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
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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 •
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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
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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.
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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
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