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By T. N. Williamson

Most U.S. coal production is bituminous coal. Some 90% of current production comes from a geographical area enclosed in a circle with a 300 mile radius and its center at about Huntington, West Virginia. There are important underground coal production areas in the western parts of the United States as well. Most U.S. coal production comes from fairly level seams, many of which pitch rather uniformly only a few feet per mile. Usually there will be several overlying seams of varying thicknesses, separated by several tens of feet. Fig. 1. 1. Seams have minor local undulations but these? are small enough not to be a major consideration in a horizontal drilling research program.

Jan 1, 1970

By L. S. Beck

"The Athabasca region forms part of the Churchill province of the Canadian Shield and is underlain by an Archean or Aphebian assemblage of rocks that underwent severe metamorphism and granitization during the Hudsonian orogeny (1750-1950 m.y. ago). In places, the eroded orogen is overlain by unmetamorphosed cover rocks (in-cluding the Martin and Athabasca formations) of probable Paleohelikian age. Basic dykes cut all the rocks of the region.There are innumerable vein-type pitchblende deposits and many syngenetic occurrences of uraninite in crystalline basement rocks. Evidence is presented to show that pitch-blende was emplaced during the final stages of the Hud-sonian granitization and followed the crystallization of syngenetic uraninite transitionally. In terms of P-T condi-tions, the pitchblende deposits belong essentially to Lindgren's mesothermal group.Based on the postulated uranium metallogenesis, the possibilities of finding further deposits of pitchblende and other types of uranium deposits are discussed."

Jan 1, 1970

By John F. Abel

In Silver Plume, Colo., there is a bachelor miner who offers individualized tours of his mine, The Silver Cloud. It is an interesting tour because he drove the mine himself and the view from the shack up there is spectacular. Beside that, he will probably invite you into his kitchen to sit around the old cook stove and drink coffee. When Andy first started his tour business he put a sign on the main street to advertise the fact. The sign read in part: "Women not welcome, but they will be tolerated at $3.00 a head”- the usual fee is $2.50. The sign lasted about 48 hours. Andy had to take it down because "all the ladies in town got mad at me. Now I take them all for $2.50 right across the board," he says. The mining industry is not only reticent about hiring women but traditionally does not even permit women to enter some mines. It would appear, what with the recent action on an equal-rights-for- women amendment in Congress, that we may be wise to examine the prospect.

Jan 1, 1970

By Donald R. Rathburn

Screening during the production of high-grade lump ore for blast furnace burden, particularly from recently developed ore deposits in Australia, South America, and Africa, has resulted in large tonnages of fine iron ore. Certain owners have decided to stockpile these fines until some later date; however, others have either sold these fines "as is" for agglomeration at the steel plant or have established their own pelletizing plants to produce a premium quality agglomerate. Normally these fines consist of the higher oxides of iron and the hydrated oxides. Unfortunately, grinding these types of materials in a wet process produces a slurry that is difficult to filter to obtain the requisite moisture level for the subsequent balling and indurating operations. The purpose of this paper is to review recent developments in fine dry grinding of iron ore and to discuss the various design and operating parameters involved. Although dry grinding of raw feed and clinker has been practiced in the cement industry for many decades, its significant application to the iron ore industry has taken place within the past ten years. Even though the basic concept of dry grinding has been borrowed from the cement industry, the successful application to iron ore grinding has not taken place without some difficulties. Consequently, the application to iron ore has required the solution of several unique design and operating problems.

Jan 1, 1970

By Gligorije Stankovic

This paper describes the fluo-solids roaster and acid plants at the new 40,000-TPY Trepca electrolytic zinc plant. The electrolytic zinc plant units were constructed to the design of Singmaster and Breyer, New York and began operation in mid-1967. The fluo-solids roaster plant, constructed according to the design of Dorr-Oliver, Paris, includes concentrate handling and storage facilities; two independent concentrate roasting circuits, each with a 110 to 155 TPD fluo-solids roaster; waste heat boilers; cyclones; electrostatic precipitators; calcine coolers; and calcine conveyors. The acid plant uses the "Petersen system" contact process. The plant has one acid circuit with a capacity of 230 tons of monohydrate per day. Gases for the acid plant are obtained from roasting zinc concentrates. When the roaster plant is operating at maximum capacity, excess SO2 is used in two other Petersen System circuits in the near vicinity.

Jan 1, 1970

By T. E. Wayland

Bentonites are clay materials composed principally of minerals in the montmorillonite group. Distinctive physical properties of the montmorillonite minerals are responsible for selected bentonite deposits having become the raw materials source of industrial clay products which are virtually essential to the maintenance of high production standards in the petroleum, foundry, taconite and other basic industries. These versatile materials have no suitable substitutes in either their major applications or in hundreds of speciality products, The economics of the bentonite mining industry follows closely the established pattern of other non-metallic raw materials. Aggressive competition, advanced technologies, progressive marketing techniques, substantial reserves, and vast unmeasured resources insure the continued supply of high quality bentonite to industry at bargain prices. The purpose of this paper is to discuss the geology and economics of bentonite deposits, summarize both major domestic mining districts and foreign deposits, and report significant results of research and development.

Jan 1, 1970

By R. F. Yap, N. Arbiter, C. C. Harris

A fully-instrumented driving mechanism has been constructed to study the power, aerating and solid suspension characteristics of several laboratory flotation machines. Machines operating over normal flotation speed ranges give substantially constant power numbers in liquid systems indicating that they operate close to fully baffled turbulent flow conditions. Owing to lack of geometrical scaling, power numbers for different sizes of cells of the same make are different. Even larger differences occur between cells of different manufacturers. For a given impeller, varying the tank size did not significantly affect the power consumption. Tank geometry and baffling has a slight effect on power consumption with shrouded impellers. For a given impeller speed, suspension height decreases while power increases with increasing mass of solids in suspension. While power consumption is hardly affected by particle size and clearance between the impeller and tank bottom, the suspension height significantly increases as clearance increases and as particle size decreases. Aeration was found to affect not only power but also the suspension characteristics of the machine. For closely sized particles, drastic sedimentation occurred when a critical value of the air flow number was exceeded. The critical air flow number decreased with increasing particle size. This effect was less marked with a wide particle size range. The self-aerating capacity of flotation machines increases with cell size at a given speed for the same impeller-shroud system, but decreases in the presence of frother and solids. Equations have been established for correlating all of the studied variables. Data taken from the literature were also correlated with these equations. The modern mechanical flotation machine has, over a period of 60 years, displaced other designs to become the dominant type. Once the correct chemical environmental conditions have been established, the major requirement, selective mineral-air adherence, is essentially a function of two operating variables — impeller speed and air rate. The special nature of this dependence is such that in the same apparatus, but under different operating conditions, adherence can be either prevented or destroyed. Another aspect of this observation is that flotation machines though differing in detail to a considerable extent can produce similar metallurgical results. It must be concluded that having determined the correct reagent levels, establishing the correct operating conditions are at least as important as machine design. Since about 1960, after 30 years of fairly stable circumstances, manufacturers have been developing new types of machines whose major feature is emphasis on pulp flow characteristics by virtue of new im-peller-stator designs. As far as can be ascertained, these new designs necessitate radical departures from accepted impeller speed-air rate values. Performance data are still awaited. Flotation machine development has been empirical, as is selection of operating conditions. The purpose of the work at Columbia University has been to elucidate the fundamentals of the subject so that the purely mechanical aspects of the flotation process can be understood in hydrodynamic terms.1-6 Hopefully, this might lead to intelligent selection of a particular machine and its operating conditions for a specific ore based on a minimum of testing, or even to new types of flotation machines. The present investigation is the most comprehensive to date.7,8 Earlier work, which was largely exploratory, has been repeated and extended and employes the most accurate measuring techniques available. Additionally, sufficient hydrodynamic data were obtained under flotation conditions to delineate the relevant operating ranges. Attention has been given to scaling in that several geometrically scaled tanks and impellers have been constructed and tested; it has been pointed out elsewhere that undistorted geometrical scaling rarely pertains in flotation machine design.5 This paper is divided into sections dealing with relevant combinations of the three phases: liquid, air and solid. Summaries of the literature have been given in previous publications2-4 and will not be repeated here. Recently, several reviews of mixing have appeared, which can be usefully referenced.9-11 It is of interest to note that flotation is not included

Jan 1, 1970

By Donald Towse

Portland cement is a basic building material in every country in the world, and, fortunately, the raw materials required in its manufacture are widely distributed. It is a low-priced bulk commodity (price one cent a pound or less, with a density of 100 pounds per cubic foot.) Table 1. Approximate price per pound of selected mineral products. Copper 48 cents per pound Aluminum 27 Lead and zinc 15 Asbestos 3 to 18 Pumice 6 Sulfur 2 Bauxite (abrasive) 1.8 Barite 1 to 1.6 Cement 1 Primitive regions may get along without any Portland cement, but most countries use some, and it is one of the most widespread building materials, even if used in small quantities. Use of cement begins early in a country's development, and, because of local availability of raw materials, cement manufacture is one of the first heavy industries many countries desire. Use and manufacture of cement usually precedes other industrial materials such as steel and heavy chemicals, and consumption levels off for a long period during development of infrastructure and an economic base. With a mature economy comes a very high consumption. Per capita consumption varies ten times or more between nations (Figure 1).

Jan 1, 1970

By Saul J. Escalera

Mechanisms involved in the depression of the sulfides: pyrite, chalcopyrite, galena and sphalerite with potassium permanganate have been investigated. Flotation tests were conducted using potassium amyl xanthate, Z-6, and pine oil in the absence and presence of potassium permanganate at around pH = 6. 5 naturally yielded by the sulfides in the pulp. On the basis of crystal chemistry considerations, the amount of xanthate adsorbed by the sulfides depends on the amount of sulfur and metal ions present on the surface; thus, the avidity of the sulfides for xanthate should increase in the order: sphalerite C chalcopyrite 4 galena 4 pyrite, and the ease of depression response to the permanganate action should be in the same order. Depression of the sulfides in the system occurs primarily due to the removal of the collector ions by the permanganate ions to form manganese dioxide and dixanthogen according to the reaction: 3 M(RX)2 + 2 Mn04 + 4 H20 2 ? MnO2 + 3(RX-XR) + 3 M+2 8OH where M represents the metal ion, RX the xanthate ion and (RX-XR) the dixanthogen molecule. Results seem to indicate that the permanganate ions play a triple role in the system: (1) they convert xanthate ions into dixanthogen, (2) they further oxidize the mineral surface and (3) if present in excess, they may oxidize the xanthate beyond the dixanthogen stage with the formation of CO2, H20 and SO4. All sulfides, except for chalcopyrite, showed a depression response in the order predicted regardless of the order of addition of xanthate and permanganate reagents. Chalcopyrite did not depress as easily; this behavior may be due to the avidity of the colloidal MnO2 to adsorb Cu+2 ions on its surface, this would destabilize the colloid making it coalesce with the formation of a layer of precipitated MnO2 on the surface of the mineral. The presence of this layer would prevent further action of the permanganate ions on chalcopyrite.

Jan 1, 1970

By N. H. Coates

The Bureau of Mines designed, constructed, and operated an 18-inch- diameter, fluidized-bed combustor for highly caking coals to evaluate the method for possible application to power generation. In initial tests, combustion was carried on successfully, with carbon losses as low as 0.8 percent. Coal ash was not satisfactory as a bed material, but mullite proved to be acceptable. Overall heat-transfer coefficients from the bed (-20 + 50 mesh mullite) to a water-cooled tube were about 75 Btu/hr-ft2- °F.

Jan 1, 1970

By Robert E. Goodwin

As man's need for minerals continues to grow and as the known mineral deposits become depleted, it may be expected that these increased demands will result in greater exploration for additional deposits and at continually increasing depths below the earth's surface. As labor and material costs continue to rise, the need for more economic material handling will be emphasized. The quest for heavier payloads, safely moved at faster speeds from deeper mines, will be vigorously pursued. Strenuous efforts are, therefore, being made in the wire rope industry to develop ropes with greater strength-to-weight ratios than presently available while maintaining the dependability and long life being received from the conventional rope manufactured today. For many years, high quality rope wire has been manufactured from rods of selected steel compositions. Carefully-controlled wire drawing combined with proper heat treatment has resulted in high quality wire and wire rope throughout this period. Refinements in the rod produced from specially-selected high carbon steels combined with the latest improvements in wire drawing and heat treatments have made it possible to manufacture higher strength rope wire of uniform composition and structure that is suitable for use in Special High Strength wire rope.

Jan 1, 1970

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 John F. Abel

In the debate between miners and ecologists, our industry has at last begun to get some of its story told. I have been told many times that it is hopeless to even try to get our side across. Some are sure that no one will believe us even when our cause is just. My reply would be that we have to tell the truth; again, again, and again. We will never convert a fanatic, but we must try to reach the reasonable and thinking people. I am encouraged because more of us are trying. Various mining companies here in Arizona have bought newspaper space to set forth some of the facts around our local environmental problems. The Arizona Mining Association co-sponsored a symposium in March: Mining and Ecology in the Arid Environment. The symposium program included tours arranged with local mining companies. The participants saw an acid plant, an acid leaching operation, an alluvial tailings dike, a tailings pond, a smelter, and a couple of open pit mines. This wouldn't phase you until you realized that half the visitors were ecologists, watershed and wild- life managers, and other assorted conservationists. It took a lot of guts. I am proud that we had that much confidence. As Pogo said, "We have met the enemy and they is us!" Actually, we met the enemy and they were just like us-concerned.

Jan 1, 1970

By Frank E. Woolley, John F. Elliott

Mathematical models of the transient thermal behavior of a high-temperature solution calorimeter1-3 have been developed. The thermal behavior of the calorimeter is appoxirrzated by linear lumped-parameter models, and hence is described by sets of linear ordinary differential equations with constant coefficients The response of the models to various inputs is shown to agree with the response of the real system. Application of the modeling to experimental design and analysis of data illustrates the usefulness of simple models of complex systems. The early eperiments1,2 with the high-temperature solution calorimeter indicated that the change in the temperature of the bath resulting from the addition of a solute sample to the bath involved not only the direct effect due to the solution process but also possibly a secondary effect arising from the change in coupling between the bath and the induction heating coil. Consequently, an extensive analysis of the calorimeter was carried out, and models of the transient thermal processes of the instrument were developed to aid in improving the design and interpreting the behavior of the system. This paper describes the dynamic modeling; the use of it in treating experimental results has been reported earlier.3 The high-temperature solution calorimeter was constructed to measure directly the partial molar heats of solution of solute elements in a variety of liquid metal solvents.1-3 The calorimeter consists of an induction-heated liquid metal bath into which small samples of a solute element can be dropped. The bath temperature is recorded continuously, and the change in the measured bath temperature with time, dTm = f(t), resulting from the solute addition are the raw data from which the enthalpy change caused by the addition is determined. To extract the rmodynamic results from the data, the temperature change must be compared with that resulting from calibration additions of known enthalpy change. Accordingly, it is necessary to understand the transient thermal processes arising as a result of the addition to the bath. Neither modeling nor experimentation alone could provide the required insight into the working of the calorimeter. The alternate use of both methods in conjunction greatly assisted the design of the equipment and experiments, and the interpretation of the data. THE PHYSICAL CHARACTER OF THE SYSTEM The essential parts of the calorimeter, Fig. 1, for model studies are the thermocouple, the liquid metal bath and the surrounding refractories. The system is the solvent metal bath and those refractories around it which undergo a temperature change as a result of an addition to the bath, and which determine the way the temperature of the bath responds to an input. The inputs are the combined transient thermal effects arising when an addition is made to the bath. They include the thermal effects of the addition itself and the results of changed coupling between the bath and the induction coil. The response is the variation in the measured bath temperature, dTm(t) = Tm(t) - Tm(O), from an initial steady state resulting from the inputs. It was assumed in this study that the physical properties of the various elements of the system are independent of the inputs and time, although these properties may vary as the result of changes in the composition and size of the bath during a series of additions. This separation of inputs and the system is equivalent to assuming that the system is linear, i.e., that its behavior can be described by linear differential equations with constant coefficients. Linear behavior can be expected whenever the departure of each portion of the system from its steady-state condition is small enough to cause negligible changes in the thermal properties of the materials and in the various heat-transfer coefficients. Radiative heat transfer is important in this system, so the assumption of linearity should be valid only for small temperature deviations. Several conclusions were drawn from operation of the calorimeter in earlier experimental studies: 1) Radiative heat transport from the top of the bath is a significant portion of the total heat lost from the bath. However, for small changes in the bath temperature the change in transport by this path could be assumed to be proportional to the change in the bath temperature. 2) A very small portion of the heat input is lost through the thermocouple to its water-cooled holder. The thermal resistance and thermal capacity of the thermocouple protection tube are small, so the temperature of the thermocouple should follow closely that of the bath. 3) The remainder of the total heat lost from the bath will pass by conduction through the crucible to, and through, the other refractories, eventually being absorbed by the water-cooled induction coil or by the water-cooled sides and bottom of the enclosure. 4) The thermal resistance between the bath and crucible is very small. Thus the thermal capacity of the crucible will affect the temperature of the bath very soon after an addition of heat to the bath. 5) The thermal resistance between the crucible and the silica sleeve is large, especially if a radiation shield is placed in the gap. The effect of the thermal capacity of the sleeve thus will be significant only at longer times. The thermal resistance through the packing below the crucible also is large, so the packing and the silica sleeve will have similar effects on the behavior of the system. 6) A large temperature drop exists across the gap containing the water-cooled induction coil. Thus for relatively small changes in the thermal input to the bath, the refractories beyond the sleeve

Jan 1, 1970

MR. RIGG: Gentlemen, I would like to welcome you all to the symposium this morning. My name is Jack Rigg, and I m a special assistant to Hollis Dole, Assistant Secretary of the Interior for Mineral Resources. Hollis is not in town this morning, and I am here to pinch-hit for him. The first order of business this morning is remarks by the Honorable Russell Train, Under Secretary of the Department of Interior. Mr. Train. MR. TRAIN: Thank you, Mr. Rigg. Lest you think that Hollis Dole is not interested in this symposium, let me just say that fie is flying back from Australia just to be here. He is heading up a United States delegation in Australia meeting on resource problems in the Pacific. And I believe he will be here about noon.

Jan 1, 1970

By Henry C. Meeves

The Bureau of Mines investigated the silver production potential of the Leadville (California) mining district, Lake County, Colo., in 1966-67. The mining history of the district, the ground conditions encountered in mining, and the mine-support methods used are reviewed. The drainage problem is discussed in detail. An initial objective was to establish the existence of potential silver resources minable by low-cost open-pit methods, particularly in the silver-bearing manganese halos surrounding the major deposits. The report concludes that under present conditions, development of the deposits in the area is not economically feasible; however, a pioneer rotary noncore drilling program demonstrated that this type of exploration is technically feasible. Potential reserves of silver and associated metals are estimated. Possible mining methods for recovery of the reserves are discussed. Future production possibilities from the various subareas of the district are analysed, considering optimum operating size. Consolidation of small individual holdings for unit operation is recommended. Type of operation, amount of rehabilitation, size and type of concentrating plants required, drainage and other mining problems, and metal price trends are discussed as they bear on economic feasibility of development.

Jan 1, 1970

By R. W. Michelson

The Bureau of Mines developed computerized mathematical models to estimate the economic availability of Mesabi Range taconite concentrates; these are a quality model, a cost model, and an economic availability model. The quality model evaluates metallurgical test data; the cost model determines iron unit cost from mining and processing cost data; and the economic availability model determines quantity from geologic and ore quality data. By correlating all of the physical resource quality factors and dimensional characteristics with the economic cost factors associated with producing iron ore pellets, these three models combine to establish a final relation between iron ore reserve quantities and iron unit cost.

Jan 1, 1970

Up to 19 chemical parameters were studied in flotation pulps in six Australian lead-zinc concentrators with the aim of obtaining a better understanding of the nature of, and changes in, the chemical environment. This paperdiscusses collector residuals, metal concentrations in solution, and other parameters.Collectors used in the plants studied were various xanthates, Z-200, and Aerofloats. Xanthate residuals varied in different ways in most plants. However the general trend was for residuals to be at the O· 5-2 p.p.m. level in lead flotation and O· 5 p.p.m. or less in zinc flotation.Aerofloat residuals were also variable but in the plant concerned were at a much higher level (8-10 p.p.m.) than xanthate residuals. Z-200 residuals were in the 10-20 p.p.m. range and it was found that the Z-200 added to zinc flotation was reporting in dam return water and entering lead flotation.Copper concentrations in solution were negligibly low in those plants where cyanide was not used. When cyanide was used, copper was at the 5-20 p.p.m. level and appeared to be present as Cu(CN)-2. However the hiocyanatepresent may be important. Xanthate was also present in these solutions.Zinc concentrations ranged from 0·1 to 800 p.p.m. in different plants. The general trend was for the zinc level to be highest in the grinding circuit and to drop during flotation. However there was always an increase in zinc concentration when copper sulphate was added, even tho.ugh this incre.ase was not permanent, and the increase was greater with higher copper sulphate additions.The manganese concentration also increased appreciably during copper-activation of marmatite. In some plants lead concentrations increased from 0·1 to 1 p.p.m. during activation of marmatite.Calcium concentrations (20-1200 p.p.m.) and magnesium concentrations (10-600 p.p.m.) tended to be fairly stable in each circuit.

Jan 1, 1970

By D. T. Peters, S. Floreen

The age hardening behavior of an Fe-8Ni-13Mo alloy was studied after the matrix had been varied to produce either ferrite, cold u~orked ferrite, or nzassive nzartensite. The aging behavior of the cold worked ferrite and murtensite structures were very similar. The martensite aging kinetics were much different from those observed in earlier studies of aging of maraging steels, even though the martensite wzatri.r had the same dislocation structure as those found in maraging steels. The results suggest that the previously observed precipitation kinetics of maraging steels ?nay have been controlled by the nucleation be-haviov, which in turn were dictated by the alloy compositions and the resultant identities of the precipitating phases. IT is well known that the rate of precipitation from solid solution depends not only on the degree of super-saturation, but also on the density and distribution of dislocations in the matrix structure. These imperfections often act as nucleation sites, and may also enhance atomic mobility. 'Thus, the presence of dislocations is important since the type and distribution of precipitates may be determined by them. The precipitate density and morphology in turn affects the mechanical properties of the alloy. A number of studies have been devoted to the precipitation characteristics in various types of maraging steels.'-" These are iron-base alloys containing 10 to 25 pct Ni along with other substitutional elements such as Mo, Ti, Al, and so forth, that are used to produce age hardening. The carbon contents of these steels are quite low, and carbide precipitation is not believed to play any significant role in the aging reactions. After solution annealing and cooling these alloys generally transfclrm to a bcc lath or massive martensite structure characterized by elongated martensite platelets that are separated from each other by low angle boundaries, and that contain a very high dislocation den~it~.~~~~~~~~-~~ Age hardening is then conducted at temperatures on the order of 800" to 1000°F to produce substitutional element precipitation within the massive martensite matrix. Most of the aging studies to date have revealed several common traits in these alloys, regardless of the particular identity of the precipitation elements. Generally hardening has been found to be extremely rapid, with incubation times that approach zero. The agng kinetics, at least up to the time when reversion of the martensite matrix to austenite begins to predominate, frequently follow a AX/~~ = ktn type law, where x is hardness or electrical resistivity, t is the time, and k and n are constants. The values of n are frequently on the order of 0.2 to 0.5, which are well below the idealized values of n based on diffusion controlled precipitate growth models. Finally, the observed activation energy values are typically on the order of 30 kcal per mole, and thus are well below the nominal value of about 60 kcal per mole found for substitutional element diffusion in ferrite. The common explanation of these observations is that the precipitation kinetics are controlled by the massive martensite matrix structure. Thus, the absence of any noticeable incubation time has been attributed, after ~ahn," to the fact that the precipitate nucleation on dislocations may occur without a finite activation energy barrier. The low values of the activation energy are generally assumed to be due to enhanced diffusivity in the highly faulted structure. If this explanation that the precipitation kinetics are dominated by the matrix structure is correct then one should observe a distinct difference in lunetics between aging in a martensitic matrix and aging the same alloy when it has a ferritic matrix. Such a comparison cannot be made with conventional maraging compositions, but could be made with the alloy used in the present study. In addition, the ferritic structure of the present alloy could be cold worked to produce a high dislocation density so that one could determine whether ferrite in this condition would age similarly to martensite. EXPERIMENTAL PROCEDURE The composition of the alloy used in this study was 8.1 pct Ni, 13.0 pct Mo, 0.10 pct Al, 0.13 pct Ti, 0.012 pct C, bal Fe. The alloy was prepared as a 40 lb vacuum induction melt. The heat was homogenized and hot forged at 2100°F to 2 by 2 in. bar, and then hot rolled at 1900°F to $ in. bar stock. The aging lunetics were followed by Rockwell C hardness and electrical resistivity measurements. Samples for hardness testing were prepared as small strips approximately 2 by $ by 4 in. thick. Electrical resistivity was studied on cylindrical samples approximately 2 in. long by 0.1 in. diam. The method for making the alloy either martensitic or ferritic was based on the fact that the alloy showed a closed y loop type of phase diagram. At high temperatures, above approximately 24003F, the alloy was entirely ferritic. Small samples on the order of the dimensions described above remained entirely ferritic after iced-brine quenching from this temperature. In practice, a heat treatment of 1 hr in an inert atmosphere at 2500°F followed by water quenching was used to produce the ferritic microstructure. These samples were quite coarse grained and usually en-

Jan 1, 1970

By D. Brabec

One of the analytical problems in exploration geochemistry is the choice of a method of sample attack which would be rapid, simple and reliable in terms of precision and discrimination between different concentration levels of elements sought. The wet sample attacks currently used in analysis of silicate rocks vary from total decomposition to leaching by weak extractants. The total decomposition of such materials is usually achieved either by alkaline fusion or hydrofluoric acid attack. The first method requires the use of platinum vessels which is both expensive and slow for batch operation. The second type of attack is more widely applied in rock geochemistry1, but it is still relatively slow for exploration purposes and requires extra care (especially when hydrofluoric acid is used in mixture with perchloric acid). Considerable improvement in speed can be achieved by using the sample attacks which release only part of the metal present in a rock.2,4 One of such attacks is the leaching of pulverized rocks by hot aqua regia.3 Another technique widely used in geochemical prospecting involves fusion of the samples with potassium pyrosulfate (or bisulfate) followed by an acid leach of the malt .5 One of the advantages of these techniques is the use of glassware in decomposition stage which considerably increases the analytical productivity. It should be noted that partial chemical attacks tend to extract from a rock mainly the non-silicate metal which may give results more significant for exploration purposes than the analysis for total metal.

Jan 1, 1970