vessels, glass drop holder and the rutile crystal were all cleaned with hot chromic acid followed by distilled water, concentrated hydrochloric acid, and again distilled water, and conductivity water. During the experiments, a nitrogen atmosphere was maintained. For this purpose, commercially purified nitrogen was further purified by passing it over hot copper wire at 450°C, then through columns of acidic chromous chloride solution, concentrated alkali solution and distilled water. APPARATUS AND METHODS Hysteresis was produced by the "captive drop" or constant volume drop method as well as by the "expanding-contracting drop" or variable volume drop method. The image of the drop while it is expanding, contracting or moving is projected on a screen and photographed. The developed film is projected through an enlarger and the contact angles measured with a protractor.

Jan 1, 1964

By Albert D. Brokaw

The accompanying charts are presented to extend and improve a chart published under the title "A Chart to Provide Approximate Correction for Temperature and Deviation from Boyle's Law."' The applicability of this earlier chart was limited by the fact that it was based on the work of Burke and Keyes² and Kvalnes and Gaddy3 whose experiments were conducted with pure methane, the adjustments suggested for natural gases of higher specific gravity were unsatisfactory except within limited ranges of temperatures and pressures, and precise interpolation was difficult. The extensive work of G. G. Brown, D. L. Katz and their associates on the heavier natural gases has provided better bases for the needed corrections, and the present charts. which are based largely on their work, are intended to simplify the computations involved. The design of the charts has been changed by plotting temperatures as a function of pressure and correction factor, on a semilogarithmic or "ratio" grid, which gives fairly even spacing of the graphs and simplifies interpolation. Charts have been prepared for natural gas with specific gravities of .60, .65, .70, .75 and .80. The standard computation for use in estimating the quantity of gas in a reservoir may be expressed as follows: _ PA X 520 X VR ZT where: Q is the volume of gas at 60°F and one atmosphere pressure PA is the absolute formation pressure in atmospheres

Jan 1, 1949

By Albert D. Brokaw

The accompanying charts are presented to extend and improve a chart published under the title "A Chart to Provide Approximate Correction for Temperature and Deviation from Boyle's Law."' The applicability of this earlier chart was limited by the fact that it was based on the work of Burke and Keyes² and Kvalnes and Gaddy3 whose experiments were conducted with pure methane, the adjustments suggested for natural gases of higher specific gravity were unsatisfactory except within limited ranges of temperatures and pressures, and precise interpolation was difficult. The extensive work of G. G. Brown, D. L. Katz and their associates on the heavier natural gases has provided better bases for the needed corrections, and the present charts. which are based largely on their work, are intended to simplify the computations involved. The design of the charts has been changed by plotting temperatures as a function of pressure and correction factor, on a semilogarithmic or "ratio" grid, which gives fairly even spacing of the graphs and simplifies interpolation. Charts have been prepared for natural gas with specific gravities of .60, .65, .70, .75 and .80. The standard computation for use in estimating the quantity of gas in a reservoir may be expressed as follows: _ PA X 520 X VR ZT where: Q is the volume of gas at 60°F and one atmosphere pressure PA is the absolute formation pressure in atmospheres

Jan 1, 1949