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By E. F. Reed

CONSIDERABLE deep hole prospect drilling has been done in the last few years in the Globe-Miami mining district about 70 miles east of Phoenix, Arizona, and in the San Manuel-Tiger area about 50 miles south of the Globe-Miami region. More than 205,000 ft of churn drilling have been completed by the San Manuel Copper Corp. at their property in the Old Hat Mining District in southern Pinal County. The deepest hole on this property is 2850 ft; there are 49 holes deeper than 2000 ft. At the adjoining Houghton property of the Anaconda Copper Mining Co., where only one hole reached 2000-ft depth, there were 27,472 ft of churn drilling and 3436 ft of diamond drilling. Three churn drill holes were deepened by diamond drilling methods. Near Miami in the Globe-Miami district the Amico Mining Corp. drilled four holes by combined churn and rotary drilling methods, the total amounting to 13,879 ft, of which 2256 ft were drilled with a portable rotary rig. In the same district, besides doing a large amount of shallow prospect drilling, the Miami Copper Co. drilled two holes of 2560 and 3787 ft, respectively, which were completed by churn drilling methods. The rocks encountered in drilling at San Manuel and Tiger are described by Steele and Rubly in their paper on the San Manuel Prospect' and by Chapman in a report on the San Manuel Copper Deposit.' The rocks are well-consolidated Gila conglomerate, quartz monzonite, and monzonite porphyry. In some places these formations stand very well while being drilled, and three holes were drilled without casing, the deepest of which was 2200 ft. In other holes faulted and fractured ground made drilling difficult. In the Globe-Miami district the deep drilling was done in the down-faulted block of Gila conglomerate east of the Miami fault and in the underlying Pinal schist. The geology of this area is described by Rannome. In the Amico holes the conglomerate varied from material consisting entirely of granite boulders and fragments to a rock made up of schist fragments in a sandy matrix; in the Miami Copper Co. holes there were more granite boulders and the material was poorly consolidated. Drilling was much more difficult and expensive in the Miami area than in the San Manuel district, mainly because of the depth of the holes and the formations drilled. All the deep hole prospecting described in this paper was done with portable rigs. The churn drill rigs were of several types, of which the Bucyrus-Erie were the most popular. Bucyrus-Erie 28L, 29W, and 36L rigs were used on some of the deeper holes on the San Manuel property. A few Fort Worth spudder types were tried, and the deepest hole at San Manuel was drilled with a Fort Worth Jumbo H. The spudder type is considerably larger than most other rigs used on this work and required a larger location site. The spudders were belt-driven machines with separate power units, and time required for setting up and moving was much longer than with the more portable drills. All the churn drilling was done by contractors or with machinery leased from them. A few of the contractors had complete equipment, including most of the necessary fishing tools. Unusual and special fishing tools were obtainable from the supply companies in the oil fields of New Mexico or in the Los Angeles area. Most of the contractors used equipment with standard API tool joints, so that much of it was interchangeable. Failure of tool joints is one of the principal causes of fishing jobs. It can be minimized if the joints are kept to the API specifications and the proper sized joints are used in the various holes. The minimum sizes that should be used with various bits are as follows: 12-in. and larger bits, 4x5-in. tool joints; 10-in. bits, 31/4x41/4-in. tool joints; 8-in. bits, 23/4x 33/4-in. tool joints; 6-in. bits, 2Y4x3Y4-in. tool joints; 4-in. bits, 15/ix25/8-in. tool joints. Two rotary drill rigs were tried at San Manuel on the same hole, and a portable rotary drill rig was used on the Amico drilling for test coring the formation and for drilling in holes 3 and 4. Rotary drilling differs from churn drilling or cable tool drilling in that the bit is revolved by a string of drill pipe and the cuttings are removed from the hole by a thin solution of mud pumped through the drill pipe. The principal parts of a rotary rig are the power unit, a rotating table to revolve the drill pipe, hoists to raise and lower the pipe and to handle casing, and a pumping system to circulate the drilling liquid. The rig used on the Amico property at Miami was mounted on a truck. The larger rig used on the San Manuel property was hauled by several trucks and had separate turntable and pumping units. Diamond drill coring equipment was used successfully with the rotary rig in the holes on the Amico property. To allow for 23/8-in. drill pipe with tool joints, 31h-in. core barrels and bits were used. With the standard 31h-in. core barrel there was considerable difficulty in maintaining circulation with mud, so a barrel was designed with a smaller inner tube and a broad-faced bit. This allowed coarser material to circulate between the barrels. Rock bits of 55/8 to 3 in. were used with the rotary rig for drilling between core runs. Diamond drill equipment is much lighter than churn drill tools, so that fishing tools can usually be obtained from supply houses by air express when needed. Three churn drill holes on the Houghton property at Tiger were deepened by diamond drilling with Longyear UG Straitline gasoline-driven machines. The open churn drill hole was cased with 21h-in. black pipe. In deep hole churn drilling, casing is one of the most important items, especially in drilling in un-consolidated material like the formations drilled by

Jan 1, 1953

By E. F. Reed

CONSIDERABLE deep hole prospect drilling has been done in the last few years in the Globe-Miami mining district about 70 miles east of Phoenix, Arizona, and in the San Manuel-Tiger area about 50 miles south of the Globe-Miami region. More than 205,000 ft of churn drilling have been completed by the San Manuel Copper Corp. at their property in the Old Hat Mining District in southern Pinal County. The deepest hole on this property is 2850 ft; there are 49 holes deeper than 2000 ft. At the adjoining Houghton property of the Anaconda Copper Mining Co., where only one hole reached 2000-ft depth, there were 27,472 ft of churn drilling and 3436 ft of diamond drilling. Three churn drill holes were deepened by diamond drilling methods. Near Miami in the Globe-Miami district the Amico Mining Corp. drilled four holes by combined churn and rotary drilling methods, the total amounting to 13,879 ft, of which 2256 ft were drilled with a portable rotary rig. In the same district, besides doing a large amount of shallow prospect drilling, the Miami Copper Co. drilled two holes of 2560 and 3787 ft, respectively, which were completed by churn drilling methods. The rocks encountered in drilling at San Manuel and Tiger are described by Steele and Rubly in their paper on the San Manuel Prospect' and by Chapman in a report on the San Manuel Copper Deposit.' The rocks are well-consolidated Gila conglomerate, quartz monzonite, and monzonite porphyry. In some places these formations stand very well while being drilled, and three holes were drilled without casing, the deepest of which was 2200 ft. In other holes faulted and fractured ground made drilling difficult. In the Globe-Miami district the deep drilling was done in the down-faulted block of Gila conglomerate east of the Miami fault and in the underlying Pinal schist. The geology of this area is described by Rannome. In the Amico holes the conglomerate varied from material consisting entirely of granite boulders and fragments to a rock made up of schist fragments in a sandy matrix; in the Miami Copper Co. holes there were more granite boulders and the material was poorly consolidated. Drilling was much more difficult and expensive in the Miami area than in the San Manuel district, mainly because of the depth of the holes and the formations drilled. All the deep hole prospecting described in this paper was done with portable rigs. The churn drill rigs were of several types, of which the Bucyrus-Erie were the most popular. Bucyrus-Erie 28L, 29W, and 36L rigs were used on some of the deeper holes on the San Manuel property. A few Fort Worth spudder types were tried, and the deepest hole at San Manuel was drilled with a Fort Worth Jumbo H. The spudder type is considerably larger than most other rigs used on this work and required a larger location site. The spudders were belt-driven machines with separate power units, and time required for setting up and moving was much longer than with the more portable drills. All the churn drilling was done by contractors or with machinery leased from them. A few of the contractors had complete equipment, including most of the necessary fishing tools. Unusual and special fishing tools were obtainable from the supply companies in the oil fields of New Mexico or in the Los Angeles area. Most of the contractors used equipment with standard API tool joints, so that much of it was interchangeable. Failure of tool joints is one of the principal causes of fishing jobs. It can be minimized if the joints are kept to the API specifications and the proper sized joints are used in the various holes. The minimum sizes that should be used with various bits are as follows: 12-in. and larger bits, 4x5-in. tool joints; 10-in. bits, 31/4x41/4-in. tool joints; 8-in. bits, 23/4x 33/4-in. tool joints; 6-in. bits, 2Y4x3Y4-in. tool joints; 4-in. bits, 15/ix25/8-in. tool joints. Two rotary drill rigs were tried at San Manuel on the same hole, and a portable rotary drill rig was used on the Amico drilling for test coring the formation and for drilling in holes 3 and 4. Rotary drilling differs from churn drilling or cable tool drilling in that the bit is revolved by a string of drill pipe and the cuttings are removed from the hole by a thin solution of mud pumped through the drill pipe. The principal parts of a rotary rig are the power unit, a rotating table to revolve the drill pipe, hoists to raise and lower the pipe and to handle casing, and a pumping system to circulate the drilling liquid. The rig used on the Amico property at Miami was mounted on a truck. The larger rig used on the San Manuel property was hauled by several trucks and had separate turntable and pumping units. Diamond drill coring equipment was used successfully with the rotary rig in the holes on the Amico property. To allow for 23/8-in. drill pipe with tool joints, 31h-in. core barrels and bits were used. With the standard 31h-in. core barrel there was considerable difficulty in maintaining circulation with mud, so a barrel was designed with a smaller inner tube and a broad-faced bit. This allowed coarser material to circulate between the barrels. Rock bits of 55/8 to 3 in. were used with the rotary rig for drilling between core runs. Diamond drill equipment is much lighter than churn drill tools, so that fishing tools can usually be obtained from supply houses by air express when needed. Three churn drill holes on the Houghton property at Tiger were deepened by diamond drilling with Longyear UG Straitline gasoline-driven machines. The open churn drill hole was cased with 21h-in. black pipe. In deep hole churn drilling, casing is one of the most important items, especially in drilling in un-consolidated material like the formations drilled by

Jan 1, 1953

By Carl R. Christiansen

Since the first pay hole in Missouri's "New Lead Belt" was drilled in 1955, this district has become one of the world's leading sources of lead. The belt extends from north of Viburnum in a southerly direction to near Eminence, a distance of about 35 miles. The St. Joseph Lead Company was the discoverer and first to develop new mines in the Viburnum area. Since the discovery of the New Lead Belt, many companies have engaged in exploration programs and several major companies have become active in development of new mines. These include Cominco American, Inc., which operates a joint venture with Dresser Industries; Ozark Lead Company, a subsidiary of Kennecott Copper Company; and Missouri Lead Operating Company, a joint venture of Arnax and Homestake. St. Joseph Lead Company, with over 100 years of experience in the Old Lead Belt, has served as a leader in development of equipment and mining techniques, making its properties some of the most efficient mining operations in the world. The new producers give the district the benefit of fresh viewpoints, as their engineers are mostly from outside of Missouri and their previous experience has been considerably different from conventional lead belt practices. While all operations are similar in that they are room-and-pillar, the diverse experience of the operators has produced a group of mines that employ a variety of equipment and mining techniques to give increased efficiency

Jan 1, 1970

By R. E. Wagner

MISSOURI's famous lead area, in what is known as Southeast Missouri, is locally termed the "Lead Belt." These deposits are in the Bonne Terre dolomite of late Cambrian age which has a thickness of nearly 400 ft. Underlying this is the La Motte sandstone which varies in thickness from 0 to 400 ft. The La Motte beds are deposited directly on the ancient erosion surface of Pre-Cambrian porphyries and granites of probably Algonkian age. The buried igneous peaks extend up into the Bonne Terre in several areas within the Lead Belt. Overlying the Bonne Terre are shales and siliceous dolomites of late Cambrian and early Ordovician age. Within the Lead Belt these have a thickness of from 0 to 500 ft. The district is bounded in general on the southwest by the Sims Mountain fault, on the northwest and north by the Big River fault, and on the

Jan 1, 1947

By Earl Oliver

IN times like these, the A. I. M. E. and similar societies have their greatest usefulness. . . . Individuals and companies acting alone in the development of public opinion are merely voices crying in the wilderness. United and organized they make a great force that can and does influence public action. . . . What part, if any, then, shall the A. I. M. E. take in these great stabilization processes of civilization? Shall it help to give direction and force to scientific knowledge which comes within its field of activity or shall it merely develop more of it? . . . Is it the A. I. M. E.'s function to help bring system, order and direction out of this situation so that the world can again have forward economic movement, or should it rest on its oars until other agenciess develop that public understanding and direction so necessary for economic progress? As we understand the functions of the A. I. M. E. Petro¬leum Division, they are to discover and promote knowl¬edge for the benefit of society on the mining of oil and gas. To the individual member of the Petroleum Division, there are certain advantages of social and professional contacts, but the collective purpose is that described. And the individual is benefited by membership only as the Division measures up to the purposes of its existence. Consequently, the welfare of this Division and that of its members depends on the extent to which it keeps pace with the needs of society on matters relating to the mining of oil and gas.

Jan 1, 1932

By Charles H. Addison, Robert W. Shields, James W. Sweeney

GIPSY: Is user oriented. Is flexible in applications. Is an ITERATIVE question answering system. Has an adaptable retrieval mechanism. Has both a batch and a teleprocessing version. Allows the user to "browse" through his information. Has ability to answer "ad hoc" queries. Is a currently working and proven system.

Jan 1, 1969

By WALTER B. JONES

PIG iron was first produced in Alabama in 1818 from limonite or brown ore and since then much of this ore has come from the so-called mineral district of northern Alabama, especially along the Cretaceous-Paleozoic contact. For many years the Russellville district in Franklin County, where the first blast furnace was erected, produced more than 100,000 tons of brown ore annually. Limonite has been reported at many places in the Coastal Plain region, where the formations are of Mesozoic and Cenozoic age, but these scattered deposits were never considered to be of much commercial importance. However, in the last three years a considerable quantity of this ore has been scraped up and shipped, particularly from the city of Greenville in Butler County.

Jan 1, 1938

H. N. EAVENSON, Gary, W. Va.-Judging from our own experience, the statement that only 40 per cent. of the accidents are caused by the human element is very low. We have adopted all the measures that Mr. Wilson recommended, such as systematic timbering, use of permissible expolsives and practically everything that anybody has suggested or can think of, and even after all that has been done, done for several years, and a systematic campaign maintained all the time to reduce accidents, we still

Jan 4, 1918

By James Gayley

The paper presented to the Institute in 1910, by H. O. Hof-man, on Recent Progress in Blast Roasting,' has called the attention of the iron industry to the adaptability of these processes to the reclamation of by-products such as flue-dust and blue billy, and the better preparation of concentrates and fine ores for use in blast-furnaces. The waste of valuable iron-ore through the production of flue-dust has increased at an enormous rate, and much of it has in

Jan 1, 1912

Terminology Relating to Nonmetallic Elements in Metals. BY T D YENSEN AND C H HERTY, JR (Tech Pub 555, Metals Tech, June 6100 words ) The paper gives arguments for confining the term "gases in metals" to its proper sphere and recommends the name "nonmetallic elements in metals" as a general title of the subject dealing with: (1) nonmetallic elements introduced into metals unintentionally or for various specific purposes; (2) phenomena occurring in metals caused by non¬metallic elements It also recommends a classification of the subject in which "gases in metals" occupies a definite, logical place

Jan 1, 1935

BUFFALO C E Moyer, Chairman (Buffalo, N Y I R M Jordan, Vice-Chairman H A Morlock, Secretary CHICAGO M E Nickel, Chairman (Chicago, Ill ) A M Kroner, Vice-Chairman W R McLain, Secretary-Treasurer

Jan 1, 1959

By John Henry Harden

WITH imperfect instruments it is impossible to make accurate surveys; the results are inaccurate maps, with their attendant consequences. The design of the writer is to describe an improved form of tripod head, and certain defects in an English transit and a miners' dial, with the method taken to remedy the defects of the transit. When the present transit superseded the surveyor's compass, there was one special objection brought against it, and with some show of reason ; namely, that the tripod of the compass with its ball and socket motion, allowed a quicker levelling-up (and, consequently, more work) than was possible with the transit. To this objection it was replied, that the ball and socket would not allow the instrument to be levelled with the same degree of precision that could be attained with the levelling screws, and that if time was sacrificed greater accuracy was attained. Nevertheless, it is a well-known fact that in this country, and especially in England, the compass or miners' dial holds its ground solely from its rapid adjustment. Ever since the introduction of the transit, efforts have been made to give to this instrument the same facility of levelling possessed by the compass or dial, and the same means have been tried, i. e., a . ball and socket motion, since a modification of this in some form was the only method that would answer. The upper part of a transit is, however, much heavier than the corresponding parts of a compass, and, therefore, requires more binding power, which cannot be ob¬tained with an ordinary ball and socket joint. It has been a study with instrument-makers to combine the facility of these two tripods -the quickness of the ball and socket with the steadiness and accuracy of the screws; but in all attempts in this direction the ball and socket of the compass has been literally followed, the entire stability of the instrument depending upon the friction of the ball in its socket. There is great need for a tripod that can be more easily manipulated than the present form, for it rarely happens that an engineer has a level surface on which to set his instrument, and very often

Jan 1, 1879

By R. B. Fuller, E. T. Casler

MANY changes were made in the methods and equipment used in the mining of pebble phosphate rock in the generation immediately preceding the present World War and it would be extremely interesting to note the improvements that will be made during the next generation. Literally, much water has gone over the dam since the days when we used local cordwood for generating steam and drying pebble phosphate rock. belt-driven centrifugal pumps operated by steam engines. and floating dipper or centrifugal dredges; when we removed overburden by small steam shovels and transported it by dinkey locomotives and six-yard cars; when washing machinery was installed on wooden structures the washers being replaced every four to six years. Those were the days when men were plentiful, and 47 different mining companies were selling their products, based on .decidedly meager information; and. like so many mining operations, little thought was given to conservation. As the importance of phosphate rock has become more prominent in the thoughts of our economists, a more intelligent approach has been made to mining problems. Vast improvements have been made in the technique and processing of the phosphate matrix and stripping of overburden, which, in turn, have brought developments in machines and equipment and a more

Jan 1, 1944

By E. S. Tankins

The main purpose of this work was to study the effect of gold on the activity coefficient of oxygen in the liquid Fe-Au alloy and to determine how copper and silver change the activity coefficient of oxygen. A preliminary investigation has been made of equilibrium in the reaction of hydrogen with oxygen in some of the liquid gold alloys. The experimental method, which has been described in detail elsewhere,' consisted of bubbling accurately known H-A-water vapor mixtures through the Fe-Au alloys contained in alumina crucibles within a vertical closed furnace. When equilibrium was reached, the samples were quenched by rapidly lowering the crucible under an atmosphere of argon to a water cooled brass fixture at the bottom of the furnace tube. The melts were found to freeze from the top in less than 4 sec. The heats were carefully prepared for oxygen analysis. The oxygen content was determined by vacuum fusion analysis.' Only high purity electrolytic materials were used in this investigation. The activity and free energy of oxygen in the liquid iron alloys were studied by means of the reaction; The data for the 80 Fe-Au alloys, obtained as a function of temperature, are summarized in Table I and presented in Fig. 1, where log is plotted against . The results can be expressed by: The data were obtained using water vapor-hydrogen ratios between 0.04 and 0.30, and a 25 pct H2-75 pct A mixture. An oxygen content between 0.030 and 0.060

Jan 1, 1970

By Charles White Merrill

Mankind's progress is measured in minerals. Man's emergence from prehistory is marked by passage through a Stone Age and a Bronze Age and into the present era, sometimes called the Iron Age or the Age of Metals. With the evolution of civilization and the development of a modem industrial economy, minerals become more and more important. Structures, roads, and machines are built largely of minerals; the energy to heat the structures and to drive the machines is mostly mineral; agricultural fertility is maintained by mineral fertilizers and water; and military strength is provided by fortresses, armaments, and munitions, largely of mineral origin. Thus in the material world, in the productivity of the economy, access to minerals has paramount importance. Every evidence indicates increasing dependence on minerals in the modem economy, particularly on the mineral fuels as energy sources to provide the power base for advancing industrialization. Both the total and the per capita consumption of almost every mineral is increasing in the industrialized nations. Moreover, nations with predominantly agrarian economies call themselves underdeveloped and universally strive to industrialize. Most mineral consumption trends in the more advanced economies have been greatly exceeding population growth-which itself has been advancing at an accelerating rate-and sometimes have surpassed the growth in real income. Some minerals have only recently been adopted or grown to importance in use. Titanium metal did not appear as a commercial product until 1948, and even coal seriously displaced wood as a source of heat less than two centuries ago. On the other hand, minerals have always played an important role in construction. The prehistoric megaliths that form the dolmens of Salisbury Plain are stone; the pyramids are andesite faced with limestone; and many other ancient structures are built of mineral materials. In modem times the whole course of architecture has been redirected by new building materials, mostly mineral. Most conspicuous is the sky-

Jan 1, 1964

By B. O. Pickard

WITH more than a score of shafts and numerous stope openings to the surface, all inter-connected underground; with underground temperatures high, often exceeding 100° wet bulb; with an ore presenting a dust health-hazard; with certain rocks giving off inert gases; with an altitude of 6000 ft. above the sea level and a dry desert climate, the Tonopah mines offered an interesting, problem to the student of metal-mine ventilation. Tonopah is not an old mining district relatively speaking. It was discovered in 1900 and Tonopah soon was a boom camp. By 1910 the mines of this district had paid many millions of dollars in dividends. At the time of the 1921 ventilation study, mining had passed its peak of production and the operators were striving to reduce costs, to discover new ore bodies, and to attract desirable workmen. In 1925, the camp was operating on a still less prosperous basis, but the several managements had not relaxed in their efforts to keep the mines on a paying basis, neither had they lost their faith in the ability of the mines and the price of the silver to "come back." Early in the fall of 1921 the Bureau of Mines was invited by the mine operators at Tonopah, Nevada, to make a detailed study of the under-ground air conditions in the Tonopah silver district. D. Harrington,? who was then directly supervising the ventilation studies of the bureau, detailed district engineer B. 0. Pickard, mining engineer E. D. Gardner, surgeon C. E. Kindall, and petrographer H. Insley to carry on the study. G. S. Rice, as chief mining engineer of the Bureau of Mines, was in general charge of the work. Upon the completion of the study each operator was furnished a report on conditions in his mine.

Jan 2, 1927

By P. A. Boeck

Discussion of the paper of P. A. BOECK, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 104, August, 1915, pp. 1539 to 1550. LAWRENCE ADDICKS, Douglas, Ariz.-It does not seem to me that the role played by carrying heat away from one surface to another has been brought out. A cellular construction prevents the motion of air currents. Also in the installation on the top of a reverberatory furnace, that Mr. Krieger mentions, where it stopped the cooling, there is besides the question of overheating. Another complex question, entirely apart from the necessity of not carrying a brick above a certain temperature, is that of not allowing acids and bases to come together at too high a temperature. J. W. BECKMAN.-What cements together the individual cells in the insulating material? Also, how does the material behave in the presence of acids and alkalies, both strong and weak? A. H. KRIEGER, New York, N. Y.-The material is formed or composed of myriads of lace-like skeleton remains of diatoms visible only -under a powerful microscope. The diatom lives in salt and fresh water. On the Pacific Coast there must have been an abundant life of the diatom, because the beds, still in existence in Southern California, are fully 1,000 ft. through, and are hard and strong, standing a pressure of more than 400 lb. per square inch. The beds must have been many ages in forming and the diatoms have become firmly packed together. The samples shown are typical of the entire deposit as it was formed at the bottom of the sea. Once this structure has been destroyed, it is impossible to reconstruct it without artificial bonding materials. With the exception

Jan 12, 1915

By William E. Ford, Edward Salisbury Dana

1. Simple Hydrocarbons. Chiefly members of the Paraffin Series C,H2,+2. SCHEERERITE. In whitish monoclinic crystals. Perhaps a polymer of marsh-gas (CHI). Found in brown coal at Uznach, Switzerland. HATCHEITITE. Mountain Tallow. In thin plates, or massive. Like soft wax. Color yellowish. Indices, 1.47-1.50. Ratio of C to H = nearly 1 : 1. From the Coal-measures near Merthyr-Tydvil in Glamorganshire, England; from Galicia. PARAFE-IN. A native crystallized paraffin has been described as occurring in cavities in basaltic lava near Paterno, Sicily. Indices, 1.49-1.52. OZOCERITE. Mineral wax in part. Like wax or spermaceti in appearance and consistency. Colorless to white when pure; often leelr-green, yellowish, brownish yellow, brown. Indices, 1.51-1'54. Essentially a paraffin, and consisting chiefly of one of the higher members of the series. Occurs in beds of coal, or associated bituminous deposits, as at Slanik, Moldavia; Roumania; Boryslaw in the Carpathians. Also occurs in southern Utah on a large scale.

Jan 1, 1922

By O. Mellgren, A. M. Gaudin, P. L. De Bruyn

The adsorption density of ethyl xanthate on pyrite was determined as a function of xanthate concentration. Surface preparation of the mineral appears to have asafunctionsome effect on the subsequent adsorption process, A monolayer of xanthate on the surface is exceeded only in presence of oxygen. The effect of OH- , HS- (and x and CN- S=)and on the amount of xanthate adsorbed was investigated. Competition between OH- and X- (xanthate) ions for specific adsorption sites is indicated over a wide pH range. IN the flotation of sulfide ores, xanthates are most commonly used to prepare the surface of the mineral to be floated so that attachment to air takes place. The quantity of agent required to make the mineral hydrophobic is usually very small, of the order of 0.1 to 0.25 lb per ton of mineral. Details of the mechanism of pyrite collection are for the most part unsettled. Adsorption of collector has long been believed to involve an ion exchange mechanism as demonstrated for galena' and for chalcocite.2 In the work on chal-cocite it was also demonstrated that a film of xanthate radicals unleachable in solvents that dissolve alkali xanthates, copper xanthate, or dixanthogen was formed at the surface of the mineral. The unleachable product increased with increasing addition of xanthate up to a maximum corresponding to an oriented monolayer of xanthate radicals. Pyrite is extremely floatable with xanthate if its surface is fresh.9 ut the floatability decreases rapidly as oxide coatings increase in abundance. Pyrite shows zero contact angle when in contact with ethyl xanthate solution at pH higher than about 10.5;4 at neutrality, a contact angle of 60" is obtained at a reagent concentration of 25 mg per liter. Alkali sulfides and cyanides are pyrite depressants. In this study of pyrite collection the writers have sought to relate measured xanthate adsorption to the method used in preparing pyrite, to the presence or absence of oxygen, to concentration of hydroxyl, hydrosulfide, sulfide, and cyanide ions. The principal experimental tool has been radioanalysis," " using xanthatcx marked with sulfur 35. Experimental Materials Pyrite: Unlike most sulfides, pyrite is a poly-sulfide. The structure given by Bragg7 resembles that of sodium chloride, the iron atoms corresponding to the position of sodium and pairs of sulfur atoms corresponding to the position of chlorine. The edge of the unit cell in pyrite is 5.40 A and in halite 5.63 A. The S-S distance in pyrite is 2.10 A; the Fe-S distance, 3.50 A: and the Fe-Fe distance, 3.82 A. Natural pyrite from Park City, Utah, was used in this investigation. Pyrite 1 was obtained by hand picking pure crystals. Pyrite 2 and Pyrite 3 were obtained from finer textured crystalline material containing inclusions of silicates. The same cleaning technique was utilized for the preparation of Pyrite 2 and Pyrite 3, whereas a different cleaning technique was used for Pyrite 1. Pyrite 1 was prepared as follows: The crystals were ground in a porcelain ball mill and the 200/400 mesh fraction was separated by wet screening with distilled water, followed by washing for 1 hr with deoxygenated distilled water acidified with sulfuric acid to pH 1.5. The acid was removed by rinsing with deoxygenated distilled water on a filter until a pH of 6.0 was reached in the effluent. This filtration was carried out under nitrogen. The sample was then dried in a desiccator under nitrogen. The period of time for which this pyrite sample was in contact with water containing oxygen was about 4 hr. The specific surface as determined by the BET gas adsorption method was 582 cm2 per g. Final material assayed 53.12 pct sulfur and 46.5 pct iron (theoretical, for FeS,: S, 53.45 pct; Fe, 46.55 pct). After crushing, Pyrite 2 and Pyrite 3 were washed with 1 M HCl. rinsed, and fed to a laboratory shakinq table to remove the small amount of silicates. The concentrate obtained was ground in a laboratory steel ball mill. The 200/400 mesh fraction was separated by classification in a Richards hindered settling tube. This fraction was then given a final wash with 0.1 M HCl and deoxygenated water was filtered through the sample. The final effluent showed a conductivity equivalent to that of a solution having a salt concentration of 0.3 ppm. Aqueous hydrogen sulfide solution was then added to the sampln (about 100 ml saturated H,S solution to about 1000 g pyrite under a few hundred milliliters of water) which was stored wet under nitrogen. The sample stored in this manner showed no indication of formation of iron oxides, whereas iron oxides appeared

Jan 1, 1957

By Willard L. Hunter

Four solvent extraction systems were studied to determine their efficiency jor extraction and separation of tantalum and columbium. Aqueous feed solutions of varying HF-HCl concentrations and metal content were contacted with equal volumes of cyclohexanone, 3-methyl-2-butanone, and 2-pentanone and solutions of varying HF-H2S04 concentrations were contacted with equal volumes of 2-pentanone. One multistage continuous test was made in a polyethylene pulse column using cy clohexanone as the organic phase. In each system studied, columbium and tantalum purities in excess of 95 pct with respect to each other were obtained in single-stage tests at low acidities in the feed solution. Separation factors ranging from 1700 to 2400 were obtained when rising HF-HCl mixtures in the aqueous phase. Best results were obtained when a solution of HF-H2S04 was used as the aqueous phase and 2-pentanone as the organic phase. A separation factor in excess of 6000 was obtained in one stage with aqueous solution concentrations of 2 _N HF and 2N H2S0,. When acid concentrations were increaszd to 52 HF and 10 _N H2S0,, 99.9 pct of the tantalum and 98.2 pct of the columbium initially present in the feed solution were transferred to the organic phase. The separation of columnbium and tantalum obtainable by means of the solvent extraction systems presented in this paper was found to corn -pare favorably with other systems, including the HF-H2SO4-methyl isobutyl ketone system currently used by most producers for the extraction and separation of these metals. TANTALUM and columbium are always found together in minerals of commercial significance, although the proportion of the two metals in ores varies within broad limits. Columbium is estimated to be 13 times more abundant than tantalum. Five methods generally employed for the separat:ion of these metals are: 1) fractional crystallization (the Marignac process),2 2) solvent separation, 3) fractional distillation of their chlorides, 4) ion exchange, and 5) selective reduction. Of these methods, the one currently used by industry to the greatest extent is that of solvent separation. One of the early technical developments in solvent separation of tantalum from columbium was reported by the Bureau of Mines: the HF-HC1-methyl isobutyl ketone system; data were presented for both laboratory and pilot-plant experimentation.3 Of twenty-eight organic solvents tested for their ability to extract tantalum from an HF-HC1 solution of columbium and tantalum, 3-pentanone (diethyl ke-tone), cyclohexanone, 2-pentanone, and 3-methyl-2-butanone were chosen for further study. Data on the HF-HC1-diethyl ketone system has been published4 and data describing the use of cy clohexanone, 2-pentanone, and 3-methyl-2-butanone as the organic phase are included in this report. RAW MATERIAL The source of tantalum and columbium oxides for this study was ('Geomines" tin slag from the Manono Smelter, Cie Geomines, Gelges, S.A., Congo. In order to extract the valuable Ta-Cb content, the slags were carbided, chlorinated, and the sublimate from chlo-rination was hydrolized and washed free of chloride with water. The washed material was air-dried and stored in a stoppered container. Throughout the paper, "feed material" refers to this mixture of hydrated oxides which was employed because of its high solubility in aqueous solutions. Typical analysis of the hydrated oxides is shown in Table I. I) HF-HC1-CYCLOHEXANONE SYSTEM Batch Separation. Effect of Acid Concentration. To determine the effect of varying the acid concentration upon the transfer of tantalum and columbium, a series of tests was made in which approximately 2.5 g of feed material was added to 25 ml solutions of 2, 4, 6, 8, and 10 N HF and 0 through 5 N HC1. Tantalum pentoxide concentration of the solu%ons was approximately 21 g per liter and columbium pentoxide was 14 g per liter. These starting solutions were shaken with equal volumes of cyclohexanone in 100 ml polyethylene bottles for 30 min. The phases were carefully separated in 125 ml glass separatory funnels. The time of contact of the solutions with the separatory funnels was kept at a minimum to reduce silica contamination. The measured phases were separated into 400 ml polyethylene beakers and the metal contents of each were precipitated by addition of an excess of ammonium hydroxide. Precipitate from each phase was filtered on ashless filter paper, ignited at 800" to 1000°C for 45 min, weighed, and analyzed by X-ray fluorescence.5 Data tabulated in Table I1 and illustrated in Fig. 1, show that maximum separation of tantalum from columbium for each HF concentration was obtained with no HCl present. The purest tantalum product was obtained with some HCl present. The highest separation factor was obtained at 2 N HF and

Jan 1, 1970