PA/340/1-91/010
d States Air Quality and Planning EPA340/1-91-010
onmental Protection Standards September 1991
cy
Standard Procedure For
Collection of Coating and Ink
Samples For Analysis By
Reference Methods 24 and 24A
Printed on Recycled Paper
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EPA-340/1-91-010
STANDARD PROCEDURE FOR
COLLECTION OF COATING AND INK SAMPLES FOR
ANALYSIS BY REFERENCE METHODS 24 AND 24A
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Air and Radiation
Office of Air Quality Planning and Standards
Stationary Source Compliance Division
Washington, DC 20460
September 1991
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DISCLAIMER
This document is a draft report submitted to the Stationary Source Compliance
Division for circulation and subsequent comment on the technical adequacy of the
contents. Any views or opinions contained herein are those of the authors and do not
necessarily reflect the conclusions of the U.S. Environmental Protection Agency.
Any mention of trade names or commercial products does not constitute
endorsement or recommendation for use by the U.S. Environmental Protection
Agency.
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CONTENTS
Section Page
1. INTRODUCTION 1
2. PROCUREMENT OF SAMPLES 5
3. CHAIN OF CUSTODY (C OF C) 11
4. QUALITY ASSURANCE/QUALITY CONTROL 13
5. HANDLING 15
6. REFERENCES 17
APPENDICES
A Coating Data Sheet 19
B Chain of Custody (C of C) Strip Seal 23
C Sample Container Label 27
D Chain of Custody Form 31
E DOT Specification 12-B for Shipping Packages 37
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SEC
INTRO
This standard operating procedure
of providing simple step-by-step instructor
and inks, for use by EPA, State, and local
instructions are presented in general term;
sufficient details for actual field sampling.
conjunction with existing health and safety
EPA or other agency training guidelines.
SOP) document is prepared with the intent
s, covering all aspects of sampling coatings
egulatory agencies nationwide. The
as much as possible while providing
(Tie procedure should be used in
programs and in accordance with existing
Standard procedures are presented
inks that require analysis by EPA Referenc
in 40 CFR 60, Appendix A. This SOP has
obtained from EPA Region II. For the
agency inspectors nationwide in terms of s
activities deemed proper and necessary to
representative of the coating or ink as app
described, questions concerning the credi
Agency inspectors are generally responsible
deciding on the date, process, and locatio
are drawn properly, and c) handling and
responsible for analysis. The inspector rai
typically requests the facility representative
sample under the agency supervision, whi
guidance for sampling.
The use of common sense and care
representative samples of industrial surfac
Several EPA offices as well as State and lo :al agencies have developed procedures
ION1
UCTION
for sampling and handling of coatings and
} Methods 24 or 24A (RM 24/24A) as found
jeen expanded from an original version
purp ose of developing consistency among
sampling conducted, it delineates the
ensure that the sample taken is
ed. If the activities are conducted as
ility of sampling performed can be avoided.
for a) planning for sampling (i.e.,
of sampling), b) ensuring that the samples
transporting samples to the laboratory
?ly draws the sample. On-site the inspector
to assign a facility employee to draw the
providing the necessary equipment and
are required in procuring and submitting
coatings and printing inks for analysis.
ampling (i.e., sampling techniques,
of samples.) ASTM also has published
1.2.3.4
for their staff, covering various aspects of
containers, as well as storage and transfer
several specific and detailed sampling procedures.
The Standard Operating Procedure (SOP) presented in this document covers all
types of industrial coating and printing ink operations, regardless of the method of
application of coating or ink (i.e., dip, spray, roll, flow, electrostatic, or electro-
deposition). The only exceptions are the source categories such as consumer,
architectural, or aerosol coatings, for which little compliance sampling experience is
available. For these categories, the local process conditions, such as the coating
storage and application methods, may dictate some minor changes in the way the
sample is collected.
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The sampling, handling, labeling, chain of custody, and quality assurance/
quality control conditions and procedures are addressed in the following sections.
The equipment, supply material, data recording forms, and labels that must be either
carried or readily available to the inspector in the field are listed below. However, the
actual use of equipment will depend upon the local process conditions existing at the
source sampled.
Sampling Supplies:
• Dual seal tin sample containers, one cup (8 fl.oz.), 1 pint (16 fl.oz.), 1 liter
(equivalent to 1 quart or 32 fl.oz.) or special plastic sample containers for
corrosive coatings
• Waterproof/solvent-proof marking pen
• Small scraper or knife/spatula
• Clean rag, paper towels
• Cooler/ice
• Long handled tongs
• Tubing
• Mixing/stirring paddles
Personal Safety Equipment:
• Eye protection
• Respiratory protection
• Hearing protection
• Steel toe shoes and gloves
• Hard hat
• Anti-sparking equipment (clamp-ended grounding cables)
Shipping Supplies:
• Packing and/or shipping box(es)
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• Packing material: bubble paper, newspaper
• Shipping labels/forms
• Strapping tape
Data Recording Forms and Labels:
Listed below are standard forms and labels which will be required to properly
record and identify samples. The inspector should plan to
have an ample supply on hand at the source as deemed necessary.
• Coating Data Sheets5 - (see Appendix A)
• Chain of Custody (C of C) strip seal (see Appendix B)
• Sample can label (see Appendix C)
• Chain of Custody (C of C) Record (see Appendix D)
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SECTION 2
PROCUREMENT OF SAMPLES
The recommended step-by-step activities for proper sampling are presented
below:
1. Confirm sample analysis arrangements (with the laboratory assigned to perform
the analysis) prior to taking samples, particularly if they are non-routine.
2. Identify coatings or inks and the processes from which they are to be sampled:
a. Identify the location in the operation where samples can best be
obtained. The sample should be taken at the point of application of
coating or ink, or as close to that point as possible, in order for the
sample to be representative of the coating material "as applied" to the
web or substrate.
b. Multi-component coatings that harden upon mixing and application to the
substrate must be sampled differently since a representative "as applied"
sample cannot be obtained in the field. Examples of these coatings are
the two and three part catalyzed polyurethane coatings. Each
component of these coatings must be sampled separately and submitted
for laboratory analysis as a mufti-part sample. The component mix ratio
must be obtained from the facility at the time of sampling and submitted
to the analytical laboratory. This will enable the laboratory to mix the
components using the same proportions as in the actual coating
operation prior to the analysis.
3. Make sure the coating is thoroughly mixed before sampling. During operation
of the coating application equipment, the coatings may be shaken mechanically
or stirred with various agitators or circulation systems. Lacquers and other
coatings containing highly volatile solvents should be agitated in closed
containers to avoid evaporation. Water-thinned coatings tend to incorporate air
bubbles if stirred too vigorously, so they should be stirred slowly. The risk of
stratification or separation of components into a non-homogeneous mixture
depends on the type of coating and is also directly proportional to the size of
the reservoir being sampled. To ensure that a representative sample is
obtained, it is essential that it be taken during steady process operation and at
the point of application to the web or substrate (or as close to it as possible).
4. Most New Source Performance Standards (NSPS) regulations cited in 40 CFR
60 for surface coating operations require the use of at least a one liter
(approximately 32 fl.oz.) sample container.
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For sampling of all sources other than NSPS sources, use a tin dual seal 8 fl.oz.
sampling container. A 16 fl. oz. container may be used, but it will result in
excessive material for later disposal. Small 4 fl. oz. sample containers may be
used for the catalyst that will be added to multi-component formulations in the
laboratory since only small proportions are normally used.
Special plastic containers or glass sample bottles have been used for corrosive
substances such as acid etch primers and paint catalysts such as MEK
peroxide.6 If a plastic container is used it must be impermeable to VOC
diffusion through the walls of the plastic container.1 Sample containers, caps,
and inner seal liners must be inert to the chemically reactive compounds in the
sample and must therefore be selected on a special case-by case basis by the
agency affected.
5. Request a copy of the blender's worksheet to obtain data on the exact coating
being sampled. Also collect manufacturer's formulation information from
product data sheets. The ink, coating, and solvent data should be available on-
site in the form of Material Safety Data Sheets (MSDS). The MSDS forms
contain recommendations for safe handling of materials as well as physical and
chemical properties data. Request data on the coating cure time and
conditions if not provided in product data sheets and MSDS forms. Determine if
exempt solvents are present or if any special handling or safety precautions will
be required.
6. Bring a blank Coating Data Sheet form5 (see Appendix A) for reference
purposes to ensure that sufficient information is gathered from plant documents
to fill out or calculate the necessary input data.
7. Only one sample is required for each coating to be characterized. The sample
can be used in the analytical laboratory for a number of repeat analyses as
required. One field replicate sample should be taken for every 10 samples
collected. A minimum of one field replicate sample should be taken for each
facility visit, even if less than 10 samples are taken. This provides a means to
check the accuracy of the methods used. If a company requests a set of
samples for its own analysis, an entirely separate set of samples should be
taken concurrently using new sample containers. A fresh new sample should
be taken if a repeat or follow-up sample is required for any reason.
8. When coating samples are procured on-site, the inspectors and other personnel
should protect themselves from exposure to potentially hazardous chemicals as
discussed below:
a. Wear proper personal protecting equipment. The MSDS may indicate
the manufacturer recommended personal protective equipment (PPE) for
use during handling of samples. The MSDS forms for the coating
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materials, including dilution solvents, should be readily available at the
point of use in the facility.
b. If a site safety plan is in effect, adhere to all of the provisions which relate
to the coating operations being sampled. These requirements may
include, but are not limited to: respiratory protective devices (e.g., air
purifying respirators, air-supplied respirators), protective clothing (e.g.,
gloves, apron), eye protection (e.g., safety goggles, face shield), hearing
protection (e.g., ear plugs or muffs), use of non-sparking tools and
equipment, and other requirements as deemed necessary by the on-site
safety personnel.
c. If no safety plans, MSDS, or on-site safety personnel are available, then
the manufacturer of the coating materials and/or the regional OSHA
office may be contacted for guidance on safety practices and the types
of PPE to be utilized during sampling.
d. At a minimum, the applicable federal and state safety and health laws
such as those found in Title 29 of the Code of Federal Regulations, Part
19107, shall be complied with by all inspection personnel supervising the
sample procurement.
9. Have a sample of the selected coating or ink drawn by the facility's designated
person. A clean rag or paper towels should be kept handy, since the filling of
the sample container may result in some spillage.
a. Inspect the sample container to ensure that the inside and outside are
clean and dry. Then hand it to the facility operator assigned to draw the
sample.
b. Have the sample container connected to an electrical ground using
grounding clips. This is particularly important when sampling from
coating operations using electrostatic or electro-deposition technologies.
c. Have the facility operator assigned to the task draw samples by filling
each sample container one-at-a-time. Work as fast as possible to avoid
loss of VOC from the sample. Depending upon the location in the
process from where the sample is taken, the steps presented below
must be followed in drawing samples.
Usually, a sample is taken from 1) a spray nozzle or other applicator; 2)
a coating bath/agitated reservoir holding coating ready for application; or
3) a bleed valve, hose, tank, or other location upstream of the point of
application. Usually it is best to take the sample at the application point,
i.e., a spray gun or nozzle. When sampling at locations other than the
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spray gun, one must make sure that the coating or ink is not thinned
beyond the sample point.
(1) When sampling from a spray gun or other application device:
• Shut off the compressed air or atomizing fluid pressure and
tilt the nozzle to about a 60° angle.
• Tilt the sample container to the same angle, insert the
nozzle or application device into the sample container, and
begin to fill the sample container using the liquid feed
pressure to provide flow, gradually tilting the sample
container upright as it fills.
• Slowly fill the container to overflowing to ensure that a
representative sample is obtained and to avoid any loss of
VOC due to volatilization to the headspace. Do not insert
the applicator tip into the coating. This may contaminate
the sample or create bubbles leading to VOC loss.
• Obtaining a representative sample from high pressure spray
gun applicators or from coatings or inks that contain high
vapor pressure VOC's may prove difficult.
(2) When sampling from an agitated/circulating coating bath or
container holding coating ready for application:
• Wipe off the sample container or make sure it is clean
before dipping it into the coating reservoir. Turn the sample
container upside down and place it in the coating,
approximately halfway down. (Do not take the sample from
the top surface.) This can be done with a clean pair of long
handled tongs to avoid contaminating the reservoir.
• Turn the sample container over and slowly bring it to the
top of the coating reservoir.
• It is important to completely fill the container to avoid any
loss of VOC due to volatilization to the headspace. A
sample filled to the top and spilling over is acceptable. This
requirement applies to the catalyst of multi-component
coatings as well as to the uncatalyzed coating.
When sampling inks, a sample may be taken directly from
the ink trough using a metal ladle, glass jar, or a clean
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paper cup to fill the sample container. A foam cup which
may dissolve upon contact with solvents should not be
used.
(3) If it is not possible to sample from the coating container or
applicator, a sample may be taken from a tap, bleed valve, paint
hose, drum, tank, or other location in the system which is as close
to the point of application as possible and therefore will provide
the best possible "as applied" coating sample. Sampling at each
of these alternate points will require some judgement, since each
coating line or process may have a different orientation and layout
of taps, valves, hoses, and reservoirs. If additional information or
guidance is needed, refer to ASTM Method D4057-88 for Standard
Practice for Manual Sampling of Petroleum and Petroleum
Products3 and ASTM Method E300-86 for Standard Practice for
Sampling Industrial Chemicals4 for detailed procedures and
recommendations. Basic instructions for sampling from larger
reservoirs or containers are:
• Flush any tap, valve, hose, or other sample line thoroughly
before sampling. Sampling from 55 gallon drums or larger
tanks should be avoided because stratification or separation
of components may occur under all but the most ideal
mixing conditions. Hold the sample container upright or at
a slight angle so that the sample tap may be inserted into
the container.
• Insert the tap, valve or hose into the sample container and
begin to fill it while attempting to avoid contamination of the
sample by contact with external parts of the sample line.
• It is important to completely fill the container to avoid any
loss of VOC due to volatilization to the headspace.
d. Once the sample is taken, the steps presented below must
be followed:
• Place the sample container on the floor or ground and insert the
inner seal on the container. The most efficient way to do this is to
place the seal inside the rim of container, invert a screw cap, and
with the open palm of the hand press down on the screw cap; this
will evenly force the inner seal into the container for a tight fit.
• Screw cap onto can.
Page9
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• Wipe all residual coating material off the sample container. To
avoid contamination, do not allow cleaning of the container prior
to inserting the inner seal.
• Sign and date the Chain of Custody (C of C) strip seal (see
Appendix B), place it over top of the screw cap and down sides of
the sample container tightly, following contours.
• Each sample should be numbered with a unique number.
• Completely fill out the sample container label. The label should
contain the following information (An example label is given in
Appendix C):
Name of Agency and inspector who obtained the sample.
Sample ID No.
~ Sample date and time.
Source identification and sample point (e.g., coating line
and coating station identification for the collection site).
Sample description - color, type, solids/water content, or
multi-component portion.
- Set-up time of multi-component coatings, if applicable.
- Plant witness (signature).
Analysis required - RM 24 or RM 24A.
- Presence of exempt solvents and their identification.
- Special handling procedures that may be required.
• Finally, affix the completed label onto the side of the sample
container over the C of C seal ends.
10. Complete the C of C form (given in Appendix D) for each sample. The
inspector should retain a copy of the C of C until the original comes back from
the analytical laboratory. All other copies and original should remain with the
sample to be sent for analysis.
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SECTION 3
CHAIN OF CUSTODY (C of C)
Chain of custody procedures are very important. They show who controlled or
handled the samples. Proper documentation of each sample handler is essential to
preserving the integrity of the sample and its use as evidence.
1. Each person who handles the sample must be identified on the accompanying
C of C Record form. (A suitable blank C of C record form is presented in
Appendix D along with a completed example.) More than one sample can be
included on a C of C record if each sample is clearly identified and the
analysis/handling instructions for each are clearly and unambiguously given.
2. If shipping of the sample is required, the C of C sheet should be enclosed in an
envelope and should travel with the sample inside the shipping box. The
analytical laboratory personnel receiving the sample are responsible for signing
the original C of C and returning it to the agency.
3. If air shipping is required the Air Cargo bill of lading (or other shipping bill/
receipt documents) becomes part of the C of C and should be attached to the
original C of C by the person receiving the delivery.
4. Before enclosing it in the shipping box, ensure that all portions of the C of C
form are filled out including specification that the RM 24 or 24A analysis is to be
performed by the analytical laboratory and including identification of exempt
solvents that may be present in the sample.
5. In most cases, use one C of C form for each sample.
6. The agency inspector should retain one copy of the C of C.
7. The original C of C form will be returned by the analytical laboratory receiving
the sample to the designated agency representative. The C of C form should
have signatures from the agency inspector, the sample custodian, the person in
charge of shipping samples, and the responsible analytical laboratory
representative before it is returned to the agency. When the C of C is returned
to the agency, a copy of the C of C should be given to the inspector and the
original kept by the person responsible for shipping or recordkeeping.
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Page 12
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SECTION 4
QUALITY ASSURANCE/QUALITY CONTROL
Documentation
1. All required information should be completely recorded on appropriate C of C,
strip seal, or label forms. Each sample recipient should check C of C, strip
seal, or label forms for completeness and should not accept samples if C of C,
strip seal, or label forms are incomplete. The recipient should require that any
key missing information be provided to adhere with procedures intended to
ensure integrity and C of C documentation of the sample.
2. Sampling activities should be documented in a logbook or recordbook in the
event verification or testimony is required at a later date.
3. The C of C form should be legibly and completely filled out, including directions
for which reference method analysis (i.e., 24 and/or 24A) should be performed
and identifying any exempt solvents that may be present.
4. MSDS or other product data sheets, blender's worksheets, coating
manufacturer's data, or trade names (as well as multi-component coating
formulation blend and set-up time information) should only be sent with samples
to the laboratory for analysis if reference to % volatile, % H2O, % exempt
solvents, VOC Ibs/gallon, specific gravity, or specific information about the
origin of the sample are removed or excluded from the data. This is to ensure
objective and unbiased analysis of the sample. MSDS and other qualitative
information describing the sample is essential to proper and safe handling in the
laboratory.
5. The person submitting the samples should indicate the presence of water, ask
for % water analysis only when applicable, identify the presence of exempt
solvents, and specifically request analysis for exempt solvents when present.
6. The shipping documents should be filled out correctly.
Labeling
7. C of C strip seal tape should be placed on container properly and securely.
8. The sample label should be completely and accurately filled out indicating the
analysis requested, the presence of exempt solvents, or if special handling is
required. It should be placed on the container so that it is readily visible.
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9. When the sample contains an exempt solvent or a multi-component coating to
be specially blended (mixed) by the analytical laboratory, a special tag should
be completed and affixed to the sample (such as a 2V£H by 4V£H label tied to the
sample can with a string) to notify the lab that the sample requires special
handling or analysis.
10. The shipping labels should be filled out correctly.
Sample Integrity
11. The sample container should be filled to overflowing prior to placing inner seal
in container. A partially filled container indicates potential VOC loss or some
other problem with the sample. A repeat sample is required.
12. To avoid potential sample contamination, the outside of the sample container
should be wiped clean immediately after being sealed.
13. If analytical laboratory personnel receive samples stored in inappropriate
containers or if there are any other problems associated with sample integrity or
documentation, they should immediately report these problems to agency
personnel.
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SECTION 5
HANDLING
Simple common sense should be used in handling collected samples to ensure
sample integrity and custody control.
1. Maintain samples at room temperature, preferably at 70°F but within the range
of 40 to 100°F. Do not store sample containers in hot areas such as a closed
vehicle. Keep out of direct sunlight and keep from freezing.
2. After properly sealing the sample container, the sample should be secured in a
safe place and maintained at a temperature that is compatible with the coating.
The packing requirements of individual samples depend on the coating's
physical and chemical properties. Coatings with relatively high vapor pressures
(i.e., those containing volatile solvents with boiling points below 100°F) should
be packed in ice to keep them within the temperature range of 40 to 100°F.
The inspector or person responsible for samples should use ice packs or other
more durable means to keep samples cool if they must be held for extended
times or may be exposed to extreme heat. Use special insulated containers to
avoid volatilization, particularly in warm climates. The temperature sensitivity of
the coating should also be checked to determine if packing in ice may have a
detrimental effect on the sample by causing solidification, separation, or any
other change in its properties. Other samples which are not volatile at low
temperatures, such as those with boiling points higher than 100°F, may be
packed and shipped at room temperature. The MSDS on coatings and dilution
solvents supply sufficient information to determine the coating properties.
3. When packaging samples for shipment, use bubble packing or crumpled paper
to line the bottom of the box. The box should be firm, adhering to
specifications given by the US Department of Transportation - DOT 12-B.8-9
Place the sample container in the box with the top up. Pack additional bubble
pack or paper around the container so that the entire inner space of the box is
sufficiently filled, to keep the sample container in the upright position and to
prevent the container from shifting while in transit.
4. Enclose both the completed C of C form and a stamped envelope addressed to
the agency for return of the C of C form in a larger envelope addressed to the
analytical laboratory to which the sample is being sent. Place it on top of the
packing over the sample containers and close the box.
5. Seal the box with strapping tape.
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6. Paint and coating samples are considered hazardous material and should be
shipped as a restricted article by Federal Express or another suitable carrier
that can provide special handling. Label the outside of the box with sender/
receiver addresses. If used, insert the completed air bill/cargo bill in its proper
pocket and seal.
7. For all mail, courier, or special delivery service shipping, the box should have
the following designations:
On top of box: TOP - THIS SIDE UP."
On all sides of box: arrows pointing up.
On bottom of box: "OTHER END UP."
On one side of box: "Flammable liquid UN No. 1263."
On opposite sides of box: "Danger" and "Flammable Liquid" labels.
On fourth side of box: Name and address of the person shipping
the samples.
• On top of box: Shipping destination name and address along with
any additional labels required by shipping company, such as the
restricted article form used by Federal Express.
8. DO NOT HOLD. Ideally, a sample should be delivered to the laboratory for
analysis on the same day it is obtained. If a sample must be stored overnight,
it should be kept in a secure place, away from extreme temperatures and away
from danger of breakage, leakage, or tampering, preferably in a locked storage
cabinet. Maintain a sample log for those samples stored overnight. The log
should contain the following information:
Sample number.
Facility name and location.
Date/time sample obtained.
Date sample was placed into locked storage cabinet.
Date when sample was mailed to the laboratory for analysis.
NOTE: SAMPLES SHOULD NOT BE MAILED ON A FRIDAY BECAUSE
THEY WILL NOT BE DELIVERED UNTIL MONDAY. THIS MAY
INTRODUCE SOME SUBSEQUENT QUESTION ABOUT ADEQUATE
CHAIN OF CUSTODY OR SAMPLE INTEGRITY.
Page 16
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6. REFERENCES
1. Standard Practice for Sampling Liquid Paints and Related Pigmented Coatings,
ASTM D3925-81 (Re-approved 1985). 1990 Annual Book of ASTM Standards,
Volume 6.01, Philadelphia, PA, 1990.
2. Standard Methods for Sampling of Testing Shellac Varnish, ASTM D1650-76,
1990 Annual Book of ASTM Standards, Volume 6.02, Philadelphia, PA, 1990.
3. Standard Practice for Manual Sampling of Petroleum Products, ASTM Method
D4057-88, Volume 5.01, Philadelphia, PA, 1990.
4. Standard Practice for Sampling Industrial Chemicals, ASTM Method E300-86,
Volume 6.03, Philadelphia, PA, 1990
5. EPA-340/1-88-003, Recordkeeping Guidance Document for Surface Coating
Operations and the Graphics Arts Industry, U.S. EPA, Stationary Source
Compliance Division, Washington, DC, May 1989.
6. "Information on Sample Taking and Sample Transport/ Field Sampling
Guidelines," (Draft), Bay Area Quality Management District, San Francisco,
California, July 1990.
7. Code of Federal Regulations, Title 29, Part 1910, Occupational Safety and
Health Standards, Department of Labor, July 1, 1989.
i
8. Dangerous Goods Regulations, 31st Edition, International Air Transport
Association, Montreal, Quebec, Canada, 1990.
9. Code of Federal Regulations, Title 49, Part 178, Subpart F- Specifications for
Fiberboard Boxes, Specification 12-B, Department of Transportation (49 CFR
178.205), October 1, 1989.
10. EPA-450/3-84-019, Procedures for Certifying Quantity of Volatile Organic
Compounds Emitted by Paint, Ink, and Other Coatings, U.S. EPA, OAQPS,
ESED, Research Triangle Park, NC, December 1984.
11. "EPA Region II Sampling Procedure," (Draft), New York, New York, June 1990.
12. "EPA Region I: VOC Sampling/Analysis," (Draft), McCusker, Boston,
Massachusetts, June 7, 1990.
13. "Sampling Techniques & Test Methods," (Draft), California Air Resources
Board, Sacramento, California, July 30, 1990.
Page 17
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14. Federal Test Method Standard No. 141c, Paint, Varnish, Lacquer, and Related
Materials; Methods of Inspection, Sampling, and Testing. General Services
Administration, January 24, 1986.
15. EPA-600/9-76-005, Quality Assurance Handbook for Air Pollution Measurement
Systems: Volume I. Principles. U.S. EPA, EMSL, Research Triangle Park, NC,
December 1984.
16. EPA-600/4-77-027b, Quality Assurance Handbook for Air Pollution
Measurement Systems: Volume III. Stationary Source Specific Methods. U.S.
EPA, EMSL, Research Triangle Park, NC, November 1976.
Note: References 10 through 16 were not directly cited in the Sampling
SOP for RM 24/24A but the methods outlined in those references were
generally incorporated. They are considered generally relevant and
useful sources for sampling information.
Page 18
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APPENDIX A
COATING DATA SHEET
Page 19
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Page 20
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Page 22
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APPENDIX B
CHAIN OF CUSTODY (C of C) STRIP SEAL
Page 23
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Page 24
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Page 26
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APPENDIX C
SAMPLE CONTAINER LABEL
Page 27
-------
Page 28
-------
Agency: lnspector:_
Sample ID#: Date/Time:.
Source ID#:
Coating Name/Type:
Plant Witness (Signature):.
Circle analysis required: RM 24 RM 24A
Exempt Solvents:
Special Handling:
Page 29
-------
Page 30
-------
APPENDIX D
CHAIN OF CUSTODY FORM
Page 31
-------
Page 32
-------
CHAIN OF CUSTODY RECORD
Agency Inspector/Address:
Source Description:
Inspection Time/Date:
Sample
ID No.
Description of Sample
Type of Analysis to be Performed/Remarks:
Person Responsible for Sample (Inspector's Signature:)
Time
Date
Relinquished By:
Received By:
Time
Date
Reason for Transfer:
Relinquished By:
Received By:
Time
Date
Reason for Transfer:
Relinquished By:
Received By:
Time
Date
Reason for Transfer:
Relinquished By:
Received By:
Time
Date
Reason for Transfer:
Page of
Page 33
-------
Page 34
-------
CHAIN OF CUSTODY RECORD
Agency Inspector/Address:
John Smith
USEPA-Region II
Air Compliance Branch
26 Federal Plaza
New York, NY 10278
Sample
ID No.
12345
Source Description:
Use a code name or number to
avoid revealing source/coating
information
Inspection Time/Date:
1500 hrs/May 7, 1991
Description of Sample
One (1) 8 fl. oz. can of red enamel coating from coating
machine 12B, station 3.
If it is known that the coating contains an exempt solvent, or is
a known (or suspected) water-borne coating, indicate this fact
also. If the sample is a multi-part coating, indicate this here
and identify the other sample ID numbers that are part of the
multi-part coating. Identify the mix ratios of each component
and the set-up time of the formulation.
Type of Analysis to be Performed/Remarks:
Method 24 or 24A
Person Responsible for Sample (Inspector's Signature:)
John Smith
Relinquished By:
John Smith
Relinquished By:
Joe Andrews
Relinquished By:
Bill Williams
Relinquished By:
Received By:
Joe Andrews
Received By:
Bill Williams
Received By:
Received By:
Mary Long
Time
1700
Time
0900
Time
1000
Time
1100
Time Date
May 7
1500 1991
Date Reason for Transfer:
May 7
1991 to custodian
Date Reason for Transfer:
May8
1991 to shipping dept.
Date Reason for Transfer:
May 8 shipped Fed Ex to
1991 analytical lab
Date Reason for Transfer:
May 9 received at lab for
1991 analysis
-EXAMPLE--
Page
of
Page 35
-------
Page 36
-------
APPENDIX E
DOT SPECIFICATION 12-B
FOR FIBERBOARD BOXES AS
SHIPPING CONTAINERS
Page 37
-------
Page 38
-------
§178.198-3
49 CFR Ch. I (10-1-89 Edition)
Subport F—Specification* for Rb«r-
board Box**, Drums, and Mailing
Tubes
SOURCE 29 PR 18951. Dec. 29,1964. unless
otherwise noted. Redesignated at 32 FR
5606, Apr. 5,1967.
§178.205 Specification
boxes.
12B; flberboard
§ 178.205-1 Compliance.
(a) Required in ail details.
(b) [Reserved]
§178.205-2 Definitions.
(a) Terms such as "200-pound test"
mean minimum strength, Mullen or
Cady test.
(b) "Joints" are where edges of parts
of box, except recessed flanged heads,
are connected together in setting up
the box. Generally done by box
maker.
(c) "Seams" are where edges of parts
of box are visible, except joints, when
box is closed.
§178.205-3 Classification of board.
(a) Fiber-board is hereby classified by
strength1 of completed board as in
first column of the following table;
weights specified in the table are the
minlmiims authorized.
Of OOfnpWtOQ DQsVQ
SoW
wtigntof
cofflpoMnt
per 1,000
•q-ft.)
Facing* tor
MMmum
_i_i_iBiiiln_Mrt
comDsisvo
Mjgttof
IftdnQv
(pound*
INT 1.000
ITS.
200.
275.
32S.
350.
37S.
400.
460.
149
ISO
237
237
283
283
283
283
75
84
138
138
180
180
180
180
92
110
110
128
180
ISO
180
* Mutton or Ctdy tnt
(b) [Reserved]
of c*ady test (nUninnun).
Page 39
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R«Motch and SfMdal Programs Administration, DOT
§17&205-9
§178.205-4 Solid fiberiKmnL
(a) To be 3-ply or more; both outer
plies water resistant.
(b) [Reserved]
§178.205-5 Corrugated fiberboard.
(a) Both outer facings water resist-
ant; corrugated sheets must be at least
0.009 inch thick and weigh not less
than 26 pounds per 1000 square feet;
all parts must be securely glued to-
gether throughout all contact areas.
(b) [Reserved]
§178.205-6 Stitching staples.
Stitching staples must be made in
such a configuration that their hold-
ing capability as installed will not be
less than that of flat steep staples
%iX 0.019 inch in cross section and not
less than %«-inch wide.
CAmdt. 178-12, 35 PR 11686. July 22. 1970]
9178.205-7 Tape.
(a) Coated with glue at least equal to
No. 1% Peter Cooper standard. Cloth
tape of strength, across the woof, at
least 70 units, Elmendorf test. Sisal
tape of 2 sheets of No. 1 Kraft paper,
total weight 80 pounds per ream (500
sheets, 24"x36"); sheets to be com-
bined with asphalt and reinforced by
unspun sisal fibers completely embed-
ded in the asphalt and extending
across the tape, except as provided in
1 178.205-ll(d). Other tapes of equal
strength and efficiency are authorized.
(b) Tape for closure of slotted con-
tainers complying with the following
requirements is authorized when ap-
plied as prescribed in § 178.205-
(1) Tape must be not less than 3
inches wide and shall be made of two
sheets of 100 percent suLfate Kraft
each not less than 30 pounds basis
weight, reinforced with glass, sisal, or
rayon fiber, combined with a ia.tpina.nt
of asphalt or other material not af-
fected by temperature extremes any
more than would standard 180*F. to
200'F. softening point asphalt.
(2) Tape must be reinforced by
lengthwise fibers spaced not more
than an average of V4 inch apart, and
by crosswise fibers spaced not less
than an average of 2 per inch except
that when a diamond pattern is em-
ployed for crosswise reinforcement,
the spacing between the parallel sides
of the diamond measured in the ma-
chine direction must be not more than
linen.
(3) Glass or sisal reinforced tape
must have a minimum tensile strength
in the machine direction of 75 pounds
per inch of width and a minimum ten-
sile strength in the cross direction of
45 pounds per inch of width; rayon re-
inforced tape mUSt have a minimum
tensile strength in the machine direc-
tion of 57 pounds per inch of width
and a minimum tensile strength in the
cross direction of 27 pounds per inch
of width with elongation not exceed-
ing 15 percent. Tensile tests on the
finished product shall be made on a 3-
inch width sample.
[29 FR 18951, Dee. 29. 1964. Redesignated at
32 FR 5606. Apr. 5, 1967, and amended by
Amdt. 178-51. 43 FR 48645. Oct. 19. 1978]
§178.205-8 Test.
(a) Acceptable board must have pre-
scribed strength, Mullen or Cady test,
after exposure for at least 3 hours to
normal atmospheric conditions (50 to
70 percent relative humidity), under
test as follows:
(1) Clamp board firmly in machine
and turn wheel thereof at constant
speed of approximately 2 revolutions
per second.
(2) Six punctures required, 3 from
each side; all results but one must
show prescribed strength.
(3) Board failing may be retested by
24 punctures, 12 from each
side; when all results but 4 show pre-
scribed strength the board is accepta-
ble.
(4) For corrugated fiberboard, doub-
lepop tests may be disregarded.
(b) [Reserved]
§ 178.205-9 Types authorized.
(a) To be of solid or corrugated fi-
berboard of the following types, or as
specifically provided for in § 178.205-
19 to § 178.205-37;
(1) Slotted box; three-piece box
without recessed ends; three-piece box
of solid fiberboard with recessed ends;
double-slide box: triple-slide box; tele-
scope box. with sections of equal
depth, or with covers, top or bottom or
Page 40
-------
§17*205-10
both, with 3 inches overlap. (See
§ 178.205-14 (d) for boxes with single-
flap closures.)
(2) [Reserved]
§ 178.205-10 Forming.
(a) Parts must be cut true to size and
so creased and slotted as to fit closely
into position without cracking, surface
breaks, separation of parts outside of
crease, or undue binding.
(b) [Reserved]
§178.205-11 Joints.
(a) For solid and corrugated fiber-
board slotted containers: Lapped 1%
inches from center of scoreline except
as in S 178.205-12; stitched at 2% inch
intervals and within 1 inch of each end
of joint; body joint must be double-
stitched (2 parallel stitches) at each
end of joint over 18 inches long.
(b) For corrugated f iberboard slotted
containers only: One butt joint taped
(See * 178.205-7) is authorized; 3 inch
tape required for boxes over 30 pounds
authorized gross weight and 2 inch
tape for others.
(c) For triple and double slide boxes:
Joints of all slides must be taped (see
S 178.205-7) for stitched; 3-inch tape
required for boxes over 30 pounds au-
thorized gross weight and 2-inch for
others.
(d) For corrugated fiberboard only:
One butt joint taped inside and out-
side with strips of one thickness of sul-
phate paper not less than 2 inches
wide extending entire length of joint
and firmly glued to box. For boxes not
exceeding 65 pounds gross weight, out-
side strip of sulphate paper to be of
basis weight not less than 60 pounds
testing not less than 60 pounds and
inside strip of sulphate paper to be of
basis weight not less than 40 pounds
testing not less than 40 pounds. For
boxes exceeding 65 pounds gross
weight, outside and inside with strips
of sulphate paper which must each be
of basis weight not less than 90
pounds testing not less than 90
pounds. Basis weight of paper shown
is for 500 sheets, 24x36 inches.
(1) For glued lap joint, the sides of
box forming joint must lap not less
than 1V4" and be firmly glued through-
out entire area of contact with a glue
or adhesive which cannot be dissolved
49 CF« Ch. I (10-1-89 EdWo«)
in water after the film application has
dried.
§178.205-12 Flanged heads.
(a) Must have 4 flanges, at least 1"
long above fillet, on each head. Re-
cessed flanged heads not authorized
for boxes of corrugated fiberboard.
(b) [Reserved]
§178.205-13 Seams which are to be
stitched.
(a) Overlap, if any. required to be at
least 1% inches from center of score-
line except as in § 178.205-12.
(b) [Reserved]
[29 PR 18951. Dec. 29.1964. Redesignated at
32 PR 5606, Apr. 5. 1967, and amended by
Amdt. 178-64.45 FR 81573, Dec. 11,1980]
§ 178.205-14 Flap closures.
(a) Fill-in pieces, of the same type fi-
berboard as used in construction of
the container, are required where it is
necessary to prevent an opening be-
tween the inner flaps, unless otherwise
provided by paragraphs (b) and (c) of
this section or by Part 173 of this
chapter.
(b) If to be dosed by adhesive, each
inner flap must cover at least one-
third of face; inner flaps must butt or
have full overlap, or fill-in pieces must
be used, unless otherwise provided by
Part 173 of this chapter, except that
fill-in pieces are not required when
outer flaps have full overlap. Outer
flaps must butt or have full overlap.
(c) In lieu of fill-in pieces between
inner flaps which do not butt, the fol-
lowing is authorized when linings are
not prescribed in $ 178.205.16.
(1) Top and bottom pads the same
dimensions as interior of container of
solid or corrugated fiberboard at least
125 pound test (Mullen or Cady).
(2) Minimum combined weight of
facings for corrugated fiberboard pads
must be at least 52 pounds per thou-
sand square feet.
(3) Minimum combined weight of
component plies for solid fiberboard
pads must be at least 114 pounds per
thousand square feet, exclusive of ad-
hesives.
(4) Complete inner box or boxes.
(d) Single-flap closures are author-
ized for boxes with one dimension not
Page 41
-------
Administration, DOT
§ 17&205-17
over 2"; each flap must be scored and
form one of the small faces of the box
and lap at least 5" on one of the larg-
est faces.
[29 FR 18951. Dec. 29. 1964. as amended by
Order 67. 30 FR 7425. June 5.1965. Redesig-
nsted at 32 FR 5606. Apr. 5.1967]
§178.205-15 Linings (when prescribed by
§ 178.205-16).
(a) Of 1-piece to extend around 4
faces with joint at center of 1 face and
with 4 flanges, at least 1V4" long, on
each end (corners may be mitered) to
bend over the other 2 faces: also 2
pads to cover the other 2 faces. Pads
may be omitted if closing flaps afford
3 thicknesses throughout face. For
boxes with 1 dimension not over 3".
one of the widest flanges may be
lengthened to cover entire face and
lap 6" on the adjoining face and the
other flanges and the pads may then
be omitted.
(b) [Reserved]
[29 FR 18951, Dec. 29. 1964. as amended by
Order 67. 30 FR 7425. June 5.1965. Redesig-
nated at 32 FR 5606. Apr. 5.1967]
§ 178.205-16 Authorized gross weight and
parts required.
(a) The authorized gross weight
(when packed) and the parts required
are as follows:
1S
an
jn
«
«S4
Strength o
nuHUMiu (iiMwnu
Solid board
Box
175
200
275
325
375
275
Lining*
175
Heeds'
<•)
275
350
O
<•)
350
m> Mutton or Caoy test
DouMtfWfd
• COmipjMd
Box
175
200
275
200
325
375
275
200
Lining'
175
175
200
DoubtaweM
corrugated
Box
200
200
200
275
275
Lining*
'For i
d.ln
i same as for the box.
1 ABJ*52'2dJn' 178JOS-Ui._Acprapm« box is acceptable in plaot of ttw lining.
' Receeeed heeds are not authorized.
4 Except as othen*ee authorized harem or by Pert 173 of this chapter.
(b) Triple slide boxes authorized for
gross weights as follows: Of board at
least 175-pound test for 40 pounds; of
board at least 200-pound test for 65
pounds.
t29 FR 18951. Dec. 29.1964. Redesignated at
32 FR 5606. Apr. 5, 1967. and amended by
Amdt. 178-85. 51 FR 5976. Feb. 18.1986]
§ 178.205-17 Closing for shipment.
(a) Slotted container, by coating
with adhesive the entire contact sur-
faces of closing flaps and fill-in pieces
where required or as prescribed in
paragraph (a) (1), (2), or (3) of this
section.
(1) By stitching with staples as pre-
scribed by § 178.205-6 at 2%-inch inter-
vals along all seams (one 5-inch space
allowed when necessary to permit use
of stitching device); or with staples
made of flat wire of hardness not less
than equivalent of Rockwell B90. and
not less than 0.037 inch thick and not
less than 0.074 inch wide, with not less
than 1V4 inch crown, may be spaced
not more than 5 inches apart. Such
staples may be used across center
seam where outside naps meet in lieu
of on both sides of center seam but
need only be used where outside flaps
overlay inner flaps; or staples made of
arcuate wire of hardness not less than
equivalent of Rockwell B90, and not
less than 0.027 inch thick and not less
than 0.095 inch wide, with not less
than 1 inch crown, may be spaced not
more than 5 inches apart. Such stitch-
es when spaced not more than 2V*
inches apart may be used across center
seam where outside flaps meet in lieu
of on both sides of center seam but
need only be used where outside flaps
overlay inner flaps.
(2) For fiberboard boxes containing
not more than 1 inside metal can not
Page 42
-------
§ 178.205-17
exceeding 1 gallon nominal capacity.
and as otherwise authorized by Part
173 of this chapter, by application of 2
strips of pressure-sensitive tape not
less than % inch in width, 1 strip to be
placed approximately equal distance
over the seam of abutting outer flaps,
the other at a right angle to the first
and spaced approximately equal dis-
tance on the closure face; strips must
be of sufficient length to extend not
less than 1 inch beyond score lines on
side and end panels-. Tape shall have a
minimum tensile strength of 160
pounds per inch of width; minimum
adhesion value of 18 ounces per inch
of width; and minimum elongation of
12 percent at break, or having a mini-
mum longitudinal tensile strength of
not less than 240 pounds per inch of
width; minimum adhesion value of 18
ounces per inch of width and a mini-
mum elongation of 3 percent at break.
(3) For slotted containers only, rein-
forced tape complying with the re-
quirements of § 178.205-7(b) is author-
ized for application over the center
seam only. Tape must extend over the
ends of box not less than 2% inches.
(4) All closing flaps may be firmly
glued with a hot-melt adhesive of 100
percent solid content of thermoplastic
material which will maintain bond at
temperature ranging from 20* F. below
zero to 165* F. above zero. Adhesive
must be applied in not less than eight
stripes (except as specified below) on
each inner flap, each stripe having a
minimum width of %e-inch after com-
pression. Stripes may not be more
than 1% inches apart and not less
than four stripes must be applied on
each side of center seam on each inner
flap for full length of flap overlap
area with one stripe not more than Vfc-
inch from each side of center seam. If
less than eight such stripes are applied
on each inner flap, adhesive must
cover and securely bond not less than
25 percent of flap contact area with
bonded areas extending to within Vt-
inch or less of center seam.
(5) For regular slotted containers,
pressure-sensitive tape is authorized
for application over the center seams
only and extending not less than two
inches over the ends of the box. Tape
must be not less than 2 inches wide
and have a plastic film backing of pol-
49 CFR Ch. I (10-1-89 Edition)
yester, polypropylene, or equivalent
material. Tape must have a minimum
tensile strength of 45 pounds per inch
of width in the machine direction and
not less than 55 pounds per inch of
width in the cross direction and may
not be affected by temperature ex-
tremes normally encountered during
transportation. Boxes closed by means
of this pressure-sensitive tape must be
capable of passing performance tests
prescribed in 5 178.210-10.
(b) Double slide boxes or triple slide
boxes, by coating the inner slides with
adhesive, or by closing with reinforced
tape capable of withstanding test pre-
scribed by paragraph (b)(l) of this sec-
tion; for single-flap closures as author-
ized for boxes with one dimension not
over 2 inches, the flaps must be fas-
tened to the body with adhesive.
(1) Boxes selected at random, con-
taining dummy contents similar to
that to be shipped and packed to au-
thorized gross weight, closed with re-
inforced tape across the ends and onto
opposite side panels at least 2 inches,
must be capable of withstanding a
drop on each end from a height of 4
feet onto solid concrete without clo-
sure failure.
(c) Fiber-board boxes with covers ex-
tending over sides but not to bottom,
covers resting on walls of box, or tele-
scope boxes of equal depth section,
covers extending to bottom, must be
secured by one of the following meth-
ods;
(1) By not less than three metal
straps, one lengthwise and others at
right angles thereto.
(2) When cover extends not less
than 3 inches over the walls of the
box, by coating with adhesive the
entire contact area of the cover.
(3) Telescope boxes having equal
depth sections may be closed by appli-
cation of reinforced water activated
tape or pressure sensitive tape under
conditions and for commodities as pre-
scribed in Part 173 of this chapter.
(d) When metal straps are specified,
boxes must be strapped with the re-
quired number; size at least %
inch x 0.015 inch.
[29 PR 18951, Dec. 29.1964. Redesignated at
32 PR 5606, Apr. 5. 1967. and amended by
Amdt. 178-41.42 PR 28135. June 2.1977]
Page 43
-------
ItoMorch and Special Programs Administration, DOT § 178.205-22
§178.205-18 Marking.
(a) On each container. Symbol in
rectangle as follows:
DOT-12B • • •
(1) Stars to be replaced by author-
ized gross weight (for example. DOT-
12B40, etc.).
(2) Name and address or symbol of
person making the mark specified in
paragraph (a)(l) of this section and lo-
cated just above or below that mark.
Symbol, if used, must be registered
with the Director, OHMT.
(3) When metal straps are pre-
scribed, boxes must be marked
" (number) METAL STRAPS
REQUIRED" just above or below the
mark specified in this paragraph.
(4) Size of markings- Specification
markings prescribed in paragraph
(a)(l) of this section must be at least
V4 inch high; other markings must be
legible.
(b) [Reserved]
[29 PR 18951. Dec. 29.1964. Redesignated at
32 PR 5606. Apr. 5, 1967. and amended by
Amdt. 178-40. 41 FR 38182. Sept. 9.1976]
Page 44
-------
TECHNICAL REPORT DATA
(Pleas* read Inttnicttons on ittt rererre In (or* comptttuw
1. REPORT NO.
EPA-340/1-91-010
4. TITLE AND SUBTITLE ,
Standard Procedure for Coll
Samples for VOC Content Ana
24 and 24A
7. AUTHORISI
Bruce A. Olson, Helinda K.
2.
ection of Coating and Ink
lysis by Reference Method
Wood, John T. Chehaske
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Pacific Environmental Services, Inc. (PES)
560 Herndon Parkway, Suite 200
Hemdon, Virginia 22070-5225
12. SPONSORING AGENCY NAME ANO ADDRESS
U.S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Stationary Source Compliance Division
Washington, O.C. 20460
3. RECIPIENT'S ACCESSION NO.
S. REPORT DATE
Nay 1991
6. PERFORMING ORGANIZATION CODE
8. PERFORMING ORGANIZATION REPORT NO.
91-133-T4/S
10. PROGRAM ELEMENT NO.
WA 91-133
11. CONTRACT/GRANT NO.
68-02-4464
13. TYPE OF REPORT ANO PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES Cfag fllSO'
SSCD, Organic Chemicals Section, 401 M St., S.W., (EN-34W) EPA-340/1-91-011: Analysis
Washington, D.C. 20460 Phone: (703) 308-8668 EPA-340/1-91-012: References
This standard operating procedure (SOP) document 1s prepared with
the intent of providing simple step-by-step instructions, covering all
aspects of sampling coatings and inks, for use by EPA, State, and local
regulatory agencies nationwide. The instructions are presented 1n
general terms as much as possible while providing sufficient details for
actual field sampling. The procedure should be used in conjunction with
existing health and safety programs and 1n accordance with existing EPA
or other agency training guidelines.
Standard procedures are presented for sampling and handling of
S??t;I2s»?iS.1nlc$ that re°.u1re analysis by EPA Reference Methods 24 or
24A (RM 24/24A) as found in 40 CFR 60, Appendix A. This SOP has been
expanded from an original version obtained from EPA Region II. For the
purpose of developing consistency among agency inspectors nationwide in
terms of sampling conducted, it delineates the activities deemed proper
and necessary to ensure that the sample taken is representative of the
coating or ink as applied. If the activities are conducted as
described, questions concerning the credibility of sampling performed
can be avoided.
7.
L
Air Pollution
Coatings
Inks
Analysis
Sol vents
KIY WORDS ANO DOCUMENT ANALYSIS
DESCRIPTORS ™~ "~"~ "~~
Sampling
VOC
ASTH Methods
b.lOENTIFIERS/OPCN ENDED TERMS
Sampling of Coatings and
Inks
19. SECURITY CLASS iTIutRtpOrtl
Unelas^lffpH
20. SECURITY CLASS /TWl p*ffT'
Uncl assif led
c. COSATI Ffel&Group
36
22. PRICE
EPA F*m 2220-1 ()<•«• 4-771 ••cvious KOITIOM •• OMOLBTC
------- |