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By M. A. Grossman

The harden ability of most steels can be predicted within 10 to I5 per cent provided the complete chemical composition is known, including "incidental" elements; and provided the as-quenched grain size is known; and provided, finally, that the composition and heating temperatures for hardening are such as to result in austenite free from carbide particles. In the method proposed herein, the steel is considered as having a base hardenability due to its carbon content alone (the hardenability of a "pure steel" of the given carbon content, without any other elements), and this base hardenability is multiplied by a multiplying factor for each chemical element present. After multiplying all these together, the final product is the hardenability. Grain size may be taken into account either in the base hardenability or after the multiplication. Hardenability is stated in terms of "ideal critical diameter", namely, the diameter of bar, in inches, that will just harden all the way through (absence of un-hardened core) in an "ideal" quench, and the calculation may also be related to the Jominy test The data bring out certain features rather clearly. For example: i. It is quite useless to attempt to predict hardenability unless all elements, including "incidentals,,) are known; thus an "incidental,, chromium content of 0.20 per cent increases the hardenability by about 50 per cent. 2. The relative effectiveness of different alloys is sometimes unexpected; thus molybdenum when calculated in this way appears to be of the same order of effectiveness as manganese, rather than much more powerful, as would appear to be common experience; observe that an increase from no manaanese to 0.20 per cent Mn provides a multiplying factor of 1.67, and an increase from no molybdenum to 0.20 per cent Mo provides a factor of 1.63, an increase of over 60 per cent in each case. However, if to a steel containing 0.50 per cent Mn there is added "20 points of manganese," the factor is raised from 2.65 (for 0.50 per cent Mn) to 3.35 (for 0.70 per cent Mn), or an increase of only 26 per cent. Thus the fist small addition of an element has a much more powerful percentage effect than an equal further addition when some is already present, and in most cases the effect of molybdenum is considered in relation to a steel in which molybdenum is absent. 3. If two elements are equally effective, a greater hardenability will be obtained by using, for example, 0.5 per cent of each than by using I.o per cent of either of them alone. 4. A knowledge of the as-quenched grain size is essential for precise work, since a difference of only one grain size number (say No. 7 instead of No. 6) makes a difference of almost 10 per cent in hardenability (in these units); this, however, does not apply to certain It should be emphasized that in chromium steels (over 0.30 per cent Cr) and chrome-molybdenum and chrome-vanadium steels, un-dissolved carbides are likely to be present in the steel as quenched, and that in such cases the charts can indicate only a maximum Passible hardenability, whereas the extent of hardening actually obtained may be much less. Thus tests on a number of chrome-molybdenum steels have indicated a degree of hardening amounting to only 50 to 65 per cent of the maximum possible, and in chromium steels from full hardening (100 per cent) down to as low as 70 per cent. On the other hand, when the amount of such elements is small (Cr under 0.30 per cent, Mo up to 0.25 per cent in the

Jan 1, 1942

By E. V. Kleber, V. F. Novy, R. C. Vickery

The constitutional diagram has been determined in part for the sgstem Gd-Fe. Seven intermetallic compounds have been found at compositions corresponding to the following Gd-Fe ratios; 2:3, 1.2, 1:3, 2:7, 1:4, 1:5, and 2:17. The GdFe, com-pound has a congruent melting point above 18000C, whereas all of the remaining compounds melt incongruently, A eutectic exists at 13 wt pct Fe at a temperature of 860°C. ALTHOUGH an increasing amount of information is becoming available on the metallurgy of pure rare earth metals, relatively few studies have been made on alloy systems of the rare earths with the transition metals; iron, nickel, and cobalt. Even less data are extant on gadolinium alloys although it could be expected that such alloys might possess interesting structural and magnetic properties. In this paper, we report investigation of the gadolinium-iron alloy system. Studies on systems containing nickel and cobalt will be presented in subsequent papers. Previous data on gadolinium-iron compounds have been reported by Endter and Klemm1 and Jep-son and Duwez.2 Both reports agree on the existence of the GdFe2 phase, which crystallizes with the C-15type structure (face-centered cubic). This is in accord with results of the present work. EXPERIMENTAL The gadolinium metal used was prepared by met-allothermic reduction of high purity gadolinium fluoride. A typical analysis of the metal thus produced indicated the principal impurities to be oxygen, 0.24 pct, and tantalum, 0.2 pct. The iron metal used for alloying was a reagent grade material. Alloys were prepared by arc melting mixtures of the respective metals. Appropriate quantities of the two component metals were carefully weighed, blended and compacted. The compacts were then melted in an arc furnace consisting of a water-cooled copper hearth plate and a water-cooled tungsten-tipped counter electrode contained in a brass vacuum chamber. The furnace was evacuated to an absolute pressure of less than 1 with the leak rate established as being less than 20 per min. The furnace was then back-filled to a pressure of 25 mm of Hg, with a 75 pct He-25 pct Ar mixture. Arc melting at 25 v and 300 amp was maintained for about 30 to 60 sec until the entire visible area of the sample became molten, by which time surface tension had drawn the molten metal pool into a large bead. After allowing the furnace to cool, the alloy button was inverted and the melting process repeated. A series of melts was made covering entire composition ranges from 100 pct Gd to 100 pct Fe. All samples were examined metallographically in the as-melted condition. As the phase diagram became rationalized, and differential thermal analysis had given indications of temperature arrests, annealing was carried out in vacuo or in argon. Generally, compositions containing more than about 60 pct Gd were heat treated at 750°C and alloys containing less than this quantity of gadolinium were annealed at 1000°C. Prolonged annealing times were of the order of 100 to 200 hr. Metallographic examination was repeated on the annealed materials. Although little material loss was noted during alloy preparation, chemical analyses were made on all specimens prepared. The following standard, analytical techniques were used. Samples were dissolved in hydrochloric acid; insoluble material was filtered off, ignited and fused with potassium pyro-sulfate. The cold melt was leached with dilute acid and the solution thus obtained added to the main sample solution. Gadolinium was always determined gravimetri-callv as oxide from oxalate ignition. Iron was removed from an aliquot sample by electrolysis on a mercury cathode at approximately six volts. Gadolinium in the iron-free electrolyte was then precipitated as oxalate which was subsequently ignited to oxide. Iron was determined volumetrically in an aliquot solution by reduction with stannous chloride fol-

Jan 1, 1962

By T. D. Murphy, G. V. Henderson

The element silicon, with its usual partner, oxygen, plays the same role relative to inorganic materials as carbon and hydrogen play with respect to living organisms. The crystallographic structure of silicon dioxide (SiO2) consists of one atom of silicon well-nigh inseparably bonded to four contiguous atoms of oxygen, a gas of but slightly more than half its atomic weight, forming a three-dimensional network of SiO4 tetrahedra (Dietz, 1968). This wispy arrangement is the fabric of the mineral quartz which is one of the harder, more abrasive, and chemically stable raw materials to be found in Mother Nature's cupboard. Most of us are vaguely familiar with the observation that nearly 60% of the lithosphere to an approximate depth of 10 miles is composed of these two elements, which proportion actually rises to about 75% if the atmosphere, hydrosphere, and biosphere are included (Parker, 1967). Elemental silicon is a brittle steel-gray metalloid with a density of 2.42 and does not occur in nature. In its limited commercial form, which is still brittle and metallic in appearance, its density drops to 2.33. It combines with oxygen to form the gaseous oxide SiO, or the solid dioxide Si02 (analogous to its congener carbon in CO and CO2); a tetrachloride SiCI4 (analogous to CC14); or, combining with oxygen and one or more metal ions, forms the largest rock-making family of all, the silicates. Further, next to the feldspars, quartz is the most abundant known mineral and, in some form or another, accounts for roughly 12% of surficial terrestrial rock. It is this so-called "free silica" to which your attention is chiefly directed in this chapter. In any such consideration of silica, its several crystalline phases with their attendant differing physical properties appear worthy of delineation. Alpha quartz is the only one of this interesting polymorphic family that is thermodynamically stable at normal pressures and temperatures up to about 573°C. The low phases of tridymite and cristobalite can exist in the so-called metastable state below 117° to 200ºC but seldom occur in nature in these two different crystal forms (Sosman, 1965). Opaline silica, now considered by most researchers to be a variety of cristobalite, occurs in abundance and is the only exception. The three remaining polymorphs, keatite, coesite, and stishovite, also are metastable under ambient conditions. Keatite, however, is not known to occur naturally and has only been synthesized in the laboratory. The other two have been identified in submicron sizes and in microscopic amounts, occurring naturally as a result of high order shock-wave pressures generating quite elevated temperatures --such as might accompany the impact of a large meteorite on a hard sandstone terrain (Chao et al., 1962). An intriguing characteristic of these silica minerals, and one which has very practical applications, is their extremely variable densities. The classic 2.65 specific gravity of alpha quartz drops to 2.20 in tridymite, cristobalite, and lechatelierite (natural silica glass), as well as in many man-made glasses of commerce which are merely noncrystalline or amorphous solids in the form of super-cooled liquids which can no longer change their shapes (Pauling, 1950). It rises again to 2.50 and 2.93 for keatite and coesite, respectively, and finally becomes a reported 4.35 for stishovite-nearly a 50% range in density for the known physical combinations that silica naturally assumes (Frondel, 1962; Konnert et al., 1973; Pecora, 1960). Pursuing its esthetic aspects, briefly, silica is well-represented among gem stones which, to qualify as such, must have the attributes of beauty, durability, and rarity (Jahns, 1983). As quartzose gems usually have but one or, at

Jan 1, 1983

By J. E. Fox Jr., J. L. Lummus, J. P. Gallus

Fresh water or brine drilling fluids may be kept free of suspended drilled solids by the addition of a water soluble acrylamide-carboxylic acid copolymer at the flowline. Addition of from .01 to 0.2 lblbbl of the polymer solution to drilling fluids containing less than 5 per cent clay solids by weight causes the solids to flocculate and settle rapidly to the bottom of the pits. Solutions of the polymer injected at the pump suction reduce the loss of water to permeable formations without impairing the permeability to oil. The use of drill-itlg fluids clarified with the polymer has resulted in increased drilling rates, extended bit life, and lower drilling fluid costs. INTRODUCTION Field experience and the results of a number of investigations have established that the accumulation of solids in drilling fluid reduces drilling rate.'-' Drilling with water makes possible higher drilling rates than can be achieved with mud but in many areas drilling with water may not be feasible because of the possibility of encountering high formation pressures or by-dratable formations. To combat these conditions, the drilling fluid must possess certain physical properties such as viscosity, density, fluid loss, etc., which require the presence of solids. The current trend in drilling fluid treatment is to maintain as low a percentage of solids as is possible without harmfully affecting the mud properties needed for drilling. Mechanical separating devices such as wet cyclones and decanting-type centrifuges are proving to be an economical means of controlling the percentage of solids and thereby maintaining low solids muds. Also: special muds have been developed for the purpose of retarding the hydration of drilled solids so that they may be more easily removed by shale shakers or settling pits. In some areas, such as West Texas, the characteristics of some formations will permit drilling with water. However, because of the dispersion of drilled solids, it is usually not possible to maintain clear water even with the aid of mechanical separators, or by utilizing large settling pits. For this reason the commonly used term "water drilling" is a misnomer since the water usually contains some solids. Because of the improved drilling rates and other benefits which might be effected, a laboratory and field study was made of the use of flocculating agents for maintaining clear water for drilling. PROCEDURE Laboratory—Solids Settling Two techniques were employed to determine the effectiveness of flocculating agents in settling solids from drilling mud. First, the rate of fall of solids was measured in graduated beakers containing mud treated with various flocculating agents. Natural gum, oil-in-water emulsions prepared with ethoxylated nonyl phenols and diesel oil. and a powdered synthetic acrylamide-carboxylic acid copolymer* (hereinafter referred to as "polymer") were tested as flocculating agents in both fresh water and salt saturated muds containing 4 per cent solids. The polymer was not added in the powder form directly to the muds but was first dissolved in water in a concentration of 3.5 lb/bbl. The polymer solution was then added directly to the mud. The concentration of the flocculating agents, including the polymer, was varied. High rates of fall of the solids indicated high flocculating efficiency. A second technique consisted of measuring the time in minutes required to obtain clear water at the pump suction after addition of the various flocculating agents at the flowline. These tests were made using a model mud circulating system having a total volume of approximately 10 gal. The natural fresh water and brine muds used contained 4 per cent solids. A sketch of the circulating system appears in Fig. 1. The circulating rate

By J. Nell

Heavy mineral deposits often contain relatively high levels of radioactive elements (thorium and uranium in particular).It is difficult to obtain clean separation of ilmenite and monazite (the main impurity mineral containing radioactive elements), and physical intergrowths of the two minerals are, in fact, not uncommon. As a result, ilmenite concentrates obtained from such deposits often contain high levels of thorium and uranium. Because of the large negative free energies of formation of ThO2and U3O8boththorium and uranium report to the slag during smelting and if an ilmenite concentrate contaminated with monazite is used to make high titania slag, the concentrations of these elements in the slag end up about 40% higher than in the ilmenite feed. Previous work, patented by RGC Mineral Sands Limited, and subsequently confirmed by Mintek, showed that radioactivity may be reduced by roasting an ilmenite concentrate with borax at 1000°C to 1100°C and leaching it with hydrochloric acid1. It is evident that the cost of an ilmenite roast/leach process will be high and there may be economic benefits in removing the radioactive elements from the slag instead (the volume of slag to be treated is smaller than the volume of ilmenite feed). To remove radioactive elements from the slag it is necessary to know how these elements occur in the slag. Inother words, the distribution of uranium and thorium between the various oxide, silicate and metallic phases in high titania slag must be determined. Once the deportment of thorium and uranium between the various phases ha sbeen determined, an appropriate process for slag purification can be developed. Test samples High-titania slag was prepared in a pilot-scale DC furnace from ilmenite concentrates with different levels of uranium and thorium. Subsequently, ten slag samples representing a range of compositions were selected for bulk chemical analysis, scanning electron microscopy and micro-analysis. The samples were crushed to a maximum particle size of 1 mm and from each sample a 20-kg batch was riffled out for analysis. Bulk chemical composition Chemical compositions of the samples selected for test work are given in Table I. TiO2, Al2O3, SiO2, MgO, MnO, FeO and V2O5were analysed by ICP-OES, Na2O, CaO andCr2O3by atomic absorption spectroscopy and U and Th by XRF (the XRF detection limit for U and Th was around 4 ppm). The ?B? series has a higher silica content than the others as a result of small silica additions that were made during smelting. All samples have elevated alumina levels as a result of furnace refractory contamination during smelting. As expected, there is an inverse relationship between the concentrations of TiO2and FeO in the samples (Figure 1).The TiO2and FeO levels are similar to the levels found in industrial slags2. Extreme conditions of reduction under which reduction of more ?refractory? oxides (e.g., chromia, magnesia, silica, alumina and even urania and thoria) might take place were not explored in the study. Note that BB1and BBB1 contain more than 7% combined silica and alumina (SiO2as a flux addition during smelting, and Al2O3from refractory contamination) and they do not fall on the general trend defined by the other samples. The U and Th concentrations of sample E2 is noteworthy. In the preparation of slag E2, monazite concentrate was added to the ilmenite to increase the concentrations of radioactive elements in the slag. This was done primarily to facilitate the detection of Th and U during the phase chemical characterization of the slag. Radioactivity measurements Gamma ray emissions from the samples were measured [ ]

Jan 1, 2007

By Charles Stein

The effects of several different prior treatments an the creep behavior of 99.9995 pct aluminum at 260°C and 1000 psi canstant stress are compared with annealed specimens. Quenching from 538oC, irradiation with 2 mev electrons, and tension-compression room temperature fatigue damage were used to change the substructure of the specimens prior to their creep testing. The quenched and the irradiated specimens showed a larger primary and transient stage contribution to the creep curve than those specimens which were only annealed prim to creep testing. The specimen receiving prior fatigue damage at room temperature showed no first stage or transient creep when tested under identical conditions as the above specimens and had an average creep rate seven orders of magnitude lower than that of either the annealed, the quenched or the irradiated creep specimens. In a previous electron transmission microscopy investigationl of the substructure developed during the creep of pure aluminum at 0.57 Tm, it was noted that a large concentration of vacancy loops and dislocation loops were present in and near the subboundaries while the interior of the subgrains contained few of these defects and had a low dislocation density, see Fig. 1. Yim and Grant2 and Hazlett3 have shown that the presence in nickel of a substructure developed by prior cold work effectively reduces the primary and transient contributions to the creep curve. Hultgren,4 McLean,5 Gervais, Norton, and Grant,6 Chang and Grant,7 and others have shown the same effect with the higher stacking fault energy material, aluminum. However, the specific defect responsible for the change in the creep behavior developed by the prior cold work was not established. Specifically, what effectively interfered with dislocation motion in these materials at elevated temperatures? Was it jogs on dislocations produced by their interaction with other dislocations or with vacancy or dipole loops, see Fig. 1, or did the subgrain walls determine the mean free path for glissile dislocations? This would be a realistic possibility only if subgrain boundaries are effective barriers to dislocation motion. The ability of a subgrain boundary to act effectively against glissile dislocations depends on the number and the arrangement of dislocations in the subboundary,8 which in turn is a function of the creep strain.' This paper compares the creep rate of specimens possessing a large vacancy concentration to that of annealed specimens and with specimens having a stable subboundary wall containing Lomer locks produced by prior fatigue damage. EXPERIMENTAL PROCEDURE Vacancy Loops. Aluminum creep specimens, 99.9995 pct pure, were machined from zone refined rod to a 2-in. gage length and a cross-sectional area of 0.025 in. These specimens were annealed at 538oC, 1000°F, for 10 min and quenched into ice water. They were then reheated to the creep test temperature of 260°C, 500°F, and held at this temperature for 18 min to al-low for vacancy condensation and loop formation. The specimens were subsequently creep tested at 1000 psi constant stress at 260°C. The temperature along the gage length was monitored by three Pt-Pt, 13 pct Rh thermocouples, two embedded in the upper and lower shoulders of the specimen and one attached to the mid-point of the gage length- The temperature gradient was held to ± l°C or less throughout the Creep test. Elongations were measured by two LVDT's 'connected in an averaging 'On-figuration, with quartz extension arms placed against the specimen at the extremes of the 2-in. gage length. i K 3J?--' * *H - >^> - ' ^L r 77 . *y J OJL, J Fig. 1—Transmission electron micrograph of pure aluminum strained 8.2 pct at 260°C and 1000 psi constant stress. Note the presence of numerous loops near the light dislocation tangle

Jan 1, 1970

By F. G. Jones, R. D. Pehlke, H. E. Gardner

The solubility of nitrogen in liquid Fe-18 pct Cr-8 pct Ni-0. 7 to 2.3 pct A1 alloys has been measured up to the solubility limit for the formation of aluminum nitride in the temperature range 1600° to 1700°C uszng the Sieverts' method. The solubility of nitrogen in 18-8 stainless steel increases with increasing aluminum content. Based on a nitride composition, AlN, the standard free energy of formation of aluminum nitride from the elements dissolved in liquid 18-8 stainless-steel alloys has been determined to be: ?G° = -42,500 + 20. IT in the range from 1600° to 1700° C. EVANS and pehlke1 have measured the equilibrium conditions for the formation of aluminum nitride, AlN, in liquid Fe-A1 alloys. The present study extends that work to the more complex solvent, liquid 18 pct Cr-8 pct Ni (18-8) stainless steel. Recent work by Small and pehlke2 has dealt with the effect of fourth-element additions on the solubility of nitrogen in 18-8 base alloys. They found the effect of aluminum additions, up to 0.74 pct, on the solubility of nitrogen to be small. The present study covered the range from 0.74 to 2.28 pct aluminum, and by extending the composition range may be used to better define the effect of aluminum on the nitrogen solubility in these alloys. EXPERIMENTAL PROCEDURE The Sieverts' method was used to measure the equilibrium solubility of nitrogen gas in liquid 18-8 stainless steel alloys containing 0.74, 1.49, 1.93, and 2.28 pct Al. The solubility was measured as a function of the nitrogen gas pressure at temperatures of 1600°, 1650°, and 1700°C. The apparatus used is the same as described by Small and Pehlke.2 The 100-g melts were made from Ferrovac-E high-purity iron, Crucible Steel Co.; 99.95 pct Cr, Union Carbide Corp.; 99.9 pct Ni, International Nickel Co.; and 99.99+ pct Al, Aluminum Co. of America. The aluminum was charged at the bottom of the crucible, surrounded by nickel and iron. The chromium was packed into the interstices to minimize vapor transport of the aluminum during initial melting. The hot volume of the system, measured for each melt with argon, ranged from 45 to 55 standard cu cm with a temperature coefficient of —8 x 10-3 cu cm per °C. The melt temperature was measured with a Leeds and Northrup disappearing-filament type optical pyrometer sighted vertically downward on the center of the melt surface. The temperature calibration of the system by Small and pehlke2 was assumed. Two problems are involved in determining the solubility product of a solid, metal nitride phase in liquid iron alloys. These are: 1) establishing the point of departure from Henrian behavior at the solubility limit of the metal nitride phase; and 2) determining the composition of the solid nitride which is precipitated. Determination of the solubility product of AlN was made by admitting small amounts of nitrogen into the reaction bulb until the deviation from Sieverts' law was clearly evident in the form of a pressure halt. To obtain the solubility product at several temperatures during one run the following procedure was used: 1) add increments of nitrogen to determine the Sieverts' law line at the lowest desired temperature; 2) continue to add nitrogen to precipitate a small amount of the nitride phase; 3) increase the melt temperature 50°C to dissolve the precipitated nitride; 4) repeat step 2 until either a nitride formed or the system reached ambient pressure; if a nitride formed at 1650°C, the sequence was repeated at 1700°C. The composition of the precipitated phase was checked by an X-ray diffraction pattern obtained from powder scraped from the surface of the solidified 1.93 pct A1 melt. RESULTS AND DISCUSSlON Solubility Measurements. Fig. 1 is a typical nitrogen-absorption curve obtained from measurements on a 1.93 pct A1 alloy. Since the initial absorption of nitrogen follows Sieverts' law the nitrogen solubility is plotted as a function of the square root of the pressure of nitrogen gas in the reaction bulb. The results of the solubility measurements for all alloys studied are summarized in Table I. The slope of the Sieverts' law line for each alloy was determined. Since this is also the solubility of nitrogen at 1 atm pressure of nitrogen gas, the latter designation is used for the data. It should be noted. however, that in most cases the value lies above the solubility limit for AlN. Fig. 2 shows the effect of aluminum on the solubility of nitrogen at this reference pressure and as a function of melt temperature. The solid portions of the lines represent attainable solutions; the dashed regions lie above the limit for precipitation of AlN.

Jan 1, 1969

By A. J. Kroha, N. Wesis

Most copper mines produce both ore and low-grade "leach" rock or acid waters that contain recoverable copper. The sulfide ores pre¬dominate, and a portion that is too low grade for milling to produce concentrates for smelting, but has to be mined and trucked away anyhow, may be leached successfully with acid in dumps. Most of this leach material consists of sulfides and silicates or carbonates, and if the gangue is such that it consumes a high quantity of acid, this factor may rule out a leach operation. There are also valuable deposits that contain mostly acid-soluble copper, or occasional sulfide ores from which a sulfide concentrate can be roasted and acid-leached to produce a copper-bearing solution. Finally, there are milling ores in which the lesser part of the copper is acid-soluble and can be precipitated with iron or synthetic inorganic precipitants that produce metallic copper or copper sulfides that will float with the sulfides. Ordinarily, ores that contain copper associated with the sulfur ion, such as in the minerals chalcopyrite, chalcocite, bornite (and others), are milled to produce a 25-30% Cu concentrate for smelting, while a lesser amount of acid-soluble copper may be converted from solution to cement copper on iron scrap. A fast-growing percentage of such copper, however, is removed from solution with exchange resins or organic compounds in organic carriers such as kerosene (solvent extraction), then eluted with strong acid and subjected to electrolytic precipitation either in marketable form or as anodes that can be refined further. From the point of view of conventional copper smelting, copper flotation concentrates and cement copper are of chief interest in this chapter. Table I is a condensed open schedule for concentrates that generally run between 25 and 35% copper, and much less frequently as low as 12-15% or as high as 65-75% copper, the former being due to intimate relationship with pyrite (like the former United Verde Extension), and the latter representing such ores as the Bolivian Coro¬coro ore in which the copper is in the form of chalcocite in sandstone. These extremes are no longer common. When they occur, a special purchase schedule has to be negotiated. Included in Table 1, copper precipitates (cement copper) generally run from 70-85%a copper, and the same basic purchase schedule is used as with flotation concentrates. Sulfide Flotation Concentrates The sulfide copper concentrate produced in the mill as a flotation froth, with water then added for transportation of the heavy mineral particles from the flotation cells to thickeners, may run 60-80% water by weight, and the removal of water down to 25-50% by weight by means of thickeners, followed by further dewatering by continuous vacuum filters to 7-18% moisture by weight (depending on size of solids by screen analysis and also by content of clay) is a critical operation. Mill operators would like to produce a filter cake with 7-9% moisture content, but even with the help of steam on the filter this desirable condition is seldom realized when the concentrate is as fine as 80% -325 mesh. More commonly, the final concentrate is reground in pro- to produce best copper recovery and grade of concentrate (or molybdenite separation). In those cases, increasingly frequent, the filter product may not be a cake at all, but a mud that is hard to handle-even requiring a thermal dryer. Greater difficulty of form¬ing a manageable cake often comes from the copper-molybdenum separation by flotation, because the alkaline sulfides and hydrosulfides, or cyanide, or other similar reagents used for the separation, may leave the now relatively molybdenite-free copper concentrate even more difficult to filter. Handling a wet filter cake is difficult enough when its destination is only a short distance away-a matter of yards rather than miles. In those cases the filter cake may be thermally dried near the point of production, using rotary or multiple hearth, or fluidized-bed dryers. Alternatively, the concentrate may be pumped or carried in slurry form to the smelter and filtered there, or it may be spray-dried and compacted. For transportation to a smelter just a few miles to a few thousand miles away by ship or railroad other factors may be important, such as: in shipping by sea, avoidance of spontaneous combustion; in shipping by rail, losses by leakage if too wet or by wind and sun if too dry. It is the responsibility of the millman-usually the mill superinten¬dent-to make sure that his concentrates are in satisfactory condition when they leave the mill so that they meet these requirements: 1) They must have been accurately sampled and dry-weighed, the latter meaning that a moisture determination and gross weight must have been taken. 2) They must be dried sufficiently when necessary to prepare them for safe transportation. 3) They must arrive at the smelter with reasonable likelihood that they can be check-weighed and sampled fairly and equitably,

Jan 1, 1985

By J. J. Pye, J. B. Drew

Mzasurements of the surface diffusion coefficients of metals have been made. Diffusion profiles for the Ag-Ag system were obtained by means of a radioactive point source and a precision auto-radiographic technique. The activation energy for silver self diffusion (=8.1 kcal per mole) is lower than that previously reported (-10 kcal per mole) on poly crystalline wire by Nickerson and Parker. The bresent data indicate an effect due to parasitic volume diffusion at temperatures above 500°C. RELATIVELY few measurements have been made of the surface self-diffusion coefficients of metals. Nickerson and arker' measured the diffusion of silver over the surface of poly crystalline wires and estimated that the activation energy was 10.3 kcal per mole. Winegard and chalmers2 carried out measurements on both polycrystalline and single crystal surfaces but did not report a value of the activation energy. They found, however, that at temperatures between 250" and 400°C the diffusion coefficients were on the order of lo-' sq cm per sec and that there was an acceleration of the migration of silver on the polycrystalline sample when a change of surface shape occurred. Winegard and Chalmers used an autoradiographic technique, hereafter designated ARG, and Nickerson and Parker used a surface scanning geiger counter in order to determine the diffusion profiles. More recently, Hackerman and simpson3 measured the surface self-diffusion coefficient of copper at a single temperature (750°C), and the value of the diffusivity (- 10-5 sq cm per sec) is in agreement with that given by jostein from his thermal grooving measurements. This paper reports the results of an investigation of the surface self-diffusion coefficients of silver over a large temperature range and describes the adaptation of autoradiographic (ARG) techniques for the determination of diffusion profiles obtained from a radioactive point source. EXPERIMENTAL PROCEDURE The experimental procedure is a modification of the method employed by Hackerman and simpson3 in their measurements on copper. A brief description of their technique is as follows: A radioactive needle which sinters to the surface during the diffusion an- neal serves as the source of diffusing atoms. After the diffusion run the needle is removed and the surface is scanned with a shielded counting arrangement. The diffusion profiles reported in this paper were obtained by a modification of the above procedure which employs a precision ARG technique. Previous investigations in this laboratory and elsewhere51B have shown that under carefully controlled developing conditions and by the use of calibration sources a linear relation exists between the concentration of the isotope and the photographic density for values below unity. The use of ARG under these conditions has advantages over the counter scanning method in that cumbersome shielding and requirements for great mechanical precision of the scanner are eliminated. Also the ARG gives a complete picture of the surface which is advantageous in studies of anisotropic diffusion. A recording microdensitometer having a 0.1 p wide slit was employed. At low temperatures the disturbing effects of subsurface radiations are negligible. The diffusion anneals are carried out in the cell shown in Fig. 1. The needle is formed by grinding down a 1.0 mm rod of high-purity silver until a tip of 0.2 mm radius or smaller is formed. This tip is plated withA"' which becomes the source of the diffusing atoms that are detected by ARG. The needle carrier and the crystal holder, Fig. 1 are constructed of quartz and ports are provided in the holder pedestal which allow free vapor circulation ((2.0 oz) and the carrier apron fits snugly over the crystal holder cap, insuring that the needle does not move and scratch the surface. Temperatures are provided by a stabilized tubular furnace which can be quickly positioned around the cell, thus bringing the crystal up to temperature in a time that is short compared to the diffusing times. The diffusion anneals range from 2 hr for the high-temperature samples to about 25 hr for those at the lowest temperature. The possibility of vapor transport of the radioactive metal as a contributing factor in the diffusion profile was investigated in two ways. One method was to suspend the needle directly over a dummy sample, raise the temperature, for periods of time equal to the diffusion times, and then take an auto-radiograph of the surface. Negligible radioactivity appeared. In the second method a thin slot in the crystal face on one side of the source provided a "cong path" for surface diffusion. If evaporation was the primary source of surface atoms the region of radioactivity around the source would be symmetrical. This was not the case. The profile dipped abruptly at the edge of the slot but on the other side of the source the usual diffusion profile appeared.

Jan 1, 1963

A General Meeting and Colloquium was held in Kelvin House, Johannesburg on Wednesday 29th September, 1971. The theme of the Colloquium was "The Ferro-alloy Industry". Prof D. D. Howat (President) was in the Chair. The meeting was attended by 106 delegates and was opened by the President at 10.05 a.m. OBITUARY The President: "It is my sad duty to announce the death of G. C. Needham, Fellow, who joined the Institute in 1966 and passed away on 27th September, 1971. As a mark of respect to the memory of the deceased and in sympathy with the bereaved I would ask you all to rise and observe a few moments silence." MEMBERSHIP The President: "I have much pleasure in announcing that the names of the following candidates, having been published in accordance with By-Law 5.2.2, Council has elected them to membership of the Institute. Fellows: Richard Lloyd Blandy, Brian Roger Borton, Brian Teversham, Peter Donald Dickson. Members: Frederick Brian Peacock, Peter John Stacey, Kenneth Niles Thanstrom, Byron J. Hayley, Ian Flemming Buchan, Abraham Hercules le Roux. Graduate: Ian William Coy. Students: Peter Boesley J ames, Kenneth Brian Perel. TRANSFERS From Member to Fellow: Cecil Eugene Fivaz, Peter Edwards. From Student to Graduate: Roy Stavely Traviss. From Student to associate: William Mitchell. I welcome the new members to the Institute and congratulate those members who have been transferred to a higher grade. COLLOQUIUM The first paper, presented by Mr S. Selmer-Olsen, Consulting Metallurgist, Amcor Limited, on 'Trends in Ferro Alloy Production' was published in the May issue of the Journal and comprised information and data relating to new developments in ferro alloy production in various parts of the world. This was followed by a paper-'Conductivity and Viscosity Properties of Slags produced in ferro-alloy manufacture' by D. 1. Ossin et al. This was a record of laboratory test work on slags containing both lime and magnesia, corresponding with the composition of slags encountered in the production of ferro chrome alloys when a dolomite flux is employed. The third paper-'Review of the work of the Pyrometallurgical Research Group of N.I.M. and Metallurgy Department, Wits.' presented by Dr P. R. Jochens, leader of the Research Group, outlined the progress made on ten different research projects presently under way in the Department of Metallurgy. These projects range from studies of the kinetics and mechanism of the reduction of chromite ores through the determination of the activities of MnO in slags to phase studies and melting point determinations in the alloy systems Cr-Fe-Si-C and Cr-Fe-Si. A new feature of this Colloquium was the introduction of the discussion panel composed of four or five individuals known to have special knowledge or interest in the subject under duscussion. Mr J. J. Coetzee was chairman of the first panel, Professor D. D. Howat of the second and Dr R. E. Robinson of the third. During the discussion of Mr Selmer-Olsen's paper an interesting contribution was made by Mr Jack Hayley of Transalloys (Pty.) Limited who pointed out that the lowest power cost in the U.S.A. was that from the TV A at 6 mils per unit (0,43 cents S.A.) while costs from other sources were 7 to 8 mils per unit (0,50 to 0,57 cents S.A.) He also referred to the use of 'pile sintering' of ore fines plus coke at certain ferro alloy plants in the V.S. and to the recent practice of 'graphitising' the paste used for Soderberg electrodes. The last session in the afternoon was devoted to a group discussion on 'Practical problems in Arc Furnace Operation', Mr H. R. Reid of Middelburg Steel Alloys (Pty) Limited occupying the chair, members of the panel being Mr J. Meintjies (Rand Carbide Limited), Mr J. Benn (Amcor) and Mr E. J. Jackson (Transalloys (Pty.) Limited). Mr Reid initiated the discussion by talking of the design and composition of electrode shoes, mentioning the use of the 85/15 Cu/Zn alloy and the comparison of hollow shoes and shoes cooled by tubes. Mr Meintjies discussed electrode management with particular reference to breakages, and dealt with casing and fin design and the welding of fins. Mr Benn dealt with aspects of closed top furnace operation with particular reference to the control of eruptions in the furnace and indicated that preheating of the raw materials might be well worth considering together with the development of a system for the detection of the water vapour present. Mr J ackson was concerned with shells, linings, refractories and tap holes. He deprecated the use of oxygen for opening the tap hole emphasising how uncontrolled use of oxygen led to loss of shape of the tap hole and quite severe burning out of the front hole resulting in time and labour in repairs. A notable feature of the Colloquium was the free discussion 'from the floor' of the hall. Many valuable and highly pertinent contributions were made spontaneously and usually in reply to some controversial topic raised by the discussion group.

By W. –E. Marx, M. Faber, R. Pollak, I. Astberg

INTRODUCTION Essentially three strategies are pursued in parallel for protecting the underground working force in mining against the consequences of methane ignitions which might lead to explosions: • Sufficient ventilation for avoiding the formation of explosive methane-air mixtures. • Avoiding sources of ignition caused possibly by electrical equipment or friction. • Structural explosion protection for limiting explosion propagation to the farthest-going extent for the case that methane is fired because of failing of the above preventive measures taken. The corresponding methods taken in mechanized roadheadings with point-attack roadheaders in German coalmining are subject of this paper. VENTILATION In ventilation of roadheading sites the following is to be considered in respect of methane control: • Sufficient air flows by volume being cycled to the heading face for diluting released methane to safe concentrations. • Sufficient local air velocities for effective mixing of methane and air in the whole heading site, in particular directly on the heading face and underneath the roof. Furthermore, ventilation needs to be laid out in a way that cut- ting does not result in health affecting dust exposure at any working place. Accordingly, the ventilation systems shown on Fig. 1 including primary and, if necessary, secondary auxiliary ventilation air ducts as well as dedusters, are used in roadheadings. This equipment is run according to the following principles: • If the roadheader is at standstill, the heading face is ventilated by the free air jet from the blowing duct closest to the face. In this operation phase the deduster is shut-down. • During cutting, the exhaust of the blowing air duct is automatically closed, and the deduster is taken into operation. The in- coming fresh air is now locally discharged via a lateral orifice, or distributed by Coanda-type ducts from the primary or secondary ventilation air duct. In this way, a stable dust wall not disturbed by the jet of the air duct is formed in front of the heading face. Only the ventilation air stream taken in by suction of the close-to-face deduster is passed through the inby zone of the heading face (over approx. 20 m). The clean exhaust of the deduster is dischayed to the roadway in some distance outby. Immediately at the heading face, methane accumulations possibly released by cutting are diluted by compressed-air jets from air-movers located near the roof which assure more rapid motion of the air without distuhing the dust wall. • In the zone of overlapping of primary and secondary duct and the deduster - that zone possibly is poorly ventilated during cutting - sufficient local air speed is assured by Coanda-type ducts or additional ventilation jets for avoiding methane accumulation. The regulations of the inspectorate specifies geometrical conditions to be met with these configurations of ventilation equipment. In-seam roadways are ventilated at rates > 0,5 m/s. For dedusters, present-day ventilation air flows are of 600-800 m+/ min. Ventilation monitoring and control is assured by units for measuring methane and ventilation air flows. If pre-set thresholds are exceeded or fallen short of, these measuring units shut-down - dependent on potential hazard - any not intrinsically safe electrical equipment in the roadheading, either totally or in limited zones. In addition, CO-measuring units near the roadway en- trance serve for early detection of mine fires. In spite of this ventilation layout and the equipment used and in spite of the water spray systems on the cutting head (discussed later in this paper) several cases of methane ignition and subsequent burning off (however, no explosions) have been recorded in the recent past. Therefore, the above-described ventilation is nowadays complemented in many cases by machine-mounted ventilation equipment for the immediate surroundings of the cutting head. Ventilation of the surroundings of the cutting head Investigations carried out subsequent to the above-mentioned gas ignitions have shown that the high ventilation air speed necessary for rapid dilution of methane could not permanently be arrived at in the following zones: • The direct zone of cutting, in particular during sumping. • The floor zone above the debris, predominantly below the cut- ting head. Accordingly, VOEST ALPINE-Bergtechnik, a producer of mining machinery, in cooperation with DMT developed for point- alttack roadheaders a novel machine-mounted ventilation equipment, the Jet-Block" (AERO SAFE Jet-Block) shown on Fig. 2. This system allows to ventilate the above-mentioned critical zones with high flow speeds. One AS Jet-Block is mounted on each side of the boom approx. 0.5 m behind the cutting head. The blocks discharge compressed-air jets with high energy from 10 nozzles per block into the hazardous zones (Fig. 3). Two nozzles of each jet block are tangentially oriented toward the upper circumference of the cutting head, the others are arranged fan-like with orientation to the heading face underneath the cutting head and the debris. The nozzle array of the blocks as well as the com-

Jan 1, 1997

By D. D. Dunlop, J. R. Welker

The growing interest in the use of CO, in crude oil recovery increases the need for data on the effect of CO, on hydrocarbon physical properties. Data are presented on the solubility of CO, in various dead oils, the swelling changes in CO2-oil solutions and the effect of CO, on dead oil viscosity. This latter property shows the most pronounced effect, with viscosity reductions up to 98 per cent of the uncarbonated viscosities. An empirical method of estimating the viscosity of carbonated oils is presented. The apparatus and procedures used are described in sufficient detail to allow others to make similar studies. INTRODUCTION The effect of dissolved carbon dioxide on the swelling and viscosity reduction of specific hydrocarbon oils has been observed and recorded by a number of investigators.'- me object of this paper is to offer a means of predicting these effects for crude oils free from natural gas, using the dead state viscosity and gravity of the crude oils. The CO, solubility and swelling of numerous crude oils were determined in a visual cell at various pressure levels. The viscosity of the oils carbonated to various pressure levels was then determined by measuring the pressure drop across a capillary tube. From these data, the physical properties were correlated empirically. The resulting correlations allow the prediction of CO, solubility, swelling and viscosity reduction if the dead state gravity and viscosity of the oils are known. SOLUBILITY AND SWELLING MEASUREMENT EQUIPMENT AND PROCEDURE A high pressure visual cell was installed in a constant temperature cabinet. A test gauge was attached at the top of the cell for pressure measurement, and a line was run through the cabinet wall to a wet test meter which was used for volumetric measurement of the gas. The first step in making a test run was to put the oil in the cell up to a level about half to two-thirds of the total volume. This required about 50 to 65 ml of oil. carbon dioxide was then bubbled up through the oil for a time during which the pressure of CO2 in the cell was kept above 800 psia. Saturation of the oil with CO2 at this pressure and ambient temperature was confirmed by slowly bleeding CO2 through a valve to the atmosphere. If the oil was completely saturated with CO2, bubbles of gas would form in the oil at the first small decrease in pressure. If the oil was under-saturated, no bubbles formed until the pressure was decreased to the saturation pressure existing in the oil. If this saturation pressure was lower than that desired, more CO2 was bubbled through the oil until the desired level was reached. After saturation at ambient temperature was completed, the cabinet temperature was adjusted to the desired level and the cell was allowed to reach temperature equilibrium. After temperature equilibrium was reached, the pressure was again decreased slightly, and the oil again checked for full CO2 saturation at the cell pressure. The pressure now had changed because of the difference in solubility of the CO, in the oil at higher temperatures and the expansion of CO2 as the temperature increased. The outlet tube from the cell was then connected to the wet test meter and the CO2 was allowed to flow slowly out of the cell and through the wet test meter at ambient temperature and pressure. The water in the wet test meter had previously been saturated with CO2 at ambient temperature and pressure by allowing CO2 to flow continuously through it lor a period of several hours. The gas flow was stopped at several pressures during the run and the cell was allowed to come to equilibrium; this made possible the measurement of solubility and swelling data at the intermediate pressures. The volume of the oil in the cell was recorded at each of the equilibrium pressures in order to obtain swelling data. DATA AND RESULTS The solubility of CO2 in the oil was calculated by the relationship V — V, where R. = solubility of CO, in crude oil, cubic feet of CO, measured at 60F and 1.0 atm/ bbl of dead state oil at the temperature under which solubility was measured, V, = volume of gas released from the cell between the saturation pressure and zero pressure, corrected to 60F and 1.0 atm, cu ft, V, = volume of CO: contained in the gas space above the oil, corrected to 60F and 1.0 atm, cu ft, and V, = volume of the dead oil in the cell in bbl at the temperature of the run. The volumetric data of Sage and Lacey' were used to calculate V., from the volume of CO2 at high pressures. The swelling factor was calculated as where V, is the volume of the C0,-

By Jan Tegtmeier, Horst Gerhardt

INTRODUCTION Under certain circumstances the closure of former mines which are located above a certain flood level can result in problems such as the emanation of detrimental substances after having completed filling and reclamation operations. This especially applies to uranium mines in which the radiation dose could far exceed the dose of natural background radiation. By means of an example of the uranium mining in Germany in the following it will be demonstrated how to cope with this problem. On the basis of comparative investigations in various vein deposits and using ventilation scheme calculations proposals for the optimization of the necessary forced ventilation can be submitted. REPORT ON SITUATION In the period 1946 - 1989 the former Soviet-German joint- stock company "Wismut" developed into the biggest European uranium producer with a total output of about 220.000 t of uranium. A major mineraldeposit district was the deposit of Schlemaf Alberoda in the Saxon Ore Mountains, in which 80.000 t of uranium were produced. Thus it is among the biggest uranium de- posits of the world, from which various other metals were at- tracted for many centuries. The exploitation of the Schlemal Alberoda deposit involved steep veins in regions near the surface as well as depths of 1.800 m. Until 1991 a total excavation space of 40 million m3, which is flooded at present, was produced. With the average increase in the water level of 80 cm per week the final flood level is expected to be reached in the year 2003. The shaft 373 at present still being used for ventilation will be no longer available since the second quarter of 1998 after flooding the -540 m level because it is not connected with the excavation system near the surface. As a study shows, a radiation dose far above the natural back- ground radiation has to be expected for the town of Schlema due to the extensive mining activities near the surface and due to the subsequent displacement with missing depression fo the main mine ventilating fan. An uncontrolled air flow containing radon leaves the open mine excavation due to the effect of the natural ventilating pressure and emanation caused by the barometric pressure drop with atmospheric pressure fluctuations. This mine air with its high-level radioactive equilibrium results in a high radiation dose in buildings (see Figure l). After having switched off the main ventilating fan in order to investigate the effect of the missing depression the increase in radon concentrations amounted up to 700% in various buildings of Schlema. This was partially due to the inversion state of the weather at that time. The high radon concentration has detrimental effects on the health of the population and of the miners working on the further reclamation in regions above the flood level. ANALYSIS OF THE RADON EMANATION RATE EXPECTED Considering the composition of the radon inflow from the mine workings it becomes evident that 80 % of the radon inflow originates from abandoned excavations and only 20 %from open ventilated mine excavations. This fact has to be taken into account for the ventilation after having reached the final state of flooding. After completing ventilation the radiation dose on the surface is mainly due to the radon emanation from excavations close to the surface. Investigations of the Wismut GmbH showed the in- crease in the specific radon emanation rate by a factor of 100 for abandoned excavations as compared to new drivings. One reason is the larger specific surface of abandoned galleries caused by displacements due to mining activities as well as by fall of hanging. Furthermore the radon can enter the gallery through joints, which have subsequently opened by convergences. All these effects result in a larger free surface available for radon diffusion. The large number of drivings in the deposit sections near the surface and the fact that the highest uranium contents are found near the surface as well as the high fracturing are further reasons for higher emanation rates. Considering these facts it can be expected that the radon inflow of 10.000 kBq/s, which refers to an open mine excavation of about 1.4 million m3, represents a minimum. Only by increasing the specific surface, for which a numerical value has still to be determined, this value will increase with certainty. An extensive radon emanation from the residual excavation, which cannot be flooded, can only be prevented by maintaining the ventilation system. The low pressure produced by the fan in the mine openings prevents the emanation of air containing radon due to the effect of the natural ventilating pressure. Without the controlled withdrawal of the radon the population as well as the miners working on the further reclamation in areas above the flood level would be endangered. Therefore the follow-

Jan 1, 1996

By T. M. Allen, W. H. White

THE Greenwood-Grand Forks area of southern central British Columbia, known as the Boundary District, has a long history of mining exploration and production. At the turn of the century this was the premier copper mining camp in the British Empire, its total production amounting to some 20 million tons. Most of this ore came from the great Granby mines at Phoenix, but the Motherlode mine at Deadwood camp, 6 miles to the west, and several mines in Summit camp, 5 miles north of Phoenix, made important contributions. The large deposits were exhausted in 1918 and the district since has seen only desultory exploration and salvage operations. The orebodies are mineralized skarn zones in limestone members of a thick series of Upper Paleozoic sedimentary and volcanic strata. Chalcopyrite is the primary ore-mineral. Copper carbonates and silicates occur sparingly in outcrops, but the oxidized zone generally is very shallow. Much of the surface is mantled by glacial drift which in most places ranges in thickness from 2 to 15 ft. In some of the hanging valleys, however, the glacial drift may be as much as 100 ft thick and may assume drumlin-like forms. In 1951 an ambitious program aimed at the discovery of new orebodies and important extensions of abandoned deposits was launched by Attwood Copper Mines, Ltd. In this district so thoroughly searched by an earlier generation of prospectors, any orebody which had remained undiscovered must have little or no surface indication. Consequently, in addition to the basic detailed geological work, the program of exploration included magnetometer and self-potential surveys. Geological bets and geophysical anomalies were tested further, prior to diamond drilling, by a study of copper distribution in tree twigs and/or in the soil. The soil sampling and analytical methods used and some of the results seem of sufficient importance to warrant this paper. The authors had done some plant sampling in this and other districts, using the dithizone neutral-color-end-point method (Warren and Delavault, 1948, 1949; White, 1950),1-3 but they were unfamiliar with its soil application. Finally, after much experimenting in the field, they adopted the methods described here. These methods are not entirely original or defensible on theoretical grounds, but under field conditions of rapid sampling and analysis the results are reliable enough to be of use. Fig. 1, which shows the results of duplicate analyses of duplicate soil samples taken at 50-ft intervals across an anomalous zone, indicates the relative dependability both of the sampling and analytical methods. Sampling and Analytical Equipment A 2-ft piece of 1-in. solid drill steel, one end sharpened to a broad, conical point. The steel is marked at 1 ft from the point. A 2-ft piece of ½-in. black iron pipe, one end filed to a bevelled cutting edge. The pipe is marked at 1 ft 3 in. from the cutting end. A 3-lb hammer. A plastic or rubberized sheet about 18 in. square. Moisture-proof assay pulp envelopes. A 10-mesh seive made from window screen with the paint burnt off. A small assay spatula. A pan balance sensitive to 10 mg. Two ignition trays about 4 in. square, made of sheet iron turned up along the edges. A Coleman two-burner gasoline stove. An asbestos board about 5x8 in., used as a hot plate on the gasoline stove. A circular aluminum rack to hold 8 test tubes while refluxing (design of Almond and Morris). Pyrex Glassware Large refluxing test tubes, 25x200 mm, marked at 40 ml volume. Breakers, 20 ml. Pipettes, 1, 5, and 10-ml capacity. Graduate, 50 ml. Shaking cylinders, 100 ml, glass stoppers. Burette, 25 or 50-ml capacity, with holder. Chemical Supplies 1 N sulphuric acid. Hydroxylamine hydrochloride, solid crystals. Fisher Alkacid test paper. Copper standard solution. Dithizone standard solution 60 mg per liter. Water reasonably free of metals. Soil Sampling Method: The problem of how to take a soil sample is extremely crucial. The method outlined below, adopted after a number of tests, has the advantages of uniform pattern, uniform depth, and uniform size of sample. The area to be tested was marked off by chain and compass lines 100 ft apart, normal to the strike of possible ore deposits. Numbered stakes were set at 50-ft intervals along these lines and a soil sample was taken at each stake in the following manner. The drill steel was driven into the ground normal to the slope of the surface to the marked depth of 1 ft, moved slightly from side to side, then carefully withdrawn. The iron pipe was inserted to the bottom of this hole, tapped down to the marked depth of 1 ft 3 in. and withdrawn; the 3-in. soil plug in the

Jan 1, 1955

By Roger W. Dewey

The opposition is all kinds. There are extremists. There are quiet, sensible sounding folk who can twist numbers and facts to make their point. But they are all out to shut you down! Some of them are genuinely concerned about miners' impact on the environment. Others are just anti- society, anti-big business - small is beautiful - live naturally. The opportunity for them to make those statements on television was provided by us, the Uranium Public Affairs Task Force, as part of a media tour of the State of Idaho in May. We fielded four representatives of the industry and got 25 hours of television coverage, 22 hours of radio coverage, and print coverage by every paper in Idaho. The tour included several debates, and these clips are from two of them. Our folks creamed them! This one was so upset that he ran off the set while his mike was still plugged in, trailing studio equipment behind him. But we don't always have the opportunity to rebut them. They are making these statements all the time, everywhere they can. They have learned their trade well. They use the hearing process like A1 Hirt uses the trumpet. If the process of intervention should shut us down or prevent us from getting a license, so much to the good. But even if it doesn't - they win - for it causes delay - delay costs money and so does complying with regulation. If they can make us uneconomic, and that's not too hard to do these days, they have won. Regulation restricts the decision process. Any time the decision process IS restricted, you face the possible loss of a more economic alternative. They are out to pile every regulation on you they can and every delay they can. Initiatives! They came after us - the uranium industry - in South Dakota and Montana last year. They won in Montana. We tried to reverse it in the legislature, but they were too frightened of public reaction to do it. They did put it on the ballot for reversal in November of '82. That puts it squarely up to us to influence the public so we can win a campaign. There will be more initiatives, and at local levels as well as at state. We must join together and win! The public generally supports the continued operation of nuclear power plants. They about split on whether to build more. But they strongly support regulating the industry more stringently. Every survey reflects concern about safety and the desire for the government to take responsibility and regulate. You and I know that regulation nearly always adds cost, and only sometimes increases safety. We need to influence the creation of regulation. We need to accept responsible regulation and fight that which is counter-productive. To win in hearings, to win initiatives, to win in getting responsible regulation, we need public support. We need an informed, understanding, and supportive public. To accomplish this, we need two kinds of efforts. The first is to reach the people at the local level with local representatives of our industry. Informal conversations at church, PTA, cocktail parties, whatever. Presentations to Kiwanis Clubs, League of Women Voters, church groups - wherever we can. Facts, information in printed form, to these same local audiences with the credibility of the local sources. The second is to reach mass audiences through the media. Positive media. This can be done by advertising, but it is very expensive. We have to look to influencing the reporters and editors to get more balanced and accurate reporting. We need to get free time - interviews, debates, letters to the editors, etc. The Uranium Public Affairs Task Force was created last year to provide tools for you to use to reach these audiences (it is affiliated with the Atomic Industrial Forum). Twenty-two companies provided money and man- power. A consultant, Denver Research Group, was retained to produce materials. In this Phase I effort, we first researched what issues were of greatest concern and what were felt to be the greatest needs in materials. We determined that we did not have the funds to go out and do the job for the industry, so we decided to develop tools for the Industry to go out and do the job for itself. From the research, we determined what tools we should develop for you to use. We first developed a set of the quest- ions most likely to be asked of you and the issues most likely to be thrown up to you. We have developed a loose-leaf notebook. Each page contains one of those questions or issues, a short verbatim response that you can use, a short discussion of the subject, and references you can cite or research for further information. It is organized by subject: tailings, water radiation, etc. This book is an extremely handy tool for anyone in the industry. Each uranium location should have at least one.

Jan 1, 1982

By H. E. Stauss, J. Hino

INTEREST in silicon has arisen again in the past decade as a result of improvements in crystal rectifiers.' Although the preparation of silicon was first reported by Berzelius in 1880, the early product was of relatively low purity, and only the need for rectifiers in World War II led to the production of a 99.9+ pct pure powder. This material in crystalline form was consolidated into massive silicon for use, and the method developed was to melt it with selected added constituents as "doping" agents. Melting techniques, therefore, are of great importance. There are two basic problems in producing silicon ingots free of doping additions; one is the prevention of spitting and the other is prevention of cracking of the ingot during freezing. The most satisfactory arrangement yet developed for producing massive silicon is to melt and freeze in a cylindrical quartz crucible surrounded by a concentric heating element and concentric radiation shields or insulation. For example, use can be made of a tubular heater with a high frequency generator as the source of power and reflecting shields of alundum cylinders. The spitting of silicon is related to gas evolution, and the gas comes from two primary causes—adsorbed gas and the reaction products of silicon and the crucible. Gas is also released from bubbles contained in the quartz crucible walls. Improved removal of adsorbed gas can be achieved by means of controlled melting and freezing. The seriousness of the problem in vacuo is reduced with an electrically operated mechanical movement of the high frequency power coil. The upper portion of the powder charge is melted first and the high frequency coil lowered until the powder is completely molten. During cooling the high frequency coil is raised slowly. These means also reduce the final nonviolent extrusion of large beads of metal through the ingot top during freezing. Better control of spitting and bead extrusion is obtained when melting is done under helium at. atmospheric pressure instead of in vacuo. The problem of reaction between silicon charge and crucible in practice is confined to the reaction between silicon and quartz. This2 apparently is: Si + SiO2 + 2SiO The part that this reaction plays in spitting has not been isolated for separate study. SiO is a volatile vapor at the melting point; of silicon and is released freely during melting in vacuo, but hardly at all in helium at atmospheric pressure. The cracking of ingots is a major difficulty in melting silicon, and its prevention requires special melting techniques or the addition of "toughening" agents such as aluminum or beryllium.' The cracking of the ingots has been explained as being the result of the expansion that occurs upon freezing; although direct observation of freezing ingots reveals visible cracks on the surface only after a red heat has been reached, suggesting that cracking is the result of differential contraction of silicon and quartz. Silicon wets quartz, and the ingot adheres tightly to the crucible. Therefore as ingot and crucible cool, the two either have to pull apart, or at least one must crack. Surprisingly, in spite of the relative thinness of the quartz and the thickness of the ingot, the ingot and the crucible both crack. Microscopic and X-ray4 studies fail to show any plastic flow other than twinning in the ingots. Slow cooling fails to prevent cracking. Another possible solution to cracking is to weaken the crucible. Use of thin-walled crucibles finally led to success with fused quartz crucibles with a wall thickness of 0.25 to 0.50 mm. With such thin-walled fused quartz crucibles consistently uniform success is secured in producing sound ingots 30 mm in diam from the purest available grade of silicon (99.9+) without the use of any type of addition. Melts are made in the size range of 50 to 100 g. Omission of a deliberately added doping agent is not sufficient to insure pure ingots. The reaction of silicon with crucibles and the resultant solution of impurities in the silicon is well-established." In this laboratory, the presence of Al, Be, and Zr has been found spectroscopically in ingots melted in contact with alumina, beryllia, and zircon. The best crucible materials reported in the literature are MgO and SiO2. Use of MgO in this laboratory has resulted in a heavy deposit of magnesium on the furnace walls, showing that a reduction of the magnesia occurred and the resulting magnesium removed from the melt by volatilization. In the case of quartz, the silica is reduced and SiO liberated to deposit on the equipment walls. There probably is real danger that oxygen is dissolved in the ingot when either magnesia or silica is used as the crucible material. Preliminary analyses by Dean Walter in his vacuum unit in this laboratory6 indicate the presence of oxygen in undoped silicon melted in quartz.

Jan 1, 1953

By Stanley Ferguson

Since 1978, the Colorado Department of Health has become involved in specific investigations of possible radiation hazards among nonminers in Colorado communities. In each instance, the improper disposal of mill tailings has precipitated concerns and allegations of radiation hazards. This presentation is a brief summary of the findings, to date, of 4 such investigations involving tailings disposal problems in Canon City, Denver, Durango and Grand Junction, Colorado. Canon City In the summer of 1979, allegations of excessive cancer incidence were made at public hearings concerning an application for a Radioactive Materials License submitted to the Colorado Department of Health by the Cotter Corporation for a uranium mill at Canon City. Canon City is the site of a uranium mill operated since 1958 by Commonwealth Edison. Local residents accumulated figures and calculated rates suggesting a 2-fold excess in total cancer mortality. These rates were not adjusted or standardized for demographic varibles. A review of cancer mortality data and computation of age standardized rates for years 1950 through 1977 showed that Canon City's cancer mortality rates were within expected limits, actually lower than rates for the State of Colorado or the United States. The first slide shows rates for every fifth year, 1950 through 1975. Further, an analysis of Canon City cancer incidence data from the Colorado Central Cancer Registry revealed that 1979 incidence rates were not significantly different from Colorado rates, with the exception of prostate cancer. The next slide shows age standardized incidence rates for lung, colon, breast and prostate cancer. Data were also reviewed for leukemia, myeloma, lymphoma and cancers of the thyroid stomach, uterine certix, ovary, kidney, bladder-and brain, however, small numbers of cases prevented meaningful rate calculation. 1980 data are presently being analyzed. None of the data yet examined support allegations of radiation-associated cancer in Canon City. Denver In February of 1979, the Department of Health became aware of a number of radium mill tailing deposits in the Denver metropolitan area, remnants of the radium milling industry of the early 1900's. Several of the deposits were situated so as to possibly contribute significantly to radiation exposure of a small number of people over a period of several decades. The Department developed protocols for radiation surveys, dosage estimates and, for a small number of persons, body burdens determinations and peripheral blood lymphocyte cytogenetic studies. The results of this investigation suggested no measurable biomedical impact as a result of the radium deposits. Durango In October of 1979, a physician residing in Durango, Colorado released information from a preliminary analysis of lung cancer data suggesting an incidence rate several times expected in that city. The data were presented at a meeting of a citizen's group concerned about the possible health hazards of 2 uranium mill tailing deposits located in the south end of the city. Since cancer incidence data generally do not exist in most of western Colorado, a team of epidemiologists was dispatched to Durango to work with local physicians and hospitals in conducting an epidemiologic study of selected cancers for the period 1969 through 1978. After case-finding and record abstracting were completed, it was determined that sufficient data were available for study of only 3 sites: lung cancer, breast cancer and leukemia. The next slide shows age standardized incidence rates for these 3 sites for 1969-1978 for Durango and the State of Colorado. There are no significant differences in these rates. The data did show a geographic peculiarity with regards to the relative proportion of tumor types near the tailings deposits as opposed to away from the deposits, however, this finding is based upon very small numbers of cases and may represent only the random excursion of rates based upon small observations. This investigation suggests that if a carcinogenic hazard is present, it is too small to be detected by the study method employed. Grand Junction The Department of Health has been involved in the Grand Junction mill tailings problem for several years. In 1966, the Department issued an order terminating the practice of free public access to a 55-acre pile of uranium mill tailings. Prior to this order, an estimated 300,000 tons of material was removed. Of this amount, an estimated 50,000 tons was presumably used in residential and commercial construction. Despite many allegations of cancer and birth defects excesses in Grant Junction since the mid 1960s, the first epidemiologic study of cancer was conducted in the spring of 1977. Data from the Colorado Central Cancer Registry were analyzed and reported to the Executive Director of the Department of Health in June of that year. The findings of the first and preliminary study were an unexplained excess of acute leukemia and chronic myelocytic leukemia. The excess was based upon small numbers but was present across all age groups. No increase in chronic lymphocytic leukemia was evident.

Jan 1, 1981

The Annual General Meeting of the Institute was held in Kelvin House, Johannesburg, on Wednesday, 25th August, 1971, at 4.15 p.m. Mr V. C. Robinson (President) was in the Chair. There were also present fifty one Fellows, twenty one Members, two Associates, two Students and fourteen Visitors, making a total of ninety one. The President declared the meeting open at 4.15 p.m. OBITUARIES The President: 'It is my sad duty to announce the death of the following members of the institute: H. J. G. C. Arndt, Life Member, joined 1933, passed away 11th May, 1971. J. H. A. Diering, Fellow, joined 1921, passed away 24th June, 1971. L. O. W. Leimer, Fellow, joined 1960, passed away 25th June, 1971. E. A. Meltzer, Fellow, joined 1941, passed away April, 1971. As a mark of respect to the memory of the deceased and in sympathy with the bereaved, I would ask you to rise and observe a few moments silence.' MINUTES The President: 'May we confirm the minutes of the General Meeting held on 17th March, 1971, as published in the July, 1971 issue of the Journal?' Agreed. WELCOME TO VISITORS The President: In welcoming you here, ladies and gentlemen, it gives me great pleasure to see so many of our office bearers-our important honorary office bearers-and particularly I would like to welcome our Honorary President, who is, as you know, the President of the Chamber of Mines, Mr John Shilling, and we are 'privileged also to have with us two of our Honorary Vice-Presidents. One in particular I am very pleased to welcome here, and that is Mr G. F. van L. Froneman, who is the Administrator of the Orange Free State, and we extend a very hearty welcome to him, because he is a long way from home. Then we have another Honorary Vice-President, Mr Tommy Gibbs, the Government Mining Engineer, and there are many distinguished guests, whose names I want to give you, so that you will know who they are. We are happy to have present: Mr R. C. J. Goode, Member of Council, I.M.M. London; Mr E. Boden, Manager, A.S. & T.S. of S.A.; Mr G. A. P. Louw, The President, The Associated Scientific and Technical Societies of S.A.; Mr I. R. G. Stephen, The President, The South African Institution of Electrical Engineers; Mr A. S. Robinson, The President, The South African Institution of Civil Engineers; Mr C. F. J. Schneider, The President, The Institute of Land Surveyors of the Transvaal; Mr R. J. Vermaak, The President, The South African Institute of Assayers & Analysts; Prof J. P. F. Sellschop, The President, Joint Council of S.A. Scientific Societies; Mr T. C. Watermeyer, The President, The Federation of Societies of Professional Engineers; Mr G. A. MacWhirther, The President, S.E.I.F.S.A.; Mr C. G. Hinds, The President, The Mine Managers Association; Mr J. F. Aldersley, The President, The South African Institute of Foundrymen; Dr H. O. Reisener, The President, The Institute of Welding; Dr F. P. A. Robinson, The President, S.A. Corrosion Council; Mr A. Bain, The Chairman, Witbank-Middelburg Branch; Prof D. J. Schoeman, The Chairman, The S.A. Institution of Chemical Engineers; Dr N. P. Finkelstein, The Chairman, The South African Chemical Institute (S.Tvl Section); Mr J. M. Meyer, Chairman, O.F.S. Branch. To all these guests and their ladies, I extend a most cordial welcome, and hope that you are going to enjoy the afternoon. MEMBERSHIP The President: 'I have pleasure in announcing that the names of the following candidates having been published in accordance with By-Law 5.2.2., Council has elected them to membership in the following grades: Fellows: Richard Lloyd Blandy, Byron J. Haley. Members: Brian Roger Borton, Frederick Brian Peacock, Peter John Stacey, Kenneth Niles Thanstrom. Students: Peter Boesley James, Kenneth Brian Perel. TRANSFERS From Member to Fellow: Cecil Eugene Fivaz, Peter Edwards. I wish to welcome the new members to the Institute and to congratulate those members who have been transferred to a higher grade. ANNUAL REPORT OF THE COUNCIL AND ACCOUNTS FOR THE YEAR ENDED 30TH JUNE 1971 THE PRESIDENT: We now come, ladies and gentlemen, to the annual report of the Council of the Institute-and our accounts for the year ended 30th June, 1971, and these documents are on your chairs; I know you probably haven't had time to study them yet, but I would like to highlight some of the things which I think are worth mentioning. I would ask you to take, first of all, ladies and gentlemen, the report of the Council as being read, and before moving adoption, however, there are certain salient points I wish to touch on, and I will leave the financial side of this entirely to our very competent and worthy, Honorary Treasurer, Mr Denis Maxwell.

By W. B. Hickman, J. J. Pickell, B. F. Swanson

Many physical properties of the porous media-immiscible liquid system are dependent upon the distribution of fluids within the pores; this in turn, is primarily a function of pore structure, liquid-liquiri interfacial tcnsion and liquid-solid wetting conditions. The cnpillary pressure hysteresis process provides a means of investigating the influence of pore structure upon fluid distribution for consistent sur/acc conditions. Invcstigntiot2s indicate that residual non-wetting-phase saturations /ollozuir,g the imbibition process (i.e.,wetting phase displacing nor2-wctting phase) are dependent upon both pore structure and initial non-raetting phase saturation and suggest that residual fluid is distributed as Discontinuous ,globules, one to a few pore sizes in dimension, thrnugh the entire range 01 pore sizes originally occupied. It clppears that air-mercury capillary pressure dala adequntely rellect the distribution of fluiris in a water-oil system when strong wetting condition preliczil. An oil-air counter-current imbibition technique has also been found to provide a rapid rneans of obtaining residual-initial saturation data. In a majority of cnses, rcsidual saturations detf-rniinecl from the oil-air or air-mercury process reasonably approximate residual oil saturation following water drive of a strongly water-wet medium. INTRODUCTION A reliable estimate of recoverable reserves depends not only on the amount of original oil-in-place but also on pore geometry and distribution of fluids within the pores. A critical parameter determining the recovery from a reservoir under waterflood, for example, is the amount and distribution of residual oil within the various rock types present. The purpose of this paper is to investigate the mechanism of capillary trapping and assess its importance in laboratory measureqents of residual oil saturation. The degree of wettability of a reservoir rock is recognized as an important factor in waterflood or imbibition experiments. In this paper, however, only the water-wet case has been considered. Considerable experimental evidence1 suggests that for water-wet rocks, capillary forces predominate in tile distribution of fluids and that viscous forces in the range normallv of interest in the reservoir have a minimum influence on residual oil saturation. It follows that if the ultimate recovery is controlled by pore geometry, a unique residual non-wetting phase saturation should exist for a given set of initial conditions. Two laboratory procedures.found to be extremely useful in the study of pore structure and degree of fluid interconnection at various saturations are decribed. Although air-nercury capillary injection curves have been used2 previously to characterize the drainage case, the withdrawal or imbibition case can provide valuable supplementary data. The air-mercury process, however, has several disadvantages; it is difficult to run in a sufficiently accurate manner, mercury does not always act as a strongly non-wetting liquid and in the air-mercury process the sample is rendered unsuitable for future analyses. An alternative process is described in which air is the non-wetting phase and naptha, hentane, octane or toluene is the wetting phase. INTERFACIAL TENSION AND CAPILLARY PRESSURE Interfacial tension between immiscible fluids is due to the difference in attraction of like molecules as compared with their attraction to molecules of the neighbouring fluid. This net attraction results in a tension at the interface. To extend the interface; thus, interfacial tension s can also be thought of as free surface energy. Interfacial tension is normally expressed as dynes/cm, and interfacial energy is measured in ergs/cm2 hence, both have dimensions ml A 2 and are numerically equal.

Jan 1, 1967

By J. C. Swartz

New measurements of graphite and cementite solubilities in ferrite have been obtained to resolve disagreements among previous data. To measure graphite solubility, specimens of iron were equilibrated with rarious carburizing atmospheres at temperatures be-twee~z 480" and 1435°C. The carbon activity of each atmosphere relative to graphite was taken from published data. After quenching from each equilibration treatment the concentration of carbon (typically 10 pprn by wt) was determined from the height of the Snoek peak in the internal friction spectrum. A few inclividual analyses by combustion support the reszdts of Smith on the solubility of graphite near the eutectoid temperature. Combination of these combustion and internal friction analyses determines In a, (at 0.01 wt pct) = 24,000/RT - 12.72, where a, is the activtity relative to graphite in ferrite at fixed cornposition. The same specimens were used to determine the solubility of self-stressed cementite precipitates. The results indicate solubilities of 6.3, 23.2, and 68 pprn carbon by wt at respectively 400°, 500". and 600°C. The once large discrepancy between the cementite solubility determined by internal frictiori and that calculated from flee energy data has been almost completely resolved. A recent study1 (hereafter designated I) on the solubility of cementite in a iron did not fully resolve the disagreement among previous data. The remaining disagreement is illustrated by the phase diagram in Fig. L The data of I are represented by the line labeled "stress-free" cementite. They determine a heat of solution of cementite of (14.8 * 0.2) kcal per mole which contrasts with the (20 * 1) kcal per mole derived from Smith's graphite solubility2 and the formation energy of cementite.3 Toward resolving this disagreement we have obtained new data on the solubilities of graphite and cementite. METHODS As in I the Snoek peak in the internal friction spectrum was used to measure the concentration of carbon dissolved in ferrite. This method relies on the relation C=kQ-1 [1] in which C is the concentration of dissolved carbon, Q-I is the Snoek peak height, and k is a proportionality factor which is a function of the peak temperature, polycrystalline texture, and other parameters characteristic of the ferrite lattice. To determine true heats of solution via Eq. [1], it is necessary to establish that k is independent of the temperature from which the specimen is quenched. Some evidence on this point is contained in a separate report.* Additional evidence is shown by the data points in Fig. 1. These represent the Snoek peaks of two specimens carburized to about 10 ppm C, copper plated, and quenched first from 888º then from 588°C. The copper plate was removed before each Snoek peak measurement. These data show that there is no detectable dependence of k on quenching temperature. The solubility of graphite was determined by repeatedly carburizing various specimens of iron wire with gas mixtures of known carbon activity relative to graphite. To cover a wide temperature range within the a phase boundaries it is desirable to use as low a carbon concentration as is compatible with reasonable precision. With the present internal friction apparatus the best compromise of these desires is a concentration near 10 wt ppm. The dashed line in Fig. 1 was used to approximate the activity of carbon* for

Jan 1, 1970