&EPA
OSWER9360405
United States
Environmental Protection
Agency
Office of Emergency and
Remedial Response
Washington, DC 20460
PB92-963406
Publication 9360.4-05
May 1992
Superiund
Compendium of ERT
Air Sampling Procedures
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OSWER Directive 9360.4-05
May 1992
COMPENDIUM OF ERT
AIR SAMPLING PROCEDURES
SUMMA Canister Cleaning
SUMMA Canister Sampling
GC/MS Analysis of Tenax/CMS Cartridges and SUMMA Canisters
Preparation of SUMMA Canister Field Standards
Low Level Methane Analysis for SUMMA Canister Gas Samples
Asbestos Sampling
Tedlar Bag Sampling
Charcoal Tube Sampling
Tenax Tube Sampling
Polyurethane Foam Sampling
Interim Final
Environmental Response Team
Emergency Response Division
Office of Emergency and Remedial Response
U.S. Environmental Protection Agency
Washington, DC 20460
U s Environmental Protection Agency
Region 5, Library (PL-12J)
77 West Jackson Boulevard, 12th Floor
Chicago, IL 60604-3590
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Notice
This document has been reviewed in accordance with U.S. Environmental Protection Agency policy and approved
for publication. Mention of trade names or commercial products does not constitute endorsement or
recommendation for use.
The policies and procedures established in this document are intended solely for the guidance of government
personnel, for use in the Superfund Removal Program. They are not intended, and cannot be relied upon, to
create any rights, substantive or procedural, enforceable by any party in litigation with the United States. The
Agency reserves the right to act at variance with these policies and procedures and to change them at any time
without public notice.
Depending on circumstances and needs, it may not be possible or appropriate to follow these procedures exactly
in all situations due to site conditions, equipment limitations, and limitations of the standard procedures.
Whenever these procedures cannot be followed as written, they may be used as general guidance with any and
all modifications fully documented in either QA Plans, Sampling Plans, or final reports of results.
Each Standard Operating Procedure in this compendium contains a discussion on quality assurance/quality
control (QA/QC). For more information on QA/QC objectives and requirements, refer to the Quality
Assurance/Quality Control Guidance for Removal Activities, OSWER directive 9360.4-01, EPA/540/G-90/004.
Questions, comments, and recommendations are welcomed regarding the Compendium of ERT Air Sampling
Procedures. Send remarks to:
Mr. William A. Coakley
Removal Program QA Coordinator
U.S. EPA - ERT
Raritan Depot - Building 18, MS-101
2890 Woodbridge Avenue
Edison, NJ 08837-3679
For additional copies of the Compendium of ERT Air Sampling Procedures, please contact:
National Technical Information Service (NTIS)
U.S. Department of Commerce
5285 Port Royal Road
Springfield, VA 22161
(703) 487-4600
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Table of Contents
Section Page
1.0 SUMMA CANISTER CLEANING: SOP #1703
1.1 Scope and Application 1
1.2 Method Summary 1
1.3 Sample Canister Handling and Storage 1
1.3.1 Canister Receipt 1
1.3.2 Canister Storage 1
1.4 Interferences and Potential Problems 1
1.5 Equipment/Apparatus 1
1.5.1 Canister 1
1.5.2 Canister Cleaning System 2
1.6 Reagents 2
1.7 Procedures 2
1.7.1 System Set-Up 2
1.7.2 Cleaning 2
1.7.3 Leak-Testing 3
1.8 Calculations 3
1.9 Quality Assurance/Quality Control 4
1.10 Data Validation 4
1.11 Health and Safety 4
2.0 SUMMA CANISTER SAMPLING: SOP #1704
2.1 Scope and Application 5
2.2 Method Summary 5
2.3 Sample Preservation, Containers, Handling, and Storage 5
2.4 Interferences and Potential Problems 5
2.5 Equipment/Apparatus 5
2.5.1 Subatmospheric Pressure Sampling Equipment 5
2.5.2 Pressurized Sampling Equipment 7
2.6 Reagents 7
2.7 Procedures 7
2.7.1 Subatmospheric Pressure Sampling 7
2.7.2 Pressurized Sampling 7
2.8 Calculations 8
2.9 Quality Assurance/Quality Control 8
2.10 Data Validation 9
2.11 Health and Safety 9
111
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Section Page
3.0 GC/MS ANALYSIS OF TENAX/CMS CARTRIDGES AND SUMMA
CANISTERS: SOP #1705
3.1 Scope and Application 11
3.2 Method Summary 11
3.2.1 Tenax/CMS Cartridges 11
3.2.2 SUMMA Canisters 11
3.3 Sample Preservation, Containers, Handling, and Storage 11
3.3.1 Tenax/CMS Cartridges 11
33.2 SUMMA Canisters 11
3.4 Interferences and Potential Problems 12
3.5 Equipment/Apparatus 12
3.6 Reagents 13
3.7 Procedures 14
3.7.1 Daily GC/MS Tuning 14
3.7.2 GC/MS Calibration 14
3.7.3 Analysis Conditions 14
3.7.4 Tenax/CMS Cartridge Analysis 15
3.7.5 Canister Sample Analysis 16
3.7.6 Analysis of Canister Samples Adsorbed onto Cartridges 17
3.8 Calculations 17
3.9 Quality Assurance/Quality Control 18
3.10 Data Validation 18
3.11 Health and Safety 18
4.0 PREPARATION OF SUMMA CANISTER FIELD STANDARDS: SOP #1706
4.1 Scope and Application 19
4.2 Method Summary 19
4.3 Sample Preservation, Containers, Handling, and Storage 19
4.4 Interferences and Potential Problems 19
4.5 Equipment/Apparatus 19
4.6 Reagents 19
4.7 Procedures 20
4.8 Calculations 20
4.9 Quality Assurance/Quality Control 21
4.10 Data Validation 21
4.11 Health and Safety 21
5.0 LOW LEVEL METHANE ANALYSIS FOR SUMMA CANISTERS GAS
SAMPLES: SOP #1708
5.1 Scope and Application 23
5.2 Method Summary 23
5.3 Sample Preservation, Containers, Handling, and Storage 23
iv
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Section Page
5.4 Interferences and Potential Problems 23
5.5 Equipment/Apparatus 23
5.6 Reagents 23
5.7 Procedures 23
5.7.1 Gas Chromatograph 23
5.7.2 Calibration 24
5.73 Injection of Sample 24
5.8 Calculations 24
5.9 Quality Assurance/Quality Control 24
5.9.1 Precision 24
5.9.2 Accuracy 25
5.10 Data Validation 25
5.11 Health and Safety 25
6.0 ASBESTOS SAMPLING: SOP #2015
6.1 Scope and Application 27
6.2 Method Summary 27
6.2.1 Pump Calibration 27
6.2.2 Outdoor/Ambient Sampling 28
6.2.3 Indoor/Ambient Sampling 28
6.2.4 Aggressive Sampling 28
6.3 Sample Preservation, Containers, Handling, and Storage 28
63.1 Filter Selection and Collection Device 28
6.3.2 Sample Handling Procedures 30
6.4 Interferences and Potential Problems 30
6.4.1 NIOSH Method 7400 (PCM) 30
6.4.2 EPA's TEM Method 30
6.5 Equipment 30
6.5.1 Personal Sampling Pump 30
652 High Flow Pump 30
6.6 Reagents 31
6.7 Procedures 31
6.7.1 Preparation 31
6.7.2 Aggressive Sampling 31
6.7.3 Personal Sampling Pump 31
6.7.4 High Flow Pump 32
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Section Page
6.7.5 Calibration 32
6.8 Calculations 32
6.9 Quality Assurance/Quality Control 33
6.9.1 Electronic Calibration - Personal Sampling Pump 33
6.9.2 Electronic Calibration - Rotameter 33
6.9.3 Sampling Pump Calibration - Rotameter 34
6.10 Data Validation 34
6.11 Health and Safety 34
7.0 TEDLAR BAG SAMPLING: SOP #2050
7.1 Scope and Application 35
7.2 Method Summary 35
7.3 Sample Preservation, Containers, Handling, and Storage 35
7.4 Interferences and Potential Problems 35
7.5 Equipment/Apparatus 36
7.6 Reagents 36
7.7 Procedures 36
7.7.1 Preparation 36
7.7.2 Field Operation 36
7.7.3 Post Operation 37
7.8 Calculations 37
7.9 Quality Assurance/Quality Control 37
7.10 Data Validation 37
7.11 Health and Safety 37
8.0 CHARCOAL TUBE SAMPLING: SOP #2051
8.1 Scope and Application 39
8.2 Method Summary 39
8.3 Sample Preservation, Containers, Handling, and Storage 39
8.4 Interferences and Potential Problems 39
8.5 Equipment/Apparatus 39
8.5.1 Equipment List 39
8.5.2 Equipment Source 40
8.6 Reagents 40
8.7 Procedures 40
8.7.1 Calibration 40
8.7.2 Field Operation 40
8.7.3 Post Operation 40
VI
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Section Eag£
8.8 Calculations 41
8.9 Quality Assurance/Quality Control 41
8.10 Data Validation 41
8.11 Health and Safety 41
9.0 TENAX TUBE SAMPLING: SOP #2052
9.1 Scope and Application 43
92 Method Summary 43
93 Sample Preservation, Containers, Handling, and Storage 43
9.4 Interferences and Potential Problems 44
9.5 Equipment 44
9.5.1 Equipment List 44
95.2 Equipment Source 44
9.6 Reagents 44
9.7 Procedures 44
9.7.1 Calibration 44
9.7.2 Field Operation 45
9.7.3 Post Operation 45
9.8 Calculations 45
9.9 Quality Assurance/Quality Control 45
9.10 Data Validation 46
9.11 Health and Safety 46
10.0 POLYURETHANE FOAM SAMPLING: SOP #2069
10.1 Scope and Application 47
10.2 Method Summary 47
103 Sample Preservation, Containers, Handling, and Storage 47
10.4 Interferences and Potential Problems 47
10.5 Equipment 47
10.5.1 Sampling Media (Sorbents) 47
10.5.2 Sampling Equipment 47
10.6 Reagents 47
10.7 Procedures 48
10.7.1 Calibration of Timer, Meters, and Standards 48
10.7.2 Field Calibration of High Volume Sampler 48
10.7.3 Sample Module Preparation 48
10.7.4 Unit Operation 49
10.7.5 Unit Shutdown and Sample Collection 50
VII
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Section Page
10.8 Calculations 50
10.9 Quality Assurance/Quality Control SO
10.10 Data Validation 50
10.11 Health and Safety 50
APPENDIX A - Figures 51
APPENDIX B - Canister Sampling Field Data Sheet 107
REFERENCES 111
vui
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Ust of Exhibits
Exhibit
Table 1
Table 2
Table 3
Table 4
Table 5
Table 6
Table 7
Table 8
Table 9
Table 10
Table 11
Figure 1
Figure 2
Figure3
Figure 4
Figure 5
Figure 6
Figure 7
Figures
Figure 9
Figure 10
Figure 11
Figure 12
Figure 13
SOP
Page
Volatile Organic Compound Data Sheet
Compounds Analyzed in Tenax/CMS Cartridges
or SUMMA Canisters
GC/MS Performance Criteria for p-Bromofluorobenzene
(EPA Method 624)
Target Compounds Analyzed for Calibration
Typical Desorber Conditions
Chromatographic Conditions
Sampling Stations for Outdoor Sampling
Sampling Stations for Indoor Sampling
Asbestos Sampling Flow Rates
Compounds Detected by Tenax/CMS
Recommended Flow Rates and Sample Volumes
SUMMA Canister Cleaning System
Pressurized and Subatmospheric Canister Sampling Systems
Tekmar Model 5010
GC/MS Printout
SUMMA Canister Sample Dilution Line
SUMMA Canister Analysis Train (Tekmar 5010 GC)
Canister Sample Absorbed onto Tenax
Teflon Tee11 Setup
SUMMA Canister Charging System
Septum Tee" Setup
Teflon Nut with Septum
Phase Contrast Microscopy Filter Cassette
Transmission Electron Microscopy Filter Cassette
1704
1705
1705
1705
1705
1705
2015
2015
2015
2052
2052
1703
1704
1705
1705
1705
1705
1705
1706
1706
1706
1706
2015
2015
6
12
14
15
16
16
29
29
33
43
44
53
55
57
59
61
63
65
67
69
71
73
75
77
IX
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Exhibit SOP Page
Figure 14 Personal Sampling Train for Asbestos 2015 79
Figure 15 High Flow Sampling Train for Asbestos 2015 81
Figure 16 Calibrating a Personal Sampling Pump with a Bubble Meter 2015 83
Figure 17 Calibrating a Rotameter with a Bubble Meter 2015 85
Figure 18 Calibrating a Personal Sampling Pump with a Rotameter 2015 87
Figure 19 Tedlar Bag Sampling Apparatus 2050 89
Figure 20 Calibrating a Double Manifold Charcoal Tube with a Rotameter 2051 91
Figure 21 Charcoal Sampling, Straight 2051 93
Figure 22 Charcoal Sampling, Single Manifold 2051 95
Figure 23 Tenax Calibration with a Secondary Calibrator 2052 97
Figure 24 Tenax/CMS Sampling Train 2052 99
Figure 25 Manometer 2069 101
Figure 26 Canister Sampling Module 2069 103
Figure 27 High Volume PUF Sampler 2069 105
Canister Sampling Field Data Sheet 1704 109
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Acknowledgments
Preparation of this document was directed by William A. Coakley, the Removal Program QA Coordinator of
the Environmental Response Team, Emergency Response Division. Additional support was provided under U.S.
EPA contract #68-03-3482 and U.S. EPA Contract #68-WO-0036.
XI
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1.0 SUMMA CANISTER CLEANING: SOP #1703
1.1 SCOPE AND APPLICATION
This procedure is intended for use when cleaning
SUMMA polished stainless steel canisters.
SUMMA canisters are able to sample gas-phase
volatile organic compounds (VOCs) on site at
concentrations of one part per billion by volume
(ppbv) and greater. This cleaning procedure
ensures that canisters have been sufficiently cleaned
prior to sampling, to the extent that no VOC
contamination is present at concentrations greater
than 0.2 ppbv.
1.2 METHOD SUMMARY
After use, canisters are logged in and physically
inspected. These canisters are vented to the outside
air under an operating exhaust hood. Canisters are
connected to a manifold which is attached to a
vacuum pump via a cryogenic trap. The canisters
and lines are evacuated and then the canisters are
heated for a prescribed time period. During the
heating period, the canisters are filled with
humidified nitrogen and pressurized. Three cycles
of filling and pressurizing, then evacuation and
heating, are required.
Confirming that the canisters are free of VOC
contamination involves pressurizing the canisters
with ultrahigh purity nitrogen and analyzing on the
gas chromatograph/mass spectrometer (GC/MS).
If no VOC contamination is present at
concentrations greater than 0.2 ppbv, the canister is
considered clean. Clean canisters are leak-tested by
pressurizing with nitrogen for 24 hours. Canisters
that have been cleaned and found to be without
leaks are evacuated. These canisters are logged as
cleaned and certified and are stored in the
evacuated state with brass cap fittings until needed
for sampling.
1.3 SAMPLE CANISTER
HANDLING AND STORAGE
1.3.1 Canister Receipt
1. Observe the overall condition of each sample
canister. Any canister having physical defects
requires corrective action.
2. Observe each canister for an attached sample
identification number.
3. Record each canister hi the dedicated
laboratory logbook by its SUMMA canister
number.
1.3.2 Canister Storage
1. Store canisters in an evacuated state of less
than O.OS mm Hg and with a brass cap in
place. The canisters remain hi this state
until needed.
2. Attach an identification tag to the neck of
each canister for field notes and chain-of-
custody purposes.
3. Record each canister in the dedicated
laboratory logbook stating the canister
status and storage location. Also, note on
the identification tag the date cleaned and
date certified dean, as well as the initials
of the operator.
1.4 INTERFERENCES AND
POTENTIAL PROBLEMS
Contamination may occur in the sample canisters if
they are not properly cleaned before use. All other
equipment used in this process must be sufficiently
clean. All gases and solvents used must be of a
certified purity to avoid contamination. Canisters
must be stored with the valve closed and the brass
caps in place to avoid vacuum loss.
1.5 EQUIPMENT/APPARATUS
1.5.1 Canister
• sample canister -- leak-free stainless steel
pressure vessels of desired volume (e.g., 6-
L), with valve and SUMMA passivated
interior surfaces or equivalent.
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Although there maybe other sources, two
readily available sources are Scientific
Instrumentation Specialists, Inc., P.O. Box
8941, Moscow, ID, 83843; or Andersen
Samplers, Inc., 4215-C Wendell Dr.,
Atlanta, GA, 30315.
1.5.2 Canister Cleaning
System
Figure 1 in Appendix A displays the canister
cleaning system.
• vacuum pump — capable of evacuating
sample canister(s) to an absolute pressure
of <0.05 mm Hg.
• manifold - stainless steel manifold with
connections for simultaneously cleaning
several canisters.
• shutoff valve(s) -- three on/off toggle
valves (Valves A, B, D).
• shutoff valve ~ one variable metering valve
(Valve C) to regulate flow of zero air.
• shutoff valve - one variable metering valve
(Valve E) used as an on/off valve between
the nitrogen regulator and the supply line.
• stainless steel vacuum gauge ~ capable of
measuring vacuum in the manifold to an
absolute pressure of 0.05 mm Hg or less.
• cryogenic trap ~ stainless steel U-shaped
open tubular trap cooled with liquid
nitrogen to prevent contamination from
back diffusion of oil from vacuum pump.
Also, a stainless steel two-stage pressure
regulator 0-690 kPa (0-100 psig) to regulate
nitrogen pressure.
• Teflon tee with a septum port - an
injection port capable of introducing
distilled, deionized water to provide
moisture to the zero air supply line.
• isothermal oven ~ a system for canisters or
equivalent. Although there may be other
sources, one readily available source is
Fisher Scientific, Pittsburgh, PA, Model
349.
1.6 REAGENTS
• gas cylinders of nitrogen, ultrahigh purity
grade.
• cylinders of liquid nitrogen, ultrahigh purity
grade.
• cryogen ~ liquid nitrogen (bp -195°C).
• distilled, deionized water, ultrahigh purity.
1.7 PROCEDURES
1.7.1 System Set-Up
1. Seal all connections in the vacuum system
except the canisters and manifold. Check all
connections, lines, and valves for leaks by
pressurizing the line to 30 psig and using a
soap solution. Check the septum for leaks by
removing it and visually inspecting it.
2. Add the liquid nitrogen to the cryogenic trap
and allow it to reach a state of equilibrium.
3. Check the pump to assure proper working
order by achieving a vacuum of 0.05 mm Hg in
the line that normally attaches to the manifold
but is now capped. Valve A is open and
Valves B, C, D, and E are closed. After the
vacuum test is completed, turn the pump off
and remove the cap to break the vacuum.
4. Check the oven to assure proper working order
by heating the oven to 100°C and measuring
the internal temperature with a thermometer.
5. Check reagents to assure proper purity.
6. Set the back pressure on the nitrogen to 30
psig.
1.7.2 Cleaning
1. Vent all canisters to the outside air under an
operating exhaust hood.
2. Connect the canisters (with the valves closed on
the canisters) to the manifold by the Swagelok
fittings. Connect the manifold to the vacuum
system by the Swagelok fitting.
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3. Open Valve A, ensure Valves B, C, D, and E
are closed, and start vacuum pump.
4. Once a vacuum (O.OS mm Hg) is obtained in
the line and the manifold, close valve A.
Examine the system for leaks by comparing the
initial vacuum reading and a second vacuum
reading 3 minutes later. If the vacuum
deteriorates more than 5 mm Hg, a leak exists
and corrective action is necessary.
5. If no leaks are observed, open valve A and the
Canister 1 valve. Evacuate Canister 1 to 0.05
mm Hg, then dose the Canister 1 valve. By
evacuating one canister at a time, the potential
for cross-contamination between canisters is
minimized.
6. Evacuate all other canisters in the same manner
as described in step 5.
7. After all four canisters are evacuated, open all
canister valves. Turn on the oven and heat to
100°C.
8. Continue evacuating canisters for 1 hour at
100°C. Document the time.
9. After 1 hour, Valve A is closed and Valves B,
C, D, and E are opened, with Valve C metering
the flow of nitrogen.
10. Inject 400 fjL of distilled deionized water via a
syringe through the septum in the nitrogen line.
11. Allow the canisters to pressurize to 30 psig.
12. Close Valves B, C, D, and E.
13. Close canister valves.
14. Repeat steps 5 through 13, twice.
15. Close valves on canisters.
16. Close Valve A.
17. Turn off vacuum pump.
18. Disconnect manifold from cleaning system.
19. Disconnect canisters from the manifold and
place a brass cap on each canister.
20. Choose one canister of this set of four that was
analyzed as being the most highly contaminated
previous to cleaning. Fill this canister with
ultrahigh purity nitrogen air to a pressure of 30
psig.
21. Analyze the above canister for VOC
contamination by GC/MS. If this canister is
sufficiently clean to the extent that no VOC
contamination is present at concentrations
greater than 0.2 ppbv, then all canisters in that
set of four are considered clean. Document
the results. If it is not sufficiently clean, see
step 23.
22. Evacuate the above canister again to 0.05 mm
Hg, cap it with a brass fitting, and store it with
the other three of the lot. Document the
location.
23. If the above canister is not sufficiently dean
(i.e., VOC contamination is present at
concentrations greater than 0.2 ppbv), then all
canisters in that lot must be cleaned again until
the canisters meet the prescribed criteria.
Document the results.
1.7.3 Leak-Testing
1. Once the canister lot is determined to be dean,
the canisters are pressurized to 30 psig with
nitrogen.
2. The initial pressure is measured, the canister
valve is closed, and the brass cap is replaced.
Document the time and pressure.
3. After 24 hours, the final pressure is checked.
Document the time and pressure.
4. If leak-proof, the pressure should not vary
more than +13.8 kPa (±2 psig) over the 24-
hour period. If this criterion is met, the
canister is capped with a brass fitting and
stored. If a leak is present, corrective action is
required. Document the results.
1.8 CALCULATIONS
There are no calculations for this SOP.
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1.9 QUALITY ASSURANCE/
QUALITY CONTROL
The following specific quality assurance/quality
control procedures are applicable for SUMMA
canister cleaning:
1. Check all connections, lines, and valves to
ensure no leaks are present.
2. Check the septum to ensure no leaks are
present, by removing the septum and visually
examining it.
3. Check the pump to ensure proper working
order by achieving a vacuum of 0.05 mm Hg
prior to cleaning.
4. Check the oven to ensure proper working order
by comparing the oven setting at 100°C to the
internal temperature with a thermometer.
5. Check the reagents to ensure sufficient purity.
6. Evacuate all canisters to 0.05 mm Hg during
each cycle of the cleaning process and
document the results.
7. Evacuate all canisters at 100°C for 1 hour
during each cycle of the cleaning process.
Document the results.
8. Evacuate, heat, and pressurize all canisters
three times during the cleaning process.
Document each cycle.
9. For the canister lot to be considered cleaned,
the selected canister from the cleaning lot to be
tested must be analyzed by GC/MS and shown
to be sufficiently cleaned to the extent that no
VOC contamination is present at concentrations
greater than 0.2 ppbv. If the VOC contam-
ination is greater than 0.2 ppbv, the canister lot
must be cleaned again. In either case,
document the results.
10. Leak-test all canisters
document the results.
for 24 hours and
11. Store and evacuate all canisters, and cap them
with a brass fitting. Document the pressure
and location of all canisters.
1.10 DATA VALIDATION
This section is not applicable to this SOP.
1.11 HEALTH AND SAFETY
When working with potentially hazardous materials,
follow U.S. EPA, OSHA, and site-specific safety
practices. More specifically:
• Liquid nitrogen is used to cool the
cryogenic trap. Its boiling point is -196°C.
Insulated gloves, lab coat, face shield, and
safety glasses must be worn when using this
material. Liquid nitrogen must be
transported only in properly constructed
containers.
• Ultrahigh purity nitrogen is used to dean
the canisters and must be labeled properly.
All cylinders must be securely fastened to
a stationary object. The cylinder valve
should only be opened by hand. The
proper regulator must be used and set
correctly.
• The oven is set to a temperature of 100°C.
Insulated gloves should be worn when
handling items heated to this temperature.
• Prior to cleaning, canisters are to be vented
to the atmosphere under an operating
exhaust hood. The hood must be in proper
working order.
• Canisters are pressurized during the
cleaning operation. No canister is to be
pressurized above 30 psig. The maximum
pressure limit for the SUMMA canisters is
40 psig.
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2.0 SUMMA CANISTER SAMPLING: SOP #1704
2.1 SCOPE AND APPLICATION
The purpose of this Standard Operating Procedure
(SOP) is to describe a procedure for sampling of
volatile organic compounds (VOCs) in ambient air.
The samples are collected as whole air samples in
passivated SUMMA stainless steel canisters. The
VOCs are subsequently separated by gas
chromatography (GC) and measured by mass-
selective detector or multidetector techniques. This
SOP describes procedures for sampling with
canisters at final pressures both above atmospheric
pressure (referred to as pressurized sampling) and
below atmospheric pressure (referred to as
subatmospheric pressure sampling).
This method is applicable to specific VOCs that
have been tested and determined to be stable when
stored in pressurized and subatmospheric pressure
canisters. The organic compounds that have been
successfully collected in pressurized canisters by this
method are listed in table 1, Volatile Organic
Compound Data. These compounds have been
measured at the parts per billion by volume (ppbv)
level.
2.2 METHOD SUMMARY
Both pressurized and subatmospheric pressure
sampling modes use an initially evacuated canister.
Both modes may also use a mass flow
controller/sample pump arrangement, fixed orifice,
capillary, or adjustable micrometering valve to
regulate flow. With this configuration, a sample of
ambient air is drawn through a sampling train
comprised of components that regulate the rate and
duration of sampling into a pre-evacuated passivated
SUMMA canister.
2.3 SAMPLE PRESERVATION,
CONTAINERS, HANDLING, AND
STORAGE
After the air sample is collected, the canister's valve
is closed, an identification tag is attached to the
canister, and the canister is transported to a
laboratory for analysis. Upon receipt at the
laboratory, the canister tag data are recorded.
Sample holding and expiration times should be
determined prior to initiating field activities.
2.4 INTERFERENCES AND
POTENTIAL PROBLEMS
Contamination may occur in the sampling system if
canisters are not properly cleaned before use.
Additionally, all other sampling equipment (e.g.,
pump and flow controllers) should be thoroughly
cleaned. Instructions for cleaning the SUMMA
canisters are described in ERT SOP #1703,
SUMMA Canister Cleaning.
2.5 EQUIPMENT/APPARATUS
See figure 2 for a diagram of pressurized and
subatmospheric canister sampling systems.
2.5.1 Subatmospheric Pressure
Sampling Equipment
• VOC canister sampler — whole air sampler
capable of filling an initially evacuated
canister by action of the flow control from
near 30 inches of mercury (Hg) vacuum to
near atmospheric pressure (such as
Andersen Samplers, Inc., NuTech,
Scientific Instrumentation Specialists (SIS),
or homemade subatmospheric canister
samplers).
• sampling inlet line -- stainless steel tubing
to connect the sampler to the sample inlet.
• sample canister (6-liter size) ~ leak-free
stainless steel pressure vessels of desired
volume with valve and SUMMA passivated
interior surfaces (SIS, Andersen Samplers,
Inc., or equivalent).
• participate matter filter — 2-/zm sintered
stainless steel in-line filter (Nupro Co.,
Model SS-2F-K4-2, or equivalent).
• chromatographic-grade stainless steel
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Table 1: Volatile Organic Compound Data Sheet
Compound Name (synonym)
Freon 12 (dichlorodifluoromethane)
methyl chloride (chloromethane)
Freon 114 (l,2-dichloro-l,l,2,2-tetrafluoroethane)
vinyl chloride (chloroethylene)
methyl bromide (bromomethane)
ethyl chloride (chloroethane)
Freon 11 (trichlorofluoromethane)
vinylidene chloride (1,1-dichloroethene)
dichloromethane (methylene chloride)
Freon 113 (l,l,2-trichloro-l,2^-trifluoroethane)
1,1-dichloroethane (ethylidene chloride)
cis-l,2-dichloroethylene
chloroform (trichloromethane)
1,2-dichloroethane (ethylene dichloride)
methyl chloroform (1,1,1-trichloroethane)
benzene (cyclohexatriene)
carbon tetrachloride (tetrachloromethane)
1,2-dichloropropane (propylene dichloride)
trichloroethylene (trichloroethene)
ds-13-dichloropropene (cis-13-dichloropropylene)
Formula
a2CF2
CH3C1
C1CF2CC1F2
CH2=CHC1
CHjBr
CH3CH2C1
CC13F
C&2C12
CH2C12
CFjClCCljF
CH3CHC12
CHC1=CHC1
CHClj
C1CH2CH2C1
CH3CC13
QH,
CO,
CH3CHC1CH2C1
C1CH=CC12
C1CH2CH=CHC1
Molecular
Weight
120.91
50.49
170.93
62.50
94.94
64.52
13738
96.95
84.94
18738
98.%
96.94
11938
98.%
133.41
78.12
153.82
112.99
131.29
110.97
Boiling
Point (°C)
-29.8
-24.2
4.1
-13.4
3.6
12.3
23.7
31.7
39.8
47.7
57.3
603
61.7
83.5
74.1
80.1
76.5
%.4
87.0
76.0
Melting
Point (°C)
-158.0
-97.1
-94.0
-1538.0
-93.6
-136.4
-111.0
-122.5
-95.1
-36.4
-97.0
-80.5
-63.5
-353
-30.4
5.5
-23.0
-100.4
-73.0
CAS
Number
74-87-3
75-01-4
74-83-9
75-00-3
......
75-35-4
75-09-2
74-34-3
67-66-3
107-06-2
71-55-6
71-43-2
56-23-5
78-87-5
79-01-6
-------
tubing and fittings for interconnections --
all materials in contact with sample,
analyte, and support gases should be
chromatographic-grade stainless steel.
• fixed orifice, capillary, or adjustable
micrometering valve ~ used in lieu of the
electronic flow controller/sample pump for
grab samples or short duration time-
integrated samples.
2.5.2 Pressurized Sampling
Equipment
• VOC canister sampler ~ whole air sampler
capable of filling an initially evacuated
canister by action of the flow controller and
pump from near 30 inches Hg vacuum to
15-20 psi atmospheric pressure (Andersen
Samplers Inc., NuTech, SIS, or equivalent
pressurized canister sampling system).
• mass flowmeter/controller - leak-free,
linearly proportioned mass flowmeter/
controller unit at desired flowrate (e.g., 100
mL/min). Although there may be other
sources, a mass flowmeter/controller is
available from Tylan, 15 Meadowview Ln,
Medford, NJ 08055.
• sampling inlet line ~ stainless steel tubing
to connect the sampler to the sample inlet.
• sample canister ~ leak-free stainless steel
pressure vessels of desired volume with
valve and SUMMA passivated interior
surfaces (SIS, Andersen Samplers, Inc., or
equivalent).
• particulate matter filter — 2-fjm sintered
stainless steel in-line filter (Nupro Co.,
Model SS-2F-K4-2, or equivalent).
• chromatographic-grade stainless steel
tubing and fittings for interconnections -
all materials in contact with sample,
analyte, and support gases should be
chromatographic-grade stainless steel.
2.6 REAGENTS
This section is not applicable to this SOP.
2.7 PROCEDURES
2.7.1 Subatmospheric Pressure
Sampling
1. Prior to sample collection, complete the
appropriate information on the Canister
Sampling Field Data Sheet (Appendix C).
2. Open a canister, which is evacuated to 28-30
inches Hg at sea level and fitted with a flow
restricting device, to the atmosphere containing
the VOCs to be sampled. The pressure
differential causes the sample to flow into the
canister. (Note: at higher elevations the
vacuum may be less.) See section 2.8 to
calculate the flow rate.
3. This technique may be used to collect grab
samples (duration of 10 to 30 seconds) or
time-integrated samples (duration of 12 to 24
hours). Sampling duration depends on the
degree to which the flow is restricted. The
flow will remain constant until the vacuum
reads approximately 11 inches Hg. When this
occurs, control the flow, either manually or
automatically, to achieve constant flow.
4. After sampling is complete, record the
appropriate information on the Canister
Sampling Field Data Sheet.
2.7.2 Pressurized Sampling
1. Prior to sample collection, complete the
appropriate information on the Canister
Sampling Field Data Sheet.
2. Use a digital time-programmer to pre-select
sample duration, and start and stop times.
3. Open a canister, which is evacuated to 28-30
inches Hg at sea level and connected in line
with the sampler, to the atmosphere containing
the VOCs to be sampled.
4. Using a direct drive blower motor assembly,
draw a whole air sample into the system
through a stainless steel inlet tube. (Some
units do not have a blower.)
5. Using a specially modified inert sample pump
in conjunction with a flow controller, pull a
small portion of this whole air sample from the
-------
6.
inlet tube. The initially evacuated canister is
filled by action of the flow controlled pump to
a positive pressure not to exceed 25 psig.
Upon sampling completion at the location,
complete the requisite information on the
Canister Sampling Field Data Sheet.
2.8 CALCULATIONS
A flow control device maintains a constant flow into
the canister over the desired sample period. This
flow rate is determined so that the canister is filled
over the desired sampling period, to 2-5 inches Hg
vacuum for subatmospheric pressure sampling or to
about one atmosphere (15 psi) above ambient
pressure for pressurized sampling.
1.
For subatmospheric sampling, the volume of
the sample must be calculated before the flow
rate can be determined. The sample volume
can be calculated by:
S = V -
where:
S = sample volume (cm3)
V = volume of the canister (cm3)
I = initial canister vacuum (in. Hg)
E = estimated final vacuum (in. Hg)
For example, to calculate the sample volume of a 6-
L canister with an initial canister vacuum of 28
inches Hg and an estimated final vacuum of 5
inches Hg.
/6000 • 5\
S - 6000 -
\ 28
S = 4929 cm3
The flow rate can be calculated by:
F =
T (60)
where:
F = flow rate (cm3/min or mL/min)
S = sample volume (cm3)
T = sample period (hours)
Using a 24-hour sampling period for the above
sample volume, the flow rate can be calculated
as:
4929
F =
24 • 60
F = 3.42 cm3/min
2. For pressurized sampling, only the flow rate
has to be calculated.
For example, if a 6-L canister is to be filled
with 12-L of sample at 2 atmospheres absolute
pressure (near 30 psia) in 24 hours, the flow
rate can be calculated by:
F =
F = 8.3 cm3/min
12000
24 • 60
3. If the canister pressure is increased for analysis,
a dilution factor (DF) is calculated and
recorded on the sampling data sheet.
DF = —-
where:
P, = canister pressure (psig) after
pressurization,
PJ = canister pressure (psig) before
pressurization
After sample analysis, detected VOC concentrations
are multiplied by the dilution factor to determine
concentration in the sampled air.
2.9 QUALITY ASSURANCE/
QUALITY CONTROL
The following general quality assurance procedures
apply:
» All data must be documented on standard
chain-of-custody forms, field data sheets, or
within site logbooks.
• All instrumentation must be operated in
accordance with operating instructions as
-------
supplied by the manufacturer, unless 2.11 HEALTH AND SAFETY
otherwise specified in the work plan.
Equipment checkout and calibration When working with potentially hazardous materials,
activities must occur prior to follow U.S. EPA, OSHA, and site-specific health
sampling/operation, and they must be and safety practices. More specifically, pressurizing
documented. of SUMMA canisters should be performed in a
well-ventilated room, or preferably under a fume
hood. Care must be taken not to exceed 40 psig in
2.10 DATA VALIDATION the canisters. Canisters are under pressure, albeit
only 20-30 psig, and should not be dented or
This section is not applicable to this SOP. punctured. They should be stored in a cool, dry
place and always be placed in their plastic shipping
boxes during transport and storage.
-------
3.0 GC/MS ANALYSIS OF TENAX/CMS CARTRIDGES
AND SUMMA CANISTERS: SOP #1705
3.1 SCOPE AND APPLICATION
The purpose of this Standard Operating Procedure
(SOP) is to describe the analysis of air samples
collected on either Tenax/Carbonized Molecular
Sieve (CMS) cartridges or in SUMMA canisters by
Gas Chromatography/Mass Spectrometry
(GC/MS). These methods are applicable to volatile
organic compounds (VOCs) that can be sampled by
one or both of these media. The VOCs that can be
routinely analyzed at the parts per billion (ppb)
level for both sample collection methods are listed
in table 2.
3.2 METHOD SUMMARY
These methods involve thermal desorption of
cartridges or canisters into a cryogenic trap. The
trap cryofocuses the sample onto the head of the
analytical column, then flash heats the sample and
separates it by gas chromatography. Following
separation, compounds are analyzed by a positive-
ion, electron-impact, mass spectrometer.
3.2.1 Tenax/CMS Cartridges
Analysis of Tenax/CMS cartridges for toxic organics
in ambient air combines methods TO1 and TO2.
The cartridges contain two different sorbent media.
The gas sample is drawn through a glass tube
containing Tenax (a porous polymer of 2,6-diphenyl
phenylene oxide, the sorbent media for TO1) and
Carbonized Molecular Sieve (CMS, the sorbent
media for TO2). Further information on
Tenax/CMS tube sampling may be found in ERT
SOP #2052, Tenax Tube Sampling.
3.2.2 SUMMA Canisters
Alternatively, air samples can be collected in
passivated, 6-liter, stainless steel SUMMA canisters
and analyzed according to method TO14, a
procedure similar to the Tenax/CMS cartridges.
Information on SUMMA canister sampling may be
found in ERT SOP #1704, SUMMA Canister
Sampling.
3.3 SAMPLE PRESERVATION,
CONTAINERS, HANDLING, AND
STORAGE
3.3.1 Tenax/CMS Cartridges
Samples collected on Tenax/CMS cartridges are
placed in clean culture tubes and forwarded as soon
as possible to the laboratory. The culture tubes
should be labeled and sealed with Teflon tape
around the cap. Samples must be accompanied by
a chain-of-custody (COC) record indicating
sampling locations, sample numbers, date collected,
sample matrix, and sample volumes. The COC
should agree with the information on the culture
tube labels, and discrepancies must be noted on the
COC at the time of receipt by the laboratory. In
addition, any looseness of culture tube caps or any
obvious physical damage or contamination (e.g.,
broken cartridges, condensate in the culture tubes,
or discoloration of the Tenax bed), must also be
recorded on the COC.
Once samples have arrived at the laboratory, they
should be refrigerated until they are analyzed.
Analysis of Tenax/CMS samples must be completed
within the 14-day holding time specified by TO1 and
TO2. The holding time begins when the sample is
first drawn onto the tube (not when the sample is
received by the laboratory).
3.3.2 SUMMA Canisters
Samples collected in canisters should arrive at the
laboratory with the canister valve closed and the
sampling port capped. An identification tag should
be attached and should agree with the information
on the COC.
One of the advantages of canister samples is that
they do not need any refrigeration or special
handling until they are analyzed. Method TOW
does not specify a holding time for canister samples.
11
-------
Table 2: Compounds Analyzed in Tenax/CMS Cartridges or SUMMA Canisters
• acetone
• Ca-Cg alcohols
• C4-C12 alkanes
• C4-CJ2 alkenes
• C,-C6 alkylbenzenes
• benzene
• bromochloromethane
• bromodichloromethane
• p-bromofluorobenzene
• 2-butanone (MEK)
• carbon tetrachloride
• chlorobenzene
• chloroethane
• chloromethane
• chlorotoluene
• Cs-Cj2 cydoalkanes
• dibromomethane
• 1,1-dichloroethane
• 1,2-dichloroethane
* CrQa dienes
• ethylbenzene
• 4-methyl-2-pentanone
(MIBK)
• methylene chloride
• napthalene
• styrene
• C10 terpenes
• 1,1,2,2-tetrachloroethane
• tetrachloroethene (PCE)
• toluene
• trans-l,2-dichloroethene
• 1,1,1-trichloroethane
• 1,1,2-trichloroethane
• trichloroethene (TCE)
• trichlorofluoromethane
• trichloromethane
• vinyl chloride
• xylenes
3.4 INTERFERENCES AND
POTENTIAL PROBLEMS
• Structural isomers having coeluting
retention times and identical mass spectra
will interfere with this method. The most
common interference seen in these
methods is between meta-xylene and para-
xylene.
• Excessive moisture in Tenax/CMS samples
will cause the cryotrap to freeze, restricting
sample flow from the desorber oven and
resulting in poor recoveries. In general,
trapping efficiencies for components with
boiling points greater than water are more
adversely affected than those with lower
boiling pouits. If excessive moisture is
suspected, the CMS section of the cartridge
should be removed prior to sample
desorption. If this step is taken, the lower
boiling point compounds trapped by the
CMS, such as chloromethane and vinyl
chloride, will not be seen in the analysis.
Canister samples suspected of having high
concentrations of carbon dioxide (such as
those collected from landfills or fire
plumes), cannot be directly analyzed since
the carbon dioxide will collect and freeze
the cryotrap. This can be avoided by
adsorbing the sample on a Tenax/CMS
cartridge, which does not adsorb carbon
dioxide, but retains the organic
contaminants.
3.5 EQUIPMENT/APPARATUS
• GC/MS - gas chromatograph capable of
sub-ambient temperature programming
interfaced with a mass spectrometric
detector (Hewlett Packard 5996 GC/MS
equipped with Series 1000E computer and
RTE-6 software, or equivalent).
• thermal desorber — capable of a -170°C to
250°C temperature range, equipped with
GC interface (Tekmar 5010 GT automatic
12
-------
thermal desorption/cryofocusing unit, or
equivalent).
chromatographic column - capillary
column, 30 m x 0.32 mm, 0.25 /an film
thickness, (J & W Scientific, Inc. DB-624,
or Restek, Inc. RTx-5, or equivalent).
pre-column - capillary fused silica column,
0.5 m x 0.32 mm, with column connector
(Restek, Inc., or equivalent).
Tenax/CMS cartridges -- 150 mg Tenax
35/50 mesh and 150 mg CMS packed into
6 x 120 mm borosilicate glass tubing with
Pyrex glass wool on each end and between
each phase, provided in sealed glass
ampoules (Supelco, Inc., or equivalent).
See the EMSL SOP for Preparation of
Clean Tenax Cartridges.
canisters - passivated 6-liter SUMMA
canisters (Andersen Samplers, Inc., or
equivalent).
mass flow controller — 0-100 mL/min, to
maintain constant flow for measuring
canister sample volumes (Unit Instruments,
Inc., UFC-1100 with URS 100 Readout
Power Supply, or equivalent).
stainless steel vacuum/pressure gauge -
capable of measuring 0 to 50 psi (Pennwalt
Corp., Wallace and Tiernan Division,
Model series 1500 dial instrument, or
equivalent).
chromatographic-grade, stainless steel
tubing and stainless steel plumbing fittings.
stainless steel cylinder regulators (5) ~
two-stage pressure regulators for cylinders
of helium, zero air, calibration standards,
and surrogate standards.
syringes - 2.5-10 mL, for injecting
calibration and surrogate standards
(Dynatech - Precision Sampling, Inc., or
equivalent).
9.5 mm septa (Supelco, Inc. Microsep
F-174, or equivalent).
culture tubes, Pyrex and Teflon tape - for
preserving Tenax/CMS samples.
rotameter - 0-100 mL/min (Matheson Gas
Products, Inc., or equivalent).
cotton cloths — 9 inch by 9 inch, for
Tenax/CMS cartridge handling (Texwipe,
Co., or equivalent).
tweezers -- for inserting and removing
cartridge samples from thermal desorber.
O-rings — Viton, 6 mm I.D., for retaining
Tenax/CMS cartridges in thermal desorber
(Hewlett-Packard part no. 5061-5867, or
equivalent).
3.6 REAGENTS
• calibration standards -- at approximately 1
ppmv with the balance as nitrogen
(Matheson Gas Products, Inc., or
equivalent).
• bromochloromethane (BCM) and p-
bromofluorobenzene (BFB) -- at
approximately 1 ppmv in nitrogen in a
separate cylinder; both compounds used as
surrogate standards, BFB also used for
tuning GC/MS (Scott Specialty Gases, Inc.
or equivalent).
• perfluorotributylamine (PFTBA) — for
tuning the mass spectrometer (Hewlett
Packard, Inc., or equivalent).
• liquid nitrogen - for cryogenic cooling
(SOS Gases, Inc., or equivalent).
• helium - ultrahigh purity, used as carrier
gas and as purge gas in the thermal
desorber (Matheson Gas Products, Inc., or
equivalent).
• carbon dioxide ~ bone-dry, high-pressure
liquid, for chromatograph oven cooling
(Matheson Gas Products, Inc., or
equivalent).
• compressed air — ultrazero grade, for
chromatograph oven door control
(Matheson Gas Products, Inc., or
equivalent).
• nitrogen — ultrahigh purity, for pressurizing
13
-------
canister samples and purging canister
analysis train lines (Matheson Gas
Products, Inc., or equivalent).
3.7 PROCEDURES
3.7.1 Daily GC/MS Tuning
At the beginning of each day, tune the GC/MS
system to verify that acceptable performance criteria
can be achieved. The mass spectrometer should
first be automatically or manually tuned on
perfluorotributylamine (PFTBA). PFTBA tuning is
done to demonstrate that the instrument is
operating properly and, upon analysis of
p-bromofluorobenzene (BFB), will give a spectrum
that meets the ion abundance criteria listed in EPA
Method 624 (table 3).
Table 3: GC/MS Performance Criteria
for p-Bromofluorobenzene
(EPA Method 624)
m/z
50
75
95
96
173
174
175
176
177
Ion Abundance Criteria
15% to 40% of mass 95
30% to 60% of mass 95
Base peak, 100% relative
abundance
5% to 9% of mass 95
< 2% of mass 174
> 50% of mass 95
5% to 9% of mass 174
95% - 101% of mass 174
5% to 9% of mass 176
After PFTBA tuning, BFB is analyzed to check GC
column performance and is used as the GC/MS
performance standard. This performance test must
be passed before any samples, standards, or blanks
are analyzed, and must be repeated for every twelve
hours of continuous operation. A background
correction mass spectrum from the performance test
must satisfy the criteria set forth in U.S. EPA
Method 624. If the criteria are not met, the analyst
must re-tune the mass spectrometer and repeat the
test until all criteria are met.
3.7.2 GC/MS Calibration
1. Initial Calibration -- Before any analysis,
initially calibrate the GC/MS using standards
contained in pressurized cylinders at
approximately 1 ppmv in nitrogen. A list of the
target compounds in the calibration standards
is given in table 4, along with the ions used for
quantitation. A multipoint calibration is
created by injecting three to five different
volumes into the thermal desorber and
analyzing them in the GC/MS. Typical
volumes range from 1-10 mL, corresponding to
concentrations of 100 ppb to 1 ppm. Following
analysis of all calibration points, a calibration
report is prepared listing the average response
factors and then- Relative Standard Deviation
(RSD), which must be less than 25% for each
compound. For each compound in the
calibration, the retention times and relative
abundances of selected ions are stored on the
hard disk of the GC/MS computer to be used
for compound identification.
2. Continuing Calibration — For each day of
analysis, check the GC/MS calibration before
sample analysis with a daily standard, usually at
the 1-ppmv concentration. The continuing
calibration is only acceptable when all
compound abundances in the daily standard are
± 25% of the average response factor of the
calibration curve.
3.7.3 Analysis Conditions
All samples are prepared for GC/MS analysis by
using a thermal desorption/cryogenic trapping unit.
The unit is equipped with a 0.25-inch by 7-inch oven
chamber for desorbing samples, an internal
cryogenic trap (C-l) consisting of a 0.125-inch
stainless-steel tube filled with Pyrex glass beads, an
eight port switching valve, and an external cryogenic
trap (C-2) located just above the head of the
pre^column (figure 3, appendix A). A 60-inch
silcosteel transfer line connects the two cryotraps.
The pre-column connects C-2 with the analytical
column, and is installed to prevent the column from
being exposed to the wide temperature swings that
occur at the trap. After surrogates have been
introduced on a sample cartridge, the sample is then
thermally desorbed by heating the oven while
14
-------
Table 4: Target Compounds
Analyzed for Calibration
Compound
benzene
bromodichloromethane
carbon tetrachloride
chloroethane
chloromethane
dibromomethane
1,1-dichloroethane
1,2-dichloroethane
1,1-dichloroethene
trans- 1,2-
dichloroethene
ethylbenzene
m-ethyltoluene
methylene chloride
styrene
1,1,2,2-
tetrachloroethane
tetrachloroethene
1,1,1-trichloroethane
1,1,2-trichloroethane
trichloroethene
trichlorofluoromethane
trichloromethane
toluene
vinyl chloride
m-xylene
o-xylene
Quantitation Ions
78
83
117
64
50
174
63
62
61
61
91
120
84
104
83
166
97
97
130
101
83
92
62
91
91
purging with helium.
The helium transfers the VOCs from the cartridge
to the C-l trap. The sample is then passed through
a heated transfer line and cryofocused at C-2, at
the front of the pre-column, where it is injected by
flash heating. Table 5 summarizes typical desorber
conditions. The chromatographic conditions used
are those listed in table 6, as modified from U.S.
EPA Method 524.2.
An example of the GC/MS Printout is found in
figure 4 (appendix A), which includes target and
surrogate compounds in elution order.
3.7.4 Tenax/CMS Cartridge Analysis
Handle all Tenax/CMS samples with cotton cloth or
gloves and tweezers to avoid contamination. To
analyze a cartridge sample, follow these steps.
1. Place the cartridge in the desorb oven, CMS
side first, so that it is downflow from the
Tenax. Start the thermal desorber going into
the purge step. Set the flow at 20 mL/min.
2. During the purge step, inject 10 mL of a 1-ppm
mixture of the surrogate standards
(bromochloromethane [BCM] and
p-bromofluorobenzene [BFB]), onto the Tenax
side of each sample cartridge. Lower the purge
flow to 5 mL/min, so that the combined flow
through the cartridge does not exceed 20
mL/min.
3. After the surrogates have been introduced on
the tube and the purge cycle has been
completed, the first cryogenic trap (C-l) is
cooled with liquid nitrogen to -160°C. At this
time, remove the cartridge, turn it around, and
reinsert it into the desorb oven; the Tenax side
of the cartridge is now downflow of the CMS.
4. Once the tube has been inverted and C-l has
been cooled, step the thermal desorber to the
desorb cycle, allowing the surrogates to desorb
from the Tenax and CMS with the sample and
flow directly to C-l.
5. At the end of desorb, step the desorber again,
cooling the C-2 cryotrap. When C-2 is cooled,
the desorber will automatically step to the
transfer step, and the sample is cryofocused at
C-2.
15
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Table 5: Typical Desorber Conditions
Parameter
Desorb Temperature
Desorb Time
Cryotrap-1 (C-l) Temperature
Cryotrap-1 Desorb Temperature
Transfer (C-l to C-2)
Cryotrap-2 (C-2) Temperature
Cryotrap-2 Desorb Temperature
Cryotrap-2 Desorb Time
Value
240°C
10.0 minutes (Tenax/CMS only)
-160°C
250°C
3.5 minutes
-160°C
2500C
2.0 minutes
Table 6: Chromatographic Conditions
Parameter
Initial Temperature
Initial Time
Ramp Rate
Final Temperature
RunTime
Value
5.0° C
3.0 minutes
8.0° C/minute
185.0° C
25.5 minutes
6. When transfer is complete, the sample will be
injected by automatic flash heating of C-2. The
analysis then follows the chromatographic
conditions in table 6.
3.7.5 Canister Sample Analysis
Canister samples are usually collected at or near
atmospheric pressure. To allow the sample to flow
from the canister, the canister pressure must be
raised above one atmosphere with ultrahigh purity
nitrogen. Normally, sample pressure is doubled for
ease of calculation.
1. Before attaching the canister sample, purge the
pressurizing line of the apparatus with nitrogen
as indicated in figure 5 (appendix A). Attach
the canister sample to the pressurizing
apparatus and close the regulator to the
nitrogen cylinder. Open the canister valve,
allow the pressure to equilibrate, and record
the initial pressure (PJ in the analysis log.
2. Open the cylinder regulator slowly so the
pressure gradually increases. When the
canister pressure reaches twice the Pj, close the
regulator, then close the canister valve, and
record the final pressure (Pj) in the analysis
log.
3. Attach the canister to the analysis train at the
desorb oven as shown in figure 6 (Appendix
A). With the mass flow controller valve closed,
open the canister valve to allow the sample to
come to equilibrium in the sample train.
4. Start the thermal desorber, and step through
16
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the purge step to the step that cools C-l.
When the desorber steps to desorb, lower the
flow to zero. Open the mass flow controller
valve and begin timing sample flow. The
controller flow rate and the desorb tune needed
for the sample to flow are calculated based on
the sample volume required and the equations
in section 3.8.
5. Close the canister valve after the precise
amount of desorb time has elapsed. Close the
mass flow controller valve after the analysis
train pressure reaches zero.
6. Replace the desorb oven cover attached to the
canister analysis train with the desorb oven
cover used for Tenax/CMS samples. Raise the
helium flow to 5 mL/min, and inject 10 mL of
the surrogate standards while still in desorb. At
the end of desorb, follow the analysis procedure
in section 7.4, steps 5 and 6.
3.7.6 Analysis of Canister Samples
Adsorbed on Cartridges
Canister samples are adsorbed on Tenax/CMS
cartridges when the samples are suspected of
containing high levels of carbon dioxide or other
permanent gases that would freeze the cryotraps.
1. Follow the procedure in section 3.7.5, steps 1
and 2, for the pressurization of the canister
sample.
2. Place a Tenax/CMS cartridge in the desorb
oven with the CMS side in first. Attach the
canister to the analysis train as shown in figure
7 (appendix A).
3. With the mass flow controller valve closed,
open the canister valve to allow the sample to
come to equilibrium in the sample train.
4. Start the thermal desorber into the purge step.
Lower the purge flow to zero. Open the mass
flow controller valve and let the desired sample
volume adsorb onto the cartridge.
5. After the sample has been adsorbed, close the
canister and mass flow controller valves, replace
the desorb oven cover, and inject 10 mL of the
surrogate standards while still in the purge step.
6. After surrogates have been spiked on the
cartridge, step the desorber to cool C-l, and
follow the Tenax/CMS analysis procedure in
section 3.7.4, steps 3 through 6.
3.8 CALCULATIONS
Concentrations of target compounds are calculated
by the GC/MS computer software. To establish
concentration limits that the GC/MS can measure,
limits of quantitation (LOQ) are calculated for each
sample. LOQs are calculated by the following:
LOQ =
(LCV) (SC)
SV
where:
LCV = lowest calibration volume
SC = standard concentration
SV = sample volume (in miUiliters)
LOQ varies inversely with the sample volume, and
can range from 500 ppb for a minimal sample
volume of 5 mL, to as low as 0.1 ppb for a 25-L
sample.
When the canister pressure is increased, the dilution
factor (DF) is calculated by the foUowing:
Pf
DF = -^
where:
P, = canister pressure (psi) after pressurization,
P, = canister pressure (psi) before
pressurization
The following equation calculates the desorb time
necessary for a given sample volume and flow rate:
where:
FR
DT = desorb tune (in minutes)
SV = sample volume (in miUiliters)
DF = dilution factor (usually 2)
FR = flow rate (in mL/min)
For example, with a DF of 2 and a flow rate of 40
mL/min, it would take 5 minutes to desorb 100 mL
of unpressurized sample (equivalent to 200 mL of
pressurized sample). For larger sample volumes, it
may be necessary to set the thermal desorber for
17
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longer than 10 minutes to desorb the sample and
allow tune for surrogate spiking.
3.9 QUALITY ASSURANCE/
QUALITY CONTROL
The following quality
procedures apply:
assurance/quality control
• Two criteria must be satisfied to verify the
identification of a target compound:
Retention Time - A sample
component's retention time (RT)
must be within ± 0.50 minutes of
the RT of the standard
component. For reference, the
standard must be run on the same
day as the sample.
Spectra - (1) All ions present in
the standard mass spectra at a
relative intensity greater than 10%
(where the most abundant ion in
the spectrum equals 100%) must
be present in the sample
spectrum. (2) The relative
intensities of the ions specified
above must agree within ± 20%
between the sample and the
reference spectra.
• The GC/MS is tuned daily for PFTBA to
meet the abundance criteria for BFB as
listed hi U.S. EPA Method 624. The tune
is adjusted when necessary.
• An acceptable three-to-five point
calibration of the standards must be run
before the analysis. A calibration is
acceptable if the Relative Standard
Deviation is <25% of the average response
factors for each compound. Samples are
quantitated on the average response factors
of the calibration range.
• A continuing calibration standard must be
run for each day of analysis. Standards
are checked against the average response
factors of the calibration range; if any
standard component varies by greater than
25% of the average response factor, re-run
the continuing calibration. If the second
continuing calibration has components
varying by greater than 25% of the average
response factor, run a new initial
calibration.
A surrogate standard of BFB and BCM is
added to all standards and samples.
Percent recoveries for samples are
calculated against daily standards.
Recoveries should be within 70% to 130%
for BFB and BCM.
Method blanks are analyzed after a
standard analysis to check for carryover,
and are also necessary after analyzing
samples with high levels of contamination.
For Tenax/CMS samples, a method blank
is an analysis of a new cartridge spiked
with surrogates. For canister samples, a
method blank is flowing the same volume
of nitrogen as the samples into the
desorber, followed by surrogate spiking.
For canister samples adsorbed onto
cartridges, a method blank is a volume of
nitrogen equal to the sample volumes
adsorbed on a cartridge, followed by
surrogate spiking and analysis.
Ten percent of all samples received are to
be analyzed hi replicate.
Performance Evaluation (PE) canisters
containing known concentrations of VOCs
should be analyzed at least once per
analysis for canister samples. The
analytical procedure is the same for
canister samples.
3.10 DATA VALIDATION
Review of the data generated should be conducted
according to the Quality Assurance/Quality Control
considerations listed hi section 3.9.
3.11 HEALTH AND SAFETY
When working with potentially hazardous materials,
follow U.S. EPA, OSHA, and laboratory health and
safety practices.
18
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4.0 PREPARATION OF SUMMA CANISTER FIELD STANDARDS:
SOP #1706
4.1 SCOPE AND APPLICATION
This Standard Operating Procedure (SOP) describes
the preparation of SUMMA canister field standards.
SUMMA polished canisters are used to store
calibration gas standards for transport to field
sampling sites. These standards will be used for
calibrating field instruments. In addition, a series of
different concentrations of gas standards, or
dilutions in the field of a single canister, can be
used to construct calibration curves and to ascertain
minimum detection limits on various field
instrumentation currently used by EPA/ERT.
4.2 METHOD SUMMARY
A certified gas standard cylinder is selected and set
for delivery pressure of 20-30 psig. The hoses are
bled with the gas standard. Then, a clean,
evacuated SUMMA canister is attached to the gas
standard line and is opened and charged to 20-30
psig with the certified gas standard cylinder. The
SUMMA canister is closed and the gas standard
lines are removed. A "tee" with a septum is
attached onto the Swagelok fitting of the SUMMA
canister. The "tee" is purged with the contents of
the SUMMA canister. The SUMMA canister valve
is opened and samples are taken via a gas-tight
syringe through the septum on the "tee." When not
La use, the valve is dosed. Tedlar bags can also be
filled from the "tee."
4.3 SAMPLE PRESERVATION,
CONTAINERS, HANDLING, AND
STORAGE
Samples and gas standards can be kept several
months in the SUMMA polished canisters. Care
must be taken to ensure no leaks occur when the
"tee" and septum are used. In addition, the needle
valve on the SUMMA canister must be completely
dosed when not in use. When transporting and
storing, the SUMMA canister is placed in a plastic
shipping container. This will protect the canister
from accidental punctures or dents.
4.4 INTERFERENCES AND
POTENTIAL PROBLEMS
As long as the gas standards and all transfer lines
are clean, no interferences are expected. The initial
pressure of the SUMMA canister should be
recorded after filling. In addition, the pressure
should be recorded after each use. A dramatic
drop in pressure (e.g., 5 psig or more) may
invalidate the use of that canister.
4.5 EQUIPMENT/APPARATUS
• SUMMA canister, 6-liter total volume.
While there may be other sources, two
readily available sources are Cat. # 87-300,
Anderson Samplers, Inc. 4215 Wendell
Drive, Atlanta, GA 30376; PN # 0650, SIS,
P.O. Box 8941, 815 Courtney St., Moscow,
Idaho 83843.
• certified gas standard from Scott Gas,
Matheson or other reliable manufacturer.
• Hamilton gas-tight syringe with Teflon-seal
plugs in various sizes.
• dean Teflon tubing, 1/4-inch OD.
• Teflon Swagelok "tee," 1/4-inch OD.
• 1/4-inch Teflon Swagelok nuts and ferrules.
• 9-mm Septa, preferably Teflon backed.
• stainless steel Swagelok on/off or needle
valve, 1/4-inch OD.
4.6 REAGENTS
All standards must be vapor-phase pressurized gas
cylinders, certified by the manufacturer to be within
±2% accuracy, and to be National Bureau of
Standards (NBS) traceable. Scott Specialty Gas or
Matheson Gas can provide these standards. If field
19
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dilution is required, a cylinder of ultrahigh purity air
is required.
4.7 PROCEDURES
1. Obtain a SUMMA polished canister that has
been cleaned and evacuated as per ERT SOP
#1703 (SUMMA Canister Cleaning) and select
a compressed-gas cylinder of a certified
standard. This standard should be certified by
the manufacturer to be within ±2% accuracy of
the concentration level and be NBS traceable.
2. Attach a high-purity, dual-stage regulator to the
standard cylinder. This must deliver 20-30 psig
pressure at an accuracy of ± 10% or better.
3. Attach a section of clean, unused 1/4-inch OD
Teflon tubing to the Teflon "tee." The side port
of the "tee" has an on/off valve or needle valve
connected to it (see figure 8, appendix A).
4. Temporarily connect a vent line to the outlet
port of the side valve and vent it to a fume
hood or to an outside vent. The SUMMA
canister charging system appears in figure 9,
appendix A.
5. Open the standard cylinder to 20-30 psig at the
outlet of the cylinder regulator.
6. The needle valve on the SUMMA canister is
still closed at this point. Open the side valve on
the "tee" and allow the standard cylinder's 1/4-
inch Teflon feed lines to vent for 1 to 2
minutes.
7. Then close the valve tightly and slowly open the
needle valve on the SUMMA canister. A
hissing noise should be heard. Allow the
canister to continue filling. Do not fill the
SUMMA canister too rapidly.
8. Periodically check the pressure on the dual
stage regulator attached to the standard
cylinder to ensure 20-30 psig is being delivered.
9. Once the hissing stops, the canister should be
filled to approximately the same pressure as
that of the source line.
10. Close the needle valve on the SUMMA canister
tightly.
11. Close the standard cylinder and vent the feed
lines.
12. Remove the feed line from the top of the
Teflon "tee."
13. Place a Swagelok back ferrule, in the inverted
position, on the top of the "tee". This will
provide a flat surface on which a Teflon-backed
septum can be placed.
14. Place the Teflon-backed septum, Teflon side
down. The septum should create a gas-tight fit
once a 1/4-inch Swagelok nut is tightened onto
the top of the "tee" (see figures 10 and 11,
appendix A).
15. Open the needle valve on the SUMMA canister
to check for leaks throughout the "tee",
particularly in the septum fitting. Do this with
the valve on the side of the "tee" closed.
16. Afterwards, slowly open the side valve of the
"tee" and vent for 1/2 minute and re-close.
The septum "tee" is now ready for sampling
from the canister using a gas-tight syringe
through the septum seal.
17. Close the SUMMA canister needle valve
between sample taking with the gas-tight
syringe.
18. Periodically, vent or flush the "tee" to provide
fresh standard for sampling. The side valve can
also be used, after flushing, to fill Tedlar bags
with the standard from the SUMMA canister.
4.8 CALCULATIONS
The procedure for performing field dilutions of the
standards from the SUMMA canisters must be
documented. This allows for the recalculation of
concentrations of standards if any discrepancies
arise in the calibration of the field instrumentation.
Simple volumetric dilutions using Hamilton gas-tight
syringes are performed using Tedlar bags with ultra-
high purity air as the diluent.
20
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4.9 QUALITY ASSURANCE/
QUALITY CONTROL
The concentration levels of the certified gas
standards must be recorded. The vendor typically
provides the analysis of certification with each
standards cylinder; a copy should be provided with
the SUMMA canister.
As previously stated, the pressure of the canister
along with the date and time, should be recorded at
the initial filling and at the end of each use of the
canister. A drop in pressure of 5-10 psig between
usages may invalidate the canister for use as a
calibration standard. Certification of canister
cleaning and evacuation should be noted prior to
filling with standards.
4.10 DATA VALIDATION
This section is not applicable to this SOP.
4.11 HEALTH AND SAFETY
Pressurizing of SUMMA canisters should be
performed in a well-ventilated room, or preferably
under a fume hood. Care must be taken not to
exceed 40 psig in the canisters. Canisters are under
pressure, albeit only 20-30 psig, and should not be
dented or punctured. They should be stored in a
cool, dry place and always be placed in their plastic
shipping boxes during transport and storage.
21
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5.0 LOW LEVEL METHANE ANALYSIS FOR
SUMMA CANISTER GAS SAMPLES: SOP# 1708
5.1 SCOPE AND APPLICATION
This Standard Operating Procedure (SOP) is
intended for use when analyzing SUMMA canister
gas samples for low parts per million volume
(ppmv) levels of methane.
5.2 METHOD SUMMARY
A flame ionization detector (FID) gas
chromatograph (GC) is used to separate and
quantitate methane in gas samples. The sample is
introduced into the carrier gas as a plug and passes
through a gas chromatography column, which then
separates it into two peaks. The first peak is
unresolved air; the second peak is resolved
methane. Peak areas are used in conjunction with
calibration plots for quantitative measurements.
This separation is completed in 5 minutes.
• carrier gas cylinder -- ultrahigh purity
helium with a two-stage regulator
delivering a pressure of 90 psi.
• 1 mL and 01 mL precision gas-tight
syringes with needles for sample
introduction.
• gas chromatography column -- 10 feet by
1/4 inch stainless steel column packed with
Spherocarb, 100/120 mesh (or equivalent),
capable of operating at 100°C, as well as
injection temperatures of 200°C.
• electronic integrator - Spectra-Physics
SP4290 integrator (or equivalent).
• septum port adaptor for SUMMA canister.
• soap film flow meter (or equivalent).
5.3 SAMPLE PRESERVATION,
CONTAINERS, HANDLING, AND
STORAGE
Refer to U.S. EPA Method TOW concerning
SUMMA canister cleaning and sample collection.
In addition, refer to ERT SOP #1703, SUMMA
Canister Cleaning and ERT SOP #1704, SUMMA
Canister Sampling.
Canisters are stored and analyzed at room
temperature.
5.6 REAGENTS
• helium — ultrahigh purity grade helium
(99.9999%).
• hydrogen - ultrahigh purity grade hydrogen
(99.9999%).
• air « ultrazero air (<0.05 ppmv total
hydrocarbon).
• calibration standards (hi the range of 5-100
ppmv) — methane standards, balance air.
5.4 INTERFERENCES AND
POTENTIAL PROBLEMS
This section is not applicable to this SOP.
5.5 EQUIPMENT/APPARATUS
• gas chromatograph ~ Varian 3400 gas
chromatograph with flame ionization
detector (or equivalent) capable of
operating at 225°C.
5.7 PROCEDURES
5.7.1 Gas Chromatograph
1. Turn the carrier gas on and adjust the flow rate
to 40 mL per minute.
2. Turn the air on and adjust the flow rate to ISO
mL per minute.
23
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3. Turn the hydrogen on and adjust the flow rate
to 30 mL per minute.
4. Check the flows with a soap film flow meter.
5. Ignite the flame ionization detector and allow it
to equilibrate for 10 minutes.
6. Turn the integrator on and zero it before
samples are introduced.
5.7.2 Calibration
L Introduce, via 1-mL syringe, aliquots (of the
same size as will be used on the sample
injections) of the standard calibration gas
mixtures into the gas chromatograph injector.
At least one injection of each standard gas
mixture is required before starting to analyze
samples. Perform the very first calibration in
triplicate.
2. Verify the initial calibration by injecting a
complete set of at least four standards (at least
five different concentrations of standards are
routinely available from commercial suppliers)
at the beginning of each day's analytical
activities. It is suggested that each sample
injection be followed systematically by a
standard injection so that many injection areas
are tabulated and averaged in the report.
5.7.3 Injection of Sample
1. Withdraw a 1-mL sample from the SUMMA
septum port using a 1-mL gas-tight syringe.
2. Quickly inject the sample, guarding against
blow-back of the plunger. Simultaneously,
activate the integrator and label the sample run.
3. End the integrator run in 5 minutes and re-zero
before the next analysis.
Samples analyzed above the calibrated linear range
can be reanalyzed by injecting a smaller volume, or
by diluting in ultrahigh purity zero air to acquire
responses within the linear range. These dilutions
may be done by injecting a measured volume of the
sample into a Tedlar bag and adding a measured
volume of zero air. For instance, 100 mL of sample
measured with a gas-tight syringe, added to 900 mL
of zero air, would be diluted by a factor of 10.
These volumes have to be recorded and taken into
account in the calculations.
5.8 CALCULATIONS
Prepare a linear standard curve of ppmv versus
peak area. Calculate the sample concentrations
using the formula y = mx + b; where y is the peak
area, m is the slope (peak area/ppmv), b is the y
intercept (peak area), and x is the concentration
(ppmv).
The above equation may be rearranged to:
x = y - —
m
where y is measured area, corresponding to a
sample injection and x is the desired methane
concentration in the sample injection. If a dilution
has been made then, of course, the concentration
obtained must be multiplied by the ratio of the final
sample volume to the initial sample volume. Most
integrator packages will handle the above
calculations but it is recommended that a
commercial spreadsheet program be used.
5.9 QUALITY ASSURANCE/
QUALITY CONTROL
The following quality assurance/quality control
procedures are applicable.
5.9.1 Precision
The precision of the method is monitored during
the second lowest calibration standard from the
linear curve. A control range is established for the
standard using three standard deviations from the
mean of 10 independent analyses. The standard is
analyzed periodically (at the beginning and end of
a series of samples or every 8 hours) and must
respond within the range of three standard
deviations for the system and data precision to be
considered under control. If the results of the
standard analysis are out of range, the system must
be repaired and the standards rerun, or a new
calibration curve must be performed.
24
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5.9.2 Accuracy 5.11 HEALTH AND SAFETY
The accuracy of the method is monitored by When working with potentially hazardous materials,
periodically analyzing blind performance evaluation refer to U.S. EPA, OSHA and site-specific health
samples. These samples should not be prepared by and safety practices.
the same outside source which provided the
calibration standards.
5.10 DATA VALIDATION
Data will be evaluated based on the information
provided in section 5.9.
25
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6.0 ASBESTOS SAMPLING: SOP #2015
6.1 SCOPE AND APPLICATION
The objective of this Standard Operating Procedure
(SOP) is to outline a method for sampling asbestos
fibers in indoor and outdoor/ambient air at
hazardous waste sites.
Regulations pertaining to asbestos have been
promulgated by U.S. EPA and OSHA. U.S. EPA's
National Emission Standards for Hazardous Air
Pollutants (NESHAP) regulates asbestos-containing
waste materials. NESHAP establishes management
practices and standards for the handling of asbestos
and emissions from waste disposal operations (40
CFR Part 61, Subparts A and M).
Both 40 CFR 763 and its addendum provide
comprehensive rules for the asbestos abatement
industry. State and local regulations on these issues
vary and may be more stringent than federal
requirements.
The OSHA regulations in 29 CFR 1910.1001 and 29
CFR 1926.58 specify work practices and safety
equipment such as respiratory protection and
protective clothing for handling asbestos. Also,
these regulations specify:
• The OSHA standard for an 8-hour, tune-
weighted average (TWA) is 0.2 fibers/cm3
of air. This standard pertains to fibers with
a length-to-width ratio of 3 to 1 with a
fiber length >5 fan.
• An action level of 0.1 fibers/cm3 (one-half
the OSHA standard) is the level U.S. EPA
has established at which employers must
initiate such activities as air monitoring,
employee training, and medical
surveillance.
References to specific analytical methodologies are
made throughout this document. Also, be aware
that EPA is developing an Environmental Asbestos
Assessment Manual. An interim draft document
titled "Superfund Method for the Determination of
Asbestos in Ambient Air, Part 1: Method" (May
1990) is available and recommended for use as the
most current method.
6.2 METHOD SUMMARY
Asbestos has been used in many commercial
products including such building materials as
flooring tiles and sheet goods, paints and coatings,
insulation, and roofing asphalt. These products and
others may be found at hazardous waste sites
hanging on overhead pipes, contained in drums,
abandoned in piles, or as part of a structure.
Asbestos tailing piles from mining operations can
also be a source of ambient asbestos fibers.
Asbestos air sampling is conducted by drawing air
through a filter at a known flow rate with a flow-
controlled pump. The sample is then analyzed
using Phase Contrast Microscopy (PCM) and/or
Transmission Electron Microscopy (TEM).
PCM analysis is widely available and is less costly
than TEM. TEM is considered the best method for
identifying airborne asbestos. TEM can detect very
thin fibers typically down to 0.0025 fan in diameter.
When TEM-produced data (U.S. EPA) is compared
with data from PCM (NIOSH), the TEM's aspect
ratio of 5 to 1 should be modified to 3 to 1.
6.2.1 Pump Calibration
In order to determine if a sampling pump is
measuring the flow rate or volume of air correctly,
it is necessary to calibrate the instrument. Sampling
pumps should be calibrated immediately before and
after each use. Preliminary calibration should be
conducted using a primary calibrator such as a soap
bubble type calibrator, (e.g., a Buck Calibrator,
Gilibrator, or equivalent primary calibrator) with a
representative filter cassette installed between the
pump and the calibrator. The representative
sampling cassette can be reused for calibrating
other pumps that will be used for asbestos sampling.
The same cassette lot used for sampling should also
be used for the calibration. A sticker should be
affixed to the outside of the extension cowl marked
"Calibration Cassette." A rotameter can be used
provided it has been recently precalibrated with a
primary calibrator. Three separate constant flow
calibration readings should be obtained both before
and after collecting the sample. Should the flow
rate change by more than 5% during the sampling
27
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period, the average of the pre- and post-calibration
rates will be used to calculate the total sample
volume. Sampling pumps can be calibrated prior to
coming on site so that time is saved when
performing onsite calibration.
Personal sampling pumps are utilized when the flow
rates are between .001 L/min to 5 L/min. Many
lightweight portable pumps are capable of providing
high or low volume air flow. See the
manufacturer's manual for pump operation.
High-flow pumps are utilized when flow rates
between 4 L/min to 16 L/min are required. High-
flow pumps are used for short sampling periods to
obtain the desired sample volume. ERT uses the
Gilian Aircon 520. An equivalent high-flow pump
can also be used.
High-flow pumps usually run on AC power and can
be plugged into a nearby outlet. If an outlet is not
available, then a generator should be obtained. The
generator should be positioned downwind from the
sampling pump. Additional voltage may be
required if more than one pump is plugged into the
same generator. Several electrical extension cords
may be required if sampling locations are remote.
6.2.2 Outdoor/Ambient Sampling
PCM analysis may be used for outdoor/ambient air
samples. When analysis shows total fiber count
above the EPA action level of 0.1 fibers/cm3 of air,
then TEM can be used to identify asbestos from
non-asbestos fibers. Some labs are able to perform
PCM and TEM analysis on the same filter,
however, this should be verified with the laboratory
prior to analysis.
High-volume pumps, for the most part, are used for
outdoor sampling in low dust areas. The samplers
should be placed above ground level, about 4 to 5
feet high, away from obstructions that may influence
air flow. Table 7 summarizes outdoor sampling
locations and the rationales for their selection.
Outdoor sampling usually requires flow rates
between 10 to 15 L/min with a sample volume of
1000 to 5000 liters. Record wind speed, wind
direction, temperature, and pressure in a field
logbook. Wind direction is particularly important
when monitoring for asbestos downwind from a
fixed source.
It is recommended that a meteorological station be
established. If possible, sample after 2 to 3 days of
dry weather and when the wind conditions are at 10
mph or greater.
6.2.3 Indoor Sampling
EPA uses PCM analysis for indoor air samples.
When analysis shows total fiber count above the
EPA action level of 0.1 fibers/cm3 of air, then TEM
can be used to identify asbestos from nonasbestos
fibers.
Sampling pumps should be placed 4 to 5 feet above
ground level, and away from obstructions that may
influence air flow. The pump can be placed on a
table or counter. Table 8 summarizes indoor
sampling locations and the rationales for their
selection.
Indoor sampling generally utilizes high-flow rates
and increased sample volumes in order to obtain
lower detection limits, i.e., 0.01 fibers/cm3 of air or
less (with PCM) and 0.005 structures/cm3 or less
(with TEM).
6.2.4 Aggressive Sampling
Sampling equipment at fixed locations may fail to
detect the presence of asbestos fiber. Due to
limited air movement, many fibers may settle out of
the air onto the floor and other surfaces and may
not be captured on the filter. In the past, an 8-hour
sampling period was recommended to cover various
air circulation conditions. A quicker and more
effective way to capture asbestos fibers is to
circulate the air artificially so that the fibers remain
airborne during sampling. The results from this
sampling option characterize the worst-case
condition. This is referred to as aggressive air
sampling for asbestos.
6.3 SAMPLE PRESERVATION,
CONTAINERS, HANDLING, AND
STORAGE
6.3.1 Filter Selection and Collection
Device
Which filter and collection device to use for sample
collection will depend upon which analytical
methodology is utilized.
28
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Table 7: Sampling Stations for Outdoor Sampling
Sampling Station Location
Upwind/Background
Downwind
Site Representative
and/or Worst Case
Procedure
Collect a minimum of 2 simultaneous
upwind/background samples 30° apart
from the prevailing windlines
Deploy a minimum of 3 sampling
stations in a 180° arc downwind from
the source
Obtain one representative sample
which shows average on-site
conditions or obtain worst-case
sample (optional)
Rationale
Establishes background fiber
levels
Indicates if asbestos is leaving
the site
Verify, continually confirm, and
document selection of proper
levels of worker protection
Note: More than one background station may be required if the asbestos originates from different sources.
Table 8: Sampling Stations for Indoor Sampling
Sampling Station Location
Procedure
Rationale
Indoor Sampling
• If a work site is a single room,
disperse five samplers throughout the
room
• If the work site contains up to five
rooms, place at least one sampler in
each room
• If the work site contains more than
five rooms, select a representative
sample of the rooms
Establishes representative
samples from a homogeneous
area
Upwind/Background
If outside sources are suspected,
deploy a minimum of two
simultaneous upwind/background
samples 30° apart from the prevailing
windlines
Establishes whether indoor
asbestos concentrations are
coming from an outside source
Worst Case
Obtain one worst-case sample by
aggressive sampling (optional)
Verify, continually confirm, and
document selection of proper
levels of worker protection
29
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• NIOSH Method 7400: Phase Contrast
Microscopy involves using a 0.8 to 1.2 fan
cellulose ester membrane, 25-mm diameter,
50-mm conductive cowl on cassette (figure
12, appendix A).
• U.S. EPA Transmission Electron
Microscopy involves using a 25-mm filter
cassette with either a polycarbonate filter
having a pore size <0.4 fan or mixed
cellulose ester filter (MCE) having a pore
size <0.4S (&n. This cassette includes an
extension cowl, a 5.0 jon MCE backup
filter to serve as a diffuser, and a support
pad (figure 13, appendix A).
6.3.2 Sample Handling Procedures
1. Place a sample label on the cassette with a
unique sampling number. Do not put sampling
cassettes in your shirt or coat pockets as the
filter can pick up fibers. ERT uses the original
cassette box to hold the samples.
2. Wrap the cassette individually hi a plastic
sample bag. Mark each bag to indicate sample
identification number, total volume, and date.
3. The wrapped sampling cassettes should be
placed upright in a rigid container so that the
cassette cap is on top and cassette base is at the
bottom. Use enough packing material to
prevent jostling or damage. If possible, hand
carry to laboratory.
4. Provide appropriate documentation with
samples (e.g., chain-of-custody form and
requested analytical methodology).
5. Follow all QA/QC requirements from the lab
as well as from the PCM/TEM analytical
methodology (e.g., field blank and lot blank
requirements).
6.4 INTERFERENCES AND
POTENTIAL PROBLEMS
Flow rates should not exceed 16 L/min due to the
possibility of asbestos fiber disintegration upon
contact with the filter.
6.4.1 NIOSH Method 7400, PCM
• PCM cannot always distinguish asbestos
from non-asbestos fibers. All particles
meeting the counting criteria are counted
as total asbestos fibers.
• Fibers less than 0.25 fan in length will not
be detected by this method.
• High levels of non-fibrous dust particles
may obscure fibers in the field of view and
increase the detection limit.
6.4.2 U.S. ERA'S TEM Method
• High concentrations of background dust
interfere with fiber identification.
6.5 EQUIPMENT/APPARATUS
6.5.1 Personal Sampling Pump
• personal sampling pump (e.g., Gilian
Personal Sampler)
• inert tubing with glass cyclone and hose
barb
sampling cassettes with conductive cowl.
appropriate membrane filters.
rotameters
whirlbags for cassettes
tools — small screw drivers
sample labels
air data sheets
container -- to keep samples upright
6.5.2 High-Flow Pump
high-flow pump (e.g., Gilian Aircon)
generator or electrical outlet
extension cords
rotameters
inert tubing - unless provided with pump
sampling cassettes with conductive cowl
appropriate membrane filters
whirlbags for cassettes
sample labels
air data sheets
container ~ to keep samples upright
30
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6.6 REAGENTS
This section is not applicable to this SOP.
6.7 PROCEDURES
6.7.1 Preparation
1. Determine the extent of the sampling effort, the
sampling methods to be employed, and what
supplies and equipment are needed.
2. Obtain necessary sampling and monitoring
equipment.
3. Decontaminate or preclean equipment, and
ensure that it is in working order.
4. Prepare schedules, and coordinate with staff,
client, and regulatory agency, as appropriate.
5. Perform a general site survey prior to entry in
accordance with the site-specific health and
safety plan.
6. Use stakes or flagging to identify and mark all
sampling locations.
6.7.2 Aggressive Sampling
1. Before starting the sampling pumps, direct
forced air (such as a 1-horsepower leaf blower
or large fan) against walls, ceilings, floors,
ledges, and other surfaces in the room to
initially dislodge fibers from surfaces. This
should last at least 5 minutes per 1000 square
feet of floor.
2. Place a 20-inch fan in the center of the room.
(Use one fan per 10,000 cubic feet of room
space.) Place the fan on slow speed and point
it toward the ceiling.
3. Start the sampling pumps and sample for the
required time.
4. Turn off the pump and then the fan(s) when
sampling is complete.
6.7.3 Personal Sampling Pump
1. Charge the unit for the maximum required time
as indicated hi the manufacturer's manual.
2. In the clean zone of the site, follow the
calibration procedures in section 6.9.1 to 6.9.3.
3. Mobilize to the sampling location.
4. To set up the sampling train, attach one end of
the polyvinyl chloride (PVC) tubing
(approximately 2 feet) to the cassette base;
attach the other end of the tubing to the inlet
plug on the pump (figure 14, appendix A). The
attachment between the cassette base and the
tubing can best be achieved by using a hose
barb with a cyclone clip.
5. Place the sampling pump 6 feet above ground
level (in the breathing zone) and in an area
that will not be affected by unusual air flow.
The sampling pump and cassette can be placed
on a sturdy structure, attached to a dowel rod
or hooked to an object.
6. Remove the cassette cap from the extension
cowl (open faced) and orient the cassette
perpendicular to the wind.
7. Adjust the time on the pump. If the pump is
programmable, turn past the zero mark before
setting the actual time.
8. Turn the pump on.
9. Record the following hi the site logbook: date,
time, location (area or room), sample
identification number, pump number, flow rate
and desired total sampling time.
10. Record weather data (e.g. ambient
temperature, wind direction, windspeed,
precipitation).
11. Check the pump at midpoint of the sampling
period if longer than 4 hours.
12. If a filter darkens in appearance or if loose
dust is seen in the filter, a second sample
should be started.
13. At the end of the sampling period, check the
fault button to obtain pump sampling tune.
(This indicates whether or not the pump ran
the full programmable timespan). Be sure to
orient the cassette in an upright position to
prevent fibers from falling from the filter when
the vacuum is released.
31
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14. Record the pump run time (finish time minus
start time).
15. Perform post-calibration procedures as shown
in section 6.9.
16. Record the post-flow rate in a field logbook.
17. Remove the PVC tubing from the sampling
cassette. While holding the cassette upright,
replace the inlet plug on the cassette cap.
18. Place the outlet plug on the cassette base.
19. Refer to section 6.3.2, steps 1-5 for sample
handling procedures.
6.7.4 High-Flow Pump
The following instructions are for a Gilian Aircon
520 Constant High-Flow Air Sampler and is used
for illustrative purposes; an equivalent high-flow
pump can be used instead.
1. Once on site, perform the calibration hi the
clean zone. The calibration procedures for
personal sampling pumps listed in section 6.9.1
are also applicable to high volume sampling
pumps.
2. After calibrating the high volume sampler,
mobilize to the sampling location.
3. To set up the sampling train, attach the air
intake hose to the cassette base. Remove the
cassette cap. The cassette should be positioned
perpendicular to the wind (figure 15, appendix
A).
4. Turn the generator on. The generator should
be placed 10 feet downwind from the sampling
pump.
5. Record the pump's cumulative time (if
applicable).
6. Record the following in a field logbook: date,
time, location, sample identification number,
pump number, flow rate, and cumulative time.
7. Record weather: wind speed, ambient
temperature, wind direction, and precipitation.
8. Turn the pump on.
9. Check the pump at sampling midpoint if longer
than 4 hours.
10. At the end of the sampling period, orient the
cassette up, and turn the pump off.
11. Record the cumulative time (if applicable).
12. Check the flow rate as shown in section 6.9.
The sampling cap is replaced before calibrating.
13. Record the post-flow rate.
14. Remove the tubing from the sampling cassette.
Still holding the cassette upright, replace the
inlet plug on the cassette cap and the outlet
plug on the cassette base.
15. Refer to section 6.3.2, steps 1 to 5, for sample
handling procedures.
6.7.5 Calibration
An electronic calibrator is used for calibrating
rotameters and pumps. Refer to section 6.9.1 to
6.9.3 for calibration procedures.
6.8 CALCULATIONS
The sampling volumes are determined on the basis
of how many fibers need to be collected for reliable
measurements. Therefore, one must estimate how
many airborne fibers may be in the sampling
location.
Since the concentration of airborne aerosol
contaminants will have some effect on the sample,
table 9 contains suggested criteria to assist in
selecting a flow rate based on real-time aerosol
monitor readings in mg/m3.
PCM utilizes flow rates between 0.5 L/min and 16
L/min. The sampling time is adjusted to obtain
optimum fiber loading on the filter. A sampling
rate of 1 to 4 L/min for 8 hours is appropriate hi
non-dusty atmospheres containing 0.1 fibers/cm3.
Dusty atmospheres (areas with high levels of
asbestos) require smaller sample volumes (<400 L)
to obtain countable samples. In such cases, take
short, consecutive samples and average the results
over the total collection time. For documenting
episodic exposures, use high-flow rates (7 to 17
L/min) over shorter sampling tunes. In relatively
32
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clean atmospheres where targeted fiber
concentrations are much less than 0.1 fibers/cm3,
use larger sample volumes (3,000 to 10,000 L) to
achieve quantifiable loadings. Take care, however,
not to overload the filter with background dust. If
more than 50% of the filter surface is covered with
particles, the filter may be too overloaded to count
and will bias the measured fiber concentration. Do
not exceed 0.5 mg total dust loading on the filter.
U.S. EPA's TEM method requires a minimum
volume of 560 L and a maximum volume of 3,800 L
in order to obtain an analytical sensitivity of 0.005
structures/cm3. The optimal volume for TEM is
1200 L to 1800 L. These volumes are determined
using a 200 mesh EM grid opening with a 25-mm
filter cassette. Changes in volume would be
necessary if a 37-mm filter cassette is used since the
effective area of a 25-mm (385 mm2) and a 37-mm
(855 mm2) filter differ.
6.9 QUALITY ASSURANCE/
QUALITY CONTROL
Follow all QA/QC requirements listed in the
analytical method.
Generally field blanks are required for each set of
samples or 10% of the total samples, whichever is
greater.
The laboratory analyzing the samples should
determine the lot blank requirements. There should
be no less than one lot blank per cassette lot. It is
preferable to have the lot blank analyzed prior to
sampling.
6.9.1 Electronic Calibration -
Personal Sampling Pump
1. See the manufacturer's manual for operational
instructions.
2. Set up the calibration train (as shown in figure
16, appendix A) using a sampling pump,
electronic calibrator, and a representative filter
cassette. The same lot sampling cassette used
for sampling should also be used for
calibrating.
3. To set up the calibration train, attach one end
of the PVC tubing (approximately 60 cm or 2
feet) to the cassette base; attach the other end
of the tubing to the inlet plug on the pump.
Another piece of tubing is attached from the
cassette cap to the electronic calibrator.
4. Turn the electronic calibrator and sampling
pump on. Create a bubble at the bottom of
the flow chamber by pressing the bubble
initiate button. The bubble should rise to the
top of the flow chamber. After the bubble runs
its course, the flow rate is shown on the LED
display.
5. Turn the flow adjust screw or knob on the
pump until the desired flow rate is attained.
6. Perform the calibration three times until the
desired flow rate of ±5% is attained.
6.9.2 Electronic Calibration -
Rotameter
1. See the manufacturer's manual for operational
instructions.
Table 9: Asbestos Sampling Flow Rates
Low real-time monitor readings
Medium real-time monitor readings
High real-time monitor readings
Concentration
< 6.0 mg/m3
> 6.0 mg/m3
> 10.0 mg/m3
Flow Rate
11 - 15 L/min
7.5 L/min
2.5 L/min
33
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2. Set up the calibration train (as shown in figure
17, appendix A) using a sampling pump,
rotameter, and electronic calibrator.
3. Assemble the base of the flow meter with the
screw provided and tighten in place. The flow
meter should be mounted within 6° of the
vertical position.
4. Turn the electronic calibrator and sampling
pump on.
5. Create a bubble at the bottom of the flow
chamber by pressing the bubble initiate button.
The bubble should rise to the top of the flow
chamber. After the bubble runs its course, the
flow rate is shown on the LED display.
6. Turn the flow adjust screw or knob on the
pump until the desired flow rate is attained.
7. Record the electronic calibrator flow rate
reading and the corresponding rotameter
reading. Indicate these values on the rotameter
(sticker). The rotameter should be able to
work within the desired flow range.
8. Perform the calibration three times until the
desired flow rate of ±5% is attained.
Once on site, a secondary calibrator, such as a
rotameter, may be used to calibrate sampling
pumps.
6.9.3 Sampling Pump Calibration ~
Rotameter
1. See the manufacturer's manual for Rotameter's
Operational Instructions.
2. Set up the calibration train as shown in (figure
18, appendix A) using a rotameter, sampling
pump, and a representative sampling cassette.
3. To set up the calibration train, attach one end
of the PVC tubing (approximately 60 cm or 2
feet) to the cassette base; attach the other end
of the tubing to the inlet plug on the pump.
Another piece of tubing is attached from the
cassette cap to the rotameter.
4. Assemble the base of the flow meter with the
screw provided and tighten in place. The flow
meter should be mounted within 6° of the
vertical position.
5. Turn the sampling pump on.
6.
Turn the flow adjust screw (or knob) on the
personal sampling pump until the float ball on
the rotameter is lined up with the precalibrated
flow rate value. A sticker on the rotameter
should indicate this value.
7.
A verification
performed on
of calibration
site in the
is generally
clean zone
immediately prior to the sampling.
6.10 DATA VALIDATION
PCM analysis does not distinguish between asbestos
and non-asbestos fibers; all fibers meeting the
criteria are counted. TEM analysis can distinguish
asbestos from non-asbestos fibers. This method of
analysis should be used when the total fiber count
is above the action level (or level of concern) so as
to determine whether the airborne fiber is of
asbestos origin.
Note: The flow rate and time should be adjusted to
obtain optimum fiber loading on the filter.
6.11 HEALTH AND SAFETY
When working with potentially hazardous materials,
follow U.S. EPA, OSHA, and site-specific health
and safety procedures. More specifically, when
entering an unknown situation involving asbestos, a
powered air purifying respirator (PAPR) (full face-
piece) is necessary in conjunction with HEPA filter
cartridges. See applicable regulations for action
level, PEL, TLV, etc. If previous sampling indicates
asbestos concentrations are below personal health
and safety levels, then Level D personal protection
is adequate.
34
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7.0 TEDLAR BAG SAMPLING: SOP #2050
7.1 SCOPE AND APPLICATION
The purpose of this Standard Operating Procedure
(SOP) is to define the use of Tedlar bags in
collecting gaseous samples. Tedlar bags are used to
collect both volatile and semi-volatile organic
compounds, including halogenated and non-
halogenated species. The sensitivity of the method
is primarily instrument dependent.
7.2 METHOD SUMMARY
When collecting gaseous samples for analysis, it is
often necessary to obtain a representative grab
sample of the medium in question. The Tedlar bag
collection system (see figure 19 in appendix A)
allows for this and consists of the following items.
• Tedlar bag complete with necessary fittings
• desiccator in which the vacuum is created
• sampling pump to create the necessary
vacuum
• appropriate Teflon and Tygon tubing
The Tedlar bag is placed into the desiccator and the
fitting is inserted into Teflon tubing. The Teflon
tubing is the path through which the gaseous
medium will travel. The pump is attached to the
Tygon tubing, which is part of the vacuum fitting on
the desiccator. The pump evacuates the air in the
desiccator, creating a pressure differential causing
the sample to be drawn into the bag. The sample
introduced into the Tedlar bag never passes through
the pump. The flow rate for the pump must be
defined prior to sampling (usually 3 L/min for bag
sampling).
7.3 SAMPLE PRESERVATION,
CONTAINERS, HANDLING, AND
STORAGE
The Tedlar bags most commonly used for sampling
have a 1-liter volume, and are held in boxes of ten.
When the sampling procedure is concluded, the
Tedlar bags are stored in either a clean cooler or a
trash bag to prevent photodegradation. It is
essential that samples be analyzed within 48 hours,
as after that tune compounds may escape or
become altered.
7.4 INTERFERENCES AND
POTENTIAL PROBLEMS
Contamination is a major concern since many of the
compounds in question will be present in the parts
per billion range. The following practices will
minimize the risk of cross-contamination.
• During transportation and storage, the
further away from the source(s) of
potential contamination the bags are, the
less likely are the chances for external
contamination.
• Bags must be attached only to clean Teflon
tubing.
• Once the sample has been collected, affix
the sample label to the edge of the bag to
prevent adhesives on the label from
permeating the body of the bag. Fill out
labels with a ballpoint pen or a pencil,
since permanent markers contain volatile
compounds that may contaminate the
sample.
• The chemical structure of Tedlar will cause
highly polar compounds to adhere to the
inner surface of the bag. Also, low
molecular weight compounds may
permeate the bag. Use real-tune monitors
such as the OVA, HNU, and CGI as a
screening device prior to sampling. Write
this information on the sample label to
inform the individuals performing the
sample analysis.
The Tedlar bag sampling system is straightforward
and easy to use. However, be aware of the
following when sampling.
• Ensure that the seal between the top half
and the bottom half of the desiccator is air
tight in order for the system to work.
• Check the O-ring gasket to see if it is hi
35
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place with the proper fit. O-rings that have
been stretched out will not remain in place,
requiring constant realignment.
• Check that all the fittings associated with
the vacuum joints are securely in place.
The fittings can be pushed loose when
inserting the valve stem into the Teflon
tubing.
• Check to ensure that a corner of the
Tedlar bag is not jutting out between the
two halves of the desiccator, thus impairing
the seal.
• Be sure not to overinflate the bags.
Overinflation will cause the bags to burst.
7.5 EQUIPMENT/APPARATUS
• Pelican cases, or desiccators ~ cleaned,
with Teflon tubing replaced, and equipped
with extra O-rings.
• pump(s) - charged, in good working order,
and set with the appropriate flow rate of 3-
L per minute.
• Tedlar bags -- free of visible contamination
and preferably new.
7.6 REAGENTS
This section is not applicable to this SOP.
7.7 PROCEDURES
7.7.1 Preparation
1. Determine the extent of the sampling effort, the
sampling methods to be employed, and which
equipment and supplies are needed.
2. Obtain necessary sampling and monitoring
equipment.
3. Decontaminate or preclean equipment, and
ensure that it is in working order.
4. Prepare a schedule. Coordinate with staff,
clients, and regulatory agency, if appropriate.
5. Perform a general site survey prior to site entry
in accordance with the site-specific health and
safety plan.
6. Use stakes, flagging, or buoys to identify and
mark all sampling locations. If required, the
proposed locations may be adjusted based on
site access, property boundaries, and surface
obstructions.
7.7.2 Field Operation
Tedlar bags are stored in boxes of 10. The valve is
in the open position when stored. Occasionally, a
piece of debris will clog the valve, necessitating the
closing of the valve stem for it to clear. The valve
stem is dosed by pulling the stem out. If the valve
stem is difficult to pull, it helps to twist the valve
stem simultaneously.
1. Remove the Tedlar bag from the carton.
2. Insert the valve stem into the Teflon tube
which runs through the desiccator.
3. Seal the desiccator by applying pressure to the
top and bottom (ensure that the "O" ring is in
place and unobstructed).
4. Connect the sampling pump to the evacuation
tube.
5. Connect the intake tube to the desired source
by placing the intake tube into the medium of
concern.
6. Turn on the sampling pump.
7. Allow the bag to fill (indicated by the look of
the bag as well as by the sound of the laboring
pump).
8. Turn off the sampling pump and remove the
evacuation tube from the pump.
9. Remove bag and pull the valve stem out.
10. Lock the valve stem.
11. Label the bag using either a tag or a sticker.
Do not write on the bag itself.
12. Place Tedlar bag in a clean cooler or opaque
trash bag to prevent photodegradation.
36
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7.7.3 Post Operation
1. Once the samples are collected, transfer bags to
the laboratory for analysis.
2. When transferring the Tedlar bags, a chain-of-
custody form must accompany the samples.
Personnel should be aware that some of the
compounds of concern will degrade within a
few hours of sampling.
3. Samples shipped must be in a clean cooler with
a trip blank (a Tedlar bag filled with zero air)
and a copy of the chain-of-custody form.
7.8 CALCULATIONS
This section is not applicable to this SOP.
consisting of upgradient/downgradient samples, or
beginning/end of day samples, or a combination of
the two. It may also be desirable to change sample
train tubing between sample locations. Tedlar bag
standards must be filled on site to identify the
contaminants' degradation from the time the sample
is collected until analysis. Tedlar bags filled with
zero air must also accompany the sample bags to
identify possible contamination during shipment and
handling.
7.10 DATA VALIDATION
Results of the quality control samples (field and lot
blanks) will be evaluated for contamination. This
information will be utilized to qualify the
environmental sample results according to the
projects' data quality objectives.
7.9 QUALITY ASSURANCE/
QUALITY CONTROL
Depending upon the Quality Assurance Work Plan
(QAWP) requirements, collect background samples
7.11 HEALTH AND SAFETY
When working with potentially hazardous materials
follow U.S. EPA, OSHA, and site-specific health
and safety procedures.
37
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8.0 CHARCOAL TUBE SAMPLING: SOP #2051
8.1 SCOPE AND APPLICATION
Charcoal tube sampling is utilized to identify
specific contaminants in ambient air. The greatest
selectivity of charcoal (activated carbon) is towards
non-polar, organic, solvent vapors, (e.g., carbon
tetrachloride, chlorobenzene and toluene). Organic
compounds that are gaseous at room temperature,
reactive, polar, or oxygenated (aldehyde alcohols
and some ketones) are either not adsorbed
(relatively early breakthrough), or inefficiently
desorbed.
8.2 METHOD SUMMARY
Charcoal tube sampling is performed by drawing a
known volume of air through a charcoal adsorption
tube. As air is drawn through the tube, gases and
vapors adsorb onto the surface of the charcoal.
After sampling, the tubes are delivered to the
laboratory for analysis.
8.3 SAMPLE PRESERVATION,
CONTAINERS, HANDLING, AND
STORAGE
Charcoal used for sampling is housed in a glass tube
that has been flame sealed. Charcoal tubes most
often used contain either 150 mg or 600 mg of
charcoal. The smaller 150-mg tube is 7-cm long
with a 6-mm ID and a 4-mm OD containing two
sections of 20/40 mesh activated carbon separated
by urethane foam. The adsorbing section contains
100 mg of charcoal, the backup section SO mg of
charcoal. The larger 600-mg tube is 11-cm long
with a 8-mm ID and a 6-mm OD containing two
sections of 20/40 mesh activated carbon separated
by urethane foam. The adsorbing section contains
400 mg of charcoal, the backup section contains 200
mg of charcoal. The larger tube can provide
greater sensitivity by using a greater volume of air.
To preserve and store samples:
1. Place plastic caps on the charcoal tube ends.
2. Place the sample in a whirl bag. If duplicate
samples have been collected, place both tubes
in one whirl bag.
3. Indicate all applicable information on the
chain-of-custody form, (e.g., sample volume,
ID#, location, date, and weather parameters).
4. If the sample tube must be stored for more
than a week, refrigeration is recommended.
Maximum recommended holding time is two
weeks.
5. Provide the name(s) of the analytical
methodology(ies) being requested with the
sample to the lab.
8.4 INTERFERENCES AND
POTENTIAL PROBLEMS
High temperature and humidity, and high sampling
flow rates may cause a decrease in the adsorption
capacity of activated carbon. Contaminants from
the front portion of the tube may migrate to the
back portion of the tube. Refrigeration may
minimize this migration.
8.5 EQUIPMENT/APPARATUS
8.5.1 Equipment List
personal sampling pump
dowel rods
single or dual rotameter with stand and
desired precalibrated flow rate
charcoal tubes (600 mg or 150 mg)
flexible PVC tubing (for attaching the tube
holder system to the suction side of the
pump)
universal tube holder system
sleeves (or support tubes to hold tubes in
place)
single or dual manifold flow controller
tube holder end (tube holder ends support
and seal the sampling tube within the
plastic housing)
glass cracker
Ziploc bag
39
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• whirl bags
• plastic caps
8.5.2 Equipment Source
While there may be other sources, tubes are readily
available from SKC, Inc., and from Mine Safety
Appliance Co., both of Pittsburgh, PA.
SKC: 1-800-752-8472
Mine Safety Appliance Co.: 1-800-MSA-2222
8.6 REAGENTS
This procedure utilizes totally dedicated equipment
and does not require reagents.
8.7 PROCEDURES
8.7.1 Calibration
To save time in the field, sampling pumps can be
precalibrated in the office prior to arriving at the
site. The calibration must be checked in the field
before and after sampling.
Assemble the calibration train as shown in figure 20
(appendix A), using a rotameter, sampling pump,
manifold (low flow only) and representative
charcoal tube. Use the same lot number of
charcoal tubes for both sampling and calibrating.
1. Depending on the flow rate, adjust the sampling
pump to the low- or high-flow mode (high flow
> 750 cm3/min).
2. For low flow calibration, turn the flow adjust
screw on the manifold until the float ball on the
rotameter is aligned with the precalibrated flow
rate value. A sticker on the rotameter should
indicate this value.
3. Affix a sticker to the manifold and pump
indicating flow rate and media.
4. Remove the representative charcoal tube from
the sleeve. The pump and manifold are
calibrated as a unit and should not be separated
until the samples have been collected. If the
charcoal tube is run straight without a manifold,
the calibration is performed by adjusting the
flow directly on the pump.
8.7.2 Field Operation
1. Mobilize to the clean zone and calibrate the
pumps.
2. Mobilize to the sampling location.
3. Crack the charcoal tube ends using a glass
cracker.
4. Insert the charcoal tube hi the sleeve with
arrow pointing in the direction of air flow. (The
smaller section is used for a backup and is
positioned nearest the sampling pump.)
5. Screw the tip onto the sleeve so the charcoal
tube is held in place.
6. Attach the sleeve(s) to a single or double
manifold. At higher flow rates (>750
cm3/min), charcoal tubes can run without a
manifold. See figure 21.
7. To set up the sampling train, attach one end of
the Tygon tubing (approximately 2 feet) to the
tip of the sleeve or manifold. Attach the other
end of the tubing to the inlet plug on the
pump, figure 23 (appendix A).
8. Adjust time on the pump by adjusting past the
zero mark several times to erase the pre-
programmed time.
9. Place the charcoal tube in a vertical position on
a dowel rod.
10. Record weather data (e.g., ambient
temperature, barometric pressure, relative
humidity, and wind direction).
11. Turn the pump on.
12. After the pump has run the full tune, check the
fault button to obtain the sample time. (This
will indicate whether the pump ran for the
scheduled time.)
13. Verify calibration.
8.7.3 Post Operation
1. Record the sampling time.
2. Remove the charcoal tube from the sleeve.
40
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3. Immediately cap charcoal tubes with plastic
caps. Never use rubber caps.
4. Place a sample ID# label on the tube.
5. Place the sample in a whirl bag labeled with the
sample ID#, total volume, and required
analysis. If duplicate samples have been
collected, place both tubes in one whirl bag.
6. Indicate all applicable information on the chain-
of-custody form (e.g., sample volume, ID#,
location, date, and weather parameters).
7. If the sample tube must be stored for more
than a week, refrigeration is recommended.
8. Provide the name(s) of the analytical
methodology(ies) being requested to the lab
with the samples.
To analyze the charcoal tubes, NIOSH Methods
1501, Aromatic Hydrocarbons; 1500, Hydrocarbons
BP 36'-126'C; and 1003, Halogenated
Hydrocarbons may be used. Other analytical
parameters may be required. Determine the
appropriate analytical methodology prior to field
activities.
8.8 CALCULATIONS
The total volume of a sample is calculated by
multiplying the total sample time by the flow rate.
The total volume for each sample should be
indicated on the chain-of-custody form.
8.9 QUALITY ASSURANCE/
QUALITY CONTROL
• Provide one field blank per sampling
period or two field blanks for every 10
samples, whichever is greater. The tube
should be handled in the same manner as
the sampling tube (break, seal, and
transport) except that no air is sampled
through this tube.
• Provide a minimum of one appropriately
labeled lot blank tube per sampling
episode. The lab analyzing the samples can
better determine the number of lot blank
tubes required. These tubes are taken
directly from the charcoal tube box. Do
not break the ends.
• Provide one duplicate sample per 10
samples.
8.10 DATA VALIDATION
Results of the quality control samples will be
evaluated. Utilize this information to qualify the
environmental sample results in accordance with
data quality objectives.
8.11 HEALTH AND SAFETY
Prior to initiating survey activities, a risk analysis is
required to determine the hazards posed to
sampling personnel. This will estimate any potential
exposures to personnel, and define the extent of
safety planning needed to complete the task.
Depending upon the hazards identified, a safety
plan may be required prior to performing any site
entry. In addition, real time monitoring may be
necessary in order to verify ambient conditions and
to determine adequate respiratory protection.
Specific hazards unique to charcoal tube sampling
include:
• Sharp edges of the cracked tubes.
• Slip, trip and fall hazards at sampling
locations.
41
-------
9.0 TENAX TUBE SAMPLING: SOP #2052
9.1 SCOPE AND APPLICATION 9.3
Tenax/carbonized molecular sieve (CMS) tube
sampling is utilized to identify specific contaminants
in air. Compounds that can be determined by
Tenax (U.S. EPA Method TO-1) are non-polar
organks having boiling points in the range of
approximately 80°C to 100°C. Compounds which
can be determined by CMS are non-polar, non-
reactive organics having boiling points in the range
15°C to 120°C. However, not all compounds falling
into these category can be determined. Listed in
table 10 below are many of the compounds which
can be detected using Tenax/CMS. Analysis is
performed by thermal desorption into a gas
chromatograph/mass spectrometer/data system
(GC/MS/DS).
SAMPLE PRESERVATION,
CONTAINERS, HANDLING, AND
STORAGE
9.2 METHOD SUMMARY
2.
Tenax/CMS tube sampling is performed by drawing
a known volume of air through a Tenax absorbent
followed by a carbonized molecular sieve (CMS)
adsorbent. Volatile organic compounds are 3.
captured on the adsorbent while major inorganic
atmospheric constituents pass through or are only
partially retained. After sampling, the tube is 4.
returned to the laboratory for analysis (U.S. EPA
Method TO-1 and TO-2).
Tenax/CMS tubes contain a granular inert chemical
compound with adsorbent properties. A
flame-sealed outer glass tube protects the
Tenax/CMS tube from contamination. This outer
glass tube must be broken prior to sampling. The
Tenax/CMS air tube is 6-mm OD and 4-mm ID
containing one section of 150 mg Tenax, 35/60
mesh and one section of 150 mg CMS 60/80 mesh.
Prior to site work, the culture tubes should be
cleaned and prepared using the following procedure:
1. Place a plug of precleaned, silanized glass wool
(methanol rinsed, baked in an oven at 120°C)
in the bottom of each tube.
2. Place the culture tubes in an oven for at least
2 hours at 120°C. Do not bake the Teflon-
lined caps.
Remove the culture tubes from the oven and
allow them to cool.
Place the culture tubes in a Ziploc bag or whirl
pack.
Table 10: Compounds Detected by Tenax/CMS
• benzene
• bromochloromethane(1)
• bromodichloromethane
• p-bromofluorobenzene
• carbon tetrachloride
• chloroethane
• chloromethane
• dibromomethane
• 1,1-dichloroethane
• 1,2-dichloroethane
• 1,1-dichloroethene
• trans-l,2-dichloroethene
• ethylbenzene
• m-ethyltoluene
• methylene chloride
• styrene
• 1,1,2,2,-tetrachloroethane
• tetrachloroethylene
• toluene
• 1,1,1-trichloroethane
• 1,1,2-trichloroethane
• trichloroethylene
• trichlorofluoromethane
• trichloromethane
• vinyl chloride
• m-xylene
• o-xylene
(i)
Surrogate - Surrogates are injected into the Tenax tube to determine adsorption efficiencies.
43
-------
Refrigerate the samples and keep out of sunlight.
Storage for more than 4 weeks is not recommended.
which holds the Tenax samples. Cleaning is
performed prior to site work.
9.4 INTERFERENCES AND
POTENTIAL PROBLEMS
Contamination of the Tenax/CMS air tubes with
the compound(s) of interest is a common problem.
To minimize this problem, be extremely careful in
preparing, storing, and handling the air tube
throughout the sampling and analysis process. To
avoid contamination from skin oils, use a lint-free
glove when handling Tenax air tubes.
9.5 EQUIPMENT/APPARATUS
9.5.1 Equipment List
calibrated personal sampling pump
dual rotameter with stand and
precalibrated flow rate
Tenax/CMS tube, preferably of the same
lot number
flexible Tygon tubing (for attaching the
tube holder system to the suction side of
the pump)
universal tube holder system
dual variable manifold flow
controller
tube holder end with rubber boot
adaptor
sleeves (clear plastic housings)
glass cracker
lint free cloth
glass wool
Teflon tape
culture tubes
9.5.2 Equipment Sources
While there may be other sources, Tenax can
readily be obtained from Supelco Inc., Bellefonte,
PA, at (800) 247-6628; Technical Service (814)
359-3441 and MSA, 1-800-MSA-2222.
9.6 REAGENTS
Methanol is used in the lab to clean the glass tubing
9.7 PROCEDURES
9.7.1 Calibration
1. Assemble the calibration train as shown in
figure 23 using a rotameter, sampling pump,
manifold, and representative Tenax tubes.
Tenax tubes from the same lot are used for
both sampling and calibration.
2. Adjust the sampling pump to the low-flow
mode.
3. Remove the cap ends on the flow controller
manifold. To adjust the flow, turn the needle
valve with a small screwdriver
(counter-clockwise to increase, clockwise to
decrease).
4. Turn the flow-adjust screw on each manifold
until the float ball on the rotameter is lined up
with the precalibrated flow rate value. A
sticker on the rotameter should indicate this
value (see figure 24).
5. Affix a sticker to the manifold and pump
indicating the calibrated flow rate and media.
6. Remove the representative Tenax tubes from
the sleeves.
The pump and manifold (including boots) are
calibrated as a unit and should not be separated
until the samples have been collected.
The pump and manifold are calibrated on-site in the
clean zone immediately prior to sample collection.
See table 11 for flow rate ranges and volumes.
Table 11:
Recommended Flow Rates
and Sample Volumes
Maximum
Optimum
Minimum
Flow Rate
50 cm3/min
30-40 cm3/min
10 cm3/min
Volume
5 liters
2 liters
0.5 liter
44
-------
9.7.2 Field Operation
1. Calibrate pumps with manifolds as shown in
section 9.7.1.
2. Crack the outer glass tube using a glass cracker.
3. Use a clean, lint-free cloth or gloves to remove
the Tenax tube from the outer glass housing.
4. Insert the Tenax tube into a boot, with the
carbonized molecular sieve section closest to
the manifold.
5. Attach a protective sleeve over the tube. Do
not enclose the Tenax tube end.
6. Set up the sampling train, by attaching one end
of the Tygon tubing (approximately 60 cm or 2
feet) to the manifold; and the other end to the
inlet plug on the pump (figure 25).
7. Place the sampling tube in the breathing zone.
The pump and tube can be placed on a drum
or hooked to a fence. A wooden dowel rod can
also be used.
8. Position the tube either vertically or
horizontally.
9. Adjust the pump time.
10. Turn the pump on.
11. Record weather data (e.g., ambient
temperature, barometric pressure, relative
humidity and wind direction).
12. Check the pump at the midpoint of the
sampling period if longer than 4 hours.
9.7.3 Post Operation
1. At the end of the sampling period, check the
fault button to obtain the run time. Record the
run time. (This indicates whether or not the
pump ran the full scheduled tune.)
2. Check the flow rate and record the values in a
field logbook.
3. Remove the Tenax tubes from sleeves using a
lint-free cloth.
4.
5.
Place the Tenax tube in a culture tube. Tenax
tubes from the same manifold and identical
flow rates can be placed in the same culture
tube.
Place a sample sticker indicating sample ID#
on the culture tube. Do not put a sample
sticker on the Tenax tube itself as this will
contaminate the tube.
6.
7.
8.
9.
Attach the culture tube lid and wrap
lid/tube interface with Teflon tape.
the
Place the culture tubes into a Ziploc bag or a
whirl pack.
Keep the samples refrigerated and out of
sunlight. Storage for more than 4 weeks is not
recommended.
Indicate all applicable information on the
chain-of-custody form (e.g., sample volume,
sample ID#).
10. Provide a copy of the air data sheets and the
name of the preferred analytical methodology
with the samples to the lab.
9.8 CALCULATIONS
The volume for each sample should be indicated on
the chain-of-custody form.
Use the formula below to obtain the total volume:
Total Volume = Flow Rate x Time (minutes)
9.9 QUALITY ASSURANCE/
QUALITY CONTROL
Varying the sample volumes at the same location
provides field QA/QC.
• Provide one appropriately labeled field
blank per 10 samples. Handle this tube in
the same manner as the sampling tube
(break, seal, and transport), except that no
air is sampled through this tube.
• Provide a minimum of one appropriately
labeled lot blank tube per sampling
episode. These tubes are taken directly
45
-------
from the Tenax tube box. Do not break
the outer glass housing. Place in a Ziploc
bag and keep with other samples. Indicate
the lot blank number on the chain-of-
custody form.
All sample stations should have duplicate
sample tubes.
9.10 DATA VALIDATION
Results of the quality control samples (lot and trip
blanks) will be evaluated for contamination. This
information will be utilized to qualify the
environmental sample results according to data
quality objectives.
Data will be qualified according to acceptable
variation on the prescribed flow rates (see table 11).
9.11 HEALTH AND SAFETY
Prior to initiating survey activities, an analysis of
risk is required to determine the hazards posed to
sampling personnel. This will estimate any potential
exposures to personnel, and define the extent of
safety planning needed to complete the task.
Depending upon the hazards identified, a safety
plan may be required prior to performing any site
entry. In addition, real time monitoring may be
necessary in order to verify ambient conditions and
to determine adequate respiratory protection.
Specific hazards associated with Tenax tube
sampling include:
• Small pieces of glass flying during
"cracking" of the tube.
• Slip, trip and fall hazards at sampling
locations.
46
-------
10.0 POLYURETHANE FOAM SAMPLING: SOP #2069
10.1
SCOPE AND APPLICATION
The purpose of this Standard Operating Procedure
(SOP) is to outline the protocol for collection of
polyurethane foam (PUF) samples. The PUF
sampler is a complete air sampling system designed
to simultaneously collect suspended airborne
particulates and to trap airborne pesticide vapors.
This system can efficiently collect a number of
organochlorine and organophosphate compounds
(e.g., dioxins, and polychlorinated biphenyls).
10.2 METHOD SUMMARY
Ambient air is drawn into a covered housing, then
through a filter and foam plug by a high-flow-rate
pump operating at a level of approximately 250
L/min (approximately 9 tf/min). This allows a
sample of total suspended particulates (TSP) to
collect on the filter surface. The foam plug allows
collection of vapor which might be stripped from
the particulates on the filter.
10.3 SAMPLE PRESERVATION,
CONTAINERS, HANDLING,
AND STORAGE
Prior to sampling, ask the laboratory whether pre-
and post-sampling filter weighing is appropriate.
After sampling, the foam plug and filter should be
stored in an 8-oz. glass jar. The foam plug should
occupy the bottom portion of the jar and the filter
should be folded into quarters and placed on top of
the plug. The jar is then wrapped with aluminum
foil (shiny side out).
10.4 INTERFERENCES AND
POTENTIAL PROBLEMS
Humidity can pose a problem; although glass fiber
filters are comparatively insensitive to changes in
relative humidity, collected particulate matter can be
hygroscopic.
10.5 EQUIPMENT/APPARATUS
Specifications for equipment and supplies for
monitoring ambient air for total suspended
particulates (TSP) are provided in U.S. EPA's
Reference Method: Determination of Suspended
Particulates in the Atmosphere (High Volume
Method) EPA/600/4-77/027a.
10.5.1 Sampling Media
(Sorbents)
• polyurethane foam (PUF). Use polyether-
type polyurethane foam (density No. 3014,
0.0225 grams/cm3, or equivalent). This
foam is the type generally used for
furniture upholstery, pillows, and
mattresses (General Metals Work's part
number PSI-16 3-inch PUF plug is
recommended, although 1- and 2-inch
pieces are also available). This type of
foam is white, and yellows on exposure to
light. It should therefore be stored in a
dark place (e.g., black trash bags or a
cooler).
• 102-mm diameter glass fiber filter.
10.5.2 Sampling Equipment
PSI PUF sampler or equivalent
calibrated scale (if weighing is required)
Teflon-coated tweezers
aluminum foil
hexane
powder-free surgical gloves
Solvex gloves
sampling module holder
plastic bag
source of electricity (AC/DC): an electrical
source of 100 volts, 15 amps is required
10.6
REAGENTS
Reagents are not used for preservation of PUF
samples. Hexane is required for decontaminating
PUF glassware. No other decontamination
solutions are required.
47
-------
10.7 PROCEDURES
10.7.1 Calibration of Timer, Meters
and Standards
Elapsed-Time Meter
Every 6 months, the elapsed-time meter should be
checked against a timepiece of known accuracy,
either on site or in the laboratory. A gain or loss of
more than 2 minutes per 24 hours warrants
adjustment or replacement of the indicator. Record
the results of these checks in the calibration
logbook.
Flow Rate Transfer Standard
Calibration of the high-volume sampler's flow
indicating device or the control device is necessary
to establish traceability of the field measurement to
a primary standard via a flow-rate transfer standard.
The calibration procedures for orifice type flow
transfer standards are listed in EPA's Test Method,
600/4-77/027a.
Upon receipt and at 1-year intervals, the calibration
of the transfer standard orifices should be certified
with a positive displacement standard volume meter
(such as a Rootsmeter) traceable to the National
Bureau of Standards (NBS). Calibration orifice
units should be visually inspected for signs of
damage before each use, and they should be
recalibrated if the inspection reveals any nicks or
dents in the orifice.
10.7.2 Field Calibration of High
Volume Sampler
Calibration of the PUF sampler is performed
without a foam plug and without filter paper in the
sampling module. However, the empty glass
cartridge must remain in the module to ensure a
good seal through the module.
1. Connect the transfer standard orifice to the
sample module. Ensure that no leaks exist
between the orifice unit and the sampler.
2. Connect the orifice manometer to the orifice
pressure tap.
3. Verify that the flow indicator is properly
connected to the pressure tap on the lower side
of the motor housing on the high volume
sampler.
4. Set the manometer to "zero" as shown in figure
25 (appendix A).
5. Fully open the ball valve.
6. Fully open the voltage control screw. (Turn the
screw next to the magnahelix gauge clockwise.)
7. Operate the sampler for at least IS minutes to
establish thermal equilibrium prior to
calibration.
8. Adjust the voltage control screw to obtain the
desired reading (perhaps 70) inches on the dial
gauge (Magnahelix Gauge). A five-point
calibration should be conducted in the range of
the desired flow rate.
9. Record the dial gauge number 70 as your first
calibration point, then read and record the
pressure drop across the transfer standard
orifice (H). Figure 25 (appendix A)
demonstrates how to read the change in
pressure drop.
10. Let the sampler run for at least 2 minutes to
re-establish the run temperature conditions.
11. Adjust the voltage by moving the ball valve (red
valve) to adjust the dial gauge down to 60
(arbitrary) inches. (Repeat steps 9-10.)
12. Using the above procedure (steps 9-11), adjust
the ball valve for readings at 50, 40, and 30
inches.
13. Fully open the ball valve.
14. Turn the voltage-control screw clockwise as far
as possible.
15. Measure and record the barometric pressure
and ambient temperature on a field data sheet.
10.7.3 Sample Module
Preparation
1. Put on powder-free surgical gloves.
2. Place the lower canister (figure 26, appendix A)
sampling module in the module holder. All
48
-------
sampling equipment should be precleaned with
hexane prior to use.
3. Check to ensure that the upper and lower
orange silicone gaskets are in place (figure 26,
appendix A).
4. Load the glass cartridge with a dean foam plug
(with tweezers), making sure the foam is evenly
distributed throughout the cartridge, and install
in the module tube. (PUF plug should have
been pre-cleaned with hexane by the laboratory
that will be analyzing the samples.)
5. Install the filter holder assembly.
6. If filter weighing is required, weigh the 102-mm
diameter glass fiber filter and record the weight
in an analytical balance logbook. Calibrate an
electronic balance; weighing paper filter is
required.
7. Install lower Teflon gasket in the filter holder.
8. Handle the filter paper with Teflon-coated
tweezers.
9. Place glass fiber filter (rough side up) into the
filter holder.
10. Install the upper Teflon gasket.
11. Replace the 4-inch hold down ring and tighten
the swing bolts.
12. Ensure that all fittings are snug, yet not
overtight. (Overtightening will distort the
gaskets.)
13. Cover the sample module with a clean plastic
bag and place in a cooler.
14. Assemble a field blank and store in the same
cooler.
It is recommended to have two sampling modules
for each sampling system so that the filter and foam
exchange can take place in the laboratory. The
second set of modules is used for the subsequent
sampling round.
10.7.4 Unit Operation
1. Transport the PUF sampler (figure 27,
appendix A) to the desired location. The PUF
sampler may be operated at ground level or
elevated on scaffolding. The sampler should be
located in an unobstructed area, at least two
meters from any obstacle to air flow. In urban
or congested areas, it is recommended that the
sampler be placed on the roof of a single story
building.
2. Calibrate the PUF sampler as indicated in
section 10.7.2.
3. Adjust the exhaust hose downwind of the
sampler.
4. Put on dean powder-free surgical gloves.
5. Place the loaded sampling module into the
quick release fitting and engage by locking the
two levers down securely.
6. Remove the plastic bag.
7. A field logbook or field data sheets should be
used to record information (e.g., location,
elapsed time meter, and time of day).
8. Turn the unit on.
9. Depending upon the desired flow rate, adjust
the magnahelix gauge by turning the voltage
control screw clockwise to increase, and
counterclockwise to decrease the reading.
10. Wait approximately 2 minutes for the
magnahelix gauge reading to stabilize, and then
record it. The magnahelix dial gauge readings
should be taken at the beginning and end of
each sampling period. Differences between the
two dial gauge numbers should be averaged.
11. Collect and average weather condition data
during the sampling period, (e.g., wind
direction, temperature, barometric pressure,
and wind speed).
49
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10.7.5 Unit Shutdown and Sample
Collection
1. Using powder-free surgical gloves, open the
shelter housing and record the magnahelix
gauge reading.
2. Turn the sampler off and record the elapsed
time meter. Also, record the time of day.
3. Remove the sample module.
4. Cover the sample module with a polyethylene
(plastic) bag. Keep the sample module in a
vertical position at all times.
5. Place the sample module in a cooler. The field
blank should also be stored in the same cooler.
6. Wearing Solvex gloves, wipe down the interior
of the sampler with hexane and chem wipes.
7. If additional sampling is scheduled, install a
new sampling module. The unit must be
decontaminated with hexane and chem wipes
prior to initiating another sampling round. If
no additional sampling is scheduled, secure the
unit.
8. Weigh the sample filter in a field laboratory, if
required.
10.8 CALCULATIONS
Calculations are provided in U.S. EPA's Reference
Method for Determination of Suspended
Particulates in the Atmosphere (High-Volume
Method), EPA/600/4-77/027a.
10.9 QUALITY ASSURANCE/
QUALITY CONTROL
Provide one field blank per sampling period or two
field blanks for every 10 samples, whichever is
greater.
10.10 DATA VALIDATION
Results of the quality control samples (field blanks)
will be evaluated for contamination. This
information will be utilized to qualify the
environmental sample results in accordance with
the data quality objectives.
10.11 HEALTH AND SAFETY
When working with potentially hazardous materials
follow U.S. EPA, OSHA, and site-specific health
and safety practices.
50
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APPENDIX A
Figures
51
-------
Figure 1: SUMMA Canister Cleaning System
SOP #1703
\—7 ZERO
V, SHUT OFF
A~>-VALVE - E
u HUMIDITY
INJECTOR PORT
ZERO
SHUT OFF
VALVE - D
PRESSURE
REGULATOR
FLOW
CONTROL
VALVE - C
EXHAUST
VACUUM PUMP
SHUT OFF
VALVE - A
TRAP
ZERO
SHUT OFF
/ \ VALVE - B
PRESSURE
GAUGE
MANIFOLD
DEVAR
FLASK
CRYOGENIC
TRAP COOLER
(LIQUID NITROGEN)
53
-------
Figure 2: Pressurized and Subatmospheric Canister Sampling Systems
SOP #1704
SAMPLING
CANE
n
SAMPLING TEE
HIGH VOLUME
PUMP EXHAUST
SAMPLE
PUMP
SAMPLING
CANE
n
SS FILTER
LEGEND
MASS FLOW CONTROLLER OR
OTHER FLOW CONTROLLING DEVICE
ON-OFF VALVE
SUMMA
I CANISTER I
55
-------
Figure 3: Tekmar Model 5010
SOP #1705
Injection
Port
rin
Focus
Fused Silles
Transfer Line
To
Detector
GC Oven
Column
57
-------
Figure 4: GC/MS Printout
SOP #1705
Operator ID: Bob Quant Rev: 6
Output File: *83874::D4
Data File: >83874::D4
Name: DAILY STANDARD
Misc: + 10 mL Surrogates
ID File: ID SCT::D3
Quant Tme: 910416 14:30
Injected at: 910416 14:09
Dilution Factor: 1.00000
Title: GC/MS ANALYSIS OF TENAX/CMS CARTRIDGES (TO-1 & TO-2)
Last Calibration: 910411 14:17
#
1)
2)
3)
4)
5)
6)
7)
8)
9)
10)
11)
12)
13)
14)
15)
16)
17)
18)
19)
20)
21)
22)
23)
24)
25)
26)
Compound
#chloromethane
#vinyl chloride
#chloroethane
#trichlorofluoromethane
# 1,1-dichloroethene
#methylene chloride
#trans-l,2-dichloroethene
#l,l-dichloroethane
#bromochloromethane
#trichloromethane
#l,l,l-trichloroethane
#l,2-dichloroethane
carbon tetrachloride
#benzene
#trichloroethylene
#dibromomethane
#bromodichloromethane
#toluene
#l,l,2-trichloroethane
#tetrachloroethylene
#ethylbenzene
#meta-xylene
#styrene
#ortho-xylene
#l,l,2,2-tetrachloroethane
#p-bromofluorobenzene
27) #meta-ethyltoluene
# Compound uses FSTD
R.T.
1.16
1.25
1.55
1.85
2.27
2.56
3.15
3.50
4.49
4.55
5.24
5.39
5.67
5.67
6.77
6.79
6.98
8.63
8.80
9.76
11.14
11.34
11.88
11.93
12.41
12.69
13.61
Scan#
6
16
47
79
123
154
216
253
358
364
432
453
482
482
598
601
620
795
813
914
1060
1081
1138
1143
1194
1223
1320
Area
13555
13287
6583
30141
24379
21909
25986
29558
60788
35369
32525
28951
25779
38009
23850
29591
35690
52178
21806
34262
72692
59722
39679
64382
53557
37795
21354
Cone.
664.87
945.36
881.16
814.42
825.44
803.94
935.12
826.53
1767.00
880.60
887.10
914.97
881.95
775.10
873.51
923.39
928.61
888.48
892.69
861.90
925.43
939.36
1004.09
1008.13
795.33
1142.98
979.34
Units
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
PPR
q
74
88
93
95
88
93
88
95
99
92
90
99
94
93
94
65
89
87
89
95
82
92
89
79
92
98
93
59
-------
Figure 5: SUMMA Canister Sample Dilution Line
SOP #1705
o
LEGEND
REGULATOR
HIGH PRESSURE
PRECISION GUAGE
VACUUM/PRESSURE
GUAGE
VALVE
1/4" STAINLESS
STEEL TUBING
| STEEL TUBING
61
-------
Figure 6: SUMMA Canister Analysis Train (Tekmar 5010 GC)
SOP #1705
PERMA-PURE
DRYER , "
MASS FLOW '
CONTROLLER j
NEEDLE VALVE j
REGULATOR |
~_ VALVE |
SURROGATE
63
-------
Figure 7: Canister Sample Absorbed onto Tenax
SOP #1705
VKX
oo ID
CANISTER
SAMPLE
I O
06666
O [
1
MASS FLOW
CONTROLLER
r
TEMPERATURE
CONTROLLER
LEGEND I
SWITCH VALVE
NEEDLE VALVE
REGULATOR
VALVE
1/4." STAINLESS
STEEL TUBING
I ™- TEFLON TUBING i
THERMAL
DESOR8ER
OVEN
65
-------
Figure 8: Teflon "Tee" Setup
SOP #1706
1/4" TEFLON NUT
1/4" TEFLON "TEE'—
1/4" O.D. TEFLON
TUBING-
CONNECTOR
SUMMA
ON/OFF
VALVE
1/4" O.D. TEFLON
TUBING-FEED LINES
1/4" ON/OFF VALVE (S.S.)
SUMMA CANISTER
1/4" O.D. TEFLON
TUBING-
CONNECTOR
1/4" O.D. TEFLON
TUBING-VENT
LINE
67
-------
Figure 9: SUMMA Canister Charging System
SOP #1706
DUAL STAGE
REGULATOR
CERTIFIED GAS
STANDARD
TEFLON
"TEE"
SUMMA
ON/OFF
VALVE
1/4" 0.0. TEFLON TUBING
FEED LINES
1/4" (S.S.) ON/OFF VALVE
1/4" O.D. TEFLON TUBING
VENT LINES
SUMMA
CANISTER
69
-------
Figure 10: Septum "Tee" Setup
SOP #1706
1/4" TEFLON NUT
WITH SEPTUM
(SEE FIG. 4)
1/4" TEFLON "TEE"
1/4" ON/OFF VALVE (S.S.)
1/4" O.D. TEFLON
TUBING-
CONNECTOR
SUMMA
ON/OFF
VALVE
1/4" O.D. TEFLON
TUBING-
CONNECTOR
1/4" O.D. TEFLON
TUBING-VENT/TEDLAR
BAG LINE
SUMMA CANISTER
71
-------
Figure 11: Teflon Nut With Septum
SOP #1706
9mm SEPTA, TEFLON
SIDE DOWN
1/4" O.D. TEFLON
"TEE"
1/4" TEFLON NUT
1/4" TEFLON BACK FERRULE
(INVERTED)
73
-------
Figure 12: Phase Contrast Microscopy Filter Cassette
SOP #2015
INLET PLUG
CASSETTE CAP
EXTENSION COWL
0.8 - 1.2 urn PORE MCE FILTER
SUPPORT PAD
OUTLET PLUG
CASSETTE BASE
75
-------
Figure 13: Transmission Electron Microscopy Filter Cassette
SOP #2015
INLET PLUG
CASSETTE CAP
EXTENSION COWL
.45 urn PORE MCE FILTER
5 urn MCE DIFFUSER
SUPPORT PAD
OUTLET PLUG
CASSETTE BASE
77
-------
Figure 14: Persona! Sampling Train for Asbestos
SOP #2015
OUTLET PLUG
SAMPLING CASSETTE
REMOVE CASSETTE
CAP BEFORE PUMP
IS ACTIVATED
PERSONAL SAMPLING PUMP
79
-------
Figure 15: High Flow Sampling Train for Asbestos
SOP #2015
AC POWER CORD
REMOVE CASSETTE
CAP BEFORE PUMP
IS ACTIVATED
FLOW ADJUST VALVE
81
-------
Figure 16: Calibrating a Personal Sampling Pump with a Bubble Meter
SOP #2015
FILTER CASSETTE
r
9
G'
HI FLO
n
BAT
CK
.
OFF
V
Irfi
" 100 m> 10
ion
W SAMPl£R
C HH. MM
r TIME
^ OUT
PRESS nan
0 0
f
i j
k,
_
\
F
1
X
-
—
BUBBLE METER/ELECTRONIC
CALIBRATOR
PERSONAL SAMPLING PUMP
83
-------
Figure 17: Calibrating a Rotameter with a Bubble Meter
SOP #2015
BUBBLE METER/ELECTRONIC
CALIBRATOR
PERSONAL SAMPLING PUMP
85
-------
Figure 18: Calibrating a Personal Sampling Pump with a Rotameter
SOP #2015
FILTER CASSETTE
ROTAMETER
f
ON
as U
OFF
cr
H FLOW S
HZ
nT !
O L
CK k
31
OFF re
V
-ar
100 mt u
an
MIPUR
^P-
TIME
O O
OUT
JS FUW
O
5T ADJ.
[ )
- 4
- J
PERSONAL SAMPLING PUMP
87
-------
Figure 19: Tedlar Bag Sampling Apparatus
SOP #2050
To Sampling Port
BAT J TIME
O «OO
CK T OUT
1. TEDLAR BAG
2. DESICATOR
3. PERSONAL SAMPLING PUMP
89
-------
Figure 20: Calibrating a Double Manifold Charcoal Tube with a Rotameter
SOP #2051
BAT '
O ?OO
CK \ OUT
<
PRESS
o o
TOT >^
1. DOUBLE ROTAMETER
2. CHARCOAL TUBE WITH DOUBLE MANIFOLD
3. PERSONAL SAMPLING PUMP
91
-------
Figure 21: Charcoal Sampling, Straight
SOP #2051
f
ON
jar •
OFF
G'
HI FLOW
TM
BAT
/••>
8
si
OFT n
V
^
an
UMPlfR
f TIME
Sn o
o\J \~>
, our
3S "jaw
3 0
1ST >oa-
J
f=
V ->
_— .
k
•2
.
\
/
_J
1. PERSONAL SAMPLING PUMP
2. CHARCOAL TUBE - STRAIGHT
93
-------
Figure 22: Carbon Sampling, Single Manifold
SOP #2051
Gi ion
H FLOW SAMPLER
BAT r TUg.
o «
CK *
OUT
PRESS fU»
o o
TOT A
-------
Figure 23: Tenax Calibration with a Secondary Calibrator
SOP #2052
M
— 9»
— *
— *
— Ji
— •
— »
— w
— »
— »
— J4
— a
— I!
— n
Gilian
M nxm SAMPLER
czn
BAT ' ™E
o so o
CK * «ff
ON
PROS FUW
?-i rnca
y o
OFF TBSr
-•3
III
1. PERSONAL SAMPLING PUMP
2. TENAX/CMS TUBE WITH DOUBLE MANIFOLD
3. DOUBLE ROTAMETER
97
-------
Figure 24: Tenax/CMS Sampling Train
SOP #2052
Gi ian
W flDW SAMPLER
8*T I^1^
O ?OO
CK V
-------
Figure 25: Manometer
SOP #2069
Pt = 3.0 in.
Water
Manometer
Zeroed
Water
Manometer
Reading
r = 3.0 in.
101
-------
Figure 26: Canister Sampling Module
SOP #2069
LOWER CANISTER
RETAINING SCREEN
FILTER HOLDER SUPPORT
GLASS CARTRIDGE
AND PDF PLUG
FILTER HOLDER
WITH SUPPORT
SCREEN
4" DIAMETER
FILTER RETAINING RING
SIUCONE RUBBER
GASKETS
SAMPLE HEAD
Af
A CONNECTS TO A'
SIUCONE
RUBBER
GASKET
103
-------
Figure 27: High Volume PUF Sampler
SOP #2069
Pipe Fitting (1/2 in.)
Bipass
Blower
Motor
Magnehelic
Gauge
0-100 in.
Exhaust
Duct
(6 in, x 10 ft.)
Voltage
Variator
Ft
.. ••
^^.^-^^ Motor
^^^ Support
]
F
1
\\N
3ase
Hate
O — < t
•
7-
Ti
Do
ne
Elapsed Tine
Meter
105
-------
APPENDIX B
Canister Sampling Field Data Sheet
107
-------
Canister Sampling Field Data Sheet
SOP #1704
A. GENERAL INFORMATION
SITE ID:
SHIPPING DATE:
SITE ADDRESS:
CANISTER SERIAL NO.:
SAMPLER ID:
OPERATOR:
SAMPLING DATE:
CANISTER LEAK CHECK DATE:
B. SAMPLING INFORMATION
PARAMETER
START
STOP
MAXIMUM
MINIMUM
LOCAL TIME
NA
NA
ELAPSED TIME METER READING
NA
NA
INTERIOR TEMPERATURE
AMBIENT TEMPERATURE
CANISTER PRESSURE
MANIFOLD FLOW RATE
CANISTER FLOW RATE
FLOW CONTROLLER READOUT
NA
NA
SAMPLING SYSTEM CERTIFICATION DATE:
QUARTERLY RECERTIFICATION DATE:
C. LABORATORY INFORMATION
DATE RECEIVED:
INITIAL PRESSURE:
RECEIVED BY:
FINAL PRESSURE:
DILUTION FACTOR:
INSTRUMENT
ANALYSIS DATE
ANALYSIS RESULT
GC-FID-ECD
GC-MSD-SCAN
GC-MSD-SIM
ADDITIONAL RESULTS/COMMENTS:
SIGNATURE/TITLE:
109
-------
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Ill
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112
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