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By R. O. Dannenberg

This Bureau of Mines report describes the results of research to develop a process for recovering additional beryllium from a commercial mill waste product, fluoferrate leach residue. Forty-five percent of the total beryllium in the leach residue was recovered in a beryllia product assaying over 98 pct Be0 by a process comprising (1) leaching with 1 N sulfuric acid, (2) adjusting the acidity of the leach liquor to pH 2, (3) extracting the beryllium with di-2-ethylhexyl phosphoric acid (EHPA), (4) stripping the loaded extract with sodium hydroxide solution, (5) boiling the sodium beryllate strip solution to precipitate beryllium hydroxide, and (6) calcining the beryllium hydroxide. Calculated reagent requirements per pound of Be° recovered by a proposed flowsheet were 28.1 lb sulfuric acid, 0.04 lb flocculent, 0.15 lb EHPA, 0.06 lb isodecanol (IDA), 0.22 gal kerosine, and 6.3 lb sodium hydroxide.

Jan 1, 1966

By R. Simon, D. J. Graue

This paper presents correlations for predicting the solu-lility, swelling and viscosity behavior of CO2-crude oil sys8i.m~. The correlations were developed from experimental data obtained by the authors. These data are also presented. The data were determined by measuring the properties of mixtures of CO, and nine different oils. Experiinental conditions covered a range of 100 to 250°F and pressures up to 2,300 psia. Properties predicted by the correlations have average deviations, expressed as per cent of experimental value, of 2 per cent for solubility, 0.5 per cent for swelling and 12 per cent for viscosity. INTRODUCTION Interest in CO2 injection as an oil recovery process has led to the development of performance prediction methods which can be applied to specific reservoirs.1 iS To use these performance prediction methods, it is necessary to know the solubility, swelling and viscosity properties of CO2-crude oil mixtures at reservoir conditions. Some information on these properties has appeared in the literature; however, this information did not cover the range of different oils and conditions needed to prepare generalized correlations for reservoir engineering purposes. Consequently, an experimental program was undertaken to collect the data needed. The data obtained and the correlations developed from the data are described in the following sections of this paper. SOLUBILITY OF CO2 IN CRUDE OILS CO2 solubility data in the literature come from six principal sources. The solubility prediction method of Welker and Dunlop3 is limited to 80F. The information in Ref. 4 is of two types: the first includes binary and ternary mixtures of CO, and light hydrocarbons (C1 to C6), and the second gives data for CO1 and heavy hydrocarbons for a temperature range of 40 to 90F. Ref. 5 contains a KCO2 chart for systems whose convergence pressure is 4,000 psia. The KCO2's are based mainly on CO2-natural gas mixtures. Poettmann's work covered CO2 solubility in one condensate and one crude oil6,7 Ja-coby and Rzasa measured CO? solubilities as a function of pressure and temperature for two natural gas-absorber oil mixtures and two natural gas-crude oil mixtures.'8 CO, concentration in these four systems was fixed at 5 mol per cent. The work reported in this paper extends CO, solubility data to a variety of different crude oil types in a temperature range from 110 to 250F and pressures up to 2,300 psia. The experimental procedure used by the authors to obtain the solubility data consisted of combining known amounts of pure CO, and crude oil in a visual cell at a fixed temperature and measuring the bubble point of the mixture. Measurements were made for a total of 40 different CO2-oil mixtures and the results are shown in Table 2. The mixtures included nine different oils (seven crude oils and two refined oils) whose properties are listed in Table 1. All nine oils had vapor pressures less than 1 atm at the experimental temperatures. Consequently, analysis of the bubble-point vapor showed a CO, concentration over 99 mol per cent. At no time during these experiments was a second, more dense, liquid phase observed. The solubility correlation which was developed from the data in Table 2 is presented in Figs. 1, 2 and 3. In these figures, solubility is expressed as xco2 the mol fraction of CO, in the CO2-oil mixture. Fig. 1 shows solubility as a function of CO2 fugacity6 and temperature. Fig. 2 shows the same solubility data expressed as a function of saturation pressure and temperature. The solubility shown in Figs. 1 and 2 is for an oil whose UOP characterization factor is 11.7. UOP characterization factors of crude oils can be determined from Ref. 10 if the viscosity and APT gravity of the oil are known. Fig. 3 gives the solubility correction factor for oils whose UOP characterization factors differ from 11.7. The solubility correlation in Figs. 1, 2 and 3 predicted

Jan 1, 1966

Oren F. Bridwell: We will close out the Institute. The President could not be here. So the Past President of the organization has been asked to take the chair. If there is no objection I will be glad to do so. We will proceed with the meeting. It seems to me we have a quorum. Minutes of last year's meetings are published in the Proceedings. If there is no objection we will dispense with the reading of the minutes. There being none we will dispense with the minutes. The Nominating Committee made its re- port last night. (See list of officers in front of Proceeding.) I move the nominations be closed. Mr. Bridwell: You have heard the motion and second. All in favor say "Aye." (Unanimous.) Motion carried. We will have a report of the Auditing Committee. Mr. Von Storch read the financial statement.

Jan 1, 1966

By J. A. Bartnik

In recent years, the need has become more and more accute for a high capacity, high intensity, wet magnetic separator for the concentration of finely ground, paramagnetic minerals. As a result of this increased interest, extensive test work has been conducted at our Central Test Laboratory, and the basic design for such a separator has been established. Three units have been developed to comprise a full line of this equipment: (a) Series 4L (laboratory), Figure I, is manually operated to permit maximum flexibility and precise control of each variable, with a capacity of 4 gallons per minute. (b) Series LOCC, Figure II, functions by automatically controlled feeding and washing cycles, and has a capacity of approximately 1.0 tons per hour. (c) Series 200CF, Figure III, basically consists of an annular pole box, rotating through the high intensity magnetic field. This unit has a capacity of approximately 20 tons per hour.

Jan 1, 1966

By A. E. Gillis

"Some or all of the following benefits can be expected following application of automatic control to a grinding circuit:1. Maintenance of Optimum Mill Load Level2. Improved Uniformity of Grind3. Increased Productivity4. Decreased Power Costs per Unit of Product5, Reduced Ball Wear per Unit of Product6. Reduced Labour Costs per Unit of Product7. Reduced Operator SupervisionTo establish an indication of the benefits that could be expected through automation of the grinding circuit at East Malartic Mines Ltd. it was agreed that the Department of Mines and Milltronics Limited should jointly conduct a survey of the existing grinding circuit and operation.Aside from establishing feasibility, an important purpose of this survey was to determine costs of a suggested control system that East Malartic Mines Ltd. management might be in a position to assess the economics of the proposal and justification of the investment.The survey involved the taking of sound recordings of rod and ball mills during manual operations, locating circuit bottlenecks, establishing time constants and determining the number and location of sensors for good automatic control."

Jan 1, 1966

By Mary S. Esfandiary

This is a revision of a directory of coal research organizations throughout the world that was first published in 1961 as Bureau of Mines Information Circular 8008. Because of the wide acceptance of the first edition, a revision which would supply up-to-date information on coal research and which would facilitate communication among organizations of similar interest seemed important. This compilation includes the names and activities of organizations of various types-government, university, private, and industry. The areas of investigation that each organization is engaged in are indicated in broad terms: Analysis and constitution, mining and geology, preparation, briquetting, combustion, high- and low-temperature carbonization, gasification, conversion to solid and liquid fuels, and health and safety. Publications issued by and describing the work of each organization are cited; almost all of the organizations also publish results of their investigations in the technical press. Selected technical and trade publications that publish information on the science and technology of coal and are not published directly by any of the organizations listed are cited in the pages following the list of organizations in each country.

Jan 1, 1966

By Jr. Norman

The Bureau of Mines investigated the thermoelectric properties of yttrium selenides and tellurides from room temperature to 900° C. X-ray crystallographic data were determined for the yttrium-selenium and yttrium-tellurium compounds that were orthorhombic with a cubic substructure. The yttrium selenides and tellurides exhibited semimetallic to insulator conduction properties with figures of merit of 10-9 to 10-4 °C-1. The mono-selenide and monotelluride behavior was partially degenerate; unsatisfied bonds were the source of the large number of charge carriers. The higher stoichiometry selenide compounds were intrinsic semiconductors) but with high electrical resistivities. A critical defect or impurity ionization energy for carrier activation appeared to exist in the majority of telluride compounds. Mobility and energy band determinations are required to interpret completely the observed effects in most of the compounds studied.

Jan 1, 1966

By Charles Goodeve

"BEFORE I begin, I should like to thank The Canadian Institute of Mining and Metallurgy for the honour they have bestowed in inviting me to give this address at the fourth annual C.I.M. Conference of Metallurgists banquet.Secondly, I should like' to convey the greetings of the Iron and Steel Institute of Great Britain in accordance with a request made by its Council at its last meeting. The I.S.I. hopes for the continued growth in strength of this annual Conference and in the collaboration between our respective societies.When I read the program of this Conference, it was brought home to me what a non-ferrons country Canada is. Also, I realized what enormous advances have been, and are being made, and what an ex-citing field non-ferrous metallurgy is for the scientist. This made me wonder, as I have done before, whether the future for steel was proof against these advances.At present, iron and steel stand astride the metallurgical world like a Colossus; I hope that the bronze industry will pardon my stealing their thunder and mixing my metaphors! Will this still be so in the future?The best way to answer this question is to take a look at the fundamentals to see why the iron atom dominates to such an extent that al! other metals are called ""non-ferrons."" Is its present position due to historical and therefore ephemeral reasons, or is there a fundamental difference between the atom of iron and those of other metals?"

Jan 1, 1966

By F. R. Lee

THE Bureau of Mines was established in July 1910 to conduct research and to establish standards for mining equipment and practices which would conserve human life, natural resources, and property in the mineral industries. Several lists of equipment approved by the Bureau as permissible for use in gassy coal mines have been issued since then. The lists covering all approved equipment except breathing apparatus and explosives have born consolidated into two publications: Bulletin 343. Permissible Equipment Approved to January 1, 1953, and Information Circular 8220, Permissible Mina Equipment Approved By The Bureau of Mines During 1953-62. The, purpose of this publication is to supplement Bulletin 343 and Information Circular 8220 with a listing of permissible equipment approved during 1963 and 1964. The schedule, (standards) under which equipment listed herein have been approved are, as follows (cities and dates of approval and revision are, given in footnotes) : Schedule 2F,3 schedule 6D,4 schedule 7C,5 schedule 8C,6 schedule 9B,7 schedule 10C,8 schedule 12D,9 schedule 22,10 schedule 24,11 schedule 25B,12 schedule 25B,13 schedule 29A,14 schedule 30,15 and schedule 31.16

Jan 1, 1966

By G. E. Johnson

Batch tests of coals and coal-derived materials were made by the Bureau of Mines to determine their effectiveness in removing organic contaminants (COD or chemical oxygen demand, comprising those organic compounds that can be chemically oxidized, and ABS or alkylbenzene sulfonate, common household detergents) from the final effluent of secondary-treated waste waters. The adsorptive capacities of flyashes, coals, including at least one sample of each rank found in this country, pretreated coals, and miscellaneous materials including commercial chars and coke, were determined and compared with that of granular activated carbon. The coals, though not as effective as activated carbon, possess an economic advantage--they are relatively inexpensive, and they can still be burned as fuel without any loss of fuel value after use in waste¬water treatment. A hvcb coal was found to be one of the best, having about one-fourth the capacity of activated carbon for COD, adsorbing about 4 percent of its weight before it became saturated. Several coals contained constituents that added to the COD content of the treated water. Thus knowledge of the performance of the coal is necessary to insure selection of a proper coal as adsorbent.

Jan 1, 1966

By G. A. Gross

"Nearly 90 per cent of the iron ore produced in Canada is derived from iron-formation or bedded iron deposits. About 70 per cent of this consists of concentrates obtained from iron-formation; another 20 per cent was formed by natural enrichment processes.Four principal varieties of iron-formation are recognized -the Algoma, Superior, Clinton and Minette types. Differences in their geology, mineralogy, chemical com-position and environment of deposition are of special significance in their evaluation as ore.The properties of the ores, including grade, beneficiation qualities and minor element content in taconites, metataconites and naturally enriched ores, reflect characteristics of the primary stratigraphie units from which they are derived. A detailed description of the stratigraphie facies is essential for efficient utilization of these source beds."

Jan 1, 1966

By William J. Shampine

The Floridan aquifer, which underlies all of Florida, yields water with a sulfate content of less than 50 parts per million in the north-western part and throughout most of the center of the State. In the southern part of Florida and along the most of the east coast, the sulfate concentration generally exceeds 100 parts per million and is as much as 1,700 parts per million. The sulfate concentration tends to be higher in the deeper zones of the aquifer. This map shows the sulfate concentration in the upper part of the aquifer. Sulfate is found in almost all natural water. Sulfate in rainwater is dissolved from impurities and gases in the atmosphere. Rankama and Sahama (1955, p. 314) report that the average sulfate content of rainwater is two parts per million; however, concentrations have been as high as 283 parts per million. Much of the sulfate in rainwater comes from hydrogen sulfide gas which is generated in shallow water on the continental shelves. The combustion of bituminous coal used for heating and industrial purposes seems to be an important local source of sulfate.

Jan 1, 1966

By L. B. Pankratzt

The heat capacity of dimo1ybdenum carbide (Mo2C) was measured from 51° to 298° K, and the entropy at 298.15° K was evaluated. Heat content measurements above 298.15° It were conducted for dimolybdenum carbide (M0caY) and monotantalum carbide (TaC). The results were combined with known heats of formation and the 298.15° K entropy for TaC to obtain values of the heat and free energy of formation from 298.15° K to 1,400° K for MoaC and from 298.15°K to 1,800° K for TaC.

Jan 1, 1966

By Walter Kawa

Coals of various rank were reacted by the Bureau of Nines in plasma jets generated from argon and argon-hydrogen mixtures containing up to 33 volume-percent hydrogen. Average plasma temperatures ranged from about 3,400° to 12,000° C. Products were a solid residue and a gas containing hydrogen, methane, acetylene, diacetylene, and oxides of carbon. The highest yield of acetylene obtained with argon plasmas was 15 percent by weight of moisture- and ash-free coal. The data indicated that acetylene yields of 40 percent or higher can be obtained from the reaction of coal in argon-hydrogen plasmas, although results from these experiments could not be correlated with operating variables because of low recoveries plasma contained sufficient energy to heat the coal to temperatures as high 9,000 or 10,000° C, but complete devolatilization did not occur in any experiment.

Jan 1, 1966

By R. B. Roberts, A. L. Mular

A simple way to determine the IEP of oxide minerals is described. The method is shown to apply for fine powders of Fe203 and ZnO. The IEP lies at pH 6.95 for Fe203 and at pH 9.08 for ZnO.

Jan 1, 1966

By Donald R. Corson

The Bureau of Mines is conducting research on the effects of various established and potential soil-stabilization additives to hydraulic backfill. This initial phase is an evaluation of the effect of inclusion of varying amounts of Portland cement and combinations of cement and a dispersant on the bearing strength of backfill. Results of unconfined compression tests are given for over 200 sample cylinders incorporating a fill material with cement or cement and dispersant. Inclusion of a minor amount of dispersant (0.2 percent by weight) is found to yield a significant increase in strength for 20-to-1 and leaner sand-cement mixes. An apparent optimum concentration of dispersant exists beyond which no further increase in strength is achieved. A dispersant-cement ratio of l.8- to-1 yielded a strength increase of 515 percent over the strength of untreated 40-to-l sand-cement mixes.

Jan 1, 1966

By C. D. Stahl, S. M. Farouq Ali

This investigation attempts to describe and simulate the alcohol displacement process by means of a cell model, as employed in chemical engineering practice. The proposed model is more simple than previously proposed models. and utilizes parameters chosen on a theoretical basis. The model successfully reproduced the formation of the stabilized bank and the breakthrough of alcohol, the latter depending on one of the model parameters, which may be correlated with the length of the porous medium. Moreover, the effects of the phase behavior of the liquid system involved, as observed in experimental studies, were reproduced. Several variations of the basic model were devised and tested on a digital computer. These included the cases in which: (1) the actual value of fractional flow was used in cell-to-cell computations; (2) the number of cells was varied within the same run; and (3) incomplete rather than complete phase equilibrium was assumed within each cell. The proposed cell model clarifies the basic mechanism of the process. Detailed concentration profiles obtained for each cell, for instance, showed the mechanism of bank formation in relation to the phase behavior characteristics. The results obtained indicated a varying degree of phase equilibrium concommitant with changes in the velocities of the phases in an actual alcohol displacement. This condition was approximated by changing the number of cells during the simulation. Interesting information was obtained on the influence of path length on the efficiency of alcohol displacement, which has been the subject of some controversy. Certain limitations preclude the use of the proposed model as a substitute for experimental studies. The results obtained were, nevertheless, of value in interpreting the experimental results. INTRODUCTION During recent years considerable effort has been directed toward an understanding of alcohol displacement, the process whereby oil and water are recovered from a porous medium by the continuous injection of a solvent. The complex nature of the physical process involved has so far defied a complete mathematical treatment. Other methods of approach, amounting to an overall material balance, have been proposed, yielding useful information on certain aspects of the process.1-3 Taber et al, in particular, defined the displacement mechanism in terms of the phase behavior of the alcohol-oil-brine system invoIved.2 Wachmann reported a mathematical treatment of alcohol displacement subject to certain simplifying assumptions? Donohue proposed the use of a "cell model" for simulating alcohol disPlacement.5 The nature of the assumptions involved limited the utility of the model. The present work attempts to examine the variables involved in the simulation of alcohol displacement and discusses several possible versions of the basic cell model. Under certain conditions the model results are similar to the experimental results. In particular, the spontaneous formation of of the stabilized bank and the effects of the system phase behavior were successfully reproduced. PREVIOUS WORK ON CELL MODELS Cell models and the theoretical plate concept are often used in solving chemical engineering problems in which an explicit mathematical solution may be difficult or impossible to obtain. Examples of such applications occur in distillation, gas-liquid chroma tography,6 reactor technology, absorption, etc. In petroleum engineering, such a model was used by Attra7 to describe non-equilibrium gas drive, and by Higgins and Leigh ton8 to calculate sweep efficiency in water flooding. Aris and Amundsen pointed out the equivalence between the diffusion model and perfectly mixed cells connected in series.9 Deans proposed a three-parameter cell model to simulate two-component

Jan 1, 1966

By James F. Devine

The radial, vertical, and transverse components of particle velocity were recorded by Bureau of Mines investigators along gage arrays extending in one or two directions for 145 to 3,170 feet at five quarries. Of the 39 quarry blasts, 12 were instantaneous blasts, 5 were of the one hole per delay type, using millisecond delayed caps, and 22 were multiple hole per delay type employing millisecond delay detonating fuse connectors. Charge weight per hole ranged from 8 to 1,500 pounds, and the charge weight per delay interval, including the instantaneous blasts, ranged from 25 to 4,620 pounds.

Jan 1, 1966

By Martin H. Stanezyk

The Bureau of Mines investigated leaching of selected copper sulfide minerals and a composite of impure flotation concentrates at elevated temperatures and pressures with ammoniacal solutions. Copper 1 (tractions of 96 percent were obtained by leaching chalcopyrite at 75° C under oxidizing conditions for 60 minutes. An extraction of 99 percent of the copper contained in the composite concentrate was obtained by leaching the product for 90 minutes at 75° C. In tests of bornite, chalcocite, and covellite, 90 to 97 percent of the copper was extracted at 20° C provided an 8-hour reaction period was used. At 75° C essentially complete dissolution of the copper from these three minerals was accomplished in 60 minutes. Additions of ammonium sulfate to the leach solutions were required to obtain high-percentage extractions of the copper from bornite, chalcocite, and covellite. Although ammonium sulfate was not required when digesting chalcopyrite, copper extraction was enhanced and less free ammonia was required when ammonium sulfate was added to the leach pulps. The chemistry of leaching copper minerals was studied. It was C, termined that chalcocite altered to covellite as one step in the dissolution When leaching iron-bearing copper sulfides, hydrated iron oxide formed on the mineral surfaces, indicating that a diffusion process prevailed. No evidence of covellite was detected.

Jan 1, 1966

By John A. Ames

Limestone for portland cement must be beneficiated to produce uniform raw material for the kiln. Careful quarrying and selective recovery are factors in this process, but the chief aspects of beneficiation are "in plant" processes, such as crushing and screening, washing, grinding, flotation, and heavy-media separation. Numerous technical and economic problems exist. Detailed studies of the limestone deposit and the stone itself are required for intelligent beneficiation. As used in this paper, beneficiation is defined as the improving of limestone composition so as to produce an economically usable raw material A limestone deposit is defined as a mass of limestone which can be recovered, by quarrying or mining, for sale or for use in a commercially profitable operation. The stone may require elaborate processing, or it may qualify with little or none. Obviously, the "commercially profitable" qualification may change as the economy changes. Potentially commercial deposits may be of much better quality than actually developed deposits, and yet may be denied development for various economic reasons.

Jan 1, 1966