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By Joël P. T. Kapusta

Back in 1995, Air Liquide and Union Minière presented a joint paper at the Copper 95 – Cobre 95 Conference in Santiago, Chile, describing the first full scale plant trials of shrouded sonic injection in a Hoboken converter at the Hoboken smelter in Belgium. Almost a quarter of a century later, the technology known as ALSI, or Air Liquide Shrouded Injection, has been tested or commercially implemented in several copper and nickel smelters. Despite these successes, the copper industry did not adopt it widely in the same manner the steel industry adopted the Savard-Lee tuyere in the 1970s and beyond, not even in the way the lead industry adopted it with the Queneau-Schuhmann-Lurgi, or QSL, process. The development and implementation of bottom-blowing smelting and converting technologies in China in the last ten years, however, changed the industry’s perception that high- and ultra-high oxygen injection in copper smelting and converting was indeed possible under specific process conditions. In this paper, I retrace the key learnings of my journey with sonic injection over the twenty five years from my humble beginnings in my early years with Air Liquide, through plant trials and technology implementation in the late 1990s and into the first decade of the new millennium, and ultimately, to the most conclusive proof that the sonic injection design methodology I established is valid, and the calculation tools I developed are accurate. I conclude by sharing my thoughts about whether the deployment of the Savard and Lee legacy within the nonferrous industry was just a pipe dream or whether it will become a reality. INTRODUCTION In the context of lower quality ores and changing economic markets, copper smelters need to continuously innovate and improve to remain competitive and respect their corporate social responsibility engagements. One avenue towards this business, social, and environmental goal is to increase process intensity while lowering fossil fuel consumption to lower greenhouse gas emissions and reducing process off-gas volumes to better capture As and SO2–laden emissions. I believe high oxygen sonic injection for submerged tuyere copper bath smelting and converting is one technology that can help smelters achieve that goal of higher business, social, and environmental performance. Twenty five years ago, when I discovered that the Savard-Lee tuyere had revolutionized the steel industry (Savard & Lee, 1966; Knuppel, Brotzmann, Fassbieder, Savard, & Lee, 1972), I had a dream — or was it a vision? — that within the first decade of the new millennium, modern copper smelters operating submerged tuyere bath smelting and converting vessels will have implemented high oxygen sonic injection and will be reaping the financial and environmental benefits that the steel industry enjoyed in the 1970s. As we approach the end of the second decade of the new millennium, I have to admit that my dream has been all but shattered as the majority of copper bath smelting and converting vessels today continue to operate under bubbling regime conditions. This mode of operation is archaic, still requires tuyere punching and blows at inherently low enrichment levels, particularly in converting, producing large volumes of process off-gases. Under such operating conditions, regulations and emission quotas for As, SO2, and particulate matter oblige smelters to use not just primary or secondary hoods, but sometimes even tertiary hoods. I vividly recall being told, fifteen or twenty years ago when visiting smelters to promote the application of the Savard-Lee tuyere in nonferrous processes, that implementing sonic injection was not economically viable due to the high cost of compressing air and oxygen. Some of the smelters I visited back then have since mandated their engineering partners to design and build secondary or even tertiary hoods. I cannot fathom how secondary and particularly tertiary hoods, with all of their auxiliary equipment and added ducting, could be more economically viable than purchasing and installing a few compressors, expanding the pipeline network for compressed air and oxygen, and installing a new control valve train to feed sonic tuyeres. Besides, adding hoods does not address the problem of As and SO2-laden fugitive emissions at its source but merely provides a costly mitigation for it by capturing larger volumes of process off-gases rather than reducing these large volumes in the first place. Moreover, hooding does not reduce energy consumption nor does it increase process intensity, two aspects that I believe are critical for smelters to remain competitive and sustainable in a deeply changing market environment.

Jan 1, 2019

By Charles Pretorius, Henk Ludik

Navachab Mine experiences difficulties with pit wall stability in certain areas of the mine. The main reason for the instability is the fact that the geology comprises many joints and faults. Blasting, without impacting negatively on the stability of the pit walls, poses a major challenge.

Jan 1, 2006

By L. Vollert

In August 2018, the first full-scale HydroFloatTM cells for the recovery of coarse composited copper and gold were commissioned at Newcrest’s Cadia Valley operation in New South Wales, Australia. The primary objective of the installation is to recover coarse value-bearing composites that are lost to conventional flotation tailings, without the need for additional power input for particle size reduction to improve mineral liberation. This paper examines the application of Eriez HydroFloatTM technology for the recovery of coarse, poorly liberated copper sulphide particles drawing on recent experience from lab scale testwork through circuit design and commissioning of the full-scale installation at Cadia Valley. INTRODUCTION In the face of declining copper head grades and a tightening regulatory environment around the use of wet tailings dams, the processing of copper ores at coarser particle sizes has become a focal point for the industry. Sulphide flotation using the Eriez HydroFloatTM is one of the emergent technologies that sits under this umbrella of coarse pre-concentration. It has been demonstrated through numerous lab and pilot scale testwork programs carried out by Newcrest and others (Awatey, Kohmuench, Thanasekaran, Skinner & Zanin, 2013), to improve the flotation recovery of sulphide-rock composite particles with low surface liberation, relative to conventional flotation technology. The HydroFloatTM technology has been used widely for the recovery of coarse potash, phosphate, coal, vermiculite, spodumene and diamonds but has never been applied at full scale in either gold or sulphide flotation. In August 2018, the first full-scale 3.4 m diameter HydroFloatTM cells for the recovery of coarse composite copper and gold were commissioned at Newcrest’s Cadia Valley operation in New South Wales. The primary objective of the installation is to recover coarse value-bearing composite particles that are lost to conventional flotation tailings, without the need for additional upfront power input for particle size reduction to improve mineral liberation.

Jan 1, 2019

By Frank van der Meer, Jorge Portocarrero, Alexandra Gruendken

"The number of High Pressure Grinding Rolls (“HPGRs”, also called Roller Press) installations instead of tertiary crushers is rapidly increasing. The technology has been largely accepted in the minerals industry and benefits, such as superior energy efficiency and a lower overall operating cost compared to alternative technologies, have been demonstrated at a number of operations throughout the world.This paper focuses on coarse hard ore operations and reviews the successful installation of the first Roller Press installed instead of a tertiary crusher at the Los Colorados Plant of CMH (Chile) in 1998. It details the experience obtained over the past ten years of operation from commissioning to the present day. It highlights examples of further developments made in the design to improve machine maintainability and availability as well as wear life of the grinding surfaces.A second focus lies on procedures to derive from small scale testing material properties such as wear life, flake formation and strength and their application to industrial size machines to optimize circuit design, especially when Roller Presses are used in closed circuit with screening.INTRODUCTIONRoller Presses (also known as HPGR, High Pressure Grinding Rolls) are considered today state of the art for the preparation of pellet feed. They are also gaining wide acceptance in coarse ore operations. One of the first successful operations in which a roller press was used to replace a conventional tertiary and quaternary crusher is the Los Colorados plant of CMH in Chile.When the Roller Press at Los Colorados was commissioned in 1988, there were 169 Humboldt Wedag roller presses in operation throughout the world. Of these, 14 were installed in the minerals industry. However, these were installed mainly for grinding pellet feed to increase the Blaine value. Up to that time, only three KHD roller presses had been applied for crushing coarse ore in specialized circuits. Moreover, the installation at Los Colorados was the first Roller Press ever to replace a conventional tertiary and quaternary crusher in a hard ore application."

Jan 1, 2009

By SDN Wessels, WA Naismith

On 16 July 2004, at 07:10 a collapse of about 1.8 million m3 (about 4 ½ million tonnes) took place on the north wall on Nchanga Open Pit This collapse was the result of a developing instability that was first identified when the benches in this area were exposed during September 2002. The NOP Geotechnical and Survey Departments closely monitored the development of the failure. Control measures were implemented to reduce risk to men and equipment. These measures were continually improved and adjusted in reaction to observations and changing conditions. The purpose of this paper is to describe in detail the monitoring results that were obtained both by traditional methods and the novel Slope Stability Radar System (SSR). Difficulties encountered in establishing critical deformation levels and deformation rates that can be used to predict the onset of collapse are described. Details of the monitoring and control measures, which led to the successful completion of mining in the area, are also described in this paper.

Jan 1, 2005

Published experimental data on thermodynamic behaviour of cobalt-containing slags have been reviewed and used in validating a recently developed thermodynamic model. The results from the exercise show that the model provides a reasonably good description of behaviour of cobalt in multi-component slag systems. The models for cobalt containing slags, matte and oxide solid solution phases were incorporated into CSIRO?s multi-phase equilibrium (MPE) package, which was used to calculate the equilibrium distribution of cobalt between matte and slag phases under various conditions. The results agreed well with the experimental data. Furthermore, the good agreement between the calculation and the plant data indicates that the operating conditions of industrial smelting and converting processes are close to equilibrium. Two diagrams showing the effects of slag chemistry and SO2and O2partial pressures on the distribution of cobalt between phases were generated for conditions similar to smelting and converting processes. These diagrams provide some useful guidelines for developing new strategies to improve cobalt recovery.

Jan 1, 2004

By Grant Davis

An International Symposium on the Ecology and Revegetation of Drastically Disturbed Areas was held at the Pennsylvania State University in August 1969. Scientists from 13 foreign countries and 18 states in the United States attended this meeting, which focused on those areas disturbed by mining. The symposium enabled scientists from all over the world to get together for two weeks and discuss informally some of the knotty problems of reclaiming these disturbed areas. Trying to present the results of each of the 64 papers delivered at the symposium might be difficult. So, I will try to bring you up to date on the general status of research on the reclamation of surface-mined areas, particularly in revegetation and hydrology. I will also mention some research that is under way but was not presented at the symposium.

Jan 1, 1970

By L. Borsch

Geochemical laboratories are commonly criticized by geologists about poor analytical reproducibility and erratic anomaly patterns, especially when gold and trace metals from resistant minerals are reported. Geochemical analysis in mineral exploration is a compromise between high productivity on the one hand, imposed by large numbers of samples, and analytical precision and accuracy on the other. However, the physical properties of resistant minerals, such as cassiterite, gold, beryl, chromite, zircon and others, interfere with both of these requirements. Therefore, the degree of sample homogeneity that can reasonably be achieved in sampling and sample preparation must be considered. Subsequently, the understanding of its effects on analytical data quality and the consequences on data interpretation will provide a basis for understanding the problems common to exploration as an interdisciplinary science. Complaints about poor and inadequate analytical performance are not confined to exploration geochemistry. They are a common feature in mining and metallurgy and wherever sampling and analysis of "grains" are concerned - the "nugget" or "grain size effect." The "grain size" effect Poor analytical reproducibility is normal for gold and a well-defined group of other elements usually found in resistant placer minerals. Those who use and interpret geochemical data must realize and appreciate the chemical, the physicochemical, the physical and the mineralogical properties of the elements and their minerals. Especially for the "placer" minerals and their elements, such comprehensive interpretation is crucial. The most important factor to consider is the behavior of a mineral and its metal component(s) during weathering and their integration into the sampled medium, in exploration mostly sediments and soils. (Data interpretation for samples of water, gas, to a certain extent rock, follows different patterns.) A mineral may be chemically and physically stable or it may easily disintegrate physically or decompose chemically, or any combination of such processes, at varying degrees. The breakdown products, in turn, may or may not, interreact with the environment. If the nature of an element or a mineral predestines it for a heterogenous distribution in the sample medium, then nature, size and number of grains likely to occur should be considered in relation to the sample portion taken for analysis. This allows the estimation of their effect on analytical precision and accuracy. Elaborate and sophisticated statistical calculations exist on this subject. But these approaches do not cope with the complexity of the natural surface environment. The miner alogical, chemical and environmental behavior of elements and minerals can be estimated but not calculated. However, the mineral grain sizes and their influence on analytical precision can be precisely calculated if certain conditions, assumptions and idealizations are made. If the geochemical and mineralogical characteristics of minerals and elements are understood, such calculations demonstrate the grain (or nugget) effects that mineral properties and (geo)chemical behavior of minerals and elements cause on the precision and accuracy of geochemical analysis through their influence on sample homogeneity. Two other factors that influence the sample homogeneity and the nugget effect are the efficiency of sample preparation and the sample portion taken for analysis. In this way, certain element- or mineral-specific parameters can be established as a guide for the sampling program. The information, for example, may assist in determining sampling procedures in the field, especially the sample weight to be taken for "representative samples." Also, it may help assess whether analytical data, as provided by the laboratory, are acceptable. Finally, it may help determine the approach in data interpretation. However, all such simplified calculations are based on idealized, that is, unreal assumptions and conditions. As such, they represent one extreme end on the scale of probabilities. The reality is found somewhere away from this extreme, towards homogeneity. An example from a study of an eluvial gold prospect may be given for illustration: •Original sample weight: 20 kg (44 lbs) of rock gravel, crushed and ground to -0.18 mm (-80 mesh). •Au content: 20 grains of Au, average size of about 0.5 mm3 (0.03 cu in.) each = 7.5 mg each, making a total of about 150 mg Au in the sample = 7.5 ppm Au. Assumptions •Au occurs in the sample as free, discrete grains only. •Not more than one grain, if any, goes into each sample split (analyte) portion (20 grains of 7.5 mg Au each). •Analysis of original rock sample: 100 g sample for analysis, 20 kg/100 g = 200 samples 20 samples with 1 grain each: result, - 75 ppm Au. 180 samples with no grain: result, 0 ppm Au chances 1:9 •10 g sample for analysis:

Jan 1, 1996

By Wade E. Cooper

INTRODUCTION How accurate are past and present employee radondaughter exposure records of underground uranium miners employed in the United States? This often-debated question is essential for future substantiation of safe exposure limits. An apparent discrepancy between company-reported exposures and Mining Enforcement and Safety Administration (MESA) projected exposures was detected in 1977. For these reasons a need for an updated comparison of these exposure data was indicated. This paper gives some of the conclusions of the earlier study and compares more recent exposure records compiled by the Atomic Industrial Forum, Inc., with projected exposures based on sampling by Federal mine inspectors. EARLIER STUDY In its 1977 Annual Report (U.S. Department of the Interior, 1978), MSHA's predecessor, the Mining Enforcement and Safety Administration (MESA), reported that there was "an apparent discrepancy between Federal inspection results and company records." Both company records and MESA's projections from samples taken during routine Federal inspections indicated reductions in the average exposure of underground uranium miners from 1975 to 1977, but the MESA projections were over 4 times higher than the company-reported averages. This apparent discrepancy however, was based on a comparison of exposure data reported for all U.S. underground uranium miners. This projection more closely represented the average exposure of U.S. underground uranium mine production workers who worked 1,500 hours or more during the year. Exposures of such workers are reported each year by the Atomic Industrial Forum, Inc. (AIF) in summaries of exposure data reported to the AIF by uranium mining companies throughout the United States. (The AIF exposure summary for 1979 appears as tables A-1 and A-2 in the appendix of this paper.) Assuming that the average exposure for each exposure range category is the midpoint of each exposure range category, table 1 compares the estimated average exposures for U.S. underground uranium mine production workers who worked underground 1,500 hours or more each year in 1975 through 1977 with the exposures projected by MESA for those years. [Table 1. - Average Exposure and Projected Average Exposure for U.S. Underground Mine Production Workers Who Worked Underground 1,500 Hours or More During the Year. Company, MESA?' Reported- Projected Year (WLM) (WLM) 1975 1.59 5.68 1976 1.84 4.64 1977 1.68 4.08 1 Atomic Industrial Forum, 1976, 1977, 1978. 2 U.S. Dept. of the Interior, 1978.] Table 1 indicates that, even after adjustment to ensure better comparability an apparent discrepancy between Federal inspection results and company reported exposures for 1975-1977 exists; however, the apparent discrepancy diminished over the 3 years. Slade, 1977, explained some of the discrepancy between company records and MESA projections of miners' average radon-daughter exposures as follows: 1) Concentrations of radon daughters in some work areas can vary greatly during any one day. A variation from 0.3 WL to 17.0 WL has been measured in the same stope on the same day. 2) Seemingly simple abatement problems indicated by the regular Federal and State inspections were solved simply by manipulating the mine ventilation. 3) The methods used by mine operators to compute cumulative exposures were such that high radiation readings were seldom or never reflected in the records. For example, a work area sampled on Monday indicated a radon-daughter level equal to 0.2 WL and this was recorded. It was sampled again on Wednesday of the following week and the level was 2.2 WL. The miners were withdrawn or told to fix the ventilation, and when this was accomplished the area was sampled and found to be at 0.2 WL again. Although the miners could have been working in the higher concentration up to 6 days, this reading might never be reflected in their records. If it was recorded, only a fraction of the day on which it was discovered would be entered into the cumulative exposure calculation (time-weighted average). 4) Some of the mines visited used a mine average radiation concentration, and every employee working underground was given the same exposure per unit of time spent underground. As a result of the 1977 study, more stringent sampling and recordkeeping standards were proposed and public hearings held in 1977. The resulting new and revised health standards on radon-daughter sampling and exposure recordkeeping became effective August 30, 1979 (Mine Safety and Health Administration, 1979). Prior to these new regulations, radondaughter sampling requirements were on an "as often as necessary" basis (Code of Federal Regulations, 1978). The new regulations required practically all active work areas in underground mines to be sampled at least once every 2 weeks, with many areas requiring weekly sampling. They also required calendar-year exposure records of all underground

Jan 1, 1981

By W. A. Griffith

Fractional replication of factorial design, a general method for planning experimentation and for analysis of data obtained, is described as applied to a flotation investigation. This method leads to determination of optimum process conditions with minimum experimental effort. Its advantages over simple factorial design are demonstrated. A METHOD for planning experimentation and for analyzing the data secured will be demonstrated. This method, termed fractional replication of factorial design, employs a relatively small number of individual experiments to determine which of a large number of process variables are controlling, to determine which combination of levels of these variables is most likely to produce optimum results, and also to predict what results will be obtained with a particular combination of conditions not already tested. Although the general method is not new, having been developed by Finney in 1945,' the extent to which it can improve the effectiveness of applied research generally has not been recognized by metallurgists. The fractional replication procedure is particularly useful in flotation experimentation and an example from such an investigation will be used in the paper. However, it has equal value in any investigation in which similar experimental difficulties are encountered. In developing a flotation process for a particular mineral separation, the investigator is inevitably confronted with the following difficulties: 1—There are a large number of potentially important process variables. 2—Results of individual experiments are not highly reproducible, due in part to the difficulty in precisely controlling all the variables. 3—Considerable effort is expended in conducting individual experiments. 4—There are practical limits on the number of individual experiments which can be made. In situations of just such a type, modern statistical methods of planning experimentation and analyzing data have their greatest value. Applications of one such technique, called factorial design, to problems of this type have been described by Dorenfeld and others.'-' The simple factorial design is an efficient procedure when the investigator hopes to provide a comprehensive understanding of the effects and interrelationships of a small number of variables over a limited range. In applied research, this is seldom the main objective. Rather, the investigator usually wishes to determine which of the many potentially important variables are in fact controlling, which levels of the controlling variables will provide opti- mum metallurgical results, and what these results will be at optimum conditions. Interest in detailed trends is limited to the controlling variables and to levels in the region of optimum conditions. Simple factorial design has serious deficiencies for such objectives and is not the most efficient method of experimental design. Deficiencies of Factorial Design In a simple factorial design, an experiment must be made at every possible combination of each level of every variable, once these have been chosen and the levels of each to be included have been decided upon. As the number of variables or levels of each increases, the experimental program quickly reaches prohibitive size. For example, an investigation of only four variables, each at four levels, requires 256 individual experiments. Often upon completion of such an extensive program, it is found that one or more of the variables has metallurgically unimportant effects or that a poor estimate has been made as to the appropriate range of levels to be investigated. The result is that only a small proportion of the data obtained falls in the range of real metallurgical interest. Indeed, it frequently can be anticipated that certain combinations of levels of variables will not produce results of interest, but they still must be included so that the essential balance, or orthogonality, of the design will be retained. It may be true that factorial design will provide the greatest amount of information from a given number of experiments, but it does not necessarily follow that it will lead to the desired information with a minimum number of experiments. Much of the information provided may be of little value. Advantages of Fractional Replication The disadvantages of simple factorial design are overcome to a great extent by a modification known as fractional replication. This is a technique for sampling systematically the potential data of a full factorial experiment, that is, the data which would have been obtained if the complete factorially designed program had been completed. Only a fraction of the total array of experiments is made, but the experiments are chosen in such a way that the important advantages of factorial design and the accompanying analysis of variance are retained. The data obtained from the first group of experiments are used to determine which of several variables are controlling and which levels of these variables are most likely to produce the desired result. Unimportant variables and levels of variables then may be

Jan 1, 1956

By Susan T. Bagley, Kenneth L. Rubow, David H. Carlson, Bruce K. Cantrell, Winthrop F. Watts

Permissible exposure limits (PELs) have been established for gaseous pollutants, carbon monoxide (CO), carbon dioxide (CO2), nitric oxide (NO), nitrogen dioxide (NO2), and some gas-phase hydrocarbons emitted in diesel exhaust. There is, as yet, no PEL recommended for diesel exhaust aerosol (DEA), nor is there a standard method for sampling this aerosol. The University of Minnesota and the U.S. Bureau of Mines have collaborated to develop a personal diesel exhaust aerosol sampler (PDEAS) which utilizes size-selective inertial impaction and gravimetric analysis. During the field tests of this sampler, numerous air quality measurements were made in underground coal mines that use diesel equipment. The mine mean DEA concentrations for the five mines surveyed, determined with the PDEAS in the haulageway, was 0.89 mg/m3 with a standard deviation of 0.44 mg/m3. DEA contributed 52 % of the respirable aerosol at this location. In three of the mines filter samples were collected for DEAassociated polynuclear aromatic hydrocarbons (PAHs) and biological activity determinations. Two of the mines were also monitored for the major gaseous constituents found in diesel exhaust. In general, the PAH and biological activity levels were similar for all three mines, and indicate that up to 25 % of the haulageway concentrations may be contributed by outby diesel vehicles. Measured concentrations of CO, C02, NO, NO2, and SO2, were well below regulated levels. INTRODUCTION Diesel exhaust contains pollutant gases, such as carbon monoxide, carbon dioxide, nitric oxide, nitrogen dioxide, and gas-phase hydrocarbons, as well as DEA. Much of the health-related concern focuses on DEA and associated organic compounds (Watts, 1992a). A wide variety of these PAHs have been identified and some are known carcinogens and/or mutagens. The U.S. Mine Safety and Health Administration (MSHA) has proposed new PELs for these and other contaminants (MSHA, 1989). MSHA has also published an advance notice of proposed rulemaking to establish a separate PEL for diesel particulate (MSHA, 1992). The U.S. Bureau of Mines has collaborated with the University of Minnesota to develop and field test a PDEAS. The PDEAS is a three stage sampler based on the MSA' personal respirable dust sampler. It utilizes a respirable cyclone preclassifier followed by a 0.8 µm cut point impactor and afterfilter operating at a flow rate of 2 L/min. Respirable aerosol greater than 0.8, µm in size is collected by the impactor while DEA, less than 0.8 µm in size, is collected by the afterfilter. Hence, gravimetric analysis of the afterfilter permits measurement of DEA concentrations. This development and laboratory evaluation of the PDEAS were described previously by Cantrell (1990) and Rubow (1990). During field tests of the sampler, numerous air quality measurements were made in continuous miner sections of five underground coal mines that use diesel haulage equipment. These air quality measurements included levels of selected PAH and biological activity associated with DEA collected in the intake and haulageway areas of three of the five underground mines, and CO, CO2, NO, and NO2 in two of the mines. The objectives of this paper are to present the DEA and associated pollutant concentrations measured in these mines and to assess the impact of diesel face-haulage equipment on underground mine air quality. MINE DESCRIPTIONS The mines used for the PDEAS evaluation were designated J, K, L, N, and 0. Mines K, N, and 0 are located in the Western United States, while mines J and L are located in the East. Each mine produces high volatile, bituminous coal with shift production levels varying from 500 to 2000 tons/section. Seam heights varied from 1.5 to 3.0 m. Mines K and N use continuous mining to develop longwall panels. The others are strictly room-and-pillar operations using continuous miners. The number and types of diesel-powered vehicles used at these mines were described by Watts (1992b). Mines J, K, N, and 0 use diesel power to assist in a wide range of activities in addition to coal haulage. These included road maintenance, personnel and materials transport, lubrication, and welding. Mine L used only three diesel-powered shuttle cars to haul coal. SAMPLING AND ANALYSIS METHODS Aerosol Measurements Aerosol samples were collected in the mine portal area, the clean air intake to the continuous miner section, the haulageway one crosscut inby from the feeder breaker and belt, in the return airway, and on selected personnel. The haulageway sampling site was located near the point where the diesel-powered shuttle cars turn around to dump their loads. Additional respirable and DEA samples were collected and have been reported by Haney (1990).

Jan 1, 1993

By L. H. Munson, D. E. Hadlock, L. F. Munson, R. L. Gilchrist, P. D. Robinson

All uranium mills are required to perform sampling and analysis for radioactive particulates in their gaseous effluent streams and in the environment. Pacific Northwest Laboratory was requested by the U.S. Nuclear Regulatory Commission (NRC) to provide technical assistance to them for their Uranium Mill Health Physics Appraisal Program. In conducting appraisals, air sampling methods used at NRC-licensed mills were reviewed and several deficiencies noted. This paper includes only environmental and effluent particulate sampling although much of the information is applicable to both in-plant and environmental samples. First, the components of a proper sampling program are discussed: program objectives, program design, sampler design, analyses, quality assurance, and data handling. Then the specific deficiencies, or the "pitfalls" from the first 8 mill appraisals are discussed. The first consideration in establishing an air sampling program is defining the objectives of the program. What is air sampling suppose to accomplish? Many of the deficiencies we have observed have resulted because the desired objectives were not clearly established in the minds of the radiation safety staff. PROGRAM OBJECTIVES An environmental air sampling program ought to fulfill the following seven objectives. The first is to: 1) [demonstrate regulatory compliance]. Although a goal of most programs, regulatory compliance, is not well understood. One has not only to comply with the conditions of the source materials licensee, but one must also demonstrate compliance with 10CFR20 and 40CFR190. For example, 10CFR20.106 states: "A licensee shall not possess, use, or transfer licensed material so as to release to an unrestricted area radioactive material in concentrations which exceed the limits specified in Appendix B, Table II of this part .... For purposes of this section, concentrations may be averaged over a period not greater than one year." Even if a mill's license does not require sampling at the site boundary of maximum concentration, a sample may be necessary to demonstrate compliance with 10CFR20. Most mill personnel are painfully familiar with 40CFRl90.10, which states: "Operations.... shall be conducted in such a manner as to provide reasonable assurance that: (a) The annual dose equivalent does not exceed 25 millirems to the whole body.... of any member of the public as the result of exposures to planned discharges of radioactive materials, radon and its daughters excepted... from uranium fuel cycle operations..." This means a licensee's sampling program must give "reasonable assurance" that the member of the general public receiving in the most exposure gets no more than 25 millirems per year. The sampling program necessary to provide that assurance may or may not be a license requirement. However, merely meeting the license requirements and the explicit regulatory requirements does not necessariarly ensure an adequate effluent and environmental air sampling program. The second objective of the environmental air sampling program, is to 2) [identify the source(s) of contaminants]. This will include not only the routine program, but special sampling for verification of sources and nonsources. Only after sampling can a mill operator be assured that roof vents, laboratory hoods, and other localized ventilation systems are not making a significant contribution to environmental releases. An environmental sampling program should also allow the mill operator to fulfill the third objective, to 3) [estimate exposures]. Even before 40CFR190, a sampling program should have provided the mill operator with the information necessary to determine the dose to the "fence post" person, or at least to determine if doses were well below the 10CFR20 limits previously allowed. The program should 4) [detect and measure unplanned releases]. If there is a fire, a scrubber failure, or if a drum of yellowcake breaks open, measured releases will almost always be lower than conservative estimates. Whether or not a system to provide sampling during accidents is needed is almost always a cost-benefit decision. In general, uranium operations do not sample just in case an accident may occur. Yet they may decide on continuous air sampling in lieu of intermittant sampling partially because of the potential for accidents. Another objective of air sampling is 5) [to provide information on the effectiveness of control systems]. This is always a concern with new or modified equipment and may dictate sampling frequency in other situations as well. For instance, if a small leak in a bag filter cannot be detected by other means, then more frequent stack sampling may be indicated. A routine effluent and environmental monitoring program should also fulfill the sixth objective,

Jan 1, 1981

By D. K. Atwood

Experiments resulted in a satisfactory laboratory method for restoring permeability to clay-containing cores damaged by fresh water. Clay contents of a number of field cores were measured, and permeabilities of plugs from these same cores were then deliberately reduced with fresh water. This damage is attributed to swollen and dispersed clays occupying the pore space. After damaging, a number of experiments were performed to meaJure the amount of damage and to establish some means by which permeability could be restored. The experiments included flooding the damaged cores with water-miscible fluids such as salt water, acetone, isopropyl alcohol and ethanol. Permeability was not successfully restored in these experiments. However, part of the damage was repaired by flooding with oil; when water was removed by distillation in the presence of immiscible fluids such as air or toluene, permeability was completely restored. This evidence suggested that swollen and dispersed clays could be collapsed to their original volume by strong interfacial and capillary forces. It was further postulated that the required forces could be generated by flooding the damaged cores with a solvent partially miscible with water. The flooding experiments were repeated using n-hex-an01 as the partially miscible solvent. Permeability was restored to five of six damaged cores and substantially increased in the sixth. A large fraction of the restored permeability was retained even after water saturation was raised to its original value with 12 per cent salt water. INTRODUCTION Sharp reductions in permeability often occur when relatively fresh water contacts clay-containing formations during drilling and workover operations. These permeability losses are caused by removing inorganic ions from the environment surrounding the clay, and consequent swelling and/or dispersion of clay minerals into the available pore space.' This phenomenon is generally termed clay damage, fresh-water damage, or simply formation damage; it causes large losses in current revenue by preventing oil wells from making their allowable production. Attempts to repair the damage and restore permeability by flowing salt water solutions or brines through clay-damaged cores containing montmorillonite have been unsuccessful.' This irreversibility is thought to result from formation of brush-heap, or edge-to-face, structures when the dispersed clay is flocculated. The brush-heap structures occupy much more space than the close packed domains present before damage.' One solution of the problem is to destroy the clay-water brush-heap and thus restore permeability. Because no satisfactory method existed for restoring permeability to clay-containing formations damaged by fresh water, the work described in this paper was under taken. The laboratory experiments generally consisted of deliberately damaging fresh cores containing clay and then attempting to repair this damage by various means. Results indicate that generating strong interfacial forces within the pore space of damaged cores collapses the clay brush-heap and restores permeability. These forces are most conveniently generated by flowing partially water-miscible solvents, such as n-hexanol, through a core. THEORY OF THE DAMAGE PROCESS The most common clay mineral groups known to cause permeability damage to formations are the mont-morillonites, kaolins, chlorites and illites. These clays are constructed of particles which can adsorb water on their surfaces and edges and, in the case of montmorillonite, between layers of the basic particle itself. This adsorption increases as water salinity decreases. At low salinities the particles disperse into the aqueous phase. When the clays present in the formation are kaolin, chlorite and illite, dispersion accounts completely for permeability damage to porous media. However, unlike the other clays, montmorillonite particles can imbibe water and adsorb ions between layers of sub-particles, or platelets. These platelets have net negative charges on their faces and are held together by exchangeable (or removable) cations such as Na and Ca decrease in ion concentration (salinity) in the fluid surrounding a particle causes migration of water into the clay layers and disperses the basic particle, while diffusion removes the original exchangeable ions from between the platelets. Once these ions are removed, the facing negative platelets repel each other, causing the montmorillonite to swell until, for all practical purposes, the individual platelets are dispersed. For this reason, fresh-water* damage is much more severe in sands containing montmorillonite than it is in sands containing other clays. Many investigators have shown that even trace amounts of montmorillonite can be responsible for marked reduction in the permeability of reservoir sands in the presence of fresh water." ." Monaghan and others have shown that fresh-water damage in montmorillonite-containing cores cannot be

Jan 1, 1965

By J. U. Messenger

A technique is described whereby the resistance of an emudian to breaking can be quantitatively determined. Produced ailfield emulsions are usually the water-in-oil type and, accordingly, do not conduct an electrical current. However, there is a threshold of A-C voltage pressure above which an emulsion will break and current will flow. The more stable an emulsion, the higher the required voltage. A Fann Emulsion Tester, modified so that low voltages (0 to 10 v) can be accurately measured, is suitable. This technique has application in evaluating the effect of a demuksifier on the stability of an emulsion. Emulsions can, in essence, be titrated with demulsifiers by adding a quuntity of demulsifier, stirring, and measuring the voltage required to cause current to flow. Any synergistic effect of two or more materials added simultaneously can be followed accurately. A demulsifier that significantly lowers the threshold voltage (from 100 to 400 v to 0 to 10 v for the emulsions in this study) is effective and can cause the enlulsion to break. A demulsifier that will bring about this drop in the threshold voltage at low concentration ir very desirable. The technique is also well adapted for rapidly screening demulsifiers. INTRODUCTION Stable emulsions in produced reservoir fluids resulting from certain well stimulation and completion procedures are common problems. The use of suitable demulsifiers can often mitigate these difficulties. At the present time, a rapid and efficient method for selecting satisfactory demulsifiers is not available. It is badly needed. Reliance is now placed primarily on trial-and-error procedures. A new test method has been developed which permits a more rapid and precise selection of demulsifiers. It involves measuring the electrical stability potential of an emulsion before and after a demulsifier has been added. This paper describes this method and shows where it should have application in field emulsion problems. NATURE OF OILFIELD EMULSIONS Two immiscible components must be present for an emuhion to form; we are concerned here with crude oil and water. An emulsifier must be present for tin emulsion to be stable. J Emulsifiers can be substances which are soluble in oil and /or mter and which lower interfacial tension. They can be colloidal solids such as bentonite, carbon, graphite, or asphalt which collect at the interface and are preferentially wet by one of these phases. Unrefined crude oils can contain both types of emulsifiers, A popular theory is that, of the two phases in an emulsion, the dispersed phase will be the one contributing most to the interfacial tension.' Usually this phase contains the least amount of emulsifier. The stability of a water-in-oil emulsion is affected by the fol1owing: l) viscosity; (2) particle or droplet size; (3) interfacial tension between the phases; (4) phase-volume ratios; and (5) the difference in density between the phases. A stable emulsion is usually characterized by high-viscosity, small droplets, low interfacial tensions, small differences in density between its phases, and slow separatian of the phases. It also has low conductivity (high electrical stability potential). Water-in-oil and oil-in-water emulsions"' are both common; however, oil field emulsions are predominantly water-in-oil emulsions. The emulsions which commonly occur during oompletion and stimulation operations contain a combination of several of the following: acids, fracturing fluids (oil, water, acid), and formation water and oil. Produced emulsions usually contain formation water and oil. Emulsions form in oil wells because oil and water are mixed together at a high rate of shear in the presence of a naturally occurring or unavoidably produced emulsifier. During the completion and stimulation of productive zones, and while formation fluids are being produced, oil and water are very often commingled. These mixtures are formed into emulsions by agitation which occurs when the fluids are pumped from the surface into the matrix of the formation or produced through the formation to the surface. Restrictions to flow (such as perforations, pumps, and chokes)".'" increase the level of agitation; tight emulsions are more likely to form under these conditions. Often an emulsified droplet is an emulsion itself.'" Therefore, emulsion-breaking problems can be quite complex. The complexity can be even greater if a third phase (gas) is included. Demulsifiers operate by tending to reverse the form of the emulsion. During this process, droplets of water become bigger, viscosity is lowered, color becomes darker, separation of the phases faster and electrical stability potential approaches zero. Any of these effects could be followed as a means of determining emulsion stability. However, electrical stability potential is the most reproducible and most easily measured parameter for following the stability of a water-in-oil emulsion.

Jan 1, 1966

By P. D. Zemany, G. W. Sear, B. W. Roberts

Vanadium metal is embrittled by hydrogen at a temperature as low as 250°C when held in the presence of manganese metal and water vapor in a rough vacuum. It is established that the property changes are caused by the catalytic decomposition of water vapor at the vanadium surface and the diffusion into and solution in the vanadium of the resultant hydrogen. It is found that manganese is a necessary component of the catalyst. The manganese is transported in the vapor phase by an unknown molecule. A deuterium tracer experiment demonstates the role of water vapor in the embrittle-ment process. VANADIUM metal foils were observed to become embrittled' at a temperature of about 300 °C when held in the presence of manganese metal and a small amount of moist air, This paper describes the investigation to find the embrittling agent and an understanding of the relatively low temperature reactions that are involved. Experimental The vanadium metal foil used was prepared by cold-rolling and pack-rolling 32 mil sheet" in a series of steps down to 1 mil foil. The original observation was confirmed by sealing vanadium foils of 3 x 10 sq cm into individual Pyrex tubes with manganese powder† and a con- trol tube containing only the vanadium foil. These tubes were evacuated to 10 -5 mm Hg without baking and sealed. After heat treatment for 200 hr at 300°C, the control foil showed no change in duetility, whereas the foil contained in the manganese— containing tube was embrittled. The visual appearance of each was unchanged. A series of Pyrex sample tubes, about 2.5 cm diam and 25 cm long, were prepared, each containing a 3 x 10 sq cm piece of foil and 5 g manganese powder at the lower end of the tube. By reducing the time of anneal and the temperature of these samples, it was found that embrittlement could be created at 250°C in a time as short as 1 hr. Since the vanadium metal used here has been drastically cold-worked by rolling, it is assumed that it contains a maximum number of dislocations. To check the possible necessity of dislocations in this low temperature reaction, a vanadium foil sample was annealed in Vycor for 2 hr at 800°C to re crystallize and reduce the dislocation concentration. Metallographic examination showed grains which were not visible before annealing. The embrittlement procedure was carried out at 300°C and 3 hr. Upon checking the foil no embrittlement was observed. Further experiments demonstrated that about 6 hr at 300°C are required to create embrittlement in the foil. This delay in the onset of embrittlement in the vanadium foil suggests but does not prove that dislocation channels play a role in the embrittlement phenomena. If manganese metal is necessary for this low temperature embrittlement, do other elements in the transition metals group yield the same result? To check this qualitatively, a group of elements of similar atomic radii were obtained and sealed as before into Pyrex tubes with a sheet of vanadium foil. These tubes were annealed at 250°C for 6 hr and included (with radii)-2 A1 (1.4A), As (1.25A), Be (1.2A), Co (1.25A), Cr (1.45A), Cu (1.25A), Fe (1.25A), Ga (1.2A), Ge (1.25L%), Mn (1.3A), Ni (1.25A), Si (1.2A), Ti (1.45A), Zn (1.3A), air, H,O, 10 cm Hg of dry hydrogen, and MnO, powder. Upon testing the above sample foils for brittleness, only the manganese-containing tube yielded a brittle foil. Manganese Transport—To eliminate contact of manganese metal powder and vanadium foil, sample tubes were prepared with fritted glass barriers. The embrittlement reaction was still found to occur. Thus, the mode of transfer of manganese is certainly vapor transport. A vanadium foil was embrittled by this mechanism in an evacuated Pyrex tube for 8 hr at 300°C. By means of X-ray fluorescence analysis,' the amount of manganese added to the surface was established at 5 ±2 x 10 -6 g per sq cm. Since the average rate of manganese deposition is known, an effective average pressure of an assumed carrier compound can be computed. ___ P = M/T v2p mkT

Jan 1, 1959

By F. W. Jessen, James N. Howell

The accumulation of paraffin deposits in tubular goods has been recognized as a major production problem since the inception of the petroleum industry. This problem is not limited to any particular geographical area nor is it limited to a specific type of crude oil.' Generally speaking, "paraffin" deposition pertains to the deposition of any predominately organic material in flow lines, and possibly even at the sand face, which would hamper the production of oil. In some fields, a continuous effort is required to remove deposits of paraffin and in order to accomplish this, many unique methods have been devised. The best solution to this problem, however, is to prevent the formation of such deposits. One method which has been tried in a number of fields is the use of plastic pipe. The purpose of this investigation is to compare the relative effectiveness of several plastic materials to aid in the reduction or prevention of paraffin accumulations in surface flow lines. COMPOSITlON OF PARAFFIN DEPOSITS By definition, paraffin deposits are those materials which are insoluble in crude oil at the prevailing producing conditions of temperature and pressure. Such deposits1 s usually consist of small particles of petroleum wax intermixed with resins, asphaltic material, and crude oil. They may also contain a variety of foreign materials such as sand, silt, water, various metal oxides, sulfates and carbonates of iron. barium, and calcium. The petroleum waxes deposited in flow strings usually consist of both a "hard" and a "soft" wax fraction. These waxes are largely aliphatic hydrocarbons with smaller amounts of aromatic and naphthenic compounds. Nathan' has classified the hard and soft wax fractions. The aliphatic hydrocarbons present are those of high molecular weight with high melting points. Reistle3 pointed out that these high molecular weight compounds first separate from the oil due to a sharp decrease in solubility as the melting point increases. The identification of the resins and asphaltic materials rests, at present, on an arbitrary solubility procedure. Under certain conditions, materials which are insoluble in pentane (ASTM D-893) are defined as resins and asphalts. Subgrouping of these materials is made on decreasing solubility in benzene and carbon disul-fide. Shock' found some correlation be-tween the solvent response and the pentane insoluble content of paraftins: higher pentane insoluble fractions are less soluble in any of the commonly used commercial solvents. PARAFFIN CONTROL METHODS The methods used in oil fields to prevent and remove paraffin accumulations can be grouped into four general classes: (1) operative methods, (2) physical methods, (3) chemical methods, and (4) combination of any of these. Operative methods attempt to prevent the formation of paraffin deposits while the other methods are concerned primarily with the removal of these deposits. Plastic coated pipe has been used for a number of years to prevent cor- rosion in wells, and in manv instances paraffin deposits have -been greatly reduced. Field observations have indicated that plastic coated pipe not only reduced paraffin accumulation but in some cases eliminated deposition completely; however, data are needed to demonstrate the relative effectiveness of plastic materials. Deposition Apparatus The pipe used to determine the effect of velocity on rates of deposition was %- and 2-in. nominal diameter, and 5 ft in length. Steel, butyrate, rigid PVC, kralastic resin-type plastic pipes, epoxy coated pipe, PVC lined glass fiber pipe, and aluminum pipe were tested. Steel pipe was used as a control. Fig. 1 is a schematic diagram of the apparatus showing the relative position of the separate units making up the equipment. In order to facilitate the installation and removal of the test pipes in the apparatus, O-ring seals capable of sustaining pressures of 50 psi were provided at each end. Test pipes were submerged in a cold water bath maintained at or below room temperature by circulating water through copper cooling coils packed in ice. A hot water bath equipped with immersion-type heaters, stirrers, and a thermoregulator was used to maintain the temperature of the oil prior to introduction into the piping manifold. The capacity of the oil reservoir was 30 gal. A 33-gal/min centrifugal pump, capable of producing turbulent flow velocities in the test pipes, was used to circulate the oil through the system when using %-in. pipe; and a 70-galjmin centrifugal pump was used in later tests using 2-in. pipe. A by-pass arrangement made it pos-

By R. W. Bartlett

The rates of oxidation of tungsten have been determined at temperatures between 1320" and 3170°C and oxygen pressures to 1 amn using a surface -recession measurement technique. Above approximately 2000°C and 10-6 atm the rate is independent of temperature and can be calculated from gas collision theory assuming a constant reaction probability, e, of 0.06. Oxygen molecules react at surface sites where oxygen atoms have previously chemisorbed. This provides a direct pressure dependence at low pressures but at high pressures tungsten oxide molecule s form an adjacent gas boundary layer which lowers the PO2 at the tungsten surface. A correction for this effect using free-convection theory fits the rate data over the entire oxygen-pressure range from 10-8 to 1 atrn as well as data using O2-A mixtures. Below 10-6 atrn and above 2000°C, e decreases with increasing temperature because of desorption of oxygen atoms. Below 2000°C the rate decreases with decreasing temperature at all oxygen pressures following an apparent activation energy of 42 kcal per mole and depending on (Po2)n with n varying between 0.55 and 0.80. MOST of the previous tungsten oxidation studies have employed gravimetric methods and have been limited to temperatures below 1000°C where the weight loss associated with evaporation of tungsten oxides is negligible compared with the weight gain from oxidation.' At higher temperatures, oxygen-consumption rates have been determined from pressure measurements, usually at constant flow rates, by Langmuir,2 Eisinger,3 Becker, Becker, and Brandes,4 and Anderson.5 The sensitivity of this method decreases with increasing pressure and, with the exception of Langmuir's work, these investigations were confined to pressures below 10-6 atm. Above approximately 1300°C, depending on the oxygen pressure, the rate of oxide evaporation is greater than the oxide-formation rate and the recession of the tungsten surface can be measured optically without interference from an oxide layer. This was first done by Perkins and crooks6 who heated tungsten rods in air pressures from 1 to 40 torr at temperatures between 1300" and 3000°C. The present investigation of the oxidation kinetics of tungsten at high temperatures emphasizes oxygen pressures from 10-6 to 1 atm. This is the range of interest for earth atmosphere re-entry applications of tungsten for which little data were previously available. APPARATUS The apparatus is a modification of the type used by Perkins and crooks.' Ground tungsten seal rods, 6 in. long by 0.125 in. diam, were mounted vertically between two water-cooled electrodes, one fixed and the other having free vertical travel. The movable counter-weighted electrode is prevented from undergoing horizontal displacement by three sets of runners mounted at 120-deg intervals. Electrical contact is made by means of a water-cooled mercury pool. A 24-in. vacuum bell jar having a volume of approximately 267 liters was used as the reaction chamber with the sample holder mounted in the middle of the chamber. Power was supplied from an 800-amp dc variable power supply. Temperature readings were made by means of a Latronics automatic two-color recording pyrometer. With this instrument, corrections for emissivity are not necessary provided the spectral emissivi-ties at two closely spaced wavelengths are equal. Supporting measurements were made with a micro-optical pyrometer corrected for emissivity of bare tungsten and window absorptivity. The micro-optical pyrometer was calibrated against a National Bureau of Standards calibrated tungsten lamp and both pyrometers were periodically checked against the melting points of tungsten and molybdenum using the oxidation apparatus. Above 10-6 atm, pressures were measured with an Alphatron gage calibrated against a McCleod gage. At 10-6 atm, a hot-filament ionization gage was employed. A magnified image of the self-illuminated tungsten rod was formed using a 360-mm objective lens mounted outside the bell jar. When the experiment exceeded 1 hr, the image was focused on a ground-glass plate about 10 ft from the tungsten rod at about X8 and the recession of the thickness of this image was monitored with a Gaertner cathe-tometer. When faster rates were encountered, a 35-mm time-lapse cinecamera with a telephoto lens and bellows extension was substituted for the ground-glass plate and cathetometer. Diameter recession rates were determined from the photograph image projected on the screen of an analytical film reader. EXPERIMENTAL PROCEDURE After installing the rod in the apparatus and cleaning it with acetone, the system was evacuated to 5 1 x 10-5 torr. Before oxygen was introduced,

Jan 1, 1964

By W. B. Gogarty, W. C. Tosch

A new recovery process for producing oil under both secondary and tertiary conditions utilizes the unique properties of micellar solutions (also known as microemulsions, swollen micelles, and soluble oils). These solutions, which displace 100 percent of the oil in the reservoir contacted, can be driven through the reservoir with water and are stable in the presence of reservoir water and rock. Basic components of micellar solutions are surfactant, hydrocarbon and water. They may also contain small amounts of electrolytes and co surfactants such as a1cohol.r. The specific reservoir application dictates the type and concentration of each component. A salient feature of [he process is the capability for mobility control. Micellar solution slug mobility, by way of viscosity control, is made equal to or less than the combined oil and water mobility. Mobility control continues with a mobility buffer that prevents drive water from contacting the micellar solution. Laboratory and field flooding have proven that the process is technically feasible and that surfactant losses by adsorption on porous media are small. Introduction projects are under way to recover the maximum amount of oil under the most favorable economic conditions.' : New techniques are being developed to increase oil recovery,3" Polymer solutions are becoming an important means of controlling mobility in a waterflood. Thermal methods such as in-situ combustion and steam injection are being used in reservoirs containing highly viscous crudes. Surfactant flooding is receiving attention as a method of reducing interfacial tension to increase recovery.*'" Exotic recovery processes have been considered primarily for ' perations. Economics are unfavorable in most cases for tertiary recovery. studies at the Denver Research Center of the Marathon oil CO. have led to a new oil recovery method.* Micellar solutions (sometimes called microemulsions, swollen micelles, and soluble oils) are used to recover oil by miscible-type waterflooding. Basically, these solutions contain surfactant, hydrocarbon, and water. The method can be used in either secondary or tertiary operations. First, thc concept of thc process is considered in terms of the requirements for an effective miscible waterflood ing operation. Next, micellar solution properties are described including structure, composition, and phase behavior with reservoir fluids. Fluid characteristics are then considered as related to mobility control, and, finally, laboratory and field results are presented to illustrate the efficiency of the process. Concept of the Process Unit displacement efficiency and conformance determine the effectiveness of any oil recovery mechanism. In theory, a miscible waterflood should be capable of a 100-percent unit displacement efficiency with a correspondingly high conformance. Requirements for the slug of a miscible waterflood include (1) 100-percent displacement of oil in the reservoir contacted, (2) controllable mobility, (3) the capability of being driven through the reservoir with water, (4) a low unit cost to enhance economics, and (5) the ability to remain stable in the presence of reservoir water and rock. Micellar solutions satisfy requirements for the slug of a miscible waterflood process. Our discovery that these solutions acted as though they were miscible by displacing all fluids in the reservoir and by being displaced by water solved the miscibility problem. Adequate mobility control is possible by variations in solution viscosity through compositional changes. Economic requirements are met since micellar solution costs below $6/bbl appear possible, Mi cellar solutions stabilize surfactant in the presence of reservoir rock and water, thus reducing the importance of the problem of surfactant loss by adsorption. Fig. 1 illustrates schematically how these solutions are used. Operations start with injection of a micellar solution slug that serves as the oil displacing agent. Next, a mobility buffer of either a water-external emulsion or water solution containing polymer (thickened water) is injected to protect the slug from water invasion. Finally, drive water (water used in a regular waterflood) is injected to propel the slug and mobility buffer through the reservoir. Reservoir oil and water are displaced ahead of the slug, and a stabilized oil and water bank develops as shown in Fig. 1. Stabilized bank saturations are independent of original oil and water saturations. This means that, for a particular type of reservoir, the displacement mechanism is the same under secondary and tertiary recovery conditions. Oil is produced first in a secondary operation. For tertiary conditions, water is produced first. Movement of the slug through the reservoir is stabilized by the mobility buffer. An unfavorable mobility ratio usually exists at the interface between the buffer and drive

Jan 1, 1969

By John N. Dew, William L. Martin, `

This paper describes the results of a laboratory investigation conducted to obtain data for an evaluation of the in situ combustion process as a method of producing crude oil from reservoirs. Air and fuel requirements, rates of advance, com-bustion temperatures, and coke and fluid distributions are presented. The mechanism of oil recovery by in stiu combustion is discussed. Five crude oils ranging in gravity from 10.9 to 34.2"' API were prodrrced from a semiadiabatic, uncon-.solidnted sand pack by in situ combustion. Experimental conditions were varied over a wide range in order to determine the inter-relation-.ships of process variables. The mini-mum air flux requirement for self-sustained combustion was found to he less than 10 scf/hr-ft'l. The rate of advance of a self-sustained combustion zone was found to be nearly proportional to the air flux at the combustion front. The effects of presrure and injected air flux were studied in a series of experiments using a 21.2" API crude. A minimum air require-ment was observed at an air .flux of 20 scf/hr-ft'. The oil saturation con-sumed as fuel averaged 5.5 per cent of pore volume. The effect of air pressure was, found to be .small for experiments having high combustion eficiencies. This study should promote a better understanding of the problems and mechanisms involved in labora-tory investigations and field applications of the in situ combustion pro-cess. The data presented will be use- ful in the interpretation of results of field tests. When tempered with volu-metric sweep efficiencies, the data can be used in making preliminary economic appraisals of the process as applied to reservoirs containing high porosity unconsolidated media. INTRODUCTION The purpose of this work was to obtain laboratory data for an evaluation of the in situ combustion process as a method of producing crude oil from reservoirs. In situ combustion basically consists of (1) injecting air into a reservoir through selected input wells to create an air sweep through the reservoir, (2) igniting the crude at the injection well, and (3) propagating the combustion front through the reservoir by continued air injection. By this means, oil is swept toward producing wells in the area. The fuel for combustion is supplied by heavy residual material (coke) which has been deposited on the sand grains during distillation and cracking of the crude oil ahead of the combustion front. Recovery of petroleum by a combustion or heat wave process is not a new idea. F. A. Howard was granted a patent in 1923 on a process in which air and a combustible gas were pumped into an injection well and ignited.' Russian engineers reported on field experiments with a crude oil gasification process in 1935'. Other known early field tests include those conducted near Bar-tlesville and Ardmore, Okla., in 1942." More recently completed field tests include an inverted seven-spot by Sinclair Oil Co. in the Delaware-Childers field, Nowata County, Okla.'; a three-well and an inverted five-spot test by Magnolia Petroleum Co. in Jefferson County, Okla."."; and a test by California Research Corp. in the Irvine-Furnace field in Kentucky. The Worthington Corp. has completed a test in cooperation with the Forest Oil Corp. in Clark County, 111.l Several field tests are now in progress. Sinclair has acquired a 600-acre lease in the Humboldt-Chanute field, Allen County, Kans., and is under way with a large-scale operation. Three field tests are under way in California. The General Petroleum Corp. is conducting an inverted five-spot pattern test in the South Bel-ridge field in Kern County under a cooperative agreement with 11 other companies, including Continental Oil Co. California Research Corp. is conducting a four-well pattern test in Midway-Sunset field near Maricopa, and Richfield Oil Corp. is under way with a test in the Ojai field in Ventura County. Although the published information is valuable concerning results of field tests, little laboratory data other than that reported by Kuhn and Koch5 are available to aid in appraising the tests from a technical or economic standpoint. Engineering data needed to evaluate the process include the amount of air required per barrel of oil recovered, minimum injection rates which will support combustion, rates of advance, air required per unit volume of reservoir cleaned, amount of oil recovered, and amount of oil consumed as fuel. The present laboratory investigation was undertaken to provide these data for that portion of the reservoir swept by the combustion zone. The first phase of this investigation was exploratory in nature and was conducted at injection pressures less than 100 psig. Data were ob-

By L Forrester

The tube bundle system is an integral part of an underground coalmine’s gas monitoring system. The maintenance of these systems is vital to ensure the quality of the data produced. Integrity testing of the tube bundle lines is required monthly, as specified in Standards Australia AS/NZ 2290.3 (1990). The various forms of integrity testing are reviewed, including pressure testing and introduction of a known gas. This paper provides a recommended and standardised methodology for those techniques where none currently exists. A strengths, weaknesses, opportunities, threats (SWOT) analysis is performed. The parameters considered for the SWOT analysis include resourcing required by the mines, time for the testing to be performed, and quality of the results produced. The suitability of such integrity testing protocols to be used in a mine emergency situation is also evaluated.CITATION:Forrester, L, 2017. Tube bundle integrity testing methodologies, in Proceedings Australian Mine Vent Conference 2017, pp 129–136 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Aug 28, 2017