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By Nelson Severinghaus

FOLLOWING the end of hostilities of World War II, a resurgence of industrial and home building has given impetus to the use of many products of the stone industry. Shortage and high prices of some building materials such as lumber have aided wider acceptance of materials such as concrete products which have been relatively plentiful and which have not risen so rapidly in price. Ingredients for many of these substituting materials come from the stone industries, often from by-products of stone operations. Most of the tonnage of the stone industry in the State of Georgia comes from granite and marble. There are extensive dimension stone operations in granite in the Elberton and in the Lithonia areas. Building and monumental marble from the Tate area has been used throughout the country. Cutting operations in both types of stone have their by-products in faulty blocks and in spalls. In the State there are three large crushed-stone plants utilizing granite, one near Camak, one near Lithonia and one at Stockbridge. All have had excess fines or screenings in the past but this excess is largely disappearing with development of new uses. At times this "waste" has amounted to as much as 20 pct of the stone quarried. Handling of this large tonnage from point of screening out to storage piles presented a costly problem and large areas were taken up by the piles. Crushed stone is generally sold with a relatively narrow margin of price over cost, so any elimination of disposal cost or increase of income by marketing of by-products is highly desirable. BY-PRODUCTS OF GRANITE DIMENSION STONE It sometimes becomes difficult to differentiate between main product and by-product. In the cutting of granite dimension stone in the Lithonia district of Georgia, a considerable quantity of remnants of uneven shape and size is produced. The larger of these pieces have long found use as building rubble, particularly for retaining walls and building foundations (Fig I). They are broken down to one man size by plug drilling and wedging and by hammer. In recent times, demand for this former by-product has grown so that quarries have been opened for the production of rubble as a main product. Local masons have attained skill in using these irregular shapes to form economical and attractive walls. Areas such as Elberton, Georgia, which do not have a large building market nearby, tend to accumulate piles of large pieces of reject stone. When a road job or other local construction offers a quantity market for crushed stone, a portable crusher works this material down to crushed aggregate. Spalls and finer chips from granite stone-cutting operations have generally found their way into crushers and thence to the many uses for crushed aggregate. One company near Lithonia started marketing the smaller by-product crushed sizes for chicken grit about ten years ago. This use has grown to nation-wide distribution and the tonnage is now so great that they have opened a large quarry with

Jan 1, 1947

G. M. TAYLOR,* Colorado Springs, Co1o.-I do not think the plan outlined in this paper would work at Cripple Creek. Most of our men have had a pretty good education. The Cripple Creek district is a lessee district-I do not think there is one mine operating in Cripple Creek to-day that does not have the leasing system. We have as many men leasing on our property as we have mining and every plan who is working for wages is looking for n lease-everyman has mined for him- self, he has been his on7n boss on n lease, either on our own property or

Jan 1, 1919

By James E. Howard

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

Mar 1, 1908

By Joseph A. Holmes

The public is already familiar with the general fact that the scope and the financial resources of the approaching St. Louis World's Fair are much larger than those of any of the preceding great expositions; and both the visitor and the exhibitor, when he comes to St. Louis in 1904, will find it to be a real World's Pair, with exhibits and visitors from every known country. Passing over the subject, as to the general Exposition, with this brief statement, I ask Sour attention to the consideration of a few important facts connected with the proposed mining exhibits at this Exposition. First of all, I may say that. reading- and writing-rooms and library facilities will be furnished in the Mines Building for miners and mining engineers, and it is expected that when they visit the Exposition they will make these rooms their headquarters, and give the Chief of the Department and his assistants an opportunity to extend to them such courtesies as may be possible. One of the exhibits in the Mines Department will consist of models and maps arranged to show the nature and extent of the mining operations in the United States at the time of the purchase of the Louisiana Territory in 1803, the event which

Jan 1, 1903

By W. G. Matteson

In 1915, the State of California passed a law of great scope and importance. This law has been in successful operation for a year and may be briefly described as an act " establishing and creating a department of the State Mining Bureau for the protection of the natural resources of petroleum and gas from waste and destrucbion through improper operations in production; providing for the inspection of petroleum and gas wells; requiring all persons operating petroleum and gas wells to make certain reports" and providing the necessary officers and assessments to carry out the provisions of the act. The statute provides for a separate department of the State Mining Bureau, under the general supervision of the State mineralogist, with a staff composed of a "state oil and gas supervisor" and four deputies. It rules that all petroleum and natural gas wells shall be drilled, operated or abandoned under the supervision of the State supervisor, who shall order such tests or remedial work as seems to him necessary to protect the interests of property owners and the general public. It also provides for a board of arbitration to consider orders given by the supervisor which are not acceptable to the well owner. Section 18 of the act, which is the provision that is directly related to this paper, requires ('the owner of any well referred to in this act to keep a careful and accurate log of the drilling of such well," and further requires that this log shall show the character and depth of the formations passed through or encountered in the drilling, particularly the location and depth of the water-bearing strata; the character of the water encountered (so far as ascertained); whether the water was shut off, and, if solat what point; that it shall show completely the amounts, kinds and size of casing used; the depth at which oil-bearing strata are encountered; the depth and character of the strata, and whether all water was successfully and permanently shut off so as to prevent percolation or penetration into the oil-bearing strata. This log is to be kept in the local office of the owner or operator, subject to the inspection of the supervisor or any of his deputies at any

Jan 1, 1917

By A. L. Holley

The general usage of engineers, manufacturers, and merchants, is gradually, bat surely, fixing the answer to this question. In every country rails, boiler-plates, and machinery bars, whether hard or soft, are almost universally called steel, when they are made from cast ingots. Other names for the softer steels, such as " homogeneous metal,'' "Bessemer iron," " Martin iron," and the like, have failed to obtain general recognition. The meaning of the term steel, before it was enlarged to cover newly developing varieties, has been traced, by a recent writer, down through Percy, Shakspeare, and the Bible, in a most interesting manner, from an archœological point of view. Undoubtedly, it did characterize hardness arid other qualities imparted by carbon. It is within the memory of most of us, that all steels were tool steels, and that the soft, structural varieties were introduced—varieties which harden but little, which bend cold, and which, in many physical properties, are akin rather to wrought-iron than to tool-steel. But, since both the hard and the soft steels are made by the same processes, and have their great, distinguishing structural feature in common, viz., homogeneity resulting from fluidity, it has come to pass, despite every other proposed nomenclature, that all the compounds of iron which have been cast in malleable masses, are called steel, the term wrought-iron being still confined to malleable iron made from pasty masses, and hence laminated in structure. No inconvenience has been found, so far, in distinguishing between the more or less carburized products, in general, by the terms " highsteel," "low-steel," "tool-steel," etc., and, in particular, by prefixing the percentage of carbon and other ingredients, to the terra steel. Steels which contain distinguishing ingredients other than carbon, are called "chrome-steel," "titanium-steel," and the like, just as variously compounded bronzes are called " phosphor bronze," " aluminium bronze," etc. Thus the combination of several words or symbols, and figures, may completely disclose the characters of the metal, in terms that are subject to no misunderstanding. But inasmuch as several high metallurgical authorities and clever writers have of late proposed to disturb this natural and somewhat settled nomenclature, it seems important to consider the claims of the various classifications. I shall attempt, in this paper, to show

By William H. Emmons

Discussion of the paper of William H. Emmons, presented at the Canal Zone meeting, November, 1910, and printed in Bulletin No. 46, October, 1910, pp. 767 to S37. CHARLES R,. KEYES, Des Moines, Ia. (communication to the Secretary*) :-It is not in a spirit of criticism that I offer a supplemental suggestion or two on the subjects covered by this valuable and highly instructive memoir. There are two points which, in my opinion, should have received greater emphasis in Mr. Emmons's excellent paper. One is the fundamental role played by the chlorides under certain conditions in ore-formation. The other is the possible establishment of geographic relationships among the four phenomena of (1) excessive chloridic content of mine-waters; (2) the abundance of chloridic compounds of the precious metals ; (3) the presence of. manganese oxides; and (4) the diminishing importance, in ore-genesis, of the metallic sulphates. Although Mr. Emmons's notes refer to gold alone, it may be pertinently asked whether the same principles do not hold good for silver and copper also, since these metals form, together with gold, a distinct and well-known chemical group. That the reactions involved apply equally well to the other two metals mentioned, is shown by a number of recent observations and discussions. Chloridic ores of silver are, as I have lately endeavored to show, mainly worked in. arid or desert regions only ; and the great deposits of disseminated copper-ores are similarly characteristic of such regions, in which both classes doubtless owe their formation to the abundance of saline materials derived from desert dusts, and to the .plentiful and almost universal presence of manganese oxide. Under these climatic conditions, silver is somewhat more abundantly deposited than copper and gold, because its chloride is so much * Received Nov. 11, 1910.

Jun 1, 1911

By V. A. Zanadvoroff

THE mine and concentrator of the Howe Sound Co., Chelan Division, are at Holden, in a remote section of the Cascade Mountains of northwestern Washington. Holden is at an elevation of 3200 ft., in the narrow valley of Railroad Creek. This creek drains into Lake Chelan, at a point some 40 miles up the lake from the town of Chelan. The concentrator treats 2000 to 2500 tons of low-grade copper-gold-zinc ore per day. Concentration is achieved by the differential flotation process, with recovery of 94 per cent copper and 82 per cent gold in the copper concentrate, followed by the recovery of 65 to 70 per cent zinc in the zinc flotation circuit. The final flotation tailing is deslimed, and coarse sands, representing 60 to 70 per cent of the total, are cyanided. The tonnage of tailing material amounts to 1900 to 2370 tons per day. GENERAL CONSIDERATIONS The property is within the Chelan National Forest. Railroad Creek is a fishing stream, being stocked regularly with trout from State hatcheries. Consequently, in planning a milling operation, the Howe Sound Co. was obliged to avoid any pollution of the stream by tailing material, and also destruction of valuable stands of timber. Moreover, the selected tailing disposal sites should not mar the natural beauty of the valley. In addition to these requirements, the problem of tailing disposal at Holden was complicated by topography and climatic conditions. The valley is long and narrow, averaging 1200 to 1500 ft. in width. Its walls are flaring at a steep angle. There are no extensive flat areas suitable for deposition of tailing. All valleys tributary to Railroad Creek, also the well-marked paths of snowslides, must be avoided. Finally, the direction of prevailing winds and possible dust hazard arising therefrom dictated the necessity of selecting the tailing-disposal sites downstream from the mill building and two campsites. Heavy snowfall during the winter months of November to March, inclusive, impedes building of the retaining dike, making it necessary to prepare the needed storage space during the summer months. It is inadvisable, also, to do any dike building during the freezing weather, because the dike becomes unstable with the spring thaws, producing inevitable "sloughing" of the built-up borders. TAILING-DISPOSAL SITES The existing tailing-disposal areas are near the south wall of the valley. They were developed, and put to use in the following sequence: No. I. Area.-Covers approximately 10 acres. Built up to the height of 60 ft.

Jan 1, 1946

By Frank A. Linforth

The object of this paper is to present a brief outline of the methods of geologic mapping employed in the Geological Department of the Anaconda Copper Mining Co., at Butte, and to show by means of a few typical examples the practical nature of the results obtained. The extremely complicated geological conditions early encountered in Butte mining led mine operators to realize the necessity of accurate detailed geologic mapping m an aid to successful development of the ore bodies. The organization of the Anaconda Geological Department was undertaken in 1900 by H. V. Winchell, who, in conjunction with D. W. Brunton, worked out the essential methods of procedure which are, in the main, followed at the present time. Since the year 1906 the geologic work has been under the direction of Reno H. Sales, and in some respects the scope of the work has been slightly enlarged. An excellent article describing the general equipment of the geological department was presented by D. W. Brunton at the British Columbia meeting of the Institute in 1905.' His idea, that data collected underground and recorded should be put to practical use and not remain a mere " inventory of the company's underground possessions," is the keynote to the success of applied geology in Butte. The geologic notes are taken as soon as possible after the ground is broken so that any mistake in the mining may be corrected at once, or any particularly advantageous procedure may be suggested before any useless work is done. Taking the notes underground is a comparatively simple matter, but a few necessary precautions may be pointed out. The essential to success is that the notes shall show exactly what geological facts are disclosed. The observer must discriminate carefully between important and unimportant exposures in making the record, especially as regards the relation between veins and stringers, between faults and minor slips, or between the characteristics of veins of different ages. A simple color scheme has been adopted for making this record. Red pencils are used to indicate

Jan 1, 1914

By Karl W. Mote

CALIFORNIA'S iron and steel industry had its beginning in San Francisco in 1849 when the first iron casting was poured at the old Union Iron Works. Soon after, in 1856 at Grass Valley, enough iron ore was smelted to supply pig iron for the castings of a quartz mill there. From 1880 to 1886, iron ore was produced from the Hotaling mine in Placer County and converted to pig iron in a local blast furnace using charcoal. From 1907 to 1914, the Noble Electric Steel Co. produced pig iron from iron ore mined at the Shasta Iron Co. mine, and followed this for three years in the production of ferro-alloys. Between 1917 and 1941, the State's industry in- creased its capacity for open hearth and electric furnace scrap treatment, but the real impetus was supplied by the need for more steel at the beginning of World War II. The result was the State's first integrated steel plant-the Kaiser Steel Corp. facilities at Fontana.

Jan 7, 1958

By J. Chipman, N. J. Grant, R. Rocca

D. E. Babcock (Republic Steel Corp., Youngstown, Ohio)—With reference to eqs 7 and 8, at what temperature do they apply John Chipman (authors' reply)—That was 1600°C. Dr. Babcock—You have l x 10-4 as the component for the lime and 1 or 4x10-. Now, is it by dividing one into the other you get the 400? That is assuming equivalent activity on the part of oxygen, sulphur, and magnesia. Dr. Chipman—Yes, they are calculated for 1600. Now, the first one for CaO was calculated before we had a glimpse of Dr. Rosenqvist's paper." If you take his calculation you get 14,000 cal which is very good agreement, but our calculation would be superseded by Dr. Rosenqvist's new data. Dr. Babcock—The state you assume those to be in is the liquid state, as near as you can measure? Dr. Chipman—Naturally it is based on the solid CaS, but if you add the effect of fusion on both sides it just about balances out, so the ratio would be about the same. B. M. Larsen (U. S. Steel Co., Kearny, N. J.)—If we knew the activity of sulphur in the slag instead of merely the percentage, we might be able to find some conflicting factors that balance one another out, and find that the FeO or oxygen pressure effect is really present over the whole range. Dr. Chipman—I am fairly sure we would. The activity of sulphur in the slag and the activity of CaO in the slag, if we just knew those quantities, would enable us to save a lot of this computation and assumption and all the approximations we are doing now. Mr. Larsen—Two other points perhaps should be included: 1—an independent effect of manganese in helping the desulphurization; and 2—the number of mols of constituents or number of mols of ions or whatever there is in the slag could vary with these compositions in such a way that you get dilution effects. Dr. Chipman—You can figure all that in if you want to and it might improve the degree of approximation a little bit. Maybe enough to justify the labor of calculation, inaybe not, but we did not do it. L. S. Darken (U. S. Steel Co., Kearny, N. J.)—The authors have tackled a very complicated problem in trying to tie together in one picture the desulphurizing problem over the wide range of basicity and oxidation level from that of the open hearth to that of the blast furnace. At the present state of our knowledge of slags such an ambitious undertaking necessarily involves the adoption of numerous hypotheses. Their formulation (eq 11) for the higher FeO range

Jan 1, 1952

By Thomas M. Drown

Remarkable as have been the direct results of Danks's puddler, there are some indirect and incidental results, which are well worthy of study for their intrinsic value and suggestiveness. The success of Danks's machine is due mainly to the nature of the lining and the manner in which it is attached to the walls of the revolving chamber. Herein lies Danks's merit and good fortune. Given such a lining, and the success of the machine, as far as puddling iron is concerned, could easily be predicted. Other important results have, however, been obtained with this machine, which, though clearly explicable, were, nevertheless, unanticipated. These are the increased yield of bar-iron over the pig-iron charged, and the elimination of phosphorus, which, though not absolutely complete, is yet more decided than in the case of hand-puddling. As regards the increased yield, this is merely what we have a right to expect if we consider the puddling process to consist in the oxida tion of the carbon and silicon of the pig by the oxygen of the oxide of iron. That this result is attained, nearly to the extent that the theory requires, in Danks's puddler, and has never been more than partially attained by the most careful experiments in band-puddling, points clearly to the fact that the contact of the molten pig-iron with the oxide of iron is much more intimate and complete in the one instance than in the other. The action of puddling in Danks's machine may be considered to be twofold: first, the removal of the carbon, silicon, and phospho rus of the pig, which is the primary object, and, second, the produc tion of wrought iron direct from the ore, which is entirely an inci dental result. Intelligent metallurgists were not long in recognizing in this latter result a fact of deeper import and greater value than the attainment of a perfect puddling process. A new method

By Thomas M. Dr. Drown

REMARKABLE as have been the direct results of Danks's puddler, there are some indirect and incidental results, which are well worthy of study for their intrinsic value and suggestiveness. The success of Danks's machine is due mainly to the nature of the lining and the manner in which it is attached to the walls of the revolving chamber. Herein lies Danks's merit and good fortune. Given such a lining, and the success of the machine, as far as puddling iron is concerned, could easily be predicted. Other important results have, however, been obtained with this machine, which, though clearly explicable, were, nevertheless, unanticipated. These are the increased yield of bar-iron over the pig-iron charged, and the elimination of phosphorus, which, though not absolutely complete, is yet more decided than in the case of hand-puddling. As regards the increased yield, this is merely what we have a right to expect if we consider the puddling process to consist in the oxidation of the carbon and silicon of the pig by the oxygen of the oxide of iron. That this result is attained, nearly to the extent that the theory requires, in Danks's puddler, and has never been more than partially attained by the most careful experiments in hand-puddling, points clearly to the fact that the contact of the molten pig-iron with the oxide of iron is much more intimate and complete in the one instance than in the other. The action of puddling in Danks's machine may be considered to be twofold first, the removal of the carbon, silicon, and phosphorus of the pig, which is the primary object, and, second, the production of wrought iron direct from the ore, which is entirely an incidental result. Intelligent metallurgists were not long in recognizing in this latter result a fact of deeper import and greater value than the attainment of a perfect puddling process. A new method

Jan 1, 1874

Jan 1, 1934

By C. D. Stahl, S. M. Farouq Ali, W. E. Culham

One- and two-dimensional mathematical models have been developed that simulate transient, two-phase flow of hydrocarbon mixtures in porous media in a manner that accounts for interphase mass transfer. Numerical simulations of one-dimensional depletion-drive experiments using a two-component hydrucarbon fluid were used to establish the validity of the mathematical models. In addition, the experimental and numerical data were used to demonstrate that production rate had a relatively insignificant effect on the recovery of individual hydrocarbon components from the experimental system, and that attainment of equilibrium between phases is possible for a wide range of liquid and vapor velocities in reservoirs containing light hydrocarbon fluids. Results of some two-dimensional numerical simulations are also presented. INTRODUCTION This study was undertaken to develop a mathematical model that would simulate transient, two-phase flow of hydrocarbon mixtures in porous media under conditions that result in interphase mass transfer and to test the validity of the assumptions used to set up the model. In addition, the study was designed to determine if production rate influences the recovery of individual hydrocarbon components from reservoirs producing by depletion drive. Two-phase flow in porous media, with interchange of components between the two phases, is important in many petroleum recovery processes. Studiesl-5 conducted within the last 3 years have outlined methods of solving multiphase flow problems incorporating mass transfer. Some of these studies have also indicated the importance of accounting for mass transfer under various producing conditions. An earlier work6 first demonstrated the importance of combining relative permeability data with equilibrium ratios in compositional balance methods. The mathematical model presented in this paper is formulated so that a phase behavior package, as described in previous papers,5,17 is not required as an integral part of the routine employed to solve for the primary dependent variables. The finite difference formulation is designed so that all the primary variables can be solved for simultaneously. This is accomplished by utilizing one basic set of equations. These innovations, which are in contrast to other models2,3,5 but are similar in some respects to the approach used by Taylor,l render the total problem computationally simpler than any of the previously referenced formulations. The mathematical model was developed by combining Darcy's law with a continuity equation for each hydrocarbon component. The principal assumptions invoked in the formulation were (1) that capillary forces and diffusional effects are negligible, and (2) that thermodynamic equilibrium exists in the reservoir at all times. No assumption as to the type of vaporization process was made in formulating this model. Experimental data were required to complete this study. These were generated by conducting several depletion drive experiments. The experimental apparatus consisted of a sandstone core enclosed in a pressurized casing. The apparatus was designed in such a manner that the core could be charged with a liquid hydrocarbon mixture and depleted at different production rates. The experimental tests were designed to determine the effect of production rate on component recovery. In addition, direct comparison of experimental and mathematically predicted

Jan 1, 1970

By T. S. Lundy, R. E. Pawel, F. R. Winslow, C. J. McHargue

The volume-diffusion coefficients of Nb-95 and Ta-182 in niobium have been measured over the temperature range 878° to 2400°C. High-temperature specimens (T 21500°C) were sectioned by conventional lathe and grinding techniques while low-temperature specimens were sectioned by an anodizing and stripping technique previously described. Over a range of more than ten orders of magnitude in diffusivity, the self-diffusion data is well-represented by the equation: D = (1.1+ 0.2) exp [- (96,000 * 900)/RT ] cm2/sec Upward deviations from this line are explained by short-circuit diffusion in combination with the loss of resolution of the sectioning techniques. Oxygen contamination within the range 100 to 450 ppm was found to have little or no effect on the self-diffusivitj 01 niobium. In a limited number of measurements, the diffusivity of Ta-182 in niobium was found to be about half that of Nb-95 in niobium. These data may be described by D = (I.0+0.90.5)exp [- (99,300 * 2400) /RT ] PREVIOUSLY reported studies of self-diffusion in niobium were by Resnick and Castleman1 and Peart, Graham, and Tomlin.2 The data of Resnick and Castleman over a temperature range 1585" to 2120°C show considerable scatter but. can be represented by D = (12.4 *0.8) exp [-(105,000+3OOO)/RT] cm2/sec The limited data of Peart, Graham, and Tomlin follow the equation D = 1.3 exp (-95,00O/RT) cm2/sec In view of recent diffusion data for ß zirconium3 and 0 titanium4 in which Arrhenius-type plots do not yield straight lines and of the potential high- temperature uses of niobium and its alloys, we thought it important to investigate the diffusion behavior of this bcc refractory metal over a large temperature range. This has recently been done for molybdenum,5 chromium,6 vanadium,"" and tantalum.9 Niobium was a particularly suitable material for this study largely because of the development of an anodizing and stripping sectioning technique which enables diffusivities as small as l0-19' sq cm per sec to be determined accurately.10 In addition to self-diffusion data, data were obtained for the diffusion of Ta-182 in niobium and for the effect of varying oxygen content on self-diffusion. I) EXPERIMENTAL PROCEDURE Materials. The niobium was obtained from three sources: 1) melting stock from Shieldalloy Corp., 2) electron-beam melted single crystals, 1/2 in. diameter, from Semi-Elements, Inc., and 3) oxygen-doped, electron-beam melted single crystals from Materials Research Corp. The melting stock was electron-beam melted and specimens 5/8 in. diameter by 1/2 in. long were machined from the center of the bar. The analysis supplied by the vendor and an interstitial analysis of one of the specimens are given in Table I. The single crystals (type 2 above) were cut with a jeweler's saw to specimens about 3/8 in. long. The interstitial analysis of this material is given in Table 11. This material was used

Jan 1, 1965

By F. N. Ward, E. H. Bailey

Camp and sample-site methods useful for determining about 0.5 to 16 ppm of mercury in soils and rocks have been devised to complement the analytical methods already widely used in geochemical prospecting. In the camp-site procedure the sample solution is obtained by digesting the finely powdered sample with hot nine-molar sulfuric acid and bromine, the latter generated in place. The solution is buffered at a pH of 4 and the mercury is extracted into a relatively small volume of an organic solvent. Estimations are made by comparing the color of the mercuric dithizonate extracted from the sample with that extracted from a standard. In the sample-site method the mercury is volatilized as the iodide and the latter is dissolved in a buffer solution from which the mercury dithizonate is extracted as in the camp-site method. The estimation is made by a similar comparison with standards or by comparing the color of the mercuric dithizonate with artificial standards prepared from Orange II, an azo dye. Except for the establishment of standards, the time required by an experienced analyst seldom exceeds 10 min for a camp-site determination and 5 min for a sample-site determination. Camp-site determinations are useful for commodity studies and intensive exploration programs; sample-site determinations are applicable to extensive and reconnaissance-type geochemical prospecting programs. The results obtained on samples taken along traverses above known mercury ore deposits in the California Coast Range and western Nevada demonstrate the usefulness of both methods in geochemical prospecting. The increasing use of the mercury content of soils, rocks, plants, or water in geochemical prospecting emphasizes the need for analytical methods which are sensitive and at the same time require a minimum of readily available equipment. Sensitive methods based on the absorption of ultraviolet light by mercury vapor are common in the literature31 12. Although none of these methods have been used to analyze the large number of samples required in geochemical prospecting, they could be extremely useful except for the expensive instrumentation usually required to make the methods quantitative Also, such methods are perhaps too sensitive for field use, especially around areas of possible contamination. Other methods involve the distillation of mercury from a relatively large sample and subsequent collection of the vapors in nitric acid6. The mercury is then estimated by titration with a suitable reagent such as thiocyanate. These methods are not trace methods because the actual amount of mercury measured is often as great as 50 to 100 milligrams. Also, such methods are unsuitable for geochemical prospecting because of the amount of equipment necessary and the time required. Still other methods involve colorimetry, and the sensitive reaction between dithizone and mercury (11).. is the basis for a number of reports on the determination of mercury in biological materials 5,7. Moreover, by the judicious use of solvent extraction and suitable complexing agents, the dithiaone method can be made almost specific for mercury. However, none of the dithizone methods have yet been applied to the determination of mercury in soils and rocks. In most colorimetric methods he sample solution

Jan 1, 1961

By John F. Elliott, John R. Rawling

The rate of reduction of silica to silicon by carbon at 1550° to 1700°C in iron blast-furnace type slag-metal systems has been investigated. In the tower portion of the temperature range oxygen transport in the metal boundary layer at the slag-tal interface is probably rate limiting. A second step, which apparently involves a chemical process in the slag at the slag-metal interface, appears to be rate limiting when the oxygen-transport limitation is avoided. Above 1650°C rate control of the reduction by carbon probably is mixed between the two steps. INVESTIGATIONS1.2 into the equilibrium distribution of silicon between graphite-saturated slags and metals typical of iron blast-furnace practice show that, under the experimental conditions specified, the reduction of silica to silicon is relatively slow compared with the rates of other slag-metal reactions under similar conditions. For this reason, the reduction of silica in blast-furnace slag-metal systems was considered to be an interesting subject for further study. Investigations of the kinetics of the reaction3-5 suggest that several possible steps may be rate controlling, and that the rate-controlling step depends not only on the physical state of the systems but also on the configuration of the apparatus. The main objects of the investigation reported here were to sug- gest plausible reaction paths for the reduction of silica under the experimental conditions chosen and to determine the step or steps which control the rate of reduction of silica. EXPERIMENTAL Two types of experiments involving the reduction of silica from the slag were carried out. In the first, the only reducing agent present was carbon (graphite), for which the over-all reaction is (SiO2) +2C(gr) —Si + 2Co(g) [l] The second type was a graphite-saturated ferro-silicon-iron concentration cell. In it silica in the slag could be reduced either by carbon according to Eq. [I], or by a reaction of electrochemical nature in which silicon was oxidized at the ferrosilicon-slag interface and silica was reduced at the slag-iron interface without the formation of CO. The two types of experiment are described below. Reduction of Silica with Carbon as the Only Available Reducing Agent. The reduction of silica was accomplished by allowing a liquid lime-alumina-silica slag and graphite-saturated iron to react in an induction-heated graphite crucible. The crucible was 2.25 in. diameter and 5 in. deep; it was fitted with a graphite stirrer which penetrated through the slag and into the metal, Fig. 1. The slag and metal charges weighed 350 g each. Pure carbon monoxide at a pressure of 1 atm was maintained above the melt by passing the purified gas through the crucible at a rate of 0.5 liter per min. The gas did not stir either the slag or metal. Temperature measurements were made by sighting an optical pyrometer down the hollow stirrer rod into a 1/4-in. hole drilled in the stirrer blade. The crucible temperature was maintained within *15"C of the required value by manual control of the power supply to the

Jan 1, 1965

By R. Maddin, A. Lawley

Single crystal Mo-Re alloys (99.99+ purity), grown by electron bombardment floating zone heating, were deformed in tension at temperatures from -196° to +200°C. At -196oC, Mo-6 pet Re and Mo-20 pct Re alloys deform by slip on systems of the type (101) [1ll]. Above-78oC, the operative slip system is of the type (112) [111], (101) [1ll], or (211) [1ll], depending upon orientation. Mo-39 pct Re alloys deform by twinning and slip at all test temperatures with a (112) [111] type twinning system. Critical resolved shear stress for slip and twinning is calculated as a function of composition and temperature, and the mechanical properties compared with those of less Pure polycrystalline alloys. HEXAGONAL close-packed rhenium, c/a = 1.615, is highly soluble in molybdenum. The bee molybdenum-rich solid solution extends to approximately 42 at. pet Re* at 2500°C,' Fig. 1. Recent work on polycrystalline alloys has shown conclusively that the addition of rhenium to molybdenum improves both the fabricability and the low-temperature ductility.2"5 Similar behavior is observed for W-Re and Cr-Re alloys.5 Initially, Geach and Hughes2 found that the Mo-30 pct Re alloy could be cold rolled to approximately 90 pct reduction before the onset of cracking. The remarkable effect of the rhenium was later confirmed by Jaffee et al. 3-5 with an optimum condition of maximum strength combined with maximum ductility at the Mo-35 pet composition. At higher rhenium contents, the ductility was severely impaired due apparently to the presence of brittle tetragonal s phase, Fig. 1. In the Mo-35 pet Re alloy, at least 110 ppm (parts per million) oxygen could be tolerated before cold workability was reduced. By comparison, the corresponding tolerance figure in unalloyed molybdenum is ~ 10 ppm. The effect of rhenium was considered in terms of: 1) a reduction in oxygen solubility in the lattice; 2) a redistribution of intergranular oxide from grain boundary films to isolated spheres; and 3) the promotion of twinning as a further mode of plastic deformation. Paradoxically, twinning is often associated with brittle fracture in iron and the silicon irons.6'7 Work to date has been restricted to are-melted and powder metallurgy polycrystalline material of ~ 99.9 pet purity. The present investigation was initiated for the purpose of determining the mode and crystallography of plastic deformation of a series of bee Mo-Re alloy single crystals over a wide temperature range from -196o to +200°C. Using high-purity zone-melted material (~ 99.99 + pet purity), the specific role of rhenium in the molybdenum lattice may be understood more fully since effects due to grain boundaries and oxide redistribution will be absent. At the same time, the study provides a comparison of single and polycrystalline deformation behavior. EXPERIMENTAL TECHNIQUES A) Preparation and Purity of Single Crystals. Alloys in the form of either are-cast and swaged or sintered and ground bar, 0.120 in. diam, were obtained from the Chase Brass and Copper Co. Alloy single crystals ~ 8-in. long were grown from the

Jan 1, 1962

By Cyril Smith

THE method of thermal analysis, so important in the development of metallographic science, has of recent years been falling into disuse owing to the development of other physical methods which give results easier of interpretation and which can be used for the study of either equilibrium or transitional conditions because they do not require a continuously changing temperature. Nevertheless thermal analysis remains useful in the study of reactions that take place rapidly, and the simplicity of the experimental technique and the general availability of the apparatus involved are points in its favor. Theoretically, thermal analysis is capable of giving specific and latent heat measurements and therefore should permit the study of reactions on a more fundamental basis than any other method. It is, however, difficult or impossible to obtain quantitative heat measurements from cooling curves obtained in the usual way. Even if the furnace containing the sample is cooled or heated at a linear rate, or if a gradient furnace is employed to maintain a constant rate over a large range of tempera-ture, the heat flow from or to the specimen depends on its previous his-tory, for the difference of temperature between the specimen and its surroundings varies. The emissivity of the specimen surface, moreover, is unlikely to be constant. The able mathematical analysis by Russell,1 although it prevents misinterpretation of data, has an effect rather the reverse of that intended, and leaves the reader doubtful of the possibility of ever obtaining quantitative results from thermal curves. Nothing can be done to apply thermal analysis to the study of equilib-rium conditions of reactions that are not completed at rates of tempera-ture change below about 1° C. per minute, and this unfortunately excludes most solid transformations in alloys. ? For the determination of liquidus

Jan 1, 1939