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By Charles R. Fettke

BefoRe the Drake well on Watson Flats below Titusville, Pa, inaugurated the modern petroleum industry on Aug. 28, 1859, a considerable industry, based on the manufacture of mineral oils through the destructive distillation at relatively low temperatures (750' to 800' F.) of cannel coals and shales in closed, air-tight retorts, had already sprung up in Europe and America because of the increasing cost of animal and vegetable oils and fats and the growing demand for illuminating and lubricating oils. In 1860, eight out of 55 such coal-oil companies in the United States had plants located in Pennsylvania.' Of these, the Lucesco Works, costing $120,000, situated near Kiskiminetas Junction, was the largest operating in the country. It was equipped with 10 revolving 2.5-ton retorts and 16 stills for rectifying the oil, each holding 2000 gal. The total output of crude oil was almost 6000 gal. per day.2 The discovery of an abundant supply of natural petroleum by the Drake and other wells stopped the distillation of coal oil in America. Most of the smaller plants were closed and others were converted into petroleum refineries. At present, in spite of the temporary over-production of petroleum, the coal and oil-shale carbonization industries are again attracting the attention of far-sighted oil companies who realize that the gradual exhaustion of the American petrol-

Jan 1, 1923

By James E. Howard

AT the request of the Council of the Institute, I have the honor to submit the following remarks upon the Program of Tests under which the current work of the Watertown Arsenal Testing Laboratory is carried on, which comprises, among other items, the tests of steel ingot metal and derivative shapes. The intended scope of the tests may be illustrated by extracts from the descriptive part of the program as submitted by the Laboratory under date of April 17, 1907, and subsequently approved by the Chief of Ordnance, U. S. A. Under Item 1, Ingot Metal-Open hearth, acid and basic; Bessemer, acid and basic; crucible; fluid compressed and uncompressed-descriptive remarks were made as follows ; " A thorough, fundamental inquiry into the physical properties of steel necessarily begins with the ingot metal. Investigations, having for their object the improvement of steels, should also begin with the ingot. A knowledge of the ingot structure is essential for judging of the subsequent behavior or appearance of the metal. Under ordinary conditions, so little information is obtained from the ingot in individual cases that practically none of importance is acquired. These remarks have particular reference to the state of physical and structural soundness of the steel. Questions of chemical composition, segregation, piping and the grosser cavities have frequently been given attention. Defects of continuity of structure, which manifest themselves in the working; of the metal, and at the final stages cause distrust in the finished forging, have generally been neglected. ? The range in physical properties in a given composition of metal, as shown in Tests of Metals, 1902 and 1903, is very great. Tests are there found which, when the results are

Mar 1, 1908

A. Scott Reid, London, Eng. (communication to the Secretary*) :—As a constructor of several glass mine-models, .I have read with much interest the description of the model of the Montana-Toriopah mine-workings by Edmund D. North.

Jan 1, 1910

By O. W. Rees, Gilbert H. Cady

Unit coal calorific values represent a close approach to pure coal values; they possess characteristics theoretically inherent in the latter values. They are essentially uniform in the same seam for areas possessing essentially uniform geological environment. They are higher in older than in younger coals in most cases, and in deeper than in shallower coals. In general, they display characteristics closely in accordance with expectation assuming that they are essentially indices of rank. Because it possesses these characteristics, the unit coal value is essentially a standard value, characteristic of each bed in each local region. Hence it can be used as a basis for determining the accuracy of results in newly established laboratories, or when new equipment is installed, or in checking the results of different laboratories, or even in determining the character of coal as mined or prepared if ash, moisture and sulfur values are known. DISCUSSION (A. C. Callen presiding) R. P. Hunson,§ Wayland, Ky. (written discussion).—One of the interesting observatioris made by the authors is that there is a more or less definite correlation between unit coal calorific values and the geological environment of the coal bed. It is very interesting to note that, in general, the unit B.t.u. value increases with the increase in the probable original depth of burial, and that each seam tends to increase in calorific value toward the areas of diastrophic instability. It is generally conceded that Parr's formula, for determining unit coal values, is about as accurate as any formula subsequently proposed for the same purpose. In his formula, Professor Parr did not differentiate between the sulfur present as iron pyrites and that present as organic sulfur. However, the practical application of the formula has shown that this is of little consequence. I agree with the authors that unit coal calorific values are useful ill determining the accuracy of calorimetric determinations, and in determining the character of the

Jan 1, 1934

By Brahm Prakash, R. Schuhmann

Maurice Rey—It may be interesting to note that depressing effects can also be obtained from cyclic compounds other than dyes. One such compound which is a dispersing agent for carbon, pigments and other compounds is known in France by the trade name "dispergine" and in the United States by the name of Lomar P W (Jacques Wolf & Co.) Dr. Rey admits that the compound is not very selective and is similar in its action to starch and dextrin.

Jan 1, 1951

By Brahm Prakash, R. Schuhmann

Maurice Rey—It may be interesting to note that depressing effects can also be obtained from cyclic compounds other than dyes. One such compound which is a dispersing agent for carbon, pigments and other compounds is known in France by the trade name "dispergine" and in the United States by the name of Lomar P W (Jacques Wolf & Co.) Dr. Rey admits that the compound is not very selective and is similar in its action to starch and dextrin.

Jan 1, 1951

By T. B. Counselman

C. G. McLachlan—In the foregoing paper the author has presented a very neat method for calculating the solution recovery for a countercurrent flowsheet. He has, however, based his calculations, as he states, on the assumption that "the concentration of dissolved value must be exactly the same in the overflow and underflow of any thickener." This assumption, which is usually made regardless of the type of calculation used, is "not strictly correct because diffusion of the dissolved gold in the solution associated with the solids as it progresses through the countercurrent system is far from being instantaneous, with the result that on a ton for ton basis, the assay of the solution in the thickener underflow is higher than in the corresponding thickener overflow. An agitator introduced into the flowsheet between thickeners will reduce, but not entirely eliminate, this difference. In practice we have found that the best way to take care of this condition— in addition to the use of one or more intermediate agitators—is to circulate 20 pct or 25 pct more solution than called for by the cheoretical calculation. This presents no difficulty provided that adequate thickener capacity is provided in the original design of the countercurrent circuit.

Jan 1, 1951

By T. B. Counselman

C. G. McLachlan—In the foregoing paper the author has presented a very neat method for calculating the solution recovery for a countercurrent flowsheet. He has, however, based his calculations, as he states, on the assumption that "the concentration of dissolved value must be exactly the same in the overflow and underflow of any thickener." This assumption, which is usually made regardless of the type of calculation used, is "not strictly correct because diffusion of the dissolved gold in the solution associated with the solids as it progresses through the countercurrent system is far from being instantaneous, with the result that on a ton for ton basis, the assay of the solution in the thickener underflow is higher than in the corresponding thickener overflow. An agitator introduced into the flowsheet between thickeners will reduce, but not entirely eliminate, this difference. In practice we have found that the best way to take care of this condition— in addition to the use of one or more intermediate agitators—is to circulate 20 pct or 25 pct more solution than called for by the cheoretical calculation. This presents no difficulty provided that adequate thickener capacity is provided in the original design of the countercurrent circuit.

Jan 1, 1951

By Hisaaki Takata, Nobukazu Nanko, Ichiro Izawa

INTRODUCTION Tochibora Mine belonged to Kamioka Mines, which are located in Gifu Prefecture, the cen- tral part of the Japanese main island, has occupied the important position as a main source of silver, lead and zinc for the smelter of Mitsui Mining & Smelting Co., Ltd.. The annual production of crude ore goes up to about 1 mil- lion metric tons with average grades of 20g/t Ag. 0.31% Pb, and 4.18% Zn. For the last 20 years, the mine has struggled with the depressed zinc metal price in yen and the escalation of operating cost, especially la- bour cost. For instance, prices of commodities and labour cost have been raised 8 times and 14 times respectively during this period. On the other hand, total operating cost has been con- trolled to increase 4.5 times. The productivity of the mine has been increased 4 times by means of improvement of individual works and adoption of perfectly mechanized trackless mining system to reform the mining method. Some improvements are presented as follows; Today, drifting is carried out by the tunnelling crew which consists of 9 operators equipped with 5 Mobile-Jumbos, 2 LHD's and a jeep for carrying and loading ex- plosives. In order to get the high utilization of these machines, each crew manages systematically and continuously adjacent 15 faces under the direction of a forceman. As a result, we have accomplished high advance of drift. Furthermore, raising is carried out by a set of the raise-borer in case of long raises like ore- passes and also by the stage blasting method in case of short ones like slot-cuts. Generally speaking, the sublevel stoping method is considered to be one of the best methods for various respects; high productivity, low cost, easy grade control and safety. This method has been introduced in Tochibora Mine since 1950 and is now widely applied to lodes that could not be mined before by this method be- cause of the shapes of them and the conditions of their country rock. Now we are convinced to be nearly accomplished for our method. This report presents some examples of the standard sublevel stoping method and its variations which are practised at the mine. STANDARD SUBLEVEL STOPING Up to 1979 since 1950 when this method was first applied at the mine, 17 million tons of crude ore have been produced by this method, which amounted to 55% of the total production of the mine. During three decades, the productivity has been increased considerably by means of trackless mining system using large-sized machines and etc.. In other words, mining efficiency has been increased from 20 tons/man.shift to 100 tons/man.shift at large stopes. Formerly undercutting was carried out above the drawing drift by jack-legs and small scrapers and then several cone-shaped glory holes were made by stopers between the undercut level and the draw level. But now, a undercut drift is driven in parallel with the haulage drift at the same level of it. And at the undercut drift, drilling upward is carried out by a large-sized machines like the fan drill in order to extract the broken ore directly at the drawing drift connected with the haulage drift. Simplification of the work as well as utilization of large- sized machines enables to get higher productivity. But if the deposit is comparatively wider and the broken ore around the middle part of the deposit cannot be extracted, several drawing drifts are driven to the deposit and in order to minimize dead ore at the final stage of operation, the

Jan 1, 1981

By John Chipman

THE equilibrium between titanium in liquid iron and titanium oxides has been studied by Hadley and Derge.' They have shown that a minimum occurs in the oxygen content of the metal between 0.1 and 1.0 pct Ti, but its exact level was not fixed. The oxide phase in this minimum range was principally TiO, containing some iron oxide. On the other hand, for concentrations above 5 pct Ti the oxide phase was TiO and the oxygen content of the metal increased rapidly with increasing titanium content. From their observations and the free energy of Ti0 and TiOz reported by Kelley and ah,' it is possible to derive approximate values for the activity coefficients of titanium and oxygen in liquid iron-titanium alloys and the conditions for equilibrium in steel deoxidation. Neglecting possible departures from the stoichio-metric composition, the condition of equilibrium with Ti0 may be expressed as follows: TiO= Ti_ + C) log K = log NTl + log [% O] + log yTi + log fQ Here as a matter of convenience the titanium concentration is expressed in mol fraction while that of oxygen is in weight percent. The activity coefficients are yTi and fo. The value of log fo approaches zero as the concentration of titanium approaches zero, while that of log yTi approaches a limiting value of In Fig. 1 the sum of log NTi + log [% 0] is plotted for mol fractions of titanium between 0.05 and 0.50. The smooth extrapolation gives a value of —4.15 which corresponds to log K — log y:i . We therefore have the equation: According to the data of Kelley and Mah,' the free energy of formation of Ti0 at 1900°K is -82,400 cal. The free energy of solution of half a mol of oxygen in iron, taking 1 pct 0 as the standard state, is -29,300 cal. From these we write: From these equations the activity coefficient of titanium at infinite dilution in iron is found to have a value of 0.011 or log y°. = -1.96. This is only an approximate value but is certainly better than the estimated 0.05 in Basic Open Hearth Steelmaking To obtain approximate values for the activity coefficient at intermediate concentrations, it is as- sumed that log yTi(l is constant and equal to -1.96. This corresponds to a value of E;: = 3 In yTi/aNTi = 9.0 which is not unreasonable We now have the value for the activity of titanium and the percentage of oxygen in equilibrium with TiO. It is therefore a simple matter to calculate the activity coefficient of oxygen which is shown in Fig. 2. The effect of titanium is rather large, being comparable to that of vanadium, but not so large as has been reported for aluminum. The slope of the line at low concentrations corresponds to E: = aln yo/ aNTi=-0.37. At concentrations below 1 pct Ti the deoxidation constant and oxygen content for equilibrium with TiO, can be calculated from the foregoing data and the free energy of formation of TiO,, which according to Kelley and Mah is -144,600 cal at 1900°K. The free energy of solution of oxygen has been given; that of Ti to form a dilute solution with 1 pct Ti as the standard state is RT ln (0.5585 y:i/47.9) = -34,800 cal. From these data we find (for concentrations in wt pct): TiO, = Ti + 2 -0; hFTgO0= + 51,200 cal log if =-5.89 The interaction coefficients, concentrations being expressed as wt pct, are e;: = alogfTi/a[% Ti] = +0.048 and e:' = a logfo,/a[ojTi] = -0.187. The calculation gives the following results which, in view of the impurity of the oxide phase, must be regarded as approximate:

Jan 1, 1961

By D. H. Shaffer, W. F. Harris, W. M. Hickam, M. H. Loeffler

Experiments have been performed on the quantitative addition to niobium of enriched isotopes 018 and 017 at the 0.1 - 40 micro-gram level and their subsequent recovery. A measured quantity of molecular oxygen of known isotopic concentration is added to niobium metal by oxidation. Recovery of the enriched isotopes as carbon monoxide is by the vacuum fusion technique. Quantitative determinations of the enriched isotopes are made in standard volumes at constant temperature using accurately calibrated micromanometers and the mass spectrometer as pressure measuring instruments. THE presence of low concentrations of nonmetallic impurities in metals can often adversely affect the physical properties of the metal. The increase in hardness and the embrittlement of refractory metals due to oxygen is well known. In metallurgical studies dealing with the diffusion rates or the effect of oxygen on the physical properties of refractory metals, it is often necessary to add small quantities of oxygen to the metal and later recover the total quantity present. It is desirable, therefore, to establish the accuracy with which microgram quantities of oxygen can be added to niobium and recovered by vacuum fusion. The successful addition of microgram quantities of oxygen to metals by the usual manometric techniques and the subsequent recovery by vacuum fusion is difficult because of the uncertainty in the accurate determination of the quantity of oxygen originally present in the metal and because of the chance of contamination by atmospheric oxygen. In order to minimize these uncertainties earlier workers have added quantities of O16 at levels much higher than the oxygen concentrations that are of interest.'-3 In order to eliminate the uncertainty associated with the O16 additions to metals at low microgram levels, experiments have been performed on the quantitative addition of oxygen highly enriched in O17 and O18 at the 0.1 to 40 pg level to niobium and the subsequent quantitative recovery of the isotopes by vacuum fusion. Since the natural abundance of O17 is 0.04 pct and of 0" is 0.2 pct this enriched oxygen provides a uniqueness from interference not achieved in earlier work.'-= A measured quantity of molecular oxygen of known isotopic concentration is diffused into the metal. Recovery of the isotopes in the form of carbon monoxide is by vacuum fusion. The total quantity of gas is determined in standard volumes at constant tempera- ture using accurately calibrated Consolidated Electrodynamics micromanometers and the mass spectrometer for pressure measurements. The molecular and isotopic composition is determined mass spectrometrically. APPARATUS A schematic of the oxygen addition apparatus is shown in Fig. 1. Take-offs are provided for the attachment of the isotope container and for sample bulbs which are used to transfer samples to the mass spectrometer. Metal valves are used throughout the system including the sample bulbs in order to achieve a vacuum of 10"6 mm Hg. Evacuation is accomplished with a 3-stage oil-diffusion pump backed by a mechanical pump. A liquid nitrogen trap is used to remove condensables and to prevent oil vapor from entering the system. A micromano-meter is used for pressure measurements. The furnace assembly is shown in Fig. 2. It consists of a quartz tube joined to the apparatus through a 40/W joint with Apiezon W low-pressure wax. The furnace cap, also a 40/W pyrex joint, is provided with a pyrex hook. The sample is suspended from this hook with a platinum wire. The total volume of the furnace section is 435 ml. All volumes were determined by expanding a known volume of gas at a known pressure into the evacuated system and re-measuring the pressure. Both the micromanometer used on the oxygen addition system and the micromanometer used on the mass spectrometer were compared to a precision

Jan 1, 1961

By J. Kent Smith

VANADIUM is generally spoken of as a rare element; but, even in the light of our resources as known a couple of years ago, this description could be accepted in a qualified sense only. In fact, vanadium is very widely distributed, being a constituent of most clays, while even caustic soda has been shown to contain almost regularly a minute proportion of it, although the quantity in each case is so small as to render impracticable the extraction of the metal there from with profit. The opening-up of a large deposit of vanadium sulphide ore in South America has put a new phase on the commercial outlook of vanadium, the technical value of which for the improvement of steel has been proved by rigorous scientific investigation.

Sep 1, 1907

By Max Boehmer

(Pittsburg Meeting, March, 1910.) AFTER 30 years of development and after an output of $350,000,000 in value of gold, silver, lead, zinc, and copper, there has not been published a satisfactory explanation of the origin of the immense deposits of the Leadville district. The original examination find survey of Leadville by members of the U. S. Geological Survey was a most magnificent piece of work, but their attempt to explain the origin of the ores was based upon the then-accepted theory of lateral secretion, originated by Sandberger, which theory was afterwards disproved in many cases by further development in numerous districts. This theory contended that the ore in the veins had been leached by surface-waters from the eruptive rocks in the immediate vicinity, and it had its origin in the fact that the neighboring eruptive rocks all contained, to an appreciable degree, the several metals found in the ore-deposits. But the practical miner, reasoning in a simple manner from the condition of things as he found them underground, soon discovered the fallacy of this proposition. He reasoned that, in the case of the Leadville deposits, this theory could not be true, because, if the ores were leached from the overlying eruptive rocks by surface-waters, they would as a matter of necessity be controlled by the action of gravity, and the main bodies would collect in- natural depressions of the underlying limestone, and at all points where such depressions existed. But this was not in accord with the channels of ore as he found there ; and hence the theory of lateral secretion in this district was never accepted. Another objection to it consisted in the fact that large areas within the ore-bearing district contained no ores whatever, although their formation was the same, and the same limestones were covered by the same thick sheet of

Feb 1, 1910

By V. F. Swanson

At the AIME meeting in Tampa in Oct. 1966, an empirically developed equation was presented which allowed the calculation of free settling velocity for any sized particle: 1 [ ] This equation requires the use of two parameters a and p which are coefficients derived from boundary layer theory.2 It was possible to develop values of a and p for several minerals by back calculation of published data. The original equation had one major flaw. When the fluid density exceeds the density of the solids, the solution to the equation becomes imaginary. A flaw was indicated also by the fact that galena and sylvite both having cubic cleavage, did not have similar values for a and b. Galena gave calculated values of a = 1.082 and g = 3.11, while sylvite gave values of a = 1.870 and p = 2.56. These flaws prompted further study of the equation, resulting in the following empirical modification: [ ] It is obvious a real solution of the equation is possible for all values of ps and p. When PL > PS, V is negative, indicating that the particles will rise against the attraction of gravity. The validity of the modification is borne out by the fact that when values of a and p were back calculated for galena and sylvite using the modified equation, both minerals gave values of a = 1.038 and p = 3.01. With the modification shown in Eq. 2, Newton's friction factor becomes [ ]

Jan 1, 1976

By Ednlund D. North

Discussion of the paper of Edmund D. North, presented at the Spokane meeting, September, 1909, and published in Bulletin No. 37, January, 1910, pp. 21 to 25. A. SCOTT REID, London, Eng. (communication to the Secretary*) :-As a constructor of several glass mine-models, I have read with much interest the description of the model of the Montana-Tonopah mine-workings by Edmund D. North. As an interchange of ideas and experience is always an advantage, and in view of the fact that such models are coming more and more into vogue, perhaps the following remarks on this subject may prove of interest to mining engineers generally and to Mr. North particularly. In the model of the Waihi gold-mine, New Zealand, which I constructed, a dust-proof case is used. The top, bottom, front, and two ends are of glass; the back only is of wood, painted a dull white, against which the mine-workings show very distinctly. Each mine-level is represented by a horizontal sheet of glass, supported on metal runners fixed to the uprights at each end of the case, in a manner similar to that described by Mr. North. The corner uprights are strengthened by having a metal band screwed to the inside face of each, to which the metal runners or supports for the sheets of glass are screwed in turn. The reason for having this additional strength is that as the mine is developed in depth, and fresh levels are opened, the increasing weight of the glass sheets, added to the model, caused the unsupported wooden uprights to bend slightly, so that the glass sheets-did not fit in with the desired nicety, and co-ordination was, to a considerable extent, lost. Strengthening the uprights in this manner is not important in models of mines in which only a few levels have been opened, or when the sheets of glass are small, but in the Waihi model there are 15 sheets of glass to be supported, and more to be added as development proceeds, and the weight is considerable.

May 1, 1910

By E. E. Thurlow

The Geology Div. of Northern Pacific Railway Co. has adapted to its exploration efforts field procedures for geochemical sampling and semi-quantitative analysis which have been developed through research by the U. S. Geological Survey. The sampling is done in conjunction with reconnaissance geologic mapping on aerial photographs or during field checking of maps which have been prepared largely by photo-geologic interpretation. Stream sediment or soil samples are taken and readily soluble combined heavy metals are extracted with ammonium citrate followed by colorimetric titration with dithizone at the sample site. The effectiveness of this approach has been demonstrated both in positive and negative results, thereby assisting in the elimination of large areas of land from further immediate attention and in providing targets for followup exploration. An occa sional sample is submitted for spectrographic analysis as a check on the possible presence of other elements of economic significance. Field laboratory procedures are also being implemented for determining molybdenum, mercury, and other metals which may be valuable in themselves or useful as pathfinder elements in outlining mineralized areas. A lead-zinc occurrence in Oregon and a copper deposit in Montana were readily detected and outlined by stream sediment and soil sampling and a heavy metal anomaly that lacks obvious interpretation has been found in northwestern Montana. Detailed mapping and additional sampling are followed by other exploration techniques if warranted. Northern Pacific's program of reconnaissance mineral evaluation of company-owned lands and adjoining areas was outlined in a paper presented at the American Mining Congress meeting in Las Vegas four years ago. That report included policies and procedures with respect to mineral development on Railway Co. lands and may be referred to for information on these matters.1 In a sense this paper is a progress report on the use of geochemical prospecting in Northern Pacific's continuing mineral evaluation program. At this time there are positive results but as yet there is no real success story in the form of a minable ore body. GEOCHEMICAL PROSPECTING PROCEDURES The decision to use geochemistry as a reconnaissance exploration tool must be followed by research into sampling and analytical methods and into the interpretation of results. Various analytical methods were tried and evaluated by the Geology Div., including hot and cold acid extraction with and without fusion of the sample, panning and magnetic separation followed by dithizone testing of the magnetite, and cold aqueous extraction of metallic ions followed by indicator tests. Samples were first sent to the laboratory for analysis; later field laboratories were established and now virtually all testing is done at the sample site. It was concluded that, where applicable, the quickest dependable methods for reconnaissance use are the dithizone field tests for readily extractable heavy metals. This involves the simultaneous treatment of a sample, usually of soil or stream sediment, with two immiscible liquids; one a cold aqueous extractant (ammonium citrate) and the other a solution of dithizone in toluene or xylene.2 Dithizone is a colorimetric indicator that reacts quantitatively with copper, lead, zinc, and several other metals to form colored complexes in organic solvents. Results may be expressed in ml of 0.001 pct dithizone that are required to reach the blue end point, or calibration of the test results can be carried out with standard solutions of zinc; conversion factors would then be expressed in ppm, zinc equivalent. Calibration of dithizone solution with zinc standards indicates that 1 ml of 0.001 pct dithizone is equivalent to approximately 0.25 ppm of zinc. An authoritative report on dithizone field tests authored by H. E. Hawkes in the June-July 1963 issue of Economic Geology* states "The appeal of these techniques has been the simplicity and speed of the determinations as compared with more tedious laboratory determinations of trace metals in weathered rocks, soils, or plant materials. This obvious appeal, however, has often been more than matched by misuse of the method in such a manner that the results are

Jan 1, 1964

By J. E. Hilliard

AS is well-known, the length per unit volume, Lv, of any lineal feature (such as grain edges in a polycrys-talline specimen) can be estimated from a count of the number of point intersections with a random plane of polish. Specifically:' Lv = 2NA in which NA is the expected number of intersections per unit area of the plane. As with all other measurements in quantitative metallography, the estimation of Lv is subject to a sampling error, the magnitude of which will depend on the number of observations. The analysis is usually performed by counting the number of intersections falling within a closed test figure of known area applied to a succession of different areas on the plane of polish. The test figure can be drawn directly on the screen of a projection microscope or else superimposed on the image of the structure by means of a reticule in a focusing eyepiece of an ordinary microscope. The use of micrographs is very inefficient unless, as in the present study, these are also needed for some other purpose. Consider an analysis in which n applications are made of a test figure within which the expected number of intersections is N. The expected total number of intersections counted is then given by NT = nN If (N) is the standard deviation in N for one application of the figure and if the latter is applied to non-overlapping regions so that the N's are independent in the statistical sense, then the standard deviation in Nt is given by: a(NT) = a(N)vn Eliminating n from Eqs. [2] and [3] we obtain: Thus, k will be a constant for a given specimen and test figure. From Eqs. [ I] and [4] we find As is to be expected, therefore, the fractional error in the estimation of Lv is inversely proportional to the square root of the total number of intersections counted. It is very desirable to have at least a rough estimate of k before starting an analysis, since it will then be possible to decide in advance by use of Eq. [5J how many counts should be made in order to achieve the desired accuracy in Lv. Without such information the investigator, unless lucky, will either do needless (and tedious) work or else obtain a result with too large an error. It is very easy to calculate k for the limiting case of N — 0, i.e., when the test figure is vanishingly small. In this case there is a negligible probability of two or more intersections falling within the figure. There are therefore only two possible outcomes: a count of one with a probability of, say, p and a zero count with a probability of (I-p). Thus and Therefore: We might expect k to depend on N and therefore on the size of the test figure. Such a dependence was observed2 in the analogous case involving the estimation of grain-boundary area per unit volume by a count of the number of intersections of a test circle with traces of the boundaries on the plane of polish. In this case the theoretical value of k at the limit N — 0 was 1.41. It was also predicted that k would display an initial sharp decrease with increasing N. Experimentally, k was observed to decrease to a value of 0.62 at N - 6 and thereafter remain approximately constant. Furthermore, the value of k for N > 6 was found to be insensitive to the form of the structure provided no pronounced anisotropy or grain-size variation was present. In order to determinewhether k would exhibit a similar dependence on N in the estimation of grain-

Jan 1, 1967

By A. G. Metcalfe, A. Siede

The hardening of annealed copper during fatigue testing appears to be independent of the applied stress and to occur largely within the first 4000 cycles. Copper hardened by fatigue is more resistant to annealing than copper hardened by static means, and softens by a multistage process. Creep studies at 300°C show that copper hardened by fatigue also has greater resistance to creep than statically hardened copper. Some theoretical explanations are discussed. RECENT interest in the behavior of metals subjected to fatigue stems from observations of phenomena which could not be explained by current theories of the structure of metals. In 1953 Bullen et al.l showed that the hardening caused by fatigue at low stresses did not cause severe bending of the lattice as did hardening by static methods. This was later confirmed by Wood, 'and Broom and Ham.3 Clarebrough et al4 showed that as the stress level used in fatigue hardening was increased, bending of the lattice was introduced, eventually approaching that of metals deformed by conventional cold-working methods. The type of hardening introduced by fatigue has other interesting characteristics. Kemsley5 showed that copper fractured by fatigue at low stresses resisted annealing as compared to copper hardened an equal amount by static means. The work of Clarebrough etal, shows that the manner of energy release during annealing differs for fatigue-hardened and statically hardened metal in both magnitude and temperature range of release. In addition to hardening of the lattice, fatigue has been shown to cause softening in materials previously hardened by static methods,5 and also in age-hardened alloys.7 The superposition of a small fatigue stress on the static loading of high-temperature alloys has been shown to increase their resistance to creep.' The present work was an attempt to determine the relationship between fatigue hardening, resistance to annealing, and the creep properties of pure copper. EXPERIMENTAL PROGRAM The program described here was designed to answer three questions: 1) Can stress-cycle combinations well below the failure values give significant increases in hardness? 2) Does hardening, under different stress-cycle combinations, give increase resistance to annealing? And if so— 3) Does superior resistance to annealing confer superior creep properties over statically hardened material? Three-quarter hard OFHC copper was annealed in vacuo at 550°C for 1 hr to produce a strain-free material having a fine grain size and uniform hardness. (The standard deviation of the mean hardness of the annealed samples was less than + 1.9 Dpn). Annealing was performed after machining the fatigue specimens so as to avoid work-hardened surfaces. Jigs were used to avoid distortion. The fatigue properties of the annealed copper were determined using an accurately aligned Baldwin-Sonntag SF1-U machine operating at 1800 cycles per min. This limited the minimum number of cycles which could be examined to about 4000 stress reversals. Since failure resulted in specimen damage, hardness increase with number of cycles was measured by testing specimens fatigued to different fractions of the failure values. The results are shown in Fig. 1, and are superimposed on the S-N curve of the copper in Fig. 2. The resistance to annealing of fatigue-hardened material was compared to that of material hardened by uniaxial tensile straining. Specimens hardened to equal values by both methods were progressively annealed for 1 hr at temperature in vacuo. After each annealing treatment the hardness was measured using a Leitz Durimet hardness tester with a 500-g load. At least five tests were made for each hardness determination. The standard deviation for individual specimens varied from 0.26 to 1.48 hardness points. The results are shown in Figs. 3 to 5. The discontinuous nature of the annealing process has been brought out by drawing idealized curves through the data points. This can be justified by the consistency of the results as well as by general agreement with results of Kemsley.5 The creep resistance of fatigue-hardened and

Jan 1, 1960

By Thomas C. Wilder

ALTHOUGH there is an abundance of thermodynamic information available in the literature today, no experimental data on the standard molar properties of formation of zinc oxide have ever been reported for the temperature range 419.5" to 908°C. This is the temperature range for which zinc metal is a liquid. so that the formation reaction is: Data have been reported for Reaction [I] where zinc is a solid or a gas. Maier. Parks, and nderson' measured the electromotive force of the cell: in order to obtain the free energy of the reaction: over a limited temperature range. With the known properties of H2O, those of ZnO were calculated. These workers found that t;j of ZnO is -75,930 ± 150 cal per gfw and Mtf is-83,000 300 cal per gfw at 25°C. akolkin made similar measurements to obtain ilF7 and AH; of -75,870 and -82,540 cal per dw respectively at the same temperature. Truesdale and arirlg and Kitchener and 1gnatowicz4 measured the equilibrium of the reactions: respectively, in order to determine Ff of ZnO from the known values of CO, CO2, and H/X The thermodynamic properties of ZnO, presumably taken from the above investigations, are tabulated by Kubaschewski and vans' and Wicks and Block" The latter reference also gives values for the range where zinc is a liquid. These numbers are probably acquired from the known extremities of the range plus Cp data of the components. In the present work the electromotive force of the cell: was measured in order to calculate the properties of ZnO from the well known values of NiO for the temperature range where zinc is a liquid. In Cell [B] the cathode reaction is: and at the anode: The overall reaction is: for which the free energy change is: where is the electromotive force in volts of cell [B] after correction for the Pt-Ta thermocouple. The standard molar free energy of formation of NiO is very well known as a function of temperature. Kiukkola and agner's data are used in most tabulations. The error is probably less than I00 cal per gfw, The latter authors were the first to use solid mixed oxide electrolytes in galvanic cells. Their work with NiO and other oxides was performed with cells similar to Cell [B] using a variety of reference electrodes of fixed oxygen potential. There may be a small composition range for which either NiO, ZnO or both exist. If nonstoichiometry does exist for these oxides, then the properties described herein are those for the metal saturated compositions. The simple cell design was the same as described elsewheres except that the molten metal electrode was about 125 g of pure zinc including a small (0.25 to 0.50 g) amount of ZnO. The mixture of pure nickel and NiO powders making up the reference electrode was contained in a tube of the ZrOl + CaO electrolyte which was immersed in the molten zinc. A platinum contact was made to the reference electrode; tantalum to the zinc. A refractory cement plug was necessary at the open end of the electrolyte tube in order to prevent zinc vapor from contaminating the reference electrode. Experimental details such as the vessel containing the cell, furnace, temperature control and measurement, and electromotive force determinations of the cell have all been outlined previously. The temperature was varied randomly in the range between the freezing and boiling points of zinc. After each temperature change, time was allowed for the drift at the new temperature to be less than +;"c whereupon a series of three cell readings was taken at least 10

Jan 1, 1970

By C. Kremer Bain

UNDER present economic conditions the necessity of mechanizing the mines of our country has become a very important problem. More and more mines are looking toward increased or complete mechanization of their operations, so in the writer's opinion it is quite pertinent that some of the associated problems that accompany such a program be pointed out. The following generalization on attempting a comparatively slight change in mining methods at the Southeast Missouri properties of the St. Joseph Lead Co. is an attempt to point out to anyone faced with a mechanization program that much time and C. KREMER BAIN, Member AIME, is Assistant to General Manager, St. Joseph Lead Co., Bonne Terre, Mo. AIME Sun Francisco Meeting, February 1949. TP 2743 A. Discussion (2 copies) may be sent to Transactions AIME before March 31, 1950. Manuscript received Dec. 27, 1948; revision received Oct. 13, 1949. effort can be saved, and many headaches avoided, if company policy can be established whereby everyone in the organization from the top down is desirous of improvement and is working towards the common objective. Any changes in mining methods, machinery, and so on, must entah coordination of all the other phases of mining as they all have to mesh as accurately as a smooth running chain of gears if satisfactory results are to be obtained. The purpose of this paper is to point out some of the problems which :have to be surmounted when any mechanization program is attempted, rather than to go into the mechanical details and actual operating data of the equipment employed. After all, machines have to be adapted to best suit the local conditions, so no general formula can be given that would apply to other properties. Although St. Josepll Lead Co. has been mechani-cally-minded for a number of years, as shown by the fact that over 110 million tons have been loaded mechanically since 1922, any further mechanization or changes always present a problem. When our ore bodies were of great height and area the breaking and loading were developed to a high degree of efficiency according to known standards. But in recent years, when our ore bodies became smaller and more scattered, the amount of tonnage we were able to break was not sufficient to supply our shovels with enough rock to keep them working to capacity. Our first step in attempting to rectify this situation was to develop a technique of moving the shovels to the broken ore in various stopes, which sometimes entailed a move each shift. A shovel is not producing when being moved, so within the last two years we have been endeavoring to devise some means of getting more rock broken in these smaller stopes and it was then that we became interested in jumbo drilling. To illustrate the fact that mechanization is a process of a chain of developments rather than a stroke of genius can best be shown by a general summary of conditions and obstacles which were encountered in our present attempt to establish template drilling of a standardized round. Our first jumbo was more or less the conventional type with two machines mounted on a crossbar. This arrangement proved to be impractical to duplicate satisfactorily the regular routine of slabbing in a more or less radial pattern as carried out by column drilling. One machine was either too close to or too far from the face and there was another disadvantage in that one drillman was frequently delayed while waiting for his partner to bottom a hole. Our next step was to eliminate the crossbar so the machines could operate independently of each other, but we still encountered the same objections mentioned above except that one drillman was free to drill three holes instead of one in a vertical plane independently of his partner. Time studies while trying to adapt the jumbo to the regular slabbing practice as accomplished by column drilling, revealed that twice as much time was spent in maneuvering the jumbo into position and aligning the holes as was consumed in drilling.

Jan 1, 1951