United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EPA-454/R-00-025C
May 2000
AiR
EPA
Final Report
Hot Mix Asphalt Plants
Truck Loading and Silo Filling
Manual Methods Testing
Asphalt Plant C
Los Angeles, California
Volume 3 of 8
Cleft®
-i_ i
v53rsiz
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FINAL REPORT
K HOT MIX ASPHALT PLANTS
> TRUCK LOADING AND SILO FILLING
-x MANUAL METHODS TESTING
Vft ASPHALT PLANT C, LOS ANGELES, CALIFORNIA
VOLUME 3 OF 8
APPENDICES C, D, E, AND F
EPA Contract No. 68-D-98-004
Work Assignment No. 3-02
Prepared for:
Mr. Michael L. Toney (MD-19)
Work Assignment Manager
SMTG, EMC, OAQPS
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
May 2000
Submitted by
PACIFIC ENVIRONMENTAL SERVICES, INC.
5001 S. Miami Blvd., Suite 300
Post Office Box 12077
Research Triangle Park, NC 27709-2077
(919) 941-0333
FAX (919) 941-0234
U.S. Environmental Protection Agency
Region 5, Library (PL-12J)
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DISCLAIMER
The information in this document has been funded wholly or in part by the Office of Air
Quality Planning and Standards, U.S. Environmental Protection Agency (EPA) under contract
to Pacific Environmental Services, Inc. (PES). PES performed the work presented in this
document under three EPA contracts and seven Work Assignments; EPA Contract No. 68-D-
98-004, Work Assignment Nos. 1-08,2-07, 3-02, and 3-05, EPA Contract No. 68-D-70002,
Work Assignment Nos. 0-05 and 1-07, and EPA Contract No. 68-D-70069, Work Assignment
No. 2-16. This document has been prepared by PES, reviewed following PES' internal
quality assurance procedures, and approved by PES for distribution. This document has been
subjected to the Agency's review, and has been approved by EPA for publication as an EPA
document. Mention of trade names does not constitute endorsement by the EPA or PES.
n
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TABLE OF CONTENTS
VOLUME 1 Page
1.0 INTRODUCTION 1-1
2.0 SUMMARY OF TEST RESULTS 2-1
2.1 OVERVIEW 2-1
2.2 TREATMENT OF NON-DETECTS AND ESTIMATES 2-2
2.3 TUNNEL EXHAUST DUCT 2-2
2.4 SILO EXHAUST DUCT RESULTS 2-12
2.5 PM AND MCEM DEPOSITION ESTIMATES 2-15
2.6 METEOROLOGICAL STATION RESULTS 2-15
3.0 PROCESS DESCRIPTION 3-1
3.1 COORDINATION BETWEEN TESTING AND PROCESS
OPERATIONS 3-3
3.2 PROCESS MONITORING DURING TESTING 3-3
3.3 PROCESS SAMPLES 3-4
3.4 VELOCITY OF AIR ACROSS TOP OF TRANSPORT TRUCKS
DURING LOAD-OUT 3-5
4.0 SAMPLING LOCATIONS 4-1
4.1 TUNNEL EXHAUST DUCT 4-1
4.2 SILO EXHAUST DUCT 4-1
5.0 SAMPLING AND ANALYTICAL PROCEDURES 5-1
5.1 LOCATION OF MEASUREMENT SITES AND
SAMPLE/VELOCITY TRAVERSE POINTS 5-1
5.2 DETERMINATION OF EXHAUST GAS VOLUMETRIC
FLOW RATE 5-1
5.3 DETERMINATION OF EXHAUST GAS DRY MOLECULAR
WEIGHT 5-3
5.4 DETERMINATION OF EXHAUST GAS MOISTURE CONTENT 5-3
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TABLE OF CONTENTS (CONTINUED)
VOLUME i ^CONTINUED;) page
5.5 DETERMINATION OF PM AND MCEM 5-3
5.6 DETERMINATION OF VOHAPs 5-3
5.7 DETERMINATION OF SVOHAPs 5-7
5.8 DETERMINATION OF WIND SPEED, WIND DIRECTION,
AMBIENT TEMPERATURE, AND AMBIENT HUMIDITY 5-7
5.9 ESTIMATE OF PM AND MCEM ON THE CEILING
OF THE LOAD-OUT TUNNEL DOWNSTREAM OF SILO NO. 5 5-7
5.10 ESTIMATE OF PM AND MCEM DEPOSITION ON THE INSIDE
WALLS OF THE SILO NO. 2 EXHAUST PLENUM 5-9
5.11 ESTIMATE OF PM AND MCEM DEPOSITION ON THE INSIDE
WALLS OF THE SILO EXHAUST DUCT 5-9
5.12 ESTIMATE OF PM AND MCEM DEPOSITION ON THE INSIDE
WALLS OF THE TUNNEL EXHAUST DUCT 5-10
6.0 QUALITY ASSURANCE/QUALITY CONTROL (QA/QC) PROCEDURES
AND RESULTS 6-1
6.1 CALIBRATION AND PREPARATION OF APPARATUS 6-1
6.2 REAGENTS AND GLASSWARE PREPARATION 6-2
6.3 ON-SITE SAMPLING 6-3
6.4 SAMPLE RECOVERY 6-4
6.5 LABORATORY ANALYTICAL QA/QC PROCEDURES 6-5
6.6 QA COORDINATOR FIELD AUDIT 6-7
APPENDIX A - TEST RESULTS AND CALCULATIONS 1
A.1 TED TEST RESULTS 3
A.2 SED TEST RESULTS 101
A.3 EXAMPLE CALCULATIONS 195
A.4 PARTICIPATE DEPOSITION DATA 204
A.5 CAPTURE EFFICIENCY CALCULATIONS 211
VOLUME 2
APPENDIX B - PROCESS DATA 1
B.I PRODUCTION RECORDS FOR 7/24/98 THROUGH 7/28/98 3
B.2 PRODUCT STORAGE RECORDS FOR 7/25/98 THROUGH 7/28/98 9
IV
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TABLE OF CONTENTS (CONTINUED)
VOLUME 2 (CONTINUED^
APPENDIX B - PROCESS DATA (CONTINUED)
B.3 LOAD-OUT RECORDS USED IN TED EMISSION CALCULATIONS . . 19
B.4 LOAD-OUT RECORDS FOR 6/18/98 THROUGH 7/26/98 33
B.5 LOAD-OUT RECORDS FOR 7/24/98 THROUGH 7/28/98 44
B.6 SILO NO. 2 LOAD-IN RECORDS USED IN SED EMISSION
CALCULATIONS 68
B.7 ASPHALT TEMPERATURES AT LOAD-OUT 90
B.8 MASS CHANGE RESULTS FROM ASTM TESTS PERFORMED ON
ASPHALT CEMENT SAMPLES 93
B.9 VELOCITY OF AIR ACROSS TOP OF TRANSPORT TRUCKS
DURING LOAD-OUT 100
B.10 METALS ANALYSIS OF PROCESS SAMPLES 104
VOLUME 3
APPENDIX C - FIELD DATA 1
C.I TED FIELD DATA 2
C.2 SED FIELD DATA 59
C.3 METEOROLOGICAL STATIONDATA 89
C.4 ON-SITE GC/MS REPORT AND DATA 118
APPENDIX D - QA/QC DATA 230
APPENDIX E - PROJECT PARTICIPANTS 280
APPENDIX F - TEST METHODS
F.I EPA METHOD 1
F.2 EPA METHOD 1A
F.3 EPA METHOD 2
F.4 EPA METHOD 4
F.5 EPA METHOD 18
F.6 EPA METHOD 315
F. 7 SW-846 METHOD 0010
F.8 SW-846 METHOD 0030
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TABLE OF CONTENTS (CONCLUDED)
VOLUME 4
APPENDIX G - ANALYTICAL DATA 1
G.I PM AND MCEM DATA la
G.2 PAH/SVOHAPS CASE NARRATIVE AND PAHDATA Ik
VOLUMES
APPENDIX G - ANALYTICAL DATA (CONTINUED) 659
G.3 SVOHAPS DATA 659
VOLUME 6
APPENDIX G - ANALYTICAL DATA (CONTINUED) 1248
G.3 SVOHAPS DATA (CONCLUDED) 1248
VOLUME?
APPENDIX G - ANALYTICAL DATA (CONTINUED) la
G.4 VOHAPS DATA Ic
VOLUMES
APPENDIX G - ANALYTICAL DATA (CONCLUDED) la
G.4 VOHAPS DATA (CONCLUDED) Ic
G.5 EPAMETHOD 18 REPORT AND DATA 260
VI
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LIST OF TABLES
Page
Table 1.1 Test Log Tunnel Exhaust Duct, Asphalt Plant C - California 1-4
Table 1.2 Test Log Silo Exhaust Duct, Asphalt Plant C - California 1-5
Table 2.1 Summary of Results, Production Emissions for PM, MCEM, PAH,
SVOHAP and VOHAP, Asphalt Plant C, California - July 1998 2-3
Table 2.2 Summary of Results, Average PM and MCEM Emissions,
Asphalt Plant C, California - July 1998 2-4
Table 2.3 Summary of Results, Average PAH and SVOHAP Emissions,
Asphalt Plant C, California - July 1998 2-5
Table 2.4 Summary of Results, Average VOHAP Emissions,
Asphalt Plant C, California - July 1998 2-6
Table 2.5 Summary of Results, PAHS, SVOHAPS, & VOHAPS Average
Emissions, Silo Exhaust Duct - Asphalt Plant C, California, July 1998 .... 2-7
Table 2.6 PM and MCEM Emissions Sampling and Exhaust Gas Parameters
Normal Operations, Tunnel Exhaust Duct, Asphalt Plant C - California . . 2-16
Table 2.7 PM and MCEM Exhaust Gas Concentrations and Emission Rates, Normal
Operations, Tunnel Exhaust Duct, Asphalt Plant C - California 2-17
Table 2.8 PAHs and Semi-Volatile Organics Emissions Sampling and
Exhaust Gas Parameters, Normal Operations, Tunnel Exhaust Duct,
Asphalt Plant C - California 2-18
Table 2.9 PAHs Exhaust Gas Concentrations and Emission Rates, Normal
Operations Tunnel Exhaust Duct, Asphalt Plant C - California 2-19
Table 2.10 Semi-Volatile Organics Exhaust Gas Concentrations and Emission Rates,
Normal Operations, Tunnel Exhaust Duct, Asphalt Plant C - California . . 2-21
Table 2.11 Volatile Organics - SW-846 Method 0030 Emissions Sampling and
Exhaust Gas Parameters, Normal Operations, Tunnel Exhaust Duct,
Asphalt Plant C - California 2-30
Table 2.12 Volatile Organics - SW-846 Method 0030 Exhaust Gas Concentrations
and Emission Rates, Normal Operation, Tunnel Exhaust Duct,
Asphalt Plant C - California 2-31
Table 2.13 Volatile Organics - EPA Method 18 Emissions Sampling and
Exhaust Gas Parameters, Normal Operations, Tunnel Exhaust Duct,
Asphalt Plant C - California 2-36
Table 2.14 Volatile Organics - EPA Method 18 Exhaust Gas Concentrations
and Emission Rates, Normal Operations, Tunnel Exhaust Duct,
Asphalt Plant C - California 2-37
Table 2.15 On-Site GC/MS Volatile Organics Exhaust Gas Concentrations and
Emission Rates with Vost (SW-846 Method 0030) and EPA Method 18
Comparison, Tunnel Exhaust Duct, Asphalt Plant C - California 7/24/98 . 2-38
Table 2.16 PM and MCEM Emissions Sampling and Exhaust Gas Parameters,
Background Condition, Tunnel Exhaust Duct, Asphalt Plant C - California 2-39
vn
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LIST OF TABLES (CONTINUED)
Page
Table 2.17 PM and MCEM Exhaust Gas Concentrations and Emission Rates,
Background Condition, Tunnel Exhaust Duct, Asphalt Plant C - California 2-40
Table 2.18 PAHs and Semi-Volatile Organics Emissions Sampling and Exhaust Gas
Parameters Background Condition, Tunnel Exhaust Duct,
Asphalt Plant C - California 2-41
Table 2.19 PAHs Exhaust Gas Concentrations and Emission Rates, Background
Condition, Tunnel Exhaust Duct, Asphalt Plant C - California 2-42
Table 2.20 Semi-Volatile Organics Exhaust Gas Concentrations and Emission Rates,
Background Condition, Tunnel Exhaust Duct, Asphalt
Plant C - California 2-44
Table 2.21 Volatile Organics - SW-846 Method 0030 Emissions Sampling and
Exhaust Gas Parameters, Background Condition, Tunnel Exhaust Duct,
Asphalt Plant C - California 2-53
Table 2.22 Volatile Organics - SW-846 Method 0030 Exhaust Gas Concentrations
and Emission Rates, Background Condition, Tunnel Exhaust Duct,
Asphalt Plant C - California 2-54
Table 2.23 Volatile Organics - EPA Method 18 Emissions Sampling and Exhaust Gas
Parameters, Background Condition, Tunnel Exhaust Duct, Asphalt
Plant C - California 2-59
Table 2.24 Volatile Organics - EPA Method 18 Exhaust Gas Concentrations and
Emission Rates, Background Condition, Tunnel Exhaust Duct,
Asphalt Plant C - California 2-60
Table 2.25 Sample Log Silo Exhaust Duct, Asphalt Plant C - California 2-61
Table 2.26 PM and MCEM Emissions Sampling and Exhaust Gas Parameters,
Silo Exhaust Duct, Asphalt Plant C - California 2-62
Table 2.27 PM and MCEM Exhaust Gas Concentrations and Emission Rates,
Silo Exhaust Duct, Asphalt Plant C - California 2-63
Table 2.28 PAHs and Semi-Volatile Organics Emissions Sampling and Exhaust Gas
Parameters, Silo Exhaust Duct, Asphalt Plant C - California 2-64
Table 2.29 PAHs Exhaust Gas Concentrations and Emission Rates, Silo Exhaust Duct,
Asphalt Plant C - California 2-65
Table 2.30 Semi-Volatile Organics Exhaust Gas Concentrations and Emission Rates,
Silo Exhaust Duct, Asphalt Plant C - California 2-67
Table 2.31 Volatile Organics - SW-846 Method 0030 Emissions Sampling and
Exhaust Gas Parameters, Silo Exhaust Duct, Asphalt Plant C - California . 2-76
Table 2.32 Volatile Organics - SW-846 Method 0030 Exhaust Gas Concentrations
and Emission Rates, Silo Exhaust Duct, Asphalt Plant C - California .... 2-77
Table 2.33 On-Site GC/MS Volatile Organics Exhaust Gas Concentrations and
Emission Rates with Vost (SW-846 Method 0030) Comparison,
Silo Exhaust Duct, Asphalt Plant C - California 7/25/98 2-82
Table 2.34 PM and MCEM Deposition Estimates, Asphalt Plant C - California 2-83
viii
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LIST OF TABLES (CONCLUDED)
Page
Table 2.35 Meteorological Data Summary, Asphalt Plant C - California 2-84
Table 3.1 Load-out Data Used in TED Emission Calculations 3-6
Table 3.2 Load-in Data for Silo No. 2 Used in SED Emission Calculations 3-7
Table 3.3 Asphalt Temperatures at Load-out, Asphalt Plant C, California 3-8
Table 3.4 Mass Change of Asphalt, Asphalt Plant C, California 3-9
Table 3.5 Results of Metals Analyses of Asphalt Samples, Asphalt Plant C,
California 3-10
Table 3.6 Air Velocity Over Transport Trucks During Load-out, Asphalt Plant C,
California 3-11
Table 5.1 Summary of Sampling and Analytical Methods, Asphalt Plant C,
California 5-2
Table 6.1 Summary of Temperature Sensor Calibration Data 6-8
Table 6.2 Summary of Pilot Tube Dimensional Data 6-9
Table 6.3 Summary of Dry Gas Meter and Orifice Calibration Data 6-10
Table 6.4 Summary of EPA Method 315 and SW-846 Method 0010
Field Sampling QA/QC Data 6-11
Table 6.5 Summary of EPA Method 315 Blank Sample Catches 6-12
Table 6.6 SW-846 Method 0010 PAHs Field and Laboratory Blanks Results,
Tunnel Exhaust Duct 6-13
Table 6.7 SW-846 Method 0010 PAHs Field and Laboratory Blanks Results,
Silo Exhaust Duct 6-14
Table 6.8 SW-846 Method 0010 PAHs Surrogate Recovery Results,
Tunnel Exhaust Duct 6-15
Table 6.9 SW-846 Method 0010 Semi-Volatile Surrogate Recovery Results
Tunnel Exhaust Duct 6-16
Table 6.10 SW-846 Method 0010 PAHs Surrogate Recovery Results,
Silo Exhaust Duct 6-17
Table 6.11 SW-846 Method 0010 Semi-Volatile Surrogate Recovery Results
Silo Exhaust Duct 6-18
Table 6.12 SW-846 Method 0030 Field and Laboratory Blanks Results
Tunnel Exhaust Duct 6-19
Table 6.13 SW-846 Method 0030 Laboratory Blank Results, Silo Exhaust Duct 6-20
Table 6.14 SW-846 Method 003 0 Surrogate Recovery Results
Tunnel Exhaust Duct 6-21
Table 6.15 SW-846 Method 003 0 Surrogate Recovery Results
Silo Exhaust Duct 6-22
IX
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LIST OF FIGURES
Page
Figure 1.1 Project Organization - US EPA Hot Mix Asphalt Load-out Operation,
Asphalt Plant C, California 1-6
Figure 2.1 Load-out Tunnel and MET Station Location and Average Wind Direction 2-85
Figure 3.1 Process Flow Schematic, Asphalt Plant C, California 3-2
Figure 3.2 Velocity Measurement Locations and Dimensions of Transport Trucks ... 3-12
Figure 4.1 Tunnel Exhaust Duct Sampling Locations, Asphalt Plant C, California .... 4-2
Figure 4.2 Tunnel Exhaust Duct Traverse Point Locations,
Asphalt Plant C, California 4-3
Figure 4.3 Silo Exhaust Duct Sampling Locations, Asphalt Plant C, California 4-4
Figure 4.4 Silo Exhaust Duct Traverse Point Locations, Asphalt Plant C, California . . 4-5
Figure 5.1 EPA Method 315 Sampling Train Schematic 5-4
Figure 5.2 SW-846 Method 0030 Sampling Train Schematic 5-6
Figure 5.3 SW-846 Method 0010 Sampling Train Schematic 5-8
Figure 5.4 Location of TED Deposition Test Plates Tj, T2, and T3 5-11
GLOSSARY OF TERMS
ASTM - American Society for Testing and Materials
CEMS - Continuous Emissions Monitoring System
CTS - Calibration Transfer Standard
EMC - Emissions Measurement Center
EMAD - Emission Monitoring and Analysis Division
ESP - Electrostatic Precipitator
FID - Flame lonization Detector
FTIR - Fourier Transform Infrared Spectroscopy
HAP - Hazardous Air Pollutant
MCEM - Methylene Chloride Extractable Matter
MRI - Midwest Research Institute
PES - Pacific Environmental Services
PM - Paniculate Matter
PTE - Permanent Total Enclosure
RAP - Recycled Asphalt
RTFOT - Rolling Thin Film Oven Test
SED - Silo Exhaust Duct
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GLOSSARY OF TERMS (CONTINUED)
SMTG - Source Measurement Technology Group
SVOHAP - Semi-Volatile Organic Hazardous Air Pollutant
TED - Tunnel Emissions Duct
TFOT - Thin Film Oven Test
THC - Total Hydrocarbons
VOHAP - Volatile Organic Hazardous Air Pollutant
VOST - Volatile Organic Sampling Train
XI
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VOLUME 3
APPENDIX C
FIELD DATA
C.I TED FIELD DATA
C.2 SED FIELD DATA
C.3 METEOROLOGICAL DATA
C.4 ON-SITE GC/MS REPORT AND DATA
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APPENDIX C.I
TED FIELD DATA
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PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
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Temperature j knpinger
°F I Temp.
Probe j fitter 1 °F
Dry Gas Meier Temp.
Inlet
fjmln0!1}
Outlet
(Tmoul°F)
Pump
Vacuum
(in.Hfl)
7/////y/////////////////////////////^^^
0
Lio_
66
75
(o
5"
O-TJ
l-
l-f
7*
JL
lo
. v
0-41
2.1
2-v
2°
5*4,
7
70
43^- 1
0-3o
I-SD
25
.LS.
zt
3*
7?
37
I4o
|.loO
1-9
0-3 *
li-
JJ
T?
60
a -3?
I./-.T
1-7
zn
0-33
frl
473-1
0-38
1.90
75-
0-3?
1-7
Sf
yt
5?
/o
043-
fo
67
7
0-3>
i
2L
l-T
iff
I
ll*
0*101
6-3?
t-10
5T
fi
55
7-
Ti-
Tm-
-------
FIELD DATA SHEET
Plant
Sampling Location
Run Number: "T-f+j/J-i, Dale: T-(ii
P^etesTLeakRate: o -01 elm @ 7.
Pretest Leak Check: Pilot: ^Orsat:
Sample Type:
Pbar:
Operator:
Ps:
O2:
in. Hg.
Probe Length/Type:
Stack Diameter: ?z
Pilot #:
As:
Nozzle ID: Q.iSJ
Assumed Bws: 3
Meter Box #: 6/4
Post-Test Leak Rate: o-oop cfm @_7_ in. Hg.
Post-Test Leak Check: Pilot: o Orsal:
Thermocouple
Filter #: O-
Y: / o -
TravwM
Numbw
San^Hnj
Tkn*
(min)
OockTima
(24-hour
dock)
Go* Meter
Reading
Velocity
H»ad
0-fo
-2-50
fo
/.SO
-05
/J-JT
0--U
I -IS
fo
f/
53?. t
I.1J
r
(0)7
i-t
7-U
0.3^
/do
031
-J5
St
/tr
103^
ffo
104
54
?t
/07,
IV
[01
10
no
1$
(09
2if
1-4
irf
ML
0.45
5J
5
It-
5}
5% 5
1-55
S«
AVm-
Ti-
TJS-
-------
PACIFIC ENVIRONMENTAL SERVICES, WC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant:
Sampling Location:,
Sample Recovery Person:
Sampling Method Type:
Run NumberT'l^S -;£
Job Number
Sample Train Recovery Data
Date:
/Pafreqc Field Team Leader.
3//~
Impinger Train ID:_
Comments:
Filter No.:
Filter Description: /?.
Filter No.: _ ..
Filter Description:.
Front Half Data
Filter Media Type:
. Filter Media Type:.
Back Half Data
Impinger Purge-
Start Time: Flow Rate:
Impinger 1
Contents: ft£ /%,&
Final Volume: (mL) r2 /£ [• I
Net Volume: (mL) lb-O
Impinger 4
Contents: ~flu& £*/
Final Volume: (mL) 7f^. /
Initial Volume: (mL) T^^/'
Net Volume: (mL) 3?. 7
Total Moisture Collected (mL): ^4-^
Description of I mpinqer catch :
Stop Time: Purae Gas:
Impinger 2 Impinger 3/
?jft f54f3
SrtZ.Z J'Z^I
St- ( 0
Impinger 5 Final Impinger
(a):
(a):
(a):
-------
FIELD DATA SHEET
Plant: 14«4 NtX.
Sampling Location
Run Number: Sf«nH
Sample Type:
Pbar: J1-P
Operator:
Nozzle ID: .
Ps: —
Thermocouple #:
Filter #:
Date: f »tj. V
ctm @ U' In. Hg.
C02: —
02: -
Pretest Leak Rate
Pretest Leak Check: Pltot: — Orsal: -
Probe LengtfVType: I*
PItol #:
Slack Diameter: -
As: --
Assumed Bws: _$
Meter Box *:t£M_ Y:
Post-Test Leak Rate: p.ol9 ctm @/f in. Hg.
Post-Test Leak Check: Pitol: - Orsat: —
iTBwrw
PoW
NumbM
to-
aan^nnB
Tbra
(win)
o
\jKKX imw
(244IOW
dock)
V&a*
\V>5^
«mm*iw
Reading
(Vm>n3
?l<,.frlV
8c?.«^
hiHZO
(AH) hi H2O
D«8ir*d
Actual
T»mp.
(Ts)
°F
Probe
Ftot
Tamp.
°F
Met
(Tmln0F)
OuUrt
(Tm out°F)
Vacuum
(in-Hg)
y//////////////////////////////////////////////////^^^
'
Tm-
-------
D PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Sample Train Recovery Data
Plant:
At
^
Date:
/&/>£/
Sampling Location:,
Sample Recovery Person:.
Sampling Method Type: df fX/"
Run Number V"T^ - TWne.
Job Number UO\t-QO>
Field Team Leader
//&/>//" /%>
. Impinger Train ID:_
Comments:
Filter No.:
Filter Description:
Filter No.:
Filter Description:.
i -
Front Half Data
. Filter Media Type:_
Filter Media Type:_
Impinger Purge-
Start Time:
Flow Rate:
Back Half Data
Stop Time:
Purge Gas:_
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):
Description of Impinger catch:_
Impinger 1
Impinger 4
Impinger 2
fi.H
Impinger 5
Impinger 3
o
Final Impinger
(9):.
(9):.
-------
FIELD DATA SHEET
Plant i4o\ WiX. Sample Type: //_>" Operator: /I/A/
Sampling Location ~TEO Pbar #7-3 < Ps: "f ?
Run Number:
T-PQ/S'l Date: T~iv
Time
(min)
-
O
SJ
C00
0^"
*v5
?5
S<>
O^
yC
ftf
/cu
/•/"
I lo
lu-
ll*
dock)
-
W/iO>
095T
£> ?j fc
O ^4/
D"?4t
Of5/
0 ? ^^
1*20 f
1 60 to
/dtl
lo(<-
(OU
/Ot<°
(0)1
IOJG,
IOHY
/o4fc
l$5l
/»r^
Ml
/(o<*
11"
III"
Id/
|lto
. Hg. Probe Lengln/Typ
/^ Slack Diameter:
v. 3' f/iif PtoAt-.tff
&' ' As: J?.^>"
Reading
—
s'fy.bA
^<} f
(oOL ^
. ^> c?jr.j
60J-*
6^,7
fr/f--?
6/7- <•
6^0-5"
6rZ>.7
^x??- <»
6?o^
(ojt?
(f J ff • f
i A*t fj
V 1 T • T
c«52 o
65^-;
G?(j/.f
U(,t.c
4?^
C17 ^
^J3.>
oh^
(i H ^(-
Velocity
He*d(Ap)
biHZO
Oriloe Pressure DMMenbel
(AhQinHZO
Desired
AckMl
Temp.
(Ts)
Nozzle ID: £> 2S^ Thermc
Assumed Bws: J[ Filler #
Meter Box #: M Y: A«/
Post-Test Leak Rate:
Post-Test Leak Check: Pilot:
Temperature
Probe
Filer
Temp.
°F
•couple if:
cfm@
/yj
in. Hg.
Orsat: x//4
Dry Gas Meier Temp.
Inlet
(Tmln0F)
Gullet
(Tm out°F)
Pump
Vacuum
f«.Hg)
Y////////////////M^^
0-11
0-11
0-2&
?*-
Q.ll
0-\(
0/19
0 j/
<5-?^
d'%,
0 >^
o-4^
0 4>
o1 55
0.1')-
o-?/
o.'7>
0.?i
O-^v
0-Srv
, Q-K
d-St,
^-—
I-67
0-^
0-9*-
/J6
l-(<»
I'O^
llf
/•f^
I-W
/. so
/ki-
ns
(•!*'
i>->
z »'
2. 6.T
(.->$
I-'IO
"S-tof
3.*/
4.lo
<{.\o
4-i»
4-'
s~
).o
0 9-
<0. 7-*-
/-*
/-t^
/'f
/•f
/o
l-
t-t
Z-71
2.^
? r
] }
>.7
<{l
4.(
1-1
4-'
/~
• 7
25b
!7 jjo
7
,><(^
2jr?
2-fr
If/
1J£>
f&
?3°
I?1
zrz.
253
in-
tyi
?5»
•^
^17
i$l
2$l
z.S"'-
2?
i? y "^
•^•T- &
C t>O
?rt
?JV
2 0^?"
^5D
?5<^
* Q. ?
ts?
150
T&'
~}%O
t&
75-0
^'tT1
/~
60
$(
^2-
S3
£~h
CeO
if'
*•
'}
/«/
^
2
C,
.pL
f
f
-------
FIELD DATA SHEET
Plant I-U
Sampling Location
Run Number:
* Date:
Sample Type:
Pbar 2?.3/
C02: •&
Operator: flj/J
.Ps:.
02:
Pretest Leak Rate:
-------
MOISTURE RECOVERY SHEET
PACIFIC ENVIRONMENTAL SERVICES, INC.
FACILITY:
SOURCE:
DATE:
RUN#:
METHOD #:
BOX#:
T-
-4
IMPINGER CONTENTS FINAL
INITIAL
TOTAL
GRAMS
D.I. WATER
D.I. WATER
EMPTY
SILICA GEL
$l J
TOTAL GRAMS COLLECTED
INITALS:
PACIFIC ENVIRONMENTAL SERVICES, INC. •
-------
FIELD DATA SHEET
Plant _____
Sampling Location
Run Number: f-J/J-J Date: 7/j?/r.s
Pretest Leak Rate: 0-00.7 elm @ ( r in. Hg.
Pretest Leak Check: Pilot: j^_ Great: /u/ff
Sample Type: 3/S
Pbar T-f-^? Pt:
C02: -0- O2:
Probe Length/Type: 5"'
Slack Diameter: .?;?*
Operator: ////
-f-.T
flt» Pilot #:
Nozzle ID:
Thermocouple
As:
Assumed Bws: _| _ Filler #:
Meter Box #: 64 Y: I'Cfif
Post-Test Leak Rale: _ elm @
Post-Test Leak Check: Pilot:
Tr«vww
Point
Numbe*
Somplna
Time
(mln)
(244iour
dock)
Guktetor
ftoacfina
(VrnJR8
V«loo«y
H«d(Ap|
inH2O
Grille* FVmcur* OidiranlUI
In H20
0«sir«d
I Actual
Stack
Temp.
(Ts|
Temperature
°F
Probe I Rttef
knpinger
Temp.
°F
Dry Gas Meier Temp.
Intel
(Tmln0F)
Gullet
(Tm out°F)
ftimp
Vacuum
fin.Hg)
Y///////////////^^^
7?
7?
to
.i
ft
f<0
1-1
0307
-¥<
40
^•vs
^7_
^
ff
l-s
sS
. "50
/.So
f.zr
1-1.
1M-
if 1
f(
±iL
I-5J
fats.
l.s-r
Jii.
<5-^^
Jfii
5>
fs
1-
7-
k
n
10
(tl.
if
8?
V.I 5
8f
V
U
[Of
16
.\o
|aO
\ol
V1
*/*•/?&
Tm-
-------
FIELD DATA SHEET
Plant AAc//
"o
Sampling Location
Run Number:
Date:
Sample Type: 3n
Pbar: 1MJ>
CO2: •&
Operator: AJO_
Pretest Leak Rate: & J elm @ in. Hg.
Pretest Leak Check: Pilot: Great:
73 Ps:_
^ O2:~
Probe Length/Type: J~'
Slack Diameter: ?*-"
As:
Nozzle ID: Q.V^ Thermocouple #:
Assumed Bws: _J Filter #:
Meter Box #: Oft Y: )--?cM &H@: >. f /
Post-Test Leak Rate: cfm @ in. Hg.
Post-Test Leak Check: Pilot: Orsat:
Point
Number
Sampln
Tlnw
Ooddlm
dock)
GM Meter
RMKfttfl
(Vmjn3
V.bcity
Hwd(Ap)
InHZO
Oriloa Rt«Mur« OHItranM
(AH) in H20
I
Actual
Stack
Ttmp.
Tamperalur*
Probe
bnpinger
Temp.
°F
Dry Gas Mater Temp.
Mel
(Tmln°F)
Outlet
(Tmout°F)
Pump
Vacuum
(in.Hfl)
Y///////////////////^^^
015 >
/•-I
ft
145
f/
US
/- 3
\.1S
fo
r/
ID/f
77
f-T
O.v,
26
1.00
If
I. to
5-5
/Of
r
; l/o
0-2.3
f(X
f 6-
o
/.o
l-tr
/.I.
/of
/A
?/
7?
fr
/or
tori
0-fo
/uo
fo/
(IIJ
/o?
04'
£4
2-7-
LOZ-
\\a
51
O-46
0-M
.1/3
[04-
IV
13°
t <>
nst
740
AVm-
AH-
T7S-
-------
PACIFIC ENVIRONMENTAL SERVICES, WC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Sample Train Recovery Data
Plant:
Date:
Sampling Location:.
Sample Recovery Person:
Sampling Method Type:_j
Run Number,
Job Number
Field Team Leader F- l~
. Impinger Train ID: 30
-DO/
Comments:
Filter No.:7=x^X/- ^ ~ S~
Filter Description: £)• ^T.3C
Filter No.:
Filter Descriotion:
Front Half Data
Filter Media Tvoe: /Z~^f/- /'^>r/~-
)
Filter Media Tvoe:
Back Half Data
Impinger Purge-
Start Time: Flow Rate: Stoo Time:
Impinger 1 Impinger 2
Contents: 0.1-. "D.J-
Final Volume: (mL) /7/-f ^-yJ.C/
Initial Volume: (mU 1-(j&-2 , <^?^j
Net Volume: (mL) ~\<&1 * 4^^ ;'
Impinger 4 Impinger 5
Contents: ^\\kc.
Final Volume: (mL} sflT. sf
Initial Volume: (mL^ ~~^J ^ 7
Net Volume: (mL) 1^
/
Total Moisture Collected (mL>: (&•*>*
Description of Impinqer catch: CAto"
Purae Gas:
Impinger 3
p\T
J'£e£/
£21 ~?
0-So '
Final Impinger
(a):
(a):
la):
-------
-------
-------
FIELD DATA SHEET
Plant
i
Sampling Location
Run Number: T-A>I>*S~< Date:
Pretest Leak Rate: -c-e><. elm @ >*> in. Hg.
Pretest Leak Check: P^tf »X Orsat: ^)A
Sample Type:
Pbar:
CO2:
Operator: frfry-y.
. p*: -?-7
O2:
Thermocouple #: Jc-
Probe LengbVType: S ' j 5 T^Pitot #: jR£_-
Stack Diameter: As: T *
Nozzle ID:A£
Assumed Bws: p? Filter #: ^ F
Meter Box *: AH@:
Post-Test Leak Rate: o^^actm
Post-Test Leak Check: Pilot:
in. Hg.
PoW
Numbw
Samplin
Tim
(min)
dock Time
(2+hour
dock)
GasMetw
Raading
(Vm)fts
Velocity
Head (Ap)
lnH20
Grille* Pressure Differential
(AH) in H20
Desired
Actual
Stack
Temp.
fTs)
Temperature
Probe
Filter
Impinger
Temp.
°F
Dry Gas Meter Temp.
Inlet
(Tmin°F)
Outlet
(Tm out°F)
Pump
Vacuum
On. Hg)
73
'**
Bo
CP Co
JO
0-7^0
5"
VO
1 .
30
I,L> \
JL
Q7S^
_k^i_
J2L
10
.5-7
-70
. 37
60
JZ4.
47
530- OSS
1-77
•7O
•fs
Si
0*4$
70
I -10
1 \
•70
P.eo
J±
"7*
S. 7 SO
"I
QSO
6,7
S3
ys-
73
%"=>
-5SO. 700
SO
/.J*
PC.O
-V6
557.
.3-7
JZJL
1 -(.7
50
JL^
7J
J7_.
/fp
sc
3D
so
•71
_7
7
3C.
/•V3
^L
^_S:
7(
^S^
53
13
1 10 fc
5(
73
xi.
Tm«
-------
Page
of
Plant Name:
Run Number:
I
Test Date:
Operator:
Traverse
Point
Number
Sampling /ClockTime
Time, / (24-hour
(min.) / clock)
Gas Meter
Reading
Velocity
leadtP.
in. IhO
Orifice Prcs. Differential
(All)llLlljO
Desired
Actual
Slack
Tcmp.«F
Probe
Temp./ Filter
Temp." F
Impinger
Temp.
•F
Dry Gas Meter Temp.
Inlel
Uullcl
Pump
Vacuum
In.ilg
/.ss
7V
JJJ2-
7
5?o.67o
-JLL
Ul
L*
JJ_
/.^7
5o
_^0
/.*/
J±
I.C.I
SO
,-ro
^o7.^Q
7
i.f-S
550
SO
•77
7
1.55
•7
Si
7
ZS£.
Sf
S> J
5/
a,
)3\Lt
.
8)
s- 1
Jos
.4-8
So
S 1
to
JlO
A, 57. 3 10
S.2.
37
i-fh
1. 7*1
5" 1
2 1
s
3.2.
Si
-------
PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Sample Train Recovery Data
Plant:
^UfWx(-r PU^V C
Date:
Sampling Location: 23
Sample Recovery Person:
Sampling Method Type:
Run Number 7~-
Job Number
V
Field Team Leader. fSfoK
Impinger Train ID:_
Comments:
Filter No.:
Filter Description:.
Filter No.:
Filter Description:.
Front Half Data
. Filter Media Type:_
. Filter Media Type:.
Back Half Data
Impinger Purge-
Start Time: Flow Rate:
Impinger 1
Contents: //(T
Final Volume: (mL) $" / 13, . *C
Initial Volume: (mL) */ ~7^> n
Net Volume: (mL) *\&-\ -
Impinger 4
Contents:
Final Volume: (mL) £> / 5" . *?
Initial Volume: (mL} t> }*/• 3>
Net Volume: (mL) 1 .fc, '
Total Moisture Collected fmL):
Description of Impinqer catch:
Stop Time: Purae Gas:
Impinger 2 Impinger 3
CM: b»l
S*C)S. "7 ~7~?£>-cir
->^-(^ •?-//• (^
-ii. } •-• -*.\.'*> s
Impinger 5 Final Impinger
TCT . & IQ). STT.^
7p -^ ;/ (a): ^R.O ^
-------
FIELD DATA SHEET
Sampling Location
Run Number: ~T-
\
Date:
Sample Type:
Pbar:
CO2:
Operator:
Pa:
O2:
Pretest Leak Rate: p.eo elm @ ,<$ In. Hg.
Pretest Leak Check: Pftot: *Xorsat:
Probe Length/Type:
Stack Diameter:
3 ' Pilot #:
As:
Nozzle ID:3Z.- . } S£ Thermocouple i
Assumed Bws: J Filter #: &F -
Meter Box #: Y: /. oocL\\@: /. .(£.(«?
l.f.tf
\ .
I-T7
).^^
JUL
•7*
•75
80
91
77
JZ2_
7?
«?«<=>
iSc?
P. 70
J50
^"=.0
111
-V7
66
•70
JZA.
75
71
74
-75
75
7-5
75
•7(0
7G-
7C.
77
_4^.
70
7 1
7 A
7 /
•71
72
79
75
75
si
T-.-
is-
G
-V?
-------
M
FIELD DATA SHEET
Plant
Sampling Location/Tltf
Run Number:
Pretest Leak Rate: O.QQ
Pretest Leak Check: Pilot:
Date:
cfrn
Sample Type: ^
Pbar: £?-J?
CO2: o.o
#$-
Ps:
02:
Operator: VV
-4*
eo
-------
PACIFIC ENVIRONMENTAL SERVICES. MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant:
Sampling Location: u.
Sample Recovery Person:_
Sampling Method Type:
Run Number ~FfZ. !*
Job Number.
Sample Train Recovery Data
.Date:
Field Team Leader.
fc
i -
Impinger Train ID:_
Comments:
Filter No.: Us* * u i«-N,U« rce)
Filter Descriotion:
Filter No.:
Filter Descriotion:
Front Half Data
Filter Media Tvoe: Vs) ^~ Ojr2»J
Filter Media Tvoe:
Impinger Purge-
Start Time:
Flow Rate:
Back Half Data
Stop Time:_
Purge Gas:.
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):.
Description of Impinger catch:_
Impinger 1
s
Impinger 4
.<
Impinger 2
-.S /
Impinger 5
"76,3.1
Impinger 3
Final Impinger
(9):_
4r-S.
-------
FIELD DATA SHEET
Plant
Sampling Location TFD
Run Number: Dfa»lf Date:
Pretest Leak Rate: 0-Offr cfm @ .[£ In. Hg.
Pretest Leak Check: Phot: — Orsat: --
Sample Type: /Hj* * Operator:
Nozzle ID: d. 2ft Thermocouple *:
Pbar
CO2:
Ps: ~
Probe Length/Type:
Slack Diameter:
O2: —
£'
Assumed Bws: ~
Meter Box
Filter #:
PHot *:
As:
/.goo AH@: /.fJ"
Post-Test Leak Rate: flo/^ cfm @/£ in. Hg.
Post-Test Leak Check: Pilot: — Orsat: -
IIBVWIH
PoM
NumbM
—
OHIflBiy
Ttow
(mln)
0
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D PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Sample Train Recovery Data
Plant:
Date:
Sampling Location: \
Sample Recovery Person:.
Sampling Method Type:
Run Number. T -
Job Number:
Field Team Leader
M.NV5
. Impinger Train ID:.
Comments:
Filter No.:
I
Filter Description:,
Filter No.:
Filter Description:,
Front Half Data
e3 Filter Media Type:_
Filter Media Type:_
Back Half Data
Impinger Purge-
Start Time:
Flow Rate:
Stop Time:_
Purge Gas:.
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):,
Description of Impinger catch:_
Impinger 1
Impinger 4
Impinger 2
Impinger 5
.0
70*9.0
- O -
Impinger 3
O
Final Impinger
(9)-..
(9):.
-------
Plant: /93pV4-V Pl^^V C
Sampling Location —,»«* t (L*
Run Number: T - t***.'s - v Date: •
Pretest Leak Rate: o.ooocftn @ )5 hi. Hg.
Pretest Leak Check: Ptot: t^Orsat: /Q/A
FIELD DATA SHEET
Sample Type: m/y\<, Operator:
Pbar: ^1. 3 \ Pt: ~S-'%
C02: __o__O2:.
Probe Length/Type: J
Stack Diameter: 30
Pilot #:
Nozzle ID: IT- .35 a Thermocouple
Assumed Bws: ^ Filter #:
Meter Box #: gft6-vsY: '.otfeAH®: )-
Post-Test Leak Rate: .ex=x=> cfm @j^'m. Hg.
'
Post-Test Leak Check: Pilot: ^t>rsat:
Traveree
PbW
Numbw
Swnplng
Tkrw
(ml")
OockTVm
|244iour
dock)
Vcbcify
Oilo* Ptatwra DWtoranlW
(AMI h H2O
Actual
Slack
Ttmp.
Temperature
°F
Probe I Filter
knpinger
Temp.
°F
Dry Gas Meier Temp.
Inlet
(Trnln0F)
Outlet
(Tmoul°F)
Pump
Vacuum
On- Hg)
9ZW/7/////////////////^^^
30
/o
• 3C
•7 -
3/
/. 9*7
IS*
7-5
6,
. 3 3
78
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77
4
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7
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/.-;*?
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32.
75
31
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s>
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so
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50
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it
fOo
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105
it in
3S&
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90/.5/0
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5-0
25
fc 1
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'TO
9/3.
'50
(=>
AVm-
C|tC?.
Tm««
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Plant
Sampling Location T^iw
FIELD DATA SHEET
Sample Type: AA.AJS. ^Operator:
Pbar ^9-"5l P»:
C02: £> O2:
Pretest Leak Rate
Run Number: T-M**s-4 Date: I-JK^^S . .._ _^ „ _ - t
<6 in. Hg. Probe LengbVType: -; - /^ TLgPitot »*: R.?-y°i Post-Test Leak Rate: c(m
<•]•• . • / f+ Cl«iJhL« B^t«BaHBahl^B« —S» *. '' A^> n^..*. T_._.•. I _._•- A^l ^_l
Pretest Leak Check: Pilot: >X Orsat: /oM Stock Diameter: .-5^ " As:
Nozzle ID: IT-.^SijiThermocouple *: Q3-k
Assumed Bws: ^L Filter #: j^ p
Meter Box #: Rf^^Y: j.ooAH®: j .*? o
_ in. Hg.
Post-Test Leak Check: Pilot: . ^ Orsat:
-------
PACIFIC ENVIRONMENTAL SERVICES. MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant:
l^fl~^VV
"
Sampling Location:,
Sample Recovery Person:_
Sampling Method Type:
Run Number 7~'—•
Job Number.
Sample Train Recovery Data
Date:
Field Team Leader. 3
. Impinger Train ID:_
Comments:
Filter No.:
Filter Description:
Filter No.:
Filter Description:
Front Half Data
Filter Media Type:
Filter Media Type:
Impinger Purge-
Start Time:
Flow Rate:
Back Half Data
Stop Time:_
Purge Gas:.
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):
Description of Impinger catch:_
Impinger 1
SO •?.(*, co
Impinger 4
fclC. .
4.-?
Impinger 2
fs-O
Impinger 5
Impinger 3
Final Impinger
(g):_
(9):.
(9):.
-------
1 /
vo
FIELD DATA SHEET
^ VV
Plant
Sampling Location 77
Run Number: T-MMS- 5 Date: 7-j?^ cftn @ ls" In. Hg.
Sample Type:
Pbar 3°(.^-
C02:
Operator:
02:
Nozzle ID: "3.-.
Assumed Bws:
Meter Box *
Thermocouple #:
Filter #:
Probe Length/Type: 3 '
i.ooQflH@;
Post-Test Leak Rate^'ff^clm @4£'in. Hg.
Pretest Leak Check: Ptot: txOrsat:
Slack Diameter:
Post-Test Leak Check: Pilot: yX" Orsal:
-------
Page
of
Plant Name:
Run Number:
Test Date: _.
Operator: _
Traverse
Point
Number
Sampling /dockTime
Time, / (24-hour
(min.) / clock)
Gas Meter
Reading
Velocity
HeadtP.)
in. IhO
Orifke Prcs. Differential
Desired
Actual
Stack
Temp. • F
Probe
Temp./ Filter
Temp.0 F
Impingcr
Temp.
•F
Dry Gas Meter Temp.
Inlet
Uutlcl
Pump
Vacuum
'Qt-S
1.31.
JJL
,3
t -
qo
i-?t
.-st
'o
Jo-
'*5d3 / ..
^LL
r .
j£.
^S
1 70 I ,
A
/ /.PSc?
(•0(o
tf
/ / OS'S
.30
o 55 ^356
91
G.
/ //oo
JL51
J^2_
JM.
0-S1
5° .
Lit.
o
li.
2$) 1 is*
ll
65
^£
11
«1
?
JLf
JS^I
-------
PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Sample Train Recovery Data
Plant:
V
Date:
Sampling Location:.
Sample Recovery Person:
Sampling Method Type:
Run Number ftf>
Job Number
Field Team Leader P" ~
. Impinger Train ID:.
- rWsn-S -
Comments:
Filter No.:
U
Filter Description:.
Filter No.:
Filter Description:,
Front Half Data
. Filter Media Type:_
. Filter Media Type:.
Back Half Data
Impinger Purge-
Start Time:
Flow Rate:
Stop Time:.
Purge Gas:_
Impinger 1
Impinger 2
Impinger 3
Contents: ^ATT OJ- "•*-
Final Volume: (mL) ^ 1 "7. Co
Initial Volume: (mL) ^ 7<^« C=>
Net Volume: (mL) 4y"0
Impinger 4
Contents: V^ \
Final Volume: (mL) (a \ 7- ^
Initial Volume: (mL) (o \ I . (/?
Net Volume: (mL) t- 3
Total Moisture Collected fmL): l^1'0 •"
Description of Impinger catch: C l«^
-7&>b. -H S/6.J?
-><*?. -S S'l^,^
0-9 P.D
Impinger 5 Final Impinger
7^5.9 taV. '$4
-------
-------
-------
at
£7 PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Customer
Facility:
Date:
Volatile Organic Sampling Train (VOST) Data Sheet
Project No.:_
Citv: LdS
Time:
Sampling Location:_
Run Number: A T'V* $- "
Meter Box No.:
Barometric Pressure, in. Hg:_
Ambient Temperature, °F: _
Meter Gamma (y) Pre:
Operator
Purge Time:
Post:
Leak Check Data
Pre-test:
Vacuum, inches Hg
Initial
tfe \Q.o
Final
18.0
Time, min
ur
Data
Sample
Time
(min)
O
7o
Clock
Time
(24-hr)
aGW
66M
0039
O#44-
064^
Meter
Volume,
liters (ft3)
Oo3?^1o
^.4^
41- r
4,^,0
^?.^74
Rotameter
Setting
-t5&-^
'??
/J3
/33
Dry Gas Meter
Temp. «£ (°F)
n\
•=»'
^"Z-
"^?
Vacuum
(in. Hg)
(l.o
II. °
(l.o
II. 0
Meter
Pressure
(in H20)
\*T-
!•?-
(.•2-
I.T-
-------
CZ71 /( 7
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Volatile Organic Sampling Train (VOST) Data Sheet
Customer
Facility: ItDr \A/W
Date:
Project No.:
Citv: Lo5
CtJ>
Time:
Sampling Location:
Run Number:
UNN«,
Meter Box No.:
'
Barometric Pressure, in. Hg:_
Ambient Temperature, °F:
Meter Gamma (y) Pre:
Post:
Purge Time:.
Leak Check Data
Pre-test:
roif
Vacuum, inches Hg
Initial
U.o
Final
vuo
Time, min
1.0
\(S-0 \(5.0 UO
Run Data
Sample
Time
(min)
6
S
(0
\£
76
•?
6^JtC
0^
t>^?<"
O^b
o^M-r
Meter
Volume,
liters (ft5) -
4Vttl
&<*
5T.33
5«-^
dn. 1
(o4. i
^a
^.64o
Rotameter
Setting
M
J^-^fi
10
Q(^
^(p
«(,
c\^
^
feN^ «^
Dry Gas Meter
Temp. SGTF)
16
7^
^T-
»
w
w
Bo
\&
Vacuum
(in. Hg)
M-C
Iv
(2-0
a^°
»7.0
M,r
d.r
Meter
Pressure
(in H20)
H
(-(
(. 1
«. (
I,/
I. \
i.(
-------
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Volatile Organic Sampling Train (VOST) Data Sheet
Customer d>
Facility: Hvr [#W
Date: ? /*4 /Tl
&*C
Project No.:_
City:_
c/l
Time:
Meter Box No.:
Barometric Pressure, in. Hg:
Ambient Temperature, °F:
ffi .
Sampling Location: MA
Run Number:
Meter Gamma (y) Pre:_
Operator.
Purge Time:
Post:
Leak Check Data
Pre-test:
Vacuum, inches Hg
Initial
U.o
Final
Ib-o
Time, min
<*3
v.*»X
Run Data
Sample
Time
(min)
0
^~-
3o
ty$
Clock
Time
(24-hr) *
(0&
rit>3 !
irt* i
\*&
\
Meter
Volume,
^tersTfty
^{*'^\
^
TTf.+ I
1K*&
, y
^0^- ^'^
«^>
yRolameter
' Setting
(0rl
M.6
I-
/-o
.
Dry Gas Meter
Temp. °J2-(°F)
^> ^^
^ T^
33 53
Vacuum
(in. Hg)
Q.-f
I/
It
Meter
Pressure
(in H20)
t.<*
1.*
i-f
-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Volatile Organic Sampling Train (VOST) Data Sheet
Customer /K £w &fa- ^ <-
Facilitv: H»r lA/ll* feftfiM" ^
Date: ^l^fctf -"W
Time: (Z0D
Meter Box No.: "Mo "L
Barometric Pressure, in. Ha: "2^-
Ambient Temperature. °F: ^ ^
Pre-test: 1
<&-«, i
-6 fl- Project No.: /?«2- - <=
^Mr He" Citv: 6c?5 Av>6tu*.
Samolinq Location: ^WA«
Run Number # T""
Meter Gamma (Y) Pre:
^^" Operator /Mv<^
6* Purge Time: Af/4-
Leak Check Data
Vacuum, inches Hg
Initial Final
s.c K.r
^o ^,«
t>l
frf
Aic*- c<«A^uSr /u1*"
\l-(-~$ il f/V\<
' Post:
Time, min
(.0
u
Run Data
Sample
Time
(min)
c/
0
r
(0
^
2o
v*r
30
Clock
Time
(24-hr)
-*M —
|2f?
/Tl^
cui
IZ34
/2-5Q
12^4-
I2^W
Meter
Volume,
liters (ft3)
•Wr?fcrn
r^
We. &^
^».oi4
^_^J
jAiv/C OxfllVW
Rotameter
Setting
o.^
6-8
2o
?o
7o
?0
?0
— *& — —
Meter
Pressure
(in H20)
U
u
t.c
l<6
16
M
i £.
-------
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Volatile Organic Sampling Train (VOST) Data Sheet
Customer: VO &W &*< <* ' 6/k
Facilitv: /-for nit*. ikftfotT \LAn
Date: >/2Sp0
Time: £>&*i
Meter Box No.: \|* 'J-
Barometric Pressure, in. Ha: 7^.3,}
Ambient Temperature, °F: ^ 'Tv
T C
Project No.:
City: _
oo i
Sampling Location:
Run Number: T
~ L
Meter Gamma (y) Pre:_
Operator:
Purge Time:
Post:
Mfr
Leak Check Data
Pre-test:
Post-test
Vacuum, inches Hg
Initial
1%.A
Wvt?
Final
jC-0
(^.*>
Time, min
I.6
L*
Run Data
Sample
Time
(min)
6
<
l^>
;<
76
?<,?
Clock
Time
(24-hr)
0#* _i
^l*- |
6^/> !
06^^ I
08«- i
\,
Meter
Volume,
Wj2^
^)^.u4fc/
w. ^^
Go*. (
600*1
Oof OZ-7-
\y
"*"*• ^^1
•
Rotameter
Setting
1 / » j
i i*1
( j/ffn
1 L
'
Dry Gas Meter
Temp. °C (°F)
^D ^
^ ( 11
^3 ^5
^-5 "^3
^4 >^
^
Vacuum
(in. Hg)
l#
/^
)&
\*
(6
-
Meter
Pressure
(in H20)
1.6
LO
M
l*(f
u
-
-------
OOr~?
r
j
7
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
H PACIFIC ENVIRONMENTAL SERVICES, INC.
Volatile Organic Sampling Train (VOST) Data Sheet
Lf^ - // ^* * ,, ,
Facility: /'
Date: "%
Time: O£
ir /VU few* /l/JMr
/wte
^
"C "
Citv. L7^ /Ivl^fe^
^^>
Samplina Location:
Run Number: /-V-
^ c^
TIwUSteL ^XAAk^a-
-1-2-
Meter Box No.:
M?(g W
Barometric Pressure, in. Hg:_
Ambient Temperature, °F:
Meter Gamma (y) Pre:_
Operator.
Purge Time:
Post:
Leak Check Data
Pre-test:
Post-test
Vacuum, inches Hg
Initial
^ro 2o
( &>-^ "
Final
7«
i6^r
Time, min
v,o
(.0
Run Data
Sample
Time
(min)
0
-r
ID
\6
7o
1$
Clock
Time
124-hr)^
0^
03*4
OW
09(4
aQtf
0^14
Meter
Volume,
litej*^3)
/I.W^
[ l,^ I
a.^
2.^
-
\5.W/
V^y
f^V)'< -0^"^
Cr^1-
Rota meter
Setting
fl/J
fl.fl
o,9
0,9
~
"
\^^
Dry Gas Meter
Temp. °C (°F)
~W 1&
^ B\
Qt- ei
$1 B
—
"
Meter
Pressure
(in H20)
(.6
(.6
LA
^
—
-------
o
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Customer:.
Facility: 6 o
?db
Final
76.0
70^
Time, min
Lo
Run Data
Sample
Time
(min)
O
$
(0
i<
lo
_2£
5lQu
Clock
Time
124-hr)
CH^ 1
6^C6?
&&[&*
tow
(oil
(t\ip
l&2$
Meter
Volume,
liters (ft3)
5.336
4><^
4.4<
U4-
5 ^
Cfi.ty'^
\J
fAd^c
Rota meter
Setting
M
6$
&A
0.^
O,4
OJ
^
Vtmr "
-
Dry Gas Meter
Temp. °C (°F)
0(0 34
^| ^4
^^ 9^
f\(e> \5?>
44 Qzf
-------
L
JL
J(
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Customer:
Facility:
Date:
, -
\ar l)VU (fafaur
Volatile Organic Sampling Train (VOST) Data Sheet
Project No.:
City: L
Time: (
V)6-\
Meter Box No.:
Barometric Pressure, in. Hg:
Ambient Temperature, °F:_
Sampling Location:
Run Number: T
Meter Gamma (y) Pre:_
Operator:
Purge Time:
Post:
Leak Check Data
P re-test:
Post-test
Vacuum, inches Hg
Initial
2^
to
Final
2,i>
lo
Time, min
t~°
U0
Run Data
Sample
Time
(min)
0
r
to
(
6.4
if^
14*
l&Co
V?
(Me W«
Xh
CL--
Rotameter
Setting
d,Q
/,<>
u
L^J
fsM>
vt
Dry Gas Meter
Temp. °C (°F)
^ /60
9S» \&
W L«(
^?6 /o/
Vacuum
(in. Hg)
IC>^>
16-0
16.0
/or
Meter
Pressure
(in H20)
If
M-
r
-------
O
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Customer:.
Facility:
Date:
..<
K
Volatile Organic Sampling Train (VOST) Data Sheet
Project No.:
City:
_
Time: 3 I* fif**
Sampling Location :_£l4£^**k-
Run Number: T~\/ '&•" *-
Meter Box No.: * Vfi . I ""
Barometric Pressure, in. Hg:
Ambient Temperature, °F:_
Meter Gamma (y) Pre:_
Operator:
Purge Time:
Post:
Leak Check Data
Pre-test:
Post-test
Vacuum, inches Hg
Initial
?6.0
&*G
Final
?£>.0
J&&
Time, min
[-$~
(3
Run Data
Sample
Time
(min)
O
^
\o
\$
10
1^
Clock
Time
124-hr)
ALi^^L^
/)"£^f^
ow
cVJK"
C$44
6945~
^W^7J
Meter
Volume,
liters (ft3)
W6
SlCD
83. 6^
^A.^v
Cft.o
\c>(n&
Rotameter
Setting
l.o
/•*
1,0
1,0
Le
Dry Gas Meter
Temp. °C (°F)
7^ e<
Bt 67
%Z &?
$£ &1
$6 W
Vacuum
(in. Hg)
/6.
16
16
((c
\li
Meter
Pressure
(in H20)
l&
(.3-
<<1
(.7-
(&
-------
OOC3 GZD
dUL t(-J
H] PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Customer:.
Facility:
Date: "
Volatile Organic Sampling Train (VOST) Data Sheet
Project NO.:
City:
Time:
/
Meter Box No.:
Barometric Pressure, in. Hg:_
Ambient Temperature, °F:
-fa
Sampling Location:
Run Number: T
Meter Gamma (y) Pre:_
Operator:
Purge Time:
Post:
Leak Check Data
Pre-test:
Post-test
Vacuum, inches Hg
lnitiaH&lN
yny$& \7(*j)
?l.o
FinafSj^
2a*« l^.o
l\
Time, min
If
Lr
Run Data
Sample
Time
(min)
&
-------
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
.Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Volatile Organic Sampling Train (VOST) Data Sheet
Customer: U 5 CTM . «W- P
Facilitv: Mr fllx IfctlMiX K
Date: ^ \~i6\%
Time: /(5^ ^
.. ... -\jff / MfVl
Meter Box No.: j/'o f vo"t
— /\ •
Barometric Pressure, in. Ha: &*-
Ambient Temperature, °F: -^"iPC
1
Pre-test: 7
Post-test $;
) Project No.: UXt -tft-
«»<- & Citv: (& ///W6rLE^
Samplina Location: /t^
S *, Run Number: T'V"4
1 ^ Meter Gamma (Y^ Pre:
?4I ^O ^ 1 ^
™ ?5^^W\ Operator: /A^vfl^
> Purae Time:
_ ?\ c<
-5^£ A
Leak Check Data
Vacuum, inches Hg
nitial Final
a o IQ.O
>.<" ?*~0
>(
ff
J/uta, f^klffh^r
%'J
Post:
Time, min
(\2~
(c6
Run Data
Sample
Time
(min)
T?
5
/^
^
12CZ-
/2^
\TA^
Meter
Volume,
liters (ft3)
/t4.^f
-
(^.61?
iSk&
/4/.6T
W-o
(00.74-
Rotameter
Setting
(9r^
^
0^
&,&'$-
O,<3K
o.e5 /tf^
Vacuum
(in. Hg)
AZ&lo
^
^>
1e>
To
16
Meter
Pressure
(in H20)
L6>
,
L(<
1.6
(.0
U
-------
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Volatile Organic Sampling Train (VOST) Data Sheet
Project No.:
City: 1 05
Time:
Sampling Location:
Run Number:
Meter Box No.:
V?./
Barometric Pressure, in. Hg:
Ambient Temperature, °F:
£ i '
Meter Gamma (y) Pre:_
Operator:
Purge Time:
Post:
5
Leak Check Data
Pre-test:
Post-test
Vacuum, inches Hg
Initial
too
'20.°
Final
2^.O
~l£> .0
Time, min
L*
LD
Run Data
Sample
Time
(min)
0
$
10
if
^e>
K
Clock
Time
^24-hr)
n^>
tfoo
[So*
I3io
&
(64: (0&
Vacuum
(in. Hg)
U
It
16
\i
(t-
Meter
Pressure
(in H20)
i^r
(.9
U
i$
IJ
-------
OSCS7 P5^
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Customer:
Facility: /4>f /My
Date:
Time:
fa
Volatile Organic Sampling Train (VOST) Data Sheet
Project No.:
City: I0?
Meter Box No.:
Mi-I
Barometric Pressure, in. Hg:_
Ambient Temperature, °F:
"C'
Sampling Location:.
Run Number: »-V '•
Meter Gamma (y) Pre:_
Operator:
Purge Time:
Post:
Leak Check Data
Pre-test:
Post-test
Vacuum, inches Hg
Initial
n.T
-------
OPACIRC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Volatile Organic Sampling Train (VOST) Data Sheet
Customer: Vf
Facility:
Date:
&Vc
'4>r
Time: /0(0
Meter Box No.:
v»- (
Barometric Pressure, in. Hg:_
Ambient Temperature, °F:
29.73
Project NO.:
City: fa
Crf-
Sampling Location:
Run Number: T-V -
Meter Gamma (y) Pre:_
Operator:
Purge Time:
Post:
Leak Check Data
Pre-test:
Post-test
Vacuum, inches Hg
Initial
a.o
/O- t>
Final
f2-o
/6,d
Time, min
/. 6
/.o
Run Data
Sample
Time
(min)
O
*>
/o
«
U
l^
Clock
Time
(24-hr)
\cxft
fo>4-
\0\*l
\02Ar
W?
I034
Meter
Volume,
liters (ft3)
ftis*
to!,*
ZCSvT
,-
tl$*z
ne.te
Rotameter
Setting
d.«
0*
0,9
—
OA
Dry Gas Meter
Temp. °C (°F)
4
/,^
/.>
—
'.T
-------
// ft.
O PACIRC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Volatile Organic Sampling Train (VOST) Data Sheet
Customer: C/^
Facilitv: ('w
Date: ^ /
Time: f#
Meter Box No.
' C//f KffrC- ^>(W
ffln /kftAKT JL#
rr
Ml-L
Barometric Pressure, in. Ha: c1-
Ambient Temp
erature, °F: /%~9t>
1
Pre-test: /C
Post-test fa
H Project No.: J-6'^- °°^
W7 ^ Citv: CiS? Mv/6tz^i( £/4-
Samplina Location: /tw/^tt^ (zoMrtrflr
Run Number: T- V - ? -^
Meter Gamma (v) Pre: Post:
25 Operator: ^^
Purae Time: ^ / "~
Leak Check Data
Vacuum, inches Hg
nitial Final Time, min
LO JO.o LO
S lo-V (^
Run Data
Sample
Time
(min)
O
6
lo
l*-
1z>
2^
?0
Clock
Time
(24-hr)
^0<1
/O^
I/^J
Ht3
niff
I&3
Meter
Volume,
litersjft3)
?(S^
?7?.^>
?2f. 3
7.T2-4-0
t&*<,
^3°|.oo
(
<1^W3.
Rota meter
Setting
e/*r
0.^
fi.^K
*&r*> oA
^
Dry Gas Meter
Temp. °C (°F)
fOf (n
(0^5 //^
jo-} |/z.
/«^ /(^
/«•?- lit-
•
o-w% t.//*.^ x: 3
Vacuum
(in. Hg)
|0-d
/0,o
fO.c)
(tf.O
f'd.c;
o f^«>* A
.) —
Meter
Pressure
(in H20)
(.6
u
(.0
<,(,
u
-------
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park V%st
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Volatile Organic Sampling Train (VOST) Data Sheet
Customer jfe tM
Facility: /Aft ////\X
Date:
Time:
Meter Box No.:
Ub. (
Barometric Pressure, in. Hg:_
Ambient Temperature, °F:
Project No.:
Citv:
C
Sampling Location:
Run Number: 7
Mater Gamma (y) Pre:_
Operator
Purge Time:
Post:
Leak Check Data
Pre-test:
Vacuum, inches Hg
Initial
jfl.o
Final
rf-o
Time, min
(^
Run Data
Sample
Time
(min)
Clock
Time
(24-hr)
Meter
Volume,
liters (ft3)
Rotameter
Setting
Dry Gas Meter
Temp. °C (°F)
Vacuum
(in. Hg)
Meter
Pressure
(in H20)
-------
Pacific Environmental Services VOST Box Calibration
Date: 7/19-98
Vost Box Number: V-l
Bubble Meter
1012 1007
1010 1007
1010 1008
1009
Average: 1009.00
Bubble Meter
1008 1010
1010 1009
1011 1007
1003
Average: 1008.29
1009 1005
1008 1003
1006 1005
1008
Average: 1006.29
Flow Rate: 1.0 1/min
Rotameter Setting:
Bubble Meter Temp. :
Run 1
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Y=
Run 2
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Y=
Run 3
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Y=
1.08
91
Meter Box
9829
9855
104
104
101
26.25
972.821
1.0372
Meter Box
9855.5
9881.5
104
103
103.5
26.25
968.505
1.0411
9882
9908
104
103
103.5
26.26
968.1358553
1.0394
Average Y=
1.0392
-------
-------
-------
-------
•tans-yijX*»»Hftiisr/
[PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
EPA Method 18 Adsorbent Tube Data Sheet
Pbnt
fjrf /fa 4(>L//
Date:
Sampling Location:.
Sampling Method Type: /115
Run I
Field Team Leader
fMtt>\
Concurrent Train ID:
DESCRIPTION OF TRAIN
Leg
A
B
Moisture Knockout
(if used, indicate type)
,
Tube a Description
trs-m^-fc^x A*.
^BD-iwt- kwl fV_
Tube b Description
~\&J>- »hfc-fci*J (&>
7B?-tf/fcXj 6b
Tube c Description
Leg
A
B
Volume (mL)
r
^ ^5
LJ r*-
\4 O
^HT
b>4 f~\
lt>«5
M
o
Vi-f5 1^,0
^$TT JVC
j-f^5~ /TO
4^CT !G>0
J4-f= /^O
^TT /fjO
2&^ 1* 0
2s*nrZos>
Z-/0
Clock Time
/~A2D
Leg A
Flow (L/min)
~73_
7/L
7 3-
7^-
71.
^4-
7 J.
>1^
71
-71-
7
(.
^/
(#
((?
r/
d^
>!.
>^L
Tlv
7-rL-
>*2-
>3-
7l~
•^
•>i-
7/L-
7*L-
74.
v
^f
•3-
"^
•^
7-
CALIBRATION - POST-TEST
Leg
A
B
Volume (mL)
-------
PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park. North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant
EPA Method 18 Adsorbent Tube Data Sheet
(L-
Date: "Wttftfc
Sampling Location: ~V
Sampling Method Type:_
\"MfS* f\
Run Number "*'"
Field Team Leaden
Concurrent Train ID:
DESCRIPTION OF TRAIN
Leg
A
B
Moisture Knockout
(if used, indicate type)
~"
Tube a Description
'—
-"
Tube b Description
•
-^"^
Tube c Description
— -
"~ —
CALIBRATION - PRETEST
Leg
A
B
Volume (mL)
• —
Temperature (°F)
• — •
•= —
Time (seconds)
-—
-—
Pbar (inches Hg)
• — -
«—
RUN DATA
Elapsed Time
2-Txj
7.3>fe
T^HO
Clock Time
I-2.51*
Leg A
Flow (Umin)
7\
•7 /
71
Vacuum (in Hg)
/,
U
if
LegB
Flow (L/min)
> I
-7 I
7l
Vacuum (in Hg)
^?-
^
1
CALIBRATION - POST-TEST
Leg
A
B
Volume (mL)
.
Temperature (°F)
^
•
Time (seconds)
Pbar (inches Hg)
>
'
P:\i012.001\misc\ml8sheetdoc
-------
PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant
EPA Method 18 Adsorbent Tube Data Sheet
(
Date:
Sampling Location: _^
*Ajs'l—
Sampling Method Type: M\ - A^ft-
>H"V\ Field Team Leader.
Concurrent Train ID: ^ p\5"
DESCRIPTION OF TRAIN
Leg
A
B
Moisture Knockout
(if used, indicate type)
— • —
Tube a Description
Ten- rv^ - (UjtKt
Ttt>- MI*, - '\UJZ, &
Tube b Description
~ien-fM?, -C^L^
R Ten-fftto-^'Lfc
Tube c Description
b " v
b —
CALIBRATION - PRETEST
Leg
A
B
Volume (mL)
lOCXb^Lx
°l°I^JiUL
Temperature (°F)
^
Time (seconds)
—
— .
Pbar (inches Hg)
f .
*
RUN DATA
Elapsed Time
fco
110
110
Clock Time
o>
Leg A
Flow (L/min)
-7 1
7 I
•7 1
7
Vacuum (in Hg)
8
B
8
LegB
Flow (L/min)
7 /
Vacuum (in Hg)
S
5
CALIBRATION - POST-TEST
Leg
A
B
Volume (mL)
^°C
o\ ^^
Temperature (°F)
— ^
—
LPW Ctett, #^Tfcf
-------
PACIFIC ENV1RONMEKTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
EPA Method 18 Adsorbent Tube Data Sheet
Plant r^-V M*X T^ffaAA- V^*ct v^_
Samp
Samp
Run!
* ^ I . t~r*t t
>linq Location: TU/ir^J f^n&^s'r i)u uj
Date: -f-/ir(96
>lina Method Tvoe: Ml-—
RUN DATA
Elapsed Time
7 ft 6
H6
t&Q
2JO
Z£*
2^o
•z-YO
Clock Time
\di(*
}<&'*>(*
it ^b
ie> <>\s
i ioC"
ili(.
1 / 2J>
Leg A
Flow (L/min)
7^
-71
~7\
7 |
Vl
71
71
Vacuum (in Hg)
ft
8
fe
<&
%
t>
%
Le
Flow (L/min)
^2-
>l
»
71
>/
? 1
^\
ae
Vacuum (in Hg)
%
%
<2
8
S
&
t>
CALIBRATION - POST-TEST
Leg
A
B
Volume (mL)
. .
Temperature (°F)
,-^
-
Time (seconds)
—
"
Pbar (inches Hg)
-~>
P:\i012.001\misc\ml8sheetdoc
-------
I*
PACIFIC ENVIRONMENTAL SERVICES. MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant
fi*
EPA Method 18 Adsorbent Tube Data Sheet
PL+ C.
Date:
Sampling Location:.
Sampling Method Type: Mlt)
Run Number TfeO- ffttf.- ^v/^ M:
±L
_Field Team Leader.
Concurrent Train ID:
DESCRIPTION OF TRAIN
Leg
A
B
Moisture Knockout
(if used, indicate type)
: —
Tube a Description
TED- WI6-&.M /k
T6D -/Wft - 0LW LV
Tube b Description
ie-0-ff)^^^ fo
1&D~Mto- ^W6b
Tube c Description
—"
CALIBRATION - PRETEST
Leg
A
B
Volume (mL)
°}^
ion
Temperature (°F)
_
— -
Time (seconds)
—
-^
Pbar (inches Hg)
. —
""
RUN DATA
Elapsed Time
/O
VD
//o
JLO
Clock Time
/o
/o
Leg A
Flow (L/min)
7-0-
71
71-
2^.
74-
-7
74
74-
71.
Vacuum (in Hg)
ft
LegB
Flow (L/min)
71.
71-
74-
Vacuum (in Hg)
8
CALIBRATION - POST-TEST
Leg
A
B
Volume (mL)
9°I5
/60fc>
Temperature (°F)
J
-------
PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park. North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
EPA Method 18 Adsorbent Tube Data Sheet
Plant *\A- MA-L A^G V\cU- V\c~A V Date: 4-teu 19%
Samp
Samp
Runt
* w ' ^ f 1
ilinq Location: "T"*-"1^*! Z* La^rr 'IXof'
>linq Method Type: /Hj %> Field Team Leaden ^60
dumber TED- JKVA- 2^— *4 Concurrent Train ID: AIA^ •A'v*'
DESCRIPTION OF TRAIN
Leg
A
B
Moisture Knockout
(if used, indicate type)
— .
^^
Tube a Description Tube b Description Tube c Description
— -^
* «
CALIBRATION - PRETEST
Leg
A
B
Volume (mL)
.
Temperature (°F) Time (seconds) Pbar (inches Hg)
— — . -s
^ --
RUN DATA
Elapsed Time
ito>
fab
LOO
^\c^
1\jt>
V**>
^t>
Clock Time
MC,
fL*(*
I*>CW
l?>ILe>
fa*
!^-*>vto
Leg A
Flow (L/min)
T\
~7\
7|
•71
71
71
7}
Vacuum (in Hg)
e
^
K
t
«>
<$
r>
LegB
Flow (L/min)
71
-7[
>|
-7\
71
•71
7\
Vacuum (in Hg)
if
e
$,
%
«
<*
%>
CALIBRATION - POST-TEST
Leg
A
B
Volume (mL)
"--"
Temperature (CF)
, — -
— —
Time (seconds)
— •
^^
Pbar (inches Hg)
~-
P:\rO 12.001 \misc\m 18shcet.doc
-------
PACIFIC ENVBONHENTM. SERVICES, DC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
EPA Mtthod 18 Adtorbenl Tube Data Sheet
I of
Plant.
Sampling Location: "\u
Sampling Method Type:.
Run Number t£P-/dlg-
Concurrent Train ID: **\
DESCRIPTION OF TRAIN
Leg
A
B
Moisture Knockout
(if used, indicate type)
—
—
Tube a Description
T^0- /»/«-&* 3 A*.
ItO-Mlt- -k^&c.
Tube b Description
TPD-'/rt/fJ- £ov"2»A-
TEO- WU«- k>irJS&
Tube c Description
b -^
^
t>
CALIBRATION - PRETEST
Leg
A
B
Volume (mL)
/6> o5 "-'/«--
/Zfctt iJ/rt.^
Temperature (°F)
Time (seconds)
— —
Pbar (inches Hg)
zazj
2«U-2>
RUN DATA
Elapsed Time
16
Yo
Clock Time
Leg A
Flow (L/min)
7 1
7 /
-7
71
7)
71
/I
Vacuum (in Hg)
1'
ft
LegB
Flow (L/min)
> 1
7/
71
7 1
7l
71
7'
71
Vacuum (in Hg)
K
fc
e
CALIBRATION - POST-TEST
Leg
A
B
Volume (mL)
10 m JL*
1 II -
lbb^> /WAv^
— 7
Temperature (°F) (/
jff Tte
Time (seconds)
. — ^
— - .
Pbar (inches Hg)
P:\r012.001\misc\ml8sheet.doc
-------
PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX; (919) 941-0234
EPA Method 18 Adsorbent Tube Data Sheet
2.
Plant -lAM IVU^ /^DXtAV ~\ \c^ \_ Date. ^/vafcfr
Sampling Locatio
Sampling Method
Run Number. T
i \ I .
n: \x> *v v\jp\ 9- ^ v\*i .x^ \7^ *-> ^-^
x
Tvoe: ^\fe ( Kr^^'Vi:V-\ Field Team Leader ^4=R
^0-MlVQ->— 3» Concurrent Train ID: MfA^. M"3,\(f
DESCRIPTION OF TRAIN
Leg
A
B
Moisture Knockout Tube a Description
(if used, indicate type)
.
»
Tube b Description
—
Tube c Description
— ^
— -
CALIBRATION - PRETEST
Leg
A
B
RUN
Volume (mL) Temperature (°F)
^
— - c.—
Time (seconds)
— ,
. — -
DATA
Elapsed Time
)££>
IffO
•?zd
7 &}£}
2.) f>
f^^&
2-30
2 V"Z>
Clock Time
/ Qj£5-tort"
4-tlC5^' JsSiT
i>-t<^ DOS'
4-f-nT it 1ST
vt^lf1 ,/2£
LJ-¥^ ii 3i.
ftf^~-f \ f t/^T
/jfe*H^--A\Tsf
>/
7y
•7/
>/
>/
7\
Vacuum (in Hg)
fc
fe
^
*§
«s
t)
%
2>
Pbar (inches Hg)
^
c--
LegB
Flow
(L/min)
--7^
7)
~?l
•yl
~?l
>|
7/
-7
i
Vacuum (in Hg)
ft
9
*fe
€
ft
t>
CALIBRATION - POST-TEST
Leg
A
B
Volume (mL) Temperature (°F)
—^ - — >
<- ^—
Time (seconds)
—
<— .
Pbar (inches Hg)
.
<-^
P:\r012.001\misc\ml8sheetdoc
-------
PACIFIC ENVIRONMENTAL SERVICES, WC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
EPA Method 18 Adsorbent Tube Data Sheet
Plant:
[U M
Date:
Sam|
Samj
Run
DES(
Leg
A
B
Dlinq Location: ~TO W.JU &
CALIBRATION - PRETEST
Leg
A
B
Volume (mL)
°\°\^r
^^
Temperature (°F) Time (seconds) Pbar (inches Hg)
-^ — ^
" ^^ *~~
RUN DATA
Elapsed Time
Clock Time
\~H&
V2><=>
Leg A
Flow (Umin)
—
. —
Vacuum (in Hg)
.Zo-uvL.
2-fertvvV\4
0
LegB
Flow (L/min)
^
—
Vacuum (in Hg)
as^\V
Z& ,V rtv
7
CALIBRATION - POST-TEST
Leg
A
B
Volume (mL)
°l°i l
^G
Temperature (°F)
—
•^
Time (seconds)
—
,
Pbar (inches Hg)
—^
— "
P:\rO 12.001 \misc\m 18sheet.doc
-------
APPENDIX C.2
SED FIELD DATA
-------
-------
1^*5 ilF^ff l^v//
1 PACIFIC ENVIRONMENTAL SERVICES, INC.
PlAOT d IA.
FIELD DATA
Plant
Dale
Sampling Location
Sample Type
Run Number
Operator 3
Daromelrie Pressure (( ) -3^**^
Static Pressure (U ) ^«
Filter Nurobei(t) •—
Pretest Leak Rale » o.
Pretest Pilot Leak Check
Pretest Onat Leak Check —
.faLllg
<*», I
CO
—
—
Oimlciixci*
V,: SMfcapcl
Total 11 (I
1'iube Ixnglli and Type
Pilot Tube I.D. No.
Nozzle I.D._Z-C
o-v
Assumed Molsluie. ft
Meier Dos Number
MelerAll® Jj
Meter Oamma
Reference p _
o -
Read and Record all Data Every
Page ) of \
Z
Minute*
Schcmalicof
Traverse Point Layout
Temp. Sensor ID No.
Post Test Uak Rale - O.o.yo cfm 0
Pott Test Pilot Leak Check QVg-
Posl Test Orsal Leak Check
.in. I If;
TllVCIM
Potal
How.
f»kt
/
/
/
OockTbM
(M-koul
dad)
UHMelCf
nun
codtf
hulllO
i
OfHiM net. Uillci c«IM
Dc
Advil
tapugef
Temp.
•F
^
GuMdctTcnp.
Uullel
Vacuum
la.lit
T- I
tSS . ^ L 1
O. »i
•Z.HH
SL.
2
0-
'i-\9
3 .'
Q. >C
T-.VS
SM
Its / \ I S
O. \ V
z.
18
JO
o.
Z.oo
1.0
\S 1
SV
o.\ i
o.it
C.
o .08
C.3
^P
i^V
&**
&*
o.
2-t.H
7.1 P
100
TO
O.i
t-co
too
S-
IL
ILUL
10
i.oo
7..'
'Z-t'O
i±l
10
o.\y
z..-
to
THvf T-MC
foS"
o-
o
L-HO
z^y
lOQ
1-
O.t-7.
8^
/
J29L
TSo
O-Otf
\.-i~
joo.
n.ou
Kb
^0.
Ji.
n
1 AI
-------
PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant:
Sampling Location: ^
Sample Recovery Person:.
Sampling Method Type:
Run Number /
Job Number
Sample Train Recovery Data
Date:
Field Team Leader.
. Impinger Train ID:.
Comments:
Filter
Filter Description:
Filter No.:
Filter Description:
Front Half Data
. Filter Media Type:
rs
Filter Media Type:_
Back Half Data
Impinger Purge-
Start Time:
Flow Rate:
Stop Time:.
Purge Gas:.
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):
Description of Impinger catch:.
Impinger 2
Impingera
\\4.
Impnger 4
Impinger 5
Final Impinger
(9):.
(9):_
(9):.
-------
liV? i_* I *rj-«flH «.'•.-!
13 PACIFIC ENVIRONMENTAL SERVICES, INC.
Hani Uor
Dale
FIELD DATA
OHLiTf LA- OA
CO
V,: Silii
CoHdcHSd*
Total l}0
Sampling Location *£& &\^o
Sample Type M>yg"
Run Number -3-vS- SC-O ~tr
Opcralnr
1'iolic Ungtli and Type
Pilot Tube I.D. No.
Nozzle ID O
Daromelric Pressure (g
Static Pressure (P, ) _r
Filler Number(s) —
Pretest Uak Rale - QjQjotrrfai @
Prelesi Pilot Leak Check o^
Pretest Onal Leak Check '
Assumed Mohlure.% o^o
ft.is.
^*»«». T-
^Lx.
o
T.OM
z.o
te>\
HOC.
Q.
(o\
to (.
M03
& /
1 O <*>
10
.SO
(i
I 10*0
uo
(.0
. V
(oO
z.*-
O-
T.o
to
tot
O.
L.
to.i
MO / \ 0
1
VC5
/ UOZ-
O.
2,*.
10*
O. 11
GO
\os
0
2^P
JfeS.
tos
10
>.0»
^L
O .'
Jli
Voo
5
•--•«» •* *^ L-* <— «
-------
O PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Sample Train Recovery Data
Plant:
Date:
Jl/o
Sampling Location:,
Sample Recovery Person:.
Sampling Method Type:
Run Number. jf
Job Number
/
Field Team Leader,
/s ' //h
ew
. Impinger Train ID:_
Comments:
Filter No.:
"-//3/f-Z-F
Front Half Data
. Filter Media Type:_
Filter Description:,
Filter No.:
Filter Description:,
. Filter Media Type:.
Impinger Purge-
Start Time:
Flow Rate:
Back Half Data
Stop Time:_
Purge Gas:.
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):
Description of Impinger catch:_
Impinger 1
JPff.S
Impinger 4
n.
Impinger 2
Impinger
Impinger 5
1-0
Final Impinger
(8):.
(9):_
(9):.
-------
FIELD DATA SHEET
$c(o
Plant
Sampling Location
Run Number: S-MW-f- Date: 1-/zd/f8
Pretest Leak Rate: g>'t?o^ cfm @ l& in. Hg.
Pretest Leak Check: Pilot: _f/Orsat: ///A
Sample T]
Pbar
CO2:
Operator: /3"fV
Nozzle ID: Q-'fe?? Thermocouple »:
Assumed Bws: HQ Filter #: - — •>
O2: 2cT
f
Probe LengbVType: S f/t& Ptot #: 0-'
Slack Diameter: t
Post-Test Leak Rate: Of>0\ cfm @ >0 in. Hg.
Post-Test Leak Check: Pilot:
Tn
NumbM
Tlnw
(mln)
OockHma
(244iour
doch)
Gaa Malar
Rawfcig
kiHZO
(AH)lnH2O
Patlrad I Actual
Stack
Tamp.
Tamparalura
°F
Proba I
Tamp.
°F
Dry Gaa Malar Tamp.
Intot
(Tmln0F)
Outtat
(Tm out°F)
Pump
Vacuum
«in.Hfl)
-is
ICo. 1
7,-
Go
O.tS"
JLO.
0-
0->M
t-MY
J%±.
13
10
0-
O- \M
0. 8%
o.gt,
fcZ
BO
O -\>
fco
fla
O -\\
t-Z/i
MO
0-08
O.°IO
P-^Q
ZMfl
O-ftfc
^.
P.OH
O.ftfe
0.6fo
o-Qfa
KSr
7,
O
0- SI
CO
0-OC,
0-foT
62,
0- 00
0 -ok
O.te's
"to
O-OS
6.C1
AH
TS-
-------
D PACIFIC ENVIRONMENTAL SERVICES, INC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant:
Sampling Location: '
Sample Recovery Person:
Sampling Method Type:
Run Number: t> —
Job Number: (T
Sample Train Recovery Data
i*s=
Date:
Field Team Leader:
Impinger Train ID:_
-OO1
Comments:
Filter No.: ( \
O. W\4
Filter Description:.
Filter No.:
Filter Description:
Front Half Data
Filter Media Type:_
Filter Media Type:_
Impinger Purge-
Start Time:
Flow Rate:
Back Half Data
Stop Time:_
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):
Description of Impinger catch:_
Impinger^
7.
t
Impinger^
530.7
Purge Gas:_
Impinger^
Impinger
S23.J
I .-? /
Impinger^f
Final Impinger
(g):_
(9):_
-------
FIELD DATA SHEET
Plant UoT
&.«,ytvAi.T
Sampling Location siiQ -fr "*
Bun Number: ^ukiavi- Date:
&A. Sample Type: MS>s"
Pbar y\ .
CO2:
Operator: T
Ps: ~
— O2:
Nozzle ID: Q.sB'O Thermocouple #:
Assumed Bws: ~ Filter #: "
Meter Box #:
Pretest Leak Rate: Q.QQ> elm @ \s In. Hg.
Pretest Leak Check: Pftot: ^ Orsat: —
Probe Length/Type:
Slack Diameter: IO.Q" As:
PHot #:
Y:o.qftS AH@: \ .^>c\
Post-Test Leak Rate: Q.OQ> c(m @\g'm. Hg.
Post-Test Leak Check: Pilot: v^ Orsat: —;
TrwwM
Polnl
Numbw
Tkn*
(mln|
CkxATIm
dock)
RMffing
InHZO
Orilc* Pr«8Mit • DWMwilU
(AH)lnH20
Actual
Stack
Twnp.
T«mp«ratur*
°F
Prob* j Fitter
Twnp.
°F
Dry Gna Mrt»r T«mp.
InUI
OuUrt
(Tmoul°F)
Pump
Vacuum
(in.Hfl)
AH-
Ti-
TS-
-------
MOISTURE RECOVERY SHEET
PACIFIC ENVIRONMENTAL SERVICES, INC.
FACILITY:
SOURCE:
DATE:
RUN#:
METHOD #:
BOX#:
21 £
IMPINGER CONTENTS FINAL INITIAL TOTAL
GRAMS GRAMS GRAMS
1
2
3
4
D.I. WATER
D.I. WATER
EMPTY
SILICA GEL
$M -1
~>^ :(j
$52.7
%0(*.3
2(si4
t*(-l
Sj-z-r
fOG.J
o
' ~e>.\
6. .2.
O.
TOTAL GRAMS COLLECTED
OA
INITALS:
JUS
PACIFIC ENVIRONMENTAL SERVICES, INC. -
-------
f PACIFIC ENVIRONMENTAL SERVICES. INC.
Plant Uor »*< / ».^pH«.ir PuvMT (L LA. Q.A .
Dale (TV - -?,M - S ft
Sampling Location S>\ to
Sample Type
Run Number SEO-
Uperalor
FIELD DATA
Daromelrlc Pressure (( )
Static Pressure (IS ) - o.2.S>
Hller Numbers) -—
t"^
Pretest Leak Rale - o. oo«-»rfm 9
Pretest Pilot Leak Check
.btllg
<>i
(X>
V,: Silica gel
ToiallJO
1'iobc I jcngih anil Type
Pilot Tube I.D. No..
n O. 3g)
Assumed Moisture. %
Meier Dos Number
Meier A II®__
Meier Oaoima
Referenda p
o.
Pretest Orsat Leak Check _ —-
Read and Record all Data Bray
Page i of
Mlnuie.
Schematic of
Traverse Point Layout
Temp. Sensor ID No.
Post Ten Leak Rale » C .
Pott Test Pilot Leak Check _
Port Teil Onwl Leak Check —
OK.
1
In.IIB
livcne
fata
(*k)
/
/
/
OockThM
(24-bour
dod)
UMMclCI
Meidb|
nun
Vctocf
ktd4
kl
ounce n
(All) h. ll}0
Acted
Temp. »T
I
Teap./ Fttct
TtBB.*F
tapiD|cr
Temp.
•F
OM Melei Tcnp.
Uulkl
rump
Vacuum
to. lit
s- <
0. JL,
foS
La
O.
7 .1
AS ?
0. (5
ZSl /
SS
ZM4
SM
as
0 ,3
».
2.CZ. /
3O
o. u
-#
<-
O.
\--\\
1 -
0.
1 -> »
^v^"V
9\
0 • ID
1.3
5\
- »
to
cuC
IS?
St.
^-^^
8\
Q-t
-------
O PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant:
14
Sampling Location: ^,'L
Sample Recovery Person:
Sampling Method Type:
Run Number. 4 -
Job Number
Sample Train Recovery Data
Date: "7 - J<( -7 Ti(p. C=
Impinger 5 Final Impinger
•S6- XAt^
*5J).^ faV. ^^S.^
^ » • faV. il-"S »/
?0
-------
1 PACIFIC ENVIRONMENTAL SERVICES, INC.
Plant I 'or K w A&.PKALT PLAMT c. LA OA
Dale 0^
FIELD DATA
Sampling Location S\ to VL-
Sample Type MMS
Run Number ^g.o - M(*e
PbJol
S»plb| /OockTkM
H~. / (2thour
(t.b.1 / dock)
Oeibcd
Taw
T«mp. »r
Artuil
TwG
Temp./ rillee
Tcmp.»F
•"Piot*'
Temp.
DryCi
Inicl
CM Meier Temp.
Uullel
ntmitf F
ISimp
Vacuum
to.Il>
s -\
/ "7IO
•Z.<=
/
0
O,i
so
Iz-
••*..'!>
^±
_3fi_
>
O. »H
Z. I
^o
/ ^30
o.
sn.
S3
£.<=
30 /
O. IO
l.S
T-^°
35 /
O.(
1. VI
Jj.
. t.
IO
o.
>. 2.
^L
\\
o. o>
..OH
as \
SO
88
\1
55 / ofcos
> -OH
> -O
-r-
foO
O.
(.5
O.
>O /
O.)
..3^
ZMM
IT.
O.IU
^JL
60 / e^oti
o.
•Z-MO
too
Jfato.Z.
o.\3
»."I
i-e>
°t
voo
10 (
It)
\OS
2^&
(07,
O.i
11
103
O.tO
LJL
55
10-5
-------
O PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Sample Train Recovery Data
Plant:
Date:
Sampling Location:.
Sample Recovery Person:
Sampling Method Type:
Run Number
Job Number
Field Team Leader.
. Impinger Train ID:
r\ / r
Comments:
Filter No.:
Filter Description:,
Filter No.:
Filter Description:,
Front Half Data
. Filter Media Type:
. Filter Media Type:_
Impinger Purge-
Start Time:
Flow Rate:
Back Half Pata
Stop Time:_
Purge Gas:.
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):
Description of Impinger catch:_
Impinger 1
/VlT
Impinger 4
Impinger 2
Impinger 5
Impinger 3
7/5?. 0
Final Impinger
(9)'._
-------
FIELD DATA SHEET
Plant HOT
-T PI-AM T C.
* 2
Sampling Location
Run Number: seo- nrts-3 Data: -3 - 7.
Samplejype:
Pbar
CO2:
O2: —•
/
Pretest Leak Rate: p. 003 cfm @ is in. Hg.
Pretest Leak Check: Pilot: *s Great:
Probe Length/Type: 3e"6wv^s Pilot #:
Stack Diameter: t o. o *' As:
Nozzle ID: Q.sSl Thermocouple i
Assumed Bws: i.s Filter #:
Meter Box #: ^ Y: o_J*M.AH@: \.asi
Post-Test Leak Rate: -;;Cab cfm @ in. Hg.
Post-Test Leak Check: Pilot: Orsat:
TfOVWM
Point
Numbw
Samplng
TkM
(mln)
OocfcTIm*
dodi)
RMcftig
Velocity
kiHZO
Oridc* Praswr* Differential
(AH) In H2O
Deslrad
Actual
Stack
Tamp.
(Ts)
Tamparatura
°F
Proba
Fdtar
Impingar
Tamp.
°F
Dry Gas Malar Tamp.
Mot
(Tmln0F)
Ouflat
(Tm out°F)
Pump
Vacuum
f«n.Hg)
Y/////////////////////^^
0 .|
s.iw
3 .
6801
0- 1
10
SSO. »
0- l>
10
osn
O- "~
Z.Mt
Z.H
SB
)0
08
0-
SI*
to
0.
_L-
7..V
ZHfe
-------
PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant:
Sampling Location: ^
Sample Recovery Person:.
Sampling Method Type:
Run Number. £.
Job Number A£
Sample Train Recovery Data
Date:
IA
Field Team Leader.
. Impinger Train ID:_
Comments:
Filter No.: (J/-. * L>*V k^r,* J
Filter Description: _ £
Filter No.:
Front Half Data
Filter Media Type:
Filter Description:
Impinger Purge-
Start Time:
Filter Media Type:
Flow Rate:
Back Half Data
Stop Time:.
Purge Gas:_
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):
Description of Impinger catch:_
Impinger 1
Impinger 2
Impinger 4
. s/
Impinger 5
Impinger 3
~? I6..
Final Impinger
(9):.
(g)-._
-------
FIELD DATA SHEET
* z
Plant
Sampling Location
Run Number: !>&o-nw;-4Date: 03.7?^
Pretest Leak Rate: 0 .oo> elm @ \i* In. Hg.
Pretest Leak Check: Pitot: ^ Orsat:
Sample T
Pbar
CO2:
HMS Operator:
r—
Ps:
O2: —
Probe Length/Type: ^"c
Stack Diameter: IQ.Q"
Ptot #:o-i-
As:
Nozzle ID: o.n^y Thermocouple #
Assumed Bws: «SX3 Filter #:
Meter Box it: -^A Y: p.'^VAH®:
Post-Test Leak Rate: QtOO(., elm @ >g in. Hg.
Post-Test Leak Check: Pilot: / Orsat: -—•
Travaraa
Polnl
Numbar
Tbm
(mln)
,0
11
It
o
to
Z.S
30
CkxfcTima
dock)
Jffl.
i^JL
'03C
30
Ga«M*t«f
FUacKng
(Vm)n3
- 0
Vabctly
HwdJApJ
kiH2O
Orilca Praaaura DMtrantial
(AH)inH20
D«sir«d
Actual
Slack
Tamp.
(Ts)
Tccnparatur*
°F
Probe
FVtar
Impingar
Tamp.
Dry Gas Mater Tarry.
Mai
(Tmln°F)
Outfat
(Trnout°F)
Q.\>
O. \O
O Oft
_0
O.Qg
O.O'V
O'.Ofc
liol
i^"
loo
1(0
IIS
Je 1
j?^(^^f
O M
0. xl
OlO
0.0%
O-O
Mb, 8
O
O.QU
0.61*
0-Ob
o.ou
0.^8
o.eo
0-
0-T^
O.VS"
o.c3
0-8O
O.VU
0.23
o.
2^.0
tol
3&b_
T-H'V
ZH^
ZTO
MS
SX
fcl
Jclc.
trO
_SJL
\oo
\oo
IOG
V03-
vo^-
103
r
\oo
tfil
vor
LjQJa
VOX
10Z.
VOl
VOv
V.OQ
SH
Tm-
Pump
Vacuum
f"n.Ho
10
u.i
1.6
-------
D PACIFIC ENVIRONMENTAL SERVICES, INC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant:
Sample Train Recovery Data
Date:
Sampling Location: rs i]
Sample Recovery Person:_
Sampling Method Type:
Run Number: fa-x>?xy??s—V
Job Number: £.013 -oo I
Field Team Leader:
Impinger Train ID:_
Comments:
Filter No.:
Filter Description:,
Filter No.:
Filter Description:,
Front Half Data
Filter Media Type: '_
Filter Media Type:_
Back Half Data
Impinger Purge-
Start Time:
Flow Rate:
Stop Time:.
Purge Gas:.
Impingtrl
Impinger 2
Impinger 3
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
^^LMoisture Collected (mL):
Description of Impinger catch:
f^A \ £} •»-
///=?. s-^s^-5 S-a-s.-? -7,
W^f ^» ^ ^— * *^ ft -^ i
* ^^ •» C ' ^** Jf * 0
Q, ^ K / *y -^ /'
Impinger 4 Impinger 5 Final
~)PQ^ ~7°l(*.o (a): ^
11$^ ~)X&.3 (Q); £
^\.-> S / /^.S / (a):
^~>1L
^CoH
>S ,(y
1 -4 -4
Impinger
^AV>>
3^. D
^7.7 /
f
91*
-------
t_2J
F PACIFIC ENVIRONMENTAL SERVICES, INC.
Plant I4OT H\f AspwUcijr Pv^itr g. ui
Dale o^
FIELD DATA
Sampling Location
EXMr*ovr
Run Number
Operator
-S
Barometric Pressure (g )
Static Pressure (IJ ) -O.
Filler Number(s) —
Pretest Leak Rale » ^.QO^ dm @
Pretest Pilot Leak Check *s
Pretest Onal Leak Check *—
('(I
„
V,: Silica gel
Total I JO
Probe I ineiJi and Type 39
" M
U
1
Smplbf /OockTkM
Ttoe. / (24-hour
doctj
\M03
rs
•20
\<\OQ
.V
-------
ii n i
D PACIFIC ENVIRONMENTAL SERVICES, INC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant:
•&
Sampling Location: ^
Sample Recovery Person:.
Sampling Method Type:
Run Number:
Job Number.
Sample Train Recovery Data
. Date: "7 -
Field Team Leader:
" ^1-7/?T5- -^
Impinger Train ID:_
Comments:
Filter No.:
Filter Description:.
Filter No.:
Filter Description:.
Front Half Data
. Filter Media Type:.
. Filter Media Type:.
Impinger Purge-
Start Time:
Flow Rate:
Back Half Data
Stop Time:
Purge Gas:_
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):
Description of Impinger catch:.
Impinger 1
/
Impinger 4
-------
FIELD DATA SHEET
Plant HorHiy A<5ft^cr?us>Jr a -
Sampling Location &U? d 2.
Run Number: &-AM*. Date: ere •
Operator:
Pretest Leak Rate: p.op? elm @ \s in. Hg.
Pretest Leak Check: Pilot: v^ Great:
Probe Length/Type: -3' GL*S»S Pitol #:
Slack Diameter: 10.0 " As:
Nozzle ID: Q.S^o Thermocouple #:
Assumed Bws: — Filter #: - •"
Meter Box 0:3* Y:,
Post-Test Leak Rate: o.pp2
Post-Test Leak Check: Pilot: */ Orsat: —
t.8S\
Ti
Pbht
Numbw
OockTlma
(244iour
docfc)
GM Malar
(Vm)f|3
Vabcity
Haad(Ap)
kiHZO
Oiloa Prasaura DMtrantfal
(AH) In H2O
Dasirad I Actual
^^«MMMPIHM«_
Stack
Tamp.
Tamparafeira
°F
Proba I F»t^
fcnpingar
Tamp.
°F
Dry Gaa Malar Tamp.
(Tmln0F)
Outfat
(Tmoul°F)
Pump
Vacuum
On.Hg)
qpo
AVm-
AH-
Ti-
Tro-
-------
PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant:
Sample Train Recovery Data
c
Date:
Sampling Location: ^>\ \o
Sample Recovery Person:
Sampling Method Type:
Run Number. -< -
Job Number. Q
Field Team Leaden
. Impinger Train ID:_
Comments:
Filter No.: I X-\AJ*\lr«r fLc)
Filter Description: Q_\«AY\
Filter No.:
Filter Description:
Front Half Data
Filter Media Tvoe: L*\\ A. 14
Filter Media Tvoe: •
Back Half Data
Impinger Purge-
Start Time:
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Contents:
Final Volume: (mL)
Initial Volume: (mL)
Net Volume: (mL)
Total Moisture Collected (mL):
Description of Impinger catch:
Flow Rate: " Stop Time:
Impinger 1 Impinger 2
syiT br
Purae Gas: *
Impinger 3
*n?. tf t*q$. 5" A. 1 3. 9
q~?-*4f <£?^/3.-S" /;«2 3 /l 6
i: 0>.^
: C(aeKX
£>
Final Impinger
(at 430.5"
faV 535. ?
-------
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Volatile Organic Sampling Train (VOST) Data Sheet
Customer
Facility:
Date: "?•
Time:
flfc
r>fsyo
5rt^«.0
«^-2-
c5,Z
Dry Gas Meter
Temp. °C (°F)
lj$
^
*79
«&
-7?
Si
7fr
7f
Vacuum
(in. Hg)
3
3
^
-5
3
4
^
V
Meter
Pressure
(in H20)
1
(
/
/
/
/
/
/
-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Volatile Organic Sampling Train (VOST) Data Sheet
Customer: HofM/* kyk*ir I
Facility: p)* A^ C_
Date: **\-7£>-<%
Time: CH ifc- O°fZ~C)
Meter Box No.: V—1— f
Barometric Pressure, in. Hg:
Ambient Temperature, °F:
*MtC JJ..CA Project No.: A^/2 . CO I
Oi*«». 1 ^ f 1 * _L ^
OltV. L* •/!• i /x( t^vo^^ii e±.
Samplinq Location: S&P - 3,' Ic ^"2_
Run Number: 5 - V — 2_
5G5
^ , Meter Gamma (Y) Pre: — Post: -
-v^^X o c»" Operator •Y'/t'
ID Purge Time: ' •
Leak Check Data
Pre-test:
Vacuum, inches Hg
Initial
/2L
Final
"7
Time, min
/
Run Data
Sample
Time
(min)
O
/O
0>
/O
0
/O
O
/6
Clock
Time
(24-hr)
CTHO
01 2O
cn^/6
£>l£(p
G^9
0359
01/0
o°tto
Meter
Volume,
liters (ft1)
WO .S3
99*J.*£
9993.^
9W.9T
?m,zi
8^^.10
yi^.13
qool.rz-
Rotameter
Setting
0,2.
O.2-
O,^
O.d
O.-z.
0.2.
O-t
6-2-
Dry Gas Meter
Temp. °C (°F)
W
-?/
^1
-75
-R
7C
TC
1^
Vacuum
(in. Hg)
(,
L,
Z
z
^5
?
z.
3>
Meter
Pressure
(in H20)
f
/
0.?
o,^
o.^
0.^
o.£"
0.?
-------
Pacific Environmental Services VOST Box Calibration
Date: 7-19-98
Vost Box Number: V-2
Bubble Meter
238.5 240.9
239.4 241.0
240.1 240.5
240.8
Average: 240.17
Bubble Meter
238.0 240.1
239.5 240.4
239.6 240.4
240.0
Average: 239.71
240.6 240.8
240.8 240.0
240.2 239.6
239.0
Average: 240.14
Flow Rate: 0.25 I/min
Rotameter Setting:
Bubble Meter Temp. :
Run 1
Meter Box
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Y=
Run 2
Meter Box
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Y=
Run 3
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Y=
0.2
91
8815.5
8822
103
102
102.5
27.3
233.228
1.0298
8822.5
8829
103
103
103
27.35
232.594
1.0306
882f.5
8836
104
104
104
27.3
232.6072273
1.0324
Average Y=
1.0309
-------
___
O PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Customer:
Facility; lA. (^ a (:&"*•"
* 7
Date: "I
Volatile Organic Sampling Train (VOST) Data Sheet
i**t ^- Project No.: 'ROl'2.. OQ I
City: LA. C^ /.' -A*-"* ."
*
Time :
Meter Box No.
Barometric Pressure, in. Ha:
Ambient Temperature, °F:
Pre-test:
Post-test
Sampling Location:,
Run Number: ^ —V—3
Meter Gamma (y) Pre:_
Operator: "PrY
Post:
Purge Time:
Leak Check Data
Vacuum, inches Hg
Initial
Aft to to {& /{j>/c>
;o
Final
JO 'O /a to jo/on
;c?
Time, min
f / ' 7-
Run Data
Sample
Time
(min)
Clock
Time
(24-hr)
Meter
Volume,
liters (ft3)
Rotameter
Setting
Dry Gas Meter
Temp. °C (°F)
Vacuum
Meter
Pressure
(in H20)
sA
l
0
0-8
. Uo
0-5
1
0-5
o
, \\
frz.
1 3.77
G.S
0
3 -ft)
o.s
0
/035
5
102 /.n
0.5
-------
Pacific Environmental Services VOST Box Calibration
Date: 7-19-98
Vost Box Number: V-2
Bubble Meter
499.9 498.7
500.9 501.3
498.9 499.8
500.2
Average: 499.96
Bubble Meter
500.2 500.0
501.0 499.8
500.8 499.6
499.8
Average: 500.17
500.0 500.9
500.6 500.7 '
501.0 500.1
499.5
Average: 500.40
Flow Rate: 0.5 1/min
Rotameter Setting:
Bubble Meter Temp. :
Run 1
Meter Box
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Y=
Run 2
Meter Box
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Y=
Run 3
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Vf
0.4'
91
8837
8852
104
104
104
27.6
530.951
0.9416
8852.25
8867.25
104
104
104
27.5
532.882
0.9386
8867.5
8882.75
105
104
104.5
27.6
539.322345
0.9278
Average Y=
0.9360
-------
PACIFIC ENVnONUENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
EPA Method 18 Adsorbent Tube Data Sheet
Plant
//' TU (L
Sampling Location: y//o T™"-1
Sampling Method Type:
Run Number J^-
Field Team Leader T/f
Concurrent Train ID:
DESCRIPTION OF TRAIN
Leg
B
Moisture Knockout
(if used, indicate type)
Tube a Description
I,
Tube b Description
Tube c Description
CALIBRATION - PRETEST
Leg
B
Volume (mL)
Temperature (°F)
Time (seconds)
Pbar (inches Hg)
RUN DATA
Elapsed Time
76 C
Clock Time
{50^
Leg A
Flow (L/min)
i
Vacuum (in Hg)
iO
/O
IL?
/O
/O
Le
Flow (L/min)
gB
Vacuum (in Hg)
/O
/o
IO
CALIBRATION - POST-TEST
Leg
B
Volume (mL)
Temperature (°F)V
Time (seconds)
I/O
Pbar (inches Hg)
P:\rO 12.00 l\misc\ml Ssheetdoc
/?
Va
-------
PACIFIC ENVIRONMENTAL SERVICES. MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, Norttl Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
^
EPA Method 18 Adsorbent Tube Data Sheet
Plant
Li'S.
Date:
Sampling Location:.
LL
CU4-
Sampling Method Type:.
Run Number 5ETO -
.Field Team Leader
- rP
Concurrent Train ID:
DESCRIPTION OF TRAIN
Leg
Moisture Knockout
(if used, indicate type)
o
Tube a Description
Tube b Description
Tube c Description
CALIBRATION - PRETEST
^ K-e-r.
Leg
B
Volume (mL)
6.
Temperature (°F)
Time (seconds)
LO
IflO
Pbar (inches Hg)
r.Lfo.
RUN DATA
Elapsed Time
o
/o
515
//O
•V
Clock Time
F?^
Leg A
Flow(Umin)
1
Vacuum (in Hg)
LegB
Flow (L/min)
Vacuum (in Hg)
/ r
CALIBRATION - POST-TEST
Leg
B
Volume (mL)
Temperattre (eF)
•^^^MH
Time (seconds)
1.0
Pbar (inches Hg)
P:\r012.001\misc\ml8sheeLdoc
-------
PACIFIC ENVIRONMENTAL SERVICES, MC
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Plant
EPA Method 18 Adsorbent Tube Data Sheet
r
Date:
Sampling Location:.
Sampling Method Type: m -
Run Number
Field Team Leader
Concurrent Train ID: DO
DESCRIPTION OF TRAIN
Leg
B
Moisture Knockout
(if used, indicate type)
Tube a Description
n<
Tube b Description
Tube c Description
CALIBRATION - PRETEST
Leg
Volume (mL)
Temperature (°F)
Time (seconds)
Pbar (inches Hg)
B
RUN DATA
Elapsed Time
cs
/O
20
2C>/^/
-4fcJ
Yf
ro
Clock Time
iO23>
/03.3
/042,
\
J/go
// *Z'fJrt43
(4. 4t
Leg A
Flow (L/min)
/
1
i
/
/
/
;
Vacuum (in Hg)
*6
i*
if
&
te
sS
15
Le
Flow (L/min)
(
i
i
/
/
/
/
gB
Vacuum (in Hg)
ft
'<
/r
/L5
-'S"
'<
'?
"-*-i
CALIBRATION-POST-TEST
Leg
B
Volume (mL)
Temperature (°F)
75-
Time (seconds)
U)
Pbar (inches Hg)
P:\rO 12.00 l\misc\ml Ssheetdoc
-------
APPENDIX C.3
METEOROLOGICAL DATA
-------
A meteorological (MET) monitoring station was positioned on top of the load-out tunnel, above
the entrance. The station monitored the wind speed, wind direction, and ambient temperature.
Readings from the MET station were recorded once per minute during the testing and downloaded to
a data acquisition system. Due to hardware problems, no data were collected on 7/24/98 (back-
ground condition testing). Ambient humidity was measured manually using a sling psychrometer
and recorded in field notebook. Table M.I below summarizes the meteorological data collected.
Figure M.I shows the position of the load-out tunnel and the MET station and the average wind
direction for each test day.
TABLE M.1
METEOROLOGICAL DATA SUMMARY
ASPHALT PLANT C, CALIFORNIA
Date
7/24/98
7/25/98
7/27/98
Time
Periods
0646-0700
0701-0800
0801-0812
0931-1000
1001-1100
1101-1200
1201-1300
Average
0548-0559
0600-0659
0700-0759
0800-0859
0900-0959
1000-1059
1100-1159
1200-1259
1300-1327
Average
0722-0759
0800-0859
0900-0959
1000-1059
1100-1159
1200-1202
Average
Wind Speed,
MPH
3.02
3.35
3.98
3.71
4.05
6.12
7.63
4.55
3.23
2.91
4.12
4.96
5.53
6.03
6.80
7.74
9.01
5.59
2.74
4.27
6.33
6.13
6.63
8.00
5.68
Ambient
Temperature
Degrees C
17.7
18.0
18.1
22.6
21.3
23.0
25.2
20.8
19.1
19.8
20.1
21.0
23.4
25.8
27.6
29.3
29.5
23.9
22.0
22.7
26.9
29.1
31.9
33.9
27.7
Wind
Direction,
Degrees*
173
184
151
228
224
233
219
202
281
218
262
225
206
219
213
206
204
226
135
213
231
223
219
198
203
Ambient
Relative
Humidity, %
90
60
75
77
61
69
70
70
* Degrees clockwise from north (e.g. 180° = wind from the south)
-------
Run 1
West
North
Run 2
South
East
Run 1 - Average wind direction on July 24,1998 (202°)
Run 2 - Average wind direction on July 25, 1998 (226°)
Run 3 - Average wind direction on July 27, 1998 (203°)
Figure M.1 Load-out Tunnel and MET Station Location and Average Wind Direction.
-------
Time
MPH
HOT MIX ASPHALT
LOS ANGELES - PLANT C
7-24-98
Direction (°)
0646-0700
0701-0800
0801-0812
0931-1000
1001-1100
1101-1200
1201-1300
3.0
3.4
4.0
3.7
4.1
6.1
7.6
17.7
18.0
18.1
22.6
21.3
23.0
25.2
173
184
151
228
224
233
219
-------
RAW Data
Time MPH °C Direction (°)
6:46:00 AM
6:47:00 AM
6:48:00 AM
6:49:00 AM
6:50:00 AM
6:51:00 AM
6:52:00 AM
6:53:00 AM
6:54:00 AM
6:55:00 AM
6:56:00 AM
6:57:00 AM
6:58:00 AM
6:59:00 AM
7:00:00 AM
7:01:00 AM
7:02:00 AM
7:03:00 AM
7:04:00 AM
7:05:00 AM
7:06:00 AM
7:07:00 AM
7:08:00 AM
7:09:00 AM
7: 10:00 AM
7: 11:00 AM
7:12:00 AM
7:13:00 AM
7:14:00 AM
7:15:00 AM
7:16:00 AM
7: 17:00 AM
7: 18:00 AM
7: 19:00 AM
7:20:00 AM
7:21 :00 AM
7:22:00 AM
7:23:00 AM
7:24:00 AM
7:25:00 AM
7:26:00 AM
7:27:00 AM
7:28:00 AM
7:29:00 AM
7:30:00 AM
7:31:00 AM
7:32:00 AM
2.5
4.5
3.2
2.5
2.6
3.3
3.6
4.1
2.6
2.0
1.6
2.4
3.4
3.3
3.7
2.9
2.8
3.5
2.8
3.0
3.4
3.5
3.1
2.5
2.8
3.0
2.4
3.1
4.1
4.1
4.0
2.6
3.4
3.3
3.2
2.8
3.8
3.1
2.9
4.0
3.8
3.2
3.1
2.5
3.2
2.7
2.6
10.8
18.0
18.3
18.4
18.4
18.3
18.2
18.2
18.1
18.2
18.2
18.3
18.1
18.2
18.0
18.1
18.2
18.1
18.1
18.2
18.1
18.1
18.0
18.0
18.0
18.0
18.0
18.0
17.9
17.9
17.9
17.9
17.9
17.9
18.0
18.1
17.9
18.0
18.2
18.1
18.1
18.1
18.1
18.3
18.3
18.1
18.1
99
139
120
130
160
191
168
158
173
142
210
221
229
232
228
206
231
229
232
226
211
207
200
161
150
151
162
158
149
129
132
171
199
206
211
220
234
216
208
205
207
226
221
206
208
200
211
Page 1 of 7
-------
(0
Q
§
CMCMCMCMCMCNCMCMCM
o o <<• h- o
•f CO CO CO CO
CO
CM O)
TJ- CO
S3
CD
ojrcoOTcocNooco
CMCM^-^-T-T-T-CM
f-
•5
CM
0>
O>
OOCNCMCMCMCMCMCM
rt
o o o o o o o
o o o o o o o
ooooooooooooooooooooooooooooooo
ooooooooooooooooooooooooooooooo
OOOOOOOOO
ppppppppO
liracbi^oo
co co co co
3
-------
RAW Data
9:39:00 AM
9:40:00 AM
9:4 1:00 AM
9:42:00 AM
9:43:00 AM
9:44:00 AM
9:45:00 AM
9:46:00 AM
9:47:00 AM
9:48:00 AM
9:49:00 AM
9:50:00 AM
9:51:00 AM
9:52:00 AM
9:53:00 AM
9:54:00 AM
9:55:00 AM
9:56:00 AM
9:57:00 AM
9:58:00 AM
9:59:00 AM
10:00:00 AM
10:01:00 AM
10:02:00 AM
10:03:00 AM
10:04:00 AM
10:05:00 AM
10:06:00 AM
10:07:00 AM
10:08:00 AM
10:09:00 AM
10: 10:00 AM
10:11:00 AM
10:12:00 AM
10: 13:00 AM
10:14:00 AM
10:15:00 AM
10: 16:00 AM
10: 17:00 AM
10: 18:00 AM
10: 19:00 AM
10:20:00 AM
10:21:00 AM
10:22:00 AM
10:23:00 AM
10:24:00 AM
10:25:00 AM
10:26:00 AM
10:27:00 AM
3.0
3.7
4.5
3.9
4.2
4.0
3.6
4.1
4.4
5.8
3.7
2.8
4.4
6.4
5.6
5.2
5.2
4.3
3.6
3.2
3.6
3.5
5.9
4.9
4.9
2.8
4.3
4.0
4.9
4.0
3.3
3.0
1.8
4.0
4.8
2.9
3.9
3.7
1.9
2.0
1.7
1.4
3.8
3.3
2.2
4.3
4.1
3.7
6.4
20.6
20.8
20.9
20.8
20.5
20.2
20.2
20.2
20.3
20.1
20.3
20.5
20.0
19.9
19.8
19.9
20.0
20.2
20.5
20.4
19.9
20.0
19.7
19.8
20.1
20.3
20.1
20.3
20.2
20.5
20.6
20.5
20.8
20.5
20.2
20.6
20.8
20.9
21.2
21.3
21.7
21.8
21.1
20.8
21.3
21.4
21.4
21.2
20.9
191
260
271
272
240
232
297
266
255
231
251
237
204
232
245
260
268
265
281
240
222
208
202
214
236
248
219
232
228
269
223
198
209
224
215
217
252
231
221
194
141
136
197
207
220
263
316
280
326
Page 3 of 7
-------
RAW Data
10:28:00 AM
10:29:00 AM
10:30:00 AM
10:31:00 AM
10:32:00 AM
10:33:00 AM
10:34:00 AM
10:35:00 AM
10:36:00 AM
10:37:00 AM
10:38:00 AM
10:39:00 AM
10:40:00 AM
10:41:00 AM
10:42:00 AM
10:43:00 AM
10:44:00 AM
10:45:00 AM
10:46:00 AM
10:47:00 AM
10:48:00 AM
10:49:00 AM
10:50:00 AM
10:51:00 AM
10:52:00 AM
10:53:00 AM
10:54:00 AM
10:55:00 AM
10:56:00 AM
10:57:00 AM
10:58:00 AM
10:59:00 AM
11:00:00 AM
11:01:00 AM
11:02:00 AM
11:03:00 AM
11:04:00 AM
11:05:00 AM
11:06:00 AM
11:07:00 AM
11:08:00 AM
11:09:00 AM
11:10:00 AM
11:11:00 AM
11:12:00 AM
11:13:00 AM
11:14:00 AM
11:15:00 AM
11:16:00 AM
5.4
2.0
1.5
2.7
6.3
5.3
3.1
3.1
2.6
3.3
5.2
6.3
4.8
6.0
3.7
5.5
4.7
5.4
4.5
5.1
4.1
4.3
5.7
3.1
5.6
5.4
5.1
3.8
3.9
3.3
4.0
6.6
3.9
6.0
7.9
6.7
5.1
4.0
4.4
4.7
4.4
6.4
5.0
6.1
4.5
3.9
5.8
4.2
7.5 -
21.1
21.5
21.9
22.0
22.0
22.0
21.9
22.0
22.4
22.4
21.5
21.1
21.1
21.1
21.4
21.5
22.1
21.6
21.6
21.4
21.4
21.6
21.7
22.6
21.9
21.7
21.5
21.5
22.0
22.7
22.6
21.8
22.2
22.0
21.8
22.2
22.7
22.4
22.1
22.2
22.4
22.5
23.2
23.1
22.8
23.3
23.2
23.5
22.2
310
165
134
220
312
315
285
312
300
258
234
211
205
152
215
255
237
224
209
186
170
213
223
274
230
198
181
192
174
144
195
187
172
204
227
270
255
192
201
189
223
244
255
256
229
206
253
212
199
Page 4 of 7
-------
.s
CD
Q
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a:
cvieDCMGOcocooom
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CMCMCMCMCMCMCMCMCMCMCMCMCMCMCMCMCMCMCMCMCNCMCMCMCMCMCMCMCMCMCMCMCMCMCMCMCMCMCNI
CM
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ooppppoppppppppppppppppppppppppppppp
^cXi^^in'eo^TOC^d'^cM^^ineor^^O)OOT— CMCO
CMCMCNCMCMCMCMCMCNcocococococococococo^^^^^^t^ri5;'i*^t"n«nin|n
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-------
RAW Data
12:06:00 PM
12:07:00 PM
12:08:00 PM
1 2:09:00 PM
12:10:00 PM
12:11:00 PM
12:12:00 PM
12:13:00 PM
12:14:00 PM
12:15:00 PM
12:16:00 PM
12:17:00 PM
12:18:00 PM
12:19:00 PM
1 2:20:00 PM
12:21:00 PM
12:22:00 PM
12:23:00 PM
12:24:00 PM
12:25:00 PM
1 2:26:00 PM
1 2:27:00 PM
12:28:00 PM
1 2:29:00 PM
12:30:00 PM
12:31:00 PM
1 2:32:00 PM
12:33:00 PM
1 2:34:00 PM
12:35:00 PM
12:36:00 PM
12:37:00 PM
12:38:00 PM
12:39:00 PM
12:40:00 PM
12:41:00 PM
12:42:00 PM
12:43:00 PM
1 2:44:00 PM
12:45:00 PM
12:46:00 PM
12:47:00 PM
12:48:00 PM
12:49:00 PM
12:50:00 PM
12:51:00 PM
12:52:00 PM
12:53:00 PM
12:54:00 PM
7.2
9.5
7.3
8.0
6.4
8.2
11.5
8.0
7.6
6.9
7.3
9.9
7.3
10.8
5.4
6.4
7.9
8.9
7.6
7.8
10.0
7.3
7.0
6.8
5.6
6.9
6.3
9.1
9.2
7.2
9.0
7.6
8.9
5.6
7.0
5.6
6.8
6.9
7.0
6.0
7.0
5.7
6.5
9.9
9.0
6.3
9.4
12.4
10.0
24.2
24.6
25.0
25.3
25.2
23.9
23.3
23.6
24.0
24.0
24.1
23.6
24.8
24.4
25.3
24.7
25.5
25.4
24.9
24.9
24.7
25.4
25.5
25.4
26.0
25.4
25.4
24.8
24.3
25.5
25.3
25.0
24.7
25.4
25.7
25.9
25.6
25.7
26.2
26.2
25.6
25.6
25.5
25.0
24.9
25.9
25.4
24.8
25.9
204
256
255
270
233
212
200
190
221
202
207
199
226
244
252
195
266
301
214
277
243
246
213
191
165
197
171
200
181
158
200
186
190
230
217
171
199
224
252
213
195
204
209
208
192
182
193
217
290
Page 6 of 7
-------
RAW Data
12:55:00 PM
12:56:00 PM
12:57:00 PM
12:58:00 PM
12:59:00 PM
1:00:00 PM
1:01:OOPM
1:02:00 PM
1:03:00 PM
1:04:00 PM
1:05:00 PM
1:06:00 PM
1:07:00 PM
1. -08:00 PM
1. -09:00 PM
1:10:00 PM
1:11:OOPM
1:12:00 PM
1:13:00 PM
1:14:00 PM
1:15:00 PM
1:16:00 PM
1:17:00 PM
1:18:00 PM
1:19:00 PM
1:20:00 PM
1:21:OOPM
1:22:00 PM
1:23:00 PM
1:24:00 PM
1:24:12 PM
5.5
7.9
8.5
6.0
5.0
9.5
9.6
9.1
8.1
7.4
8.1
7.9
7.4
8.5
7.2
4.5
8.1
9.8
10.9
7.9
9.0
6.0
6.6
7.3
3.6
-0.1
0.0
0.0
0.0
0.0
0:0
26.6
26.7
27.1
26.9
26.9
25.9
25.7
25.4
26.1
26.3
25.6
25.3
26.4
26.2
26.6
27.8
26.3
25.8
25.8
26.7
26.9
26.9
26.3
26.2
129.2
211.9
192.6
201.8
212.3
217.1
42.0
268
266
262
226
234
195
202
192
232
208
194
209
253
196
242
177
211
213
238
282
261
233
200
201
110
-1
-1
0
0
0
0
Page 7 of 7
-------
HOT MIX ASPHALT
LOS ANGELES - PLANT C
7-25-98
Time MPH °c Direction (°)
0548-0559 3.2 19.1 280.8
0600-0659 2.9 19.8 218.0
0700-0759 4.1 20.1 261.9
0800-0859 5.0 21.0 225.4
0900-0959 5.5 23.4 205.7
1000-1059 6.0 25.8 218.6
1100-1159 6.8 27.6 212.8
1200-1259 7.7 29.3 206.1
1300-1327 9.0 29.5 204.3
JffO
-------
Raw Data
Time MPH °C Direction (°)
5:48:00 AM 4.6 18.3 321
5:49:00 AM 3.4 18.4 318
5:50:00 AM 3.2 18.6 312
5:51:00 AM 3.6 18.8 309
5:52:00 AM 3.7 18.9 323
5:53:00 AM 4.2 19 322
5:54:00 AM 5.1 19 321
5:55:00 AM 2.5 19.1 198
5:56:00 AM 1.9 19.4 260
5:57:00 AM 3 19.6 260
5:58:00 AM 2 19.8 227
5:59:00 AM 1.6 19.7 199
6:00:00 AM 1.6 19.7 175
6:01:00 AM 2.8 19.9 264
6:02:00 AM 2.7 20 264
6:03:00 AM 3.8 19.6 293
6:04:00 AM 2.5 19.6 231
6:05:00 AM 2.8 19.8 256
6:06:00 AM 2.3 19.9 178
6:07:00 AM 1.9 19.9 141
6:08:00 AM 2.3 19.9 171
6:09:00 AM 3.2 19.9 168
6:10:00 AM 2.5 19.9 278
6:11:00 AM 2.7 20 237
6:12:00 AM 2.6 20 274
6:13:00 AM 2.1 20 282
6:14:00 AM 2.5 19.9 253
6:15:00 AM 2.4 20 225
6:16:00 AM 2.4 20 243
6:17:00 AM 2.5 20.1 198
6:18:00 AM 3.7 20.1 206
6:19:00 AM 3.9 20.1 198
6:20:00 AM 3.1 20 240
6:21:00 AM 3 20.1 269
6:22:00 AM 3.1 19.9 279
6:23:00 AM 2.3 19.9 209
6:24:00 AM 2.5 19.9 232
6:25:00 AM 4 19.6 299
6:26:00 AM 4.4 19.3 320
6:27:00 AM 2.8 19.3 286
6:28:00 AM 3.1 19.2 291
6:29:00 AM 2.7 19.4 194
6:30:00 AM 4.1 19.5 165
6:31:00 AM 3.2 19.7 163
6:32:00 AM 5.5 19.7 140
6:33:00 AM 4.9 19.8 104
6:34:00 AM 5 19.6 64
6:35:00 AM 3.2 19.6 153
Page 2 of 11
-------
Raw Data
6:36:00 AM 2.6 19.8 172
6:37:00 AM 2.4 19.9 166
6:38:00 AM 2.2 19.9 236
6:39:00 AM 2.8 19.7 309
6:40:00 AM 2.3 19.9 248
6:41:00 AM 1.7 19.9 235
6:42:00 AM 2.3 19.9 289
6:43:00 AM 4 19.7 275
6:44:00 AM 3.7 19.7 188
6:45:00 AM 4.3 19.7 51
6:46:00 AM 2.5 19.8 301
6:47:00 AM 1.8 19.7 151
6:48:00 AM 2.3 19.6 85
6:49:00 AM 1.4 19.8 178
6:50:00 AM 2.5 19.8 265
6:51:00 AM 2.8 19.7 291
6:52:00 AM 1.9 19.8 114
6:53:00 AM 3.2 19.8 310
6:54:00 AM 3.9 19.7 321
6:55:00 AM 3.7 19.8 297
6:56:00 AM 2.6 19.9 138
6:57:00 AM 2.5 20 94
6:58:00 AM 2.4 20.1 155
6:59:00 AM 2.6 20.3 270
7:00:00 AM 3.4 20 287
7:01:00 AM 3.1 20 272
7:02:00 AM 3.5 19.9 272
7:03:00 AM 3.9 19.9 312
7:04:00 AM 2.8 19.9 280
7:05:00 AM 2.2 19.9 261
7:06:00 AM 3.3 19.7 241
7:07:00 AM 4.2 19.7 288
7:08:00 AM 3.3 19.7 296
7:09:00 AM 5.4 19.9 296
7:10:00 AM 5.2 19.8 272
7:11:00 AM 5.5 19.6 258
7:12:00 AM 5.6 19.6 281
7:13:00 AM 4.8 19.6 270
7:14:00 AM 5.7 19.7 284
7:15:00 AM 4.4 19.8 284
7:16:00 AM 5.4 19.9 282
7:17:00 AM 5.3 19.8 295
7:18:00 AM 4.6 19.9 290
7:19:00 AM 3.4 19.8 267
7:20:00 AM 4.7 19.9 261
7:21:00 AM 3.8 19.8 276
7:22:00 AM 4.1 20 300
7:23:00 AM 4.2 20 286
7:24:00 AM 3.7 19.9 259
Page 3 of 11
-------
Raw Data
7:25:00 AM 3 20 274
7:26:00 AM 3.2 20.1 260
7:27:00 AM 5.5 19.9 313
7:28:00 AM 3.5 19.8 314
7:29:00 AM 2.6 19.8 272
7:30:00 AM 5.5 19.6 237
7:31:00 AM 5.2 19.8 271
7:32:00 AM 4.8 19.9 289
7:33:00 AM 4.2 20.1 288
7:34:00 AM 3.9 20.1 266
7:35:00 AM 4.1 20 271
7:36:00 AM 3.2 20.1 280
7:37:00 AM 4.2 20.1 299
7:38:00 AM 3.8 20.1 311
7:39:00 AM 6.2 20.1 289
7:40:00 AM 4.8 20.2 282
7:41:00 AM 4.5 20.2 265
7:42:00 AM 4.2 20 230
7:43:00 AM 5.1 19.9 232
7:44:00 AM 3.4 20 238
7:45:00 AM 4 20 223
7:46:00 AM 5 20.1 234
7:47:00 AM 5.2 19.9 244
7:48:00 AM 4.2 20 230
7:49:00 AM 4.1 20.2 261
7:50:00 AM 4.2 20.3 234
7:51:00 AM 3.8 20.3 253
7:52:00 AM 2.3 20.6 195
7:53:00 AM 1.8 20.9 111
7:54:00 AM 3.4 20.8 57
7:55:00 AM 2.1 21 161
7:56:00 AM 3.5 21.2 310
7:57:00 AM 4.4 21 253
7:58:00 AM 4.3 20.8 249
7:59:00 AM 4.4 20.7 248
8:00:00 AM 3.4 20.6 250
8:01:00 AM 4.8 20.8 265
8:02:00 AM 3.1 20.7 258
8:03:00 AM 3.7 21 290
8:04:00 AM 4 21.1 261
8:05:00 AM 5.2 20.6 253
8:06:00 AM 3.4 20.8 242
8:07:00 AM 3.2 20.7 215
8:08:00 AM 5.4 20.7 242
8:09:00 AM 5.3 20.5 244
8:10:00 AM 5.2 20.8 231
8:11:00 AM 4.9 20.5 259
8:12:00 AM 6.9 20.6 249
8:13:00 AM 6.1 20.4 239
Page 4 of 11
-------
Raw Data
8:14:00 AM 6.3 20.4 243
8:15:00 AM 6.6 20 235
8:16:00 AM 6.1 20.2 249
8:17:00 AM 4.8 20.6 265
8:18:00 AM 3.4 20.9 263
8:19:00 AM 3.3 20.9 203
8:20:00 AM 4.8 20.6 212
8:21:00 AM 3.5 20.8 235
8:22:00 AM 4 21.1 236
8:23:00 AM 5.3 21.1 209
8:24:00 AM 4.3 21 198
8:25:00 AM 3.8 20.9 204
8:26:00 AM 4.5 20.8 218
8:27:00 AM 4.6 20.7 196
8:28:00 AM 5.8 20.5 200
8:29:00 AM 5.8 20.6 216
8:30:00 AM 6.6 20.7 265
8:31:00 AM 7.3 20.5 260
8:32:00 AM 6.5 20.5 249
8:33:00 AM 6.8 20.4 259
8:34:00 AM 5.6 20.5 232
8:35:00 AM 5.3 20.5 208
8:36:00 AM 5.8 20.2 230
8:37:00 AM 5.6 20.2 205
8:38:00 AM 5.6 20.3 218
8:39:00 AM 4.8 20.4 204
8:40:00 AM 5.2 20.2 184
8:41:00 AM 3.8 20.4 178
8:42:00 AM 5 20.4 181
8:43:00 AM 4 20.8 174
8:44:00 AM 5.5 21 192
8:45:00 AM 4.4 21.5 172
8:46:00 AM 6.5 21.9 128
8:47:00 AM 5 22.6 132
8:48:00 AM 3.9 22.6 161
8:49:00 AM 2.5 23.1 172
8:50:00 AM 4.1 22.6 250
8:51:00 AM 6.4 22.5 292
8:52:00 AM 5.3 22.1 239
8:53:00 AM 6.4 21.7 238
8:54:00 AM 5.9 21.8 253
8:55:00 AM 4.6 22.6 256
8:56:00 AM 2.5 22.7 222
8:57:00 AM 4.9 21.7 215
8:58:00 AM 5.8 21.5 235
8:59:00 AM 4.4 22.1 242
9:00:00 AM 3.8 22.4 237
9:01:00 AM 3.8 22 172
9:02:00 AM 3 22.4 186
Page 5 of 11
-------
O CM O
CM CM CM
£
CO
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CO
a:
CMCMCM
CMCNCNCMCM
CMCMCM
CNC^CMCMCvlCMCslCsl
cqOTCDr^cDcq
c>ic>ic>i<>icN
CNICNCMCNCMCMCMCMCMCMCMCNCM CMCMCMCMCMCMCMCMCM
O
CO
0)
O)
CO
a.
CM
co co
co' in CM
10 cd
cc
CD ui
cd oo'
oS
c 10
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ooooooooooooooooooooooooooooooooooooooooooooooooo
000000000000000,00000000000000000000
co^ib'cbt^wroo'^cN'co^ib'cbf^raroo^cN'co^iocb
OOOOOOOTT-T-T-T-T-r-T--r-CNCNCNCNeNtN
-------
Raw Data
9:52:00 AM 6.7 24.5 221
9:53:00 AM 5.4 24.3 219
9:54:00 AM 6.9 24.2 236
9:55:00 AM 5.5 24.5 249
9:56:00 AM 6.8 24.5 217
9:57:00 AM 7.1 23.9 210
9:58:00 AM 5 23.9 209
9:59:00 AM 6.2 24 198
10:00:00 AM 4.5 24.7 224
10:01:00 AM 6.9 24.2 193
10:02:00 AM 6.7 24 221
10:03:00 AM 5.4 24.4 220
10:04:00 AM 4 24.9 257
10:05:00 AM 4 25.5 219
10:06:00 AM 6.8 24.2 189
10:07:00 AM 3.4 24.7 205
10:08:00 AM 7.4 24.5 215
10:09:00 AM 7.9 24.9 250
10:10:00 AM 6.8 24.7 244
10:11:00 AM 5.9 24.6 226
10:12:00 AM 6.1 25.1 253
10:13:00 AM 5.4 24.8 179
10:14:00 AM 4 25.4 212
10:15:00 AM 5.2 25.1 216
10:16:00 AM 6.1 25.6 277
10:17:00 AM 3.2 26.5 208
10:18:00 AM 4.2 26.2 186
10:19:00 AM 6.2 25 203
10:20:00 AM 5.9 24.8 204
10:21:00 AM 5.3 24.9 226
10:22:00 AM 4.5 25.8 228
10:23:00 AM 6.3 24.9 220
10:24:00 AM 8.5 25 218
10:25:00 AM 8.5 23.9 190
10:26:00 AM 5.8 25 173
10:27:00 AM 8.7 23.5 193
10:28:00 AM 5.8 24.8 180
10:29:00 AM 6.8 26 200
10:30:00 AM 7.5 26.1 199
10:31:00 AM 5.4 27 206
10:32:00 AM 8 26.6 207
10:33:00 AM 7.3 26.6 213
10:34:00 AM 5.6 26.6 198
10:35:00 AM 5.3 26.7 192
10:36:00 AM 6.5 .26.5 206
10:37:00 AM 9 26.4 235
10:38:00 AM 7.6 27 265
10:39:00 AM 6.4 26.6 266
10:40:00 AM 4.2 26.8 244
Page 7 of 11
-------
Raw Data
10:41:00 AM 8.1 26.2 202
10:42:00 AM 6.2 25.8 207
10:43:00 AM 6.1 25.9 203
10:44:00 AM 6.7 25.8 204
10:45:00 AM 8.5 26.2 243
10:46:00 AM 4.1 27.4 274
10:47:00 AM 5.8 26.8 206
10:48:00 AM 7.3 25.6 187
10:49:00 AM 5 25.9 191
10:50:00 AM 5.8 26 205
10:51:00 AM 6.5 26 202
10:52:00 AM 7.4 25.7 191
10:53:00 AM 5.1 26.1 191
10:54:00 AM 2.7 27.9 178
10:55:00 AM 3.8 28.5 263
10:56:00 AM 7.2 27.4 306
10:57:00 AM 5.4 27.4 255
10:58:00 AM 5.6 27.8 275
10:59:00 AM 5.6 28.3 273
11:00:00 AM 3.6 27.8 282
11:01:00 AM 5.9 26.7 216
11:02:00 AM 6.7 26.1 206
11:03:00 AM 8.1 25.5 186
11:04:00 AM 6.2 26.8 161
11:05:00 AM 6.7 27.1 232
11-.06:00 AM 5.8 27 232
11:07:00 AM 4.6 27.1 227
11:08:00 AM 6.4 26.8 229
11:09:00 AM 6.6 26.5 216
11:10:00 AM 4.2 26.7 198
11:11:00 AM 6.7 27.1 231
11:12:00 AM 6 26.8 199
11:13:00 AM 6.1 27 218
11:14:00 AM 8.4 26.3 204
11:15:00 AM 9.4 26.8 244
11:16:00 AM 7.5 27.2 239
11:17:00 AM 7.7 26.6 200
11:18:00 AM 6.1 26.6 198
11:19:00 AM 6.3 27.2 193
11:20:00 AM 8.2 26.5 191
11:21:00 AM 8.2 26.5 204
11:22:00 AM 5.7 27.4 221
11:23:00 AM 7.4 28 249
11:24:00 AM 5.2 28.5 231
11:25:00 AM 5.7 28.1 197
11:26:00 AM 7.7 27.7 212
11:27:00 AM 8.1 27.1 195
11:28:00 AM 9.6 27.2 230
11:29:00 AM 7.2 28.1 251
Page 8 of 11
-------
Raw Data
11:30:00 AM
11:31:00 AM
11:32:00 AM
11:33:00 AM
11:34:00 AM
11:35:00 AM
11:36:00 AM
11:37:00 AM
11:38:00 AM
11:39:00 AM
11:40:00 AM
11:41:00 AM
11:42:00 AM
11:43:00 AM
11:44:00 AM
11:45:00 AM
11:46:00 AM
11:47:00 AM
11-.48:00 AM
11:49:00 AM
11:50:00 AM
11:51:00 AM
11-.52:00 AM
11:53:00 AM
11:54:00 AM
11:55:00 AM
11:56:00 AM
11:57:00 AM
11:58:00 AM
11:59:00 AM
12:00:00 PM
12:01:00 PM
12:02:00 PM
12:03:00 PM
12:04:00 PM
12:05:00 PM
12:06:00 PM
12:07:00 PM
12:08:00 PM
12:09:00 PM
12:10:00 PM
12:11:00 PM
12:12:00 PM
12:13:00 PM
12:14:00 PM
12:15:00 PM
12:16:00 PM
12:17:00 PM
12:18:00 PM
6.2
4.7
7.8
10.3
5.9
6.9
6.1
6.9
10
7.6
5.9
4.2
7.3
6.3
5.6
6.4
5.4
8.4
7.1
7.6
8.1
6.4
6.3
7.7
7.7
7.7
5.4
7.5
7.8
4.6
4.5
4
8
7
4.9
6.6
6.8
7.5
6.1
7.6
6.5
8.4
6.9
7.5
5.5
5.9
8.3
6.9
7.3
28.2
28.9
27.5
27.9
28.4
28.1
27.7
27.6
27.1
27.5
28.2
29.2
27.9
27.7
28.6
28.2
28.4
28.2
27.9
28.2
28.5
28.3
28.6
28.3
27.8
27.8
28.4
28.4
28
29.1
29.4
29.5
28.6
28.2
29.1
28.7
28.6
28.5
28.8
28.7
28.8
28.5
28.4
28.5
28.8
29.4
29.2
28.7
29
265
223
210
246
259
225
211
185
185
206
222
210
194
185
186
208
196
191
235
225
233
210
206
163
197
203
211
217
185
182
236
191
205
217
187
206
193
206
203
212
195
233
193
192
216
208
219
198
206
JOB
Page 9 of 11
-------
Raw Data
12:19:00 PM
12:20:00 PM
12:21:00 PM
12:22:00 PM
12:23:00 PM
12:24:00 PM
12:25:00 PM
12:26:00 PM
12:27:00 PM
12:28:00 PM
12:29:00 PM
12:30:00 PM
12:31:00 PM
12:32:00 PM
12:33:00 PM
12:34:00 PM
12:35:00 PM
12:36:00 PM
12:37:00 PM
12:38:00 PM
12:39:00 PM
12:40:00 PM
12:41:00 PM
12:42:00 PM
12:43:00 PM
12:44:00 PM
12:45:00 PM
12:46:00 PM
12:47:00 PM
12:48:00 PM
12:49:00 PM
12:50:00 PM
12:51:00 PM
12:52:00 PM
12:53:00 PM
12:54:00 PM
12:55:00 PM
12:56:00 PM
12:57:00 PM
12:58:00 PM
12:59:00 PM
1:00:00 PM
1:01:OOPM
1:02:00 PM
1:03:00 PM
1:04:00 PM
1:05:00 PM
1:06:00 PM
1:07:00 PM
7.1
7
8.7
7.3
6.2
8
8.4
7.8
7.6
5.4
8.9
7.6
8,5
9.6
8.6
8.3
8.1
7.6
7.5
10.2
9.6
9.8
5.6
9.2
8.3
7.8
7.9
7.2
9.4
7.9
9.9
9
6.9
8.9
7.9
8.6
9.1
8.6
9.6
8.7
9.7
8.1
7.6
9.1
8.6
9.4
9.6
11.8
7.5
29
29
29.1
29.4
30.1
29.7
30.3
30.5
29.6
30.1
29.5
29
29.2
28.6
28.9
28.7
29.1
29.6
29.9
29.6
29
29.3
30.3
29.7
29.3
29.5
29.6
30
29.4
29.8
29.4
29.8
29.9
29.3
29.7
29.8
30
29.9
30.1
29.8
29.4
29.8
30
29.3
30.1
29.3
29.6
29
29.6
206
194
194
246
243
221
253
252
236
244
210
210
222
199
189
196
165
188
195
165
186
209
203
195
192
191
200
180
194
182
223
213
213
195
184
195
218
231
227
201
189
222
216
207
186
200
206
198
215
to?
Page 10 of 11
-------
Raw Data
1:08:00 PM
1:09:00 PM
1:10:OOPM
1:11:00 PM
1: 12:00 PM
1:13:00 PM
1:14:00 PM
1:15:00 PM
1:16:00 PM
1:1 7:00 PM
1:18:00 PM
1:1 9:00 PM
1:20:00 PM
1:21:OOPM
1:22:00 PM
1 -.23:00 PM
1:24:00 PM
1:25:00 PM
1:26:00 PM
1:27:00 PM
1:27:00 PM
8.9
9.4
7.9
9.1
10.7
8.3
9.5
10.9
6.8
7
7.7
8.8
10.2
9.5
10.8
9.3
9.3
7.7
8.5
10.2
9.2
29.4
29.2
29.2
29.3
29
29.7
29.6
28.8
29.7
30
30.1
29.9
29.6
29.6
29.3
29.6
28.8
29.3
29.4
29.1
29.1
211
211
190
215
194
178
216
192
172
205
236
205
192
219
235
231
193
199
198
190
192
Page 11 of 11
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HOT MIX ASPHALT
LOS ANGELES - PLANT C
7-27-98
Time MPH °C Direction (°)
0722-0759
0800-0859
0900-0959
1000-1059
1100-1159
1200-1202
2.7
4.3
6.3
6.1
6.6
8.0
22.0
22.7
26.9
29.1
31.9
33.9
135
213
231
223
219
198
-------
Raw Data
Time MPH °c Direction (°)
7:22:00 AM 2.0 20.3 128
7:23:00 AM 2.0 20.2 125
7:24:00 AM 2.0 20.3 196
7:25:00 AM 2.0 20.7 112
7:26:00 AM 2.0 20.9 181
7:27:00 AM 2.0 21.0 196
7:28:00 AM 3.0 20.5 187
7:29:00 AM 3.0 21.1 116
7:30:00 AM 3.0 21.7 116
7:31:00 AM 3.0 22.0 73
7:32:00 AM 2.0 22.2 135
7:33:00 AM 2.0 22.7 176
7:34:00 AM 2.0 22.9 117
7:35:00 AM 2.0 23.1 92
7:36:00 AM 3.0 23.3 121
7:37:00 AM 3.0 23.5 66
7:38:00 AM 2.0 24.0 79
7:39:00 AM 3.0 24.1 108
7:40:00 AM 3.0 24.2 79
7:41:00 AM 3.0 24.4 68
7:42:00 AM 3.0 24.1 80
7:43:00 AM 3.0 23.7 66
7:44:00 AM 3.0 22.6 59
7:45:00 AM 3.0 21.5 98
7:46:00 AM 3.0 21.0 71
7:47:00 AM 2.0 21.0 188
7:48:00 AM 2.0 20.9 155
7:49:00 AM 2.0 20.7 167
7:50:00 AM 2.0 20.4 135
7:51:00 AM 3.0 20.9 108
7:52:00 AM 4.0 21.2 142
7:53:00 AM 4.0 21.2 153
7:54:00 AM 3.0 21.5 170
7:55:00 AM 3.0 21.7 204
7:56:00 AM 3.0 22.1 219
7:57:00 AM 4.0 22.3 220
7:58:00 AM 4.0 22.3 211
7:59:00 AM 4.0 22.2 207
8:00:00 AM 4.0 22.5 210
8:01:00 AM 4.0 22.3 202
8:02:00 AM 4.0 22.4 204
8:03:00 AM 4.0 22.6 203
8:04:00 AM 4.0 22.6 204
8:05:00 AM 4.0 22.6 201
8:06:00 AM 4.0 23.0 205
8:07:00 AM 4.0 22.7 197
8:08:00 AM 4.0 23.0 195
8:09:00 AM 5.0 23.0 195
Page 2 of 7
-------
Raw Data
8:10:00 AM 5.0 23.0 201
8:11:00 AM 5.0 23.1 206
8:12:00 AM 4.0 23.3 217
8:13:00 AM 4.0 23.4 204
8:14:00 AM 5.0 23.1 202
8:15:00 AM 5.0 23.0 205
8:16:00 AM 5.0 22.9 214
8:17:00 AM 4.0 21.9 201
8:18:00 AM 5.0 21.0 203
8:19:00 AM 5.0 19.8 196
8:20:00 AM 4.0 19.7 198
8:21:00 AM 4.0 19.9 195
8:22:00 AM 4.0 19.7 198
8:23:00 AM 3.0 19.5 212
8:24:00 AM 3.0 19.8 205
8:25:00 AM 4.0 20.8 219
8:26:00 AM 4.0 21.6 204
8:27:00 AM 3.0 22.0 191
8:28:00 AM 4.0 22.1 188
8:29:00 AM 4.0 22.5 201
8:30:00 AM 4.0 22.7 199
8:31:00 AM 3.0 23.1 214
8:32:00 AM 3.0 23.9 218
8:33:00 AM 4.0 24.0 211
8:34:00 AM 4.0 24.1 227
8:35:00 AM 4.0 24.5 237
8:36:00 AM 4.0 24.4 217
8:37:00 AM 6.0 23.8 199
8:38:00 AM 4.0 24.0 207
8:39:00 AM 4.0 24.1 193
8:40:00 AM 4.0 24.5 206
8:41:00 AM 4.0 25.0 236
8:42:00 AM 5.0 25.0 257
8:43:00 AM 4.0 25.8 272
8:44:00 AM 4.0 25.4 213
8:45:00 AM 4.0 24.7 211
8:46:00 AM 4.0 23.7 232
8:47:00 AM 4.0 23.6 230
8:48:00 AM 4.0 23.0 224
8:49:00 AM 4.0 22.5 230
8:50:00 AM 5.0 21.7 218
8:51:00 AM 5.0 21.1 216
8:52:00 AM 4.0 21.7 251
8:53:00 AM 5.0 21.4 208
8:54:00 AM 4.0 21.5 219
8:55:00 AM 5.0 21.3 201
8:56:00 AM 5.0 21.1 227
8:57:00 AM 5.0 21.5 224
8:58:00 AM 6.0 23.1 244
Page 3 of 7
-------
Raw Data
8:59:00 AM 6.0 24.1 262
9:00:00 AM 4.0 25.1 255
9:01:00 AM 5.0 24.6 205
9:02:00 AM 6.0 24.9 199
9:03:00 AM 7.0 24.8 240
9:04:00 AM 7.0 25.1 258
9:05:00 AM 6.0 24.8 232
9:06:00 AM 6.0 24.9 251
9:07:00 AM 6.0 25.1 230
9:08:00 AM 7.0 25.2 183
9:09:00 AM 6.0 25.4 211
9:10:00 AM 5.0 25.6 261
9:11:00 AM 7.0 25.0 230
9:12:00 AM 7.0 25.3 247
9:13:00 AM 6.0 25.9 244
9:14:00 AM 6.0 25.9 231
9:15:00 AM 7.0 26.3 229
9:16:00 AM 7.0 26.9 261
9:17:00 AM 6.0 27.2 260
9:18:00 AM 5.0 27.1 217
9:19:00 AM 5.0 27.3 237
9:20:00 AM • 5.0 27.3 235
9:21:00 AM 7.0 27.3 234
9:22:00 AM 6.0 27.3 237
9:23:00 AM 6.0 27.3 232
9:24:00 AM 6.0 27.4 236
9:25:00 AM 5.0 27.7 232
9:26:00 AM 6.0 27.6 240
9:27:00 AM 7.0 27.6 242
9:28:00 AM 7.0 27.4 247
9:29:00 AM 7.0 27.7 261
9:30:00 AM 7.0 27.7 243
9:31:00 AM 7.0 27.5 252
9:32:00 AM 6.0 27.4 254
9:33:00 AM 6.0 27.8 237
9:34:00 AM 7.0 27.3 225
9:35:00 AM 7.0 27.4 230
9:36:00 AM 7.0 27.5 235
9:37:00 AM 8.0 27.5 243
9:38:00 AM 6.0 27.9 254
9:39:00 AM 7.0 27.8 247
9:40:00 AM 6.0 27.4 240
9:41:00 AM 8.0 28.0 245
9:42:00 AM 6.0 27.6 239
9:43:00 AM 6.0 27.2 210
9:44:00 AM 7.0 27.1 208
9:45:00 AM 5.0 27.5 218
9:46:00 AM 8.0 27.1 200
9:47:00 AM 6.0 27.3 208
l/f
Page 4 of 7
-------
Raw Data
9:48:00 AM 7.0 27.2 204
9:49:00 AM 6.0 27.8 218
9:50:00 AM 7.0 27.5 200
9:51:00 AM 7.0 27.3 202
9:52:00 AM 5.0 28.2 212
9:53:00 AM 5.0 28.3 223
9:54:00 AM 7.0 27.7 214
9:55:00 AM 7.0 27.9 222
9:56:00 AM 6.0 28.4 234
9:57:00 AM 7.0 27.8 200
9:58:00 AM 7.0 27.9 227
9:59:00 AM 6.0 28.4 257
10:00:00 AM 8.0 28.5 • 259
10:01:00 AM 7.0 28.5 226
10:02:00 AM 6.0 27.6 209
10:03:00 AM 7.0 28.4 225
10:04:00 AM 7.0 28.6 245
10:05:00 AM 6.0 28.0 231
10:06:00 AM 6.0 27.9 237
10:07:00 AM 6.0 27.7 269
10:08:00 AM 7.0 27.6 255
10:09:00 AM 7.0 27.0 255
10:10:00 AM 8.0 27.4 262
10:11:00 AM 7.0 27.5 219
10:12:00 AM 7.0 28.5 258
10:13:00 AM 6.0 29.1 236
10:14:00 AM 6.0 29.0 232
10:15:00 AM 8.0 28.9 223
10:16:00 AM 6.0 29.3 229
10:17:00 AM . 7.0 29.4 236
10:18:00 AM 7.0 29.3 239
10:19:00 AM 6.0 29.1 260
10:20:00 AM 6.0 30.4 221
10:21:00 AM 8.0 30.3 218
10:22:00 AM 9.0 29.7 211
10:23:00 AM 6.0 30.2 209
10:24:00 AM 7.0 30.3 229
10:25:00 AM 7.0 29.4 235
10:26:00 AM 6.0 28.9 240
10:27:00 AM 5.0 28.9 223
10:28:00 AM 6.0 28.8 239
10:29:00 AM 7.0 28.7 226
10:30:00 AM 7.0 29.0 235
10:31:00 AM 6.0 28.9 213
10:32:00 AM 4.0 29.3 210
10:33:00 AM 3.0 30.3 245
10:34:00 AM 4.0 30.9 255
10:35:00 AM 4.0 30.5 211
10:36:00 AM 6.0 29.5 146
Page 5 of 7
-------
m to
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CD (N O O CO
o> o> o)oo)Oo>ooooooooT— cNOOJOOT— T— CNJ^~I«~OO
c>4C\ieNiCNiesiCNiCNje\icocNicoc\icorococococNirococococ\icococococococococo
cocorocococococowSro
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0000000000000000000000000000000000000000000000000
cocDi^i^cbr^cD(Di^od(Dinr^^^^^K
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0>ICMCMCMCMCMCMl
-------
APPENDIX C.4
ON-SITE GC/MS REPORT AND DATA
-------
EMISSION MONITORING
INC.
EFFECTIVE SOLUTIONS AND ADVANCED TECHNOLOGIES
DIRECT INTERFACE GCMS TESTING
TUNNEL EXHAUST DUCT
SILO EXHAUST DUCT
Prepared Under Subcontract to:
Pacific Environmental Services
Subcontract NO. 68-D-98-004-FP-002
U.S. EPA Contract NO. 68-D-98-004
Prepared for:
Mr. John T. Chehaske
Program Manager
And
Mr. Frank J. Phoenix
Project Manager
Pacific Environmental Services, Inc.
560 Herndon Parkway, Suite 200
Herndon, VA 20170-5240
Prepared by:
Laura L. Kinner Ph.D. and James W. Peeler
Emission Monitoring Incorporated
8901 Glenwood Ave.
Raleigh, NC 27612
, o 8901 GLENWOOD AVENUE • RALEIGH. NC 27612-7503 • PHONE (919) 781-3824 • FAX (919) 782-9476
-------
TABLE OF CONTENTS
SECTION PAGE*
1.0 INTRODUCTION.
2.0 SUMMARY OF TEST RESULTS
2.1 Tunnel Exhaust Duct 2
2.2 Silo Exhaust Duct 3
3.0 PROCESS DESCRIPTION 8
4.0 SAMPLING LOCATIONS 8
5.0 SAMPLING AND ANALYTICAL PROCEDURES 12
6.0 QUALITY ASSURANCE/QUALITY CONTROL 18
7.0 CONCLUSIONS AND RECOMMENDATIONS 23
APPENDICES
APPENDIX A DIRECT INTERFACE GCMS TEST METHOD
MANUFACTURERS CERTIFICATES OF ANALYSIS
APPENDDCB THREE POINT CALIBRATION RAW DATA
APPENDDC C SELECTED EXAMPLE FIELD DATA
-------
LIST OF TABLES
TABLE PAGE#
Table 2-1 Direct Interface and Tedlar Bag Sample Results - Tunnel Exhaust Duct 4
Table 2-2 Hot Mix Load Out Tedlar Bag Sample Results - Tunnel Exhaust Duct 5
Table 2-3 Direct Interface GCMS Results - Silo Exhaust Duct 6
Table 2-4 Direct Interface GCMS Results - Silo Exhaust Duct (Compounds Not In Calibration Library)...?
Table 6-1 GCMS Three-Point Calibration Results and Estimated Detection Limits 19
Table 6-2 Daily System Continuing Calibration Check Results 7-23-98 20
Table 6-3 Daily System Continuing Calibration Check Results 7-24-98 21
Table 6-4 Daily System Continuing Calibration Check Results 7-25-98 22
LIST OF FIGURES
FIGURE PAGE*
Figure 3-1 Process Air Flow Schematic 9
Figure 4-1 Tunnel Exhaust Duct Sampling Location 10
Figure 4-2 Silo Exhaust Duct Sampling Location 11
Figure 5-1 Ambient Direct Interface Sampling System Schematic 13
Figure 5-2 High Moisture Direct Interface Sampling System Schematic 14
Figure 5-3 Direct Interface GCMS Method Operational Flowchart 17
-------
DISCLAIMER
This report presents the results of direct interface GCMS testing conducted at the "hot mix" load out tunnel
exhaust duct, and asphalt silo storage exhaust ducu
Concentration results only are presented.
This document was prepared by Emission Monitoring Incorporated (EMI) under Pacific Environmental
Services Incorporated (PES) Subcontract NO. 68-D-98-004-FP-002 and EPA Contract NO. 68-D-98-004.
It has undergone the internal QA policies of EMI. The contents do not necessarily reflect the views and
policies of the EPA. and mention of trade names does not constitute endorsement by the EPA or by EMI.
111
-------
1.0 INTRODUCTION
The United States Environmental Protection Agency (U.S. EPA) requested use of a portable gas
chromatograph-mass spectrometer based analyzer (flAPSITE™) to iflentiry*and quantify volatilcttrganic
hazardous air pollutants from various emissions points at the 4MHMMHIHMBMHIV
MHHBM- The EPA requested specifically that the instrumentation be operated in the fully portable
mode, without use of a heated extractive sampling system, so that the test locations could be accessed
quickly and easily.
The GCMS instrumentation was developed by Leybold-Inficon. and has been evaluated extensively by
Emission Monitoring Incorporated (EMI)1. Numerous industrial stationary sources have been tested using
this instrumentation in accordance with the method entitled "Determination of Gaseous Organic
Compounds by Direct Interface GCMS". This method was developed by EMI and Inficon and has been
accepted by the U.S. EPA as an alternate test method for numerous stationary sources (ALT-017). and as a
conditional test method (CTM-28). The method and documentation are available on-line from the EPA
Website, and a copy of the method is provided in Appendix A.
Pacific Environmental Services (PES) subcontracted EMI to perform direct interface GCMS testing at the
hot mix asphalt truck loading tunnel, and at the asphalt silo storage vent at flflHHHHfll While
on-site, EMI was asked to conduct additional testing at the aggregate dryer baghouse stack and at the exit
of the load out tunnel. The results from testing performed at the aggregate dryer baghouse stack are
presented in a separate report. The primary objective of the testing was to characterize and quantify nine
specific volatile organic hazardous air pollutants (benzene, toluene, o,m,p-xylenes, styrene. ethyl benzene.
1,3-butadiene, and hexane) from each source tested. EMI focused the testing for these nine specific
analytes in addition to those identified in Section 1 of the Method, because previous testing indicated these
compounds to be present at measurable concentrations.
Two separate portable sampling systems were used during this testing effort. One sampling system
employed an unheated stainless steel probe, 0.3 micron quartz fiber filter. Teflon-head diaphragm pump,
and Teflon tubing to convey sample gas to the GCMS instrumentation. This was used for direct interface
GCMS testing at the tunnel exhaust duct This sampling system was used also to collect a Tedlar bag
sample from the tunnel exhaust duct and one from above the truck beds during asphalt load out This
sampling system configurauon was used to collect samples at essentially ambient air conditions where
effluent moisture was not a concern.
The second sampling system used employed an unheated stainless steel probe and 0.3 micron quartz fiber
filter, a stainless steel heat exchanger and two glass mini impingers for moisture removal, a Teflon-head
diaphragm pump, and Teflon tubing to convey sample gas to the GCMS instrumentation. This
configuration was used at the silo exhaust duct because the moisture content of the effluent exceeded that
acceptable for the instrumentation. Use of these portable sampling systems allowed for direct measurement
of volatile organic compounds at remote sources, and allowed for quicker set-up and sampling and analysis
than could be achieved using conventional heated sample transport lines.
On-site analysis after each sample acquisition was performed to determine whether the method QA was
achieved, and to inform the PES Project Manager of the concentration levels observed in the various
effluent matrices. Numerous Representatives from the EPA and CAAP were on-site to observe the testing,
the method QA/QC activities, and the on-site data analysis procedures and results. Representatives from
Research Triangle Institute were present also to serve as test program auditors.
'. "Evaluation of HAPSITE and a Direct Interface GCMS Test Method for Measurement of Volatile
Organic Compounds in Stationary Source Emissions." Vol. I &II. Prepared for Leybold Inficon
Incorporated by Emission Monitoring Incorporated July 1997.
/Z3
-------
2.0 SUMMARY OF RESULTS
The sampling and analysis procedures used during this testing program followed those detailed in the direct
interface GCMS Method (Appendix A). Some additional sampling was conducted using Tedlar bags with
immediate on-site GCMS analysis. This section provides test results obtained from the tunnel exhaust duct
and the silo exhaust duct Volatile organic compounds are reported in concentration units of parts per
billion at the effluent temperature and pressure. Results from the tunnel exhaust duct are presented at stack
moisture conditions, and results from the silo exhaust duct are presented on a "dry" basis (approximately
2% moisture by volume).
The instrumentation utilizes a grab sample technique where effluent sample gas is co-mixed with the
internal standard mixture (in a constant ratio of 10:1) in the GC sampling loop for approximately 1 minute
before injection into the GCMS. The total sample equilibration time within the GC loop was varied for
testing at the tunnel exhaust duct to obtain a sample representing the highest concentration from the truck
load out operation. The GCMS run time was varied between 10 and 15 minutes depending upon the
number of compounds observed in the effluent, and the potential for heavier compounds to be retained on
the column during the relatively short isothermal GC run. For example, the GCMS run time at the silo
exhaust duct was extended to 15 minutes in order to chromatograph all of the compounds present in the
effluent. Extending the run time prevented "cany-over" of analytes from one GCMS run to the next
2.1 Tunnel Exhaust Duct
Testing at the tunnel exhaust duct was conducted on 7-23 and 7-24. Testing on 7-23 consisted of collecting
two samples only before a faulty damper in the exhaust duct interrupted the run. Testing was then focussed
at the tunnel exit to determine what compounds escape the tunnel exhaust system when trucks are loaded
and then travel through the tunnel with the fuming asphalt. No compounds were detected in the three
samples acquired at the tunnel exit. An additional upwind sample was obtained at the tunnel entrance. No
compounds were detected in the single sample acquired upwind of the hot mix load out tunnel.
Testing on 7-24 began after the damper was replaced. Numerous GCMS sample runs were conducted
using various sample acquisition profiles to obtain results representing the highest concentration of analytes
during the actual load out of the hot mix asphalt. The direct interface GCMS testing was concurrent with
EPA Methods 18 and 315, and SW846-0010 and -0030.
The process of filling a truck with hot mix asphalt consists of a truck entering the tunnel and positioning
under one of the five silo storage chutes. Hot asphalt concrete is loaded into the truck in an approximately
30 second dump. Fumes from the dumping of asphalt cause an immediate spike in the concentration of
volatile organic compounds in the tunnel exhaust. In an effort to characterize the maximum emissions from
this process, EMI attempted to coordinate the timing of the hot mix loading process with GCMS sample
acquisition. This proved difficult because the residence time of the "spike" in the tunnel exhaust duct was
unknown, and some trucks loaded different quantities hot mix asphalt
Because the standard GCMS run employs a 60 second sample loop equilibration before GC introduction,
the first few samples did not contain many of the target analytes. It was speculated that the maximum of
the concentration peak was missed with the relatively long loop equilibration time. Next the loop
equilibration time was shortened to 30 seconds. For sample loop equilibration times of 30 seconds or less it
was discovered that the internal standard mixture was not co-added with the effluent. (Internal standards
are necessary to perform the sample quantitation and to assess instrument performance, so this time period
was not acceptable.) The sample loop equilibration time was then extended to 45 seconds and the load out
process monitoring personnel were instructed to give a 15 second notice before the dumping process begaa
The 45 second equilibration with the 15 second notice gave the most consistent and highest observed
concentration results from run to run.
-------
Two separate Tedlar bag samples were collected at this location in order to verify that the sample timing
issues had been resolved. One bag sample was collected from the same location that the direct interface
GCMS testing was conducted. The bag was filled during three successive hot mix dumps while EMI
personnel observed and visually coordinated the load out process. The four samples identified as
TEDBAG01 (02.03.04) represent on-site analysis of this bag sample immediately following its collection.
The second Tedlar bag was filled by sampling directly above the truck bed. inside the tunnel while hot
asphalt was loaded into the trucks. Samples identified as HMLOBAG1 (2. 3) represent on-site analysis of
this bag sample immediately following its collection in the tunnel.
Tables 2.1 and 2.2 present the GCMS concentration results from testing conducted at the tunnel exhaust
duct and the instrument specific detection limits based on the acquisition/calibration method used.
Concentration levels of the detected target analytes were generally below 20 ppb at the tunnel exhaust duct.
It is important to note that the results from the direct interface testing and the results from collecting bag
samples with subsequent immediate on-site analysis provided results at similar concentration levels. This
verifies the timing sequence used during sample collection in the direct interface mode of operation. It is
unclear if collecting bag samples with subsequent off-site analysis would provide similar results
considering the very low concentration levels quantified in the effluent. It is likely that the time required to
ship bag samples to an off-site laboratory would allow adsorption or reaction of the contained gases.
2.2 Asphalt Silo Exhaust Duct
Testing at the silo exhaust duct was conducted on 7-25. The GCMS and portable sampling system were
hoisted to the top of the silo via a pulley system to sample directly from the vent Four 15-minute GCMS
sample runs were performed in succession. Because of the high moisture content of the effluent, the
sampling system employing the heat exchanger and moisture removal apparatus were used to dry the
sample before introduction into the instrumentation.
Numerous peaks were observed in the chromatography. Most of the target analytes were detected at
concentrations of from SO to 500 ppb. Methyl Ethyl Ketone was quantified also in all of the samples at
concentrations of from 1.4 and 1.69 ppm. Carbon disulfide was detected also in this effluent stream.
Although these compound were not identified as target analytes for this test program, they are contained in
Section 1 of the Method and in the instrument specific calibration. It is likely that results reported for MEK
are biased low because of the high moisture encountered at this location and because of the water soluble
nature of MEK. Numerous additional analytes that are not contained in the instrument specific calibration
were identified also in the silo exhaust
Table 2.3 presents the GCMS concentration results for compounds contained in the instrument specific
calibration and the instrument detection limits associated with the acquisition/calibration method used.
Table 2.4 presents the estimated concentration results for those compounds identified in the silo exhaust
duct that are not contained in the instrument specific calibration (the target analyte list of nine compounds
or the analytes identified in Section 1 of the Method).
The specifically listed compounds in Table 2-4 were identified using first principals of mass spectroscopy
and the NIST library contained in the instrument software. By tuning the mass spectrometer according to
the criteria identified in the method, searches of the NIST Mass Spectral Library are made possible.
Tentatively identified compounds (TICs) in Table 2-4 are identified with a double asterisk (**). These
TICs represent compounds whose peaks in both the GC and selected ion trace have a minimal signal-to-
noise ratios (S:N). For S:N ratios of less than 5:1, complicated hydrocarbon spectra are very difficult to
interpret accurately, particularly for those compounds having a molecular weight over 100 amu. Therefore,
these compounds have been tentatively identified only. Their molecular weight and estimated
concentration have been presented as "<" or ">" values.
-------
T.bl.2.1. Dlracl InUrfm CCMS RtiuittiBBII^nl
Sample l«tnlrn<=»tlo«i
TED«I
TED«2
Remarks - Balch process u
Sanpfe IdrflttflaltM
rED~240l
TED-2402
rF.D-2403"
TlD-2407
TED-J408
TED-2409
TED724IO
rED'2411
TEDBAGOr
iom 12 30 10 12 -12
PEDBAG02-
)a( simple collected
iom 12,30 to 12 42
TEDBA003-
Bag simple collected
from 12.30 101242
TEDBAG04-
Bat simple collected
from 12 30 to 1242
1 LFS- United fill scin
SIM I Specific for
i
BPn^Tunnri Eiagiisl
i
Due .AcqulsMonTlme Compouodi Detected
7/23r98 ,1030 .nVp-Xylene
•'as'W
philt loat
Data
irivn
7.'24'»S
7a4^9«
7'24'W
774.9I
7/J4.'W
7^24,'W
~rn*>l
T24'98
7.'24'9«
7.24'9«
1,24'98
1048 Benzene
.Toluene
me operation. GCMS
AcqulfMMl Tim.
914
929
941
II 17
1128
1146
1203
12 P
1243
1254
I30«
1320
GCMS operation from XI-125 ir
l,3buttdiene
hetine
bcnxene
toluene
ethyl benzene
ojnjxyfenes
sniene
m^p-Xylene
usms 60 second simple looi
Ceaawndi DetacM
none
Toluene
m/p-Xylene
Tohiene
None
Toluene
Toluene
Ethyl Benzene
m/p-Xyfcne
Tohiene
Elhyl Benzene
m^p-Xykne
Senzene
Tohiene
mto-Xytene
Tohiene
ElhyJ Benzene
mVXylene
Toluene
Ethyl Benzene
m'p-Xytenc
Benzene
Tohiene
ro'p-Xylene
Benzene
Toluene
Elh\1 Benzene
nvp-Xykne
nu
S1M2 spen6c for
>IKt
C
-------
Table 2-2. Direct Interface GCMS Results -JHBHHHBHR Hot Mix Load Out Bae Sample
Sample Identification1 Date
HMLOBAG1
7/25/98
HMLOBAG2
HMLOBAG3
HMLOBAG4
7/25/98
7/25/98
7/25/98
Acquisition Time
12:40
12:50
13:00
13:11
Compounds Detected
None
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
o-Xvlene
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
o-Xylene
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
o-Xylene
i
Concentration - PPB
n/a
GCMS Method2
LFS
10
SIM2
9:
5;
20|
5i
10
5
5
15
BDL*
10
9
SIM1
SM2
3,
25:
BDL
1. Four separate analysis of single bag sample collected over three successive asphalt truck loadings from 12:20 to 12:35
Matrix Specific Detection Limit
n/a
0 9ppb
09ppb
Ippb
Ippb
2ppb
2ppb
2ppb
2ppb
2ppb
5ppb
0.9 ppb
0.9 ppb
Ippb
Ippb
2 ppb
Samples are replicate analysis of single bag sample using different GCMS methods, HMLOBAG2 and HMLOBAG3 are duplicates
2. LFS - limited full scan operation from 50-125 amu
SIM2 - selected ion method specific for:
.
.
benzene
toluene
ethyl benzene
o,m,p-xylenes
styrene
* BDL = Below Detectable Limit of Quantitation Method
SIM1 - selected ion method specific for:
i
1.3-butadiene
hexane
benzene
toluene
ethvl benzene
o.m.p-xvlenes
stvrene
-------
N
Table 2-3 Direct Interface GCMS Results -|
Simple ID
SED72501
SED72502
SED72503
SED72504
Date
7 '25 '98
7/25'98
7/25/98
7/25 '98
Acquisition Time
8:59
9:20
9:44
10.03
HHIpHHEsUo Exhaust Duct
Compounds Detected
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
o-Xylene
Carbon Disulfide
MEK
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
o-Xylene
Carbon Disulfide
MEK
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
o-Xylene
Carbon Disulfide
MEK
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
o-Xylene
Carbon Disulfide
MEK
Concentration - PPB
110
40
100
50
250
90
100
1460
BDL*
50
170
290
300
280
80
1400
BDL*
50
170
290
360
280
50
1690
BDL*
30
140
190
360
180
20
1090
1 . LFS * Limited Full Scan Mass Spectrometer Operation from 50-125 amu
FS - Full Scan Mass Spectrometer Operation from 45-300 amu
* BDL * below detectable level
CMS Method1
LFS
Full Scan
Full Scan
Full Scan
Matrix Detection Limits - PPB
60
12
5
12
7
15
30
75
100
10
10
10
15
15
L_ 1°
75
100
10
10
10
15
15
10
75
100
10
10
10
15
15
10
75
-------
Sample ID
SED72501
SED72502
SE072503
SED72504
Not Com
OMt
7/24/98
7/24/98
7/24/98
7/24/98
I 1
•mM in Instrument £
Acquisition Tim*
859
920
rif
1003
• Estimated concentration results n PPB
- Tentatwtv Mentfrad Compounds fTICrt
pecific Calibration
Cyclopentane
3-methyl Cyclopentane
6 member nng alky) substituted cyclic amlne**
5-hexenot
2.4-dimelhyl pentene
Alky) substituted cyclic alcohol**
Alkyl substituted cyclohexanol**
Tnmethyl pentane
Tnmethyl Cyclohexane
Alkyl multiply substituted pentanor*
Octahydro-Methyl-Pentalene
Ethyl Methyl Cyclopentine
Cyclopentane '
3-methyl Cydopentane
6 member mg cyclic amine**
5-hexenol
2,4-dimethy! pentene
Alkyl substituted cyclic alcohol-*
Heptyne
Alkyl substituted cyclohexanor*
Trimethyl pentane
rrtmemyl Cyclohexane
Alkyl multiply substituted pentanor*
Octahydro-Methyt-Pentalene
Ethyl Mettiyl Cydopentane
Cyclopentane
3-methyl Cydopentane
> member mg cyclic amme~
5-hexenol
2.4-dimethyl pentene
Ukyl substituted cycle alcohol**
Heptyne
Ukyl substituted cyclohexanor*
rnmethyl pentane
rnmethyl Cyclohexane
Alkyl multiply •ubsttuted pentanor*
Ethyl Methyl CycloiMntvnv
Cyclopentane
3-methyl Cyclopentane
S member mg cydtc amine**
S-he>enol
2,4-dimethyl pentene
Alkyl substtuted cycle alcohol**
•feptyrw
Ukyl substituted cyclohexanor*
rrimethyl Cydohmane
Ukyl multiply tubsttuted pentanor*
Dctahydro- Methyl- Pentalene
Estimated concentration values presented '<* vi
MW
68
82
8!
100
98
>«0
96
>130
114
126
>100
124
681
82
85
100
98
>90
96 1
>130
114
126
>100
124
68
82
85
100
98
•90
96
•130
114
126
MOO
112
68
82
85
too
98
•90
96
•130
126
• 100
124
Compound RF Used
Benzene
Benzene
none
MEK
Hemne
Hemne
none
Heica ne
Ethyl Benzene
Ethyl Benzene
Benzene
Benzene
none
MEK
Hexane
none
Hexane
none
Hexane
Ethyl Benzene
none
Ethyl Benzene
Ethyl Benzene
Benzene
Benzene
none
MEK
Hexane
none
Henane
none
Hexane
Ethyl Benzene
none
Ethyf Benzene
Benzene
Benzene
none
MEK
Hexane
none
Hexane
none
Ethyl Benzene
none
Ethyl Benzene
Estimated Concentration*
53
113
<50 ppb
1567
604
< 50 ppb
<100 ppb
600
198
< 50 ppb
160
46
108
<»PPb ,
463
231
«»" PP"
515
<100 ppb
245
58
< 50 ppb
77
58
32
59
< 50 ppb
444
208
<50 ppb
325
<100ppb
252
62
•Mppb
65
17
33
<50ppb
288
337
< 50 ppb
120
<100 ppb
43
< 50 ppb
33
«se ratio lest than 31 I
, OCMS Method
LFS
! j
FS
FS
FS
-------
3.0 PROCESS DESCRIPTION
schematic is shown in Figure 3-1. The plant was built in 1994 and has an asphalt production rate of 650
tons per hour. The plant produces five categories of asphalt concrete. 3/8 inch. 'A inch . 3/< inch fines, and
recycled asphalt (RAP). The RAP production process adds small amounts of recycled asphalt to the hot
aggregate mix.
The plant uses two varieties of liquid asphalt, each having a different content of volatile organic
compounds. The percent of liquid asphalt added to the aggregate varies form 4.8 to 6 percent depending on
the aggregate size.
Five 200 ton heated storage silos are situated on top of the truck load out tunnel. The storage silos hold the
asphalt between the production time and the load out time. During normal operations, trucks load out
approximately once every three minutes. Single bed trucks hold approximately 21 tons of asphalt, while
dual bed trucks can hold up to 25 tons. It typically takes about 30 seconds to load a truck.
The load out tunnel is approximately 183 feet long by 16 feet wide by 16 feet high Attached to the ceiling
of the tunnel and below each silo is an air plenum that draw vapors from the load out operations and directs
them through a small electrostatic precipitator (the Smog Hog®), and to the stack.
Normal operations produce between 2000 and 6000 tons of asphalt per day. Load out starts at 4 am and
continues for approximately 10 hours. On a typical day, the average load out rate matches the average
production rate so that asphalt is not stored in the silos overnight.
4.0 SAMPLING LOCATIONS
4.1 Tunnel Exhaust Duct
The tunnel exhaust duct is a horizontal 32-inch diameter duct that leads from the load out tunnel to the
Smog Hog®. Sampling ports and the physical dimensions of the tunnel exhaust duct are shown in Figure
4-1.
Single point constant rate (approximately 7 liters per minute) sampling was conducted from a point located
approximately one foot within the duct
4.2 Silo Exhaust Duct
Fumes from the silo exhaust duct exit through a 24 inch diameter duct, a 10 inch diameter duct, and finally
a 12 inch common header before being directed to the Smog Hog®. For this testing, fumes from silo
number 3 were tested. Sampling ports and the physical dimensions of the silo exhaust duct are shown in
Figure 4-2.
Single point constant rate (approximately 7 liters per minute) sampling was conducted from a point
approximately one foot within the duct
-------
Atmosphere
Silo Exhaust
Duct
Sampling
Location
Asphalt
Atmosphere Cement
i
Stack
Baghouse
Rotary Drum
Dryer
Secondary
Chamber
Natural Gas-Fired
Llquid Asphalt
Tunnel
Exhaust Duct
Sampling Location
RAP
Aggregate
Liquid Asphalt Storage Tanks
Figure 3.1 Process Flow Schematic,,
-------
From Silo No. I
To Smog
Method 3 15
\
rA
Section A-A
MM5
VOST Method 18
\
GC/MS
/ FTIR
From Silo No. 2
From Silo
-Nos.3,4,
and 5
Figure ^ I Tunnel Exhaust Duct Sampling Port Locations,.
-------
Temporary Duct
Extension
To Smog
Hog
Method 315
u
Port Locations,
-------
5.0 SAMPLING AND ANALYTICAL PROCEDURES
The sampling and analytical procedures used during this testing program followed those detailed in the
direct interface GCMS test method (Appendix A). The instrument was calibrated specifically for this test
project using the nine of the target analytes. The instrument was calibrated also for all compounds
identified in Section 1 of the method approximately one month before this test and this calibration was used
also to identify any other potential analytes not specific to this test program (such as MEK and CS2).
Instrument specific calibrations were conducted in the full scan mode (and limited full scan) of operation
where all of the mass fragments in a compounds mass spectrum are generated in every run. Additional
instrument calibrations were conducted for the nine test specific target analytes using a selected ion
monitoring (SIM) mode of operation. In this mode, only a select few ions are measured in each compounds
mass spectrum. Although this method of operation gives less information regarding the compounds true
identity, it necessarily improves the instrument sensitivity because of the increased number of scans
achieved per chromatographic peak. The combination of using the full scan, limited full scan, and SIM
scan modes of operation gives positive identification of the individual analytes while increasing the
instrument sensitivity.
System continuing calibration verification was conducted daily through the portable sampling system using
all of the nine test specific target analytes. The system calibrations were performed in the rear
compartment of a rental minivan. For testing conducted at the tunnel exhaust duct the GCMS was
calibrated and operated directly from the rear compartment the minivan. For testing conducted at the silo
exhaust stack, the GCMS was disconnected from the sampling system, transported to the actual sampling
location, and then reconnected to the sampling system after passing a leak check.
5.1 Sampling Procedures
5.1.1 Direct Interface GCMS Sampling
Effluent gas samples were withdrawn at a constant flow rate from a single point located approximately one
foot inside of the each duct or stack using a Teflon head diaphragm pump. Effluent was withdrawn at
approximately 3 liters per minute through the sampling system for no less than 5 minutes before sample
acquisition in order to equilibrate fully all sampling system components. It is estimated that the gas
residence time through the sampling system is less than 1 minute at this sampling rate.
Two sampling systems were used during this testing program depending on the effluent volumetric
moisture content Sampling system #1 is used primarily for ambient moisture applications and was used
for testing at the tunnel exhaust duct. It is constructed out of stainless steel, and utilizes a 0.3 p. quartz
Balston filter for paniculate removal. Sampling system #2 is used for applications where the volumetric
moisture content of the effluent exceeds 8% (the instrumental operating limit). These conditions were
encountered at the silo exhaust stack. Sampling system #2 is constructed out of stainless steel and utilizes a
0.3(1 quartz Balston filter for paniculate removal, followed by a heat exchanger and two mini impingers for
moisture removal.
The gas flow through sampling system #1 is relatively simple. Sample gas is filtered and transported
directly to the instrumentation at essentially stack conditions. The gas flow through sampling system #2 is
unique in that after passing through the heat exchanger and mini impingers, the dried gas is directed back
through the heat exchanger for reheating before introduction into the instrumentation. Figures 5-1 and 5-2
present simplified diagrams of both sampling systems used during this testing project.
12
-------
Excess Sample
Rotameter
GCMSAnalyzer
Bypass Control
Teflon Head
Pump
25 Foot Teflon Sample Line
Atmospheric Vent
316 Stainless Probe Sintered Filter
0.3 micron
quartz filter
t
Calibration Gas Introduction
Figure 5-1 Low Moisture Portable Sampling System
-------
Excess Sample
Rotameter
GCMSAnalyzer
Bypass
Control
0.3 micron
quartz filter
25 Foot Teflon
Sample Line
316 Stainless Probe
Sintered
Filter
Calibration Gas
Counter Current
Flow Heat Exchanger
Condensate Knock Out
Traps in Ice Bath
Atmospheric Vent
Figure 5-2 High Moisture Portable Sampling System
-------
5.1.2 Tedlar Bag Sampling
A Tedlar bag was used to collect a composite sample from tunnel exhaust duct. Three truck load outs were
monitored visually and coordinated with sample collection. Sample acquisition was performed using
sampling system #1 to extract gas samples from the same point as that used for the direct interface testing.
Before sampling, the Tedlar bag was filled twice with dry nitrogen and then the contained nitrogen was
analyzed for the presence of any detectable analytes. No analytes were found in the blank bag sample.
Samples identified as TEDBAG01.02, 03 and 04 (Table 2-1) represent separate analysis of this single bag
sample.
A Second Tedlar Bag sample was collected from inside the tunnel, above truck beds while loading asphalt.
Sampling system #1 was used to collect a composite sample from three successive truck load outs. Before
sampling, the Tedlar bag was filled twice with dry nitrogen and then the contained nitrogen was analyzed
for the presence of any detectable analytes. No analytes were found in the blank bag sample. Samples
identified as HMLOBAG1,2, and 3 represent separate analysis of this single bag sample.
5.1.3 GCMS Operation
The GCMS instrumentation was operated using a non-evaporative getter (NEC) pump to maintain the
requisite high internal vacuum needed to generate mass spectra. For some of the testing the GCMS used its
own internal batteries for power if none was available.
Internal standards are co-added with every effluent sample in the GC sample loop before injection into the
GC. The internal standards used are 1,3,5-trifluoromethyl benzene (THIS) and bromopentafluoro benzene
(BPFB). These compounds are not found in industrial processes. They are used to tune the mass
spectrometer, to assess the stability and performance of the GCMS on each sample run, and to determine
adherence to the method QA/QC.
The GC was operated isothermally at 60°C to separate and detect the target analytes. The mass
spectrometer was operated in full scan (45-300 amu), limited full scan (50-125 amu), and selected ion
monitoring modes of operation to optimize identification and quantification of the largest number of
volatile organic compounds. All internal GCMS components were maintained at 60°C.
The GCMS internal sample pump withdrew sample from the sampling system (either #1 or #2) at
atmospheric pressure for a period of approximately one minute for testing conducted at the silo and from 30
seconds to one minute for testing at the tunnel exhaust duct For testing conducted at the runnel exhaust
duct, the sample timing was critical in obtaining the maximum in the concentration from the asphalt load
out Many parameters were tried, but the sample loop equilibration of 45 seconds with a 15 second notice
from the process monitoring individual gas the most consistent results. (See Section 2.11 of this document
for a complete description of the procedures leading to this conclusion.)
Daily QA/QC activities were conducted in the rear compartment of a rental minivan. GCMS operation was
conducted from the minivan for testing at the tunnel exhaust duct The GCMS was operated from on top of
the silo for testing at the silo exhaust duct.
5.2 Analytical Procedures
The procedures detailed in the direct interface GCMS method (Appendix A) were followed for this testing
program. See Figure 5-3 for a method operational flowchart
The GCMS was calibrated at the EMI laboratory using duplicate injections at three concentration levels for
each specific calibration curve. The calibration and internal standards used for this testing were certified by
Spectra Gas, and by Scott Specialty Gases (manufacturer's certifications of analysis are included in
Appendix A).
15
-------
Two full scan calibrations were performed for the nine test specific target analytes and for all of the
analytes listed in Section 1 of the method. Full scan operation is generally defined to be from 45-300 amu
for the HAPSITE GCMS. and from 50-125 for the rune test specific analytes identified for this test.
Therefore, compounds having a molecular weight of less than tliat identified are not detected, and
compounds weighing greater than that identified will have resultant mass spectra in the scan range only.
Full scan calibration curves were established at concentration levels of 10 ppm, 1 ppm and 300 ppb.
Two SIM scan calibrations were performed also at much lower concentration levels of 100 ppb, 50 ppb and
20 ppb. Ions specific to the nine target analytes were used to generate these curves (i.e.. 78 for benzene. 91
for toluene etc..).
Sample acquisition was performed using one of the four acquisition methods that correspond to the
individual calibration curves. All analytes contained in the instrument specific calibrations elute from the
GC column during a ten-minute run. Sample quantification was performed using the internal standards and
the selected three-point calibration curve that matched the GCMS acquisition profile. Section 10 of the
method details the mathematical process by which the results are calculated (for those compounds
contained in the calibration curve).
Results are reported also for compounds not contained in the calibration curve from testing conducted at
the silo exhaust duct. Because the GC separates the individual compounds from each other, and the mass
spectrometer fragments each compound in a virtually unique pattern, positive identification of compounds
not contained in the instrument specific calibration is possible. Identification of compounds not contained
in the instrument specific calibration was performed by mass spectral pattern recognition and by
conducting searches of the NIST Mass Spectral Library that is contained in the instrument software.
Response factors of chemically similar compounds contained in the instrument specific calibration were
used to quantify these compounds based on the manually integrated area of a specific mass spectral
quantification ion.
The following steps are used to identify and to quantify compounds not contained in the instrument specific
calibration.
Obtain the compounds mass spectrum
Identify the compound using the NIST Library and first principals of mass spectrometry
Determine the compounds molecular weight and assign a Quantification Ion (QI)
Manually integrate the area contained under the peak of the QI
Determine a chemically similar compound contained in the instrument specific calibration
Use the chemically similar compounds instrument specific response factor (RF) as follows:
ppm = (QIarea I RF\ISconc.l ISarea)
Where:
ppm = Estimated concentration of compound
QI area = Manually integrated area of compound quantification ion
Rf = Response factor of most chemically similar compound from instrument specific calibration
IS cone. = Concentration of internal standard used
IS area = Area of internal standard quantification ion
126
16
-------
Warm-up
Establish Stable Operations
retune
no
yes
,,•*•
Tune/Mass Alignment
Tune criteria met?
no
no
no
0>
>
0.
CM
no
Check Tune
yes
3-Point Calibration
- Do RT values replicate?
- Do IS meet criteria?
- Sensitivity (S/N) sufficient
for required measurement
range?
- %RSD criteria met for RRFs?
yes
Surrogate System Continuing Calibration
- Do RT values replicate?
- Do IS meet criteria?
- (S/N) sufficient
- Do results meet 20% criteria and
indicate valid three-point calibration?
yes
System Zero
Is 50 ppb system
zero criterion met?
yes
Sampling/Analysis
Do RT values meet criteria'
Do IS meet criteria?
yes
Continue Sampling
After 12 hours of continuous
operation, instrument shut-do\i
or malfunction
Figure 5-.1 Dirccl Interface GCMS Method Operational Flowchart
17
-------
6.0 QUALITY ASSURANCE/QUALITY CONTROL
6.1 Initial Calibration and Daily Calibration Check Procedures
Establishing a valid three-point calibration requires a 20 percent relative standard deviation (%RSD) for
each individual analyte over the calibration range. Two calibration curves were generated in each of the
full scan and SIM scan acquisition methods. Calibration was performed by conducting two successive
GCMS runs at each of three concentration levels: 10 ppm. 1 ppm and 300 ppb for the full scan calibration
curves, and 100 ppb. 50 ppb and 20 ppb for the SIM scan calibration curves. Section 10 of the method
details the calculation procedures used to determine the %RSD for each of the analytes. Table 6-1 presents
the target analytes. the results from the three-point calibration in terms of %RSD for each of the four
calibration curves, and the estimated detection limits.
Daily system calibrations were conducted to check both the validity of the initial instrument three-point
calibration and the effectiveness of the sampling system to transport the target analytes. Daily system
calibration check procedures were conducted after accomplishing a successful instrument tune using the
blended mixture of the internal standards. Immediately following the system continuing calibration.
nitrogen was allowed to flow through the system and a system blank was acquired. No analvtes were
detected in any of the system blank analyses.
The direct interface GCMS test methods requires that continuing system calibrations be conducted using a
blended mixture of six surrogate compounds at 1 ppm. (See Table 6 of the method.) Because this testing
project had nine specific target analytes expected to be at much lower concentration levels than 1 ppm,
continuing system calibrations were conducted using the nine target analytes themselves at a 300 ppb
concentration level. This procedure gave a much better indication of the GCMS ability to quantify
accurately the target analryes at such low concentration levels.
Achieving the criteria for a valid mass spectral tune and achieving the internal standard relative mass
abundances during each GCMS run (see Tables 3 and 4 of the method) verify the continuing instrument
performance and ensure that the QA/QC of the method are achieved. Achieving the criteria for a valid tune
also allows searches of the MIST Mass Spectral library for compounds that are not contained in the
instrument specific calibration. Tables 6-2 through 6-4 present the daily system continuing calibration
results.
18
-------
Table 6-1. GCMS Three
-Point Calibration Ri
Full Scan Calibration (45-300 amu)
Compounds
FSM
Chloroethane
Mcthylenc Chloride
1 . 1 -dichloroethane
c- 1 ,3-dichloroethene
1 . 1 , 1 -trichloroethane
1 ,2-dichloropropane
1 , 1 ,2-trichlorocthanc
Dibromochloromethane
&iylbcnzene
p-xylene
, 1 ,2,2-tetrachloroethane
)rofnomcthane
1,1-dichloroelhenc
t- 1 ,2-dichloroethcne
MEK
l,2-dichloroeth«ne
Carbon tetrachloride
rrichloroethene
c- 1 ,2-dichloropropene
t- 1 ,2-dicMoropropene
-hexanone
CMorobenzene
m-xylene
0-xylene
Vinyl chloride
Carbon disulfidc
Vinyl acetate
Chloroform
Benzene
Bromodichloromelhane
MffiK
roluene
FCE
Bromoform
Styrene
3-Point Calibration1
%RSDs-
6.1
6.3
7.5
8.1
3 9
7^
5.9
63
4.6
4 5
09
6.6
4.8
5.5
3.9
7.8
6.6
4.1
5.1
5.8
8.1
3.7
4.8
8.9
2.3
1.3
2.6
2.6
1.6
3.7
10.1
4.1
1.6
2.1
2.9
•suits and Ei
Estimated
DU-PPB
3C
3d
30
3t
30
15
15
15
12
10
15
30
30
30
75
30
15
15
15
15
500
50
10
15
15
7
75
15
15
15
500
7
15
15
25
1 . Calibration conducted at 1 0 ppm, 1 ppm and 300 ppb
2. Calibration conducted at 100 ppb, 50 ppb, and 20 ppb
ittmated Detect
Limited Full S
Compounds
LFS
HexiiK
Benzene
Toluene
Ethyl Benzene
Styrene
o-Xylene
' GCMS method criteria for valid calibration ii within 20''. RSD
ion Limits
can Calibration (50-1
3-Point Calibration1
•/. RSDs •
6.4
3 1
3.3
2.1
3.9
3.4
'.S amu)
Estimated
60
12
5
12
10
15
SIM1 (ions 57, 1
13 Butadiene
Hexanc
Benzene
Ethyl Benzene
m/p-Xylenes
o-Xylene
16, 78, 91, 104, 69 & 1
3-Point Calibration1
1.6
10.1
g.5
111
98
8_J^
73
17)
Estimated
50
20
2
2
2
5
5
SIM2 (ions 78,
Compounds
Benzene
Toluene
Ethyl Benzene
m/p-Xylenes
Styrene
o-Xylene
91,104, 69 &\ 17) i
3-Polnt Calibration2
29
55
g
53
7 2
95
Estimated
09
09
i
-------
Table 6-2 System Continuing Calibration Check Results
7/23/98
Cylinder #ICCR
Compound
TRIS
BPFB
1 ,3-Butadiene
Hexane
Benzene
Toluene
Ethvl Benzene
m/p-Xylene
St>Tene
o-Xvlene
Area
3271835
7014327
nd
111798
1537111
1305132
1667974
2378401
679144
1291092
* ARRF and ARF from Calibration Curve
RF
3.29E+05J
1.45E+06
RRF
LVALUE!
1.12
15.41
13.22
3.81
2.71
1.57j
2.98
DF =0.03
ARF*
2.80E+05
1.50E+06
ARRF
0.31
1.45
15.26
15.22
4.02
3.39
2.05
3.35
** Valid System Continuing Calibration QA are within 20% for 1 ppm.
ppm - tag
NA
NA
10.00
10.10
10.10
10.00
10.10
20.20
10.00
10.00
No criteria have been established for system continuing calibrations at 300 ppb.
ppm-exp
NA
NA
0.30
0.30
0.30
0.30
0.30
0.61
0.30
0.30
ppm-obs
NA
NA
nd
0.29
0.31
0.34
0.38
0.69
0.38
0.38
%Diff**
NA
NA
#VALUE!
-4%
2%
13%
25%
r 14%
1 27%
27%
-------
Table 6-3 System Continuing Calibration Check Results
7/24/98
Cylinder #ICCR
Compound
TRIS
BPFB
1,3 -Butadiene
Hexane
Benzene
Toluene
Ethvl Benzene
m/p-Xylene
Stvrene
o-Xylene
Area
3745367
8321812
23687
122209
1381665
1132306
1287195
1822517
549654
1044418
* ARRF and ARF from Calibration Curve
RF
3.77E+05
1.72E+06
RRF
0.21
1.07
12.10
10.02
2.48
1.75
1.07
2.03
DF = 0.03
ARF*
2.80E+05
1.50E+06
ARRF
0.31
1.45
15.26
15.22
4.02
3.39
2.05
3.35
ppm - tag
NA
NA
10.00
10.10
10.10
10.00
10.10
20.20
10.00
10.00
** Valid System Continuing Calibration QA are within 20% for 1 ppm.
No criteria have been established for system continuing calibrations at 300 ppb.
ppm-exp
NA
NA
0.30
0.30
0.30
0.30
0.30
0.61
0.30
0.30
ppm-obs
NA
NA
0.3
0.28
0.25
0.28
0.3
0.55
0.33
0.31
%Diff**
NA
NA
0%
-8%
-17%
-7%
-1%
-9%
10%
3%
-------
Table 6-4 System Continuing Calibration Check Results
7/25/98
Cylinder «CCR
Compound
TRIS
BPFB
1,3-Butadiene
Hexane
Benzene
Toluene
Ethvl Benzene
m/p-Xylene
Styrene
o-Xylene
Area
3802228
9090581
29967
114860
1178802
920989
1321394
1998716
568219
954218
1
i
* ARRF and ARF from Calibration Curve
RF
3.83E-K)5
1.87E+06
RRF
0.26
0.99
10.17
8.03
2.33
1.76
1.01
1.70
DF = 0.03
ARF*
2.80E+05
1.50E+06
ARRF
0.31
1.45
15.26
15.22
4.02
3.39
2.05
3.35
ppm - tag
NA
NA
10.00
10.10
10.10
10.00
10.10
20.20
10.00
10.00
** Valid System Continuing Calibration QA are within 20% for 1 ppra.
No criteria have been established for system continuing calibrations at 300 ppb.
ppm-exp
NA
NA
0.30
0.30
0.30
0.30
0.30
0.61
0.30
0.30
ppm-obs
NA
NA
0.35
0.26
0.21
0.25
0.29
0.55
0.32
0.29
%Diff**
NA
NA
17%
-14%
-31%
-17%
-4%
-9%
7%
-3%
-------
7.0 DISCUSSION OF TEST PROGRAM AND RESULTS
Concentration results from the tunnel exhaust duct were very low. generally less than 20 parts per billion
for the compounds detected. Timing issues regarding how to sample the effluent effectively during the
batch load out process were resolved using the 45 second GC sample loop equilibration combined with the
15 second notice from the process monitoring personnel. The validity of the sample timing in the direct
interface mode of operation was verified using the secondary Tedlar bag sampling/analysis technique.
Results from direct interface testing were generally in good agreement with the Tedlar bag samples.
Concentration results from the silo exhaust duct were higher that those observed from the tunnel load out
operations. Numerous compounds were detected in the silo exhaust Compounds that were test program
specific (as well as those that were not) were identified and quantified from this location. One compound,
methyl ethyl ketone (MEK), was quantified in two samples at much higher concentrations than the other
compounds detected from this source. It is likely that results for MEK are biased low due to the relatively
high water vapor content of the effluent and the water soluble nature of this compound.
Using the HAPSITE GCMS in the fully portable mode of operation combined with using the portable
sampling systems allowed for collection and on-site data analysis from four separate locations over a three-
day period. All sampling, QA/QC activities, and analytical procedures were conducted from the rear
compartment of a rental mini-van or at the actual sampling location. Transporting the instrumentation to
the actual test location eliminated much of the conventional sampling apparatus and electrical power
requirements. Operation in this fully portable mode proved to be efficient while providing data that met the
Q A requirements of the test method and the data quality objectives of the test program.
23
-------
-------
EMISSION MONITORING
INC.
EFFECTIVE SOLUTIONS AND ADVANCED TECHNOLOGIES
DIRECT INTERFACE GCMS TESTING
AGGREGATE DRYER BAGHOUSE STACK
Prepared Under Subcontract to:
Pacific Environmental Services
Subcontract NO. 68-D-98-004-FP-002
U.S. EPA Contract NO. 68-D-98-004
Prepared for:
Mr. John T. Chehaske
Program Manager
And
Mr. Frank J. Phoenix
Project Manager
Pacific Environmental Services, Inc.
560 Herndon Parkway, Suite 200
Heradon, VA 20170-5240
Prepared by:
Laura L. Kinner Ph.D. and James W. Peeler
Emission Monitoring Incorporated
8901 Glenwood Ave.
Raleigh, NC 27612
8901 GLENWOOD AVENUE • RALEIGH, NC 27612-7503 • PHONE (919) 781-3824 • FAX (919) 782-9476
-------
TABLE OF CONTENTS
SECTION PAGE#
1.0 INTRODUCTION 1
2.0 SUMMARY OF TEST RESULTS 2
3.0 PROCESS DESCRIPTION 2
4.0 SAMPLING LOCATIONS 2
5.0 SAMPLING AND ANALYTICAL PROCEDURES 2
6.0 QUALITY ASSURANCE/QUALITY CONTROL 7
7.0 CONCLUSIONS AND RECOMMENDATIONS 7
-------
LIST OF TABLES
TABLE PAGES
Table 2-1 Direct Interface GCMS Results - Aggregate Dryer Baghouse Stack 4
Table 6-1 GCMS Three-Point Calibration Results and Estimated Detection Limits 8
Table 6-2 Daily System Continuing Calibration Check Results 7-25-98 9
LIST OF FIGURES
FIGURE PAGE*
Figure 5-1 High Moisture Direct Interface Sampling System Schematics 5
Figure 5-2 Direct Interface GCMS Method Operational Flowchart 6
-------
1.0 INTRODUCTION
The United States Environmental Protection Agency (U.S. EPA) requested use of a portable gas
chromatograph-mass spectrometer based analyzer (HAPSITE™) to identify and quantiry^volatile organic
liazardous air pollutants from various emissions points at fHMHHIHHHHHMHHBlf^
VHHHHfe The EPA requested specifically that the instrumentation be operated in the fully portable
mode without use of a heated extractive sampling system so that the test locations could be accessed
quickly and easily. The GCMS instrumentation was developed by Leybold-Inficon, and has been evaluated
extensively by Emission Monitoring Incorporated (EMI)'. Numerous industrial stationary sources have
been tested using this instrumentation in accordance with the method entitled "Determination of Gaseous
Organic Compounds by Direct Interface GCMS". This method was developed by EMI and Inficon and has
been accepted by the U.S. EPA as an alternate test method for numerous stationary sources (ALT-017), and
as a conditional test method (CTM-28). The method and documentation are available on-line from the
EPA Website, and a copy of the method is provided in Appendix A.
Pacific Environmental Services (PES) subcontracted EMI to perform direct interface GCMS testing at the
hot mix asphalt load out tunnel, and at the asphalt silo storage vent While on-site, EMI was asked to
conduct additional testing at the aggregate dryer baghouse stack and at the exit of the load out tunnel. The
results from testing performed at the aggregate dryer baghouse stack only are presented in this report The
primary objective of the testing was to characterize and quantify nine specific volatile organic hazardous air
pollutants (benzene, toluene, o,m,p-xylenes, styrene. ethyl benzene. 1,3-butadiene, and hexane). EMI was
asked to focus the testing for these specific analytes as a subset of the analytes identified in Section 1 of the
Method.
The sampling system used employs an unheated stainless steel probe and 0.3 micron quartz fiber filter, a
stainless steel heat exchanger and two glass mini impingers for moisture removal, a Teflon head diaphragm
pump, and Teflon tubing to convey sample gas to the GCMS instrumentation. This configuration was used
because the moisture content of the effluent exceeded that acceptable for the instrumentation. Use of this
sampling methodology allows for direct measurement of volatile organic compounds at remote sources and
allows for quicker set-up, and sampling and analysis than could be achieved using conventional heated
sample transport lines.
On-site analysis after each sample acquisition was performed to determine whether the method QA was
achieved, and to inform the PES Project Manager of the concentration levels observed in the effluent
matrix. Numerous representatives from the EPA and CAAP were present to observe the testing, QA/QC
activities and the on-site data analysis. Representatives from Research Triangle Institute were present also
to serve as test program auditors.
1 "Evaluation of HAPSITE and a Direct Interface GCMS Test Method for Measurement of Volatile
Organic Compounds in Stationary Source Emissions." Vol. I &II. Prepared for Leybold Inficon
Incorporated by Emission Monitoring Incorporated July 1997.
-------
2.0 AGGREGATE DRYER BAGHOUSE STACK CONCENTRATION RESULTS
Testing at the dryer baghouse stack was conducted on 7-25. The GCMS and portable sampling system
were pulled up on top of the baghouse to sample directly from the port. This location was very challenging
for the instrumentation because of vibration and high ambient temperatures (approximately 95-100°F).
Three 10-nunute GCMS sample runs were performed in succession. Most of the target anaJytes were
detected at concentrations of from 10 to 330 ppb. Immediately after acquiring the second sample, the dryer
was observed visually to shut down, and then later observed to restart. It is unknown whether the second
and third sample are representative of normal dryer operation. The measurement system passed the
individual run criteria at this challenging location.
Table 2-1 presents the GCMS concentration results for the aggregate dryer baghouse stack, and the
associated instrument detection limits.
3.0 PROCESS DESCRIPTION
No process specific information is available at this time.
4.0 SAMPLING LOCATION
No sampling location information is available at this time.
5.0 SAMPLING AND ANALYTICAL PROCEDURES
The sampling and analytical procedures used during this testing program followed those detailed in the
direct interface GCMS test method (Appendix A). Figure 5-1 presents a method operational flow chart.
The instrument was calibrated specifically for this test project using nine of the target analytes identified in
Section 1 of the method. Additionally, the instrument was calibrated for all compounds identified in
Section 1 of the method approximately one month before this test. Both calibration curves were used to
identify and to quantify the detected volatile organic compounds.
Instrument specific calibrations were conducted in the laboratory using the limited full scan mode of
operation. In the limited full scan, all of the mass fragments in the nine-target analytes mass spectrum are
generated in every run. Additional instrument calibrations were conducted for these nine analytes using a
selected ion monitoring (SIM) mode of operation. In this mode, only a select few ions are measured in
each compounds mass spectrum. Although this method of operation gives less information regarding the
compounds true identity, it necessarily improves the instrument sensitivity because of the increased number
of scans achieved per chromatographic peak. The combination of using limited full scan and SIM scan
modes of operation give positive identification of the individual analytes while increasing the instrument
sensitivity.
System continuing calibration verification was conducted daily through the portable sampling system using
all of the test specific target analytes. The system calibrations were preformed in the rear compartment of a
rental minivan. For testing conducted at the dryer baghouse stack, the GCMS was disconnected from the
sampling system, transported to the actual sampling location, and then reconnected to the sampling system
after passing a leak check.
5.1 Sampling Procedures
5.1.1 Direct Interface GCMS Sampling
Effluent gas samples were withdrawn at a constant flow rate from a single point located approximately one
foot inside of the stack using a Teflon head diaphragm pump. Effluent was sampled at approximately 3
liters per minute for no less than 5 minutes before sample acquisition in order to equilibrate fully all
sampling system components. It is estimated that the sample residence time through the sampling system is
less than one-minute at this flow rate.
-------
The sampling system used for application is constructed out of stainless steel and utilizes a 0.3(i quartz
Balston filter for paniculate removal, followed by a heat exchanger and two mini impingers for moisture
removal.
The gas flow through the sampling system is unique in that after passing through the heat exchanger and
mini impingers. the dried gas is directed back through the heat exchanger for reheating before introduction
into the instrumentation. Figure 5-2 presents a simplified diagram of the portable sampling system used at
the aggregate dryer baghousc stack.
ttn
-------
Table 2-1. Direct Interface GCMS Results - ^•••••H Agzreg
j
Sample Identification i Date Acquisition Time
DryerOl
Drver02'
Dryer032
7/25/98 13:53
7/25/98! 14:05
1
1
7/25/98 14:17
!
.
Compounds Detected
Benzene
Toluene
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
Styrene
o-Xylene
Benzene
Toluene
Ethvl Benzene
m/p-Xylene
Sryrene
ate Dryer Baghouse Stack
Concentration - PPB
10
110
260
80
10
50
50
18
330
110
10
80
130
1 . Plant upset condition - rotary dryer shuts down approximately 2 minutes after sample acquisition
2. Sample acquired approximately 15 minutes after rotary dryer re-start
3. LFS - limited full scan operation from 50-125 amu
SIM2 - selected ion method specific for:
benzene
toluene
ethyl benzene
o,m,p-xylenes
styrene
GCMS Method1
LFS
SIM2
SIM2
1
1
Matrix Specific Detection Limit
5ppb
5PPb
0.9 ppb
0.9 ppb
I ppb
Ippb
2 ppb
2 ppb
0.9 ppb
0.9 ppb
Ippb
Ippb
2 ppb
-------
Warm-up
Establish Stable Operations
retune
no
yes
Tune/Mass Alignment
Tune criteria met?
Check Tune
no
no
no
O)
CM
Z
no
yes
3-Point Calibration
- Do RT values replicate?
- Do IS meet criteria?
- Sensitivity (S/N) sufficient
for required measurement
range?
- %RSD criteria met for RRFs?
yes
Surrogate System Continuing Calibration
- Do RT values replicate?
- Do IS meet criteria?
- (S/N) sufficient
- Do results meet 20% criteria and
indicate valid three-point calibration?
no
yes
System Zero
Is 50 ppb system
zero criterion met?
yes
Sampling/Analysis
Do RT values meet criter
Do IS meet criteria?
yes
Continue Sampling
After 12 hours of continuou
operation, instrument shut-i
or malfunction
Figure 5-| Direct Interface GCMS Method Operational Flowchart
5
-------
Excess Sample
Rotameter
GCMSAnalyzer
Bypass
Control
Flow
Control
Teflon Head
Pump
0.3 micron
quartz filter
25 Foot Teflon
Sample Line
316 Stainless Probe
Sintered
Filter
Calibration Gas
Counter Current
Flow Heat Exchanger
Condensate Knock Out
Traps in Ice Bath
Atmospheric Vent
Figure 5-2 High Moisture Portable Sampling System
-------
6.0 QUALITY ASSURANCE/QUALITY CONTROL
6.1 Initial Calibration and Daily Calibration Check Procedures
Establishing a valid three-point calibration requires a 20 percent relative standard deviation (%RSD) for
each individual analyte over the calibration range. Two calibration curves were generated in each of the
full scan and SIM scan acquisition methods in the EMI Laboratory. Calibration was performed by
conducting two successive GCMS runs each at three concentration levels; 10 ppm. 1 ppm and 300 ppb for
the full scan calibration curves, and 100 ppb. 50 ppb and 20 ppb for the SIM scan calibration curves.
Section 10 of the method details the calculation procedures used to determine the %RSD for each of the
analytes. Table 6-1 presents the target analytes. the results from the three-point calibration in terms of
%RSD. and the estimated detection limits for each of the four calibration curves.
Daily system calibrations were conducted to check both the validity of the initial instrument three-point
calibration and the effectiveness of the sampling system to transport the target analytes. Daily system
calibration check procedures were conducted after accomplishing a successful instrument tune using the
blended mixture of the internal standards. Immediately following the system continuing calibration.
nitrogen was allowed to flow through the system and a system blank was acquired. No analytes were
detected in the blank analysis.
The direct interface GCMS test methods requires that continuing system calibrations be conducted using a
blended mixture of six surrogate compounds at 1 ppm. (See Table 6 of the method.) Because this testing
project had nine specific target analytes expected to be at much lower concentration levels than 1 ppm.
continuing system calibrations were conducted using the nine target analytes themselves at a 300 ppb
concentration level. This procedure gives a much more realistic estimate of the ability of the GCMS to
quantify accurately the target analytes at low concentration levels.
Achieving the criteria for a valid mass spectral tune and achieving the internal standard relative mass
abundances during each GCMS run (see Tables 3 and 4 of the method) verify the continuing instrument
performance and ensure that the QA/QC of the method are achieved. Table 6-2 presents the daily system
continuing calibration results.
-------
Full Scan Calibration (4
Compounds
Chloroethanc
Mcthylcne Chloride
1 . 1 -dichloroethane
c- 1 ,3-dichlorocthcne
1.1,1 -trichlorocdiane
1 .2-dichloropropane
1 . 1 ,2-lrichloroclhane
Dtbromochloromethane
Ethylbcnzenc
p-xylene
1.1 ,2,2-tctrachlorocthane
iromomethane
1 . 1 -dichloroethcne
t- 1 ,2-dichloroetKcne
MEK
1 .2-dichloroelh«ne
Carbon tetrachloride
Trichloroethene
c- 1 ,2-dichloropropenc
t- 1 ,2-dichloropropene
2-hex«none
Chlorobenzene
m-xylcne
O-.tylene
V inyl chloride
Carbon disulfide
Vinyl acetate
Chloroform
Benzene
Bromodichloromethanc
NflBK
Toluene
TCE
Bromoform
Styrene
5-300 amu)
3-Polnt Calibration1
•/. RSDj-
6.1
6.3
7.5
8.1
39
7.9
5.9
6.3
46
4.3
0.9
6.6
4.8
5.5
3.9
7.8
6.6
4.1
5.1
5.8
8.1
3.7
4.8
8.9
2.3
1.3
2.6
2.6
1.6
3.7
IO.I
4.1
1.6
2.1
2.9
Estimated
DLs - PPB
30
3C
3C
3C
30
13
15
15
12
10
15
30
30
30
75
30
15
15
15
15
500
50
10
15
15
7
75
15
15
15
500
7
15
15
25
1 . Calibration conducted at 10 ppm, 1 pom and 300 ppb
2. Calibration conducted at 100 ppb, 50 ppb, and 20 ppb
Limited Full Scan Calibration (50-125 amu)
Compounds
LFS
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylenes
Styrene
B-Xylene
• GCMS method criteria for valid calibration it within 20% RSD
3-Polnt Calibration1
% USDs'
6.4
3.1
33
2.1
1.8
19
3.4
Estimated
60
12
5
12
7.5
10
15
SIM1 (Ions 57, 86. 78, 91, 104, 69 & 117)
Compounds .3-Pelnt Calibration1
1.3 Butadiene . 1_6_
Hexane 10.1
Benzene 8.5
Ethyl Benzene ' 11. 1
m/p-Xylenes 9.8,
Styrene 81
o-Xylene 7 3
i
Estimated
50
20
2
2
2
5
5
SLM2 (ions 78,
Compounds
Benzene
Toluene
Ethyl Benzene
m/p-Xylene»
Styrene
o-Xylene
91,104, 69 All?)
3-Polnl Calibration2
2.9
5 5
6
5 3
72
95
Estimated
09
09
1
1
2
2
-------
Table 6-2 System Continuing Calibration Check Results
7/25/98
Cylinder #ICCR
Compound
THIS
BPFB
1.3 -Butadiene
Hexane
Benzene
Toluene
Ethvl Benzene
m/p-Xylene
Stvrene
o-Xvlene
Area
3802228
9090581
29967
114860
1178802
920989
1321394
1998716
568219
954218
* ARRF and ARF from Calibration Curve
RF
3.83E+05
1.87E+06
RRF
0.26
0.99
10.17
8.03
2.33
1.76
1.01
1.70
W = 0.03
ARF*
2.80E+05
1.50E+06
ARRF
0.31
1.45
15.26
15.22
4.02
3.39
2.05
3.35
ppm - tag
NA
NA
10.00
10.10
10.10
10.00
10.10
20.20
10.00
10.00
** Valid System Continuing Calibration QA are within 20% for 1 ppm.
No criteria have been established for system continuing calibrations at 300 ppb.
ppm-exp
NA
NA
0.30
0.30
0.30
0.30
0.30
0.61
0.30
0.30
ppm-obs
NA
NA
0.35
0.26
0.21
0.25
0.29
0.55
0.32
0.29
%Diff**
NA
NA
17%
-14%
-31%
-17%
-4%
-9%
7%
-3%
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APPENDIX A
DIRECT INTERFACE GCMS TEST METHOD
MANUFACTURERS CERTIFICATES OF ANALYSIS
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DETERMINATION OF GASEOUS ORGANIC COMPOUNDS BY DIRECT INTERFACE GAS
CHROMATOGRAPHY-MASS SPECTROMETRY
INTRODUCTION
This document describes the key elements of a. sampling and analytical method for measurement of specific
volatile organic hazardous air pollutants (VOHAPs) using a direct interface gas chromatograph/mass spectrometer
(GCMS) for on-site analysis of emissions from stationary sources. The method provides concentration measurement
results for the extracted gas samples. The performance-based approach validates each GCMS analysis by placing
boundaries on the instrument response to internal standards and their specific mass spectral relative abundances.
1.0 SCOPE and APPLICATION
1.1 Analytes This method employs a direct interface GCMS measurement system designed for the
identification and quantification of the specific 36 volatile organic compounds listed below. The method has potential to
be extended to many other compounds provided the performance criteria detailed in this method are met.
Benzene-71432 Dibromochloromethane-124481 Carbon Tetrachloride-5623 5
Bromodichloromethane-75274 1,1 -Dichloroethane-107062 Chlorobenzene-108907
Carbon Disulfide-75150 1,2-Dichloropropane-78875 c-l>Dichloropropene-10061015
Cloroform-67663 Ethyl benzene-100414 1,2,-Dichloroethane-156592
Methyl iso-ButylKetone-108101 Ethyl chloride-75003 l,l-Dichloroethene-75354
Styrene-100425 Methy lene Chloride-75092 t-1,2-Dichloroethene-156605
Tetrachloroethylene-127184 1,1,2,2-Tetrachloroethane-79349 Methyl Ethyl Ketone-78933
Toluene-108883 l,l,l-Trichloroethane-71556 2-Hexanone-591786
Bromoform-75252 l,l,2-Trichloroethane-79005 t-l,2-Dichloropropene-542756
Vinyl Acetate-108054 p-Xylene-106423 Trichloroethene-79016
Vinyl Chloride-75014 Bromomethane-74839 m-Xylene-108383
Chloromethane-74873 o-Xylene-95476
cis-1,2-Dichloroethene-156592
1.2 Applicability.
1.2.1 The method is applicable for the determination of the above listed compounds in emissions from
stationary sources. Individual volatile hazardous air pollutants (VOHAPs) are detected and quantified by direct interface
of a gas chromatograph/mass spectrometer (GCMS) measurement system to the source effluent. This method applies
specifically to full scan operation (between 45 and 300 amu) of the mass spectrometer.
1.2.2 The method is applicable to direct measurement of unconditioned sample streams having moisture
content less than the saturation value at applicable instrument operating limits. Sample streams having higher moisture
content require conditioning before introduction into the analytical instrumentation that prevents moisture condensation
within the instrument. Additional QA requirements are provided in the method for the analysis of polar, water-soluble
compounds
1.3 Method Range and Sensitivity.
1.3.1 The instrument range shall be sufficient to measure from 150 ppbv to 100 ppmv. Measurement of
concentrations outside of this range may be conducted provided that the specific performance requirements of the
method are met and either a) the concentrations used to prepare the three-point and conduct the continuing calibration
concentration are adjusted appropriately or b) the three-point calibration is extended to include additional
concentrations. The sensitivity of the GCMS measurement system for the individual target analytes depends upon, a)
the specific instrumental response for each target analyte, and the number of mass spectral quantification ions available,
b) the amount of instrument noise, and c) the percent moisture content of the sample gas.
1.4 Data Quality Objectives
1.4.1 The overall data quality objectives are to achieve an accuracy of ±20% and precision of ± 10% for each
October 27, 1997
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measurement value. Specific method performance criteria are detailed in Section 10 and listed in Tables 1, 2,3, and 4
Achieving the method performance criteria enable meeting the data quality objectives.
1.4.2 The mass spectrometer tune should be established according to the manufacturers written instructions.
1.4.2.1 If NIST Library search able mass spectra are needed to identify compounds not included in the three-
point calibration or to facilitate comparison with other mass spectral analyses, the mass spectrometer tune must be able
to produce mass spectra for bromofluorobenzene (BFB) that meet the relative abundance criteria listed in Table 2.
NIST Library search able spectra are not required for the quantification of target analytes.
1.4.2.2 Table 3 presents a specific example of applicable MS tune limits for the mixture of two recommended
internal standards (1,3,5 (TRIS) trifluoromethylbenzene and bromopentafluorobenzene (BPFB)). These criteria have
been demonstrated to produce an acceptable instrumental response for BFB. Table 4 presents a specific example of
applicable ion abundance criteria for the two co-injected, GC separated, internal standards. Proper and consistent
GCMS response is ensured in each run by meeting the Table 3 and Table 4 QA criteria.
1.4.3 An initial three-point calibration must be conducted to establish the instrument response for each target
analyte over the measurement range. At a minimum, duplicate GCMS analyses at each of three calibration levels are
required. The percent relative standard deviation (RSD) must be within 20% for these analyses. The signal to noise
ratio also must be sufficient to establish the target analytes responses at the lowest concentration level in full scan
operation. A signal to noise ratio of 10:1, and an average relative response factor >0.25 (Section 10. Equation 2) should
be sufficient. The same MS tune conditions, GC operating conditions, and data quantification procedures that are used
to establish the three-point calibration curve must be used also to acquire and quantify samples and to perform
continuing calibrations.
1.4.4 A system continuing calibration check must be conducted each day before performing effluent
measurements, before resuming sampling after each instrument shut down for maintenance or corrective action, and
before analyzing additional samples after twelve hours of continuous operation. The six surrogate check compounds
listed in Table 5 may be used to determine the validity of the three-point calibration curve for the 36 analytes listed in
1.1. Acceptable results are indicated if analysis of the continuing system calibration using the three-point calibration
curve produces results within ±20% of the expected value (i.e., manufacturer's certified value for compressed gas
standards). Acceptable continuing calibration results for each analyte or each surrogate allow use of the previously
developed three-point calibration for analysis of effluent samples for those analytes or for those analytes that correspond
to each surrogate (see Table 6).
1.4.5 A system continuing calibration check must be performed after each test run when analyzing for polar,
water-soluble compounds when moisture removal is used. (The polar-water soluble compounds include methyl ethyl
ketone, 2-hexanone, vinyl acetate, and methyl isobutyl ketone.) This continuing calibration check must be performed
immediately after sampling the effluent (i.e., while the potential for residual moisture in the sample conditioning
components is greatest). Unacceptable results for this continuing calibration check invalidate the run for polar, water-
soluble compounds. Such results may indicate loss of water-soluble compounds in the sample conditioning components.
Corrective action shall be taken before the next sample run. Specific sampling system designs that have been
demonstrated to achieve adequate sample recoveries for water soluble compounds at higher moisture levels than
encountered during the test are exempt from the requirement to conduct the post-test continuing calibration check.
(Such demonstrations can be accomplished by performing analyte spiking at elevated moisture levels. The tester shall
maintain documentation of such sampling system demonstrations.) For sampling systems that qualify for this exemption,
the effluent shall be sampled for a period of at least 15 minutes prior to conducting the system continuing calibration
check in 1.4.4.
2.0 METHOD SUMMARY
2.1 Analytical Principle. Gas chromatography (GC) is a means of separating gaseous mixtures of molecules
by their affinity for the column's stationary and mobile phases. Sample gas is introduced into the GCMS via a
pneumatic valve assembly or equivalent. In this application, an internal standard mixture must be quantitatively co-
added to every sample.
2.1.1 As molecules elute from the GC column, they must be separated from the mobile phase carrier gas and
enter the mass spectrometer. Because the GC operates at near ambient pressure and the MS operates at greatly reduced
pressure (approximately 1x10 Ton), an interface is required. Upon entering the mass spectrometer, separated
molecules are subjected to ionizing energy that causes an electron(s) to be ejected from the molecule. The result is a
positively charged molecule (for electron ionization) that fragments while achieving a stable electronic configuration
2.1.2 The mass spectrometer scans a defined mass range (from 45-300 amu in this application) enabling
detection of the individually charged fragments, which are virtually unique for every molecule. Positive identification of
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target analytes is achieved by; 1) comparing eluting analyte GC peak retention times in the total ion chromatogram to
those contained in the three-point calibration, and 2) by examining the mass spectral pattern of the eluted peaks.
2.1.3 The compounds listed in 1.1 and the internal standards can be separated and detected in a 10 to 15
minute isothermal GC run.
2.2 Sampling. The sample interface system must have a response time that provides a fully equilibrated
sample to the GCMS analyzer within the GC sample analysis cycle time. The sample interface system should include
provisions to facilitate direct calibrations of the GCMS instrument and system calibrations where calibration gases are
introduced at the extractive probe outlet, upstream of the primary particulate filter. The sample interface system also
must extract continuously effluent sample during the period between the consecutive GCMS sample acquisitions.
2.2.1 Sample Extraction. Sample is extracted from the stack or duct and passes through the enure sample
interface system at a constant rate. The sample interface consists of a heated primary particulate filter, a heated pump,
heated Teflon sample line, and sample conditioning unit. All sample extraction components must be maintained at
temperatures sufficient to prevent moisture condensation within the measurement system components. (Other sampling
techniques involving bags, canisters, adsorbents, etc. are not addressed by this method.)
2.2.2 Sample Conditioning. The conditioning unit is operated to protect the GCMS instrument from
particulate and other condensable mater and remove excess sample moisture, if necessary. The following information is
provided as an example of an acceptable arrangement. All components within the conditioning unit (except for the
condenser, if applicable) must be maintained at, or above, the temperature of the GC introduction valve assembly. The
secondary particulate filters should be maintained at a temperature approximating that of the GC introduction valve
assembly. Sample gases that are free of condensable acids and that contain less than the saturated moisture at the
highest dew point (i.e., lowest temperature, and highest pressure) within the instrument can be analyzed without
moisture removal by allowing the entire sample stream to bypass the condenser. Sample streams containing higher
moisture levels may be dried by directing the entire sample stream through the condenser to reduce the moisture content
to an acceptable level. Alternatively, a portion of the sample stream may be directed through the condenser and a
portion of the sample stream may bypass the condenser to reduce the loss of certain analytes. The flow of sample that
bypasses the condenser and the condenser operating temperature must be carefully chosen based on knowledge of the
unconditioned gas stream moisture content The flow rate of sample gas through the condenser and the total sample flow
rate must be monitored using calibrated precision rotometers and recorded.
2.2.3. Sample Transfer Line. A connection line that is heated to the temperature of the GC introduction valve
conveys sample gas exiting the conditioning unit to the GCMS analyze r. An internal sample pump within the GCMS
analyzer is required to draw sample gas through the connection line at a rate substantially less than the total sampling
rate. The excess sample gas exiting the conditioning unit must be vented at atmospheric pressure so that the inlet on the
connection line is not pressurized.
2.3 Operator Requirements. The operator should have rudimentary knowledge of the GCMS instrumental
operating conditions that are sufficient to determine if the operation is consistent with the data quality objectives of the
method.
3.0 DEFINITIONS
Refer to Appendix A of this document for a list of definitions.
4.0 INTERFERENCES
4.1 Analytical Interferences. Analytical interferences are defined as those interferences which result in
chromatographic peak and quantion overlap to such an extent that quantification of specific target compounds is
prohibited. The nature of the GCMS technique virtually eliminates analytical interferences.
4.2 Sampling System Interferences. Sampling system interferences prevent the transport of target analytes to
the instrumentation or have the potential to damage the measurement system components. Water, reactive particulate
matter, adsorptive sites within the sampling system components, and acid gases are examples of such potential sampling
system interferences. Specific provisions and performance criteria are included in this method to detect the presence of
sampling system interferences.
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5.0 SAFETY
5.1 Target Analytes. Many of the compounds listed in Section 1 are toxic and carcinogenic. Therefore.
exposure to these chemicals should be limited. Compound mixtures are contained in compressed gas cylinders, and the
appropriate safety precautions should be taken to avoid accidents in their transport and use.
5.2 Sampling Location. This method may involve sampling at locations having a high positive or negative
pressure, or have a high temperature, elevated height, or high concentration of hazardous or toxic pollutants.
5.3 Mobile or Remote Laboratory. A leak check of the sampling system and an inspection of sample exhaust
equipment should be performed before sampling the calibration standards or effluent to protect personnel in the
laboratory.
6.0 EQUIPMENT AND SUPPLES
The equipment and supplies are based on the generalized sampling system schematic shown in
Figure 1.
6.1 Instrumentation
6.1.1 Gas Chromatograph/Mass Spectrometer. A GCMS system capable of separating the analyte mixture and
detecting compounds having a 45-300 atomic mass unit (amu) range. This system must also include a means of co-
injectmg a gaseous internal standard mixture with sample gas at a precise and known ratio. A personal computer with
compatible GCMS software is needed for data quantification.
6.1.2 Data Acquisition System. A data acquisition system and appropriate software that enables the analyst to
acquire and quantify the target analytes and which allows for adequate storage of data.
6.2 Sampling System
6.2.1 Sampling Probe. Glass, stainless steel or other appropriate material of sufficient length and physical
integrity to sustain heating, prevent adsorption of analytes and to reach the gas sampling point.
6.2.2 Pump. A leak-free, heated head pump (KNF Neuberger or equivalent) capable of maintaining an
adequate sample flow rate (at least 1.51pm).
6.2.3 Calibration Assembly. Apparatus allowing the introduction of calibration gases into the sampling system
at the probe outlet, upstream of the primary paniculate filter. The apparatus shall be designed to ensure that calibration
gases are introduced at the same pressure as effluent samples or shall include provisions for monitoring the sample
pressure at the calibration introduction point both during calibrations and during effluent sampling. The calibration
assembly shall ensure that the calibration gases are at the same temperature as the sample gases at the introduction point.
6.2.4 Sampling,Line. Heated to a temperature sufficient to prevent sample condensation, and fabricated of
stainless steel, Teflon , or other material that minimizes adsorption of analytes and transports effluent to the GCMS.
The length of heated transport line should be minimized.
6.2.5 Sample Condenser System. Peltier Cooler (or equivalent) capable of reducing the moisture of the sample
gas to a level acceptable for sample injection.
6.2.6 Sample Flow Rotometers. Calibrated rotometers capable of withstanding sample gas conditions.
6.2.7 Sample Transfer Line. Sample line used to convey sample from the sample interface system to the inlet of
the GCMS instrumentftjion. Heated to a temperature sufficient to prevent sample condensation and fabricated of
stainless steel. Teflon , PEEK™, or other material to minimize adsorption of analytes. The length of heated transport
line should be minimized. TM
6.2.8 Paniculate Filters. A filter (Balston or equivalent) rated at 0.3 micron for paniculate removal is
required, and should be placed immediately after the heated probe, and at any place in the sampling system where the
physical conditions of the flue gas are changed (i.e. moisture removal).
6.3 Auxiliary Equipment
6.3.1 Calibration Gas Manifold. Gas manifold capable of delivering nitrogen or calibration gases through
sampling system, or directly to the instrumentation. The calibration gas manifold should include provisions to provide
for accurate dilution of the calibration gases as necessary.
6.3.2 Mass Flow Meters or Controllers. To measure accurately calibration gas flow rate. The
meters/controllers should have a stated calibrated range and accuracy (e.g., ±2% of scale from 0-500 cc/min or 0-5
L/min).
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6 3.3 Digital Bubble Meter (or equivalent). MIST traceable with an accuracy of ±2% of reading and with an
adequate range to calibrate mass flow meters or controllers and rotometers at the specific flow rates ±10% required to
perform the method.
63.4 Teflon Tubing. Diameter and length suitable to connect cylinder regulators.
6.3.5 Stainless Steel Tubing. 316, appropriate length and diameter for heated connections.
6.3.6 Gas Regulators. Appropriate for individual gas cylinders and constructed of materials that minimize
adsorption of analy tes.
7 0 REAGENTS AND STANDARDS
7.1 Calibration Gases. Compressed calibration gas standards having a manufacturer's certification of analysis
(i.e., a certified analytical accuracy) must be used for the initial calibration and for the continuing calibrations.
(Commercially available compressed gaseous standards typically carry manufacturer's certificates of analysis of ±5 to
±10% accuracy.)
7.2 Internal Standards. Gaseous internal standard mixtures for co-injection with sample gas having a
manufacturers certification must be used.
7.3 High Purity (HP) Nitrogen or Zero Air. For purging sample lines, sampling system components and for
performance of blank runs.
8.0 SAMPLE COLLECTION, PRESERVATION AND STORAGE
8.1 Initial Calibration. An initial three-point calibration for each target compound at nominal concentrations of
300 ppb, 1 ppm and 10 ppm must be prepared to quantify the GCMS data. There are two options available for
generating the necessary gas concentrations. (Because of the incompatibility of some target compounds, several
cylinders at each concentration are needed to construct a calibration for all of the 36 target analytes listed in 1.1.)
8.1.1 Option 1. Obtain calibration gas standards for the target compounds at the three specified concentration
levels.
8.1.2 Option 2. Obtain 10 ppm calibration standards for the target analy tes. Perform successive dilutions of the
10 ppm standard with nitrogen using mass flow meters that are calibrated against a NIST traceable digital bubble meter
at the specific flow rates (±10%) necessary for dilutions. Dilute the 10 ppm standard to 1 ppm and 300 ppb. If Option
2 is used, analyze the surrogate continuing calibration check standard (see Table 5), or other independent manufacturer's
certified gas standard, as a QA audit using the three-point calibration. The audit gas must be a separate gaseous
standard. Audit results using the calibrated GCMS must be within ±20% of the manufacturer's certified value for each
compound (or for each surrogate compound) to use the three-point calibration for analysis of those analytes (or those
analytes for which the surrogates represent).
8.1.3 Perform duplicate GCMS analysis at each concentration level. Calculate relative response factors (RRFs)
and average relative response factors (ARRF's) for each target compound at each concentration level (Section 10 Eq I
and 2). The %RSDs from the three sets of duplicate analyses must be within 20%.
Tables 1 -6 contain method QA/QC performance criteria for conducting initial three-point calibrations, and for
continuing calibration checks.
8.2 Pretest Preparations and Evaluations.
8.2.1 Flow Rate and Moisture Determination. Perform EPA Methods 1 through 3 if effluent flow rates are
required. Perform Method 4, or use wet-bulb dry-bulb measurements, saturation calculations or other applicable means
that will afford a moisture determination within ±2%. (If the moisture content of the flue gas is greater than the
applicable instrument operating limit, the sample gas must be conditioned before introduction into the GCMS.)
8.2.2 Sample Interface Preparation. Assemble the sampling system (Figure 1 is a generalized schematic of one
possible sampling system configuration). Allow the sample interface system components to reach operating
temperatures. Operate the sample interface system at a constant sampling rate during the entire test.
8.2.3 MS Tune. Perform the mass spectrometer instrumental tune according to the manufacturer's written
instructions. See criteria for the recommended TRIS/BPFB blend listed in Table 3.
8.2.4 Calibration. Perform the surrogate system continuing calibration check (or other continuing calibration
October 27, 1997
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check). The continuing calibration check standards must be introduced into the sampling system at the extractive probe
outlet, upstream of the paniculate matter filter. The standards must flow through the sampling system for a period
sufficient to ensure equilibration within the sampling system components but not longer than the GC run time. The
calibration check responses must agree to within ±20% of the manufacturers certified value for the compressed gas
standards. Tables 1, 3, and 4 contain calibration QA/QC criteria. Tables 5 and 6 provide surrogate compound
calibration check information.
8.2.5 System Zero Analysis. After performing the surrogate system continuing calibration, perform a system
zero by directing nitrogen or zero air through the entire sampling system including the paniculate filter. Analyze
nitrogen samples until the measurement system background levels are less than 50 ppb for the target analytes of interest.
8.3 Sampling
8.3.1 Sample Analysis. Extract effluent sample gas through the sampling system for a period equal to or greater
than GC run time before acquisition of the first sample. Perform sample analysis according to manufacturers written
procedures. Continuously extract the effluent between consecutive GCMS sample acquisitions to ensure constant
sample equilibration within the sample interface system. Each sample analysis shall represent the emissions
concentration over a period of approximately 15 minutes. The QA/QC criteria listed in Table 1 must be met for each
run.
8.3.2 Run Duration. Each test run shall be composed of a minimum of three samples, unless otherwise
specified in the applicable regulation. For sample run durations longer than 45 minutes, continue to acquire and analyze
additional samples for each 15 minute period.
8.4 Data Storage and Reporting. Identify all samples with a unique file name. Store backup copies of data files.
Report the results for the individual GCMS analyses, and the mean of all samples for each target analyte for each run.
Include copies of the three-point calibration including %RSD, RRFs and ARRFs, surrogate continuing system
calibration(s) results and other method QA/QC activities in the test report.
9.0 QUALITY CONTROL
9. ] Follow the manufacturer's written instructions for the set-up, tune, operation, and calibration of the GCMS
instrument and any sample interface equipment. All hardware or software settings of temperatures, pressures, and other
operational parameters used for sample acquisition and data quantification shall be the same as those used when
constructing the three-point calibration.
9.2 Records of the manufacturer's certificates of analysis for calibration standards and internal standards must
be stored and included in all test reports.
10 CALIBRATION AND STANDARDIZATION
10.1 Tune. Perform mass spectrometer tune according to the manufacturer's written instructions.
10.2 Initial Three-Point Calibration. Calibrate the GCMS with mixtures of the target analytes. The mixtures
should be prepared at nominal concentrations of 300 ppb, and 1 and 10 ppm in a balance of ultra high purity nitrogen
(the dilution technique described in Section 8. 1 .2 may be employed).
The internal standards must be coinjected with each external calibration standard. The flow mixture should
approximate a ratio of 1 : 10 (one part internal standard to 9 parts sample gas).
Analyze the three levels of standards in duplicate. Calculate the mean of the six relative response factors (RRFs)
for each target analyte and report as the average relative response factors (ARRFs). Table 1 contains the QA/QC
catena for valid initial and surrogate continuing system calibration checks. See the following equations for a complete
explanation.
Equation 1 . RRF = Relative Response Factor
RRF = (Aj/Ajs) x (Cis/Cx)
Ax = Peak area of selected target VOHAP quantion.
AJS = Peak area of corresponding selected internal standard quantion.
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Cjs = Concentration of corresponding selected internal standard.
Cx = Concentration of target VOHAP.
Equation 2: ARRF = Average Relative Response Factor
ARRF = (RRFj) In
RRFj = Individual RRFs calculated from calibration run.
n = 6
Equation 3: %RSD = Percent Relative Standard Deviation
%RSD=(sxlOO)/ARRF
s = Standard Deviation
The %RSD of the RRFs must be <20% for all target analytes to establish a valid calibration curve.
10.3 Surrogate Continuing (system) Calibration Check (CCC). A system continuing calibration check must be
performed each day before performing effluent measurements, before resuming sampling after each instrument shut
down for maintenance or corrective action, and before analyzing additional samples after twelve hours of continuous
operation. The surrogate continuing calibration mixture is a manufacturer certified gas standard that is not from the
same gas cylinder used to develop the initial three-point calibration. Alternatively, the continuing calibration check may
be performed for all of the target analytes using the mid-range concentration level used to develop the three-point
calibration. (Section 8.1.2 requires the use of an independent standard to audit the three-point calibration when
developed by dilution techniques.) Direct the continuing system calibration standard through the entire measurement
system including the paniculate filters, and calculate the %D.
Equation 4. %D = Difference of Results from Expected Value
%D = (Expected Value - Instrument Analysis Results)/Expected Value X 100
Expected Value = Certified Value of Cylinder
Instrument Analysis Results = Instrument output
The results from Equation 4 must be within ±20% of the manufacturers certified value for a successful continuing
calibration for all target analytes, or for all surrogates that represent those target analytes. Additionally, the response
factors of the internal standards must be within -50% to +100% of their average response factors obtained during the
initial three-point calibration. If these criteria are not met, corrective action must be taken. If the corrective action does
not result in a successful CCC, a new three-point calibration must be performed. Table 1 lists the acceptance criteria for
calibrations and quantification.
11 ANALYTICAL PROCEDURE
11.1 Sampling and Instrumental Analysis. Refer to Figure 2 for method operation flowchart.
October 21, 1997
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12 DATA ANALYSIS AND CALCULATIONS
1 2. 1 Quantitation of Results. Use the following equation to quantify the concentration of VOHAPs in gas samples.
5) ppmv Target VOHAP = parts per million by volume of target VOHAP in sample
ppmv Target VOHAP =
Ax = Peak area of target VOHAP quantion.
Ais = Peak area of corresponding selected internal standard quantion.
Cjs = Concentration of corresponding selected internal standard.
ARRF = Average Relative Response Factor of target VOHAP calculated from three-point calibration.
The internal standards used to quantify the results and the individual quantification ions used must be identified in the
test report.
12.2 Alternative Quantification Calculations. Alternative quantification algorithms may be used in the
development of calibration files and sample analysis quantification. For example, regression analyses may be performed
to determine the "best fit line" for the three-point calibration responses for each analyte rather than relying on the
average relative response factor. In some cases, calculation procedures allowing a non-zero y-axis intercept may
improve the accuracy of measurement results. Such procedures may show improvement of the RSDs for the three-point
calibration. For each analyte, a consistent numerical procedure must be applied in developing the three-point calibration
and in performing all sample analysis for the test series.
13 METHOD PERFORMANCE
13.1 Instrument Performance. Gaseous internal standards must be co-injected with every sample. The internal
standards are used to verify continuously the tune status and GC performance. Tables 1, 3 and 4 specify criteria to
ensure meeting the overall method data quality objectives.
14 POLLUTION PREVENTION
Take appropriate measures to prevent excess venting of calibration standards to the atmosphere.
15 REFERENCES
1 ). Method 624 - Purgeables, U.S. EPA 40 CFR part 1 36, App. A, (49 FR 43234), October 26, 1 984.
2). "EPA Method Study 29 EPA Method 624 - Purgeables," EPA 600/4-84-054, National Technical Information
Service, PB84-209915, Springfield, Virginia 22161, June 1984.
3). Method 1624 - Volatile Organic Compounds by Isotope Dilution GCMS, U.S. EPA Office of Water Regulations
and Standards, Industrial Technology Division, Office of Water, June 1 989.
4). Peeler, J.W., Kinner, L.L., and DeLuca, S., "General Field Test Method Approval Process and Specific
Application for a Direct Interface GCMS Source Test Method," Air and Waste Management Association, Nashville,
TN, 96-RP 132.01, June 23-28, 1996.
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5) Kinner. L.L., and Peeler. J.W, "Evaluation of HAPSITE and a Direct Interface GCMS Test Method for
Measurement of Volatile Organic Compounds in Stationary Source Emissions" Prepared for Leybold Inficon Inc., July
1997.
16 TABLES, FIGURES AND FLOWCHARTS
16.1 Table 1. Table 1 outlines the method QA/QC criteria.
16.2 Table 2. Table 2 outlines the mass spectral relative abundance criteria for BFB.
16.3 Table 3. Table 3 outlines recommended tune criteria for a blended mixture of BPFB/TR1S
16.4 Table 4. Table 4 outlines recommended mass spectral relative abundance criteria for the
GC separated BPFB and TRIS.
16.5 Table 5. Table 5 contains the surrogate continuing system calibration compounds.
16.6 Figure 1. Figure 1 illustrates a generalized sampling system diagram.
16.7 Figure 2. Figure 2 is a flowchart representing the GCMS operational method.
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TABLE 1. Calibration and Sampling QA/QC Criteria
Operational
Mode
IS
Recommended
Requirements
GC Retention Time
Requirements
Extracted Ion Chromatographic
Criteria
Accuracy and Sensitivity
Mass
Spectrometer
Tune
See Table 3
Three-Point
Calibration
See Table 4
RTs for individual
VOHAPS must be within
±6% of each other from
run to run.
% RSDs calculated from the
individual RRFs at each
calibration point must be
±20% for each target analyte.
The RFs of the internal
standards must be within -50
%- 100% of the mean for the
initial three-point
calibration.
ARRFs must be 30.25 to ensure
proper instrumental response.
A signal to noise of 10:1 is
recommended for the low
concentration level.
Surrogate
Continuing
Calibration
Check (CCC)
See Table 4
RTs for individual
VOHAPS must be within
±6% of the initial
three-point
calibration.
The RFs of the internal
standards must be within -50
%- 100% of their ARFs from
the initial three-point
calibration.
Surrogate Continuing System
Calibration results must be
within ±20% of the
manufacturers certified value
from analysis by the three-
point calibration for valid
continuing calibration.
Sampling
See Table 4
RTs for detected VOHAPS
must be within ±6% of
those in the initial
three-point
calibration.
The RFs of the internal
standards must be within -50
%- 100% of their ARFs from
the initial three-point
calibration.
Spectral ions of greater than
10% abundance in the
identified compounds mass
spectrum must also be
contained in the reference
calibration spectrum for that
particular target analyte.
October 27, 1997
10
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Table 2. Relative Ion Abundance Criteria for Bromofluorobenzene
Mass Fragment
50
75
95
96
173
174
175
176
177
ION ABUNDANCE CRITERIA
15-40%
30-60%
Base Peak
5-9% of mass 95
<2% of mass 174
>50% of mass 95
5-9% of mass 174
>95% but <101% of mass 174
5-9% of mass 174
Table 3. Instrument Performance for Blended TRIS/BPFB Internal Standard Mixture in Tune
Mass Fragment
50
55
69
93
117
167
248
263
282
Percent Relative Low
Abundance
5
5
33
39
100
50
30
20
10
Percent Relative High
Abundance
8
8
36
45
100
65
99
50
30
Table 4. Instrument Performance for Separated Internal Standard Mixture
Internal Standard
Tris
BPFB
Mass
50
69
75
213
263
282
93
117
167
245
246
247
248
249
Ion Abundance Criteria
5-20% of mass 69
Base Peak
40-60% of mass 69
50-90% of mass 69
75-95% of mass 69
30-70% of mass 69
20-50% of mass 117
Base Peak
45-75% of mass 117
< 2% of mass 246
> 25% of mass 117
5-9% of mass 246
> 25% of mass 117
5-9% of mass 248
October 27, 1997
11
-------
Table 5 Surrogate System Continuing Calibration Compounds
COMPOUND
Methylene
Chloride
Methyl Ethyl
Ketone (MEK)
Carbon
Tetrachlorlde
Toluene
Chlorobenzene
O-Xylene
CLASS
REPRESENTING
Chlorinated
Polar
Chlorinated
Aromatic
Chlorinated
Aromatic
Aromatic
MOLECULAR
WEIGHT
84
72
152
92
112
91
QUANT -I ON
84
72
117
91
112
91
RETENTION TIME
2:41 mins
2:57 mins
3:35 mins
5:08 mins
7:22 mins
9:44 min
October 27, 1997
12
-------
Table 6 Surrogates and Corresponding Analytes
Compound
Chloromethane
vinyl chloride
Bromomethane
Chloroethane
Methvlene Chlonde
1,1-dichloroethene
carbon disulfide
t- 1 ,2-dichloroethene
1 . 1 -dichloroethane
vinyl acetate
Methyl Elhvl Ketone
c- 1 ,2-dichloroethene
chloroform
1.2-dichloroethane
1 , 1 , 1 -tnchloroethane
benzene
carbon tetrachloride
1 ,2-dichloropropane
bromodichloromethane
trichloroethene
c- 1 ,2-dichloropropene
MffiK
t- 1 ,2-dichloropropene
1 , 1 ,2-trichloroethane
Toluene
2-hexanone
dibromochloromethane
Tetrachloroethvlene
chlorobenzene
ethylbenzene
bromoform
p-xvlene
m-xvlene
styrene
1 , 1 ,2,2-tetrachloroethane
0-xvlene
Retention
Time*
:09
:11
:13
:15
:25
:25
:31
:34
:36
:36
:40
:44
1:48
:58
2:01
2:10
2:12
2:25
2:29
2:30
2:54
2:56
3:12
3:17
3:31
3:48
3:49
4:33
5:27
6:07
6:28
6:30
6:30
7:17
7:30
7-31
Suggested Quantion
50
62
94
64
49
61
76
96
63
86
72
61
83
62
97
78
117
63
129
95
75
85
75
83
91
58
129
94
77
91
173
91
91
104
83
91
Surrogate
Methvlene Chloride
Methvlene Chloride
Methvlene Chlonde
Methvlene Chloride
Methvlene Chloride
Methvlene Chloride
Toluene
Methvlene Chloride
Methvlene Chloride
MEK
MEK
Methvlene Chloride
Methvlene Chloride
Methvlene Chloride
Methvlene Chloride
Toluene
Carbon Tetrachloride
Carbon Tetrachloride
Carbon Tetrachloride
Carbon Tetrachloride
Carbon Tetrachloride
MEK
Carbon Tetrachloride
Carbon Tetrachloride
Toluene
MEK
Carbon Tetrachloride
Carbon Tetrachloride
Chlorobenzene
Toluene
Carbon Tetrachloride
o-xvlene
o-xvlene
o-xvlene
Carbon Tetrachloride
o-xvlene
Suggested Surrogate
Quantion
49/84
49/84
49/84
49/84
49/84
49/84
91/92
49/84
49/84
72
72
49/84
49/84
49/84
49/84
91/92
117
117
117
117
117
72
117
117
91/92
72
117
117
112
91/92
152
91
91
91
117/152
91
* Retention Time based on a 60 C isothennal separation on a SPB - 1 GC Column, 30 meters long, 0.32 mm ID,
1 micron film thickness
October 27, 1997
13
-------
APPENDIX A - DEFINITIONS
AMU = Atomic Mass Unit, molecular weight of positively charged fragmented ions detected by mass
spectrometer electron multiplier.
ARRF = Average Relative Response Factor (see Section 10.2, equation 2)
Blank Analysis = Injection of zero air or nitrogen into the GCMS to determine background levels of the target
analytes.
BFB = Bromofluorobenzene, A standard mass spectrometer tuning compound.
BPFB = Bromopentafluorobenzene, one of the recommended internal standards.
CCC = Continuing calibration check. Performed before each testing day, before resuming sampling after
instrument shutdown or malfunction, and before continuation of sampling after 12 hours of continuous
instrument operation. •
GC = Gas Chromatograph
GCMS = Analytical technique using a mass spectrometer as a GC detector.
Internal Standard (IS) = Compounds used as markers in the analysis of GCMS data. The purpose of the
internal standards is to correct for hardware related error such as, different injection volumes, operational
temperature fluctuations, and electron multiplier drift.
MS = Mass Spectrometer
ppbv = Parts per billion by volume
ppmv = Parts per million by volume
Quantion - Quantification ion, A specific ion in the analytes mass spectrum that is used for quantification.
RRF = Relative Response Factor (see Section 10.2, equation 1)
RT = Retention time, the time corresponding to the elution of a peak (scan number) from the chromatographic
column measured from the injection point.
System Calibration = A means of injecting the calibration standard(s) through the entire sampling system. In a
system calibration, the sample pump draws calibration gas only through the sampling system. See Figure 1.
System Zero = A means of injecting dry nitrogen or zero gas through the entire sampling system to determine
the system background levels of the target analytes.
Three-point calibration = The initial instrument calibration using 300 ppb, 1 and 10 ppm VOHAP mixture
standards.
TRIS = 1,3,5-trifluoromethylbenzene, One of the recommended internal standards
October 27, 1997
16
-------
Primary Particulate Filter
Heated Extractive Probe
Atmospheric vent
Heated Sample
Transport Line
Analytical
Instumentation
Contains moisture
removal apparatus
Flow Meters
Calibration Gas and
Dilution Manifold
Sample Flow = Q1
Probe
Primary Particulate Filter
Total System Flow
*" Qf=Q1+Q2
Calibration Ga's flow = Q2
A = Heated Calibration Assembly
Total System Flow = Qf
Surrogate Calibration Gas Flow
Q2>Qf
Heated Head Pump
Figure 1. Example Sample Interface System and Plumbing Schematic for Surrogate System Continuing Caiibratic
-------
Warm-up
Establish Stable Operations
retune
no
yes
Tune/Mass Alignment
Tune criteria met?
no
Check Tune
yes
3-Point Calibration
- Do RT values replicate?
- Do IS meet criteria?
- Sensitivity (S/N) sufficient
for required measurement
range?
- %RSD criteria met for RRFs?
no
no
yes
Surrogate System Continuing Calibration
- Do RT values replicate?
- Do IS meet criteria?
- (S/N) sufficient
- Do results meet 20% criteria and
indicate valid three-point calibration?
0)
P
CL
CO
z
yes
no
System Zero
Is 50 ppb system
zero criterion met?
yes
Sampling/Analysis
Do RT values meet criteria'
Do IS meet criteria?
yes
Continue Sampling
After 12 hours of continuous
operation, instrument shut-do
or malfunction
Figure 2. Method Operational Procedure
-------
SPECTRR GflSES
277 Coit Street • Irvington. NJ 07111 USA Tel: (973) 372-2060 • (800) 929-2427 • Fax: (<
SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL: (908) 454-7455
SHIPPED TO:
Emission Monitoring Inc.
416 Emery Wood Drive
Raleigh, NC27615
"To
CERTIFICATE
OF
ANALYSIS
li/C
'-><>. u -7 3<-i^
SGI ORDER #: 133913
ITEM*: 1
CERTIFICATION DATE: 6/18/98
P.O.* : Verbal - Laura
BLEND TYPE: CERTIFIED
CYLINDER #: CC91245
CYLINDER PRES: 2000 psig
CYLINDER VALVE: CGA 350
ANALYTICAL ACCURACY: + / - 2%
COMPONENT
REQUESTED GAS
CONC
ANALYSIS
1,3-Butadiene
Hexane
Benzene
Toluene
Ethylbenzene
P-Xylene
M-Xylene
Styrene
O-Xylene
10.0 ppm
10.0 ppm
10.0 ppm
10.0 pprr
10.0 ppm
10.0 ppm
10.0 ppm
10.0 ppm
10.0 ppm
10.0 ppm
10.1 ppm
10.1 ppm
10.0 ppm
10.1 ppm
10.1 ppm
10.1 ppm
10.0 ppm
10.0 ppm
Nitrogen
Balance
Balance
ANALYST:
Ted Neeme
DATE:
6/18/98
USA • United Kingdom • Germany • Japan
-------
PAGE
Scott Specialty Gases
lipped
From:
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
PA 18949-0310
CERTIFICATE OF
PO BOX 310
Fax: 215-766-2070
ANALYSIS
LEYBOLD INFICON INC
DR.LAURA KINNER
C/0 EMMISSIONS MONITORING
301 EAST DURHAM RD.
GARY NC 27513
PROJECT #: 01-65495-001
P0#: P61339
ITEM #: 0102AE004204AL
DATE: 3/08/95
CYLINDER #: ALM057596
ANALYTICAL ACCURACY: +/-5%
BLEND TYPE : CERTIFIED MASTER GAS
COMPONENT
ACETONE
BENZENE
BROMODICHLOROMETHAN E
CARBON DISULFIDE
CHLOROFORM
ETHYLENE
METHYL ISOBUTYL KETONE
STYRENE
SULFUR HEXAFLUORIDE
TETRACHLOROETHYLENE
TOLUENE
TRIBROMOMETHANE
VINYL ACETATE
VINYL CHLORIDE
NITROGEN
REQUESTED GAS
CONG
1.
1.
1.
1.
1.
100.
1.
1.
1.
1.
1.
1.
1.
1.
MOLES
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
ANALYSIS
f MOLES)
.938
1.04
1.01
.924
1.07
100.
1.01
1.06
1.00
1.04
1.05
.995
.921
1.01
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
— e
o
<§?
ANALYTICAL METHOD: GC-FID/GC-FPD
ANALYST:
JAMES T. KRAUS
FREMONT CA SAN BERNARDINO. CA IONGMONT CO I HOY Ml CHtCAOO. «. SARMA. ONTARIO HOUSTON rx
OURHAM NC PIUMSTEAOVK.LE. PA SOUOIPLAINFIELO.NJ WAKEFIEIO. MA onEOA. TMENETHEIILANUS si«Frono IUIFAT nntfiAN
-------
PAUL
Scott Specialty Gases, Inc.
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
PA 18949-0310
CERTIFICATE OF
PO BOX 310
Fax: 215-766-2070
ANALYSIS
LEYBOLD INFICON INC
C/0 ENTROPY ENVRNMNTLSTS
8724 GLENWOOD AVENUE
RALEIGH
NC 27612
PROJECT #: 01-60491-002
P0#: P56873
ITEM ff: 0102AK004104AL
DATE: 9/28/94
CYLINDER #: ALM034607
ANALYTICAL ACCURACY: +/- 2%
(p
BLEND TYPE : CERTIFIED MASTER GAS
COMPONENT
—ACETONE
^BENZENE
BROMODICHLOROMETHANE --
-.rCARBON DISULFIDE
CHLOROFORM-*
—ETHYLENE
•^METHYL ISOBUTYL KETONE
—STYRENE
SULFUR HEXAFLUORIDE-
^TETRACHLOROETHYLENE
-TOLUENE
-TRIBROMOMETHAN E~
^VINYL ACETATE
•-VINYL CHLORIDE
NITROGEN
REQUESTED GAS
CONG MOLES
10,
10,
10,
10,
10,
100.
10.
10.
1,
10.
10.
5.
10.
10.
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
ANALYSIS
I MOLES1
10
1
9.97
9.97
9.27
9.98
100.
10.1
9.99
1.01
10.2
9.99
5.38
10.
10.
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
ANALYTICAL METHOD: GC - FID
•: Cl 7- X.
ANALYST!
JAMES T. KRAUS
FREMONT CA SAN MMMMMNO CA IONOMONT CO TPOV. Ml CtflCAOO.lt. SARMA. ONTARIO AVON LAKE. CXI HOUSTON. TX
BATON nOUGE. LA MAMCTTA. QA OOHHAM. NC PIUMSTCAOVHU. PA SOUTH «. AMFKLO. Ml WAKEriClO. MA HflLOA. IIIF NTtllini ANUS
-------
A Scott Specialty Gases, Inc.
JTFTpped
From:
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
PO BOX 310
PA 18949-0310
CERTIFICATE OF
Fax: 215-766-2070
ANALYSIS
LEYDOLD INFICON INC
C/O ENTROPY ENVRNMNTLSTS
8724 GLENWOOD AVENUE
RALEIGH
NC 27612
PROJECT Ii 01-60729-008
PO#: P5GB73
ITEM #: 0102DF004504AL
DATE: 9/26/94
CYLINDER #: ALM050124
ANALYTICAL ACCURACY: +/- 5%
BLEND TYPE : CERTIFIED MASTER GAS
COMPONENT
BROMOMETHANE
CARBON TETRACHLORIDE
CHLOROBENZENE
CIS 1,3-DICHLOROPROPENE
1,2-DICHLOROETHANE
1,1-DICHLOROETHENE
ETHYLENE
ETHYLENE 1,2 DICHLORO (TRANS)
METHYL ETHYL KETONE
METHYL N-BUTYL KETONE
SULFUR HEXAFLUORIDE
TRANS 1,3-DICHLOROPROPENE
TRICHLOROETHYLENE
M-XYLENE
O-XYLENE
NITROGEN
REQUESTED GAS
CONG MOLES
1.
1.
1.
1.2
1.
1.
100.
1.
1.
1.
1.
.8
1.
1.
1.
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
ANALYSIS
( MOLES!
.918
.901
.999
1.31
1.91
.975
93.9
.936
1.04
1.05
.978
.936
.954
1.06
1.09
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
ANALYTICAL
ANALYST:
HOD: GC - FID
T. KRAUS
IONOMONTCO r"°¥Mt CHCAOO.ll SAnNU.ONTATO AVONUWE.OH HOUSTON TX
OA DURHAM. NC PIOMSIEAOVHU. FA SOUTH PUUNFiet.0. NJ WAKEFCIO. MA OHEOA.
-------
PAGE
Scott Specialty Gases, Inc.
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
PA 18949-0310
CERTIFICATE OF
PO BOX 310
Fax: 215-766-2070
ANALYSIS
LEYBOLD INFICON INC
C/0 ENTROPY ENVRNMNTLSTS
8724 GLENWOOD AVENUE
RALEIGH NC
27612
PROJECT #: 01-60729-007
PO#: P56873
ITEM #: 0102BF004404AL
DATE: 9/27/94
CYLINDER #: ALM050128
ANALYTICAL ACCURACY: +/- 2%
BLEND TYPE : CERTIFIED MASTER GAS
COMPONENT
BROMOMETHANE "'
CARBON TETRACHLORIDE —
\XiHLOROBENZENE
,CIS 1,3-DICHLOROPROPENE
1,2-DICHLOROETHANE -
- 1,1-DICHLOROETHENE
/ETHYLENE
,/ETHYLENE 1,2 DICHLORO (TRANS)
/'METHYL ETHYL KETONE
.^METHYL N-BUTYL KETONE
SULFUR HEXAFLUORIDE
yTRANS 1,3-DICHLOROPROPENE
/TRICHLOROETHYLENE
^M-XYLENE
6-XYLENE
NITROGEN
REQUESTED GAS
CONG
10.
10.
10.
12.
10.
10.
100.
10.
10.
5.
1.
8.
10.
10.
10.
MOLES
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
ANALYSIS
( MOLES)
9.04
9.20
9.86
12.1
18.4
10.0
98.3
9.62
9.57
5.11
.983
8.36
9.56
9.18
9.18
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
ANALYTICAL^HSTHOD: GC - FID
ANALYST:
JAMES T. KRAUS
CA SANBCnNAnOINOCA IONOMONT.CO inOV.MI CIMCAOO.il SAflNU ONFAHIO AVONIAKE.OH HOUSTON. TX
,,^ri» M«r»iFrr« r.n numi.u NT PUMRTMnvtUE. PA SOUTHFLAMFIELD.HI WAKEFIEIO.MA Of*lM. It* NEMICnLANUS
-------
PAG I
Scott Specialty Gases, Inc.
snipped
From:
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
PO BOX 310
PA 18949-0310
CERTIFICATE OF
Fax: 215-766-2070
ANALYSIS
LEYBOLD INFICON INC
C/O ENTROPY ENVRNMNTLSTS
8724 GLENWOOD AVENUE
RALEIGH
NC 27612
PROJECT #: 01-60491-01
POJ: P56873
ITEM #: 0102CE000504AL
DATE: 9/27/94
I
CYLINDER #: ALM050069 ANALYTICAL ACCURACY: +/- 5%
i^~~
BLEND TYPE : CERTIFIED MASTER GAS
REQUESTED GAS ANALYSIS
COMPONENT
CHLOROMETHANE
CIS 1 , 2-DICHLOROETHYLENE
DIBROMOCHLOROMETHANE
1 , 1-DICHLOROETHANE
1 , 2-DICHLOROPROPANE
ETHYLBENZENE
ETHYL CHLORIDE
ETHYLENE
METHYLENE CHLORIDE
SULFUR HEXAFLUORIDE
1,1,2, 2-TETRACHLOROETHANE
1,1, 1-TRICHLOROETHANE
1,1, 2-TRICHLOROETHANE
P-XYLENE
NITROGEN
CONG
1.
1.
1.
1.
1.
1.
1.
100.
1.
1.
1.
1.
1.
1.
MOLES
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
f MOLES)
1.00
1.01
.982
1.02
1.01
.992
.986
100.
1.01
1.00
1.03
1.03
1.00
.983
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
ANALYTICAL METHOD:
ANALYST
T. H. RICHARDS
FREMONT CA SANBERNAROMO.CA IONOMONT.CO TROY. Ml CHICAGO. N. SARMA. ONTARIO AVON LAKE. OH HOUSTON. TX
BATON ROUOE. LA MARIETTA. OA OUWHAM.NC PIUMSTEAOVS.LE. PA SOUTH njUNTIELO. HI WAKCflEU). MA IW1EOA HIE NETHEnLANOS
-------
PAGE
Scott Specialty Gases, Inc.
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
CERTIFICATE
PO BOX 310
PA 18949-0310
O F
Fax: 215-766-2070
ANALYSIS
LEYBOLD INFICON INC
C/0 ENTROPY ENVRNMNTLSTS
8724 GLENWOOD AVENUE
RALEIGH
NC 27612
PROJECT I: 01-60491-012
PO#: P56873
ITEM #: 0102CE000404AL
DATE: 9/30/94
CYLINDER #: ALM050123
ANALYTICAL ACCURACY: +/- 2%
BLEND TYPE : CERTIFIED MASTER GAS
COMPONENT
CHLOROMETHANE
CIS 1,2-DICHLOROETHYLENE
DIBROMOCHLOROMETHAN E
1,1-DICHLOROETHANE
1,2-DICHLOROPROPANE
ETHYLBENZENE
ETHYL CHLORIDE
ETHYLENE
METHYLENE CHLORIDE
SULFUR HEXAFLUORIDE
1,1,2,2-TETRACHLOROETHANE
1,1,1-TRICHLOROETHANE
1,1,2-TRICHLOROETHANE
P-XYLENE
NITROGEN
REQUESTED GAS
CQNC MOLES
10,
10.
10.
10.
10.
10.
10.
100.
10.
1.
5.
10.
10.
10.
ANALYSIS
fMOLES
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
9.99
10.0
9.97
9.96
9.98
10.0
9.98
101.
9.99
1.
5.09
9.98
9.99
10.
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
PPM
BALANCE
ANALYTICAL METHOD: GC - FID
o ~
ANALYST:
181
JAMES T. KRAUS
IONOMOWCO "«».•• OflCAOO.il SAflMA ONTAHIO AVONLAKS.OH HOUSTON tX
OA OUBHAM. NC PIUMSTEAOVHIE. PA SOUTH PUUNFIEID. HI WAK6FIELD.MA WKOA. 1IIE NSntentANOS
-------
PAGE
ScottSpecialty Gases
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
PA 18949-0310
CERTIFICATE OF
PO BOX 310
Fax: 215-766-2070
ANALYSIS
SCOTT SPECIALTY GASES
C/0 EMISSION MONITORING
301 EAST DURHAM ROAD
CARY
PROJECT #: 01-69630-001
P0#: 6/26/95
ITEM #: 0102B3012914AL
DATE: 7/12/95
NC 27513
CYLINDER #: ALM035013
ANALYTICAL ACCURACY: +/-!%
BLEND TYPE : CERTIFIED MASTER GAS
COMPONENT
DROMOPENTAFLUOROBENZENE
135TRIS(TRIFLUOROMETHYL)BENZEN
NITROGEN
REQUESTED GAS
CONG VOLUME
50. PPM
100. PPM
BALANCE
ANALYSIS
(VOLUME1
51.5 PPM
102.5 PPM
BALANCE
ANALYST:
T),,,
APPROVED BY
KEN WONG
PAUL PAINTER
FREMONT. CA SAN BERNARDINO. CA IONOMONT.CO TROY. Ml CHICAGO, 1 SARMA. ONTARIO HOUSTON. TX
DURHAM NC C1UMSTEADVM.E.PA SOUTH PtAINDElO. NJ WAKEFCLO. MA RREOA. TflE NETIIEnLANOS SHEtrOnO ORFAt nfHllAM
-------
APPENDIX B
THREE-POINT CALIBRATION RAW DATA
-------
Title:
FULL SCAN DATA ;
Acquired
Peak Search Method
PQUAN Library
Last Calibration
Kesponse Table
C:\PROGRA>Jr\HAPSRUN\DATA\AAA\LFSCALS\ICCR300C
07/09/:
14:59:36
C:\PROGRA~1\HAPSRUN\METHOD\AAA.LSM
C: \PROGRA~1\HAPSRUN\METHOD\AAA
07/10/98 at 09:04:28
C : \ PROGRA- 1 \HAPSRUN\METHOD\LLKLFS . FSM
Acquisition Method
Tune/Cal File :
Datafile title:
ICCR - New Gas
10 ppm diluted to 0.3 ppm
Can E
W = RT +- ( 0:45.00 / 2 + RT * 0.010 )
Min Fit=0.650; Min Pur=0.650; Min Area=5000
Width= 5-100 scans; Res= 6 scans; NLM=2.0
Linear calibration curve
Internal Standards:
I.S. #1 ~ TRIS
Concentration = 9.940 ppm; 6 calib points
pt. File Man.
1 ICCR10A
2 ICCR10B
3 ICCR001A
4 ICCR001B
5 ICCR300A
6 ICCR300C
Area
2932843
2980580
2687084
2851831
2577534
2657386
Average RF •
Resp. Factor
295054.61191
299857.12675
270330.36777
286904.51175
259309.24160
267342.64157
= 2.79800e+05
I.S. #2 -- BPFB
Concentration = 4.850 ppm; 6 calib points
pt. File Man.
1 ICCR10A
2 ICCR10B
3 ICCR001A
4 ICCR001B
5 ICCR300A
6 ICCR300C
Area
7776438
8196344
7124059
7288881
6679921
6,69^100
Average RF
Resp. Factor
1603389.30988
1689967.86828
1468878.17321
1502862.09141
1377303.32605
1379608.27455
= 1.50367e+06
Analytes:
Analyte #1 — 1,3-butadiene
5 calib points
pt. File M I Cone. Cratio
1 ICCR10A I 10.00 1.006e+00
2 ICCR10B I 10.00 1.0066+00
Area Aratio
933824 3.184e-01
1041395 3.494e-01
Resp. Factor
3.16492e-01
3.47297e-01
-------
4 ICCR001B |
5 ICCR300C I
1.00 1.006e-01
1.00 1.006e-01
0.30 3.018e-02
70864
90859
24371
2.637e-02
3.186e-02
9.171e-03
I
2.62139e-C
3.16687e-C
3.03867e-C
Average RF = 3.09296e
Deviation = 7.45103%
Analyte #2 — Hexane
6 calib points
pt. File M I
1 ICCR10A |
2 ICCR10B |
3 ICCR001A |
4 ICCR001B |
5 ICCR300A |
6 ICCR300C I
Cone:. Cratio
10.10 1.016e+00
10.10 1.016e+00
1.01 1.016e-01
1.01 1.0166-01
0.30 3.048e-02
0.30 3.048e-02
Area
4530171
4970370
391153
435586
106016
100366
Aratio I
1.545e+00 I
1.668e+00 I
1.456e-01 !
1.527e-01 I
4.113e-02 |
3.777e-02 1
Average RF
Deviation
Resp. Factc
1.52017e+C
1.64117e+C
1.43262e+C
1.503196+C
1.349316+0
1.239016+0
1.447586
6.39510%
Analyte #3 — Benzene
6 calib points
pt. File M
1 ICCR10A
2 ICCR10B
3 ICCR001A
4 ICCR001B
5 ICCR300A
6 TCCR300C
Cone. Cratio I Area
10.10 1.016e+00 | 45438832
10.10 1.0166+00 I 4793300Q
1.01 1.016e-01 I 4294511
1.01 1.0166-01 | 4451729
0.30 3.048e-02 | 1190114
0.30 3.048e-02 I 1157577
Aratio I Resp. Facto
1.549e+01 I
1.6Q8e+Ql I
1.598e+00 I
1.5616+00 I
4.617e-01 i
4.356e-01 I
Average RF
Deviation
1.52477e+0
1.58270e+0
1.57289e+0
1.53628e+0
1.514706+0
1.42902e+Q
= 1.52673e
= 3.14150%
Analyte #4 — Toluene
6 calib points
pt. File M !
1 ICCR10A |
2 ICCR10B I
3 TCCR001A |
4 ICCR001B I
5 ICCR300A I
6 ICCR300C |
Cone. Cratio
10.00 1.006e+00
10.00 1.006e+00
1.00 1.Q06e-01
1.00 1.0066-01
0.30 3.018e-02
0.30 3.018e-02
Area
50571376
53416740
4199091
4247383
1036666
1019161
Aratio I Resp. Facto
1.724e+01 I 1
1.792e+01 I 1
1.5636+00 I 1
1.489e+00 I 1
4.022e-01 I 1
3.835e-01 ! 1
Average RF =
Deviation. =
.71397e+0
.78141e+0
.55332e+0
.48042e+0
.33260e+0
. ?7073p+0
1.52?.07e
3.30817%
Analyte #5 — Ethyl Benzene
6 calib points
pt. File M
1 ICCR10A
2 TCCR10B
3 ICCR001A
4 ICCR001B
5 TCCR300A
6 TCCR300C
Cone. Cratio
10.10 2.082e+00
10.10 2.08?e+00
1.01 2.082e-01
1.01 2.082e-01
0.30 6.247e-02
0.30 6.247e-02
Area
79391136
819?59?8
5884071
6047727
1419815
1288873
Aratio
1.021e+01
9.995P+00
8.2596-01
8.297e-01
2.125e-01
1.926e-01
Resp. Facto
4.90243e+0
4 .79Q7Re+0
3.96616e+0
3.984306+0
3.40220e+0
3.08327e+0
Average RF = 4.023Q2e
Deviation = 2.05843%
Analyte #6 — m/p-Xylene
6 calib points
pt. File M | Cone.
Cratio
Area
Aratio I Resp. Facto
-------
2 ICCR10B
3 ICCR001A
4 ICCR001B
5 ICCR300A
6 ICCR300C
Analyte #7 -- Styrene
6 calib points
pt. File M I
1 ICCR10A |
2 ICCR10B |
3 ICCR001A |
4 ICCR001B |
5 ICCR300A |
6 ICCR300C I
Analyte #8 — 0-Xylene
6 calib points
pt. File M |
1 ICCR10A |
2 ICCR10B |
3 ICCR001A |
4 ICCR001B |
5 ICCR300A |
6 ICCR300C I
2U.20
20.20
2.02
2.02
0.61
0.61
Cone.
10.00
10.00
1.00
1.00
0.30
0.30
Cone.
10.00
10.00
1.00
1.00
0.30
0.30
4.165e+00
4.165e+00
4.165e-01
4.165e-01
1.249e-01
1.249e-01
Cratio
2.062e+00
2.062e+00
2.0626-01
2.062e-01
6.186e-02
6.186e-02
Cratio
2.062e+00
2.062e+00
2.062e-01
2.062e-01
6.186e-02
6.186e-02
136964640
141405296
10346079
10648626
2194581
1982834
1.761e+01
1 .7256+01
1.452e+00
i.461e+00
3.285e-01
2.963e-01
4.22881e+Q(
4.14225e+OC
3.48689e+OC
3.5Q77Qe+OC
2.62936e+OC
2.37169e+QQ
Average RF = 3.39445e+
Deviation = 1.83123%
Area
42591352
46812688
2877482
2972343
604688
624207
Aratio
5.477e+00
5.711e+00
4.039e-01
4.078e-01
9.052e-02
9.329e-02
Resp. Factor
2.656336+00
2.77003e+00
1.95897e+00
1.97779e+00
1.46346e+00
1.50817e+00
Average RF = 2.05579e+0
Deviation = 3.88139%
Area
67677544
68584080
4886995
4965403
1074403
1071390
Aratio
8.703e+00
8.368e-t-00
6.860e-01
6.812e-01
1.608e-01
1.601e-01
Resp. Factor
4.22091e+00
4.058316+00
3.327036+-00
3.30396e+00
2.60026e+00
2.58863e+00
Average RF = 3. 34985e+0(
Deviation = 3.44283%
-------
vLictuLitation Report
Title:
FULL SCAN DATA :
Acquired
This Quantitation
Peak Search Method
PQUAN Library
Last Calibration
Acquisition Method
Tune/Cal File :
Datafile title:
ICCR - New Gas
10 ppm diluted to 0.3 ppm
Can E
Total FS
C:\PROGRA~i\HAPSRUN\DATA\AAA\LFSCALS\ICCR300B
07/09/9^at 14:42:27 f'
07/10/98 at 09:12:10 >V
C:\PROGRA-1\HAPSRUN\METHOD\AAA.LSM
C:\PROGRA~1\HAPSRUN\METHOD\AAA
07/10/98 at 09:04:28
C:\PROGRA~1\HAPSRUN\METHOD\LLKLFS.FSM
f
0
W = RT +- ( 0:45.00 / 2 + RT * 0.010 )
Min Fit=0.650; Min Pur=0.650; Min Area=5000
Width= 5-100 scans; Res= 6 scans; NLM=2.0
REC NO
1
Target
2
Rec#
1
2
REC NO
Rec#
* 1
2
3
4
5
6
7
8
1
2
3
4
5
6
7
8
Target
69
117
69
117
ret.
1:
5:
54
41
Target
Target
53
57
78
91
91
91
104
91
53
57
78
91
91
91
104
91
ret.
Not
1:
2:
3:
5:
6:
6:
7:
Pred
1:
5:
tm.
.14
.04
Pred
1:
1:
2:
3:
5:
6:
7:
7:
tm.
. RT.
54
45
TS
.
•
0
0
79
43
fit
.996
.999
. RT.
11
46
09
28
59
21
06
18
TS
.
,
.
^
.
.
*
•
79
45
07
22
71
57
06
85
fit
Internal Standard Nam<
TRIS
BPFB
purity MS
0.714
0.844
Analyte Name
1, 3-butadiene
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
Styrene
0-Xylene
purity MS
area
2689308
6410456
area
Found £0 <
46
08
25
54
15
59
13
.89
.58
.92
.77
.69
.03
.53
0
0
0
0
0
0
0
.968
.997
.998
.996
.991
.995
.987
0.946
0.983
0.992
0.979
0.979
0.933
0.974
110989
1336144
1060263
1540299
2366199
591206
1046399
ppm
9.94
4.85
ppm
0.33
0.33
0.33
0.38
0.72
0.38
0.35
man.
%RF(
-3.'
-12.!
man,
,3
,3
-------
yuantitation Report
Title:
FULL SCAN DATA : C:\PROGRA~1\HAPSRUN\DATA\AAA\LFSCALS\ICCR300C
Acquired 07/09/,£5^at 14:59:36
This Quantitation 07/10/98 at 09:11:35
Peak Search Method
PQUAN Library
Last Calibration
C:\PROGRA~1\HAPSRUN\METHOD\AAA.LSM
C:\PROGRA~1\HAPSRUN\METHOD\AAA
07/10/98 at 09:04:28
C:\PROGRA~1\HAPSRUN\METHOD\LLKLFS.FSM
Acquisition Method
Tune/Cal File :
Datafile title:
ICCR - New Gas
10 ppm diluted to 0.3 ppm
Can E
W = RT +- ( 0:45.00 / 2 + RT * 0.010 )
Min Fit=0.650; Min Pur=0.650; Min Area=5000
Width= 5-100 scans; Res= 6 scans; NLM=2.0
REC NO.
Rec#
I
2
1
2
REC NO.
Rec#
1
2
3
4
5
6
7
8
1
2
3
4
5
6
7
8
Target
Target
69
117
69
117
ret.
1:
5:
55
46
Target
Target
53
57
78
91
91
91
104
91
53
57
78
91
91
91
104
91
ret.
1:
1:
2:
3:
6:
6:
7:
7:
11
46
09
28
02
23
08
21
Pred
1:
5:
tm.
.57
.97
Pred
1:
1:
2:
3:
5:
6:
7:
7:
tm.
.08
.50
.13
.28
.02
.16
.37
.16
. RT.
54
45
TS
.
•
0
1
79
43
fit
.995
.000
. RT.
11
46
09
28
59
21
06
18
TS
•
•
•
.
*
.
*
•
0
0
0
0
0
1
0
0
79
45
07
22
71
57
06
85
fit
.887
.968
.999
.999
.998
.000
.985
.983
Internal Standard Nam<
TRIS
BPFB
purity MS
0.986
0.997
Analyte Name
1, 3-butadiene
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
Styrene
0-Xylene
purity MS
0.722
0.963
0.999
0.998
0.994
0.993
0.963
0.979
area
2657386
6691100
area
24371
100366
1157577
1019161
1288873
1982834
624207
1071390
ppm
9.94
4.85
ppm
0.39
0.31
0.29
0.33
0.34
0.64
0.38
0.35
man.
%RFC
-4.6
-8.6
man,
.3
/ee>
-------
Keoort
Title:
FULL SCAN DATA : C:\PROGRA~1\HAPSRUN\DATA\AAA\LFSCALS\ICCR001B
Acquired 07/09/>££at 15:20:56
This Quantitation 07/10/98 at 09:10:11
Peak Search Method
PQUAN Library
Last Calibration
Acquisition Method
Tune/Cal File
Datafile title:
ICCR - New Gas
10 ppm diluted to 1
Can E
C:\PROGRA-1\HAPSRUN\METHOD\AAA.LSM
C:\PROGRA-1\HAPSRUN\METHOD\AAA
07/10/98 at 09:04:28
C:\PROGRA~1\HAPSRUN\METHOD\LLKLFS.FSM
ppm
W = RT +- ( 0:45.00 / 2 + RT * 0.010 )
Min Fit=0.650; Min Pur=0.650; Min Area=5000
Width= 5-100 scans; Res= 6 scans; NLM=2.0
REC NO
Rec#
1
2
1
2
REC NO
Rec#
1
2
3
4
5
1
2
3
4
5
6
7
8
6
7
8
Target
Target
69
117
69
117
ret.
1:
5:
54
46
Target
Target
53
57
78
91
91
91
104
91
53
57
78
91
91
91
104
91
ret.
1:
1:
2:
3:
6:
6:
7:
7:
11
46
09
28
00
21
06
19
Pred
1:
5:
tm.
.80
.20
Pred
1:
1:
2:
3:
5:
6:
7:
7:
tm.
.85
.51
.14
.29
.54
.63
.83
.69
. RT.
54
45
TS
•
•
0
0
79
43
fit
.997
.999
. RT.
11
46
09
28
59
21
06
18
TS
.
.
.
.
.
.
.
•
0
0
0
1
0
79
45
07
22
71
57
06
85
fit
.960
.997
.998
.000
.999
0.997
0.999
0
.985
Internal Standard Nam<
TRIS
BPFB
purity MS
0.989
0.995
Analyte Name
1,3-butadiene
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
Styrene
0-Xylene
purity MS
0.944
0.994
0.998
0.999
0.996
0.995
0.982
0.984
area
2851831
7288881
area
90859
435586
4451729
4247383
6047727
10648626
2972343
4965403
ppm
9.94
4.85
ppm
1.06
1.03
1.01
0.95
0.97
1.97
0.93
0.95
man.
%RF
2.
-0.
man
I&7
-------
Report
Title:
FULL SCAN DATA : C:\PROGRA%1\HAPSRUN\DATA\AAA\LFSCALS\ICCR10B
Acquired 07/09/>^at 15:42:26
This Quantitation 07/10/98 at 09:10:55
Peak Search Method :
PQUAN Library :
Last Calibration
Acquisition Method :
Tune/Cal File :
Datafile title:
ICCR - New Gas
10 ppm straight shot
Can E
C:\PROGRA~1\HAPSRUN\METHOD\AAA.LSM
C:\PROGRA~1\HAPSRUN\METHOD\AAA
07/10/98 at 09:04:28
C:\PROGRA~1\HAPSRUN\METHOD\LLKLFS.FSM
W = RT +- ( 0:45.00 / 2 + RT * 0.010 }
Min Fit=0.650; Min Pur=0.650; Min Area=5000
Width= 5-100 scans; Res= 6 scans; NLM=2.0
REC NO.
Rec#
1
2
1
2
REC NO.
Rec#
1
2
3
4
5
6
7
8
1
2
3
4
5
6
7
8
Target
Target
69
117
69
117
ret.
1:
5:
54
45
Target
Target
53
57
78
91
91
91
104
91
53
57
78
91
91
91
104
91
ret.
1:
1:
2:
3:
6:
6:
7:
7:
12
46
09
28
00
21
06
18
Pred
1:
5:
tin.
.79
.43
Pred
1:
1:
2:
3:
5:
6:
7:
7:
tin.
.56
.45
.07
.22
.48
.57
.06
.85
. RT.
54
45
TS
.
•
0
1
79
43
fit
.998
.000
. RT.
11
46
09
28
59
21
06
18
TS
.
•
,
•
*
•
*
•
0
1
1
1
1
1
1
0
79
45
07
22
71
57
06
85
fit
.994
.000
.000
.000
.000
.000
.000
.986
Internal Standard Nam<
TRIS
BPFB
purity MS
0.990
0.998
Analyte Name
1, 3-butadiene
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
Styrene
0-Xylene
purity MS
0.993
0.999
1.000
1.000
0.998
area
2980580
8196344
area
1041395
4970370
47933000
53416740
81925928
0.998 141405296
0.998
0.985
46812688
68584080
ppm
9.94
4.85
man.
ppm
10.44
10.47
10.28
10.19
10.00
20.00
10.20
9.81
%RFC
6.9
11.7
man.
to
tO
i0
tO
(O
iO
10
-------
MID SCAN Calibration Response Table
Title:
MID SCAN DATA
Acquired
Peak Search Method
PQUAN Library
Last Calibration
C:\PROGRA~1\HAPSRUN\DATA\AAA\SIM002B
07/13/98 at 10:58:38
C:\PROGRA~1\HAPSRUN\METHOD\SIMAAA.LSM
C:\PROGRA~1\HAPSRUN\METHOD\SIMAAA
07/14/98 at 14:57:18
C:\PROGRA-1\HAPSRUN\METHOD\AAA.MIM
Acquisition Method
Tune/Cal File :
Datafile title:
iccr gas DF = 0.002
iccr gas diluted to 21 ppb
can E
W = RT +- ( 0:15.00 / 2 + RT * 0.010 )
Min Fit=0.500; Min Pur=0.000; Min Area=2000
Width= 10-200 scans; Res= 6 scans; NLM=2.0
Linear calibration curve
Internal Standards:
I.S. #1 — TRIS
Concentration = 9.940 ppm; 6 calib points
pt. File Man. Area
1 SIM01A 7502923
2 SIM01B 8096245
3 SIM005A 8229477
4 SIM005B 7931064
5 SIM002A * 5711226
6 SIM002B 8127841
Average RF =
Resp. Factor
754821.18681
814511.52565
827915.14666
797893.71971
574569.98925
817690.19752
= 7.64567e+05
I.S. #2 — BPFB
Concentration = 4.850 ppm; 6 calib points
pt. File Man. Area
1 SIM01A 22737388
2 SIM01B 23432816
3 SIM005A 23605052
4 SIM005B 21918912
5 SIM002A 23517340
6 SIM002B 23633006
Average RF =
Resp. Factor
4688121.32930
4831508.54861
4867021.12663
4519363.38784
4848936.17782
4872784.83808
= 4.77129e+06
Analytes:
Analyte #1 — 1, 3-butadiene
4 calib points
pt. File M I Cone. Cratio
1 SIM01A I 0.10 1.006e-02
2 SIM01B | 0.10 1.0066-02
Area Aratio
23668 3.155e-03
26138 3.228e-03
Resp. Fact
3.13558e-
3.209046-
-------
i biMUU^A 1
4 SIM005B |
Analyte #2 — Hexane
5 calib points
pt. File M |
1 SIM01A I
2 SIM01B |
3 SIM005A |
4 SIM005B * |
5 SIM002B * |
Analyte #3 — Benzene
6 calib points
pt. File M I
1 SIM01A I
2 SIM01B |
3 SIM005A |
4 SIM005B 1
5 SIM002A 1
6 SIM002B |
U.Ub
0.05
Cone.
0.10
0.10
0.05
0.05
0.02
Cone.
0.10
0.10
0.05
0.05
0.02
0.02
b . ujue-u j
5.030e-03
Cratio
1.016e-02
1.0166-02
5.080e-03
5.080e-03
2.032e-03
Cratio
1.0166-02
1.0166-02
5.0806-03
5.080e-03
2.0326-03
2.032e-03
12954
11993
Area
72602
93759
37273
36813
15619
Area
1072065
1075874
503815
453725
185948
192551
1.5746-03 1
1.512e-03 1
Average RF
Deviation
Aratio I
9.676e-03 1
1.158e-02 1
4.529e-03 I
4.642e-03 I
1.922e-03 1
Average RF
Deviation
Aratio I
1.429e-01 I
1.329e-01 1
6.122e-02 i
5.7216-02 I
3.256e-02 I
2.3696-02 |
3.12931e-01
3.00617e-01
= 3.12002e-
= 1.59087%
Resp. Factor
9.52320e-01
1.13971e+00
8.914916-01
9.13618e-01
9.45612e-01
= 9.685506-
= 10.13368%
Resp. Factor
1.406236+01
1.30780e+01
1.20502e+01
1.12605e+01
1.602136+01
1.165756+01
Average RF = 1.30216e+(
Deviation
= 8.51472%
Analyte #4 — Toluene
0 calib points
Analyte #5 — Ethyl Benzene
6 calib points
Pt
.
1
2
3
4
5
6
File M
SIM01A *
SIM01B
SIM005A
SIM005B
SIM002A
SIM002B *
Cone.
0
0
0
0
0
0
.10
.10
.05
.05
.02
.02
2.
2.
1.
1.
4.
4.
Cratio 1
082e-02 I
082e-02 i
0416-02 1
041e-02 I
165e-03 1
1656-03 1
Area
436796 '
1878925
613597
628430
241033
215464
/
1
8
2
2
1
9
Aratio
.921e-02
.018e-02
.599e-02
.867e-02
.025e-02
.117e-03
Average
I Resp. Factor
1 9.
I 3.
1 2.
1 2.
1 2.
1 2.
RF =
22483e-01
85040e+00
49648e+00
753526+00
46081e+00
189006+00
2.44545e+
Analyte #6 — m/p-Xylene
6 calib points
pt.
1
2
3
4
5
6
File
SIM01A
SIM01B
SIM005A
SIM005B
SIM002A
SIM002B
M
Cone.
0.20
0.20
0.10
0.10
0.04
0.04
Cratio
4.165e-02
4.165e-02
2.082e-02
2.082e-02
8.3306-03
8.3306-03
Area
2809694
2680206
900517
831158
270068
285057
/T5ev i a'tfion = 4b.b45^Si
Aratio Resp. Factor
1.236e-01
1.144e-01
3.8156-02
3.792e-02
1.148e-02
1.206e-02
Average RF
Deviation
2.966946+00
2.746216+00
1.83192e+00
1.820906+00
1.378626+00
1.448026+00
= 2.03210e+0
= 9.80775%
Analyte #7 — Styrene
6 calib points
-------
pt. File M
1 SIM01A
2 SIM01B
3 SIM005A
4 SIM005B
5 SIM002A
6 SIM002B
Analyte #8 — o-Xylene
6 calib points
pt. File M I
1 SIM01A I
2 SIM01B |
3 SIM005A |
4 SIM005B |
5 SIM002A I
6 SIM002B |
Cone. Cratio
0.10 2.062e-02
0.10 2.062e-02
0.05 1.031e-02
0.05 1.031e-02
0.02 4.124e-03
0.02 4.124e-03
Area
658985
663986
191696
189592
12712
38506
Area
1241802
1189744
383434
415801
65816
88112
Aratio 1 Resp. Facto]
2
2
8
8
5
1
5
5
1
1
2
3
.8986-02 1
.834e-02 1
.121e-03 1
.6506-03 1
.4056-04 1
.6296-03 1
Average RF
Deviation
Aratio 1
.461e-02 1
.077e-02 I
.624e-02 I
.897e-02 1
.7996-03 I
.7286-03 1
Average RF
Deviation
1.40565e+0(
1.37428e+0(
7.87734e-0:
8.39021e-0
1.31080e-0
3.95113e-0
= 8.221476
= 8.04836%
Resp. Facto
2.64883e+0
2.46247e+0
1.575646+0
1.840096+0
6.786646-C
9.041246-C
= 1.68497e
= 7.349851
-------
MID SCAN Calibration Response Table
Title:
MID SCAN DATA
Acquired
Peak Search Method
PQUAN Library
Last Calibration
C:\PROGRA~I\HAPSRUN\DATA\AAA\AAA002B
07/14/98 at 13:27:06
C:\PROGRA~1\HAPSRUN\METHOD\SIMAAA2.LSM
C:\PROGRA~1\HAPSRUN\METHOD\SIMAAA2
07/14/98 at 15:06:10
C:\PROGRA~1\HAPSRUN\METHOD\AAA2.MIM
Acquisition Method
Tune/Cal File :
Datafile title:
Sim Cals ICCR gas DF = .002
Can D
W = RT +- ( 0:45.00 / 2 + RT * 0.010 )
Min Fit=0.500; Min Pur=0.000; Min Area=2000
Width= 5-150 scans; Res= 6 scans; NLM=2.0
Linear calibration curve
Internal Standards:
I.S. #1 — Tris
Concentration = 9.940 ppm; 6 calib points
pt. File Man.
1 AAA010A
2 AAA010B
3 AAA005A
4 AAA005B
5 AAA002A
6 AAA002B
Area
7667186
7622166
7819453
7725098
7890010
7979764
Average RF =
Resp. Factor
771346.63864
766817.46383
786665.24948
777172.79527
793763.53884
802793.11582
= 7.83093e+05
I.S. #2 — BPFB
Concentration = 4.850 ppm; 6 calib points
pt. File Man.
1 AAA010A
2 AAA010B
3 AAA005A
4 AAA005B
5 AAA002A
6 AAA002B
Analytes:
Analyte #1 — Benzene
6 calib points
pt. File M I
1 AAA010A I
2 AAA010B I
3 AAA005A I
Area
16369912
16086901
16103032
16431683
16493355
16836116
Average RF
Resp. Factor
3375239.65400
3316886.86934
3320212
3387975
3400691
3471364
84879
94291
81945
19197
= 3.37873e+06
Cone.
0.10
0.10
Cratio
1.016e-02
1.016e-02
0.05 5.080e-03
Area Aratio
1195389 1.559e-01
1159839 1.522e-01
588034 7.520e-02
Resp. Fad
1.534406-
1.497566-
1.48020e-
-------
4 AAA005B
5 AAA002A
6 AAA002B
Analyte #2 —
6 calib -points
pt. File
1 AAA010A
2 AAA010B
3 AAA005A
4 AAA005B
5 AAA002A
6 AAA002B
Analyte #3 —
6 calib points
pt. File
1 AAA010A
2 AAA010B
3 AAA005A
4 AAA005B
5 AAA002A
6 AAA002B
Analyte #4 —
6 calib points
pt. File
1 AAA010A
2 AAA010B
3 AAA005A
4 AAA005B
5 AAA002A
6 AAA002B
Analyte #5 --
6 calib points
pt. File
1 AAA010A
2 AAA010B
3 AAA005A
4 AAA005B
5 AAA002A
6 AAA002B
0.05
0.02
0.02
Toluene
M 1 Cone.
0.10
1 0.10
1 0.05
1 0.05
1 0.02
I 0.02
Ethyl benzene
M I Cone.
1 0.10
1 0.10
1 0.05
1 0.05
1 0.02
1 0.02
m/p-Xylene
M | Cone.
1 0.20
1 0.20
1 0.10
1 0.10
1 0.04
1 0.04
Styrene
M | Cone.
1 0.10
1 0.10
1 0.05
1 0.05
1 0.02
* 1 0.02
5.Q80e-03
2.032e-03
2.032e-03
Cratio
1.006e-02
1.006e-02
5.030e-03
5.030e-03
2.012e-03
2.012e-03
Cratio
2.082e-02
2.082e-02
1.041e-02
1.041e-02
4.165e-03
4.165e-03
Cratio
4.165e-02
4.1656-02
2.082e-02
2.082e-02
8.3306-03
8.330e-03
Cratio
2.062e-02
2.062e-02
1.031e-02
1.0316-02
4.124e-03
4.124e-03
584426
194609
255073
Area
1055384
1021144
586991
505124
164738
210069
Area
1059879
1044530
468581
571365
140214
215662
Area
1404183
1484753
616493
691130
162938
249387
Area
393875
371736
170978
199072
29485
60920
7.565e-02 | 1.48909e+01
2.467e-02 I 1.21373e+0i
3.196e-02 1 1.57293e+01
Average RF = 1.46465e-^
Deviation = 2.91434%
Aratio I Resp. Factor
1.376e-01 1 1.36824e+01
1.3406-01 1 1.33167e-(-01
7.507e-02 | 1.49235e+01
6.5396-02 I 1.29990e+01
2.0886-02 | 1.037706+01
2.6336-02 I 1.30836e+01
Average RF = 1.30637e+
Deviation = 5.51358%
Aratio 1 Resp. Factor
6.4756-02 | 3.10907e+00
6.4936-02 1 3.117956+00
2.910e-02 I 2.794656+00
3.4776-02 I 3.33950e+00
8.501e-03 1 2.04114e+00
1.281e-02 1 3.07554e+00
Average RF = 2.91298e+<
Deviation = 6.00032%
Aratio I Resp. Factor
8.5786-02 I 2.059536+00
9.2306-02 | 2.21601e+00
3.828e-02 I 1.838406+00
4.2066-02 | 2.019756+00
9.8796-03 I 1.18597e+00
1.4816-02 | 1.778256+00
Average RF = 1.84965e+(
Deviation = 5.28587%
Aratio 1 Resp. Factor
2.406e-02 I 1.16695e+00
2.3116-02 | 1.120746+00
1.062e-02 | 1.02992e+00
1.2126-02 I 1.17517e+00
1.788e-03 I 4.335156-01
3.618e-03 1 8.77465e-01
Average RF = 9.67294e-C
Deviation = 6.17581%
Analyte #6 — o-Xylene
6 calib points
pt. File M I Cone.
Cratio
Area
Aratio I Resp. Factor
-------
2
3
4
5
6
AAA010A
AAA010B
AAA005A
AAA005B
AAA002A
AAA002B
0.10
0.10
0.05
0.05
0.02
0.02
2
2
1
-L
4
4
.062e-02 725983
.062e-02 i 681613
.031e-02 373294
.031e-02 I 386564
.124e-03
.1246-03
57744
152918
725983
681613
373294
386564
57744
152918
4.435e-02
4.237e-02
2.3186-02
2.353e-02
3,501e-03
9.0836-03
2.150916+0
2.054986+0
2.248626+0
2.28198e+0
8.490046-0
2.202566+0
Average RF = 1.96467e
Deviation = 9.45649%
-------
MIL) t'LAN (juantitation Reoort
Title:
MID SCAN DATA
Acquired
This Quantitation
Peak Search Method
PQUAN Library
Last Calibration
C : \ PROGRA-1 \HAPSRUN\DATA\AAA\AAAO0
07/14/98 at 13:39:42
07/14/98 at 15:12:33
C:\PROGRA-1\HAPSRUN\METH
C:\PROGRA~1\HAPSRUN\METH
07/14/98 at 15:06:10
C:\PROGRA~1\HAPSRUN\METHOD\AAA2.HIM
\SIMAAA2.LSM
\SIMAAA2
Acquisition Method
Tune/Cal File :
Datafile title:
Sim Cals ICCR gas DF = .005
Can D
W = RT +- ( 0:45.00 / 2 + RT * 0.010 )
Min Fit=0.500; Min Pur=0.000; Min Area=2000
Width= 5-150 scans; Res= 6 scans; NLM=2.0
REC
NO.
1
2
Rec#
REC
1
2
NO.
1
2
3
4
5
6
Rec#
1
2
3
4
5
6
Target
Target
69
117
69
117
ret.
1:
5:
53
39
Target
Target
78
91
91
91
104
91
78
91
91
91
104
91
ret.
2:
3:
5:
6:
6:
7:
07
24
54
14
58
Pred
1:
5:
tm.
.94
.32
Pred
2:
3:
5:
6:
6:
7:
tm.
.51
.73
.65
.80
.96
. RT.
54
39
TS
•
*
1
1
65
99
fit
.000
.000
. RT.
08
26
54
15
58
11
TS
12.92
•
.
.
.
.
•
1
1
1
1
1
1
22
10
98
47
97
82
fit
.000
.000
.000
.000
.000
.000
Internal Standard Nairn
Tris
BPFB
purity MS
*N/A*
*N/A*
Analyte Name
Benzene
Toluene
Ethyl benzene
m/p-Xylene
Styrene
o-Xylene
purity MS
*N/A*
*N/A*
*N/A*
*N/A*
*N/A*
*N/A*
area
7819453
16103032
area
588034
586991
468581
616493
170978
373294
ppm
9.94
4.85
man.
ppm
0.05
0.06
0.05
0.10
0.05
0.05
%R
0
-1
man.
o
i
-------
MID SCAN Quantitation Report
Title:
MID SCAN DATA : C:\PROGRA~1\HAPSRUN\DATA\AAA\AAA010A
Acquired 07/14/98 at 14:07:35
This Quantitation 07/14/98 at 15:12:01
Peak Search Method
PQUAN Library
Last Calibration
Acquisition Method
Tune/Cal File
Datafile title:
Sim Cals ICCR gas DF = .01
Can D
C:\PROGRA~1\HAPSRUN\METHOD\SIMAAA2.LSM
C:\PROGRA~1\HAPSRUN\METHOD\SIMAAA2
07/14/98 at 15:06:10
C:\PROGRA~1\HAPSRUN\METHOD\AAA2.MIM
W = RT +- ( 0:45.00 / 2 + RT * 0.010 )
Min Fit=0.500; Min Pur=0.000; Min Area=2000
Width= 5-150 scans; Res= 6 scans; NLM=2.0
REC
NO
1
2
Rec#
REC
1
2
NO
1
2
3
4
5
6
Rec#
1
2
3
4
5
6
Target
Target
69
117
69
117
ret.
1:
5:
54
39
Target
Target
78
91
91
91
104
91
78
91
91
91
104
91
ret.
2:
3:
5:
6:
6:
7:
08
26
54
15
58
11
Pred
1:
5:
tm.
.65
.66
Pred
2:
3:
5:
6:
6:
7:
tm.
.22
.10
.60
.14
.97
.82
. RT.
54
39
TS
•
•
1
1
65
99
fit
.000
.000
. RT.
08
26
54
15
58
11
TS
•
.
.
.
•
•
1
1
1
1
1
1
22
10
98
47
97
82
fit
.000
.000
.000
.000
.000
.000
Internal Standard Nami
Tris
BPFB
purity MS
*N/A*
*N/A*
Analyte. Name
Benzene
Toluene
Ethyl benzene
m/p-Xylene
Styrene
o-Xylene
purity MS
*N/A*
*N/A*
*N/A*
*N/A*
*N/A*
*N/A*
area
7667186
16369912
area
1195389
1055384
1059879
1404183
393875
725983
ppm
9.94
4.85
man.
ppm
0.10
0.10
0.10
0.20
0.10
0.10
%RFC
-1.5
-0.1
man.
. /
-------
MID SCAN Quantitation Report
Title:
MID SCAN DATA
Acquired
This Quantitation
Peak Search Method
PQUAN Library
Last Calibration
C:\PROGRA-1\HAPSRUN\DATA\AAA\AAA002A
07/14/98 at 13:15:06
07/14/98 at 15:13:11
C:\PROGRA-1\HAPSRUN\METHOD\SIMAAA2.LSM
C:\PROGRA-1\HAPSRUN\METHOD\SIMAAA2
07/14/98 at 15:06:10
C:\PROGRA~1\HAPSRUN\METHOD\AAA2.MIM
Acquisition Method
Tune/Cal File :
Datafile title:
Sim Cals ICCR gas DF = .002
Can D
W = RT +- ( 0:45.00 / 2 + RT * 0.010 }
Min Fit=0.500; Min Pur=0.000; Min Area=2000
Width= 5-150 scans; Res= 6 scans; NLM=2.0
REC
NO.
1
2
Rec#
REC
1
2
NO.
1
2
3
4
5
6
Rec#
1
2
3
4
5
6
Target
Target
69
117
69
117
ret.
1:
5:
53
39
Target
Target
78
91
91
91
104
91
78
91
91
91
104
91
ret.
2:
3:
5:
6:
7:
7:
07
25
54
14
00
11
Pred
1:
5:
tm.
.94
.65
Pred
2:
3:
5:
6:
6:
7:
tm.
.83
.44
.59
.42
.72
.82
. RT.
54
39
TS
•
•
1
1
65
99 .
fit
.000
.000
. RT.
08
26
54
15
58
11
TS
•
.
.
.
•
•
1
1
1
0
0
1
22
10
98
47
97
82
fit
.000
.000
.000
.999
.997
.000
Internal Standard Nartu
Tris
BPFB
purity MS
*N/A*
*N/A* 1
Analyte Name
Benzene
Toluene
Ethyl benzene
m/p-Xylene
Styrene
o-Xylene
purity MS
*N/A*
*N/A*
*N/A*
*N/A*
*N/A*
*N/A*
area
7890010
6493355
area
194609
164738
140214
162938
29485
57744
ppm
9.94
4.85
man.
ppm
0.02
0.02
0.02
0.04
0.02
0.01
1.
0
man.
1
-------
(juantitation Report
Title:
MID SCAN DATA : C:\PROGRA~1\HAPSRUN\DATA\AAA\SIM01A
Acquired 07/13/98 at 11:51:39
This Quantitation 07/14/98 at 15:19:25
Peak Search Method
PQUAN Library
Last Calibration
Acquisition Method
Tune/Cal File :
Datafile title:
iccr gas DF = 0.01
iccr gas diluted to 100 ppb
can E
C:\PROGRA~l\HAPSRUN\METHOp\SIMAAA.LSM
C:\PROGRA~1\HAPSRUN\METHOP\SIMAAA
07/14/98 at 14:57:18
C:\PROGRA~1\HAPSRUN\METHODV
W = RT +- ( 0:15.00 / 2 + RT * 0.010 )
Min Fit=0.500; Min Pur=0.000; Min Area=2000
Width= 10-200 scans; Res= 6 scans; NLM=2.0
REC NO.
Rec#
1
2
I
2
REC NO.
Rec#
1
2
3
* 4
5
6
7
8
1
2
3
4
5
6
7
8
Target
Target
69
117
69
117
ret .
1:
4:
54
52
Target
Target
53
57
78
91
91
91
104
91
53
57
78
91
91
91
104
91
ret.
1:
1:
2:
Not
5:
5:
6:
6:
12
46
08
Pred
1:
4:
tm.
.48
.63
Pred
1:
1:
2:
2:
5:
5:
6:
6:
tm.
.69
.68
.43
. RT.
54
51
TS
.
•
1
1
48
32
fit
.000
.000
. RT.
12
46
08
37
06
27
10
24
TS
.
.
.
.
.
.
.
•
1
1
1
25
25
00
24
75
24
93
23
fit
.000
.000
.000
Internal Standard Nam<
TRIS
BPFB
purity MS
*N/A*
*N/A*
Analyte Name
1,3-butadiene
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
Styrene
o-Xylene
purity MS
*N/A*
*N/A*
*N/A*
area
7502923
22737388
area
23668
72602
1072065
Found
07
28
11
25
.41
.12
.98
.76
1
1
1
1
.000
.000
.000
.000
*N/A*
*N/A*
*N/A*
*N/A*
1815518
2809694
658985
1241802
ppm
9.94
4.85
man. %RFC
-1.3
-1.8
ppm
0.10
0.09
0.11
0.11
0.21
0.10
0.10
-------
'AID SCAN Calibration Report
Title:
MID SCAN DATA
Acquired
This Calibration
Peak Search Method
PQUAN Library
Acquisition Method
Tune/Cal File :
Datafile title:
iccr gas DF = 0.002
iccr gas diluted to 21 ppb
can E
C: \PROGRA-1 \HAPSRUN\DATA\AAA\S IM002A/-;
07/13/98 at 10:44:04
07/14/98 at 14:57:17
C:\PROGRA~1\HAPSRUN\METHODXSIMAAA.LSM
C:\PROGRA~1\HAPSRUN\METHOB\SIMAAA
C:\PROGRA~1\HAPSRUN\METHODVAAA.MIM
W = RT +- ( 0:15.00 / 2 + RT * 0.010 )
Min Fit=0.500; Min Pur=0.000; Min Area=2000
Width= 10-200 scans; Res= 6 scans; NLM=2.0
REC NO. Target Pred. RT. Internal Standard Name
1 69 1:54.48 TRIS
2 117 4:51.32 BPFB
Rec# Target
1 69
2 117
ret.tm. TS fit purity
1:53.93 1.000 *N/A*
4:50.82 1.000 *N/A*
MS
area
5711226
23517340
ppm
9.94
4.85
man,
*
Analyte Name
1,3-butadiene
Hexane
Benzene
Toluene
Ethyl Benzene
m/p-Xylene
Styrene
o-Xylene
Rec# Target ret.tm. TS fit purity MS
REC
NO.
1
2
3
4
5
6
7
8
Target
53
57
78
91
91
91
104
91
Pred. RT.
1:12.25
1:46.25
2:08.00
2:37.24
5:06.75
5:27.24
6:10.93
6:24.23
1
2
3
4
5
6
7
53
57
78
91
91
91
104
91
1:23.01
1:44.65
2:07.61
Not Found
5:06.31
5:26.80
6:10.16
6:24.72
1.000
1.000
1.000
1.000
1.000
1.000
1.000
*N/A*
*N/A*
*N/A*
*N/A*
*N/A*
*N/A*
*N/A*
area ppm
2489 Short peak.
8042 Short peak. °
185948 0.02
241033
270068
12712
65816
0.02
0.04
0.02
0.02
man
0
-------
L;'JAW
Title: trona
FULL SCAN DATA : C:\FROGRA-i\HAPSRUN\DATA\CAECALS\CAE1300B
Acquired 05/12/98 at 17:00:02
Peak Search Method
PQUAN Library
Last Calibration
C:\PROGRA-1\HAPSRUN\METHOD\CAE1.LSM
C : \ PROGRA-1 \11APSRUN\METIIOD\TGPC1
05/13/98 at 11:23:40
Acquisition Method
Tune/Cal File :
Pafnf i IP H HP:
Cylinder #J - JOO ppb
CAE/EMI OCI-TG Test
5-12-98
C:\PROGRA-1\HAPSRUN\METHOD\LLK.FSM
W = RT + - ( 0:45.00 / 2 + RT * 0.010 )
Min Fit=0.650; Min Pur=0.650; Min Area=5000
Width= 5-100 scans; Res= 6 scans; NLM=2 . 0
Linear calibration curve
Internal Standards:
Concentration = 9.940 ppm; 6 calib points
pt. File Man.
1 CAE1010A
2 CAE1010B
3 CAE1001A
4 CAE1001B
5 CAE1300A
6 CAE1300B
Area
1531445
1450186
1613940
1615176
1682897
1659603
Average RF =
Resp. Factor
154068.90520
145893.95594
162368.20053
162492.54660
169305.52410
166962.06346
= 1.60182e+05
I.S. #2 — BPFB
Concentration = 4.850 ppm; 6 calib points
pt. File Man.
1 CAE1010A
2 CAE1010B
3 CAE1001A
4 CAE1001B
5 CAE1300A
6 CAE1300B
Area
2876444
2790694
2941213
2921814
3076968
3042285
Average RF =
Resp. Factor
593081.24878
575400.83606
606435.68203
602435.88813
634426.40423
627275.27007
= 6.06509e+05
Analytes:
Analyte #1 -- Chloromethane
6 caiib points
pt. File M I Cone. Cratio
1 CAE1010A I 9.99 1.005e+00
2 CAE1010B
9.99 1.005e+00
Area Aratio
859035 5.609e-01
878564 6.058e-01
Resp. Fact
5.58124e-
6.02796e-
-------
4 CAE1001B
5 CAE1300A
6 CAE1300B
j. . UU i .
1.00 l.OOSe-01
0.30 3.015e-02
0.30 3.015e-02
3 J J Z. / J . / O J fc! " U ^ !
86273 5.341e-02 I
21403 1.2720-02 1
32808 1.977e-02 I
Average RF
5.31467e-01
4.218106-01
6.55655e-01
- rj.57r>35e-
Deviation = 6.54791%
Analyte #2 — Chloroethane
6 calib points
pt. File M I
1 CAE1010A |
2 CAE1010B |
3 CAE1001A I
4 CAE1001B |
5 CAE1300A |
6 CAE1300B I
Cone. Cratio
9.98 1.004e+00
9.98 1.0040+00
1.00 1.0040-01
1.00 1.004e-01
0.30 3.012e-02
0.30 3.012e-02
Area
2546828
2593230
236929
248772
71831
80993
Aratio
1.663e+00
1.7880+00
1.4680-01
1.5406-01
4.268e-02
4.880e-02
Average RF
Deviation
Resp. Factor
1.65636e+00
1.78104e+00
1.46213e+00
1.534046+00
1.417060+00
1.620236+00
1.578480+
6.16326%
Analyte #3 — Methylene Chloride
6 calib points
pt. File M I
1 CAE1010A i
2 CAE1010B |
3 CAE1001A |
4 CAE1001B |
5 CAE1300A |
6 CAE1300B |
Cone. Cratio
9.99 1.0050+00
9.99 1.005e+00
1.00 l.OOSe-01
1.00 l.OOSe-01
0.30 3.015e-02
0.30 3.0156-02
Area
6503620
6640100
653535
664074
173766
186268
Aratio I Resp. Factor
4.2476+00 I 4
4.5796+00 I 4
4.0496-01 | 4
4.1116-01 I 4
1.0336-01 | 3
1.1226-01 I 3
Average RF =
Deviation =
,22547e+00
55588e+00
029056+00
09089e+00
42458e+00
,72249e+00
4.00806e+
6.27712%
Analyte #4 — 1,1-dichloroethane
6 calib points
pt. File M I
1 CAE1010A |
2 CAE1010B |
3 CAE1001A J
4 CAE1001B I
5 CAE1300A |
6 CAE1300B |
Cone. Cratio I Area
9.96 1.0020+00 I 7941977 5
9.96 1.0020+00 I 8228796 5
1.00 1.0020-01 i 787538 4
1.00 1.0020-01 i 792629 4
0.30 3.006e-02 I 242718 1
0.30 3.006e-02 I 242543 1
Aratio I Resp. Factor
.186e+00 | 5.175526+00
.6746+00 I 5.66291e+00
. 880e-01 I 4.86980e + 00
,907e-01 I 4.89753e+00
.442e-01 I 4.79789e+00
.4616-01 I 4.86172e+00
Average RF = 5.04423e+(
Deviation = 7.53477%
Analyte #5 -- c-1,2-dichloroethene
6 calib points
pt. File M I
1 CAE1010A |
2 CAE1010B |
3 CAE1001A |
4 CAE1001B |
5 CAE1300A |
6 CAE1300B |
Cone. Cratio I Area
10.00 1.006e+00 I 6149913
10.00 1.0060+00 I 6408859
1.00 1.006e-01 I 502310
1.00 1.006e-01 I 557686
0.30 3.0186-02 I 167332
0.30 3.018e-02 I 148603
Aratio I Resp. Factor
4.016e+00 I J
4.4196+00 I 4
3.1126-01 I 3
3.453e-01 I 3
9.943e-02 I 3
8.9546-02 | 2
Average RF =
Deviation =
,991666+00
392826+00
.09365e+00
,43207e+00
,294486+00
,96680e+00
3.52858e+C
8.13740%
Analyte #6 — 1,1,1-trichloroethane
6 ealib points
-------
PL. r j. it;
1 CAE1010A
2 CAE1010B
3 CAE1001A
4 CAE1001B
5 CAE1300A
6 CAE1300B
9.98 1.0046+00 I
9.98 1.004e+00 I
1.00 1.004e-01 |
1.00 1.0046-01 I
0.30 3.012e-02 I
0.30 3.012e-02 I
Analyte #7 — 1,2-dichloropropane
6 calib points
pt. File M I
1 CAE1010A I
2 CAE1010B I
3 CAE1001A I
4 CAE1001B I
5 CAE1300A I
6 CAE1300B |
Cone. Cratio I
9.98 1.004e+00 |
9.98 1.004e+00 I
1.00 1.004e-01 I
1.00 1.004e-01 |
0.30 3.012e-02 I
0.30 3.0126-02 I
Analyte #8 — 1,1,2-trichloroethane
6 calib points
pt. File M I
1 CAE1010A I
2 CAE1010B I
3 CAE1001A |
4 CAE1001B I
5 CAE1300A |
6 CAE1300B I
Cone. Cratio
9.99 1.005e+00
9.99 1.005e+00
1.00 1.005e-01
1.00 l.OOSe-01
0.30 3.0156-02
0.30 3.015e-02
Analyte #9 — Dibromochloromethane
6 calib points
pt. File M I
1 CAE1010A |
2 CAE1010B |
3 CAE1001A I
4 CAE1001B I
5 CAE1300A |
6 CAE1300B I
Cone. Cratio I
9.97 2.056e+00 I
9.97 2.0566+00 I
1.00 2.056e-01 I
1.00 2.056e-01 I
0.30 6.167e-02 I
0.30 6.167e-02 I
Analyte #10 — Ethyl Benzene
6 calib points
pt. File M I
1 CAE1010A I
2 CAE1010B I
3 CAE1001A I
4 CAE1001B I
5 CAE1300A l
6 CAE1300B I
Cone. Cratio I
10.00 2.062e+00 I
10.00 2.062e+00 I
1.00 2.062e-01 I
1.00 2.062e-01 I
0.30 6.186e-02 I
0.30 6.186e-02 I
r\j- era
7941901
7872220
772968
781629
233874
221625
Area
7148643
7442873
655377
693076
202418
213647
Area
12254564
12449066
1153711
1123639
315623
319910
Area
7064662
7386689
626688
638013
157000
168594
Area
45610096
46299072
2946939
2976477
622158
758907
5.186e+00
5.428e+00 1
4 .789e-01
4.8396-01 1
1.390e-01
1.335e-01 1
Average RF
Deviation
Aratio 1
4.668e+00 1
5.132e+00 I
4.061e-01 I
4.291e-01 1
1.2036-01 1
1.287e-01 1
Average RF
Deviation
Aratio 1
8.002e+00 I
8.584e+00 1
7.1486-01 1
6.957e-01 i
1.8756-01 1
1.9286-01 1
Average RF
Deviation
Aratio 1
2.456e+00 1
2.647e+00 I
2.1316-01
2.1846-01 1
5.1026-02 |
5.5426-02 |
Average RF
Deviation
Aratio
1.586e+01
1.659e+01
1.002e+00
1 .019e-tOO
2.0226-01
2.4956-01
Average RF
Deviation
5.16510e+OC
5.40666e+0(
4 .77013e+0(
4.81988e+0(
4.61380e+0(
4.43353e+0(
= 4.86818e-
= 3.86414%
Resp. Facto
4.64920e+0
5.11179e+0
4.04445e+0
4.27383e+0
3.99325e+0
4.27393e+0
= 4.39107e
= 7.97975%
Resp. Factc
7.96191e+C
8.54150e+C
7.11264e+C
6.92194e+C
6.22029e+C
6.39327e+C
= 7.19193?
= 5.91686^
Resp. Factc
1.19476e+(
1.28761e+(
1.03651e+i
1.06224e+i
8.27374e-i
8.98602e-'
= 1.05118'
= 6.25527
Resp. Fact
7.69036e+
8.04640e+
4.85944e+
4.94074ei
3.26887e->
4.03282e^
= 5.4731]
= 4.59934
-------
Analyte #11 -- p-Xylene
6 calib points
pt. File M I
I CAE1010A i
2 CAE1010B i
3 CAE1001A i
4 CAE1001B I
5 CAE1300A |
6 CAE1300B I
Cone. Cratio I Area
10.00 2.062e+00 I 35860888 1
10.00 2.062.6 + 00 I 36158800 1
1.00 2.0626-01 I 2132630 7
1.00 2.0626-01 I 2145611 7
0.30 6.186e-02 I 522128 1
0.30 6.186e-02 I 523291 1
Aratio I Resp. Factor
.247e+01 | 6.04654e+00
.296e+01 I 6.28411e+00
.2516-01 I 3.51666e+00
.343e-01 | 3.561566+00
.6976-01 | 2.74331e+00
.7206-01 | 2.780766+00
Average RF = 4.15549e+C
Deviation = 4.51725%
Analyte #12 -- 1,1,2,2-tetrachloroethane
6 calib points
pt. File M
1 CAE1010A
2 CAE1010B
3 CAE1001A
4 CAE1001B
5 CAE1300A
6 CAE1300B
Cone. Cratio
5.09 1.049e+00
5.09 1.049e+00
0.51 1.049e-01
0.51 1.049e-01
0.15 3.148e-02
0.15 3.1486-02
Area
20311168
19883932
1831837
1795553
453519
477855
Aratio I Resp. Factor
6.728266+00
6.789136+00
5.93450e+00
5.85558e+00
4.68139e+00
4.98883e+00
= 5.82962e+0
= 0.96430%
7.
7.1256+00 |
6.2286-01 I
6.145e-01 I
1.474e-01 |
1.571e-01 |
Average RF
Deviation
-------
:-'ULL . Lai-J Ldiicration Kesoonse
Title: trona
FULL 3CAN DATA
Acquired
Peak Search Method
PQUAN Library
Last Calibration
C:\PROGRA~i\HAPSRUN\DATA\CAECALS\CAE3300B
05/12/98 at 15:39:16
C:\PROGRA~1\HAPSRUN\METHOD\CAE3.LSM
C:\PROGRA~1\HAPSRUN\METHOD\TGPC3
05/13/98 at 11:03:00
Acquisition Method : C:\PROGRA~1\HAPSRUN\METHOD\LLK.FSM
Tune/Cal File :
Datafile title:
Cylinder §3 - 300 ppb
CAE/EMI OCI-TG Test
5-12-98
W = RT +- ( 0:45.00 / 2 + RT * 0.010 )
Min Fit=0.650; Min Pur=0.650; Min Area=5000
Width= 5-100 scans; Res= 6 scans; NLM=2.0
Linear calibration curve
Internal Standards:
I.S. #1 -- TRIS
Concentration = 9.940 ppm; 6 calib points
pt. File Man.
1 CAE3010A
2 CAE3010B
3 CAE3001A
4 CAE3001B
5 CAE3300A
6 CAE3300B
Area
1443182
1582543
1685525
1647299
1629043
1674469
Average RF
Resp. Factor
145189.32822
159209.54879
169569.91041
165724.23657
163887.61695
168457.63682
= 1.62006e+05
I.S. #2 -- BPFB
Concentration = 4.850
ppm; 6 calib points
pt. File Man.
1 CAE3010A
2 CAE3010B
3 CAE3001A
4 CAE3001B
5 CAE3300A
6 CAE3300B
Analytes:
Analyte #1 — Bromomethane
6 calib points
pt. File M I Cone.
1 CAE3010A I 10.00
Area
3251967
3192356
3081741
3181594
3254150
2872759
Average RF
Resp. Factor
670508.67298
658217.74490
635410.52796
655998.77579
670958.77608
592321.45495
= 6.47236e+05
Cratio
1.006e+00
CAE3010B
10.00 1.006e+00 I
Area Aratio
3429096 2.376e+00
3474695 2.196e+00
Resp. Factor
2.36181e+OQ
2.18247e+00
-------
r-nr^om a
< CAE3001A
-•; CAE3003B
l; CAE3300A
6 CAE3300B
Anaiyte #2 -- 1,
6 calib points
pt . File M
1 CAE3010A
2 CAE3010B
3 CAE3001A
4 CAE3001B
5 CAE3300A
6 CAE3300B
Anaiyte #3 -- t-
6 calib points
pt. File M
1 CAE3010A
2 CAE3010B
3 CAE3001A
4 CAE3001B
5 CAE3300A
6 CAE3300B
i inn inn£/-i_ni i
1 1 .00 1 .0060-01 i
; 1.00 i.006e-01 i
1 0.30 "J. 018e-02 1
0.30 3.018e-02 i
1-dichloroethene
1 Cone. Cratio 1
i 10.20 1.0266+00 1
1 10.20 1.0266+00 1
1 1.02 1.026e-01 1
1 1.02 1.0266-01 1
1 0.31 3.078e-02 I
1 0.31 3.0786-02 1
1 , 2-dichloroethene
1 Cone. Cratio 1
1 10.50 1.056e+00 I
1 10.50 1.056e+00 1
1 1.05 1.0566-01 1
1 1.05 1.0566-01 1
1 0.31 3.169e-02 I
1 0.31 3.169e-02 1
Anaiyte #4 -- MEK
5 calib points
pt. File M
1 CAE3010A
2 CAE3010B
3 CAE3001A
4 CAE3001B
5 CAE3300A
Anaiyte #5 — 1,
4 calib points
pt. File M
1 CAE3010A
2 CAE3010B
3 CAE3001A
4 CAE3001B
jfftrf**,
Anaiyte #6 — Ca
6 calib points
pt. File M
1 CAE3010A
: CAE3010B
1 Cone. Cratio 1
1 10.20 1.026e+00 1
1 10.20 1.026e+00 I
1 1.02 1.0266-01 1
1 1.02 1.026e-01 1
1 0.31 3.078e-02 I
2-dichloroehane
1 Cone. Cratio 1
1 10.50 1.0566+00 1
1 10.50 1.056e+00 1
1 1.05 1.0566-01 1
1 1.05 1.0566-01 1
••fS** <*''
/v*^
1
rbon Tot r-ii chloride
1 Cone. Cratio 1
1 10.00 1.006e+00 1
1 10.00 1.0066+00 1
3 A A 1 3 ()
148719
333992
93222
101310
Area
3893971
4040971
361871
360731
105111
104990
Area
6294969
6470831
591593
586701
170717
172445
Area
2542307
2684464
135561
159584
18676
Area
10346109
10193005
1008668
1027144
Area
3696945
3747467
M ,1 ) ^ _ i ' 1 • , , 1 , ( 1 „ w „ , ,
?.069e-01 1 2.05649e+0
2.028e-01 , ^.01535e+0
'3.723e-02 i 1.89606e + 0
6.050e-02 , 2.00466e+0
Average RF = 2.08614e
Deviation = 6.61873%
Aratio 1 Resp. Factc
2.698e+00 1 2.62941e+C
2.553e+00 i 2.48838e+C
2.147e-01 ! 2.09221e+C
2.190e-01 1 2.13401e)C
6.452e-02 1 2.09595e+C
6.270e-02 1 2.03674e+C
Average RF = 2.24612e
Deviation = 4.80168?
Aratio 1 Resp. Factc
4.362e+00 1 4.12924e+(
4.089e+00 1 3.87081e + (
3.510e-01 1 3.32265e+i
3.562e-01 1 3.37164e+<
1.048e-01 1 3.30689e+
1.0306-01 1 3.24975e+
Average RF = 3.54183
Deviation = 5.53441
Aratio 1 Resp. Fact
1.762e+00 i 1.716696+
1.696e+00 1 1.65306e+
8.043e-02 1 7.83765e-
9.688e-02 1 9.44068e-
1.1466-02 1 3.72406e-
Average RF = 1.0940C
Deviation = 3.86804
Aratio 1 Resp. Fact
7.169e+00 1 6.78661e-
6.441e+00 1 6.097396-
5.984e-01 1 5.66513e-
6.235e-01 1 5.90277e
Average RF = 6.1129
Deviation = 7.8300
Aratio 1 Resp. Fac
2.562e+00 j 2.54629e
2.3686+00 1 2.35380e
-------
•1 CAE3001B
.- CAE3300A
•3 ':AE3300B
1.00 i.006e-01 !
0.30 3.018e-02 I
0.30 3.018e-02 i
Anaiyte #7 -- Trichloroethene
h calib points
pt. File M I Cone. Cratio
1 CAE3010A I 10.00 i.006e+00
2 CAE3010B I 10.00 1.006e+00
3 CAE3001A I 1.00 1.006e-01
4 CAE3001B I 1.00 1.006e-01
5 CAE3300A I 0.30 3.018e-02
6 CAE3300B I 0.30 3.018e-02
Anaiyte
-- c-1, 2-dichloropropene
6 calib points
pt. File M
I CAE3010A
2 CAE3010B
3 CAE3001A
4 CAE3001B
5 CAE3300A
6 CAE3300B
Cone.
12.50
12.50
1.25
1.25
0.38
0.38
Cratio I
1.2586+00 I
1.258e+00 I
1.258e-01 I
1.258e-01 I
3.773e-02 I
3.773e-02 I
Anaiyte #9 -- t-1,2-dichloropropene
6 calib points
pt.
1
2
3
4
5
6
File
CAE3010A
CAE3010B
CAE3001A
CAE3001B
CAE3300A
CAE3300B
M
Cone.
8.10
8.10
8
0
0.
0.
81
81
24
0.24
Cratio
149e-01
8.149e-01
8.149e-02
8.149e-02
2.445e-02
2.445e-02
Anaiyte #10 -- 2-Hexanone
2 calib points
pt. File Ml Cone.
1 CAE3010A I b.OO
2 CAE3010B I 5.00
Anaiyte §11 — Chlorobenzene
(j caJ it; points
pt. File M I Cone.
1 CAE3010A I 10.00
2 CAE3010B I 10.00
3 CAE3001A i 1.00
Cratio I
5.030e-01 |
5.030e-01 I
Cratio I
2.062e+00 I
2.062e+00 I
2.062e-01 |
352687
76911
96624
Area
10395648
10883738
949865
970459
248561
267033
Area
30013118
31121156
2388666
2437939
680521
657748
Area
19640928
20223152
1450673
1512153
417885
394180
Area
728897
713493
Area
29124048
29607180
1967362
2.1416-01 i 2.12316e + OC
'1.721e-02 1 1.5b430e+OC
'.3.7706-02 ; ;.91193e + OC
Average RF - 2.08899e+
Deviation = 6.58137%
Aratio Resp. Factor
7.203e+00 1 7.16006e+00
6.877e+00 1 6.83611e+00
5.635e-01 I 5.60161e+00
5.891e-01 1 5.85587e+00
1.526e-01 5.05552e+00
1.595e-01 1 5.28388e+00
Average RF = 5.96551e+
Deviation = 4.06582%
Aratio 1 Resp. Factor
2.080e+01 1.653746+01
1.967e+01 1 1.563786+01
1.417e+00 1 1.12693e+01
1.480e+00 1 1.1768764-01
4.177e-01 | 1.107306+01
3.9286-01 1 1.041216+01
Average RF = 1.27830e+l
Deviation = 5.15498%
Aratio Resp. Factor
1.361e+01 1.67010e+01
1.278e+01 1.56818e+01
8.607e-01 1.05617e+01
9.1806-01 1.126486+01
2.565e-01 1.04931e+01
2.354e-01 9.62936e+00
Average RF = 1.23886e+C
Deviation = 5.81765%
Arat Lo 1 Resp. Factor
L-.Oble-Ol 1 1.004066+00
4.509e-01 1 8.962946-01
Average RF = 9.50179e-C
Deviation = 8.02004%
Aratio 1 Resp. Factor
H.956e+00 1 4.34358e+00
9.274e+00 1 4.49808e+00
6.384e-01 1 3.09621e+00
-------
5 "AE3300A
6 CAE3300B
0.3C
1 0.30
b. 1 6 be- 02 ;
6.186e-02 1
Analyte #12 -- m-Xylene
f> calib points
pt. File M
1 CAE3010A
2 CAE3010B
3 CAE3001A
4 CAE3001B
5 CAE3300A
6 CAE3300B
1 Cone.
I 10.00
1 10.00
i 1.00
1 1.00
j 0.30
1 0.30
Cratio 1
2.062e+00 1
2.062e+00 1
2.062e-01 I
2.062e-01 1
6.186e-02 |
6.186e-02 I
Analyte #13 -- o-Xylene
6 calib points
pt. File M
1 CAE3010A
2 CAE3010B
3 CAE3001A
4 CAE3001B
5 CAE3300A
6 CAE3300B
Cone.
10.00
10.00
1.00
1.00
0.30
0.30
Cratio I
2.062e+00 I
2.062e+00 1
2.062e-01 1
2.062e-01 I
6.186e-02 I
6.1866-02 I
557963
533478
Area
39678100
40909728
2587431
2675522
639796
677163
Area
40901988
44594104
2654372
2781677
690180
692750
±
I
1
I
Q
8
1
2
1
1
8
8
2
2
. 715e-01 i
.857e-01 !
Average RF
Deviation
Aratio i
.220e+01 !
.281e+01 1
.396e-01 I
.409e-01 1
.966e-01 I
.357e-01 1
Average RF
Deviation
Aratio 1
.258e+01 I
.397e+01 1
.613e-01 1
.743e-01 1
.121e-01 1
.4116-01 1
Average RF
Deviation
/
3.
=
77207e+l
00219e+C
3. 48755s
3.68364?
Resp. Factc
5.
h.
A .
4 .
3.
3.
=
91761e+(
21523e + (
07206e+(
07855e + (
17852e+(
81079e + (
4.54546<
4. 75628'
Resp. Fact<
6.
6.
4.
4.
3.
3.
=
=
10014e+'
77498e+'
17741e+
24037e+
42882e+
89850e+
4.77004
8.99319
-------
I,L ./,i\[\ < ..-j i i oran j/,n r^.spo
Title: rrona
FULL GCMJ DATA
Acquired
PeaK Search Method
PQUAN Library
Last Calibration
C:\PROGRA~I\HAPSRUN\DATA\CAECALC\CAE5300B
05/12/98 at 14:08:55
C:\PROGRA-1\HAPSRUN\METHOD\CAE5.LSM
C:\PROGRA~1\HAPSRUN\METHOD\TGPC5
05/13/98 at 15:04:40
Acquisition Method : C:\PROGRA~1\HAPSRUN\METHOD\LLK.FSM
Tune/Cal File :
Datafile title:
Cylinder #5 - 300 ppb
CAE/EMI OCI-TG Test
5-12-98
W = RT +- ( 0:45.00 / 2 + RT * 0.010 )
Min Fit=0.650; Min Pur=0.650; Min Area=5000
Width= 5-100 scans; Res= 6 scans; NLM=2.0
Linear calibration curve
Internal Standards:
I.S. #1 ~ TRIS
Concentration = 9.940 ppm; 6 calib points
pt. File Man.
1 CAE5010A
2 CAE5010B
3 CAE5001A
4 CAE5001B
5 CAE5300A
6 CAE5300B
Area
1582120
1621917
1723046
1587595
1586445
1679727
Average RF
Resp. Factor
159166.99346
163170.71558
173344.65869
159717.79826
159602.10410
168986.61064
= 1.63998e+05
Q
I.S. #2 -- BPFB
Concentration = 4.850
ppm; 6 calib points
pt. File Man.
1 CAE5010A
2 CAE5010B
3 CAE5001A
4 CAE5001B
5 CAE5300A
6 CAE5300B
Analytes:
Analyte Jf 1 — Vinyl Chloride
6 calib points
pt. File M I Cone.
I CAE5010A ( 10.00
2 CAE5010B I 10.00
Area
3358073
3410616
3539976
3509273
3236082
3314609
Average RF =
Resp. Factor
692386.19918
703219.80764
729891.97312
723561.45753
667233.41518
683424.54952
6.99953e+05
Cratio I
1.006e+00 I
1.006e+00 I
Area
2165622
2160957
Aratio
1.369e+00
1.332e+00
Resp. Fact
1.36060e+
1.32435e+
210
-------
4 CAE5001B
5 CAE5300A
b CAE5300B
1.UU l.U06e-ul i
1.00 1.0066-01 i
0.30 3.018e-02 I
0.30 3.0186-02 I
Analyte #2 -- Carbon Disulfide
6 calib points
pt. File M
1 CAE5010A
2 CAE5010B
3 CAE5001A
4 CAE5001B
5 CAE5300A
6 CAE5300B
Cone. Cratio
9.27 9.326e-01
9.27 9.326e-01
0.93 9.326e-02
0.93 9.326e-02
0.28 2.798e-02
0.28 2.798e-02
Analyte #3 — Vinyl Acetate
6 calib points
pt. File M I
1 CAE5010A |
2 CAE5010B i
3 CAE5001A |
4 CAE5001B I
5 CAE5300A I
6 CAE5300B I
Cone. Cratio
10.00 1.006e+00
10.00 1.0066+00
1.00 1.0066-01
1.00 1.006e-01
0.30 3.018e-02
0.30 3.018e-02
Analyte #4 — Chloroform
6 calib points
pt. File M I Cone.
1 CAE5010A | 9.98
2 CAE5010B | 9.98
3 CAE5001A | 1.00
4 CAE5001B | 1.00
5 CAE5300A I 0.30
6 CAE5300B I 0.30
Analyte #5 — Benzene
6 calib points
pt. File M I Cone.
1 CAE5010A | 9.97
2 CAE5010B 9.97
3 CAE5001A 1.00
4 CAE5001B 1.00
5 CAE5300A 0.30
6 CAE5300B 0.30
Cratio
,0046+00
004e+00
004e-01
004e-01
3.012e-02
3.012e-02
Cratio
,003e+00
,003e+00
,003e-01
003e-01
,009e-02
3.0096-02 I
^7305
206588
58750
63814
l.jlye-'Ji •
1.3016-01 i
3.7036-02 !
3.799e-02 i
L.jiizye-i-UL
1.29346e+OC
L.227016+OC
i.25876e+OC
Average RF = 1.29591e+
Area
27700628
28016282
2757646
2750234
780285
793336
Area
15574405
15489580
1586515
1581212
442870
446005
Area
15574405
15489580
1586515
1581212
442870
446005
Area
29162668
29444264
2654030
2625366
707165
652889
Deviation
Aratio 1
1.7516+01 !
1.727e+01 1
1.600e+00 1
1.732e+00 1
4.918e-01 1
4.723e-01 1
Average RF
Deviation
Aratio 1
9.844e+00 1
9.550e+00 I
9.208e-01 1
9.960e-01 1
2.792e-01 I
2.655e-01 1
Average RF
Deviation
Aratio 1
9.844e+00 I
9.550e+00 1
9.208e-01 I
9.960e-01 I
2.792e-01 1
2.655e-01 1
Average RF
Deviation
Aratio 1
1.843e+01 1
1.815e+01 1
1.540e+00 1
1.654e+00 1
4.458e-01 1
3.887e-01 1
Average RF
Deviation
= 2.26639%
Resp. Factor
1.87740e+01
1.852206+01
1.71612e+01
1.857536+01
1.757986+01
1.688126+01
= 1.79156e+
= 1.32425%
Resp. Factor
9.78495e+00
9.49287e+00
9.15237e+00
9.900046+00
9.249466+00
8.797646+00
= 9.39622e+(
= 2.62476%
Resp. Factor
9.804566+00
9.511896+00
9.17071e+00
9.919886+00
9.268006+00
8.81527e+00
= 9.41505e+C
= 2.62476%
Resp. Factor
1.837726+01
1.809946+01
1.535686+01
1.64870e+01
1.48138e+01
1.29173e+01
= 1.600866+0
= 1.57232%
Analyte #6 — Bromodichloromethane
6 calib points
3
-------
' 0.1'J 1-1 I
1 f,'AE5010A i
2 CAE5010B I
'i CAE5001A i
4 CAE5001B I-
5 CAE5300A I
6 CAE5300B I
. uIlC. .CdLlO I Al'-d
'*.97 1.0036 + 00 i 22716664
9.97 1.0036+00 I 22289668
1.00 1.003e-01 ! 2241200
1.00 1.0036-01 I 2257115
0.30 3.0096-02 I 625526
0.30 3.009e-02 I 607161
I
J_
1
3
3
i \ L d L -I ,,
. 4 36e-t 01
.374e+01
.301e+00
.422e+00
.943e-01
.6156-01
Average
Ueviat
' i
i
I
i
1
i
1
RF
ion
\i;
1
1
1
1
1
1
=
=
Op. I -Ji t_ L ,.
.'13l64e + C
.37014e+C
.29681e+t
.4l744e+C
.31036e+f
.20125e+C
1.33794C
3. 747005
Anaiyte §7 -- MIBK
3 calib points
pt. File M I
1 CAE5010A I
2 CAE5010B |
3 CAE5300A I
Anaiyte #8 -- Toluene
6 calib points
pt. File M I
1 CAE5010A I
2 CAE5010B I
3 CAE5001A I
4 CAE5001B I
5 CAE5300A I
6 CAE5300B I
Cone. Cratio I
10.10 1.016e+00 I
10.10 1.016e+00 I
0.30 3.048e-02 I
Cone. Cratio I
9.99 1.005e+00 I
9.99 l.OOSe+00 I
1.00 l.OOSe-Ol I
1.00 l.OOSe-01 I
0.30 3.015e-02 I
0.30 3.015e-02 I
Anaiyte #9 — Tetrachloroethene
6 calib points
pt. File M |
1 CAE5010A I
2 CAE5010B I
3 CAE5001A |
4 CAE5001B I
5 CAE5300A I
6 CAE5300B I
Cone. Cratio
10.22 2.107e+00
10.22 2.107e+00
1.02 2.107e-01
1.02 2.107e-01
0.31 6.322e-02
0.31 6.322e-02
Anaiyte #10 — Bromoform
6 calib points
pt. File M I
1 CAE5010A I
2 CAE5010B I
3 CAE5001A I
4 CAE5001B I
5 CAE5300A I
6 CAE5300B I
Cone. Cratio I
5.38 1.1096+00 I
5.38 1.109e+00 I
0.54 1.109e-01 I
0.54 1.1096-01 I
0.16 3.328e-02 I
0.16 3.328e-02 I
Area
978934
1152249
25106
Area
32334980
31693392
2554943
2469059
639063
673848
Area
8034173
8030984
689925
704770
148601
150283
Area
4634349
4629078
358207
376628
81094
88169
Aratio I Resp. Factc
6
7
I
.187e-01
.104e-01
.583e-02
Average
Deviat
i
1
1
RF
ion
6.
6.
5.
08946e-(
99170e-(
191546-1
6.09090<
10.0533!
\ .^CP
Aratio 1 Resp. Fact<
2.044e+01 I 2
1.9546+01 I 1
1.4836+00 I 1
1.555e+00 I 1
4.028e-01 i 1
4.012e-01 I 1
Average RF =
Deviation =
Aratio I Resp. Fact
,03355e+
,94429e+
,47538e+
,54744e+
,33604e+
. 33052e+
1.61120
4.12348
2.392e+00 I 1
2.355e+00 I 1
1.949e-01 i 9
2.008e-01 I 9
4.592e-02 | 7
4.534e-02 I 7
Average RF =
Deviation =
,13538e+
11745e+
24895e-
,53062e-
26393e-
.172116-
9.29065
1.55812
v - \-i-
Aratio I Resp. Fact
l.J80e+00 I 1.
1.357e+00 I 1.
1.012e-01 I 9,
1.0736-01 I 9.
2.506e-02 I 7,
2.660e-02 I 7,
Average RF =
Deviation =
22355e-
12207e-
67509e-
53022e-
99322e-
9.8328'
2.1659
Anaiyte #11 -- Styrene
o cdlib points
-------
CAE5010A
CAE5010B
CAE5001A
CAE5001B
CAE5300A
CAE5300B
A red
4430152
4705562
L 4 7 4 0 1 3
1543280
299676
293701
7
7
4
4
9
8
/il'ciC 1'J
.2756+00
.2446+00
. 164e-0i
.398e-01
.2606-02
.8616-02
Average
Deviat
1
I
1
1
RF
ion
rv,'0
3 .
3 _
,-. .
^L .
± .
1.
=
=
p . L j e. L v L
53193e+00
51672e+00
02152e+OC
13503e+00
49861e+00
43393e+00
2.35629e+(
2.98926%
-------
APPENDIX C
SELECTED EXAMPLE FIELD DATA
-------
Chrotnatogram: c: \progra~l\hapsrun\data\aaa\7-25\725cc#5
Run: 07/25/98 at 07:39:13
ccc 300ppb Ifs
Max=3337600
100
V)
Scans 1 to 649
RTime 0:10.77 to 8:19.16
75
50
25
SYSTEM CONTINUING CALIBRATION
Internal Standard
Benzene
TIC
Internal Standard #2
Ethyl Benzene
m/p-Xylene
>\tyrene n f\ o-Xylene
-------
JThromatogram: c:\progra~l\hapsrun\data\aaa\7-24\ted72401 Scans 1 to 786
Run: 07/24/98 at 09:14:20 RTime 0:10.82 to 10:02.48
Tunnel Exhaust Duct
.4ax=2551038 TUNNEL EXHAUST DUCT FULL GC TRACE
100
75
50
25
TIC
LfS
T
Air Peak
Internal Standard #1
Internal Standard #2
0 I
-------
SIM Set #1 c:\progra~l\hapsrun\data\aaa\7-24\ted72411
Run: 07/24/98 at 12:17:50
Tunnel Exhaust Duct fsim2 |
Scans 1 to 677
RTime 1:00.38 to 4:59.58
Max=701513
100
"V 75
50
25
Max=29244
100-
75
50-
25
0
Max=19360
100
75
50
25
40 second equilibration
Internal Standard #1
Benzene
Mass 69.00
i'T" r' i
Mass 78.00
Mass 91.00
\ Toluene
-------
SIM Set #2 c:\progra~l\hapsrun\data\aaa\7-24\ted72411
Run: 07/24/98 at 12:17:50
Tunnel Exhaust Duct sim2
40 second equilibration
Max=25591
100
Scans 1 to 674
RTime 5:00.39 to 8:58.49
>
75
50
25
0
Max=13019
100
75
50
25
0
Max=742508
100
75
50
25
0
Mass 91.00
(\
m/p-Xylene
v^
A
\
^^ ,,n ,. , |'ai|.i:i| .i,| B
Mass 104.00
Mass 117.00
30 60 90 120 150 180 210 240 270 300 330 360 390 420 450 480 510 540 570 600
-------
:hromatogram: c:\progra~l\hapsrun\data\aaa\7-25\sed72502 Scans 1 to 1380
£un: 07/25/98 at 09:20:01 RTime 0:10.82 to 16:47.22
Silo Exhaust Duct complete fs
.4ax=4847004
100 : 'SILO EXHAUST DUCT FULL GC TRACE
75
50
25
Internal Standard #1 (TRIS)
Internal Standard #2 (BPFB)
TIC
80 160 240
320 400 480* 560 640* ' 720 800 880 960 1040 1120 1200 1280
-------
50
25
0
Max=71843
100
75
50
25
n •
Ihromatogram: c : \progra~l\hapsrun\data\aaa\7-25\sed72502
Run: 07/25/98 at 09:20:01
Silo Exhaust Duct complete fs
Max=4847004 ZOOM GC TRACE
100
75
Scans 114 to 720
RTime 1:32.44 to 8:50.36
initmtjiin|iiii|iip;nnpii:iT^;tin[iiii[mp[Mi^^ ii[iiiii'i\|
m/p-Xyl
TIC
Mass 91
o-Xylene
V-..W' Vv-,, <.,...,,
1 t i* '» i ' • i i • • i
-T-,, , [I it..,,,. 1- • _._-.r-r J.,1 J |-
-------
Full Scan c:\progra~l\hapsrun\data\aaa\7-25\sed72502
Normalization Mass: 91; Run: 07/25/98 at 09:20:01
Silo Exhaust Duct complete fs
Max=40904 Spectrum 280; Background 196-267, 294-340
1.0 m/z;
RTime 3:32.40
100
N
75
50
25
91
65
51
52
56
70
79 86
71
I72|!
Toluene
92
93
95
-------
NIST hit #2 of 100; 1.0 m/z; Toluene
NIST hits of S [280]B[196-267,294-340] SED72502
Silo Exhaust Duct complete fs
SI=790; Formula=C7H8; MW=92; CAS#=108883; EPA#=61278;
Run: 07/25/98 at 09:20:01
100
75-
50
25
65
51
45
52
66 77
91
Toluene from NIST Library
92
93
-------
Chroma togram: c : \progra~l\hapsrun\data\aaa\7-25\sed72502
Run: 07/25/98 at 09:20:01
Silo Exhaust Duct complete fs
Max=4847004
100
75
50
25
0
Max=57306
100
75
50
25
IS#1
I"'" "I '•'! ' r "I"' i"'!'' I •T'Y"H™l'Tlli'TIn '''|<"'«<|'''»'|»'>H™ITI"T"
Scans 114 to 720
RTime 1:32.44 to 8:50.36
TIC
IS#2
Mass 78
..fI ;i.(
120 150 180 210 240 270 300 330 360 390 420 450 480 510 540 570 600 fiin
-------
Chromatogram: c:\progra~l\hapsrun\data\aaa\7-25\sed72502
Run: 07/25/98 at 09:20:01
Silo Exhaust Duct complete fs
Max=4847004
Scans 59 to 580
RTime 0:52.73 to 7:09.19
TIC
NS
Max=116414
] j "•'
Internal Standard #1
Internal Standard
Mass 72
Methyl Ethyl Ketone
tMi|i!H|mi|Hii^
A*>n
/IQO MO
-------
Fall Scan c:\progra~l\hapsrun\data\aaa\7-25\sed72502
Normalization Mass: 72; Run: 07/25/98 at 09:20:01
Silo Exhaust Duct complete fs
Max=103404 Spectrum 125; Background 83-118, 132-149
72
Mass Spectrum of MEK
1.0 m/z;
RTime 1:40.41
Mass
57
I 59
|MM|iiti|litt|mt|M<
60
73
8691 98
80 100
i j u < t j i •
120
* j 1 1 » < i n 1 1 j
140
1 fin
f 1 1 1 n 1 1 1 1 j i n i ' * m } 1 1 * i n t uj * ' M u " ' | < t J ", t <
isn onn
i jr * M xt !| ) m i mi) m> ntuji • • \ m !, " t(
O A f\ ^ r r\
-------
..'.romatogram: c: \progra~l\hapsrun\data\aaa\7-25\sed72502
-jn: 07/25/98 at 09:20:01
Silo Exhaust Duct complete fs
:ax=4847004
Nl
.-Iax=105130
Internal Standard #1
Carbon Disulfide
tti|i!iijiitT|Tiinn!i-i*'miti|iiii|iiiiiT' ^ii|mi[mr]™TjTT'iri''|ni
i ^/\ 1 c A i QH 71 n
Scans 59 to 580
RTime 0:52.73 to 7:09.19
TIC
Internal Standard
j!iifiiti(|mi|im|' mtiit(Hii|imj
Mass 76
ftj»ii|iiiijniipiT|TTTTpinf^I]TApffi]Tiii|^^
330 360 390 420 450 480 510 540
-------
-"ull Scan c:\progra~l\hapsrun\data\aaa\7-25\sed72502
iormalization Mass: 76; Run: 07/25/98 at 09:20:01
Silo Exhaust Duct complete fs
-------
5IM Set #1 C:\progra~l\hapsrun\data\aaa\7-25\hmlobag2
Run: 07/25/98 at 12:50:27
Hot Mix Load Out - Bag Sample sim
,4ax=681157
100
Scans 1 to 677
RTime 1:00.39 to 4:59.64
75
50
25-
0
Max=29759
100
75
50
25-
J
,4ax=17677
100
75-
50
25
Mass 69.00
Interal Standard #1
W|MipM|mfii|iu|nN|iifiiipiiii|iii|iiyin|ijpiiii|iii|iiu|^ r
A i \ Benzene
J1
A...^
^-;.! .|nl | , lp ( ,., [(., ln| , ..^:,
Mass 78.00
,-. ' ;.-' ••.
""I ......... |"»I
Mass 91.00
30 60 90 120 150 180 210 240 270 300 330 360 390 420 450 480 510 540 570 600 630
-------
SIM Set #2 C:\progra~l\hapsrun\data\aaa\7-25\hmlobag2
Run: 07/25/98 at 12:50:27
Hot Mix Load Out - Bag Sample sim
Max=24270
100
Scans 1 to 674
RTime 5:00.39 to 8:58.55
Mass 91.00
50
25-
0
Internal Standard #2
irpp-npnr-y
Max=11000
100
75
50
Max=711732
100
75
50
25
0
,.^11 1,11,1
; m/p-Xylene
thy! Benzene
o-Xylene
-.'
, i ii| i ii'ini n,, :,'i
Mass 104.00
Mass 117.00
r\ r\ /rin
-------
VOLUME 3
APPENDIX D
QA/QC DATA
-------
£)
All American Asphalt Plant
Irvine, California
Date
Page
1998
l of 2
Quality Control Check
Prior to Start of Tests
Keep all cleaned glassware sealed until train assembly
Assemble trains in dust free environment
Visually inspect each train for proper assembly
Level and zero manometer
Calculate proper sampling nozzle size
Visually inspect sampling nozzle for chips
Visually inspect Type S Phot tube
Leak check each leg of Type S Phot tube
Leak check entire sampling train
During Testing
Read temperatures ana ainerenuiu pressures at each
traverse point
Sample data and calculations recorded on preformatted
datasheets
Unusual occurrences noted in test log
Properly maintain the roll and pitch of axis of Type S
Phots a"d sampling nozzle
Leak check train before and after any component
changes during test
Maintain the probe and filter temperature
Maintain ice in ice water bath and maintain impinger
Calibration forms reviewed for completeness and
accuracy
Data sheets reviewed by PM daily during testing
Observation
cW
C*4SWJ^
-------
Date July*?/, 1998
Page 2 of 2
Quality Control Check
After Testing
Visually inspect sampling nozzle
Visually inspect Type S Pitot tube
Leak check each leg of the Type S Pitot tube
Leak check the entire sampling train
Record observations if any
Field Log
Project name/ID and location
Sampling personnel (names/position)
Geological observations including map
Sample run times and dates \\A ^c
Sample descriptions
Description of QC samples
Deviations from QAPP
Difficulties in sampling or unusual conditions
Sample Labels
Sample ID
Date and time of collection
Lab technician initials
Analytical parameter
Preservative required
Observation
AJ^x^~-
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yi • f\jiL HI /i •/ >/ /
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f LJr ^ UJJ u^U^^ Liiij1^
^toi/^'J4By6«,j) 7/?//gP fer
A61&1 ^ff/r ^^»-*ic /W"
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LT
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JMfMA flfff QUltif pm\
\r\'»'-f ^ t- *J * \ \ o^AXjuJs^t.^
f^xjL^ ^O^A^jtkie CL»i»V
-------
All American Aspnalt rxanc
Irvine, California
, 1990
1 of 5
I. Test Run Observations Date
R - Recommended
M - Mandatory
1. Train set ap ' filter ID
filter weight
filter checked for holes
filter centered
nozzle clean • • •
nozz le • undamaged
nozzle diameter (in;}
probe liner clean
probe markings correct
probe heated along
entire- length
impingers- charged
impittgers- iced
meter* box leveled- • • •
pitot manometer* zeroed
orifice- manometer- zeroed
filter- box- or- holder- at- temp-.
all ball joints lightly
• greased ' •
all -openings -capped.
2. Train leak check LC- H
at nozzle: initial (R-)- • VAC
v '
• •it&>
• -tit* •
><^i
• /<5fe3' ' '
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-i—
Test
Run
3
•
Test
Run
4
i
233
-------
Date
R - Recoooended
M " Mandatory
4. M-3 sampling train check:
initial \nJ
(should hold
10 in. vacuum zinai \ni
for- i/2* min. )
Pur^e sample train- with- stack- gas
Constant' rate sampling 1' par
5. Time- test' started*
• Time test" ended-
6. Dry gas ( * - )• p_orf initial
meter final
volume: (* * * )• port' initial - *
final
( • )• port- initial
• • final
( ) • port initial
TED
Test
Run
1
•frSfrf
' i i
I\
'"/l/'/rr
• *
• • K/
-7'0^
• • /3{ ^fe
*tq*y> %'
\
final \'&?7,yt£
7. Train operation Nozzle changed
during run during run -
NOT ALLOWED
pitch' and- yaw of- probe- o.kv
nozzle* not scraped- on- nipple
effective- seal- around- probe
probe moved- af proper* time
probe .heated* • •
calculator constants or nomograph
changed when TS and /or TM
changes- significantly
average time to set
isokenetics after probe
moved* to- next* point
Average values:
impinger temperature
should be •£ 7u F
Post filter gas streamer or
Filter box temggj-ttui>« -y^.
« circle one
stack- temperature- •
barometric- P taken* and* value
was probe ever disconnected
from filter holder while in
stack?
was filter chanced during run?
/t/o .
-• •tyx4 •
• • *7UV •
• '<«VCA
• ^\j~^
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Test
Run
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vo
July^1/, 199G
•"•S6 2 of 5
Test
Run
3
Test
Run
4
t • • •
f • • •
• • •
• • ••(••••
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3&, 3J (• • • •
>oc)
AJo \ AJ &
-------
•July (9 y, 1993
., , ,
3 of 3
Date
R * Recommended
M - Mandatory
Check on filter holder loosening of
clamping device holder
was silica gel changed
during^ run?
was any particulate lost*?
Accurate ftp $4n*cn*<, Sj Kl &P(/*Mt.b) Th-
reading Of* AH XhKA**LLf /^tAl" fa, ... IWtu/U. lit H- 1.0
meter temperature- • » • • • . • • - •
stack temperature
meter* vacuum*
tune- per' point
imoinger* temperature
filter- box temperature
Minimum sample time of 'p^fJOi ' min met
Minimum sample volume of /kf;3Vrd«ef collected
8. Post test: •* All* openings* sealed
- recovery- area* clean* sheltered
-• filter handled- with- gloves*, * forceps*
- petri" dish sealed, labeled*
- any,- sample lost * * •
grad cyl.
weighed
water- measured- raL • gms
- silica- gel" weighed-, * net- gow
- condition - color
Z* spent
- probe* cooled* sufficiently
- nozzle removed- and' brushed
- probe brushed 6* times * * •
- nozzle- brushes- clean *
- wash bottles clean
- acetone clean
- M-8 15* minute* purge
- water/solution clean
- blank taken: acetone*, water; other-
Probe brush- and extension clean'. '
Sample container*- Clean
Capped*
Lane led
Sealed
Liouid- level* marked-
Ten
Test
Run
1
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Run
4
* ' '
•
... .
-------
Date
R - Recommended
M • Mandatory
*
9. Post test Orsat Analysis of Initial (M)
integrated bag sample Orsat
analyzer - Analyzer leak check
(levels should not fall below Final (M)
cap. Cubing and not more than
0.2 mL in burrette for 2 rain.)
Orsaf samples? Each bag analyzed" 3- times-
Z C0«> agrees- within- 0-.2X' • • •
X" Oy agrees- within 0-.2X
I- CO- agrees- within- 0;2X
Analysis at end of test. Orsat analyzer
checked against air' (20i9 *• 0;3)
Orsat Analysis:
CO ft,
OtZ
obi
Fo - 20.9' — T02
z co7
Fuel- • ••"•"" •'"
Ffl range- for- fuel
Orsat- analysis" valid"
Orsat solutions changed
when calculated F0
exceeds fuel type- range-
ID. All samoles locked uo
All samoiing" components- clean* and- sealed
All data- sheets submitted to* — fr~— — T*"--j4-
- Orsat
- Run- isokenetie" • • • Team/ Ob server
- Particuiate- recovery
- Process- data
- Charts •
• -• Calibration sheets
1?P
Test
Run
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4 of 5
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4
1- • • •
1" " •
1"
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1 . . .
r • •
f
Hud.
-------
Page
5 of 5
J. NOTES: Care should be taken, when sampling for organic compounds, to
follow stringent quality control guidelines to avoid contamination of the
sample and sampling train. Take note of any occurences which could bias
the sample in any manner.
Include: (1) General comments; (2) Changes to pretest agreement with
justification; (3) Identify (manufacturer) and describe condition of
sampling equipment; (4) any abnormal occurrences during test program.
(Additional page(s) attached: Yes »X, No • .)
Signature of Observer
Affiliation of Observer
Date
23?-
-------
All American Asphalt Plant
Irvine, California
• or
Date Juiy,7J~, 1998
Page l of 2
ftn«IHv tf"\Mi*ml ffiiifir
Prior to Start of Tests
Keep all cleaned glassware sealed until tram assembly
Assemble trains in dust free environment
Visually inspect each train for proper assembly
Pal 1 t» suunnltnvfuvtviesize
Laicuiaie proper &uupi g »
visuauy inspect irnpipi"ig niuuie iu» uiips
Visually inspect Type S Pitot tube
Leak check each leg of Type S Pitot tube
T.eak check entire samolinK train
During Testing
_. . ,
Read temperatures and dinercntial pressures at each
iiAveise point
SaniDie *ifl^ii tmd ffliiCWiftiMMis recorded on irr^Torniattfiu
data sneets
Unusual occurrences noted in test log
Property maintain the roll and pitch of axis of Type S
Pitots and sampling nozde
Lfyic check train before and after any component
changes during test
. —
Maintain the probe and niter temperature
Maintain ice in ice water bath and maintain impinger
exit temperature
accuracy
Data sheets reviewed by PM daily during testing
Ohonr.
UoscrvaaoB
d
-------
Date July«?.T» 1998
Page 2 of 2
Quality Control Cheek
After Testing
Visually inspect sampling nozzle
Visually inspect Type S Pilot tube
T Mlr dwlr MrJt leff ofthe TVDB S PltOttUbC
Leftk check the entire sampling train
*
Record observations if any
Field Log
Project name/ID and location
Sampling personnel (names/position)
Sample ran times and dates
Sample des criptioos
Description of QC samples
Deviations from QAPP
Difficulties in sampling of unusual conditions
Sample Labels
Sample ID
Date and time of collection
Trfih technician initials
Analytical parameter
_ . • j
Preservative lequired
Observation
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If.
-------
All American Asphalt Plant
Irvine. Califo
~
A
July ;?J7~ 199 G
Pa8« 1 of 5
I. Test Run Observations Date
R - Recomneoded
M * Mandatory
1. Train set up - filter ID
filter weight
filter checked for holes
filter centered
nozzle clean • • •
nozz le • undamaged
nozzle diameter (ini)
probe liner clean
probe markings correct
probe heated along
entire- length
impingers- charged
impingers- iced
meter- box leveled- • - • • • •
pitot manometer- zeroed
orifice- manometer* zeroed
filter- boar or- holder- ar temp-.
all ball joints lightly
greased '
all- openings- canned
2. Train leak check LC-
at nozzle: initial
(Uf,^
f
• I/
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1
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-------
, 199G
2 of 5
Date
R - Recommended
H " Mandatory
4. M-3 sampling train check:
initial \nj
(should hold
10 in. vacuum final' \M) •
for- 1/2- min. )
Purge sample train- with- stack- gas
Constant rate sampling 1- pnr
5. Time- test' started-
Time tesf ended-
6. Dry gas (' ' ')* port- initial
meter final
volume: (" ' ' )• port- initial " "
/> 4- T / -,"™.-T ™..f\?*,i"" -'-- — ,
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4
. .
t '
1 . . . .
t • • • •
-------
3 of 5
Date .
R - Recommended
M - Mandatory
Check on filter holder loosening of
clamping device holder
was silica gel changed
during run?
was any particulate lost?
Accurate 6P
reading of* AH • •
meter temperature . • •
stack temperature
meter* vacuum
tine- per* point
impinger- temoerature
filter- box temoerature
Minimum sample time of _• / • min met
Minimum sample volume of • • uS dacf collected
8. Post test: — All- openings- sealed
- recovery- area- clean* sheltered
- filter handled- with- gloves',' forceps-
- petri dish sealed, labeled-
- any- sample lost
grad cyl.
weighed
water* measured- mL • • gins
- silica gel weighed; net- gas
- condition - color
f- spent*
- probe- cooled- sufficiently
- nozzle removed- and' brushed
- probe brushed 6- times • '
- nozzle- brushes- clean
- wash bottles clean
- acetone clean
- M— 8 15- minute- purge
- water/ solution clean
-blank taken: acetone; water; other-
Probe brush- and extension clean; '
Sample container?- Clean
Capped-
Laoeied
Sealed
Liouid- level* narked-
7^
Test
Run
1
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r
| . . .
-------
Page
4 of 5
Date-
R • Recommended
M - Mandatory
9. Post test Orsat Analysis of Initial (M)
integrated bag sample Orsat
analyzer - Analyzer leak check
(levels should not fall below Final (M)
cap. tubing and not more than
0.2 mL in burrette for 2- min. ) •
Or sac- samples:- Each bag- analyzed- 3- tines'
2 CO? agrees- within- Ov2X • •
V Of agrees- within 0-.2X
-co- agrees- within- 0-.2X
Analysis at end of teat. Orsat analyzer
Orsat Analysis:
o?* . . . . .
coz
Fo » 20.9 — Z Qt
% CO.,
Fuel
F^rantTe for- fuel
Orsat analysis- valid 1
Orsat solutions changed /
when calculated Fo
exceeds fuel type -range
10. All samples locked up
All sampling- components- clean- and- sealed
- Orsat
- Run' isokenetic* • • • Team/Observer
- Particuiate- recovery
— Process* daca
- Charts
Test
Run
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.
-------
Page 5 of 5
J. NOTES: Care should be taken, when sampling for organic compounds, to
follow stringent quality control guidelines to avoid contamination of the
sample and sampling train. Take note of any oceurences which could bias
the sample in any manner.
Include: (1) General comments; (2) Changes to pretest agreement with
justification; (3) Identify (manufacturer) and describe condition of
sampling equipment; (4) any abnormal occurrences during test program.
(Additional page(s) attached: Yes
-------
All American Asphalt Plant
Irvine, California
Date
Page
1998
1 of 2
Quality Control Check
Prior to Start of Tests
Keep all cleaned glassware sealed until train assembly
Assemble trains in dust five environment
Visually inspect each train for proper assembly
Level and zero manometer
Calculate proper sampling nozzie size
Visually inspect sampling nozzle for chips
Visually inspect Type S Pitot tube
T frit rhrrk Mich lev of TVP* S Phot tube
During Testing
traverse point
datasheets
Unusual occurrences noted in test log
Properly maintain the roll and pitch of axis of Type S
Pitots and sampling nozzle
Leak check train before and after any component
changes during test
Maintain the probe and fiber temperature
Calibration forms reviewed for completeness and
accuracy
Data sheets reviewed by PM daily during testing
Observation
ji.
QV-AVJc.
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/.
-------
Date Juiyo?/, 1998
Page 2 of 2
Quality Control Check
After Testing
Visually inspect sampling nozzle
Visually inspect Type S Pitot tube
Leak check each leg of me Type S Pitot tube
Record observations if any
Field Log
Project name/ID and location
Sampling personnel (names/position)
Geological observations including map
Sample run times and dates
*• i j • •
Sample descriptions
Description of QC samples
Deviations from QAPP
Difficulties in sampling or unusual conditions
Sample Labels
Sample ID
Date and time of collection
Lab technician initials
Analytical parameter
Preservative required
Observation
0Ur»«_k_
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-------
All American Asphalt Fiant
, Irvine, California
^35*^
Page
, 1990
1 of 5
I. Test Run Observations Date
R * Recommended
M « Mandatory
1. Train set-op ' filter ID
filter weight
filter checked for holes
filter centered
nozzle clean • • •
nozzle • undamaged
nozzle diameter (in;)
probe liner clean
probe markings correct
probe heated along
entire- length
impingers- charged
impingers- iced
meter- box leveled- - - - • • • •
pitot manometer- zeroed
orifice- manometer* zeroed
filter- box- or- holder- at- teimr.
all ball joints lightly
- - greased
all openings -capped
2. Train leak check LC-
at nozzle: initial (R-)- • VAC
«QP2 cfm @ 15 LC ^
in. Hg initial, intermediate (R) VAC
Intermediate and LC'
final at highest intermediate (R) VAC
Vacuum during LC
test run.) intermediate (R) VAC
final (H) LC
VAC
3. Pitot lines leak initial positive line (R)
check: negative- line (R-)- • •
(hold 3 in. f^OJ
final* • positive* line* (M-)' • *
on manometer for
(15 sec.; negative- line- \R)
' pitot- tube* undamaged-
M-3 bag initial leak check (M)
Tedlar bag: Should hold 2 to 4 in. H^O
pressure- for- 10 minutes- or
zero flow meter reading on
continuous evacuation* or-
Completely fill bag and let
stand overnight— no deflation.
set
Test
Run
1
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-------
Page
, 199G
2 of 5
Date
R - Recommended
M » Mandatory
4. M-3 sampling train check:
initial \Mv
(should hold
10 in. vacuum rinai \.n)
for- 1/2-min. J
Pnr^e sample train- with- stack- gas
Constant rate sampling 1 pn
5. Time- tesf started-
Time tesf ended
6. Dry zas 1- • •)• port- initiai
meter finai
volume: (• )• port- initiai -
finai
( ) port- initiai
• • • finai
(.' • ) • port initiai
/Mr
Test
Run
1
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7. Train operation Nozzle changed
during run during ran -
HOT" ALLOWED
pitch- and- yaw of- probe- o-.kr.
nozzle- not scraped- on- nipple
effective- seai- around- probe
probe moved- af proper- time
probe .heated •
calculator constants or nomograph
changed when TS and /or TM
changes- significantlv
average time to set
isokenetics after probe
moved* to- next* point
Average values:
impinger temperature
should be S 70 F
Post filter gas streamer or
Filter box cempera^ttju^^
^250*F + 2^b <320T.
r circle one
stack' temperature- •
barometric- P taken- and- value
was probe ever disconnected
from filter holder while in
scack?
was filter chanced du.ri.ne run?
tsv
• • --to**s •
• • */-tLo-
• •>c--pca-
MM"
Test
Run
2
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-------
, 1993
3 of 5
Date
R - Recommended
M - Mandatory
Check on filter holder loosening of
clan-pine device holder
was silica gel changed
during run?
was any particulate lost?
Accurate 6P Ibn^,.^, ffa. £jk A? ( /*> .flt-i)) 'S1"
reading of* AH 'A*Ttj'j(u fajfa $J?,± f tu //i.0 '
meter temperature* * /• • • . - * - •
stack temperature
meter- vacuum
time- per* point
impinger- temperature
filter* box temperature
Minimum sample time of • • J3&- min met
Minimum sample volume of d«cf collected
8. Post test: — All- openings- sealed
- recovery- area- clean- sheltered
- filter handled* with* gloves", • forceps-
- petri* dish sealed, labeled* *
- any* sample lost *
grad cyl.
water measured 9^' faL •• gms
- silica gel weighed-, net* gun
- condition - color
5- spent '
- probe- cooled- sufficiently
- nozzle removed- and* brushed
- probe brushed 6- times * * •
- nozzle- brushes- clean
- wash bottles clean
- acetone clean
- M-8 15- minute- purge
- water/solution clean
- blank caken: acetone-, water*. other-
Probe brush' and extension clean*. *
Samoie container-* Clean
Capped*
Labeled
Sealed
Liouid* level* marked*
-5£>
Test
Run
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-------
Page
of 5
Date
R • Recommended
M - Mandatory
9. Post test Orsat Analysis of Initial (MJ
integrated bag sample orsat
analyzer - Analyzer leak check
(levels should not fall below Final (M)
cap. tubing and not more than
0.2 mL in barrette for 2'min. ) •
Orsaf samples: Each bar analyzed 3' times-
Z' CO? agrees- within- 0-.2X- • •
I' 0? agrees- within 0-.2X
X- COvajrees- within- 0-.2X
Analysis at end of test. Orsat analyzer
checked against air (20;9' +• 0-.3)
Orsat Analysis:
cd'f
Fo « 20.9 -iS Q?
• z co9
Fuel
F^range for- fuel
Orsat- analysis' valid'
Orsat solutions changed
when calculated F0
exceeds fuel type -range-
10. All samoles locked up
All samoiing- components- clean- and- sealed
- Orsat
rlfefl
Test
Run
1 _
MM i
fA ..
i
•/HA"
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-------
Page 5 of 5
NOTES: Care should be taken, when sampling for organic compounds, to
follow stringent quality control guidelines to avoid contamination of the
sample and sampling train. Take note of any occurences which could bias
the sample in any manner.
Include: (1) General comments; (2) Changes to pretest agreement with
justification; (3) Identify (manufacturer) and describe condition of
sampling equipment; (4) any abnormal occurrences during test program.
(Additional page(s) attached: Yes X. No • .)
Signature of Observer Affiliation of Observer Date
-------
All American Asphalt Plant
/
Date
Page
1998
l of 2
Quality Control Check
Prior to Start of Tests
Keep ail cleaned glassware sealed until train assembly
Assemble trains in dust free environment
•
Visually inspect each train for proper assembly
Level and zero manometer
Calculate proper sampling nozzle size
Visually inspect sampling nozzle for chips
Visually inspect Type S Phot tube
Leak check each leg of Type S Phot tube
, , , , . ,.
Leak check enure sampling tram
During Testing
rl jfiffiunrtilll n O.
traverse point
{Samnl* riiitii anH calciltfltions recnffrii*H on nrgfai miitliui
riftft sheets
TTm««nal rti-N • i • ii'^»cga tinted in tatf loff
Properly maintain the roll and pitch of axis of Type S
Pitots and sampling nozzle
Leak check train before and after any component
changes during test
Maintain the probe and filter temperature
Maintain ice in ice water bath and maintain imptngcr
exit icnipcfsturc
Calibration forms reviewed for completeness and
accuracy
Data sheets reviewed by PM dairy during testing
Observation
^TLXr^t o
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-------
Date Juiy«?J , 1998
Page 2 of 2
Quality Control Cheek
Observation
After Testing
Visually inspect sampling nozzle
<*1>S"1>-
Visually inspect Type S Phot tube
Leak check each leg of the Type S Pitot tube
Leak rhrrlf the entire sampling train
Record observations if any
Field Log
at
Project name/ID and location
Sampling personnel (names/position)
Geological observations including map
Sample run times and dates
Sample descriptions
Description of QC samples
Deviations from QAPP
Difficulties in sampling or unusual conditions
Sample Labels
Sample ID
Date and time of collection
Lab technician initials
X//5
Analytical parameter
.i; V
Preservative required
-------
All American Asphalt Fiant
2
fit.
Pa8*
1990
of 5
I. Test Run Observations Date
R • Recommended
M - Mandatory
1. Train set up • filter ID
filter weight
filter checked for holes
filter centered
nozzle clean • • •
nozz le • undamaged
nozzle diameter (in;)
probe liner clean
probe markings correct
probe heated along
entire- length
impingers- charged
impingers- iced
meter- box leveled- •
• • • • pitot manometer- zeroed
orifice* manometer- zeroed
filter- box- or- holder- ar temp-.
all ball joints lightly
greased
all' openings- capped
2. Train leak check LC* •
at nozzle: initial (R-)- • VAC
«QP2 cfm @ 15 LC
in. Hg initial, intermediate (R) VAC
Intermediate and LC •
final at highest intermediate (R) VAC
Vacuum during LC
test run.) intermediate (R) VAC
final CM) LC
VAC
3. Pitot lines leak initial positive line (R)
check: negative- line (R-)" * -
(hold 3 in. H2O)
final- • positive- line- (M->- * *
on manometer for
(15 sec.) negative- line- (R)*
citot* tube* undamaged- '
M-3 bag initial leak check (M)
Tedlar bag: Should hold 2 to 4 in. H->0
pressure* for- 10' minutes* or
zero flow meter reading on
continuous evacuation* or-
Completely fill bag and lee
stand overnight— no deflation.
5% J
Test
Run
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-------
Pa«e
2 of 5
Date,
R « Recommended
M - Mandatory
4. M-3 sampling train check:
initial vnv
(should hold
10 in. vacuum final (M) •
for- l/2-min.-J
Purge sample train- with- stack- gas
Constant- rate- sampling 1- OB-
5. Time- tesf started-
- Time tesf ended-
6. Dry aas (• ' )• porf initial
meter final
volume: {' ' J- porf initial
final
(. • •)• porf initial
• ' -final
{ • )• port initial- • •
final
7. Train operatipn Nozzle changed
during run during run —
NUl ALLOWED
pitch- and- yaw of- probe- o.kv
nozzle* not scraped- on nipple
effective- seal- around* probe
probe moved- at- proper* time
probe .heated- • • •
calculator constants or nomograph
changed when TS and /or TM
changes- significantly-
average time to set
isokenetics after probe
moved to next point • • • • • • .
Average values:
impinger temperature
snouio DB i iv i
Post filter gas streamer or
Filter box temperature
2Sn-v^~2S7> <320*F,
• "F circle one
barometric- P taken- and- value
was probe ever disconnected
from filter holder while in
stack?
was filter chanced during run?
~fO
Test
Run
1
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Test
Run
3
• •
. .
1
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Test
Run
4
•
....
-------
Date
R » Recommended
M " Mandatory
Check on filter holder loosening of
clamping device holder
was silica gel changed
during run?
was any particulate lost?
Accurate & P /t»H<^ >SL fLt~ f\P( I'M /-hb)'/**1
reading of-: AH /Wu^l fliJh* VnLL:.* Kjii4A*Jm^
meter temperature- • f • * . • * * *
stack temperature
meter* vacuum-
time- per- point
impinge r- tenner a ture
filter' box tetnoerature
Minimum sample time of JJJJJ^ min met
Minimum sample volume or ____"___ dacf collected
8. Post test: -• All- openinres- sealed
- recovery area- clean* sheltered
— filter handled- with- gloves',- forceps-
- pecri dish sealed, labeled
- any* sample lost
grad cyl.
weighed
vater- measured* raL • • RIDS
- silica gel- weighed*, net' gnu
- condition - color
t* spent
- probe- cooled- sufficiently
- nozzle' removed* and' brushed
- probe brushed 6- times • • •
- nozzle* brushes* clean*
- wash bottles clean
- acetone clean
- M-8 15" minute- ourge
- water/solution clean*
- blank taken: acetone*,'- vater; other-
Probe brush and extension clean*, *
Satnoie container-: • Clean
Capped-
Laoeied
Sealed
Liouid* level* marked*
sen
Test
Run
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-------
Page
4 of 5
Date
R - Recommended
H * Mandatory
-
9. Post test Orsat Analysis of Initial (MJ
integrated bag sample Orsat
analyzer - Analyzer leak check
(levels should not fall below Final (M)
cap. tubing and not more than
0.2 raL in barrette for 2-min.) •
Orsaf samples: • Each bag analyzed 3- times-
%• COt agrees- within- 0-.2X' • • •
t- 0? agrees- within 0-.2X
X CO- agrees- within- 0;2X
Analysis at end of test. Orsat analyser
checked against air (20;9' +• Q-.3)
Orsat Analysis:
/*n V. ...
CO?*
o?z
cox
Fo - 20.9 — Z 62
• z co?
Fuel
F,.., range for- fuel
Orsat analysis- valid
Orsat solutions changed
when calculated F0
exceeds fuel type- range-
ID. All saraol.es locked up
All sampling- components- clean- and- sealed-
All data- sheets submitted to- observer
- Orsat
- Run- isokenetic- • • • Team/Observer *i
- Particuiace' recovery
- Process- data
- Charts
— Calibration sheets
,5>P
Test
Run
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] If"
T j| •
/ '
•^Y^
•>«L»
s
S0^t^' "t" x£pX ' '
,^L,>t
•^A*^
• >iiuv '
' *-\*^ '
*At*S\
Test
Run
3
Test
Run
4
t
•- |- - H
1-
* *
,
i
. . . . i
t ' ' 1!
, . . . .j. . . fe
• • r n
t • • • }
• f t
1
f
t •
(• • ....
•fife' -<2iK
-------
, 1993
Page 5 of 5
J. NOTES: Care should be taken, when sampling for organic compounds, to
follow stringent quality control guidelines to avoid contamination of the
sample and sampling train. Take note of any occurences which could bias
the sample in any manner.
Include: (1) General comments; (2) Changes to pretest agreement with
justification; (3) Identify (manufacturer) and describe condition of
sampling equipment; (4) any abnormal occurrences during test program.
(Additional page(s) attached: Yes f>/t No ' .)
-?V<5XV
Signature of Obsatver Affiliation of Observer Date
-------
THERMOCOUPLE CALIBRATION
CALIBRATED BY: J".
DATE :
Thermocouple
number
S-3A
S-4A
S-14A
S-15A
S-16A
S-17A
S-19A
ES 78
ES 87
P-14
TC 20
TC 21
TC 22
TC 23
TC 24
TC 25
Thermocouple
reading
(°C)
0
0
0
0
1
1
0
1
1
0
0
1
0
0
-1
2
22
21
21
21
22
21
22
22
22
22
22
21
21
22
22
24
100
100
99
99
100
100
100
99
100
100
99
99
100
99
100
101
Thermometer
reading
(°C)
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
2
22
21
21
21
21
22
22
22
22
22
22
22
22
22
22
24
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
Thermometer Serial Number: A98-289
Certification Date: 03/19/98
Test Number: 157797
Thermometer Standard Serial Number: 128239
NIST I.D. Number: 88024
-------
TEMPERATURE SENSOR CALffiRATION FORM
Temperature Sensor No.
Ambient Temp. °F
Sensor Type \< - t c. Length
Reference Temp. Sensor:
Barometric Pressure, "Hg ^^-
Date
.«-<»*
r \
. t
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
VA^*
N^
*£lO
Temp. °F
Ref.
Sensor
-*•*.
^3>
**c.
Test
Sensor
3C
73
-LOG
Temp.
Diff. %
,fcv3
o
Ci
Within
Limits
Y/N
X"
S
Y
Calibrated
By
\u^>
\Jv\^»
Xu^
. _ _. „ U?ef. Temp + 460) - ( Test Temp.
% Temp. Diff - — tn *—xr~ ..-,..
* (Ref. Temp. + 460)
460)
100 a: 1.5 %
-------
TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No.
Ambient Temp. °F T3
Sensor Type \C - 1 CL Length
Reference Temp. Sensor:
Barometric Pressure, "Hg "Sex 2.=
Date
• Z/t-'nY
t I
£ 1
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
iCir
KT.O
toAAk,
NAK>.
Bo i<-,
HrO
Temp. °F
Ref.
Sensor
S^
-13
t.^
Test
Sensor
1>T-
^.Sr
2- /o
Temp.
Diff. %
0
-.^•Sb
,'IV\
Within
Limits
Y/N
V
Y
N
Calibrated
By
\w>>
\uV
V^\3
V
% Temp. Diff = (j?ef • TemP ; 4f0) - ( Test TeinP- +
(Ref . Temp. + 460)
46°)
x 100 S 1 5 V
-------
TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No.
Ambient Temp. °F
Sensor Type
Reference Temp. Sensor:
Length
Barometric Pressure, "Hg 2
Date
I -IWt
1 1
i >
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
ice
H*-°
fc/v\A.
t>r\r<~
^oit-j
HZ.O
Temp. °F
Ref.
Sensor
*^-^
TC
1. to
Test
Sensor
^t.
^^
-Z-\ 0
Temp.
Diff. %
c
— o • ?& c«<
6
Within
Limits
Y/N
Y
X"
x:
Calibrated
By
\^
^
Vort>
% Temp. Diff
(Ref ' TemP
reznp. ^ 460)
(Ref. Temp. + 460)
-------
9/30/94: CD2-1
CALIBRATION DATA SHEET 2
Typa S Phot Tuba Inspection
D*gfM Mtartng tov*l futtbftt ft*
0i Md fk
1 mum! •nri PanuHwtlr^ilar?
Damagad?
a, MO«Sff, s +10»)
e, M0«*0zsi 410*)
ft, «-5« * ^ * -t-5'l
ft, f~6» S ft, S +5»)
r
e
z- Atanr 1* 0.125'!
w - Atane Is 0.03125')
Of (3/16* S O, S 3/8')
A
AOO, n-os s PA/D, «1.5)
v^^>
Nc
/V'^
o
I
o
I
0
o
o
o
Vs-
.*t'5V
/. -<£-V
OAAZCCtodr
Completeness
LagibUtv
I certify that the Type Sptot tuba/probe O*
Accuracy
Specific atlona
Reasonableness
meets or exceeds an specifications.
criteria and/or applicable design features and is hereby assigned a pilot tuba caibration factor C, of 0.84.
Certified by:
Personnel (Sionatuie/Datak
• (Signature/Date)
-------
CALIBRATION DATA S WET 2
Type S Pftot Tub* Inspection
9/30/94: CD2-1
determining 6t
Level and Perpendteulaf?
Obstruction?
Damaged?
a, (-10* se, s -H0«)
o2 MO«S02 * + 10»)
&, f«* s ft, S +5*1
ft, (-5« i &, S 4-B«)
r
e
z - Atanr (* 0.125')
w - AtanO Is 0^3125*1
o, one' s o, s 3/8-)
A
A/2D, (1^)5 « P^/D, £1.5)
Ves
o^
p— '
/Oi 2>
o
0
o
l"
^
v>
\
0
- .0 l TV
l/v
|, O's-c.
/, i>u
QAXDCCAN*
Completanass
UglbBty
Accuracy
Specifications
Reasonableness
I carttfy thattha Typa S pitot tubc/brab* Of
Rf -Ji
meats or aiccaadi an specifications.
criteria and/or applicable design features and is hereby assigned a pitot tube caHbratkm factor C. of 0.84.
S ^ \
Certified by: ,' \>J -^
'J Personnel (Sionature/D*te)
(Signature/Daw)
-------
TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No. PC M >ooT Sensor Type
Temp. °F ~
Reference Temp. Sensor:
-l*'1*
/•
•'
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
H^s
M A.
%^'
•
Temp. °F
Ref.
Sensor
9 ***
So
1* .
T~o1>
Test
Sensor
3.3
•7.3"
to-y
•
Temp.
Diff. %
0
.1^7
0
•-••
Within
Y/N
V
Y
Y
- -
Calibrated
By
Ai^>
S(Lrt>
ku%
^
•
*
% Temp. Diff -
" ( regt
460)
(.Ref. Tenp. * 460)
x 100 s 1.5 V
-------
TEMPERATURE SENSOR CAUBRATION FORM
Temperature Sensor No. D&M - \
Ambient Temp. °F _ 14
Reference Temp. Sensor:
^ .
Sensor Type K -TC Length v
___ Barometric Pressure, "He
Date
^1 *•"»&'
«
tf
Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
l-Uo
te\ <*-
"^okc.
•
Temp. °F
Ref.
Sensor
33
7&
1*r
"*,{ O
•
Temp.
Diff. %
.4
-------
REFERENCE METER CALIBRATION
ENGLISN REFERENCE METER UNITS
Barometric Pressure 29.82
Meter VH 1.00000
K ( deg R/ Inches Ng) 17.64
Dry Gas Meter
Tim Pressure Meter Readings
(•In) (In. N20)
20.50
5.00
13.00
8.50
27.50
26.50
14.00
15.50
12.50
23.50
17.50
15.00
32.00
35.Cy
15.00
-8.000
-8.000
-8.000
-5.400
-5.400
-5.400
-3.800
-3.800
-3.800
-2.400
-2.400
-2.400
-1.600
-1.600
-1.600
Initial
742.719
768.193
774.402
790.575
798.821
825.423
850.983
861.899
953.219
962.970
976.611
986.740
995.413
1008.596
1022.986
DGN Serial f 6841495
Date 10/5/97 Filei
Revii
(DGM) Tesperature Wet Test Meter (UTN)
Votuee Initial Final Meter Readings Voluee T<
Final (cubic feet)
768
774
790
798
825
850
861
873
962
976
986
.193
.402
.375
.821
.423
.983
.899
.960
.970
.611
.740
995.413
1008.596
1022.986
1029.158
25.474
6.209
16.173
8.246
26.602
25.560
10.916
12.061
9.751
13.641
10.129
8.673
13.183
14.390
6.172
(deg F)
78.0
79.0
79.0
79.0
79.0
80.0
81.0
81.0
86.0
86.0
87.0
87.0
88.0
89.0
89.0
(deg F)
79.0
79.0
79.0
79.0
80.0
81.0
81.0
82.0
86.0
87.0
87.0
88.0
89.0
89.0
90.0
Initial
671.890
697.180
703.325
719.309
727.485
753.809
779.025
789.820
879.651
889.205
902.599
912.545
921.069
934.025
948.175
Final (cubic feet) (d
697.180
703.325
719.309
727.485
753.809
779.025
789.820
801.740
889.205.
902.599
912.545
921.069
934.025
948.175
954.255
25
6
15
Max
8
26
25
Max
.290
.145
.984
Yds - Nil
AvftTiW
.176
.324
.216
Yds - Mil
Averaoi
10.795
11
9
Max
.920
.554
Yds - Mil
eWcrMi
13.394
9.946
8.524
Max
Yds - Nil
Averam
12.956
14.150
6.080
I F:\DATAFILE\CALIBRAT\CAL MENU.DSKVDGN REF.
06/08/95
OGM
Coefficient
Flow
ap Coefficient Variation Rate
0 F) Yds Vds-(Avg.Yds) (CFM)
77.0 1.016 0.002 1.208
77.0 1.013 0.000 1.204
77.0 1.012 -0.002 1.204
Yds -0.003626886 Must be no greater than 0.030
Yds -1.013636253 Must be between 0.95 to 1.05
77.0 1.009 0.001 0.942
77.0 1.008 0.000 0.938
77,0 1.006 -0.001 0.932
Min Yds -0.002262496 Must be no greater than 0.030
Yds -1.007525980 Must be between 0.95 to 1.05
77.0 1.006 0.001 0.755
77.0 1.006 0.001 0.753
78.0 1.004 -0.001 0.747
Min Yds -0.002245979 Must be no greater than 0.030
Yds -1.005164785 Must be between 0.95 to 1.05
78.0 1.003 -0.001 0.557
78.0 1.004 0.000 0.556
78.0 1.006 0.002 0.556
Nin Yds -0.002785363 Must be no greater than 0.030
Average Yds -1.004591811 Must be between 0.95 to 1.05
78.0 1.006 -0.002 0.396
78.0 1.007 0.000 0.395
78.0 1.010 0.002 0.396
Max Yds - Min Yds -0.004205886 Must be no greater than 0.030
Average Yds -1.007822494 Must be between 0.95 to 1.05
Overall Average Yds -1.007748265
I certify that the above Dry Gas Meter was calibrated in accordance with E.P.A. Method 5 , paragraph 7.1 ;CFR 40 Part 60.
using the Precision Uet Test Meter f 11AE6, which In turn was calibrated using the Ann-lean tell Prover f 3785.
certificate * F107, whJcX is traceable to the National Bureau of Standards (N.I.S.T.).
Signature
Date
-------
of2
PACIFIC ENVIRONMENTAL SERVICES. INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Date:
PD«, in Hg
10/13/97
29.86
Calibrator MMD
Meter Box No.: RMB-15
Reference Meter Correction Factor 1.0077 (10/5/97)
AH = 0.5
Trial
1
2
3
Trial
Duration
(min)
15
13
12
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
48.833
54.722
59.821
Final
(ft3)
54.722
59.821
64.544
Net
(ft3)
5.089
5.099
4.723
Meter Temperatures
Initial, Inlet
CR
73
78
80
Final, Inlet
CR
77
80
83
Avg. Inlet
CR
75
79
81.5
Initial, Outlet
CF)
72
74
76
inal, Outle
CF)
75
75
77
Avg. Cutlet
CF)
73.5
74.5
76.5
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
34.044
39.829
44.843
Final
(ft3)
39.829
• 44.843
49.463
Net
(ft3)
5.785
5.014
4.620
Meter Temperature
Initial
CF)
71
71
Final
CF)
70
70
71
Avg.
CF)
70
70.5
71
Meter Box
Correction
Factor
T
0.997
1.001
0.999
Reference
Orifice Press
AHe
(in. H20)
1.86
1.86
1.86
AH = 0.75
Trial
1
2
3
Trial
Duration
(min)
8
21
13
Dry Gas Meter RMB-15
Gas Volume
Initial
_J?!L_,
69.524
73.327
83.322
Final
(ft3)
73.327
83.322
89.571
Net
(^
3.803
9.995
6.249
Meter Temperatures
Initial, Inlet
CF)
74
77
78
Final, Inlet
CF)
74
83
82
Avg. Inlet
CF)
74
80
80
Initial, Outlet
CF)
77
76
78
inal, Outle
CR
75
77
74
Avg. Outlet
CF)
76
76.5
76
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
54.365
58.108
67.912
Final
(ft3)
58.108
67.912
74.036
Net
(ft3)
3.743
9.804
6.124
Meter Temperature
Initial
CF)
72
72
73
Rnal
CF)
72
73
73
Avg.
CF)
72
72.5
73
Meter Box
Coueution
Factor
Y
0.996
0.997
0.995
Reference
Orifice Press
AH0
(in. H20)
1.91
1.91
1.88
AH= 1.0
Trial
1
2
3
Trial
Duration
(min)
19
8
16
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
89.777
100.214
104.614
Final
(ft3)
100.214
104.614
113.404
Net
10.437
4.400
8.790
Meter Temperatures
Initial, Inlet
CR
82
85
85
Final, Inlet
CR
86
87
88
Avg. Inlet
CR
84
86
86.5
Initial, Outlet
CR
79
81
82
inal, Outle
CR
80
81
83
Avg. Outlet
CR
79.5
81
82.5
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
74.254
84.440
88.743
Final
(ft3)
84.44
88.743
97.302
Net
(ft3)
10.186
4.303
8.559
Meter Temperature
Initial
CR
73
73
73
Rnal
CR
73
73
73
Avg.
CR
73
73
73
Meter Box
Correction
Factor
T
0.997
1.002
1.000
Reference
Orifice Press
AH0
(in. HjO)
1.92
1.91
1.92
15 10137.XLS
Printed: 6/11/98
-------
2of2
PACIFIC ENVIRONMENTAL SERVICES. INC.
Central Park West
5001 South Miami Boulevard. P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
AH = 2.0
Trial
1
2
3
Trial
Duration
(min)
9
7
7
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
13.863
20.884
26.372
Final
^
20.884
26.372
31.871
Net
(ft3)
7.021
5.488
5.499
Meter Temperatures
Initial, Inlet
CF)
87
90
90
Final, Inlet
CF)
91
92
93
Avg. Inlet
CF)
89
91
91.5
Initial, Outlet
CF)
83
84
84
inal, Outle
(°F)
83
84
84
Avg. Outlet
CF)
83
84
84
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
97.749
104.591
109.929
Final
(ft3)
104.591
109.929
115.281
Net
(ft1)
6.842
5.338
5.352
Meter Temperature
Initial
CF)
73
73
73
Final
CF)
73
73
74
Avg.
CF)
73
73
73.5
Meter Box
Correction
Factor
1
1.001
1.002
1.002
Reference
Orifice Press
AH0
(in. H20)
1.90
1.89
1.88
AH = 4.0
Trial
1
2
Trial
Duration
(min)
6.5
15.5
Dry Gas Meter RMB-15
Gas Volume
Initial
(ft3)
32.371
39.484
Final
(ft3)
39.484
56.484
Net
(If)
7.113
17.000
Meter Temperatures
Initial, Inlet
CF)
92
93
Final, Inlet
CF)
94
97
Avg. Inlet
CF)
93
95
Initial, Outlet
CF)
85
87
inal, Outle
CF)
85
87
Avg. Outlet
CF)
85
87
Trial
1
2
Reference Meter
Gas Volume
Initial
(ft3)
15.775
22.732
Final
(ft3)
22.732
39.287
Net
(ft3)
6.957
16.555
Meter Temperature
Initial
CF)
73
73
Rnal
CF)
74
73
Avg.
CF)
73.5
73
Meter Box
Correction
Factor
y
1.004
1.005
Reference
Orifice Press
AH0
(in. H2O)
1.92
1.92
Calibration Results
AH
0.50
0.75
1.0
2.0
4.0
r I
0.999
0.996
1.000
1.002
1.004
AHe
1.86
1.
1.
1.
1.
90
92
89
92
Dry Gas Meter RMB-1S on 10/13/97
Meter Box Calibration Factor
Meter Box Reference Orifice Pressure
• Two Trial Average
1.000
1.90
15 10137.XLS
Printed: 6/11/98
-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
Central Park West
5001 South Miami Boulevard, P.O. Box 12077
Research Triangle Park, North Carolina 27709-2077
(919) 941-0333 FAX: (919) 941-0234
Posttest Dry Gas Meter Calibration Form (English Units)
Pretest Calibration Factor
System Vacuum Setting, (in Hg)
Reference Meter Correction Factor
Date: 8/5/98 Pbar- in Hg
1.000
18.6
1.008
30.20 Calibrator: JB
Meter Box No.
RMB-15
AH= 1.41
Trial
1
2
3
Duration
(min)
10
10.5
10
Dry Gas Meter
Initial
(ft3)
187.547
194.69
202.214
Final
(ft3)
194.69
202.214
209.383
Net
(ft3)
7.143
7.524
7.169
Initial, Inlet
(°F)
72
73
73
Final, Inle
(°F)
73
73
74
Avg. Inlet
(°F)
72.5
73
73.5
Initial, Outlet
(°F)
70
71
72
Final, Outlet
(°F)
71
72
72
Avg. Outlet
(°F)
70.5
71.5
72
Trial
1
2
3
Reference Meter
Gas Volume
Initial
(ft3)
496.874
503.931
511.377
Final
(ft3)
503.931
511.377
518.444
Net
(ft3)
7.057
7.446
7.067
Meter Temperature
Initial
(°F)
68
68
69
Final
<°F)
68
68
69
Avg.
(°F)
68
68
69
Meter Box
Correction
Factor
Y
0.999
1.002
0.997
Reference
Orifice Press
AHg
(in. H20)
1.55
1.53
1.55
15 10137
PostTest08-5-98
9/15/98
-------
AUG-H-98TOE 3:56 PM PES-BALDW PARK. CA FAI N0. 8188140820
P. 4
DICKMUNNS COMPANY
Liquid end Cat • Ftowmcler Calibration Service
10571 Calle Lee - 133 • LosAlamitos, California 90720
Telephone (562) 596-JSS9 - Telefax (714)827-0823
CERTIFICATE OF CALIBRATION
Client Name:
Reference Number:
Instrument Manufacturer:
Instrument Description:
Model Number:
Serial Number:
Mfg.Rated Accuracy:
Accuracy Given:
PES INC.
ROCKWELL
P.O.METER
S-190
25507
V-.5%
AS RECEIVED
Calibration Date:
Calibration Due:
Calibration Fluid:
Test Unil(s):
NIST Traceability Per:
Ambient Conditions:
CERT NUMBER:
PROCEDURE*:
03-27-1998
03-27-1999
AIR § 14.7 PSIA 70S-'
A-4 DUE 4-5-98
M-0122
29.90"HGA 70F
PES25507
NAVAIR-17-20MG
1
2
3
4
5
6
7
8
9
10
IND.SCFM
0.100
0.200
0.300
0.400
0.604
0.802
1.002
1.522
2.551
3.002
ACT.SCFM
0.100
0.200
0.300
0.400
0.605
0.803
1.003
1.523
2.553
3.004
Comments:
All instruments used in the performance of the above calibration are traceabile lo • N.I.S.T. • Calibration has
been performed in accordance with MIL-STD-45662A, ISO 10012-1 and ANSI/NCSL-Z-540-l.(MlN TOLER-
ANCE( )OUT OF TOLERANCE( )USE WITH CALIBRATION CURVE y
TECHNICIAN:
MM,NAVAIR17-20MG-06
Approved By:
MICHAEL MUNHS
-------
2
i
n
I
R
s
D
3
J)
1
Dry Gas Metar No.:
Barometric Press\ne:
Orifice
ManomMei
Setting
0.5
1.0
3.0.
.4.0
Initial
Hefeienctt
DGM
Reading
V-M3
596.775
635.803
648.332
6&8.8S7
Fbnt
Reference
DGM
V-fl3
608.320
647.985
658.45*
669.842
8804737
29.63
Reference
Gas
Vokmte
11.5*5
.t 2.182
.10.123
: 10.985
DRY GAS METER AND ORIFICE CALIBRATION
M«ier Box Mo.: 6A Reference Dry Gas Meter No.:
Calibration Oet«:
Initial
DGM
Holding
V-ft3
150.300
189.100
201.600
212.100
Flrul
DGM
Reading
V-H3
161.767
201.246
111.712
223.062
Tett
OGM
Volume
V-«g«
(d
- '^'J
•••:!$*''•
'rJ/^Sl
f^gr;
Run
Time
minutes
30.5
23.0
13.5
10.O
25507 Rockwell
Joe Rubio
Ftow
fUte
O>cfm
:/fi«ft- -•
";!<$&£': ':-
.'S'^f :•,'••'
'•!%&&••
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*
Avai age
Grnnm*
i vi.Al 1 : .
•?Si^
\y '•• :••.'
TM^O;^
Delt* H @
.1.979 •
? ;-».9^T
L^L-9*^-
'^j&a^
:, K018V
:; VASti''-
c:
G"
I
I
cc
ex
tl
o.
I
tic
Si=>
t—
tr
*
tz
>c
p=
<—
s»
a:
oc
oc
CD
CO
0*1
OH
-------
DRY GAS METER AND ORIFICE CALIBRATION
Dry Gas Meter No.: 8804737
Meter Box No.:
6A
Reference Dry Gas Meter No.: 25507 Rockwell
Barometric Pressure: 29.56
Calibration Date:
6/30/98
Calibration Performed By:
Joe Rubio
Orifice
Manometer
Setting
H = "H20
O.S
1,0
2.0
4,0
Initial
Reference
DGM
Reading
V-ft3
447.200
457.703
468.213
479.460
Final
Reference
DGM
Reading
V = ft3
457.372
467.948
478.925
490.396
Reference
Gas
Volume
Vr = ft3
10*172
10.245
10.712
10.936
Initial
DGM
Reading
V=ft3
158.000
168.600
179.200
190.500
Final
DGM
Reading
V = ft3
168.258
178.917
189.971
201.433
Test
DGM
Volume
Vd = ft3
10.288
10,317
10.771
10,933
Temperature
Reference
DGM
tr = F
74
77
76
75
DGM
Inlet
t = F
78
83
88
82
DGM
Outlet
t = F
75
78
84
81
DGM
Average
td
77
81
86
82
Run
Time
minutes
27.0
19.0
14.0
10.0
Flow
Rate
Q = cfm
0.37
O.S2
0,74
1.07
Meter
Gamma
0*995
0.987
1,008
1,002
Delta H @
2,008
1.969
1.928
1,896
Average
1,001
1,050
-------
DRY GAS METER AND ORIFICE CALIBRATION
Dry Gas Meter No.: 6846739
Meter Box No.:
3A
Reference Dry Gas Meter No.: 25507 (Rockwell)
Barometric Pressure:
29.65
Calibration Date:
8/6/98
Calibration Performed By:
J.Rubio
Orifice
Manometer
Setting
H = 'H2O
0.5
1,0
2.0
4.0
Initial
Reference
DGM
Reading
V=ft3
548.190
559.243
570.059
581.690
Final
Reference
DGM
Reading
V»ft3
558.822
569.638
580.761
595.765
Reference
Gas
Volume
Vr-ft3
10.632
10,395
10.702
14,075
Initial
DGM
Reading
V = ft3
806.000
817.000
827.800
839.400
Final
DGM
Reading
V = ft3
816.600
827.375
838.482
853.475
Test
DGM
Volume
Vd = f t3
10.600
10,375
10.682
14.075
Temperature
Reference
DGM
tr = F
75
76
77
78
DGM
Inlet
t = F
76
79
82
87
DGM
Outlet
t = F
71
72
75
80
DGM
Average
td
74
76
79
84
Run
Time
minutes
26.5
18.0
13.5
13.5
Flow
Rate
Q = cfm
0.39
0.56
0.77
1.01
Meter
Gamma
0.999
0.999
1,000
1.000
Delta H @
1.782
1.720
1.822
2.095
Average
0.999
1.855
-------
DRY GAS METER AND ORIFICE CALIBRATION
Dry Gas Meter No.: 6846739
Meter Box No.:
3A
Reference Dry Gas Meter No.: 25507 (Rockwell)
Barometric Pressure: 29.60
Calibration Date:
4/15/98
Calibration Performed By:
J.Rubio
Orifice
Manometer
Setting
H = 'H2O
0.5
1.0
2.0
4.0
Initial
Reference
DGM
Reading
V = ft3
251.776
262.662
273.310
284.997
Final
Reference
DGM
Reading
V = ft3
262.166
272.751
283.679
295.231
Reference
Gas
Volume
Vr = ft3
10.390
10.089
10.369
10,234
Initial
DGM
Reading
V = ft3
369.841
380.766
391.500
402.247
Final
DGM
Reading
V = ft3
380.265
390.952
401.942
412.527
Test
DGM
Volume
Vd = ft3
10.424
10.186
10.442
10,280
Temperature
Reference
DGM
tr = F
68
70
71
72
DGM
Inlet
t-F
71
84
91
96
DGM
Outlet
t = F
66
73
77
80
DGM
Average
td
69
79
84
88
Run
Time
minutes
26.0
18.0
13.0
10.0
Flow
Rate
Q = cfm
0.40
0.55
0.78
1.00
Meter
Gamma
0.996
1.004
1.012
1.015
Delta H @
1.769
1.778
1.745
2.112
Average [ 1.007 | 1.851
-------
FROM : Panasonic FflX SYSTEM
PHONE NO.
Sep. 17 1998 10:40PM F
SENSIDYNE, INC.
CALIBRATION CERTIFICATE
CELL S/N: 168S9-S DATE: 05 -13 -1998
This is to certify that the above referenced Gilibrator Flow Cell
was calibrated using film flowmeter MCS-102-A, which has been
calibrated by instruments cirectiy traceable to, the National institute
of Standards and Technology. NIST Report 8361604.
Results:
REFERENCE
MCS-102-A
cc/min
2009
2012
2011
2011
2012
2015
2013
2009
2016
2019
S/N
1S899-S
cc/min
2011
2012
2013
2013
2013
2015
2016
2009
2017
2021
RELATIVE
DiFF.
cc/min
2
0
2
2
'1
0
3
0
1
^
PERCENT
DIFF.
0.1
0.0
0.1
0.1
0.05
0.0
0.15
0.0
0.05
0.1
0.15
1EA.N 2012.7
CALIBRATED BY
2014
vSS/ DATE:OS-18-1998
CODE 300
-------
DRY GAS METER AND ORIFICE CALIBRATION
Dry Gas Meter No.: J169391
Meter Box No.:
VB-6
Reference Dry Gas Meter No.: 25507 Rockwell
Barometric Pressure: 29.54
Calibration Date:
7/14/98
Calibration Performed By:
J Rubio
Orifice
Manometer
Setting
H="H20
t.7
t.7
Initial
Reference
DGM
Reading
V = ft3
544.354
544.695
Final
Reference
DGM
Reading
V-ft3
544.695
545.377
Reference
Gas
Volume
Vr=ft3
0.341
0.682
Initial
DGM
Reading
V=ft3
0.000
0.356
Final
DGM
Reading
V=ft3
0.356
1.075
Test
DGM
Volume
Vd = ft3
0.356
0.719
Temperature
Reference
DGM
tr = F
69
70
DGM
Inlet
t = F
77
79
DGM
Outlet
t = F
79
83
DGM
Average
td
78
81
Run
Time
minutes
10.0
20.0
Flow
Rate
Q-cfm
0,03
0.03
Meter
Gamma
0.970
0.964
Average 0,967
-------
EVER READY THERMOMETER CO., INC.
228 LACKAWANNA AVENUE
WEST PATTERSON, NJ 07424
(973) 812-7474
PAGE 1 OF
REPORT OF CALIBRATION
LIQUID-IN-GLAS S-THERMOMETER
CALIBRATED BY EVER READY THERMOMETER CO.
MARKED: ERTCO CAT 611-3FC S/N-A98-289
RANGE: -20 TO +110 DEGREES C IN 1 DEGREE GRADUATIONS.
THERMOMETER
READING
0.0 C
37.0
56.0
CORRECTION
(ITS-90)**
0.0 C
0.0
-0.1
** ALL TEMPERATURES IN THIS REPORT ARE BASED ON THE INTERNATIONAL
TEMPERATURE SCALE OF 1990 (ITS-90) PUBLISHED IN THE METROLGIA 27,
NO. 1, 3/10/90.
THIS THERMOMETER WAS CALIBRATED AGAINST A STANDARD CALIBRATED AT THE
NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY (NIST) FORMERLY THE
NATIONAL BUREAU OF STANDARDS (NBS) IN ACCORDANCE WITH ASTM METHOD
E 77, AND NBS MONOGRAPH 174.
FOR A DISCUSSION OF ACCURACIES ATTAINABLE WITH SUCH THERMOMETERS SEE
NBS MONOGRAPH 250-23.
IF NO SIGN IS GIVEN ON THE CORRECTION, THE TRUE TEMPERATURE IS HIGHER
THAN THE INDICATED TEMPERATURE; IF THE SIGN GIVEN IS NEGATIVE, THE TRUE
TEMPERATURE IS LOWER THAN THE INDICATED TEMPERATURE. TO USE THE CORREC-
TIONS PROPERLY, REFERENCE SHOULD BE MADE TO THE NOTES GIVEN BELOW.
THE THERMOMETER WAS TESTED IN A LARGE, CLOSED-TOP, ELECTRICALLY HEATED,
LIQUID BATH, BEING "IMMERSED" 76MM. THE TEMPERATURE OF THE ROOM WAS
ABOUT 25 DEGREES C (77 DEGREES F). IF THE THERMOMETER IS USED UNDER
CONDITIONS WHICH WOULD CAUSE THE AVERAGE TEMPERATURE OF THE EMERGENT
LIQUID COLUMN TO DIFFER MARKEDLY FROM THAT PREVAILING IN THE TEST,
APPRECIABLE DIFFERENCES IN THE INDICATIONS OF THE THERMOMETER WOULD
RESULT.
THE TABULATED CORRECTIONS APPLY PROVIDED THE ICE POINT READING IS
0.0 DEGREES C. IF THE ICE-POINT READING IS FOUND TO BE HIGHER (OR LOWER)
THAN STATED, ALL OTHER READINGS WILL BE HIGHER (OR LOWER) TO THE SAME
EXTENT.
TEST NUMBER: 157797
DATE: 03/19/98
STANDARD SERIAL NO. 128239
NIST IDENTIFICATION NO. 88024
Charles Tang-Nian
QUALITY CONTROL
.GER
-------
Pitot Tube Calibration Data Sheet
Calibrated by: ^
Date.: '
Pitot Tube I.D.
Effective Length:
Pitot Tube Assembly Level ? H Yes D No
Pitot Tube Openings Damaged ? D Yes IS No
If Yes, Explain
8 -
Z = A sin 7 = O . Ol 5 cm (in.) 0.32 cm (
-------
-------
-------
-------
VOLUME 3
APPENDIX E
PROJECT PARTICIPANTS
-------
-------
PROJECT PARTICIPANTS
Affiliation
USEPA
Pacific Environmental Services,
Inc.
Emission Monitoring, Inc.
(PES Subcontractor)
Enthalpy Analytical, Inc.
(PES Subcontractor)
Name
Michael L. Toney, EMC
John Chehaske
Frank Phoenix
Dennis P. Holzschuh
Michael Maret
Dennis D. Holzschuh
Nick Nielson
Troy Abernathy
Joe Rubio
Josh Letorneau
Jessica Swift
Jairo Barreda
Laura Kinner, Ph.D
James Peeler
Brian Purser
Responsibility
Work Assignment Manager
Program Manager
Project Manager and
Field Team Leader
QA Coordinator
Site Leader/Console Operator
Site Leader/Console Operator
Site Leader/Console Operator
Site Leader/Console Operator
Site Leader/Console Operator
Process Monitor
Process Sample and Met.
Station Coordinator
Sample Recovery Coordinator
GC/MS Operator
GC/MS Operator
EPA Method 18 Console
Operator
-------
VOLUME 3
APPENDIX F
TEST METHODS
F.I EPA METHOD 1
F.2 EPA METHOD 1A
F.3 EPA METHOD 2
F.4 EPA METHOD 4
F.5 EPA METHOD 18
F.6 EPA METHOD 315
F.7 SW-846 METHOD 0010
F.8 SW-846 METHOD 0030
-------
APPENDIX F.I
EPA METHOD 1
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 1 - Sample and Velocity Traverses for Stationary Sources
1. PRINCIPLE AND APPLICABILITY
1.1 Principle. To aid in the representative measurement of
pollutant emissions and/or total volumetric flow rate from a
stationary source, a measurement site where the effluent stream is
flowing in a known direction is selected, and the cross-section of
the stack is divided into a number of equal areas. A traverse
point is then located within each of these equal areas.
1.2 Applicability. This method is applicable to flowing gas
streams in ducts, stacks, and flues. The method cannot be used
when: (1) flow is cyclonic or swirling (see Section 2.4), (2) a
stack is smaller than about 0.30 meter (12 in.) in diameter, or
0.071 m2 (113 in.2) in cross-sectional area, or (3) the measurement
site is less than two stack or duct diameters downstream or less
than a half diameter ups1;ream from a flow disturbance.
The requirements of this method must be considered before
construction of a new facility from which emissions will be
measured; failure to do so may require subsequent alterations to
the stack or deviation from the standard procedure. Cases
involving variants are subject to approval by the Administrator,
U.S. Environmental Protection Agency.
2. PROCEDURE
2.1 Selection of Measurement Site. Sampling or velocity
measurement is performed at a site located at least eight stack or
duct diameters downstream and two diameters upstream from any flow
disturbance such as a bend, expansion, or contraction in the stack,
or from a visible flame. If necessary, an alternative location may
Prepared by Emission Measurement Branch EMTIC TM-001
Technical Support Division, OAQPS, EPA
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
be selected, at a position at least two stack or duct diameters
downstream and a half diameter upstream from any flow disturbance.
For a rectangular cross section, an equivalent diameter (De) shall
be calculated from the following equation, to determine the
upstream and downstream distances:
2LW
D =
(L + W)
Eq. 1-1
Where
L = Length and W = width.
An alternative procedure is available for determining the
acceptability of a measurement location not meeting the criteria
above. This procedure,
determination of gas flow angles at the sampling points and
comparing the results with acceptability criteria, is described in
Section 2.5.
2.2 Determining the Number of Traverse Points.
2.2.1 Particulate Traverses. When the eight- and two-diameter
criterion can be met, the minimum number of traverse points shall
be: (1) twelve, for circular or rectangular stacks with diameters
(or equivalent diameters) greater than 0.61 meter (24 in.); (2)
eight, for circular stacks with diameters between 0.30 and 0.61
meter (12 and 24 in.); and (3) nine, for rectangular stacks with
equivalent diameters between 0.30 and 0.61 meter (12 and 24 in.).
When the eight- and two-diameter criterion cannot be met, the
minimum number of traverse points is determined from Figure 1-1.
Before referring to the figure, however, determine the distances
Prepared by Emission Measurement Branch EMTIC TM-001
Technical Support Division, OAQPS, EPA
-------
EMTIC TM-001 EMTIC NSPS TEST METHOD Page 3
from the chosen measurement site to the nearest upstream and
downstream disturbances, and divide each distance by the stack
diameter or equivalent diameter, to determine the distance in terms
of the number of duct diameters. Then, determine from Figure 1-1
the minimum number of traverse points that corresponds: (1) to the
number of duct diameters upstream; and (2) to the number of
diameters downstream. Select the higher of the two minimum numbers
of traverse points, or a greater value, so that for circular stacks
the number is a multiple of 4, and for rectangular stacks, the
number is one of those shown in Table 1-1.
2.2.2 Velocity (Non-Particulate) Traverses. When velocity or
volumetric flow rate is to be determined (but not particulate
matter), the same procedure as that used for particulate traverses
(Section 2.2.1) is followed, except that Figure 1-2 may be used
instead of Figure 1-1.
2.3 Cross-Sectional Layout and Location of Traverse Points.
2.3.1 Circular Stacks. Locate the traverse points on two
perpendicular diameters according to Table 1-2 and the example
shown in Figure 1-3. Any equation (for examples, see Citations 2
and 3 in the Bibliography) that gives the same values as those in
Table 1-2 may be used in lieu of Table 1-2.
For particulate traverses, one of the diameters must be in a plane
containing the greatest expected concentration variation, e.g.,
after bends, one diameter shall be in the plane of the bend. This
requirement becomes less critical as the distance from the
disturbance increases; therefore, other diameter locations may be
used, subject to the approval of the Administrator.
In addition, for stacks having diameters greater than 0.61 m (24
in.), no traverse points shall be within 2.5 centimeters (1.00 in.)
of the stack walls; and for stack diameters equal to or less than
0.61 m (24 in.), no traverse points shall be located within 1.3 cm
(0.50 in.) of the stack walls. To meet these criteria, observe the
procedures given below.
2.3.1.1 Stacks With Diameters Greater Than 0.61 m (24 in.). When
-------
EMTIC TM-001 EMTIC NSPS TEST METHOD Page 4
any of the traverse points as located in Section 2.3.1 fall within
2.5 cm (1.00 in.) of the
stack walls, relocate them away from the stack walls to: (1) a
distance of
2.5 cm (1.00 in.); or (2) a distance equal to the nozzle inside
diameter, whichever is larger. These relocated traverse points (on
each end of a diameter) shall be the "adjusted" traverse points.
Whenever two successive traverse points are combined to form a
single adjusted traverse point, treat the adjusted point as two
separate traverse points, both in the sampling (or velocity
measurement) procedure, and in recording the data.
2.3.1.2 Stacks With Diameters Equal To or Less Than 0.61 m (24
in.). Follow the procedure in Section 2.3.1.1, noting only that
any "adjusted" points should be relocated away from the stack walls
to: (1) a distance of 1.3 cm (0.50 in.); or (2) a distance equal to
the nozzle inside diameter, whichever is larger.
2.3.2 Rectangular Stacks. Determine the number of traverse points
as explained in Sections 2.1 and 2.2 of this method. From Table 1-
1, determine the grid configuration. Divide the stack cross-
section into as many equal rectangular elemental areas as traverse
points, and then locate a traverse point at the centroid of each
equal area according to the example in Figure 1-4.
If the tester desires to use more than the minimum number of
traverse points, expand the "minimum number of traverse points"
matrix (see Table 1-1) by adding the extra traverse points along
one or the other or both legs of the matrix; the final matrix need
not be balanced. For example, if a 4 x 3 "minimum number of
points" matrix were expanded to 36 points, the final matrix could
be 9 x 4 or 12 x 3, and would not necessarily have to be 6 x 6.
After constructing the final matrix, divide the stack cross-section
into as many equal rectangular, elemental areas as traverse points,
and locate a traverse point at the centroid of each equal area. The
situation of traverse points being too close to the stack walls is
not expected to arise with rectangular stacks. If this problem
should ever arise, the Administrator must be contacted for
resolution of the matter.
-------
EMTIC TM-001 EMTIC NSPS TEST METHOD Page 5
2.4 Verification of Absence of Cyclonic Flow. In most stationary
sources, the direction of stack gas flow is essentially parallel to
the stack walls. However, cyclonic flow may exist (1) after such
devices as cyclones and inertial demisters following venturi
scrubbers, or (2) in stacks having tangential inlets or other duct
configurations which tend to induce swirling; in these instances,
the presence or absence of cyclonic flow at the sampling location
must be determined. The following techniques are acceptable for
this determination. Level and zero the manometer. Connect a Type
S pitot tube to the manometer. Position the Type S pitot tube at
each traverse point, in succession, so that the planes of the face
openings of the pitot tube are perpendicular to the stack cross-
sectional plane; when the Type S pitot tube is in this position, it
is at "0° reference." Note the differential pressure (Ap) reading
at each traverse point. If a null (zero) pitot reading is obtained
at 0° reference at a given traverse point, an acceptable flow
condition exists at that point. If the pitot reading is not zero
at 0° reference, rotate the pitot tube (up to ±90° yaw angle),
until a null reading is obtained. Carefully determine and record
the value of the rotation angle (a) to the nearest degree. After
the null technique
has been applied at each traverse point, calculate the average of
the absolute values of a; assign a value.s of 0° to those points for
which no rotation was required, and include these in the overall
average. If the average value of a is greater than 20°, the
overall flow condition in the stack is unacceptable, and
alternative methodology, subject to the approval of the
Administrator, must be used to perform accurate sample and velocity
traverses. The alternative procedure described in Section 2.5 may
be used to determine the rotation angles in lieu of the procedure
described above.
2.5 Alternative Measurement Site Selection Procedure. This
alternative applies to sources where measurement locations are less
than 2 equivalent or duct diameters downstream or less than one-
half duct diameter upstream from a flow disturbance. The
alternative should be limited to ducts larger than 24 in. in
diameter where blockage and wall effects are minimal. A
directional flow-sensing probe is used to measure pitch and yaw
angles of the gas flow at 40 or more traverse points; the resultant
-------
EMTIC TM-001 EMTIC NSPS TEST METHOD Page 6
angle is calculated and compared with acceptable criteria for mean
and standard deviation.
NOTE: Both the pitch and yaw angles are measured from a line
passing through the traverse point and parallel to the stack axis.
The pitch angle is the angle of the gas flow component in the plane
that INCLUDES the traverse line and is parallel to the stack axis.
The yaw angle is the angle of the gas flow component in the plane
PERPENDICULAR to the traverse line at the traverse point and is
measured from the line passing through the traverse point and
parallel to the stack axis.
2.5.1 Apparatus.
2.5.1.1 Directional Probe. Any directional probe, such as United
Sensor Type DA Three-Dimensional Directional Probe, capable of
measuring both the pitch and yaw angles of gas flows is acceptable.
(NOTE: Mention of trade name or specific products does not
constitute endorsement by the U.S. Environmental Protection
Agency.) Assign an identification number to the directional probe,
and permanently mark or engrave the number on the body of the
probe. The pressure holes of directional probes are susceptible to
plugging when used in particulate-laden gas streams. Therefore, a
system for cleaning the pressure holes by "back-purging" with
pressurized air is required.
2.5.1.2 Differential Pressure Gauges. Inclined manometers, U-tube
manometers, or other differential pressure gauges (e.g., magnehelic
gauges) that meet the specifications described in Method 2, Section
2.2.
NOTE: If the differential pressure gauge produces both negative
and positive readings, then both negative and positive pressure
readings shall be calibrated at a minimum of three points as
specified in Method 2, Section 2.2.
2.5.2 Traverse Points. Use a minimum of 40 traverse points for
circular ducts and 42 points for rectangular ducts for the gas flow
angle determinations. Follow Section 2.3 and Table 1-1 or 1-2 for
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 7
the location and layout of the traverse points. If the measurement
location is determined to be acceptable
according to the criteria in this alternative procedure, use the
same traverse point number and locations for sampling and velocity
measurements.
2.5.3 Measurement Procedure.
2.5.3.1 Prepare the directional probe and differential pressure
gauges as recommended by the manufacturer. Capillary tubing or
surge tanks may be used to dampen pressure fluctuations. It is
recommended, but not required, that a pretest leak check be
conducted. To perform a leak check, pressurize or use suction on
the impact opening until a reading of at least 7.6 cm (3 in.) H20
registers on the differential pressure gauge, then plug the impact
opening. The pressure of a leak-free system will remain stable for
at least 15 seconds.
2.5.3.2 Level and zero the manometers. Since the manometer level
and zero may drift because of vibrations and temperature changes,
periodically check the level and zero during the traverse.
2.5.3.3 Position the probe at the appropriate locations in the gas
stream, and rotate until zero deflection is indicated for the yaw
angle pressure gauge. Determine and record the yaw angle. Record
the pressure gauge readings for the pitch angle, and determine the
pitch angle from the calibration curve. Repeat this procedure for
each traverse point. Complete a "back-purge" of the pressure lines
and the impact openings prior to measurements of each traverse
point.
A post-test check as described in Section 2.5.3.1 is required. If
the criteria for a leak-free system are not met, repair the
equipment, and repeat the flow angle measurements.
2.5.4 Calculate the resultant angle at each traverse point, the
average resultant angle, and the standard deviation using the
following equations. Complete the calculations retaining at least
one extra significant figure beyond that of the acquired data.
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 8
Round the values after the final calculations.
2.5.4.1 Calculate the resultant angle at each traverse point:
RA = arc cosine [ (cosineY^ (cosineP^ ]
Eq. 1-2
Where :
Ri = resultant angle at traverse point i, degree.
Yi = yaw angle at traverse point i, degree.
Pi = pitch angle at traverse point i, degree.
2.5.4.2 Calculate the average resultant for the measurements:
n
Eq. 1-3
Where :
Ravg = average resultant angle, degree.
n = total number of traverse points.
2.5.4.3 Calculate the standard deviations:
S =
(n-1)
Bj. 1-4
Where:
Sd = standard deviation, degree.
2.5.5 The measurement location is acceptable if Ravg * 20° and S«
10°.
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 9
2.5.6 Calibration. Use a flow system as described in Sections
4.1.2.1 and 4.1.2.2 of Method 2. In addition, the flow system
shall have the capacity to generate two test-section velocities:
one between 365 and 730 m/min (1200 and 2400 ft/min) and one
between 730 and 1100 m/min (2400 and 3600 ft/min).
2.5.6.1 Cut two entry ports in the test section. The axes through
the entry ports shall be perpendicular to each other and intersect
in the centroid of the test section. The ports should be elongated
slots parallel to the axis of the test section and of sufficient
length to allow measurement of pitch angles while maintaining the
pitot head position at the test-section centroid. To facilitate
alignment of the directional probe during calibration, the test
section should be constructed of plexiglass or some other
transparent material. All calibration measurements should be made
at the same point in the test section, preferably at the centroid
of the test section.
2.5.6.2 To ensure that the gas flow is parallel to the central
axis of the test section, follow the procedure in Section 2.4 for
cyclonic flow determination to measure the gas flow angles at the
centroid of the test section from two test ports located 90° apart.
The gas flow angle measured in each port must be ±2° of 0°.
Straightening vanes should be installed, if necessary, to meet this
criterion.
2.5.6.3 Pitch Angle Calibration. Perform a calibration traverse
according to the manufacturer's recommended protocol in 5°
increments for angles from -60° to +60° at one velocity in each of
the two ranges specified above. Average the pressure ratio values
obtained for each angle in the two flow ranges, and plot a
calibration curve with the average values of the pressure ratio (or
other suitable measurement factor as recommended by the
manufacturer) versus the pitch angle. Draw a smooth line through
the data points. Plot also the data values for each traverse
point. Determine the differences between the measured datavalues
and the angle from the calibration curve at the same pressure
ratio. The difference at each comparison must be within 2° for
angles between 0° and 40° and within 3° for angles between 40° and
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 10
60°.
2.5.6.4 Yaw Angle Calibration. Mark the three-dimensional probe
to allow the determination of the yaw position of the probe. This
is usually a line extending the length of the probe and aligned
with the impact opening. To determine the accuracy of measurements
of the yaw angle, only the zero or null position need be calibrated
as follows: Place the directional probe in the test section, and
rotate the probe until the zero position is found. With a
protractor or other angle measuring device, measure the angle
indicated by the yaw angle indicator on the three-dimensional
probe. This should be within 2° of 0°. Repeat this measurement
for any other points along the length of the pitot where yaw angle
measurements could be read in order to account for variations in
the pitot markings used to indicate pitot head positions.
BIBLIOGRAPHY
1. Determining Dust Concentration in a Gas Stream, ASME
Performance Test Code No. 27. New York. 1957.
2. DeVorkin, Howard, et al. Air Pollution Source Testing Manual.
Air Pollution Control District. Los Angeles, CA. November
1963.
3. Methods for Determining of Velocity, Volume, Dust and Mist
Content of Gases. Western Precipitation Division of Joy
Manufacturing Co. Los Angeles, CA. Bulletin WP-50. 1968.
4. Standard Method for Sampling Stacks for Particulate Matter.
In: 1971 Book of ASTM Standards, Part 23. ASTM Designation D
2928-71. Philadelphia, PA. 1971.
5. Hanson, H.A., et al. Particulate Sampling Strategies for
Large Power Plants Including Nonuniform Flow. USEPA, ORD,
ESRL, Research Triangle Park, NC. EPA-600/2-76-170. June
1976.
6. Entropy Environmentalists, Inc. Determination of the Optimum
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 11
Number of Sampling Points: An Analysis of Method 1 Criteria.
Environmental Protection Agency. Research Triangle Park, NC.
EPA Contract No. 68-01-3172, Task 7.
7. Hanson, H.A., R.J. Davini, J.K. Morgan, and A.A. Iversen.
Particulate Sampling Strategies for Large Power Plants
Including Nonuniform Flow. USEPA, Research Triangle Park, NC.
Publication No. EPA-600/2-76-170. June 1976. 350 p.
8. Brooks, E.F., and R.L. Williams. Flow and Gas Sampling
Manual. U.S. Environmental Protection Agency. Research
Triangle Park, NC. Publication No. EPA-600/2-76-203. July
1976. 93 p.
9. Entropy Environmentalists, Inc. Traverse Point Study. EPA
Contract No. 68-02-3172. June 1977. 19 p.
10. Brown, J. and K. Yu. Test Report: Particulate Sampling
Strategy in Circular Ducts. Emission Measurement Branch.
Emission Standards and Engineering Division. U.S.
Environmental Protection Agency, Research Triangle Park, NC
27711. July 31, 1980. 12 p.
11. Hawksley, P.G.W., S. Badzioch, and J.H. Blackett. Measurement
of Solids in Flue Gases. Leatherhead, England, The British
Coal Utilisation Research Association. 1961. p. 129-133.
12. Knapp, K.T. The Number of Sampling Points Needed for
Representative Source Sampling. In: Proceedings of the Fourth
National Conference on Energy and Environment. Theodore, L.
et al. (ed) . Dayton, Dayton Section of the American Institute
of Chemical Engineers. October 3-7, 1976. p. 563-568.
13. Smith, W.S. and D.J. Grove. A Proposed Extension of EPA
Method 1 Criteria. Pollution Engineering. XV (8):36-37.
August 1983.
14. Gerhart, P.M. and M.J. Dorsey. Investigation of Field Test
Procedures for Large Fans. University of Akron. Akron, OH.
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EMTIC TM-001 EMTIC NSPS TEST METHOD Page 12
(EPRI Contract CS-1651) . Final Report (RP-1649-5). December
1980.
15. Smith, W.S. and D.J. Grove. A New Look at Isokinetic Sampling
Theory and Applications. Source Evaluation Society
Newsletter. VIII (3):19-24. August 1983.
-------
EMTIC TM-001 EMTIC NSPS TEST METHOD Page 13
Table 1-1. CROSS-SECTION LAYOUT FOR
RECTANGULAR STACKS
-Number of traverse points
Matrix layout
9 ,
12 ,
16
20
25
30
36
42
49
3x3
4x3
4x4
5x4
5x5
6x5
6x6
7x6
7x7
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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 14
TABLE 1-2
LOCATION OF TRAVERSE POINTS IN CIRCULAR STACKS
(Percent of stack diameter from inside
wall to traverse point)
Traverse
Point
Number on a
Diameter
1 ...
2 .....
3
4
5
6
7 ....
8
9
10 ....
11 ....
Number of traverse points on a diameter
2
14
.6
85
.4
4
6.
7
25
.0
75
.0
93
.3
6
4.
4
14
.6
29
.6
70
.4
85
.4
95
.6
3
3.
2
10
.5
19
.4
32
.3
67
.7
80
.6
89
.5
96
.8
10
2.6
8.2
14.
6
22.
6
34.
2
65.
8
77.
4
85.
4
91.
8
97.
4
12
2.1
6.7
11.
8
17.
7
25.
0
35.
6
64.
4
75.
0
82.
3
88.
2
93.
3
14
1.8
5.7
9.9
14.
6
20.
1
26.
9
36.
6
63.
4
73.
1
79.
9
85.
4
16
1.6
4.9
8.5
12.
5
16.
9
22.
0
28.
3
37.
5
62.
5
71.
7
78.
0
18
1.
4
4.
4
7.
5
10
.9
14
.6
18
.8
23
.6
29
.6
38
.2
61
.8
70
.4
20
1.
3
3.
9
6.
7
9.
7
11
2.
9
16
.5
20
.4
25
.0
30
.6
38
.8
61
.2
22
1.1
3.5
6.0
8.7
11.
6
14.
6
18.
0
21.
8
26.
2
31.
5
39.
3
24
1.1
3.2
5.5
7.9
10.
5
13.
2
16.
1
19.
4
23.
0
27.
2
32.
3
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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 15
12 ....
13 ....
14 ....
15 ....
16 ....
17 ....
18 ....
19 ....
20 ....
21 ....
22 ....
23 ....
24 ....
97.
9
90.
1
94.
3
98.
2
83.
1
87.
5
91.
5
95.
1
98.
4
76
.4
81
.2
85
.4
89
.1
92
.5
95
.6
98
.6
69
.4
75
.0
79
.6
83
.5
87
.1
90
.3
93
.3
96
.1
98
.7
60.
7
68.
5
73.
8
78.
2
82.
0
85.
4
88.
4
91.
3
94.
0
96.
5
98.
9
39.
8
60.
2
67.
7
72.
8
77.
0
80.
6
83.
9
86.
8
89.
5
92.
1
94.
5
96.
8
98.
9
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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 16
so
0.5
Duel DtoiMtora Up.treim tram Flew Dbtuitanei* (Dfetane* A)
1.0 1.5 2.0
2.5
SO
20
10
Hlghir NIMH tar fcbr
JO
• Fiwn P»M of Any T»t if
ri, EiptMlM. CwitaeUM, «k J
lot
OJO to CJ1» 02-24 h.)
I I
» 4 S 6 7 •
Duct Dbmttera Down»tr»«m Item Flew Dtotuibaim* (DMcne* B)
Figure 1-1. Minimum number of traverse points for
particulate traverses.
-------
EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 17
SO
0.5
40 -
20 -
10 -
Duct Diameters Upstream from Flow Disturbance* (Dfetanoo A)
1.0 1.5 2.0
2.5
I I I I I I
'Higher Number la tar
1* Stack Dta
1
^
t
!
\
i
TDMurbanca
UeMumment
~ 8"*
Dleturtwnee
-
meter >0.eim (24 ki.)
- ' From Point of Any Type gf
Disturbance (Bend, Expansion, Contraction, etc.)
StKk Diametoi
1 1 1 1 1 1
12
.o,.1
« O.JO to 041 m (12-24 ki.)
I
345678
Duct Diameter* Downitream from Flow Dleturbance* (Dlatanca B)
10
Figure 1-2. Minimum number of traverse points for velocity
(nonparticulate) traverses.
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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 18
4.4
14.7
J»J
70.5
MJ
MJ
Figure 1-3. Example showing circular stack cross section
divided into 12 equal areas, with location of traverse
points indicated.
-------
EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 19
o
o
o
o
o
1 1
0
o
o
1
0
o
o
o
Figure 1-4. Example showing rectangular stack cross section
divided into 12 equal areas, with a traverse point at centroid
of each area.
-------
-------
-------
APPENDIX F.2
EPA METHOD1A
-------
METHOD 1A - SAMPLE AND VELOCITY TRAVERSES FOR STATIONARY
SOURCES WITH SMALL STACKS OR DUCTS
NOTE: This method does not include all of the
specifications (e.g., equipment and supplies) and procedures
(e.g., sampling) essential to its performance. Some
material is incorporated by reference from other methods in
this part. Therefore, to obtain reliable results, persons
using this method should have a thorough knowledge of at
least the following additional test method: Method 1.
1.0 Scope and Application.
1.1 Measured Parameters. The purpose of the method is
to guide the selection of sampling ports and traverse points
at which sampling for air pollutants will be performed
pursuant to regulations set forth in this part.
1.2 Applicability. The applicability and principle of
this method are identical to Method 1, except its
applicability is limited to stacks or ducts. This method is
applicable to flowing gas streams in ducts, stacks, and
flues of less than about O.30 meter (12 in.) in diameter, or
0.071 m2 (113 in.2) in cross-sectional area, but equal to or
greater than about O.10 meter (4 in.) in diameter, or 0.0081
m2 (12.57 in.2) in cross-sectional area. This method cannot
be used when the flow is cyclonic or swirling.
1.3 Data Quality Objectives. Adherence to the
requirements of this method will enhance the quality of the
data obtained from air pollutant sampling methods.
2.0 Summary of Method.
2.1 To aid in the representative measurement of
pollutant emissions and/or total volumetric flow rate from a
stationary source, a measurement site or a pair of
measurement sites where the effluent stream is flowing in a
known direction is (are) selected. The cross-section of the
stack is divided into a number of equal areas. A traverse
point is then located within each of these equal areas.
2.2 In these small diameter stacks or ducts, the
conventional Method 5 stack assembly (consisting of a Type S
pitot tube attached to a sampling probe, equipped with a
nozzle and thermocouple) blocks a significant portion of the
cross-section of the duct and causes inaccurate
measurements. Therefore, for particulate matter (PM)
sampling in small stacks or ducts, the gas velocity is
measured using a standard pitot tube downstream of the
actual emission sampling site. The straight run of duct
between the PM sampling and velocity measurement sites
1A-1 June 1996
-------
allows the flow profile, temporarily disturbed by the
presence of the sampling probe, to redevelop and stabilize.
3.0 Definitions. [Reserved]
4.0 Interferences. [Reserved]
5.0 Safety.
5.1 Disclaimer. This method may involve hazardous
materials, operations, and equipment. This test method does
not purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this
test method to establish appropriate safety and health
practices and determine the applicability of regulatory
limitations prior to performing this test method.
6.0 Equipment and Supplies. [Reserved]
7.0 Reagents and Standards. [Reserved]
8.0 Sample Collection, Preservation, Storage, and
Transport. [Reserved]
9.0 Quality Control. [Reserved]
10.0 Calibration and Standardization. [Reserved]
11.0 Procedure.
11.1 Selection of Measurement Site.
11.1.1 Particulate Measurements - Steady or Unsteady
Flow. Select a particulate measurement site located
preferably at least eight equivalent stack or duct diameters
downstream and 10 equivalent diameters upstream from any
flow disturbances such as bends, expansions, or
contractions in the stack, or from a visible flame. Next,
locate the velocity measurement site eight equivalent
diameters downstream of the particulate measurement site
(see Figure 1A-1). If such locations are not available,
select an alternative particulate measurement location at
least two equivalent stack or duct diameters downstream and
two and one-half diameters upstream from any flow
disturbance. Then, locate the velocity measurement site two
equivalent diameters downstream from the particulate
measurement site. (See Section 12.2 of Method 1 for
calculating equivalent diameters for a rectangular cross-
section.)
1A-2 June 1996
-------
11.1.2 PM Sampling (Steady Flow) or Velocity (Steady or
Unsteady Flow) Measurements. For PM sampling when the
volumetric flow rate in a duct is constant with respect to
time, Section 11.1.1 of Method 1 may be followed, with the
PM sampling and velocity measurement performed at one
location. To demonstrate that the flow rate is constant
(within 10 percent) when PM measurements are made, perform
complete velocity traverses before and after the PM sampling
run, and calculate the deviation of the flow rate derived
after the PM sampling run from the one derived before the PM
sampling run. The PM sampling run is acceptable if the
deviation does not exceed 10 percent.
11.2 Determining the Number of Traverse Points.
11.2.1 Particulate Measurements (Steady or Unsteady
Flow). Use Figure 1-1 of Method 1 to determine the number
of traverse points to use at both the velocity measurement
and PM sampling locations. Before referring to the figure,
however, determine the distances between both the velocity
measurement and PM sampling sites to the nearest upstream
and downstream disturbances. Then divide each distance by
the stack diameter or equivalent diameter to express the
distances in terms of the number of duct diameters. Then,
determine the number of traverse points from Figure 1-1 of
Method 1 corresponding to each of these four distances.
Choose the highest of the four numbers of traverse points
(or a greater number) so that, for circular ducts the number
is a multiple of four; and for rectangular ducts, the number
is one of those shown in Table 1-1 of Method 1. When the
optimum duct diameter location criteria can be satisfied,
the minimum number of traverse points required is eight for
circular ducts and nine for rectangular ducts.
11.2.2 PM Sampling (Steady Flow) or only Velocity (Non-
Particulate) Measurements. Use Figure 1-2 of Method 1 to
determine number of traverse points, following the same
procedure used for PM sampling as described in Section
11.2.1 of Method 1. When the optimum duct diameter location
criteria can be satisfied, the minimum number of traverse
points required is eight for circular ducts and nine for
rectangular ducts.
11.3 Cross-sectional Layout, Location of Traverse
Points, and Verification of the Absence of Cyclonic Flow.
Same as Method 1, Sections 11.3 and 11.4, respectively.
12.0 Data Analysis and Calculations. [Reserved]
13.0 Method Performance. [Reserved]
14.0 Pollution Prevention. [Reserved]
15.0 Waste Management. [Reserved]
1A-3 June 1996
-------
16.0 References. Same as Method 1, Section 16.0,
Figure 1A-1. Recommended sampling arrangement for small ducts
References 1 through 6, with the addition of the following:
1. Vollaro, Robert F. Recommended Procedure for Sample
Traverses in Ducts Smaller Than 12 Inches in
Diameter. U.S. Environmental Protection Agency,
Emission Measurement Branch, Research Triangle Park,
North Carolina. January 1977.
17.0 Tables, Diagrams, Flowcharts, and Validation Data.
1A-4
June 1996
-------
APPENDIX F.3
EPA METHOD 2
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 2 - Determination of Stack Gas Velocity and Volumetric
Flow Rate (Type S Pitot Tube)
1. PRINCIPLE AND APPLICABILITY
1.1 Principle. The average gas velocity in a stack is determined from the gas
density and from measurement of the average velocity head with a Type S
(Stausscheibe or reverse type) pitot tube.
1.2 Applicability. This method is applicable for measurement of the average
velocity of a gas stream and for quantifying gas flow.
This procedure is not applicable at measurement sites that fail to meet the
criteria of Method 1, Section 2.1. Also, the method cannot be used for direct
measurement in cyclonic or swirling gas streams; Section 2.4 of Method 1 shows
how to determine cyclonic or swirling flow conditions. When unacceptable
conditions exist, alternative procedures, subject to the approval of the
Administrator, U.S. Environmental Protection Agency, must be employed to make
accurate flow rate determinations; examples of such alternative procedures are:
(1) to install straightening vanes; (2) to calculate the total volumetric flow
rate stoichiometrically, or (3) to move to another measurement site at which the
flow is acceptable.
2. APPARATUS
Specifications for the apparatus are given below. Any other apparatus that has
been demonstrated (subject to approval of the Administrator) to be capable of
meeting the specifications will be considered acceptable.
2.1 Type S Pitot Tube. Pitot tube made of metal tubing (e.g., stainless steel)
as shown in Figure 2-1. It is recommended that the external tubing diameter
(dimension Dt, Figure 2-2b) be between 0.48 and 0.95 cm (3/16 and 3/8 inch).
There shall be an equal distance from the base of each leg of the pitot tube to
its face-opening plane (dimensions PA and ft, Figure 2-2b); it is recommended
that this distance be between 1.05 and 1.50 times the external tubing diameter.
The face openings of the pitot tube shall, preferably, be aligned as shown in
Figure 2-2; however, slight misalignments of the openings are permissible (see
Figure 2-3).
The Type S pitot tube shall have a known coefficient, determined as outlined in
Section 4. An identification number shall be assigned to the pitot tube; this
Prepared by Emission Measurement Branch BMTIC M-002
Technical Support Division, OAQPS, EPA
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
number shall be permanently marked or engraved on the body of the tube. A
standard pitot tube may be used instead of a Type S, provided that it meets the
specifications of Sections 2.7 and 4.2; note, however, that the static and impact
pressure holes of standard pitot tubes are susceptible to plugging in
particulate-laden gas streams. Therefore, whenever a standard pitot tube is used
to perform a traverse, adequate proof must be furnished that the openings of the
pitot tube have not plugged up during the traverse period; this can be done by
taking a velocity head (Ap) reading at the final traverse point, cleaning out the
impact and static holes of the standard pitot tube by "back-purging" with
pressurized air, and then taking another Ap reading. If the Ap readings made
before and after the air purge are the same (±5 percent) , the traverse is
acceptable. Otherwise, reject the run. Note that if Ap at the final traverse
point is unsuitably low, another point may be selected. If "back-purging" at
regular intervals is part of the procedure, then comparative Ap readings shall
be taken, as above, for the last two back purges at which suitably high Ap
readings are observed.
2.2 Differential Pressure Gauge. An inclined manometer or equivalent device.
Most sampling trains are equipped with a 10-in. (water column) inclined-vertical
manometer, having 0.01-in. H2O divisions on the 0- to 1-in. inclined scale, and
O.l-in. H20 divisions on the 1- to 10-in. vertical scale. This type of manometer
(or other gauge of equivalent sensitivity) is satisfactory for the measurement
of Ap values as low as 1.3 mm (0.05 in.) H20. However, a differential pressure
gauge of greater sensitivity shall be used (subject to the approval of the
Administrator), if any of the following is found to be true: (1) the arithmetic
average of all Ap readings at the traverse points in the stack is less than
1.3 mm (0.05 in.) H20; (2) for traverses of 12 or more points, more than 10
percent of the individual Ap readings are below 1.3 mm (0.05 in.) H»0; (3) for
traverses of fewer than 12 points, more than one Ap reading is below 1.3 mm
(0.05 in.) H20. Citation 18 in the Bibliography describes commercially available
instrumentation for the measurement of low-range gas velocities.
As an alternative to criteria (1) through (3) above, the following calculation
may be performed to determine the necessity of using a more sensitive
differential pressure gauge:
Prepared by Emission Measurement Branch EMTIC M-002
Technical Support Division, OAQPS, EPA
-------
EMTIC TM-002
NSPS TEST METHOD
Page 3
T =
1=1
1=1
Where:
Api = Individual velocity head reading at a traverse point, mm (in.)
H20.
n = Total number of traverse points.
K = 0.13 mm H20 when metric units are used and 0.005 in. H,0 when
English units are used.
If T is greater than 1.05, the velocity head data are unacceptable and a more
sensitive differential pressure gauge must be used.
MOTE: If differential pressure gauges other than inclined manometers are used
(e.g., magnehelic gauges), their calibration must be checked after each test
series. To check the calibration of a differential pressure gauge, compare Ap
readings of the gauge with those of a gauge-oil manometer at a minimum of three
points, approximately representing the range of Ap values in the stack. If, at
each point, the values of Ap as read by the differential pressure gauge and
gauge-oil manometer agree to within 5 percent, the differential pressure gauge
shall be considered to be in proper calibration. Otherwise, the test series
shall either be voided, or procedures to adjust the measured Ap values and final
results shall be used, subject to the approval of the Administrator.
2.3 Temperature Gauge. A thermocouple, liquid-filled bulb thermometer,
bimetallic thermometer, mercury-in-glass thermometer, or other gauge capable of
measuring temperature to within 1.5 percent of the minimum absolute stack
temperature. The temperature gauge shall be attached to the pitot tube such that
the sensor tip does not touch any metal; the gauge shall be in an interference-
free arrangement with respect to the pitot tube face openings (see Figure 2-1 and
also Figure 2-7 in Section 4) . Alternative positions may be used if the pitot
tube-temperature gauge,system is calibrated according to the procedure of Section
4. Provided that a difference of not more than 1 percent in the average velocity
measurement is introduced, the temperature gauge need not be attached to the
pitot tube; this alternative is subject to the approval of the Administrator.
2.4 Pressure Probe and Gauge. A piezometer tube and mercury- or water-filled
U-tube manometer capable of measuring stack pressure to within 2.5 mm (0.1 in.)
Hg. The static tap of a standard type pitot tube or one leg of a Type S pitot
tube with the face opening planes positioned parallel to the gas flow may also
be used as the pressure probe.
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EMTIC TM-002 NSPS TEST METHOD Page 4
2.5 Barometer. A mercury, aneroid, or other barometer capable of measuring
atmospheric pressure to within 2.5 mm (0.1 in.) Hg. See NOTE in Method 5,
Section 2.1.9.
2.6 Gas Density Determination Equipment. Method 3 equipment, if needed (see
Section 3.6), to determine the stack gas dry molecular weight, and Reference
Method 4 or Method 5 equipment for moisture content determination; other methods
may be used subject to approval of the Administrator,
2.7 Calibration Pitot Tube. When calibration of the Type S pitot tube is
necessary (see Section 4), a standard pitot tube for a reference. The standard
pitot tube shall, preferably, have a known coefficient, obtained either (1)
directly from the National Bureau of Standards, Route 70 S, Quince Orchard Road,
Gaithersburg, Maryland, or (2) by calibration against another standard pitot tube
with an NBS-traceable coefficient* Alternatively, a standard pitot tube designed
according to the criteria given in Sections 2.7.1 through 2.7.5 below and
illustrated in figure 2-4 (see also Citations 7, 8, and 17 in the Bibliography)
may be used. Pitot tubes designed according to these specifications will have
baseline coefficients of about 0.99 ± 0.01.
2.7.1 Hemispherical (shown in Figure 2-4) ellipsoidal, or conical tip.
2.7.2 A minimum of six diameters straight run (based upon D, the external
diameter of the tube) between the tip and the static pressure holes.
2.7.3 A minimum of eight diameters straight run between the static pressure
holes and the centerline of the external tube, following the 90-degree bend.
2.7.4 Static pressure holes of equal size (approximately 0.1 D), equally spaced
in a piezometer ring configuration.
2.7.5 Ninety-degree bend, with curved or mitered junction.
2.8 Differential Pressure Gauge for Type S Pitot Tube Calibration. An inclined
manometer or equivalent. If the single-velocity calibration technique is
employed (see Section 4.1.2.3), the calibration differential pressure gauge shall
be readable to the nearest 0.13 mm (0.005 in.) H20. For multivelocity
calibrations, the gauge shall be readable to the nearest 0.13 mm (0.005 in.) H20
for Ap values between 1.3 and 25 mm (0.05 and 1.0 in.) H20, and to the nearest
1.3 mm (0.05 in.) H20 for Ap values above 25 mm (1.0 in.) H20. A special, more
sensitive gauge will be required to read Ap values below 1.3 mm (0.05 in.) H20
(see Citation 18 in the Bibliography).
3. PROCEDURE
3.1 Set up the apparatus as shown in Figure 2-1. Capillary tubing or surge
tanks installed between the manometer and pitot tube may be used to dampen Ap
fluctuations. It is recommended, but not required, that a pretest leak-check be
conducted as follows: (1) blow through the pitot impact opening until at least
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EMTIC TM-002 NSPS TEST METHOD Page 5
7.6 cm (3 in.) H,0 velocity pressure registers on the manometer; then, close off
the impact opening. The pressure shall remain stable for at least 15 seconds;
(2) do the same for the static pressure side, except using suction to obtain the
minimum of 7.6 cm (3 in.) H20. Other leak-check procedures, subject to the
approval of the Administrator, may be used.
3.2 Level and zero the manometer. Because the manometer level and zero may
drift due to vibrations and temperature changes, make periodic checks during the
traverse. Record all necessary data as shown in the example data sheet
(Figure 2-5) .
3.3 Measure the velocity head and temperature at the traverse points specified
by Method 1. Ensure that the proper differential pressure gauge is being used
for the range of Ap values encountered (see Section 2.2) . If it is necessary to
change to a more sensitive gauge, do so, and remeasure the Ap and temperature
readings at each traverse point. Conduct a post-test leak-check (mandatory), as
described in Section 3.1 above, to validate the traverse run.
3.4 Measure the static pressure in the stack. One reading is usually adequate.
3.5 Determine the atmospheric pressure.
3.6 Determine the stack gas dry molecular weight. For combustion processes or
processes that emit essentially C02, 0,, CO, and N2, use Method 3. For processes
emitting essentially air, an analysis need not be conducted; use a dry molecular
weight of 29.0. For other processes, other methods, subject to the approval of
the Administrator, must be used.
3.7 Obtain the moisture content from Reference Method 4 (or equivalent) or from
Method 5.
3.8 Determine the cross-sectional area of the stack or duct at the sampling
location. Whenever possible, physically measure the stack dimensions rather than
using blueprints.
4. CALIBRATION
4.1 Type S Pitot Tube. Before its initial use, carefully examine the Type S
pitot tube in top, side, and end views to verify that the face openings of the
tube are aligned within the specifications illustrated in Figure 2-2 or 2-3. The
pitot tube shall not be used if it fails to meet these alignment specifications.
After verifying the face opening alignment, measure and record the following
dimensions of the pitot tube: (a) the external tubing diameter (dimension Dt,
Figure 2-2b) ; and (b) the base-to-opening plane distances (dimensions PA and PB,
Figure 2-2b) . If Dt is between 0.48 and 0.95 cm (3/16 and 3/8 in.), and if %
and PB are equal and between 1.05 and 1.50 DC, there are two possible options:
(1) the pitot tube may be calibrated according to the procedure outlined in
Sections 4.1.2 through 4.1.5 below, or (2) a baseline (isolated tube) coefficient
value of 0.84 may be assigned to the pitot tube. Note, however, that if the
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EMTIC TM-002 NSPS TBST METHOD Page 6
pitot tube is part of an assembly, calibration may still be required, despite
knowledge of the baseline coefficient value (see Section 4.1.1).
If Dt, Qt, and f are outside the. specified limits, the pitot tube must be
calibrated as outlined in Sections 4.1.2 through 4.1.S below.
4.1.1 Typ« S Pitot Tube Assemblies. During sample and velocity traverses, the
isolated Type S pitot tube is not always used; in many instances, the pitot tube
is used in combination with other source-sampling components (thermocouple,
sampling probe, nozzle) as part of an "assembly." The presence of other sampling
components can sometimes affect the baseline value of the Type S pitot tube
coefficient (Citation 9 in the Bibliography); therefore an assigned (or otherwise
known) baseline coefficient value may or may not be valid for a given assembly.
The baseline and assembly coefficient values will be identical only when the
relative placement of the components in the assembly is such that aerodynamic
interference effects are eliminated. Figures 2-6 through 2-8 illustrate
interference-free component arrangements for Type S pitot tubes having external
tubing diameters between 0.48 and 0.95 cm (3/16 and 3/8 in.). Type S pitot tube
assemblies that fail to meet any or all of the specifications of Figures 2-6
through 2-8 shall be calibrated according to the procedure outlined in Sections
4.1.2 through 4.1.5 below, and prior to calibration, the values of the
intercomponent spacings (pitot-nozzle, pitot-thermocouple, pitot-probe sheath)
shall be measured and recorded.
NOTE: Do not use any Type S pitot tube assembly which is constructed such that
the impact pressure opening plane of the pitot tube is below the entry plane of
the nozzle (see Figure 2-6B).
4.1.2 Calibration Setup. If the Type S pitot tube is to be calibrated, one leg
of the tube shall be permanently marked A, and the other, B. Calibration shall
be done in a flow system having the following essential design features:
4.1.2.1 The flowing gas stream must be confined to a duct of definite cross-
sectional area, either circular or rectangular. For circular cross sections, the
minimum duct diameter shall be 30.5 cm (12 in.); for rectangular cross sections,
the width (shorter side) shall be at least 25.4 cm (10 in.).
4.1.2.2 The cross-sectional area of the calibration duct must be constant over
a distance of 10 or more duct diameters. For a rectangular cross section, use
an equivalent diameter, calculated from the following equation, to determine the
number of duct diameters:
2LW
D =
' (L + W)
Eq. 2-1
Where:
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EMTIC TM-002 NSPS TEST METHOD Page 7
D, = Equivalent diameter.
L • Length.
W = Width.
To ensure the presence of stable, fully developed flow patterns at the
calibration site, or "test section," the site must be located at least eight
diameters downstream and two diameters upstream from the nearest disturbances.
NOTE: The eight- and two-diameter criteria are not absolute; other test section
locations may be used (subject to approval of the Administrator), provided that
the flow at the test site is stable and demonstrably parallel to the duct axis.
4.1.2.3 The flow system shall have the capacity to generate a test-section
velocity around 915 m/min (3,000 ft/min). This velocity must be constant with
time to guarantee steady flow during calibration. Note that Type S pitot tube
coefficients obtained by single-velocity calibration at 915 m/min (3,000 ft/min)
will generally be valid to ±3 percent for the measurement of velocities above 305
m/min (1,000 ft/min) and to ±5 to 6 percent for the measurement of velocities
between 180 and 305 m/min (600 and 1,000 f t/min) . If a more precise correlation
between Cp and velocity is desired, the flow system shall have the capacity to
generate at least four distinct, time-invariant test-section velocities covering
the velocity range from 180 to 1,525 m/min (600 to 5,000 f t/min), and calibration
data shall be taken at regular velocity intervals over this range (see Citations
9 and 14 in the Bibliography for details).
4.1.2.4 Two entry ports, one each for the standard and Type S pitot tubes, shall
be cut in the test section; the standard pitot entry port shall be located
slightly downstream of the Type S port, so that the standard and Type S impact
openings will lie in the same cross-sectional plane during calibration. To
facilitate alignment of the pitot tubes during calibration, it is advisable that
the test section be constructed of plexiglas or some other transparent material.
4.1.3 Calibration Procedure. Note that this procedure is a general one and must
not be used without first referring to the special considerations presented in
Section 4.1.5. Note also that this procedure applies only to single-velocity
calibration. To obtain calibration data for the A and B sides of the Type S
pitot tube, proceed as follows:
4.1.3.1 Make sure that the manometer is properly filled and that the oil is free
from contamination and is of the proper density. Inspect and leak-check all
pitot lines; repair or replace if necessary.
4.1.3.2 Level and zero the manometer. Turn on the fan, and allow the flow to
stabilize. Seal the Type S entry port.
4.1.3.3 Ensure that the manometer is level and zeroed. Position the standard
pitot tube at the calibration point (determined as outlined in Section 4.1.5.1),
and align the tube so that its tip is pointed directly into the flow. Particular
care should be taken in aligning the tube to avoid yaw and pitch angles. Make
sure that the entry port surrounding the tube is properly sealed.
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EMTIC TM-002 NSPS TEST METHOD Page 8
4.1.3.4 Read Apscd, and record its value in a data table similar to the one shown
in Figure 2-9. Remove the standard pitot tube from the duct, and disconnect it
from the manometer. Seal the standard entry port.
4.1.3.5 Connect the Type S pitot tube to the manometer. Open the Type S entry
port. Check the manometer level and zero. Insert and align the Type S pitot
tube so that its A side impact opening is at the same point as was the standard
pitot tube and is pointed directly into the flow. Make sure that the entry port
surrounding the tube is properly sealed.
4.1.3.6 Read Ap., and enter its value in the data table. Remove the Type S
pitot tube from the duct, and disconnect it from the manometer.
4.1.3.7 Repeat Steps 4.1.3.3 through 4.1.3.6 above until three pairs of Ap
readings have been obtained.
4.1.3.8 Repeat Steps 4.1.3.3 through 4.1.3.7 above for the B side of the Type
S pitot tube.
4.1.3.9 Perform calculations, as described in Section 4.1.4 below.
4.1.4 Calculations.
4.1.4.1 For each of the six pairs of Ap readings (i.e., three from side A and
three from side B) obtained in Section 4.1.3 above, calculate the value of
the Type S pitot tube coefficient as follows:
C =C *"
PCs) ptstd).
Eg. 2-2
Where:
Cp,,, - Type S pitot tube coefficient.
Cp(.cd, = Standard pitot tube coefficient; use 0.99 if the
coefficient is unknown and the tube is designed according
to the criteria of Sections 2.7.1 to 2.7.5 of this
method.
Ap»td = Velocity head measured by the standard pitot tube, cm
(in.) HjO.
Ap. = Velocity head measured by the Type S pitot tube, cm (in.).
HjO.
4.1.4.2 Calculate Cp (side A), the mean A-side coefficient, and Cp (side B) , the
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EMTIC TM-002 NSPS TEST METHOD Page 9
mean B-side coefficient; calculate the difference between these two average
values.
4.1.4.3 Calculate the deviation of each of the three A-side values of
Cp,., from Cp (side A) , and the deviation of each B-side values of Cp(I) from
Cp (side B). Use the following equation:
Deviation = C -C (A or B)
Eq. 2-3
4.1.4.4 Calculate a, the average deviation from the mean, for both the A and B
sides of the pitot tube. Use the following equation:
- C (A or B)
p
cKslde A or B) =
Eq. 2-4
4.1.4.5 Use the Type S pitot tube only if the values of o (side A) and a (side
B) are less than or equal to 0.01 and if the absolute value of the difference
between Cp (A) and Cp (B) is 0.01 or less.
4.1.5 Special Considerations.
4.1.5.1 Selection of Calibration Point.
4.1.5.1.1 When an isolated Type S pitot tube is calibrated, select a calibration
point at or near the center of the duct, and follow the procedures outlined in
Sections 4.1.3 and 4.1.4 above. The Type S pitot coefficients so obtained,
i.e., Cp (side A) and <; (side B), will be valid, so long as either: (1) the
isolated pitot tube is used; or (2) the pitot tube is used with other components
(nozzle, thermocouple, sample probe) in an arrangement that is free from
aerodynamic interference effects (see Figures 2-6 through 2-8).
4.1.5.1.2 For Type S pitot tube-thermocouple combinations (without sample
probe), select a calibration point at or near the center of the duct, and follow
the procedures outlined in Sections 4.1.3 and 4.1.4 above. The coefficients so
obtained will be valid so long as the pitot tube-thermocouple combination is used
by itself or with other components in an interference-free arrangement (Figures
2-6 and 2-8).
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EMTZC TM-002 NSPS TEST METHOD Page 10
4.1.5.1.3 For assemblies with sample probes, the calibration point should be
located at or near the center of the duct; however, insertion of a probe sheath
into a small duct may cause significant cross-sectional area blockage and yield
incorrect coefficient values (Citation 9 in the Bibliography). Therefore, to
minimize the blockage effect, the calibration point may be a few inches off-
center if necessary. The actual blockage effect will be negligible when the
theoretical blockage, as determined by a projected-area model of the probe
sheath, is 2 percent or less of the duct cross-sectional area for assemblies
without external sheaths (Figure 2-10a), and 3 percent or less for assemblies
with external sheaths (Figure 2-10b).
4.1.5.2 For those probe assemblies in which pitot tube-nozzle interference is
a factor (i.e., those in which the pitot-nozzle separation distance fails to meet
the specification illustrated in Figure 2-6A), the value of Cp,., depends upon the
amount of free-space between the tube and nozzle, and therefore is a function of
nozzle size. In these instances, separate calibrations shall be performed with
each of the commonly used nozzle sizes in place. Note that the single-velocity
calibration technique is acceptable for this purpose, even though the larger
nozzle sizes (>0.635 cm or 1/4 in.) are not ordinarily used for isokinetic
sampling at velocities around 915 m/min (3,000 ft/min), which is the calibration
velocity; note also that it is not necessary to draw an isokinetic sample during
calibration (see Citation 19 in the Bibliography).
4.1.5.3 For a probe assembly constructed such that its pitot tube is always used
in the same orientation, only one side of the pitot tube need be calibrated (the
side which will face the flow). The pitot tube must still meet the alignment
specifications of Figure 2-2 or 2-3, however, and must have an average deviation
(a) value of 0.01 or less (see Section 4.1.4.4.)
4.1.6 Field Use and Recalibration.
4.1.6.1 Field Use.
4.1.6.1.1 When a Type S pitot tube (isolated or in an assembly) is used in the
field, the appropriate coefficient value (whether assigned or obtained by
calibration) shall be used to perform velocity calculations. For calibrated Type
S pitot tubes, the A side coefficient shall be used when the A side of the tube
faces the flow, and the B side coefficient shall be used when the B side faces
the flow; alternatively, the arithmetic average of the A and B side coefficient
values may be used, irrespective of which side faces the flow.
4.1.6.1.2 When a probe assembly is used to sample a small duct, 30.5 to 91.4 cm
(12 to 36 in.) in diameter, the probe sheath sometimes blocks a significant part
of the duct cross-section, causing a reduction in the effective value of Cp,.,.
Consult Citation 9 in the Bibliography for details. Conventional pitot-sampling
probe assemblies are not recommended for use in ducts having inside diameters
smaller than 30.5 cm. (12 in.) (see Citation 16 in the Bibliography).
4.1.6.2 Recalibration.
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EMTIC TM-002 NSPS TEST METHOD Page 11
4.1.6.2.1 Isolated Pitot Tubes. After each field use, the pitot tube shall be
carefully reexamined in top, side, and end views. If the pitot face openings are
still aligned within the specifications illustrated in Figure 2-2 or 2-3, it can
be assumed that the baseline coefficient of the pitot tube has not changed. If,
however, the tube has been damaged to the extent that it no longer meets the
specifications of the Figure 2-2 or 2-3, the damage shall either be repaired to
restore proper alignment of the face openings, or the tube shall be discarded.
4.1.6.2.2 Pitot Tube Assemblies. After each field use, check the face opening
alignment of the pitot tube, as in Section 4.1.6.2.1; also, remeasure the
intercomponent spacings of the assembly. If the intercomponent spacings have not
changed and the face opening alignment is acceptable, it can be assumed that the
coefficient of the assembly has not changed. If the face opening alignment is
no longer within the specifications of Figure 2-2 or 2-3, either repair the
damage or replace the pitot tube (calibrating the new assembly, if necessary) .
If the intercomponent spacings have changed, restore the original spacings, or
recalibrate the assembly.
4.2 Standard Pitot Tuba (if applicable). If a standard pitot tube is used for
the velocity traverse, the tube shall be constructed according to the criteria
of Section 2.7 and shall be assigned a baseline coefficient value of 0.99. If
the standard pitot tube is used as part of an assembly, the tube shall be in an
interference-free arrangement (subject to the approval of the Administrator).
4.3 Temperature Gauges. After each field use, calibrate dial thermometers,
liquid-filled bulb thermometers, thermocouple-potentiometer systems, and other
gauges at a temperature within 10 percent of the average absolute stack
temperature. For temperatures up to 405°C (761°F) , use an ASTM mercury-in-glass
reference thermometer, or equivalent, as a reference; alternatively, either
a reference thermocouple and potentiometer (calibrated by NBS) or thermometric
fixed points, e.g., ice bath and boiling water (corrected for barometric
pressure) may be used. For temperatures above 405eC (761°F), use an NBS-
calibrated reference thermocouple-potentiometer system or an alternative
reference, subject to the approval of the Administrator.
If, during calibration, the absolute temperature measured with the gauge being
calibrated and the reference gauge agree within 1.5 percent, the temperature data
taken in the field shall be considered valid. Otherwise, the pollutant emission
test shall either be considered invalid or adjustments (if appropriate) of the
test results shall be made, subject to the approval of the Administrator.
4.4 Barometer. Calibrate the barometer used against a mercury barometer.
5. CALCULATIONS
Carry out calculations, retaining at least one extra decimal figure beyond that
of the acquired data. Round off figures after final calculation.
5.1 Nomenclature.
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EMTIC TM-002
NSPS TBST METHOD
Page 12
Cross-sectional area of stack, m2 (ft2) .
Water vapor in the gas stream (from Method 5 or Reference
Method 4), proportion by volume.
Pitot tube coefficient, dimensionless.
Pitot tube constant,
34.97
sec
(g/g -BoleHmHg)
1/2
(«nH20)
for the metric system.
85.49
ft
sec
lb/lb-iole) dn.Hg)
(1n.H20>
for the English system.
^ = Molecular weight of stack gas, dry basis (see Section 3.6) ,
g/g-mole (Ib/lb-mole).
M, • Molecular weight of stack gas, wet basis, g/g-mole (Ib/lb-
mole).
P.
Eq. 2-5
Barometric pressure at measurement site, mm Hg (in. Hg)
Stack static pressure, mm Hg (in. Hg).
Absolute stack pressure, mm Hg (in. Hg),
= Pk + P
bar g
Eq. 2-6
Standard absolute pressure, 760 mm Hg (29.92 in. Hg) .
Dry volumetric stack gas flow rate corrected to standard
conditions, dsm3/hr (dscf/hr).
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EMTIC TM-002
NSPS TEST METHOD
Page 13
t.
T.
Stack temperature, *C (°F) .
Absolute stack temperature, °K (CR)
=273 + t
for metric.
=460 + t
Eq. 2-7
for English.
Ap =
3,600°
18.0 =
Eq. 2-8
Standard absolute temperature, 293°K (528°R).
Average stack gas velocity, m/sec (ft/sec).
Velocity head of stack gas, mm H20 (in. H20) .
Conversion factor, sec/hr.
Molecular weight of water, g/g-mole (Ib/lb-mole).
5.2 Average Stack Gas Velocity.
P,Hs
Eq. 2-9
5.3 Average Stack Gas Dry Volumetric Flow Rate
T
Qfd =3.600(l-BM)v/
ltd
s(avg) ttd
BIBLIOGRAPHY
1. Mark, L.S. Mechanical Engineers' Handbook.
Co., Inc. 1951.
Eq. 2-10
New York. McGraw-Hill Book
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EMTIC TM-002 NSPS TEST METHOD Page 14
2. Perry. J.H. Chemical Engineers' Handbook. New York. McGraw-Hill Book
Co., Inc. 1960.
3. Shigehara, R.T., W.F. Todd, and W.S. Smith. Significance of Errors in
Stack Sampling Measurements. U.S. Environmental Protection Agency,
Research Triangle Park, N.C. (Presented at the Annual Meeting of the Air
Pollution Control Association, St. Louis, MO., June 14-19, 1970).
4. Standard Method for Sampling Stacks for Particulate Matter. In: 1971 Book
of ASTM Standards, Part 23. Philadelphia, PA. 1971. ASTM Designation
D 2928-71.
5. Vennard, J.K. Elementary Fluid Mechanics. New York. John Wiley and Sons,
Inc. 1947.
6. Fluid Meters - Their Theory and Application. American Society of
Mechanical Engineers, New York, N.Y. 1959.
7. ASHRAE Handbook of Fundamentals. 1972. p. 208.
8. Annual Book of ASTM Standards, Part 26. 1974. p. 648.
9. Vollaro, R.F. Guidelines for Type S Pitot Tube Calibration. U.S.
Environmental Protection Agency, Research Triangle Park, N.C. (Presented
at 1st Annual Meeting, Source Evaluation Society, Dayton, OH,
September 18, 1975.)
10. Vollaro, R.F. A Type S Pitot Tube Calibration Study. U.S. Environmental
Protection Agency, Emission Measurement Branch, Research Triangle Park,
N.C. July 1974.
11. Vollaro, R.F. The Effects of Impact Opening Misalignment on the Value of
the Type S Pitot Tube Coefficient. U.S. Environmental Protection Agency,
Emission Measurement Branch, Research Triangle Park, NC. October 1976.
12. Vollaro, R.F. Establishment of a Baseline Coefficient Value for Properly
Constructed Type S Pitot Tubes. U.S. Environmental Protection Agency,
Emission Measurement Branch, Research Triangle Park, NC. November 1976.
13. Vollaro, R.F. An Evaluation of Single-Velocity Calibration Technique as a
Means of Determining Type S Pitot Tube Coefficients. U.S. Environmental
Protection Agency, Emission Measurement Branch, Research Triangle Park, NC.
August 1975.
14. Vollaro, R.F. The Use of Type S Pitot Tubes for the Measurement of Low
Velocities. U.S. Environmental Protection Agency, Emission Measurement
Branch, Research Triangle Park, NC. November 1976.
15. Smith, Marvin L. Velocity Calibration of EPA Type Source Sampling Probe.
United Technologies Corporation, Pratt and Whitney Aircraft Division, East
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EMTIC TM-002 NSPS TEST METHOD Page 15
Hartford, CT. 1975.
16. Vollaro, R.F. Recommended Procedure for Sample Traverses in Ducts Smaller
than 12 Inches in Diameter. U.S. Environmental Protection Agency, Emission
Measurement Branch, Research Triangle Park, NC. November 1976.
17. Ower, E. and R.C. Pankhurst. The Measurement of Air Plow, 4th Ed. London,
Pergamon Press. 1966.
18. Vollaro, R.F. A Survey of Commercially Available Instrumentation for the
Measurement of Low-Range Gas Velocities. U.S. Environmental Protection
Agency, Emission Measurement Branch, Research Triangle Park, NC.
November 1976. (Unpublished Paper).
19. Gnyp, A.W., C.C. St. Pierre, D.S. Smith, D. Mozzon, and J. Steiner. An
Experimental Investigation of the Effect of Pitot Tube-Sampling Probe
Configurations on the Magnitude of the S Type Pitot Tube Coefficient for
Commercially Available Source Sampling Probes. Prepared by the University
of Windsor for the Ministry of the Environment, Toronto, Canada.
February 1975.
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EMTIC TM-002
NSPS TEST METHOD
Page 16
140-2.54 cm*
(0.75 -1.0 In.)
CT
7.82 cm (J In.)*
Ttmpcratura Sm>or
y
J L
TypiSPNotTulM
' SuggMtod (Intocttranc* Fm)
P«ottub«/Th«nnocoupk Spacing
Figure 2-1. Type S pitot tube manometer assembly.
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EMTIC TM-002
NSPS TBST METHOD
Page 17
TnnmiM
Tub* Ax*
LongHudkul
Tub. Ail.
F«.
OpMhtg ..
Ptan.i I
A-SM* Ptam
B-Skte Plan*
(b)
(•) end it**: h
to kwwniM uk:
(b) top vlev: he* ee*flk« pbnm pwdel to
Q~ AerB V 7
(e)
(c) *ide vltw; eeft hg> el eqiMl l»njlh and
cwitonkwc colncUvnl, whMi vtowsd from
bothiktoi. iMclMeo^ffielMiimueeel
0 M miy be mlgned IB (*« tub«« een-
Figure 2-2. Properly constructed Type S pitot tube.
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EMTIC TM-002
NSPS TKST METHOD
Page 18
Figure 2-3. Types of face-opening misalignment that can result from field use
or improper construction of Type S pitot tubes. These will not affect the
baseline value of Cp(s) so long as a1 and a2 ilO°, p1 and P2 *5*, z £0.32 cm (1/8
in.) and w £0.08 cm (1/32 in.) (citation 11 in Bibliography).
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EMTIC TM-002
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Page 19
Figure 2-4. Standard pi tot tube design specifications.
-------
EMTIC TM-002 NSPS TEST METHOD Page 20
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EMTIC TM-002
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PLANT
DATE
DIMENSIONS,
(in. Hg) _
OPERATORS _
STACK DIA. OR
m (in.) BAROMETRIC PRESS., mm Hg
CROSS SECTIONAL AREA, m2 (ft2)
RUN NO.
(in.) _
PITOT TUBE I.D. NO.
AVG. COEFFICIENT, Cp =
LAST DATE CALIBRATED _
SCHEMATIC OF STACK
CROSS SECTION
Traverse
Pt. No.
Vel. Hd., AP
mm ( in . ) H2O
Stack Temperature
T.,
°C (°F)
Average
T.,
°V 1 °O \
JS. \ KJ
nun Hcf
(in.Hg)
Up)1/2
Figure 2-5. Velocity traverse data.
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EMTIC TM-002
NSPS TEST METHOD
Page 22
TyptSPIetTub.
a
«.HJI..fllk,)h.D , IJ — C
Sim ping NozHt
A. Bottom Vfcw, thowkij Minimum pIM Iub*-Mali §»(>»r»tk)n.
B. Skto Vtaw. to prev.nl plot tub* tram tatortotkig wWi gu
Dow itraMilMi tppr»Khlng ttw noata, Kit Impact pnuurt
opining ptuw ol«ni ptotkib* «h»l b* mnwMi orakov* «w
nczzh inby ptalw.
Figure 2-6. Proper pitot tube-sampling nozzle configuration to prevent
aerodynamic interference; button-hook type nozzle: centers of nozzle and
pitot opening aligned; Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).
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EMTIC TM-002
NSPS TEST METHOD
Page 23
CO
Ji.
\JL.
run
(•mpkPnM
Figure 2-7. Proper thermocouple placement to prevent interference; Dt
between 0.48 and 0.95 cm (3/16 and 3/8 in.).
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EMTIC TM-002
NSPS TEST METHOD
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Typ*S Pilot Tub*
Sampw Prob*
Figure 2-8. Minimum pilot-sample probe separation needed to prevent
interference; Dt between 0.48 and 0.95 cm (3/16 and 3/8 in.).
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EMTIC TM-002
NSPS TEST METHOD
Page 25
PITOT TUBE IDENTIFICATION NUMBEI
I: DATE: CALIBRATED BY:
RUN NO.
1
2
3
RUN NO.
1
2
3
"A" SIDE CALIBRATION
cm H2O
(in H2O)
cm H2O
(in H2O)
Cp,»vg
(SIDE A)
c,,.,
« B" SIDE CALIBRATION
cm H2O
(in H2O)
A wnra/tartaw Hat-inn — CT
cm H2O
(in H2O)
(SIDE B)
Deviation
c_, , - c_ (A)
^»p{() **p \**/
Deviation
Cp,., - CP(B)
3
2-f p(S) p(AorB)
- - **.. -. 4-Mlir.tRp <[) HI
(AorB)
C (SideA) -C (S1deB) -HustBe^O.Ol
p P |
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EMTIC TM-002 MSPS TEST METHOD Page 26
Figure 2-9. Pitot tube calibration data.
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EMTIC TM-002
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Page 27
Figure 2-10. Projected-area models for typical pitot tube assemblies.
-------
APPENDIX F.4
EPA METHOD 4
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
Method 4 - Determination of Moisture Content
in Stack Gases
1. PRINCIPLE AND APPLICABILITY
1.1 Principle. A gas sample is extracted at a constant rate from
the source; moisture is removed from the sample stream and
determined either volumetrically or gravimetrically.
1.2 Applicability. This method is applicable for determining the
moisture content of stack gas.
1.2.1 Two procedures are given. The first is a reference method,
for accurate determinations of moisture content (such as are needed
to calculate emission data). The second is an approximation
method, which provides estimates of percent moisture to aid in
setting isokinetic sampling rates prior to a pollutant emission
measurement run. The approximation method described herein is only
a suggested approach; alternative means for approximating the
moisture content, e.g., drying tubes, wet bulb-dry bulb techniques,
condensation techniques, stoichiometric calculations, previous
experience, etc., are also acceptable.
1.2.2 The reference method is often conducted simultaneously with
a pollutant emission measurement run; when it is, calculation of
percent isokinetic, pollutant emission rate, etc., for the run
shall be based upon the results of the reference method or its
equivalent; these calculations shall not be based upon the results
of the approximation method, unless the approximation method is
shown, to the satisfaction of the Administrator, U.S. Environmental
Protection Agency, to be capable of yielding results within 1
percent H20 of the reference method.
Prepared by Emission Measurement Branch EMTIC TM-004
Technical Support Division, OAQPS, EPA July 11, 1989
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
1.2.3 Note: The reference method may yield questionable results
when applied to saturated gas streams or to streams that contain
water droplets. Therefore, when these conditions exist or are
suspected, a second determination of the moisture content shall be
made simultaneously with the reference method, as follows: Assume
that the gas stream is saturated. Attach a temperature sensor
[capable of measuring to within 1°C (2°F)] to the reference method
probe. Measure the stack gas temperature at each traverse point
(see Section 2.2.1} during the reference method traverse; calculate
the average stack gas temperature. Next, determine the moisture
percentage, either by: (1) using a psychrometric chart and making
appropriate corrections if stack pressure is different from that of
the chart, or (2) using saturation vapor pressure tables. In cases
where the psychrometric chart or the saturation vapor pressure
tables are not applicable (based on evaluation of the process),
alternative methods, subject to the approval of the Administrator,
shall be used.
2. REFERENCE METHOD
The procedure described in Method 5 for determining moisture
content is acceptable as a reference method.
2.1 Apparatus. A schematic of the sampling train used in this
reference method is shown in Figure 4-1. All components shall be
maintained and calibrated according to the procedures in Method 5.
2.1.1 Probe. Stainless steel or glass tubing, sufficiently heated
to prevent water condensation, and equipped with a filter, either
in-stack (e.g., a plug of glass wool inserted into the end of the
probe) or heated out-stack (e.g., as described in Method 5), to
remove particulate matter. -When stack conditions permit, other
metals or plastic tubing may be used for the probe, subject to the
approval of the Administrator.
Prepared by Emission Measurement Branch EMTIC TM-004
Technical Support Division, OAQPS, EPA July 11, 1989
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 3
2.1.2 Condenser. See Method 5, Section 2.1.7, for a description
of an acceptable type of condenser and for alternative measurement
systems.
2.1.3 Cooling System. An ice bath container and crushed ice (or
equivalent), to aid in condensing moisture.
2.1.4 Metering System. Same as in Method 5, Section 2.1.8, except
do not use sampling systems designed for flow rates higher than
0.0283 mVmin (1.0 cfm). Other metering systems, capable of
maintaining a constant sampling rate to within 10 percent and
determining sample gas volume to within 2 percent, may be used,
subject to the approval of the Administrator.
2.1.5 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm (0.1 in.) Hg. See
NOTE in Method 5, Section 2.1.9.
2.1.6 Graduated Cylinder and/or Balance. To measure condensed
water and moisture caught in the silica gel to within 1 ml or 0.5
g. Graduated cylinders shall have subdivisions no greater than 2
ml. Most laboratory balances are capable of weighing to the
nearest 0.5 g or less. These balances are suitable for use here.
2.2 Procedure. The following procedure is written for a condenser
system (such as the impinger system described in Section 2.1.7 of
Method 5) incorporating volumetric analysis to measure the
condensed moisture, and silica gel and gravimetric analysis to
measure the moisture leaving the condenser.
2.2.1 Unless otherwise specified by the Administrator, a minimum
of eight traverse points shall be used for circular stacks having
diameters less than 0.61 m (24 in.), a minimum of nine points shall
be used for rectangular stacks
having equivalent diameters less than 0.61 m (24 in.), and a
minimum of twelve traverse points shall be used in all other cases.
The traverse points shall be located according to Method 1. The
use of fewer points is subject to the approval of the
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 4
Administrator. Select a suitable probe and probe length such that
all traverse points can be sampled. Consider sampling from
opposite sides
of the stack (four total sampling ports) for large stacks, to
permit use of shorter probe lengths. Mark the probe with heat
resistant tape or by some other method to denote the proper
distance into the stack or duct for each sampling point. Place
known volumes of water in the first two impingers. Weigh and
record the weight of the silica gel to the nearest 0.5 g, and
transfer the silica gel to the fourth impinger; alternatively, the
silica gel may first be transferred to the impinger, and the weight
of the silica gel plus impinger recorded.
2.2.2 Select a total sampling time such that a minimum total gas
volume of 0.60 scm (21 scf) will be collected, at a rate no greater
than 0.021 mVmin (0.75 cfm). When both moisture content and
pollutant emission rate are to be determined, the moisture
determination shall be simultaneous with, and for the same total
length of time as, the pollutant emission rate run, unless
otherwise specified in an applicable subpart of the standards.
2.2.3 Set up the sampling train as shown in Figure 4-1. Turn on
the probe heater and (if applicable) the filter heating system to
temperatures of about 120°C (248°F), to prevent water condensation
ahead of the condenser; allow time for the temperatures to
stabilize. Place crushed ice in the ice bath container. It is
recommended, but not required, that a leak check be done, as
follows: Disconnect the probe from the first impinger or (if
applicable) from the filter holder. Plug the inlet to the first
impinger (or filter holder), and pull a 380 mm (15 in.) Hg vacuum;
a lower vacuum may be used, provided that it is not exceeded during
the test. A leakage rate in excess of 4 percent of the average
sampling rate or 0.00057 m3/min (0.02 cfm), whichever is less, is
unacceptable. Following the leak check, reconnect the probe to the
sampling train.
2.2.4 During the sampling run, maintain a sampling rate within 10
percent of constant rate, or as specified by the Administrator.
For each run, record the data required on the example data sheet
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 5
shown in Figure 4-2. Be sure to record the dry gas meter reading
at the beginning and end of each sampling time increment and
whenever sampling is halted. Take other appropriate readings at
each sample point, at least once during each time increment.
2.2.5 To begin sampling, position the probe tip at the first
traverse point. Immediately start the pump, and adjust the flow to
the desired rate. Traverse the cross section, sampling at each
traverse point for an equal length of time. Add more ice and, if
necessary, salt to maintain a temperature of less than 20°C (68°F)
at the silica gel outlet.
2.2.6 After collecting the sample, disconnect the probe from the
filter holder (or from the first impinger) , and conduct a leak
check (mandatory) as described in Section 2.2.3. Record the leak
rate. If the leakage rate exceeds the allowable rate, the tester
shall either reject the test results or shall correct the sample
volume as in Section 6.3 of Method 5. Next, measure the volume of
the moisture condensed to the nearest ml. Determine the increase
in weight of the silica gel (or silica gel plus impinger) to the
nearest 0.5 g. Record this information (see example data sheet,
Figure 4-3), and calculate the moisture percentage, as described in
2.3 below.
2.2.7 A quality control check of the volume metering system at the
field site is suggested before collecting the sample following the
procedure in Method 5, Section 4.4.
2.3 Calculations. Carry out the following calculations, retaining
at least one extra decimal figure beyond that of the acquired data.
Round off figures after final calculation.
2.3.1 Nomenclature.
BWB = Proportion of water vapor, by volume, in the gas stream.
M,, = Molecular weight of water, 18.0 g/g-mole (18.0 Ib/lb-
mole).
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 6
Pm = Absolute pressure (for this method, same as barometric
pressure) at the dry gas meter, mm Hg (in. Hg).
Pscd = Standard absolute pressure, 760 mm Hg (29.92 in. Hg) .
R = Ideal gas constant, 0.06236 (mm Hg) (m3) / (g-mole) (°K) for
metric units and 21.85 (in. Hg) (ft3) / (Ib-mole) (°R) for
English units.
Tm = Absolute temperature at meter, °K (°R) .
Tstd = Standard absolute temperature, 293°K (528°R) .
Vm = Dry gas volume measured by dry gas meter, dcm (dcf).
AVm = Incremental dry gas volume measured by dry gas meter at
each traverse point, dcm (dcf).
Vm(std> = DrY 9as volume measured by the dry gas meter, corrected to
standard conditions, dscm (dscf).
VWC(std> = Volume of water vapor condensed, corrected to standard
conditions, scm (scf).
VWSgfstd> = Volume of water vapor collected in silica gel, corrected
to standard conditions, scm (scf).
V£ = Final volume of condenser water, ml.
VA = Initial volume, if any, of condenser water, ml.
Wf = Final weight of silica gel or silica gel plus impinger, g.
Wi = Initial weight of silica gel or silica gel plus impinger,
g.
Y = Dry gas meter calibration factor.
pw = Density of water, 0.9982 g/ml (0.002201 Ib/ml).
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 7
2.3.2 Volume of Water Vapor Condensed.
RT
= (V -V)p 8td
* i PstdM* ES- 4'1
= K (V -V )
Where :
K! = 0.001333 m3/ml for metric units,
= 0.04707 ft3 /ml for English units.
2.3.3 Volume of Water Collected in Silica Gel.
_ (Wf - W,) RT,td
w.g(.td)
— W
Where :
K2 = 0.001335 m3/g for metric units,
= 0.04715 ft3/g for English units
2.3.4 Sample Gas Volume.
(PJ (T )
/ = v Y gtd
m(std) m ^p \ /T \
= K,Y
3
"td m Prr A T
V p E(3- 4'3
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 8
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 9
Where:
K3 = 0.3858 °K/mm Hg for metric units,
= 17.64 °R/in. Hg for English units.
NOTE: If the post-test leak rate (Section 2.2.6) exceeds the
allowable rate, correct the value of Vm in Equation 4-3, as
described in Section 6.3 of Method 5.
2.3.5 Moisture Content.
B Vwc(8td) +Vw.g(.td) Eq. 4-4
ws V +V +V
wc(std) wsg(std) m(std)
NOTE: In saturated or moisture droplet-laden gas streams, two
calculations of the moisture content of the stack gas shall be
made, one using a value based upon the saturated conditions (see
Section 1.2), and another based upon the results of the impinger
analysis. The lower of these two values of Bws shall be considered
correct.
2.3.6 Verification of Constant Sampling Rate. For each time
increment, determine the AVm. Calculate the average. If the value
for any time increment differs from the average by more than 10
percent, reject the results, and repeat the run.
3. APPROXIMATION METHOD
The approximation method described below is presented only as a
suggested method (see Section 1.2).
3.1 Apparatus. See Figure 4-4.
3.1.1 Probe. Stainless steel or glass tubing, sufficiently heated
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 10
to prevent water condensation and equipped with a filter (either
in-stack or heated out-stack) to remove particulate matter. A plug
of glass wool, inserted into the end of the probe, is a
satisfactory filter.
3.1.2 Impingers. Two midget impingers, each with 30-ml capacity,
or equivalent.
3.1.3 Ice Bath. Container and ice, to aid in condensing moisture
in impingers.
3.1.4 Drying Tube. Tube packed with new or regenerated 6- to 16-
mesh indicating-type silica gel (or equivalent desiccant), to dry
the sample gas and to protect the meter and pump.
3.1.5 Valve. Needle valve, to regulate the sample gas flow rate.
3.1.6 Pump. Leak-free, diaphragm type, or equivalent, to pull the
gas sample through the train.
3.1.7 Volume Meter. Dry gas meter, sufficiently accurate to
measure the sample volume to within 2 percent, and calibrated over
the range of flow rates and conditions actually encountered during
sampling.
3.1.8 Rate Meter. Rotameter, to measure the flow range from 0 to
3 liters/min (0 to 0.11 cfm).
3.1.9 Graduated Cylinder. 25-ml.
•
3.1.10 Barometer. Mercury, aneroid, or other barometer, as
described in Section 2.1.5 above.
3.1.11 Vacuum Gauge. At least 760-mm (30-in.) Hg gauge, to be
used for the sampling leak check.
3.2 Procedure.
3.2.1 Place exactly 5 ml water in each impinger. Leak check the
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 11
sampling train as follows: Temporarily insert a vacuum gauge at or
near the probe inlet; then, plug the probe inlet, and pull a vacuum
of at least 250 mm (10 in.) Hg. Note the time rate of change of
the dry gas meter dial; alternatively, a rotameter (0 to 40 cc/min)
may be temporarily attached to the dry gas meter outlet to
determine the leakage rate. A leak rate not in excess of 2 percent
of the average sampling rate is acceptable. NOTE: Carefully
release the probe inlet plug before turning off the pump.
3.2.2 Connect the probe, insert it into the stack, and sample at
a constant rate of 2 liters/min (0.071 cfm). Continue sampling
until the dry gas meter registers about 30 liters (1.1 ft3) or
until visible liquid droplets are carried over from the first
impinger to the second. Record temperature, pressure, and dry gas
meter readings as required by Figure 4-5.
3.2.3 After collecting the sample, combine the contents of the two
impingers, and measure the volume to the nearest 0.5 ml.
3.3 Calculations. The calculation method presented is designed to
estimate the moisture in the stack gas; therefore, other data,
which are only necessary for accurate moisture determinations, are
not collected. The following equations adequately estimate the
moisture content, for the purpose of determining isokinetic
sampling rate settings.
3.3.1 Nomenclature.
Em = Approximate proportion by volume of water vapor in the gas
stream leaving the second impinger, 0.025.
Bws = Water vapor in the gas stream, proportion by volume.
M« = Molecular weight of water, 18.0 g/g-mole (18.0 Ib/lb-
mole).
Pm = Absolute pressure (for this method, same as barometric
pressure) at the dry gas meter, mm Hg (in. Hg).
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EMTIC TM-004 EMTIC NSPS TEST METHOD
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Pstd = Standard absolute pressure, 760 mm Hg (29.92 in. Hg) .
R = Ideal gas constant, 0.06236 [(mm Hg) (m3) ] / [ (g-mole) (°K) ]
for metric units and 21.85 [(in. Hg) (ft3) ] / [ (Ib-mole) (°R)]
for English units.
Tm = Absolute temperature at meter, °K (°R) .
Tstd = Standard absolute temperature, 293°R (528°R) .
Vf = Final volume of impinger contents, ml.
Vi = Initial volume of impinger contents, ml.
Vm = Dry gas volume measured by dry gas meter, dcm (dcf ) .
vm(std) - DrY 9as volume measured by dry gas meter, corrected to
standard conditions, dscm (dscf ) .
Y = Dry gas meter calibration factor.
pw = Density of water, 0.9982 g/ml (0.002201 Ib/ml) .
3.3.2 Volume of Water Vapor Collected.
V
PatdMw Eq. 4-5
Where :
Kx = 0.001333 m3/ml for metric units,
= 0.04.707 ft3/ml for English units
3.3.3 Gas Volume .
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 13
Eq. 4-6
Where:
K2 = 0.03858 °K/mm Hg for metric units,
= 17.64 °R/in. Hg for English units.
3.3.4 Approximate Moisture Content.
B = 2 +B
ws V +V wm
we m(std)
= — + (0.025)
V +V
vwc vm(std)
4. CALIBRATION
4.1 For the reference method, calibrate the metering system,
temperature gauges, and barometer according to Sections 5.3, 5.5,
and 5.7, respectively, of Method 5. The recommended leak check of
the metering system (Section 5.6 of Method 5) also applies to the
reference method. For the approximation method, use the procedures
outlined in Section 5.1.1 of Method 6 to calibrate the metering
system, and the procedure of Method 5, Section 5.7, to calibrate
the barometer.
5. BIBLIOGRAPHY
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EMTIC TM-004 EMTIC NSPS TEST METHOD
Page 14
1. Air Pollution Engineering Manual (Second Edition). Danielson,
J.A. (ed.). U.S. Environmental Protection Agency, Office of Air
Quality Planning and Standards. Research Triangle Park, NC.
Publication No. AP-40. 1973.
2. Devorkin, Howard, et al. Air Pollution Source Testing Manual.
Air Pollution Control District, Los Angeles, CA. November 1963.
3. Methods for Determination of Velocity, Volume, Dust and Mist
Content of Gases. Western Precipitation Division of Joy
Manufacturing Co. Los Angeles, CA. Bulletin WP-50. 1968.
-------
APPENDIX F.5
EPA METHOD 18
-------
METHOD 18 - MEASUREMENT OF GASEOUS ORGANIC COMPOUND
EMISSIONS BY GAS CHROMATOGRAPHY
NOTE: This method is not inclusive with respect to
specifications (e.g., equipment and supplies) and procedures
(e.g., sampling and analytical) essential to its
performance. Some material is incorporated by reference
from other methods in this part. Therefore, to obtain
reliable results, persons using this method should have a
thorough knowledge of at least the following additional test
methods: Method 1, Method 2, Method 3.
NOTE: This method should not be attempted by persons
unfamiliar with the performance characteristics of gas
Chromatography, nor by those persons who are unfamiliar with
source sampling. Particular care should be exercised in the
area of safety concerning choice of equipment and operation
in potentially explosive atmospheres.
1.0 Scope and Application.
1.1 Analyte. Total gaseous organic compounds.
1.2 Applicability.
1.2.1 This method applies to the analysis of
approximately 90 percent of the total gaseous organics
emitted from an industrial source. It does not include
techniques to identify and measure trace amounts of organic
compounds, such as those found in building air and fugitive
emission sources.
1.2.2 This method will not determine compounds that (1).
are polymeric (high molecular weight), (2) can polymerize
before analysis, or (3) have very low vapor pressures at
stack or instrument conditions.
1.3 Range. The lower range of this method is determined
by the sampling system; adsorbents may be used to
concentrate the sample, thus lowering the limit of detection
below the 1 part per million (ppm) typically achievable with
direct interface or bag sampling. The upper limit is
governed by GC detector saturation or column overloading;
the upper range can be extended by dilution of sample with
an inert gas or by using smaller volume gas sampling loops.
18-1 September 1996
-------
The upper limit can also be governed by condensation of
higher boiling compounds.
1.4 Sensitivity. The sensitivity limit for a compound
is defined as the minimum detectable concentration of that
compound, or the concentration that produces a
signal-to-noise ratio of three to one. The minimum
detectable concentration is determined during the presurvey
calibration for each compound.
2.0 Summary of Method. The major organic components of a
gas mixture are separated by gas chromatography (GC) and
individually quantified by flame ionization,
photoionization, electron capture, or other appropriate
detection principles. The retention times of each separated
component are compared with those of known compounds under
identical conditions. Therefore, the analyst confirms the
identity and approximate concentrations of the organic
emission components beforehand. With this information, the
analyst then prepares or purchases commercially available
standard mixtures to calibrate the GC under conditions
identical to those of the samples. The analyst also
determines the need for sample dilution to avoid detector
saturation, gas stream filtration to eliminate particulate
matter, and prevention of moisture condensation.
3.0 Definitions. [Reserved]
4.0 Interferences.
4.1 Resolution interferences that may occur can be
eliminated by appropriate GC column and detector choice or
by shifting the retention times through changes in the
column flow rate and the use of temperature programming.
4.2 The analytical system is demonstrated to be
essentially free from contaminants by periodically analyzing
blanks that consist of hydrocarbon-free air or nitrogen.
4.3 Sample cross-contamination that occurs when
high-level and low-level samples or standards are analyzed
alternately, is best dealt with by thorough purging of the
GC sample loop between samples.
4.4 To assure consistent detector response, calibration
gases are contained in dry air. To adjust gaseous organic
concentrations when water vapor is present in the sample,
18-2 September 1996
-------
water vapor concentrations are determined for those samples,
and a correction factor is applied.
5.0 Safety.
5.1 Disclaimer. This method amy involve hazardous
materials, operations, and equipment. This test method does
not purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this
test method to establish appropriate safety and health
practices and determine the applicability of regulatory
limitations prior to performing this test method. The
analyzer users manual should be consulted for specific
precautions to be taken with regard to the analytical
procedure.
18-3 September 1996
-------
6.0 Equipment and Supplies.
6.1 Equipment needed for the presurvey sampling
procedure can be found in Section 8.1.1.
6.2 Equipment needed for the evacuated container
sampling procedure can be found in Section 8.2.1.1.1.
6.3 Equipment needed for the analysis of bag samples can
be found in Section 8.2.1.5.1.
6.4 Equipment needed for the direct interface sampling
and analysis can be found in Section 8.2.2.1.
7.0 Reagents and Standards.
7.1 Reagents needed for the presurvey sampling procedure
can be found in Section 8.1.2.
8.0 Sample Collection, Preservation, Storage, and
Transport.
8.1 Presurvey and Presurvey Sampling. Perform a
presurvey for each source to be tested. Refer to Figure
18-1. Some of the information can be collected from
literature surveys and source personnel. Collect gas
samples that can be analyzed to confirm the identities and
approximate concentrations of the organic emissions.
8.1.1 Apparatus. This apparatus list also applies to
Sections S.2 and 11.
8.1.1.1 Teflon® Tubing. (Mention of trade names or
specific products does not constitute endorsement by the
U.S. Environmental Protection Agency.) Diameter and length
determined by connection requirements of cylinder regulators
and the GC. Additional tubing is necessary to connect the
GC sample loop to the sample.
8.1.1.2 Gas Chromatograph. GC with suitable detector,
columns, temperature-controlled sample loop and valve
assembly, and temperature programmable oven, if necessary.
The GC shall achieve sensitivity requirements for the
compounds under study.
8.1.1.3 Pump. Capable of pumping 100 ml/min. For
flushing sample loop.
8.1.1.4 Flow Meter. To measure flow rates.
8.1.1.5 Regulators. Used on gas cylinders for GC and
for cylinder standards.
18-4 September 1996
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8.1.1.6 Recorder. Recorder with linear strip chart is
minimum acceptable. Integrator (optional) is recommended.
8.1.1.7 Syringes. 0.5-ml, l.O- and 10-microliter size,
calibrated, maximum accuracy (gas tight) for preparing
calibration standards. Other appropriate sizes can be used.
8.1.1.8 Tubing Fittings. To plumb GC and gas cylinders.
8.1.1.9 Septums. For syringe injections.
8.1.1.10 Glass Jars. If necessary, clean, colored glass
jars with Teflon®-lined lids for condensate sample
collection. Size depends on volume of condensate.
8.1.1.11 Soap Film Flowmeter. To determine flow rates.
8.1.1.12 Tedlar Bags. 10- and 50-liter capacity, for
preparation of standards.
8.1.1.13 Dry Gas Meter with Temperature and Pressure
Gauges. Accurate to ± 2 percent, for preparation of gas
standards.
8.1.1.14 Midget Impinger/Hot Plate Assembly. For
preparation of gas standards.
8.1.1.15 Sample Flasks. For presurvey samples, must
have gas-tight seals.
8.1.1.16 Adsorption Tubes. If necessary, blank tubes
filled with necessary adsorbent (charcoal, Tenax, XAD-2,
etc.) for presurvey samples.
8.1.1.17 Personnel Sampling Pump. Calibrated, for
collecting adsorbent tube presurvey samples.
8.1.1.18 Dilution System. Calibrated, the dilution
system is to be constructed following the specifications of
an acceptable method.
8.1.1.19 Sample Probes. Pyrex or stainless steel, of
sufficient length to reach centroid of stack, or a point no
closer to the walls than 1 m.
8.1.1.20 Barometer. To measure barometric pressure.
8.1.2 Reagents.
8.1.2.1 Water. Deionized distilled.
8.1.2.2 Methylene Dichloride.
8.1.2.3 Calibration Gases. A series of standards
prepared for every compound of interest.
8.1.2.4 Organic Compound Solutions. Pure (99.9
percent), or a s pure as can reasonably be obtained, liquid
samples of all the organic compounds needed to prepare
calibration standards.
8.1.2.5 Extraction Solvents. For extraction of
adsorbent tube samples in preparation for analysis.
18-5 September 1996
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8.1.2.6 Fuel. As recommended by the manufacturer for
operation of the GC.
8.1.2.7 Carrier Gas. Hydrocarbon free, as recommended
by the manufacturer for operation of the detector and
compatibility with the column.
8.1.2.8 Zero Gas. Hydrocarbon free air or nitrogen, to
be used for dilutions, blank preparation, and standard
preparation.
8.1.3 Sampling.
8.1.3.1 Collection of Samples with Glass Sampling
Flasks. Presurvey samples can be collected in precleaned
250-ml double-ended glass sampling flasks. Teflon®
stopcocks, without grease, are preferred. Flasks should be
cleaned as follows: Remove the stopcocks from both ends of
the flasks, and wipe the parts to remove any grease. Clean
the stopcocks, barrels, and receivers with methylene
dichloride. Clean all glass ports with a soap solution,
then rinse with tap and deionized distilled water. Place
the flask in a cool glass annealing furnace, and apply heat
up to 500°C. Maintain at this temperature for 1 hours.
After this time period, shut off and open the furnace to
allow the flask to cool. Grease the stopcocks with stopcock
grease, and return them to the flask receivers. Purge the
assembly with high- purity nitrogen for 2 to 5 minutes.
Close off the stopcocks after purging to maintain a slight
positive nitrogen pressure. Secure the stopcocks with tape.
Presurvey samples can be obtained either by drawing the
gases into the previously evacuated flask or by drawing the
gases into and purging the flask with a rubber suction bulb.
8.1.3.1.1 Evacuated Flask Procedure. Use a high-vacuum
pump to evacuate the flask to the capacity of the pump; then
close off the stopcock leading to the pump. Attach a 6-mm
outside diameter (OD) glass tee to the flask inlet with a
short piece of Teflon® tubing. Select a 6-mm OD
borosilicate sampling probe, enlarged at one end to a 12-mm
OD and of sufficient length to reach the centroid of the
duct to be sampled. Insert a glass wool plug in the
enlarged end of the probe to remove particulate matter.
Attach the other end of the probe to the tee with a short
piece of Teflon® tubing. Connect a rubber suction bulb to
the third leg of the tee. Place the filter end of the probe
at the centroid of the duct, and purge the probe with the
rubber suction bulb. After the probe is completely purged
18-6 September 1996
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and filled with duct gases, open the stopcock to the grab
flask until the pressure in the flask reaches duct pressure.
Close off the stopcock, and remove the probe from the duct.
Remove the tee from the flask and tape the stopcocks to
prevent leaks during shipment. Measure and record the duct
temperature and pressure.
8.1.3.1.2 Purged Flask Procedure. Attach one end of the
sampling flask to a rubber suction bulb. Attach the other
end to a 6-mm OD glass probe as described in Section
8.3.3.1.1. Place the filter end of the probe at the
centroid of the duct, or at a point no closer to the walls
than 1 m, and apply suction with the bulb to completely
purge the probe and flask. After the flask has been purged,
close off the stopcock near the suction bulb, and then close
off the stopcock near the probe. Remove the probe from the
duct, and disconnect both the probe and suction bulb. Tape
the stopcocks to prevent leakage during shipment. Measure
and record the duct temperature and pressure.
8.1.3.2 Flexible Bag Procedure. Tedlar or aluminized
Mylar bags can also be used to obtain the presurvey sample.
Use new bags, and leak check them before field use. In
addition, check the bag before use for contamination by
filling it with nitrogen or air, and analyzing the gas by GC
at high sensitivity. Experience indicates that it is
desirable to allow the inert gas to remain in the bag about
24 hours or longer to check for desorption of organics from
the bag. Follow the leak-check and sample collection
procedures given in Section 8.2.1.
8.1.3.3 Determination of Moisture Content. For
combustion or water- controlled processes, obtain the
moisture content from plant personnel or by measurement
during the presurvey. If the source is below 59°C, measure
the wet bulb and dry bulb temperatures, and calculate the
moisture content using a psychrometric chart. At higher
temperatures, use Method 4 to determine the moisture
content.
8.1.4 Determination of Static Pressure. Obtain the
static pressure from the plant personnel or measurement. If
a type S pitot tube and an inclined manometer are used, take
care to align the pitot tube 90° from the direction of the
flow. Disconnect one of the tubes to the manometer, and
read the static pressure; note whether the reading is
positive or negative.
18-7 September 1996
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8.1.5 Collection of Presurvey Samples with Adsorption
Tube. Follow Section 16.1 for presurvey sampling.
8.2 Final Sampling and Analysis Procedure. Considering
safety (flame hazards) and the source conditions, select an
appropriate sampling and analysis procedure (Section 8.2.1,
8.2.2, 8.2.3 or 16.1). In situations where a hydrogen flame
is a hazard and no intrinsically safe GC is suitable, use
the flexible bag collection technique or an adsorption
technique. If the source temperature is below 100°C, and the
organic concentrations are suitable for the detector to be
used, use the direct interface method. If the source gases
require dilution, use a dilution interface and either the
bag sample or adsorption tubes. The choice between these
two techniques will depend on the physical layout of the
site, the source temperature, and the storage stability of
the compounds if collected in the bag. Sample polar
compounds by direct interfacing or dilution interfacing to
prevent sample loss by adsorption on the bag.
8.2.1 Integrated Bag Sampling and Analysis.
8.2.1.1 Evacuated Container Sampling Procedure. In this
procedure, the bags are filled by evacuating the rigid
air-tight container holding the bags. Use a field sample
data sheet as shown in Figure 18-10. Collect triplicate
sample from each sample location.
8.2.1.1.1 Apparatus.
8.2.1.1.1.1 Probe. Stainless steel, Pyrex glass, or
Teflon® tubing probe, according to the duct temperature,
with 6.4-mm OD Teflon® tubing of sufficient length to
connect to the sample bag. Use stainless steel or Teflon®
unions to connect probe and sample line.
8.2.1.1.1.2 Quick Connects. Male (2) and female (2) of
stainless steel construction.
8.2.1.1.1.3 Needle Valve. To control gas flow.
8.2.1.1.1.4 Pump. Leakless Teflon®-coated
diaphragm-type pump or equivalent. To deliver at least 1
liter/min.
8.2.1.1.1.5 Charcoal Adsorption Tube. Tube filled with
activated charcoal, with glass wool plugs at each end, to
adsorb organic vapors.
8.2.1.1.1.6 Flowmeter. 0 to 500-ml flow range; with
manufacturer's calibration curve.
8.2.1.1.2 Sampling Procedure. To obtain a sample,
assemble the sample train as shown in Figure 18-9. Leak
18-8 September 1996
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check both the bag and the container. Connect the vacuum
line from the needle valve to the Teflon® sample line from
the probe. Place the end of the probe at the centroid of
the stack or at a point no closer to the walls than 1 m, and
start the pump with the needle valve adjusted to yield a
flow of 0.5 liter/minute. After allowing sufficient time to
purge the line several times, connect the vacuum line to the
bag, and evacuate until the rotameter indicates no flow.
Then position the sample and vacuum lines for sampling, and
begin the actual sampling, keeping the rate proportional to
the stack velocity. As a precaution, direct the gas exiting
the rotameter away from sampling personnel. At the end of
the sample period, shut off the pump, disconnect the sample
line from the bag, and disconnect the vacuum line from the
bag container. Record the source temperature, barometric
pressure, ambient temperature, sampling flow rate, and
initial and final sampling time on the data sheet shown in
Figure 18-10. Protect the Tedlar bag and its container from
sunlight. When possible, perform the analysis within 2
hours of sample collection.
8.2.1.2 Direct Pump Sampling Procedure. Follow 8.2.1.1,
except place the pump and needle valve between the probe and
the bag. Use a pump and needle valve constructed of
stainless steel or some other material not affected by the
stack gas. Leak-check the system, and then purge with stack
gas before connecting to the previously evacuated bag.
8.2.1.3 Explosion Risk Area Bag Sampling Procedure.
Follow 8.2.1.1 except replace the pump with another
evacuated can (see Figure 18-9a). Use this method whenever
there is a possibility of an explosion due to pumps, heated
probes, or other flame producing equipment.
8.2.1.4 Other Modified Bag Sampling Procedures. In the
event that condensation is observed in the bag while
collecting the sample and a direct interface system cannot
be used, heat the bag during collection, and maintain it at
a suitably elevated temperature during all subsequent
operations. (NOTE: Take care to leak-check the system prior
to the dilutions so as not to create a potentially explosive
atmosphere.) As an alternative, collect the sample gas, and
simultaneously dilute it in the Tedlar bag.
8.2.1.4.1 In the first procedure, heat the box
containing the sample bag to the source temperature,
provided the components of the bag and the surrounding box
18-9 September 1996
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can withstand this temperature. Then transport the bag as
rapidly as possible to the analytical area while maintaining
the heating, or cover the box with an insulating blanket.
In the analytical area, keep the box heated to source
temperature until analysis. Be sure that the method of
heating the box and the control for the heating circuit are
compatible with the safety restrictions required in each
area.
8.2.1.4.2 To use the second procedure, prefill the
Tedlar bag with a known quantity of inert gas. Meter the
inert gas into the bag according to the procedure for the
preparation of gas concentration standards of volatile
liquid materials (Section 10.1.2.2), but eliminate the
midget impinger section. Take the partly filled bag to the
source, and meter the source gas into the bag through heated
sampling lines and a heated flowmeter, or Teflon® positive
displacement pump. Verify the dilution factors periodically
through dilution and analysis of gases of known
concentration.
8.2.1.5 Analysis of Bag Samples.
8.2.1.5.1 Apparatus. Same as Section 8.1. A minimum of
three gas standards are required.
8.2.1.5.2 Procedure.
8.2.1.5.2.1 Establish proper GC operating conditions as
described in Section 10.2, and record all data listed in
Figure 18-7. Prepare the GC so that gas can be drawn
through the sample valve. Flush the sample loop with gas
from one of the three Tedlar bags containing a calibration
mixture, and activate the valve. Obtain at least two
chromatograms for the mixture. The results are acceptable
when the peak areas from two consecutive injections agree to
within 5 percent' of their average. If they do not agree,
run additional samples or correct the analytical techniques
until this requirement is met. Then analyze the other two
calibration mixtures in the same manner. Prepare a
calibration curve as described in the same manner. Prepare
a calibration curve as described in Section 10.2. If the
results are acceptable, analyze the other two calibration
gas mixtures in the same manner. Prepare the calibration
curve by using the least squares method.
8.2.1.5.2.2 Analyze the two field audit samples as
described in Section 9.2 by connecting each Tedlar bag
containing an audit gas mixture to the sampling valve.
18-10 September 1996
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Calculate the results; record and report the data to the
audit supervisor. If the results are acceptable, proceed
with the analysis of the source samples.
8.2.1.5.2.3 Analyze the source gas samples by connecting
each bag to the sampling valve with a piece of Teflon®
tubing identified with that bag. Follow the restrictions on
replicate samples specified for the calibration gases.
Record the data in Figure 18-11. If certain items do not
apply, use the notation "N.A.". If the bag has been
maintained at an elevated temperature as described in
Section 8.2.1.4, determine the stack gas water content by
Method 4. After all samples have been analyzed, repeat the
analysis of the calibration gas mixtures, and generate a
second calibration curve. Use an average of the two curves
to determine the sample second calibration curve gas
concentrations. If the two calibration curves differ by
more than 5 percent from their mean value, then report the
final results by comparison to both calibration curves.
8.2.1.6 Determination of Bag Water Vapor Content.
Measure the ambient temperature and barometric pressure near
the bag. From a water saturation vapor pressure table,
determine and record the water vapor content of the bag as a
decimal figure. (Assume the relative humidity to be 100
percent unless a lesser value is known.) If the bag has
been maintained at an elevated temperature as described in
Section 8.2.1.4, determine the stack gas water content by
Method 4.
8.2.1.7 Quality Assurance. Immediately prior to the
analysis of the stack gas samples, perform audit analyses as
described in Section 9.2. The audit analyses must agree
with the audit concentrations within 10 percent. If the
results are acceptable, proceed with the analyses of the
source samples. If they do not agree within 10 percent,
then determine the reason for the discrepancy, and take
corrective action before proceeding.
8.2.1.8 Emission Calculations. From the average
calibration curve described in Section 8.2.1.5, select the
value of Cs that corresponds to the peak area. Calculate
the concentration Cc in ppm, dry basis, of each organic in
the sample using Equation 18-5 in Section 12.6.
8.2.2 Direct Interface Sampling and Analysis Procedure.
The direct interface procedure can be used provided that the
moisture content of the gas does not interfere with the
18-11 September 1996
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analysis procedure, the physical requirements of the
equipment can be met at the site, and the source gas
concentration is low enough that detector saturation is not
a problem. Adhere to all safety requirements with this
method.
8.2.2.1 Apparatus.
8.2.2.1.1 Probe. Constructed of stainless steel, Pyrex
glass, or Teflon® tubing as required by duct temperature,
6.4-mm OD. enlarged at duct end to contain glass wool plug.
If necessary, heat the probe with heating tape or a special
heating unit capable of maintaining duct temperature.
8.2.2.1.2 Sample Lines. 6.4-mm OD Teflon® lines,
heat-traced to prevent condensation of material.
8.2.2.1.3 Quick Connects. To connect sample line to gas
sampling valve on GC instrument and to pump unit used to
withdraw source gas. Use a quick connect or equivalent on
the cylinder or bag containing calibration gas to allow
connection of the calibration gas to the gas sampling valve.
8.2.2.1.4 Thermocouple Readout Device. Potentiometer or
digital thermometer, to measure source temperature and probe
temperature.
8.2.2.1.5 Heated Gas Sampling Valve. Of two-position,
six-port design, to allow sample loop to be purged with
source gas or to direct source gas into the GC instrument.
8.2.2,1.6 Needle Valve. To control gas sampling rate
from the source.
8.2.2.1.7 Pump. Leakless Teflon®-coated diaphragm-type
pump or equivalent, capable of at least 1 liter/minute
sampling rate.
8.2.2.1.8 Flowmeter. Of suitable range to measure
sampling rate.
8.2.2.1.9 Charcoal Adsorber. To adsorb organic vapor
collected from the source to prevent exposure of personnel
to source gas.
8.2.2.1.10 Gas Cylinders. Carrier gas (helium or
nitrogen), and oxygen and hydrogen for a flame ionization
detector (FID) if one is used.
8.2.2.1.11 Gas Chromatograph. Capable of being moved
into the field, with detector, heated gas sampling valve,
column required to complete separation of desired
components, and option for temperature programming.
8.2.2.1.12 Recorder/Integrator. To record results.
18-12 September 1996
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8.2.2.2 Procedure. To obtain a sample, assemble the
sampling system as shown in Figure 18-12. Make sure all
connections are tight. Turn on the probe and sample line
heaters. As the temperature of the probe and heated line
approaches the source temperature as indicated on the
thermocouple readout device, control the heating to maintain
a temperature of O to 3°C above the source temperature.
While the probe and heated line are being heated, disconnect
the sample line from the gas sampling valve, and attach the
line from the calibration gas mixture. Flush the sample
loop with calibration gas and analyze a portion of that gas.
Record the results. After the calibration gas sample has
been flushed into the GC instrument, turn the gas sampling
valve to flush position, then reconnect the probe sample
line to the valve. Place the inlet of the probe at the
centroid of the duct, or at a point no closer to the walls
than 1 m, and draw source gas into the probe, heated line,
and sample loop. After thorough flushing, analyze the
sample using the same conditions as for the calibration gas
mixture. Repeat the analysis on an additional sample.
Measure the peak areas for the two samples, and if they do
not agree to within 5 percent of their mean value, analyze
additional samples until two consecutive analyses meet this
criteria. Record the data. After consistent results are
obtained, remove the probe from the source and analyze a
second calibration gas mixture. Record this calibration
data and the other required data on the data sheet shown in
Figure 18-11, deleting the dilution gas information.
(NOTE: Take care to draw all samples, calibration
mixtures, and audits through the sample loop at the same
pressure.)
8.2.2.3 Determination of Stack Gas Moisture Content.
Use Method 4 to measure the stack gas moisture content.
8.2.2.4 Quality Assurance. Same as Section 8.2.1.7.
Introduce the audit gases in the sample line immediately
following the probe.
8.2.2.5 Emission Calculations. Same as Section 8.2.1.8.
8.2.3 Dilution Interface Sampling and Analysis
Procedure. Source samples that contain a high concentration
of organic materials may require dilution prior to analysis
to prevent saturating the GC detector. The apparatus
required for this direct interface procedure is basically
the same as that described in the Section 8.2.2, except a
18-13 September 1996
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dilution system is added between the heated sample line and
the gas sampling valve. The apparatus is arranged so that
either a 10:1 or 100:1 dilution of the source gas can be
directed to the chromatograph. A pump of larger capacity is
also required, and this pump must be heated and placed in
the system between the sample line and the dilution
apparatus.
8.2.3.1 Apparatus. The equipment required in addition
to that specified for the direct interface system is as
follows:
8.2.3.1.1 Sample Pump. Leakless Teflon®-coated
diaphragm-type that can withstand being heated to 120°C and
deliver 1.5 liters/minute.
8.2.3.1.2 Dilution Pumps. Two Model A-150 Komhyr
Teflon® positive displacement type delivering 150 cc/minute,
or equivalent. As an option, calibrated flowmeters can be
used in conjunction with Teflon®-coated diaphragm pumps.
8.2.3.1.3 Valves. Two Teflon® three-way valves,
suitable for connecting to 6.4-mm OD Teflon® tubing.
8.2.3.1.4 Flowmeters. Two, for measurement of diluent
gas, expected delivery flow rate to be 1,350 cc/min.
8.2.3.1.5 Diluent Gas with Cylinders and Regulators.
Gas can be nitrogen or clean dry air, depending on the
nature of the source gases.
8.2.3.1.6 Heated Box. Suitable for being heated to
120°C, to contain the three pumps, three-way valves, and
associated connections. The box should be equipped with
quick connect fittings to facilitate connection of: (1) the
heated sample line from the probe, (2) the gas sampling
valve, (3) the calibration gas mixtures, and (4) diluent gas
lines. A schematic diagram of the components and
connections is shown in Figure 18-13. The heated box shown
in Figure 18-13 is designed to receive a heated line from
the probe. An optional design is to build a probe unit that
attaches directly to the heated box. In this way, the
heated box contains the controls for the probe heaters, or,
if the box is placed against the duct being sampled, it may
be possible to eliminate the probe heaters. In either case,
a heated Teflon® line is used to connect the heated box to
the gas sampling valve on the chromatograph.
18-14 September 1996
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NOTE: Care must be taken to leak-check the system prior
to the dilutions so as not to create a potentially explosive
atmosphere.
8.2.3.2 Procedure.
8.2.3.2.1 Assemble the apparatus by connecting the
heated box, shown in Figure 18-13, between the heated sample
line from the probe and the gas sampling valve on the
chromatograph. Vent the source gas from the gas sampling
valve directly to the charcoal filter, eliminating the pump
and rotameter. Heat the sample probe, sample line, and
heated box. Insert the probe and source thermocouple at the
centroid of the duct, or to a point no closer to the walls
than 1 m. Measure the source temperature, and adjust all
heating units to a temperature O to 3°C above this
temperature. If this temperature is above the safe
operating temperature of the Teflon® components, adjust the
heating to maintain a temperature high enough to prevent
condensation of water and organic compounds. Verify the
operation of the dilution system by analyzing a high
concentration gas of known composition through either the
10:1 or 100:1 dilution stages, as appropriate. (If
necessary, vary the flow of the diluent gas to obtain other
dilution ratios.) Determine the concentration of the
diluted calibration gas using the dilution factor and the
calibration curves prepared in the laboratory. Record the
pertinent data on the data sheet shown in Figure 18-11. If
the data on the diluted calibration gas are not within 10
percent of the expected values, determine whether the
chromatograph or the dilution system is in error, and
correct it. Verify the GC operation using a low
concentration standard by diverting the gas into the sample
loop, bypassing the dilution system. If these analyses are
not within acceptable limits, correct the dilution system to
provide the desired dilution factors. Make this correction
by diluting a high-concentration standard gas mixture to
adjust the dilution ratio as required.
8.2.3.2.2 Once the dilution system and GC operations are
satisfactory, proceed with the analysis of source gas,
maintaining the same dilution settings as used for the
standards. Repeat the analyses until two consecutive values
do not vary by more than 5 percent from their mean value are
obtained.
18-15 September 1996
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8.2.3.2.3 Repeat the analysis of the calibration gas
mixtures to verify equipment operation. Analyze the two
field audit samples using either the dilution system, or
directly connect to the gas sampling valve as required.
Record all data and report the results to the audit
supervisor.
8.2.3.3 Determination of Stack Gas Moisture Content.
Same as Section 8.2.2.3.
8.2.3.4 Quality Assurance. Same as Section 8.2.2.4.
8.2.3.5 Emission Calculations. Same as section 8.2.2.5,
with the dilution factor applied.
8.3 Reporting of Results. At the completion of the
field analysis portion of the study, ensure that the data
sheets shown in Figure 18-11 have been completed. Summarize
this data on the data sheets shown in Figure 18-15.
8.4 Recovery Study. After conducting the presurvey and
identifying all of the pollutants of interest, conduct the
appropriate recovery study during the test based on the
sampling system chosen for the compounds of interest.
8.4.1 Recovery Study for Direct Interface or Dilution
Interface Sampling. If the procedures in Section 8.2.2 or
8.2.3 are to be used to analyze the stack gas, conduct the
calibration procedure as stated in Section 8.2.2.2 or
8.2.3.2, as appropriate. Upon successful completion of the
appropriate calibration procedure, attach the mid-level
calibration gas for at least one target compound to the
inlet of the probe or as close as possible to the inlet of
the probe, but before the filter. Repeat the calibration
procedure by sampling and analyzing the mid-level
calibration gas through the entire sampling and analytical
system until two consecutive samples are within 5 percent of
their mean value. The mean of the calibration gas response
directly to the analyzer and the mean of the calibration gas
response sampled through the probe shall be within 10
percent of each other. If the difference in the two means
is greater than 10 percent, check for leaks throughout the
sampling system and repeat the analysis of the standard
through the sampling system until this criterion is met.
8.4.2 Recovery Study for Bag Sampling.
8.4.2.1 Follow the procedures for the bag sampling and
analysis in Section 8.2.1. After analyzing all three bag
samples, choose one of the bag samples and analyze twice
more (this bag will become the spiked bag). Spike the
18-16 September 1996
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chosen bag sample with a known mixture (gaseous or liquid)
of all of the target pollutants. Follow a procedure similar
to the calibration standard preparation procedure listed in
Section 10.1, as appropriate. The theoretical
concentration, in ppm, of each spiked compound in the bag
shall be 40 to 60 percent of the average concentration
measured in the three bag samples. If a target compound was
not detected in the bag samples, the concentration of that
compound to be spiked shall be 5 times the limit of
detection for that compound. Analyze the bag three times
after spiking. Calculate the average fraction recovered (R)
of each spiked target compound with the equation in Section
12.7.
8.4.2.2 For the bag sampling technique to be considered
valid for a compound, 0.70 <, R <, 1.30. If the R value does
not meet this criterion for a target compound, the sampling
technique is not acceptable for that compound, and therefore
another sampling technique shall be evaluated for acceptance
(by repeating the recovery study with another sampling
technique). Report the R value in the test report and
correct all field measurements with the calculated R value
for that compound by using the equation in Section 12.8.
8.4.3 Recovery Study for Adsorption Tube Sampling. If
following the adsorption tube procedure in Section 16.1,
conduct a recovery study of the compounds of interest during
the actual field test. Set up two identical sampling
trains. Collocate the two sampling probes in the stack.
The probes shall be placed in the same horizontal plane,
where the first probe tip is 2.5 cm from the outside edge of
the other and with a pitot tube on the outside of each
probe. One of the sampling trains shall be designated the
spiked train and the other the unspiked train. Spike all of
the compounds of interest (in gaseous or liquid form) onto
the adsorbent tube(s) in the spiked train before sampling.
The mass of each spiked compound shall be 40 to 60 percent
of the mass expected to be collected with the unspiked
train. Sample the stack gas into the two trains
simultaneously. Analyze the adsorbents from the two trains
utilizing the same analytical procedure and instrumentation.
Determine the fraction of spiked compound recovered (R)
using the equations in Section 12.9.
8.4.3.1 Repeat the procedure in Section 8.4.3 twice
more, for a total of three runs. In order for the adsorbent
18-17 September 1996
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tube sampling and analytical procedure to be acceptable for
a compound, O.VO^R^l.30 (R in this case is the average of
three runs). If the average R value does not meet this
criterion for a target compound, the sampling technique is
not acceptable for that compound, and therefore another
sampling technique shall be evaluated for acceptance (by
repeating the recovery study with another sampling
technique). Report the R value in the test report and
correct all field measurements with the calculated R value
for that compound by using the equation in Section 12.8.
18-18 September 1996
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9.0 Quality Control.
9.1
Section
Quality Control
Measure
Effect
8.4.1 Recovery study for
direct interface or
dilution interface
sampling.
8.4.2 Recovery study for
bag sampling.
8.4.3 Recovery study for
adsorption tube
sampling.
Ensure that there are no
significant leaks in the
sampling system.
Ensure that there are no
significant leaks in the
sampling system.
Ensure that there are no
significant leaks in the
sampling system.
9.2 Quality Assurance for Laboratory Procedures.
Immediately after the preparation of the calibration curves
and prior to the presurvey sample analysis, the analysis
audit described in 40 CFR Part 61, Appendix C, Procedure 2:
"Procedure for Field Auditing GC Analysis," should be
performed. The information required to document the
analysis of the audit samples has been included on the
example data sheets shown in Figures 18-3 and 18-7. The
audit analyses should agree with the audit concentrations
within 10 percent. When available, the tester may obtain
audit cylinders by contacting: U.S. Environmental
Protection Agency, Environmental Monitoring Systems
Laboratory, Quality Assurance Division (MD-77), Research
Triangle Park, North Carolina 27711. Audit cylinders
obtained from a commercial gas manufacturer may be used
provided that (a) the gas manufacturer certifies the audit
cylinder in a manner similar to the procedure described in
40 CFR Part 61, Appendix B, Method 106, Section 7.2.3.1, and
(b) the gas manufacturer obtains an independent analysis of
the audit cylinders to verify this analysis. Independent
analysis is defined as an analysis performed by an
individual other than the individual who performs the gas
manufacturer's analysis, while using calibration standards
18-19
September 1996
-------
and analysis equipment different from those used for the gas
manufacturer's analysis. Verification is complete and
acceptable when the independent analysis concentration is
within 5 percent of the gas manufacturer's concentration.
18-20 September 1996
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10.0 Calibration and Standardization.
10.1 Calibration Standards. Prepare or obtain enough
calibration standards so that there are three different
concentrations of each organic compound expected to be
measured in the source sample. For each organic compound,
select those concentrations that bracket the concentrations
expected in the source samples. A calibration standard may
contain more than one organic compound. If available,
commercial cylinder gases may be used if their
concentrations have been certified by direct analysis. If
samples are collected in adsorbent tubes (charcoal, XAD-2,
Tenax, etc.), prepare or obtain standards in the same
solvent used for the sample extraction procedure. Refer to
Section 16.1. Verify the stability of all standards for the
time periods they are used. If gas standards are prepared
in the laboratory, use one or more of the following
procedures.
10.1.1 Preparation of Standards from High Concentration
Cylinder Standards.
10.1.1.1 Obtain enough high concentration cylinder
standards to represent all the organic compounds expected in
the source samples.
10.1.1.2 Use these high concentration standards to
prepare lower concentration standards by dilution, as shown
by Figures 18-5 and 18-6.
10.1.1.3 To prepare the diluted calibration samples,
calibrated rotameters are normally used to meter both the
high concentration calibration gas and the diluent gas.
Other types of flowmeters and commercially available
dilution systems can also be used.
10.1.1.4 Calibrate each flowmeter before use by placing
it between the diluent gas supply and suitably sized bubble
meter, spirometer, or wet test meter. Record all data shown
on Figure 18-4. While it is desirable to calibrate the
cylinder gas flowmeter with cylinder gas, the available
quantity and cost may preclude it. The error introduced by
using the diluent gas for calibration is insignificant for
gas mixtures of up to 1,000 to 2,000 ppm of each organic
component.
10.1.1.5 Once the flowmeters are calibrated, connect the
flowmeters to the calibration and diluent gas supplies using
6-mm Teflon® tubing. Connect the outlet side of the
18-21 September 1996
-------
flowmeters through a connector to a leak-free Tedlar bag as
shown in Figure 18-5. (See Section 8.2.1 for bag leak-check
procedures.) Adjust the gas flow to provide the desired
dilution, and fill the bag with sufficient gas for GC
calibration. Be careful not to overfill and cause the bag
to apply additional pressure on the dilution system. Record
the flow rates of both flowmeters, and the laboratory
temperature and atmospheric pressure. Calculate the
concentration Cs in ppm of each organic in the diluted gas
using Equation 18-1 in Section 12.2.
10.1.1.6 Single-stage dilutions should be used to
prepare calibration mixtures up to about 1:20 dilution
factor.
10.1.1.7 For greater dilutions, a double dilution system
is recommended, as shown in Figure 18-6. Fill the Tedlar
bag with the dilute gas from the second stage. Record the
laboratory temperature, barometric pressure, and static
pressure readings. Correct the flow reading for temperature
and pressure. Calculate the concentration Cs in ppm of the
organic in the final gas mixture using Equation 18-2 in
Section 12.3.
10.1.1.8 Further details of the calibration methods for
flowmeters and the dilution system can be found in Reference
21 in the Section 17.
10.1.2 Preparation of Standards from Volatile Materials.
Record all data shown on Figure 18-3.
10.1.2.1 Gas Injection Technique. This procedure is
applicable to organic compounds that exist entirely as a gas
at ambient conditions. Evacuate a 10-liter Tedlar bag that
has passed a leak-check (see Section 8.2.1), and meter in
5.0 liters of air or nitrogen through a dry gas meter that
has been calibrated in a manner consistent with the
procedure described in Section 10.3.1 of Method 5. While
the bag is filling use a 0.5-ml syringe to inject a known
quantity of "pure" gas of the organic compound through the
wall of the bag, or through a septum-capped tee at the bag
inlet. Withdraw the syringe needle, and immediately cover
the resulting hole with a piece of masking tape. In a like
manner, prepare dilutions having other concentrations.
Prepare a minimum of three concentrations. Prepare a
minimum of three concentrations. Place each bag on a smooth
surface, and alternately depress opposite sides of the bag
50 times to mix the gases. Record the average meter
18-22 September 1996
-------
temperature and pressure, the gas volume and the barometric
pressure. Record the syringe temperature and pressure
before injection. Calculate each organic standard
concentration Cs in ppm using Equation 18-3 in Section 12.4.
10.1.2.2 Liquid Injection Technique.
10.1.2.2.1 Use the equipment shown in Figure 18-8.
Calibrate the dry gas meter as described in Section 10.1.2.1
with a set test meter or a spirometer. Use a water
manometer for the pressure gauge and glass, Teflon®, brass,
or stainless steel for all connections. Connect a valve to
the inlet of the 50-liter Tedlar bag.
10.1.2.2.2 To prepare the standards, assemble the
equipment as shown in Figure 18-8, and leak-check the
system. Completely evacuate the bag. Fill the bag with
hydrocarbon-free air, and evacuate the bag again. Close the
inlet valve.
10.1.2.2.3 Turn on the hot plate, and allow the water to
reach boiling. Connect the bag to the impinger outlet.
Record the initial meter reading, open the bag inlet valve,
and open the cylinder. Adjust the rate so that the bag will
be completely filled in approximately 15 minutes. Record
meter pressure and temperature, and local barometric
pressure.
10.1.2.2.4 Allow the liquid organic to equilibrate to
room temperature. Fill the 1.0- or 10-microliter syringe to
the desired liquid volume with the organic. Place the
syringe needle into the impinger inlet using the septum
provided, and inject the liquid into the flowing air stream.
Use a needle of sufficient length to permit injection of the
liquid below the air inlet branch of the tee. Remove the
syringe.
10.1.2.2.5 When the bag is filled, stop the pump, and
close the bag inlet valve. Record the final meter reading,
temperature, and pressure.
10.1.2.2.6 Disconnect the bag from the impinger outlet,
and either set it aside for at least 1 hour, or massage the
bag to insure complete mixing.
10.1.2.2.7 Measure the solvent liquid density at room
temperature by accurately weighing a known volume of the
material on an analytical balance to the nearest 1.0
milligram. A ground-glass stoppered 25-ml volumetric flask
or a glass-stoppered specific gravity bottle is suitable for
weighing. Calculate the result in terms of g/ml. As an
18-23 September 1996
-------
alternative, literature values of the density of the liquid
at 20°C may be used.
10.1.2.2.8 Calculate each organic standard
concentration, Cs in ppm using Equation 18-4 in Section
12.5.
10.2 Preparation of Calibration Curves.
10.2.1 Establish proper GC conditions, then flush the
sampling loop for 30 seconds at a rate of 100 ml/min. Allow
the sample loop pressure to equilibrate to atmospheric
pressure, and activate the injection valve. Record the
standard concentration, attenuator factor, injection time,
chart speed, retention time, peak area, sample loop
temperature, column temperature, and carrier gas flow rate.
Repeat the standard injection until two consecutive
injections give area counts within 5 percent of their
average. The average value multiplied by the attenuator
factor is then the calibration area value for the
concentration.
10.2.2 Repeat this procedure for each standard. Prepare
a graphical plot of concentration (Cs) versus the
calibration area values. Perform a regression analysis, and
draw the least square line.
10.3 Relative Response Factors. The calibration curve
generated from the standards for a single organic can
usually be related to each of the individual GC response
curves that are developed in the laboratory for all the
compounds in the source. In the field, standards for that
single organic can then be used to "calibrate" the GC for
all the organics present. This procedure should first be
confirmed in the laboratory by preparing and analyzing
calibration standards containing multiple organic compounds.
11.0 Analytical Procedures.
11.1 Analysis Development.
11.1.1 Selection of GC Parameters.
11.1.1.1 Column Choice. Based on the initial contact
with plant personnel concerning the plant process and the
anticipated emissions, choose a column that provides good
resolution and rapid analysis time. The choice of an
appropriate column can be aided by a literature search,
contact with manufacturers of GC columns, and discussion
with personnel at the emission source.
18-24 September 1996
-------
NOTE: Most column manufacturers keep excellent records
on their products. Their technical service departments may
be able to recommend appropriate columns and detector type
for separating the anticipated compounds, and they may be
able to provide information on interferences, optimum
operating conditions, and column limitations. Plants with
analytical laboratories may be able to provide information
on their analytical procedures.
11.1.1.2 Preliminary GC Adjustment. Using the standards
and column obtained in Section 11.1.1.1, perform initial
tests to determine appropriate GC conditions that provide
good resolution and minimum analysis time for the compounds
of interest.
11.1.1.3 Preparation of Presurvey Samples. If the
samples were collected on an adsorbent, extract the sample
as recommended by the manufacturer for removal of the
compounds with a solvent suitable to the type of GC
analysis. Prepare other samples in an appropriate manner.
11.1.1.4 Presurvey Sample Analysis.
11.1.1.4.1 Before analysis, heat the presurvey sample to
the duct temperature to vaporize any condensed material.
Analyze the samples by the GC procedure, and compare the
retention times against those of the calibration samples
that contain the components expected to be in the stream.
If any compounds cannot be identified with certainty by this
procedure, identify them by other means such as GC/mass
spectroscopy (GC/MS) or GC/infrared techniques. A GC/MS
system is recommended.
11.1.1.4.2 Use the GC conditions determined by the
procedure of Section 11.1.1.2 for the first injection. Vary
the GC parameters during subsequent injections to determine
the optimum settings. Once the optimum settings have been
determined, perform repeat injections of the sample to
determine the retention time of each compound. To inject a
sample, draw sample through the loop at a constant rate (100
ml/min for 30 seconds). Be careful not to pressurize the
gas in the loop. Turn off the pump and allow the gas in the
sample loop to come to ambient pressure. Activate the
sample valve, and record injection time, loop temperature,
column temperature, carrier flow rate, chart speed, and
attenuator setting. Calculate the retention time of each
peak using the distance from injection to the peak maximum
18-25 September 1996
-------
divided by the chart speed. Retention times should be
repeatable within 0.5 seconds.
11.1.1.4.3 If the concentrations are too high for
appropriate detector response, a smaller sample loop or
dilutions may be used for gas samples, and, for liquid
samples, dilution with solvent is appropriate. Use the
standard curves (Section 10.2) to obtain an estimate of the
concentrations .
11.1.1.4.4 Identify all peaks by comparing the known
retention times of compounds expected to be in the retention
times of peaks in the sample. Identify any remaining
unidentified peaks which have areas larger than 5 percent of
the total using a GC/MS, or estimation of possible compounds
by their retention times compared to known compounds, with
confirmation by further GC analysis.
12.0 Data Analysis and Calculations.
12.1 Nomenclature .
Bws = Water vapor content of the bag sample or stack
gas, proportion by volume.
Cs = Concentration of the organic from the calibration
curve , ppm ,
Fr = Relative response factor (if applicable, see
Section 10.3)
Gv = Gas volume or organic compound injected, ml.
Lv = Liquid volume of organic injected,/^!.
M = Molecular weight of organic, g/g-mole.
ms = Total mass of compound measured on adsorbent with
spiked train (//g) .
mu = Total mass of compound measured on adsorbent with
unspiked train (fig) .
nv = Mass per volume of spiked compound measured
.
Pi = Barometric or absolute sample loop pressure at
time of sample analysis, mm Hg.
Pm = Absolute pressure of dry gas meter, mm Hg.
Pr = Reference pressure, the barometric pressure or
absolute sample loop pressure recorded during
calibration, mm Hg.
Ps = Absolute pressure of syringe before injection, mm
Hg.
18-26 September 1996
-------
qc = Flow rate of the calibration gas to be diluted.
qcl = Flow rate of the calibration gas to be diluted in
stage 1.
qc2 = Flow rate of the calibration gas to be diluted in
stage 2.
qd = Diluent gas flow rate.
qdl = Flow rate of diluent gas in stage 1.
qd2 = Flow rate of diluent gas in stage 2.
s = Theoretical concentration (ppm) of spiked target
compound in the bag.
S = Theoretical mass of compound spiked onto adsorbent
in spiked train (//g) .
t = Measured average concentration (ppm) of target
compound and source sample (analysis results
subsequent to bag spiking)
Ti = Sample loop temperature at the time of sample
analysis, °K.
Tm = Absolute temperature of dry gas meter, °K.
Ts = Absolute temperature of syringe before injection,
°K.
u = Source sample average concentration (ppm) of
target compound in the bag (analysis results
before bag spiking).
Vm = Gas volume indicated by dry gas meter, liters.
vs = volume of stack gas sampled with spiked train (L).
vu = volume of stack gas sampled with unspiked train
(L) .
X = Mole or volume fraction of the organic in the
calibration gas to be diluted.
Y = Dry gas meter calibration factor, dimensionless.
fj.1 = Liquid organic density as determined, g/ml.
24.055 = Ideal gas molar volume at 293 °K and 760 mm Hg,
liters/g-mole.
1000 = Conversion factor, ml/liter.
106 = Conversion to ppm.
12.2 Calculate the concentration, Cs, in ppm using the
following equation:
106 (X q )
C = — Eq. 18-1
18-27 September 1996
-------
12.3 Calculate the concentration, Cs, in ppm of the
organic in the final gas mixture using the following
equation:
c = I06x
Eq. 18-2
12.4 Calculate each organic standard concentration, Cs,
in ppm using the following equation:
G x 106
293
760
c =
V Y
T 760
— 1000
P T
G x 103 -i -=
V Y
Eq. 18-3
18-28
September 1996
-------
12.5 Calculate each organic standard concentration, Cs,
in ppm using the following equation:
^p(24.055x10')
C = — =6.24x10* vP m Eq 18-4
s 093 P MV YP q'
V Y-^i——1000 m m
m T 760
12.6 Calculate the concentration, Cc, in ppm, dry basis,
of each organic is the sample using the following equation:
CsPrTiFr
C = S r i r Eg. 18-5
C -
12.7 Calculate the average fraction recovered (R) of
each spiked target compound using the following equation:
R = -^—^ Eq. 18-6
s
12.8 Correct all field measurements with the calculated
R value for that compound using the following equation:
, _ . Measured Concentration (ppm)
Reported Result = ^K Eq. 18-7
R
12.9 Determine the mass per volume of spiked compound
measured using the following equation:
m m
m = —-- —- Eq. 18-8
v v v
12.10 Calculate the fraction of spiked compound
recovered, R, using the following equation:
m x v
R = —"- i Eq. 18-9
13.0 Method Performance.
13.1 Gas chromatographic techniques typically provide a
precision of 5 to 10 percent relative standard deviation
(RSD), but an experienced GC operator with a reliable
instrument can readily achieve 5 percent RSD. For this
18-29 September 1996
-------
method, the following combined GC/operator values are
required.
(a) Precision. Duplicate analyses are within 5
percent of their mean value.
(b) Accuracy. Analysis results of prepared audit
samples are within 10 percent of preparation values.
(c) Recovery. After developing an appropriate sampling
and analytical system for the pollutants of interest,
conduct the procedure in Section 8.4. Conduct the
appropriate recovery study in Section 8.4 at each sampling
point where the method is being applied. Submit the data
and results of the recovery procedure with the reporting of
results under Section 8.3.
14.0 Pollution Prevention. [Reserved]
15.0 Waste Management. [Reserved]
16.0 Alternative Procedures.
16.1 Adsorption Tube Procedure (Alternative Procedure).
It is suggested that the tester refer to the National
Institute for Occupational Safety and Health (NIOSH) method
for the particular organics to be sampled. The principal
interferent will be water vapor. If water vapor is present
at concentrations above 3 percent, silica gel should be used
in front of the charcoal. Where more than one compound is
present in the emissions, then develop relative adsorptive
capacity information.
16.1.1 Additional Apparatus. In addition to the
equipment listed in the NIOSH method for the particular
organic(s) to be sampled, the following items (or
equivalent) are suggested.
16.1.1.1 Probe (Optional). Borosilicate glass or
stainless steel, approximately 6-mm ID, with a heating
system if water condensation is a problem, and a filter
(either in-stack or out-stack heated to stack
temperature) to remove particulate matter. In most
instances, a plug of glass wool is a satisfactory filter.
16.1.1.2 Flexible Tubing. To connect probe to
adsorption tubes. Use a material that exhibits minimal
sample adsorption.
18-30 September 1996
-------
16.1.1.3 Leakless Sample Pump. Flow controlled,
constant rate pump, with a set of limiting (sonic) orifices
to provide pumping rates from approximately 10 to 100
cc/min.
16.1.1.4 Bubble-Tube Flowmeter. Volume accuracy within
1 percent, to calibrate pump.
16.1.1.5 Stopwatch. To time sampling and pump rate
calibration.
16.1.1.6 Adsorption Tubes. Similar to ones specified by
NIOSH, except the amounts of adsorbent per primary/backup
sections are 800/200 mg for charcoal tubes and 1040/260 mg
for silica gel tubes. As an alternative, the tubes may
contain a porous polymer adsorbent such as Tenax GC or
XAD-2.
16.1.1.7 Barometer. Accurate to 5 mm Hg, to measure
atmospheric pressure during sampling and pump calibration.
16.1.1.8 Rotameter. O to 100 cc/min, to detect changes
in flow rate during sampling.
16.1.2 Sampling and Analysis.
16.1.2.1 It is suggested that the tester follow the
sampling and analysis portion of the respective NIOSH method
section entitled "Procedure." Calibrate the pump and
limiting orifice flow rate through adsorption tubes with the
bubble tube flowmeter before sampling. The sample system
can be operated as a "recirculating loop" for this
operation. Record the ambient temperature and barometric
pressure. Then, during sampling, use the rotameter to
verify that the pump and orifice sampling rate remains
constant.
16.1.2.2 Use a sample probe, if required, to obtain the
sample at the centroid of the duct, or at a point no closer
to the walls than 1 m. Minimize the length of flexible
tubing between the probe and adsorption tubes. Several
adsorption tubes can be connected in series, if the extra
adsorptive capacity is needed. Provide the gas sample to
the sample system at a pressure sufficient for the limiting
orifice to function as a sonic orifice. Record the total
time and sample flow rate (or the number of pump strokes),
the barometric pressure, and ambient temperature. Obtain a
total sample volume commensurate with the expected
concentration(s) of the volatile organic(s) present, and
recommended sample loading factors (weight sample per weight
adsorption media). Laboratory tests prior to actual
18-31 September 1996
-------
sampling may be necessary to predetermine this volume.' When
more than one organic is present in the emissions, then
develop relative adsorptive capacity information. If water
vapor is present in the sample at concentrations above 2 to
3 percent, the adsorptive capacity may be severely reduced.
Operate the gas chromatograph according to the
manufacturer's instructions. After establishing optimum
conditions, verify and document these conditions during all
operations. Analyze the audit samples (see Section
16.1.4.3), then the emission samples. Repeat the analysis
of each sample until the relative deviation of two
consecutive injections does not exceed 5 percent.
16.1.3 Standards and Calibration. The standards can be
prepared according to the respective NIOSH method. Use a
minimum of three different standards; select the
concentrations to bracket the expected average sample
concentration. Perform the calibration before and after each
day's sample analyses. Prepare the calibration curve by
using the least squares method.
16.1.4 Quality Assurance.
16.1.4.1 Determine the recovery efficiency of the
pollutants of interest according to Section 8.4.
16.1.4.2 Determination of Sample Collection Efficiency.
For the source samples, analyze the primary and backup
portions of the adsorption tubes separately. If the backup
portion exceeds 10 percent of the total amount (primary and
back-up), repeat the sampling with a larger sampling
portion.
16.1.4.3 Analysis Audit. Immediately before the sample
analyses, analyze the two audits in accordance with Section
16.1.2. The analysis audit shall agree with the audit
concentration within 10 percent.
16.1.4.4 Pump Leak Checks and Volume Flow Rate Checks.
Perform both of these checks immediately after sampling with
all sampling train components in place. Perform all
leak-checks according to the manufacturer's instructions,
and record the results. Use the bubble-tube flowmeter to
measure the pump volume flow rate with the orifice used in
the test sampling, and record the result. If it has changed
by more than 5 but less than 20 percent, calculate an
average flow rate for the test. If the flow rate has
changed by more than 20 percent, recalibrate the pump and
repeat the sampling.
18-32 September 1996
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16.1.4.5 Calculations. All calculations can be
performed according to the respective NIOSH method. Correct
all sample volumes to standard conditions. If a sample
dilution system has been used, multiply the results by the
appropriate dilution ratio. Correct all results according
to the applicable procedure in Section 8.4. Report results
as ppm by volume, dry basis.
17.0 References.
1. American Society for Testing and Materials. Cl
Through C5 Hydrocarbons in the Atmosphere by Gas
Chromatography. ASTM D 2820-72, Part 23.
Philadelphia, Pa. 23:950-958. 1973.
2. Corazon, V.V. Methodology for Collecting and
Analyzing Organic Air Pollutants. U.S. Environmental
Protection Agency. Research Triangle Park, N.C.
Publication No. EPA-600/2-79-042. February 1979.
3. Dravnieks, A., B.K. Krotoszynski, J. Whitfield, A.
O'Donnell, and T. Burgwald. Environmental Science
and Technology. 5 (12) : 1200-1222 . 1971.
4. Eggertsen, F.T., and P.M. Nelsen. Gas
Chromatographic Analysis of Engine Exhaust and
Atmosphere. Analytical Chemistry. 30(6): 1040-1043.
1958.
5. Feairheller, W.R., P.J. Marn, D.H. Harris, and D.L.
Harris. Technical Manual for Process Sampling
Strategies for Organic Materials. U.S. Environmental
Protection Agency. Research Triangle Park, N.C.
Publication No. EPA 600/2-76-122. April 1976.
172 p.
6. Federal Register, 39 FR 9319-9323. 1974.
7. Federal Register, 39 FR 32857-32860. 1974.
8. Federal Register, 23069-23072 and 23076-23090. 1976.
9. Federal Register, 46569-46571. 1976.
18-33 September 1996
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10. Federal Register, 41771-41776. 1977.
11. Fishbein, L. Chromatography of Environmental
Hazards, Volume II. Elesevier Scientific Publishing
Company. New York, N.Y. 1973.
12. Hamersma, J.W., S.L. Reynolds, and R.F. Maddalone.
EPA/IERL-RTP Procedures Manual: Level 1
Environmental Assessment. U.S. Environmental
Protection Agency. Research Triangle Park, N.C.
Publication No. EPA 600/276-160a. June 1976.
130 p.
13. Harris, J.C., M.J. Hayes, P.L. Levins, and D.B.
Lindsay. EPA/IERL-RTP Procedures for Level 2
Sampling and Analysis of Organic Materials. U.S.
Environmental Protection Agency. Research Triangle
Park, N.C. Publication No. EPA 600/7-79-033.
February 1979. 154 p.
14. Harris, W.E., H.W. Habgood. Programmed Temperature
Gas Chromatography. John Wiley and Sons, Inc. New
York. 1966.
15. Intersociety Committee. Methods of Air Sampling and
Analysis. American Health Association. Washington,
B.C. 1972.
16. Jones, P.W., R.D. Grammer, P.E. Strup, and T.B.
Stanford. Environmental Science and Technology.
10:806-810. 1976,
17. McNair Han Bunelli, E.J. Basic Gas Chromatography.
Consolidated Printers. Berkeley. 1969.
18. Nelson, G.O. Controlled Test Atmospheres, Principles
and Techniques. Ann Arbor. Ann Arbor Science
Publishers. 1971. 247 p.
19. NIOSH Manual of Analytical Methods, Volumes 1, 2, 3,
4, 5, 6, 7. U.S. Department of Health and Human
Services, National Institute for Occupational Safety
and Health. Center for Disease Control. 4676
18-34 September 1996
-------
Columbia Parkway, Cincinnati, Ohio 45226. April 1977
- August 1981. May be available from the
Superintendent of Documents, Government Printing
Office, Washington, B.C. 20402. Stock Number/Price:
Volume 1 - 017-033-00267-3/$13
Volume 2 - 017-033-00260-6/$ll
Volume 3 - 017-033-00261-4/$14
Volume 4 - 017-033-00317-3/$7.25
Volume 5 - O17-033-00349-l/$10,
Volume 6 - 017-033-00369-6/$9,
Volume 7 - O17-033-00396-5/$7.
Prices subject to change. Foreign orders add 25 percent.
20. Schuetzle, D., T.J. Prater, and S.R. Ruddell.
Sampling and Analysis of Emissions from Stationary
Sources; I. Odor and Total Hydrocarbons. Journal of
the Air Pollution Control Association. 25(9) :
925-932. 1975.
21. Snyder, A.D., F.N. Hodgson, M.A. Kemmer and J.R.
McKendree. Utility of Solid Sorbents for Sampling
Organic Emissions from Stationary Sources. U.S.
Environmental Protection Agency. Research Triangle
Park, N.C. Publication No. EPA 600/2-76-201. July
1976. 71 p.
22. Tentative Method for Continuous Analysis of Total
Hydrocarbons in the Atmosphere. Intersociety
Committee, American Public Health Association.
Washington, D.C. 1972. p. 184-186.
23. Zwerg, G. CRC Handbook of Chromatography, Volumes I
and II. Sherma, Joseph (ed.). CRC Press.
Cleveland. 1972.
18.0 Tables, Diagrams, Flowcharts, and Validation Data.
18-35 September 1996
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I. Name of company Date
Address
Contacts Phone
Process to be sampled_
Duct or vent to be sampled
II. Process description
Raw material
Products
Operating cycle
Check: Batch Continuous Cyclic
Timing of batch or cycle
18-36 September 1996
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Best time to test
Figure 18-1. Preliminary survey data sheet.
18-37 September 1996
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III. Sampling site
A. Description
Site description
Duct shape and size
Material
Wall thickness inches
Upstream distance inches diameter
Downstream distance inches diameter
Size of port .
Size of access area
Hazards Ambient temp.
B. Properties of gas stream
Temperature °C °F, Date source_
Velocity , Data source_
Static pressure inches H2O, Data source_
Moisture content %, Data source
Particulate content , Data source
Gaseous components
N2 % Hydrocarbons ppm
02 %
CO %
CO2 %
S02 %
Hydrocarbon components
ppm
Figure 18-1 (continued) . Preliminary survey data sheet
18-38 September 1996
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C. Sampling considerations
Location to set up GC
Special hazards to be considered
Power available at duct
Power available for GC
Plant safety requirements
Vehicle traffic rules
Plant entry requirements
Security agreements
Potential problems
D. Site diagrams. (Attach additional sheets if required)
Figure 18-1 (continued). Preliminary survey data sheet.
18-39 September 1996
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Component s_to_be_analyzed
Expected_concentrat ion
Suggested chromatographic column
Column flow rate
Column temperature:
Isothermal
ml/min
Head pressure
Programmed from
'C to
3C at
Injection port/sample loop temperature
Detector temperature °C
Detector flow rates: Hydrogen
mm Hg
3C/min
Chart speed
ml/min.
head pressure mm Hg
Air/Oxygen ml/min.
head pressure mm Hg
inches/minute
Compound data:
Compound
Retention time
Attenuation
18-40
September 1996
-------
Figure 18-2. Chromatographic conditions data sheet.
18-41 September 1996
-------
Figure 18-3. Preparation of Standards in Tedlar Bags and
Calibration Curve.
Standards Preparation Data:
Organic :
Bag number or identification
Dry gas meter calibration factor
Final meter reading (liters)
Initial meter reading (liters)
Metered volume (liters)
Average meter temperature ( °K)
Average meter pressure, gauge
(mm Hg)
Average atmospheric pressure (mm
Hg)
Average meter pressure, absolute
(mm Hg)
Syringe temperature (°K)
(see Section 10.1.2.1)
Syringe pressure, absolute (mm
Hg)
(see Section 10.1.2.1)
Volume of gas in syringe (ml)
(Section 10.1.2.1)
Density of liquid organic (g/ml)
(Section 10.1.2.2)
Volume of liquid in syringe (ml)
(Section 10.1.2.2)
Standards
Mixture
#1
Mixture
#2
Mixture
#3
GC Operating Conditions:
18-42
September 1996
-------
Sample loop volume (ml)
Sample loop temperature (°C)
Carrier gas flow rate (ml/min)
Column temperature
Initial (°C)
Rate change (°C/min)
Final (°C)
Organic Peak Identification and Calculated Concentrations:
Injection time (24 hour clock)
Distance to peak (cm)
Chart speed (cm/min)
Organic retention time (min)
Attenuation factor
Peak height (mm)
Peak area (mm2)
Peak area * attenuation factor
(mm2)
Calculated concentration (ppm)
(Equation 18-3 or 18-4)
Plot peak area * attenuation factor
concentration to obtain calibration
against calculated
curve.
Figure 18-3 (continued). Standards prepared in Tedlar bags and
calibration curve.
18-43
September 1996
-------
Figure 18-4. Flowmeter Calibration.
Flowmeter number or identification
Flowmeter Type
Method: Bubble meter
Spirometer
Wet test meter
Readings at laboratory conditions:
Laboratory temperature (Tlab) _
Laboratory barometric pressure (P lab)
mm Hg
Flow data:
Flowmeter
reading (as marked)
temp. (°K)
pressure (absolute)
Calibration device
Time (min)
Gas Volume3
Flow Rateb
aVol. of gas may be measured in milliliters, liters or cubic
feet.
bConvert to standard conditions (20°C and 760 mm Hg).
18-44
September 1996
-------
Plot flowmeter reading against flow rate (standard conditions),
and draw a smooth curve. If the flowmeter being calibrated is a
rotameter or other flow device that is viscosity dependent, it
may be necessary to generate a "family" of calibration curves
that cover the operating pressure and temperature ranges of the
flowmeter.
While the following technique should be verified before
application, it may be possible to calculate flow rate reading
for rotameters at standard conditions Qstd as follows:
( 760 * TlabV/2
Qstd"Qiab I Plab x 293 I
Flow rate Flow rate
[laboratory conditions) (STD_conditions)
Figure 18-4 (continued). Flowmeter calibration.
18-45 September 1996
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Component
Gal
Cylinder
Diluent
Gai
Cylinder
Component Rotameters
With Flow Control
Velvet
CZ1
T" Connector
Tedlar Bag
Figure 18-5. Single-stage Calibration Gas Dilution System.
18-46
September 1996
-------
High
Concentration
Watte
- Needle Valves
Rotameters
Low
Concentration
Gas
Pressure
" Regulator
Pressure
Regulator
Diluent Air
Diluent Air
Pure Substance or
Pure Substance/Nitrogen Mixture
Figure 18-6. Two-Stage Dilution Apparatus.
18-47
September 1996
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Preparation of Standards by Dilution of Cylinder Standard
Cylinder Standard: Organic
Concentration ppm
Certified
Standards Preparation Data:
Stage 1
Standard gas flowmeter
reading
Diluent gas flowmeter reading
Laboratory temperature (°K)
Barometric pressure (mm Hg)
Flowmeter gage pressure (mm
Hg)
Flow rate cylinder gas at
standard conditions (ml/min)
Flow rate diluent gas at
standard conditions (ml/min)
Calculated concentration
(ppm)
Stage 2 (if used)
Standard gas flowmeter
reading
Diluent gas flowmeter reading
Flow rate Stage 1 gas at
standard conditions (ml/min)
Flow rate diluent gas at
standard conditions
Calculated concentration
(ppm)
Date:
Mixture
1
Mixture 2
Mixture 3
GC Operating
Conditions :
18-48
September 1996
-------
Sample loop volume (ml)
Sample loop temperature
(°C)
Carrier gas flow rate
(ml/min)
Column temperature :
Initial (°C)
Program rate (°C/min)
Final (°C)
Organic Peak Identification
and Calculated
Concentrations :
Injection time (24-hour
clock)
Distance to peak (cm)
Chart speed (cm/min)
Retention time (min)
Attenuation factor
Peak area (mm2)
Peak area * attenuation
factor
Plot peak area * attenuation factor against calculated
concentration to obtain calibration curve.
Figure 18-7. Standards prepared by dilution of
cylinder s tandard.
18-49
September 1996
-------
• Syringe
Tedlar Bag
Capacity
50 Liters
Nitrogen
Cylinder
Figure 18-8. Apparatus for Preparation of Liquid Materials.
18-.50
September 1996
-------
Rigid Leak-Proof
Container
Figure 18-9. Integrated Bag Sampling Train.
18-51
September 1996
-------
5' Teflon Tubing
PVC Tubing
Probe
Pinch Clamp
Grommet .
Flowmeter .
Air Tight Steel Drum
LI HJ—L_H
(Sample Bag ^
Directional
Needle Valve
Evacuated Steel
Drum
Figure 18-9a. Explosion Risk Gas Sampling Method.
18-52
September 1996
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Plant Date
Site
Sample_l Sample_2 Sample_3
Source temperature (°C)
Barometric pressure (mm Hg)
Ambient temperature (°C)
Sample flow rate (appr.)
Bag number
Start time
Finish time
Figure 18-10. Field sample data sheet - Tedlar bag
collection method.
18-53 September 1996
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Plant Date
Location
1. General information
Source temperature (°C)
Probe temperature (°C)
Ambient temperature (°C)
Atmospheric pressure (mm)
Source pressure ("Hg)
Absolute source pressure (mm)
Sampling rate (liter/min)
Sample loop volume (ml)
Sample loop temperature (°C)
Columnar temperature:
Initial (°C) time (min)
Program rate (°C/min)
Final (°C)/time (min)
Carrier gas flow rate (ml/min)
Detector temperature (°C)
Injection time (24-hour basis)
Chart speed (mm/min)
Dilution gas flow rate (ml/min)
Dilution gas used (symbol)
Dilution ratio
18-54 September 1996
-------
Figure 18-11. Field analysis data sheets.
18-55 September 1996
-------
2. Field Analysis Data - Calibration Gas
Run No.
Time
Components Area Attenuation A_x_A_Factor Conc._(ppm)
Run No.
Time
Components Area Attenuation A_x_A_Factor Conc._(ppm)
Run No.
Time
Components Area Attenuation A_x_A_Factor Conc._(ppm)
18-56
September 1996
-------
Figure 18-11 (continued). Field analysis data sheets.
18-57 September 1996
-------
Stack
Will
Figure 18-12. Direct Interface Sampling System.
18-58
September 1996
-------
Vent to Charcoal Adsorbers
Heated Box at 120'C or Source Temperature
Flowmeters
(On Outside
of Box)
Flow Rate
of
1350cc/Mln
Figure 18-13. Schematic Diagram of the Heated Box Required for Dilution
of Sample Gas.
18-59
September 1996
-------
1.
2.
Gaseous Organic Sampling and Analysis Check List
(Respond with initials or number as appropriate)
Presurvey data . _Date_
A. Grab sample collected | |
B. Grab sample analyzed for composition | |
Method GC I I
GC/MS
Other
C. GC-FID analysis performed
Laboratory calibration data
A. Calibration curves prepared
Number of components
Number of concentrations/
component (3 required)
B. Audit samples (optional)
Analysis completed
Verified for concentration
OK obtained for field work
3. Sampling procedures
A. Method
Bag sample
Direct interface
Dilution interface
B. Number of samples collected
4. Field Analysis
A. Total hydrocarbon analysis performed
18-60
September 1996
-------
B. Calibration curve prepared
Number of components
Number of concentrations per
component (3 required)
18-61 September 1996
-------
Gaseous Organic Sampling and Analysis Data
Plant
Date
Location
Source Source Source
sample_l sample_2 sample_3
1. General information
Source temperature (°C)
Probe temperature (°C)
Ambient temperature (°C)
Atmospheric pressure (mm Hg)
Source pressure (mm Hg)
Sampling rate (ml/min)
Sample loop volume (ml)
Sample loop temperature (°C)
Sample collection time
(24-hr basis)
Column temperature
Initial (°C)
Program rate (°C/min)
Final (°C)
Carrier gas flow rate (ml/min)
Detector temperature (°C) _
Chart speed (cm/min) _
Dilution gas flow rate
(ml/min)
Diluent gas used (symbol)
Dilution ratio
Performed by:
(signature) : Date:
Figure 18-14. Sampling and analysis sheet.
18-62 September 1996
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APPENDIX F.6
EPA METHOD 315
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APPENDIX A TO PART 63-TEST METHODS
*****
METHOD 315 - DETERMINATION OF PARTICULATE AND METHYLENE CHLORIDE
EXTRACTABLE MATTER (MCE\f> FROM SELECTED SOURCES
AT PRIMARY ALUMINUM PRODUCTION FACILITIES
NOTE: This method does not include all of die specifications (e.g., equipment and supplies) and
procedures (e.g., sampling and analytical) essential to its performance. Some material is incorporated by
reference from other methods in this part Therefore, to obtain reliable results, persons using this method
should have a thorough knowledge of at least the following additional test methods: Method 1, Method
2, Method 3, and Method 5 of 40 CFR part 60, appendix A.
l.Q Scope and Application.
1.1 Analytes. Particulate matter (PM). No CAS number assigned. Methylene chloride
extractable matter (MCEM). No CAS number assigned.
1.2 Applicability. This method is applicable for the simultaneous determination of PM and
MCEM when specified in an applicable regulation. This method was developed by consensus with the
Aluminum Association and the U.S. Environmental Protection Agency (EPA) and has limited precision
estimates for MCEM; it should have similar precision to Method 5 for PM in 40 CFR part 60, appendix
A since the procedures are similar for PM.
1.3 Data quality objectives. Adherence to the requirements of this method will enhance the
quality of the data obtained from air pollutant sampling methods.
2.0 Summary of Method.
Particulate matter and MCEM are withdrawn isokinetically from the source. PM is collected on
a glass fiber filter maintained at a temperature in the range of 120 ± 14°C (248 ± 25°F) or such other
temperature as specified by an applicable subpart of the standards or approved by the Administrator for a
particular application. The PM mass, which includes any material that condenses on the probe and is
subsequently removed in an acetone rinse or on the filter at or above the filtration temperature, is
determined gravimetrically after removal of uncombined water. MCEM is then determined by adding a
methylene chloride rinse of the probe and filter holder, extracting the condensable hydrocarbons
collected in the impinger water, adding an acetone rinse followed by a methylene chloride rinse of the
sampling train components after the filter and before the silica gel impinger, and determining residue
gravimetrically after evaporating the solvents.
3.0 Definitions. [Reserved]
4.0 Interferences. [Reserved]
5.0 Safety.
This method may involve hazardous materials, operations, and equipment. This method does not
purport to address all of the safety problems associated with its use. It is the responsibility of the user of
this method to establish appropriate safety and health practices and determine the applicability of
regulatory limitations prior to performing this test method.
6.0 Equipment and Supplies.
NOTE: Mention of trade names or specific products does not constitute endorsement by the
EPA.
6.1 Sample collection. The following items are required for sample collection:
6.1.1 Sampling train. A-schematic of the sampling train used in this method is shown in Figure
5-1, Method 5,40 CFR part 60, appendix A. Complete construction details are given in APTD-0581
(Reference 2 in section 17.0 of this method); commercial models of this train are also available. For
changes from APTD-0581 and for allowable modifications of the train shown in Figure 5-1, Method 5,40
CFR part 60, appendix, A see the following subsections.
NJ2IE: The operating and maintenance procedures for the sampling train are described in
APTD-0576 (Reference 3 in section 17.0 of this method). Since correct usage is important in obtaining
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valid results, all users should read APTD-0576 and adopt the operating and maintenance procedures
outlined in it, unless otherwise specified herein. The use of grease for sealing sampling train components
is not recommended because many greases are soluble in methylene chloride. The sampling train
consists of die following components:
6.1.1.1 Probe nozzle. Glass or glass lined with sharp, tapered leading edge. The angle of taper
shall be s30°, and the taper shall be on the outside to preserve a constant internal diameter. The probe
nozzle shall be of the button-hook or elbow design, unless otherwise specified by the Administrator.
Other materials of construction may be used, subject to the approval of the Administrator. A range of
nozzle sizes suitable for isokinetic sampling should be available. Typical nozzle sizes range from 0.32 to
1.27 cm (1/8 to 1/2 in.) inside diameter (ID) in increments of 0.16 cm (1/16 in.). Larger nozzle sizes are
also available if higher volume sampling trains are used. Each nozzle shall be calibrated according to the
procedures outlined in section 10.0 of this method.
6.1.1.2 Probe liner. Borosilicate or quartz glass tubing with a heating system capable of
maintaining a probe gas temperature at the exit end during sampling of 120 ± 14°C (248 ± 25°F), or such
other temperature as specified by an applicable subpart of the standards or approved by the
Administrator for a particular application. Because the actual temperature at the outlet of the probe is
not usually monitored during sampling, probes constructed according to APTD-0581 and using the
calibration curves of APTD-0576 (or calibrated according to the procedure outlined in APTD-0576) will
be considered acceptable. Either borosilicate or quartz glass probe liners may be used for stack
temperatures up to about 480°C (900°F); quartz liners shall be used for temperatures between 480 and
900°C (900 and 1,650°F). Both types of liners may be used at higher temperatures than specified for
short periods of time, subject to the approval of the Administrator. The softening temperature for
borosilicate glass is 820°C (1,500°F) and for quartz glass it is 1,500°C (2,700°F).
6.1.1.3 Pitot tube. Type S, as described in section 6.1 of Method 2,40 CFR part 60, appendix A,
or other device approved by the Administrator. The pitot tube shall be attached to the probe (as shown in
Figure 5-1 of Method 5, 40 CFR part 60, appendix A) to allow constant monitoring of the stack gas
velocity. The impact (high pressure) opening plane of the pitot tube shall be even with or above the
nozzle entry plane (see Method 2, Figure 2-6b, 40 CFR part 60, appendix A) during sampling. The Type
S pitot tube assembly shall have a known coefficient, determined as outlined in section 10.0 of Method 2,
40 CFR part 60, appendix A.
6.1.1.4 Differential pressure gauge. Inclined manometer or equivalent device (two), as described
in section 6.2 of Method 2,40 CFR part 60, appendix A. One manometer shall be used for velocity head
(Dp) readings, and the other, for orifice differential pressure readings.
6.1.1.5 Filter holder. Borosilicate glass, with a glass frit filter support and a silicone rubber
gasket. The holder design shall provide a positive seal against leakage from the outside or around the
filter. The holder shall be attached immediately at the outlet of the probe (or cyclone, if used).
6.1.1.6 Filter heating system. Any heating system capable of maintaining a temperature around
the filter holder of 120 ± 14°C (248 ± 25°F) during sampling, or such other temperature as specified by an
applicable subpart of the standards or approved by the Administrator for a particular application.
Alternatively, the tester may opt to operate the equipment at a temperature lower than that specified. A
temperature gauge capable of measuring temperature to within 3°C (5.4°F) shall be installed so that the
temperature around the filter holder can be regulated and monitored during sampling. Heating systems
other than the one shown in APTD-0581 may be used.
6.1.1.7 Temperature sensor. A temperature sensor capable of measuring temperature to within
±3 °C (5.4°F) shall be installed so that the sensing tip of the temperature sensor is in direct contact with
the sample gas, and the temperature around the filter holder can be regulated and monitored during
sampling.
6.1.1.8 Condenser. The following system shall be used to determine the stack gas moisture
content: four glass impingers connected in series with leak-free ground glass fittings. The first, third,
-------
and fourth impingers shall be of the Greenburg-Smith design, modified by replacing the tip with a 13 cm
(1/2 in.) ID glass tube extending to about 1.3 cm (1/2 in.) from the bottom of die flask. The second
impinger shall be of the Greenburg-Smith design with the standard tip. The first and second impingers
shall contain known quantities of water (section 8.3.1 of this method), the third shall be empty, and the
fourth shall contain a known weight of silica gel or equivalent desiccant A temperature sensor capable
of measuring temperature to within 1°C (2°F) shall be placed at the outlet of the fourth impinger for
monitoring.
6.1.1.9 Metering system. Vacuum gauge, leak-free pump, temperature sensors capable of
measuring temperature to within 3°C (5.4°F), dry gas meter (DGM) capable of measuring volume to
within 2 percent, and related equipment, as shown in Figure 5-1 of Method 5,40 CFR part 60, appendix
A. Other metering systems capable of maintaining sampling rates within 10 percent of isokinetic and of
determining sample volumes to within 2 percent may be used, subject to the approval of the
Administrator. When the metering system is used in conjunction with a pitot tube, the system shall allow
periodic checks of isokinetic rates.
6.1.1.10 Sampling trains using metering systems designed for higher flow rates than mat
described in APTD-0581 or APTD-0576 may be used provided that the specifications of this method are
met
6.1.2 Barometer. Mercury, aneroid, or other barometer capable of measuring atmospheric
pressure to within 2.5 mm (0.1 in.) Hg.
NOTE: The barometric reading may be obtained from a nearby National Weather Service
station. In this case, the station value (which is the absolute barometric pressure) shall be requested and
an adjustment for elevation differences between the weather station and sampling point shall be made at
a rate of minus 2.5 mm (0.1 in) Hg per 30 m (100 ft) elevation increase or plus 2.5 mm (0.1 in) Hg per 30
m (100 ft) elevation decrease.
6.1.3 Gas density determination equipment Temperature sensor and pressure gauge, as
described in sections 6.3 and 6.4 of Method 2,40 CFR part 60, appendix A, and gas analyzer, if
necessary, as described in Method 3,40 CFR part 60, appendix A. The temperature sensor shall,
preferably, be permanently attached to the pitot tube or sampling probe in a fixed configuration, such mat
the tip of the sensor extends beyond the leading edge of the probe sheath and does not touch any metal.
Alternatively, the sensor may be attached just prior to use in the field. Note, however, that if the
temperature sensor is attached in the field, the sensor must be placed in an interference-free arrangement
with respect to the Type S pitot tube openings (see Method 2, Figure 2-4,40 CFR part 60, appendix A).
As a second alternative, if a difference of not more than 1 percent in the average velocity measurement is
to be introduced, the temperature sensor need not be attached to the probe or pitot tube. (This alternative
is subject to the approval of the Administrator.)
6.2 Sample recovery. The following items are required for sample recovery:
6.2.1 Probe-liner and probe-nozzle brushes. Nylon or Teflon® bristle brushes with stainless
steel wire handles. The probe brush shall have extensions (at least as long as the probe) constructed of
stainless steel, nylon, Teflon®, or similarly inert material. The brushes shall be properly sized and
shaped to brush out the probe liner and nozzle.
6.2.2 Wash bottles. Glass wash bottles are recommended. Polyethylene or tetrafluoroethylene
(TFE) wash bottles may be used, but they may introduce a positive bias due to contamination from the
bottle. It is recommended that acetone not be stored in polyethylene or TFE bottles for longer than a
month.
6.2.3 Glass sample storage containers. Chemically resistant, borosilicate glass bottles, for
acetone and methylene chloride washes and impinger water, 500 ml or 1,000 ml. Screw-cap liners shall
either be rubber-backed Teflon® or shall be constructed so as to be leak-free and resistant to chemical
attack by acetone or methylene chloride. (Narrow-mouth glass bottles have been found to be less prone
to leakage.) Alternatively, polyethylene bottles may be used.
6.2.4 Petri dishes. For filter samples, glass, unless otherwise specified by the Administrator.
6.2.5 Graduated cylinder and/or balance. To measure condensed water, acetone wash and
-------
methylene chloride wash used during field recovery of the samples, to within 1 ml or 1 g. Graduated
cylinders shall have subdivisions no greater than 2 ml. Most laboratory balances are capable of weighing
to the nearest 0.5 g or less. Any such balance is suitable for use here and in section 6.3.4 of this method.
6.2.6 Plastic storage containers. Air-tight containers to store silica gel.
6.2.7 Funnel and rubber policeman. To aid in transfer of silica gel to container; not necessary if
silica gel is weighed in the field.
6.2.8 Funnel. Glass or polyethylene, to aid in sample recovery.
6.3 Sample analysis. The following equipment is required for sample analysis:
6.3.1 Glass or Teflon® weighing dishes.
6.3.2 Desiccator. It is recommended that fresh desiccant be used to minimize the chance for
positive bias due to absorption of organic material during drying.
6.3.3 Analytical balance. To measure to within 0.1 mg.
6.3.4 Balance. To measure to within 0.5 g.
6.3.5 Beakers. 250ml.
6.3.6 Hygrometer. To measure the relative humidity of the laboratory environment.
' * ' 6.3.7 Temperature sensor. To measure the temperature of the laboratory environment
6.3.8 Buchner fritted funnel. 30 ml size, fine (<50 micron)-porosity fritted glass.
6.3.9 Pressure filtration apparatus.
6.3.10 Aluminum dish. Flat bottom, smooth sides, and flanged top, 18 mm deep and with an
inside diameter of approximately 60 mm.
7.0 Reagents and Standards.
7.1 Sample collection. The following reagents are required for sample collection:
7.1.1 Filters. Glass fiber filters, without organic binder, exhibiting at least 99.95 percent
efficiency (<0.05 percent penetration) on 03 micron dioctyl phthalate smoke particles. The filter
efficiency test shall be conducted in accordance with ASTM Method D 2986-95A (incorporated by
reference in § 63.841 of this part). Test data from the supplier's quality control program are sufficient for
this purpose. In sources containing S02 or S03, the filter material must be of a type that is unreactive to
S02 or S03. Reference 10 in section 17.0 of this method may be used to select the appropriate filter.
7.1.2 Silica gel. Indicating type, 6 to 16 mesh. If previously used, dry at 175°C (350°F) for 2
hours. New silica gel may be used as received. Alternatively, other types of desiccants (equivalent or
better) may be used, subject to the approval of the Administrator.
7.1.3 Water. When analysis of the material caught in the impingers is required, deionized
distilled water shall be used. Run blanks prior to field use to eliminate a high blank on test samples.
7.1.4 Crushed ice.
7.1.5 Stopcock grease. Acetone-insoluble, heat-stable silicone grease. This is not necessary if
screw-on connectors with Teflon® sleeves, or similar, are used. Alternatively, other types of stopcock
grease may be used, subject to the approval of the Administrator. [Caution: Many stopcock greases are
methylene chloride-soluble. Use sparingly and carefully remove prior to recovery to prevent
contamination of the MCEM analysis.]
7.2 Sample recovery. The following reagents are required for sample recovery:
7.2.1 Acetone. Acetone with blank values < 1 ppm, by weight residue, is required. Acetone
blanks may be run prior to field use, and only acetone with low blank values may be used. In no case
shall a blank value of greater than 1E-06 of the weight of acetone used be subtracted from the sample
weight
NOTE: This is more restrictive than Method 5,40 CFR part 60, appendix A. At least one
vendor (Supelco Incorporated located in Bellefonte, Pennsylvania) lists <1 mg/1 as residue for its
Environmental Analysis Solvents.
7.2.2 Methylene chloride. Methylene chloride with a blank value <1.5 ppm, by weight, residue.
Methylene chloride blanks may be run prior to field use, and only methylene chloride with low blank
values may be used. In no case shall a blank value of greater than 1.6E-06 of the weight of methylene
chloride used be subtracted from the sample weight.
-------
NOTE: A least one vendor quotes <1 mg/1 for Environmental Analysis Solvents-grade
methylene chloride.
7.3 Sample analysis. The following reagents are required for sample analysis:
7.3.1 Acetone. Same as in section 7.2.1 of this method.
7.3.2 Desiccant Anhydrous calcium sulfate, indicating type. Alternatively, other types of
desiccants may be used, subject to the approval of the Administrator.
7.3.3 Methylene chloride. Same as in section 7.2.2 of this method.
8.0 Sample Collection. Preservation. Storage, and Transport.
NOTE: The complexity of this method is such that, in order to obtain reliable results, testers
should be trained and experienced with the test procedures.
8.1 Pretest preparation. It is suggested that sampling equipment be maintained according to the
procedures described in APTD-0576.
8.1.1 Weigh several 200 g to 300 g portions of silica gel in airtight containers to the nearest 0.5
g. Record on each container the total weight of the silica gel plus container. As an alternative, the silica
gel need not be preweighed but may be weighed directly in its impinger or sampling holder just prior to
train assembly.
8.1.2 A batch of glass fiber filters, no more than SO at a time, should placed in a soxhlet
extraction apparatus and extracted using methylene chloride for at least 16 hours. After extraction, check
filters visually against light for irregularities, flaws, or pinhole leaks. Label the shipping containers
(glass or plastic petri dishes), and keep the filters in these containers at all times except during sampling
and weighing.
8.1.3 Desiccate the filters at 20 ± 5.6°C (68 ± 10°F) and ambient pressure for at least 24 hours
and weigh at intervals of at least 6 hours to a constant weight, i.e., <0.5 mg change from previous
weighing; record results to the nearest 0.1 mg. During each weighing the filter must not be exposed to
the laboratory atmosphere for longer than 2 minutes and a relative humidity above SO percent
Alternatively (unless otherwise specified by the Administrator), the filters may be oven-dried at 104°C
(220°F) for 2 to 3 hours, desiccated for 2 hours, and weighed. Procedures other than those described,
which account for relative humidity effects, may be used, subject to the approval of the Administrator.
8.2 Preliminary determinations.
8.2.1 Select the sampling site and the minimum number of sampling points according to Method
1,40 CFR part 60, appendix A or as specified by the Administrator. Determine the stack pressure,
temperature, and the range of velocity heads using Method 2,40 CFR part 60, appendix A; it is
recommended that a leak check of the phot lines (see section 8.1 of Method 2,40 CFR part 60, appendix
A) be performed. Determine the moisture content using Approximation Method 4 (section 1.2 of
Method 4,40 CFR part 60, appendix A) or its alternatives to make isokinetic sampling rate settings.
Determine the stack gas dry molecular weight, as described in section 8.6 of Method 2,40 CFR part 60,
appendix A; if integrated Method 3 sampling is used for molecular weight determination, the integrated
bag sample shall be taken simultaneously with, and for the same total length of time as, the particulate
sample run.
8.2.2 Select a nozzle size based on the range of velocity heads such that it is not necessary to
change the nozzle size in order to maintain isokinetic sampling rates. During the run, do not change the
nozzle size. Ensure that the proper differential pressure gauge is chosen for the range of velocity heads
encountered (see section 8.2 of Method 2,40 CFR part 60, appendix A).
8.2.3 Select a suitable probe liner and probe length such that all traverse points can be sampled.
For large stacks, consider sampling from opposite sides of the stack to reduce the required probe length.
8.2.4 Select a total sampling time greater than or equal to the minimum total sampling time
specified in the test procedures for the specific industry such that: (1) The sampling time per point is not
less than 2 minutes (or some greater time interval as specified by the Administrator); and (2) the sample
volume taken (corrected to standard conditions) will exceed the required minimum total gas sample
volume. The latter is based on an approximate average sampling rate.
8.2.S The sampling time at each point shall be the same. It is recommended that the number of
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minutes sampled at each point be an integer or an integer plus one-half minute, in order to eliminate
timekeeping errors.
8.2.6 In some circumstances (e.g., batch cycles), it may be necessary to sample for shorter times
at the traverse points and to obtain smaller gas sample volumes. In these cases, the Administrator's
approval must first be obtained.
8.3 Preparation of sampling train.
8.3.1 During preparation and assembly of the sampling train, keep all openings where
contamination can occur covered until just prior to assembly or until sampling is about to begin. Place
100 ml of water in each of the first two impingers, leave the third impinger empty, and transfer
approximately 200 to 300 g of preweighed silica gel from its container to the fourth impinger. More
silica gel may be used, but care should be taken to ensure that it is not entrained and carried out from the
impinger during sampling. Place the container in a clean place for later use in the sample recovery.
Alternatively, the weight of the silica gel plus impinger may be determined to the nearest 0.5 g and
recorded.
8.3.2 Using a tweezer or clean disposable surgical gloves, place a labeled (identified) and
weighed filter in the filter holder. Be sure that the filter is properly centered and the gasket properly
placed so as to prevent the sample gas stream from circumventing the filter. Check the filter for tears
after assembly is completed.
8.3.3 When glass liners are used, install the selected nozzle using a Viton A 0-ring when stack
temperatures are less than 260°C (SOOT) and an asbestos string gasket when temperatures are higher.
See APTD-0576 for details. Mark the probe with heat-resistant tape or by some other method to denote
the proper distance into the stack or duct for each sampling point
8.3.4 Set up the train as in Figure 5-1 of Method 5, 40 CFR part 60, appendix A, using (if
necessary) a very light coat of silicone grease on all ground glass joints, greasing only the outer portion
(see APTD-0576) to avoid possibility of contamination by the silicone grease. Subject to the approval of
the Administrator, a glass cyclone may be used between the probe and filter holder when the total
particulate catch is expected to exceed 100 mg or when water droplets are present in the stack gas.
8.3.5 Place crushed ice around the impingers.
8.4 Leak-check procedures.
8.4.1 Leak check of metering system shown in
Figure 5-1 of Method 5,40 CFR part 60, appendix A. That portion of the sampling train from the pump
to the orifice meter should be leak-checked prior to initial use and after each shipment Leakage after the
pump will result in less volume being recorded than is actually sampled. The following procedure is
suggested (see Figure 5-2 of Method 5,40 CFR part 60, appendix A): Close die main valve on the meter
box. Insert a one-hole rubber stopper with rubber tubing attached into the orifice exhaust pipe.
Disconnect and vent the low side of the orifice manometer. Close off the low side orifice tap. Pressurize
the system to 13 to 18 cm (5 to 7 in.) water column by blowing into the rubber tubing. Pinch off the
tubing, and observe the manometer for 1 minute. A loss of pressure on the manometer indicates a leak in
the meter box; leaks, if present, must be corrected.
8.4.2 Pretest leak check. A pretest leak-check is recommended but not required. If the pretest
leak-check is conducted, the following procedure should be used.
8.4.2.1 After the sampling train has been assembled, turn on and set the filter and probe heating
systems to the desired operating temperatures. Allow time for the temperatures to stabilize. If a Viton A
0-ring or other leak-free connection is used in assembling the probe nozzle to the probe liner, leak-check
the train at the sampling site by plugging the nozzle and pulling a 380 mm (15 in.) Hg vacuum.
NOTE: A lower vacuum may be used, provided that it is not exceeded during the test.
8.4.2.2 If an asbestos string is used, do not connect the probe to the train during the leak check.
Instead, leak-check the train by first plugging the inlet to the filter holder (cyclone, if applicable) and
pulling a 380 mm (15 in.) Hg vacuum. (See NOTE in section 8.4.2.1 of this method). Then connect the
probe to the train and perform the leak check at approximately 25 mm (1 in.) Hg vacuum; alternatively,
the probe may be leak-checked with the rest of the sampling train, in one step, at 380 mm (15 in.) Hg
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vacuum. Leakage rates in excess of 4 percent of the average sampling rate or 0.00057 mVmin (0.02
cfm), whichever is less, are unacceptable.
8.4.2.3 The following leak check instructions for the sampling train described in APTD-0576
and APTD-0581 may be helpful. Start the pump with the bypass valve fully open and the coarse adjust
valve completely closed. Partially open the coarse adjust valve and slowly close the bypass valve until
the desired vacuum is reached. Do not reverse the direction of the bypass valve, as this will cause water
to back up into the filter holder. If the desired vacuum is exceeded, either leak-check at this higher
vacuum or end the leak check as shown below and start over.
8.4.2.4 When the leak check is completed, first slowly remove the plug from the inlet to the
probe, filter holder, or cyclone (if applicable) and immediately turn off the vacuum pump. This prevents
the water in the impingers from being forced backward into the filter holder and the silica gel from being
entrained backward into the third impinger.
8.4.3 Leak checks during sample run. If, during the sampling run, a component (e.g., filter
assembly or impinger) change becomes necessary, a leak check shall be conducted immediately before
the change is made. The leak check shall be done according to the procedure outlined in section 8.4.2 of
this method, except that it shall be done at a vacuum equal to or greater than the maximum value
recorded up to that point in the test. If the leakage rate is found to be no greater than 0.00057 mVmin
(0.02 cfm) or 4 percent of the average sampling rate (whichever is less), the results are acceptable, and
no correction will need to be applied to the total volume of dry gas metered; if, however, a higher
leakage rate is obtained, either record the leakage rate and plan to correct the sample volume as shown in
section 12.3 of this method or void the sample run.
NOTE: Immediately after component changes, leak checks are optional; if such leak checks are
done, the procedure outlined in section 8.42 of this method should be used.
8.4.4 Post-test leak check. A leak check is mandatory at the conclusion of each sampling run.
The leak check shall be performed in accordance with the procedures outlined in section 8.4.2 of this
method, except that it shall be conducted at a vacuum equal to or greater than the maximum value
reached during the sampling run. If the leakage rate is found to be no greater than 0.00057 nrVmin
(0.02 cfm) or 4 percent of the average sampling rate (whichever is less), the results are acceptable, and
no correction need be applied to the total volume of dry gas metered. If, however, a higher leakage rate
is obtained, either record the leakage rate and correct the sample volume, as shown in section 12.4 of this
method, or void the sampling run.
8.5 Sampling train operation. During the sampling run, maintain an isokinetic sampling rate
(within 10 percent of true isokinetic unless otherwise specified by the Administrator) and a temperature
around the filter of 120 ± 14°C (248 ± 25°F), or such other temperature as specified by an applicable
subpart of the standards or approved by the Administrator.
8.5.1 For each run, record the data required on a data sheet such as the one shown in Figure 5-2
of Method 5,40 CFR part 60, appendix A. Be sure to record the initial reading. Record the DGM
readings at the beginning and end of each sampling time increment, when changes in flow rates are
made, before and after each leak-check, and when sampling is halted. Take other readings indicated by
Figure 5-2 of Method 5,40 CFR part 60, appendix A at least once at each sample point during each time
increment and additional readings when significant changes (20 percent variation in velocity head
readings) necessitate additional adjustments in flow rate. Level and zero the manometer. Because the
manometer level and zero may drift due to vibrations and temperature changes, make periodic checks
during the traverse.
8.5.2 Clean the portholes prior to the test run to minimize the chance of sampling deposited
material. To begin sampling, remove the nozzle cap and verify that the filter and probe heating systems
are up to temperature and that the pitot tube and probe are properly positioned. Position the nozzle at the
first traverse point with the tip pointing directly into the gas stream. Immediately start the pump and
adjust the flow to isokinetic conditions. Nomographs are available, which aid in the rapid adjustment of
the isokinetic sampling rate without excessive computations. These nomographs are designed for use
when the Type S pitot tube coefficient (Cp) is 0.85 ± 0.02 and the stack gas equivalent density (dry
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molecular weight) is 29 ± 4. APTD-0576 details the procedure for using the nomographs. If Cp and Mj
are outside the above-stated ranges, do not use the nomographs unless appropriate steps (see Reference 7
in section 17.0 of this method) are taken to compensate for the deviations.
8.S.3 When the stack is under significant negative pressure (height of impinger stem), close the
coarse adjust valve before inserting the probe into the stack to prevent water from backing into the filter
holder. If necessary, the pump may be turned on with the coarse adjust valve closed.
8.S.4 When the probe is in position, block off the openings around the probe and porthole to
prevent unrepresentative dilution of the gas stream.
8.5.5 Traverse the stack cross-section, as required by Method 1,40 CFR part 60, appendix A or
as specified by the Administrator, being careful not to bump the probe nozzle into the stack walls when
sampling near the walls or when removing or inserting the probe through the portholes; this minimizes
the chance of extracting deposited material.
8.5.6 During the test run, make periodic adjustments to keep the temperature around the filter
holder at the proper level; add more ice and, if necessary, salt to maintain a temperature of less man 20°C
(68°F) at the condenser/silica gel outlet. Also, periodically check the level and zero of the manometer.
8.5.7 If the pressure drop across the filter becomes too high, making isokinetic sampling
difficult to maintain, the filter may be replaced in the midst of the sample run. It is recommended mat
another complete filter assembly be used rather than attempting to change the filter itself. Before a new
filter assembly is installed, conduct a leak check (see section 8.4.3 of this method). The total PM weight
shall include the summation of the filter assembly catches.
8.5.8 A single train shall be used for the entire sample run, except in cases where simultaneous
sampling is required in two or more separate ducts or at two or more different locations within the same
duct, or in cases where equipment failure necessitates a change of trains. In all other situations, the use
of two or more trains will be subject to the approval of the Administrator.
NOTE: When two or more trains are used, separate analyses of the front-half and (if applicable)
impinger catches from each train shall be performed, unless identical nozzle sizes were used in all trains,
in which case the front-half catches from the individual trains may be combined (as may the impinger
catches) and one analysis of the front-half catch and one analysis of the impinger catch may be
performed.
8.5.9 At the end of the sample run, turn off the coarse adjust valve, remove the probe and nozzle
from the stack, turn off the pump, record the final DGM reading, and then conduct a post-test leak check,
as outlined in section 8.4.4 of this method. Also leak-check the pitot lines as described in section 8.1 of
Method 2,40 CFR part 60, appendix A. The lines must pass this leak check in order to validate the
velocity head data.
8.6 Calculation of percent isokinetic. Calculate percent isokinetic (see Calculations, section
12.12 of this method) to determine whether a run was valid or another test run should be made. If there
was difficulty in maintaining isokinetic rates because of source conditions, consult the Administrator for
possible variance on the isokinetic rates.
8.7 Sample recovery.
8.7.1 Proper cleanup procedure begins as soon as the probe is removed from the stack at the end
of the sampling period. Allow the probe to cool.
8.7.2 When the probe can be safely handled, wipe off all external PM near the tip of the probe
nozzle and place a cap over it to prevent losing or gaining PM. Do not cap off the probe tip tightly while
the sampling train is cooling down. This would create a vacuum in the filter holder, thus drawing water
from the impingers into the filter holder.
8.7.3 Before moving the sample train to the cleanup site, remove the probe from the sample
train, wipe off the silicone grease, and cap the open outlet of the probe. Be careful not to lose any
condensate that might be present. Wipe off the silicone grease from the filter inlet where the probe was
fastened and cap it. Remove the umbilical cord from the last impinger and cap the impinger. If a
flexible line is used between the first impinger or condenser and the filter holder, disconnect the line at
the filter holder and let any condensed water or liquid drain into the impingers or condenser. After
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wiping off the silicone grease, cap off the filter holder outlet and impinger inlet Ground-glass stoppers,
plastic caps, or serum caps may be used to close these openings.
8.7.4 Transfer the probe and filter-impinger assembly to the cleanup area. This area should be
clean and protected from the wind so that the chances of contaminating or losing the sample will be
minimized.
8.7.5 Save a portion of the acetone and methylene chloride used for cleanup as blanks. Take
200 ml of each solvent directly from the wash bottle being used and place it in glass sample containers
labeled "acetone blank" and "methylene chloride blank," respectively.
8.7.6 Inspect the train prior to and during disassembly and note any abnormal conditions. Treat
the samples as follows:
8.7.6.1 Container No. 1. Carefully remove the filter from the filter holder, and place it in its
identified petri dish container. Use a pair of tweezers and/or clean disposable surgical gloves to handle
the filter. If it is necessary to fold the filter, do so such that the PM cake is inside the fold. Using a dry
nylon bristle brush and/or a sharp-edged blade, carefully transfer to the petri dish any PM and/or filter
fibers that adhere to the filter holder gasket. Seal the container.
8.7.6.2 Container No. 2. Taking care to see that dust on the outside of the probe or other
exterior surfaces does not get into the sample, quantitatively recover PM or any condensate from the
probe nozzle, probe fitting, probe liner, and front half of the filter holder by washing these components
with acetone and placing the wash in a glass container. Perform the acetone rinse as follows:
8.7.6.2.1 Carefully remove the probe nozzle and clean the inside surface by rinsing with acetone
from a wash bottle and brushing with a nylon bristle brush. Brush until the acetone rinse shows no
visible particles, after which make a final rinse of the inside surface with acetone.
8.7.6.2.2 Brush and rinse the inside parts of the Swagelok fitting with acetone in a similar way
until no visible particles remain.
8.7.6.2.3 Rinse the probe liner with acetone by tilting and rotating the probe while squirting
acetone into its upper end so that all inside surfaces are wetted with acetone. Let the acetone drain from
the lower end into the sample container. A runnel (glass or polyethylene) may be used to aid in
transferring liquid washes to the container. Follow the acetone rinse with a probe brush. Hold the probe
in an inclined position, squirt acetone into the upper end as the probe brush is being pushed with a
twisting action through the probe, hold a sample container under the lower end of the probe, and catch
any acetone and PM that is brushed from the probe. Run the brush through the probe three times or more
until no visible PM is carried out with the acetone or until none remains in the probe liner on visual
inspection. With stainless steel or other metal probes, run the brush through in the above-described
manner at least six times, since metal probes have small crevices in which PM can be entrapped. Rinse
the brush with acetone and quantitatively collect these washings in the sample container. After the
brushing, make a final acetone rinse of the probe as described above.
8.7.6.2.4 It is recommended that two people clean the probe to minimize sample losses.
Between sampling runs, keep brushes clean and protected from contamination.
8.7.6.2.5 After ensuring that all joints have been wiped clean of silicone grease, clean the inside
of the front half of the filter holder by rubbing the surfaces with a nylon bristle brush and rinsing with
acetone. Rinse each surface three times or more if needed to remove visible particulate. Make a final
rinse of the brush and filter holder. Carefully rinse out the glass cyclone also (if applicable).
8.7.6.2.6 After rinsing the nozzle, probe, and front half of the filter holder with acetone, repeat
the entire procedure with methylene chloride and save in a separate No. 2M container.
8.7.6.2.7 After acetone and methylene chloride washings and PM have been collected in the
proper sample containers, tighten the lid on the sample containers so that acetone and methylene chloride
will not leak out when it is shipped to the laboratory. Mark the height of the fluid level to determine
whether leakage occurs during transport. Label each container to identify clearly its contents.
8.7.6.3 Container No. 3. Note the color of the indicating silica gel to determine whether it has
been completely spent, and make a notation of its condition. Transfer the silica gel from the fourth
impinger to its original container and seal the container. A funnel may make it easier to pour the silica
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gel without spilling. A rubber policeman may be used as an aid in removing the silica gel from the
impinger. It is not necessary to remove the small amount of dust particles that may adhere to the
impinger wall and are difficult to remove. Since the gain in weight is to be used for moisture
calculations, do not use any water or other liquids to transfer the silica gel. If a balance is available in
the field, follow the procedure for Container No. 3 in section 112.3 of this method.
8.7.6.4 Impinger water. Treat the impingers as follows:
8.7.6.4.1 Make a notation of any color or film in the liquid catch. Measure the liquid mat is in
the first three impingers to within 1 ml by using a graduated cylinder or by weighing it to within 0.5 g by
using a balance (if one is available). Record the volume or weight of liquid present This information is
required to calculate the moisture content of the effluent gas.
8.7.6.4.2 Following the determination of the volume of liquid present, rinse the back half of the
train with water, add it to the impinger catch, and store it in a container labeled 3 W (water).
8.7.6.4.3 Following the water rinse, rinse the back half of the train with acetone to remove the
excess water to enhance subsequent organic recovery with methylene chloride and quantitatively recover
to a container labeled 3S (solvent) followed by at least three sequential rinsings with aliquots of
methylene chloride. Quantitatively recover to the same container labeled 3S. Record separately the
amount of both acetone and methylene chloride used to the nearest 1 ml or O.Sg.
NOTE: Because the subsequent analytical finish is gravimetric, it is okay to recover both
solvents to the same container. This would not be recommended if other analytical finishes were
required.
8.8 Sample transport. Whenever possible, containers should be shipped in such a way that they
remain upright at all times.
9.0 Quality Control.
9.1 Miscellaneous quality control measures.
Section Quality Control Measure Effect
8.4, Sampling and equipment Ensure accurate
10.1-10.6 leak check and calibration measurement of
stack gas flow rate,
sample volume
9.2 Volume metering system checks. The following quality control procedures are suggested to
check the volume metering system calibration values at the field test site prior to sample collection.
These procedures are optional.
9.2.1 Meter orifice check. Using the calibration data obtained during the calibration procedure
described in section 10.3 of this method, determine the AH@ for the metering system orifice. The AH@ is
the orifice pressure differential in units of in. H20 that correlates to 0.75 cfm of air at 528°R and 29.92 in.
Hg. The AH@ is calculated as follows:
= 0.0319 AH m
P Y2 V2
rbar J vm
where
0.0319 =(0.0567 in. Hg/°RX0.75 cfm)2;
AH = Average pressure differential across the orifice meter, in. H20;
T., =. Absolute average DGM temperature, °R;
6 = Total sampling time, min;
Pto = Barometric pressure, in. Hg;
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Y « DGM calibration factor, dimensionless;
Vn = Volume of gas sample as measured by DGM, dcf.
9.2.1.1 Before beginning the field test (a set of three runs usually constitutes a field test),
operate the metering system (i.e., pump, volume meter, and orifice) at the AH@ pressure differential for
10 minutes. Record the volume collected, the DGM temperature, and the barometric pressure. Calculate
a DGM calibration check value, Y0 as follows:
10
0.0319 T
m
where
Yc = DGM calibration check value, dimensionless;
10 = Run time, min.
9.2.1.2 Compare the Ye value with the dry gas meter calibration factor Y to determine that 0.97
Y < Yc < 1.03 Y. If the Ye value is not within this range, the volume metering system should be
investigated before beginning the test
9.2.2 Calibrated critical orifice. A calibrated critical orifice, calibrated against a wet test meter
or spirometer and designed to be inserted at the inlet of the sampling meter box, may be used as a quality
control check by following the procedure of section 16.2 of this method.
IQ.Q Calibration and Standardization.
NOTE: Maintain a laboratory log of all calibrations.
10.1 Probe nozzle. Probe nozzles shall be calibrated before their initial use in the field. Using a
micrometer, measure the ID of the nozzle to the nearest 0.02S mm (0.001 in.). Make three separate
measurements using different diameters each time, and obtain the average of the measurements. The
difference between the high and low numbers shall not exceed 0.1 mm (0.004 in.). When nozzles
become nicked, dented, or corroded, they shall be reshaped, sharpened, and recalibrated before use.
Each nozzle shall be permanently and uniquely identified.
10.2 Pitot tube assembly. The Type S pitot tube assembly shall be calibrated according to the
procedure outlined in section 10.1 of Method 2,40 CFR part 60, appendix A.
10.3 Metering system.
10.3.1 Calibration prior to use. Before its initial use in the field, the metering system shall be
calibrated as follows: Connect the metering system inlet to the outlet of a wet test meter that is accurate
to within 1 percent. Refer to Figure 5-5 of Method 5,40 CFR part 60, appendix A. The wet test meter
should have a capacity of 30 liters/revolution (1 fWrev). A spirometer of 400 liters (14 ft3) or more
capacity, or equivalent, may be used for this calibration, although a wet test meter is usually more
practical. The wet test meter should be periodically calibrated with a spirometer or a liquid displacement
meter to ensure the accuracy of the wet test meter. Spirometers or wet test meters of other sizes may be
used, provided that the specified accuracies of the procedure are maintained. Run the metering system
pump for about 15 minutes with the orifice manometer indicating a median reading, as expected in field
use, to allow the pump to warm up and to permit the interior surface of the wet test meter to be
thoroughly wetted. Then, at each of a minimum of three orifice manometer settings, pass an exact
quantity of gas through the wet test meter and note the gas volume indicated by the DGM. Also note the
barometric pressure and the temperatures of the wet test meter, the inlet of the DGM, and the outlet of
the DGM. Select the highest and lowest orifice settings to bracket the expected field operating range of
the orifice. Use a minimum volume of 0.15 m3 (5 cf) at all orifice settings. Record all the data on a form
similar to Figure 5-6 of Method 5,40 CFR part 60, appendix A, and calculate Y (the DGM calibration
factor) and AH@ (the orifice calibration factor) at each orifice setting, as shown on Figure 5-6 of Method
5,40 CFR part 60, appendix A. Allowable tolerances for individual Y and AH$ values are given in
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Figure 5-6 of Method 5,40 CFR part 60, appendix A. Use the average of the Y values in the calculations
in section 12 of this method.
10.3.1.1. Before calibrating the metering system, it is suggested that a leak check be conducted.
For metering systems having diaphragm pumps, the normal leak check procedure will not detect
leakages •within the pump. For these cases the following leak check procedure is suggested: make a 10-
minute calibration run at 0.00057 mVmin (0.02 cftn); at the end of the run, take the difference of the
measured wet test meter and DGM volumes; divide the difference by 10 to get the leak rate. The leak
rate should not exceed 0.00057 nWmin (0.02 cfin).
10.3.2 Calibration after use. After each field use, the calibration of the metering system shall be
checked by performing three calibration runs at a single, intermediate orifice setting (based on the
previous field test) with the vacuum set at the maximum value reached during the test series. To adjust
the vacuum, insert a valve between the wet test meter and the inlet of the metering system. Calculate the
average value of the DGM calibration factor. If the value has changed by more than 5 percent,
recalibrate the meter over the full range of orifice settings, as previously detailed.
NOTE: Alternative procedures, e.g., rechecking the orifice meter coefficient, may be used,
subject to the approval of the Administrator.
10.3.3 Acceptable variation in calibration. If the DGM coefficient values obtained before and
after a test series differ by more than 5 percent, either the test series shall be voided or calculations for
the test series shall be performed using whichever meter coefficient value (i.e., before or after) gives the
lower value of total sample volume.
10.4 Probe heater calibration. Use a heat source to generate air heated to selected temperatures
that approximate those expected to occur in the sources to be sampled. Pass this air through the probe at
a typical sample flow rate while measuring the probe inlet and outlet temperatures at various probe
heater settings. For each air temperature generated, construct a graph of probe heating system setting
versus probe outlet temperature. The procedure outlined in APTD-0576 can also be used. Probes
constructed according to APTD-0581 need not be calibrated if the calibration curves in APTD-0576 are
used. Also, probes with outlet temperature monitoring capabilities do not require calibration.
NOTE: The probe heating system shall be calibrated before its initial use in the field.
10.5 Temperature sensors. Use the procedure in section 10.3 of Method 2,40 CFR part 60,
appendix A to calibrate in-stack temperature sensors. Dial thermometers, such as are used for the DGM
and condenser outlet, shall be calibrated against mercury-in-glass thermometers.
10.6 Barometer. Calibrate against a mercury barometer.
11.0 Analytical Procedure.
11.1 Record the data required on a sheet such as the one shown in Figure 315-1 of this method.
11.2 Handle each sample container as follows:
11.2.1 Container No. 1.
11.2.1.1 PM analysis. Leave the contents in the shipping container or transfer the filter and any
loose PM from the sample container to a tared glass weighing dish. Desiccate for 24 hours in a
desiccator containing anhydrous calcium sulfate. Weigh to a constant weight and report the results to the
nearest 0.1 mg. For purposes of this section, the term "constant weight" means a difference of no more
than 0.5 mg or 1 percent of total weight less tare weight, whichever is greater, between two consecutive
weighings, with no less than 6 hours of desiccation time between weighings (overnight desiccation is a
common practice). If a third weighing is required and it agrees within ±0.5 mg, then the results of the
second weighing should be used. For quality assurance purposes, record and report each individual
weighing; if more than three weighings are required, note this in the results for the subsequent MCEM
results.
11.2.1.2 MCEM analysis. Transfer the filter and contents quantitatively into a beaker. Add 100
ml of methylene chloride and cover with aluminum foil. Sonicate for 3 minutes then allow to stand for
20 minutes. Set up the filtration apparatus. Decant the solution into a clean Buchner fritted funnel.
Immediately pressure filter the solution through the tube into another clean, dry beaker. Continue
decanting and pressure filtration until all the solvent is transferred. Rinse the beaker and filter with 10 to
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20 mi methylene chloride, decant into the Buchner fritted funnel and pressure filter. Place the beaker on
a low-temperature hot plate (maximum 40°C) and slowly evaporate almost to dryness. Transfer the
remaining last few milliliters of solution quantitatively from the beaker (using at least three aliquots of
methylene chloride rinse) to a tared clean dry aluminum dish and evaporate to complete dryness.
Remove from heat once solvent is evaporated. Reweigh the dish after a 30-minute equilibrium in the
balance room and determine the weight to the nearest 0.1 mg. Conduct a methylene chloride blank run
in an identical fashion.
11.2.2 Container No. 2.
11.2.2.1 PM analysis. Note the level of liquid in the container, and confirm on the analysis
sheet whether leakage occurred during transport If a noticeable amount of leakage has occurred, either
void the sample or use methods, subject to the approval of the Administrator, to correct the final results.
Measure the liquid in this container either volumetrically to ±1 ml or gravimetricaUy to ±0.5 g. Transfer
the contents to a tared 250 ml beaker and evaporate to dryness at ambient temperature and pressure.
Desiccate for 24 hours, and weigh to a constant weight Report the results to the nearest 0.1 mg.
11.2.2.2 MCEM analysis. Add 25 ml methylene chloride to the beaker and cover with
aluminum foil. Sonicate for 3 minutes then allow to stand for 20 minutes; combine with contents of
Container No. 2M and pressure filter and evaporate as described for Container 1 in section 11.2.1.2 of
this method.
NOTES FOR MCEM ANALYSIS:
1. Light finger pressure only is necessary on 24/40 adaptor. A Chemplast adapter #15055-240
has been found satisfactory.
2. Avoid aluminum dishes made with fluted sides, as these may promote solvent "creep,"
resulting in possible sample loss.
3. If multiple samples are being run, rinse the Buchner fritted funnel twice between samples
with 5 ml solvent using pressure filtration. After the second rinse, continue the flow of air until the glass
frit is completely dry. Clean the Buchner fritted funnels thoroughly after filtering five or six samples.
11.2.3 Container No. 3. Weigh the spent silica gel (or silica gel plus impinger) to the nearest 0.5
g using a balance. This step may be conducted in the field.
11.2.4 Container 3W (impinger water).
11.2.4.1 MCEM analysis. Transfer the solution into a 1,000 ml separatory funnel quantitatively
with methylene chloride washes. Add enough solvent to total approximately 50 ml, if necessary. Shake
the funnel for 1 minute, allow the phases to separate, and drain the solvent layer into a 250 ml beaker.
Repeat the extraction twice. Evaporate with low heat (less than 40°C) until near dryness. Transfer the
remaining few milliliters of solvent quantitatively with small solvent washes into a clean, dry, tared
aluminum dish and evaporate to dryness. Remove from heat once solvent is evaporated. Reweigh the
dish after a 30-minute equilibration in the balance room and determine the weight to the nearest 0.1 mg.
11.2.5 Container 3S (solvent).
11.2.5.1 MCEM analysis. Transfer the mixed solvent to 250 ml beaker(s). Evaporate and weigh
following the procedures detailed for container 3 W in section 11.2.4 of this method.
11.2.6 Blank containers. Measure the distilled water, acetone, or methylene chloride in each
container either volumetrically or gravimetricaUy. Transfer the "solvent" to a tared 250 ml beaker, and
evaporate to dryness at ambient temperature and pressure. (Conduct a solvent blank on the distilled
deionized water blank in an identical fashion to that described in section 112.4.1 of this method.)
Desiccate for 24 hours, and weigh to a constant weight. Report the results to the nearest 0.1 mg.
NOTE: The contents of Containers No. 2,3 W, and 3M as well as the blank containers may be
evaporated at temperatures higher than ambient If evaporation is done at an elevated temperature, the
temperature must be below the boiling point of the solvent, also, to prevent "bumping," the evaporation
process must be closely supervised, and the contents of the beaker must be swirled occasionally to
maintain an even temperature. Use extreme care, as acetone and methylene chloride are highly
flammable and have a low flash point.
-------
12.0 Data Analysis and Calculations.
12.1 Carry out calculations, retaining at least one extra decimal figure beyond that of the
acquired data. Round off figures after the final calculation. Other forms of the equations may be used as
long as they give equivalent results.
12.2 Nomenclature.
A, - Cross-sectional area of nozzle, m3 (ft3).
B,, = Water vapor in the gas stream, proportion by volume.
C. = Acetone blank residue concentration, mg/g.
C, = Concentration of paniculate matter in stack gas, dry basis, corrected to standard
conditions, g/dscm (g/dscf).
I = Percent of isokinetic sampling.
L. = Maximum acceptable leakage rate for either a pretest leak check or for a leak check
following a component change; equal to 0.00057 mVmin (0.02 cfm) or 4 percent of the
average sampling rate, whichever is less.
LJ = Individual leakage rate observed during the leak check conducted prior to the "i*"
component change (I = 1,2,3...n), mVmin (cfm).
Lp = Leakage rate observed during the post-test leak check, mVmin (cfm).
m. = Mass of residue of acetone after evaporation, mg.
m. = Total amount of particulate matter collected, mg.
M, = Molecular weight of water, 18.0 g/g-mole (18.0 Ib/lb-mole).
P,,^ = Barometric pressure at the sampling site, mm Hg (in Hg).
P, = Absolute stack gas pressure, mm Hg (in. Hg).
PM » Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R = Ideal gas constant, 0.06236 [(mm HgXm3)]/[(°K.)
(g-mole)] {21.85 [(in. HgXft3)]/[(°RXlb-mole)]}.
Tm = Absolute average dry gas meter (DGM) temperature (see Figure 5-2 of Method 5, 40
CFR part 60, appendix A), °K (°R).
T, = Absolute average stack gas temperature (see Figure 5-2 of Method 5,40 CFR part 60,
appendix A), °K(0R).
TM = Standard absolute temperature, 293°K (528°R).
V, = Volume of acetone blank, ml.
Vm = Volume of acetone used in wash, ml.
V, = Volume of methylene chloride blank, ml.
Vw = Volume of methylene chloride used in wash, ml.
Vte = Total volume liquid collected in impingers and silica gel (see Figure 5-3 of Method 5,
40 CFR part 60, appendix A), ml.
Vm = Volume of gas sample as measured by dry gas meter, dcm (dcf).
vm(«td) = Volume of gas sample measured by the dry gas meter, corrected to standard conditions,
dscm (dscf).
V^ad) = Volume of water vapor in the gas sample, corrected to standard conditions, scm (scf).
V, = Stack gas velocity, calculated by Equation 2-9 in Method 2,40 CFR part 60, appendix
A, using data obtained from Method 5, 40 CFR part 60, appendix A, m/sec (ft/sec).
W. = Weight of residue in acetone wash, mg.
Y = Dry gas meter calibration factor.
AH = Average pressure differential across the orifice meter (see Figure 5-2 of Method 5,40
CFR part 60, appendix A), mm H20 (in H20).
p. = Density of acetone, 785.1 mg/ml (or see label on bottle).
pw - Density of water, 0.9982 g/ml (0.002201 Ib/ml).
p, = Density of methylene chloride, 1316.8 mg/ml (or see label on bottle).
9 = Total sampling time, min.
6, = Sampling time interval, from the beginning of a run until the first component change,
-------
mm.
0i = Sampling time interval, between two successive component changes, beginning with the
interval between the first and second changes, min.
9p = Sampling time interval, from the final (n*) component change until the end of the
sampling run, min.
13.6 = Specific gravity of mercury.
60 = Sec/min.
100 = Conversion to percent
12.3 Average dry gas meter temperature and average orifice pressure drop. See data sheet
(Figure 5-2 of Method 5,40 CFR part 60, appendix A).
12.4 Dry gas volume. Correct the sample volume measured by the dry gas meter to standard
conditions (20°C, 760 mm Hg or 68°F, 29.92 in Hg) by using Equation 315-1.
ir _ lw.w/ Ed. 315-1
13'6
where
K, = 0.3858 °K/mra Hg for metric units,
= 1 7.64 °R/in Hg for English units.
NOTE: Equation 3 1 5- 1 can be used as written unless the leakage rate observed during any of the
mandatory leak checks (i.e., the post-test leak check or leak checks conducted prior to component
changes) exceeds L.. If Lp or L, exceeds L., Equation 315-1 must be modified as follows:
(a) Case I. No component changes made during sampling run. In this case, replace Vn in Equation
315-1 with the expression:
(b) Case II. One or more component changes made during the sampling run. In this case, replace
VB in Equation
3 15- 1 by the expression:
[Vm - (L, - L.) 0, - £ (L, - L.) 0, - (Lp - L.) 0p]
1=2
and substitute only for those leakage rates (L, or Lp) which exceed L,.
12.5 Volume of water vapor condensed.
-------
= vic * SM = K2 vic Eg. 315-2
D
Pstd
where
K2 = 0.001333 mVml for metric units;
= 0.04706 ftVml for English units.
12.6 Moisture content.
Eg. 315-3
ws \j M
K
NOTE: In saturated or water droplet-laden gas streams, two calculations of the moisture content
of the stack gas shall be made, one from the impinger analysis (Equation 315-3), and a second from the
assumption of saturated conditions. The lower of the two values of Bm shall be considered correct. The
procedure for determining the moisture content based upon assumption of saturated conditions is given
in section 4.0 of Method 4,40 CFR part 60, appendix A. For the purposes of this method, the average
stack gas temperature from Figure 5-2 of Method 5,40 CFR part 60, appendix A may be used to make
this determination, provided that the accuracy of the in-stack temperature sensor is ±1°C (2°F).
12.7 Acetone blank concentration.
Ed. 315-4
12.8 Acetone wash blank.
W. = C.VMp. Eq. 315-5
12.9 Total particulate weight. Determine the total PM catch from the sum of the weights
obtained from Containers 1 and 2 less the acetone blank associated with these two containers (see Figure
315-1).
NOTE: Refer to section 8.5.8 of this method to assist in calculation of results involving two or
more filter assemblies or two or more sampling trains.
12.10 Particulate concentration.
c, = K, m./V.n, Eq.31S-6
where
K = 0.001 g/mg for metric units;
= 0.0154 gr/mg for English units.
12.11 Conversion factors.
From
ft3
gr
gr/ft3
mg
12
m3
mg
mg/m3
g
Ib
12.12 Isokinetic variation.
Multiply by
0.02832
64.80004
2288.4
0.001
1.429X10-4
-------
12.12.1 Calculation from raw data.
100 Ta
/ =
13.6
EQ. 315-7
60 0 v. P. An
where
K4 = 0.003454 [(mm HgXm3)]/[(mlX°K)] for metric units;
= 0.002669 [(in HgXft3)]/[(mlX°R)] for English units.
12.12.2 Calculation from intermediate values.
60
= Kf
where
K5 = 4.320 for metric units;
= 0.09450 for English units.
12.12.3 Acceptable results. If 90 percent * I * 110 percent, the results are acceptable. If the
PM or MCEM results are low in comparison to the standard, and "I" is over 110 percent or less than 90
percent, the Administrator may opt to accept the results. Reference 4 in the Bibliography may be used to
make acceptability judgments. If "I" is judged to be unacceptable, reject the results, and repeat the test.
12.13 Stack gas velocity and volumetric flow rate. Calculate the average stack gas velocity and
volumetric flow rate, if needed, using data obtained in this method and the equations in sections 5.2 and
5.3 of Method 2,40 CFR part 60, appendix A.
12.14 MCEM results. Determine the MCEM concentration from the results from Containers 1,
2,2M, 3W, and 3S less the acetone, methylene chloride, and filter blanks value as determined in the
following equation:
w» ~ wt ~ *b
13.0 Method Performance. [Reserved]
14.0 Pollution Prevention. [Reserved]
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15.0 Waste Management [Reserved]
16.0 Alternative Procedures.
16.1 Dry gas meter as a calibration standard. A DGM may be used as a calibration standard for
volume measurements in place of the wet test meter specified in section 16.1 of this method, provided
that it is calibrated initially and recalibrated periodically as follows:
16.1.1 Standard dry gas meter calibration.
16.1.1.1. The DGM to be calibrated and used as a secondary reference meter should be of high
quality and have an appropriately sized capacity, e.g., 3 liters/rev (0.1 fWrev). A spirometer (400 liters
or more capacity), or equivalent, may be used for this calibration, although a wet test meter is usually
more practical. The wet test meter should have a capacity of 30 liters/rev (1 ft3/rev) and be capable of
measuring volume to within 1.0 percent; wet test meters should be checked against a spirometer or a
liquid displacement meter to ensure the accuracy of the wet test meter. Spirometers or wet test meters of
other sizes may be used, provided that the specified accuracies of the procedure are maintained.
16.1.1.2 Set up the components as shown in Figure 5-7 of Method 5,40 CFRpart 60, appendix
A. A spirometer, or equivalent, may be used in place of the wet test meter in the system. Run the pump
for at least 5 minutes at a flow rate of about 10 liters/min (0.35 cfm) to condition the interior surface of
the wet test meter. The pressure drop indicated by the manometer at the inlet side of the DGM should be
minimized (no greater than 100 mm H2O [4 in. H2O] at a flow rate of 30 liters/min [1 cfm]). This can be
accomplished by using large- diameter tubing connections and straight pipe fittings.
16.1.1.3 Collect the data as shown in the example data sheet (see Figure 5-8 of Method 5,40
CFR part 60, appendix A). Make triplicate runs at each of the flow rates and at no less than five different
flow rates. The range of flow rates should be between 10 and 34 liters/min (0.35 and 1.2 cfm) or over
the expected operating range.
16.1.1.4 Calculate flow rate, Q, for each run using the wet test meter volume, V,, and the run
time, q. Calculate the DGM coefficient, Y^ for each run. These calculations are as follows:
P V
Q = K. bar W Eq. 315-9
(Td, + T.M) Pb
'd» 'ttd/ ' b«r
rd. =
V (T + T HP + --) Eq. 315-10
vd« I'w '•td'l'bar 135'
where
K, = 0.3858 for international system of units (SI);
17.64 for English units;
P^ = Barometric pressure, mm Hg (in Hg);
Vw = Wet test meter volume, liter (ft3);
t* = Average wet test meter temperature, °C (°F);
t^, = 273°C for SI units; 460°F for English units;
Q = Run time, min;
tj, = Average dry gas meter temperature, °C (°F);
V,,, = Dry gas meter volume, liter (ft3);
Ap = Dry gas meter inlet differential pressure, mm H2O (in H2O).
16.1.1.5 Compare the three Yj, values at each of the flow rates and determine the maximum and
minimum values. The difference between the maximum and minimum values at each flow rate should
be no greater than 0.030. Extra sets of triplicate runs may be made in order to complete this requirement
In addition, the meter coefficients should be between 0.95 and 1.05. If these specifications cannot be
-------
met in three sets of successive triplicate runs, the meter is not suitable as a calibration standard and
should not be used as such. If these specifications are met, average the three Y* values at each flow rate
resulting in five average meter coefficients, Y*.
16.1.1.6 Prepare a curve of meter coefficient, Yj,, versus flow rate, Q, for the DGM. This curve
shall be used as a reference when the meter is used to calibrate other DGMs and to determine whether
recalibration is required.
16.1.2 Standard dry gas meter recalibration.
16.1.2.1 Recalibrate the standard DGM against a wet test meter or spirometer annually or after
every 200 hours of operation, whichever comes first. This requirement is valid provided the standard
DGM is kept in a laboratory and, if transported, cared for as any other laboratory instrument Abuse to
the standard meter may cause a change in the calibration and will require more frequent recalibrations.
16.1.2.2 As an alternative to full recalibration, a two-point calibration check may be made.
Follow the same procedure and equipment arrangement as for a full recalibration, but run the meter at
only two flow rates (suggested rates are 14 and 28 liters/min [0.5 and 1.0 cfin]). Calculate the meter
coefficients for these two points, and compare the values with the meter calibration curve. If die two
coefficients are within 1.5 percent of the calibration curve values at the same flow rates, the meter need
not be recalibrated until the next date for a recalibration check.
16.2 Critical orifices as calibration standards. Critical orifices may be used as calibration
standards in place of the wet test meter specified in section 10.3 of this method, provided that they are
selected, calibrated, and used as follows:
16.2.1 Selection of critical orifices.
16.2.1.1 The procedure that follows describes the use of hypodermic needles or stainless steel
needle tubing that has been found suitable for use as critical orifices. Other materials and critical orifice
designs may be used provided the orifices act as true critical orifices; i.e., a critical vacuum can be
obtained, as described in section 7.2.2.2.3 of Method 5,40 CFR part 60, appendix A. Select five critical
orifices that are appropriately sized to cover the range of flow rates between 10 and 34 liters/min or the
expected operating range. Two of the critical orifices should bracket the expected operating range. A
minimum of three critical orifices will be needed to calibrate a Method 5 DGM; the other two critical
orifices can serve as spares and provide better selection for bracketing the range of operating flow rates.
The needle sizes and tubing lengths shown in Table 315-1 give the approximate flow rates indicated in
the table.
16.2.1.2 These needles can be adapted to a Method 5 type sampling train as follows: Insert a
serum bottle stopper, 13 x 20 mm sleeve type, into a 0.5 in Swagelok quick connect. Insert the needle
into the stopper as shown in Figure 5-9 of Method 5,40 CFR part 60, appendix A.
16.2.2 Critical orifice calibration. The procedure described in this section uses the Method 5
meter box configuration with a DGM as described in section 6.1.1.9 of this method to calibrate the
critical orifices. Other schemes may be used, subject to the approval of the Administrator.
16.2.2.1 Calibration of meter box. The critical orifices must be calibrated in the same
configuration as they will be used; i.e., there should be no connections to the inlet of the orifice.
16.2.2.1.1 Before calibrating the meter box, leak-check the system as follows: Fully open the
coarse adjust valve and completely close the bypass valve. Plug die inlet Then turn on the pump and
determine whether there is any leakage. The leakage rate shall be zero; i.e., no detectable movement of
the DGM dial shall be seen for 1 minute.
16.2.2.1.2 Check also for leakages in that portion of the sampling train between the pump and
the orifice meter. See section 5.6 of Method 5,40 CFR part 60, appendix A for die procedure; make any
corrections, if necessary. If leakage is detected, check for cracked gaskets, loose fittings, worn 0-rings,
etc. and make die necessary repairs.
16.2.2.1.3 After determining that die meter box is leakless, calibrate die meter box according to
die procedure given in section 5.3 of Method 5,40 CFR part 60, appendix A. Make sure tiiat die wet test
meter meets die requirements stated in section 7.1.1.1 of Mediod 5,40 CFR part 60, appendix A. Check
die water level in die wet test meter. Record die DGM calibration factor, Y.
-------
16.2.2.2 Calibration of critical orifices. Set up the apparatus as shown in Figure 5-10 of Method
5,40 CFR part 60, appendix A.
16.2.2.2.1 Allow a warm-up time of IS minutes. This step is important to equilibrate the
temperature conditions through the DGM.
16.2.2.2.2 Leak-check the system as in section 7.2.2.1.1 of Method 5,40 CFR part 60, appendix
A. The leakage rate shall be zero.
16.2.2.2.3 Before calibrating the critical orifice, determine its suitability and the appropriate
operating vacuum as follows: turn on the pump, fully open the coarse adjust valve, and adjust the bypass
valve to give a vacuum reading corresponding to about half of atmospheric pressure. Observe the meter
box orifice manometer reading, DH. Slowly increase the vacuum reading until a stable reading is
obtained on the meter box orifice manometer. Record the critical vacuum for each orifice. Orifices that
do not reach a critical value shall not be used.
16.2.2.2.4 Obtain the barometric pressure using a barometer as described in section 6.1.2 of this
method. Record the barometric pressure, PbB, in mm Hg (in. Hg).
16.2.2.2.5 Conduct duplicate runs at a vacuum of 25 to 50 mm Hg (1 to 2 in. Hg) above the
critical vacuum. The runs shall be at least 5 minutes each. The DGM volume readings shall be in
increments of complete revolutions of the DGM. As a guideline, the times should not differ by more
than 3.0 seconds (this includes allowance for changes in the DGM temperatures) to achieve ±0.5 percent
in K'. Record the information listed in Figure 5-11 of Method 5,40 CFR part 60, appendix A.
16.2.22.6 Calculate K' using Equation 315-11.
. _ ,^.o Ea. 315-11
K — ———^^————
P*.r
where
K' = Critical orifice coefficient, [m3X°K)«]/
[(mm HgXmin)] {[(ffXWl/Kin. HgXmin)]};
T«»b = Absolute ambient temperature, °K(°R).
16.2.2.2.7 Average the K' values. The individual K' values should not differ by more than ±0.5
percent from the average.
16.2.3 Using the critical orifices as calibration standards.
16.2.3.1 Record the barometric pressure.
16.2.3.2 Calibrate the metering system according to the procedure outlined in sections 7.2.2.2. 1
to 7.2.2.2.5 of Method 5, 40 CFR part 60, appendix A. Record the information listed in Figure 5-12 of
Method 5, 40 CFR part 60, appendix A.
1 6.2.3.3 Calculate the standard volumes of air passed through the DGM and the critical orifices,
and calculate the DGM calibration factor, Y, using the equations below:
- K., Vw [Pto + (AH/1 3.6)]/Tm £$
Eq.31S-13
Eg. 3 15-14
where
Verbid) ~ Volume of gas sample passed through the
critical orifice, corrected to standard conditions, dscm (dscf).
K1 = 0.3858 °K/mm Hg for metric units
= 1 7.64 °R/in Hg for English units.
16.2.3.4 Average the DGM calibration values for each of the flow rates. The calibration factor,
Y, at each of the flow rates should not differ by more than ±2 percent from the average.
1 6.2.3.5 To determine the need for recalibrating the critical orifices, compare the DGM Y
-------
factors obtained from two adjacent orifices each time a DGM is calibrated; for example, when checking
orifice 13/2.5, use orifices 12/10.2 and 13/5.1. If any critical orifice yields a DGM Y factor differing by
more than 2 percent from the others, recalibrate the critical orifice according to section 7.2.2.2 of Method
5, 40 CFR part 60, appendix A.
17.0 References.
1. Addendum to Specifications for Incinerator Testing at Federal Facilities. PHS, NCAPC.
December 6,1967.
2. Martin, Robert M. Construction Details of Isokinetic Source-Sampling Equipment
Environmental Protection Agency. Research Triangle Park, NC. APTD-0581. April 1971.
3. Rom, Jerome J. Maintenance, Calibration, and Operation of Isokinetic Source Sampling
Equipment Environmental Protection Agency. Research Triangle Park, NC. APTD-0576. March 1972.
4. Smith, W.S., R.T. Shigehara, and W.F. Todd. A Method of Interpreting Stack Sampling Data.
Paper Presented at the 63rd Annual Meeting of the Air Pollution Control Association, St Louis, MO.
June 14-19,1970.
5. Smith, W.S., et al. Stack Gas Sampling Improved and Simplified With New Equipment
APCA Paper No. 67-119. 1967.
6.. Specifications for Incinerator Testing at Federal Facilities. PHS, NCAPC. 1967.
7. Shigehara, R.T. Adjustment in the EPA Nomograph for Different Phot Tube Coefficients and
Dry Molecular Weights. Stack Sampling News 2:4-11. October 1974.
8. Vollaro, R.F. A Survey of Commercially Available Instrumentation for the Measurement of
Low-Range Gas Velocities. U.S. Environmental Protection Agency, Emission Measurement Branch.
Research Triangle Park, NC. November 1976 (unpublished paper).
9. Annual Book of ASTM Standards. Part 26. Gaseous Fuels; Coal and Coke; Atmospheric
Analysis. American Society for Testing and Materials. Philadelphia, PA. 1974. pp. 617-622.
10. Felix, L.G., G.I. Clinard, G.E. Lacy, and J.D. McCain. Inertial Cascade Impactor Substrate
Media for Flue Gas Sampling. U.S. Environmental Protection Agency. Research Triangle Park, NC
27711. Publication No. EPA-600/7-77-060. June 1977. 83 p.
11. Westlin, P.R., and R.T. Shigehara. Procedure for Calibrating and Using Dry Gas Volume
Meters as Calibration Standards. Source Evaluation Society Newsletter. 2(1):I7-30. February 1978.
12. Lodge, J.P., Jr., J.B. Pate, B.E. Ammons, and G.A. Swanson. The Use of Hypodermic
Needles as Critical Orifices in Air Sampling. J. Air Pollution Control Association. 16.: 197-200. 1966.
18.0 Tables. Diagrams. Flowcharts, and Validation Data
TABLE 31 S-l. Flow Rates for Various Needle Sizes and Tube Lengths.
Gauge/length
(cm)
12/7.6
12/10.2
13/2.5
13/5.1
13/7.6
13/10.2
Flow rate
(liters/min)
32.56
30.02
25.77
23.50
22.37
20.67
Gauge/length
(cm)
14/2.5
14/5.1
14/7.6
15/3.2
15/7.6
15/10.2
Flow rate
(liters/min)
19.54
17.27
16.14
14.16
11.61
10.48
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Paniculate analysis
Plant
Date
Run No.
Filter No.
Amount liquid lost during
transport
Acetone blank volume (ml)
Acetone blank concentration (Eq.3 15-4) (mg/mg)
Acetone wash blank (Eq.3 15-5) (mg)
Container
No. 1
Container
No. 2
Final weight
(mg)
Tare weight (mg)
Total
Less Acetone blank
Weight of particulate matter
Weight gain (mg)
Moisture analysis
Impingers
Silica gel
Final volume
(mg)
Note 1
Initial volume (mg)
Notel
Total
Liquid collected (mg)
FIGURE 315-1. Particulate and MCEM Analyses
Note 1: Convert volume of water to weight by multiplying by the density of water (1 g/ml).
-------
MCEM analysis
Container No.
1
2+2M
3W
3S
Final
weight
(mg)
Tare of
aluminum
dish (mg)
Total
Less acetone wash blank (mg)
(not to exceed 1 mg/1 of
acetone used)
Less methylene chloride wash
blank (mg) (not to exceed
1.5 mg/1 of methylene
chloride used)
Less filter blank (mg)
(not to exceed....
(mg/filter)
MCEM weight (mg)
Weight
gain
E^tof./
Acetone
wash volume
(ml)
E"..
MetS^teinte
wash
volume
(ml)
X>hr
w. =c. P. E^w
wt = CAE^
F>
mUCEOM = 2* mtot»l W» ~ Wt ~ *b
FIGURE 315-1 (ContinuedV Particuiate And MCEM Analyses
*****
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APPENDIX F.7
SW-846 METHOD 0010
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METHOD 0010
MODIFIED METHOD 5 SAMPLING TRAIN
1.0 SCOPE AND APPLICATION
1.1 This method 1s applicable to the determination of Destruction and
Removal Efficiency (ORE) of semivolatile Principal Organic Hazardous Compounds
(POHCs) from incineration systems (PHS, 1967). This method also may be used
to determine particulate emission rates from stationary sources as per EPA
Method 5 (see References at end of this method).
2.0 SUMMARY OF METHOD
2.1 Gaseous and particulate pollutants are withdrawn from an emission
source at an isokinetlc sampling rate and are collected 1n a multicomponent
sampling train. Principal components of the train include a high-efficiency
glass- or quartz-fiber filter and a packed bed of porous polymeric adsorbent
resin. The filter is used to collect organic-laden particulate materials and
the porous polymeric resin to adsorb semivolatile organic species.
Semivolatile species are defined as compounds with boiling points >100*C.
2.2 Comprehensive chemical analyses of the collected sample are
conducted to determine the concentration and Identity of the organic
materials.
3.0 INTERFERENCES
3.1 Oxides of nitrogen (NOX) are possiale interferents 1n the
determination of certain water-soluble compounds such as dloxane, phenol, and
urethane; reaction of these compounds with NOX in the presence of moisture
will reduce their concentration. Other possibilities that could result in
positive or negative bias are (1) stability of the compounds 1n methylene
chloride, (2) the formation of water-soluble organic salts on the resin 1n the
presence of moisture, and (3) the solvent extraction efficiency of water-
soluble compounds from aqueous media. Use of two or more ions per compound
for qualitative and quantitative analysis can overcome interference at one
mass. These concerns should be addressed on a compound-by-compound basis
before using this method.
4.0 APPARATUS AND MATERIALS
4.1 Sampling train;
4.1.1 A schematic of the sampling train used in this method is
shown in Figure 1. This sampling train configuration is adapted from EPA
Method 5 procedures, and, as such, the majority of the required equipment
0010 - 1
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Date September 1986
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o
o
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o
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ro
O 70
PI ro
rt- <
n ->'
ro
a
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II
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CO
en
Healed Area
Tempeiature Sensor
Probe
Reverse-Type Pitol Tube
nsor T Slack Wall
tine'
X*
f
L ^
P
-md
45P
\ •
Thermometer
Filler Holder
Thermometer
Check Valve
Pilot Manometer
Rccirculation Pump
Orifice
Impingers Ice Bath
Pass Valve
Vacuum Line
Thermometers
Dry Gas Meter Air right Pump
Finure 1. Modified Method 5 Sampling Train.
J
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I
wn™ c
NOZZLE
TEMPERATURE
SENSORV THERMOMETER
HEATED AREA
TEMPERATURE SENSOR
FILTER HOLDER
CONDENSER
THERMOMETER
x j T
' ICE BATH \
COOLANT PUMP-^ KNOCKOUT ' 100 m\fl(Water
TEMPERATURE SENSOR
MAIN VACUUM
VALVE ^ GAUGE
METHOD 5
METERING
CONSOLE
VACUUM
LINE
PITOT TUBE
NOZZLE P.RO&E
PROBE TIP DETAIL
Figure 4.2. Schematic of the I2PA Method sampling train.
-------
Is identical to that used in EPA Method 5 determinations. The new
components required are a condenser coll and a sorbent module, which are
used to collect semivolatile organic materials that pass through the
glass- or quartz-fiber filter in the gas phase.
4.1.2 Construction details for the basic train components are given
in APTD-0581 (see Martin, 1971, in Section 13.0, References); commercial
models of this equipment are also available. Specifications for the
sorbent module are provided in the following subsections. Additionally,
the following subsections list changes to APTD-0581 and identify
allowable train configuration modifications.
4.1.3 Basic operating and maintenance procedures for the sampling
train are described in APTD-0576 (see Rom, 1972, in Section 13.0,
References). As correct usage is Important in obtaining valid results,
all users should refer to APTD-0576 and adopt the operating and
maintenance procedures outlined therein unless otherwise specified. The
sampling train consists of the components detailed below.
4.1.3.1 Probe nozzle; Stainless steel (316) or glass with
, sharp, tapered (30* angle) leading edge. The taper shall be on the
outside to preserve a constant I.D. The nozzle shall be buttonhook
or elbow design and constructed from seamless tubing (if made of
stainless steel). Other construction materials may be considered
for particular applications. A range of nozzle sizes suitable for
isokinetic sampling should be available in increments of 0.16 cm
(1/16 in.), e.g., 0.32-1.27 cm (1/8-1/2 in.), or larger if higher
volume sampling trains are used. Each nozzle shall be calibrated
according to the procedures outlined 1n Paragraph 9.1.
4.1.3.2 Probe liner; Borosilicate or quartz-glass tubing with
a heating system capable of maintaining a gas temperature of 120 +
14*C (248 + 25*F) at the exit end during sampling. (The tester may
opt to operate the equipment at a temperature lower than that
specified.) Because the actual temperature at the outlet of the
probe is not usually monitored during sampling, probes constructed
according to APTD-0581 and utilizing the calibration curves of APTD-
0576 (or calibrated according to the procedure outlined in APTD-
0576) are considered acceptable. Either borosillcate or quartz-
glass probe liners may be used for stack temperatures up to about
480*C (900*F). Quartz liners shall be used for temperatures between
480 and 900*C (900 and 1650*F). (The softening temperature for
borosillcate is 820'C (1508*F), and for quartz 1500»C (2732'F).)
Water-cool ing of the stainless steel sheath will be necessary at
temperatures approaching and exceeding 500*C.
4.1.3.3 Pi tot tube; Type S, as described 1n Section 2.1 of
EPA Method 2, or other appropriate devices (Vollaro, 1976). The
pi tot tube shall be attached to the probe to allow constant
monitoring of the stack-gas velocity. The Impact (high-pressure)
opening plane of the pitot tube shall be even with or above the
nozzle entry plane (see EPA Method 2, Figure 2-6b) during sampling.
The Type S pltot tube assembly shall have a known coefficient,
determined as outlined 1n Section 4 of EPA Method 2.
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4.1.3.4 Differential pressure gauge; Inclined manometer or
equivalent device as described in Section 2.2 of EPA Method 2. One
manometer shall be used for velocity-head (AP) readings and the
other for orifice differential pressure (AH) readings. _
4.1.3.5 Filter holder; Boroslllcate glass, with a glass frit
filter support and a sealing gasket. The sealing gasket should be
made of materials that will not Introduce organic material Into the
gas stream at the temperature at which the filter holder will be
maintained. The gasket shall be constructed of Teflon or materials
of equal or better characteristics. The holder design shall provide
a positive seal against leakage at any point along the filter
circumference. The holder shall be attached Immediately to the
outlet of the cyclone or cyclone bypass.
4.1.3.6 Filter heating system; Any heating system capable of
maintaining a temperature of 120 + 14*C (248 + 25*F) around the
filter holder during sampling. Other temperatures may be
appropriate for particular applications. Alternatively, the tester
may opt to operate the equipment at temperatures other than that
specified. A temperature gauge capable of measuring temperature to
within 3*C (5.4*F) shall be Installed so that the temperature around
the filter holder can be regulated and monitored during sampling.
Heating systems other than the one shown in APTD-0581 may be used.
4.1.3.7 Organic sampling module; This unit consists of three
sections, Including a gas-conditioning section, a sorbent trap, and
a condensate knockout trap. The gas-conditioning system shall be
capable of conditioning the gas leaving the back half of the filter
holder to a temperature not exceeding 20'C (68*F). The sorbent trap
shall be sized to contain approximately 20 g of porous polymeric
resin (Rohm and Haas XAD-2 or equivalent) and shall be jacketed to
maintain the internal gas temperature at 17 + 3*C (62.5 + 5.4*F).
The most commonly used coolant is ice water from the impinger Ice-
water bath, constantly circulated through the outer jacket, using
rubber or plastic tubing and a peristaltic pump. The sorbent trap
should be outfitted with a glass well or depression, appropriately
sized to accommodate a small thermocouple in the trap for monitoring
the gas entry temperature. The condensate knockout trap shall be of
sufficient size to collect the condensate following gas
conditioning. The organic module components shall be oriented to
direct the flow of condensate formed vertically downward from the
conditioning section, through the adsorbent media, and Into the
condensate knockout trap. The knockout trap is usually similar 1n
appearance to an empty Impinger directly underneath the sorbent
module; it may be oversized but should have a shortened center stem
(at a minimum, one-half the length of the normal impinger stems) to
collect a large volume of condensate without bubbling and
overflowing Into the impinger train. All surfaces of the organic
module wetted by the gas sample shall be fabricated of boroslUcate
glass, Teflon, or other inert materials. Commercial versions of the
0010 - 4
Revision
Date September 1986
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complete organic module are not currently available, but may be
assembled from commercially available laboratory glassware and a
custom-fabricated sorbent trap. Details of two acceptable designs
are shown In Figures 2 and 3 (the thermocouple well 1s shown 1n
< Figure 2).
4.1.3.8 Implnqer train; To determine the stack-gas moisture
content, four 500-mL impingers, connected 1n series with leak-free
ground-glass joints, follow the knockout trap. The first, third,
and fourth Impingers shall be of the Greenburg-Smlth design,
modified by replacing the tip with a 1.3-cm (1/2-1n.) I.D. glass
tube extending about 1.3 cm (1/2 1n.) from the bottom of the outer
cylinder. The second Impinger shall be of the Greenburg-Smlth
design with the standard tip. The first and second Impingers shall
contain known quantities of water or appropriate trapping solution.
The third shall be empty or charged with a caustic solution, should
the stack gas contain hydrochloric acid (HC1). The fourth shall
contain a known weight of silica gel or equivalent desiccant.
4.1.3.9 Metering system; The necessary components are a
vacuum gauge, leak-freepump, thermometers capable of measuring
temperature to within 3'C (5.4*F), dry-gas meter capable of
measuring volume to within 1%, and related equipment, as shown 1n
Figure 1. At a minimum, the pump should be capable of 4 cfm free
flow, and the dry-gas meter should have a recording capacity of
0-999.9 cu ft with a resolution of 0.005 cu ft. Other metering
systems capable of maintaining sampling rates within 10X of
isokineticlty and of determining sample volumes to within 2% may be
used. The metering system must be used 1n conjunction with a pi tot
tube to enable checks of 1sok1net1c sampling rates. Sampling trains
using metering systems designed for flow rates higher than those
described 1n APTD-0581 and APTD-0576 may be used, provided that the
specifications of this method are met.
4.1.3.10 Barometer; Mercury, aneroid, or other barometer
capable of measuring atmospheric pressure to within 2.5 mm Hg (0.1
in. Hg). In many cases the barometric reading may be obtained from
a nearby National Weather Service station, 1n which case the station
value (which is the absolute barometric pressure) 1s requested and
an adjustment for elevation differences between the weather station
and sampling point is applied at a rate of minus 2.5 mm Hg (0.1 in.
Hg) per 30-m (100 ft) elevation increase (vice versa for elevation
decrease).
4.1.3.11 Gas density determination equipment; Temperature
sensor and pressure gauge (asdescribedin Sections 2.3 and 2.4 of
EPA Method 2), and gas analyzer, 1f necessary (as described in EPA
Method 3). The temperature sensor Ideally should be permanently
attached to the pltot tube or sampling probe in a fixed
configuration such that the tip of the sensor extends beyond the
leading edge of the probe sheath and does not touch any metal.
0010 - 5
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Date September 1986
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or
168 mm
o
o
t—'
o
I
I
28/12
Ball Joint
l-11/16" or 45 mm
I
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3
0
40 RC Glass Frit
Figure 2. Adsorbent Sampling System.
28/12 Socket Joint
Water Jacket
J
-------
28/12
XAD-2Trap. —
Coarse Frit
28/12
Thermocouple Well
28/12
XAD • 2 Trap and Condenser Coil
-------
0010 - 7
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Date September 1986
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Alternatively, the sensor may be attached just prior to use in the
field. Note, however, that 1f the temperature sensor is attached in
the field, the sensor must be placed in an interference-free
arrangement with respect to the Type S pi tot tube openings (see EPA
Method 2, Figure 2-7). As a second alternative, if a difference of
no more than IX in the average velocity measurement is to be
introduced, the temperature gauge need not be attached to the probe
or pi tot tube.
4.1.3.12 Cal1bratlon/f1 eld-preparation record; A permanently
bound laboratory notebook, in which duplicate copies of data may be
made as they are being recorded, is required for documenting and
recording calibrations and preparation procedures (I.e., filter and
silica gel tare weights, clean XAD-2, quality assurance/quality
control check results, dry-gas meter, and thermocouple calibrations,
etc.). The duplicate copies should be detachable and should be
stored separately in the test program archives.
4.2 Sample Recovery;
4.2.1 Probe liner: Probe nozzle and organic module conditioning
section brushes; nylon bristle brushes with stainless steel wire handles
are required. The probe brush shall have extensions of stainless steel,
Teflon, or inert material at least as long as the probe. The brushes
shall be properly sized and shaped to brush out the probe liner, the
probe nozzle, and the organic module conditioning section.
4.2.2 Wash bottles: Three. Teflon or glass wash bottles are
recommended; polyethylene wash bottles should not be used because organic
contaminants may be extracted by exposure to organic solvents used for
sample recovery.
4.2.3 Glass sample storage containers: Chemically resistant,
borosilicate amber and clear glass bottles, 500-mL or 1,000-mL. Bottles
should be tinted to prevent action of light on sample. Screw-cap liners
shall be either Teflon or constructed so as to be leak-free and resistant
to chemical attack by organic recovery solvents. Narrow-mouth glass
bottles have been found to exhibit less tendency toward leakage.
4.2.4 Petrl dishes: Glass, sealed around the circumference with
wide (1-1n.) Teflon tape, for storage and transport of filter samples.
4.2.5 Graduated cylinder and/or balances: To measure condensed
water to the nearest 1 mL or 1 g. Graduated cylinders shall have
subdivisions not >2 mL. Laboratory triple-beam balances capable of
weighing to +0.5 g or better are required.
4.2.6 Plastic storage containers: Screw-cap polypropylene or
polyethylene containers to store silica gel.
4.2.7 Funnel and rubber policeman: To aid in transfer of silica
gel to container (not necessary if silica gel is weighed in field).
0010 - 8
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Date September 1986
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4.2.8 Funnels: Glass, to aid 1n sample recovery.
4.3 Filters: Glass- or quartz-fiber filters, without organic binder,
exhibiting at least 99.95% efficiency «0.05X penetration) on 0.3-ura dloctyl
phthalate smoke particles. The filter efficiency test shall be conducted In
accordance with ASTM standard method 02986-71. Test data from the supplier's
quality control program are sufficient for this purpose. In sources
containing S02 or $03, the filter material must be of a type that 1s
unreactlve to SO? or $03. Reeve Angel 934 AH or Schlelcher and Schwell 13
filters work well under these conditions.
4.4 Crushed 1ce; Quantities ranging from 10-50 Ib may be necessary
during a sampling run, depending on ambient air temperature.
4.5 Stopcock grease; Solvent-Insoluble, heat-stable s111cone grease.
Use of s111 cone grease upstream of the module 1s not permitted, and amounts
used on components located downstream of the organic module shall be
minimized. SlUcone grease usage 1s not necessary if screw-on connectors and
Teflon sleeves or ground-glass joints are used.
4-6 Glass wool; Used to plug the unfritted end of the sorbent module.
The glass-wool fiber should be solvent-extracted with methylene chloride 1n a
Soxhlet extractor for 12 hr and air-dried prior to use.
5.0 REAGENTS
5.1 Adsorbent resin; Porous polymeric resin (XAD-2 or equivalent) Is
recommended"!These resins shall be cleaned prior to their use for sample
collection. Appendix A of this method should be consulted to determine
appropriate precleanlng procedure. For best results, resin used should not
exhibit a blank of higher than 4 mg/kg of total chromatographable organics
(TCO) (see Appendix B) prior to use. Once cleaned, resin should be stored In
an airtight, wide-mouth amber glass container with a Teflon-lined cap or
placed in one of the glass sorbent modules tightly sealed with Teflon film and
elastic bands. The resin should be used within 4 wk of the preparation.
5.2 Silica gel; Indicating type, 6-16 mesh. If.previously used, dry at
175'C (350*F) for 2 hr before using. New silica gel may be used as received.
Alternatively, other types of desiccants (equivalent or better) may be used,
subject to the approval of the Administrator.
5.3 Impinqer solutions; Distilled organic-free water (Type II) shall be
used, unless sampling is Intended to quantify a particular inorganic gaseous
species. If sampling is intended to quantify the concentration of additional
species, the impinger solution of choice shall be subject to Administrator
approval. This water should be prescreened for any compounds of Interest.
One hundred mL will be added to the specified impinger; the third implnger 1n
the train may be charged with a basic solution (1 N sodium hydroxide or sodium
acetate) to protect the sampling pump from acidic gases. Sodium acetate
should be used when large sample volumes are anticipated because sodium
hydroxide will react with carbon dioxide 1n aqueous media to form sodium
carbonate, which may possibly plug the Impinger.
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Date September 1986
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5.4 Sample recovery reagents;
5.4.1 Methylene chloride: D1st1lled-1n-glass grade 1s required for
sample recovery and cleanup (see Note to 5.4.2 below).
5.4.2 Methyl alcohol: D1st1lled-1n-glass grade 1s required for
sample recovery and cleanup.
NOTE: Organic solvents from metal containers may have a high
residue blank and should not be used. Sometimes suppliers
transfer solvents from metal to glass bottles; thus blanks shall
be run prior to field use and only solvents with low blank value
(<0.001%) shall be used.
5.4.3 Water: Water (Type II) shall be used for rinsing the organic
module and condenser component.
6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
6.1 Because of complexity of this method, field personnel should be
trained 1n and experienced with the test procedures 1n order to obtain
reliable results.
6.2 Laboratory preparation;
6.2.1 All the components shall be maintained and calibrated
according to the procedure described 1n APTD-0576, unless otherwise
specified.
6.2.2 Weigh several 200- to 300-g portions of silica gel 1n
airtight containers to the nearest 0.5 g. Record on each container the
total weight of the silica gel plus containers. As an alternative to
prewelghlng the silica gel, It may Instead be weighed directly 1n the
Implnger or sampling holder just prior to train assembly.
6.2.3 Check filters visually against light for irregularities and
flaws or pinhole leaks. Label the shipping containers (glass Petrl
dishes) and keep the filters 1n these containers at all times except
during sampling and weighing.
6.2.4 Desiccate the filters at 20 + 5.6*C (68 + 10»F) and ambient
pressure for at least 24 hr, and weigh at intervals of~at least 6 hr to a
constant weight (I.e., <0.5-mg change from previous weighing), recording
results to the nearest 0.1 mg. During each weighing the filter must not
be exposed for more than a 2-m1n period to the laboratory atmosphere and
relative humidity above 50%. Alternatively (unless otherwise specified
by the Administrator), the filters may be oven-dried at 105»C (220*F) for
2-3 hr, desiccated for 2 hr, and weighed.
0010 - 10
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Date September 1986
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6.3 Preliminary field determinations:
6.3.1 Select the sampling site and the minimum number of sampling
points according to EPA Method 1 or as specified by the Administrator.
Determine the stack pressure, temperature, and range of velocity heads
using EPA Method 2. It 1s recommended that a leak-check of the pitot
lines (see EPA Method 2, Section 3.1) be performed. Determine the stack-
gas moisture content using EPA Approximation Method 4 or Its alternatives
to establish estimates of isokinetic sampling-rate settings. Determine
the stack-gas dry molecular weight, as described In EPA Method 2, Section
3.6. If Integrated EPA Method 3 sampling 1s used for molecular weight
determination, the Integrated bag sample shall be taken simultaneously
with, and for the same total length of time as, the sample run.
6.3.2 Select a nozzle size based on the range of velocity heads so
that 1t 1s not necessary to change the nozzle size 1n order to maintain
1sok1net1c sampling rates. During the run, do not change the nozzle.
Ensure that the proper differential pressure gauge 1s chosen for the
range of velocity heads encountered (see Section 2.2 of EPA Method 2).
6.3.3 Select a suitable probe Uner and probe length so that all
traverse points can be sampled. For large stacks, to reduce the length
of the probe, consider sampling from opposite sides of the stack.
6.3.4 A minimum of 3 dscm (105.9 dscf) of sample volume 1s required
for the determination of the Destruction and Removal Efficiency (ORE) of
POHCs from incineration systems. Additional sample volume shall be
collected as necessitated by analytical detection limit constraints. To
determine the minimum sample volume required, refer to sample
calculations 1n Section 10.0.
6.3.5 Determine the total length of sampling time needed to obtain
the identified minimum volume by comparing the anticipated average
sampling rate with the volume requirement. Allocate the same time to all
traverse points defined by EPA Method 1. To avoid timekeeping errors,
the length of time sampled at each traverse point should be an Integer or
an integer plus one-half min.
6.3.6 In some circumstances (e.g., batch cycles) 1t may be
necessary to sample for shorter times at the traverse points and to
obtain smaller gas-sample volumes. In these cases, the Administrator's
approval must first be obtained.
6.4 Preparation of collection train;
6.4.1 During preparation and assembly of the sampling train, keep
all openings where contamination can occur covered with Teflon film or
aluminum foil until just prior to assembly or until sampling 1s about to
begin.
0010 - 11
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Date September 1986
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6.4.2 Fill the sorbent trap section of the organic module with
approximately 20 g of clean adsorbent resin. While filling, ensure that
the trap packs uniformly, to eliminate the possibility of channeling.
When freshly cleaned, many adsorbent resins carry a static charge, which
will cause clinging to trap walls. This may be minimized by filling the
trap in the presence of an antistatic device. Commercial antistatic
devices include Model-204 and Model-210 manufactured by the 3M Company,
St. Paul, Minnesota.
6.4.3 If an impinger train is used to collect moisture, place 100
ml of water in each of the first two impingers, leave the third Impinger
empty (or charge with caustic solution, as necessary), and transfer
approximately 200-300 g of prewelghed silica gel from Its container to
the fourth Impinger. More silica gel may be used, but care should be
taken to ensure that it 1s not entrained and carried out from the
Impinger during sampling. Place the container 1n a clean place for later
use in the sample recovery. Alternatively, the weight of the silica gel
plus Impinger may be determined to the nearest 0.5 g and recorded.
6.4.4 Using a tweezer or clean disposable surgical gloves, place a
labeled (Identified) and weighed filter 1n the filter holder. Be sure
that the filter 1s properly centered and the gasket properly placed to
prevent the sample gas stream from circumventing the filter. Check the
filter for tears after assembly 1s completed.
6.4.5 When glass liners are used, Install the selected nozzle using
a V1ton-A 0-r1ng when stack temperatures are <260*C (500*F) and a woven
glass-fiber gasket when temperatures are higher. See APTD-0576 (Rom,
1972) for details. Other connecting systems utilizing either 316
stainless steel or Teflon ferrules may be used. When metal liners are
used, install the nozzle as above, or by a leak-free direct mechanical
connection. Mark the probe with heat-resistant tape or by some other
method to denote the proper distance Into the stack or duct for each
sampling point.
6.4.6 Set up the train as 1n Figure 1. During assembly, do not use
any silicone grease on ground-glass joints that are located upstream of
the organic module. A very light coating of sill cone grease may be used
on all ground-glass joints that are located downstream of the organic
module, but it should be limited to the outer portion (see APTD-0576) of
the ground-glass joints to minimize sillcone-grease contamination.
Subject to the approval of the Administrator, a glass cyclone may be used
between the probe and the filter holder when the total particulate catch
is expected to exceed 100 mg or when water droplets are present in the
stack. The organic module condenser must be maintained at a temperature
of 17 + 3*C. Connect all temperature sensors to an appropriate
potentiometer/display unit. Check all temperature sensors at ambient
temperature.
6.4.7 Place crushed ice around the Impingers and the organic module
condensate knockout.
0010 - 12
Revision
Date September 1986
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6.4.8 Turn on the sorbent module and condenser coll coolant
redrculatlng pump and begin monitoring the sorbent module gas entry
temperature. Ensure proper sorbent module gas entry temperature before
proceeding and again before any sampling 1s Initiated. It 1s extremely
Important that the XAD-2 resin temperature never exceed 50*C (122'F),
because thermal decomposition will occur. During testing, the XAD-2
temperature must not exceed 20*C (68*F) for efficient capture of the
semi volatile species of Interest.
6.4.9 Turn on and set the filter and probe heating systems at the
desired operating temperatures. Allow time for the temperatures to
stabilize.
6.5 Leak-check procedures
6.5.1 Pre-test leak-check:
6.5.1.1 Because the number of additional Intercomponent
connections 1n the Semi-VOST train (over the M5 Train) Increases the
possibility of leakage, a pre-test leak-check 1s required.
6.5.1.2 After the sampling train has been assembled, turn on
and set the filter and probe heating systems at the desired
operating temperatures. Allow time for the temperatures to
stabilize. If a V1ton A 0-r1ng or other leak-free connection 1s
used 1n assembling the probe nozzle to the probe Uner, leak-check
the train at the sampling site by plugging the nozzle and pulling a
381-mm Hg (15-1n. Hg) vacuum.
(NOTE: A lower vacuum may be used, provided that 1t Is not exceeded
during the test.)
6.5.1.3 If an asbestos string 1s used, do not connect the
probe to the train during the leak-check. Instead, leak-check the
train by first attaching a carbon-filled leak-check 1mp1nger (shown
1n Figure 4) to the Inlet of the filter holder (cyclone, 1f applic-
able) and then plugging the Inlet and pulling a 381-mm Hg (15-1n.
Hg) vacuum. (Again, a lower vacuum may be used, provided that 1t 1s
not exceeded during the test.) Then, connect the probe to the train
and leak-check at about 25-mro Hg (l-1n. Hg) vacuum; alternatively,
leak-check the probe with the rest of the sampling train 1n one step
at 381-mm Hg (15-1n. Hg) vacuum. Leakage rates 1n excess of 4X of
the average sampling rate or >0.00057 m3/m1n (0.02 cfm), whichever
1s less, are unacceptable.
6.5.1.4 The following leak-check Instructions for the sampling
train described 1n APVD-0576 and APTD-0581 may be helpful. Start
the pump with fine-adjust valve fully open and coarse-adjust valve
completely closed. Partially open the coarse-adjust valve and
slowly close the fine-adjust valve until the desired vacuum 1s
reached. Do not reverse direction of the fine-adjust valve; this
will cause water to back up Into the organic module. If the desired
vacuum 1s exceeded, either leak-check at this higher vacuum or end
the leak-check, as shown below, and start over.
0010 - 13
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Date September 1986
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CKOSS SECTIQMI
Lt»k Testing Apparatus
2t/12 Fwwlt
«o«1f
|
-------
6.5.1.5 When the leak-check 1s completed, first slowly remove
the plug from the Inlet to the probe, filter holder, or cyclone (1f
applicable). When the vacuum drops to 127 mm (5 1n.) Hg or less,
Immediately close the coarse-adjust valve. Switch off the pumping
system and reopen the fine-adjust valve. Do not reopen the fine-
adjust valve until the coarse-adjust valve has been closed. This
prevents the water 1n the 1mp1ngers from being forced backward Into
the organic module and silica gel from being entrained backward Into
the third 1mp1nger.
6.5.2 Leak-checks during sampling run:
6.5.2.1 If, during the sampling run, a component (e.g., filter
assembly, 1mp1nger, or sorbent trap) change becomes necessary, a
leak-check shall be conducted Immediately after the Interruption of
sampling and before the change is made. The leak-check shall be
done according to the procedure outlined 1n Paragraph 6.5.1, except
that 1t shall be done at a vacuum greater than or equal to the
maximum value recorded up to that point 1n the test. If the leakage
rate 1s found to be no greater than 0.00057 m3/m1n (0.02 cfm) or 4X
of the average sampling rate (whichever 1s less), the results are
acceptable, and no correction will need to be applied to the total
volume of dry gas metered. If a higher leakage rate Is obtained,
the tester shall void the sampling run. (It should be noted that
any "correction" of the sample volume by calculation by calculation
reduces the Integrity of the pollutant concentrations data generated
and must be avoided.)
6.5.2.2 Immediately after a component change, and before
sampling is reinitiated, a leak-check similar to a pre-test leak-
check must also be conducted.
6.5.3 Post-test leak-check:
6.5.3.1 A leak-check 1s mandatory at the conclusion of each
. sampling run. The leak-check shall be done with the same procedures
as those with the pre-test leak-check, except that 1t shall be
conducted at a vacuum greater than or equal to the maximum value
reached during the sampling run. If the leakage rate 1s found to be
no greater than 0.00057 m3/min (0.02 cfm) or 4% of the average
sampling rate (whichever 1s less), the results are acceptable, and
no correction need be applied to the total volume of dry gas
metered. If, however, a higher leakage rate is obtained, the tester
shall either record the leakage rate, correct the sample volume (as
shown 1n the calculation section of this method), and consider the
data obtained of questionable reliability, or void the sampling run.
6.6 Sampling-train operation;
6.6.1 During the sampling run, maintain an 1sok1netic sampling rate
to within 10X of true 1sok1net1c, unless otherwise specified by the
Administrator. Maintain a temperature around the filter of 120 + 14*C
(248 + 25*F) and a gas temperature entering the sorbent trap at a maximum
of 20TC (68'F).
0010 - 15
Revision 0
Date September 1986
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6.6.2 For each run, record the data required on a data sheet such
as the one shown 1n Figure 5. Be sure to record the initial dry-gas
meter reading. Record the dry-gas meter readings at the beginning and
end of each sampling time increment, when changes 1n flow rates are made
before and after each leak-check, and when sampling 1s halted. Take
other readings required by Figure 5 at least once at each sample point
during each time increment and additional readings when significant
changes (20X variation in velocity-head readings) necessitate additional
adjustments 1n flow rate. Level and zero the manometer. Because the
manometer level and zero may drift due to vibrations and temperature
changes, make periodic checks during the traverse.
6.6.3 Clean the stack access ports prior to the test run to
eliminate the chance of sampling deposited material. To begin sampling,
remove the nozzle cap, verify that the filter and probe heating systems
are at the specified temperature, and verify that the pitot tube and
probe are properly positioned. Position the nozzle at the first traverse
point, with the tip pointing directly into the gas stream. Immediately
start the pump and adjust the flow to 1sokinet1c conditions. Nomographs,
which aid in the rapid adjustment of the 1sok1net1c sampling rate without
excessive computations, are available. These nomographs are designed for
use when the Type S pilot-tube coefficient is 0.84 + 0.02 and the stack-
gas equivalent density (dry molecular weight) 1s equal to 29 + 4. APTD-
0576 details the procedure for using the nomographs. If the stack-gas
molecular weight and the pitot-tube coefficient are outside the above
ranges, do not use the nomographs unless appropriate steps (SMgehara,
1974) are taken to compensate for the deviations.
6.6.4 When the stack 1s under significant negative pressure
(equivalent to the height of the Implnger stem), take care to close the
coarse-adjust valve before Inserting the probe into the stack, to prevent
water from backing into the organic module. If necessary, the pump may
be turned on with the coarse-adjust valve closed.
6.6.5 When the probe is 1n position, block off the openings around
the probe and stack access port to prevent unrepresentative dilution of
the gas stream.
6.6.6 Traverse the stack cross section, as required by EPA Method 1
or as specified by the Administrator, being careful not to bump the probe
nozzle into the stack walls when sampling near the walls or when removing
or Inserting the probe through the access port, 1n order to minimize the
chance of extracting deposited material.
6.6.7 During the test run, make periodic adjustments to keep the
temperature around the filter holder and the organic module at the proper
levels; add more ice and, If necessary, salt to maintain a temperature of
<20»C (68»F) at the condenser/silica gel outlet. Also, periodically
check the level and zero of the manometer.
0010 - 16
Revision
Date September 1986
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Plant
location
Operator
Date
Ron Ho.
Sample Boi No.
Meter Box Ho.
Meter W»
C Factor
SchematIr. or Stack Cross Section
PI tot Tube Coefficient Cp
Amhlent Tenderatore
Barometric Pressure ___^____________
Assumed Moisture f
Prohe length. • (ft)
No//le Identification No.
Averaqe Calibrated Nonle Diameter, cm fin)
Prohe Heater Settlnq
leak Rat*. m3/mln. (cfm)
Prohe Liner Material
Static Pressure, mn Mq (In. Hq)
Filter No.
o
o
>-•
o
I
O 70
O> O>
r* <
n -*
o
ft> 3
o
r*
(6
n
CO
en
Traverse Point
Numher
Total
*»er«qe
Sampling
Time
(B) mln.
VKUM
*M Hq
(In. Hq)
Stack
Temperature
4Wi
1
Velocity
Heart
J P>>
mn ( In) H?0
Pressure
ntfferentlal
Across
Orifice
Heter
HI. (H?OJ
( In HpO)
Gas Sample
Volume
«3 Ct3)
Cas Sample Temp.
at Pry f.«s Meter
Inlet Outlet
•CCF) -C(F')
Avq. Avq.
Filter Holder
Temperature
'C(F-)
Temperaturr
of Gas
Enter inn
Sorhet
Trap T.(r')
Temperature
of das
1/MvJnq
Condenser
or last
Impinqer
Figure 5. Partlculatc field data.
-------
6.6.8 If the pressure drop across the filter or sorbent trap
becomes too high, making 1sok1net1c sampling difficult to maintain, the
fllter/sorbent trap may be replaced 1n the midst of a sample run. Using
another complete filter holder/sorbent trap assembly 1s recommended,
rather than attempting to change the filter and resin themselves. After
a new fllter/sorbent trap assembly 1s Installed, conduct a leak-check.
The total particulate weight shall Include the summation of all filter
assembly catches.
6.6.9 A single train shall be used for the entire sample run,
except 1n cases where simultaneous sampling 1s required 1n two or more
separate ducts or at two or more different locations within the same
duct, or 1n cases where equipment failure necessitates a change of
trains. In all other situations, the use of two or more trains will be
subject to the approval of the Administrator.
6.6.10 Note that when two or more trains are used, separate
analysis of the front-half (1f applicable) organic-module and 1mp1nger
(If applicable) catches from each train shall be performed, unless
Identical nozzle sizes were used on all trains. In that case, the front-
half catches from the Individual trains may be combined (as may the
Implnger catches), and one analysis of front-half catch and one analysis
of Implnger catch may be performed.
6.6.11 At the end of the sample run, turn off the coarse-adjust
valve, remove the probe and nozzle from the stack, turn off the pump,
record the final dry-gas meter reading, and conduct a post-test leak-
check. Also, leak-check the pltot lines as described 1n EPA Method 2.
The lines must pass this leak-check 1n order to validate the velocity-
head data.
6.6.12 Calculate percent 1sok1net1c1ty (see Section 10.8) to
determine whether the run was valid or another test run should be made.
7.0 SAMPLE RECOVERY
7.1 Preparation:
7.1.1 Proper cleanup procedure begins as soon as the probe Is
removed from the stack at the end of the sampling period. Allow the
probe to cool. When the probe can be safely handled, wipe off all
external particulate matter near the tip of the probe nozzle and place a
cap over the tip to prevent losing or gaining particulate matter. Do not
cap the probe tip tightly while the sampling train 1s cooling down
because this will create a vacuum 1n the filter holder, drawing water
from the 1mp1ngers Into the sorbent module.
7.1.2 Before moving the sample train to the cleanup site, remove
the probe from the sample train and cap the open outlet, being careful
not to lose any condensate that might be present. Cap the filter Inlet.
0010 - 18
Revision
Date September 1986
-------
Remove the umbilical cord from the last Impinger and cap the 1mp1nger.
If a flexible line 1s used between the organic module and the filter
holder, disconnect the line at the filter holder and let any condensed
water or liquid drain Into the organic module.
7.1.3 Cap the filter-holder outlet and the Inlet to the organic
module. Separate the sorbent trap section of the organic module from the
condensate knockout trap and the gas-conditioning section. Cap all
organic module openings. Disconnect the organic-module knockout trap
from the Impinger train Inlet and cap both of these openings. Ground-
glass stoppers, Teflon caps, or caps of other Inert materials may be used
to seal all openings.
7.1.4 Transfer the probe, the filter, the organic-module
components, and the impinger/condenser assembly to the cleanup area.
This area should be clean and protected from the weather to minimize
sample contamination or loss.
7.1.5 Save a portion of all washing solutions (methanol/methylene
chloride, Type II water) used for cleanup as a blank. Transfer 200 ml of
each solution directly from the wash bottle being used and place each 1n
a separate, prelabeled glass sample container.
7.1.6 Inspect the train prior to and during disassembly and note
any abnormal conditions.
7.2 Sample containers;
7.2.1 Container no. 1: Carefully remove the filter from the filter
holder and place 1t 1n Its Identified Petrl dish container. Use a pair
or pairs of tweezers to handle the filter. If 1t 1s necessary to fold
the filter, ensure that the partlculate cake 1s Inside the fold.
Carefully transfer to the Petrl dish any partlculate matter or filter
fibers that adhere to the filter-holder gasket, using a dry nylon bristle
brush or sharp-edged blade, or both. Label the container and seal with
l-1n.-wide Teflon tape around the circumference of the I1d.
7.2.2 Container no. 2: Taking care that dust on the outside of the
probe or other exterior surfaces does not get Into the sample,
quantitatively recover partlculate matter or any condensate from the
probe nozzle, probe fitting, probe liner, and front half of the filter
holder by washing these components first with, methanol/methylene chloride
(1:1 v/v) into a glass container. Distilled water may also be used.
Retain a water and solvent blank and analyze in the same manner as with
the samples. Perform rinses as follows:
7.2.2.1 Carefully remove the probe nozzle and clean the Inside
surface by rinsing with the solvent mixture (1:1 v/v methanol/-
methylene chloride) from a wash bottle and brushing with a nylon
bristle brush. Brush until the Hnse shows no visible particles;
then make a final rinse of the Inside surface with the solvent mix.
Brush and rinse the Inside parts of the Swagelok fitting with the
solvent mix in a similar way until no visible particles remain.
0010 - 19
Revision 0
Date September 1986
-------
7.2.2.2 Have two people rinse the probe Uner with the solvent
mix by tilting and rotating the probe while squirting solvent Into
Its upper end so that all Inside surfaces will be wetted with
solvent. Let the solvent drain from the lower end Into the sample
container. A glass funnel may be used to aid 1n transferring liquid
washes to the container.
7.2.2.3 Follow the solvent rinse with a probe brush. Hold the
probe in an Inclined position and squirt solvent Into the upper end
while pushing the probe brush through the probe with a twisting
action; place a sample container underneath the lower end of the
probe and catch any solvent and particulate matter that 1s brushed
from the probe. Run the brush through the probe three times or more
until no visible particulate matter 1s carried out with the solvent
or until none remains 1n the probe Uner on visual Inspection^ With
stainless steel or other metal probes, run the brush through 1n the
above-prescribed manner at least six times (metal probes have small
crevices In which partlculate matter can be entrapped). Rinse the
brush with solvent and quantitatively collect these washings 1n the
sample container. After the brushing, make a final solvent rinse of
the probe as described above.
7.2.2.4 It 1s recommended that two people work together to
clean the probe to minimize sample losses. Between sampling runs,
keep brushes clean and protected from contamination.
7.2.2.5 Clean the Inside of the front half of the filter
holder and cyclone/cyclone flask, 1f used, by rubbing the surfaces
with a nylon bristle brush and rinsing with methanol/methylene
chloride (1:1 v/v) mixture. Rinse each surface three times or more
1f needed to remove visible partlculate. Make a final rinse of the
brush and filter holder. Carefully rinse out the glass cyclone and
cyclone flask (1f applicable). Brush and rinse any partlculate
material adhering to the Inner surfaces of these components Into the
front-half rinse sample. After all solvent washings and partlculate
matter have been collected In the sample container, tighten the lid
on the sample container so that solvent will not leak out when 1t Is
shipped to the laboratory. Mark the height of the fluid level to
determine whether leakage occurs during transport. Label the
container to identify Its contents.
7.2.3 Container no. 3: The sorbent trap section of the organic
module may be used as a sample transport container, or the spent resin
may be transferred to a separate glass bottle for shipment. If the
sorbent trap Itself 1s used as the transport container, both ends should
be sealed with tightly fitting caps or plugs. Ground-glass stoppers or
Teflon caps may be used. The sorbent trap should then be labeled,
covered with aluminum foil, and packaged on ice for transport to the
laboratory. If a separate bottle 1s used, the spent resin should be
quantitatively transferred from the trap Into the clean bottle. Resin
that adheres to the walls of the trap should be recovered using a rubber
policeman or spatula and added to this bottle.
0010 - 20
Revision 0
Date September 1986
-------
7.2.4 Container no. 4: Measure the volume of condensate collected
in the condensate knockout section of the organic module to within +1 ml
by using a graduated cylinder or by weighing to within +0.5 g using a
triple-beam balance. Record the volume or weight, of liquid present and
note any discoloration or film in the liquid catch. Transfer this liquid
to a prelabeled glass sample container. Inspect the back half of the
filter housing and the gas-cond1t1on1ng section of the organic module.
If condensate is observed, transfer it to a graduated or weighing bottle
and measure the volume, as described above. Add this material to the
condensate knockout-trap catch.
7.2.5 Container no. 5: All sampling train components located
between the high-efficiency glass- or quartz-fiber filter and the first
'wet Impinger or the final condenser system (including the heated Teflon
line connecting the filter outlet to the condenser) should be thoroughly
rinsed with methanol/methylene chloride (1:1 v/v) and the rinsings
combined. This rinse shall be separated from the condensate. If the
spent resin is transferred from the sorbent trap to a separate sample
container for transport, the sorbent trap shall be thoroughly rinsed
until all sample-wetted surfaces appear clean. Visible films should be
removed by brushing. Whenever train components are brushed, the brush
should be subsequently rinsed with solvent mixture and the rinsings added
to this container.
7.2.6 Container no. 6: Note the color of the Indicating silica gel
to determine if 1t has been completely spent and make a notation of its
condition. Transfer the silica gel from the fourth impinger to its
original container and seal. A funnel may make it easier to pour the
silica gel without spilling. A rubber policeman may be used as an aid in
removing the silica gel from the impinger. It is not necessary to remove
the small amount of dust particles that may adhere strongly to the
Impinger wall. Because the gain in weight 1s to be used for moisture
calculations, do not use any water or other liquids to transfer the
silica gel. If a balance is available in the field, weigh the container
and Its contents to 0.5 g or better.
7.3 Impinger water;
7.3.1 Make a notation of any color or film 1n the liquid catch.
Measure the liquid 1n the first three impingers to within ±1 ml by using
a graduated cylinder or by weighing 1t to within +0.5 g by using a
balance (1f one 1s available). Record the volume or weight of liquid
present. This information is required to calculate the moisture content
of the effluent gas.
7.3.2 Discard the liquid after measuring and recording the volume
or weight, unless analysis of the Impinger catch 1s required (see
Paragraph 4.1.3.7). Amber glass containers should be used for storage of
Impinger catch, if required.
7.3.3 If a different type of condenser is used, measure the amount
of moisture condensed either volumetrlcally or gravimetrically.
0010 - 21
Revision 0
Date September 1986
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7.4 Sample preparation for shipment; Prior to shipment, recheck all
sample centalners to ensure that the capsare well secured. Seal the lids of
all containers around the circumference with Teflon tape. Ship all liquid
samples upright on 1ce and all partlculate filters with the paniculate catch
facing upward. The paniculate filters should be shipped unrefrlgerated.
8.0 ANALYSIS
8.1 Sample preparation;
8.1.1 General: The preparation steps for all samples will result
1n a finite volume of concentrated solvent. The final sample volume
(usually 1n the 1- to 10-mL range) 1s then subjected to analysis by
GC/MS. All samples should be Inspected and the appearance documented.
All samples are to be spiked with surrogate standards as received from
the field prior to any sample manipulations. The spike should be at a
level equivalent to 10 times the MDL when the solvent 1s reduced 1n
volume to the desired level (I.e., 10 ml). The spiking compounds should
be the stable 1 sotopically labeled analog of the compounds of Interest or
a compound that would exhibit properties similar to the compounds of
Interest, be easily chromatographed, and not Interfere with the analysis
of the compounds of Interest. Suggested surrogate spiking compounds are:
deuterated naphthalene, chrysene, phenol, nitrobenzene, chlorobenzene,
toluene, and carbon-13-labeled pentachlorophenol.
8.1.2 Condensate: The "condensate" 1s the moisture collected 1n
the first 1mp1nger following the XAD-2 module. Spike the condensate with
the surrogate standards. The volume 1s measured and recorded and then
transferred to a separatory funnel. The pH 1s to be adjusted to pH 2
with 6 N sulfuric add, if necessary. The sample container and graduated
cylinder are sequentially rinsed with three successive 10-mL allquots of
the extraction solvent and added to the separatory funnel. The ratio of
solvent to aqueous sample should be maintained at 1:3. Extract the
sample by vigorously shaking the separatory funnel for 5 m1n. After
complete separation of the phases, remove the solvent and transfer to a
Kuderna-Dan1sh concentrator (K-D), filtering through a bed of precleaned,
dry sodium sulfate. Repeat the extraction step two additional times.
Adjust the pH to 11 with 6 N sodium hydroxide and reextract combining the
add and base extracts. Rinse the sodium sulfate into the K-D with fresh
solvent and discard the desiccant. Add Teflon boiling chips and
concentrate to 10 mL by reducing the volume to slightly less than 10 mL
and then bringing to volume with fresh solvent. In order to achieve the
necessary detection limit, the sample volume can be further reduced to 1
mL by using a micro column K-D or nitrogen blow-down. Should the sample
start to exhibit precipitation, the concentration step should be stopped
and the sample redissolved with fresh solvent taking the volume to some
finite amount. After adding a standard (for the purpose of quantltatlon
by GC/MS), the sample is ready for analysis, as discussed 1n Paragraph
8.2.
0010 - 22
Revision
Date September 1986
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8.1.3 Implnger: Spike the sample with the surrogate standards;
measure and record the volume and transfer to a separatory funnel.
Proceed as described 1n Paragraph 8.1.2.
8.1.4 XAD-2: Spike the resin directly with the surrogate
standards. Transfer the resin to the all-glass thimbles by the following
procedure (care should be taken so as not to contaminate the thimble by
touching 1t with anything other than tweezers or other solvent-rinsed
mechanical holding devices). Suspend the XAD-2 module directly over the
thimble. The glass frit of the module (see Figure 2) should be 1n the up
position. The thimble 1s contained 1n a clean beaker, which will serve
to catch the solvent rinses. Using a Teflon squeeze bottle, flush the
XAD-2 Into the thimble. Thoroughly rinse the glass module with solvent
Into the beaker containing the thimble. Add the XAD-2 glass-wool plug to
the thimble. Cover the XAD-2 1n the thimble with a precleaned glass-wool
plug sufficient to prevent the resin from floating Into the solvent
reservoir of the extractor. If the resin 1s wet, effective extraction
can be accomplished by loosely packing the resin in the thimble. If a
question arises concerning the completeness of the extraction, a second
extraction, without a spike, 1s advised. The thimble 1s placed 1n the
extractor and the rinse solvent contained 1n the beaker 1s added to the
solvent reservoir. Additional solvent 1s added to make the reservoir
approximately two-thirds full. Add .Teflon boiling chips and assemble the
apparatus. Adjust the heat source to cause the extractor to cycle 5-6
times per hr. Extract the resin for 16 hr. Transfer the solvent and
three 10-mL rinses of the reservoir to a K-D and concentrate as described
1n Paragraph 8.1.2.
8.1.5 Parti oil ate filter (and cyclone catch): If partlculate
loading 1s to be determined, weigh the filter (and cyclone catch, If
applicable). The partlculate filter (and cyclone catch, 1f applicable)
1s transferred to the glass thimble and extracted simultaneously with the
XAD-2 resin.
8.1.6 Train solvent rinses: All train rinses (I.e., probe,
Implnger, filter housing) using the extraction solvent and methanol are
returned to the laboratory as a single sample. If the rinses are
contained 1n more than one container, the Intended spike Is divided
equally among the containers proportioned from a single syringe volume.
Transfer the rinse to a separatory funnel and add a sufficient amount of
organic-free water so that the methylene chloride becomes Immiscible and
Its volume no longer Increases with the addition of more water. The
extraction and concentration steps are then performed as described 1n
Paragraph 8.1.2.
8.2 Sample analysis;
8.2.1 The primary analytical tool for the measurement of emissions
from hazardous waste Incinerators 1s GC/MS using fused-s1!1ca capillary
GC columns, as described In Method 8270 1n Chapter Four of this manual.
Because of the nature of GC/MS Instrumentation and the cost associated
0010 - 23
Revision
Date September 1986
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with sample analysis, prescreenlng of the sample extracts by gas
chromatography/flame lonization detection (GC/FID) or with electron
capture (GC/ECD) is encouraged. Information regarding the complexity and
concentration level of a sample prior to GC/MS analysis can be of
enormous help. This Information can be obtained by using either
capillary columns or less expensive packed columns. However, the FID
screen should be performed with a column similar to that used with the
GC/MS. Keep 1n mind that GC/FID has a slightly lower detection limit
than GC/MS and, therefore, that the concentration of the sample can be
adjusted either up or down prior to analysis by GC/MS.
8.2.2 The mass spectrometer will be operated 1n a full scan (40-
450) mode for most of the analyses. The range for which data are
acquired in a GC/MS run will be sufficiently broad to encompass the major
ions, as listed In Chapter Four, Method 8270, for each of the designated
POHCs in an incinerator effluent analysis.
8.2.3 For most purposes, electron lonization (El) spectra will be
collected because a majority of the POHCs give reasonable El spectra.
Also, El spectra are compatible with the NBS Library of Mass Spectra and
other mass spectral references, which aid 1n the identification process
for other components in the incinerator process streams.
8.2.4 To clarify some Identifications, chemical lonization (CI)
spectra using either positive ions or negative ions will be used to
elucidate molecular-weight information and simplify the fragmentation
patterns of some compounds. In no case, however, should CI spectra alone
be used for compound identification. Refer to Chapter Four, Method 8270,
for complete descriptions of GC conditions, MS conditions, and
quantitative and quantitative identification.
9.0 CALIBRATION
9.1 Probe nozzle: Probe nozzles shall be calibrated before their
initial use in the field. Using a micrometer, measure the inside diameter of
the nozzle to the nearest 0.025 mm (0.001 in.). Make measurements at three
separate places across the diameter and obtain the average of the
measurements. The difference between the high and low numbers shall not
exceed 0.1 mm (0.004 in.). When nozzles become nicked, dented, or corroded,
they shall be reshaped, sharpened, and recalibrated before use. Each nozzle
shall be permanently and uniquely Identified.
9.2 Pi tot tube; The Type S pltot tube assembly shall be calibrated
according to the procedure outlined in Section 4 of EPA Method 2, or assigned
a nominal coefficient of 0,84 if 1t is not visibly nicked, dented, or corroded
and if it meets design and intercomponent spacing specifications.
0010 - 24
Revision
Date September 1986
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9.3 Metering system;
9.3.1 Before Its Initial use In the field, the metering system
shall be calibrated according to the procedure outlined 1n APTD-0576.
Instead of physically adjusting the dry-gas meter dial readings to
correspond to the wet-test meter readings, calibration factors may be
used to correct the gas meter dial readings mathematically to the proper
values. Before calibrating the metering system, 1t is suggested that a
leak-check be conducted. For metering systems having diaphragm pumps,
the normal leak-check procedure will not detect leakages within the pump.
For these cases the following leak-check procedure is suggested: Make a
10-min calibration run at 0.00057 m3/min (0.02 cfm); at the end of the
run, take the difference of the measured wet-test and dry-gas meter
volumes and divide the difference by 10 to get the leak rate. The leak
rate should not exceed 0.00057 m3/min (0.02 cfm).
9.3.2 After each field use, the calibration of the metering system
shall be checked by performing three calibration runs at a single
intermediate orifice setting (based on the previous field test). The
vacuum shall be set at the maximum value reached during the test series.
To adjust the vacuum, insert a valve between the wet-test meter and the
inlet of the metering system. Calculate the average value of the
calibration factor. If the calibration has changed by more than 5%,
recalibrate the meter over the full range of orifice settings, as
outlined 1n APTD-0576.
9.3.3 Leak-check of metering system: That portion of the sampling
train from the pump to the orifice meter (see Figure 1) should be leak-
checked prior to Initial use and after each shipment. Leakage after the
pump will result in less volume being recorded than is actually sampled.
The following procedure is suggested (see Figure 6): Close the main
valve on the meter box. Insert a one-hole rubber stopper with rubber
tubing attached into the orifice exhaust pipe. Disconnect and vent the
low side of the orifice manometer. Close off the low side orifice tap.
Pressurize the system to 13-18 cm (5-7 in.) water column by blowing into
the rubber tubing. Pinch off the tubing and observe the manometer for 1
min. A loss of pressure on the manometer indicates a leak in the meter
box. Leaks, if present, must be corrected.
NOTE: If the dry-gas-meter coefficient values obtained before and after
a test series differ by >5%, either the test series shall be
voided or calculations for test series shall be performed using
whichever meter coefficient value (i.e., before or after) gives
the lower value of total sample volume.
9.4 Probe heater: The probe-heating system shall be calibrated before
its initial use in the field according to the procedure outlined 1n APTD-0576.
Probes constructed according to APTD-0581 need not be calibrated if the
calibration curves in APTD-0576 are used.
0010 - 25
Revision 0
Date September 1986
-------
o
o
I-*
o
I
M
01
RUBBER
TUBING
RUBBER
STOPPER
ORIFICE
BY PASS VALVE
VACUUM
GAUGE
HOW INTO TUIINC
UNTIL MAKOMf UN
MIADSSTOHNCHIS
WATIMCOIUMN
•3 30
V A
t- <
D •*
VI
/> O
o a
omnci
MANOMtTEM
MAIN VALVE CLOSED
AIR-TIGHT
PUMP
Figure 6. Leak-check of meter box.
D
-------
9.5 Temperature gauges: Each thermocouple must be permanently and
uniquely marked onthe casting; all mercury-1n-glass reference thermometers
must conform to ASTM E-l 63C or 63F specifications. Thermocouples should be
calibrated 1n the laboratory with and without the use of extension leads. If
extension leads are used 1n the field, the thermocouple readings at ambient
air temperatures, with and without the extension lead, must be noted and
recorded. Correction 1s necessary 1f the use of an extension lead produces a
change >1.5X.
9.5.1 Implnger, organic module, and dry-gas meter thermocouples:
For the thermocouples used to measure the temperature of the gas leaving
the Implnger train and the XAD-2 resin bed, three-point calibration at
Ice-water, room-air, and boiling-water temperatures 1s necessary. Accept
the thermocouples only 1f the readings at all three temperatures agree to
+2*C (3.6*F) with those of the absolute value of the reference
thermometer.
9.5.2 Probe and stack thermocouple: For the thermocouples used to
Indicate the probe and stack temperatures, a three-point calibration at
Ice-water, boiling-water, and hot-oil-bath temperatures must be
performed; 1t Is recommended that room-air temperature be added, and that
the thermometer and the thermocouple agree to within 1.5X at each of the
calibration points. A calibration curve (equation) may be constructed
(calculated) and the data extrapolated to cover the entire temperature
range suggested by the manufacturer.
9.6 Barometer; Adjust the barometer Initially and before each test
series to agree to within +25 mm Hg (0.1 1n. Hg) of the mercury barometer or
the corrected barometric pressure value reported by a nearby National Weather
Service Station (same altitude above sea level).
9.7 Triple-beam balance; Calibrate the triple-beam balance before each
test series, using Class-S standard weights; the weights must be within +0.5%
of the standards, or the balance must be adjusted to meet these limits.
10.0 CALCULATIONS
10.1 Carry out calculations. Round off figures after the final
calculation to the correct number of significant figures.
10.2 Nomenclature;
An =* Cross-sectional area of nozzle, m2 (ft2).
Bws = Water vapor 1n the gas stream, proportion by volume.
Cd - Type S pltot tube coefficient (nominally 0.84 + 0.02),
dlmensionless.
I = Percent of 1sok1net1c sampling.
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La « Maximum acceptable leakage rate for a leak-check, either pre-test
or following a component change; equal to 0.00057 m3/m1n (0.02
cfm) or 4X of the average sampling rate, whichever 1s less.
l_i = Individual leakage rate observed during the leak-check conducted
prior to the "itn» component change (1 = 1, 2, 3...n) m3/m1n
(cfm).
LD - Leakage rate observed during the post-test leak-check, m3/min
H (cfm).
Md * Stack-gas dry molecular weight, g/g-mole (Ib/lb-mole).
Mw - Molecular weight of water, 18.0 g/g-mole (18.0 Ib/lb-mole).
Pbar s Barometric pressure at the sampling site, mm Hg (In. Hg).
Ps = Absolute stack-gas pressure, mm Hg (In. Hg).
Pstd = Standard absolute pressure, 760 mm Hg (29.92 1n. Hg).
R = Ideal gas constant, 0.06236 mm Hg-m3/K-g-mole (21.85 1n.
Hg-ft3/'R-lb-mole).
Tro = Absolute average dry-gas meter temperature (see Figure 6), K
CR).
Ts = Absolute average stack-gas temperature (see Figure 6), K (*R).
Tstd z Standard absolute temperature, 293K (528*R).
Vic = Total volume of liquid collected 1n the organic module condensate
knockout trap, the 1mp1ngers, and silica gel, ml.
Vra = Volume of gas sample as measured by dry-gas meter, dscm (dscf).
vm(std) = Volume of gas sample measured by the dry-gas meter, corrected
to standard conditions, dscm (dscf).
vw(std) s Volume of water vapor 1n the gas sample, corrected to standard
conditions, son (scf).
Vs = Stack-gas velocity, calculated by Method 2, Equation 2-9, using
data obtained from Method 5, m/sec (ft/sec).
Wa = Weight of residue in acetone wash, mg.
7 = Dry-gas-meter calibration factor, dimensionless.
AH = Average pressure differential across the orifice meter (see
Figure 2), mm H£0 (1n. H20).
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/>w = Density of water, 0.9982 g/mL (0.002201 Ib/mL).
8 = Total sampling time, m1n.
BI = Sampling time Interval from the beginning of a run until the
first component change, m1n.
61 = Sampling time Interval between two successive component
changes, beginning with the interval between the first and
second changes, min.
Bn = Sampling time Interval from the final (ntn) component change
until the end of the sampling run, min.
13.6 = Specific gravity of mercury.
60 = sec/mi n.
100 = Conversion to percent.
10.3 Average dry-gas-meter temperature and average orifice pressure
drop; See data sheet (Figure 5, above).
10.4 Dry-gas volume; Correct the sample measured by the dry-gas meter
to standard conditions [20*C, 760 mm Hg [68'F, 29.92 in. HgJ) by using
Equation 1:
Tstd "W + 4H/13'6 Pbar * 4H/13'6
' V —, -- r- --
Tm pstd Tm
where;
KI = 0.3858 K/mm Hg for metric units, or
K! = !7.64*R/1n. Hg for English units.
It should be noted that Equation 1 can be used as written, unless the leakage
rate observed during any of the mandatory leak-checks (I.e., the post-test
leak-check or leak-checks conducted prior to component changes) exceeds La.
If Lp or Lj exceeds La, Equation 1 must be modified as follows:
a. Case I (no component changes made during sampling run): Replace Vm
1n Equation 1 with the expression:
Vm - (L - La)
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b. Case II (one or more component changes made during the sampling
run): Replace Vm 1n Equation 1 by the expression:
- '4 - L.'8l - el - S * L»)9
and substitute only for those leakage rates (LI or LD) that exceed
La-
10.5 Volume of water vapor;
Pw RTstd
Vw(std) " Vlc 7 — - K2 Vic (2)
Mw pstd
where:
K2 * 0.001333 m3/mL for metric units, or
Kg • 0.04707 ft3/mL for English units.
10.6 Moisture content;
Vw(std)
Bws - - (3)
Vm(std) * Vw(std)
NOTE: In saturated or water-droplet-laden gas streams, two calculations
of the moisture content of the stack gas shall be made, one from
the Impinger analysis (Equation 3) and a second from the
assumption of saturated conditions. The lower of the two values
of By, shall be considered correct. The procedure for determining
the moisture content based upon assumption of saturated conditions
1s given 1n the Note to Section 1.2 of Method 4. For the purposes
of this method, the average stack-gas temperature from Figure 6
may be used to make this determination, provided that the accuracy
of the 1n-stack temperature sensor 1s +1*C (2*F).
10.7 Conversion factors;
From To Multiply by
scT" in3" 0.02832
g/ft3 gr/ft3 15.43
g/ft3 lb/ft3 2.205 x 10~3
g/ft3 g/m3 35.31
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where:
10.8 Isok1net1c variation:
10.8.1 Calculation from raw data:
100 Ts[K3Flc + (Vra/Tm) (Pbar + AH/13.6)]
I (4)
608VsPsAn
KS » 0.003454 mm Hg-m3/mL-K for metric units, or
K3 = 0.002669 1n. Hg-ft3/mL-*R for English units.
10.8.2 Calculation for Intermediate values:
T TsVmfStd)Pstd100
•*• — T II QA D <*rT/"1 ~D"~ ~ \
OM r DU(1"D J
5 n s ws (5)
TsVm(std)
where:
<4 = 4.320 for metric units, or
K4 = 0.09450 for English units.
10.8.3 Acceptable results: If 90% £ I £ 110%, the results are
acceptable. If the results are low 1n comparison with the standard and
I 1s beyond the acceptable range, or 1f I 1s less than 90%, the
Administrator may opt to accept the results.
10.9 To determine the minimum sample volume that shall be collected, the
following sequence of calculations shall be used.
10.9.1 From prior analysis of the waste feed, the concentration of
POHCs Introduced Into the combustion system can be calculated. The
degree of destruction and removal efficiency that 1s required 1s used to
determine the maximum amount of POHC allowed to be present 1n the
effluent. This may be expressed as:
(WF) (POHC1 cone) (100-%DRE)
= Max POHC, Mass (6)
100 100
where:
WF = mass flow rate of waste feed per hr, g/hr (Ib/hr).
POHCj = concentration of Principal Organic Hazardous Compound (wt %)
Introduced Into the combustion process.
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ORE = percent Destruction and Removal Efficiency required.
Max POHC * mass flow rate (g/hr [lb/hr]) of POHC emitted from the
combustion source.
10.9.2 The average discharge concentration of the POHC 1n the
effluent gas 1s determined by comparing the Max POHC with the volumetric
flow rate being exhausted from the source. Volumetric flow rate data are
available as a result of preliminary Method 1-4 determinations:
Max POHC, Mass
- = Max POHC1 cone (7)
DVeff(std)
where:
DVeff(std) * volumetric flow rate of exhaust gas, dscm (dscf).
POHCi cone » anticipated concentration of the POHC 1n the
exhaust gas stream, g/dscm (Ib/dscf).
10.9.3 In making this calculation, 1t 1s recommended that a safety
margin of at least ten be Included:
LDLpOHC x 10
VTBC
•0\,
1 cone
where :
LDLpoHC = detectable amount of POHC 1n entire sampling train.
NOTE: The whole extract from an XAD-2 cartridge 1s seldom 1f ever,
Injected at once. Therefore, 1f all quoting factors are
Involved, the LDLpgHC 1s not the same as the analytical (or
column) detection limit.
VTBC = minimum dry standard volume to be collected at dry-gas
meter.
10.10 Concentration of any given POHC 1n the gaseous emissions of a
combustion process;
1) Multiply the concentration of the POHC as determined 1n Method 8270
by the final concentration volume, typically 10 ml.
CPOHC (ug/mL) x sample volume (ml) = amount (ug) of POHC 1n sample (9)
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where:
CPOHC = concentration of POHC as analyzed by Method 8270.
2) Sum the amount of POHC found 1n all samples associated with a single
train.
Total (ug) = XAD-2 (ug) + condensate (ug) + rinses (ug) + 1mp1nger (ug) (10)
3) Divide the total ug found by the volume of stack gas sampled (m3).
(Total ug)/ (train sample volume) = concentration of POHC (ug/m3) (11)
11.0 QUALITY CONTROL
11.1 Sampling; See EPA Manual 600/4-77-027b for Method 5 quality
control .
11.2 Analysis; The quality assurance program required for this study
Includes the analysis of field and method blanks, procedure validations,
incorporation of stable labeled surrogate compounds, quant 1tat1 on versus
stable labeled internal standards, capillary column performance checks, and
external performance tests. The surrogate spiking compounds selected for a
particular analysis are used as primary Indicators of the quality of the
analytical data for a wide range of compounds and a variety of sample
matrices. The assessment of combustion data, positive Identification, and
quantltatlon of the selected compounds are dependent on the Integrity of the
samples received and the precision and accuracy of the analytical methods
employed. The quality assurance procedures for this method are designed to
monitor the performance of the analytical method and to provide the required
information to take corrective action 1f problems are observed in laboratory
operations or 1n field sampling activities.
11.2.1 Field Blanks: Field blanks must be submitted with the
samples collected at each sampling site. The field blanks Include the
sample bottles containing allquots of sample recovery solvents, unused
filters, and resin cartridges. At a minimum, one complete sampling train
will be assembled in the field staging area, taken to the sampling area,
and leak-checked at the beginning and end of the testing (or for the same
total number of times as the actual test train). The filter housing and
probe of the blank train will be heated during the sample test. The
train will be recovered as if 1t were an actual test sample. No gaseous
sample will be passed through the sampling train.
11.2.2 Method blanks: A method blank must be prepared for each set
of analytical operations, to evaluate contamination and artifacts that
can be derived from glassware, reagents, and sample handling 1n the
laboratory.
11.2.3 Refer to Method 8270 for additional quality control
considerations.
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12.0 METHOD PERFORMANCE
12.1 Method performance evaluation; Evaluation of analytical procedures
for a selectedseriesofcompounds must Include the sample-preparation
procedures and each associated analytical determination. The analytical
procedures should be challenged by the test compounds spiked at appropriate
levels and carried through the procedures.
12.2 Method detection limit; The overall method detection limits (lower
and upper)mustbedetermined on a compound-by-compound basis because
different compounds may exhibit different collection, retention, and
extraction efficiencies as well as Instrumental minimum detection limit (MDL).
The method detection limit must be quoted relative to a given sample volume.
The upper limits for the method must be determined relative to compound
retention volumes (breakthrough).
12.3 Method precision and bias; The overall method precision and bias
must be determined onacompound-by-compound basis at a given concentration
level. The method precision value would Include a combined variability due to
sampling, sample preparation, and Instrumental analysis. The method bias
would be dependent upon the collection, retention, and extraction efficiency
of the train components. From evaluation studies to date using a dynamic
spiking system, method biases of -13X and -16X have been determined for
toluene and 1,1,2,2-tetrachloroethane, respectively. A precision of 19.9% was
calculated from a field test data set representing seven degrees of freedom
which resulted from a series of paired, unspiked Semivolatile Organic Sampling
trains (Semi-VOST) sampling emissions from a hazardous waste incinerator.
13.0 REFERENCES
1. Addendum to Specifications for Incinerator Testing at Federal Facilities,
PHS, NCAPC, December 6, 1967.
2. Bursey, J., Homolya, J., McAllister, R., and McGangley, J., Laboratory
and Field Evaluation of the Semi-VOST Method, Vols. 1 and 2, U.S.
Environmental Protection Agency, EPA/600/4-851/075A, 075B (1985).
3. Martin, R.M., Construction Details of Isoklnetic Source-Sampling
Equipment, Research Triangle Park, NC, U.S. Environmental Protection Agency,
April 1971, PB-203 060/BE, APTD-0581, 35 pp.
4. Rom, J.J., Maintenance, Calibration, and Operation of Isokinetic Source-
Sampling Equipment, Research Triangle Park, NC, U.S. Environmental Protection
Agency, March 1972, PB-209 022/BE, APTD-0576, 39 pp.
5. Schlickenrieder, L.M., Adams, J.W., and Thrun, K.E., Modified Method 5
Train and Source Assessment Sampling System: Operator's Manual, U.S.
Environmental Protection Agency, EPA/600/8-85/003, (1985).
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6. Shlgehara, R.T., Adjustments 1n the EPA Nomography for Different P1tot
Tube Coefficients and Dry Molecular Weights, Stack Sampling News, 2:4-11
(October 1974).
C 7. U.S. Environmental Protection Agency, CFR 40 Part 60, Appendix A, Methods
A" 3 •
8. Vollaro, R.F., A Survey of Commercially Available Instrumentation for the
Measurement of Low-Range Gas Velocities, Research Triangle Park, NC, U.S.
Environmental Protection Agency, Emissions Measurement Branch, November 1976
(unpublished paper).
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METHOD 0010, APPENDIX A
PREPARATION OF XAD-2 SORBENT RESIN
1.0 SCOPE AND APPLICATION
1.1 XAD-2 resin as supplied by the manufacturer 1s Impregnated with a
bicarbonate solution to Inhibit mlcroblal growth during storage. Both the
salt solution and any residual extractable monomer and polymer species must be
removed before use. The resin 1s prepared by a series of water and organic
extractions, followed by careful drying.
2.0 EXTRACTION
2.1 Method 1:
extractor.
The procedure may be carried out 1n a giant Soxhlet
An all-glass thimble containing an extra-coarse frit 1s used for
extraction of XAD-2. The frit is recessed 10-15 mm above a crenellated ring
at the bottom of the thimble to facilitate drainage. The resin must be
carefully retained in the extractor cup with a glass-wool plug and stainless
steel screen because 1t floats on methylene chloride.. This process Involves
sequential extraction in the following order.
Solvent
Water
Water
Methyl alcohol
Methylene chloride
Methylene chloride (fresh)
2.2 Method 2:
Procedure
Initial rinse: Place resin 1n a beaker,
rinse once with Type II water, and
discard. Fill with water a second time,
let stand overnight, and discard.
Extract with H20 for 8 hr.
Extract for 22 hr.
Extract for 22 hr.
Extract for 22 hr.
2.2.1 As an alternative to Soxhlet extraction, a continuous
extractor has been fabricated for the extraction sequence. This extractor has
been found to be acceptable. The particular canister used for the apparatus
shown in Figure A-l contains about 500 g of finished XAD-2. Any size may be
constructed; the choice is dependent on the needs of the sampling programs.
The XAD-2 is held under light spring tension between a pair of coarse and fine
screens. Spacers under the bottom screen allow for even distribution of clean
solvent. The three-necked flask should be of sufficient size (3-Hter In this
case) to hold solvent
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: 0.22 en Union
Ttflon Gvtktt
teaming
Coant ^l«u
ftneScrwn
Drain
Optional Pump
Figure A-1. XAD-2 cleanup extraction apparatus.
0010 - A - 2
cinn
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equal to twice the dead volume of the XAD-2 canister. Solvent 1s refluxed
through the Snyder column, and the distillate Is continuously cycled up
through the XAD-2 for extraction and returned to the flask. The flow 1s
maintained upward through the XAD-2 to allow maximum solvent contact and
prevent channeling. A valve at the bottom of the canister allows removal of
solvent from the canister between changes.
2.2.2 Experience has shown that 1t 1s very difficult to cycle
sufficient water 1n this mode. Therefore the aqueous rinse 1s accomplished by
simply flushing the canister with about 20 liters of distilled water. A small
pump may be useful for pumping the water through the canister. The water
extraction should be carried out at the rate of about 20-40 mL/m1n.
2.2.3 After draining the water, subsequent methyl alcohol and
methylene chloride extractions are carried out using the refluxlng apparatus.
An overnight or 10- to 20-hr period 1s normally sufficient for each
extraction.
2.2.4 All materials of construction are glass, Teflon, or stainless
steel. Pumps, 1f used, should not contain extractable materials. Pumps are
not used with methanol and methylene chloride.
3.0 DRYING
3.1 After evaluation of several methods of removing residual solvent, a
fluldlzed-bed technique has proved to be the fastest and most reliable drying
method.
3.2 A simple column with suitable retainers, as shown 1n Figure A-2,
will serve as a satisfactory column. A 10.2-cm (4-1n.) Pyrex pipe 0.6 m (2
ft) long will hold all of the XAD-2 from the extractor shown 1n Figure A-l or
the Soxhlet extractor, with sufficient space for flu1d1z1ng the bed while
generating a minimum resin load at the exit of the column.
3.3 Method 1; The gas used to remove the solvent 1s the key to
preserving the cleanliness of the XAD-2. Liquid nitrogen from a standard
commercial liquid nitrogen cylinder has routinely proved to be a reliable
source of large volumes of gas free from organic contaminants. The liquid
nitrogen cylinder 1s connected to the column by a length of precleaned 0.95-cm
(3/8-1n.) copper tubing, colled to pass through a heat source. As nitrogen 1s
bled from the cylinder, 1t 1s vaporized 1n the heat source and passes through
the column. A convenient heat source Is a water bath heated from a steam
line. The final nitrogen temperature should only be warm to the touch and not
over 40*C. Experience has shown that about 500 g of XAD-2 may be dried
overnight by consuming a full 160-liter cylinder of liquid nitrogen.
3.4 Method 2; As a second choice, h1gh-pur1ty tank nitrogen may be used
to dry the XAD-2. The h1gh-pur1ty nitrogen must first be passed through a bed
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LOOM Wt*vt Nylon
Fabric Cow
1CL2cm
(4 Inch) Pyrvx
Pip*
Liquid T«ki off
0.95 em (3/B in) Tubirtf
Liquid Nifrogtn
Cylinder
(1COX)
HutSourc*
Figure A-2. XAD-2 fluidized-bed drying apparatus.
0010 - A - 4
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of activated charcoal approximately 150 ml 1n volume. With either type of
drying method, the rate of flow should gently agitate the bed. Excessive
flu1d1zat1on may cause the particles to break up.
4.0 QUALITY CONTROL PROCEDURES
4.1 For both Methods 1 and 2, the quality control results must be
reported for the batch. The batch must be reextracted 1f the residual
extractable organlcs are >20 ug/mL by TCO analysis or the gravimetric residue
1s >0.5 mg/20 g XAD-2 extracted. (See also section 5.1, Method 0010.)
4.2 Four control procedures are used with the final XAD-2 to check for
(1) residual methylene chloride, (2) extractable organlcs (TCO), (3) specific
compounds of Interest as determined by GC/MS, as described In Section 4.5
below, and (4) residue (GRAY).
4.3 Procedure for residual methylene chloride;
4.3.1 Description: A 1+0.1-g sample of dried resin 1s weighed Into
a small vial, 3 mL of toluene are added, and the vial 1s capped and well
shaken. Five uL of toluene (now containing extracted methylene chloride) are
Injected Into a gas chromatograph, and the resulting Integrated area 1s
compared with a reference standard. The reference solution consists of 2.5 uL
of methylene chloride 1n 100 mL of toluene, simulating 100 ug of residual
methylene chloride on the resin. The acceptable maximum content Is 1,000 ug/g
resin.
4.3.2 Experimental: The gas chromatograph conditions are as
follows:
6-ft x 1/8-1n. stainless steel column containing 10X OV-101 on
100/120 Supelcoport;
Helium carrier at 30 mL/m1n;
FID operated on 4 x 10-11 A/mV;
Injection port temperature: 250*C;
Detector temperature: 305*C;
Program: 30*C(4 m1n) 40*C/m1n 250»C (hold); and
Program terminated at 1,000 sec.
4.4 Procedure for residual extractable organlcs;
4.4.1 Description: A 20+0.1-g sample of cleaned, dried resin 1s
weighed Into a precleaned alundum or cellulose thimble which 1s plugged with
cleaned glass wool. (Note that 20 g of resin will fill a thimble, and the
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resin will float out unless well plugged.) The thimble containing the resin
1s extracted for 24 hr with 200-mL of pesticide- grade methylene chloride
(Burdlck and Jackson pesticide-grade or equivalent purity). The 200-mL
extract 1s reduced 1n volume to 10-mL using a Kuderna-Dan1sh concentrator
and/or a nitrogen evaporation stream. Five uL of that solution are analyzed
by gas chromatography using the TCO analysis procedure. The concentrated
solution should not contain >20 ug/mL of TCO extracted from the XAD-2. This
1s equivalent to 10 ug/g of TCO 1n the XAD-2 and would correspond to 1.3 mg of
TCO 1n the extract of the 130-g XAD-2 module. Care should be taken to correct
the TCO data for a solvent blank prepared (200 ml reduced to 10 ml) 1n a
similar manner.
4.4.2 Experimental: Use the TCO analysis conditions described 1n
the revised Level 1 manual (EPA 600/7-78-201).
4.5 GC/HS Screen; The extract, as prepared 1n paragraph 4.4.1, 1s
subjected to GC/MS analysis for each of the Individual compounds of Interest.
The GC/MS procedure 1s described 1n Chapter Four, Method 8270. The extract 1s
screened at the MDL of each compound. The presence of any compound at a
concentration >25 ug/mL 1n the concentrated extract will require the XAD-2 to
be recleaned by repeating the methylene chloride step.
4.6 Methodology for residual gravimetric determination; After the TCO
value and GC/MS data are obtained for the resin batch by the above procedures,
dry the remainder of the extract 1n a tared vessel. There must be <0.5 mg
residue registered or the batch of resin will have to be extracted with fresh
methylene chloride again until 1t meets this criterion. This level
corresponds to 25 ug/g 1n the XAD-2, or about 3.25 mg 1n a resin charge of
130 g.
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METHOD 0010, APPENDIX B
TOTAL CHROMATOGRAPHABLE ORGANIC MATERIAL ANALYSIS
1.0 SCOPE AND APPLICATION
1.1 In this procedure, gas chromatography 1s used to determine the
quantity of lower boiling hydrocarbons (boiling points between 90* and 300*C)
1n the concentrates of all organic solvent rinses, XAD-2 resin and LC
fractions - when Method 1 1s used (see References, Method 0010) - encountered
in Level 1 environmental sample analyses. Data obtained using this procedure
serve a twofold purpose. First, the total quantity of the lower boiling
hydrocarbons 1n the sample 1s determined. Then whenever the hydrocarbon
concentrations 1n the original concentrates exceed 75 ug/m3, the
chromatography results are reexamlned to determine the amounts of Individual
species.
The extent of compound Identification 1s limited to representing all
materials as normal alkanes based upon comparison of boiling points. Thus the
method 1s not qualitative. In a similar manner, the analysis 1s
semiquant1tat1ve; calibrations are prepared using only one hydrocarbon. They
are replicated but samples routinely are not.
1.2 Application; This procedure applies solely to the Level 1 C7-C16
gas chromatographlc analysis of concentrates of organic extracts, neat
liquids, and of LC fractions. Throughout the procedure, 1t 1s assumed the
analyst has been given a properly prepared sample.
1,3 Sensitivity; The sensitivity of this procedure, defined as the
slope of a plot of response versus concentration, 1s dependent on the
Instrument and must be verified regularly. TRW experience Indicates the
nominal range is of the order of 77 uV-V-sec-uL/ng of n-heptane and 79
uV'sec-ul/ng of n-hexadecane. The instrument 1s capable of perhaps one
hundredfold greater sensitivity. The level specified here 1s sufficient for
Level 1 analysis.
1.4 Detection limit; The detection limit of this procedure as written
1s 1.3 ng/uL for a I ul injection of n-decane. This limit is arbitrarily
based on defining the minimum detectable response as 100 uvsec. This 1s an
easier operational definition than defining the minimum detection limit to be
that amount of material which yields a signal twice the noise level.
1.5 Range; The range of the procedure will be concentrations of 1.3
ng/uL and greater.
1.6 Limitations
1.6.1 Reporting limitations: It should be noted that a typical
environmental sample will contain compounds which: (a) will not elute 1n
the specified boiling ranges and thus will not be reported, and/or (b)
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will not elute from the column at all and thus will not be reported.
Consequently, the organic content of the sample as reported 1s a lower
bound and should be regarded as such.
1.6.2 Calibration limitations: Quant1tat1on 1s based on
calibration with n-decane. Data should therefore be reported as, e.g.,
mg C8/m3 as n-decane. Since response varies linearly with carbon number
(over a wide range the assumption may Involve a 20X error), 1t 1s clear
that heptane (C7) detected 1n a sample and quantltated as decane will be
overestimated. Likewise, hexadecane (C16) quantltated as decane will be
underestimated. From previous data, 1t 1s estimated the error Involved
1s on the order of 6-7X.
1.6.3 Detection limitations: The sensitivity of the flame
1on1zat1on detector varies from compound to compound. However, n-alkanes
have a greater response than other classes. Consequently, using an n-
alkane as a callbrant and assuming equal responses of all other compounds
tends to give low reported values.
2.0 SUMMARY OF METHOD
2.1 A ml aliquot of all 10-mL concentrates 1s disbursed for GC-TCO
analysis. With boiling point-retention time and response-amount calibration
curves, the data (peak retention times and peak areas) are Interpreted by
first summing peak areas 1n the ranges obtained from the boiling point-
retention time calibration. Then, with the response-amount calibration curve,
the area sums are converted to amounts of material 1n the reported boiling
point ranges.
2.2 After the Instrument 1s set up, the boiling point-retention time
calibration 1s effected by Injecting a mixture of n-C7 through n-C16
hydrocarbons and operating the standard temperature program. Response-
quantity calibrations are accomplished by Injecting n-decane in n-pentane
standards and performing the standard temperature program.
2.3 Definitions
2.3.1 GC: Gas chromatography or gas chromatograph.
2.3.2 C7-C16 n-alkanes: Heptane through hexadecane.
2.3.3 GCA temperature program: 4 m1n Isothermal at 60*C, lO*C/m1n
from 60* to 220*C.
2.3.4 TRW temperature program: 5 m1n Isothermal at room
temperature, then program from 30*C to 250*C at !5*C/m1n.
3.0 INTERFERENCES
Not applicable.
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Date September 1986
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4.0 APPARATUS AND MATERIALS
4.1 Gas chromatoqraph: This procedure 1s Intended for use on a Varlan
1860 gas chromatograph, equipped with dual flame 1on1zat1on detectors and a
C linear temperature programmer. Any equivalent Instrument can be used provided
that electrometer settings, etc., be changed appropriately.
4.2 Gases;
4.2.1 Helium: Minimum quality 1s reactor grade. A 4A or 13X
molecular sieve drying tube 1s required. A filter must be placed between
the trap and the Instrument. The trap should be recharged after every
third tank of helium.
4.2.2 Air: Zero grade 1s satisfactory.
4.2.3 Hydrogen: Zero grade.
4.3 Syringe; Syringes are Hamilton 701N, 10 uL, or equivalent.
4.4 Septa; Septa will be of such quality as to produce very low bleed
during the temperature program. An appropriate septum 1s Supelco Mlcrosep
138, which 1s Teflon-backed. If septum bleed cannot be reduced to a
negligible level, 1t will be necessary to Install septum swingers on the
Instrument.
4.5 Recorder: The recorder of this procedure must be capable of not
less than 1 mV full-scale display, a 1-sec time constant and 0.5 1n. per m1n
chart rate.
4.6 Integrator; An Integrator 1s required. Peak area measurement by
hand 1s satisfactory but too time-consuming. If manual Integration 1s
required, the method of "height times width at half height" 1s used.
4.7 Columns;
4.7.1 Preferred column: 6 ft x 1/8 1n. O.D. stainless steel column
of 10% OV-101 on 100/120 mesh Supelcoport.
4.7.2 Alternate column: 6 ft x 1/8 1n. O.D. stainless steel column
of 10X OV-1 (or other silicon phase) on 100/120 mesh Supelcoport.
4.8 Syringe cleaner; Hamilton syringe cleaner or equivalent connected
to a suitable vacuum source.
5.0 REAGENTS
5.1 Pentane; "D1st1lled-1n-Glass" (reg. trademark) or "Nanograde" (reg.
trademark) for standards and for syringe cleaning.
0010 - B - 3
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Date September 1986
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5.2 Methylene chloride; "Distilled-in-Glass" (reg. trademark) or
"Nanograde" (reg. trademark) for syringe cleaning.
6.0 SAMPLING HANDLING AND PRESERVATION
6.1 The extracts are concentrated 1n a Kuderna-Danlsh evaporator to a
volume less than 10 mL. The concentrate is then quantitatively transferred to
a 10-mL volumetric flask and diluted to volume. A 1-mL aliquot 1s taken for
both this analysis and possible subsequent GC/MS analysis and set aside in the
sample bank. For each GC-TCO analysis, obtain the sample sufficiently 1n
advance to allow 1t to warm to room temperature. For example, after one
analysis 1s started, return that sample to the sample bank and take the next
sample.
7.0 PROCEDURES
7.1 Setup and checkout; Each day, the operator will verify the
following:
7.1.1 That supplies of carrier gas, air and hydrogen are
sufficient, i.e., that each tank contains > 100 psig.
7.1.2 That, after replacement of any gas cylinder, all connections
leading to the chromatograph have been leak-checked.
7.1.3 That the carrier gas flow rate 1s 30 + 2 mL/m1n, "the hydrogen
flow rate is 30 + 2 mL/min, and the air flow rate is 300 + 20 mL/m1n.
7.1.4 That the electrometer 1s functioning properly.
7.1.5 That the recorder and integrator are functioning properly.
7.1.6 That the septa have been leak-checked (leak-checking 1s
effected by placing the soap bubble flow meter inlet tube over the
injection port adaptors), and that no septum will be used for more than
20 Injections.
7.1.7 That the 11st of samples to be run is ready.
7.2 Retention time calibration;
7.2.1 To obtain the temperature ranges for reporting the results of
the analyses, the chromatograph 1s given a normal boiling point-retention
time calibration. The n-alkanes, their boiling points, and data
reporting ranges are given in the table below:
0010 - B - 4
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Date September 1986
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NBP.'C Reporting Range,*C Report As
n-heptane 98 90-110 C7
n-octane 126 110-140 C8
n-nonane 151 140-160 C9
n-decane 174 160-180 CIO
n-undecane 194 180-200 Cll
n-dodecane 214 200-220 C12
n-tr1decane 234 220-240 C13
n-tetradecane 252 240-260 C14
n-pentadecane 270 260-280 C15
n-hexadecane 288 280-300 C16
7.2.2 Preparation of standards: Preparing a mixture of the C7-C16
alkanes 1s required. There are two approaches: (1) use of a standards
kit (e.g., Polysdence Kit) containing bottles of mixtures of selected n-
alkanes which may be combined to produce a C7-C16 standard; or (2) use of
bottles of the Individual C7-C16 alkanes from which accurately known
volumes may be taken and combined to give a C7-C16 mixture.
7.2.3 Procedure for retention time calibration: This calibration
1s performed at the start of an analytical program; the mixture 1s
chromatographed at the start of each day. To attain the required
retention time precision, both the carrier gas flow rate and the
temperature program specifications must be observed. Details of the
procedure depend on the Instrument being used. The general procedure 1s
as follows:
7.2.3.1 Set the programmer upper limit at 250*C. If this
setting does not produce a column temperature of 250*C, find the
correct setting.
7.2.3.2 Set the programmer lower limit at 30*C.
7.2.3.3 Verify that the Instrument and samples are at room
temperature.
7.2.3.4 Inject 1 uL of the n-alkane mixture.
7.2.3.5 Start the Integrator and recorder.
7.2.3.6 Allow the Instrument to run Isothermally at room
temperature for five m1n.
7.2.3.7 Shut the oven door.
7.2.3.8 Change the mode to Automatic and start the temperature
program.
7.2.3.9 Repeat Steps 1-9 a sufficient number of times so that
the relative standard deviation of the retention times for each peak
1s <5%.
0010 - B - 5
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7.3 Response calibration;
7.3.1 For the purposes .of a Level 1 analysis, response-quantity
calibration with n-decane 1s adequate. A 10-uL volume of n-decane 1s
Injected Into a tared 10 mL volumetric flask. The weight Injected 1s
obtained and the flask 1s diluted to the mark with n-pentane. This •
standard contains about 730 ng n-decane per uL n-pentane. The exact
concentration depends on temperature, so that a weight 1s required. Two
serial tenfold dilutions are made from this standard, giving standards at
about 730, 73, and 7.3 ng n-decane per uL n-pentane, respectively.
7.3.2 Procedure for response calibration: This calibration 1s
performed at the start of an analytical program and monthly thereafter.
The most concentrated standard 1s Injected once each day. Any change In
calibration necessitates a full calibration with new standards.
Standards are stored 1n the refrigerator locker and are made up monthly.
7.3.2.1 Verify that the Instrument 1s set up properly.
7.3.2.2 Set electrometer at 1 x lO'10 A/mV.
7.3.2.3 Inject 1 uL of the highest concentration standard.
7.3.2.4 Run standard temperature program as specified above.
7.3.2.5 Clean syringe.
7.3.2.6 Make repeated Injections of all three standards until
the relative standard deviations of the areas of each standard are
7.4 Sample analysis procedure;
7.4.1 The following apparatus 1s required:
7.4.1.1 Gas chroroatograph set up and working.
7.4.1.2 Recorder, Integrator working.
7.4.1.3 Syringe and syringe cleaning apparatus.
7.4.1.4 Parameters: Electrometer setting 1s 1 x 10~10 A/mV;
recorder 1s set at 0.5 1n./m1n and 1 mV full -scale.
7.4.2 Steps 1n the procedure are:
7.4.2.1 Label chromatogram with the data, sample number, etc.
0010 - B - 6
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Date Sf»nt«»mKev. ir»r
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7.4.2.2 Inject sample.
7.4.2.3 Start integrator and recorder.
7.4.2.4 After isothermal operation for 5 min, begin
temperature program.
7.4.2.5 Clean syringe.
7.4.2.6 Return sample; obtain new sample.
7.4.2.7 When analysis is finished, allow instrument to cool.
Turn chromatogram and integrator output and data sheet over to data
analyst.
7.5 Syringe cleaning procedure:
7.5.1 Remove plunger from syringe.
7.5.2 Insert syringe into cleaner; turn on aspirator.
7.5.3 Fill pipet with pentane; run pentane through syringe.
7.5.4 Repeat with methylene chloride from a separate pipet.
7.5.5 Flush plunger with pentane followed by methylene chloride.
7.5.6 Repeat with methylene chloride.
7.6 Sample analysis decision criterion; The data from the TCO analyses
of organic extract and rinse concentrates are first used to calculate the
total concentration of C7-C16 hydrocarbon-equivalents (Paragraph 7.7.3) in the
sample with respect to the volume of air actually sampled, I.e., ug/m3. On
this basis, a decision 1s made both on whether to calculate the quantity of
each n-alkane equivalent present and on which analytical procedural pathway
will be followed. If the total organic content is great enough to warrant
continuing the analysis — >500 ug/m3 — a TCO of less than 75 ug/m3 will
require only LC fractionalon and gravimetric determinations and IR spectra to
be obtained on each fraction. If the TCO 1s greater than 75 ug/m3, then the
first seven LC fractions of each sample will be reanalyzed using this same gas
chromatographic technique.
7.7 Calculations;
7.7.1 Boiling Point - Retention Time Calibration: The required
data for this calibration are on the chromatogram and on the data sheet.
The data reduction is performed as follows:
7.7.1.1 Average the retention times and calculate relative
standard deviations for each n-hydrocarbon.
0010 - B - 7
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Date September 1986
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7.7.1.2 Plot average retention times as abscissae versus
normal boiling points as ordlnates.
7.7.1.3 Draw 1n calibration curve.
7.7.1.4 Locate and record retention times corresondlng to
boiling ranges 90-100, 110-140, 140-160, 160-180, 180-200, 200-220,
220-240, 240-260, 260-280, 280-300*C.
7.7.2 Response-amount calibration: The required data for this
calibration are on the chromatogram and on the data sheet. The data
reduction 1s performed as follows:
7.7.2.1 Average the area responses of each standard and
calculate relative standard deviations.
7.7.2.2 Plot response (uvsec) as ordlnate versus ng/uL as
abscissa.
7.7.2.3 Draw 1n the curve. Perform least squares regression
and obtain slope (uV-sec-uL/ng).
7.7.3 Total C7-C16 hydrocarbons analysis: The required data for
this calculation are on the chromatogram and on the data sheet. The data
reduction 1s performed as follows:
7.7.3.1 Sum the areas of all peaks within the retention time
range of Interest.
7.7.3.2 Convert this area (uV*sec) to ng/uL by dividing by the
weight response for n-decane (uV»sec.uL/ng).
7.7.3.3 Multiply this weight by the total concentrate volume
(10 ml) to get the weight of the C7-C16 hydrocarbons 1n the sample.
7.7.3.4 Using the volume of gas sampled or the total weight of
sample acquired, convert the result of Step 7.7.3.3 above to ug/m3.
7.7.3.5 If the value of total C7-C16 hydrocarbons from Step
7.7.3.4 above exceeds 75 ug/m3, calculate Individual hydrocarbon
concentrations 1n accordance with the Instructions 1n Paragraph
7.7.5.5 below.
7.7.4 Individual C7-C16 n-Alkane Equivalent Analysis: The required
data from the analyses are on the chromatogram and on the data sheet.
The data reduction 1s performed as follows:
7.7.4.1 Sum the areas of peaks 1n the proper retention time
ranges.
0010 - B - 8
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Date September 1986
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7.7A.2 Convert areas (uV-sec) to ng/uL by dividing by the
proper weight response (uV-sec-uL/ng).
/--- 7.7.4.3 Multiply each weight by total concentrate volume (10
ml) to get weight of species 1n each range of the sample.
7.7.4.4 Using the volume of gas sampled on the total weight of
sample acquired, convert the result of Step 7.7.4.3 above to ug/m3.
8.0 QUALITY CONTROL
8.1 Appropriate QC Is found 1n the pertinent procedures throughout the
method.
9.0 METHOD PERFORMANCE
9.1 Even relatively comprehensive error propagation analysis 1s beyond
the scope of this procedure. With reasonable care, peak area reproduc1b1l1ty
of a standard should be of the order of 1% RSD. The relative standard
deviation of the sum of all peaks 1n a fairly complex waste might be of the
order of 5-10%. Accuracy 1s more difficult to assess. With good analytical
technique, accuracy and precision should be of the order of 10-20X.
10.0 REFERENCES
1. Emissions Assessment of Conventional Stationary Combustion Systems:
Methods and Procedure Manual for Sampling and Analysis, Interagency
Energy/Environmental R&D Program, Industrial Environmental Research
Laboratory, Research Triangle Park, NC 27711, EPA-600/7-79-029a, January 1979.
0010 - B - 9
Revision
Date September 1986
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APPENDIX F.8
SW-846 METHOD 0030
-------
METHOD 0030
VOLATILE ORGANIC SAMPLING TRAIN
1.0 PRINCIPLE AND APPLICATION
1.1 Principle
1.1.1 This method describes the collection of volatile principal
organic hazardous constituents (POHCs) from the stack gas effluents of
hazardous waste Incinerators. For the purpose of definition, volatile
POHCs are those POHCs with boiling points less than 100*C. If the
boiling point of a POHC of Interest Is less than 30*C, the POHC may break
through the sorbent under the conditions of the sample collection
procedure.
1.1.2 Field application for POHCs of this type should be supported
by laboratory data which demonstrate the efficiency of a volatile organic
sampling train (VOST) to collect POHCs with boiling points less than
30*C. This may require using reduced sample volumes collected at flow
rates between 250 and 500 mL/m1n. Many compounds which boll above 100'C
(e.g., chlorobenzene) may also be efficiently collected and analyzed
using this method. VOST collection efficiency for these compounds should
be demonstrated, where necessary, by laboratory data of the type
described above.
1.1.3 This method employs a 20-11 ter sample of effluent gas
containing volatile POHCs which Is withdrawn from a gaseous effluent
source at a flow rate of 1 L/m1n, using a glass-lined probe and a
volatile organic sampling train (VOST). (Operation of the VOST under
these conditions has been called FAST-VOST.) The gas stream Is cooled to
20*C by passage through a water-cooled condenser and volatile POHCs are
collected on a pair of sorbent resin traps. Liquid condensate 1s
collected 1n ah Implnger placed between the two resin traps. The first
resin trap (front trap) contains approximately 1.6 g Tenax and the second
trap (back trap) contains approximately 1 g each of Tenax and petroleum-
based charcoal (SKC Lot 104 or equivalent), 3:1 by volume. A total of
six pairs of sorbent traps may be used to collect volatile POHCs from the
effluent gas stream.
1.1.4 An alternative set of conditions for sample collection has
been used. This method Involves collecting sample volume of 20 liters or
less at reduced flow rate. (Operation of the VOST under these conditions
has been referred to as SLO-VOST.) This method has been used to collect
5 liters of sample (0.25 L/m1n for 20 m1n) or 20 liters of sample
(0.5 L/m1n for 40 mln) on each pair of sorbent cartridges. Smaller
sample volumes collected at lower flow rates should be considered when
the boiling points of the POHCs of Interest are below 35*C. A total of
six pairs of sorbent traps may be used to collect volatile POHCs from the
effluent gas stream.
0030 - 1
Revision 0
Date September 1986
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1.1.5 Analysis of the traps 1s carried out by thermal desorptlon
purge-and-trap by gas chromatography/mass spectrometry (see Method 5040).
The VOST 1s designed to be operated at 1 L/m1n with traps being replaced
every 20 m1n for a total sampling time of 2 hr. Traps may be analyzed
separately or combined onto one trap to Improve detection limit.
However, additional flow rates and sampling times are acceptable. Recent
experience has shown that when less than maximum detection ability Is
required, 1t 1s acceptable and probably preferable to operate the VOST at
0.5 L/m1n for a total of three 40-m1n periods. This preserves the 2-hr
sampling period, but reduces the number of cartridge changes In the field
as well as the number of analyses required.
1.2 Application
1.2.1 This method 1s applicable to the determination of volatile
POHCs 1n the stack gas effluent of hazardous waste Incinerators. This
method Is designed for use 1n calculating destruction and removal
efficiency (ORE) for the volatile POHCs and to enable a determination
that ORE values for removal of the volatile POHCs are equal to or greater
than 99.99%.
1.2.2 The sensitivity of this method 1s dependent upon the level of
Interferences 1n the sample and the presence of detectable levels of
volatile POHCs In blanks. The target detection limit of this method Is
0.1 ug/m3 (ng/L) of flue gas, to permit calculation of a ORE equal to or
greater than 99.99X for volatile POHCs which may be present 1n the waste
stream at 100 ppm. The upper end of the range of applicability of this
method 1s limited by breakthrough of the volatile POHCs on the sorbent
traps used to collect the sample. Laboratory development data have
demonstrated a range of 0.1 to 100 ug/m3 (ng/L) for selected volatile
POHCs collected on a pair of sorbent traps using a total sample volume of
20 liters or less (see Paragraph 1.1.4).
1.2.3 This method 1s recommended for use only by experienced
sampling personnel and analytical chemists or under close supervision by
such qualified persons.
1.2.4 Interferences arise primarily from background contamination
of sorbent traps prior to or after use In sample collection. Many
potential Interferences can be due to exposure of the sorbent materials
to solvent vapors prior to assembly and exposure to significant
concentrations of volatile POHCs 1n the ambient air at hazardous waste
Incinerator sites.
1.2.5 To avoid or minimize the low-level contamination of train
components with volatile POHCs, care should be taken to avoid contact of
all Interior surface or train components with synthetic organic materials
(e.g., organic solvents, lubricating and sealing greases), and train
components should be carefully cleaned and conditioned according to the
procedures described 1n this protocol.
0030 - 2
Revision
Date September 1986
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2.0 APPARATUS
2.1 Volatile Organic Sampling Train; A schematic diagram of the
principal components of the MOST 1 s shown 1n Figure 1 and a diagram of one
acceptable version of the VOST 1s shown 1n Figure 2. The VOST consists of a
glass-lined probe followed by an Isolation valve, a water-cooled glass
condenser, a sorbent cartridge containing Tenax (1.6 g), an empty Implnger for
condensate removal, a second water-cooled glass condenser, a second sorbent
cartridge containing Tenax and petroleum-based charcoal (3:1 by volume;
approximately 1 g of each), a silica gel drying tube, a calibrated rotameter,
a sampling pump, and a dry gas meter. The gas pressure during sampling and
for leak-checking Is monitored by pressure gauges which are In line and
downstream of the silica gel drying tube. The components of the sampling
train are described below.
2.1.1 Probe: The probe should be made of stainless steel with a
boroslllcate or quartz glass Uner. The temperature of the probe 1s to
be maintained above 130*C but low enough to ensure a resin temperature of
20*C. A water-cooled probe may be required at elevated stack
temperatures to protect the probe and meet the above requirements.
Isoklnetlc sample collection 1s not a requirement for the use of VOST
since the compounds of Interest are 1n the vapor phase at the point of
sample collection.
2.1.2 Isolation valve: The Isolation valve should be a greaseless
stopcock with a glass bore and sliding Teflon plug with Teflon wipers
(Ace 8193 or equivalent).
2.1.3 Condensers: The condensers (Ace 5979-14 or equivalent)
should be of sufficient capacity to cool the gas stream to 20*C or less
prior to passage through the first sorbent cartridge. The top connection
of the condenser should be able to form a leak-free, vacuum-tight seal
without using sealing greases.
2.1.4 Sorbent cartridges:
2.1.4.1 The sorbent cartridges used for the VOST may be used
1n either of two configurations: the 1ns1de-outs1de (I/O)
configuration In which the cartridge 1s held within an outer glass
tube and 1n a metal carrier, and the 1ns1de-1ns1de (I/I)
configuration 1n which only a single glass tube Is used, with or
without a metal carrier. In either case, the sorbent packing will
be the same.
2.1.4.1.1 The first of a pair of sorbent cartridges shall
be packed with approximately 1.6 g Tenax GC resin and the
second cartridge of a pair shall be packed with Tenax GC and
petroleum-based charcoal (3:1 by volume; approximately 1 g of
each) .
2.1.4.1.2 The second sorbent cartridge shall be packed so
that the sample gas stream passes through the Tenax layer first
and then through the charcoal layer.
0030 - 3
Revision 0
Date September 1986
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Heated Probe
Gins Wool
Paniculate
Filter
o
o
to
o
STACK
(or test System)
O30
(u «
rt <
rt -*
vt
00 o
n> =3
O
r*
o>
Comfens«f«
Trv
Impin^er
Vacuum
Indiciitor
—+ Exhaust
Empty Silica Gel
Implnger
10
00
Figure 1. Schematic of Volatile Organic Sampling Train (VOST).
-------
Teflon Plug Valve w/Socket Joint
Condensers
Tubing
Tenax Trap
Tenax/Charcoal
Trap
Impinger
Ice Water Bath
Case
Figure 2. Volatile Organic Sampling Train (VOST).
0030 - 5
Revision 0
Date September 1986
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2.1.4.2 The sorbent cartridges shall be glass tubes with
approximate dimensions of 10 cm by 1.6 cm I.D. The two acceptable
designs (I/O, I/I) for the sorbent cartridge are described 1n
further detail below.
2.1.4.2.1 Inside/Inside sorbent cartridge: A diagram of
an III sorbent cartridge 1s shown 1n Figure 3. This cartridge
1s a single glass tube (10 cm by 1.6 cm I.D.) which has the
ends reduced 1n size to accommodate a 1/4- or 3/8-1n. Swagelok
or Cajon gas fitting. The resin 1s held 1n place by glass wool
at each end of the resin layer. The amounts of each type of
sorbent material used 1n the I/I design are the same as for the
I/O design. Threaded end caps are placed on the sorbent
cartridge after packing with sorbent to protect the sorbent
from contamination during storage and transport.
2.1.4.2.2 Inside/Outside type sorbent cartridge: A
diagram of an I/O sorbent cartridge 1s shown 1n Figure 4. In
this design the sorbent materials are held 1n the glass tube
with a fine mesh stainless steel screen and a C-cl1p. The
glass tube 1s then placed within a larger diameter glass tube
and held 1n place using V1ton 0-rlngs. The purpose of the
outer glass tube 1s to protect the exterior of the resin-
containing tube from contamination. The two glass tubes are
held 1n a stainless steel cartridge holder, where the ends of
the glass tubes are held 1n place by V1ton 0-r1ngs placed 1n
machine grooves 1n each metal end piece. The three cylindrical
rods are secured 1n one of the metal end pieces and fastened to
the other end piece using knurled nuts, thus sealing the glass
tubes Into the cartridge holder. The end pieces are fitted
with a threaded nut onto which a threaded end cap 1s fitted
with a V1ton 0-r1ng seal, to protect the resin from
contamination during transport and storage.
2.1.5 Metering system: The metering system for YOST shall consist
of vacuum gauges, a leak-free pump (Thomas Model 107 or equivalent,
Thomas Industries, Sheboygan, Wisconsin), a calibrated rotameter (Unde
Model 150, Unde Division of Union Carbide, Keasbey, New Jersey) for
monitoring the gas flow rate, a dry gas meter with 2% accuracy at the
required sampling rate, and related valves and equipment. Provisions
should be made for monitoring the temperature of the sample gas stream
between the first condenser and first sorbent cartridge. This can be
done by placing a thermocouple on the exterior glass surface of the
outlet from the first condenser. The temperature at that point should be
less than 20*C. If 1t 1s not, an alternative condenser providing the
required cooling capacity must be used.
2.1.6 Sample transfer lines: All sample transfer lines to connect
the probe to the VOST shall be less than 5 ft 1n length, and shall be
heat-traced Teflon with connecting fittings which are capable of forming
leak-free, vacuum-tight connections without the use of sealing grease.
0030 - 6
Revision
Date September 1986
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O
O
to
O
I Ocm
- GLASS WOOL
OR
STAINLESS STEEL SCREEN
n -*
-------
o
o
u»
o
00
050
oi n
rt- <
m -*
CO
u>o
s3
r+
fO
§
n
VD
oo
TOP
BOTTOM
Section cut through flan tub**
lehovlnq •cr««n. C-«lip and O-ring in place)
LEGEND
A - Stainlns Stwl Ofiw
B • Gins Tube (9.84 L x 2.22 ID)
C • Small Glass Tub* (10cm x 1.6cm ID)
0 • Fine Mesh Stainless Sleet Screen
E • Stainless Steel C-CliP
F-ORing(Viton|
G - Nuts (+)
H - End Cap with Viton 0 Ring
I • Metal Rod with Threaded End (3)
J • Tenax/Charcoal Sorbent
K • Cajon Fitting
Aa»«*bl«d Trap
NTS
Figure 4. Sorbent Trap Assembly (I/O)
Volatile Organic Sampling Train (VOST)
-------
All other sample transfer lines used with the VOST shall be Teflon with
connecting fittings that are capable of forming leak-free, vacuum-tight
connections without the use of sealing grease.
3.0 REAGENTS AND MATERIALS
3.1 2.6-D1phenv1ene oxide polymer (Tenax, 35/60 mesh):
3.1.1 The new Tenax 1s Soxhlet extracted for 24 hr with methanol
(Burdlck & Jackson, pesticide grade or equivalent). The Tenax Is dried
for 6 hr 1n a vacuum oven at 50*C before use. Users of I/O and I/I
sorbent cartridges have used slightly different thermal conditioning
procedures. I/O sorbent cartridges packed with Tenax are thermally
conditioned by flowing organic-free nitrogen (30 ml/mln) through the
resin while heating to 190*C. Some users have extracted new Tenax and
charcoal with pentane to remove nonpolar Impurities. However, these
users.have experienced problems with residual pentane 1n the sorbents
during analysis.
3.1.2 If very high concentrations of volatile POHCs have been
collected on the resin (e.g., mlcrograms of analytes), the sorbent may
require Soxhlet extraction as described above. Previously used Tenax
cartridges are thermally reconditioned by the method described above.
3.2 Charcoal (SKC petroleum-base or equivalent): New charcoal 1s
prepared and charcoal 1s reconditioned as described In Paragraph 4.4. New
charcoal does not require treatment prior to assembly Into sorbent cartridges.
Users of VOST have restricted the types of charcoal used 1n sorbent cartridges
to only petroleum-based types. Criteria for other types of charcoal are
acceptable If recovery of POHC 1n laboratory evaluations meet the criteria of
50 to 150X.
3.3 V1ton-0-R1ng; All 0-rlngs used 1n VOST shall be V1ton. Prior to
use, these 0-r1ngs should be thermally conditioned at 200*C for 48 hr.
0-rings should be stored 1n clean, screw-capped glass containers prior to use.
3.4 Glass tubes/Condensers; The glass resin tubes and condensers should
be cleaned with a nonlonlc detergent In an ultrasonic bath, rinsed well with
organic-free water, and dried at 110'C. Resin tubes of the I/O design should
be assembled prior to storage as described 1n Paragraph 4.1. Resin tubes of
the III design can be stored 1n glass culture tube containers with cotton
cushioning and Teflon-Hned screw caps. Condensers can be capped with
appropriate end caps prior to use.
3.5 Metal parts; The stainless steel carriers, C-cl1ps, end plugs, and
screens used 1n the I/O VOST design are cleaned by ultrasonlcation 1n a warm
nonlonlc detergent solution, rinsed with distilled water, air-dried, and
heated In a muffle furnace for 2 hr at 400*C. Resin tubes of the I/I design
require Swagelok or equivalent end caps with Supelco M-l ferrules. These
should be heated at 190*C along with the assembled cartridges.
0030 - 9
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3.6 Silica gel (Indicating type, 6-16 mesh): New silica gel may be used
as received^Silica gel which has been previously used should be dried for 2
hr at 175*C (35(TF).
3.7 Cold packs; Any commercially available reusable liquids or gels
that can be repeatedly frozen are acceptable. They are typically sold 1n
plastic containers as "Blue Ice" or "Ice-Packs." Enough should be used to
keep cartridges at or near 4*C.
3.8 Water; Water used for cooling train components 1n the field may be
tap water; and water used for rinsing glassware should be organic-free.
3.9 Glass wool; Glass wool should be Soxhlet extracted for 8 to 16 hr,
using methanol, and oven dried at 110*C before use.
4.0 SAMPLE HANDLING AND PROCEDURE
4.1 Assembly;
4.1.1 The assembly and packing of the sorbent cartridges should be
carried out 1n an area free of volatile organic material, preferably a
laboratory 1n which no organic solvents are handled or stored and 1n
which the laboratory air Is charcoal filtered. Alternatively, the
assembly procedures can be conducted 1n a glove box which can be purged
with organic-free nitrogen.
4.2 Tenax cartridges;
4.2.1 The Tenax, glass tubes, and metal cartridge parts are cleaned
and stored (see Section 3.0). Approximately 1.6 g of Tenax Is weighed
and packed Into the sorbent tube which has a stainless steel screen and
C-c11p (I/O design) or glass wool (I/I design) 1n the downstream end.
The Tenax 1s held In place by Inserting a stainless steel screen and
C-cl1ps1n the upstream end (I/O design) or glass wool (I/I design).
Each cartridge should be marked, using an engraving tool, with an arrow
to Indicate the direction of sample flow, and a serial number.
4.2.2 Conditioned resin tubes of the I/O design are then assembled
Into the metal carriers according to the previously described
1ns1de/1ns1de or 1ns1de/outs1de procedures (with end caps) and are placed
on cold packs for storage and transport. Conditioned resin tubes of the
I/I design are capped and placed on cold packs for storage and transport.
4.3 Tenax/Charcoal tubes
4.3.1 The Tenax, charcoal, and metal cartridge parts are cleaned
and stored as previously described (see Section 3.0). The tubes are
packed with approximately a 3:1 volume ratio of Tenax and charcoal
(approximately 1 g each). The Tenax and charcoal are held 1n place by
the stainless steel screens and C-cl1ps (I/O design) or by glass wool
(I/I design). The glass tubes containing the Tenax and charcoal are then
0030 - 10
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Date September 1986
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conditioned as described below (see Paragraph 4.4). Place the I/O glass
tubes In the metal carriers (see Paragraph 2.1.4.2.2), put end caps on
the assembled cartridges, mark direction of sample flow and serial
number, and place the assembled cartridges on cold packs for storage and
transport.
4.3.2 Glass tubes of the I/I design are conditioned, and stored 1n
the same manner as the I/O tubes.
4.4 Trap Conditioning - QC
4.4.1 Following assembly and leak-checking, the traps are connected
1n reverse direction to sampling to a source of organic-free nitrogen,
and nitrogen 1s passed through each trap at a flow rate of 40 ml_/m1n,
while the traps are heated to 190'C for 12-28 hr. The actual
conditioning period may be determined based on adequacy of the resulting
blank checks.
4.4.2 The following procedure 1s used to blank check each set of
sampling cartridges prior to sampling to ensure cleanliness. The
procedure provides semi-quantitative data for organic compounds with
boiling points below 110*C on Tenax and Tenax/Charcoal cartridges. It 1s
not Intended as a substitute for Method 5040.
4.4.2.1 The procedure 1s based on thermal desorptlon of each
set of two cartridges, cryofocuslng with liquid nitrogen onto a trap
packed with glass beads, followed by thermal desorptlon from the
trap and analysis by GC/FID.
4.4.2.2 The detection limit 1s based on the analysis of Tenax
cartridges spiked with benzene and toluene and 1s around 2 ng for
each compound.
4.4.2.3 The results of analyzing spiked cartridges on a dally
basis should not vary by more than 20 percent. If the results are
outside this range, the analytical system must be evaluated for the
probable cause and a second spiked cartridge analyzed.
4.4.2.4 The GC operating conditions are as follows:
GC Operating Conditions
Column: Packed column 6 ft x 1/8" stainless steel 1.0 percent
SP-1000 on Carbopack B 60/80, or equivalent.
Temperature program: 50*C for 5 m1n, 20*C/m1n Increase to
190»C, hold 13 m1n.
Injector: 200*C.
Detector: F.I.D. 250«C.
Carrier Gas: Helium at 25 mL/m1n.
Sample valve: Valco 6-port with 40" x 1/16" stainless steel
trap packed with 60/80 mesh glass beads.
Cryogen: Liquid nitrogen.
Trap heater: Boiling water, hot oil, or electrically heated.
0030 - 11
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Date September 1986
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Desorptlon heater: Supelco "clam shell" (high capacity carrier
gas purifier) heater and Varlac, adjusted to 180*C to
200»C.
4.4.2.5 Calibration 1s accomplished by preparing a spiked
Tenax cartridge with benzene and toluene and analyzing according to
the standard operating procedure. A standard of benzene, toluene
and bromof 1 uorobenzene (BFB) 1s prepared by Injecting 2.0 uL of
benzene and toluene and 1.0 uL of BFB Into 10 ml of methanol. The
concentration of this stock 1s 175 ng/uL of benzene and toluene, and
150 ng/uL BFB. One m1crol1ter of the stock standard 1s Injected
onto a Tenax cartridge through a heated Injection port set at 150*C.
A GC oven can be used for this with the oven at room temperature.
Helium carrier gas 1s set at 50 mL/m1n. The solvent flush technique
should be used. After two m1n, remove the Tenax cartridge and place
1n the desorptlon heater for analysis. BFB Is also used as an
Internal standard spike for GC/HS analysis which provides a good
comparison between GC/FID and GC/MS. The results of this spike
analysis should not vary more than 20 percent day to day. Initially
and then periodically this spiked Tenax should be reanalyzed a
second time to verify that the 10 m1n desorptlon time and 180-200*C
temperature are adequate to remove all of the spiked components. It
should be noted that only one spiked Tenax cartridge need be
prepared and analyzed dally unless otherwise needed to ensure proper
Instrument operation.
An acceptable blank level 1s left to the discretion of the
method analyst. An acceptable level Is one that allows adequate
determination of expected components emitted from the waste being
burned.
4.4.3 After conditioning, traps are sealed and placed on cold packs
until sampling Is accomplished. Conditioned traps should be held for a
minimum amount of time to prevent the possibility of contamination.
4.4.4 It may be useful to spike the Tenax and Tenax/charcoal traps
with the compounds of Interest to ensure that they can be thermally
desorbed under laboratory conditions. After spiked traps are analyzed
they may be reconditioned and packed for sampling.
4.5 Pretest preparation;
4.5.1 All train components shall be cleaned and assembled as
previously described. A dry gas meter shall have been calibrated within
30 days prior to use, using an EPA-suppl1ed standard orifice.
4.5.2 The VOST 1s assembled according to the schematic diagram 1n
Figure 1. The cartridges should be positioned so that sample flow 1s
0030 - 12
Revision
Date September 1986
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through the Tcnax first and then the Tenax/charcoal. Cooling water
should be circulated to the condensers and the temperature of the cooling
water should be maintained near 0*C. The end caps of the sorbent
cartridges should be placed 1n a clean screw-capped glass container
during sample collection.
4.6 Leak-checking;
4.6.1 The train 1s leak-checked by closing the valve at the Inlet
to the first condenser and pulling a vacuum of 250 mm (10 1n. Hg) above
the normal operating pressure. The traps and condensers are Isolated
from the pump and the leak rate noted. The leak rate should be less than
2.5 mm Hg after 1 m1n. The train 1s then returned to atmospheric
pressure by attaching a charcoal-filled tube to the train Inlet and
admitting ambient air filtered through the charcoal. This procedure will
minimize contamination of the VOST components by excessive exposure to
the fugitive emissions at hazardous waste Incinerator sites.
4.7 ' Sample Collection
4.7.1 After leak-checking, sample collection Is accomplished by
opening the valve at the Inlet to the first condenser, turning on the
pump, and sampling at a rate of 1 I1ter/m1n for 20 m1n. The volume of
sample for any pair of traps should not exceed 20 liters.
4.7.2 Following collection of 20 liters of sample, the train 1s
leak-checked a second time at the highest pressure drop encountered
during the run to minimize the .chance of vacuum desorptlon of organlcs
from the Tenax. The train 1s returned to atmospheric pressure, using the
method discussed 1n Paragraph 4.1 and the two sorbent cartridges are
removed. The end caps are replaced and the cartridges shall be placed In
a suitable environment for storage and transport until analysis. The
sample 1s considered Invalid 1f the leak test does not meet
specification.
4.7.3 A new pair of cartridges 1s placed 1n the VOST, the VOST
leak-checked, and the sample collection process repeated as described
above. Sample collection continues until six pairs of traps have been
used.
4.7.4 All sample cartridges should be kept on cold packs until they
are ready for analysis.
4.8 Blanks
4.8.1 Field blanks/trip blanks: Blank Tenax and Tenax/charcoal
cartridges are taken to the sampling site and the end caps removed for
the period of time required to exchange two pairs of traps on VOST.
After the two VOST traps have been exchanged, the end caps are replaced
on the blank Tenax and Tenax/charcoal tubes and these are returned to the
cold packs and analyzed with the sample traps. At least one pair of
field blanks (one Tenax, one Tenax/charcoal) shall be Included with each
0030 - 13
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Date September 1986
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six pairs of sample cartridges collected (or for each field trial using
VOST to collect volatile POHCs).
4.8.2 Trip blanks: At least one pair of blank cartridges (one
Tenax, one Tenax/charcoal ) shall be Included with shipment of cartridges
to a hazardous waste Incinerator site. These "field blanks* will be
treated like any other cartridges except that the end caps will not be
removed during storage at the site. This pair of traps will be analyzed
to monitor potential contamination which may occur during storage and
shipment.
4.8.3 Laboratory blanks: One pair of blank cartridges (one Tenax,
one Tenax/charcoal) will remain 1n the laboratory using the method of
storage which 1s used for field samples. If the field and trip blanks
contain high concentrations of contaminants (e.g., greater than 2 ng of a
particular POHC), the laboratory blank shall be analyzed In order to
Identify the source of contamination.
5.0 CALCULATIONS (for sample volume)
5.1 The following nomenclature are used 1n the calculation of sample
volume:
pbar * Barometric pressure at the exit orifice of the dry gas meter, mm
Hg.
Pstd " Standard absolute pressure, 760 mm (29.92 1n.) Hg.
Tm * DrY 9*s meter average absolute temperature, K (*R).
Tstd " Standard absolute temperature, 293K (528*R).
vm s Dry 9as volume measured by dry gas meter, dcm (dcf).
vm(std) • Dry gas volume measured by dry gas meter, corrected to standard
conditions, dscm (dscf).
7 « Dry gas meter calibration factor.
5.2 The volume of gas sampled 1s calculated as follows:
u = v « Tstd pbar r Vm pbar
V«d) V T, Pstd hi ~V~
where:
K! = 0.3858 K/mm Hg for metric units, or
KI * 17.64 *R/1n. Hg for English units.
0030 - 14
Revision
Date September 1986
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6.0 ANALYTICAL PROCEDURE
See Method 5040.
7.0 PRECISION AND ACCURACY REQUIREMENTS
7.1 Method Performance Check
Prior to field operation of the VOST at a hazardous waste Incine-
rator, a method performance check should be conducted using either
selected volatile POHCs of Interest or two or more of the volatile POHCs
for which data are available. This check may be conducted on the entire
system (VOST/GC/MS) by analysis of a gas cylinder containing POHCs of
Interest or on only the analytical system by spiking of the POHCs onto
the traps. The results of this check for replicate pairs of traps should
demonstrate that recovery of the analytes fall within SOX to 150X of the
expected values.
7.2 Performance Audit
During a trial burn a performance audit must be completed. The
audit results should agree within 50% to 150X of the expected value for
each specific target compound. This audit consists of collecting a gas
sample containing one or more POHCs 1n the VOST from an EPA ppb gas
cylinder. Collection of the audit sample In the,VOST may be conducted
either 1n the laboratory or at the trial burn slte^ Anaysls of the VOST
audit sample must be by the same person, at the same time, and with the
same analytical procedure as used for the regular VOST trail burn
samples. EPA ppb gas cylinders currently available for VOST Audit are
shown 1n Table 1 below.
The audit procedure, audit equipment and audit cylinder may be
obtained by writing:
Audit Cylinder Gas Coordinator (MD-77B)
Quality Assurance Division
Environmental Monitoring Systems Laboratory
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
or by calling the Audit Cylinder Gas Coordinator at (919) 541-4531.
The request for the audit must be made at least 30 days prior to the
scheduled trial burn. If a POHC Is selected for which EPA does not have
an audit cylinder, this audit Is not required.
0030 - 15
Revision
Date September 1986
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8.0 REFERENCES
1. Protocol for the Collection and Analysis of Volatile POHCs Using VOST.
EPA/600/8-84/007, March 1984.
2. Sykes, A.L., Standard Operating Procedure for Blanking Tenax and
Tenax/Charcoal Sampling Cartridges for Volatile Organic Sampling Train (VOST),
Radlon Corporation, P.O. Box 13000, Research Triangle Park, NC 27709.
3. Validation of the Volatile Organic Sampling Train (VOST) Protocol, Vols. I
and II, EPA/600/4-86/014a, January 1986.
0030 - 16
Revision
Date September 1986
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TABLE 1: Organic Gases 1n the ppb Audit Repository
Group I
5 Organlcs In N£:
Carbon tetrachlorlde
Chloroform
Perchloroethylene
Vinyl chloride
Benzene
Ranges of cylinders
currently available;
7-90 ppb
90 - 430 ppb
430 - 10,000 ppb
Group II
9 Organlcs In N£
Trlchloroethylene
1,2-01chloroethane
1,2-01bromoethane
F-12
F-ll
Bromomethane
Methyl ethyl ketone
1,1,1-Trlchloroethane
Acetron1tr1le
Ranges of cylinders
currently available;
7-90 ppb
90 - 430 ppb
0030 - 17
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Date September 1986
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TABLE 1: Organic Gases 1n the ppb Audit Repository (Continued)
Group III
7 Organlcs 1n N£:
V1ny11dene chloride
F-113
F-114
Acetone
l,4-D1oxane
Toluene
Chlorobenzene
Ranges of cylinders
currently available;
7-90 ppb
90 - 430 ppb
Group IV
6 Organlcs 1n Ng:
Acrylon1tr1le
l,3-Butad1ene
Ethylene oxide
Methylene chloride
Propylene oxide
Ortho-xylene
Ranges of cylinders
currently available!
7-90 ppb
430 - 10,000
0030 - 18
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Date September 1986
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TECHNICAL REPORT DATA
Please read instructions on the reverse before completing
1. REPORT NO.
EPA-454/R-00-025C
4. TITLE AND SUBTITLE
Final Report
Hot Mix Asphalt Plants,
Truck Loading and Silo Filling,
Manual Methods Testing,
Asphalt Plant C,
Los Angeles, California
Volume 3 of 8
2.
7. AUTHOR(S)
Frank J. Phoenix
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Pacific Environmental Services, Inc.
Post Office Box 12077
Research Triangle Park, North Carolina 27709-2077
12. SPONSORING AGENCY NAME AND ADDRESS
U.S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Emissions, Monitoring and Analysis Division
Research Triangle Park, North Carolina 277 1 1
3. RECIPIENT'S ACCESSION NO.
5. REPORT DATE
May 2000
6. PERFORMING ORGANIZATION CODE
8. PERFORMING ORGANIZATION REPORT NO.
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-D-98004
13. TYPE OF REPORT AND PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
EPA/200/04
15. SUPPLEMENTARY NOTES
16. ABSTRACT
The United States Environmental Protection Agency (EPA) Office of Air Quality Planning and Standards (OAQPS) is investigating hot mix
asphalt plants to identify and quantify particulate matter (PM), methylene chloride extractable matter (MCEM), and organic hazardous air pollutant
(HAP) emissions during asphalt concrete loading operations. In support of this investigation, the OAQPS issued Pacific Environmental Services, Inc.
(PES) a series of work assignments to conduct emissions testing at a hot mix asphalt plant during load-out operations.
The primary objective of the emissions testing was to characterize the uncontrolled emissions of PM, MCEM, polynuclear aromatic hydrocarbons
(PAHs), semi-volatile organic hazardous air pollutants (SVOHAPS), and volatile organic hazardous air pollutants (VOHAPS) from a hox mix
production plant during loading operations. An asphalt plant south of Los Angeles, California was selected by EPA as the host facility. Testing
was performed over five consecutive days beginning on July 24, 1998. Testing was performed under two conditions. Under normal operations, testing
was performed to characterize load-out emissions from the tunnel exhaust and load-in emissions from the asphalt concrete storage silo. Under
background conditions, testing was performed to characterize emissions from the combustion of diesel fuel in transport trucks.
The entire report consists of eight volumes totaling 4,234 pages, Vol. 1 (388 pages), Vol. 2 (308 pages), Vol. 3 ( 573 pages), Vol. 4 (694 pages),
Vol. 5 (606 pages), Vol. 6 (564 pages), Vol. 7 (570 pages), and Vol. 8 (531 pages).
17.
a. DESCRIPTIONS
Hazardous Air Pollutants
Methylene Chloride Extractable
Matter
Particulate Matter
Polynuclear Aromatic Hydrocarbons
Semi-volatile Organic Hazardous Air
Pollutants
Volatile Organic Hazardous Air
Pollutants
18. DISTRIBUTION STATEMENT
Unlimited
KEY WORDS AND DOCUMENT ANALYSIS
b. IDENTIFIERS/OPEN ENDED TERMS
' ' : •':
1 9. SECURITY CLASS (This Report)
Unclassified
20. SECURITY CLASS (This page)
Unclassified
c. COASTI Field/Group
. ., . i - •• r
21. NO. OF PAGES
Vol. 3 - 573
22. PRICE
EPA Form 2220-1 (Rev. 4-77) PREVIOUS EDITION IS OBSOLETE
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