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With the inauguration of Petroleum Technology this year, and approval by the Board to add an Assistant Secretary to the New York staff to serve the Petroleum and Coal Divisions, the Petroleum Division looks forward to greater opportunities and responsibilities. An improved medium of publication offers further incentive to engineers and investigators in the oil industry to make contributions. The authorization by the Board of Directors of a new Assistant Secretary is an appreciation of the splendid contributions made to the industry by the open forum of the Petroleum Division. It is also a recognition of the possibilities of greater service to the membership along the lines established ten to fifteen years ago by DeGolyer, Fohs, Ambrose and Lovejoy, to mention a few leaders. It isexpected that the new officer will spend a substantial part of his time in the field, visiting the student sections, the respective Divisions, helping in the arrangement of papers and Section meetings and intensifying interest in the Institute. The Petroleum Division will hold three meetings this year. The Fall Meetings will be held on Oct. 6 and 7 in San Antonio and on Oct. 20 and 21 in Los Angeles. The programs for these meetings will deal chiefly with engineering research and production engineering problems. Papers on production statistics and general economics of the industry are reserved for the Annual Meeting in New York. The annual production symposium and statistics are accepted as standard for the industry. With continuously deeper penetration into the earth in search for and exploitation of petroleum, it is necessary to have a better understanding of reservoir conditions and to place more phases of the operation under engineering control. Among the subjects relating to reservoir conditions tha thave been proposed for the fall meeting programs are phase equilibria at high pressures, interfacial tension between oil and water, the flow of oil and water through sands, the chemistry of films and underground temperatures. Investigations relating to control of operations include methods of continuously logging while drilling both visually and electrically, methods of studying drilling samples, properties of drilling fluids, improved cementing practices for isolating thin sands under high-temperature conditions and gas conservation, particularly production from high-pressure reservoirs. Additional suggestions of general themes or individual subjects will be welcomed, since it is desirable to build a backlog of material for Petroleum Technology. 9

Jan 1, 1938

By Warren L. Howes

LITERALLY hundreds of designs of mill liners are in use in current grinding operations, varying in contour from smooth to the roughest of surfaces, and in materials from scrap rail to alloy steels. A certain amount of variation in materials can be expected, owing to differences in local market conditions and the character of ores. However, when one attempts to rationalize the designs in current operations of a parallel nature, there is little that can be called standard practice. Designs and opinions of designs are as divergent as day and night. Somewhere in this maze there must be clues to better practice. The purpose of this paper is to examine the factors for consideration in liner design, and to propose a vigorous campaign of exploration in this phase of grinding operations. The paramount considerations in the choice of mill liners for a grinding operation are: (I) durability, in view of the cost, and (2) developed grinding capacity. Because of the strategic nature of grinding circuits in controlling the production of most mining operations,1 grinding capacity usually is the greater consideration. GRINDING CAPACITY Mill liners affect grinding capacity in two ways: (I) by establishing dead space within a mill shell, which could be usefully occupied by live grinding media, and (2) by controlling the grinding action of the media. The extent to which liner thickness affects the potential volume of live grinding media, and thereby the grinding capacity, is shown in Table I. In a ball mill 7 ft. in diameter, for example, an inch of liner thickness reduces ball volume and corresponding grinding capacity by 5 per cent. With grinding capacity at a premium, this makes consideration something more than first cost of liner materials. A low-cost, voluminous material, made extra thick to secure adequate life, can be very expensive in terms of grinding capacity. On the other hand, in increased grinding capacity, a long-wearing material in a thinner pattern can save many times its value. [ ] From the standpoint of mechanics, the function of mill liners is to provide the means of driving or tumbling the load of grinding media. In this respect, an internal-spur gear-and-pinion assembly resembles a rotating mill shell with its contained load of grinding media, the mill-shell liners

Jan 1, 1945

By V 7. 0 / 300 dpi

WHEN the copper smelters were built, in Montana, all of the refractory products which were used in their construction were shipped in from Eastern factories. It was apparent that if a material suitable for the manufacture of these products could be found within the State, a saving of freight could be effected and a new industry built up. Prospecting for such materials was started and experiments were made with samples from numerous deposits. Considerable effort and funds were expended in an attempt to manufacture silica brick from Dillon quartz, a light colored sandstone that is found near Dillon, Mont., on the Oregon Shortline railroad. As a brick material the Dillon quartz was a failure, but it has proved very satisfactory as a silica cement. It is now being used in laying silica brick and for reverberatory furnace bottoms. A bed of quartzite that is particularly suited to the manufacture of high-grade silica brick -was finally discovered at Browns Spur, 6 miles west of Anaconda. The material from this deposit is now being used in the manufacture of the Anaconda silica brick, which have gained a wide reputation for heat-resisting and lasting qualities. The analysis of all average sample of this quartz is: SiO2,, 96.7; Fe203, 0.3; Al203, 2.5; CaO, 0.3 per cent. The very low percentage of fluxing ingredients makes this a most refractory material. All of the Anaconda silica brick are hand molded. Various types of brick machines have been tried, but the hand-mold process proved the best suited to the manufacture of silica brick from this material. The silica is first put through a jaw crusher and is then clumped into wet pans, where 4 per cent. of lime paste is added, to produce a bond. Without the lime the. material would not be plastic enough to mold. After a few minutes' grinding in the wet pans the material is conveyed to the molder, who forces it into the molds by hand. The brick are then dumped on pallets and placed in the drier, where they are left until dry enough to be set in the kilns. Some of the brick are re-pressed before being dried. They are burned about five days, in round down-draft kilns. It is not necessary to have as much heat in the kilns as the brick will be subjected

Jan 9, 1913

El Indio, eighty percent -owned by Compania Minera an Jose Inc., a subsidiary of St. Joe Minerals, and twenty percent-owned by private Chilean investors, will open their new flotation and Carbon -In -Pulp plant near La Serena, 480 km (300 miles) north of Santiago, Chile, in early 1981. The underground mine, at an altitude of 4,270 m (14,000 ft), will produce about 1,270 mt per day (1,400 st per day) of ore containing about 2. 2570 Cu, and gold and silver to the extent of 16 and 254 g per mt (0.47 and 7.4 oz per st) respectively. While construction of the plant was underway, development ore, containing some 1,400 kg (45,000 oz) of gold, was shipped to the United States for recovery in a copper smelter. At El Indio the underground ore is rail-hauled to the mill a short distance from the portal where it is crushed, ground, and floated to produce a copper concentrate containing both gold and silver. The crushing plant also crushes waste for use as mine backfill. Approximately 92% of the copper and 60% of the gold and silver are recovered in the flotation concentrate. Flotation tailings, at a grade of 19 g Au and 116 g Ag per mt (3.4 oz Au and 0.55 oz Ag per st), are cyanided for 72 hours in six Pachucas with auxiliary air lifts for pulp transfer. Lime, cyanide, lead nitrate, and a phosphate are also fed to the cyanidation Pachucas. After cyanidation, the pulp is treated in four air lift Carbon-In-Pulp tanks equipped with external vibrating screens for carbon advance. Loaded carbon is stripped in two pressure vessels in parallel. Pressure stripping must be used because of the high altitude. Stripped carbon is dewatered in a spiral classifier before being reactivated in a rotary kiln and returned to the C. I. P. circuit. Pregnant solution is then sent to four banks of four Zadra cells for gold and silver recovery on steel wool. Zadra cell cathodes.are washed with the slimes being captured in a plate and frame filter. The filter cake and the washed cathodes are then dried on an infrared dryer and smelted in two stages to bullion bars. Published reports indicate that the total investment for this unique operation was in the neighborhood of $80 million.

Jan 1, 1981

By Willard Jillson

WITHIN the last ten years Kentucky has become celebrated for its low-sulfur bituminous coals. Prior to this time, many investigators had discovered the abundance of this coal but the fact was unknown to the general public until the last extension of Kentucky's mountain railroads was completed. The coals of Kentucky are, broadly, separated into two geographic units-the eastern and the western coal fields. On a basis of their sulfur content these coal fields fall into three units, which are indicated on the accompanying map, by numbers, 1, 2, and 3. The area marked 1, the very southeastern part of the State, shows the lowest sulfur, all coals being averaged. In this field the maximum is 1.04 per cent. and the minimum as low as 0.68 per cent.-both averages and not individual analyses, which would of course show much greater variation. Included in this group are the following counties: Lawrence, 0.87 per cent.; Martin, 0.75 per cent.; Johnson, 0.73 per cent.; Magoffin, 0.S7 per cent.; Floyd, 0.88 per cent.; Pike, 0.68 per cent.; Knott, 1.04 per cent.; Perry, 0.77 per cent.; Letcher, 0.80 per cent.; Leslie, 0.70 per cent.; Harlan, 0.79 per cent.; Knox, 0.86 per cent.; and Bell, 0.92 per cent. The total average sulfur content for these thirteen counties is 0.82 per cent. Bordering the restricted low-sulfur field of eastern Kentucky is the No. 2 belt (slightly darker), which is commonly known as the western border of the eastern coal field. Here the maximum sulfur is 2.91 per cent. and the minimum 1.05 per cent. Again these are averages and not individual analyses. The counties in this group are: Greenup, 2.60 per cent.; Boyd, 1.67 per cent.; Carter, 1.07 per cent.; Morgan, 1.40 per cent.; Wolfe, 1.83 per cent.; Lee, 2.93 per cent.; Breathitt, 1.85. per cent.; Owsley, 1.09 per cent.; Jackson, 1.06 per cent.; Rockcastle, 2.30 per cent.; Clay, 1.09 per cent.; Laurel, 1.08 per cent.; Pulaski, 2.24 per cent.; Whitley, 1.05 per cent.; McCreary, 1.50 per cent.; and Wayne. The sulfur percentage average for this area including fifteen important counties is 1.65 per cent.

Jan 9, 1919

By Joseph E. Pogue, F. G. Coqueron

Prior to 1934, published information covering expenditures by oil companies for properties, plant, and equipment and the residual investments in the various segments of the petroleum industry was not readily available. This paper presents an analysis of the funds invested by a selected group of oil companies during the years 1934 through 1942, based on an extensive study of the individual records of 30 oil companies. The sources, disposition, and characteristics of the capital employed by this group of companies are traced through a series of combined statements and appropriate charts, covering financial and operating data. The analysis of these statements not only constitutes a record useful for comparative purposes but also serves as a basis for a number of broad conclusions, as follows: 1. The petroleum industry generates the capital needed for its expansion almost entirely from its own operations and is therefore a singularly self-contained economic unit. 2. The long-term debt contained in the financial structure of the industry is small relative to the total capital employed, is less than the net working capital, and has increased but slightly during the period under review. 3. The capital expenditures of the group of 30 oil companies for 9 years amounted to 6.1 billion dollars, 58.3 per cent of which went into crude-oil producing facilities. The trend of this segment of expenditures has been downward since 1937. In 1942, expenditures for refining facilities increased sharply and for marketing facilities declined drastically. 4. The net working capital of the group increased 380 million dollars over the period, and the industry is in a favorable position of liquidity. The ratio of combined current assets to current liabilities was 3.21 at the close of the period. 5. The net income of the group displayed an upward trend for the period but with rather sharp cyclical fluctuations. 6. In 1942, Government funds entered the industry for the first time in substantial amounts and were utilized for the provision of war facilities needed for emergency use. 7. The group has paid out a relatively low percentage of net income in the form of dividends. For the period the average was 55 per cent of net income. 8. The rate of return on invested capital for the group averaged 6.4 per cent for the

Jan 1, 1944

Following the usual custom, three meetings are planned for the year. The Mid-Continent meeting will be held at Oklahoma City, Okla., Oct. 7 and 8, and the California meeting is planned for Los Angeles, probably also early in October. A program along the usual lines is under way for the annual New York meeting. Discussion and planning of the year's activity started in March. An effort is under way to secure papers dealing with some overlapping phases of engineering, petroleum geology, geophysics, law, economics, refining, etc. The main reason for attempting a program along these lines is the belief that unusually interesting technical papers can be obtained. The degree of specialization in the technical and related fields has permitted but few individuals to develop a sufficiently comprehensive viewpoint. Also, at times the developments in a particular field are capable of giving great stimulus toward much needed solutions of difficult problems in others fields of activity. With the coming of the period of restriction of production to market demand, many changes have occurred in policy and technique of petroleum production. Some changes have been advances, others have been of retrograde nature. It seems doubtful whether the adjustment to the condition of excess producing capacity has been complete or sound in some major respects. Many changes are in progress and others need to be initiated. The industry has excessive producing capacity so far as immediate market demand is concerned, but reserves for several years hence are generally believed insufficient. Exploration and discovery should go forward but development should proceed with caution and under control. Property rights should be clarified and protected for the new condition— without excessive cost for drilling wells that serve no purpose except that of giving some protection to property rights at the cost of an increased price to the consumer. Under the more steady condition of assured supply for the immediate future, as compared to the hand-to-mouth condition of wide-open production, a greatly advanced technique of development and production is possible and is being developed. Great progress has been made, but much remains to be done. Along some important lines progress can be effected only by better understanding between the engineer and the geologist, the lawyer, the politician, the geophysicist, etc. There is need

Jan 1, 1937

By H. W. Reid

One of the outstanding features of the year was a further marked decline in the footage drilled. This is estimated at 169,000 ft., as against 218,000 ft. for the previous year, and 372,500 ft. in 1930. Owing to repair work and improved production methods, there was an increase of about 4.25 per cent in the amount of oil won, the production being estimated at 10,160,000 bbl., or an increase of 400,000 bbl. over 1931 and nearly 750,000 bbl. more than in 1930. (See Table 1.) At the end of November there were 28 rigs in operation. During the first 11 months of the year 54 new wells were started; the average depth of those completed was 2476 feet. Owing to the continued restriction of drilling programs there has been little of outstanding interest in the way of new plant or technique. The use of the acid bottle, for testing the verticality of wells while drilling, has increased considerably, and this is now in use in practically every well except the very shallowest. During the last six months of the year fairly extensive use has been made of electrical coring. The number of wells started in the Colony up to the end of November, 1932, was 1894. The average number of producing wells during the year was 789, or 41.7 per cent of the total. Of these, 214 were flowing wells, 473 pumping, 80 bailing or swabbing, and 22 were produced by air or gas-lift. Although the last category represents less than 3 per cent of the total, there has been a marked increase in the use of air or gas-lift as compared with 1931. During the year there were 16 companies engaged in producing oil, as compared with 14 in the two previous years. In addition to one small refinery which started to operate at the beginning of the year, the five existing refineries worked continuously. At the latter very little has taken place in the way of extensions, except at one in the Parry Lands—Pitch Lake—Point Fortin area, where extensive alterations and additions are in progress, including the building of a deep-water pipe-line pier. When this is completed there will be five loading terminals, all situated in the sheltered Gulf of Paria, or west, coast, capable of accommodating ocean-going tank steamers. There

Jan 1, 1933

By B. C. Craft

Oil and gas development in Mississippi during the year 1933 was rather active and a number of important wildcat wells were drilled throughout the state. Mississippi showed an increase in drilling operations during 1933. There were 58 completions from 22 counties during this period, compared with 53 completions in 10 counties during 1932. The Jackson gas field in Hinds and Rankin counties continued to be the most active area with 26 completions, resulting in 17 gas wells, 2 oil wells, and 7 dry holes, compared with 38 gas wells, 1 oil well and 5 dry holes during 1932. A further attempt to extend the producing limits of the Amory gas field resulted in a dry hole. Extensive exploration in south Mississippi has proved the existence of ample source beds and presence of an extensive sandbody near the top of Cockfield. Core tests, supplemented by extensive geophysical work, have been carried on in Jackson, George, Harrison, Pearl River and Stone counties. Exploration will be continued in 1934. The most important deep test drilled in 1933, and the deepest well ever drilled in a southeastern state, was the Eastman Gardner et al., Bank of Seminary No. 1, sec. 26-8N.-15W., Covington County. This well went through about 1300 ft. of Selma chalk, and was abandoned in the Eutaw at 8004 ft. Another interesting operation during the past year was the Foster Creek Oil Corporation's Foster Creek Lumber Co. No. 1, sec. 14-2N.-2W., in the "Eastern Conroe Trend." This test is shut down at 3687 ft. in the Catahoula sandstone and has not encountered any important shows of oil or gas. A total of 107 of the 117 gas wells completed in the Jackson gas field since its discovery in 1930 are still producing, and have a combined open flow of approximately 3,724,896,000 cu. ft. It is reasonable to assume that this area will be rather inactive during 1934 as the maximum daily production during 1933 was 3,476,000 cu. ft. The 10 wells that have gone dead were edge wells. The water level is now between the sub-sea depths of 2190 and 2195 ft. The Gulf Refining Company's Rainey No. 1, sec. 13-5N.-lE., one of the early wells in the field, had gas and water at —2225 ft. That the field is under hydraulic control is

Jan 1, 1934

By L. O. Howard

WHAT was perhaps the first attempt at basic converting in the Southwest was made by the late Charles F. Shelby at Cananea early in 1907, when he removed the acid lining from one of the 8 by 12-ft. barrel-type converters then in use at the reduction works of the Cananea Consolidated Copper Co. and substituted a lining of one course of magnesite brick. In this shell, he blew 21 taps (about 180 tons) of matte to white metal before the brick gave out along the tuyère line. In every case, the white metal so made was transferred and blown to copper in other converters. The cost of the lining was $700 and Mr. Shelby gave up the experiment as impracticable. No further serious effort to bessemerize copper mattes in a vessel having a more or less permanent lining of basic brick was made by any of the large copper smelters in the Southwest until some months after Messrs. Peirce and Smith had brought the question permanently before the public, and had proved it to be a metallurgical and financial success by their work at Baltimore and Garfield. Early in 1911, the Cananea Consolidated Copper Co. had in operation at its reduction works at Cananea, Mex., several 8 by 12-ft. barrel-type converters lined with magnesite brick which had previously been operating with acid linings. In the 18 months following, these converters produced 50,000 tons of copper. In June, 1912, this company installed the first of its new equipment of six stands of electrically operated 12-ft. Great Falls type converters, and shortly afterward discontinued the use of the smaller shells. In September, 1911, the Consolidated Kansas City Smelting & Refining Co. had installed at its El Paso plant two 10 by 26-ft. Peirce-Smith converters. Later, in March, 1913, one standard Great Falls type converter was added. .About the time the Peirce-Smith converters were going in at El Paso, the Calumet & Arizona Mining Co. was experimenting with basic linings in 7-ft. by 10-ft. 6-in. barrel converters at its plant in Douglas, Ariz. These efforts were sufficiently successful to enable the plant to handle the total output of copper in these small shells until the standard. Great Falls converters were substituted in June, 1914.

Jan 9, 1916

By H. G. Botset

A KNOWLEDGE of the water content of producing sands is becoming of increasing importance to the petroleum industry. It is now a generally accepted fact that practically all oil sands contain some free water. Recent experiments1 have shown that an appreciable fraction of the pore space of a sand may be filled with water while oil production from this sand is water-free. Crowther and Haines,2 in experiments on electro-endosmosis in soils, reported that there was no endosmotic flow of water when the moisture content of the soil was 14 per cent or less, indicating that the moisture content of the soil below 14 per cent was held by dif-ferent forces than the water content above this value. This result is confirmed qualitatively by Dunlap,1 who found that "as the volume of water in the voids exceeds approximately 15 per cent of the pore volume, the permeability of the core to kerosene is markedly reduced." The author3 has also found in other experiments that the gas flow through a water-saturated sand reaches essentially 100 per cent when the pores of the sand still contain from 10 to 15 per cent water. The velocities of the flowing fluid in the experiments cited were comparatively high, so that in practice one may expect, at lower fluid velocities, an even higher moisture content of the sands with water-free oil or gas production. Thus a knowledge of the water content of oil-field sands becomes of con-siderable importance in estimating petroleum and gas reserves, and effi-ciency of fluid recoveries from depleted reservoirs. Rapid and reasonably accurate methods of measuring the water content of sand cores have not been described so far in any literature that has come to our attention.4 The method described below is devel-oped from methods that have been used for some time to measure the water content of alcohols.5,6,7 It is an application of the fact that in the presence of certain organic liquids such as kerosene, carbon tetrachloride, xylol, etc., water and alcohol are only partly miscible. This relation-ship has been used for some time in the study of gasoline-alcohol mixtures where the presence of small quantities of water affect the solubility of

Jan 1, 1938

By John J. Stokes

Literature on the electrolysis of aluminum from cryolite melts and on the structure of these .melts is surveyed critically. Data on density, freezing point, and other properties are reviewed. Theories of the electrolysis are examined in the light of these data. Two theories are presented which account equally well for the observations. In the early days, the process was thought of as a simple one. The actual mechanisms must be tremendously more complex. This paper is devoted to a rather narrow part of the whole subject, namely, what ions are present in the bath, and by what mechanism the current is carried. Using cryoscopic data, Rolin has determined the following composition for molten cryolite. Na2,AlF 3Na + 3F + AlF [1] He postulates the following equation for the ioniza-tion of alumina at low concentrations Al2O3 Al + AlO2 +O. [2] At concentrations above 0.025M he supposes the ionization of alumina to proceed as follows Al2O3 AlO + AlO2. [3] Rolin's mechanism of electrolysis for the more concentrated solution in Eq. 3 is as follows. The AlO' ion migrates to the cathode. where it is dis- charged, giving metallic aluminum and 0' ions which migrate to the anode. The AlO2- ion migrates to the anode, where it is discharged, giving Al ions and oxygen which reacts with carbon to form CO2 In the case of the extremely dilute solution in Eq. 2 the Al ion migrates to the cathode and the AlO2-and 0 migrate to the anode as before. Another possible mechanism for the electrolysis follows. Ionization of Cryolite Na3AlF4 = 2Na + 2F + NaAlF, Na + AlF-AlF+Na + F [4] Addition of Alumina 2Na2AlF+ 2AL2O4 6Na + 3A12O3F4 [5a] Al2O2F 2AlOF2 [5b] Cathode Process AlF, + 3e+ 4F + Al. [6] Anode Process AlOF2 + 2F AlF1 + 1/20, + 2e or A12O2F + 4F-2A1F; + 0, + 4e. [7] Although both Rolin's and the present mechanism of the Hall process may be qualitatively satisfactory, present data are not adequate for quantitative tests of the theories.

Jan 1, 1959

The Similkameen mine is located about 100 miles east of Vancouver, British Columbia, and ten miles west of Princeton, where the mine personnel live. Princeton was the first town in the British Columbia interior, originally the home of Cree and Blackfoot Indians and later settled by men of the Hudson's Bay Company, miners, cattlemen, and others looking for gold. After gold, there were coal mines and then copper mines . The Granby Consolidated Mining Company, Limited, operated the Copper Mountain ore bodies from 1926 to 1930 and from 1937 to 1957, mining 34 million tons of about 170 copper ore, mainly from underground. In 1966, Newmont Mining Corporation acquired the Ingerbelle property on the west side of the Similkameen River. Newmont then purchased the assets of Granby and formed Similkameen Mining Company to develop and operate the Ingerbelle and Copper Mountain ore bodies on both sides of the Similkameen River canyon. The Ingerbelle and Copper Mountain ore bodies lie within rocks composed of andesite tuffs, agglomerates, and argillites. Chalcopyrite mineralization occurs as a dissemination. Original ore reserves were estimated at approximately 75 million tons grading 0.52% copper. Mining is carried out on a three-shift, seven-day-week schedule at a rate of about 60,000 tons of ore and waste per day with four 10 cu yd P & H 1900 shovels which mine and load a fleet of 100-ton Lectra Haul trucks. Among the unique features of the design and construction of the Similkameen project was the construction of 4. 5 miles (7. 24 km) of new Trans-Provincial No. 3 highway by the company to the specifications of the British Columbia Department of Highways. The old highway traversed the Ingerbelle pit area. Along the relocated highway is a 4, 000 ft (1219 m) long berm which conceals the mine pit. This area has been replanted and now looks like the original forest scenery. Another interesting feature is that the tailings from the concentrator flow by gravity over a 1000 ft (34% m) suspension bridge, which crosses the Similkameen River canyon then passes through a tunnel to the dam site, a distance of 59,000 ft (17,980 m) to the cyclone station. When the Copper Mountain ore bodies are mined, the ore will be transported by belt conveyor on a second suspension bridge across the canyon to the Ingerbelle concentrator. After being loaded by the shovels into the 100-ton trucks, the ore is

Jan 1, 1978

By E. P. Hindes

The total amount of oil produced in the state of Oklahoma during the year 1928 was 242,286,400 bbl., as compared to 273,372,650 bbl. in 1927; 177,650,000 bbl. in 1926; and 167,900,000 bbl. in 1925. The year 1928 ranks second to 1927 in which more oil was produced in the state than in any previous year. The large in in 1927 and 1928 was due principally to the development of the Greater Seminole district. The decrease of approximately 31,000,000 bbl. in the 1928 production as compared with the production in 1927, was caused by a drop of nearly 8,500,000 bbl. in the Seminole district production and a more or less normal decline in the production of practically all the other older and more settled fields. During 1928 approximately 1800 producing wells were drilled in Oklahoma, which yielded during the year approximately 90,000,000 bbl. of oil. The average initial production of these wells was 850 bbl. per day, and the average daily production per well for the year was 137 bbl. The average daily production per well of the total number of wells producing in 1928 was 10.9 bbl., which is a 13.5 per cent. decrease from the 1927 average of 12.6 barrels. At the close of 1928 a total of 95,400 producing wells had been drilled in the state, and approximately 61,000 were still producing. The grand total amount of oil produced in the state from the time the first well was drilled up to and including 1928 was 2,553,000,000 bbl. The production in 1928 was 9.5 per cent. of the total oil produced in the state. Texas led all other states in 1928, with a production of 251,835,200 bbl. Oklahoma was second with 242,286,400 bbl., and California was third with 231,982,600 barrels. Fields outside Greater. Seminole District Practically all the old settled fields in Oklahoma experienced a normal and expected decline during the year 1928. The fields showing the most, pronounced decline as compared to 1927 were: Burbank, which dropped from 15,230,400 to 11,939, 150 bbl.; Tonkawa, from 7,692,000 to 4,952,900 bbl.; Garber, from 5,056,300 to 3,139,400 bbl., and Wewoka, from 6,188,-800 to 2,450,400 bbl. There were no new extensions, discoveries of

Jan 1, 1929

By R. F. Domagala, M. Hansen, D. J. McPherson

Iodide zirconium was combined with calculated amounts of nitrided zirconium sponge and arc melted to prepare alloys in the 0 to 6 wt pct N region. Annealing treatments were carried out at 21 temperature levels. Metallographic examination of the heat-treated specimens permitted construction of the binary phase diagram from 0 to 6 pct N. Features of the diagram include the peritectic formation of both a and ß solid solutions. The maximum solubility of nitrogen is 0.8 pct in 8 zirconium and 4.8 pct in a zirconium. An X-ray study of nitrided materials was made in the range 6 to 13 wt pct N region because serious nitrogen losses were experienced when attempts were made to arc melt these high nitrogen alloys. PHASE relationships in the Zr-N system have been determined. Due to the inability to retain nitrogen in nitrogen-rich alloys subjected to arc melting, definitive work was possible only in the range 0 to 6 wt pct (0 to 30 atomic pct) N. Sufficient complementary X-ray work was done to permit construction of the binary phase diagram up to 13.3 wt pct (50 atomic pct) N (ZrN). Small ingots were prepared by arc melting master alloys with enough zirconium to produce an alloy of the desired composition. Following pretreatment, alloys were annealed at temperature levels between 600" and 2020°C. Determination of the phase boundaries was then accomplished by metallographic evaluation of specimens quenched from the various temperatures. Incipient melting techniques were used to corroborate solidus curves, and X-ray diffraction was employed to study the nitrogen-rich region of the a + ZrN phase field. Materials Westinghouse Grade 1 iodide zirconium crystal bar served as the base material for this investigation. The as-received bars were lightly sandblasted, pickled in a 20 pct HN0-5 pct HF aqueous solution, rinsed in water and acetone, and dried. They were rolled to about 1/32 in. strip and acid-pickled, followed by water and then acetone rinses. The material was sheared to approximately 1/4 in. squares, cleaned with acetone, and stored for use. Pure zirconium nitride is not commercially available, according to correspondence with possible suppliers. A literature survey indicated that nitrogen may be introduced into zirconium metal by passing nitrogen or ammonia gas over zirconium at an elevated temperature. After considerable experimentation, a train was devised whereby high quality nitrogen was passed through a series of bubblers to remove the last traces of oxygen, through an H,SO, bubbler and a cold trap to remove moisture, and finally over zirconium within a resistance furnace. Hand-picked Bureau of Mines magnesium-reduced zirconium sponge proved more amenable to nitriding than the crystal bar. The nitrogen used was extra pure gas purchased from Linde Air Products Co. The first two bubblers through which the gas was passed contained a solution suggested by L. F. Fieser" as being ideal for removing the last traces of oxygen from nitrogen. The solution contains 20 g KOH, 2 g sodium-anthraquinone ,9-sulphonate, and 15 g NaHSO, dissolved in 100 ml water. It is blood-red and turns brown when contaminated with oxygen. A saturated lead acetate solution, next in the series of bubblers, removed any H2S which might have formed in the 0, removal stage. An H,SO, bubbler and cold trap removed moisture before the nitrogen was passed over the zirconium. The zirconium was contained in a stainless steel screen within a Vycor or quartz tube in a resistance furnace. Unreacted nitrogen passed out of the system through a mercury bubbler. A nitriding run was performed in the following manner: Zirconium was placed in the screen within the furnace tube. The unit was assembled, suitably clamped off, and evacuated to remove the air and moisture within the tube and that trapped by the zirconium sponge. The unit was flushed with nitrogen and evacuated twice. After nitrogen was allowed to pass over the zirconium for about 30 min, the furnace was turned on; several hours were required to reach temperature. The reaction was allowed to continue at temperature for about 4 hr and the screen was then withdrawn from the hot zone of the furnace by means of a Nichrome or Kanthal rod. The screen and its contents were allowed to cool at the end of the tube and were then removed. At 800°C no more than about 5 pct N could be introduced into the sponge zirconium. This material was designated M-1 (master alloy No. 1) and reserved for the preparation of alloys in the dilute nitrogen region. A second set of experiments was conducted at 1000°C; no more than 7.2 pct N could be introduced into the zirconium at this temperature. Enough material (M-2) of this nitrogen content was prepared to produce a second set of alloys to complement the first and to provide alloys in the 0 to 6 wt pct N range. It was hoped that a diffusion anneal plus a re-nitriding might yield a material of higher nitrogen content. The material containing about 7 pct N was therefore given a homogenization treatment at 1000°C for 6 hr under an argon atmosphere. It was

Jan 1, 1957

By D. J. Schmatz, H. I. Aaronson, H. A. Domian

Diffusion kinetics in disordered hcp Cd-Mg alloys have been investigated by means of the Kirkendall effect and concentration-penetration curves determined with an electron-microprobe analyzer. Self-diffusion coefficients of both species were determined at the three marker compositions obtained, averaging 27.6, 46. 7, and 78.1 at. pct Mg, by means of the Darken analysis. These coefficients were then corrected for the unequal and concentration-dependent partial molar volumes of the two elements with the Balluffi analysis, and for the vacancy flux effect by the Manning analysis. The latter correction reduced the Balluffi correction produced larger changes in the self-diffusiv-ities; neither, however, produced statistically significant changes in the Do's or the H'S. The most striking result of this investigation is that at all three compositions and at all temperatures studied both the uncorrected and corrected self-difjusivities of magnesium are higher than those of cadmium. The Cd-Mg system is the first one found in which the higher melting, lower vapor pressure element diffuses more rapidly. Both an empirical correlation due to Toth and Searcy and considerations of the atomic mechanism of diffusion indicate that this anomaly is probably due to a comparatively low value of the activation energy required for a magnesium atom and a vacancy to exchange sites, perhaps occasioned by the higher compressibility of magnesium atoms. KIRKENDALL effect studies have been previously reported for only two hcp solid solutions: the E phase of the Zn-Cu system1 and the a phase of the Cd-Hg system.' In neither investigation were the marker-movement studies supplemented with the concentration-penetration curve determinations necessary to evaluate self-diffusivities by means of the atano and the Darken analyses. The present program was undertaken to obtain both types of data on a hexagonal solid solution in order to provide more detailed information relevant to the mechanism of diffusion in this type of lattice. The Cd-Mg system was chosen for this study because the disordered solid solution extends across the entire phase diagram at temperatures above 253"c5 and the substantial difference in the melting points of the component pure metals promised that marker movements would occur at reasonably rapid rates should the diffusivities of the two species be as unequal as might be anticipated. The experimental convenience of the relatively low melting points of cad-miun and magnesium and the availability of extensive and accurate activity data6 (required for application of the Darken analysis) were additional reasons for selecting this alloy system. Since the anisotropy of diffusion is not large in either pure cadmium7 or pure magnesium,' the diffusion couples were prepared from polycrystalline components. The presence of a well-defined texture in the couples—the c axis of individual crystals tended to be normal to the diffusion direction— however, provides a fair degree of crystallographic definition to the data obtained. The principal (and entirely unexpected) finding of this investigation, that magnesium, the high-melting low-vapor pressure element, diffuses more rapidly than cadmium, in contradiction to a broad range of results in fcc and bcc alloys, as well as in the previously studied hcp alloys,172 makes the self-diffusivity determinations of immediate interest in understanding the origin of this anomalous result. EXPERIMENTAL PROCEDURE The cadmium (Belmont Smelting and Refining Co.) and magnesium (Dow Chemical Co.) used in this study were both of 99.99 pct purity. Alloys containing 51.0 and 65.6 at. pct Mg were prepared from these materials by melting under a MgC12-base flux in a high-purity graphite crucible. These alloys were subsequently hot-worked and then homogenized in a helium atmosphere at temperatures close to their solidus points. Sandwich-type diffusion couples of the type g/d/g were prepared from the pure metals by solid-state diffusion. Two-piece alloy couples of Mg/65.5 at. pct Mg (Mg/gCd) and Cd/51.0 at. pct Mg (Cd/CdMg) were welded by a liquation technique. The individual components of both types of couple were initially cylinders 1.27 cm in diam and in length; the ends of these cylinders were machined accurately flat and parallel. For both welding techniques, the pure cadmium cylinders and the alloys were chemically polished in a mixture of 40 pct ethyl alcohol, 40 pct hydrogen peroxide (30 pct conc), and 20 pct nitric acid,g while those of pure magnesium were polished in a solution of 10 pct nitric acid in ethyl alcohol.' Immediately afterwards, both metals were rinsed in freshly distilled acetone, and then in similarly purified methanol.' The Mg/Cd/g couples were assembled in a carefully cleaned stainless-steel welding fixture, in which a screw operating through a self-centering arrangement permitted a controlled pressure to be exerted upon a couple prior to welding.'' Tungsten marker wires 0.005 cm in diam were placed at the d:g interfaces of some of these couples, and imbedded in the couples during the application of pressure. As soon as a couple had been assembled, the welding fixture was inserted into a Pyrex capsule containing a packet of zirconium chips at each end. The capsule

Jan 1, 1967

By G. N. Goldberg, Robert A. Rapp

The steady-state kinetics and microstructures of simultaneous internal oxidation and external scale formation were investigated for the oxidation of Cb-Zr and Ch-Zr-Re alloys in pure oxygen at 1000°C. For each binary alloy, a constant rate of scale formation was observed at steady state; the internal oxidatton zone reached a steady-state, time-independent thickness. The dependence of the scaling rate on zirconium content exhibited a maximum at a low zirconium colttent; more concentrated alloys oxidized at a slower rate than pure columbium. This composition dependence of the scaling rate may be partially attributed to the effect of the internal oxidation process as an intenla1 sink for oxygen, with the formation of voluminous, and relatively impermeable ZrO2 precipitates. However, the morphologies of the ZrO2 internal oxide precipitates also affected the scaling rate. The internal oxide precipitates were distributed uniformly in the external scale. The steady-state thicknesses of the internal oxidation zones were not in agreement with those predicted theoretically from an idealized simple model. However, in this particular alloy systen1 the ideal model is not satisfied experitmentally. For ternary Cb- Zr - Re alloys with Nr10e = 0.02 or 0.05, the steady-state thicknesses of the internal oxidation zones were less than those for the corresponding binary Cb-Zr alloys. For ternary alloys with NRe(0) - 0.05, a more adherent and much less porous external scale was formed, and a reduction in the kinetics of scale formation was observed. A number of authors'-7 have reported linear oxidation kinetics for the reaction of pure columbium at 1000°C in air or in oxygen of about 1 atm pressure. A thin and tightly adherent oxide layer is found at the metal/oxide interface beneath a porous external layer of scale. Although the suboxides CbO and CbO2 represent thermodynamically stable phases at 100O°C, generally only Cb2O5* is identified as a reaction product in quenched specimens. Studies at 1000°C at lower oxygen pressures8,10 (Po2 - 10-4 Torr) show that both CbO and CbO2 do form and that CbO2 is a protective oxide. The growth of CbO2 results in parabolic kinetics until Cb2O5 is nucleated and grows. Apparently because of the large volume change associated with its formation, Cb2O5 is porous and does not serve as a diffusion barrier; linear kinetics prevail after the surface is covered with Cb2o5. On the basis of these observations, several authors5,9,10 have suggested that the linear oxidation of pure columbium at 1000°C in air or oxygen of 1 atm is limited by a Loriers-type mechanism,11 whereby the total rate or reaction is controlled by ionic diffusion through a thin layer of CbO2 which is maintained at a constant thickness throughout the linear oxidation. However, the concept of a Loriers model for a three-phase CbOlCbO2 Cb2O5 scale, with the only oxygen activity gradient across the NbO2 phase, is not self-consistent. Further, the suboxides CbO and CbO2 were not observed in the high-temperature X-ray diffraction study of columbium oxidation by Goldschmidt.8 From investigations in which the large PO2, dependence of the linear scaling rate was demonstrated, the importance of an oxygen adsorption or dissolution step has been suggested.4,5,7,10,12 Thus the mechanism for the linear oxidation of pure columbium remains quite controversial. Since further insight into the oxidation mechanism of pure columbium is not provided by this investigation, the authors wish to emphasize at the outset that their experimental results are not interpreted in terms of a particular rate controlling step for the oxidation of pure columbium. Previous investigations13-18 of the oxidation of Cb-Zr solid-solution alloys in air or oxygen at 1000°C suggest a remarkable dependence upon zirconium content. For an alloy of bulk zirconium mole fraction, N2r(0) equal to 0.05 or 0.10, the oxygen uptake is reported to be as high as four times greater than that for pure columbium;13,14 for alloys with NZr(0) 0.05 or 0.10 the oxygen uptake is reported to decrease with increasing NZr(0); to a minimum uptake of about one quarter that for pure columbium at NZr(0): = 0.50.13-15Since zirconium forms a more stable oxide (ZrO2) than the lowest columbium oxide (CbO), and since columbium exhibits a high solubility19,20 and diffusivity21,23 for oxygen, the internal oxidation of the zirconium component to ZrO2 is expected at a reaction front ahead of the advancing metal/scale interface. The external scale is then formed at the metal/scale interface by the inward migration of oxygen through the scale, probably through a series combination of molecular and ionic diffusion. Internal oxidation in conjunction with external scale formation has been investigated by Maak24 for the oxidation of dilute Cu-Be alloys in pure oxygen at 850°C. For cu-Be and many other binary alloys,24-27 very small, essentially uniaxial internal oxide particles are formed in the most dilute compositions; for somewhat more concentrated alloys. the internal oxide particles precipitate as platelets or needles. From pertinent solutions to the diffusion equation, Maak28

Jan 1, 1967

By H. Biloni, R. Morando

The surface structure and substructure of Al-Cu alloys solidified as conventional ingots and under particular conditions such as those used by Bower and Flemings are studied. The influence of lampblack coating on the mold walls is especially considered and the results compared with those obtained in copper and graphite molds where no coatings exist. When high heat extraction conditions exist the observations show that mechanism of copious nucleation is responsible for most of the chill zone. When the heat extraction through the mold walls is low, a coarse grain structure with dendritic morphology arises, with a size that depends on the degree of convection present, analogous to that analyzed by Bower and Flemings. In both cases the effect of the convection on the macroscopic and microscopic appearance is discussed. The ingot macrostructure consists of one or more of three zones: "chill zone", "columnar zone", and central "equiaxed zone". The mechanism of the columnar-equiaxed transition has been subject of considerable interest and at present at least three theories exist about the formation of the equiaxed region: 1) the constitutional supercooling theory1 maintains that the equiaxed crystals nucleate after the columnar zone has formed, as a result of the constitutional supercooling of the remaining liquid; 2) chalmers2 pointed out, however, that there were several objections to this proposal, and that consideration should be given to the possibility that all the crystals, equiaxed as well as columnar, originated during the initial chilling of the liquid layer in contact with the mold; 3) Jackson et aL3 and O'Hara and ~iller~ suggested that a remelting mechanism of the dendrite arms is responsible for the formation of the equiaxed region. After the work of Cole and Bolling and other authors6 it became evident that convection (natural, reduced, or forced) plays a very important role in the transition from columnar to equiaxed and on the size of the resultant equiaxed structure. Until recently the accepted explanation of the chill zone was that it occurs as a result of copious nucleation in the liquid layer in contact with the mold walls.798 The columnar region is a subsequent result of the growth of favorably oriented grains and, as a result of a selection mechanism studied by Walton and Chalmers,9 elongated grains with marked texture are formed. Recently, however, Bower and Flemings" using an ingenious laboratory experiment introduced the idea that the "copious nucleation" mechanism is not responsible for the formation of the chill zone and that the presence of convection, introducing some form of "crystal multiplication", plays a decisive role in the formation of the chill zone. Unfortunately, it is important to consider that for their conclusions Bower and Flemings extrapolated the results obtained in their special experiments to the case of conventional ingots, and that these authors only analyzed the macrostructures of the specimens. Let us consider the work by Biloni and chalmers" concerning predendritic solidification. These authors were able to show that a study of the segregation substructure of A1-Cu gives information about the nucleation and growth of crystals formed in contact with a cold surface. A spherical predendritic region characterizes the first part of every grain nucleated in contact with the surface as a result of the chill effect. The aim of this paper is to elucidate through the observation of the segregation substructure the conditions under which (in the Bower and Flemings type of experiments and in conventional ingots) either the nucleation or the multiplication mechanism gives rise to the structure in contact with the mold walls. I) EXPERIMENTAL TECHNIQUES The experiments were performed on two alloys: Al-1 wt pct Cu and A1-5 wt pct Cu. The purity of the aluminum was 99.99 pct and the copper 99.999 pct. The results obtained with both alloys were similar. In the Bower and Flemings type of experiments the apparatus employed to obtain rapid solidification against a surface was similar to that used by those authors. The liquid was drawn by partial vacuum into the thin section mold cavity. Plate casts were 5 cm wide and usually 7.5 cm high. The thicknesses of the cast were 0.1 and 0.3 cm. Two different materials were used for the mold, copper and nuclear-grade graphite. The internal mold surfaces were polished and left uncoated for some experiments. In other experiments, the copper or graphite surface was coated with a thin film of lampblack material. In some of these particular experiments one of the mold walls was left with an uncoated region (usually in the form of a cross). The conventional ingots were cast in graphite or copper molds. In different experiments the mold walls were sometimes uncoated or coated with lampblack material. The results obtained in conventional and Bower and Flemings copper molds were compared with those obtained with copper molds coated with a very thin film of graphite; the results obtained were essentially similar. The size of the conventional ingots was 5 cm diam and 7 cm high in all cases. The cast surfaces produced by the Bower and Flemings type of experiments and conventional methods were observed macroscopically and microscopically without any metallographic preparation. As Biloni and Chalmers showed," the observation of the chill surface can give considerable information about the structure and segregation substructure.

Jan 1, 1969

By J. G. Faller, L. P. Skolnick

The distribution of cobalt and vanadium over non-equivalent crystallographic sites in C14-type Zr(VCo), alloys has been investigated. An anomalous X-ray scattering technique developed by Skolnick, Kondo. and lavine7 by which the separation in the scattering factors of two similar atoms can be enhanced was employed. Six alloys spanning the pseudobinary section ZrV1.6Co0.4-ZrVO.6CO1.4 at 10pct steps showed a nonrandom compositionally dependent distribution. Specifically, at high vanadium content cobalt preferentially occupied sites of type (6h) and vanadium, sites of type (2a; at low vanadium content the reverse was observed. In addition to the distribution fraction the structural parameters x and z were obtained. There was no significant deviation of these parameters from those obtained in the ideal C14 structure. Certain suggestions are made to account for the observed nonrandomness in the distribution of atoms on the two types of sites. INTERMETALLIC compounds of formula AB2 iso-morphous with MgCu2, MgZn2, and MgNi2 are known as Laves phases. Because Laves phases exhibit high symmetry and coordination numbers, the highest possible for an AB2-type compound,1 they are among the most frequently observed compounds in nature. In recent years interest has centered about the purely transition metal Laves phases2-' in efforts to understand the function of atomic size and electronic structure in the formation of these compounds. It has been observed that pseudobinary Laves phase systems often show a variation of structure across the phase diagram. Such a system is the ZrV2-ZrCo2 in which the structure varies from cubic MgCu2 to hexagonal MgZn2 to cubic MgCu2.4 Some understanding about the conditions under which the second modification is stable can perhaps be gained by studying the distribution of cobalt and vanadium atoms on lattice sites in the MgZn2 modification of the system ZrV2-ZrCo2. In both the MgZn2 and MgNi2-types there exist nonequivalent positions open to occupancy by the B element, whereas in the MgCu2 prototype all sites are equivalent. Skolnick, Kondo, and La-vine7 have developed an anomalous scattering technique suitable for this type of investigation. Whereas the influence of size on the formation of a Laves phase is well recognized, no substantial evidence has been put forth in support of the size ratio dependence of a particular prototype. Berry and Raynor8 suggested that RA /RB ratio does indeed affect the type of structure that is chosen, MgZn2 compounds tending to cluster about 1.225 while MgCu2 compounds were found at larger deviations from this ratio. Dwight,3 however, from a study of 164 Laves phases does not believe this generalization to be justified. Electronic effects are certain to play a part in the stability of Laves phases in general and in the choice of a structure type in particular. For example, size along would favor the formation of Laves compounds of Ti, Zr, Hf, Ta, or Nb as the A element with nickel or copper as the B element. The absence of such is attributed to an unfavorable electron : atom ratio by Elliott and rostoker.4 Early experiments of Laves and witte9 with pseudobinary and pseudoternary systems of the three prototypes established the dependence of crystal structure upon electron: atom ratios. They observed that the MgCu2 structure dissolved elements of higher valency until the electron: atom ratio of =1.8 was reached; the MgZn2 likewise dissolved elements of lower valency replacing zinc. witte,6 from calculations of the electron : atom volumes of Brillouin Zones, obtained limits of stability for the prototypes MgCu2 and MgZn2. Elliott and Rostoker4 used these limits with considerable success in the all-transition element Laves phases they investigated. According to witte,6 compounds between the electron :atom ratios of 1.80 and 2.32 were of the MgZn2 type; those above and below exhibited the MgCu2-type structure. On the basis of these limits and an assumed valency of zirconium based upon the near tetra-valence of titanium, Elliott and Rostoker obtained valencies for the first transition series elements. For the Laves phases with which this investigation is concerned, ZrV2 and ZrCo2, the authors calculated electron :atom ratios of 2.54 and 1.56, respectively. These ratios are for the MgCu2-type structure and straddle the stability band of the MgZn2 modification. One could, therefore, predict that a pseudobinary system ZrV2-ZrCo2 should pass through the MgZn2 modification in traversing the composition diagram from one end to the other. Implicit in this assumption is a smooth change of the electron: atom ratio from 2'54 to 1.56. MOSS10 states that his finding the low temperature structure of ZrCr2 to be C15 instead of C14 alters greatly Elliott's valency of zirconium and hence the assumed valencies of the other metals. Such a quantitative correlation of structure with electron : atom

Jan 1, 1963

By Shiou-Chuan Sun

THE fact that coals of different ranks and even of the same rank differ greatly in their amenability to iroth flotation is well known. In recognition of the need for an explanation of this phenomenon, two hypotheses have been suggested. Wilkinsl reported that the floatability of coals increased with an increase of the carbon content or rank. This postulate is handicapped by the fact that bituminous coals that possess moderate carbon contents are actually more floatable than anthracite coals that have high carbon contents, as shown in columns 6 and 9 of Table I. Taggart and his associates' implied that the difference of floatability between bituminous and anthracite coal was caused by the variation of carbon-hydrogen ratio. This is not applicable to the relative floatability of other coals and carbons. For example, column 11 of Table I shows that the carbon-hydrogen ratios of low-floating lignitic coal and non-floating animal charcoal are not only smaller than the moderate-floating anthracite coal, but are also similar to the high-floating bituminous coal. Furthermore, according to this hypothesis, high temperature coke-A (464), Ceylon graphite (1238), and lamp-black (357), all possessing extremely high carbon-hydrogen ratios, should be less floatable than other substances having much lower carbon-hydrogen ratios such as high volatile-B bituminous coal (11.9 to 22), anthracite coal (35.7 to 60.5), lignitic coal (15.6 to 33.6), and charcoal (13 to 26.2). However the former group is actually more floatable than the latter group. In this paper, a surface components hypothesis is Proposed to explain the different floatabilities of coals, carbons, and hydrocarbon minerals. The validity of the hypothesis is experimentally supported by the actual floatability, natural floatability, wettability, and adsorbability for neutral oils of coals, carbons, and hydrocarbon minerals tested. The combustible recovery of the flotation results, as used in this paper. was calculated from Eq. 1: P (100-Ep) 100 RWCP Rc= [1] F (100-E,) C, where R, is the percent combustible recovery; F and P are, respectively, the weight of feed and the weight of concentrate or product; E, and Ep are, respectively, the total percent of ash plus moisture in feed and in concentrate; Ru. is the percent weight recovery: and C, and C, are, respectively, the percent of combustible in feed and in concentrate. Except for ash and moisture content, all chemical components of a coal are assumed combustible. The experimental work included studies on flotation, ultimate and proximate analyses, contact angle tests, extractions of bitumen-A with benzene, adsorptions for liquid hydrocarbons, and wetting tests. Most of the flotation experiments were performed in a laboratory Fagergren machine; others were tested in a small Denver machine. The solid feed for the former was 300 g and for the latter was 30 g. The solid materials used for flotation were crushed to —48 mesh. After the mineral pulp in the flotation cell was agitated for 6 min and the pH was adjusted to 7.5 & 0.2 with sodium hydroxide or hydrochloric acid, a petroleum light oil having a viscosity of 5.73 centipoises at 77 °F was added and conditioned for 2 min. Finally, pine oil was introduced and the froth was collected for exactly 3 min. The weight ratio of petroleum light oil to pine oil was kept constant at 1.5 to 1. Tap water was used for all flotation tests. Contact angles were measured with a captive bubble machine. For each coal sample, three specimens were mounted in transoptic mounts and polished with levigated alumina, first on a sheet glass, then on a cloth-covered metal polishing wheel. The polished specimen was first washed with distilled water and wiped thoroughly on a cleaned linen pad, then transferred into the pyrex cell of the captive bubble machine and conditioned for 6 min., and finally measured for contact angles at three or more points. Except where otherwise stated, the induction time for each measurement was 1 min. The contact angle representing each material was obtained by averaging the measurements of three specimens. The linen pad was first washed with warm distilled water, then boiled 30 min in a 2N sodium hydroxide solution, and finally washed with distilled water until no trace of sodium hydroxide could be detected in the decanted solution. The cleaned linen pad was stored under distilled water. Immediately before using, the pad was rewashed and transferred into a clean pyrex petri dish partly filled with distilled water. The glassware and rubber gloves used were cleaned by soaking in sulphuric acid-potassium dichromate cleaning solution, followed by rinsing with distilled water. The polished specimens were handled only by glass forceps. The ultimate and proximate analyses were made in accordance with the ASTM standard procedures for coal and coke. The extractable bitumen-A was determined by weighing 1 g of —100 mesh sample and placing it in a desiccated and weighed ASTM aluminum-extraction thimble. The thimble was placed in condenser hooks and inserted into an extraction flask containing 100 cu cm of benzene. The flask was heated and the benzene vapor was condensed by water coils. At the end of 24 hr of percolation, the thimble was removed, desiccated, and weighed. Loss in weight of sample was taken as bitumen-A and calculated to dry and ash-free basis.

Jan 1, 1955