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By Jan Visman, James W. Parkinson

GENERAL INTRODUCTION Sample collection, preparation and analysis are all steps in a single process designed to provide information about a much larger amount of material than the sample itself. For example, information about the ash content of a unit train load of coal may be derived from a single, relatively small sample of perhaps a few hundred pounds (liters) extracted from the entire shipment. These three steps can be thought of as links in a chain, allowing the simple analogy that the strength of the chain, or, in other words, the value of the information is only as strong as the weakest link. Sample collection, discussed in Part 1 of this chapter, is critical because analytical procedures can do no more than reveal the characteristics of the sample presented to the laboratory. If that sample does not properly represent the population to be characterized, neither will the analysis of that sample. Sample preparation is also a critical part of the chain. Any change in the nature of a sample between the time it is collected and the time it is analyzed will appear to reflect the nature of the population. For example, sample preparation procedures that allow air to partially dry the coal sample before reaching the laboratory will cause the sample analysis to indicate a lower moisture content than the sample originally had. Other changes can be more subtle. Second only to moisture loss, oxidation reactions generally cause the greatest problems. Oxidation of a coal sample can alter surface properties, changing flotation response. In extreme cases, combustion parameters, such as caking or agglomerating properties or mineral composition, such as pyrite content, can change. Water samples can also be altered by oxidation. For example, ferrous iron can oxidize to ferric iron, possibly changing water quality parameters such as pH. Sample analysis, the subject of Part 2 of this chapter, is the final link in the chain. Obviously, no laboratory procedure can correct for problems created by improper sample collection and preparation. At the same time, poor analytical techniques will create incorrect information about the total amount of coal from which the sample was extracted (the population) in the same manner as improper sample collection and preparation. The key to gaining correct information about the population is to view these three steps as parts of a single process. Following proper techniques through only one or two steps of the process will not produce accurate information.

Jan 1, 1991

By G. Robert Moorehead, Peter T. Luckie, Harold L. Lovell, David J. Akers, James K. Kindig

Jigging is a process of particle stratification in which the particle re- arrangement results from an alternate expansion and compaction of a bed of particles by pulsating fluid flow. The vertical direction of fluid flow is reversed periodically. The rearrangement results in layers of particles that are arranged by increasing density from top to bottom of the bed. This response, developed from the many and continuously varying forces acting upon the particles, permits a solid-solid separation more related to particle density and less to particle size than any other "hydraulic-type" process. The stratification is usually carried out in a rectangular, open-top container called a jig, in which the mass of particles (termed a "bed") is supported on a perforated base through which the water flows in alternating directions. The coal particles, in addition to the vertically expanded and compacted bed motion, move continuously, horizontally across the supporting screen. Following the particle stratification, the particle bed is physically "cut" at a desired horizontal particle density plane to separate the desired clean coal product from the more dense refuse. The jig system includes means for continuously introducing the raw coal and for moving the water through the coal bed in a controllable manner, as well as for separating and removing the stratified particles from the system as two or more product streams. In coal preparation, this highly versatile unit operation is applied preferably to a wide size range of particles with top sizes up to 8 in. (20 cm) rather than to a closely sized fraction. In gravity ranges, the process has been applied to gold particles with a density of 19.3 and to coal particles having densities less than 1.30. Single jig washers have capacities from 5 (4.6) to greater than 700 tph (637 t/h) of feed coal. The separation results attainable by jigging have favored this unit operation as optimum for creating a clean coal product as required by steam coal specifications. Al- though the jig is used in preparing coals which are difficult to separate, its limitations to achieve both quality products and high recovery are being recognized in comparison with heavy media-based processes which make sharper separations from feeds having high "near-gravity" contents. The accu- racy of the densimetric stratification in the upper portions of the jig bed are less precise. It follows that coals with more than 10% near-gravity material

Jan 1, 1991

By Roe-Hoan Yoon

INTRODUCTION In 1960, coal accounted for 49% of the world energy consumption, an amount that was reduced to 29% in 1973 because of the availability of cheap oil. At that time, it seemed that oil would remain available for a long time in unlimited quantities. However, this situation changed drastically in 1973/74 when a series of closely spaced price increases from $3 per to $12 per bbl by mid-1974 hit both industrialized and developing countries. Another sharp price increase in 1979/80 to the $34 to $38 per bbl level also hit the world economy hard and, at the same time, set in motion powerful technology development forces for increased coal utilization. At this point, the price of coal was approximately $1.50 per MM Btu, while that of oil approached $6.00 per MM Btu. This huge price differential offered an incentive for developing new coal technologies including liquefaction, gasification, fluidized bed combustion, coal-water mixture (CWM), etc. The CWM technology was of particular interest to the utility industry, which consumes more than 80% of the coal mined in the US for power generation. In this technology, a powdered coal is mixed with water to produce a stable slurry that can be stored for an extended period of time without settling and is readily pumpable. Various reagents in the amount of approximately 1% by weight of the coal are added to inhibit sedimentation during storage and to reduce the viscosity for atomization in burners. The coal loading is in the range of 50 to 80% solids, depending on the particle size and its distribution. With very fine particles, it is difficult to increase the coal loading above 50%, and a binomial distribution helps increase the coal loading. The presence of water consumes a relatively small amount of the heating value of the coal during combustion; for a coal-water slurry containing 30% water, less than 5% of the calorific value of coal is usually consumed due to evaporation. The major advantage of burning coal as a slurry is that many of the oil-burning furnaces can be converted to coal-burning with a minimum retrofit cost. Considering the substantial price margin between coal and oil, the pay- back period for retrofit costs can be relatively short. Nevertheless, the retrofit cost can be further reduced if low-ash coals are used as feedstocks for CWM; there will be savings in the capital cost of installing bag filters or electrostatic precipitators that are designed to remove the ash from the combustion gases. Furthermore, the use of low-ash coals can minimize derating of boilers because the velocity of the combustion gases can be maximized without creating erosion

Jan 1, 1991

Application of Gy?s formula is appropriate for calculation of the Fundamental Error (FE) prior to samples being collected at any stage of the minerals process, provided that sampling parameters K and a (alpha) have been determined by calibration of the ores. Two types of calibration procedure are well established in the industry, the Hetrogeneity test and the 32-piece sampling tree experiment. The sampling tree experiment uses the variance and average grade of metal analyses from four series of samples at different nominal fragment size, as the basic input data. Pierre Gy suggested the cube as an appropriate exponent of the nominal fragment size for use in his equation. More recent work suggests that this exponent is variable and characteristic of specific ores and therefore requires calibration. The method described here explains the experimental procedure of the calibration. It is then possible to calculate a sampling nomogram using the sampling parameters K and a. This allows the sampler to determine a suitable protocol for the sampling event that will ensure that the FE does not exceed a predetermined precision at any point in the sampling procedure.

Jan 1, 2007

By John T. Cantwell

INTRODUCTION The process engineer usually is responsible for the design operating philosophy and/or day-to-day operations of a process. Since instrumentation is an integral part of the operation, it is essential that engineers understand the general capabilities of the different types of control equipment available. Many "noncontrol" engineers have become involved with instrumentation for machinery monitoring and control as well as other plant applications. The advent of the microprocessor has led to significant changes in control, both in systems configurations and man-machine interfaces. Today's concept is called simply "distributed control." What is distributed control? Distributed control is exactly what the name implies; the control system is divided into several functional segments and spread out to cover a process. The systems are distributed for physical, functional, and risk reasons. Before delving further into the specifics of distributed control, let's look at the evolution of control systems to see how we got here. Instruments initially were located near measurement and control points in the field. Operators physically had to go to the instrument to change setpoints or take measurements. As processes became more complex, it became evident that a central control area was required. This allowed an operator to monitor and control many variables. The operator's effectiveness was increased dramatically, which resulted in greater efficiency, better quality control, and lower personnel requirements. At the same time, plants became much larger, control applications became more complex, energy became expensive, and the industry became more competitive. All of these factors placed pressure on process and production engineers to get the most for the money. The result was a continuing push to put more instrumentation into a central control room to maximize efficiency and productivity and minimize manpower. This chapter deals in some detail with devices for measuring physical and chemical properties of coal; devices for measuring the weight and weight-rate of flow of coal; devices for the monitoring and control of conveyor systems, solids inventory, fluid flow, liquid level, density, and specific gravity. These instruments have a multitude of uses throughout a coal preparation plant. The discussions cover advancements in "on-line analysis," nuclear control devices, and distributed control using microprocessors, mainframes, and soft-

Jan 1, 1991

By Peter T. Luckie, Joseph W. III Leonard

INTRODUCTION In a bed of fine coal, water can be found in the interstices created by the particle surfaces and in the pores within the coal particles. The extent of the interstices voidage is obviously a function of the particle sizes and morphologies, as shown by the fact that the bulk density of coarse coal is greater than that of fine coal. After drainage, the voids can be completely or partially filled. By increasing the suction pressure across the bed, as is done in vacuum filtering, the quantity of water in the voids can be reduced. But eventually the increased suction pressure has little influence on the moisture reduction. In addition, the moisture in the pore structure of the coal is unaffected by the mechanical removal of the moisture in the interstices. When this condition is reached, the total moisture content of the coal can only be reduced further by evaporating the water. Evaporative drying is done for one or more of the following reasons: 1. To avoid freezing difficulties and to facilitate handling during shipment, storage, and transfer to the points of utilization. 2. To reduce the heat loss due to evaporation of the moisture from the coal during the combustion process, thus increasing heating efficiency. 3. To decrease transportation costs. The heating value of coal is equally improved for each percentage point reduction in the noncombustibles in coal. It is estimated that a reduction of 1%22 in the total moisture in the coal increases the thermal efficiency of the heat-raising process by about 0. Some coal buyers consider 1 % moisture content to be the equivalent of a 4% ash content.23 It is important to avoid drying the coal to too low a moisture level, since the complete removal of surface moisture to produce a bone dry product can result in a serious dust, wind lost, and safety problem. Surface moisture con- tents of 3% or less for shipped coal are not uncommon. However, the evaporatively dried coal may be lower, Y, to 1%, since the mechanically dewatered coal may be higher. Evaporatively dried coal can be treated (sprayed) with chemicals in order to control the dustiness and any freezing difficulties, thereby providing the producer with more operational flexibility. The evaporative drying of coal is essentially a process of simultaneous transfer of energy, usually in the form of heat, and water, in the form of vapor, from the coal. In order to remove the undesired moisture, it is necessary to raise the temperature of the water from the entering temperature of the feed stream, TF, to the boiling point of the water (usually taken as 212"F), vaporize

Jan 1, 1991

By James D. Hervol, Josepph W. III Leonard, Barbara J. Arnold

INTRODUCTION Dry concentration or pneumatic cleaning uses air currents as the separating medium. Pneumatic cleaning in the United States today is limited to three or four operations. In fact, the quantity of bituminous coal cleaned pneumatically has declined from its peak in 1965 of about 25.4 million tons (23.1 Mt) to its current level (1988) of less than 4 million tons (3.64 Mt) annually, as shown in Fig. 7-9 1. In 1940, pneumatic methods accounted for 15% of the bituminous coal and lignite cleaned in the United States as given in Table 7-32. Currently, pneumatic methods account for less than 2%. The largest air plant was built in Pennsylvania about 1968 with 14 units processing 1400 tph (1280 t/h) of 3/, in. X 0 (19 mm X 0) raw feed and two additional units retreating middlings. This same plant is one of only three or four plants still operating air-cleaning devices in the US. A wet plant was added in 1985 to increase the efficiency of cleaning the fines. The air plant is still used as a scalping operation for the coarse material. Five additional operations are either no longer in production or have discontinued the use of air tables within the last year. Wet cleaning methods are now being employed at the facilities that have discontinued air table operation. he advantage of dry cleaning techniques is the low moisture content of the clean coal product. However, to decrease respirable dust, mining operations must use water sprays on modem mining equipment. This water adds to the moisture content of the run-of-mine coal and decreases the effectiveness of dry cleaning processes that rely on low surface moistures in the feed to allow for good separations. Wet cleaning methods are preferred, especially since they also allow for much sharper separations. The advantage of dry cleaning techniques is the low moisture content of the clean coal product. However, to decrease respirable dust, mining operations must use water sprays on modem mining equipment. This water adds to the moisture content of the run-of-mine coal and decreases the effectiveness of dry cleaning processes that rely on low surface moistures in the feed to allow for good separations. Wet cleaning methods are preferred, especially since they also allow for much sharper separations. Despite dry concentration's drawbacks, research has continued into dry concentrating methods, including both electrostatic and magnetic separation techniques. The real application for future dry cleaning processes is probably at the power plant between the pulverizer and the boiler feed where particles are already dry and ground to fine sizes (- 200 mesh [ -0.075 mm]), increasing the effectiveness of the separation and also, possibly, increasing the liberation of clean coal from finely disseminated impurities. From a utility's viewpoint, pneumatic cleaning offers the best delivered Btu cost, based on the premise that a percent of moisture is just as detrimental as a percent of ash. Additionally, several other advantages are inherent in dry concentration techniques. The main advantage is that dry concentration re-

Jan 1, 1991

By J. Davitt McAteer

Dear Mine Operator, Training for new employees, refresher training for new employees, refresher training, and new task training can mean the difference between life and death for workers. Part 46 spells out how you can develop a training program to protect workers for on-the-job hazards. Together, labor, industry, and the U.S. Department of Labor reached a milestone with the development and publication of Part 46. We want to continue working together toward the next milestone, October 2000, when the regulations take effect. We want to make sure you have all the information you need about these new training requirements. Throughout the next 12 months, MSHA personnel will be holding regional meetings across the country, delivering information and sample training plans to your operation, and offering you help to develop your plan. If you are among the many operators who are already providing training to your workers, keep up the good work. The rule will tell you exactly what is expected. If you currently have no training program, we can help you develop one. A brochure is being distributed, which highlights the main provisions of the rule. It is designed to introduce the rule to you. More detailed materials will be delivered to you. If you want information right away, simply call us, or e-mail us. We also welcome your comments, suggestions, and success stories. Part 46 will be successful and beneficial to miners through our combined efforts. Together, we can make our mines safe and healthier for everyone. Sincerely, J. Davitt McAteer, Assistant Secretary of Labor Mine Safety and Health Administration

Jan 1, 1999

By Richard B. Muter

In determining the layout or combination of unit operations to be utilized in a modem preparation plant, several factors must be taken into account. Among these are the washability data, size consist data, the particular market or markets for the coal, the mining method used, the degree to which the coal must be prepared, expected fluctuations in raw coal and markets, and the overall economics of the process. In addition, there are the health and safety aspects of coal utilization and preparation. Chapter 1 of this book discusses the characteristics of coal and coal markets, while Chapter 2 deals with the design of preparation plants. Once the unit operations for a particular plant have been decided upon, these arrangement may be depicted by using a flowsheet. A coal preparation plant flowsheet is a two-dimensional graphical representation of the sequence of operations, the arrangement of machinery, and the flow of materials for a particular coal cleaning operation. The flowsheet is usually qualitative in nature, becoming more quantitative as material balances, water balances, numbers and sizes of various pieces of equipment, etc. are added. The usual convention in preparing a flowsheet is to show the feed flowing from left to right, starting at the top left and working down as in an all-gravity process. Various symbols are used for each unit operation as depicted on a flowsheet, and Fig. 14-37 is a compilation of the commonly accepted international standard symbols for each unit operation. Fig. 14-38 through Fig. 14-40 are flowsheets of various coal cleaning processes as published in the January 1976 issue of Coal Age. Each process has its own unique features which, among others, depend upon the coal being cleaned, the coal market, and the mining operation. Fig. 14-38, for example, is a flow diagram for a jig plant preparing steam coal from two strip mines located a few miles apart. In addition to the jig washer, cyclones are used to treat the finer size coal. Fig. 14-39 is a flowsheet of a heavy media plant using a heavy media washer for + %-in. (+6.3-mm) coal, froth flotation for -28 Tyler mesh (-0.6 mm) material, and dewatering phase units (dwp) for Y, in. x 28 Tyler mesh (6.3 x 0.6-mm) cleaning of steam coal. In addition, thermal drying, centrifuge drying, and the use of vacuum disk filters and thickeners for dewatering are depicted. Fig. 14-40 is a flowsheet of a plant producing metallurgical coal. In addition to the heavy media and froth flotation circuits, a tabling circuit is also employed. These flowsheets are intended to give the reader an example of how the various unit operations for coal cleaning may be linked together. Figs. 14-41 and 14-42 illustrate the conversion of block diagrams into an IS0 prescribed set of symbols.

Jan 1, 1991

By Richard B. Muter

1. Coal Preparation Terms (General) 1.1 Coal preparation-collectively, physical and mechanical processes applied to coal to make it suitable for a particular use. 1.2 Run of mine (ROM coal)-coal produced by mining operations, before screening, crushing, or preparation. 1.3 Raw coal-coal that has received no preparation other than possibly screening or crushing. 1.4 Raw coal feed-raw coal supplied to a plant or machine, in which it undergoes some form of preparation. 1.5 Coal cleaning-the treatment of coal to lower the mineral matter content (ash). 1.6 Cleaned coal; clean coal-coal produced by a cleaning process (wet or dry). 1.7 Middlings-a product of coal preparation that, by reason of its ash content, is intermediate between coal and discard. It follows therefore that the relative density of middlings is intermediate between those of coal and discard. Middlings may be reprocessed. 1.8 True middlings; bone comparatively high ash particles so nearly homogeneous that their quality cannot readily be improved by crushing and recleaning. 1.9 False middlings; interbanded middlings-middliigs in which the particles consist of bands of coal and shale, and from which the coal may be liberated by crushing 1.10 Refuse-waste material in the raw coal which the cleaning process removes. (See also discard; dirt; stone, No. 1.12). 1.1 1 Reject-the material extracted from the feed during cleaning, for retreatment or discard. 1.12 Discard; dirt; stone--the material extracted from the raw coal and finally discarded. 1.13 Recirculation-the operation in which the whole or part of a product from a process is returned to the feed to the process, e.g., the return of the crushed overflow from a screen to the screen feed for rescreening. 1.14 Foreign coal-coal received at a preparation plant from a colliery other than that to which the plant is attached. 1.15 Imported coal-coal coming from a foreign country, or other state within the country. 1.16 Low-grade coal combustible material that has only limited uses owing to undesirable characteristics (eg., ash content or size). 1.17 Segregation-partial separation of a previously mixed material into its constituents, occurring as a result of differences in either particle size or relative density. 2. Cleaning Characteristics 2.1 Washability-amenability of coal to improvement in quality by cleaning. 2.2 Float-and-sink analysis-the division of a sample into relative density fractions with defined limits, the proportions of the fractions being expressed as percentages of the total sample, commonly with an indication of the ash percentage (and other characteristics, if required) of each fraction.

Jan 1, 1991

By John H. Weigand, Stephen V. Crum

"VIBRONICS, INC. instrumented and monitored a residential structure for response to,blasting at aMidwestern surface coal operation. The residence was owned by the mining company and was extremely close to the operation. Blasting was conducted within 120 feet (36.5 meters) of the test structure. Up to seventeen (17), four (4)-channel seismographs were used during the monitoring period. The basement walls and floor were monitored. VIBRONICS, INC. also monitored a brick chimney in the basement and attic. Structural responses were then compared to outside vibration measurements taken in the soil near the foundation."

Jan 1, 1998

The question of earth models has repeatedly arisen in our work. An accurate representation of the seismic properties is required for three reasons: 1.To be able to determine from a set of received arrival times, the location of a seismic source in the earth, and secondly the degree of accuracy required in the model used for calculating source location from the set of arrival time differences. 2. To be able to determine the expected arrival times at an array of geophones produced in response to a hypothetical source in the earth. 3. To be able to estimate received signal strengths more accurately. The work reported here on earth models is based on information from sever- al consultants and from others who expressed an interest in the problem and supplied information to us. II. COAL MINE GEOLOGY On one of our earlier assignments for the Bureau of Mines, Earth Science Research Inc. of Cambridge, Massachusetts prepared for us a short description of the lithology to be expected at coal mine sites. This description follows, together with the ranges of compressional seismic velocities (Figure I*) associated with typical materials comprising the layered structure of a coal mine area. Coal is primarily associated with fresh water sediments including sandstones, shales, and clays, and occasionally may be metamorphased to varying degrees. In the Appalachian Basin the coal beds occur within cyclical sequences of non-marine shales, sands tones, conglomerates, limes tones, and clays. The beds range in thickness from a few inches to 60 feet, averaging between 2 feet and 10 feet. They have generally broad areal extent, occasionally up to 5,000 square miles, and have an overall tabular or lens-like shape. Within a particular lens, local changes in thickness are normal.

Jan 1, 1974

During the first quarter of 1973 ADL worked closely with PMSRC staff, under an extremely compressed time schedule, on all aspects of the detailed planning, organization and overall coordination and preparation of the lectures and in-mine demonstrations for the Bureau's Technology Transfer Seminar on Mine Communications given in March of 1973 to representatives of the mining industry. Our efforts centered on the detailed organization and preparation of each of the five technical seminar lectures and associated supporting material, and the coordination of tasks assigned to ADL and other seminar participants. Revised and expanded drafts of the seminar papers were prepared from rough draft versions obtained from PMSRC, Collins Radio and ADL staff. Measurements were made to gather key data on the operation and performance of each of the following systems installed in the Bruceton Safety Research Mine; call alert paging, roof bolt paging, section wireless radio, and guided wireless radio systems. These data were analyzed, manufacturer's equipment specifications utilized, and calculations made to provide performance curves and data for each of the above systems. A substantial amount of artwork was conceived and prepared for 35 m slides, system identification posters in the mine, and seminar handouts. This artwork included some forty 8-1/2" x 11" line sketches, graphs, block diagrams, circuit diagrams, coverage maps, and other line drawings; five 30" x 40" block diagram system identification posters suitable for in-mine use; a 20" x 30" detail perspective illustration of a representative coal mine layout; forty viewgraphs; and seventy 35 m slides of the artwork and word charts. Conferences, discussions and review sessions were held with conference participants to help coordinate the various efforts, obtain technical information, and make final plans regarding the lecture presentations, associated visual aids, and the communication system installations to be demonstrated in the Bruceton mine. These meetings included final systems checkouts and dry run presentations and reviews of the lectures and mine demonstrations. This phase of the seminar effort concluded with R. Lagace and R. Spencer of ADL participating in two days of seminar presentations in the lecture hall and in the Bruceton mine.

Jan 1, 1974

The instrumentation specification in the National Academy of Engineering (NAE) report of March, 1970, set forth some rather general guidelines that the seismic surface system should follow. The fact that there was no comparable equipment in existence at that time, and the need to produce a system from presently available equipment, was spelled out in that document. The features that the system should include were listed, and included: • Quick and simple deployment • Portability • Battery-powered operation • All-weather operation • Computational simplicity and speed • High reliability and long shelf-life • Dual service for location and communication • Adaptability to widely varying seismic velocities. topography, and geologic structures • Minimum maintenance • Capability of continuous operation for extended periods, and • Reasonable cost Since that report, there has been a substantial amount of field work addressing the trapped miner detection and location problem carried out by Westinghouse Corporation under contract with the Bureau of Mines. Two complete surface systems have been designed, built, and field tested and substantial documentation has been produced on the mine environment and background noise using these systems. These systems, built from off-the-shelf equipment, have been designed with maximum flexibility in mind in order to explore what con¬figuration a field unit should have.

Jan 1, 1974

By Clément F. Bernier

One of the chief sources of the world's supply of asbestos lies in a belt of ultrabasic rocks which runs northeastward through an area called the Eastern Townships, south of the St. Lawrence River in the Province of Québec. The productive portion of this belt extends from the town of Asbestos in the south, for a distance of some 9,5 km to beyond the village of East-Broughton. The first discovery of asbestos in this region was made in 1874. Only crude fibre was produced until 1888 when the first mill was erected near the town of Black Lake. Since the inception of the industry, almost 100 years ago, no less than 100 different compa¬nies have been formed and 46 different mines have been operated. There are presently 5 active companies in the area providing direct employment for 4100 workers, down from 6000 during the seventies.

Jan 1, 1984

By John C. McDonald

CONTROLLED cold work is used between solution heat treatment and precipitation heat treatment for producing certain tempers of the commercial aluminum base alloy 2219 (designation of the Aluminum Association, U.S.A.) which contains 6.3 pet Cu as the major ingredient responsible for the age hardening. The complete composition limits for this alloy are listed in Table I. The alloy has been described in detail,' and the control of the heat treatment has also been published.2 Beneficial effects of such cold work in other alloys have also been pointed out.3'4 NO data have been published on the effects of varying amounts of cold work under fixed aging conditions. In connection with an investigation of the possibility of providing the desired cold work by explosively generated shock waves, it became desirable to investigate the effect of variable cold work, and to compare the re -sults with those obtained from explosives. The general principles of explosive hardening are well-described in the literature.' All material used was guaranteed by the supplier

Jan 1, 1968

By T. Kilner, A. Plumtree

DURING an investigation of electro-deposited silver structures, samples were prepared for metallographic examination by cold mounting in plastic, grinding on successive grades of emery paper down to 3/0, and chemically polishing by swabbing using the chromic acid solution described by Gilpin and Worzala.1 Attempts to etch these samples using the standard solutions described for silver (e.g., 5 pet KCN-5 pet Na2S2O8, H2O2-NH4OH, and various potassium dichro-mate solutions) all failed to give good results due to staining of the samples and to rapid etching. The staining was caused by the chromic acid polishing solution being trapped in small fissures between the sample and the mounting plastic, and also in small fissures in the sample itself. To overcome these difficulties, an etchant was developed which prevented staining at the same time as it slowly etched the sample. This resulted in a very clean, crisply etched surface as shown in Figs. 1 and 2. This etch consisted of 10 ml of orthophosphoric acid, 10 ml of distilled water, and 2 drops of the polishing solution noted above,' which is made by mixing 100 ml of saturated CrO3 solution, 45 ml of 10 pet HC1 solution, and 800 ml of distilled water. The etching procedure involved taking the final polished sample, either immersing or swabbing in the etchant for a period of 1 to 2 min, rinsing as quickly as possible in distilled water, alcohol, and ethyl ether in that order, and then immediately drying. This etch is easily controlled due to its slow rate of etching, and produces samples with clean, sharp surfaces. Pits due to overetching produced varying contrast effects when viewed under polarized light, and are therefore obviously useful for revealing many structural details within the sample. Another effect of overetching was to produce a height varia-

Jan 1, 1968

By J. H. Swisher

ALUMINUM deoxidation equilibrium in liquid iron has been the subject of many investigations. Sawamura and Sano1 have written a critical survey of the literature on this subject and consider the data of Gokcen and chipman2 and of d'Entremont, Guernsey, and Chip-man3 to be most reliable. The present study was undertaken to check these data and extend the range of the experiments to lower temperature. The experiments consisted of equilibrating 5-lb Fe-Al melts with recrystallized alumina crucibles at 1580o + 10oC, and analyzing the solidified ingots for aluminum and oxygen. The electrolytic iron stock contained 100 ppm C, 20 ppm 0, and trace amounts of other elements.* The stock was induction-melted in an atmosphere of 5 pet H2 in argon to attain equilibrium between the melt and the crucible. The temperature was measured with a W, 3 pet Re/W, 26 pet Re thermocouple, and the equilibration time was about 4 hr. The results are plotted in Fig. 1 along with curves obtained from the data of d'Entremont et al.,3 for temperatures of 1740o and 1910°C. The present results can be seen to be consistent with the previously reported high-temperature data. The reaction under study is AI2O3 (s) = 2 Al (l) +3O [1] for which the deoxidation product is Kl =[% Al]2 [%O]3 [2] (Under the experimental conditions, Fe A12O4 is not expected to form.4) In Fig. 2, values of log Ki evaluated at 0.01 pet A1 are plotted against 1/T, using data obtained from all the investigations under consideration. The deoxidation product is plotted in Fig. 2 in lieu of the equilibrium constant (normally obtained by evaluating Ki as pet A1 — 0) because of the uncertainty involved in extrapolating to zero concentration. The difficulty in extrapolating the present data for 1580°C is apparent curvature in the log Ki vs pet Al plot. This curvature is perhaps due to the uncertainty in oxygen analysis for concentrations of 5 ppm and below. For the data of Gokeen and chipman,' the extrapolation is also difficult because of experimental scatter. The line drawn through the points plotted in Fig. 2 may be represented by the equation:

Jan 1, 1968

By H. L. Luo

SYSTEMATIC investigations of the Fe-Ga system have been reported only very recently."' The maximum solid solubility of gallium in a-Fe is nearly 50 at. pet at 900°C. However, from Ref. 1, it was not evident that the a-Fe solid solution could be retained successfully beyond 17.38 at. pet Ga by solid-state quenching. The present investigation reports the retention of a-Fe solid solution at 50 at. pet Ga by quenching from the liquid. An ordered phase of CsC1-type B2) structure was observed between 34 - 50 at. pet Ga. Since it was considered very probable that the CsCl structure would occur at high temperatures, alloy filings were also quenched by the conventional quenching technique. In addition to the CsCl phase, a second ordered phase of BiF3-type (DO3) structure was found in the range 25 - 30 at. pet Ga. Alloys were prepared from elements of 99.99 pet purity or better, induction-melted in alumina crucibles under hydrogen. After reweighing, the alloy ingots were cast into wires under argon. From the weight losses and the reproducibility of the lattice parameters, compositions were estimated to be within ± 0.3 at. pet. The techniques of quenching from the liquid state were reported before.3-5 Prior to quenching, a small section of cast alloy wire (30 - 50 mg) was melted in an alumina insert under an argon flow. The quenched specimens were in the form of flakes, typically 1 sq mm in area. For solid-state quenching, alloy filings passing 200 mesh were sealed under a reduced helium atmosphere in a thin-bottom silica tube. After heating for -30 min at the desired temperature in a vertical furnace, the sealed tube was rapidly dropped into ice water so that the thin bottom of the tube broke on impact. The quenched alloy filings were always ferromagnetic and could be collected by a magnet. X-ray diffraction patterns were taken with iron-filtered cobalt radiation in a 114.6-mm-diam Debye-Scherrer camera. High-angle lines were always resolved and spacings were computed relative to ? (CoKa1) = 1.78890Å. Lattice parameters were obtained from extrapolation against the Nelson-Riley function. The variation of lattice parameter with composition is shown in Fig. 1, together with the data of Dasarathy and Hume-Rothery.1 Uncertainties in the present measurements are within the dimensions of the symbols or indicated by error bars. X-ray diffraction lines indicative of CsC1-type ordering could be clearly identified for alloys of 34 - 50 at. pet Ga quenched from the liquid and alloys of 35 - 41 at. pet Ga quenched from -975°C. Within experimental error, no difference in

Jan 1, 1968

By R. Taggart, R. H. Ericksen, D. H. Polonis

MarTENSITIC a has been observed to form spontaneously from the retained ß phase during the preparation of thin foil specimens of metastable Ti-Cr alloys containing from 6.9 to 20 wt pet Cr. Similar spontaneous martensite reactions have been reported in thin foils of 0 brass' and other alloys.2 4 The absence of retained austenite in iron-based alloys has also been attributed to spontaneous decomposition during thinning.5 The present work indicates that a unique situation occurs during which the spontaneous transformation takes place when the transitional ? phase is present in the as-quenched or partially aged ß phase. Alloys containing 6.9, 7.0, 8.0, 12.0, and 20.0 wt pet Cr were prepared by the levitation melting of "io-chrome" chromium and iodide titanium. The 0.5-in.-diam ingots were vacuum-annealed at 1000oC, and wafers 0.020 in. thick were then cut from the ingots. These wafers were wrapped in molybdenum foil, encapsulated in Vycor under a reduced pressure of purified helium, and then held for 30 min at 1000°C. The specimens were quenched in water to retain the metastable high-temperature ß phase. The quenched alloys were thinned by mechanical grinding to about 0.005 in. thick, then electropolished in a solution of 300 ml methyl alcohol, 175 ml n-butyl alcohol, and 30 ml perchloric acid at a temperature of -40°C. Needle specimens 0.005 to 0.010 in. diam were taken from each ingot and heat-treated with the foil specimens. X-ray diffraction patterns indicated the structure of the 6.9, 7.0, and 8 wt pet alloys to be a

Jan 1, 1968