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By A. U. Seybolt

DURING the course of experiments involving oxygen equilibrations with a high-purity Pd-5 at. pct Rh alloy, the appearance of a subscale was noted. Most of the heat treatments in a pure oxygen atmosphere were performed at 900°C. The presence of the subscale was noted when the oxygen partial pressure was in excess of approximately 95 mm, up to 1 atm, the highest pressure used. According to available thermodynamic information' on the free energy of formation of Rh2O3 (the only reliably reported solid oxide of rhodium), this oxide should not be stable under these conditions, nor, of course, any oxide of palladium. Extraction of the subscale from the matrix was affected by treatment with aqua regia, and the resulting X-ray diffraction powder pattern is shown in Table I. This pattern is not that of Rh2O3, nor that of any known rhodium or palladium oxide. It can be indexed on a hexagonal lattice with a. = 5.22Å and co = 6.0Å. In addition to this unknown material, there was a weak Rh2O3 pattern. An X-ray fluorescence analysis of the powder gave 3214 palladium counts per sec and 5381 rhodium counts per sec, thus indicating the likelihood of a double oxide of palladium and rhodium. In view of the fact that the above result was obtained on a single sample, it is perhaps best not to insist upon the above ratio of about 0.6, but possibly to tentatively assume 0.5 or 1/1. The small amount of Rh2O3 in the X-ray pattern might have occurred on cooling, and it seems possible that the double oxide, below some temperature level, is not as stable as Rh2O3. To examine this point, some of the extracted double oxide was heated on a sheet of pure palladium in air at 900°C, and allowed to furnace-cool over a period of several hours. The X-ray diffraction pattern of the powder showed approximately the same intensity of Rh2O3 and the "hexagonal" oxide as before, but, in addition, a rather faint pattern of another crystalline species made its appearance. This finding again suggests partial transformation of the major (double) oxide to other oxides on cooling from 900°C. Application of the phase rule shows that only one equilibrium oxide (subscale) could have been present at temperature. Vacuum-fusion, oxygen analysis of the extracted subscale showed 7.7 ± 0.7 pct O. Combining this information with that of the X-ray fluorescence analysis suggests the formula PdRhO. This compound should have an oxygen content of 7.07 pct, which is within the range of error of the oxygen analysis. However, until a more careful stoichiometric study is made, it is suggested that the formula be written

Jan 1, 1965

By J. F. Myers, F. M. Lewis

C. G. McLACHLAN*-I have read this paper with considerable interest and wish to congratulate the authors on the care with which they carried out their experiments and for the detailed sizing data they have presented. 011 the other hand I do not feel that these data establish their contention that "with other factors the same, the work accomplished in a fine crushing rod mill is directly proportional to the rotating speed." My reason for making this statement is that their conclusion is based on the percentage of minus 65 mesh material produced at each of the speeds at which their tests were run. The rod mill is, however, not a fine grinding machine and therefore figures based on minus 65 mesh production are figures outside the range at which it operates to best advantage. Further, if rod mill performance is to be judged on the production of such material it should have been established that a rod mill will produce it as effectively as a ball mill. To check this last point I have gone over some of the rod and ball mill grind-ing figures for our Waite-Atnulet operation and find that the ball mill at that property produces more minus 65 mesh material per horsepower than the rod mill. Moreover, this comparison is even more favorable to the ball mill if it is limited to minus 100 mesh production. It therefore seems to me that the most satisfactory basis on which to try to com-pare the performance of the rod mill in the present case is by taking a weighted average of all the new surface produced per horsepower. W. H. Coghill3 has published data which can be applied to the sizing figures presented by the authors, and if this is done the units of new surface per horsepower produced in the Tennessee tests are as follows: Admittedly the increment of increase in new surface per horsepower shown in the foregoing figures is not great, but its trend is nevertheless definitely in favor of slower speed operation, for the conditions under which these particular tests were run. I also feel that some information regarding liner contour should have been given as I think it will be found that a mill which is equipped with liners which lift the rod load can be run at a slower speed than a mill in which the liners are comparatively smooth. J. F. MYERS and F. M. LEWIS (authors' reply)—The position taken by Mr. McLachlan is to be respected even though we are all aware of the faults of surface considerations. As he points out. the increment of increase is very small. It is so small in fact that for all practical purposes it does not conflict with the conclusions of the paper. The authors appreciate Mr. McLachlan's comprehensive study of the data.

Jan 1, 1950

By S. C. Sircar, B. K. Dhindaw

KINETICS and mechanism of sulfation reactions have been studied extensively. Qualitative and quantitative data are reported for the kinetics and mechanism of sulfation reaction of copper oxide pellets;''2 yet it remains a controversial Subject. The mechanism and kinetics of the sulfation of zinc oxide powder (B.D.H. analar quality) were studied by gravimetric technique. A spring of high-carbon steel wire with accuracy well within 0.2 mg was used for measuring weight change. The sample was taken in a Pyrex glass bucket, hanging freely inside a Pyrex glass tube reactor, with a gold wire attached to the spring, the reactor being surrounded by a movable furnace (double wound type) with a temperature control within *5"C. Flow of oxygen, 60 cu cm per min, and sulfur dioxide, 45 cu cm per min, were measured through calibrated flowmeters and the mixture dried over PZ05 before entering the reactor. The experimental results are presented in Figs. 1 and 2. The plot of weight change of zinc oxide, giving the amount of zinc sulfate formed, was found to be linear over the temperature range of 500" to 700° C and up to a conversion of approximately 60 pct, as beyond it they divert from linearity.' The rate of sulfation was found to be affected by total flow rate of gases at a fixed ratio of SO2/O2, up to 60 cu cm per min, and was found to be linearly dependent on quantity of total powdered sample taken. The plot of rate of sulfation of zinc oxide, 70 mg, with varying amounts of vanadium pentoxide, at a constant ratio of gases as mentioned above, and at a constant temperature of 625"C, was also found to be linear as seen in Fig. 2. Extrapolation to zero V2O5 addition gives the same rate of sulfation, as in case of pure zinc oxide, 70 mg. Vz05 was prepared by heating ammonium vanadate at 600°C for 15 min in a muffle furnace. The available literature points out that the theory of sulfation that has received the maximum support postulates the following mechanism for sulfation of ZnS: 2ZnS + 30, = 2Zn0 + 2SOZ; the ZnO formed acts as a catalyst for the reaction, 2 S02 + O2 = 2S03. This SO3 reacts with ZnO to give zinc sulfate. It is suggested here that the above widely supported mechanism is operative in the sulfation reaction and that the rate-controlling step in the sulfation reaction of ZnO is the formation of SO3 from SO, and 0,. The authors are carrying on further work in this line, and the details will be published later. The authors wish to acknowledge the facilities provided and the help extended by Prof. P. R. Dhar, Head, Department of Metallurgical Engineering, and the permission granted to publish this note by the Director, I. I. T., Kharagpur.

Jan 1, 1969

By Maurice Rey, H. Brevers

THROUGH circumstances connected with the war, the senior author lost his records therefore it has been impossible to include numerical data in this paper. The arsenical quicksilver ore investigated had been roasted, with poor metallurgical results. The vapor-tension temperature curves of mercury and arsenious trioxide are similar, and the arsenical compound hampers the coalescence of mercury drops in the condenser and is the cause of large stack losses. The ore was a gray limestone carrying small amounts of carbon and mineralized with cinnabar and two arsenic minerals, realgar (As2S2) and arsenopyrite (FeAsS). The proportion of realgar often exceeded that of cinnabar; the proportion of arsenopyrite was smaller. The grade of the ore varied between 0.8 and 4 per cent Hg. The problem was to make a high-grade mercury concentrate, as free from arsenic as possible. The water used throughout the testing was hard, having a pH- of about 8. FLOTATION OF REALGAR Realgar showed a very strong tendency to float. It formed a film at the surface of the pulp and floated in abundance with only pine oil. Therefore an attempt was made to float the realgar before the cinnabar, but this was not very successful; the percentage of mercury in the realgar concentrate could never be brought below 2 or 3 per cent. Cinnabar slimed easily and floated with pine oil, so that some of it always accompanied the realgar. There was also the question of the cinnabar-arsenopyrite separation. On further investigation it was found that realgar can be floated not only with pine oil but even better with a combination of hydrocarbons and pine oil. Washing the ore with ether revealed that it contained hydrocarbons, which helped to float the realgar. In this connection it belongs to the same class as carbon, sulphur and talc. It can be floated also with a xanthate, when activated by a heavy-metal salt. The conditions favoring the two types of flotation are opposed, as activation by a copper salt facilitates xanthate flotation (in fact, is even necessary to it), whereas it hinders pine oil and petroleum flotation. One type of flotation can be termed nonpolar and the other polar, a distinction that has been stressed in a previous paper. DEPRESSION OF REALGAR AND FLOTATION OF CINNABAR Many chemicals were tested in an attempt to float the cinnabar and depress the realgar. Finally starch rendered soluble with caustic soda was tried, also several grades of commercial soluble starch, and dextrin was found to be the best and the most convenient reagent. Several of these starch preparations have a strong flocculating effect on the pulp, which is a distinct disadvantage. Dextrin, with its low flocculating power, is excellent. It is noteworthy that starch preparations are also depressants for carbon and talc, so that the fact apparently has a general

Jan 1, 1941

By J. Gross

G. H. Clevenger, Chairman of the Milling Methods Committee of the Institute, made the following introductory remarks: "Several years ago, a number of us felt that the time was ripe for a fundamental investigation of crushing and grinding. At the outset, it appeared that the first thing we needed was a yardstick whereby grinding efficiency could be measured. "The U. S. Bureau of Mines has been most generous in cooperating with the Milling Methods Committee in getting this work well under way. John Gross, who served the committee for a year as secretary, was placed in charge of the investigation and has been ably assisted by S. R. Zimmerley. "Messrs. Gross and Zimmerley will now present the Progress Report covering their work to date." PROGRESS REPORT J. Gross, Salt Lake City, Utah. -This has not been a simple problem, and when I tell you that we can give you a verbal report of what we have done during three years in five or ten minutes you will realize that we have necessarily done a great deal of work that does not appear in the final results. We have been in a virtually new field. Therefore, we have had to feel our way at each step so as to be fairly sure we were correct. The first thing that was realized in this problem was that unless we had some method of measuring what happened when we crushed an ore, we might as well quit and not go further. We realized that if we tried to measure the results of crushing or grinding by the ordinary sizing test we would not get anywhere. We could sieve down to say 200 mesh fairly accurately; we could even go one sieve size further with a little less accuracy, and then we were absolutely lost, unless we went into microscopic measurement. Even this latter method would not have been satisfactory. The question was: what were we going to measure? If we were going to measure size, we might measure one particular dimension of a particle and be off 200 per cent. or more. If we tried to measure surface, we would have something tangible; the surface of a particle, no matter how irregular, is something definite, far more definite than any linear dimension would be. Moreover, if we could measure surface, we would immediately have a method of checking the Rittinger law as to whether it was or was not correct. So the first thing that we sought was a method whereby we could measure surface on crushed particles or, we will say, on particles; it would not make any difference whether crushed or not. It then became a question of what kind of particles we were going to use in obtaining a method for surface measurement. We realized that it would be rather a com-

Jan 1, 1928

By H. Brevers, Maurice Rey

Through circumstances connected with the war, the senior author lost his records, therefore it has been impossible to include numerical data in this paper. The arsenical quicksilver ore investigated had been roasted, with poor metallurgical results. The vapor-tension temperature curves of mercury and arsenious trioxide are similar, and the arsenical compound hampers the coalescence of mercury drops in the condenser and is the cause of large stack losses. The ore was a gray limestone carrying small amounts of carbon and mineralized with cinnabar and two arsenic minerals, realgar (As2S2) and arsenopyrite (FeAsS). The proportion of realgar often exceeded that of cinnabar; the proportion of arsenopyrite was smaller. The grade of the ore varied between 0.8 and 4 per cent Hg. The problem was to make a high-grade mercury concentrate, as free from arsenic as possible. The water used throughout the testing was hard, having a pH of about 8. Flotation of Realgar Realgar showed a very strong tendency to float. It formed a film at the surface of the pulp and floated in abundance with only pine oil. Therefore an attempt was made to float the realgar before the cinnabar, but this was not very successful; the percentage of mercury in the realgar concentrate could never be brought below 2 or 3 per cent. Cinnabar slimed easily and floated with pine oil, so that some of it always accompanied the realgar. There was also the question of the cinnabar-arseno-pyrite separation. On further investigation it was found that realgar can be floated not only with pine oil but even better with a combination of hydrocarbons and pine oil. Washing the ore with ether revealed that it contained hydrocarbons, which helped to float the realgar. In this connection it belongs to the same class as carbon, sulphur and talc. It can be floated also with a xanthate, when activated by a heavy-metal salt. The conditions favoring the two types of flotation are opposed, as activation by a copper salt facilitates xanthate flotation (in fact, is even necessary to it), whereas it hinders pine oil and petroleum flotation. One type of flotation can be termed non-polar and the other polar, a distinction that has been stressed in a previous paper.' Depression of Realgar and Flotation of Cinnabar Many chemicals were tested in an attempt to float the cinnabar and depress the realgar. Finally starch rendered soluble with caustic soda was tried, also several grades of commercial soluble starch, and dextrin was found to be the best and the most convenient reagent. Several of these starch preparations have a strong flocculating effect on the pulp, which is a distinct disadvantage. Dextrin, with its low flocculating power, is excellent. It is noteworthy that starch preparations are also depressants for carbon and talc, so that the fact apparently has a general

Jan 1, 1943

THE fall meeting of the Petroleum Division at Fort Worth, Texas, Oct. 19 and 20, attracted even a larger number of members and guests than had been expected. Over three hundred registered the first day though the attendance and interest in the program was so keen that it was necessary to begin technical sessions without. waiting for registration. Members were present from as far away as Venezuela and while the larger attendance was from the Mid-Continent and Texas fields, California and the eastern states were represented by influential delegations. One pleasing feature of the meeting was the presence of a number of the older executives of the oil industry who evi-dently have come to realize the importance of the work the Division is doing in advancing technology. The meeting was held under the auspices of the Production Engineering section of the Division. E. 0. Bennett, chief production engineer for the Marland Oil Co. of Texas, and chairman of the Fort Worth Sec-tion. of the A.I.M.E., served as general chairman. J. B. Umpleby, president of the Petroleum Reclamation Co. and vice-chairman of the. Division was in charge of. the program with a special committee in charge of the technical sessions, of which A. C. Rubel of the Union Oil Co. was chairman. The sessions were held in the ball room of the Texas Hotel, which also served as general headquarters. The Wednesday morning session was devoted to the air-gas lift, John M. Lovejoy, chairman of the Division, presiding. The first paper, on the "Principles Under-lying the Air-Gas Lift." by J. 0. Lewis, was presented by R. R. Brandenthaler and discussed by Messrs. Love-joy and Millikan. Mr. Brandenthaler's own paper on the "Effect of Gas Lift on Physical Properties of Oil" followed and was discussed by Messrs. Umpleby, Walker, Mills, Bennett, Williams and Van der Gracht, the dis-cussion turning mainly on what is known and what unknown regarding oxidation of oil under various con-ditions. The third paper of the morning, "Handling Recirculated Gas," by R. D. Gibbs, was presented by Mr. Taylor. The discussion that followed was general and brought out a large amount of data on the costs and results of compression versus, absorption in total gasoline recovery from gas. The next group of papers dealt with "Mechanical Installations of Air-Gas Lift," the first by E. V. Foran on the Texas district outside the Gulf Coast, the second by L. L. Brundred on the Gulf Coast, the third on Kansas and Oklahoma other than Seminole by R. W. Bond, the fourth on Seminole by C. R. Swartz, and the fifth relating to California by H. C. Miller. Some of these were read by title in order to give more time for discussion which was active and participated in by. Mills, Griswold and others.

Jan 11, 1927

By T. W. Smoot

Bentonites are composed chiefly of montmorillonites which are clay minerals generally distinguished from other clay minerals by their surface activity and extremely fine particle sizes. The uses of bentonite are many and varied, depending principally on one or more of the following characteristics: 1) Thixotropy, 2) Dispersion, 3) Plasticity, 4) Swelling, 5) Surface area, activity, ab- and adsorbtive properties. Some of the major uses of bentonite are briefly reviewed as are the mineralogical and physical properties. The uses of X-ray diffraction, differential thermal analysis and other tests for physical properties are reviewed as to their uses in evaluation. In the past 40 years, the industrial uses of bentonite have grown to include many applications. The physical and chemical properties of bentonites are such that they can be used as catalysts, adsorbants, plasticizers, binders, drilling muds, and pelletizers. Not all bentonites, however, can be used for all of these purposes and some are probably of little or no value for any use. The purpose of this paper is to briefly review the mineralogical, physical, and chemical characteristics and variations of bentonites. The determination of these characteristics and their uses in industry are also reviewed so that these determinations can be used as guides for evaluation. DEFINITION OF BENTONITE The word bentonite, as used in this paper, refers to a clay material, usually (but not necessarily) the result of the in-place-weathering of volcanic ash. Its mineralogical composition is dominated by the clay mineral montmorillonite and generally carries other clay minerals and silica minerals as the major 'impurities'. For this discussion, such a definition is justified since most of the economic uses of bentonite~ depend upon the physical and chemical characteristics of the montmorillonite minerals involved. The terms montmorillonite and bentonite have been used almost interchangeably in industry although the latter is much more commonly used. Therefore, where montmorillonite is discussed, it should be understood that the major feature of a bentonite is the subject. STRUCTIJRE OF MONTMORILLONlTE The economic importance of bentonites is generally based on one or more of the following characteristics of montmorillonite: 1) high-thixotropy and easy dispersion in water, 2) high-plasticity, 3) swelling properties, 4) large surface area/unit mass, 5) high surface activity, and 6) adsorptive properties. To understand these properties, an appreciation of the structural scheme of montmorillonite is helpful. Montmorillonite IS one of the three-layer clay minerals composed essentially of hydrous aluminum silicates. The essential building blocks of these layered silicate:; are: 1) silica tetrahedron composed of a silicon atom surrounded by four oxygen atoms, and 2) aluminun (iron, magnesium, etc.) octahedral unit that, ideally, has one of these atoms surrounded by six hydroxal units. Fig. 1 is a diagrammatic sketch of the montmorillonite structure. In the montmorillonite structure, the tetrahedron are pointed inward and attached to the octahedral units so that the O= atoms replace the hydroxal units where they are bonded; hence two-thirds of the hydroxal units

Jan 1, 1962

By E. A. Kilinski

THE mineral production of Dutch Guiana has been of little consequence. This is due to several rea-sons. Inaccessibility is probably the greatest factor, for the Guianas are off the main commercial route. More or less closely related causes are the tropi-cal climate and the temperament of the inhabitants. Small quantities of gold have come from Dutch Guiana for many years, and recently bauxite has entered the list of exports. It is likely that other minerals may be found in commercial quantities. The Colony is on the northeast coast of South Amer-ica. It is known by two names, that of Dutch Guiana, and that of Surinam. - British Guiana (Demerara) adjoins it on the west, French Guiana (Cayenne) on the east, and Brazil on the south. It covers an area of approximately 58,000 sq. miles. The population, in the. neighborhood of a hundred thousand,, is small, but the variety of races and the sub-sequent mixtures of these is almost incredible. This unusual and colorful population readily falls into three groups, (1) those of the bush, (2) those of the planta-tion, and (3) those of the towns. The bush people con-sist of two groups, the Indians and the bush-negro. The Indians, of whom there are but a little over two thousand, keep entirely to themselves, lead a. very primi-tive existence, and rarely come into the towns. The bush-negro gives the touch of human life to the thick jungles. A descendant of escaped slaves of by-gone days, he is at present a proud, stalwart, happy, clean, moral, carefree and ease-loving individual-a distinct personality. Work is not his pal, although he does cheerfully that which is necessary for his existence. He will transport passengers and goods in his dugout and guide the stranger through the jungles, but that is all. The plantations employ some negroes, but more Javanese, imported as contract labor from the East Indies. Paramaribo, the only large town in Dutch Guiana, is the center of all government, commercial, and social activities. It has a motley population of 40,000, in-cluding negroes native to Dutch Guiana and many from all parts of the West Indies. In addition, there are Javanese, Chinese, and some Hindus. The two latter groups control most of the retail trade. The Dutch and a few scattered Germans are the only Europeans. All of the higher government offices are held by the Dutch, the others are filled from the ranks of the natives. Marriages and intermarriages among these various groups have produced types that defy almost any effort to decipher an individual's forbears. Dutch is the official language, but among the people a jargon known as Tahki-Tahki holds sway. English is taught in the schools, consequently many speak it, and many more can make themselves understood in that language.

Jan 2, 1928

Secondary blast holes are now being pierced in quartzite and sandstone quarries, using multiple hand-operated Jet-Piercing units supplied with oxygen, fuel and water from a compact mobile carrier. A unit of this type, operating in a Canadian quarry, enabled four Jet-Piercing blowpipes to pierce blast holes for two hours without shutdown. The piercing blowpipes used were developed by Linde Air Products Co., a division of Union Carbide and Carbon Corp. The mobile supply carrier was constructed by the quarry from specifications supplied by Linde and modified by the quarry operators for their particular use. Employment of the new self-contained unit, which allows up to four operators to pierce approximately 450 ft of blast hole without shutdown, accelerates rock removal operations. Normally, only two blowpipes are in operation at one time. Large boulders or ledges, which sometimes remain after primary blasting to hamper loading operations, can, in the case of certain hard rock, be prepared for reduction more rapidly with these new units than by any other means. A special feature of the new manual Jet-Piercing unit is the mobile gas and fluid supply carrier. It consists of a standard truck chassis fitted out with four banks of large standard-capacity oxygen cylinders, a steel-holding tank for fuel oil, and a gasoline-driven air compressor and tank for pressurizing the fuel oil tank. Cooling water for the blowpipes is supplied to the unit from a hose extension to the quarry supply line. Feeder lines from the oxygen cylinder manifolds and the oil and water tanks terminate in four sets of take-off stations on the control panel at the rear of the truck. As many as four hand Jet-Piercing blowpipes can be connected to the take-off panel by high-pressure rubber hoses. The hand Jet-Piercing blowpipe used with the mobile supply carrier is a highly portable device which can be manipulated comfortably by one operator. The blowpipe can pierce blast holes at rates up to 60 ft per hour, depending on the properties of the rock. Blast holes can be pierced at any angle from the vertical to the horizontal, making it necessary for the operator to drill from the top of the boulder. Hole diameter is held to approximately that which allows the use of a standard 11/8-in. diameter dynamite. The manual Jet-Piercing blowpipe has these important design features: a burner from which the combustion gases emerge at supersonic speeds (in excess of 6000 ft per sec); a hole-sizing shell which controls the minimum size of the hole and protects the copper burner; and a sliding shield which protects the operator against the steam and spallings ejected from the hole during the piercing. The Jet piercing process has been applied successfully in United States and Canadian quarries within the last several years as an advanced method of "drilling" blast holes.

Jan 1, 1952

By L. D. Jaffe, D. C. Buffum, F. L. Carr, M. Goldman

IN an earlier investigation by Jaffe and Buffum,' a time-temperature transformation diagram for isothermal temper embrittlement of an SAE 3140 steel showed some suggestion of two overlapping "noses." These authors mentioned, as a possible explanation, that their specimens embrittled at 525°C were slightly softer than expected, perhaps because of some slight unknown variation in tempering treatment. Because a double nose would be of considerable importance in elucidating the mechanism of the temper brittleness reaction,' it appeared worthwhile to redetermine the portion of the diagram near 525°C. The same heat of SAE 3140 steel was used as in the previous work, and experimental procedures were the same.' Blanks were austenitized 1 hr at 900°C, water-quenched, tempered 1 hr at 675°C, and water-quenched. Groups were then embrittled isothermally at the temperatures and for the times shown in Table I, and water-quenched. For comparison, one series was tempered various times at 675°C, water-quenched, and given no further treatment. V-notched Charpy impact specimens machined from the blanks were tested over a range of temperatures. Energy absorption and percentage of fibrous fracture were plotted vs test temperature for each group, utilizing both the new data and those for the same treatment obtained in the earlier work,' except that the earlier data at 525°C were discarded.* are given in Table I. After a small correction (-0.28°C/BHN) for the variation of hardness" from Rockwell C24, the transition temperatures were plotted against embrittling time for each embrittling temperature, using the data of Table I for the range of treatments covered there, and using previous dataL for other treatments. By cross-plotting, Fig. 1 was finally obtained. It appears from this figure that if there are two noses to the time-temperature-transformation diagram for isothermal temper embrittlement of SAE 3140 steel, the upper nose must lie above 575°C. As interest had been primarily in the region near 525°C, a thorough study of embrittlement above 575°C was not made. Fig. 1 shows that such a study is needed, especially since preliminary measurements at the tempering temperature of 675°C reveal much more rapid embrittlement than would be expected from the data at lower temperatures. The transition temperature increased, approximately, as the logarithm of the tempering time (about 81/2°C, after correction for hardness, for each doubling of the time).& Since three tensile specimens tempered 240 hr at 675°C and water-quenched had an average yield-tensile ratio of 0.844, with 70.7 pct reduction of area, it is assumed1 that the tempering temperature is not above Ae1. The omission of a quench-and-reheat operation below Ae1, for the groups tempered at 675°C, as compared to groups embrittled at lower temperatures, should not affect results." More detailed investigation of embrittlement above 575°C is now under way.

Jan 1, 1954

By F. W. Bloecher

S. Mortsell and J. Svenssofi (Royal Institute of Technology, Stockholm, Sweden)—Bloecher states that the apparatus described by him should be a suitable instrument in the mineral dressing laboratories for determining the specific surface of such granular products that are generally investigated. We want to express a somewhat different opinion, as we doubt that the gas adsorption method of surface measurement really is the most suitable method in mineral dressing laboratories. It is well known that the surface area, as measured by this method, does not coincide with the surface area calculated from the size, shape, and number of particles, i.e. the superficial surface of the particles. It can be seen easily from Mr. Bloecher's own determination on ilmenite-leucoxene concentrate that the surface area measured according to this method may be several hundred times larger than the superficial surface. It is supposed that the surface of cracks, fissures, and pores within the particles also is included in the measured surface. However, this is an assumption which scarcely can be proved and certainly has not been proved. We believe that the mineral engineer could better use a method giving the superficial surface of the particles, as in most cases this surface only is of importance to him. Such is certainly the case when calculating the resistance of the fluid flow through granu- lar materials and the capillary forces of such materials, problems which are of great importance in connection with dewatering, filtration, and pelletizing'" etc. The same may also be the case when studying flotation problems, partly since the quantities of the introduced reagents usually are so small that they can only cover the most accessible surface of the particles, and partly since the molecules of at least the collecting reagents are so large that they cannot enter the smallest cracks and pores. As to the surface, which is of consequence in the application of Rittinger's law of crushing, one is inclined to believe, from theoretical reasons and from the work by Gross and Zimmerley, that the total surface here is the most important one. However, it seems as if in that case the superficial surface was as important as the total surface. Other reasons making the gas adsorption method less suitable for use in the mineral dressing laboratories are that the granular materials there very often are too coarse to be measured by this method, that the experimental technique is rather difficult, and that it takes a long time to measure the specific surface of a sample. Besides, the validity of the method must still be considered questionable. It is thus well known that with different gases one usually gets different values of the specific surface of the same sample, which values, even with such an ideal material as metal foils, can differ as much as about 50 pct.'" Still more serious

Jan 1, 1952

By D. H. Baldwin, R. E. Reed-Hill

DURING the course of experiments involving oxygen equilibrations with a high-purity Pd-5 at. pct Rh alloy, the appearance of a subscale was noted. Most of the heat treatments in a pure oxygen atmosphere were performed at 900°C. The presence of the subscale was noted when the oxygen partial pressure was in excess of approximately 95 mm, up to 1 atm, the highest pressure used. According to available thermodynamic information' on the free energy of formation of Rh2O3 (the only reliably reported solid oxide of rhodium), this oxide should not be stable under these conditions, nor, of course, any oxide of palladium. Extraction of the subscale from the matrix was affected by treatment with aqua regia, and the resulting X-ray diffraction powder pattern is shown in Table I. This pattern is not that of Rh2O3, nor that of any known rhodium or palladium oxide. It can be indexed on a hexagonal lattice with a. = 5.22Å and co = 6.0Å. In addition to this unknown material, there was a weak Rh2O3 pattern. An X-ray fluorescence analysis of the powder gave 3214 palladium counts per sec and 5381 rhodium counts per sec, thus indicating the likelihood of a double oxide of palladium and rhodium. In view of the fact that the above result was obtained on a single sample, it is perhaps best not to insist upon the above ratio of about 0.6, but possibly to tentatively assume 0.5 or 1/1. The small amount of Rh2O3 in the X-ray pattern might have occurred on cooling, and it seems possible that the double oxide, below some temperature level, is not as stable as Rh2O3. To examine this point, some of the extracted double oxide was heated on a sheet of pure palladium in air at 900°C, and allowed to furnace-cool over a period of several hours. The X-ray diffraction pattern of the powder showed approximately the same intensity of Rh2O3 and the "hexagonal" oxide as before, but, in addition, a rather faint pattern of another crystalline species made its appearance. This finding again suggests partial transformation of the major (double) oxide to other oxides on cooling from 900°C. Application of the phase rule shows that only one equilibrium oxide (subscale) could have been present at temperature. Vacuum-fusion, oxygen analysis of the extracted subscale showed 7.7 ± 0.7 pct O. Combining this information with that of the X-ray fluorescence analysis suggests the formula PdRhO. This compound should have an oxygen content of 7.07 pct, which is within the range of error of the oxygen analysis. However, until a more careful stoichiometric study is made, it is suggested that the formula be written

Jan 1, 1965

By W. Julian Patron

TREATMENT of the breaker wash-water discharges to remove the suspended particles of finely divided material is usually most efficiently and economically accomplished in settling or thickening tanks. The purpose of these tanks is to separate the excess water from the solids by sedimentation whereby the solid particles suspended in the water are thickened by the force of gravity. The water overflowing these tanks is either reused for coal cleaning or discharged directly to the streams. The settled solids, which are in a relatively concentrated condition, forming a sludge or thick pulp, can be disposed of by pumping to a storage dam, by slushing into mine workings, by processing for recovery of coal, or filtering by vacuum or centrifugal means and discharging with the breaker refuse. The scope of this paper will be limited to the discussion of settling and thickening equipment, the factors that influence the settlement of solids, and a brief description of tests that can be made to determine the size of settling facilities required for any particular condition. The practical application of sedimentation to the treatment of coal falls into two groups, one of classification or hydro- separation, and the other of clarification and thickening. Classification may be employed to prepare a relatively low- grade fuel, which can be used as is or can be further processed separately. Clarification and thickening is employed where the primary objective is to recover a relatively dewatered solid and return a satisfactorily clear water to breaker or streams. When a stream of water flows across a tank, the time required for a particle to travel from the feed inlet to the overflow must be a little greater than that required for the finest particles or flocs in the feed to settle out of the stream. OPERATION AND TYPES OF SETTLING EQUIPMENT Theoretically, the liquid in a settling tank should rise at a more or less constant rate throughout the area of the tank Under these conditions the rising velocity of the water must be less than the settling rate of the finest particles if clarification is to be obtained. When classification of particles is to be made in the tank, the overflow velocity must be greater than the settling velocity of the particles that are to be removed with the tank overflow. The performance of a settling tank, then, depends on the settling rate of the solids and the current velocities in the tank. The oldest types of sedimentation employ intermittent types of settling tanks of any convenient shape. Means are provided for filling the tank with pulp and allowing it to settle until quiet, for moving the clean liquor and for removing the thickened sludge. The operation is necessarily intermittent but a sufficient number of tanks is employed so that a continuous flow of clear water is maintained. Continuous methods for the sedimentation of slurries were developed in the metallurgical industry. Cones from which settled solids were discharged by gravity

Jan 1, 1946

By D. S. Sanders, E. W. Witcomb

FLOTATION tests, from which the flowsheet for the concentrator was determined, were made in a pilot mill at Chuquicamata and later comparative testing of full size flotation cells was done at the Andes Copper Mining Co. concentrator in Potrerillos. The principal sulphide copper mineral is chalcocite with varying amounts of covellite, enargite, and chalcopyrite. The oxidized portion is principally antlerite, a green basic copper sulphate. The gangue minerals include quartz, sericite, pyrite, feldspars and kaolin. Chuquicamata pit ores have proved to be hard grinding. The results of the flotation and metallurgical work prove that good extraction and concentrate grade can be obtained under a rather wide range of conditions. Metallurgy In general the metallurgy of the ore requires a fairly close control of the grind to the primary rougher flotation and of the regrind of the primary rougher concentrate before cleaning. Regrinding is necessary to reduce the insoluble content of the final concentrate since a large part of the middling combinations are between the copper and silica minerals. The alkalinity of the pulps can vary between wide limits and control of the percent solids gives the desired grind. Alkalinity Control Arroyo Salado water is supplied to the concentrator head tanks. It contains about 5000 ppm of salts but test work shows no deleterious effect. Actually this water permits a decrease of as much as 1 lb of lime per ton of ore as compared to San Pedro water, which is used for leaching oxide ore. About one quarter of the water flow through the concentrator will be new water from the reservoir. The remainder will be reclaimed from the thickeners. For primary grinding and rougher flotation, new and reclaimed water are combined in the head tanks. To avoid erratic results, only new water is used in the regrind system. Milk of lime is added to the rod mill feed chute to obtain the maximum benefit of mixing with the ore. This protects the equipment from corrosion due to entrained acids and soluble copper salts. Lime consumption is 3 to 5 lb per ton of ore. Grinding and Flotation The six bin gates over each belt feeder are opened in controlled combination and sequence to keep a live bed of ore in the bin to prevent arching and to obtain mixing. The milk of lime added ahead of the rod mill is regulated to suit rougher flotation requirements. The primary promoter reagent, Aerofloat 238, is added to the 10-mesh discharge of the rod mill as it is laundered to the ball mill scoop box. The classifier overflow is regulated to produce a grind of about 12 to 15 pct +65 mesh and 60 pct -200 mesh. A secondary promoter Z-4 (aml zanthate) and the pine oil frother are added in the overflow launder where a pH of 10 to 11 is maintained. Comparatively heavy beds of froth on the

Jan 1, 1952

A general discussion on the subject of Crushing and Grinding was held on August 24, 1927, during the meeting of the Institute at Salt, Lake City. G. H. Clevenger, Chairman of the Milling Methods Committee of the Institute, made the following introductory remarks "Several years ago, a number of us felt that the time was ripe for a fundamental investigation of crushing and grinding. At the outset, it appeared that the first thing we needed was a yardstick whereby grinding efficiency could be measured. "The U. S. Bureau of Mines has been most generous in cooperating with the Milling Methods Committee in getting this work well undrr way. John Gross, who served the committee for a year as secretary, was placed in charge of the investigation and has been ably assisted by S. R. Zimmerley. "Messrs. Gross and Zimmerley will now present the Progrcss Report covering their work to date." Progress Report J. Gross, Salt Lake City, Utah.—-This has not been a simple problem, and when I tell you that me can give you a verbal report of what we have done during three years in five or ten minutes you will realize that we have necessarily done a great deal of work that dors riot appear in the final results. We have been in a virtually new field. Therefore, we have had to feel our way at each step so as to be fairly sure we were correet. The first thing that was realized in this problem ass that unless we had some method of measuring what happened when we crushed an ore, we might as well quit and not go further. we realized that if we tried to measure the results of crushing or grinding by the ordiuary sizing test we would not get anywhere. We could sieve down to say 200 mesh fairly accurately; we could even go one sieve size further with a little less accuracy, and then we were absolutely lost, unless we went into microscopic measurement. Even this latter method would not have been satisfactory. The question was: what were we going to measure? If we were going to measure size, we might measure one particular dimension of a particle and be off 200 per cent. or more. If we tried to measure surfaee, we would have something tangible; the surface of a particle, no matter how irregular, is something definite, far more definite than any linear dimension would be. Moreover, if we could measure surface, we would immediately have a method of checking the Rittinger law as to whether it was or was not correct. So the first thing that we sought. was a method whereby we could measure surface on crushed particles or, we will sag., on particles; it would not make any difference whether crushed or not. It then became a question of what kind of particles we were going to use in obtaining a method for surface measurement. We realizcd that it would be rather a corn-

Jan 1, 1928

By Maurice Rey, H. Brevers

Through circumstances connected with the war, the senior author lost his records, therefore it has been impossible to include numerical data in this paper. The arsenical quicksilver ore investigated had been roasted, with poor metallurgical results. The vapor-tension temperature curves of mercury and arsenious trioxide are similar, and the arsenical compound hampers the coalescence of mercury drops in the condenser and is the cause of large stack losses. The ore was a gray limestone carrying small amounts of carbon and mineralized with cinnabar and two arsenic minerals, realgar (As2S2) and arsenopyrite (FeAsS). The proportion of realgar often exceeded that of cinnabar; the proportion of arsenopyrite was smaller. The grade of the ore varied between 0.8 and 4 per cent Hg. The problem was to make a high-grade mercury concentrate, as free from arsenic as possible. The water used throughout the testing was hard, having a pH of about 8. Flotation of Realgar Realgar showed a very strong tendency to float. It formed a film at the surface of the pulp and floated in abundance with only pine oil. Therefore an attempt was made to float the realgar before the cinnabar, but this was not very successful; the percentage of mercury in the realgar concentrate could never be brought below 2 or 3 per cent. Cinnabar slimed easily and floated with pine oil, so that some of it always accompanied the realgar. There was also the question of the cinnabar-arseno-pyrite separation. On further investigation it was found that realgar can be floated not only with pine oil but even better with a combination of hydrocarbons and pine oil. Washing the ore with ether revealed that it contained hydrocarbons, which helped to float the realgar. In this connection it belongs to the same class as carbon, sulphur and talc. It can be floated also with a xanthate, when activated by a heavy-metal salt. The conditions favoring the two types of flotation are opposed, as activation by a copper salt facilitates xanthate flotation (in fact, is even necessary to it), whereas it hinders pine oil and petroleum flotation. One type of flotation can be termed non-polar and the other polar, a distinction that has been stressed in a previous paper.' Depression of Realgar and Flotation of Cinnabar Many chemicals were tested in an attempt to float the cinnabar and depress the realgar. Finally starch rendered soluble with caustic soda was tried, also several grades of commercial soluble starch, and dextrin was found to be the best and the most convenient reagent. Several of these starch preparations have a strong flocculating effect on the pulp, which is a distinct disadvantage. Dextrin, with its low flocculating power, is excellent. It is noteworthy that starch preparations are also depressants for carbon and talc, so that the fact apparently has a general

Jan 1, 1943

By M. L. Lissberger

entirely suitable for certain uses and even possess advantages over present solders at high temperatures, but they are certainly not suitable for all uses. However, it is conceivable that their use in many places will effect a material conservation of tin. It will probably be wiser to use cadmium in solders where good results have been obtained than in brass where this element will be a source of possible trouble. F. F. Colcord,* New York, N. Y.-—The cadmium-lead solder has a higher conductivity than the lead-tin alloy, which ought to make it advantageous in the manufacture of electrical machinery. In the case of solder for tin-can work, one of the high officials of the American Can Co. said that he fully intended to .give it a good trial, and I do not believe they are going to reach hasty conclusions and run the risk of poisoning the public. Solder, Its Use and Abuse Milton L. LissbeRgeR,† New York, N. Y.—Solder is a mechanical mixture of tin and lead, a fact which is susceptible of very simple demonstration. A bar of solder of a grade even as low as 30 per cent. tin and 70 per cent. lead, passed through a buffing machine, will show a surface practically identical with that of a bar of second-quality or reclaimed tin. The buffings, on chemical analysis, will prove to be almost pure lead. According to the best practice, solder is made in the following manner. Virgin pig lead is first melted, and when it is thoroughly liquefied, virgin pig tin is added, together with a small amount of flux; the latter is for the purpose of bringing to the surface the so-called "liver," consisting of impurities that may have remained in either the lead or the tin as a result of incomplete refining. The combined material, when completely liquid, is thoroughly stirred for some hours, and is then cast into small pigs. Just before casting, and continuously during this operation, the molten metal yields dross, consisting largely of the oxides of lead and tin; this should be carefully skimmed off. After the pigs have cooled, they are taken to a smaller kettle, re-melted, and cast into the desired shape for use; or if wires, ribbons, etc., are to be made, the solder is cast into slugs suitable for extrusion and rolling. During this second operation, the skimming of dross should be even more carefully done than at first. Hand mixing has proved to be the only reliable method for the production of the best quality of solder, irrespective of its percentages of lead and tin. The best quality of solder is not necessarily that which contains the highest percentage of tin, but rather is that composition which performs best on the required piece of work. In order to produce

Jan 1, 1919

By Babbitts and Solder

G. w. Thompson,* Brooklyn, N. Y.—This subject has two aspects, neither of which can be ignored: these are the economic aspect and the technical aspect. Under ordinary conditions, economic law will take care of the conservation of tin. Under present conditions it seems desirable that economic law should still be permitted to operate as far as is practicable. It is true that this law operates rather slowly, and that under war conditions it cannot be depended upon to give our Government the supply it immediately needs. There should, therefore, be a designation of the essential industries by the Government, and tin should be supplied for those needs, letting the non-essential industries take what is left. At the same time, information ought to be forthcoming as to how tin can be conserved; with tin selling at 80 c. per pound, more or less, it is to the interest of every consumer to get the best information he can as to how he can save tin. Economic law would properly punish those who do not study their own interests in this way. I deprecate, therefore, any centralized socialistic effort toward avoiding penalties through failure to observe and obey economic law. In saying this, however, I am not unmindful that it is desirable for our Government to take such control of the tin situation as may be necessary to the prosecution of the war, practically regardless of the effect of such action upon individual industry, which should studiously seek to adjust itself to the new condition. The Government should promulgate such technical information as it can collect, showing how .tin can be conserved, and should urge upon every consumer the exercise of his common sense in self-protection. There is very little danger of any one attempting to hoard or corner tin, in the present state of the market. Most consumers will be glad to live from hand to mouth, covering their sales by purchases, or vice versa. As to the technical aspects: Tin and tin alloys are used to give certain practical and also certain artistic results. The practical factors are those involved in proper adhesion, continuity of surface, protection, the right degree of hardness, proper working qualities, etc. The artistic results are those that appeal purely to the eye or to our cultivated sense of what is desirable. There is no doubt that a great deal of tin could be saved if there were not a demand for certain pleasing effects. Row can this saving be brought about? The users of tin bearing alloys are not the only ones involved in this question. The manufacturers of solder and babbitt have for a long time sought to give certain appearances to their fabricated bars and ingots in order to make them more salable. The user of a solder is very apt to judge of its working qualities by the appearance of the bar; the same thing is true with regard to babbitts. Under ordinary conditions, manufacturers are justified in trying to

Jan 1, 1919

By John C. Robison

INTRODUCTION Sensitivity analysis is a means of gauging the impact of individual risks on a financing. Key risks can occur in three time periods: - Feasibility, engineering and construction phase; - Start up phase (usually through completion); - Operating phase (post completion). If a company has agreed to cover these risks prior to completion, then less attention will be paid to the sensitivity of the project in the first two time periods. Since the operating phase of the project generates cash for both operations and debt service and generally does not begin until two to six years after the loan is signed, it is wise to look at scenarios other than the projected "base-case" scenario in order to determine the project's capability to operate successfully under a broad range of probable future events. Lenders are compensated at a fixed spread over their borrowing base and generally are not compensated if the project is successful beyond expectation. They are also subject to the loss of principal plus funding costs if the project performs below expectation. Because of this, lenders establish sensitivities around the parameters of conservative projections developed in the project feasibility studies and the cash flows resulting from these projections. The initial cash flow projections should demonstrate the project's ability to meet cash costs, debt service requirements (principal and interest), and still have sufficient cushion to cover contingencies such as strikes, price fluctuations, force majeur situations, etc. (See Schreiber, Chapter 10). The selection of the level of sensitivity analysis to be performed is the result of both objective criteria, including probabilistic analysis applied to the technical parameters, and, of equal importance, subjective criteria applied by the analysts, especially with regard to the economic and financial parameters impacting the project cash flows. RISK SENSITIVITY Assumptions used in the cash flow projections should be realistic. Risks identified by the lenders should be identified and cash flows prepared to assess whether these project risks are acceptable. Typical project risks include the following (see also Chapter 9): - Sufficient reserves - quantity and quality - Product price - Production level - Operating costs - Availability of energy and supplies - Transportation and infrastructure requirements and costs - Interest rate - Completion risks - Tax level - Political risks - Cost over-run risks - Operator experience - Management - Technological risks - Environmental permits and risks - Foreign exchange risks - Insurance coverage - Equity of sponsors - Inflation rate - Capital expenditure during project life In order to see the effect on the cash flow projections, each risk should be analyzed for its impact on the cash flow generating capacity of the project. Sensitivities can be examined to see if the resultant cash flow projection will meet the lenders minimum credit standards. 1.Reserve Sensitivity In general, lenders will not assume the reserve risk. However, it should also be noted that lenders receive loan proposals in which reserves range anywhere from proven to possible. Sensitivities are not generally run for various reserve levels and reserve estimates are either considered acceptable or not acceptable by the lenders.

Jan 1, 1985