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By Herbert Herman, M. E. Fine

THE first decomposition product of a supersaturated aluminum-rich A1-Ag alloy at low tempera- tures is Guinier-Preston zones.'-, The zones are ideal and each consists of a spherical shaped silver-rich cluster about 16 A in diam syrounded by a silver-poor shell approximately 72A in diam.' The composition of the two regions is not known with certainty., After quenching from the solution anneal, these zones form rapidly on aging at temperatures as low as -30°C.5 The rate of zone formation increases with aging temperature; the activation

Jan 1, 1961

By R. L. Smith, J. L. Rutherford

ALTHOUGH considerable effort has been devoted toward the determination of the mechanical properties of pure metals, it is extremely difficult to compare the results of such work. This is because of differences in method and type of test, grain size, heat treatment, and purity of material. There is very little information on the properties of most of the high melting point reactive metals with purities greater than 99.9 pct. Previous evidence concerning the tensile properties of unalloyed metals show that: body-centered-cubic metals are brittle at low temperatures; face-centered-cubic metals remain ductile; some hexagonal metals remain ductile, others become brittle. It may be that traces of impurities decrease the low temperature ductility of the body-centered-cubic lattice. This would suppose that a body-centered-cubic lattice free from impurities would exhibit nearly the same ductility as a face-centered-cubic structure. The present investigation has been an evaluation of the tensile properties of zone refined iron in order to determine whether higher purity material than that previously evaluated behaves differently. Experimental Procedure In this investigation, high purity iron was zone purified using the floating zone method.' The starting stock was obtained from two sources. The first,

Jan 1, 1958

By Donald L. Katz

Charts for predicting the pressure to which natural gases may be expanded without hydrate formation have been prepared for gases of even gravity. Pressure-temperature curves for hydrate formation were established for gases having gravities from 0.6 to 1.0. These curves and the thermal behavior of the gases during free and adiabatic expansion were used to prepare the charts for estimating the permissible expansion of natural gases without hydrate formation. The problem was solved by L. F, Albright, W. T. Boyd, J. J. McKetta, G. Martin, P. Poettman. and A. P. Snyder.-, who are first-year graduate students in the department of Chemical and Metallurgical Engineering at the University of Michigan. This paper is essentially a summary of their results. Prediction of Conditions for Hydrate Formation in Natural Gases Each natural gas under a given pressure will form solid hydrates at a corresponding temperature provided sufficient water is present.1-5 The temperature of natural gases below about 5000 lb. per sq. in. decreases when the gases are expanded freely.6,7 This decrease in temperature may cause the expanding gas to enter the region of temperature and pressure at which hydrates will form' The final pressure to which a natural gas may 'be expanded without hydrate formation depends upon the initial temperature and pressure and the gas composition. This paper presents charts that give the final pressures to which gases of gravity 0.6 to 1.0 at given initial temperatures and pressures may be expanded without formation of hydrate. Hydrate-forming Temperatures and Pressures as a Function OF Gas -Gravity Experimental data of pressure versus temperature at which solid hydrate will form, provided sufficient water is present, are available for a series of gases.2,3 A method of predicting the pressure-temperature curve for a given gas composition has been reported.' The solution to this problem requires that these curves relating pressure to temperature be established for gases of given gravities.

Jan 1, 1945

By L. C. Weiner

For zinc single crystals, xo = 3o, a surface coating raises both the cleavage and yield strengths over a large temperature range. The "brittle temperature," associated with slip after completion of twinning, does not coincide with the point of intersection of the flow and cleavage curves, which is associated with twinning. A surface film has no effect on the brittle temperature, while it lowers the intersection temperature some 20°. For crystals, yn = 83o, a coating decreases the cleavage strength, making it temperature independent, as well as increases the brittle temperature or its equivalent, the intersection temperature, 20°. These observations are described on the basis of a dislocation-pile-up-at-a-barrier model for brittle fracture; in crystals x,, = 3o the number and distribution of twins play a vital role. IN a recent investigation on the effects of solid environments on the brittle fracture of zinc single crystals,' it was demonstrated that the presence of a surface film changes the cleavage strength of these crystals, either increasing or decreasing it, depending on the crystal orientation. An increase in cleavage strength of some 43 per cent was found for coated crystals oriented x, — 3o K = 28",* while a decrease of 48 per cent was observed with crystals X" = y» — 83". Moreover, these effects were found

Jan 1, 1959

By J. G. Giddings, R. Kobayashi

Residual viscosity, the ViSCOSitY at a given pressure and temperature minus the dilute gas viscosity at the same temperature, has been found to be independent of temperature for pure components and mixtures for simple molecules and light hydrocarbons. The residual viscosities for methane, ethane, propane and four mixtures were correlated as a function of reduced density and molecular weight. INTRODUCTION Earlier efforts in correlating the viscosity of light hydrocarbons and associated gases under pressure, primarily by some form of the corresponding states principle, have been reported elsewhere.7 The formal theory of corresponding states principle for viscosity from non-equilibrium statistical mechanical arguments for simple molecules has been developed by Helfand and Rice.13 The most serious obstacle to the development of a generalized corresponding states representation of viscosity data, even for simple molecules, has been the limited quantity of precise viscosity data of pure components and mixtures over a wide range of pressure and temperature conditions. Viscosity data on light hydrocarbons have recently been contributed by several laboratories.2,6,8,23,25,26 In the study of the viscosity of nitrogen, Michels and Gibson" observed that the viscosities of nitrogen as a function of density gave parallel isotherms. The same behavior has since been reported for other gases.".= The observed behavior indicates that the residual viscosity or the viscosity at a given pressure and temperature minus the dilute gas viscosity at the same temperature is a unique function of the density. Abas-Zade,1 Michels and Botzen,18 and Michels, Bot-Zen, Friedman and Sengers,19 observed similar behavior for thermal conductivity, the residual thermal conductivity being defined in a manner parallel to that of residual viscosity. Thodos and co-workers 4,15,24 applied the residual viscosity concept to the viscosity of pure monatomic and diatomic gases. Ellington and co-workers10,25 made the residual viscosity vs density plots for ethane and propane, but omitted the region below a residual viscosity of 15 micropoise and showed a systematic separation of the ethane isotherms in the low density region. Eakin correlated the residual viscosity of methane, ethane, propane and n-butane empirically as a function of density and molecular weight: Carmichael and Sage6 recently presented ethane residual viscosity vs density values in the gaseous liquid, and near critical regions as a single univariant function of density. Flynn, Hanks, Lemaire and ROSS" have contributed extremely accurate viscosity data to confirm that the residual viscosity concept is essentially correct, but may not be accurate within 0.1 per cent of the viscosity value for the gaseous state- The recent studies by Giddings12 indicate that the residual viscosity of methane, propane and each of four methane-propane mixtures are unique functions of density Over the temperature and the density ranges studied.

Jan 1, 1965

By Mourad Aissa

From our previous work (Gardner, Aissa, and Verghese, 1982) on determining the residence time distribution of ball mi 11s from radiotracer data taken in closed-circuit operation without interruption of the process, it occurred to us that the data taken for this purpose also contained information on the breakage rates of all the sizes present. It is the purpose of the present work to evaluate methods to obtain breakage rates from this data. A numerical solution for the impulse injection and subsequent detection of radiotracer in a closed-circuit linear comminution process is developed and used with typical breakage parameters, residence time distribution, and classifier functions to study and evaluate these methods.

Jan 1, 1984

By Henry Louis

Four alloys of gold and silver were prepared, containing the metals in the following proportions by weight: I. Gold:Silver::1:2.62.

Jan 1, 1894

By C. T. Young, J. L. Lytton

In recent investigations,1,2 the strength and thermal stability of dislocation substructures prepared by 5 to 25 pct room temperature tensile straining and recovery annealing at 120°, 160°, and 200°C have been studied in randomly oriented polycrystalline high purity aluminum. The techniques of transmission electron microscopy revealed that a major source of the strength and stability of dislocation substructures was the formation, during room temperature straining, of well-defined cells bounded by dislocation tangles which rearranged into nearly perfect dislocation networks during recovery, forming the boundaries of subgrains. The strength of such substructures increases with decreasing cell or subgrain size,2"6 and the formation of fine subgrain structures can provide thermally metastable strength at low temperatures and can favorably alter the course of primary creep at elevated temperatures.7'8 For maximum benefit, however, sub-grain growth should be reduced or eliminated. It was, therefore, decided to investigate the use of heterogeneous precipitation on dislocation networks as a means of imparting increased strength and thermal stability to subgrain structures through effective pinning. C.T. YOUNG, STUDENT MEMBER AIME, and J. L. LYTTON, Member

Jan 1, 1970

By John F. Allan

This paper does not pretend to advance any facts or improvements not known to many members of the Institute, but is intended merely to give a few practical hints on preliminary tests, and to call attention to a possible enlarged field for the cyanide process in the treatment of some silver-ores, which merits investigation. Broadly considered, the choice of a process for the treatment of silver-ores in Mexico is confined to the following alternatives: (1) Concentration for treatment by smelting; (2) milling and pan-amalgamation; (3) the patio and Ortega process; [4) chloridizing roast and lixiviation; (5) chloridizing roast and cyaniding; and (6) cyaniding of the crude ore. These methods of treatment may also be combined, and cyaniding or concentration, or both, may be introduced, at what-ever stage it is found to be most advantageous. The characteristics of the ore (especially its gold-content) and local conditions, such as distance from railway, cost of fuel, amount of water available, vary so much that it is impossible to make general comparisons between the different processes, either as to extraction or cost. Concentration and subsequent smelting may be made very expensive by long-distance transportation of concentrates; pan-amalgamation is undoubtedly expensive; and the patio process is barred when the ore contains appreciable amounts of gold, by reason of its poor extraction of that metal; yet there are many ores for which each of these processes is especially adapted, and the expense of treatment is compensated by the results obtained.

Jan 1, 1905

By T. H. Weldon, L. V. Whiton, R. R. McNaughton, J. H. Hargrave

R. H. McNAUGHTON*—The Smelting Co. and Mr. Reid and his men at Selby are to be congratulated on the job they have done on sinter gas recircula-

Jan 1, 1950

By R. Roberge, H. Herman

Jan 1, 1969

By Roger N. Dokken

It is well-known1-4 that Fe-Si alloys from approximately 9 to 27 at. pct Si show an ordered structure of the Fe3Si type at room temperature. Recently Meinhardt and Krisement,' through an investigation of Fe-Si alloys at room temperature by neutron diffraction, discovered that at 10.8 at. pct Si ordering of the FeSi type occurs while above this composition the normal Fe3Si-type superstructure appears. This FeSi type of ordering was also found by Davies8 as indicated by X-ray diffraction measurements on an Fe-8.7 at. pct Si alloy. Meinhardt and Krisement7 extended their neutron-diffraction work and determined the phase-boundary temperatures for both FeSi- and Fe3Si-type ordering. Ordering phenomena can also be studied by resistance measurements.4,8-11 Krivoglas and Maty-sina" carried out a theoretical development of the

Jan 1, 1965

Robert H. Richards, Boston, Mass.: Mr. Goodale calls attention to the difficulty of obtaining clean tailings from the jigs which are fed by the spigots of the hydraulic separator. This difficulty is universally encountered. The Lake Superior copper mills practically overcome it by running the beds of those jigs loose, carrying into the hutch all of the available copper and some sand. These hutches are again jigged upon threesieve Collom jigs, where the treatment is very slow and gentle; and on the successive jigs lighter and lighter bedding is used. The last sieve is run thin enough to let some sand into the hutch. With these precautions most of the free copper is extracted, as well as a fair proportion of the included copper.

Jan 1, 1897

By William P. Blake

IntroductioN.............989 The Blake stone- Breaker Prize.......989 Great Labor-Saving Inventions.. 990 I. Biographical NoticE OF the Inventor......990 II. Former Methods of Breaking Stone......992 Ragging and Spalling......... 992 Cornish Rolls..........993 III. Construction of the Blake Stone-Breaker.. .. 993 The Lever.Pattern.........994 The Eccentric Pattern.........997 The Challenge Pattern......... 999 The Monarch Pattern.........1001 The Multiple-Jaw Pattern........1001 Movable Dies for Jaws......... 1004 Cheek.Plates,..........1007 IV. The Capacity OF Blake Breakers......1007 Position and Feeding of Breakers...... 1008 V. Gyratory Jaw Crushers.........1010 The Gates Rock- and Ore-Crusher......1010 The Comet Crusher.........1010 VI. Some Unusual Forms OF the Breaker......1010 The Smith Hydraulic Pattern.......1012 The Forster Crusher.........1012 The Stafford Crusher.........1013 The Gates Crusher.........1013 The Dodge Pattern.........1013 The Rawson Crusher.........1014 The Duplex Breaker.........1015 Booth's Modification of Wedge-Block......1015 Marsden's Eccentric Pattern.......1017 The Lancaster Machine........ 1017 VII. Combined Crushing and Grinding Impracticable,. . 1018 The Hanscomb Machine ...1019 Howland's Crusher and Pulverizer..1020 The Oliver Crusher and Pulverizer..1021

Jan 1, 1903

By W. D. Robertson, W. L. Phillips Jr.

Stress-strain curves were obtained for single crystals of alpha brass in tension and in direct shear. Specimens were strained various amounts in a given slip direction, unloaded, and immediately strained in a second slip direction 60°, 120°, or 180&apos; from the original slip direction. Crystals strained in tension and direct shear had comparable critical resolved shear stresses and stress-strain curves. The density of slip lines in direct shear and in tension was essentially the same. The stress-strain curves obtained in shear were independent of initial orientation, choice of {111 } slip plane, choice of <110> slip direction, prior annealing temperature, and rate of cooling after annealing. There was no recovery after annealing for 4 hr at room temperature or 200°C; recovery was observed after 4 hr at 400°C. The crystals showed no asterism and mechanical properties were completely recoverable up to 20 pct strain. It was found that there is a barrier to slip in all latent close-packed directions, and that the magnitude of these barriers, evaluated at 3 pct strain, is proportional to prior strain and independent of the choice of latent direction in the {111} plane. The formation of Cottrell-Lomer barriers is discussed as a possible explanation for the hardening of the latent systems. AN idealized concept of plastic deformation indicates that a single crystal should yield at some stress that is dependent on crystal perfection and it should then continue to deform plastically by the process of "easy glide," which is characterized by a linear stress-strain curve and a low coefficient, ds/dE, of work-hardening. Hexagonal metal crystals generally conform to this ideal concept of laminar flow. In face-centered cubic metals the range of easy glide is always restricted in magnitude and it is strongly dependent on orientation, composition, crystal size, shape, surface preparation, and temperature. Since one of the principal differences between the two crystal systems, both of which deform by slip on close-packed planes, is the existence of secondary (latent) slip planes in the face-centered cubic crystals, it has been proposed that the transition from easy glide to turbulent flow, characterized by rapid linear hardening, is due to slip on secondary planes intersecting the primary plane.&apos;-.; However, the characteristic differences between individual face-centered cubic metals remain to be explained; in particular, it is not clear why the range of easy glide should vary so greatly in different metals and alloys similarly oriented for single slip. An investigation and comparison of different metals with respect to latent hardening on the primary slip plane should provide some of the information required to specify the necessary and sufficient conditions governing the transition from easy glide to turbulent flow. But, in order to accomplish this purpose, plastic strain must be produced by simple shear in a chosen plane and in a predetermined direction by some form of directed shear apparatus, the results of which must be correlated with the corresponding tension experiments. Two such experiments have been performed previously with zinc and with aluminum. Edwards, Washburn, and Parker" and Edwards and Washburn7 found that the strain-hardening coefficients in two latent directions in the basal plane of zinc were the same as in the primary direction. However, to initiate and propagate slip in either the [2110] or the [1210] direction, following primary slip in the [1l20] direction, it was necessary to increase the stress above that required to continue slip in the primary direction; when the direction of shear was reversed 180 deg plastic strain began at a much lower stress than that required to initiate slip in the original direction and the stress to propagate slip in the reverse direction was lower than the stress to continue slip in the forward direction, indicating a permanent loss of strain-hardening. Rohm and Kochendorfer observed softening in aluminum for all latent close-packed planes and directions. They also found that the critical resolved shear stress obtained from their direct shear apparatus was 50 pct lower than the value obtained from conventional tension tests, that the stress-strain curve was linear at 50 pct plastic strain, and that slip lines were not visible at strains less than 30 pct. At present it is uncertain whether these diverse results correspond to real differences in work-hardening characteristics of the close-packed planes of aluminum and zinc or to differences in experimental technique. In view of Read&apos;s analysis &apos;" of the stress distribution in the experimental arrangement of Rohm and Kochendorfer, there is some reason to question the significance of the latter results. In order to resolve this problem it is necessary to re-valuate the direct-shear technique and either repeat the previous measurements or investigate a third system. The latter choice seemed most likely to produce significant results with respect to work-hardening, and accordingly, it was decided to examine the hardening characteristics of the latent slip directions in alpha-brass. The choice of alpha-brass was dictated by the fact that easy glide is more extensive in this alloy than in any other face-centered cubic metal or alloy and, presumably, more nearly like the idealized hexagonal system. Experimental Procedure Crystals were made in graphite by the Bridge-man method in the form of cylinders, 11/2 in. diam and 8 to 9 in. long. Material for the crystals was 70/30 brass containing the following impurities:

Jan 1, 1959

By Reed W. Hyde

Some information has been published on the sulphur dioxide concentration of gases from D wight-Lloyd machines sintering lead ores but most of this relates to the customary practice in which the charge is relatively high in lead and is sintered in two passes Over the machine. It is thought, therefore, that the following observations on sintering in one pass a low-lead, low-sulphur charge may be of interest. The data were obtained in sintering lead sulphide notation concentrates mixed with minus 20.mesh oxide ore, the mixture carrying 16,8 per cent Pb and 5.3 per cent S. No returns were used because of the limited amount of sulphur available as fuel, but the mixture pelletized readily. to make a satisfactorily permeable bed on the sintering machine. As there was a possibility that the SO z might be utilized, a series of runs was made to determine the concentration ofSO2 in the gases at different points along the wind box, and the effect on this concentration of changes in the wind-box vacuum. Several runs each were made with vacuums (as measured in inches of water at the wind box) of (1 2 to 1 in., (&apos;1 4 to 3% in. and (3) 6 to 5% in. The averages of the determinations from each series are platted On the graph (Fig, 1). The vertical scale shows the percentage by volume of SOz (as determined by the Reich method), and the horizontal scale shows the time e~pressed as percentage of the total sintering time. Sintering was considered to be complete when no SOz could be detected in the gases. In all cases the depth of bed was 4 1/2 in. and the weight of dry charge per square foot of hearth area was 45.2 lb. Other data are given in the table. The volume of gases corresponding to the several points along the wind box at which SO2 determinations were made could not be measured, but has been calculated from the SO2 Content and sulphur elimination on the assumption that the volume is uniform throughout the sintering period. This is not strictly true, as with a given vacuum the volume usually will drop slightly toward the middle of the period and increase toward the end. However, this made is a reasonable approximation. several interesting features are brought out by these data. In general, the published data on SO 2 concentration in sintering under ordinary conditions show a high SO2 concentration in the early stages followed by a rapid decrease in concentration and with relatively little SOz in the gases from the last half or third of the operation. In other words, the greater part of the sulphur elimination is obtained in the first third or half of the period. In these runs, the 6-in. vacuum, which approximates the usual operating condition, gives a curve that follows this customary pattern. Maximum SO2 concentration is obtained 234 min. after

Jan 1, 1944

By Robert G. Nisle

In conducting a pressure build-up test on an oil well, it is often necessary to shut-in the well for a short time prior to initiation of the test. The effect of such a short tern shut-in on the resulting pressure build-up curve is derived. The derivation is based on the Kelvin point-source solution and is a straight forward extension of the fundarnental theory. The magnitude of the effect is evaluatecl and illustrated by an example. It is shown that if the production subsequent to the short term shut-in is at least 10 times the duration of the shrct-in, the effect will he less than 10 per cent. INTRODUCTION It often happens that before a pressure build-up test can be made an additional valve must be mounted on the wellhead, or on arrival at the well, it might be learned that the well had been shut-in several hours the previous day because of a shortage of tankage. In such cases the question is How will such an interruption of production affect the results of a pressure buildup test This work explains how to take account of such a short term shut-in in order that the test can proceed without further delay. The solution presented here makes use of the Kelvin point-source solution used by Horne1 in his treatment of the pressure build-up in wells. Use is also made of the super-position theorem. MATHEMATICAL DERIVATION The well is assumed to have been in production at a constant rate for a relatively long time (several days or more). It is then shut-in for a short time, after which it is again placed in production at the previous constant rate. It continues to produce at this rate until shut-in for a pressure build-up test. The Kelvin point-source solution is expressed by Eq. 1. The sequence of production rates is listed in Table I. TABLE 1 — SEQUENCE OF PRODUCTION RATES Time interval Production Rate At time AT the pressure will be the resultant of the sequence of production rates shown in Table 1. An expression for the super-posed effects may be derived from this table. (Effect of + q for T + ? T) + (Effect of - q for T + ?T-t,) + (Effect of + q for T + ? T - t,) + (Effect of - q for ? T) = Resultant........(2) The desired result is obtained by substituting the effect defined by Eq. 1 for the terms in Eq. 2. The result is Eq. 3. When the logarithmic approximation is made for the exponential integrals and the terms collected the result is Eq. 4. Let T — t2 = T = flowing time following short term shut-in t2 — t1 = 6 = duration of short term shut-in Then T - t1 = r + 6 Substitution of these quantities in Eq. 4 gives p(rw ?T) = P,, -When d<<t - AT then d—&apos;-, T— approaches 1. r + AT In this case the effect of the short term shut-in may be ignored. In order to get some idea of the numerical magnitudes involved take the worst possible case, when AT = 0, that is at shut-in. If the error is made less than some maximum acceptable value at this time, it will be less than the maximum for all subsequent times. d + r Let the difference between the value of y-— and 1 be less than 0.1. Then —6+r — 1 < 0.1 S < O.l T Therefore, if the flowing time following a short term shut-in is at least 10 times the duration of the short term shut-in, the error introduced by ignoring the short term shut-in will not exceed 10 per cent of T+AT A T

Jan 1, 1957

By Bunting S. Crocker

Bunting S. Crocker (Executive Vice President, Kilborn Engineering Ltd., Toronto, Ont., Canada)-This is an interesting report on laboratory-scale testing with pebble charges in 12-in.-diam mills, and the author correctly concludes that useful laboratory testing can be done. In the opening paragraphs he states, "laboratory pebble-milling tests have been considered too difficult to perform and not relevant enough to the actual grinding situation"!! This is definitely not so! The writer published detailed tests done in a 12-in.-diam mill comparing pebble and steel balls in 1952 6 and again in 1954 7. We note that our review paper in 1963 was the only one mentioned in the References. The author states that "a smooth lining is more frequently used in commercial-scale pebble grinding." The writer has designed some 22 plants treating 134,000 tpd in North America and Australia. He has also visited pebble installations in Norway, Sweden, Finland, and South Africa. All these plants correctly use heavier lifters than would be considered standard for ball mills of a similar size. Smooth liners are not recommended in wet ore treating plants. In the 1952 paper6 it was clearly demonstrated in the test work that the individual ore pebbles had to be the same weight-not the same diameter or size-as the steel balls if comparable grinding results were to be obtained. In the tests performed in this study most of the pebbles "passed 50-mm round hole screen openings and remained on a 40-mm round hole sieve. Correspondingly most of the ball mill experiments were performed with 50 or 40-mm steel balls". Thus, the balls and pebbles were essentially the same size or diameter. This means we are comparing apples and oranges. When the feed being ground is fine enough the pebbles will be superior. When the feed is coarse the steel balls will be the better. This is similar to grinding tests in which two sizes of steel balls are compared. In the middle of the article, "Crocker5 has reported that equal weights of pebbles and steel balls achieve the same grinding capacities under similar conditions …", then he proceeds to question this postulate. In the eight reports that I have published, I have never made this statement. What I have said is "for comparable grinding, the individual pebbles in the mill charge should be the same weight as the individual steel balls." This is not the first time that I have been misquoted on this point! It is most unfortunate that this test work has been done with a ball and pebble of the same diameter and not the same weight. It is impossible to properly evaluate the results. I also regret the fact that the screen analyses of the tests were not shown. Many of us who have been 40 years or less in the grinding game can easily read screen analyses at a glance. We can tell whether the top meshes are being ground by the ball charge, etc., etc. The graphs are fine for the summary or to illustrate conclusions but are often misleading in the report itself. However, we do agree that useful pebble grinding tests can be done in a 12-in. mill.

Jan 1, 1973

By L. W. Strock

Metallurgists handling lead and zinc ores have long been familiar with the spectrograph as a routine analytical tool, as its earliest regular use by American industry was in controlling impurities of zinc metal and its alloys. This application has been extended to other metal industries on an extensive scale, accompanied by refinements of procedure to such an extent that a large part of some metals produced, especially magnesium, aluminum and steel, are checked only by spectrographic methods for conformity to specifications. The spectrographic analysis of ores and other poorly conducting powdered solids presents difficulties not encountered with metallic samples, which can be arced or sparked as self-electrodes or can be readily dissolved, so that their solutions can be analyzed, as in the American Society for Testing Materials standard methods for zinc and zinc-base alloys. Spectra of powdered solid samples can be prepared by using carbon electrodes provided with a crater of suitable size, into which the sample is packed. Ore samples and many other powdered solid materials usually analyzed in the chemical and metallurgical laboratory are more complex and varied in composition than samples of metals produced in large tonnages. &apos;lore preliminary work therefore is usually necessary in devising a spectrographic method for analyzing a given type of powdered sample than for analyzing metal samples, in order to use that method with confidence. The howledge that the standard samples and unknowns produce equivalent line intensities at equal concentration is the fundamental basis of any quantitative spectrographic method. On the other hand, powdered samples have an advantage over metals in that any desired number of chemical compounds can be mixed dry in any desired ratio to produce a synthetic standard. Expcrience has shown, however, that spectra of elements in finely divided compounds introduced into a standard in preparing a synthetic ore sample do not always behave in the electric arc in a manner that produces spectral line intensities similar to those observed at the same concentration in a natural mineral. In ore samples minor elements frequently are contained in the crystal lattice of larger particles of an abundant ore mineral. Their dissociation and volatilization from the sample into the arc then proceeds differently in the standard and sample, with resultant differences in intensity. During the past 10 years I have devised and applied several quantitative spectrographic methods for determining various elements in rocks and minerals in connection with studies on their geochemistry,&apos; but the incentive has gradually changed since the summer 0. 1940 to the specific practical problem of searching for domestic sources of rare and stratcgic metals. The

Jan 1, 1949

By Edgar Dunn

PART I.-DETERMINATION OF GASES IN SMELTER FLUES. IN 1907, upon arriving in Anaconda to take up work in the testing department of the Washoe Reduction Works, the. following problem was met at the car step, so to speak: complete and. exact analysis of gases, not only at the stack, but also in all departmental flues. Taken up to employ time not otherwise needed for regular testing department work, instructions were extremely liberal for a commercial plant, to the effect that accuracy should not be sacrificed to speed. In December, 1907, the work was temporarily transferred to the Great Falls Smelter, and some of the methods here given were there worked out. Differences in smelting operations at Great Falls and Anaconda, however, necessitated further investigations and the development of a new method for S03 determinations at the latter plant, where work was resumed in July, 1908, and completed about a year later. At the time of inception of the work, data (not only on percentages, but even on methods) were found to be meager in the extreme, for one or the other of two reasons: either entire lack of experiment at a large proportion of smelters, or disinclination on the part of the managements to divulge data of any description pertaining to either results or methods. In making determinations of gaseous constituents of flues, two methods are open to consideration: 1, the drawing out of a sample, and collection of the same as a whole, to be removed to the laboratory for later analysis; and 2, the absorption in situ on the flue of one certain constituent, disregarding others for the time being, or perhaps combining two or three in one determination. The first is generally the more rapid, but it is also the more inaccurate, method of analysis, even with special type absorption apparatus, being the more largely subject to error, both of reading, and also because of leakage during complicated manipulation in the laboratory. The amount used for analysis must also, because of limit of container, be small for the first method, and an average gas is very seldom obtained, necessitating for a fair average result a large number of determinations. Consequently, when we balance the time spent in a dozen determinations of short-time samples as against the time employed in making two or three long-time determinations of various constituents in situ, we are not so certain in our statement as to the relative speed of the two methods. Moreover, the method of analysis in the laboratory of 100 cc. of flue gas is satisfactory only when constituents thus determined are present in considerable quantity, results being simply approximate when determining such compounds as sulphur dioxide, sulphur trioxide, carbon monoxide and dioxide, and arsenic trioxide and water vapor, none of which are carried in all smelter flues in amounts in excess of (or even approaching) 1 per cent by volume. Special condi-

Jan 8, 1913