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By Alfonso Rizo-Patrón, A.M. Gaudin

Previous studies of activation in flotation have directed attention to the action of the activator on the mineral to be floated rather than to the relationship of the activator to the collector. The latter phase of the problem, however, seems to have definite scientific, if not also practical, interest. In the investigation reported in this paper, experiments were carried out, largely with quartz as subject, barium as activator, and oleate as collector. The results obtained indicate that a I: I ratio of collector ion to activator ion gives optimum results, and that a 2:1 ratio almost fails to achieve activation and flotation. Yet, a 2:I ratio would have been expected on stoichiometric grounds, had the coating been a normal salt of the activator ion with the collector ion, since barium is a divalent cation and oleate a monovalent anion. To interpret and rationalize the observations, considerations of the crystal chemistry of quartz are helpful. The point of view to which these considerations lead may be of general applicability to systems involving suspensions of solids in liquids; they confirm that an adsorbed coating is inescapable. Apparatus and Supplies The experimental work consisted in barium-ion abstraction tests, hydrogen-ion and hydroxyl-ion abstraction tests, flotation tests, and determinations of the surface of the crushed quartz. The flotation machine was built according to the design of D. W. McGlashan.* It consists of a drill press in which the bit has been replaced by a stainless-steel impellor surrounding a stainless-steel sta-tor, as in the Fagergren laboratory machine. The air intake is controlled by a valve, and the cell consists of a beaker. The quartz was obtained from vein quartz stored in large chunks. It was first crushed to 20 mesh, then sized on a 28-mesh screen. The 20 to 28-mesh size alone was retained for use. This size was freed of coarse iron by passage through a Ball-Norton magnetic separator, bleached with boiling hydrochloric acid to remove residual abraded iron, washed with distilled water until the washings were thoroughly free of ferrous, ferric, and excess hydrogen ion, and stored in covered Pyrex beakers under water until used. The barium was used as barium chloride, Baker's analyzed C. P. The oleate was used as sodium oleate. It was prepared from sodium hydroxide, Baker's analyzed C. P., and oleic acid purified by R. R. de Arellano3 in the laboratories at the Massachusetts Institute of Technology. The purification procedure was elaborated from the recent $researches of Brown and Shinowara.2 It consisted in: (I) saponification of olive oil with potassium

Jan 1, 1943

By Alfonso Rizo-Patrón, A. M. Gaudin

Previous studies of activation in flotation have directed attention to the action of the activator on the mineral to be floated rather than to the relationship of the activator to the collector. The latter phase of the problem, however, seems to have definite scientific, if not also practical, interest. In the investigation reported in this paper, experiments were carried out, largely with quartz as subject, barium as activator, and oleate as collector. The results obtained indicate that a I: I ratio of collector ion to activator ion gives optimum results, and that a 2:1 ratio almost fails to achieve activation and flotation. Yet, a 2:I ratio would have been expected on stoichiometric grounds, had the coating been a normal salt of the activator ion with the collector ion, since barium is a divalent cation and oleate a monovalent anion. To interpret and rationalize the observations, considerations of the crystal chemistry of quartz are helpful. The point of view to which these considerations lead may be of general applicability to systems involving suspensions of solids in liquids; they confirm that an adsorbed coating is inescapable. Apparatus and Supplies The experimental work consisted in barium-ion abstraction tests, hydrogen-ion and hydroxyl-ion abstraction tests, flotation tests, and determinations of the surface of the crushed quartz. The flotation machine was built according to the design of D. W. McGlashan.* It consists of a drill press in which the bit has been replaced by a stainless-steel impellor surrounding a stainless-steel sta-tor, as in the Fagergren laboratory machine. The air intake is controlled by a valve, and the cell consists of a beaker. The quartz was obtained from vein quartz stored in large chunks. It was first crushed to 20 mesh, then sized on a 28-mesh screen. The 20 to 28-mesh size alone was retained for use. This size was freed of coarse iron by passage through a Ball-Norton magnetic separator, bleached with boiling hydrochloric acid to remove residual abraded iron, washed with distilled water until the washings were thoroughly free of ferrous, ferric, and excess hydrogen ion, and stored in covered Pyrex beakers under water until used. The barium was used as barium chloride, Baker's analyzed C. P. The oleate was used as sodium oleate. It was prepared from sodium hydroxide, Baker's analyzed C. P., and oleic acid purified by R. R. de Arellano3 in the laboratories at the Massachusetts Institute of Technology. The purification procedure was elaborated from the recent $researches of Brown and Shinowara.2 It consisted in: (I) saponification of olive oil with potassium

Jan 1, 1943

By Rizo-Pairón Alfonso, A. M. Gaudin

PREVIOUS studies of activation in flotation have directed attention to the action of the activator on the mineral to be floated rather than to the relationship of the activator to the collector The latter phase of the problem, however, seems to have definite scientific, if not also practical, interest In the investigation reported in this paper, experiments were carried out, largely with quartz as subject, barium as activator, and oleate as collector The results obtained indicate that a I I ratio of collector ion to activator ion gives optimum results, and that a 2 I ratio almost fails to achieve activation and flotation Yet, a 2 I ratio would have been expected on stoichiometric grounds, had the coating been a normal salt of the activator ion with the collector ion, since barium is a divalent cation and oleate a monovalent anion To interpret and rationalize the observations, considerations of the crystal chemistry of quartz are helpful The point of view to which these considerations lead may be of general applicability to systems involving suspensions of solids in liquids, they confirm that an adsorbed coating is inescapable APPARATUS AND SUPPLIES The experimental work consisted in barium-ion abstraction tests, hydrogen-ion and hydroxyl-ion abstraction tests, flotation tests, and determinations of the surface of the crushed quartz The flotation machine was built according to the design of D W McGlashan It consists of a drill press in which the bit has been replaced by a stainless-steel impellor surrounding a stainless-steel stator, as in the Fagergren laboratory machine The air intake is controlled by a valve, and the cell consists of a beaker The quartz was obtained from vein quartz stored in large chunks It was first crushed to 20 mesh, then sized on a 28-mesh screen The 20 to 28-mesh size alone was retained for use This size was freed of coarse iron by passage through a Ball-Norton magnetic separator, bleached with boiling hydrochloric acid to remove residual abraded iron, washed with distilled water until the washings were thoroughly free of ferrous, ferric, and excess hydrogen ion, and stored in covered Pyrex beakers under water until used The barium was used as barium chloride, Baker's analyzed C P The oleate was used as sodium oleate It was prepared from sodium hydroxide, Baker's analyzed C P , and oleic acid purified by R R de Arellano3 in the laboratories at the Massachusetts Institute of Technology The purification procedure was elaborated from the recent researches of Brown and Shinowara 2 It consisted in (I) saponification of olive oil with potassium

Jan 1, 1942

By John L. Lamont, Walter Crafts

SELECTION of an alloy steel for a heat-treated article has been facilitated by methods for the calculation of hardenability,1 as-quenched hardness,2,3 and tempered tensile strength.4 Ductility and toughness may also be estimated if the steel is completely hardened on quenching,5,6 and the present study was carried out in order to develop a basis for estimating the Izod impact strength of partially hardened steel. The investigation was directed toward the prediction of Izod impact strength in steels of normal commercial quality without consideration of special compositions or heat-treatments that might produce abnormal brittleness. It was found that Izod impact strength of alloy steel is controlled by hardness, degree of hardening on quenching, and grain size. In fine-grained steels the impact strength for any given degree of hardening is inversely proportional to the tempered Rockwell C hardness, and the relation of impact strength to hardness is lowered by incomplete hardening. Calculation of the tensile strength and impact strength of heat-treating steels has shown that, except at very high strengths, tensile strength is raised by alloys without loss of impact strength whereas the tensile strength gained by higher carbon contents tends to be accompanied by a disproportionate loss of toughness. Plain carbon steels give relatively low and unpredictable impact strength. The calculation is sufficiently accurate to be helpful in the selection of alloy steel, and common grades of alloy steel have been evaluated with respect to combinations of tensile strength and impact strength attainable after heat-treatment in sections from I to 4 in. in diameter. PROCEDURE The study of the relation of hardness to impact strength was based on test data derived from 24 heats from four producers. The steels included the following SAE and AISI compositions: 1020, 1o30, 1040, 1340, 3310, 3316, 4320, 4330, 4340, 8620, 8630, 8640, 8720, 8730, 8740, 9310, 9317, 9440, 9917 and three high-alloy chromium-nickel-molybdenum steels. As far as is known, the steels tested were of normal commercial quality. They were supplied in 4-in. sections, which were forged to smaller sizes, prenormalized, and machined to final dimensions. Heat-treatment was carried out by heating to the usual austenitizing temperature for the grade of steel, holding for one hour per inch of thickness and quenching in still oil at room temperature. Previous work had indicated that this quenching treatment approximates a severity of H = 0.35. The bars were tempered as follows: ½ in., I in., and I 5/8 in., 2 hr; 2 ½ in., 3 hr; 4 in., 5 hr. All bars were air-cooled from the tempering tem-

Jan 1, 1947

By J. A. Lund, A. M. Lawson

THE structures of quenched eutectoid and hypereu-tectoid Fe-Cu alloys have been examined by X-ray diffraction and by optical and electron microscopy. The relevant portion of the Fe-Cu phase diagram is given in Fig. 1. Several values have been reported for the solubility of copper in a Fe at the eutectoid temperature, including 1.4 wt pct by orton' and 2.13 wt pct by Wreidt and Darken.2 Alloys containing 4.8 and 7.5 wt pct Cu have been prepared from two batches of Ferrovac E iron (0.005C and 0.013C) and electrolytic tough pitch copper (99.90 Cu). Specimens of dimensions 0.8 by 0.8 by 0.1 in. were cut from hot-rolled material, austenitized, and quenched into brine at 25°C. Similar specimens were also cooled in the furnace, after a short soaking treatment at 1100°C, at a rate estimated to be 10°C per min in the temperature range of 900" to 500°C. X-ray diffractometry was performed on quenched and on furnace-cooled bulk specimens using iron radiation. Only a bcc phase could be detected in all samples. Lattice parameters were calculated from measurements on four lines, made up of two resolved high-angle doublets. Comparisons were made against a silicon standard. Results are shown in Table I. Based on X-ray diffraction studies of a series of alloys of lower copper concentrations, orton' estimated that the tattice constant of a Fe at 25°C increases 0.0014A per wt pct Cu in solution. Extrapolating Norton's data, it may be concluded that all copper was retained in solution in the brine-quenched 4.8 pct Cu alloy, and that approximately 5 pct Cu was also held in solution on quenching the 7.5 pct Cu alloy. Typical microstructures of brine-quenched specimens, as observed by optical microscopy, are shown in Figs. 2 and 3. Precipitation of the E phase (copper-rich) occurred along the y grain boundaries on quenching the 7.5 pct Cu alloy, rendering them readily detectable in the microstructure, Fig. 3. The original boundaries in the 4.8 pct Cu specimens were gener- ally not discernible, however. This indicates that the z phase which was seen in the higher-copper alloy was probably of proeutectoid origin. Thin foils for transmission electron microscopy were obtained from bulk specimens by spark machining to 0.006 in. thickness, followed by electrolytic polishing. Typical transmission electron micrographs

Jan 1, 1967

By William J. McCaughey, Richard L. Barrett

FOR sixty years-in fact, ever since the inception of the basic steelmaking process -basic slags have been the subject of study by chemists, metallurgists and petrographers, with the purpose of providing a better understanding of the reactions between the slag and the metal during the refining process. The result of this work and of the researches of mineralogists and physical chemists into the chemistry of oxide systems is a considerable body of literature dealing not only with slags themselves but with equilibrium relationships in systems synthesized from pure components. Since any actual slag is a multicomponent system more complex than any yet worked out in the laboratory, a complete solution to the problem is still far away. The writers have recently published a paper1 which they believe sheds light on the role of the slag in the elimination of phosphorus and it is the purpose of the present paper to discuss the metallurgical applications of that work. Since the pioneer investigations on the constitution of basic slags carried on by Stead and Risdale, Carnot and Richards, Hilgenstock and others in the 1880's, a considerable body of literature on this subject has appeared. Many of the more important of these papers were summarized in the previous paper,' therefore they will not be reviewed here. PETROGRAPHIC STUDY The present writers have had occasion, over a period of years, to examine petrographically a great number of basic steel- making slags having a very wide range of chemical compositions and made under various conditions of operating practice. Although certain of these slags exhibit some unusual features, it is a remarkable fact that the great majority of mature slags show certain typical characteristics, which persist throughout the wide range of chemical compositions. The typical mature slag usually appears under the microscope to consist of two phases. The phase of primary crystallization is light colored and doubly refracting. If separated mechanically and subjected to chemical analysis, it is found to consist essentially of SiO2, CaO, and P2O5. Sometimes, although not usually, two such silicate-phosphate phases are found. The other conspicuous phase is dark in color and optically isotropic, and occurs as the interstitial material between the grains of the light colored phase. This dark colored interstitial phase when analyzed is found to consist essentially of FeO,Fe2O3, MnO, and MgO. In some slags high in iron oxide, particularly those from low-carbon heats, dicalcium ferrite is found. This phase is dark reddish brown in color and anisotropic.

Jan 1, 1944

By W. J. Reagan

IN a study of the life of ingot molds, it is essential to eliminate all of the variables. In the commercial manufacture of steel this is almost an impossibility. In this study many of the variables have been eliminated, and because of the unusually consistent furnace practice, with small variations in the type of steel manufactured, and a similar type of mold design for all ingot sizes, it is possible to determine with some degree of accuracy the cause of variations in ingot-mold life. All of the ingot molds in this study were used in the production of basic open-hearth killed steel with chemical analyses within the following range: C, 0.50-0.85 per cent; Mn, 0.60-0.80; Si, 0.20-0.30; S, 0.04 max.; P, 0.04 max. All ingot molds were of the closed-bottom type and used for bottom casting only. None of the molds in the study failed from cutting of the sides due to top casting; in fact, on only rare occasions are any molds used for top casting. The general type of this mold is shown in Fig. 1. All sizes have rather a heavy band of metal, about 6 in. wide, at the top to give mechanical strength at this point, and all have cast lugs. Cross sections of the vari-ous sizes from top and bottom sections are shown in Fig. 2. Ratios of wall thickness to ingot weight, ratio of ingot diameter to ingot length, and other figures of interest are shown in Table 1. In. the majority of cases, the cause of failure in this type of mold is due to heavy fire cracking on the "flats" at a point from 3 to 6 in. from the bottom radius of the mold. Fig. 3 pictures this type of failure. The start of failure at these points usually begins with a very small section of the interior surface becoming involved. As a rule, a section of 1 or 2 sq. in. is the first noticeable 'indication that mold failure is taking place. Gradually the small section increases until a sizable cavity develops, causing a protuberance on the bottom of the ingot, which eventually becomes too large to be stripped. The mold is then removed from service. At the time of failure, this cavity often reaches a size of about 5 sq. in. and about 1/2 in. deep. Sometimes cavities are found on only two or three sides and at other times all twelve sides appear to be involved.

Jan 1, 1936

By Walter Knox, J. D. Doherty

In 1939, at the request of The Koppers Coal Co., the Koppers Company Research Department established a Stoker Coal Research Laboratory for the purpose of investigating the performance characteristics of stoker coals in typical domestic stoker installations. Fig. I is a photograph of part of the laboratory. The material in this paper deals with the performance of one coal in a single installation. Presented are details of this installation, mechanical characteristics of the stoker, and the results of a series of burning tests in which adjustments were systematically varied. Summary OF Results Mechanical Features I. A large percentage of the total power consumed by a domestic stoker is used to operate the gear case and motor (Fig. 3)- 2' The power consumption per ton goes down with an increase in rate of coal feed (Fig. 4). 3. The automatic air control in this stoker showed advantages Over manual control (Fig. 5). 4. The air velocities through the retort tuyeres were uniform around the retort, but varied between the rows of tuyere rings (Fig. 6). 5. The crushing of coal with this stoker increased the minus 1/8-in. from 11.6 per cent to 19.2 per cent. There was a notice- able segregation of coal as it came from the retort and distribution was not uniform (Fig. 7). 6. Measurement of air entering over the fire showed that with some not uncommon adjustments this air may be a high percentage of the total air supply (Fig. 8 and Table I). Operating Performance ,. The, removal of clinker was shown to give a period of poor performance characterized by a high fuel-bed resistance and a high percentage of carbon monoxide in the flue gases (Fig. 10). 2. The fuel-bed resistance was found to decrease as the fuel bed built up in a normal response to heat demand after a prolonged hold-fire (Fig. II). 3. with intermittent operation the burning rate was almost always less than the feeding rate, The wide variations were found to be greatly dependent upon the length of the On period and the length of the intervals between On periods (Fig. 12). 4. The maintenance of a low furnace draft led to less fly ash, better clinker formation, and higher efficiencies (Fig. 13). 5. The maintenance of a minimum of excess air also resulted in less fly ash, better clinker formation, and higher efficiencies (Fig. 14). Guiding Principles In planning the investigations, the following principles were adopted: Selection of Heating Equipment.—Use only standard models of stokers and furnaces representative of those widely used.

Jan 1, 1942

By Walter Knox, J. D. Doherty

In 1939, at the request of The Koppers Coal Co., the Koppers Company Research Department established a Stoker Coal Research Laboratory for the purpose of investigating the performance characteristics of stoker coals in typical domestic stoker installations. Fig. I is a photograph of part of the laboratory. The material in this paper deals with the performance of one coal in a single installation. Presented are details of this installation, mechanical characteristics of the stoker, and the results of a series of burning tests in which adjustments were systematically varied. Summary OF Results Mechanical Features I. A large percentage of the total power consumed by a domestic stoker is used to operate the gear case and motor (Fig. 3)- 2' The power consumption per ton goes down with an increase in rate of coal feed (Fig. 4). 3. The automatic air control in this stoker showed advantages Over manual control (Fig. 5). 4. The air velocities through the retort tuyeres were uniform around the retort, but varied between the rows of tuyere rings (Fig. 6). 5. The crushing of coal with this stoker increased the minus 1/8-in. from 11.6 per cent to 19.2 per cent. There was a notice- able segregation of coal as it came from the retort and distribution was not uniform (Fig. 7). 6. Measurement of air entering over the fire showed that with some not uncommon adjustments this air may be a high percentage of the total air supply (Fig. 8 and Table I). Operating Performance ,. The, removal of clinker was shown to give a period of poor performance characterized by a high fuel-bed resistance and a high percentage of carbon monoxide in the flue gases (Fig. 10). 2. The fuel-bed resistance was found to decrease as the fuel bed built up in a normal response to heat demand after a prolonged hold-fire (Fig. II). 3. with intermittent operation the burning rate was almost always less than the feeding rate, The wide variations were found to be greatly dependent upon the length of the On period and the length of the intervals between On periods (Fig. 12). 4. The maintenance of a low furnace draft led to less fly ash, better clinker formation, and higher efficiencies (Fig. 13). 5. The maintenance of a minimum of excess air also resulted in less fly ash, better clinker formation, and higher efficiencies (Fig. 14). Guiding Principles In planning the investigations, the following principles were adopted: Selection of Heating Equipment.—Use only standard models of stokers and furnaces representative of those widely used.

Jan 1, 1942

By Walter Knox, J. D. Doherty

IN 1939, at the request of The Koppers Coal Co., the Koppers Company Research Department established a Stoker Coal Research Laboratory for the purpose of investigating the performance characteristics of stoker coals in typical domestic stoker installations. Fig. I is a photograph of part of the laboratory. The material in this paper deals with the performance of one coal in a single installation. Presented are details of this installation, mechanical characteristics of the stoker, and the results of a series of burning tests in which adjustments were systematically varied. SUMMARY OF RESULTS Mechanical Features I. A large percentage of the total power consumed by a domestic stoker is used to operate the gear case and motor (Fig. 3). 2. The power consumption per ton goes down with an increase in rate of coal feed (Fig. 4). 3. The automatic air control in this stoker showed advantages over manual control (Fig. 5). 4. The air velocities through the retort tuyeres were uniform around the retort, but varied between the rows of tuyere rings (Fig. 6). 5. The crushing of coal with this stoker increased the minus 1/8-in. from 1 1.6 per cent to 19.2 per cent. There was a noticeable segregation of coal as it came from the retort and distribution was not uniform (Fig. 7). 6. Measurement of air entering over the fire showed that with some not uncommon adjustments this air may he a high percentage of the total air supply (Fig. 8 and Table I). Operating Performance I. The removal of clinker was shown to give a period of poor performance characterized by a high fuel-bed resistance and a high percentage of carbon monoxide in the flue gases (Fig. 10). 2. The fuel-bed resistance was found to decrease as the fuel bed built up in a normal response to heat demand after a prolonged hold-fire (Fig. II). 3. With intermittent operation the burning rate was almost always less than the feeding rate. The wide variations were found to be greatly dependent upon the length of the On period and the length of the intervals between On periods (Fig. 12). 4. The maintenance of a low furnace draft led to less fly ash, better clinker formation, and higher efficiencies (Fig. I3). 5. The maintenance of a minimum of excess air also resulted in less fly ash, better clinker formation, and higher efficiencies (Fig. 14). GUIDING PRINCIPLES In planning the investigations, the following principles were adopted: Selection of Healing Equipment.-Use only standard models of stokers and furnaces representative of those widely used.

Jan 1, 1942

By P More

US 4,132,621-In the electrowinning of aluminum, the cells are aligned in a lengthwise direction so as to lessen the harmful influence of the induced magnetic fields Each cell is supplied with current from the preceding cell both via the head arid at least one side riser The output of the cathode bars is divided into two separate groups, the upstream group supplying the head of the subsequent cell arid the downstream group supplying the side risers of the subsequent cell This produces a substantial improvement in cell efficiency arid a greater regularity P Morel, J P Dugois, arid B Langon, assigned to Aluminium Pechiney. Jan 2, 1979 12 pp. (204¬243M) Filed 1-12-78 (868,861) Priority: France, 1-19-77 (77/2,213) US 4,134,806-Cells, anodes, arid methods for use in the electrowinning of nickel, cobalt, copper, zinc, or other metals from an acid ore leach solution or the like The cell is provided with vertically immersed stationary cathodes and stationary rod anodes which are noncorrodible by the electrolyte arid are electrocatalytic to the anode reaction. The spaced parallel anode rods are connected to electric current supply bars The anode rods have an electroconductive core made of a metal alloy arid a surface coating of an oxide of platinum or a platinum group metal The ratio of active cathode surface area to active anode surface area is preferably at least 3 0. De Nora arid C Traini, assigned to Diamond Shamrock Tech¬nologies, SA Jan 16, 1979 13 pp. (204-105R) Filed 9-15-77 (833,661) Priority Italy, 1-29-73 (19738 A/73). Same British 1,434,334-5, dated May 5, 1976 US 4,135,994-In the electrowinning of aluminum at a high current efficiency, the electrolytic bath is a mixed molten salt consisting of 2-15% by weight of aluminum trichloride, 15-83% of sodium chloride, 15-70% of combined calcium chloride arid magnesium chloride but riot more than 40% of calcium chloride, arid optionally up to 10% of barium chloride Preferably, plate-shaped graphite electrodes used for both cathodes and anodes are arranged in parallel inclined relation so that the axis in the lengthwise direction makes an angle of from 10° to 45° to the horizontal. T Ishikawa arid H Ichikawa, assigned to Nippon Light Metal Co Ltd Jan 23, 1979 4 pp (204-67) Filed 11-15-77(851,632) Same British 1,550,502, dated Aug 15, 1979

Jan 1, 1980

By James A. Barr

The writer's first experience with flotation was during World War I, in the bene-ficiation of Alabama graphite schist ores. One plant used a cone with a peripheral overflow; dried ore was distributed by a rotating disk onto the surface of the water. No reagents were added' The flake-graphite film floated along with some fine silica. Dewatering screens separated the flake. Naturally unit capacities were low but results were satisfactory. Minerals separation mechanical flotation machines were used in another graphite mill. pine oil was added directly to the head cells, with very good results. All the graphite concentrates from both types of flotation were carefully refined after drying by passing through burr mills, followed by very close sizing on sifters. In March 1927, the writer ran a very successful flotation test on minus 28-mesh, deslimed, Tennessee brown phosphate "sand,"† using a mechanical laboratory machine built in the shops of the Anaconda Copper Mining Co., through the courtesy of Ernest Klepetko. The machine was soon converted to a subaeration type, with improved results. This phosphate research program was greatly enlarged and led to the formation of the phosphate Recovery corporation. The development of nonmetallic flotation followed rapidly. The first flotation machine for bene- ficiation of phosphate was installed in January 1928, in a pilot mill, by International Minerals and Chemical Corporation, at Mulberry, Florida. These machines were Minerals Separation, 24-in., sub-,,,tion types, with weir control of pulp between cells. The sand bleeders were very small—about 1¼-in. diameter. As the feed flake. Is to 25 per cent plus 28-mesh material, the cells choked up frequently. This was corrected by cutting a 2 by 6-in. bleeder opening above the impellers, at grid level, which short-circuited the coarse fractions directly into the feed of the next cell. The matter of size classification and grinding was a considerable problem, which does not come within the scope of this article. Because of the troubles noted above, cascade-type roughers were installed in the second flotation plant, built about 1930. Experimental cells had been tried in 1928. General plant layout is shown in Fig. 1 and details of the cascade construction in Fig. 2. The cascade installation in plant NO. 2 gave good results and eliminated troubles due to choke-ups and coarse feed. The capacities and metallurgical results equaled those of the modified 24-in. Minerals Separation flotation machines in plant No. I The objections to the cascade installation are the floor space and mill height required. In 1939 an improved Minerals Separation machine was tested in parallel with the cascades. Extensive tests indicated

Jan 1, 1947

By James A. Barr

The writer's first experience with flotation was during World War I, in the bene-ficiation of Alabama graphite schist ores. One plant used a cone with a peripheral overflow; dried ore was distributed by a rotating disk onto the surface of the water. No reagents were added' The flake-graphite film floated along with some fine silica. Dewatering screens separated the flake. Naturally unit capacities were low but results were satisfactory. Minerals separation mechanical flotation machines were used in another graphite mill. pine oil was added directly to the head cells, with very good results. All the graphite concentrates from both types of flotation were carefully refined after drying by passing through burr mills, followed by very close sizing on sifters. In March 1927, the writer ran a very successful flotation test on minus 28-mesh, deslimed, Tennessee brown phosphate "sand,"† using a mechanical laboratory machine built in the shops of the Anaconda Copper Mining Co., through the courtesy of Ernest Klepetko. The machine was soon converted to a subaeration type, with improved results. This phosphate research program was greatly enlarged and led to the formation of the phosphate Recovery corporation. The development of nonmetallic flotation followed rapidly. The first flotation machine for bene- ficiation of phosphate was installed in January 1928, in a pilot mill, by International Minerals and Chemical Corporation, at Mulberry, Florida. These machines were Minerals Separation, 24-in., sub-,,,tion types, with weir control of pulp between cells. The sand bleeders were very small—about 1¼-in. diameter. As the feed flake. Is to 25 per cent plus 28-mesh material, the cells choked up frequently. This was corrected by cutting a 2 by 6-in. bleeder opening above the impellers, at grid level, which short-circuited the coarse fractions directly into the feed of the next cell. The matter of size classification and grinding was a considerable problem, which does not come within the scope of this article. Because of the troubles noted above, cascade-type roughers were installed in the second flotation plant, built about 1930. Experimental cells had been tried in 1928. General plant layout is shown in Fig. 1 and details of the cascade construction in Fig. 2. The cascade installation in plant NO. 2 gave good results and eliminated troubles due to choke-ups and coarse feed. The capacities and metallurgical results equaled those of the modified 24-in. Minerals Separation flotation machines in plant No. I The objections to the cascade installation are the floor space and mill height required. In 1939 an improved Minerals Separation machine was tested in parallel with the cascades. Extensive tests indicated

Jan 1, 1947

By H. M. Chance, T. M. Chance

The term 'Llow-sulfur coal," as used in this discussion, is limited to coals containing less, or very little more, than 1 per cent. sulfur. For certain purposes it might be advantageous to include coals that contain as much as 1.25 per cent. sulfur, because such coals have been considered as available for making metallurgic coke of fair grade; but the same reasoning might apply to coals containing as much as.1 1/2 per cent. sulfur, if facilities exist for utilizing such coal by admixture with coal containing less sulfur. , In Pennsylvania, it is not possible to define the exact geographic limits of the areas in which coals relatively low in sulfur exist, because variations in the percentage of sulfur occur irregularly and often abruptly. It is not uncommon to find areas, more or less circumscribed in extent, in which the coal is relatively high in sulfur although all the surrounding territory contains low-sulfur coal; and, similarly, small areas of low-sul. fur coal exist in districts where the coal is normally high in sulfur. These generalizations apply, with few exceptions, to the whole area underlaid with bituminous coal in the State of Pennsylvania, and also to each of the individual beds of coal in this state. Pennsylvania is poorly supplied with coals of the low-sulfur class. We find, however, as an offset to this condition, very large areas in which coal ranging from 1 to 2 1/2 per cent. sulfur exists in beds of good workable thickness. This coal, by washing, can be reduced in sulfur low enough to make coke of a high grade. While a considerable tonnage of workable low-sulfur coal remains in the Pennsylvania bituminous districts, it has been necessary to turn to the areas of higher sulfur coal for the supply of metallurgical coke. This utilization of the higher sulfur areas has been made possible either by washing or by selective mining. Washing.—Fine crushing of the entire feed is not generally necessary to the successful washing of Pennsylvania coals. This is due to the fact that the pyrite is rarely finely and uniformly disseminated throughout the coal but is usually confined to high-sulfur benches in the bed or to concentrations on the cleavage planes of the coal. Hence, by graded crushing and sizing it is frequently possible to at once reclaim those portions of the coal bed containing coal that is relatively free from pyrite.

Jan 1, 1920

By Roswell P. Angier, Herbert S. Kalish, Henry H. Hausner

POWDER metallurgical methods as applied to zirconium are of great interest because they permit not only the fabrication of parts directly to shape with a minimum loss of material but also the utilization of scrap, and the metal may be processed at temperatures well below the melting point. There are two difficulties involved in the melting of zirconium: 1—High vacuum is necessary for melting, and 2—zirconium reduces nearly all oxides so that it is difficult to find a suitable crucible material. The purest material, zirconium crystal bar, is expensive, and the methods of subsequent fabrication are limited. Cold rolling or extrusion of zirconium crystal bar is suitable for making certain shaped parts, but where melting is involved, the purity of the metal is invariably decreased, and a method of casting to a definite shape does not seem to be feasible. Where it is necessary to hot roll, zirconium must be covered with a steel or copper jacket to protect it from the air. This is necessarily a costly operation. Where annealing of zirconium is necessary it must be conducted in a high vacuum. In an investigation of powder metallurgical methods for zirconium, the zirconium powder used should be characterized by the following properties: 1— Highest degree of purity, 2—uniformity in particle shape and particle size distribution, 3—low compression ratio, and 4—satisfactory strength of the compacted powder (green strength). Zirconium powders have been made by two methods: By the reduction of zirconium tetrachloride (ZrC1,) with sodium,2' *•B "nd by the reduction of zirconium oxide with calcium and calcium chloride." The first method represents one of the earliest attempts to make pure zirconium metal, and the sintered product from this powder is extremely brittle. The second method of making zirconium powder is far more successful, but the powder made in this way has an extremely low apparent density and, therefore, a high compression ratio which makes it difficult to use it for powder metallurgical purposes. For these reasons the above-mentioned zirconium powders were not used in this investigation. To obtain sintered zirconium compacts of highest 'purity and good ductility, it was first necessary to produce a suitable powder. Pure zirconium has been made chiefly by two methods. The iodide method, from which the product is "crystal bar" zirconium, was developed first.'." By this purification process very soft, pure, and ductile zirconium metal can be produced. The second method, developed by the U. S. Bureau of Mines, is the reduction of zirconium chloride with magnesium." The sponge zirconium thus produced is also soft, pure, and ductile.

Jan 1, 1952

By Clarence Zener

THE internal friction of nonferrous metals vibrating at low stress amplitudes has so far always been successfully interpreted in terms of inhomogeneities of one sort or another. Examples are the fluctuation of stress across a specimen vibrating transversely,1,2,3 the stress inhomogeneities due to the elastic anisotropy and partial random orientation of the individual crystallites,4,5 localized weak regions introduced by cold-working,6,7 grain boundaries and possibly twinning planes.8.9 Perfect single crystals are, by definition, homogeneous. Actual single crystals usually, perhaps always, contains some imperfections. The present investigation was undertaken to determine whether the internal friction of single crystals may likewise be attributed to inhomogeneities. This study was made possible through the gift of a large single crystal of 70-30 alpha brass by H. L. Burghoff, of the Chase Brass and Copper Co. The specimen, 3-s in. in diameter and 10 in. long, was similar to samples previously described by Mr. Burghoff.10 EXPERIMENTAL METHOD The experimental method used has previously been described in Institute papers.5,6.9 The measure of internal friction adopted here, I/Q, is (p) X the logarithmic decrement, a measure used by some writers, and is also (I/2p) X the specific damping capacity, a measure used by other writers. In all measurements the stress level was kept so low that the measurements were independent of stress level. In all measurements in which the temperature was varied, observations were made as the specimen slowly cooled from its highest temperature. The specimen was vibrated transversely. Observations were made at the fundamental frequency and at the first overtone, of about 620 and 1710 cycles per second, respectively. No attempt was made to avoid acoustical losses. EXPERIMENTAL RESULTS The specimen was annealed for several hours at 450°C. The temperature dependence of the internal friction was then determined from room temperature to 400°°C. As shown in Fig. i, the internal friction increased by only a factor of 2 from room temperature to 300°°C., then by a factor of 100 during the next :too' interval. These measurements are consistent with the view that the observed internal friction is the superposition of two distinct parts. One, dominant at room temperature, is nearly independent of temperature. This part may be accounted for by acoustical losses and by transverse thermal currents. It was not further investigated. The second part, when plotted in the manner of Fig. I, lies upon a straight line. Therefore it has a heat of activation H; i.e., it varies with temperature as Internal friction ~ e-HI/RT [I]

Jan 1, 1942

By B. M. Larsen, T. E. Brower

INTRODUCTION THIS discussion is based on statistical manipulation and evaluation of operating data from several commercial blast furnaces which include rather wide variations in practice. We are concerned here mainly with the effect of manganese on sulphur elimination under operating conditions in commercial blast furnaces, but this effect can be outlined more clearly by including certain other variables such as silicon in iron and slag basicity, which are all in part interrelated. Real progress in understanding all of the smelting-zone reactions in this process requires more laboratory studies of slagmetal melts similar to those in the blast furnace, with careful control of oxygen pressure. Such experimental work is very difficult, however, and in the meantime, with the present scarcity of more fundamental data, such statistical trends and correlations as can be obtained from commercial furnace operating records may help in choosing laboratory test conditions as well as adding to our knowledge of operating procedures. We do not know just why the furnace data are apparently so irregular that statistical treatment of large numbers is needed to obtain accurate trends. It is .partly caused, no doubt, by the many simultaneous variables present, but there are perhaps also such factors as: (I) the continual swings up and down so characteristic of the process; (2) difficulty of accurate sampling of co-existing phases, as well as (3) the presence of both equilibrium and rate factors as a result of the fast driving of the process, In desulphurization, for example, the flow of thin layers of slag and metal over solid coke surfaces, plus the contact between droplets of iron falling through the slag layer in the hearth, would lead one to expect a close approach to equilibrium, On the other hand, most of the critical part of sulphur removal may occur in a short time and distance below the tuyeres with perhaps an accompanying decrease in oxygen pressure and the concurrent reduction of much of the silicon and manganese, so its degree of approach to equilibrium may be quite variable. PROBABLE CHEMISTRY OF DESULPHURIZATION Since there is little evidence that sulphur atoms in the iron solution are associated to any appreciable extent in molecules such as MnS, the transfer from slag to metal and back again can be written:* [(FeS) -, [FeS],[I] hence the following reactions seem most probable in the slag phase, (FeS) + (CaO) = (CaS) + (FeO), [2] and, (FeS) + (MnO) ;:2 (MnS) + (FeO). [31]

Jan 1, 1948

By Harold Markus, Arthur H. Grobe, Gerhard Derge

THE high corrosion resistance possessed by tin under most circumstances, combined with its generally satisfactory appearance and useful physical properties, has led to many and varied uses for the metal. These uses have been partly limited by the fact that tin is an expensive metal, therefore many applications have been developed in which tin has been employed in combination with lead, either by coating, as in tin-lined collapsible tubes, or by the formation of alloys containing various proportions of tin-rich and lead-rich phases, as terne plate. A detailed knowledge of the corrosion characteristics of the tin-lead couple therefore is of general interest and has become specially important at the present time, when every effort is being made to conserve tin as much as possible. The present study. has been limited to carbonate solutions with a pH range from 8.4 to 11.2 so that the results may be related to earlier work on the corrosion of tin and its alloys.1-3,6 In these papers, the effects of a number of anion and cation additions to these solutions have been observed. APPARATUS AND METHOD The electrodes for the corrosion cell were cut from rolled sheet about 1/16 in. thick. The length of all specimens was held constant at 7 in., while the width was varied from 1/2 to 2 in. These electrodes were fastened to brass electrode supports, which were attached to rubber stoppers fitting into tall-type one-liter Pyrex beakers that contained the electrolyte. The lead electrodes were prepared from Omaha pig* and the tin was rolled from a slab of Chempur.? After cutting to size, the sheets were polished with No. I emery paper and cleaned with carbon tetrachloride. The edges, back and upper parts of the specimen were coated with a synthetic lacquer, which was supplemented with beeswax for the lead electrodes. The binding posts were coated with beeswax after the electrodes had been damped. The pH of the electrolyte was controlled? by adjusting the ratio of carbonate to bicarbonate. Approximately 600 ml. of electrolyte was used in each beaker. The entire assembly was placed in an oil bath thermostatically adjusted to operate at 30°C. ± 0.10. Potentials were measured against a saturated calomel electrode connected. to the cell by an agar-agar salt bridge. The carbonate solution used in the salt bridge was the same as that used in the corrosion cell. Currents were measured with a milliam-

Jan 1, 1942

By J. Gordon Parr, D. H. Polonis

High purity alloys of titanium and iron, made by a technique of levitation melting, have been investigated with particular reference to martensite formation and decomposition in the hypoeutectoid range. A preliminary study has been made of the occurrence of the phase corresponding to the structure Ti2Fe. MANY of the previous investigations of Fe-Ti alloys have been made using Kroll sponge as a source of titanium; and the subsequent heat treatments to which alloys have been subjected has, on occasion, led to further contamination. Worrier,',' who suggested a part of the equilibrium diagram for the binary system, and Wallbaum and coworkers,3-5 who worked largely with iron-rich alloys, all used Kroll sponge. Van Thyne, Kessler, and Hansen,6 in their determination of the equilibrium diagram, used iodide titanium for alloys up to 30 pct Fe. Duwez,7 who measured the M. temperature of titanium binary alloys with many solute elements, used iodide titanium in all cases except in his work on Ti-Fe alloys for which he used Kroll sponge. The investigation of the supposed phase Ti2Fe by Rostoker8 nvolved the use of iodide titanium. A section of the constitutional diagram, after Van Thyne et al., is reproduced in Fig. 1. Frequently too much stress is placed on the effect of contaminants in equilibrium and nonequilibrium systems, but there is no doubt that titanium alloys are extremely susceptible to interstitial atoms. Consequently, the main purpose of the work to be described was to determine those features of phase transformations in pure Ti-Fe alloys that were considered of importance in commercial heat treatments. For, although commercial alloys may not be of high purity, the investigation of a system uncomplicated by traces of impurity is a desirable starting point. Another incidental feature, the occurrence of Ti2Fe, was also investigated. The entire study was carried out using powders obtained from alloy ingots, for diffusion reactions are often more rapid in small particles than in bulk specimens. The frequently adopted practice of ascertaining phase constitutions by X-ray analysis of powders, and relating these to the microstructures and mechanical properties of bulk specimens, is considered by the authors to be open to criticism. In the martensite reactions in the Fe-Mn system, for example, it has been shown- hat similar phase distributions in solid and powder may result in different hardness values and appearance under the microscope; and it is possible that similar anomalies might occur in the Ti-Fe system. Consequently, in order to

Jan 1, 1955

By Charles C. Hawes

DETERMINATION OF SILICA OXIDE iron ores usually are found in intimate association with silica and phosphorus compounds. Their quantitative separation and purification sometimes present difficult problems to the chemist. Silicic acids may represent various degrees of dehydration. They are exeedingly weak, but combine with metallic oxides and form some of the most stable oxides in nature, the silicates. When iron ores are treated with hydrochloric acid, they yield practically all their iron. However, apart from rare exceptions, varying amounts of insoluble residues of silica, alumina, lime, magnesia and compounds of phosphorus, sulphur, titanium, chromium and others will be left. If the oxides of silicon, aluminum and titanium are present in small quantities, the insoluble residue is generally very small, but the presence of these oxides is more usual in larger quantities. Therefore, only a special treatment can break the bond between these elements. Ore Residues Acids remove the soluble constituent of the ore, leaving the insoluble residue, which chemically is rock or gangue and must be treated accordingly. Alkali carbonates are used frequently to break up the residue, but other fluxes have also been recommended, such as a number of lead and boron salts. The introduction 0f these salts, which offers certain advantages, requires, however, their removal before the other constituents can be analyzed, and this elimination is sometimes difficult. Usually in quantitative analysis silicates are dissociated by fusing them in a platinum crucible with sodium carbonate, thereby forming sodium silicate, Na2SiO3, sodium aluminate, Na2Al204, sodium titanate, Na2TiO3, and carbonates of other elements. All the carbonates are soluble in hydrochloric acid, but also some silicic acid is formed that must be rendered insoluble. To this end the solution is evaporated several times, as the first evaporation still leaves as much as 5 per cent of the silica soluble. Even after a number of evaporations, minute quantities of silica may be found with the iron and alumina present. Perchloric Acid as an Agent for Dehydrating Silicic Acid Perchloric acid, HC104, (60 per cent), has been used for years as a solvent, but few chemists have used it to dehydrate silica. It is derived from anhydrous perchloric C1207, which is most unstable and dangerous. Perchloric acid is a strong oxidizing agent, which boils at 203°C. It is more effective in rendering silica insoluble than any other known agent, and most rapid in action. After perchloric acid is added to a mixture containing silicic acid, the resultant solution is

Jan 1, 1945