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

-------