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By Jean-Louis Robert

Field work inaugurated in 1962 in the townships of Lemieux and Lesseps, in the Gaspe Peninsula of Quebec, has permitted the author to delineate the lithologic units of the area, to elucidate a few stratigraphic problems and to outline several zones of alteration. Certain features of these zones and the numerous mineralized showings in the area merit the attention of prospectors and exploration companies.

Jan 1, 1966

By Lester G. Morrell

THE WORLDWIDE economic expansion that has characterized the first 3 years of the 1960's continued through 1964 and was reflected in North America by strength in the industrial economy of the United States, which again was dominant. Advances in production were recorded in virtually all industries, including the mineral industry; 1964 mineral production established a new high, 5.4 percent above the previous peak recorded in 1963. However, the percentage increase in value of North American mineral production was slightly below overall economic growth. For industry in general, consumer demand held firm throughout the year and overall commodity prices averaged 2 percent higher than in 1963. Wages and salary payments also were up. With the single exception of the dock strike in the United States, the year was free of serious labor troubles and unemployment in both Canada and the States was at a low level. Despite the Viet-Nam situation, relatively tranquil international relations contributed to the forward movement of North American business. Total gross national product (GNP) for Canada and United States, in current dollars, was estimated at US$672.2 billion; 6.8 percent above the previous year's figure. Combined national income in 1964 amounted to US$546.9 billion, which was nearly 7.0 percent more than in 1963. In 1964, gains were recorded in each of more than 50 metals, nonmetals, and fuels commodities that comprise the North American output. The greatest category increase was 13 percent in metals, which was in part attributable to the 14 percent rise to a new record in value of iron and steel in United States, a 29 percent higher value of Canadian iron ore and a 57 percent rise in Canadian zinc. Despite a moderate decline in prices of iron ore and iron and steel products, generally favorable markets and rising prices for metallic ores and metals were a stimulant to the metals industry. Nonmetallic materials, with a total value in excess of US$5.25 billion were 7.3 percent higher than in 1963. High levels of highway and building construction and expanding demand for fertilizers and chemicals continued throughout the year. Noteworthy output increases were recorded for lime,

Jan 1, 1966

By Alla D. Mah

Compilation of data on materials of metallurgical interest is one of the important activities of the Berkeley Thermodynamics Laboratory of the Bureau of Mines. Recent renewed interest in metallurgy of vanadium renders the present compilation a timely guide for experimentation to improve present methods or to develop better methods of extractive metallurgy. Thermodynamic data for vanadium and its inorganic compounds have been critically surveyed, selected, and compiled into one convenient reference from which information can be readily obtained for evaluating heat balances, determining trends, and establishing limits of metallurgical processes. By indicating the direction of experimentation, this report enables the saving of time, effort, and expense which would otherwise be necessary for trial and error experimentation. Much of the data has been obtained experimentally at the Berkeley laboratory. Other data were collected through an extensive survey of worldwide literature through April 1965. Estimates were made when no data were avail-able. Data on the vanadium halides was sparse, and the results derived from existing data were at times divergent. Some of the selected values for the halides may need modification as more or better experimental data become available.

Jan 1, 1966

By W. M. Houston

The phosphate formations of the Pliocene epoch were deposited along the coastal shelf of the eastern seaboard. The deposition of the phosphate is thought to be somewhat contiguous along the early shoreline, and the deposit can be more or less traced over an 800 to 930 mile path from the Florida Gulf Coast, near Ft. Myers, to the Pamlico Sound of North Carolina. This is illustrated in Figure 1. Three areas of commercial importance are currently being exploited from this extensive known deposit: 1 - The so-called ?Bone valley? in Central Florida (multiple operations) 2 - Hamilton County in North Florida (Occidental Corporation operation) 3 - Beaufort County in North Carolina (Texas Gulf Sulphur operation)

Jan 1, 1966

By P. O. Ripley

Into this tumultuous twentieth century, every second, two new babies are born. This is 5,412 per hour, and 130,000 per day. Relentlessly, consistently, alarmingly, they add to the more than three billion human beings who already inhabit the earth. Every tick of tier clock brings with it a problem child, the problem of another mouth to feed, another body to clothe, another human being for whom to provide. On the other hand, medical science has achieved a postponement of death, considerably past the period of a few years ago. Thus, life expectancy has been increased and world population has increased accordingly. Darwin (4) writing in 1962, suggests "It is curious how long the world is taking to perceive that we are living in what is a fantastically abnormal period of history, and one which must inevitably end soon, The first warning note of a possible population explosion was given by Malthus in 1799". He suggested that population increases geometrical while production increases only arithmetically and that soon we would not be able to feed the rapidly increasing population.

Jan 1, 1966

By W. V. McKnight

The paper discusses the equipment and methods used to establish some of the characteristics of a braking system. Some typical tests are described and an explanation of the approach used to derive information from the recorder charts is given.

Jan 1, 1966

By E. Allen

Quebec Cartier Mining Company operates approximately two hundred and fifty pieces of equipment in a climate with a temperature that has averaged 27.5°F during the last seven years. The use of special-purpose lubricants, fuels, antifreeze, rubber compounds, and alloy steels have reduced the cold-weather hazards. In some areas, high-cost cold-weather protective heating devices are being eliminated with experience.

Jan 1, 1966

By G. C. Bernard, L. W. Bernard, L. W. Holm, W. L. Jacobs

The effect of loam on the permeability of porous media to water was studied as a {unction of foaming agent concentration, specific permeability, pressure gradient, length of a porous medium and its oil saturation. At a given fluid saturation in a porous medium, the permeability to water was found to be the same whether loam was present or not. Foam decreases the permeability to water by developing a higher trapped gas saturation than that obtained by water flooding without loam present, increasing the concentration of foaming agent increased the trapped gas saturation and thereby decreased the permeability to water. The presence of oil reduced the capability of most foaming agents to decrease the permeability of a porous medium to water. A few surfactants were found to be effective loaming agents even in the presence of oil. These results are similar to those reported in a previous paper on the effect of loam on the permeability of porous media to gas. The effect of loam was found to persist in long porous media at moderately high reservoir temperatures and during the passage of many pore volumes of surfactant-free water. INTRODUCTION This paper describes part of a study on a novel approach in the use of surfactants for oil recovery; the use of foam rather than water to displace oil. Previously it was found that foam can displace oil which normally is not displaced by water.4 The foam is formed by successively injecting a suitable surfactant solution and gas into a porous medium. Foam appears to have at least two uses in the field: (1) it shows promise as a superior oil recovery agent, and (2) it shows promise as a selective permeability reducing agent. Foam may be very useful in water floods, or in other oil recovery processes, where highly permeable streaks or unfavorable mobility ratios are a problem. A previous paper reported the effect of foam on the permeability of porous media to gas.1 In the present study the effect of foam on the permeability of porous media to water is reported. The specific objectives of the study were to determine: (1) the effect of foam on the permeability to water in porous media of various specific permeabilities, (2) the effect of foam on the permeability to water in the presence of oil, (3) the effect of foam and crude oil on the trapped gas saturation, (4) the effect of foam on permeability to water at trapped gas saturation, (5) the effect of pressure gradient on the permeability to water under foaming conditions, (6) the persistence of foam during the passage of surfactant-free water through the porous medium, and (7) the effect of various foaming agents, length of the porous medium and temperature on the permeability reduction caused by foam. EXPERIMENTAL PROCEDURES EQUIPMENT AND MATERIALS The experimental apparatus consisted of consolidated and unco n soli dated porous media, wet test meters and constant delivery pumps. The porous media consisted of consolidated sandstone cores (6 to 36 in. long), and unconsolidated sand packs (3 to 30 ft long). The consolidated cores had permeabilities of 32 and 1,000 md and porosities of about 20 per cent. The sand packs had permeabilities of 3,500 to 211,000 md and porosities of about 40 per cent. (Throughout this report a term such as 100 md sand" is used. This term means that the porous medium had a dry, nitrogen permeability of 100 md.) Fluids used in the experiments were distilled water, 1 per cent NaCl solution, aqueous solutions of foaming agents, nitrogen gas, air and crude oil.

Jan 1, 1966

The Bluebell mine of The Consolidated Mining and Smelting Company of Canada Limited extends under Kootenay lake, in southern British Columbia, and water control underground has always been a major problem. This paper gives a brief history of the operation, and then de-scribes the methods used by Cominco to keep the combination of lake seepage, ground water and thermal spring water under control. The pumping arrangements are de-scribed in considerable detail, with illustrations to show the various stages of development, and the power supply sys-tem is outlined.

Jan 1, 1966

By Alton B. Cook

A material balance equation was derived for calculating (1) the initial oil volume and (2) the relationship of average reservoir pressure to net gas in storage in reservoirs used for natural gas storage operations. The equation is also applicable to secondary-recovery operations where reservoirs are completely repressured and gas cycled. Using this equation minimized two probable sources of appreciable error in conventional material balance calculations: inaccurate measuring of and accounting for produced gas, and differences between true reservoir pressure and average reservoir pressures as derived from bottom-hole pressure measurements. A new procedure is presented for calculating water encroachment. By solving the conventional material balance equation and the derived equation for gas storage simultaneously, the values for initial oil in place and net water encroachment can both be determined.

Jan 1, 1966

By A. J. Conelius, D. P. Sobocinski

This paper presents a correlation for predicting the behavior of a water cone as it builds from the static water-oil contact to breakthrough conditions. The correlation is partly empirical and involves dimensionless groups of reservoir and fluid properties and of production and well characteristics. The groups were deduced from the scaling criteria for the immiscible displacement of oil by water. The correlation is based on a limited amount of experimenfal data from a laboratory sand-packed model and on results from a computer program for a two-dimensional, incompressible system. Because the correlating groups are dimensionless, they can be used to estimate the performance of water coning cases not specifically considered in the correlation. However, despite its dimensionless nature, the correlation is not completely general and will not provide meaningful estimates of cone behavior in many situations. INTRODUCTION AND BACKGROUND The production of water from oil wells is a common occurrence which increases the cost of producing operations and may reduce the efficiency of the depletion mechanism and the recovery of reserves. We will deal with one cause of this water production, namely, coning. The coning of water into a producing well is caused by pressure gradients established around the wellbore by the production of fluids from the well. These pressure gradients can raise the water-oil contact near the well where gradients are most severe. Gravity forces that arise from fluid density differences counterbalance the flowing pressure gradients and tend to keep the water out of the oil zone. Therefore, at any given time, there is a balance between gravitational and viscous forces at points on and away from the completion interval. When the dynamic forces at the wellbore exceed gravitational forces, a cone of water will ultimately break into the well to produce water along with the oil. We can expand on this basic visualization of coning by introducing the concepts of stable cone, unstable cone and critical production rate. For instance, if a well is produced at a constant rate and the pressure gradients in the drainage system have become constant, a steady-state condition is reached. If, at this condition, the dynamic forces at the well are less than the gravity forces, then the water or gas cone that has formed will not extend to the well. Moreover, the cone will neither advance nor recede, thus establishing what is known as a stable cone. Conversely, if the pressure in the system is in an unsteady-state condition, then an unstable cone will continue to advance until steady-state conditions prevail. If the flowing pressure drop at the well is suffcient to overcome the gravity forces, the unstable cone will grow and ultimately break into the well. It is important to note that in a realistic sense, stable cones may only be "pseudostable" because the drainage system and pressure distribution generally change. For example, with reservoir depletion, the water-oil contact may advance toward the completion interval, thereby increasing chances for coning. As another example, reduced productivity due to well damage requires a corresponding increase in the flowing pressure drop LO maintain a given production rate. This increase in pressure drop may force an otherwise stable cone into a well. The critical production rate, well known in the literature, is the rate above which the flowing pressure gradient at the well causes water (or gas) to cone into the well. It is, therefore, the maximum rate of oil production without concurrent production of the displacing phase by coning. At the critical rate, a built-up cone is stable but is at a position of incipient breakthrough. Numerous papers have been published on critical rates. Some of the better known of these include the work of (1) Muskat and Wyckoff,' who first dealt with the coning problem; (2) Chaney, et al,' who developed expressions similar to those of Muskat but who presented results in a conven ient-to-use graphical form (the "Sun" method); and (3) Meyer and Garder,b hose analysis is based on radial-flow formulas. One assumption in critical production rate analyses is that the cone has built-up to just before its breakthrough into the well. But, these analyses reveal nothing directly about the time it takes for the cone to build up to this incipient breakthrough position. Thus, water-free oil can be produced from a well for prolonged periods at rates above the critical rate before the well reaches the condition to which the critical rate applies. The published literature contains little on the rate of growth of a cone. Experimentally, Meyer and Searcy studied the rate of rise of a cone in a Hele-Shaw model.' Additional related work on water breakthrough and produced water-oil ratios in water driven reservoirs was reported by Muskat," Hutchinson and Kemp," Henley, et al,' and Stevens, et a1.B Theoretically, the basic coning equations for a water-oil system can be developed by applying the conservation of mass to each of the phases, relating flow velocities with pressure by Darcy's law, and relating pressures across water-oil interfaces by capillary pressure. With the usual boundaries at the well and reservoir limits, the solution of the resulting equations for the time behavior of a water-oil interface constitutes a free-surface, boundary-value problem. The shape of the boundary depends on the internal potential distribution, while this

Jan 1, 1966

By J. W. Stevenson

The Bureau of Mines investigated the influence that atmospheric pressure changes exert in a gassy coal mil on a ventilating air current with a system of bleeder entries. During the season when abnormal barometric fluctuations usually occur, recording instruments monitored the air current ventilating an active coal-producing area. It HL he rate of coal production caused a more significant change in methane concentration than did barometric change. The hazard that accompanies methane release due to expansion of the gob gases during atmospheric lows was minimized by the effective bleeder system.

Jan 1, 1966

By Donald Towse

The Permanente plant of Kaiser Cement & Gypsum Corporation is located at a unique thick deposit of Calera Limestone (Figure 1) on the southwest side of San Francisco Bay. Limestone is rare in the eugeosynclinal Franciscan assemblage, constituting less than 0.1 percent of the total volume. On the northwest part of the San Francisco peninsula Calera Limestone is present as isolated masses from the type sect ion near Rockaway Beach southeastward for ten miles, where the belt is truncated by the San Andreas fault. The large Permanente deposit is sixteen miles south of the truncated belt, on the northeast side of the San Andreas fault. Scattered small exposures are known for about twenty miles southeasterly from Permanente. (1,2) Most deposits of Calera are thin; the type section is about two hundred feet thick. At Permanente, however, the normal limestone section contains at least four hundred feet of limestone; and, due to folding and extensive faulting, the total vertical thickness of the limestone section is over 1400 feet. The unusual thickness of limestone is due to low angle thrust faulting. This fortuitous structure formed a deposit of limestone that supplies an 8,500,000 barrel cement plant in a major metropolitan market.

Jan 1, 1966

By Ramon B. Santos

The Atlas Concentrator, reputedly the largest in the Far East today, is located on the island of Cebu in the Republic of the Philippines. It started operation on a 4000 TPD capacity in 1955. An expansion program, coupled with significant improvements both in the Crushing Plant and the Mil, made the Atlas Concentrator what it is today, treating about 14,000 tons of ore per day at a comparatively low cost of about $0.50 per ton treated. The Atlas Copper Mine is at present mainly an open pit operation, with ore supplied from two pits (Lutopan and Biga) north of the Concen¬trator. Development of an Underground Mine, situated on the main ore body at Lutopan, which will be a block caving operation, has been underway since 1963, and this underground mining operation is expected to b e in full production by the latter part of 1966.

Jan 1, 1966

By Robert C. Sutter

In 1958, it became obvious to some of us in the solution mining business that there were certain problems in connection with our sodium chloride brining operations which were industry- wide. These were the types of problems which, while they were important to the safe and economical operation of our salt brining operations, were not such that their solutions would give an individual company a great competitive advantage over his competitor; and since they involve the safe and efficient mining of a natural resource, it was obvious that the answers would, in any event, be shared industry-wide. Since we were dealing with underground solution mining and, consequently, unseen and remotely controlled operations, the problems are formidable and the solutions difficult. While all of us were doing work to improve our operations, none of us could justify the expenditures necessary for basic research in these areas. Consequently, the idea was conceived of research sponsored by many companies with the same problems. In 1960, 11 companies entered into a' formal agreement to jointly support research on a specific problem of sodium chloride solution mining. The project to be undertaken was the development of a method for measuring the size and extent of underground solution cavities in sedimentary salt beds. It was agreed that all research was to be performed by independent research organizations. A part-time consultant or administrator was retained to administer the research contracts and to provide technical advice.

Jan 1, 1966

By E. H. Dudgeon

In order to make increased use of automation in copper smelting, it is evident that a useful first step .world be the accurate determination of the copper end point in the converter operation. After laboratory tests, the copper end points in a copper converter at Gaspe Copper Mmes Ltd. were determined without reference to melt samples or other observations. The results indicated that the rapid measurement of the S02 level in the gas released from the converter has potential as a new and independent method of determining the copper end point in converter operation.

Jan 1, 1966

By C. Gatlin, M. E. Chenevert

The effects of bedding plane orientation on the elastic constants and the yield strengths of three laminated rocks (one sandstone and two shales) and one isotropic rock (a limestone) were studied. The directional dependence of the elastic properties of these rocks was experimentally evaluated using a triaxial compression cell and auxiliary stress-strain measuring equipment. Symmetry of Poisson's ratios within the bedding plane suggested that horizontal isotropy exists, but the bedding planes do give rise to an appreciable difference between properties in the horizontal and vertical directions. For the three bedded rocks studied, Young's modulus was lower normal to bedding than along bedding. Yield strengths were determined at confining pressures from 0 to 12,000 psi in a triaxial compression cell. The rocks studied showed strength reductions as high as 40 per cent when the test specimen was oriented at 20°-30° to the bedding planes. The mechanical behavior of these rocks suggested that the rock properties of shear strength and/or coefficient of internal friction can vary with direction, depending on the particular rock tested. Tensile strengths were also measured and found to be lowest when failure occurred along bedding. This work shows that bedded formations exhibit sizable directional variations in both their elastic constants and yield strengths. It is suggested that these variations may be accounted for by using the "elastic laminate" model and the "variable coefficients" failure model. INTRODUCTION The nature of rock deformation at elevated pressures has been studied by many workers; papers by Handin,l,2 and Robinson3 illustrate the present state of knowledge. Most investigators have either chosen rocks which were as isotropic as possible (in order to avoid complications of data interpretation and analysis) or they have oriented their samples so that the effects of anisotropies (such as bedding planes) have been avoided. Of the studies performed, few were concerned specifically with mechanical anisotrop-ies. Griggs4 has presented limited data for specimens cut parallel, normal, and 45° to the bedding plane; he relates the strength anisotropy observed to the fabric (bedding) anisotropy. His tests were primarily concerned with large deformations (20 per cent strain); thus, no directional values of the elastic constants were reported. Handin has reported the results of similar experiments. Bott5has discussed rock strength anisotropies due to faults, cleavage, or bedding. He was concerned primari ly with determining the shear stress on such planes and did not mention the effect of friction. Jaeger6 later generalized Bott's work by taking friction into account and presented a limited theory for the failure of rocks having a "single plane of weakness", and also for rocks having a constant coefficient of friction, and a shear strength which varies with bedding plane orientation. Donath and Cohen,7 and Donathg have evaluated rock strengths from shale and slate specimens cut normal and parallel to bedding. A dependence of cohesive strength (7,) on the specimen orientation was also shown. Adler9 has also studied this problem and lists similar results. He assumes that all bedded rocks behave according to Jaeger's single-plane-of-weakness theory. Kalinin and Belorussov10 list results for strength tests parallel and perpendicular to bedding and use this information as a basis for hole deviation analysis. From the literature it is apparent that sedimentary rocks have been tested under widely varying conditions of stress; however, the assumption of isotropy is generally, but not always, made. Since geologic sedimentation often deposits sediments in very definite lavers.,. it seems that more svstema tic attention should be given to the possible effects of this natural bedding. Bedding, as used here, refers to visible regularities of grain size or orientation resulting from depositional processes. The mechanical strength anisotropies, which bedding may present, is not the only anisotronic property to be considered, since the elastic

Jan 1, 1966

By P. B. Demarsh

"Location: - On highway 59, 17 miles east of Val d 10r near junction of Montreal highway in Northwestern Quebec.Life; - Started production 1952, ceased 1965.Ore: - Pyrite, chalcopyrite and small amounts of free gold and goldsilver tellurides in narrow quartz-carbonate-tourmaline veins in granodiorite. Specific gravity 2, 70.Capacity: - 700 tons daily Bevcon ore supply, l 000 tons daily when custom ore available.Assay: - Heads 0 .140 oz. per ton; tails 0. 009 per ton; extraction 92.5%.Grind: - 75% minus 200 mesh at 700 tons; 68% minus 200 mesh at 1000 tons. Detention time 28 hours and 21 hours respectively.Treatment: - Cyanidation process.Reagents: - Per ton. Aero Cyanide (NaCn) 0, 50; crushed unslaked lime 1. 75; zinc 0. 03; litharge 0. 10; steel consumption 2. 25.Water: - Pumped from land-lock spring fed lake l 1/2 miles distant.Cost: - Per ton. Crushing 0. 13; grinding 0 .32; filtration 0. 07; cyanidation 0.14; miscellaneous 0.29; total 0.95.Power: - Hydro-electric, 25 cycle, 12, 000 volts reduced to 550 volts.Labour: - Predominantly French Canadian, nucleus English Canadians.Tailings: - Impounded low lying pond.Personnel: - 15 including supervision.Flow sheet: - Canadian Mining Manual l 9 5 6 .Building: - Wood truss construction: 3/ 4 in. siding, ten test and 1/ 4 in. transite outside. Corrugated galvanized iron roof. Ground level foundations. Internal self induced heating. Wood stave tank equipment."

Jan 1, 1966

By R. G. Jones, W. L. Kinney, R. E. Schilson, R. S. Wilson, G. A. Clark, H. Suralo

This paper discusses the results of the Fry conventional or cocurrent in situ combustion test, which was conduct-ed in a 3.3-acre inverted five-spot. The depth of the formation was between 880 and 936 ft; the oil had a specific gravity of 28.6° APl and a viscosity of about 40 cp at the reservoir temperature of 65°F. Preceding the combustion test, air injection tests were conducted which, in conjunction with geological studies, were used to evaluate the characteristics of the reservoir. Combustion was initiated on Oct. 13, 1961, with ignition being accomplished by a 40 kw electrical heater. The test phase of the project ended on Oct. 1, 1963. During the test, the average air injection rate was 1,520.-000 scf/D. Throughout the test, production of all fluids— gas, oil, and water—was monitored. Cumulative oil production credited to the project was 100,586 bbl. The cumulative air-oil ratio was 11,500 scf/bbl oil, and the oxygen uti1ization efficiency was 87 per cent. INTRODUCTION The Marathon Oil Co. conducted a successful in situ combustion test, beginning Aug. 22, 1961, at the Fry unit, Crawford County, 111. The purpose of the project was to test the feasibility of cocurrent in situ combustion as a means of oil recovery in the Fry type reservoir. Interest in in situ combulstion as an oil recovery tool has been stimulated mostly by the existence of large reserves of heavy viscous crudes with low expected recovery, usually less than 10 per cent. These are the so-called unrecoverable reserves, and most combustion tests to date have been conducted in this type of reservoir.1-4 In contrast, the Fry combustion test was conducted in a reservoir with a relatively high gravity oil having a relatively low viscosity. This paper discusses the performance of the test. The geology of the reservoir and the field operations are discussed in separate papers.5 TEST SITE The Fry combustion test was carried out in a 3.3-acre inverted five-spot portion of a lenticular body of Robinson sandstone. Net sand was 50 ft thick, porosity averaged 19.7 per cent, oil saturation was 68 per cent of pore volume, and water saturation was 20 per cent of pore volume. The oil in place was estimated at 1,040 bbl/acre-foot, or 171,600 bbl within the 3.3-acre pattern. The water in place was 326 bbl/acre-foot, or 53,800 bbl. The oil has a specific gravity of 28.7° API and a viscosity of 40 cp at the reservoir temperature of 65°F. AIR INJECTION PERFORMANCE Air injection took place in two phases, the phases separated by ignition of the reservoir. In the pre-ignition phase, air injection tests were conducted in the summers of 1960 and 1961. These indicated that the Fry reservoir was confined, and a high return rate of injected air could be expected. This proved to be an outstanding characteristic of the project, as cumulative gas production was 95.3 per cent of the air injected. The difference between the cumulative air injected and the total gas produced can be largely accounted for by the quantity of air stored in the reservoir. An estimated 16 X 10 cf of air remained in the burned-out portion of the reservoir and an indeterminate amount of gas was stored in the unburned but pressurized reservoir. Hence, a complete material balance of gases would account for nearly 100 per cent of the air injected. At times during the test, the daily gas production rate was 98 per cent of the daily air injection rate. Fig. 1 presents the air injection history of the Fry com-

Jan 1, 1966

By R. E. Stiles

The modified perchloric--EDTA method devised by the Bureau of Mines for the determination of copper in high-grade samples gives results that are more precise and more accurate than those from the classical sulfuric-iodometric method. Although the perchloric--EDTA method is more costly than the conventional method, the savings in time alone largely offsets this difference. Specifically, the modifications wade in the more conventional procedure comprise (1) use of perchloric acid instead of sulfuric acid for dissolution of copper minerals, (2) precipitation of copper as copper sulfide from dilute perchloric acid solution, (3) wet oxidation and dissolution of the precipitated copper sulfide, (4) use of larger amounts of indicator than those employed in the Schwarzenbach method of titrating low-tenor copper solutions with disodium ethylenedinitri10-tetraacetate and murexide indicator, and (5) use of refrigeration to partially stabilize aqueous solutions of the indicator.

Jan 1, 1966