United States Environmental Protection Agency Environmental Monitoring Systems Laboratory Research Triangle Park NC 27711 Research and Development EPA-600/S4-81-032 Aug. 1981 Project Summary Design of a Laboratory for Particulate Analysis R. J. Lee, J. S. Lally, and R. M. Fisher In this study the need for a state-of- the-art laboratory for paniculate anal- ysis, particularly asbestos, is reviewed. The proposed equipment and operating expenses are justified, and a conceptual framework for the laboratory is formu- lated. The basis for selection of opti- mum equipment and the results of a detailed survey of equipment manu- facturers are given. The design of the laboratory, the availability of skilled personnel, and a review of analysis methodology are summarized. It is concluded that c'urrent and past problems in particulates analysis can best be resolved by organizing the laboratory as a center of excellence. Functions of the laboratory should include methods development, train- ing, refereeing, standard sample de- velopment and evaluation, and the analysis of difficult samples. It is recommended that an advisory panel of experts be established to review the scientific quality and effectiveness of these activities. An acknowledged expert in asbestos analysis should be the director of a staff of seven to fourteen highly qualified members. Fourteen is suggested as the optimal size of the staff. The initial capital cost for laboratory instrumentation and specialized air- handling equipment is estimated at $764,000, excluding the cost of the building. Start-up within one year after completion of the building is believed to be achievable. Minimum staffing and an initial level of support of $308,000 per year are recommended to inaugurate the proposed laboratory. At the optimal staffing, an operating budget of $534,000 per year is antici- pated with about $260,000 generated by requests for services from outside groups or agencies. This Project Summary was devel- oped by EPA's Environmental Monitor- ing Systems Laboratory, Research Triangle Park. NC, to announce key findings of the research project that is fully documented in a separate report of the same title (see Project Report ordering information at back). Introduction The assessment of air quality and other environmental factors for effects on health, control strategy, standards setting, and compliance demands ac- curate monitoring data. Establishment of relationships between health effects and environmental levels have suffered from the lack of proven monitoring methodologies for the identification and quantification of the different species of asbestos. For some time the analysis of asbestos by electron microscopy has been a source of scientific controversy. The highly elongated shape of all asbes- tos material has long been recognized as a determining factor in the produc- tion of adverse health effects in exposed individuals. In the past, morphological identification of asbestos by phase con- trast optical microscopy was the only reliable method for monitoring the con- centration of asbestos fibers in the work place. The basic assumption in the use of this method is that any fibrous particle is asbestos. This technique is only effective ------- in environments where asbestos is known to occur in significant quantity. Optical microscopy is not reliable for monitoring asbestos fibers less than 0.5 //m in diameter and 5 fjm in length or for low concentrations. Accurate knowledge about the occurrence of such suboptical particles has become increasingly im- portant as concern has increased about their potential health effects. Tradition and acceptance of optical data on asbestos by the medical com- munity prompted attempts to extend the use of optical microscopy to environ- mental monitoring. Electron microscopy has the desired resolution for suboptical determinations but requires a much higher level of sophistication for sample preparation, counting, and identification of asbestos. Electron microscope meth- ods for suboptical particles have been developed, but with limited success. As a result, electron microscopy is not gen- erally regarded as a quantitative tech- nique for the measurement of "asbestos." To strengthen national environmental research, EPA commissioned the design of a model participates analysis labora- tory, with an emphasis on asbestos. Specific objectives were development of specifications and recommendations for a laboratory with special emphasis on the identification and measurement of serpentine and amphibole asbestos. Specimen preparation methods; clean room standards; and equipment for optical microscopy, x-ray diffraction, electron diffraction, and computer data processing were to be evaluated and prescribed. The number, qualifications, and availability of all personnel neces- sary to supervise and operate the facility were to be defined. This report addresses EPA needs for a particulates analysis laboratory and contains recommendations based on extensive experience in this area by U.S. Steel Research Laboratory. In addition to utilization of customary light and electron optical methods, the adoption of newly developed techniques for auto- matic measurement of particle size, shape, and composition is highly recom- mended. These methods have been in use in the U.S. Steel Research Labora- tory for three years and have proven to be rapid, accurate, and consistent in a wide variety of samples. The report contains the following sections. The conceptual framework, rationale, justi- fication, functions, setting, and recom- mended support levels for the laboratory are described in Section 1. The recom- mended methodology is discussed in Section 2 with emphasis on emerging techniques. In Section 3 the physical plant is described; in Section 4 the selected instruments are discussed; and in Section 5 personnel requirements are specified. Section 6 provides an estimate of initial and annual costs and the timetable required to bring the laboratory into existence. Conclusions Functions and Operation The creation of a laboratory devoted to developing and maintaining excellence in the field of particulates analysis, particularly asbestos, should be of the highest priority. The establishment of this laboratory must be the responsibility of the Federal administrative agency. No other organization has the resources to acquire state-of-the-art instrumentation on a continuing basis, to assemble a well trained and experienced staff, and to commit them to the long-term objec- tive of improving particulates analysis methods. The primary service function of the laboratory should be that of a center of excellence. It would provide a wide variety of essential services to other laboratories or agencies concerned with the acquisition or interpretation of data about the occurrence of particulates. These functions would include acting as a national reference laboratory, per- forming difficult particulate analyses, acting as a quality assurance laboratory, assisting in contract monitoring, assist- ing in enforcement actions, providing training, and performing methods de- velopment in the area of particulate analysis. It is presumed that the proposed facil- ity would be located near an existing national laboratory and would be housed within its administrative structure. However, to effectively carry out the multiplicity of functions described and to attract the caliber of staff required, the laboratory should be staffed with highly qualified specialists setting their own priorities. Every effort must be made to insulate the laboratory from sudden changes in focus or priority, yet the laboratory's objectives and projects must be responsive to agency needs. The formation of an advisory panel of knowledgeable persons from govern- ment agencies, academic institutions, and industrial laboratories could pro- vide peer review of programs, evaluate progress, and assist in setting long-terml goals. ™ Approximately fifty percent of the operating budget should cover the cost of methods development, participation in collaborative analysis programs, enforcement assistance, technical pub- lications, and travel. The remainder of the support could be derived from services charged to groups requesting such services. Analytical Methodology The methods of analysis required in the laboratory range from binocular screening, phase-contrast and polar- ized-light microscopy to scanning and transmission electron microscopy with capabilities for x-ray spectroscopy and electron diffraction. For suboptical par- ticulates the scanning electron micro- scope (SEM) can provide particle infor- mation based on manual characterization of morphology and composition. With newly developed digital beam-control devices, automated measurement of particle size, shape, and probable identity are also possible. The scanning-trans- mission electron microscope (STEM) will permit conventional manual x-ray and electron diffraction analysis and with the addition of beam-scan-control accessories automated particle charac- terization. The SEM and STEM instru- ments provide similar chemical and size information about particles but on an increasingly finer scale. Correspondingly, an increased level of sophistication is required to operate and maintain the instruments and to interpret the infor- mation derived from each. The sample flow and proposed methods of analysis are shown in Figure 1. Facilities The general design of a building (Fig- ure 2) to house the proposed facilities is based on the following general premises. It is to be a freestanding, one-story structure large enough to house an optimal staff and all essential require- ments. The structure will include a self- contained sample receiving area, clean rooms, laboratory space, staff and ad- ministrative offices, air-handling equip- ment, computer room, conference room, library, and canteen. This structure must be freestanding to afford protec- tion from the contamination that will inevitably result from the air-handling system should the facility be incorporated into or contiguous to a larger structure. , Obviously, the local institutional setting • ------- Preparation and Dispatch of Filters for Field Sampling Air and Water Sampling \ Bulk Samples Rocks, Sedi- - ments. Asbestos Products Sample Receipt and Log-In Short-Term Storage Air/Water Samples - Filters -Water Samples Bulk Sample Preparation Preliminary Optical Screening I i Y Sample Routing Preparation of EM Specimens Preparation of X-ray Samples and Standards X-ray Diffraction Analysis I Data Processing and Recording Summary Printout and Reporting Figure 1. Sample flow sheet. will affect some of these choices. The nominal dimensions of the proposed building are 56 feet by 104 feet for a total area of about 5600 square feet. Approximately one-fourth of the space is devoted to clean rooms, one-fourth to laboratories, one-fourth to offices, and one-fourth to utilities. The philosophy underlying the design of the building is that the clean areas, laboratory areas, and office areas should be spacially separated. The air-handling Sample Flow Information Flow equipment for the building can then be installed so that pressure differentials are maintained between the clean areas, the laboratories, and the office space. This will permit smoking and other activities in the office space without affecting the laboratory and clean areas. Instrumentation To keep abreast of and contribute to advances in particulate analysis meth- odology, to analyze a wide variety of air and water samples, and to corroborate data obtained by others, the laboratory must be equipped with top quality light and electron microscopes and an x-ray diffractometer. A multiterminal computer system is also required to monitor the status of current samples and to retrieve data needed for comparison in reporting programs. The criteria for selection of particular instrumentation include specifications, performance, actual compatibility with expected future devel- opments, availability of replacement parts, service, and relative cost. Recom- mended major equipment for the labo- ratory includes a Siemens 0-500 x-ray diffraction system; an AMR SEM; a Hitachi HU-6002 STEM, A Tracer North- ern TN-4000 Energy Dispersive spec- trometer; and an Ohio Scientific Chal- lenger data base manager system. Specifications of major instruments, costs, and lists of other required equip- ment are given in the report. Personnel The challenging role to be assumed by the proposed laboratory demands that it be staffed by scientists and technicians of the highest caliber. Anything less will negate the point of establishing a new facility dedicated to excellence in par- ticulate analysis. The key individual is the senior scientist selected to inaugu- rate and direct the facility. Considerable emphasis should be placed on obtaining an experienced perSon with outstanding credentials. The specific educational background of this person is not as important as established reputation and experience in particulates research. There are very few persons with the necessary qualifications. To attract one of these persons will require adequate initial and ongoing funding for develop- ing and maintaining expertise of the highest caliber. If the laboratory is established as recommended in this report, the excellent opportunity pre- sented should be sufficient to attract one of the best individuals in the country. The scanning electron microscopists required should have expertise in com- puter-based data collection and manip- ulation systems. Knowledge of mineral- ogy and of x-ray microanalysis is es- sential to this position. Candidates with these skills are available. The optimum staff would comprise trained specialists for each type of instrumentation installed in the labora- tory with sufficient support personnel to ------- Conference J Room "- Central Mechanical Equipment 12' x20' Storage 12' x 10' Office 2' x 12' Scanning Microscopy 12' x24' Transmission Microscopy 12' x 24; Office 10' x 12- E: a Computer s| Room 12' x 12' Instrument Shop 12' x 10' \X-Ray Diffraction \12' x 16' 1 'I J y > —Clean Room Lab" clean R°°m Lab Class 104f Class 1° Sample ^Special ProiectsH^Sffing 12' x 18'. Lunch Room 12' x 12' Secretary—*. Receptionist A Clean Rm Lab Clean Rm Lab \\Clean Rm Lab Specimen Prep. ||'2' x 1 12' x 12' lass 100 6 Optical Micro- Mechanical Equipment 12' x 12' File Room 12'x 12' scopy 12'x 10' Class 100 Administrative Office Equipment Legend: 1. Scanning Electron Microscope 8. 2. Scanning Transmission Microscopy 9. 3. Automatic X-Ray Diffractometer 10. 4. Computer Terminal 11 • 5. Disk Storage 12. 6. Optical Microscope 13. 7. Work Benches 14. Floor Plan 1 Desks "Logetronics" Printer Enlarger Image Analysis Equipment Evaporator Class 100 Fume Hoods Circulating Fan & pre-Filter Enclosure (Typ. Five Places) Figure 2. Plan of proposed laboratory. run all the instrumentation at full capacity. The minimum staff is that required to maintain the instrumentation, stay abreast of developments, and perform a very limited number of special analyses. The optimum staff would include two electron microscopists, one petrographer, one senior scientist, eight technicians, a secretary, and a computer operator. The minimum staff would include one electron microscopist, one petrographer, four technicians, and a secretary. Implementation Plan and Cost A two-year schedule for the comple- tion of this project is projected. When the laboratory is approved, the distin- guished scientist who will eventually direct the laboratory should be brought into the project along with the architect. This scientist and the architect should work closely together in designing the building in detail using the conceptual design as a model. There will be ade- quate time available for the scientist selected to make the necessary visits to other laboratories and to become fully versed in the latest methodologies, instrumentation, and federal regulations on particulates. After the completion of the architects' work, bids for construction may be requested. Four months after approval of the laboratory the construction con- tract for the building may be awarded. At this time the scientist in charge should order long-lead-time equipment such as electron optical instruments, x- ray diffractometers, and clean-room modules. Interviewing of the skeletal staff for the laboratory (two senior technicians and one more scientist) should begin eight months after approval equipment such as optical microscopes of the laboratory. Short-lead-time and evaporators should be ordered at this point in the schedule. With the completion of the building and clean rooms after ten months, the equipment installation and testing period should begin. Calibration and trial runs on the equipment using well- characterized paniculate samples should be carried out during this period. After twelve months the laboratory should be able to handle some real-world speci- mens at a limited rate, with full capabil- ities taking an additional twelve months to develop. The number of staff to be added with time will be determined by the sample demand. The initial cost of equipment, exclud- ing the building, will be $764,000. The annual laboratory operating cost includ- ing salaries, supplies, and equipment maintenance for minimal staffing will be $308,000. For optimum staffing this figure is $534,000. ------- lecommendations The recommended conceptual design of the particulate analysis laboratory, if fully implemented, will achieve the objectives established by the EPA in commissioning this project. The broad purpose is to rectify the lack of reliable information about the exposure to asbestos and other particulates in non- occupational settings and their health effects. The current situation is not the result of a lack of effort on the part of EPA or other groups. To a large extent, it is a direct result of the ambiguity in the definition of asbestos and the intrinsic complexity and interdisciplinary nature of the analysis. Unfortunately, many of the projects sponsored to develop rigor- ous, robust methods for the analysis of asbestos and other particles have had limited success, and studies using recommended methods have been found wanting. Clearly a new approach is needed. Thus, establishment of a center of excellence for particulates analysis within EPA is timely and well conceived. Specific recommendations stemming from this project are listed below: 1. Establishment of a federal labo- ratory specializing in the analysis of particulates should be of the highest priority. 2. The laboratory should be equipped with the best available instru- ments and staffed with highly qualified and experienced per- sonnel. 3. It should function as a center of excellence qualified to monitor and evaluate relevant efforts in any laboratory. 4. An advisory panel should be es- tablished to aid in selecting pro- grams, setting priorities, and evaluating progress, but other- wise the laboratory should be autonomous. 5. Peer review of the quality of the research program should be con- ducted under the auspices of the advisory panel. 6. A substantial part of the program should be devoted to methods development and to providing a definitive analysis for critical samples; a minimum portion should be devoted to routine analysis. 7. After start-up, funding should be provided to maintain state-of- the-art instrumentation as im- provements become available. 8. A contract should be arranged with a qualified laboratory to develop the necessary hardware and software to measure and interpret electron diffraction pat- terns from particulates. 9. Initial research programs should be aimed at the development of suitable standards and reference samples, such as synthetic mix- tures of asbestos and other mate- rials, for general use. 10. The laboratory should participate actively in round-robin studies sponsored by ASTM or other groups to establish the degree of reproducibility that can be achieved and should initiate such studies if necessary. 11. The laboratory should screen and evaluate existing sample prepa- ration techniques and develop new methods particularly suitable for automatic image analysis in both the scanning electron mi- croscope and scanning trans- mission electron microscope. 12. The laboratory should develop automatic image analysis meth- ods, including more sophisticated computer software. R. J. Lee, J. S. Lally, and R. M. Fisher are with the Research Laboratory, United States Steel Corporation, Monroeville, PA 15146. R. J. Thompson is the EPA Project Officer (see below). The complete report, entitled "Design of a Laboratory for Particulate Analysis," (Order No. PB 81-191 132; Cost: $9.50, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telephone: 703-487-4650 The EPA Project Officer can be contacted at: Environmental Monitoring Systems Laboratory U.S. Environmental Protection Agency Research Triangle Park, NC 27711 J US GOVERNMENT PRINTING OFFICE 1961 757-012/7244 ------- 4 United States Environmental Protection Agency Center for Environmental Research Information Cincinnati OH 45268 Postage and Fees Paid Environmental Protection Agency EPA 335 Official Business Penalty for Private Use $300 PS 0000329 U S EMVIR PKOTtCTIQN REGION 5 LIBRAKY 230 S DEARbORM STREET CHICAGO IL 60604 I ------- |