United States
Environmental Protectior
Agency
EPA/600/R-22/037 | -July 2022
www.epa.gov/emergency-response-
research
Decontamination Options for
Surface Layers Containing
Permeated Chemical Warfare
Agents HD and VX and Pesticides
Malathion and Fipronil
Office of Research and Development
Homeland Security Research Program
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Decontamination Options for Surface Layers Containing Permeated Chemical
Warfare Agents HD and VX and Pesticides Malathion and Fipronil
Lukas Oudejans
Matthew Magnuson
Katherine Ratliff
Anne Mikelonis
U.S. Environmental Protection Agency
Office of Research and Development
Center for Environmental Solutions and Emergency Response
Research Triangle Park, NC 27711
Thomas Malloy
David See
Carissa Dodds
Battelle's Hazardous Materials Research Center (HMRC)
West Jefferson, Ohio
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DISCLAIMER
The U.S. Environmental Protection Agency (EPA) through its Office of Research and
Development (ORD) funded and managed the research described herein under Contract Number
EP-C-16-014, Task Order 6 8HERC20F0187 with Battelle. It has been subjected to the Agency's
review and has been approved for publication. Note that approval does not signify that the
contents necessarily reflect the views of the Agency. Any mention of trade names, products, or
services does not imply an endorsement by the U.S. Government or EPA. The EPA does not
endorse any commercial products, services, or enterprises. The contractor role did not include
establishing Agency policy.
Questions concerning this document, or its application should be addressed to:
Lukas Oudejans, Ph.D.
Homeland Security and Materials Management Division
Center for Environmental Solutions and Emergency Response
Office of Research and Development
U.S. Environmental Protection Agency (MD-E343-06)
109 T.W. Alexander Drive
Research Triangle Park, NC 27711
Phone: 919-541-2973
Fax:919-541-0496
E-mail: Oudeians.Lukas@epa.gov
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FOREWORD
The U.S. Environmental Protection Agency (EPA) is charged by Congress with protecting the
Nation's land, air, and water resources. Under a mandate of national environmental laws, the
Agency strives to formulate and implement actions leading to a compatible balance between
human activities and the ability of natural systems to support and nurture life. To meet this
mandate, EPA's research program is providing data and technical support for solving
environmental problems today and building a science knowledge base necessary to manage our
ecological resources wisely, understand how pollutants affect our health, and prevent or reduce
environmental risks in the future.
The Center for Environmental Solutions and Emergency Response (CESER) within the Office of
Research and Development (ORD) conducts applied, stakeholder-driven research and provides
responsive technical support to help solve the Nation's environmental challenges. The Center's
research focuses on innovative approaches to address environmental challenges associated with
the built environment. We develop technologies and decision-support tools to help safeguard
public water systems and groundwater, guide sustainable materials management, remediate sites
from traditional contamination sources and emerging environmental stressors, and address
potential threats from terrorism and natural disasters. CESER collaborates with both public and
private sector partners to foster technologies that improve the effectiveness and reduce the cost
of compliance, while anticipating emerging problems. We provide technical support to EPA
regions and programs, states, tribal nations, and federal partners, and serve as the interagency
liaison for EPA in homeland security research and technology. The Center is a leader in
providing scientific solutions to protect human health and the environment.
This report assesses various decontamination technologies and strategies to degrade toxic
persistent chemicals on the surface of permeable layers (paints and sealants) and any chemical
that permeated past the coatings and into underlying porous materials.
Gregory Sayles, Director
Center for Environmental Solutions and Emergency Response
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ACKNOWLEDGMENTS
This research is part of the U.S. Environmental Protection Agency's (EPA's) Homeland Security
Research Program's (HSRP) efforts to seek improvements in the decontamination of porous or
permeable materials that are contaminated with a persistent chemical warfare agent. This effort
was directed by the principal investigator (PI) from the Office of Research and Development's
(ORD's) Homeland Security and Materials Management Division (HSMMD) within the Center
for Environmental Solutions and Emergency Response (CESER). The contributions of the
following individuals have been a valued asset throughout this effort.
EPA Project Team
Lukas Oudejans, ORD/CESER/HSMMD (PI)
Matthew Magnuson, ORD/CESER/HSMMD
Katherine Ratliff, ORD/CESER/HSMMD
Anne Mikelonis, ORD/CESER/HSMMD
Battelle
Thomas Malloy
David See
Carissa Dodds
William Hayes
Melany Corlew
Ted Piatkowski
Jordan Vasko
Mandy Grzeskowiak
US EPA Technical Reviewers of Report
Paul Lemieux, ORD/CESER/HSMMD
Veera Boddu, ORD/CESER/HSMMD
US EPA Quality Assurance
Ramona Sherman, ORD/CESER/HSMMD
US EPA Technical Editing
Joan Bursey, ORD/CESER/HSMMD, SEE program
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EXECUTIVE SUMMARY
Under the U.S. Environmental Protection Agency's (EPA's) Homeland Security Research
Program (HSRP), research is being conducted necessary for identification of methods and
technologies that can be used during hazardous materials remediation and cleanup efforts. The
threat of a chemical warfare agent (CWA) or pesticide release into the environment is driving
EPA's HSRP to systematically evaluate potential decontamination technologies for CWAs and
mis- or overused pesticides. The efficacy of many liquid decontaminants has been observed to be
material-dependent, attributable in part to the permeability or porosity of the materials to which
the decontaminants are applied. Transport of CWA/pesticide into a permeable material often
leaves the material more difficult to decontaminate, as water-based decontaminants may not be
capable of similar penetration to reach the CWA/pesticide. Adequate decontamination then often
becomes even more difficult to achieve if CWA/pesticide permeates into a porous material under
a surface film or coating (e.g., paint or sealant).
The purpose here was to evaluate the efficacy of various liquid-based decontamination
technologies to degrade CWAs and pesticides on the surface of coating layers (films), within the
layer, and into an underlying porous material. Prior to decontamination testing, fate and transport
testing was performed for CWAs and pesticides to quantify the amount of each target chemical
that remained on the paint or sealant film surface, permeated into (and remained in) the film, and
permeated through the film to the porous material during a selected contact time.
Decontaminants were then first tested (baseline decontamination condition) to determine which
would be efficacious in decontamination of CWAs and pesticides from two freestanding coating
layers, paint and sealant. The decontaminants that were initially used for efficacy testing of
surfaces contaminated with the CWAs HD and VX included: bleach, Dahlgren Decon, and
Decon7 (D7). The decontaminants that were initially used for efficacy testing of surfaces
contaminated with the pesticides malathion and fipronil included: lOx diluted bleach and D7.
Following initial baseline decontamination technology testing, two decontaminants (full strength
bleach and Dahlgren Decon) were used in additional efficacy testing, with three evaluated
decontamination approach modifications. The modified approaches were:
• CWA Decontamination Modification 1: a double (120-minute (min)) decontamination
dwell time;
• CWA Decontamination Modification 2: application of 2-butoxyethanol (Chemical A) or
Zep® Foaming Wall Cleaner (Chemical B), followed by a water rinse, and 60-minute
bleach dwell time; and
• CWA Decontamination Modification 3: application of Chemical A, followed by a water
rinse, and 60-minute Dahlgren Decon dwell time.
Selection of Chemicals A and B was based on their use in paint strippers and as household
cleaners with stated ability to lift stains from painted surfaces.
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For pesticides, one decontaminant (D7) was included in the additional efficacy testing, with two
decontamination approach modifications evaluated:
• Pesticide Decontamination Modification 1: 60-minute D7 dwell time, followed by a
water rinse, and second 60-minute D7 dwell time.
• Pesticide Decontamination Modification 2: 120-minute D7 time.
The average total decontamination efficacy (combined efficacy based on the sum of chemical
mass recoveries from wipe sampling, film extraction, and solid-phase extraction (SPE) disk)
measured during CWA testing was low (< 50% efficacy) across all the baseline and modification
testing for both paint and sealant films; see Table E 1 for a summary of the highest CWA total
decontamination efficacies. The highest decontamination efficacy measured for HD-
contaminated paint films was demonstrated during Modification 2 testing of bleach with
Chemical A (35% average efficacy); the highest decontamination efficacy for HD-contaminated
sealant films was demonstrated during Modification 2 testing of bleach with Chemical B (14%
average efficacy). The highest decontamination efficacy measured for VX-contaminated paint
films was demonstrated during Modification 1 testing with full strength bleach (approximately
6% hypochlorite solution, with 39% average efficacy), and for VX-contaminated sealant films
was demonstrated during baseline testing with bleach (50% average efficacy). For comparison,
efficacies for decontamination of only the surface ranged from 91% to 99.99% (see Table E 1)
indicating that the degradation of these CWAs occurs but is limited to the agent on the surface.
The inclusion of Chemical A or B in the decontamination approach for the tested paint and
sealant did not assist in the reversed transfer of HD or VX to the surface for degradation of any
of the tested decontaminants. The same was absorbed for chemical transferred into the porous
sublayer (SPE disk).
Table E1. Highest HD and VX Average Total Decontamination Efficacy
Analyte
Material
Decontamination
Measurement
Decontaminant
Optimum
Decontamination
Scenario
Average
Decontamination
Efficacy
Paint
Surface
Bleach
Mod 2 w/ Chemical B
91%
HD
Total
Bleach
Mod 2 w/ Chemical A
35%
Sealant
Surface
None
None
0%!
Total
Bleach
Mod 2 w/ Chemical B
14%
Paint
Surface
Bleach
Mod 2 w/ Chemical B
99.9%
VX
Total
Bleach
Modification 1
39%
Sealant
Surface
Bleach
Modification 1
99.99%
Total
Bleach
Baseline
50%
1 Artificially low because HD was not detected for all positive control wipe samples.
Figure E 1 and Figure E 2 summarize the average total percent decontamination efficacy
measured for each test condition during baseline and modification testing for CWA.
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HD Average Total Percent Efficacy
100%
re 60%
Sealant
I I I
0%
Baseline Baseline Baseline D7 Modi Mod 1D7 Mod 2 Mod 2 Mod 3
Bleach Dahlgren Bleach Bleach w/ Bleach w/ Dahlgren
ChemA ChemB w/ChemA
Decontaminant/Modification
Figure E1. Average Total Decontamination Efficacy for HD
100%
80%
VX Average Total Percent Efficacy
>
S 60%
£
LU
£
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were mostly high (>90%) across all the baseline and modification testing for both paint and
sealant films. The highest decontamination efficacy measured for fipronil-contaminated paint
films was demonstrated during Modification 1 testing with D7 (98% average efficacy), and for
fipronil contaminated sealant films was demonstrated during baseline testing with lOx diluted
bleach (99.1% average efficacy). Fipronil does not transfer appreciably into the paint or sealant
layer in comparison to malathion. See Table E 2 for a summary of the highest pesticide surface
decontamination efficacy and total decontamination efficacy. As with CWAs, the degradation of
these pesticides occurs but is limited to analyte on the surface of the paint or sealant.
Table E 2. Highest Malathion and Fipronil Average Total Decontamination Efficacy
Analyte
Material
Decontamination
Measurement
Decontaminant
Optimum
Decontamination
Scenario
Average
Decontamination
Efficacy
Paint
Surface
None
None
OVo1
Malathion
Total
lOx Diluted Bleach
Baseline
6.8%
Sealant
Surface
D7
Modification 1
>79%
Total
D7
Modification 1
43%
Paint
Surface
D7
Modification 1
99%
Fipronil
Total
D7
Modification 1
98%
Sealant
Surface
lOx Diluted Bleach
Baseline
99.3%
Total
lOx Diluted Bleach
Baseline
99.1%
1 Artificially low because malathion was not detected for all positive control wipe samples.
Figure E 3 and Figure E 4 summarize the average total percent decontamination efficacy
measured for each test condition during baseline and modification testing for pesticides.
100%
80%
Malathion Average Total Percent Efficacy
C
QJ
" 40%
O)
a.
20%
0%
oo
Baseline lOx Diluted
Bleach
o
Baseline D7
Mod 1 D7
Decontaminant/Modification
o
Mod 2 D7
Paint
Sealant
Figure E 3. Average Total Decontamination Efficacy for Malathion
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Fipronil Average Total Percent Efficacy
100%
80%
8 60%
c
OJ
u 40%
20%
0%
Baseline lOx Diluted Baseline D7
Bleach
Mod 1 D7
Decontaminant/Modification
Mod 2 D7
I Paint
Sealant
Figure E 4. Average Total Decontamination Efficacy for Fipronil
Efficacy results for the evaluated decontamination products, both during baseline and
modification testing indicate that degradation of a chemical agent that had permeated into a paint
or sealant remains a challenge. The addition of a household cleaner with stated ability to lift
stains from a paint or sealant prior to the decontaminant application did not result in an
appreciable improvement in total decontamination efficacy. Following surface decontamination,
chemicals that permeated into the paint or sealant layer may eventually resurface over time
thereby recreating the hazard.
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TABLE OF CONTENTS
FOREWORD V
ACKNOWLEDGMENTS VI
EXECUTIVE SUMMARY VII
LIST OF FIGURES XIV
LIST OF TABLES XV
LIST OF ACRONYMS AND ABBREVIATIONS XVII
A. INTRODUCTION 1
A. 1 Proj ect Obj ectives 1
A.2 Quality Objectives and Criteria 2
A.3 Test Facility Description 3
B. RESEARCH APPROACH 4
C. MATERIALS AND METHODS 6
C. 1 CWAs and Pesticides 6
C.2 Freestanding Paint and Sealant Films 8
C.3 LVAP Assemblies 12
C.4 Decontamination Technologies 15
C.5 Wipe Sampling 18
C.6 Solvent Extraction 19
C.7 Quantitative Analysis by GC/MS 19
C.8 Quantitative Analysis by LC-MS/MS 22
C.9 Calculations 25
D. TESTING APPROACH 27
D.l Wipe Sampling Demonstration 27
D.2 Solvent Extraction Demonstration 28
D.3 Decontaminant Quench Demonstration 29
D.4 Fate and Transport Assessment 31
D.5 Baseline Decontamination Efficacy Testing 32
D.6 Modified Decontamination Efficacy Testing - CWAs 34
D.7 Modified Decontamination Efficacy Testing - Pesticides 45
E. RESULTS 47
E. 1 Wipe Sampling Demonstration Results 47
E.2 Solvent Extraction Demonstration Results 48
E.3 Decontaminant Quench Demonstration Results 49
E.4 Fate and Transport Assessment 51
E.5 Baseline Decontamination - CWAs 56
E.6 Baseline Decontamination - Pesticides 61
E.7 CWA Modification Decontamination Testing 65
E.8 Pesticide Modification Decontamination Testing 76
F. QUALITY ASSURANCE/QUALITY CONTROL 80
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F. 1 Data Quality Indicators 80
F.2 Quality Control Elements 81
F.3 Quality Assurance Audits 82
F.4 QAPP 83
G. SUMMARY 84
H. REFERENCES 89
APPENDIX A 90
APPENDIX B 92
APPENDIX C 94
APPENDIX D 96
APPENDIX E 172
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LIST OF FIGURES
Figure E 1. Average Total Decontamination Efficacy for HD ix
Figure E 2. Average Total Decontamination Efficacy for VX ix
Figure E 3. Average Total Decontamination Efficacy for Malathion x
Figure E 4. Average Total Decontamination Efficacy for Fipronil xi
Figure 1. Ortho Max Solution After 1 Day 8
Figure 2. Film Thickness Measurement Locations 9
Figure 3. SEM Image of Paint Films at Increased Magnifications (left to right) 11
Figure 4. SEM Image of Sealant Films at Increased Magnifications (left to right) 12
Figure 5. Paint Film Built into LVAP Assembly 14
Figure 6. Example of the Photo Contrast Evaluation of Bleach on Sealant 17
Figure 7. Wipe Sample Collection Pattern 18
Figure 8. Evaluation of Paint Coupons with Modification 2/3 Chemicals 37
Figure 9. Evaluation of Sealant Coupons with Modification 2/3 Chemicals 38
Figure 10. Observations of Paint Coupons After Chemical Dried 39
Figure 11. Observations of Sealant Coupons After Chemical Dried 40
Figure 12. Representative Coupons After Water Rinse 42
Figure 13. VX Interaction on Paint and Sealant Films 52
Figure 14. HD Interaction on Paint and Sealant Film Coupons 52
Figure 15. Malathion Interactions on Paint and Sealant Film Coupons 53
Figure 16. Fipronil Interactions on Paint and Sealant Films 54
Figure 17. Total Recovered Malathion for Fate and Transport Testing 55
Figure 18. Total Recovered Fipronil for Fate and Transport Testing 56
Figure 19. Decontaminant Observations when Applied to Film Coupons 56
Figure 20. Decontaminant Observations after 60-Minute Dwell Time 57
Figure 21. Sealant Film Coupon Decontaminant Observations after Dwell Time 57
Figure 22. Paint Film Decontaminant Observations after Dwell Time 58
Figure 23. HD Baseline Decontaminant Test, Average Total Mass Recoveries 60
Figure 24. VX Baseline Decontaminant Test, Average Total Mass Recoveries 61
Figure 25. Malathion Baseline Decontaminant Test, Average Total Mass Recoveries 64
Figure 26. Fipronil Baseline Decontaminant Test, Average Total Mass Recoveries 65
Figure 27. Chem A and B Observations 66
Figure 28. HD Mod 1 Decontaminant Test, Average Total Mass Recoveries 69
Figure 29. HD Mod 2 Chem A and Chem B Evaluation, Average Total Mass Recoveries 70
Figure 30. HD Mod 2 Chem A Decontaminant Test, Average Total Mass Recoveries 70
Figure 31. HD Mod 2 Chem B Decontaminant Test, Average Total Mass Recoveries 71
Figure 32. HD Mod 3 Chem A Decontaminant Test, Average Total Mass Recoveries 71
Figure 33. VX Mod 1 Decontaminant Test, Average Total Mass Recoveries 74
Figure 34. VX Mod 2 Chem A and Chem B Evaluation, Average Total Mass Recoveries 74
Figure 35. VX Mod 2 Chem A Decontaminant Test, Average Total Mass Recoveries 75
Figure 36. VX Mod 2 Chem B Decontaminant Test, Average Total Mass Recoveries 75
Figure 37. VX Mod 3 Chem A Decontaminant Test, Average Total Mass Recoveries 76
Figure 38. Malathion Modification Decontaminant Test, Average Total Mass Recoveries 78
Figure 39. Fipronil Modification Decontaminant Test, Average Total Mass Recoveries 79
Figure 40. HD Average Total Percent Efficacy 86
Figure 41. VX Average Total Percent Efficacy 87
Figure 42. Malathion Average Total Percent Efficacy 87
Figure 43. Fipronil Average Total Percent Efficacy 88
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LIST OF TABLES
Table 1. CWA Purity Sample GC/FID Analysis Method Parameters 6
Table 2. Paint and Sealant Information 8
Table 3. Prepared Paint Films and Measured Thickness 10
Table 4. Prepared Sealant Films and Measured Thickness 10
Table 5. Sprayer Characterization Results 17
Table 6. Expected Analyte Ion Transitions 20
Table 7. GC/MS Conditions for All Analyses 20
Table 8. Analysis Performance Parameters and Acceptance Criteria 22
Table 9. Analyte Ion Transitions 23
Table 10. LC-MS/MS Conditions for Analysis of VX 23
Table 11. LC-MS/MS Conditions for Analysis ofFipronil 23
Table 12. LC-MS/MS Conditions for Quantitative Analysis ofFipronil 24
Table 13. Wipe Sampling Demonstration Matrix 27
Table 14. Solvent Extraction Demonstration Matrix 28
Table 15. HD and VX Decontaminant Quench Demonstration Matrix 30
Table 16. Malathion and Fipronil Decontaminant Quench Demonstration Matrix 30
Table 17. CWA Fate and Transport Matrix 31
Table 18. Pesticide Fate and Transport Matrix 32
Table 19. CWA Baseline Decontamination Efficacy Matrix 33
Table 20. Pesticide Baseline Decontamination Efficacy Matrix 34
Table 21. HD Modification 1 Decontamination Efficacy Matrix 35
Table 22. VX Modification 1 Decontamination Efficacy Matrix 35
Table 23. Post-Spike CWA Recovery from Water Rinse 41
Table 24. CWA Modification 2 Rinse Matrix 43
Table 25. CWA Modification 2 Decontamination Efficacy Matrix 44
Table 26. CWA Modification 3 Decontamination Efficacy Matrix 45
Table 27. Pesticide Modification 1 and 2 Decontamination Efficacy Matrix 46
Table 28. CWA Wipe Sampling Results 47
Table 29. Pesticide Wipe Sampling Results 48
Table 30. CWA Extraction Sampling Results 48
Table 31. Pesticide Extraction Sampling Results 49
Table 32. CWA Quench Recovery 50
Table 33. Pesticide Quench Recovery 51
Table 34. CWA Fate and Transport Results 53
Table 35. Malathion Fate and Transport Results 54
Table 36. Fipronil Fate and Transport Results 55
Table 37. Baseline Decontaminant Efficacy Testing - CWA Average Spike Control Results 58
Table 38. Average HD Mass Recovered for Paint Film Coupons - Baseline 59
Table 39. Average HD Mass Recovered for Sealant Film Coupons - Baseline 59
Table 40. Average VX Mass Recovered for Paint Films - Baseline 60
Table 41. Average VX Mass Recovered for Sealant Films - Baseline 61
Table 42. Pesticide Average Spike Control Results - Baseline 62
Table 43. Average Malathion Mass Recovered for Paint Film Coupons - Baseline 62
Table 44. Average Malathion Mass Recovered for Sealant Films - Baseline 63
Table 45. MalaoxonMass Recovered - Baseline 63
Table 46. Average Fipronil Mass Recovered for Paint Film Coupons - Baseline 64
Table 47. Average Fipronil Mass Recovered for Sealant Film Coupons - Baseline 64
Table 48. Average CWA Spike Control Results - Modification Testing 66
Table 49. Average HD Mass Recovered for Paint Films - Modification Testing 67
Table 50. Average HD Mass Recovered for Sealant Films - Modification Testing 69
Table 51. Average VX Mass Recovered for Paint Films - Modification Testing 72
Table 52. Average VX Mass Recovered for Sealant Film Coupons - Modification Testing 73
Table 53. Pesticide Average Spike Control Results - Modification Testing 76
Table 54. Average Malathion Mass Recovered for Paint Films - Modification Testing 77
Table 55. Average Malathion Mass Recovered for Sealant Films - Modification Testing 77
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Table 56. Average Fipronil Mass Recovered for Paint Film Coupons - Modification Testing 78
Table 57. Average Fipronil Mass Recovered for Sealant Film Coupons - Modification Testing 78
Table 58. Data Quality Indicators and Results 80
Table 59. Instrument Calibration Frequency 82
Table 60. Decontaminant Downselection and Modification for CWA 85
Table 61. Decontaminant Downselection and Modification for Pesticides 85
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LIST OF ACRONYMS AND ABBREVIATIONS
°C Degree(s) Celsius
°F Degree(s) Fahrenheit
|ig microgram(s)
|iL microliter(s)
|im micrometer(s)
AMC Army Materiel Command
ANOVA Analysis of Variance
ASTM American Society for Testing and Materials (ASTM) International
BE 2-butoxyethanol
CAS Chemical Abstract Services
CCDC Combat Capabilities Development Command
CCV Continuing Calibration Verification
CESER Center for Environmental Solutions and Emergency Response
cm centimeter(s)
cm2 square centimeter(s)
CoC Chain of Custody
CWA Chemical Warfare Agent
DFTPP decafluorotriphenylphosphine
EPA U.S. Environmental Protection Agency
FID flame ionization detector
FWC Foaming Wall Cleaner
g gram
GC/MS gas chromatography/mass spectrometry
HD Sulfur Mustard
HMRC Hazardous Materials Research Center
HPLC high performance liquid chromatography
HSMMD Homeland Security and Materials Management Division
HSRP Homeland Security Research Program
ID inside diameter
in-lb inch pound(s)
IPA isopropyl alcohol
IS internal standard
LB laboratory blank
LC-MS/MS liquid chromatography - tandem mass spectrometry
LLOQ lower limit of quantitation
LRB laboratory record book
LVAP Low Volatility Agent Permeation
M molar
m2 square meter(s)
mg milligram(s)
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min
minute(s)
mL
milliliter(s)
mm
millimeter(s)
MQL
method quantification limit
MRM
multiple reaction monitoring
NIST
National Institute of Standards and Testing
OD
outside diameter
OP
organophosphate
ORD
Office of Research and Development (EPA)
PB
procedural blank
PC
positive control
PFPP
pentafluorophenylpropyl
PI
principal investigator
PTFE
polytetrafluoroethylene
QA
quality assurance
QAPP
Quality Assurance Project Plan
r2
coefficient of determination
RH
relative humidity
rpm
revolution(s) per minute
RSD
relative standard deviation
SC
spike control
SEM
scanning electron microscope
SD
standard deviation
SDS
Safety Data Sheet
SIM
selected ion monitoring
SOP
standard operating procedure
SPE
solid phase extraction
STREAMS
Scientific, Technical, Research, Engineering, and Modeling Support
STS
sodium thiosulfate
TPCS
test parameter control sheet
TSA
Technical System Audit
VR
Russian VX; O-(iso-Butyl) S-(2-diethylaminoethyl) methylphosphonothiolate
VX
O-ethyl S-(2-[diisopropylamino]-ethyl) methylphosphonothioate
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A. INTRODUCTION
The efficacy of liquid decontaminants for surfaces contaminated with chemical warfare agents
(CWAs) or pesticides has been observed in many cases (both experimentally and during field
use) to be material dependent, attributable in part to the permeability or porosity of the materials
to which the decontaminants are applied. Liquid decontaminants are often water-based, and
many are capable of high efficacy if applied to CWA contamination on nonporous materials.
However, transfer of CWA into a permeable material often leaves the material more difficult to
decontaminate, as water-based decontaminants may not be capable of similar penetration to
reach the permeated CWA. Adequate decontamination generally becomes even more difficult to
achieve if the CWA permeates into a porous material underneath a film or other coating on the
surface (e.g., paint or sealant). A CWA permeated into porous materials may also resurface
sometime after surface decontamination has taken place, recreating a potential hazard.
Decontamination technologies/approaches that can reach and degrade CWA contamination that
has permeated through surface coatings and into porous subsurfaces are therefore needed, and
this need has been identified by United States Environmental Protection Agency (EPA) as a high
priority research gap.
Testing conducted previously [1] to study CWA fate and transport characteristics utilized a
layered test sample system consisting of a freestanding film of a selected paint or sealant placed
over a solid-phase extraction (SPE) disk to simulate a permeable coating on a porous substrate
(e.g., painted wood or sealed concrete). Representative sample setups referred to as low volatility
agent permeation (LVAP) assemblies were designed for those studies. This approach allows to
readily separate the paint or sealant from the substrate below without impacting the CWA mass
distribution. The freestanding film was contaminated with either sulfur mustard (bis(2-
chloroethyl) sulfide; HD) or O-ethyl S-(2-[diisopropylamino]-ethyl) methylphosphonothioate
(VX), the CWA was allowed to permeate the film for a predetermined time period, and the
LVAP assembly components (film surface, film, and SPE disk) were subsequently sampled via
wipe collection or solvent extraction to detect and quantify HD or VX in each component.
Results indicated that the CWAs absorbed into the permeable surface coatings and transfer into
the underlying porous SPE disks.
A. 1 Project Objectives
Testing conducted during this study utilized methods based on methods developed during
previous studies [1], Objectives of this study were twofold:
• Assess the efficacy of selected decontamination technologies applied as liquids to
degrade CWA or pesticide contamination on the surface of coating layers, as well as
CWA or pesticide that has permeated through the coatings and into underlying porous
materials; and
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• Evaluate modifications to the selected decontaminants and/or decontaminant application
procedures to improve the initially measured efficacy.
Fate and transport testing was performed according to procedures developed during earlier
studies with HD and VX while using a modified LVAP assembly (refer to Section C.3). HD in
film wipe samples and extracts of films and SPE disks was quantified using gas
chromatography/mass spectrometry (GC/MS). VX was quantified in wipe and LVAP component
extracts using liquid chromatography - tandem mass spectrometry (LC-MS/MS).
Following fate and transport testing, a decontamination step was incorporated into the test
procedure, and any changes in CWA amounts recovered from the film surface (via wipe
sampling), the permeable film itself (via solvent extraction), and the underlying porous material
(SPE disk, via solvent extraction) were measured to assess decontamination efficacy.
Modifications to the decontamination step were made to attempt to improve the initially
measured efficacy of the tested decontaminants. Demonstration of measured improvements in
decontamination efficacy of the test decontaminants when applied to contaminated permeable
materials was the main focus of the testing conducted in this work.
Testing included the persistent CWAs HD and VX, as well as selected pesticides reported to be
misused in situations leading to remedial action, including malathion and fipronil. Malathion is
an organophosphate (OP)-based insecticide widely used in agriculture, outdoor pest control, and
residential landscaping. Fipronil is a broad-spectrum insecticide that belongs to the
phenylpyrazole family.
A. 2 Quality Objectives and Criteria
This work was performed under a Quality Assurance Project Plan (QAPP) [2],
The quality objectives and performance criteria described in the QAPP provide the requirements
for determining the adequacy of data generated during this project. Methods were considered
acceptable and valid data were assumed if the quality objectives for the test measurements were
met, and the Technical System Audit (TSA) and data quality audits show acceptable results.
Accuracy was ensured by the calibration of the instruments used during testing, including the
GC/MS and LC-MS/MS systems as described in Sections C.7 and C.8, respectively.
The representativeness and uniformity of the test materials were critical attributes to assure
reliable test results. For this study, representativeness meant that the freestanding paint/sealant
films used in LVAP assemblies were typical of films of the selected paints/sealants commonly
encountered in "real world" settings (e.g., painted wood or drywall, or sealed concrete) in terms
of quality, surface characteristics, thickness, etc. Uniformity meant that all films (per
paint/sealant type) were essentially equivalent for the purposes of testing. Replicate films were
obtained using as few "production batches" as possible (refer to Section C.2) so that the replicate
films were presumed to have uniform characteristics. Films and SPE disks were visually
examined and any with abnormalities on the test surfaces were rejected from use as control or
test samples.
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A. 3 Test Facility Description
All testing was performed at Battelle's Hazardous Materials Research Center (HMRC) located in
West Jefferson, Ohio. The HMRC is certified to work with chemical surety materials under a
provisioning agreement with oversight by the U.S. Army Materiel Command (AMC;
Provisioning Agreement Battelle-1). Wherever applicable and required, the reporting
requirements of this agreement were followed.
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B. RESEARCH APPROACH
The study objectives were achieved through execution of a series of tests, completed in phases
that evaluated:
• Fate and transport of the CWAs HD and VX and the pesticides malathion and fipronil
through selected paints and sealants. Fate and transport tests were performed using
modified LVAP assemblies. Pesticide fate and transport testing was conducted for 24
hours and 72 hours to ascertain the degree of malathion and fipronil permeation during
these times.
• Efficacy of select decontaminants to destroy CWAs/pesticides on the surface of paint and
sealant, as well as CW As/pesticides that have permeated the paint/sealant layers and
subsequently migrated into underlying porous materials. Measurement of the mass of
CWA/pesticide on the surface of paint/sealant films, within the films, and below the
surface of the films (within the underlying SPE disks) were performed both with
decontamination (test samples) and without decontamination (positive controls). The
efficacy of the decontamination procedures was determined by comparison of the results.
• Modifications (designed and developed based on the initially measured decontamination
efficacy) made to the selected decontamination technologies, the decontaminant
application methods, or both, to improve efficacy of the decontaminants to degrade
CWA/pesticide contamination on the surface of permeable layers as well as
CWA/pesticide that has permeated into underlying porous materials.
Prior to fate and transport and decontamination efficacy testing, methods demonstration was
performed to ensure:
• Acceptable recovery of CW As/pesticides from the surface of freestanding films of one
(1) selected paint and one (1) selected sealant via wipe sampling.
• Acceptable recovery of CW As/pesticides that have permeated into freestanding
paint/sealant films and SPE disks via solvent extraction.
• Neutralization (quench) of the reactions of tested decontaminants (i.e., decontaminant
quench), so that decontamination efficacies could be measured as a function of
decontaminant dwell time and valid efficacy data were generated.
• As part of quench testing, no extracted compounds (from wipes, freestanding
paint/sealant films, or SPE disks), test decontaminants, or quench agents present in test
samples interfere with accurate quantitation of CWAs or pesticides by LC-MS/MS and
GC/MS.
During this study, test articles consisted of freestanding films of the paint and sealant selected for
testing positioned over (and held in close contact to) SPE disks in the LVAP assemblies. Refer to
Section C.2 for more information on the specific paint and sealant that were evaluated during
testing, the methods that were used to produce freestanding films of the paint and sealant, and the
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methods for measurement of the thickness of the freestanding paint/sealant films that were
produced. This test sample setup was intended to mimic the characteristics of commonly
encountered painted or sealed porous materials (e.g., painted wood or drywall, or sealed
concrete). Refer to reference 1 for more information on the design of the LVAP assembly and
the arrangement of the assembly components.
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C. MATERIALS AND METHODS
C.1 CWAs and Pesticides
HD (Chemical Abstract Services (CAS) # 505-60-2) and VX (CAS # 50782-69-9) used for this
testing were synthesized at Battelle's HMRC under Chemical Weapons Convention program
guidelines, with accountability through the U.S. AMC. All CWAs originated from the same
synthesis lot.
HD and VX purity were determined by dissolving a known mass of the neat CWA into a known
volume of solvent (targets of 3,500 |ig/milliliter (mL) concentration for HD and 900 |ag/m L
concentration for VX) and analyzing the samples by GC/flame ionization detector (FID) to
determine the relative abundance of HD or VX as determined by peak area and reported as
percent purity. Solvent blanks were used to correct for possible solvent contaminants. Measured
purities are shown in Table 1. HD and VX purity were > 90% for all testing per QAPP
requirements.
Table 1. CWA Purity Sample GC/FID Analysis Method Parameters
CWA
Lot Number
Analysis Date
Purity
HD
C066-2
7/16/2020
100%
C066-2
10/27/2020
100%
C066-2
12/15/2020
98.9%
C066-2
1/11/2021
98.9%
C066-2
3/22/2021
99.4%
VX
C070-7-1
7/16/2020
94.7%
C070-7-1
8/19/2020
94.5%
C070-7-1
11/2/2020
92.4%
C070-7-2
12/2/2020
93.3%
C070-7-2
3/25/2021
91.6%
A commercial formulation of malathion (Ortho® Max® Malathion) was purchased for use in
testing. This formulation contained 50% malathion (CAS # 121-75-5) and 50% other ingredients;
the Ortho Max Malathion Safety Data Sheet (SDS) identified the other ingredients as solvent
naphtha (petroleum), CAS # 64742-95-6. A commercial formulation of fipronil (Termidor® SC)
was purchased for use in testing. This formulation contained 9.1% fipronil (CAS # 120068-37-
3); two other ingredients were listed on the SDS: 0.3 - 1.0% sodium N-methyl-N-oleoyltaurate
(CAS # 137-20-2) and <0.1% l,2-Benzisothiazol-3(2H)-one (CAS # 2634-33-5); the balance of
components was not identified on the SDS. The Ortho Max and Termidor SC were stored under
ambient laboratory conditions. Termidor SC was kept in its original container; however, the
Ortho Max was transferred to a new polypropylene container as the cap on the original container
leaked.
During all phases of testing involving deposition of neat CWA onto paint and sealant films,
CWA was applied using a 100-|iL Hamilton syringe equipped with a repeating dispenser. The
dispenser delivered 1/50th of the syringe volume with each actuation, thus each "click" delivered
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a 2-|iL droplet. During wipe sampling and solvent extraction methods demonstration testing, fate
and transport testing, and all decontamination efficacy testing conducted during this project,
paint and sealant films were each contaminated with a single 2-|iL droplet deposited in the
middle of the film. Mass contamination targets were thus 2,540 |ig of HD and 2,016 |ig of VX
based on density. These contamination amounts are equivalent to 2.65 and 2.10 g/ meters
squared (m2) surface concentrations, respectively, using the exposed area of the freestanding film
in the LVAP assembly (approximately 9.6 cm2). Actual mass contamination depended on percent
purity of the CWAs, as well as the precision and accuracy of the deposition method; the purity
was verified experimentally during each test through generation of three spike control samples
per test. Spike controls were generated by delivering the same quantity of CWA (2 |iL) directly
into an extraction jar (i.e., onto the side-surface of the inside of the jar) and dissolution of the
CWA in 10 mL of extraction solvent. The three spike controls were prepared at the start, middle,
and end of each test, bracketing sample spiking. Following preparation, spike controls were
sonicated and aliquoted as described below for wipe, film, and SPE disk extracts. The spike
control extract was then analyzed alongside the test and control samples.
A malathion mass contamination of 4.0 |ig/centimeters squared (cm2) and a fipronil
contamination density of 1.5 |ig/cm2 were targeted. These values were based on highest observed
surface concentrations in two pesticide misuse cases that required remediation. Based on this
target contamination mass level and the exposed area of the freestanding film in the LVAP
assembly (approximately 9.6 cm2), a target contamination mass of 38.3 |ig of malathion and 14.4
|ig of fipronil needed to be applied to the surface of films during testing. Solutions of each
pesticide were prepared in distilled water (Crystal Springs, Lakeland, FL) at the highest
concentration recommended by each manufacturer. Note that malathion is only very slightly
soluble in water [3] and fipronil has very poor solubility in water [4], To minimize the volume of
prepared pesticide solutions, three final volumes were evaluated: 4 L, 500 mL, and 100 mL.
Multiple spiking studies were performed with prepared solutions to determine the correct spiking
volume of pesticide solution. For fipronil, dilution of 1.2 mL of Termidor SC into a final volume
of 100 mL of water, and a 12-|iL volume application to a surface resulted in an average mass of
12.6 |ig of fipronil (88% of the target). This preparation was selected for all testing with fipronil.
For malathion, dilution of 0.78 mL of Ortho Max into a final volume of 100 mL of water, and a
12-|iL volume application to a surface resulted in an average mass of 34.8 |ig of malathion (91%
of target). A calibrated positive displacement pipette was used to apply a single 12 |iL droplet in
the coupon center for all testing.
As with CWA application operations, three spike controls were prepared during each test to
verify the mass of pesticide applied to test and control samples. Fresh pesticide solutions were
prepared for each day of testing.
While initial spike determination studies for malathion resulted in accurate and reproducible
surface mass loadings, the malathion surface wipe method development study indicated high and
variable mass loadings for the three spike controls (326% average recovery and 127% relative
standard deviation (RSD)). The preparation of the Ortho Max solution was then revisited. When
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prepared, the Ortho Max solution was white and cloudy, and it was noted that after being
allowed to sit overnight, a white precipitate formed (see Figure 1). The cloudiness of the
preparation may be due to the naphtha, which has very low water solubility.
Figure 1. Ortho Max Solution After 1 Day
Based on the observation of this precipitate, the Ortho Max solution was stirred with a stir bar
prior to spiking samples, and continued to be stirred while spiking samples, to help ensure a
uniform mixture. To evaluate this stirring approach, a second spiking study was performed with
three separate Ortho Max solution preparations. The average malathion recoveries for these three
solutions were 91%, 88%, and 88% with RSDs of 19%, 5.4%, and 19%, respectively. Based on
these results, continuous stirring of the solution was implemented. Additionally, the solution was
stirred for at least I hour after preparation prior to spiking samples.
C.2 Freestanding Paint and Sealant Films
The permeable surface coatings that were evaluated during this testing were:
• Behr® Premium Plus Low Odor, Paint and Primer in One Semi-Gloss Enamel
• Rust-Oleum® 6711 System Waterborne Oil-Modified Polyurethane Floor Coating.
Acrylic enamel is a low-odor coating appropriate for application onto brick, drywall, masonry,
plaster, stucco, vinyl, and wood, and the acrylic enamel is less permeable to some solvents,
resulting in easier cleaning in its intended application (the permeability of this coating to the
CWAs and pesticides is not known). Polyurethane coating/sealant is generally considered to be
highly flexible and elastic, making it suitable for application onto high traffic areas. See Table 2
for additional information.
Table 2. Paint and Sealant Information
Coating
Product
Part No.
Vendor,
Location
Paint
Behr® Premium Plus Low Odor, Paint and Primer in One
Semi-Gloss Enamel (Ultra-Pure White). 100% acrylic
202761530
Home Depot
Atlanta, GA
Sealant
Rust-Oleum® 6711 System Waterborne Oil-Modified
Polyurethane Floor Coating (Clear)
4MG61
Grainger,
Lake Forest,
1L
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Quality and uniformity of free films, both paint and sealant, are highly dependent on the
rheological behavior of the liquid, the application method, and the release substrate to which they
are applied. Freestanding films of the paint and sealant shown in Table 2 were prepared using
ASTM International (ASTM) method D823 "Standard Practices for Producing Films of Uniform
Thickness of Paint, Varnish, and Related Products on Test Panels" [5], A Universal Blade
Applicator (AP-G08, Paul N. Gardner Company, Pompano Beach, FL) was used.
Each gallon of paint/sealant was placed on a standard paint shaker (Northern Tool, Burnsville,
MN) for 10 minutes to ensure a homogenous mix. Due to the excessive air entrapped in the
coatings during this process, a de-gas step was also used. Small batches of approximately 80
grams (g) were de-gassed in a Speed Mixer™ (FlackTeck, Louisville, CO) for 3 minutes at 3,000
revolutions per minute (rpm) to remove entrapped air.
A polytetrafluoroethylene (PTFE) (Teflon®) (Chemfab CF1, Saint-Gobain, Elk Grove, IL)
coated fabric was selected as the release substrate for the Behr® semi-gloss enamel and a
polyethylene film (Silthene, Siliconature, Caledonia, MI) was selected as the release substrate for
the Rust-Oleum® polyurethane coating. Additional substrate surface preparation techniques in
the form of plasma treatment (to promote good surface wetting and film quality during the
drying process) were required. An AtomFlo 500 (Surfx, Redondo Beach, CA) plasma treater
using helium and oxygen plasma gases at 160 watts of power was used.
Following preparation, all freestanding films were visually examined and any areas with obvious
abnormalities on the test surface, such as bubbles, pinholes, or visible contaminants in the paint
were rejected from use as test samples. Thickness of the freestanding paint and sealant films was
measured using an eddy current gauge (PosiTector® 6000, DeFelsko Corporation, Ogdensburg,
NY) according to ASTM method E376 "Standard Practice for Measuring Coating Thickness by
Magnetic-Field or Eddy-Current (Electromagnetic) Test Methods" [6], Thickness was measured
in each of six (6) unique areas on each film sheet, as identified in Figure 2.
Figure 2. Film Thickness Measurement Locations
Individual coupons were cut from the film sheets using a 4.5-centimeter (cm) diameter die, then
allowed to cure for a minimum of 14 days at constant temperature (24 °C) and relative humidity
(50% RH). Table 3 and Table 4 provide the thickness measurements collected for each of the
freestanding films prepared, and the number of coupons collected from each film. The thickness
across each sheet was quite consistent, typically < 6% RSD. Average film thickness was also
consistent across sheets: 5.3% RSD for paint sheets and 4.3% RSD for sealant sheets. A total of
382 paint coupons and 336 sealant coupons were prepared. Note that coupons were cut from
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Sheets B1 and B5 on 1/21/21, approximately 6 months after other coupons used in testing. These
two sheets had been held at 24 °C and 50% RH prior to cutting. The "new" coupons were used
during malathion and fipronil developmental testing. Paint and sealant films were inspected
visually prior to testing to ensure no coupons with surface anomalies were used. As discussed
below, no notable differences in performance of these sheets were obvious in the data.
Table 3. Prepared Paint Films and Measured Thickness
Sheet ID
Draw
Wet Film
Thickness
(mils)
Dry Film Thickness (mils)
No.
Coupons
Collected
Down Date
2
3
5
6
Average
RSD
B1
6/5/2020
10
2.27
2.29
2.13
2.26
2.41
2.20
2.3
3.9%
29
B2
6/5/2020
10
2.25
2.30
2.31
2.18
2.33
2.39
2.3
3.0%
Uncut
B3
6/5/2020
10
2.15
2.12
2.19
2.39
2.21
2.25
2.2
4.5%
Uncut
B4
6/5/2020
10
2.21
2.25
2.33
2.25
2.23
2.18
2.2
2.3%
Uncut
B5
6/8/2020
10
2.32
2.20
2.40
2.26
2.32
2.23
2.3
3.0%
34
B6
6/8/2020
10
2.39
2.23
2.55
2.19
2.35
2.20
2.3
6.1%
Uncut
B7
6/9/2020
10
2.53
2.47
2.30
2.27
2.50
2.45
2.4
4.6%
Uncut
B8
6/9/2020
10
2.51
2.38
2.47
2.48
2.69
2.32
2.5
5.2%
Uncut
B9
6/9/2020
10
2.74
2.53
2.82
2.56
2.59
2.62
2.6
4.2%
Uncut
B10
6/10/2020
10
2.56
2.43
2.52
2.80
2.75
2.43
2.6
6.2%
34
Bll
6/10/2020
10
2.48
2.36
2.60
2.48
2.57
2.63
2.5
4.0%
42
B12
6/10/2020
10
2.35
2.38
2.40
2.30
2.53
2.58
2.4
4.6%
48
B13
6/10/2020
10
2.23
2.37
2.24
2.30
2.31
2.27
2.3
2.2%
32
B14
6/10/2020
10
2.20
2.25
2.23
2.52
2.31
2.28
2.3
5.2%
29
B15
6/10/2020
10
2.21
2.48
2.65
2.59
2.38
2.42
2.5
6.4%
45
B16
6/10/2020
10
2.43
2.52
2.63
2.59
2.62
2.42
2.5
3.6%
45
B17
6/10/2020
10
2.56
2.34
2.56
2.36
2.31
2.47
2.4
4.6%
44
Table 4. Prepared Sealant Films and Measured Thickness
Draw
Wet Film
Dry Film Thickness (mils)
No.
Sheet ID
Down Date
Thickness
(mils)
2
3
D
5
6
Average
RSD
Coupons
Collected
R1
6/5/2020
10
2.51
2.68
2.58
2.53
2.45
2.56
2.6
3.1%
33
R2
6/5/2020
10
2.23
2.19
2.36
2.25
2.27
2.29
2.3
2.6%
43
R3
6/5/2020
10
2.47
2.28
2.23
2.54
2.49
2.61
2.4
6.3%
38
R4
6/5/2020
10
2.57
2.42
2.44
2.63
2.51
2.48
2.5
3.2%
38
R5
6/5/2020
10
2.20
2.55
2.39
2.27
2.17
1.55
2.2
15%
38
R6
6/5/2020
10
2.44
2.23
2.48
2.20
2.53
2.53
2.4
6.3%
36
R7
6/5/2020
10
2.58
2.49
2.36
2.44
2.31
2.45
2.4
4.2%
26
R8
6/8/2020
10
2.28
2.26
2.50
2.27
2.38
2.52
2.4
5.0%
50
R9
6/8/2020
10
2.28
2.31
2.53
2.49
2.35
2.45
2.4
4.2%
34
R10
6/8/2020
10
2.47
2.62
2.50
2.46
2.27
2.62
2.5
5.2%
Uncut
Rll
6/8/2020
10
2.55
2.61
2.32
2.24
2.51
2.43
2.4
5.8%
Uncut
Scanning electron microscope (SEM) images were taken of paint and sealant film samples. SEM
images were taken in August 2020 (just prior to the start of testing) and again in February 2021
(see Figure 3 and Figure 4). No significant differences were observed in the images taken at the
two time points, indicating that the films were not physically changing over time. Closeups of
paint and sealant films reveal localized but isolated depressions (2-10 |im in diameter).
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s
Figure 3. SEM Image of Paint Films at Increased Magnifications (left to right).
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Figure 4. SEM Image of Sealant Films at Increased Magnifications (left to right).
C.3 LVAPAssemblies
The LVAP test methodology was used during previous studies [1] to evaluate fate and transport
of HD and VX on, into, and across films of various paints and sealants in contact with SPE disks
(to simulate a permeable coating over a porous subsurface). The CWA was spiked onto the
surface of paint/sealant films, and as CWA permeated through the films, it was absorbed and
retained by the underlying SPE disk. A weight placed on top of the LVAP assembly compressed
the assembly components and held the paint/sealant film and SPE disk in close contact.
A modified version of the LVAP arrangement used during previous studies was used for this
work that eliminated the need for a weight to be placed on top of the LVAP assembly to
compress the assembly components, so that formation of a limited headspace above the
CWA/pesticide-contaminated film was avoided. Rather than using a weight, a top compression
plate was placed onto bolts attached to a bottom support plate. The bottom support plate was
constructed of Type 316 stainless steel and measured 3 inches by 3 inches with 14-inch thickness.
Four 1-inch long V4-20 thread hex head screws were attached to the bottom support plate at each
side. A 5-cm diameter PTFE disk was placed on the bottom support plate centered between the
hex screws. As used previously, a CDS Empore™ SDB-XC SPE disk (a
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poly(styrenedivinylbenzene) copolymer used as a reversed phase sorbent for SPE) was used to
simulate a porous subsurface. Each 47-mm diameter SPE disk was die cut to a diameter of 36
mm to provide a contact area of approximately 10 cm2 beneath the paint/sealant film and the SPE
disk was centered on top of the PTFE disk. A latex gasket die cut to 36 mm inside diameter [ID],
51 mm outside diameter [OD], was placed around the SPE disk. A freestanding film coupon
(4.5-cm diameter) of the paint or sealant selected for evaluation was then placed directly on top
of the SPE disk/latex gasket and held in close contact using a steel washer (1.375-inch ID, 1.875-
inch OD, 0.125-inch thickness, type 316 stainless steel). The exposed surface area of the
paint/sealant film coupon inside the steel washer was approximately 9.6 cm2.
The steel washer worked in conjunction with the latex gasket around the SPE disk to isolate the
outside edge of the SPE disk and prevent fugitive CWA or pesticide from reaching the SPE disk,
mitigating the possibility of false positive results. A top compression was placed on top of the
steel washer onto the screws attached to the bottom support plate to compress the assembly and
ensure adequate contact between the paint/sealant film and the underlying SPE disk. Nuts
threaded onto the screws secured the top compression plate in place. A torque wrench was used
to tighten the nuts (target torque of 4 inch-pounds [in-lb]) to ensure consistent compression
across the plate. The opening in the top compression plate allowed films to be spiked with the
compression plate in place. Figure 5 depicts the step-by-step procedure for loading a freestanding
paint film coupon into an LVAP assembly for fate and transport testing.
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Bottom support plate with screws
5-cm diameter PTFE disk
Latex gasket (36-mm, 51-mm OD)
36-mm OD SPE disk
Paint/sealant film coupon over SPE
Type 316 stainless steel washer
Top compression plate (open
center)
Nuts to anchor and compress plates
1.
2.
3.
4.
5.
6.
7.
Figure 5. Paint Film Built into LVAPAssembly
The completed LVAP assemblies were placed in 3.75-inch square (1.5-inch deep) hard clear
acrylic boxes during the CWA/pesticide contact period to prevent cross contamination of the
films by fugitive CWA/pesticide vapors from other nearby LVAP assemblies. The acrylic boxes
were loosely closed so that any CWA/pesticide that evaporated from the surface of the film
could slowly and passively escape the box (drawn toward the back of the chemical fume hood in
which testing was performed) so buildup of vapor in the local test environment was avoided, and
buildup of vapor within the box was avoided. The acrylic boxes used to contain LVAP
assemblies were disposed of following each test.
Following application of CWA or pesticide to the film coupon surface, samples remained
undisturbed under ambient laboratory conditions. Laboratory temperature and relative humidity
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were monitored and recorded for the duration of all tests but not controlled. Appendix B provides
the starting temperature and RH for each trial.
C.4 Decontamination Technologies
The following three decontaminant technologies were selected for testing:
1. Bleach (Arocep Ultra Bleach, Champion Packaging & Distribution Inc., Woodridge, IL).
Commercially available 6% sodium hypochlorite solution. Purchased as 1-gallon
containers and used as received.
2. Decon7 (D7), (Part # 7001702, Decon7 Systems, Scottsdale, AZ) is a three-component
decontaminant system that is purchased as premeasured components (Part 1, Part 2, Part
3) and mixed in a ratio of 49:49:2. The components include surfactants/inorganic salts
(Part 1), hydrogen peroxide (Part 2), and diacetin (Part 3) as a hydrogen peroxide booster.
3. Dahlgren Decon (DD-006-RTU, First Line Technology, Chantilly, VA) is a three-
component decontaminant system including water and a surfactant package (Part A),
sodium hydroxide (Part Bl), and peracetyl borate (active ingredient; Part B2; releases
peracetic acid upon dissolution in water). Normally, Part A comes as a solid and must be
dissolved in water before mixing with Parts Bl and B2, but for this testing a "ready-to-
use" (RTU) version was used that provides Part A already dissolved in water from the
manufacturer.
Fresh solutions of Decon7 and Dahlgren Decon were prepared prior to use on each day of
testing. The pH and activity of each test decontaminant (following any necessary preparation)
were measured prior to use on each day of testing (see Appendix A). The pH of each
decontaminant was measured using a calibrated pH meter (Orion Star™ A221 pH portable
meter, STARA2210). Hypochlorite concentration for bleach was measured with a Hach model
CN-HRDT hypochlorite test kit. Bleach hypochlorite concentration was quite consistent across
all testing, ranging from 5.5 - 6.4%. Hypochlorite concentrations for bleach diluted 10-fold were
correspondingly lower, ranging from 0.63 - 0.67%. Hydrogen peroxide concentration for D7 was
measured with a Hach model HYP-1 hydrogen peroxide test kit. D7 hydrogen peroxide was
generally consistent, ranging from 3.9 - 5.8%. However, for the pesticide quench study the
hydrogen peroxide activity was only 1.2%. This low reading ultimately did not impact test result
interpretation, as it apparently still provided the needed stoichiometric excess of oxidant. The
peracetic acid concentration in Dahlgren Decon was measured using a titration approach
provided by First Line Technology (see Appendix C for the titration procedure, list of chemicals
and materials, and the equation for calculating percent peracetic acid). Dahlgren Decon peracetic
acid levels ranged from 6.3-11%.
An oil mister/sprayer (CHEFVANTAGE, model# S02-P02-V20-SS-2) was used to apply
decontaminant to the surface of paint and sealant film coupons in the LVAP assemblies with an
application approach based on the approach used during previous testing [7], A different sprayer
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was used for each test decontaminant. New sprayers were used for each test day and then
disposed of after one use. The following procedure was used to apply decontaminant:
1. The sprayer was filled to approximately half full (-80 mL) with decontaminant. The
sprayer reservoir was marked to indicate the fill level. The sprayer was then pumped
twenty times to pressurize.
2. The sprayer was held approximately 10 inches directly above the film coupon in the
LVAP assembly. The sash of the test hood was set to a height of 10 inches and the
operator used the sash as a guide to ensure the sprayer standoff distance was maintained
throughout each application.
3. The sprayer was actuated to begin spray delivery of decontaminant and the sprayer was
passed over the film in the LVAP assembly three times (using a "back, forth, back"
motion/pattern) to completely cover the film surface. Only one LVAP assembly was
sprayed at a time.
4. The sprayer was pumped three additional times after each set of three replicate three-pass
applications to maintain pressurization of the sprayer.
5. Before each test, each sprayer filled with decontaminant was checked to verify
reproducible spray application (RSD < 15%). Three replicate Teflon disks (1.65"
diameter) were sprayed with each decontaminant following the same spray procedure
used for the film coupons. The weight of the applied decontaminant on each Teflon disk
was recorded, and RSD was calculated.
Given the nature of the LVAP assembly, the decontaminant applied to the film coupons
remained within the ID of the stainless-steel washer compressed against the paint/sealant film.
Water was used to perform sprayer characterization using five sprayer units. PTFE disks were
installed in LVAP assemblies, and the above procedure was followed. Following each three-pass
application of water, the PTFE disks were removed from LVAP assemblies and weighed to
determine the mass of water delivered to the exposed disk area, which was then converted to
volume of water. One LVAP assembly was repeatedly set up with PTFE disks to allow collection
of three replicates with a single sprayer (Collection Set 1), after which the sprayer was pumped
three times to maintain pressure, and then an additional three replicates were collected
(Collection Set 2). Average measured masses for the three replicates are shown in Table 5 along
with the mass converted to volume. The average volume of water applied from the five sprayers
was 111 |iL (13% RSD) for Collection Set 1 and 110 |iL (7.9% RSD) for Collection Set 2. These
results indicated consistent water application between sprayers and following re-pressurization of
the sprayers.
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Table 5. Sprayer Characterization Results
Collection
Set
Water Delivered
Sprayer
1
Sprayer
2
Sprayer
3
Sprayer
4
Sprayer
5
Average
All
Sprayers
1
Average Mass (g)
0.1046
0.1026
0.1289
0.0973
0.1236
0.1114
Average Volume (uL)
105
103
129
97
124
111
RSD
3.3%
8.1%
6.1%
19%
16%
13%
Pumped three times to maintain pressure
2
Average Mass (g)
0.1074
0.0972
0.1179
0.1096
0.1182
0.1101
Average Volume (|iL)
107
97
118
110
118
110
RSD
22%
22%
13%
12%
7.7%
7.9%
Representative photographs of paint and sealant film coupons covered with decontaminant in
LVAP assemblies following spray-application were taken and processed using ImageJ image
processing software. Only bleach was evaluated in this manner because D7 and Dahlgren Decon
visually exhibited uniform coverage. Five pictures of the same sealant coupon were individually
evaluated using the ImageJ software. There was some variation based on reflection between each
of the pictures. On average, the film coupon was measured to be 88±3% wet (see example photo
and ImageJ evaluation in Figure 6). The Figure 6 image evaluation determined 0.208 square
inches of dry surface for the 2.40 square inch-coupon or 91% of the coupon being wet.
Bleach on Sealant Coupon Photo ImageJ Software Evaluation of Photo
Figure 6. Example of the Photo Contrast Evaluation of Bleach on Sealant
Following application, the decontaminants were allowed to remain undisturbed on the surface of
films for a predetermined period of time (60 minutes during baseline decontamination efficacy
testing). Films were left uncovered in LVAP assemblies during the decontaminant dwell period.
Visual observations of the wetness of each film surface at the end of the decontami nant dwell
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period (prior to wipe sampling) was recorded. Following the decontaminant dwell period, the
surface of each film was sampled via wiping according to procedures described in Section C.5.
C.5 Wipe Sampling
The wipe-sampling method used during this testing to recover HD, VX, malathion, and fipronil
from the surface of freestanding paint and sealant film coupons was consistent with the method
developed during previous studies to recover VX and HD from the surface of films of the same
paint and sealant selected for evaluation during this work:
• Lint-free 2-inch by 2-inch, four (4)-ply rayon/polyester blend (gauze) sponges (22-037-
921, Fisher Scientific, Pittsburgh, PA) were used.
• Wipes used to sample HD and malathion-contaminated films were wetted with 1.5 mL of
hexane. Wipes used to sample VX and fipronil-contaminated films were wetted with 1.5
mL of isopropyl alcohol (IPA). This wetting volume is half of the volume of solvent
determined experimentally during previous studies to be necessary to saturate the gauze
wipe. Compatibility of the solvents with the paint and sealant films had been
demonstrated during previous studies.
• During fate and transport and decontamination efficacy testing, film coupons were wiped
while still built into LVAP assemblies, i.e., LVAP assemblies were not disassembled, and
films removed prior to wipe sampling.
• Films were wiped using a defined 3-pass wipe pattern including four horizontal strokes,
four vertical strokes, and a perimeter stroke. Wipes were folded between passes so that
the CWA-/pesticide-exposed surface of the wipe was folded into the wipe. Figure 7
illustrates the wipe sampling pattern that was used.
Fold wipe Fold wipe
(contamination inside fold} (contamination inside fold)
• Four (4) vertical • Four (4) horizontal ¦ Perimeter
strokes strokes
Figure 7. Wipe Sample Collection Pattern
• Given the small surface area of the film coupons inside the stainless-steel washer in the
LVAP assemblies, wipe passes were short (film length/width) and partially placed on top
of each other.
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• During most of the decontamination efficacy testing, no blotting or rinsing of any excess
liquid decontaminant remaining on the surface of films was performed. The excess
decontaminant was absorbed into the wipe during the wiping action. As discussed in
Section D.3, adequate methods for quenching the decontaminant reactions were
demonstrated prior to decontamination efficacy testing.
Following collection, wipes were extracted in solvent using the same method used to extract
freestanding films and SPE disks, as described in Section C.6, using the same solvents as those
used to wet the wipes. Wipe extracts were analyzed via GC/MS (HD and malathion) or LC-
MS/MS (VX and fipronil) as described in Sections C.7 and C.8, respectively.
C. 6 Solvent Extraction
Recovery of HD, VX, malathion, and fipronil via solvent extraction from wipes, freestanding
film coupons of paint and sealant, and SPE disks during this testing was accomplished using the
extraction methods developed and used in previous studies to recover HD and VX from the same
films and SPE disks selected for this work.
Wipes, film coupons, and SPE disks were extracted by placing each into a separate 60-mL glass
jar containing 10 mL of extraction solvent. //-Hexane (Fisher Scientific, Part # H306-4) was
selected for extraction of HD and malathion from wipes and films; isopropanol (Fisher
Scientific, Part # A464-4) was selected for extraction of VX and fipronil from wipes and films;
and acetone (Fisher Scientific, Part # A929-4) was selected for extraction of all target chemicals
from SPE disks. All solvents were high-performance liquid chromatography (HPLC)-grade or
better. Prior to extraction of samples, 5 mL of a 3 molar (M) solution of sodium thiosulfate (STS,
Fisher Scientific, Part # S446-500) in water was included in each jar with the solvent as a quench
for the decontaminants. Wipes, film coupons, and SPE disks were able to lie flat within the
inside diameter of the extraction jars fully submerged in the extraction solvent.
Following addition of each wipe, film coupon, and SPE disk to the extraction solvent, the jars
were swirled by hand for approximately 5 to 10 seconds and placed into an ultrasonic bath.
Extraction jars were sonicated at 40 to 60 kHz for 10 min. The temperature of the water in the
ultrasonic bath was not allowed to increase by more than 10 °C above ambient temperature.
Within 30 minutes of completing sonication, approximately 0.5 mL aliquots from each extraction
jar were transferred to duplicate GC or LC autosampler vials and capped. One vial served as a
primary analysis sample, and the second was stored as an archive sample. Samples that were not
analyzed the day of preparation were stored at -20 ± 10 °C until analysis was performed.
Samples were analyzed within 3 days for CWAs or 4 days for pesticides after they were prepared
during testing (in accordance with the decontaminant quench and sample preservation method
demonstrated during method development testing, as described in Section D.3).
C. 7 Quantitative Analysis by GC/MS
Extracts of wipe samples, film coupons, and SPE disks from samples contaminated with HD and
malathion were analyzed in selected ion monitoring (SIM) mode on an Agilent 7890 or 8890 GC
using an Agilent 5977A or 5977B Agilent mass selective detector. Data were acquired using
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Agilent MassHunter Software. Naphthalene-d8 was used as an internal standard (IS) for HD mass
quantification while malathion-dio was used as the internal stand for malathion mass
quantification. Malaoxon (CAS # 1634-78-2), a malathion degradation product, was also
quantified; malathion-dio was used as the IS for malaoxon. Quantification and qualifier ions for
each analyte are shown in Table 6.
Table 6. Expected Analyte Ion Transitions
Analyte
Quantification
m/z
Qualifier
m/z
HD
109
111, 158, 160
Naphthalene-dg
136
134, 137, 108
Malathion
173
127, 99
Malathion-dio
183
132, 100
Malaoxon
99
127, 142
The GC/MS was tuned initially and as needed following manufacturer's guidelines. Prior to
running each set of samples, a decafluorotriphenylphosphine (DFTPP) tune check analysis was
performed with the MS run in the full scan mode to ensure proper MS operation. A 12-hour tune
time was not employed.
Table 7. GC/MS Conditions for All Analyses
Parameter
DFTPP Analysis
HD Analysis
Malathion Analysis
Column
Rxi-5Sil MS, 30.0 meters by 0.25 millimeters (mm), 0.25 micrometers (|im)
film thickness
Liner Type
4 mm split/splitless
Carrier Gas Flow
1.5 mL/min
1.2 mL/min
1.5 mL/min
50 °C initial temp.,
hold 0.0 minutes,
30 °C/minute to 280
°C,
hold 3.0 minutes
50 °C initial temp..
100 °C initial temp.,
hold 0.50 minutes, 20
Column
hold 0.50 minutes.
°C/minute to 250 °C,
Temperature
30 °C/minute to 280
hold 1.0 minute.
°C, hold 0.50 minutes.
30 °C/minute to 280 °C,
hold 0.50 minutes.
Injection Volume
1.0 uL
2.0 uL
2.0 uL
Injection Temp.
250 °C
MS Quad Temp.
150 °C
MS Source Temp.
230 °C
HD stock solutions were prepared in hexane and acetone from HD Lot Number C066-2. Stock
solution concentrations were calculated using Equation 1:
^ _ vA xda xpa
Ca~p- (1)
where:
Ca = analyte concentration in the solution (milligrams (mg)/mL)
Va = volume of the analyte added to the solvent (|iL)
Da = density of the analyte (mg/|iL)
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Pa = purity of the analyte (refer to Table 1)
Vs = volume of the solvent (mL)
Naphthalene-d8 was purchased from Supelco (part # 442716, 250 mg). A 505 |ag/m L
naphthalene-d8 solution was prepared in //-hexane. Malathion was purchased from Sigma-
Aldrich (part # 36143, 100 mg) as was malaoxon (part # 36142, 100 mg vial). Stock solutions
containing a cocktail of malathion and malaoxon at an equal concentration were prepared by
dissolving a known mass of each analyte in a known volume of solvent. Malathion/malaoxon
stock solutions were prepared in both hexane and acetone. Malathion-dio was purchased from
Sigma-Aldrich (part # 3514, 10 mg). A 250-micrograms (|ig)/mL malathion-dio solution was
prepared in «-hexane.
Stock solutions were used to prepare separate HD and malathion/malaoxon calibration standards
in both //-hexane and acetone to allow matrix matching of calibration standards with sample
extracts. A six-point calibration was analyzed prior to each set of sample analyses; concentration
levels for both HD, malathion, and malaoxon were: 0.10, 0.50, 1.0, 2.5, 5.0, and 10 |ig/mL.
Continuing calibration verification (CCV) standards were prepared by a second analyst at 0.10
and 5.0 |ig/mL. CCV analysis was performed after every five samples, alternating between low
and high concentration CCVs, and at the end of the analytical sequence. Prior to analysis
calibration standards, CCVs, and samples were spiked with naphthalene-d8 or malathion-dio at a
final concentration of 5.0 |ig/ml. The expiration date for HD and malathion calibration standards
was six months, while CCVs had a three-month expiration date. Calibration standards and CCVs
were stored in a freezer at -20 ± 10 °C when not in use.
A linear or quadratic regression was used to describe the data with 1/x or 1/x2 weighting with the
origin excluded. Refer to Table 8 for analysis performance parameters and acceptance criteria.
The GC/MS was recalibrated if the coefficient of determination (r2) from the regression analysis
of the standards was less than 0.990. Each calibration standard or CCV was required to calculate
back (using the established calibration curve) to within ±15% of the nominal standard
concentration. The lowest calibration standard and CCV were required to be within ±25% of the
nominal standard concentration. Following analysis of the calibration standards at the beginning
of each analytical run, a solvent blank sample was analyzed to confirm that no target analyte
carryover above the lowest calibration standard had occurred. Internal standard area in the test
samples was compared to the area of internal standard in the nearest passing calibration standard
or passing CCV.
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Table 8. Analysis Performance Parameters and Acceptance Criteria
Parameter
Criterion
Calibration curve coefficient of determination (r2)
>0.990
Acceptance limit for lowest calibration standard processed
against curve
75 - 125%
Acceptance limit for remaining calibration standards processed
against curve
85 - 115%
Solvent blank samples
< lowest calibration standard
Acceptance limit for lowest CCV
75 - 125%
Acceptance limit for remaining CCVs
85 - 115%
Signal-to-noise ratio for the lowest calibration standard
Minimum of 3:1
Retention time for target compound and IS
±0.1 min as same compounds in mid-
level calibration standard
IS area in samples
50% to 200% area of nearest passing
calibration standard or passing CCV,
criteria per EPA Method 8000D [81
The concentration of analyte in samples was interpolated using the analyte area/IS area ratio and
the regression equation generated from calibration standards. Samples that quantitated below the
lowest calibration standard concentration of the curve were reported as less than the Lower Limit
of Quantitation (LLOQ), e.g., <0.10 |ig/mL. Samples that quantitated above the highest
calibration standard of the curve were diluted using calibrated positive displacement pipettes and
reanalyzed. If the internal standard area was outside the acceptance range of 50% - 200%, the
sample dilution factor was increased to reduce matrix effects until a passing internal standard
area was obtained; the LLOQ was adjusted on a per-sample basis to account for any required
dilutions. All data were reported to two significant figures.
C. 8 Quantitative Analysis by LC-MS/MS
Extracts of wipes, film coupons, and SPE disks contaminated with VX and fipronil were
analyzed using reversed-phase HPLC and multiple reaction monitoring (MRM) mass
spectrometry on an AB Sciex 5500 triple quadrupole MS coupled to a Shimadzu 20 XR series
LC. VR (Russian VX; CAS # 159939-87-4) was obtained from the U.S. Army Combat
Capabilities Development Command (CCDC) Chemical Biological Center as a solution (85.7
|ig/mL, lot # RVX/IPA-7145-R&T-DIL-C) and used as the internal standard for quantitation of
VX. Labeled fipronil (13C4, 15N2; CNLM-9650-1.2, Cambridge Isotope Laboratories, Inc.) was
used as the internal standard for quantitation of fipronil. Internal standard was added to
calibration standards, controls, and test sample extracts just prior to LC-MS/MS analysis using a
solution of VR or labeled fipronil in water as the sample diluent. Table 9 provides the ion
transitions used for quantitation of the analytes, and Table 10 and Table 11 provide additional
LC-MS/MS method conditions for each analyte.
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Table 9. Anafyte Ion Transitions
Analyte
Precursor Ion
Product Ion Quantifier
VX
268
128
VR
268
100
Fipronil
435
330
Labeled Fipronil
441
336
The most sensitive transitions for fipronil and fipronil 13C4 internal standard are 435 > 330 and
439 > 334, respectively. However, the fipronil molecule contains two chlorine atoms causing its
chlorine isotopes to add significant area to the most sensitive fipronil 13C4 transition, resulting in
varied internal standard areas based on the concentration of fipronil in the sample. For this
reason, the second most abundant carbon isotope of fipronil, 13C4, was selected as the internal
standard transition, 441 > 336.
Table 10. LC-MS/MS Conditions for Analysis ofVX
Parameter
Description
Ionization Mode and Polarity
Electrospray ionization, positive mode
HPLC Column
Restek Allure pentafluorophenylpropyl (PFPP), 2.1 x 50 mm, 5 |im.
part 9169552
Column Temperature
Ambient
Mobile Phase
A: 2 millimoles (inM) Formic Acid/2 mM Ammonium Formate in
Water
B: 2 mM Formic Acid/2 mM Ammonium Formate in Methanol
Mobile Phase Gradient
Time (minutes)
%B
Flow Rate (mL/min)
0.0
20
0.5
1.0
20
0.5
2.0
100
0.7
4.0
100
0.7
4.1
20
0.5
4.5
20
0.5
Typical Injection Volume
5 uL
Run Time
4.5 minutes
Table 11. LC-MS/MS Conditions for Analysis of Fipronil
Parameter
Description
Ionization Mode and Polarity
Electrospray ionization, negative mode
HPLC Column
Waters Atlantis dC18, 2.1 x 50 mm, 3 |im. part 186001291
Column Temperature
Ambient
Mobile Phase
A: 2 mM Formic Acid/2 mM Ammonium Formate in Water
B: 2 mM Formic Acid/2 mM Ammonium Formate in Methanol
Mobile Phase Gradient
Time (minutes)
%B
Flow Rate (mL/min)
0.0
15
0.3
1.0
15
0.3
3.0
100
0.3
4.0
100
0.3
4.1
15
0.3
5.0
15
0.3
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Typical Injection Volume
10 uL
Run Time
5.0 minutes
Neat VX and a purchased fipronil stock (AccuStandard P-738S-A, 100 jag/mL in acetone) were
used to prepare calibration standards in both isopropanol and acetone to allow matrix matching
of calibration standards with sample extracts. Stock solutions of VX were prepared from Lot
Number C070-7-1 or C070-7-2 (refer to Table 1). Table 12 provides a summary of the
calibration level concentrations for standards and CCVs. The expiration date for VX and fipronil
calibration standards was three months from the date of preparation. The expiration date for VX
CC V standards was one month from the date of preparation. The expiration date for fipronil
CCV standards was three months from the date of preparation. Calibration standards and CCVs
were stored at -20 ± 10 °C. The signal-to-noise ratio of the lowest calibration standard was
required to be 3:1 at minimum.
Table 12. LC-MS/MS Conditions for Quantitative Analysis of Fipronil
Calibration
VX
Fipronil
Level
(ng/mL)
(ng/mL)
1
0.010
0.010
2
0.020
0.040
3
0.040
0.20
4
0.20
0.40
5
0.40
1.0
6
1.0
2.0
7
2.0
5.0
Low CCV
0.010
0.010
High CCV
1.0
2.0
IS
0.45
1.8
CCVs prepared by a second analyst were analyzed prior to sample analysis and after no more
than every ten samples. Quantifiable samples bracketed by a failing CCV were reanalyzed.
Calibration standards and CCVs were matrix-matched to the samples as closely as possible. For
example, test samples in IPA prepared for analysis by a 10-fold dilution in water were
quantitated using calibration standards and CCVs prepared in 10% IPA. Note that due to this 10-
fold dilution performed during sample preparation, the LLOQs for VX and fipronil were 0.10
ng/mL.
A linear or quadratic regression was used to describe the data with 1/x2 weighting with the origin
excluded. Each calibration standard or CCV was required to calculate back (using the established
calibration curve) to within ±15% of the nominal standard concentration. The lowest calibration
standard and CCV were required to be within ±25% of the nominal standard concentration.
Table 8 provides a summary of the analytical run acceptance criteria for various parameters.
The concentration of analyte in samples was interpolated using the analyte area/IS area ratio and
the regression equation generated from calibration standards. Samples that quantitated below the
lowest calibration standard concentration, or displayed area counts below the area counts of the
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lowest concentration on the calibration curve, were reported as less than the LLOQ corrected to
account for the sample dilution factor (e.g., <0.10 ng/mL). Samples that quantitated above the
highest calibration standard were diluted using calibrated positive displacement pipettes and
reanalyzed. If the internal standard area was outside the acceptance range of 50% - 200%, the
sample dilution factor was increased to reduce matrix effects until a passing internal standard
area was obtained. All data were reported to two significant figures.
C. 9 Calculations
Wipe, film coupon, and SPE disk extract concentrations of CWAs and pesticides for all test,
control, and blank samples were calculated in units of |ag/m L for GC/MS analyses and ng/mL for
LC-MS/MS analyses. All calibrations used an internal standard. Instrument software was used to
calibrate each instrument. A quadratic regression or weighted quadratic regression was typically
used for a calibration fit for all compounds.
Mass recovered from the wipe samples, film coupons, and SPE disks via extraction was
determined according to Equation 2:
MassRec = x VolExt (2)
Conv v
where: MassRec = CWA or pesticide mass recovered from the wipe/film coupon/SPE disk
fog)
ConcExt = Wipe, film, or SPE disk extract CWA/pesticide concentration (in units of
ng/mL or |ig/mL)
VolExt = Volume of wipe/film/SPE disk extraction solvent (mL)
Conv = Conversion factor (1000 for LC-MS/MS analyses; 1 for GC/MS analyses)
Total sample mass was determined using the average masses recovered from the wipe sample,
paint/sealant film coupon, and SPE disk according to Equation 3:
MassTot MassRec (wipe) McLSSRgC (film) MassRec (spe) (3)
where: MassTot= Average total CW A/pesticide mass recovered (|ig)
MassRec (wipe) = Average CWA/pesticide mass recovered from the wipe sample (|ig)
MassRec (film) = Average CWA/pesticide mass recovered from the film (|ig)
MassRec (spe) = Average CWA/pesticide mass recovered from the SPE disk (|ig)
CWA or pesticide total decontamination efficacy was calculated using the average total mass
recovered from the test samples and associated positive controls according to Equation 4:
£ _ {MassTotjpos) - MassTot(test)\ ^ ^
^ \ MassTot (pos) )
where: Et = Total decontamination efficacy (%)
MassTot (test) = Average total CWA/pesticide mass recovered from a test sample (|ig)
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MassTot (Pos) = Average total CWA/pesticide mass recovered from the associated
positive control (|ig)
Surface decontamination efficacy was calculated based only on wipe results using Equation 5.
For surface decontamination efficacy, the average total mass recovered was replaced with
average wipe mass recovered for the test samples and average wipe mass recovered for the
positive controls.
g f Masswipe (pos) ~ Masswipe(test)\ ^ ^QQ (5^
\ Ma.SSwipe (pos) )
where: Es = Surface decontamination efficacy (%)
Masswipe (test) = Average wipe CW A/pesticide mass recovered from a
test sample (|ig)
Masswipe (pos) = Average wipe CW A/pesticide mass recovered from the associated
positive control (|ig)
For each CWA or pesticide, film type, and decontamination technology (or technology
modification) combination, the surface and total decontamination efficacy was reported.
The propagation of error for the surface and total decontamination efficacy was also calculated.
Equation 4 and equation 5 can be rewritten as Equation 6:
£=^2=1- a/6 (6)
where: a = MassTot (test)
b MassTot (pos)
The decontamination efficacy error (AE) was calculated using Equation 7:
AE = (1 - E) + (%f (7)
where: A a = the standard deviation of a
Ab = the standard deviation of b
In cases where one or more replicates was a nondetect, for either the test sample or positive
control, a standard deviation could not reasonably be calculated for those samples, and therefore
the efficacy error was not calculated.
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D. TESTING APPROACH
D. 1 Wipe Sampling Demonstration
The film surface wipe sampling methods developed for CWAs during previous testing [1] were
evaluated for use in recovering residual surface HD, VX, malathion, and fipronil contamination
from the surface of paint and sealant films during this testing. The wipe sampling method
demonstration testing evaluated recovery of HD, VX, malathion, and fipronil from freestanding
films of the paint and sealant selected for this project. Freestanding films of the paint and sealant
were contaminated with 2 |iL of CWA or 12 |iL of pesticide solution, and the solutions were
allowed to be in contact with the surface of the film coupons for 60 minutes. Following the
contact period, film coupons were wiped, extracted, and analyzed as described above.
Table 13 provides the wipe-sampling method demonstration test matrix. The matrix was
completed a total of four times, one time each for HD, VX, malathion, and fipronil. Three
replicates of paint film and sealant film coupons were evaluated for wipe recovery along with
three replicates of stainless steel coupons (2-inch diameter 18-8 stainless steel disk shim) used as
a nonpermeable control material. One replicate of each film and one replicate stainless steel
coupon were sampled via direct extraction rather than by wipe sampling to assess the mass of
CWA/pesticide that evaporates from the surface of the films during the 60-minute contact period
(i.e., evaporation controls).
In addition to the test sample film coupons and evaporation controls, a single procedural blank
per material type was included. Procedural blanks were not spiked with CWA or pesticide but
were wipe-sampled and analyzed alongside the test samples. A single laboratory blank per
material type was also included. Laboratory blanks were not spiked with CWA or pesticide and
were sampled via direct solvent extraction. Three spike control samples were prepared to
confirm the CWA/pesticide application mass.
Table 13. Wipe Sampling Demonstration Matrix
Sample
Type
Material
Contaminant
Spike Vol.
Contaminant
Contact Period
Sampling
Method
Replicates
Test
Paint
2 nL or 12 nL
60 minutes
Wipe Sampling
3
Test
Sealant
2 nL or 12 nL
60 minutes
Wipe Sampling
3
Control
Stainless Steel
2 nL or 12 nL
60 minutes
Wipe Sampling
3
Evaporation Control
Paint
2 nL or 12 nL
60 minutes
Extraction
1
Evaporation Control
Sealant
2 nL or 12 nL
60 minutes
Extraction
1
Evaporation Control
Stainless Steel
2 nL or 12 nL
60 minutes
Extraction
1
Procedural Blank
Paint
None
NA
Wipe Sampling
1
Procedural Blank
Sealant
None
NA
Wipe Sampling
1
Procedural Blank
Stainless Steel
None
NA
Wipe Sampling
1
Laboratory Blank
Paint
None
NA
Extraction
1
Laboratory Blank
Sealant
None
NA
Extraction
1
Laboratory Blank
Stainless Steel
None
NA
Extraction
1
Spike Control
None
2 nL or 12 nL
NA
Extraction
3
NA = not applicable
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The average recoveries from the spike controls were required to be within 80% to 120% of the
theoretical target amount with a replicate RSD of < 30% (n=3). The wipe-sampling method was
deemed acceptable for use during subsequent fate and transport and decontamination efficacy
testing if the average wipe-sampling recoveries were within the range of 70% to 120% of the
average of the spike control results with a replicate RSD < 30% (n=3). Procedural blanks and
laboratory blanks should have had less than 50% of the lowest detected amount on the test
coupon.
I). 2 Solvent Extraction Demonstration
Recovery of HD, VX, malathion, and fipronil via extraction of paint and sealant film coupons
and SPE disks in solvent was evaluated. Solvent extraction methods were based on the methods
developed and used during previous testing [1], Solvent extraction method demonstration testing
evaluated recovery of HD, VX, malathion, and fipronil from freestanding film coupons of the
paint and sealant selected for this project and from SPE disks. Freestanding film coupons of the
paint and sealant and SPE disks were contaminated with 2 |iL of CWA or 12 |iL of pesticide
solution, and the solution was allowed to be in contact with the surface of film coupons/within
the SPE disks for 60 minutes. Following the contact period, film coupons and SPE disks were
extracted and analyzed as described above.
Table 14 provides the solvent extraction method demonstration test matrix. The matrix was
completed four times, once each for HD, VX, malathion, and fipronil. Three replicates of paint
and sealant films and SPE disks were evaluated for solvent extraction recovery along with three
replicates of stainless steel used as a nonpermeable control material.
In addition to the test sample film coupons, SPE disks, and evaporation controls, a single
laboratory blank per material type was included. Laboratory blanks were not spiked with CWA
or pesticide. Three spike control samples were prepared to confirm the CWA/pesticide
application mass.
Table 14. Solvent Extraction Demonstration Matrix
Sample
Type
Material
Contaminant
Spike Vol.
Contaminant
Contact Period
Replicates
Test
Paint
2 nL or 12 nL
60 minutes
3
Test
Sealant
2 nL or 12 nL
60 minutes
3
Test
SPE Disk
2 nL or 12 nL
60 minutes
3
Control
Stainless Steel
2 nL or 12 nL
60 minutes
3
Laboratory Blank
Paint
None
NA
1
Laboratory Blank
Sealant
None
NA
1
Laboratory Blank
SPE Disk
None
NA
1
Laboratory Blank
Stainless Steel
None
NA
1
Spike Control
None
2 nL or 12 nL
NA
3
The average recoveries from the spike controls were required to be within 80% to 120% of the
target amount and a replicate RSD of < 30% (n=3). The solvent extraction method was deemed
acceptable for use during subsequent fate and transport and decontamination efficacy testing if
the average wipe-sampling recoveries were within the range of 70% to 120% of the average of
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the spike control results with a replicate RSD < 30% (n=3). Laboratory blanks should have had
less than 50% of the lowest detected amount on the test coupon.
D.3 Decontaminant Quench Demonstration
During decontamination efficacy testing residual decontaminant (absorbed into wipes and
potentially present in film and SPE disk extracts) could continue to decontaminate CWA and
pesticides beyond the defined decontaminant dwell periods, create complex sample matrices,
and/or cause analytical interference such as false-positive or false-negative results or analyte
enhancement or suppression. Effective methods for quenching decontaminants following the
decontaminant dwell period were determined to allow efficacy of each tested decontaminant to
be evaluated as a function of dwell time. Additionally, assessment of matrix effects was
evaluated to ensure the sample matrices did not interfere with analysis.
Prior to decontamination efficacy testing, the method for quenching (i.e., halting) the reactions of
three decontaminants were demonstrated so that decontamination efficacy could be measured as
solely a function of decontaminant dwell time on the films. During a previous study [9], a 3 M
solution of STS in water was found to effectively halt the reaction of various test
decontaminants, including decontaminants based on hypochlorite, peroxide, and peracetic acid
active ingredients. Procedurally, 5 mL of 3 M STS was included with the 10 mL of solvent used
to extract decontaminated samples. This method was evaluated for use during this testing to halt
the reactions of test decontaminants so that CWAs/pesticides in extracts of wipes, films, and SPE
disks following the decontaminant dwell period were preserved for quantitation.
Table 15 provides the experimental matrix for HD and VX decontaminant quench that was
intended to serve two purposes: to evaluate 3 M STS as an appropriate quench solution for
neutralizing the decontaminant reaction with HD and VX and to evaluate possible effects from
residual decontaminant, the 3 M STS quench agent itself, and/or extracted wipe/film coupon/SPE
disk compounds on the analysis of HD and VX and the response of the associated internal
standards. Each sample was spiked with a mass of HD that represented 2% of the total mass used
for testing or 0.001% of the total VX mass used for testing. Note that each replicate resulted in
one wipe sample, one film sample, and one SPE disk sample. This experimental matrix was
completed twice, once for HD and once for VX.
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Table 15. HD and VX Decontaniinant Quench Demonstration Matrix
Sample Type
Decontaminant
Decontaminant
Dwell Period
Spike Mass
Replicates
Test
Bleach
60 minutes
HD = 49 ug
3
VX = 20 ng
3
Test
D7
60 minutes
HD = 49 ug
3
VX = 20 ng
3
Test
Dahlgren Decon
60 minutes
HD = 49 ug
3
VX = 20 ng
3
Positive Control
None
NA
HD = 49 ug
3
VX = 20 ng
3
Procedural Blank
Bleach
60 minutes
NA
1
Procedural Blank
D7
60 minutes
NA
1
Procedural Blank
Dahlgren Decon
60 minutes
NA
1
Laboratory Blank
None
NA
NA
1
Spike Control
None
NA
HD = 49 ug
VX = 20 ng
3
Table 16 provides the experimental matrix for malathion and fipronil decontaminant quench that
serves the same purposes as the matrix for the HD and VX. Note that a 10-fold dilution of bleach
in water and D7 were the only decontaminants selected for pesticide testing. Each sample was
spiked with the same mass of malathion or fipronil as was used in testing. Note that each
replicate resulted in one wipe sample, one film sample, and one SPE disk sample. This matrix
was completed twice, once for malathion and once for fipronil.
Table 16. Malathion and Fipronil Decontaminant Quench Demonstration Matrix
Sample Type
Decontaminant
Decontaminant
Dwell Period
Spike Mass
Replicates
Test
lOx Diluted
Bleach
60 minutes
malathion = 37 ug
fipronil = 14 ug
3
Test
D7
60 minutes
malathion = 37 ug
fipronil = 14 ug/mL
3
Positive Control
None
NA
malathion = 37 ug
fipronil = 14 ug
3
Procedural Blank
10 x Bleach
60 minutes
NA
1
Procedural Blank
D7
60 minutes
NA
1
Laboratory Blank
None
NA
NA
1
Spike Control
None
NA
malathion = 37 ug
fipronil = 14 ug
3
Decontaminant quench samples representative of decontamination efficacy testing were prepared
by applying decontaminants by spray application as described above to paint film coupons in
LVAP assemblies and allowing the decontaminants to contact the films for 60 minutes. Note that
only paint film coupons were used for decontaminant quench demonstration. Following the
decontaminant contact period, the paint film coupons were wiped, and the wipe samples
extracted by sonication. The LVAP assemblies were then disassembled and the paint films and
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SPE disks were solvent extracted by sonication. Quench solution (5 mL of 3 M STS) was added
to the jars containing the 10 mL of solvent for extraction of the wipes, film coupons, and SPE
disks.
Each target analyte was added to the 10 mL of extraction solvent at a known concentration. The
final concentrations in solvent were as follows: HD = 4.9 |ig/mL, VX = 2.0 ng/mL, malathion =
3.7 |ig/mL, and fipronil =1.4 |ig/mL. Aliquots of the extracts were collected from the solvent
layer following sonication and analyzed by GC/MS for HD and malathion and LC-MS/MS for
VX and fipronil. Following the initial analyses, the HD and VX extracts were stored at -20 ±10
°C for 3 days (nominal 72 hours) and the malathion and fipronil extracts were stored for 4 days
(nominal 96 hours). Following the 3-day or 4-day storage period, the extracts were analyzed
again via LC-MS/MS or GC/MS. The initial and reanalysis results were compared to each other,
the nominal spike concentration, and to positive controls to determine the effectiveness of the
quench method.
The following acceptance criteria needed to be met for the quench demonstration to have been
successful:
• Recovery of CWA/pesticide mass was > 70% relative to the positive control for samples
containing representative amounts of test decontaminants (quench samples).
• The criteria for internal standard response were satisfied.
Additionally, the results for sample extracts analyzed after 72 hours or 96 hours were compared
to the initial analyses to determine if sample extract archives could be stored without
degradation.
D.4 Fate and Transport Assessment
Previous fate and transport evaluations [1] used LVAP test methodologies to determine that HD
and VX applied to the surface of paint and sealant films would penetrate the permeable films and
migrate into underlying porous materials. Fate and transport testing conducted during this project
was conducted to replicate earlier testing.
Fate and transport testing was conducted using the modified LVAP test cell assemblies as
described in Section C.3. Table 17 provides the CWA fate and transport test matrix; this matrix
was performed twice, once using HD with a 24-hour contact time and once using VX with 72-
hour contact time. Note that each replicate resulted in one wipe sample, one film coupon sample,
and one SPE disk sample.
Table 17. CWA Fate and Transport Matrix
Sample Type
Material
CWA Spike
Vol.
Replicates
Test
Paint
2 uL
3
Test
Sealant
2 uL
3
Lab Blank
Paint
NA
1
Lab Blank
Sealant
NA
1
Spike Control
None
2 uL
3
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For malathion and fipronil, a contact period of 24 and 72 hours was determined to be evaluated
as these data had not previously been collected. Table 18 provides a matrix for fate and transport
testing using the two pesticides. This matrix was performed twice, once using malathion and
once using fipronil. Note that each replicate resulted in one wipe sample, one film coupon
sample, and one SPE disk sample.
Table 18. Pesticide Fate and Transport Matrix
Sample Type
Material
Pesticide
Solution
Spike Vol.
Contact
Period
Replicates
Test
Paint
12 uL
24 hours
3
Test
Paint
12 uL
72 hours
3
Test
Sealant
12 uL
24 hours
3
Test
Sealant
12 uL
72 hours
3
Lab Blank
Paint
NA
24 hours
1
Lab Blank
Paint
NA
72 hours
1
Lab Blank
Sealant
NA
24 hours
1
Lab Blank
Sealant
NA
72 hours
1
Spike Control
None
12 uL
NA
3
Neat CWA was applied to the films as a single 2-|iL droplet, and pesticide solutions were
applied as a single 12-|iL droplet. Following the contact period all films were sampled via
wiping. LVAP assemblies were disassembled and paint/sealant film coupons and SPE disks were
extracted in solvent. Sample extracts were analyzed by GC/MS for HD and malathion or LC-
MS/MS for VX and fipronil to quantify CWAs/pesticides in each LVAP assembly component.
Laboratory blanks were included and sampled and analyzed alongside the test samples. Three
spike controls were prepared during each test to confirm the mass of CWA/pesticide applied to
test samples.
Based on the results of the 24-hour and 72-hour malathion and fipronil wipe, film, and SPE disk
samples (see Section D.4), a 72-hour contact time was selected for use with malathion and
fipronil decontamination efficacy testing.
I). 5 Baseline Decontamination Efficacy Testing
Following fate and transport testing, the decontamination step was incorporated to evaluate
baseline efficacy of selected decontaminants for CWAs and pesticides. Test samples were
contaminated, decontaminated, sampled, and analyzed for CWA/pesticide. Decontamination
efficacy was defined as the percentage of CWA or pesticide remaining in the LVAP test sample
assembly components (total from the wipe sample, freestanding film, and SPE disk extracts)
compared to the positive control samples. Surface decontamination efficacy was defined as the
percentage of CWA or pesticide remaining on the surface (wipe sample) compared to the
positive control samples.
Table 19 provides a test matrix for evaluating the baseline efficacy of three decontaminants
(bleach, D7, and Dahlgren Decon) against HD and VX applied to the surface of paint and sealant
film coupons; this matrix was performed twice, once using HD with a 24-hour contact time and
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once using VX with 72-hour contact time. Decontaminant dwell time was 60 minutes for all
baseline testing. Paint and sealant films were tested in triplicate. Note that each replicate resulted
in one wipe sample, one film sample, and one SPE disk sample.
CWA positive control samples were also prepared in triplicate but did not have decontaminant
applied. Procedural blank samples were not contaminated with CWA but were decontaminated
and processed alongside the test samples. Laboratory blank samples were neither contaminated
nor decontaminated and were also processed alongside the test samples. Procedural blanks and
laboratory blanks should have had less than 50% of the lowest detected amount on the test
coupon. Three spike controls were prepared during each test to confirm the mass of CWA
applied to the test samples. The average recoveries from the spike controls were required to be
within 80% to 120% of the theoretical target amount with a replicate RSD of < 30% (n=3).
Table 19. CWA Baseline Decontamination Efficacy Matrix
Sample Type
Material
CWA Spike
Vol.
Decontaminant
Replicates
Test
Paint
2 uL
Bleach
3
Test
Paint
2 uL
D7
3
Test
Paint
2 uL
Dahlgren Decon
3
Test
Sealant
2 uL
Bleach
3
Test
Sealant
2 uL
D7
3
Test
Sealant
2 uL
Dahlgren Decon
3
Positive Control
Paint
2 uL
None
3
Positive Control
Sealant
2 uL
None
3
Procedural Blank
Paint
NA
Bleach
1
Procedural Blank
Paint
NA
D7
1
Procedural Blank
Paint
NA
Dahlgren Decon
1
Procedural Blank
Sealant
NA
Bleach
1
Procedural Blank
Sealant
NA
D7
1
Procedural Blank
Sealant
NA
Dahlgren Decon
1
Lab Blank
Paint
NA
None
1
Lab Blank
Sealant
NA
None
1
Spike Control
None
2 uL
None
3
Table 20 provides a test matrix for evaluating the baseline efficacy of two decontaminants (10-
fold dilution of bleach in water and D7) against malathion and fipronil applied to the surface of
paint and sealant films; this matrix was performed twice, once using malathion and once using
fipronil, both with a 72-hour pesticide contact time. Decontaminant dwell time was 60 minutes
for all baseline testing. Paint and sealant film coupons were tested in triplicate. Note that each
replicate resulted in one wipe sample, one film coupon sample, and one SPE disk sample.
Pesticide positive control samples were also prepared in triplicate but did not have
decontaminant applied. Procedural blank samples were not contaminated with pesticide but were
decontaminated and processed alongside the test samples. Laboratory blank samples were neither
contaminated nor decontaminated and were also processed alongside the test samples. Procedural
blanks and laboratory blanks should have had less than 50% of the lowest detected amount on
the test coupon. Three spike controls were prepared during each test to confirm the mass of
pesticide applied to the test samples. The average recoveries from the spike controls were
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required to be within 80% to 120% of the theoretical target amount with a replicate RSD of <
30% (n=3).
Table 20. Pesticide Baseline Decontamination Efficacy Matrix
Sample Type
Material
Pesticide
Solution
Spike Vol.
Decontaminant
Replicates
Test
Paint
12 uL
lOx Diluted Bleach
3
Test
Paint
12 uL
D7
3
Test
Sealant
12 uL
lOx Diluted Bleach
3
Test
Sealant
12 uL
D7
3
Positive Control
Paint
12 uL
None
3
Positive Control
Sealant
12 uL
None
3
Procedural Blank
Paint
NA
lOx Diluted Bleach
1
Procedural Blank
Paint
NA
D7
1
Procedural Blank
Sealant
NA
lOx Diluted Bleach
1
Procedural Blank
Sealant
NA
D7
1
Lab Blank
Paint
NA
None
1
Lab Blank
Sealant
NA
None
1
Spike Control
None
12 uL
None
3
Following the CWA/pesticide contact period, decontaminants were sprayed onto the film
surfaces as described in Section C.4. Following the decontaminant dwell time, film coupons
were wiped, and the wipes were solvent-extracted. The LVAP assemblies were then
disassembled and paint/sealant film coupons and SPE disks were solvent-extracted. Wipe, film,
and SPE disk extracts were analyzed via GC/MS for HD and malathion or LC-MS/MS for VX
and fipronil to quantify residual CWA/pesticide.
Baseline efficacy of the decontaminants was determined through comparison of CWA/pesticide
masses recovered from decontaminated test samples to the CWA/pesticide masses recovered
from positive control samples.
D. 6 Modified Decontamination Efficacy Testing - CWAs
Based on the results of testing to determine the baseline performance of the selected
decontaminants, modifications to the decontamination approaches were made to improve the
measured decontamination efficacies. Also based on the result of baseline testing, a down
selection to two decontaminants was made for CWA testing and to one decontaminant for
pesticide testing. Aside from the modifications, testing was conducted in a manner identical to
baseline decontamination efficacy testing. Efficacy of the modified decontamination approaches
was determined through comparison of CWA/pesticide masses recovered from decontaminated
test samples to the CWA/pesticide masses recovered from positive controls. Calculated efficacies
of the modified decontamination approaches were also compared to the baseline efficacies to
determine if any of the modifications made to the decontamination approaches resulted in
efficacy improvements.
Modification 1 for HD and VX decontamination evaluated the effect of increasing
decontaminant dwell time from 60 minutes to 120 minutes. Table 21 provides a test matrix for
evaluating the Modification 1 efficacy of two decontaminants (bleach and D7) against HD
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applied to the surface of paint and sealant film coupons with a 24-hour contact time. Table 22
provides a test matrix for evaluating the Modification 1 efficacy of two decontaminants (bleach
and Dahlgren Decon) against VX applied to the surface of paint and sealant films with a 72-hour
contact time. For HD and VX, paint and sealant film coupons were tested in triplicate. Note that
each replicate resulted in one wipe sample, one film extraction sample, and one SPE disk sample.
CWA positive control samples were also prepared in triplicate but did not have decontaminant
applied. Procedural blank samples were not contaminated with CWA but were decontaminated
and processed alongside the test samples. Laboratory blank samples were neither contaminated
nor decontaminated and were also processed alongside the test samples. Procedural blanks and
laboratory blanks should have had less than 50% of the lowest detected amount on the test
coupon. Three spike controls were prepared during each test to confirm the mass of CWA
applied to the test samples. The average recoveries from the spike controls were required to be
within 80% to 120% of the theoretical target amount with a replicate RSD of < 30% (n=3).
Table 21. HD Modification 1 Decontamination Efficacy Matrix
Sample Type
Material
CWA Spike
Vol.
Decontaminant
Replicates
Test
Paint
2 uL
Bleach
3
Test
Paint
2 uL
D7
3
Test
Sealant
2 uL
Bleach
3
Test
Sealant
2 uL
D7
3
Positive Control
Paint
2 uL
None
3
Positive Control
Sealant
2 uL
None
3
Procedural Blank
Paint
NA
Bleach
1
Procedural Blank
Paint
NA
D7
1
Procedural Blank
Sealant
NA
Bleach
1
Procedural Blank
Sealant
NA
D7
1
Lab Blank
Paint
NA
None
1
Lab Blank
Sealant
NA
None
1
Spike Control
None
2 uL
None
3
Table 22. VX Modification 1 Decontamination Efficacy Matrix
Sample Type
Material
CWA Spike
Vol.
Decontaminant
Replicates
Test
Paint
2 uL
Bleach
3
Test
Paint
2 uL
Dahlgren Decon
3
Test
Sealant
2 uL
Bleach
3
Test
Sealant
2 uL
Dahlgren Decon
3
Positive Control
Paint
2 uL
None
3
Positive Control
Sealant
2 uL
None
3
Procedural Blank
Paint
NA
Bleach
1
Procedural Blank
Paint
NA
Dahlgren Decon
1
Procedural Blank
Sealant
NA
Bleach
1
Procedural Blank
Sealant
NA
Dahlgren Decon
1
Lab Blank
Paint
NA
None
1
Lab Blank
Sealant
NA
None
1
Spike Control
None
2 uL
None
3
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Modification 2 and Modification 3 both evaluated the use of chemical treatments to potentially
extract CWA from paint and sealant film coupons prior to the application of decontaminant. The
chemicals that were selected for testing were 2-butoxyethanol (CAS # 111-76-2), (Fisher
Scientific, Part # AC154330010) and Zep® Foaming Wall Cleaner (FWC) with primary active
ingredients per the SDS of l-butoxypropan-2-ol (CAS # 5131-66-8), 1-5 % and 2-(2-
butoxyethoxy)ethanol (CAS # 112-34-5), 1-5 %. These chemicals were selected based on their
commercial use as cleansers with the ability to "lift" stains from surfaces. A proof-of-concept
testing was initially performed to evaluate the effects of both chemicals on the paint and sealant
films. The effects of each chemical on the analysis of HD and VX were also evaluated. Three
different solutions of 2-butoxyethanol (BE) in distilled water were evaluated: 30% BE, 10% BE,
and 0.5% BE. Zep FWC was purchased as an 18-ounce spray can and used as received (shaken
well before each use).
All three BE solutions and the FWC were separately applied to a single paint coupon and a
single sealant coupon installed in an LVAP assembly. A calibrated positive displacement pipette
was used to apply 1.0 mL of the BE solutions; the 30% and 10% solutions covered 100% of the
coupon surface while the 0.5% solution appeared to cover < 90% of the surface due to beading
on the surface. The can of FWC was held about 9 inches above the coupon and applied by
performing three spray-passes across the coupons. The mass of applied FWC was characterized
by spraying the chemical to a Teflon disk (10 replicates) following the same spray procedure,
then using a balance to weigh the amount of chemical on the Teflon disk. The average mass
applied to the 20 cm2 surface was 0.30 g with an RSD of 7.9%.
Observations were made and photographs taken at different time points (see Figure 8 and Figure
9) until each chemical was visibly dry on the coupon surface or until 4 hours had passed (see
Figure 10 and Figure 11). Each chemical was also applied to stainless steel coupons for visual
evaluation of residue after drying; no visible residue was observed for either chemical (photos
not shown). As the 30% BE appeared to interact too aggressively with the films and the 0.5% BE
did not cover the film surface well, the 10% BE was selected for testing. A residence time of 10
minutes on the paint film and 60 minutes on the sealant film was selected not to damage the film
coupons (see highlighted photos in Figure 8 and Figure 9); the 10% BE solution had not dried at
either of these time points. A residence time of 5 minutes was selected for the FWC (see
highlighted photos in Figure 8 and Figure 9, during which the FWC remained wet.
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After 1 hour
After 2 hours
After 3 hours (d
Immediate!
After 1 hour
After 2 hours
After 3 hours (dry)
Immediate!
After 1 hour
After 2.5 hours
After 4 hours (dry)
Immcdiatcl
After 5 min
After 10 min
After 30 min
Immediately
Figure 8. Evaluation of Paint Coupons with Modification 2/3 Chemicals
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Figure 9. Evaluation of Sealant Coupons with Modification 2/3 Chemicals
After 30 min
After 10 min
After 30 min
After 3 hours (dry)
After 3 hours (dry)
After 4 hours (wet)
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• Coupon was deformed/wrinkled
• Teflon below coupon was wet
• Coupon was slightly tacky
Coupon was defonned/wrinkled/stretched
Coupon was shriveling up once removed
Teflon below coupon was wet
Coupon was tacky
• Coupon was deformed/wrinkled
• Dry residue observed on Teflon
• Coupon was not tacky
• Coupon was slightly deformed/w rinkled
• Dry residue observed on Teflon
• Coupon was slightly tacky
Figure 10. Observations of Paint Coupons After Chemical Dried
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10%
BE
I - ^HD
• Coupon was deformed/wrinkled
• No chemical breakthrough to Teflon
• Coupon was slightly tacky
30%
BE
lit HJL- ^
• Coupon was deformed/wrinkled
• Coupon difficult to remove from LVAP assembly
• Coupon was shriveling up once removed
• Teflon below coupon was wet
• Coupon was tacky
0.5% BE
• Chemical not dry after 4 hours
• No visible deformation/deterioration
• No chemical breakthrough to Teflon
• Coupon was not tacky
FWC
• No visible deformation
• Slight residue/discoloration
• No chemical breakthrough to Teflon
• Coupon was not tacky
Figure 11. Observations of Sealant Coupons After Chemical Dried
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A water rinse was then evaluated for removal of each chemical following treatment prior to
application of decontaminant. Each chemical (1.0 mL of 10% BE and 0.3 g of FWC spray) were
applied to paint and sealant coupons installed in LVAP assemblies and allowed to remain on the
surface for the selected residence times; tests were performed in triplicate. Rinsing consisted of 3
x 2.0 mL applications of distilled water applied to the coupon with a positive displacement
pipette. Each water application was allowed to sit for 5 minutes prior to removal with a Pasteur
pipette; all three rinses were combined in a glass vial and inspected for evidence of dissolved
paint/sealant. No visible dissolved paint/sealant was observed in any of the water rinse samples,
however, the water rinse for FWC on paint was slightly foamy.
An aliquot of the combined rinsate was postspiked with VX at a concentration of 2.0 ng/mL and
analyzed. To isolate HD from the combined rinsate a 1.0 mL aliquot was postspiked with HD at
concentration of 1.0 |ag/m L and extracted 1:1 with //-hexane, which resulted in a gel-like
emulsion for all samples. A 1.0-mL aliquot was then postspiked with HD at concentration of 2.5
|ig/mL and extracted 1:5 with hexane, which resulted in cloudy samples but no emulsions. The
HD samples were then centrifuged at 1,000 rpm for 5 minutes to form two layers. The top
organic layer was analyzed for HD. Table 23 shows the recovery of HD and VX for each
chemical applied to each film type; all recoveries were > 90%. Unspiked rinsate was also
analyzed for HD and VX. Results were all below the detection limit: <0.50 jag/mL for the 1:5
HD extraction and <0.10 ng/mL for VX.
Table 23. Post-Spike CWA Recovery from Water Rinse
Chemical
Material
Average HD
Recovery
HDRSD
Average VX
Recovery
VXRSD
10% BE
Paint
97%
0.12%
97%
3.5%
Sealant
125%
2.8%
101%
1.9%
FWC
Paint
98%
0.80%
95%
4.9%
Sealant
98%
1.9%
94%
0.65%
Based on these results, no negative or positive interferences for HD or VX were expected during
the analysis of water used to rinse the two test chemicals from paint and sealant coupons.
After rinsing was complete, the paint and sealant coupons were removed from the LVAP
assemblies and inspected to immediately determine if any residual chemical remained on the
coupons and if the coupons were negatively impacted by the chemicals. No obvious residue was
observed on any of the coupons, however, the paint coupons that had FWC applied were tacky.
Coupons were inspected a second time after 30 minutes, at which point all coupons were dry and
the paint/ FWC coupons were no longer tacky. Representative coupons are shown in Figure 12.
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Coupons After Rinsing
Chemical
Paint Sealant
Figure 12. Representative Coupons After Water Rinse
Prior to conducting CWA Modification 2 and 3 testing, a study was performed to evaluate use of
10% BE (designated as "Chemical A" or "Chem A" during testing) and FWC (Chem B) to
remove HD and VX without the addition of decontaminants, as shown in Table 24. This matrix
was performed twice, once using ITD with a 24-hour contact time and once using VX with 72-
hour contact time. Following the CWA contact time, 1.0 mL of Chem A was applied with a
residence time of 10 minutes on the paint film and 60 minutes on the sealant film. Chem B was
sprayed onto the coupons with a residence time of 5 minutes. Following the chemical treatment
residence time, each coupon was rinsed with 3 x 2.0 mL of water. The water rinses were
aggregated and analyzed for HD or VX as described above. Following the water rinse, films
were wiped, and the wipe solvent was extracted. The LVAP assemblies were then disassembled
and paint/sealant films and SPE disks were solvent extracted. Paint and sealant films were tested
in triplicate. Note that each replicate resulted in one wipe sample, one film coupon sample, and
one SPE disk sample.
CWA positive control samples were also prepared in triplicate but did not have decontaminant
applied; two sets of positive controls were prepared: one without chemical treatment and one
with chemical treatment. Procedural blank samples were not contaminated with CWA but were
exposed to Chem A or Chem B and processed alongside the test samples. Laboratory blank
samples were neither contaminated nor exposed to chemicals and were also processed alongside
the test samples. Three spike controls were prepared during each test to confirm the mass of
CWA applied to the test samples.
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Table 24. CWA Modification 2 Rinse Matrix
Sample Type
Material
CWA Spike
Vol.
Chemical
Chemical
Residence
(Minutes)
Replicates
Test
Paint
2 uL
Chem A
10
3
Test
Paint
2 uL
Chem B
5
3
Test
Sealant
2 uL
Chem A
60
3
Test
Sealant
2 uL
Chem B
5
3
Positive Control
Paint
2 uL
None
10
3
Positive Control
Sealant
2 uL
None
60
3
Positive Control
Paint
2 uL
Chem B
5
3
Positive Control
Sealant
2 uL
Chem B
5
3
Procedural Blank
Paint
NA
Chem A
10
1
Procedural Blank
Paint
NA
Chem B
5
1
Procedural Blank
Sealant
NA
Chem A
60
1
Procedural Blank
Sealant
NA
Chem B
5
1
Lab Blank
Paint
NA
None
NA
1
Lab Blank
Sealant
NA
None
NA
1
Spike Control
None
2 uL
None
NA
3
For Modification 2, the effect of Chem A and Chem B chemical treatment on HD and VX
contaminated films prior to bleach application was evaluated as shown in the Table 25 test
matrix. This matrix was performed twice, once using HD with a 24-hour contact time and once
using VX with 72-hour contact time. Following the CWA contact time, 1.0 mL of Chem A was
applied with a residence time of 10 minutes on the paint film and 60 minutes on the sealant film.
Chem B was sprayed onto the coupons with a residence time of 5 minutes. Following the
chemical treatment residence time, each coupon was rinsed with 3 x 2.0 mL of water. The water
rinses were aggregated and analyzed for HD or VX as described above. Bleach was then sprayed
onto the coupons with a 60-minute dwell time prior to sample processing. Paint and sealant film
coupons were tested in triplicate. Note that each replicate resulted in one wipe sample, one film
coupon sample, and one SPE disk sample.
CWA positive control samples were also prepared in triplicate but did not have decontaminant
applied; two sets of positive controls were prepared: one without chemical treatment and one
with chemical treatment. Procedural blank samples were not contaminated with CWA but were
decontaminated and processed alongside the test samples. Laboratory blank samples were neither
contaminated nor decontaminated and were also processed alongside the test samples. Procedural
blanks and laboratory blanks should have had less than 50% of the lowest detected amount on
the test coupon. Three spike controls were prepared during each test to confirm the mass of
CWA applied to the test samples. The average recoveries from the spike controls were required
to be within 80% to 120% of the theoretical target amount with a replicate RSD of < 30% (n=3).
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Table 25. CWA Modification 2 Decontamination Efficacy Matrix
Sample Type
Material
CWA Spike
Volume
Decontaminant
Chemical
Chemical
Residence
(Minutes)
Replicates
Test
Paint
2 uL
Bleach
Chem A
10
3
Test
Paint
2 uL
Bleach
Chem B
5
3
Test
Sealant
2 uL
Bleach
Chem A
60
3
Test
Sealant
2 uL
Bleach
Chem B
5
3
Positive Control
Paint
2 uL
None
None
NA
3
Positive Control
Sealant
2 uL
None
None
NA
3
Positive Control
Paint
2 uL
None
Chem A
10
3
Positive Control
Sealant
2 uL
None
Chem A
60
3
Positive Control
Paint
2 uL
None
Chem B
5
3
Positive Control
Sealant
2 uL
None
Chem B
5
3
Procedural Blank
Paint
NA
Bleach
Chem A
10
1
Procedural Blank
Paint
NA
Bleach
Chem B
5
1
Procedural Blank
Sealant
NA
Bleach
Chem A
60
1
Procedural Blank
Sealant
NA
Bleach
Chem B
5
1
Lab Blank
Paint
NA
None
None
NA
1
Lab Blank
Sealant
NA
None
None
NA
1
Spike Control
None
2 uL
None
None
NA
3
For Modification 3, the effect of Chem A (10% BE) chemical treatment on HD- and VX-
contaminated films prior to Dahlgren Decon application was evaluated, as shown in the Table 26
test matrix. This matrix was performed twice, once using HD with a 24-hour contact time and
once using VX with 72-hour contact time. Following the CWA contact time, 1.0 mL of Chem A
was applied with a residence time of 10 minutes on the paint film coupon and 60 minutes on the
sealant film. Following the chemical treatment residence time, each coupon was rinsed with 3 x
2.0 mL of water. The water rinses were aggregated and analyzed for HD and VX as described
above. Dahlgren Decon was then sprayed onto the coupons with a 60-minute dwell time prior to
sample processing. Paint and sealant films were tested in triplicate. Note that each replicate
resulted in one wipe sample, one film coupon sample, and one SPE disk sample.
CWA positive control samples were also prepared in triplicate but did not have decontaminant
applied; two sets of positive controls were prepared: one without chemical treatment and one
with chemical treatment. Procedural blank samples were not contaminated with CWA but were
decontaminated and processed alongside the test samples. Laboratory blank samples were neither
contaminated nor decontaminated and were also processed alongside the test samples. Procedural
blanks and laboratory blanks should have had less than 50% of the lowest detected amount on
the test coupon. Three spike controls were prepared during each test to confirm the mass of
CWA applied to the test samples. The average recoveries from the spike controls were required
to be within 80% to 120% of the theoretical target amount with a replicate RSD of < 30% (n=3).
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Table 26. CWA Modification 3 Decontamination Efficacy Matrix
CWA
Spike Vol.
Chemical
Sample Type
Material
Decontaminant
Chemical
Residence
(Minutes)
Replicates
Test
Paint
2 uL
Dahlgren Decon
Chem A
10
3
Test
Sealant
2 uL
Dahlgren Decon
Chem A
60
3
Positive Control
Paint
2 uL
None
None
NA
3
Positive Control
Sealant
2 uL
None
None
NA
3
Positive Control
Paint
2 uL
None
Chem A
10
3
Positive Control
Sealant
2 uL
None
Chem A
60
3
Procedural Blank
Paint
NA
Dahlgren Decon
Chem A
10
1
Procedural Blank
Sealant
NA
Dahlgren Decon
Chem A
60
1
Lab Blank
Paint
NA
None
None
NA
1
Lab Blank
Sealant
NA
None
None
NA
1
Spike Control
None
2 uL
None
None
NA
3
D. 7 Modified Decontamination Efficacy Testing - Pesticides
Table 27 provides the matrix for decontamination efficacy testing to evaluate modifications to
decontamination technologies to improve the initially measured efficacies against two pesticides.
Use of lOx diluted bleach and D7 evaluated during baseline testing was downselected to just D7
for decontamination approach modifications. The pesticide Modification 1 and 2 test matrix was
performed twice, once with malathion and once with fipronil, with both pesticides having a 72-
hour contact time on the test coupons. The results from the modifications to the decontamination
approach as evaluated for the CWAs (see Section D.6) assisted in the determination of the
modifications to the decontamination approaches for the two pesticides.
Two modifications to the decontamination technology were evaluated. Modification 1 involved
application of D7 with a 60-minute dwell time, followed by 3 x 2.0 mL water rinses, and then a
second application of D7 with a 60-minute dwell time. The water rinses were aggregated and
analyzed for malathion or fipronil in a manner similar to water rinse analysis performed for HD
and VX. Modification 2 extended the D7 dwell time from 60 minutes to 120 minutes. However,
at the 60-minute time point, samples were visually evaluated for dryness to determine if
additional D7 should be applied. No samples required D7 reapplication during testing. Paint and
sealant films were tested in triplicate. Note that each replicate resulted in one wipe sample, one
film coupon sample, and one SPE disk sample.
Pesticide positive control samples were also prepared in triplicate but did not have
decontaminant applied. Procedural blank samples were not contaminated with pesticide but were
decontaminated and processed alongside the test samples. Laboratory blank samples were neither
contaminated nor decontaminated and were also processed alongside the test samples. Procedural
blanks and laboratory blanks should have had less than 50% of the lowest detected amount on
the test coupon. Three spike controls were prepared during each test to confirm the mass of
pesticide applied to the test samples. The average recoveries from the spike controls were
required to be within 80% to 120% of the theoretical target amount with a replicate RSD of <
30% (n=3).
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Table 27. Pesticide Modification 1 and2 Decontamination Efficacy Matrix
Sample Type
Material
Pesticide
Solution
Spike
Volume
Decontaminant
Replicates
Test
Paint
12 nL
D7
3
Test
Sealant
12 nL
D7
3
Positive Control
Paint
12 nL
None
3
Positive Control
Sealant
12 nL
None
3
Procedural Blank
Paint
NA
D7
1
Procedural Blank
Sealant
NA
D7
1
Lab Blank
Paint
NA
None
1
Lab Blank
Sealant
NA
None
1
Spike Control
None
12 nL
None
3
For all modification testing, following the CWA/pesticide contact period, decontaminants were
sprayed onto the film surfaces as described in Section C.4. Following the decontaminant dwell
time, films were wiped, and the wipes were solvent-extracted. The LVAP assemblies were then
disassembled and paint/sealant film coupons and SPE disks were solvent-extracted. Wipe, film,
and SPE disk extracts were analyzed via GC/MS for HD and malathion or LC-MS/MS for VX
and fipronil to quantify residual CWA/pesticide.
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E. RESULTS
Results for the wipe sampling, solvent extraction, and decontaminant quench demonstrations are
shown in Sections E. 1 - E.3. Fate and transport results can be found in Section E.4 while results
from the baseline decontamination tests are presented in Sections E.5 (CWAs HD and VX) and
E.6 (pesticides malathion and fipronil). Finally, Sections E.7 and E.8 display results for
modifications to the baseline decontamination approach for the two CWAs and two pesticides,
respectively. Results are provided, as applicable, for spike controls (chemical spiked into
extraction solution); for stainless steel coupons (chemical applied to stainless steel and
extracted); for paint or sealant coupon (chemical applied to surface of paint/sealant coupon; then
surface wiped followed by extraction of the paint or sealant coupon); for chemical recovered in a
water rinse; and for the SPE disk below the paint or sealant coupon. Positive control results are
associated with results for the surface wipe sampled paint/sealant to which a chemical was
applied but was not decontaminated.
E.l Wipe Sampling Demonstration Results
Wipe sampling testing was completed per Section D. 1. The results of HD and VX wipe sampling
studies are shown in Table 28; standard deviations (SDs) and RSDs are also provided. The wipe-
sampling method was deemed acceptable for use if the average wipe-sampling recoveries were
within the range of 70% to 120% of the average of the spike control results with a replicate RSD
< 30%. These criteria were met except for the VX recovery from sealant which was different by
1%. As the stainless-steel wipe recovery for VX was within acceptance limits, the wipe-sampling
method was deemed acceptable for all CWAs.
Table 28. CWA Wipe Sampling Results
Sample
Type
HD Average Mass
Recovered ± SD
(jig) (n=3)
HD
Recovery
(vs SC)"
HD
Recovery
RSD
VX Average
Mass Recovered
± SD (jig) (n=3)
VX
Recovery
(vs SC)"
VX
Recovery
RSD
Spike Control
2,600±110
NA
4.1%
1,800±56
NA
3.0%
Paint
1,900±150
76%
7.5%
1,300±240
70%
19%
Sealant
2,000±140
78%
7.2%
1,300±76
69%
6.0%
Stainless Steel
2,600±40
102%
1.6%
1,800±92
95%
5.3%
All CWA wipe quality control data were also acceptable: HD and VX spike controls were within
20% of the theoretical spike mass; recoveries for HD evaporation controls were as follows: paint
90%, sealant 102%, and stainless steel 98%; recoveries for VX evaporation controls were as
follows: paint 100%, sealant 95%, and stainless steel 100%; all HD and VX procedural blanks
and laboratory blanks were nondetects.
The results of the malathion and fipronil wipe sampling studies are shown in Table 29; SDs and
RSDs are also provided. This test was the second malathion wipe trial; the first trial had highly
variable spike control recoveries (326% RSD). The results from the first trial (and the first
malathion solvent extraction trial, see below) drove the decision to stir the malathion solution
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prior to and during spiking as described in Section C.l. Wipe acceptance criteria were met
except for the malathion recovery from paint and sealant. As the stainless-steel wipe recovery for
malathion was within acceptance limits, the wipe sampling method was deemed acceptable for
all pesticides.
Table 29. Pesticide Wipe Sampling Results
Sample
Type
Malathion
Average Mass
Recovered ± SD
(Hg) (n=3)
Malathion
Recovery
(vs SC)"
Malathion
Recovery
RSD
Fipronil
Average Mass
Recovered ± SD
(jig) (n=3)
Fipronil
Recovery
(vs SC)"
Fipronil
Recovery
RSD
Spike Control
33±4.4
NA
13%
14±1.0
NA
7.3%
Paint
9.2±1.4
28%
15%
13±1.8
91%
15%
Sealant
18±2.0
56%
11%
16±1.9
115%
12%
Stainless Steel
30±2.3
90%
7.9%
16±1.3
118%
7.9%
Malathion and fipronil spike controls for the second trial were within 20% of the theoretical
spike mass. Recoveries for malathion evaporation controls were as follows: paint 56%, sealant
75%, and stainless steel 90%. The low malathion recovery for the paint evaporation controls
might reflect poor extraction efficiency; see extraction results in section E. 1. Recoveries for
fipronil evaporation controls were as follows: paint 112%, sealant 112%, and stainless steel
118%. All malathion and fipronil procedural blanks and laboratory blanks were nondetects.
E.2 Solvent Extraction Demonstration Results
Solvent extraction testing was completed per Section D.2 for extraction of the target chemical
from paint and sealant film coupons and SPE disk. The results of HD and VX solvent extraction
studies are shown in Table 30; SDs and RSDs are also provided. The solvent extraction method
was deemed acceptable for use if the average wipe-sampling recoveries were within the range of
70% to 120% of the average of the spike control results with a replicate RSD < 30%. These
criteria were met for both HD and VX. All CWA extraction quality control data were also
acceptable: HD and VX spike controls were within 20% of the theoretical spike mass, and all
HD and VX laboratory blanks were nondetects.
Table 30. CWA Extraction Sampling Results
Sample
Type
HD Average
Mass Recovered
± SD
ftig) (n=3)
HD
Recovery
(vs SC)"
HD
Recovery
RSD
VX Average
Mass Recovered
± SD
Gig) (n=3)
VX
Recovery
(vs SC)"
VX
Recovery
RSD
Spike Control
2,500±51
NA
2.1%
1,900±80
NA
4.3%
Paint
2,400±230
97%
9.5%
1,700±160
92%
9.1%
Sealant
2,400±32
98%
1.3%
1,700±32
92%
1.9%
SPE
2,500±180
103%
7.1%
2,000±230
108%
11%
Stainless Steel
2,500±59
102%
2.4%
1,600±100
86%
6.3%
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The results of the malathion and fipronil solvent extraction studies are shown in Table 31; SDs
and RSDs are also provided. This testwas the second malathion solvent extraction trial; the first
trial had highly variable spike control recoveries (205% RSD). While the spike control RSD was
acceptable for the second malathion extraction trial (18%), the average malathion spike control
recovery was only 60% of theoretical. Fipronil spike controls were within 20% of theoretical
spike mass. All malathion and fipronil laboratory blanks were nondetects. The recovery criteria
for fipronil were met for all sample types, however, low recovery was observed for malathion
from paint and sealant, with high RSDs. The decision was made to continue with testing despite
the low recoveries and RSDs for malathion.
Table 31. Pesticide Extraction Sampling Results
Sample
Type
Malathion
Average Mass
Recovered ± SD
(Hg) (n=3)
Malathion
Recovery
(vs SC)"
Malathion
Recovery
RSD
Fipronil
Average Mass
Recovered ± SD
(jig) (n=3)
Fipronil
Recovery
(vs SC)"
Fipronil
Recovery
RSD
Spike Control
22±4.0
NA
18%
13±0.23
NA
1.8%
Paint
12±5.4
55%
44%
12±0.21
99%
1.6%
Sealant
12±5.9
53%
50%
13±0.50
101%
3.9%
SPE
19±4.6
85%
24%
14±0.33
109%
2.4%
Stainless Steel
24±6.9
108%
28%
11±2.0
91%
17%
E.3 Decontaminant Quench Demonstration Results
Decontaminant quench testing was performed for CWA per Section D.3. The quench method
was deemed acceptable for use if the average recovery of CWA in the quench samples was >
70% relative to the average positive control results. Average HD spike control recovery on Day 0
was 102% versus theoretical and on Day 3 was 88%, with all positive control recoveries greater
than 70% compared to the spike controls for both days of analysis, with one exception. The HD
SPE positive control exhibited only 39% recovery compared to the spike control on Day 0; this
recovery improved to 71% on Day 3. The SPE sample extracts required a 10-fold sample dilution
to get the internal standard within acceptance range, which indicated some type of interference
from the SPE disk in combination with quench and in the absence of decontaminant. Average
VX spike control recovery on Day 0 was 98% versus theoretical and on Day 3 was 95%, with all
positive control recoveries greater than 80% compared to the spike controls for both days of
analysis. HD and VX process and laboratory blanks were all nondetects.
Table 32 shows the results of the CWA quench study. Average HD recovery compared to the
positive controls was greater than 80% for all decontaminants with all materials for all Day 0 and
most Day 3 analysis time points, with the D7 SPE average recovery on Day 3 being 69%. The
average VX recovery compared to the positive controls was greater than 90% for all
decontaminants with for all materials at both the Day 0 and Day 3 analysis time points. Based on
these results, we determined that the quench approach was sufficient for both decontaminants in
the presence of HD and VX. Also, a 3-day hold time was acceptable if needed for analysis of
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both CWAs (in the presence of any products resulting from quenching of the decontaminants,
including excess quantities of 3 M STS).
Table 32. CWA Quench Recovery
Sample
Type
Analysis
Time Point
Material
HD
Average Mass
Recovered ± SD
(Hg) (n=3)
HD
Recovery
(vs PC)"
vx
Average Mass
Recovered ± SD
(jig) (n=3)
VX
Recovery
(vs PC)"
Positive Control
(PC)
Day 0
Wipe
45±1.1
NA
17±0.80
NA
Coupon
50±1.4
NA
17±0.19
NA
SPE
20±0.11
NA
19±0.29
NA
Bleach
Day 0
Wipe
46±1.2
102%
16±0.16
92%
Coupon
48±2.0
97%
17±0.28
101%
SPE
23±2.4
115%
19±0.59
102%
Dahlgren Decon
Day 0
Wipe
46±0.55
102%
18±0.58
104%
Coupon
49±1.2
97%
18±0.29
108%
SPE
22±3.8
113%
20±2.6
110%
D7
Day 0
Wipe
46±2.1
102%
17±1.2
96%
Coupon
51±1.4
103%
17±0.61
102%
SPE
16±5.3
81%
18±0.94
98%
Positive Control
Day 3
Wipe
34±1.2
NA
17±0.42
NA
Coupon
38±1.7
NA
16±0.40
NA
SPE
31±1.8
NA
18±0.25
NA
Bleach
Day 3
Wipe
36±1.1
106%
16±0.14
94%
Coupon
39±1.5
102%
16±0.59
99%
SPE
31±1.7
101%
19±1.1
103%
Dahlgren Decon
Day3
Wipe
35±0.72
103%
17±0.34
104%
Coupon
37±1.7
99%
18±0.49
113%
SPE
33±2.3
105%
19±0.22
103%
D7
Day3
Wipe
35±1.2
102%
17±1.3
100%
Coupon
38±2.0
101%
17±0.91
102%
SPE
21±17
69%
18±0.49
98%
Decontaminant quench testing was performed for pesticides per Section D.3. The quench method
was deemed acceptable for use if the average recovery of pesticide in the quench samples was >
70% relative to the average positive control results. Average malathion spike control recovery on
Day 0 was 87% versus theoretical, and on Day 4 was 83%, with all positive control recoveries
greater than 90% compared to the spike controls for both days of analysis. Average fipronil spike
control recovery on Day 0 was 105% versus theoretical, and on Day 4 was 103%, with all
positive control recoveries greater than 85% compared to the spike controls for both days of
analysis. Malathion and fipronil process and laboratory blanks were all nondetects.
Table 33 shows the results of the pesticide quench study. Average malathion recovery compared
to the positive controls was greater than 80% for both lOx diluted bleach and D7 with all
materials at both the Day 0 and Day 4 analysis time points. Similarly, the average fipronil
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recovery compared to the positive controls was greater than 85% for both lOx diluted bleach and
D7 with all materials at both the Day 0 and Day 4 analysis time points. Based on these results,
we determined that the quench approach was sufficient for both decontaminants in the presence
of malathion and fipronil. Also, a 4-day hold time was acceptable if needed for analysis of both
pesticides (in the presence of any products resulting from quenching of the decontaminants,
including excess quantities of 3 M STS).
Table 33. Pesticide Quench Recovery
Sample
Type
Analysis
Time Point
Material
Malathion
Average Mass
Recovered ± SD
(jig) (n=3)
Malathion
Recovery
(vs PC)"
Fipronil
Average Mass
Recovered ± SD
(jig) (n=3)
Fipronil
Recovery
(vs PC)"
Positive Control
Day 0
Wipe
36±5.7
NA
13±1.4
NA
Coupon
32±6.4
NA
13±1.5
NA
SPE
30±9.6
NA
14±0.78
NA
lOx Diluted
Bleach
Day 0
Wipe
30±3.7
85%
12±0.80
88%
Coupon
26±4.2
83%
13±1.3
97%
SPE
30±5.7
87%
15±1.8
102%
D7
Day 0
Wipe
34±11
97%
13±0.78
95%
Coupon
29±3.1
92%
14±2.6
102%
SPE
29±5.4
99%
15±0.87
102%
Positive Control
Day 4
Wipe
35±5.1
NA
13±1.3
NA
Coupon
31±5.9
NA
13±1.3
NA
SPE
32±11
NA
13±0.63
NA
lOx Diluted
Bleach
Day 4
Wipe
29±3.8
81%
12±1.0
90%
Coupon
26±4.9
83%
13±0.92
99%
SPE
33±9.2
103%
14±1.3
106%
D7
Day 4
Wipe
32±9.4
91%
13±0.94
100%
Coupon
28±2.5
92%
14±2.6
103%
SPE
30±5.7
92%
15±0.87
110%
E.4 Fate and Transport Assessment
HD and VX fate and transport testing was performed per Section D.4. Both HD and VX
primarily beaded on paint film coupons or formed a pancake shape on sealant film coupons when
spiked. Both HD and VX caused a blistering of all test films after the 24- or 72-hour agent
contact period. Representative photographs of VX interactions on films are shown in Figure 13,
and HD interactions on films are shown in Figure 14. Note that color differences in the photos
were due to limitations of photography and should not be taken to represent actual changes in
film coloration.
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Droplet Beaded after
Spiking on Paint
Droplet Blistered after
72-hour Contact on
Paint
Droplet Pancake Shape
after Spiking on Sealant
Droplet Blistered after
72-hour Contact on
Sealant
Figure 13. VX Interaction on Paint and Sealant Films
Droplet Beaded after
Spiking on Paint
Droplet Blistered after
24-hour Contact on
Paint
Droplet Pancake Shape
after Spiking on Sealant
Droplet Blistered after 24-
hour Contact on Sealant
Figure 14. HD Interaction on Paint and Sealant Film Coupons
Average HD spike control mass was 1,800 jig (72% of theoretical) with a 60% RSD; the mass of
the first spike control replicate was 20% of the mass of the other two replicates, indicating a
possibly mis-spiked sample. The low spike control sample was the first prepared sample in the
trial. It is possible that an air bubble in the syringe caused this error. No other samples in the trial
resulted in apparent low spike levels. Note that all laboratory blanks were nondetects for this
testing. The results of the fate and transport are shown in Table 34 for paint and sealant coupons.
For both the paint and sealant coupons, most of the HD permeated through the coupon to the
SPE disk, with less than 1% of all HD collected from the surface on wipes. The total HD amount
recovered is comparable to the spiked amount, which suggests that HD does not degrade
appreciable while the evaporation is significantly reduced due to the competing permeation into
the paint or sealant layer.
Average VX spike control mass was 1,800 jig (95% of theoretical) with a 1.8% RSD. While
there were very low level VX detections for some laboratory blank samples, all laboratory blanks
met the quality control criteria of less than 50% of the lowest detected amount on the test
coupon. The results of the fate and transport study are shown in Table 34 for paint and sealant
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coupons. For both the paint and seal ant coupons, most of the VX was found within the coupon.
The total VX amount recovered from the paint sample is comparable to the spiked amount while
only half of the VX was recovered from the sealant material. Considering the low volatility of
VX, it is plausible that VX degrades upon interaction with the sealant rather than being lost due
to evaporation. However, it is also possible that VX adheres more strongly to the sealant layer
over time (72 hours) leading to poorer extraction efficiencies. The conducted research cannot
decouple these two interpretations of the lower total VX recovery from the sealant sample.
Table 34. CWA Fate and Transport Results
Analyte
Sample Type
Average Mass Recovered ± SD (ug) [% of Total]
Wipe
Coupon
SPE
Total
HD
Paint
14±2.9 [0.7%]
520±320 [26%]
1,500±390 [75%]
2,000±130
Sealant
1.21 [0.06%]
380±91 [20%]
1,500+370 [79%]
1,900+270
VX
Paint
440+201 [26%]
1,000+247 [59%]
290+177 [17%]
L700±68
Sealant
69+5.2 [7.5%]
650±87 [71%]
200+234 [22%]
920+155
1 One replicate detection (1.3 fig) averaged with two nondetect replicates set equal to quantitation limit (1.1 |ig)
Based on the observed results, the decision was made to conduct all decontamination testing with
a 24-hour HD contact time and 72-hour VX contact time as performed previously.
Malathion and fipronil fate and transport testing was performed per Section D.4. Both malathion
and fipronil beaded or formed a pancake shape on the paint and sealant film coupons when
spiked. The malathion solution was dry with a visible spot or blister where the droplet was
applied on test film coupons after the 24- or 72-hour contact period. The fipronil solution was
dry with a visible spot where the droplet was applied on all test films after the 24- or 72-hour
contact period. Representative photographs of the malathion solution interaction on film coupons
are shown in Figure 15, and fipronil solution interactions on film coupons are shown in Figure
16.
Droplet Beaded after
Spiking on Paint
Droplet Beaded after
Spiking on Sealant
Dry Visible Spot after
72-hour Contact on
Sealant
Droplet Blistered after
72-hour Contact on
Paint
Figure 15. Malathion Interactions on Paint and Sealant Film Coupons
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Droplet Pancake Shape
after Spiking on Paint
Dry Visible Spot after
72-hour Contact on
Paint
Droplet Beaded after
Spiking on Sealant
Dry, Visible Spot after
72-hour Contact on
Sealant
Figure 16. Fipronil Interactions on Paint and Sealant Films
Average malathion spike control mass was 31 jug (85% of theoretical) with a 13% RSD. All
laboratory blanks were nondetects. The results of the fate and transport comparison of a 24-hour
malathion contact time to a 72-hour contact time are shown in Table 35 for paint and sealant. A
/-test was performed to compare the 24-hour and 72-hour contact times; the /-test was two-tailed
for heteroscedastic (i.e., different variances) data. Similar behavior was observed for malathion
on the paint films However, significantly less malathion was recovered from the sealant wipe
after 72 hours. A 72-hour contact time was selected for malathion, representing a potentially
conservative scenario in the field while still providing sufficient target chemical for surface
analysis.
Table 35. Malathion Fate and Transport Results
Sample
Material
Average Mass Recovered ± SD (fig)
[% of Total]
/-Test
Significant
Type
24-Hour
72-Hour
P Value
Difference
Wipe
2.3±0.35 [12%]
1.6±0.33 [8%]
0.081
No
Paint
Coupon
I8±4.5 [90%]
18±6.6 [90%]
0.99
No
SPE
<1.0 |<5%]
<1.0 [<5%]
NA
Total
20±4.8
20+7.0
0.91
No
Wipe
mmm [58%]
2.8+0.45 [23%]
0.0015
Yes
Sealant
Coupon
7.5±2.3 [44%]
8.8+1.8 [73%]
0.46
No
SPE
<1.0 [<6%]
<1.0 [<8%]
NA
Total
17±1.8
12+2.2
0.028
Yes
Figure 17 shows the total recovered malathion for the paint and sealant 24-hour and 72-hour
contact times with error bars of one standard deviati on.
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Malathion Fate and Transport
an
T3
0)
j_
> 25 f—
O
u
QJ
j
¦¦
S_15
QJ bD
I
M 0
< Pa
1
nt See
¦ 24 Hour
¦ 72 Hour
ilant
Figure 17. Total Recovered Malathion for Fate and Transport Testing
Average fipronil spike control mass was 13 |ig (92% of theoretical) with a 1.4% RSD. All
laboratory blanks were nondetects. The results of the fate and transport comparison of a 24-hour
fipronil contact time to a 72-hour contact time are shown in Table 27 for paint and sealant
coupons. A Student's Mest was performed to compare the 24-hour and 72-hour contact times;
the Mest was two-tailed for heteroscedastic data. Similar behavior was observed for fipronil on
the sealant film coupons. However, significantly less fipronil was recovered from the paint
coupon wipe after 72 hours. A 72-hour contact time was selected for fipronil representing a
potentially conservative scenario in the field while still providing sufficient target chemical for
surface analysis.
Table 36. Fipronil Fate and Transport Results
Sample
Material
Average Mass Recovered ± SD
(jig) (n=3)
?-Test
Significant
Type
24-Hour
72-Hour
P Value
Difference
Paint
Wipe
10±0.43
7.2±0.51
0.0019
Yes
Coupon
3.0±0.77
4.7±0.0076
0.057
No
SPE
<0.001
<0.001
NA
Total
13±0.84
12±0.55
0.12
No
Sealant
Wipe
9.7±2.2
9.4±0.46
0.85
No
Coupon
1.7±0.64
2.3±0.25
0.25
No
SPE
0.00191
<0.001
NA
Total
11±1.6
12±0.28
0.77
No
1 One replicate detection (0.005 |ig) averaged with two nondetect replicates equal to quantitation limit (0.001 |ig)
Figure 18 shows the total recovered fipronil for the paint and sealant coupon 24-hour and 72-
hour contact times with error bars of one standard deviation.
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Fi
18
T3
QJ
S 16
pronil Fate arid Transj
3ort
>
I 14 ^
S U
1 10
-S g s
n
go 0
< Pa
¦
lint Sea
¦ 24 Hour
¦ 72 Hour
lant
Figure 18. Total Recovered Fipronil for Fate and Transport Testing
E.5 Baseline Decontamination - CWAs
During CWA testing, decontaminants were sprayed onto the surfaces of paint and sealant film
coupons to coat the entire exposed surface with decontaminant. The bleach wetted the surface of
the paint film coupons and beaded on the surface of the sealant film coupons. The Dahlgren
Decon and D7 decontaminants both foamed when applied to the surface of the film coupons.
During baseline and Mod 1 testing, decontaminants appeared mostly dry and crusty after the 60-
minute dwell period. During Mod 2 and Mod 3 testing, decontaminants appeared wet. The
difference in observed decontaminant wetness over time may have been related to slightly higher
laboratory RH during Mod 2 and 3 testing (refer to Appendix B ). Representative photographs of
the decontamination observations on the films are shown in Figure 19 and Figure 20.
Figure 19. Decontaminant Observations when Applied to Film Coupons
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Dry, Crusty Decontaminant
(Dahlgren on Paint)
Wet Decontaminant
(Bleach on Sealant)
Figure 20. Decontaminant Observations after 60-Minute Dwell Time
During pesticide testing, the lOx diluted bleach wetted the surface of the paint film coupons and
beaded on the surface of the sealant film coupons. The D7 decontaminant foamed when applied
to the surface of the film coupons. These observations were consistent with the decontamination
application observations from chemical agent testing, and representative photos are shown in
Figure 19. The lOx diluted bleach looked wet after the 60-minute dwell period, and the D7
decontaminant looked wet and foamy after the 60-minute or 120-minute dwell periods.
Representative photographs of the decontaminant observations after the dwell time are shown in
Figure 21.
Wet Foamy D7 on Sealant
Wet lOx Bleach on Sealant
Figure 21. Sealant Film Coupon Decontaminant Observations after Dwell Time
After the 60-minute dwell period for lOx diluted bleach, paint films looked wrinkled, and sealant
films looked unchanged. After the 60-minute or 120-minute dwell periods for D7, paint films
looked wrinkled, and sealant films looked unchanged. For the trials using fipronil, a yellow spot
was present where the pesticide was applied after the lOx diluted bleach and D7 dwell periods.
Representative photographs of the paint film observations after decontamination are shown in
Figure 22.
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Wrinkled Paint Coupon after 60-
min lOx Diluted Bleach Dwell
Period
Fipronil Yellow Spot on Paint
Coupon after 60-min D7 Dwell
Period
Figure 22. Paint Film Decontaminant Observations after Dwell Time
The CWA baseline testing included two trials, one for HD and one for VX. Each trial included
two test materials (paint and sealant film coupons) and three decontaminants (bleach, Dahlgren
Decon, and D7) with a 60-minute decontaminant dwell time. All CWA spike control results
(shown in Table 37) met the acceptance criteria described in Section D.5.
Table 3 7. Baseline Decontaminant Efficacy Testing - CWA Average Spike Control Results
CWA
Average Mass
Recovered
Gig)
Percent Recovery
(vs Theoretical)*
RSD
HD
2,400
93%
2.8%
VX
2.100
113%
5.5%
* See Table 1 for purity and mass contamination targets of 2,540 |ig for HD
and 2,016 ji " for VX based on density
All HD and VX laboratory blank results and a majority of the procedural blank results met the
acceptance criteria described in Section D.5. One procedural blank had a low-level result for HD
(slightly above the detection limit); no impact to the data was expected. Chromatographic peak
splitting was observed for all HD SPE laboratory and procedural blanks. Hence, samples were
diluted 2:1 to mitigate the matrix effect for these blanks. Internal standard responses for all HD
and VX results met the acceptance criteria described in Section C.7 and C.8.
The average HD mass recoveries for each sample component for the positive controls and
decontaminants, as well as total mass (combined recoveries of the wipe, coupon, and SPE) are
provided in Table 38 for paint film coupons and Table 39 for sealant film coupons.
Decontaminant efficacy for just the wipe samples collected from the coupon surface (surface
decontamination efficacy) was calculated using Equation 5. Total decontamination efficacy
against all test components (wipe, extracted coupon, and SPE) was calculated by comparing the
summed total of the average mass recovered for all components for each decontaminant test to
the summed total of the average massed recovered for all components for the Positive Controls
using Equation 4. The surface decontamination efficacy and total decontamination efficacy error,
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calculated using Equation 7, is also provided as a ± percentage. Note that results for all measured
target analyte masses are considered accurate to two significant figures. Reported values,
including total average mass recovered and decontaminant efficacy, are calculated prior to
rounding. Small differences in presented data are due to rounding.
If replicate results for the positive controls and/or decontaminants were below the detection limit,
the standard deviation, and associated percent efficacy and/or error were not calculated. In these
cases, a standard deviation is not provided. For bleach and Dahlgren paint testing, all replicate
wipe results were below the quantitation limit. For calculation purposes, the quantitation limit
(1.1 |ig) was used, and wipe efficacy results were expressed with > symbol. For Dahlgren and
D7 paint testing the average mass recovered for the decontaminant samples was greater than the
average total mass recovered for positive controls; therefore, the total efficacy is reported as 0%.
Table 38. Average HD Mass Recoveredfor Paint Film Coupons - Baseline
Sample Type
Average Mass Recovered ± SD (jig)
Decontamination Efficacy
Wipe
Coupon
SPE
Total
Surface
Total
Positive Control
6.1±2.8
320±130
880±120
1,200±250
NA
NA
Bleach
<1.1
110±44
1,000±200
1,100±230
>82%
6.1±27%
Dahlgren
<1.1
310±110
1,000±110
1,300±20
>82%
0%
D7
2.2±0.68
240±80
1,000±69
1,300±72
64±20%
0%
NA = Not Applicable
Table 39. Average HD Mass Recovered for Sealant Film Coupons - Baseline
Sample Type
Average Mass Recovered ± SD (jug)
Decontamination Efficacy
Wipe
Coupon
SPE
Total
Surface
Total
Positive Control
<1.1
190±74
1,100±57
1,300±38
NA
NA
Bleach
<1.1
190±17
1,100±106
1,300±92
NA
0%
Dahlgren
<1.1
210±19
LlOOillO
1,300±110
NA
0%
D7
3.0±0.55
270±62
1,000±12
1,300±65
0%
0%
NA = Not Applicable
For bleach, Dahlgren, and D7 sealant testing, the average total mass recovered for the
decontaminant samples was greater than the average total mass recovered for positive controls.
Therefore, the total decontamination efficacy is reported as 0%. Similarly, the average total mass
recovered for the D7 wipe samples was greater than the average wipe mass recovered for
positive controls; therefore, the surface decontamination efficacy is reported as 0%.
Some observations from the results in Table 38 and Table 39 include that minimal HD remained
on the surface of film coupons following the contact period and that most of the HD (> 70%)
penetrated through all film coupons to the SPE disk. There was minimal difference between
positive controls and decontaminant samples for either coupon type. Total HD decontamination
efficacy was less than 7% for both film types, although surface decontamination efficacy
indicated that at least 60% of surface HD was decontaminated for decontaminant types. See
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Appendix D for statistical interpretation of the HD baseline results and discussion of whether
decontaminants had a significant effect on HD levels. See also Section E.7 for a summary of
statistical observations.
Figure 23 summarizes the paint and sealant HD average total mass recoveries including error
bars equal to one standard deviation.
HD Baseline Decontamination Test
(Error bars equal ± one standard deviation)
1,800
tT 1,600
01
aj 1,400 T t T j
i
!i ^
M 0
< Paint Sealant
Figure 23. HD Baseline Decontaminant Test, Average Total Mass Recoveries
The average VX mass recoveries for each sample component for the positive controls and
decontaminants, as well as total mass (combined recoveries of the wipe, coupon, and SPE) are
provided in Table 40 for paint film coupons and Table 41 for sealant film coupons. The average
total mass recovered for the bleach paint wipe samples was greater than the average wipe mass
recovered for positive controls; therefore, the surface decontamination efficacy was reported as
0%. For the paint samples, no decontaminants appeared to reduce the level of VX compared to
the positive control; approximately the same mass of VX remained on the surface of all coupons,
and approximately equal masses of VX remained within all coupons and penetrated to the SPE
disk. Total VX decontamination on paint range from only 4% to 16%, with surface
decontamination ranging from 0% to 50%.
Table 40. Average VX Mass Recovered for Paint Films - Baseline
Sample Type
Average Mass Recovered ± SD (jig)
Decontamination Efficacy
Wipe
Coupon
SPE
Total
Surface
Total
Positive Control
92±30
290±24
230±93
620±94
NA
NA
Bleach
140±45
230±86
150±27
520±14
0%
16±13%
Dahlgren
46±11
230±32
320±29
590±69
50±20%
4.3±18%
D7
70±11
190±23
330±80
580±46
24±27%
6.0±16%
The average total mass recovered for the D7 sealant wipe samples was greater than the average
wipe mass recovered for positive controls; therefore, the surface decontamination efficacy was
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reported as 0%. For the sealant samples, bleach and Dahlgren Decon both appeared to reduce the
mass of VX on the surface relative to the positive controls and the majority of VX (> 90%) was
within the coupon. Total VX decontamination efficacy was better on sealant than paint, with
50% efficacy measured for bleach. Surface decontamination ranged from a low of 0% for D7 up
to 96% and 97% for bleach and Dahlgren Decon, respectively.
Table 41. Average VX Mass Recovered for Sealant Films - Baseline
Sample Type
Average Mass Recovered ± SD (jig)
Decontamination Efficacy
Wipe
Coupon
SPE
Total
Surface
Total
Positive Control
31±4.0
820±49
8.7±14
860±65
NA
NA
Bleach
1.1±2.0
420±101
9.9±17
430±107
96±6.4%
50±13%
Dahlgren
0.97±0.76
730±72
23±27
750±52
97±2.5%
12±8.9%
D7
42±2.0
570±39
15±14
630±50
0%
27±8.0%
See Appendix D for statistical interpretation of the VX baseline results and discussion of whether
decontaminants had a significant effect on VX levels. See also Section E.7 for a summary of
statistical observations.
Figure 24 summarizes the paint and sealant VX average total mass recoveries including error
bars equal to one standard deviation.
VX Baseline Decontamination Test
(Error bars equal ± one standard deviation)
m 1,200
"S 1,000
8 800 M t ¦ Positive Control
600 J J ¦ ¦ ¦ Bleach
j I || | || | "
bb
< Paint Sealant
Figure 24. VX Baseline Decontaminant Test, Average Total Mass Recoveries
E. 6 Baseline Decontamination - Pesticides
The baseline testing for pesticides included two trials, one for malathion and one for fipronil.
Each trial included two test materials (paint and sealant film coupons) and two decontaminants
(lOx diluted bleach and D7) with a 60-minute decontaminant dwell time.
Pesticide spike control results are shown in Table 42. The malathion spike controls did not meet
the acceptance criteria and had an average of 51% recovery and 38% RSD. No reason for the low
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recovery and high RSD could be ascertained other than possibly nonrepresentative samples being
collected from the stirred malathion solution. All the fipronil spike controls met the acceptance
criteria described in Section D.5.
Table 42. Pesticide Average Spike Control Results - Baseline
Pesticide
Average Mass
Recovered
(Mg)
Percent Recovery
(vs Theoretical)
RSD
Malathion
19
51%
38%
Fipronil
13
89%
1.1%
One laboratory blank wipe had a low-level result for fipronil (slightly above the detection limit),
no impact to the data was expected. All other laboratory blank results and procedural blank
results met the acceptance criteria for both malathion and fipronil described in Section D.5.
Internal standard response for all malathion and fipronil baseline testing results met the
acceptance criteria described in Section C.7 and C.8. Most of the wipe and coupon procedural
blanks required a 100-fold dilution (rather than the typical 10-fold) to ensure IS response was
acceptable.
The average malathion mass recoveries for each sample component for the positive controls and
decontaminants, as well as total mass (combined recoveries of the wipe, coupon, and SPE) are
provided in Table 43 for paint film coupons and Table 44 for sealant film coupons. Note that the
D7 paint wipe samples needed to be diluted 10-fold to get the internal standard within the
acceptance range. Because all three wipe samples were nondetects at this dilution level, the wipe
results are reported as < 11 |ig due to the elevated quantitation limit. The average total mass
recovered for the lOx diluted bleach and D7 paint wipe samples was greater than the average
wipe mass recovered for positive controls; therefore, the surface decontamination efficacy was
reported as 0%. For the paint samples, lOx diluted bleach and D7 coupons were not different
from the positive controls. Total malathion decontamination efficacy was less than 7% for paints.
Table 43. Average Malathion Mass Recovered for Paint Film Coupons - Baseline
Sample Type
Average Mass Recovered ± SD
(US)
Decontamination Efficacy
Wipe
Coupon
SPE
Total
Surface
Total
Positive Control
<1.1
12±4.6
<1.0
12±4.6
NA
NA
lOx Diluted
Bleach
l.l1
10±1.0
<1.0
12±1.7
0%
6.8±37%
D7
<11
12±3.7
<1.0
12±3.7
0%
5.5±46%
'SD could not be calculated; only one replicate mass above the quantitation limit
Note that the D7 sealant wipe samples needed to be diluted 5-fold to get the internal standard
within the acceptance range. Because all three wipe samples were nondetects at this dilution
level, the wipe results are reported as < 5.5 |ig due to the elevated quantitation limit. For 1 Ox
diluted bleach sealant testing, all replicate wipe, coupon, and SPE results were below the
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quantitation limit. For calculation purposes, the quantitation limit (1.1 |ig) was used, and surface
decontamination efficacy results and 3.1 |ig were used for the Total Decontamination Efficacy
results. Both lOx diluted bleach efficacy results were expressed with > symbol. The average
mass recovered for the D7 sealant wipe samples and D7 sealant total was greater than the
average wipe mass recovered for the corresponding positive controls; therefore, the surface
decontamination efficacy and Total Decontamination Efficacy was reported as 0%. Total
malathion decontamination efficacy may be above 28% for sealant using lOx diluted bleach.
Table 44. Average Malathion Mass Recovered for Sealant Films - Baseline
Sample Type
Average Mass Recovered ± SD
(US)
Decontamination Efficacy
Wipe
Coupon
SPE
Total
Surface
Total
Positive Control
3.2±1.6
l.l1
<1.0
4.3±0.93
NA
NA
lOx Diluted
Bleach
<1.1
<1.0
<1.0
<3.1
>66 %
>28 %
D7
<5.5
5.0±0.32
<1.0
5.0±0.32
0%
0%
1SD could not be calculated; only one replicate mass above the quantitation limit
See Appendix E for statistical interpretation of the malathion baseline results and discussion of
whether decontaminants had a significant effect on malathion levels. See also Section E.8 for a
summary of statistical observations.
In addition to malathion analysis, samples were analyzed for malaoxon, a malathion degradation
product. Several wipe and coupon samples using lOx diluted bleach had malaoxon present;
results are shown in Table 45. No other malathion samples contained measurable malaoxon
above the quantitation limit.
Table 45. Malaoxon Mass Recovered - Baseline
Sample Type
Film
HI
Wipe
Coupon
lOx Diluted
Bleach
Paint Rep 1
1.1
1.2
Paint Rep 2
Not Detected
1.2
Paint Rep 3
1.2
1.2
Sealant Rep 2
1.2
1.0
Figure 25 summarizes the paint and sealant malathion average total malathion mass recoveries
including error bars equal to one standard deviation. Note that for lOx diluted bleach on sealant,
the quantitation limit was 3.1 ng.
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Bfl 18
3
"o 16
aj
% 14
o
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Figure 26 summarizes the paint and sealant fipronil average total mass recoveries including error
bars equal to one standard deviation.
Fipronil Baseline Decontamination Test
(Error bars equal ± one standard deviation)
1 &
"P 1C
QJ -LO
i-
OJ
> 1A
5 14
u
OJ n
UL
IA
fK 1 (1
m
¦ Positive Control
A3 -LU
S
/i i Q
110x Diluted Bleach
QJ o
¦D
S fi
¦ D7
¦M b
in
<
Paint
Sealant
Figure 26. Fipronil Baseline Decontaminant Test, Average Total Mass Recoveries
E. 7 CWA Modification Decontamination Testing
CWA modification testing included a total of ten trials, five each for HD and VX. Each trial
included two test materials (paint and sealant film coupons) and each of the five decontaminant
modification tests described below:
• Modification 1 - two decontaminants tested (bleach and D7 for HD, bleach and Dahlgren
for VX). Each decontaminant was applied twice with a 60-minute dwell time following
each application.
• Modification 2 (Evaluation) - Evaluation of Chemical A (10% butoxyethanol) and
Chemical B (Zep Foaming Wall Cleaner) application followed by triple water rinse. No
decontaminants added during these trials.
• Modification 2 (Chem A) - Chemical A application and triple water rinse followed by a
single application of bleach with a 60-minute dwell time.
• Modification 2 (Chem B) - Chemical B application and triple water rinse followed by a
single application of bleach with a 60-minute dwell time.
• Modification 3 (Chem A) - Chemical A application and triple water rinse followed by a
single application of Dahlgren Decon with a 60-minute dwell time.
During Mod 2 and Mod 3 testing, Chem A and Chem B were applied to the films before
decontamination. The paint film coupons looked wrinkled after Chem A and Chem B
application. The agent blister on sealant film coupons looked more pronounced after Chem A
application; no change was observed on the sealant films after Chem B application.
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Representative photographs of the Chem A and Chem B interactions with the films are
shown in Figure 27.
Figure 27. Chem A and B Observations
All HD and VX spike control results (shown in Table 48) met the acceptance criteria
described in Section D.6. All HD and VX laboratory blank results, and most of the
procedural blank results met the acceptance criteria described in Section D.6. Several
procedural blanks in the Modification 2 Chem A and Chem B tests had low-level results for
VX; no impact to the data was expected. Internal standard response for all CWA
modification testing results met the acceptance criteria described in Sections C.7 and C.8.
Peak splitting was observed for Modification 1 HD SPE laboratory and procedural blanks;
samples were diluted 2:1 to mitigate the matrix effect. For Dahlgren Decon procedural blanks
(Modification 1 and Modification 3 tests), samples required a 100-fold or 1000-fold dilution
as opposed to typical 10-fold dilution to get internal standard response within acceptance
criteria.
Table 48. Average CWA Spike Control Results - Modification Testing
RSD
CWA
Test
Average Mass
Recovered
(Hg)
Percent Recovery
(vs Theoretical)
HD
Mod 1
2,200
87%
5.3%
Mod 2 - Evaluation
2,700
106%
6.4%
Mod 2 - Chem A
2,600
103%
2.4%
Mod 2 - Chem B
2,700
105%
1.1%
Mod 3 - Chem A
2,800
113%
2.2%
VX
Mod 1
1,900
99%
2.1%
Mod 2 - Evaluation
1,900
101%
7.0%
Mod 2 - Chem A
1,900
103%
9.0%
Mod 2 - Chem B
1,800
95%
4.1%
Mod 3 - Chem A
1,800
96%
4.0%
The average HD mass recoveries for each sample component for the positive controls and
decontaminants, as well as total mass (combined recoveries of the rinse, wipe, coupon, and SPE)
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are provided in Table 49 for paint film coupons and Table 50 for sealant film coupons. The
efficacy calculations for Modification 2 and Modification 3 are calculated against the Positive
Control without addition of Chem A or B (not the Positive with Chem A or Positive with Chem
B). For all modification paint tests, all replicate wipe results were below the quantitation limit.
For calculation purposes, the quantitation limit (1.1 |ig) was used, and surface decontamination
efficacy results were expressed with the > symbol. All test modifications resulted in improved
total HD decontamination efficacy for paint film coupons compared to baseline testing, although
efficacies still ranged from only 24 to 35%. As all wipe samples were below the quantitation
limit, the surface decontamination efficacy for all tests was generally high (> 85%).
Table 49. Average HD Mass Recoveredfor Paint Films — Modification Testing
Test
Sample Type
Average Mass Recovered ± SD (jig)
Rinse
Wipe
Coupon
SPE
Total
Surface
Total
Positive Control
NA
10±1.7
470±49
1,100±170
1,600±130
NA
NA
Mod 1
Bleach
NA
<1.1
47±16
1,200±14
1,200±30
>89 %
24±6.3%
D7
NA
<1.1
82±42
1,100±140
1,200±120
>89 %
25±9.2%
Positive Control
4.7±0.56
NA
170±36
1,400±110
1,600±120
NA
NA
Mod 2
Eval
Chem A
(no decontaminant)
12±2.3
NA
210±44
1,400±12
1,700±58
NA
NA
Chem B
(no decontaminant)
llil.l
NA
220±105
1,400±150
1,600±110
NA
NA
Mod 2
Chem A
Positive Control
NA
11±0.083
620±106
1,100±76
1,700±67
NA
NA
Positive with Chem A
16±3.5
4.5±2.1
310±120
1,200±190
1,500±72
NA
NA
Bleach with Chem A
14±7.0
<1.1
74±42
1,000±70
1,100±83
>90 %
35±5.6%
Mod 2
Chem B
Positive Control
NA
12±3.8
490±80
1,100±44
1,600±40
NA
NA
Positive w / Chem B
15±2.9
5.2±1.3
380±95
1,100±120
1,500±66
NA
NA
Bleach w/ Chem B
16±1.7
<1.1
88±31
1,000±55
1,100±86
>91 %
32±5.5%
Mod 3
Chem A
Positive Control
NA
8.6±3.8
420±100
1,100±83
1,500±18
NA
NA
Positive w/ Chem A
16±4.0
5.8±1.3
370±96
1,100±160
1,500±200
NA
NA
Dahlgren w/ Chem A
13±1.9
<1.1
130±70
1,100±94
1,200±57
>87 %
21±3.8%
NA = not applicable
For Modification 1 sealant testing, the average mass recovered for the D7 wipe samples was
greater than the average wipe mass recovered for positive controls; therefore, the surface
decontamination efficacy was reported as 0%. Also, the average total mass recovered for the
bleach and D7 samples was greater than the average mass recovered for the positive controls,
with the Total decontamination efficacy reported as 0%. Modifications 2 and 3 resulted in slight
improvements for total HD decontamination efficacy compared to baseline, ranging from 6 to
14% efficacy.
See Appendix D for detailed statistical interpretation of the HD Modification 1, 2, and 3 results
and discussion of whether decontaminants had a significant effect on HD levels. The statistical
HD evaluations for baseline and modification testing resulted in the following:
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Bleach Modification 1 paint coupon wipe samples resulted in lower HD values (lower
HD recovery) compared to Modification 2 with Chem A and Modification 2 with Chem
B. Note that bleach Modification 1 was not different from Baseline for HD paint coupon
wipes.
Bleach Modification 1 sealant coupon wipe samples resulted in lower HD values
compared to Modification 2 with Chem A and Modification 2 with Chem B. Note that
bleach Mod 1 was not different from Baseline for HD sealant coupon wipes.
Mod 1 with D7 typically did not result in improved HD decontamination compared to
Baseline for any material/sample type.
Most Modification 1 comparisons of bleach to D7 did not have significantly different HD
recoveries across all material and sample types.
Most Modification 2 comparisons were not significantly different. Where differences did
exist, there was no clear pattern as to whether Chem A or Chem B provided improved
decontamination results
Most Chemical A comparisons were not significantly different. Where differences did
exist, there was no clear pattern as to whether bleach or Dahlgren Decon provided
improved decontamination
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Table 50. Average HD Mass Recoveredfor Sealant Films — Modification Testing
Test
Sample Type
Average Mass Recovered ± SD
(WO
¦MOfi
Rinse
Wipe
Coupon
SPE
Total
Surface
Total
Mod 1
Positive Control
NA
<1.1
250±43
1,100±49
1,400±91
NA
NA
Bleach
NA
<1.1
130±16
1,300±170
1,400±170
ND
0%
D7
NA
3.8±0.4
2
180±29
1,200±120
1,400±96
0%
0%
Mod 2
Eval
Positive Control
<3.0
NA
220±15
1,300±100
1,500±110
NA
NA
Chem A
(no decontaminant)
8.7±1.1
NA
160±36
1,400±64
1,500±43
NA
NA
Chem B
(no decontaminant)
9.9±1.5
NA
270±36
1,200±270
1,500±240
NA
NA
Mod 2
Chem
A
Positive Control
NA
<1.1
210±27
1,100±57
1,300±81
NA
NA
Positive with/ Chem A
9.4±0.97
<1.1
210±39
1,100±47
1,400±9.7
NA
NA
Bleach with Chem A
8.0±0.23
<1.1
68±42
1,100±83
1,200±113
ND
6.7±11%
Mod 2
Chem
B
Positive Control
NA
<1.1
250±52
1,200±10
1,400±58
NA
NA
Positive with Chem B
13±1.4
<1.1
200±38
1,000±45
1,300±42
NA
NA
Bleach with Chem B
11±0.39
<1.1
130±12
1,100±59
1,200±51
ND
14±5.0%
Mod 3
Chem
A
Positive Control
NA
<1.1
276±37
1,100±43
1,400±11
NA
NA
Positive with Chem A
8.2±1.9
<1.1
200±49
1,100±91
1,300±42
NA
NA
Dahlgren with Chem A
9.4±0.78
<1.1
160±28
1,100±120
1,300±110
ND
6.3±7.5%
NA = not applicable ND = not determined
Figure 28 through Figure 32 summarize the Modification 1, 2, and 3 paint and sealant coupon
HD average total mass recoveries including error bars equal to one standard deviation for each of
the modification tests.
1,800
3
-a 1,600
QJ
5 1,400
>
8 1,200
a;
* 1,000
in '
J 800
< 600
u 400
¦2 200
O
I—
0
HD Mod 1 Decontamination Test
(Error bars equal ± one standard deviation)
Positive Control
I Bleach
I D7
M
>
<
Paint
Sealant
Figure 28. HD Mod 1 Decontaminant Test, Average Total Mass Recoveries
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HD Mod 2 Chem A and Chem B Evaluation
(Error bars equal ± one standard deviation)
bd
¦a
aj
k_
OJ
>
o
u
OJ
ec
M
>
<
1,800
1,600
1,400
1,200
1,000
800
600
400
200
0
Paint
Sealant
Positive Control
Chem A
I Chem B
Figure 29. HD Mod 2 Chem A and Chem B Evaluation, Average Total Mass Recoveries
M 1,800
^ 1,600
01
aj 1,400
>
8 1,200
aj
^ 1,000
^ 800
< 600
U 400
ra
3 200
>
<
HD Mod 2 Chem A Decontamination Test
(Error bars equal ± one standard deviation)
Positive Control
Pos. Ctrl w/ ChemA
I Bleach w/ ChemA
Paint
Sealant
Figure 30. HD Mod 2 Chem A Decontaminant Test, Average Total Mass Recoveries
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HD Mod 2 Chem B Decontamination Test
(Error bars equal ± one standard deviation)
If 1,800
f 1,600 ^
1,400
¦ T I 1 ^
¦ ¦ ¦ ¦
^ I Chem
^ ¦ I a Bleach w/ Chem
1 ™ III III
60 U
< Paint Sealant
Figure 31. HD Mod 2 Chem B Decontaminant Test, Average Total Mass Recoveries
M
2.
"O
01
1,800
1,600
g 1,400
§ 1,200
w 1,000
l/i
ro
^ 800
^ 600
400
200
0
U
"ro
+J
o
W)
>
<
HD Mod 3 Chem A Decontamination Test
(Error bars equal ± one standard deviation)
I Positive Control
Pos. Ctrl w/ ChemA
Dahlgren w/ ChemA
Paint
Sealant
Figure 32. HD Mod 3 Chem A Decontaminant Test, Average Total Mass Recoveries
The average VX mass recoveries for each sample component for the positive controls and
decontaminants, as well as total mass (combined recoveries of the rinse, wipe, coupon, and SPE)
are provided in Table 51 for paint film coupons and Table 52 for sealant film coupons. The
efficacy calculations for Modification 2 and Modification 3 are calculated against the true
Positive Control (not the Positive with Chem A or Positive with Chem B). For Modification 3,
all paint replicate wipe results were below the quantitation limit. For calculation purposes, the
quantitation limit (0.1 |ig) was used, and surface decontamination efficacy results were
expressed with the > symbol. Also, for paint Modification 3, the average total mass recovered for
the Dahlgren Decon samples was greater than the average mass recovered for the positive
controls, with the total decontamination efficacy reported as 0%. Doubling bleach dwell time on
paint for Modification 1 resulted in approximately doubled VX total decontamination efficacy
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compared to baseline testing (39% vs 16%). Modification 2 also provided improved total
efficacy compared to the baseline for Dahlgren Decon.
Table 51. Average VX Mass Recoveredfor Paint Films — Modification Testing
Test
Sample Type
Average Mass Recovered ± SD
(WS)
Decontamination
Efficacy
Rinse
Wipe
Coupon
SPE
Total
Surface
Total
Mod 1
Positive Control
NA
88±14
260±40
280±38
620±15
NA
NA
Bleach
NA
15±6.9
160±36
210±62
380±40
83±8.2%
39±6.6%
Dahlgren
NA
18±8.6
200±39
270±53
490±22
79±10%
21±4.1%
Mod 2
Eval
Positive Control
260±49
NA
220±20
510±87
990±67
NA
NA
Chem A
(no decontaminant)
280±74
NA
240±56
430±50
960±37
NA
NA
Chem B
(no decontaminant)
390±60
NA
220±24
320±136
930±80
NA
NA
Mod 2
Chem A
Positive Control
NA
180±83
370±95
390±180
940±86
NA
NA
Positive with Chem
A
330±39
29±16
270±38
350±58
980±7.5
NA
NA
Bleach with Chem A
350±29
0.52±0.59
120±97
250±10
730±120
99.7±0.35%
23±15%
Mod 2
Chem B
Positive Control
NA
110±18
200±18
230±29
540±6.5
NA
NA
Positive with Chem B
140±9.9
7.5±0.72
150±42
170±98
460±47
NA
NA
Bleach with Chem B
180±31
0.082±0.073
84±8.0
209±31
470±40
99.9±0.068
%
13±7.6%
Mod 3
Chem A
Positive Control
NA
100±5.3
150±18
220±26
460±23
NA
NA
Positive with Chem
A
260±35
5.8±1.6
110±10
200±64
580±33
NA
NA
Dahlgren with Chem
A
250±3.5
<0.10
80±43
230±38
560±8.3
>99.9
0%
NA = not applicable
For sealant Modification 3, the average total mass recovered for the Dahlgren Decon samples
was greater than the average mass recovered for the positive controls, with the total
decontamination efficacy reported as 0%. Modification 1 resulted in similar total VX
decontamination efficacy for bleach but approximately doubled efficacy for Dahlgren Decon
compared to baseline (26% vs 12%). Modification 2 did not provide apparent improvement in
efficacy for Dahlgren Decon compared to the baseline. See Appendix D for detailed statistical
interpretation of the VX Modification 1, 2, and 3 results and discussion of whether
decontaminants had a significant effect on VX levels. Statistical VX evaluations of baseline and
modification testing resulted in the following:
• Bleach Modification 1 paint coupon wipe resulted in lower VX values than Baseline,
Modification 2 with Chem A, and Modification 2 with Chem B.
• Bleach Modification 1 sealant coupon wipe samples resulted in lower VX values
compared to Modification 2 with Chem A and Modification 2 with Chem B. Note that
bleach Modification 1 was not statistically different from Baseline for VX sealant wipes.
• Modification 3 with Dahlgren typically did not result in improved VX decontamination
compared to Baseline for any material/sample type.
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• Most Modification 1 comparisons of bleach to Dahlgren Decon did not have statistically
significant different VX recoveries across all material and sample types.
• Most Modification 2 comparisons were not significantly different. Where differences did
exist, there was no clear pattern as to whether Chem A or Chem B provided improved
decontamination results
• Most Chemical A comparisons were not significantly different. Where differences did
exist, there was no clear pattern as to whether bleach or Dahlgren Decon provided
improved decontamination
Table 52. Average VX Mass Recovered for Sealant Film Coupons - Modification Testing
Test
Sample Type
Average Mass Recovered ± SD
(US)
Rinse
Wipe
Coupon
SPE
Total
Surface
Total
Mod 1
Positive Control
NA
35±5.3
890±27
1.7±2.3
930±24
NA
NA
Bleach
NA
0.0049±
0.0023
510±89
201
530±98
99.99
±0.0068%
43±11%
Dahlgren
NA
0.37±0.28
680±23
5.6±7.3
690±29
99.0
±0.79%
26±3.6%
Mod 2
Eval
Positive Control
470±21
NA
370±71
140±145
980±89
NA
NA
Chem A
(no decontaminant)
410±110
NA
410±35
3.0±3.9
820±94
NA
NA
Chem B
(no decontaminant)
390±18
NA
500±30
0.56±0.41
900±41
NA
NA
Mod 2
Chem A
Positive Control
NA
29±8.6
550±100
110±190
690±96
NA
NA
Positive with Chem
A
400±50
11±7.7
200±18
21±30
630±29
NA
NA
Bleach with Chem A
360±120
0.0070±
0.0038
250±32
2.2±3.6
610±108
99.98±
0.015%
11±20%
Mod 2
Chem B
Positive Control
NA
32±3.9
720±47
0.58±0.75
750±51
NA
NA
Positive with Chem B
300±70
17±0.52
340±39
1.0±2.0
660±100
NA
NA
Bleach with Chem B
290±34
0.091±
0.093
330±6.0
0.041±
0.018
620±28
99.7±
0.29%
17±6.8%
Mod 3
Chem A
Positive Control
NA
38±3.8
650±41
0.80±0.65
680±44
NA
NA
Positive w/ Chem A
500±47
4.3±2.1
180±42
100±86
780±4.3
NA
NA
Dahlgren w/ Chem A
520±13
0.261
250±15
3.3±2.5
780±8.7
99.3
0%
NA = not applicable
1SD could not be calculated; only one replicate mass above the quantitation limit
Figure 33 through Figure 37 summarizes the Modification 1, 2, and 3 paint and sealant film
coupon VX average total mass recoveries, including error bars equal to one standard deviation
for each of the modification tests.
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VX Mod 1 Decontamination Test
(Error bars equal ± one standard deviation)
m 1,200
3
"S 1,000
L.
01
>
0
u
01
0£
800
600
400
- 200
Positive Control
I Bleach
Dahlgren
M
>
<
Paint
Sealant
Figure 33. VX Mod 1 Decontaminant Test, Average Total Mass Recoveries
VX Mod 2 Chem A and Chem B Evaluation
(Error bars equal ± one standard deviation)
m 1,200
"S 1,000
01
>
8 800
aj
cc
% 600
ro
400
m 200
Positive Control
ChemA
I ChemB
60
>
<
Paint
Sealant
Figure 34. VX Mod 2 Chem A and Chem B Evaluation, Average Total Mass Recoveries
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VX Mod 2 Chem A Decontamination Test
(Error bars equal ± one standard deviation)
1,200
£ 1,000
aj
>
o
u
aj
C£
U
"ro
4->
O
60
>
<
800
600
400
200
I Positive Control
Pos. Ctrl w/ ChemA
I Bleach w/ ChemA
Paint
Sealant
Figure 35. VX Mod 2 Chem A Decontaminant Test, Average Total Mass Recoveries
m 1,200
"S 1,000
01
>
8 800
aj
cc
W 600
400
m 200
>
<
VX Mod 2 Chem B Decontamination Test
(Error bars equal ± one standard deviation)
I Positive Control
Pos. Ctrl w/ ChemB
I Bleach w/ ChemB
Paint
Sealant
Figure 36. VX Mod 2 Chem B Decontaminant Test, Average Total Mass Recoveries
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VX Mod 3 Chem A Decontamination Test
(Error bars equal ± one standard deviation)
m 1,200
3
"S 1,000
l.
01
>
° 800 _
cc I ¦ Positive Control
J ^ I
< 400 ¦ ¦ ¦ ¦ ¦ H Dahlgren w/ ChemA
l". III III
cub
^ Paint Sealant
Figure 3 7. VX Mod 3 Chem A Decontaminant Test, Average Total Mass Recoveries
E. 8 Pesticide Modification Decontamination Testing
Pesticide modification testing included a total of two trials, one each for malathion and fipronil.
Each trial included two test materials (paint and sealant film coupons), one decontaminant (D7),
and two decontaminant modifications as described below:
• Modification 1 - two applications of D7, each with a 60-minute dwell time. A triple
water rinse was performed after the first application of D7.
• Modification 2 - one application of D7 with a 120-minute dwell time.
All pesticide spike control results (shown in Table 53) met the acceptance criteria described in
Section D.6. All malathion and fipronil laboratory blank results and a majority of the procedural
blank results met the acceptance criteria described in Section D.6. One procedural blank wipe
sample had a low-level result for fipronil; no impact to the data was observed. Internal standard
response for all fipronil and malathion results met the acceptance criteria described in Sections
C.7 and C.8. Most of the wipe and coupon procedural blanks required a 100-fold dilution (rather
than the typical 10-fold) to ensure internal standard response was acceptable.
Table 53. Pesticide Average Spike Control Results — Modification Testing
Pesticide
Test
Average Mass
Recovered
(Mg)
Percent
Recovery
(vs Theoretical)
RSD
Malathion
Mod 1/Mod 2
32
85%
12%
Fipronil
Mod 1/Mod 2
13
90%
0.88%
The average malathion mass recoveries for each sample component for the positive controls and
decontaminants, as well as total mass (combined recoveries of the rinse, wipe, coupon, and SPE)
are provided in Table 54 for paint films and Table 55 for sealant films. For paint Modification 1
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and 2, the average total mass recovered for the decontaminated samples was greater than the
average mass recovered for the positive controls, with the total decontamination efficacy
reported as 0%, which was below Baseline efficacy.
Table 54. Average Malathion Mass Recovered for Paint Films — Modification Testing
Sample Type
Average Mass Recovered ± SD
(US)
Decontamination Efficacy
Rinse
Wipe
Coupon
SPE
Total
Surface
Total
Positive Control
NA
<1.1
13±7.7
<1.0
13±7.7
NA
NA
Mod 1
<5.0
<1.1
17±3.1
<1.0
17±3.1
ND
0%
Mod 2
NA
<1.1
14±7.2
<1.0
14±7.2
ND
0%
NA = not applicable ND = not determined
For Modification 1, all sealant coupon replicate wipe results were below the quantitation limit.
For calculation purposes, the quantitation limit (1.1 |ig) was used, and surface decontamination
efficacy results were expressed with the > symbol. Modification 1 and 2 both resulted in
improved total malathion decontamination efficacy compared to the baseline result, which was
0% for D7. In addition to malathion analysis, samples were also analyzed for malaoxon. No
samples had any measurable malaoxon above the quantitation limit.
Table 55. Average Malathion Mass Recovered for Sealant Films — Modification Testing
Sample Type
Average Mass Recovered ± SD
(Ug)
Decontamination Efficacy
Rinse
Wipe
Coupon
SPE
Total
Surface
Total
Positive Control
NA
5.2±3.4
7.6±6.8
<1.0
13±4.5
NA
NA
Mod 1
<5.0
<1.1
7.3±0.99
<1.0
7.3±0.99
>79 %
43±22%
Mod 2
NA
1.31
9.7±1.8
<1.0
11±2.4
74%
14±36%
NA = not applicable
'SD could not be calculated; only one replicate mass above the quantitation limit
See Appendix E for statistical interpretation of the malathion Modification 1 and 2 results and
discussion of whether decontaminants had a significant effect on malathion levels. Statistical
malathion evaluations of baseline and modification testing resulted in the following:
• For Baseline comparisons, lOx diluted bleach resulted in lower malathion values only for
sealant coupons.
• For D7, Baseline sealant coupon samples resulted in lower malathion values compared to
Modification 1 or Modification 2. For malathion, there were no statistical differences for
Baseline, Modification 1, or Modification 2 paint coupon sample recoveries.
Figure 38 summarizes the Modification 1 and 2 paint and sealant malathion average total mass
recoveries including error bars equal to one standard deviation for the modification test.
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Malathion Mod Decontamination Test
(Error bars equal ± one standard deviation)
^ 30
T3
o
u
OJ
CC 20
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• For D7 comparisons, Modification 1 paint and sealant coupon samples resulted in
statistically significant lower fipronil values (lower fipronil recovery) compared to
baseline and Modification 2.
• For Baseline comparisons, D7 resulted in statistically significant lower fipronil values for
both paint wipes and paint coupons compared to lOx diluted bleach. D7 also resulted in
statistically significant lower fipronil values for sealant coupons compared to lOx diluted
bleach.
Figure 39 summarizes the Modification 1 and 2 paint and sealant fipronil average total mass
recoveries including error bars equal to one standard deviation for the modification test.
Fipronil Mod Decontamination Test
(Error bars equal ± one standard deviation)
"m 18
¦a 16
aj
w 14
o
K 12 I
# 10 ¦ Positive Control
S 8 ¦ ¦ D7 Mod 1
H ¦
¦ D7 Mod 2
i: L. I .
< Paint Sealant
Figure 39. Fipronil Modification Decontannnant Test, Average Total Mass Recoveries
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F. QUALITY ASSURANCE/QUALITY CONTROL
Data quality indicators, quality control elements, and quality assurance audits described in the
sections below provide the requirements for determining the adequacy of data generated during
this project. Methods were considered acceptable and the data valid if the data quality indicators
for the test measurements were met, and the performance evaluation, TSA, and data quality
audits demonstrated acceptable results.
F.l Data Quality Indicators
Data quality indicators and results are provided in Table 58. Most of the data quality indicator
results were acceptable per the QAPP for Decontamination Options for Chemical Warfare
Agents Permeated into Surface Layers (May 18, 2020), as amended, including checks of the
measurement methods for time, temperature, RH, volume, mass, pH, and CWA and pesticide
levels in blank samples and spike controls.
Table 58. Data Quality Indicators and Results
Parameter
Measurement
Method
Data Quality Indicator
Results
Time
(seconds)
Timer/data logger
Compare to time provided at
NIST.time.gov once before testing;
agree ±2 seconds/hour.
No difference was observed between the timers and NIST.time.gov
after one hour.
Temperature
(°C)
National Institute of
Standards and
Testing (NIST*)-
traceable
thermometer
Compare against calibrated
thermometer once before testing;
agree ±1 °C through 60 min.
The HOBO UX100 datalogger remained within 0.12 °C of the
calibrated reference through 60 min.
Relative
Humidity
(%)'
NIST-traceable
hygrometer
Compare against calibrated
hygrometer once before testing; agree
±10% through 60 min.
The HOBO UX100 datalogger remained within 0.50% of the
calibrated reference through 60 min.
Volume
(kiL)
Syringe with
repeating dispenser
or calibrated pipette
(CW A/pesticide
application)
Syringe and pipette were checked for
accuracy and repeatability once before
use by determining the mass of water
delivered onto a calibrated balance.
The syringe and pipette were
acceptable if the average mass of five
replicate droplets was ±10% of
expected (percent error).
The syringe used for CWA application and pipette used for pesticide
application were checked. Percent error was calculated using the
following equation:
., \Expected Weight-Mean Weight\ .AA
% Error X lUU
Expected Weight
Percent error results for each are provided below:
• 100 nL syringe: 5.8% (2-^iL droplet)
• 3-25 ^iL pipette: 2.6% (13-^.L droplet)
Volume
(ML)
Calibrated pipettes
(LC-MS/MS sample
dilution)
Pipettes were checked for accuracy
and repeatability before use by the
manufacturer. The pipette was
acceptable if the percent error was
±10% of expected.
Pipettes used for LC-MS/MS sample dilution were checked.
Systematic error for each is provided below:
• MR-10 at 5 ^L: 0.39%
• MR-50 at 35 ^L: 1.3%
• MR-250 at 100 ^iL: 0.42%
• MR-1000 at 500 ^iL: -0.13%
Weight
(g)
Oil mister/sprayer
(decontaminant
delivery)
Checks of each sprayer were
performed before each test by
weighing the amount of delivered
decontaminant. Spray application was
acceptable if the RSD of three
replicates was < 15%.
The balance was within calibration
and checked daily with weights
bracketing the mass of sprayed
decontaminant.
Three replicate spray applications of each decontaminant were
delivered to Teflon disks before each trial. All RSDs met the stated
criteria.
All balance calibration checks met acceptance criteria of ± 2.0% of
nominal mass
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Parameter
Measurement
Method
Data Quality Indicator
Results
PH
Calibrated pH meter
Meter was checked for accuracy prior
to each use using buffer solutions at:
• pH 4 (910104, Fisher Scientific)
• pH 7 (1552-16, Fisher Scientific)
• pH 10 (1602-16, Fisher Scientific)
• pH 12.5 (1618-16, Fisher Scientific)
Check value must be within ±0.1 pH
units of the buffer value.
pH meter was checked before each use using the specified buffer
solutions and was within tolerance during all checks. All buffer
solutions were within the expiration date.
CW A/pesticide
in LB** sample
extracts
Extraction,
LC/MS/MS or
GC/MS
LBs should have had less than 50% of
the lowest detected amount on the test
coupon or 1% of the amount on the
positive controls, whichever was
lower.
No CW A/pesticide outside the stated criteria was measured in any of
the LBs throughout testing.
CW A/pesticide
in PB***
sample extracts
Extraction,
LC/MS/MS or
GC/MS
PBs should have had less than 50% of
the lowest detected amount on the test
coupon or 1% of the amount on the
positive controls, whichever was
lower.
Most of the PBs met the stated criteria, several replicates had low-
level CW A/pesticide detected (see also discussion in Section E.5 and
F.6):
• VX Mod 2 Chem A - 0.0024 ^ig detected in sealant wipe sample
• VX Mod 2 Chem B - 0.010 ^ig detected in sealant wipe sample
• Fipronil Mod - 0.014 ^ig detected in paint wipe sample
CW A/pesticide
in SCs
LC/MS/MS or
GC/MS
The mean of the SCs included with
each test should have been within
80% to 120% of the target amount and
had an RSD of < 30% between
replicates.
Mean and RSD of the following SC sets were outside tolerance:
• HD FandT - 72% avg SC recovery, 60% RSD (see also discussion
in Section E.4)
• Malathion Baseline - 51% avg SC recovery, 38% RSD (see also
discussion in Section E.6)
*: NIST: National Institute of Standards and Testing
**: LB: Laboratory blank
***: PB: Procedural blank
F.2 Quality Control Elements
Data accuracy was ensured by the calibration of all instruments. Instrumentation used during
this project was maintained and operated according to the quality requirements and
documentation described in the approved QAPP and associated standard operating procedures
(SOPs). Except for the GC/MS and LC-MS/MS, all instruments utilized during the project were
calibrated as stipulated by the manufacturer or, at a minimum, annually. The GC/MS and LC-
MS/MS were calibrated according to the approved QAPP and associated SOPs. Table 59
provides calibration frequency for instruments that were used during this project.
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Table 59. Instrument Calibration Frequency
Instrument
Frequency
Timer
Prior to testing, performed by the manufacturer. After the manufacturer-
provided calibration expired, use of the expired unit was discontinued and
the unit was discarded. A new manufacturer-calibrated unit was obtained
for use.
Calibrated UX100 HOBO
Thermometer/Hygrometer
Prior to testing, performed by the manufacturer. After the manufacturer-
provided calibration expired, use of the expired unit was discontinued and
the unit was discarded. A new manufacturer-calibrated unit was obtained
for use.
Calibrated Pipettes
Prior to testing by the vendor and annually thereafter. Calibration/accuracy
was also verified as described in Table 58.
Balances
Prior to testing by the vendor and annually thereafter. Calibration/accuracy
was also verified as described in Table 58.
pH Meter
Calibration/accuracy was verified prior to each use as described in Table
58.
GC/MS
Calibrated prior to analysis of each set of test samples (calibration curve)
and a calibration verification standard was analyzed after every five
samples and at the end of a set of samples (see detailed discussion in
Section C.7).
LC-MS/MS
Calibrated prior to analysis of each set of test samples (calibration curve)
and a calibration verification standard was analyzed after every ten samples
and at the end of a set of samples (see detailed discussion in Section C.8).
At all times during the project, protocols required by Battelle's HMRC were followed in the
movement and use of CWA within the test facility. Chain of Custody (CoC) forms were used to
ensure that test samples generated during the work were traceable throughout all phases of
testing. Test measurements and information were recorded on Test Parameter Control Sheets
(TPCSs) or in a laboratory record book (LRB). Monitoring of test conditions, parameters, and
times was performed by technical staff familiar with the QAPP and testing and was documented
on the TPCS. The results of each test set were provided to the client electronically in the form of
Microsoft Excel™ files. Each Excel file included the CoC, GC/MS or LC-MS/MS analytical
results, final results for each sample showing all calculations, and a summary of the results. Each
sample was traceable from the CoC, to the analytical results, to the final results.
F.3 Quality Assurance Audits
Performance evaluation audits were essentially conducted continuously and addressed those
reference measurements that factored into the data used in quantitative analysis during the
evaluation, including volume, mass, and time measurements and GC/MS or LC-MS/MS
calibration and performance; see results provided in Table 58. The volume of CWA and
pesticides dispensed correlated directly to the mass of CWA and pesticides on the coupons.
Daily calibration of the GC/MS and LC-MS/MS, CCVs, and internal standard recovery provided
confidence that the analysis system was providing accurate data.
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While temperature and RH were measured and recorded for all testing using a calibrated device,
these parameters were not controlled; therefore, no performance evaluation audit could be
performed. See Appendix B for a summary table of measured temperature and RH at the start of
each test.
A Battelle Quality Assurance (QA) Officer performed a TSA at the HMRC facility in West
Jefferson, Ohio, for this testing on January 18, 2021, and on April 12, 2021. The purpose of the
TSA was to ensure that testing was performed in accordance with the QAPP. The QA Officer
reviewed the investigation methods, compared test procedures to those specified in the QAPP,
and reviewed data acquisition and handling procedures. The Battelle QA Officer did not identify
any findings that required corrective action.
A data quality audit provided validation of the data, including verification of the completeness of
the data, compliance with the acceptance criteria in the QAPP, recalculation checks, and tracing
of the data from instrument outputs through the final report. One hundred percent (100%) of the
data was reviewed prior to use in calculations or any data manipulation, and review was
completed before the data were provided to QA for the data quality audit.
The QA Officer, operating independently of the laboratory testing effort, audited at least 10% of
the data generated during testing. Data were traced from initial acquisition through reduction and
to final reporting. All calculations were checked.
Through the data quality audit, the TSA, and review of reports, the QA Officer ensured that data
generated during testing were valid, meeting the requirements of the QAPP.
F.4 QAPP
Two amendments to the QAPP were prepared during the project:
• Amendment 1 (dated January 11, 2021) identified which three decontaminants were
selected for CWA decontamination testing; identified the two decontaminants that were
downselected for use in CWA decontamination modification testing; and included the
titration approach for determining the percent peracetic acid concentration in Dahlgren
Decon.
• Amendment 2 (dated March 22, 2021) included the use of 10% butoxyethanol in water
and Zep Foaming Wall Cleaner for Modification 2 and 3 CWA testing; identified the use
of lOx bleach and D7 decontaminants for pesticide testing; established 24-hour and 72-
hour pesticide contact time tests for fate and transport testing; noted that all freestanding
paint and film coupons used in testing had been 4.5 cm instead of 5 cm and that 4.5 cm
coupons would continue to be used; stated that malathion and fipronil would be
purchased as commercially available materials for use in testing; and added malaoxon as
a target degradation product for malathion testing.
No deviations to the QAPP or QAPP amendments occurred.
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G. SUMMARY
The purpose of this project was to evaluate the efficacy of various liquid decontaminants to
degrade CWA and pesticide on the surface of coating layers, as well as CWAs and pesticides
that permeated past the coatings and into underlying porous materials. Decontaminants were
initially tested to determine which would be efficacious in decontamination of CWAs and
pesticides from the two freestanding coating layers, paint and sealant. The decontaminants that
were initially used for efficacy testing of the CWAs HD and VX included: bleach (nominal
hypochlorite concentration of 5% active ingredient), Dahlgren Decon (peracetic acid as active
ingredient), and Decon7 (D7) (H2O2 active ingredient). The decontaminants that were initially
used for efficacy testing of the pesticides (malathion and fipronil) included: lOx diluted bleach
(nominal hypochlorite concentration of 0.5%) and D7 (H2O2 active ingredient). A 2-|iL volume
of CWA or a 12-|iL volume of aqueous pesticide solution was applied to the surface of replicate
paint and sealant film coupons installed in LVAP assemblies and allowed to make contact for 24
hours (HD only) or for 72 hours (VX and both pesticides). Decontaminants were then applied via
spray to the surface of the films and allowed to dwell for 60 minutes. Following the
decontaminant dwell period, the surfaces of the film coupons were wipe-sampled and the film
coupons and SPE disks (underlying porous material) were solvent-extracted. HD and malathion
in wipe samples and extracts of film coupons and SPE disks were quantified using gas
chromatography/mass spectrometry (GC/MS) analysis. VX and fipronil were quantified in wipe
and LVAP component extracts using liquid chromatography-tandem mass spectrometry (LC-
MS/MS) analysis.
Based on the initial Baseline decontamination results, the decontaminants were down-selected
for additional testing to evaluate efficacy of decontamination modifications. For CWAs, two
decontaminants were included in the additional efficacy testing, with three decontamination
approach modifications were evaluated, as shown in Table 60. For pesticides, one decontaminant
was included in the additional efficacy testing, with two decontamination approach modifications
evaluated, as shown in Table 61.
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Table 60. Decontaminant Downselection and Modification for CWA
Modification
CWA
Decontaminant
Modification Description
1
HD
Bleach
120-minute decontamination dwell time
Dahlgren
VX
Bleach
D7
2
HD
Bleach
Application of 2-butoxyethanol (Chemical A) or
Zep Foaming Wall Cleaner (Chemical B),
followed by a water rinse, and 60-minute
decontamination dwell time
VX
Bleach
3
HD
Dahlgren
Application of Chemical A, followed by a water
rinse, and 60-minute decontamination dwell time
VX
Dahlgren
Table 61. Decontaminant Downselection and Modification for Pesticides
Modification
Pesticide
Decontaminant
Modification Description
1
Malathion
D7
60-minute decontamination dwell time, followed
¦ by a water rinse, and second 60-minute
decontamination dwell time
Fipronil
Bleach
2
Malathion
D7
¦ 120-minute decontamination dwell time
Fipronil
D7
The average total (combined efficacy of wipe sampling, film coupon extraction, and SPE disk
extraction) decontamination efficacies measured during CWA testing were low (< 50% efficacy)
across all the Baseline and modification testing for both paint and sealant films. The highest
decontamination efficacy measured for HD-contaminated paint films was demonstrated during
Modification 2 testing of bleach with Chemical A (average 35% efficacy) and for HD
contaminated sealant films, was demonstrated during Modification 2 testing of bleach with
Chemical B (average 14% efficacy). The highest decontamination efficacy measured for VX-
contaminated paint film coupons was demonstrated during Modification 1 testing with bleach
(average 39% efficacy), and for VX-contaminated sealant films was demonstrated during
Baseline testing with bleach (average 50% efficacy). Figure 40 and Figure 41 summarize the
average total percent decontamination efficacy measured for each test condition during Baseline
and modification testing for CWAs. While occasional improvements in the total recoveries were
noticed for some of the modifications that included the use of Chemical A or B, the general trend
appears to be that these chemicals do not help in the extraction of CWAs from the paint or
sealant followed by degradation at the surface with the selected decontaminant based on total
decontamination efficacy. Degradation of CWAs as present in the SPE disk (representing a
porous material under the film) was not observed for any of the tested modifications. All HD
paint and sealant wipe recoveries were significantly different compared to the positive controls
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that occurred for the Baseline and Modification 1 decontamination tests while all the HD paint
and sealant coupon differences occurred for Modification 1, Modification 2, and Modification 3.
In all cases, the difference was due to the test samples being less than the positive controls. All
the VX paint wipe differences occurred for Modification 1 and all of the VX sealant wipe and
coupon extraction differences occurred for Baseline and Modification 1. In all cases, the
difference was due to the test samples being less than the positive controls. Almost no significant
differences were observed between test samples and positive controls for SPE disks extracted for
HD or VX.
The average total decontamination efficacy measured during pesticide testing with malathion
was low across all the Baseline and modification testing for paint films, with the highest efficacy
demonstrated during Baseline testing using lOx diluted bleach (average 6.8% efficacy). The
average total decontamination efficacy measured during pesticide testing with malathion were
highest during Baseline testing for sealant films using lOx diluted bleach (average 77% efficacy).
The average total decontamination efficacy measured during pesticide testing with fipronil was
mostly high across all the Baseline and modification testing for both paint and sealant films. The
highest decontamination efficacy measured for fipronil-contaminated paint films was
demonstrated during Modification 1 testing with D7 (average 98% efficacy), and for fipronil
contaminated sealant films was demonstrated during Baseline testing with lOx diluted bleach
(average 99% efficacy). Figure 43 and Figure 42 summarize the average total percent
decontamination efficacies measured for each test condition during Baseline and modification
testing for pesticides.
HD Average Total Percent Efficacy
100%
80%
>
ro 60%
u
3=
LU
¦M
£
ai
£ 40%
Q.
20%
0%
Figure 40. HD Average Total Percent Efficacy
"J
ii
Baseline
Bleach
Baseline
Dahlgren
Baseline D7
Mod 1
Bleach
Mod 1 D7
Mod 2
Bleach w/
ChemA
Decontaminant/Modification
Paint
Sealant
1
Mod 2 Mod 3
Bleach w/ Dahlgren
ChemB w/ ChemA
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VX Average Total Percent Efficacy
100%
80%
Baseline Baseline Baseline D7 Mod 1 Mod 1 Mod 2 Mod 2 Mod 3
Bleach Dahlgren Bleach Dahlgren Bleach w/ Bleach w/ Dahlgren
ChemA ChemB w/ ChemA
Decontaminant/Modification
¦ Paint
Sealant
Figure 41. VX Average Total Percent Efficacy
100%
Malathion Average Total Percent Efficacy
>
u
nj
80%
60%
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Fipronil Average Total Percent Efficacy
100%
80%
3 60%
C
u 40%
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H. REFERENCES
1. Fate and Transport of Chemical Warfare Agents VX and HD across a Permeable Layer of
Paint or Sealant into Porous Subsurfaces. U.S. EPA Office of Research and
Development, Washington, DC, EPA/600/R-16/173, 2016
2. How EPA Manages the Quality of its Environmental Information | US EPA last accessed
3/31/2022.
3. https://pubchem.ncbi.nlm.nih.gov/compound/Malathion#section=Solubilitv. last accessed
3/31/2022.
4. https://pubchem.ncbi.nlm.nih.gov/compound/Fipronil#section= Solubility. last accessed
3/31/2022.
5. ASTM Standard D823-18, "Standard Practices for Producing Films of Uniform
Thickness of Paint, Varnish, and Related Products on Test Panels," ASTM International,
West Conshohocken, PA, 2018
6. ASTM Standard E376-19, "Standard Practice for Measuring Coating Thickness by
Magnetic-Field or Eddy-Current (Electromagnetic) Test Methods," ASTM International,
West Conshohocken, PA, 2019
7. U.S. EPA. Remediation Options for Porous Materials Contaminated with Persistent
Chemical Warfare Agents VX and HD. U.S. Environmental Protection Agency,
Washington, DC, EPA/600/R-17/348, 2017
8. Method 8000D, Determinative Chromatographic Separations, Revision 4, July 2014,
Final Update V to the Third Edition of the Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods, U.S. EPA publication SW-846
9. Oudejans, L. Remediation Options for Fentanyl Contaminated Indoor Environments. U.S.
Environmental Protection Agency, Washington, DC, EPA/600/R-21/105, 2021
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APPENDIX A
DECONTAMINANT ACTIVITY DATA
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Bleach Concentration andpH Results
Trial
Decontaminant Lot #
Concentration
(Hypochlorite)
pH
Quench (HD/VX)
20248
5.5%
12.26
Baseline (HD)
20265
5.8%
12.18
Baseline (VX)
20258
5.8%
12.32
Mod 1 (HD)
20258
5.5%
12.34
Mod 1 (VX)
20260
5.8%
12.31
Mod 2 Chem A (HD)
21060
6.8%
12.32
Mod 2 Chem A (VX)
21060
6.4%
12.27
Mod 2 Chem B (HD)
21029
6.1%
12.31
Mod 2 Chem B (VX)
21060
6.2%
12.30
Dahlgren Decon Concentration and pH Results
Trial
Decontaminant Lot #
Concentration
(Peracetic Acid)
pH
Quench (HD/VX)
8/2020
6.6%
6.92
Baseline (HD)
8/2020
7.9%
6.71
Baseline (VX)
8/2020
11.0%
6.69
Mod 1 (VX)
8/2020
7.8%
6.97
Mod 3 Chem A (HD)
16621-17421-16221
6.3%
6.84
Mod 3 Chem A (VX)
16621-17421-16221
8.3%
6.86
D7 Concentration and pH Results
Trial
Decontaminant Lot #
Concentration
(Hydrogen Peroxide)
pH
Quench (HD/VX)
06-09-20-01M
4.3%
9.66
Baseline (HD)
06-09-20-01M
4.5%
9.58
Baseline (VX)
06-09-20-01M
4.9%
9.67
Mod 1 (HD)
06-09-20-01M
5.8%
9.71
Quench (Pesticides)
06-03-20-01M
1.2%
10.08
Baseline (Fipronil)
06-03-20-01M
4.5%
9.69
Baseline (Malathion)
06-03-20-01M
3.9%
9.66
Mod 1 (Fipronil)
06-09-20-01M
4.6%
9.51
Mod 1 (Malathion)
06-03-20-01M
4.5%
9.72
lOx Diluted Bleach Concentration and pH Results
Trial
Decontaminant Lot #
Concentration
(Hypochlorite)
pH
Quench (Pesticides)
55444-86-7
0.63%
11.54
Baseline (Fipronil)
55444-91-2
0.67%
11.38
Baseline (Malathion)
55444-94-2
0.63%
11.44
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APPENDIX B
LABORATORY ENVIRONMENTAL CONDITIONS
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Laboratory Environmental Conditions at Start of Test
Trial
Laboratory Environmental
Conditions at Test Start
Temp (°F)
RH (%)
Wipe MD* (HD)
68.3
59.5
Wipe MD (VX)
68.4
59.3
Extraction MD (HD)
67.5
59.1
Extraction MD (VX)
68.5
59.1
Fate and Transport (HD)
67.6
58.9
Fate and Transport (VX)
66.8
62.4
Quench (HD)
68.3
17.0
Quench (VX)
68.3
17.0
Baseline (HD)
70.3
15.0
Baseline (VX)
69.2
22.0
Mod 1 (HD)
71.2
15.0
Mod 1 (VX)
70.4
24.6
Mod 2 Evaluation (HD)
72.7
15.0
Mod 2 Evaluation (VX)
71.7
36.2
Mod 2 Chem A (HD)
67.1
37.3
Mod 2 Chem A (VX)
69.5
50.3
Mod 2 Chem B (HD)
70.3
22.4
Mod 2 Chem B (VX)
70.9
17.6
Mod 3 Chem A (HD)
69.4
53.6
Mod 3 Chem A (VX)
70.3
33.6
Wipe MD (Fipronil)
69.5
24.3
Wipe MD (Malathion)
69.2
48.2
Wipe MD 2 (Malathion)
67.9
62.7
Extraction MD (Fipronil)
68.5
51.5
Extraction MD (Malathion)
69.2
54.4
Extraction MD 2 (Malathion)
68.4
57.7
Fate and Transport (Fipronil)
68.0
61.5
Fate and Transport (Malathion)
68.4
58.6
Quench (Fipronil)
71.5
52.3
Quench (Malathion)
69.5
55.2
Baseline (Fipronil)
68.7
55.7
Baseline (Malathion)
67.4
60.6
Mod 1 (Fipronil)
67.1
61.7
Mod 1 (Malathion)
69.8
38.3
*MD = method development
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APPENDIX C
PERACETIC ACID TITRATION
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Step
Action
Color
1
Set up a 300-mL Erlenmeyer flask in an ice bath on a stir plate.
2
Insert a glass thermometer into the Erlenmeyer flask.
(Temperatures of solution were required not to exceed 5 °C during
the titration)
3
Add 100 mL of 10% sulfuric acid to the Erlenmeyer flask.
4
Add 2 drops of ferroin solution to the Erlenmeyer flask.
Orange
5
Add one drop of cerium (IV) sulfate solution to the Erlenmeyer
flask.
Blue/nearly colorless
6
Weigh 0.3 g ± 0.05 g of prepared Dahlgren Decon and add to the
Erlenmeyer flask.
Orange
7
Titrate dropwise with cerium (IV) sulfate solution.
Until changes back to
blue/nearly colorless
8
Add 10 mL of potassium iodide solution and 5 mL starch solution
to the Erlenmeyer flask.
Opaque brown
9
Immediately titrate dropwise with sodium thiosulfate solution (1
drop = 50 (iL titrant).
Until changes to clear light
orange
Reagent
Vendor
Catalpg
Number
Sulfuric Acid, 10% (v/v) Aqueous Solution, Ricca Chemical
Fisher Scientific
8150-16
Honeywell Fluka™ Ferroin Indicator Solution, 0.025 M,
Honeywell™ Fluka™
Fisher Scientific
60-046-934
Aqua Solutions Starch Solution 1% 500 mL
Fisher Scientific
NC9195165
Sodium thiosulfate solution, Volumetric, Reag. Ph. Eur., 0.1 M
Na2S203 (0.1 N), Honeywell Fluka™
Fisher Scientific
60-026-21
Potassium Iodide Solution (10% w/v), Fisher Chemical™
Fisher Scientific
SP242-500
Cerium(IV) sulfate solution, 0.1M Ce(S04)2, Honeywell™
Millipore Sigma
1090921003
Equipment used for the titration included the following:
• Glass burette, 25 mL with 0.1 mL increments
• Balance (Mettler Toledo, model # PG6002-S)
• Stir Plate (Fisherbrand Isotemp, catalog # SP88857200)
• Refrigerated/Heated Bath Circulator (Fisherbrand Isotemp, model # 6200 R28)
• Glass Thermometer (Thermco, -20 to 150 °C, Thomas Scientific catalog # 1221C73)
Calculation of percent peracetic acid concentration was performed using the below equation:
((>jiL Na2S203')X(LNormality of titrant)xf 39'osS X(100%)1
%PAA = - - - - — - -
/0 (, „ T, „ ^,/iooo
^ (.jj Dahlgren Decon) X(^ — I |
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APPENDIX D
CWA STATISTICAL ANALYSIS
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The objective of this statistical analysis was to compare total HD and VX mass recovered from
each of two different materials (paint and sealant) and on each of three different sample types
(surface wipes, extracted coupons, and extracted SPE disks) using eight different combinations
of one of three decontaminants applied under one of four testing methods (see Table Dl). Three
replicates were tested for each condition. Table D2 summarizes the study design.
Additional evaluation was performed using positive control tests. The positive control tests
excluded application of the target decontaminant but may include the preapplication of a
chemical with a water rinse. The decontamination test conditions were compared to their
analogous positive control tests to determine if statistically significant decontamination occurred.
Positive controls were also compared between testing methods to evaluate whether the
differences between methods might be attributable to external factors besides the
decontamination process.
Table Dl. Description of Testing Methods and Decontaminant Combinations
Testing
Method
Dwell Time
Preapplication of
Chemical with
Water Rinse?
Decontaminant Application
Baseline
0 minutes
No
Bleach, D7, or Dahlgren Decon
Mod 1
120 minutes
No
Bleach, D7 (HD only), or Dahlgren Decon (VX
only)
Mod 2
0 minutes
Yes (Chem A or B)
Bleach
Mod 3
0 minutes
Yes (Chem A only)
Dahlgren Decon
Observations below the method quantification limit (MQL) were set equal to the MQL, which
was 1.1 |ig for HD wipe masses and ranged from 0.001 |ig to 0.11 |ig for VX, dependent on
sample type and required sample dilutions. Table D3 displays the percentage of observations
below the MQL in each test condition, as well as the overall percentage of < MQL observations
within each agent/material/sample type analysis. Many substitutions at the MQL value likely
biases the estimates high and using a single substitution value artificially reduces the variance
associated with the estimates. The reduction in variance may make the estimates more likely to
be significantly different from other estimates when a real difference is not present.
For Mod 2 and Mod 3 where a preapplication of a chemical with a water rinse was performed,
the mass recovery from the rinse data was added to the mass recovery from the wipe data to
obtain the total mass recovered for each replicate. The counts of data below the MQL in the wipe
conditions (see Table D3) reflect whether either the rinse or the wipe extraction mass was <
MQL; samples with both rinse and wipe values below the MQL and samples with only one of
the rinse or wipe values below the MQL were counted similarly.
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Table D2. Study Design for Testing Method and Decontaminant Comparison
Testing
Method
Number of Replicates
Agent
Material
Decontaminant
Wipe
Samples
Extracted
Coupon
Samples
SPE Disk
Samples
HD
Paint
Baseline
Bleach
3
3
3
HD
Paint
Baseline
Dahlgren Decon
3
3
3
HD
Paint
Baseline
D7
3
3
3
HD
Paint
Mod 1
Bleach
3
3
3
HD
Paint
Mod 1
D7
3
3
3
HD
Paint
Mod 2
Bleach + Chem A
3
3
3
HD
Paint
Mod 2
Bleach + Chem B
3
3
3
HD
Paint
Mod 3
Dahlgren Decon + Chem A
3
3
3
HD
Sealant
Baseline
Bleach
3
3
3
HD
Sealant
Baseline
Dahlgren Decon
3
3
3
HD
Sealant
Baseline
D7
3
3
3
HD
Sealant
Mod 1
Bleach
3
3
3
HD
Sealant
Mod 1
D7
3
3
3
HD
Sealant
Mod 2
Bleach + Chem A
3
3
3
HD
Sealant
Mod 2
Bleach + Chem B
3
3
3
HD
Sealant
Mod 3
Dahlgren Decon + Chem A
3
3
3
VX
Paint
Baseline
Bleach
3
3
3
VX
Paint
Baseline
Dahlgren Decon
3
3
3
VX
Paint
Baseline
D7
3
3
3
VX
Paint
Mod 1
Bleach
3
3
3
VX
Paint
Mod 1
Dahlgren Decon
3
3
3
VX
Paint
Mod 2
Bleach + Chem A
3
3
3
VX
Paint
Mod 2
Bleach + Chem B
3
3
3
VX
Paint
Mod 3
Dahlgren Decon + Chem A
3
3
3
VX
Sealant
Baseline
Bleach
3
3
3
VX
Sealant
Baseline
Dahlgren Decon
3
3
3
VX
Sealant
Baseline
D7
3
3
3
VX
Sealant
Mod 1
Bleach
3
3
3
VX
Sealant
Mod 1
Dahlgren Decon
3
3
3
VX
Sealant
Mod 2
Bleach + Chem A
3
3
3
VX
Sealant
Mod 2
Bleach + Chem B
3
3
3
VX
Sealant
Mod 3
Dahlgren Decon + Chem A
3
3
3
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Table D3. Percent of Observations < MQL in Each Test Condition
Agent
Material
Testing
Method
Decontaminant
Percent of Replicates
Wipe „ . SPE Disk
„ , Samples „ ,
Samples Samples
HD
Paint
Baseline
Bleach
100%
0%
0%
HD
Paint
Baseline
Dahlgren
100%
0%
0%
HD
Paint
Baseline
D7
0%
0%
0%
HD
Paint
Mod 1
Bleach
100%
0%
0%
HD
Paint
Mod 1
D7
100%
0%
0%
HD
Paint
Mod 2
Bleach + Chem A
100%
0%
0%
HD
Paint
Mod 2
Bleach + Chem B
100%
0%
0%
HD
Paint
Mod 3
Dahlgren Decon + Chem A
100%
0%
0%
HD
Paint
Total
87.5%
0%
0%
HD
Sealant
Baseline
Bleach
100%
0%
0%
HD
Sealant
Baseline
Dahlgren Decon
100%
0%
0%
HD
Sealant
Baseline
D7
0%
0%
0%
HD
Sealant
Mod 1
Bleach
100%
0%
0%
HD
Sealant
Mod 1
D7
0%
0%
0%
HD
Sealant
Mod 2
Bleach + Chem A
100%
0%
0%
HD
Sealant
Mod 2
Bleach + Chem B
100%
0%
0%
HD
Sealant
Mod 3
Dahlgren Decon + Chem A
100%
0%
0%
HD
Sealant
Total
75%
0%
0%
VX
Paint
Baseline
Bleach
0%
0%
0%
vx
Paint
Baseline
Dahlgren Decon
0%
0%
0%
VX
Paint
Baseline
D7
0%
0%
0%
vx
Paint
Mod 1
Bleach
0%
0%
0%
vx
Paint
Mod 1
Dahlgren Decon
0%
0%
0%
vx
Paint
Mod 2
Bleach + Chem A
0%
0%
0%
vx
Paint
Mod 2
Bleach + Chem B
0%
0%
0%
vx
Paint
Mod 3
Dahlgren Decon + Chem A
100%
0%
0%
vx
Paint
Total
12.5%
0%
0%
vx
Sealant
Baseline
Bleach
0%
0%
0%
vx
Sealant
Baseline
Dahlgren Decon
0%
0%
0%
vx
Sealant
Baseline
D7
0%
0%
0%
vx
Sealant
Mod 1
Bleach
0%
0%
66.7%
vx
Sealant
Mod 1
Dahlgren Decon
0%
0%
0%
vx
Sealant
Mod 2
Bleach + Chem A
0%
0%
0%
vx
Sealant
Mod 2
Bleach + Chem B
0%
0%
0%
vx
Sealant
Mod 3
Dahlgren Decon + Chem A
66.7%
0%
0%
vx
Sealant
Total
8.33%
0%
8.33%
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CWA Analysis of Variance (ANOVA)
Comparison of Test Sample Results
A fixed effects ANOVA model was fitted to the total mass recovery data over all testing method
and decontaminant combinations separately for each agent, material, and sample type condition.
The models contained an effect for the combination of testing method and decontaminant and a
residual error term. No random effect of trial was fitted due to only one trial being run for all
replicates of each agent and material condition.
The assumptions of normally distributed errors with approximately equal variances were better
met with untransformed data than with natural logarithm-transformed data, so data were left
untransformed for the analysis. For some models, however, Levene's test [Dl] still indicated that
the Homogeneity of Variances assumption was not satisfied (p < 0.05). For the wipe samples for
HD on paint and sealant, the unequal variances were believed to be driven by the large
proportion of values below the MQL (see Table D3). For these models, residual variances
estimates were first calculated from only the values above the MQL, and then were used for all
conditions in the full model over all data. This approach assumes that, if the true masses for the <
MQL samples could have been measured, then the variance in the corresponding data would
have been similar to the variance of the samples measured above the MQL.
The models were fitted using SAS (version 9.4, 64-bit). The form of the model is presented in
Equation Dl.
Mass (Jug) = (10 + /% + eijk
Equation Dl
where:
• /?0 = intercept or overall mean total mass collected.
• Pij = the fixed effect for the z'th testing method and/h decontaminant.
• £ijk = random error for the k'h replicate from the ith testing method, and/h decontaminant.
The random error is assumed to be N{0,
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2. The six comparisons between different decontaminants using the same testing method
(e.g., the Baseline method with bleach vs Baseline with D7).
These pairwise comparisons amounted to 14 total comparisons for each of the 12
agent/material/sample type conditions, or 168 total comparisons. See also Table D4 and Table
D5 for a summary of the comparisons performed for HD on paint and sealant and VX on paint
and sealant, respectively. Conditions of the same color within a column were compared to each
other, which resulted in seven HD comparisons for paint and seven for sealant, and six VX
comparisons for paint and six for sealant.
Table D4. HD Paint and Sealant Comparison Sets
Test
Comparison Set 1
Comparison Set 2
Comparison Set 3
Sample Typt
Baseline
Bleach
Bleach
Bleach
Wipe
Extracted
Coupon
SPE
Dahlgren Decon
Dahlgren Decon
Dahlgren Decon
Wipe
Extracted
Coupon
SPE
D7
D7
D7
Wipe
Extracted
Coupon
SPE
Mod 1
Bleach
Bleach
Bleach
Wipe
Extracted
Coupon
SPE
D7
D7
D7
Wipe
Extracted
Coupon
SPE
Mod 2
Bleach/Chem A
Bleach/Chem A
Bleach/Chem A
Wipe
Extracted
Coupon
SPE
Bleach/Chem B
Bleach/Chem B
Bleach / Chem B
Wipe
Extracted
Coupon
SPE
Mod 3
Dahlgren
Decon/Chem A
Dahlgren
Decon/Chem A
Dahlgren
Decon/Chem A
Wipe
Extracted
Coupon
SPE
Table D5. VX Paint and Sealant Comparison Sets
Test
Comparison Set 1
Comparison Set 2
Comparison Set 3
Sample Type
Baseline
Bleach
Bleach
Bleach
Wipe
Extracted
Coupon
SPE
Dahlgren Decon
Dahlgren Decon
Dahlgren Decon
Wipe
Extracted
Coupon
SPE
D7
D7
D7
Wipe
Extracted
Coupon
SPE
Mod 1
Bleach
Bleach
Bleach
Wipe
Extracted
Coupon
SPE
Dahlgren Decon
Dahlgren Decon
Dahlgren Decon
Wipe
Extracted
Coupon
SPE
Mod 2
Bleach/Chem A
Bleach/Chem A
Bleach/Chem A
Wipe
Extracted
Coupon
SPE
Bleach/Chem B
Bleach/Chem B
Bleach/Chem B
Wipe
Extracted
Coupon
SPE
Mod 3
Dahlgren
Decon/Chem A
Dahlgren
Decon/Chem A
Dahlgren
Decon/Chem A
Wipe
Extracted
Coupon
SPE
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The Bonferroni-Holm multiple comparisons procedure was performed to adjust the ^-values of
the pairwise comparisons so that a familywise error rate of 0.05 was maintained over all fourteen
comparisons of interest within an agent/material/sample type condition. This procedure limits the
probability of a difference being falsely identified as statistically significant when no observable
difference exists, and the difference is due to sampling variability. The familywise error rate
means that the chance of a sampling-based falsely significant result is no more than 1 in 20 for
the entire set of fourteen comparisons. The Bonferroni-Holm procedure was selected due to its
power in detecting true differences when performing a restricted number of pairwise
comparisons.
Comparison of Test Sample Results with Positive Controls
A fixed-effects ANOVA model was fitted to the total mass recovery data for decontaminants and
positive controls results within each agent/material/sample type/testing method condition. In the
cases for Mod 2 and Mod 3 where positive controls were tested both with and without the
application of an additional chemical, only the positive controls from the conditions with
chemical application were included in the model. The models contained an effect for the
combination of decontaminant/positive control status and a residual error term. No random effect
of trial was fitted due to only one trial being run for all replicates of each agent and material
condition.
The assumptions of normality and equality of variances were better met with untransformed data
than with natural logarithm-transformed data, so data were left untransformed for the analysis.
The models were fitted using SAS (version 9.4, 64-bit). The form of the model is presented in
Equation D2.
Mass (jig) = (10 + /?,• + £tj
Equation D2
where:
• /?0 = intercept or overall mean total mass collected.
• /?,• = the fixed effect for the z'th decontaminant / positive control condition.
• E[j = random error for the jh replicate from the z'th decontaminant/positive control
condition. The random error is assumed to be N{0,
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The Bonferroni-Holm multiple comparisons procedure was performed to adjust the ^-values of
the pairwise comparisons so that a familywise error rate of 0.05 was maintained over all
comparisons of interest within an agent/material/sample type/testing method condition. The
Bonferroni-Holm procedure was selected due to its power in detecting true differences when
performing a restricted number of pairwise comparisons.
Comparison of Positive Control Results
A fixed effects ANOVA model was fitted to the total mass recovery data for positive controls
results under each testing method within each agent/material/sample type condition. In the cases
for Mod 2 and Mod 3 where positive controls were tested both with and without the application
of an additional chemical, the positive controls from both the conditions with chemical
application and those without the application were included in the model. The Fate and Transport
data without Headspace for each agent/material/sample type were also included as a test method
condition in this analysis. The models contained an effect for the combination of testing method
under which the positive control was collected and the chemical application, and a residual error
term. No random effect of trial was fitted due to only one trial being run for all replicates of each
agent and material condition. Data were left untransformed for the analysis to remain consistent
with analyses of test samples and test samples vs positive controls.
The models were fitted using SAS (version 9.4, 64-bit). The form of the model is presented in
Equation D3.
Mass (jug) = (10 + /% + eijk
Equation D3
where:
• /?0 = intercept or overall mean total mass collected.
• Pij = the fixed effect for the positive controls from the z'th testing method and jth chemical
application condition.
• £ijk = random error for the kh positive control from the z'th testing method//7'' chemical
application condition. The random error is assumed to be N{0,
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comparisons of interest within an agent/material/sample type. The Bonferroni-Holm procedure
was selected for consistency with the previous analyses.
Outliers
Potential outliers were determined by calculating the deleted (externally) studentized residuals.
If the absolute value of the standardized residual was greater than 3, then the observation was
considered a potential outlier. If potential outliers were found, the results were checked to
determine the validity of the outlying data and probable causes for the outliers. If no probable
cause was found, the outlier was included in the subsequent analysis.
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CWA ANOVA Results
Table D6 through Table D8 display the potential outliers identified by examining the externally
studentized residuals in each study condition. Two of the outliers from the SPE disks in the VX
Sealant condition were excluded from all analyses after investigator confirmation that observed
data may not have reflected the intended experimental outcomes (denoted with * in the tables
below).
Table D6. Potential Outliers Identifiedfrom Test Samples
Analysis
Agent
Material
Sample
Type
Test
Method
Decontaminant
Total
Mass
Recovery
(MS)
Externally
Studentized
Residual
HD
Paint
SPE
Baseline
Bleach
1266.50
3.46
HD
Sealant
Extracted
Coupon
Baseline
D7
194.30
-3.58
Test
Samples
VX
Paint
Wipe
Baseline
Bleach
94.72
3.46
VX
Paint
Extracted
Coupon
Mod 2
Bleach + Chem A
9.60
-3.58
VX
Sealant
Wipe
Mod 2
Bleach + Chem A
467.58
-3.01
VX
Sealant
Wipe
Mod 2
Bleach + Chem A
241.15
-3.17
VX
Sealant
SPE
Mod 1
Bleach
59.61
4.30
105
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Table D 7. Potential Outliers Identified from Test Samples vs. Positive Controls
Analysis
Agent
Material
Sample
Type
Test Method
Decontaminant or
Positive Control
(PC)
Total
Mass
Recovery
(M)
Externally
Studentized
Residual
HD
Paint
Wipe
Baseline
PC
2.84
-9.82
HD
Paint
Wipe
Mod 1
PC
12.0
12.4
HD
Paint
Extracted
Coupon
Mod 2 + Chem A
PC
173
-4.76
HD
Paint
Extracted
Coupon
Mod 2 + Chem B
PC
274
-5.06
HD
Paint
SPE
Baseline
Bleach
1270
3.08
HD
Paint
SPE
Mod 2 + Chem A
PC
1400
3.65
HD
Sealant
Wipe
Baseline
D7
2.33
-20.6
HD
Sealant
Wipe
Mod 1
D7
4.26
19.9
HD
Sealant
Wipe
Mod 2 + Chem A
PC
9.49
-3.57
HD
Sealant
Wipe
Mod 2 + Chem B
PC
16.1
5.24
HD
Sealant
Wipe
Mod 3 + Chem A
PC
7.13
-4.01
HD
Sealant
Extracted
Coupon
Mod 2 + Chem B
PC
244.1
4.96
VX
Paint
Wipe
Mod 2 + Chem B
Bleach + Chem B
210.1
4.46
Test Samples
VX
Paint
Wipe
Mod 3 + Chem A
Positive Control
303.8
3.52
vs. Positive
Control
VX
Paint
Extracted
Coupon
Baseline
Bleach
321.3
3.73
Comparison
VX
Paint
Extracted
Coupon
Mod 2 + Chem A
Bleach + Chem A
9.60
-4.26
VX
Paint
Extracted
Coupon
Mod 2 - Chem B
PC
195
6.00
VX
Paint
Extracted
Coupon
Mod 3 + Chem A
Dahlgren + Chem A
129
5.22
VX
Paint
SPE
Mod 2 + Chem B
PC
59.4
-4.23
VX
Sealant
Wipe
Baseline
PC
35.3
3.37
VX
Sealant
Wipe
Mod 1
PC
30.0
-4.42
VX
Sealant
Wipe
Mod 1
PC
40.6
3.39
VX
Sealant
Wipe
Mod 2 + Chem B
PC
400
3.39
VX
Sealant
Wipe
Mod 3 + Chem A
PC
560
6.14
VX
Sealant
Extracted
Coupon
Mod 1
Bleach
421
-3.42
VX
Sealant
Extracted
Coupon
Mod 2 + Chem B
PC
300
-3.11
VX
Sealant
SPE
Mod 1
Bleach
59.6*
10.02
VX
Sealant
SPE
Mod 2 + Chem A
PC
55.5
12.06
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Analysis
Agent
Material
Sample
Type
Test Method
Decontaminant or
Positive Control
(PC)
Total
Mass
Recovery
(MS)
Externally
Studentized
Residual
VX
Sealant
SPE
Mod 2 + Chem B
PC
2.93
75.67
vx
Sealant
SPE
Mod 3 + Chem A
PC
4.89
-5.98
* Outlier excluded from analyses.
Table D8. Potential Outliers Identifiedfrom Positive Controls Analysis
Analysis
Agent
Material
Sample
Type
Test
Method
Decontaminant
or Positive
Control (PC)
Total
Mass
Recovery
(MS)
Externally
Studentized
Residual
HE)
Paint
Extracted
Coupon
Fate &
Transport
Fate & Transport
893
4.73
HE)
Paint
SPE
Fate &
Transport
Fate & Transport
1100
-3.81
HE)
Sealant
Wipe
Mod 3 +
Chem A
PC + Chem A
7.13
-4.59
HE)
Sealant
SPE
Fate &
Transport
Fate & Transport
1050
-9.35
VX
Paint
Wipe
Fate &
Transport
Fate & Transport
670
7.16
Positive
Controls
vx
Paint
Extracted
Coupon
Fate &
Transport
Fate & Transport
1297
7.37
VX
Paint
Extracted
Coupon
Fate &
Transport
Fate & Transport
826
-3.14
VX
Sealant
Wipe
Mod 2 +
ChemB
PC + ChemB
400
4.13
VX
Sealant
Extracted
Coupon
Mod 2 -
Chem A
PC
436
-3.03
VX
Sealant
SPE
Fate &
Transport
Fate & Transport
459
4.30
VX
Sealant
SPE
Mod 2 -
Chem A
PC
324*
3.05
* Outlier excluded from the analyses.
Figure D1 to Figure D2 displays the total mass recoveries for the replicates in each
agent/material/sample type condition. Statistical summaries including arithmetic means and 95%
confidence intervals are presented in Table D9 to Table D12 and are sorted in order of estimated
mean total mass recovery within each agent, material, and sample type. Confidence bounds were
not adjusted for multiple comparisons between test conditions and thus should not be used to
evaluate significant differences between test conditions.
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Figure Dl. Total recovery mass of test samples for all testing method and decontaminant combinations over all sample types for
HD on Paint
1500 -
3 1 000 -
c/i
cr>
ro
"ro
"S 500 -
I-
0 -
Baseline Mod 1 Mod 2 Mod 2 Mod 3 Baseline Mod 1 Mod 2 Mod 2 Mod 3 Baseline Mod 1 Mod 2 Mod 2 Mod 3
(+Chern A)(+Chem B)(+Chem A) (+Chem A)(+Chem B)(+Chem A) (+Chem A)(+Chem B)(+Chem A)
Testing Method
Decontaminant O Bleach + D7 X Dahlgren
SampleType= Coupon
SampleType = SPE
SampleType = Wipe
OO
+ +
XX X
dD
++
OGD
OD
XXX
O O
+ +
XX X
(ID
++ +
o o
ODO
X X
QSD + >fi9< CEDt+f O O X
t 1 1 1 1 1 1 1 1 1 1 1 1 1 r
108
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Figure D2. Total recovery mass of test samples for all testing method and decontaminant combinations over all sample types for
HD on Sealant
1500 -
3 1 000 -
c/i
cr>
ro
"ro
"S 500 -
I-
0 -
Baseline Mod 1 Mod 2 Mod 2 Mod 3 Baseline Mod 1 Mod 2 Mod 2 Mod 3 Baseline Mod 1 Mod 2 Mod 2 Mod 3
(+Chern A)(+Chem B)(+Chem A) (+Chem A)(+Chem B)(+Chem A) (+Chem A)(+Chem B)(+Chem A)
Testing Method
Decontaminant O Bleach + 07 X Dahlgren
SampleType = Coupon
SampleType = SPE
SampleType = Wipe
§+;* e* co § S
O
O
+
8 x 8+ ° „ X
_ ± ^ + @ ®
o ^ x ox
asD+>69< ced+ am o x
109
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Figure D3. Total recovery mass of test samples for all testing method and decontaminant combinations over all sample types for
VX on Paint
SampleType = Coupon
SampleType = SPE
SampleType = Wipe
8 * % S & § v
O "
, ^ O ^ Q Q V
g 9 x i *
R 8 m
+ X OK
Baseline Mod 1 Mod 2 Mod 2 Mod 3 Baseline Mod 1 Mod 2 Mod 2 Mod 3 Baseline Mod 1 Mod 2 Mod 2 Mod 3
C+Chetn A)(+Chem B)(+Chem A) (+Chem A)(+Chem B)(+Chem A) (+Chem A)(+Chem B)(+Chem A)
Testing Method
Decontaminant O Bleach + D7 X Dahlgren
110
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Figure D4. Total recovery mass of test samples for all testing method and decontaminant combinations over all sample types for
VX on Sealant
1 500 -
3 iooo-
C/l
(/)
ro
he
"ro
¦5 500 -
I-
0 -
Baseline Mod 1 Mod 2 Mod 2 Mod 3 Baseline Mod 1 Mod 2 Mod 2 Mod 3 Baseline Mod 1 Mod 2 Mod 2 Mod 3
C+Chem A)(+Chem B)(+Chem A) (+Chem A)(+Chem B)(+Chem A) (+Chem A)(+Chem B)(+Chem A)
Testing Method
Decontaminant O Bleach + D7 X Dahlgren
SampleType = Coupon
SampleType = SPE
SampleType = Wipe
X
±* o*
8¥ °
0 § 0 X
@ + ^ ODX (ED OED X
OO
OO O
111
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Table D9. Sorted Arithmetic Means and Unadjusted 95% Confidence Intervals (HD-Paint)
Agent
Material
Sample
Type
Test
Method
Decontaminant
Mean Total
Mass
Recovery
(fig)
Lower 95%
Confidence
Bound
Upper 95%
Confidence
Bound
HD
Paint
Wipe
Baseline
Bleach
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Table D10. Sorted Arithmetic Means and Unadjusted 95% Confidence Intervals (HD-Sealant)
Agent
Material
Sample
Type
Test
Method
Decontaminant
Mean Total
Mass
Recovery
(fig)
Lower 95%
Confidence
Bound
Upper 95%
Confidence
Bound
HD
Sealant
Wipe
Mod 1
Bleach
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Table Dll. Sorted Arithmetic Means and Unadjusted 95% Confidence Intervals (VX-Paint)
Agent
Material
Sample
Type
Test
Method
Decontaminant
Mean Total
Mass
Recovery
(Mg)
Lower 95%
Confidence
Bound
Upper 95%
Confidence
Bound
VX
Paint
Wipe
Mod 1
Bleach
14.7
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Table D12. Sorted Arithmetic Means and Unadjusted 95% Confidence Intervals (VX-Sealant)
Agent
Material
Sample
Type
Test
Method
Decontaminant
Mean Total
Mass
Recovery
(fig)
Lower 95%
Confidence
Bound
Upper 95%
Confidence
Bound
VX
Sealant
Wipe
Mod 1
Bleach
0.0049
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Table D15 to Table D92 display the results of the Bonferroni-Holm-adjusted pairwise
comparisons for the specified comparisons between the sample test conditions. Of the 168
pairwise comparisons between agent/material/sample type condition combinations, 51 were
statistically significant.
The capital letters in the "Similarity Designation" column of Table D15 to Table D92 indicate
the statistical similarity of the mean total mass of a given testing method and decontaminant
combination to that of all other combinations tested for the given agent/material/sample type
condition. All rows with the same similarity designation value are not statistically significantly
different from each other, while rows that did not share any similarity designation values are
significantly different. For example, in Table D15 for the HD/Paint/Wipe condition, the baseline
method with the bleach decontaminant has similarity designation A, indicating that it is similar
to other combinations with the A designation, including Mod 1 with bleach (designation A), but
it is different from combinations without an A in the designation, such as Mod 2 with bleach
(designation C).
The results of the test sample comparisons are summarized below.
Bleach comparisons:
• Bleach Mod 1 paint wipe samples resulted in lower HD values (lower HD recovery)
compared to Mod 2 with Chem A and Mod 2 with Chem B. Note that bleach Mod 1 was
not different from Baseline for HD paint wipes.
• Bleach Mod 1 sealant wipe samples resulted in lower HD values compared to Mod 2 with
Chem A and Mod 2 with Chem B. Note that bleach Mod 1 was not different from
Baseline for HD sealant wipes.
• Bleach Mod 1 paint wipe resulted in lower VX values than Baseline, Mod 2 with Chem
A and Mod 2 with Chem B.
• Bleach Mod 1 sealant wipe samples resulted in lower VX values compared to Mod 2 with
Chem A and Mod 2 with Chem B. Note that bleach Mod 1 was not different from
Baseline for VX sealant wipes.
Dahlgren Decon comparisons and D7 comparisons:
• Mod 1 with D7 typically did not result in improved HD decontamination compared to
Baseline for any material/sample type.
• Mod 3 with Dahlgren typically did not result in improved VX decontamination compared
to Baseline for any material/sample type.
Baseline comparisons:
• Across all material and sample types, bleach resulted in the greatest number of
significantly lower HD and VX recoveries (6 out of 36 comparisons).
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Modification 1 comparisons:
• Most Mod 1 comparisons of bleach to D7 did not have significantly different HD
recoveries across all material and sample types.
• Most Mod 1 comparisons of bleach to Dahlgren did not have significantly different VX
recoveries across all material and sample types.
Modification 2 comparisons:
• Most comparisons were not significantly different. Lower HD and VX recoveries
occurred only for wipe samples.
• Where differences did exist, there was no clear pattern as to whether Chem A or Chem B
provided improved decontamination results.
Chemical A comparisons:
• Most comparisons were not significantly different. Where differences did exist, there was
no clear pattern as to whether bleach or Dahlgren Decon provided improved
decontamination.
Table D93 to Table D104 display the results of the Bonferroni-Holm-adjusted pairwise
comparisons between the test samples and positive controls. A summary of these results showing
the significant differences for the 8 comparisons between test samples to positive controls for
each agent/material/sample combination is shown in Table D13. All the HD paint and sealant
wipe differences occurred for Baseline and Mod 1 tests while all the HD paint and sealant
extracted coupon differences occurred for Mod 1, Mod 2, and Mod 3. In all cases, the difference
was due to the test samples being less than the positive controls. Relative to the positive controls,
Mod 1 with D7 resulted in significantly lower HD levels on the surface of paint and sealant films
and within the extracted coupons of paint and sealant films. Relative to the positive controls,
Mod 1 with bleach resulted in significantly lower HD levels on the surface of paint films and
within the extracted coupon of paint and sealant films. All the VX paint wipe differences
occurred for Modification 1 and all of the VX sealant wipe and extracted coupon differences
occurred for Baseline and Modification 1.
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Table D13. Summary of Test Sample to Positive Control Comparisons
Chemical
Material
Wipe
Extracted
Coupon
SPE
HD
Paint
5 differences
5 differences
No differences
Sealant
2 differences
4 differences
No differences
VX
Paint
2 differences
1 difference
1 difference
Sealant
5 differences
4 differences
No differences
Table D105 to Table D116 display the results of the Bonferroni-Holm-adjusted pairwise
comparisons between the positive control conditions. A summary of these results showing
significant differences for the 36 comparisons between positive controls for each agent/material
/sample combination is shown in Table D14. Wipe differences were driven primarily by
comparison of positive controls that included Chemical A or B (where rinse results were added
to wipe results) to the positive controls that did not include Chemical A or B, indicating an effect
of Chemical A or B in combination with water rinse on the positive controls. The HD sealant and
VX paint extracted coupon differences were associated primarily with comparisons to the Fate
and Transport Data; the reason for these differences is not apparent. Of particular note are the
large number of differences for the VX sealant extracted coupons. These differences may be
driven by variable permeation of VX into the sealant extracted coupon, with deeper permeation
leading to lower extraction recoveries.
Table D14. Summary of Positive Control Comparisons
Chemical
Material
Wipe
Extracted
Coupon
SPE
HD
Paint
7 differences
No differences
1 Difference
Sealant
17 differences
6 differences
1 Difference
VX
Paint
10 differences
8 differences
No differences
Sealant
20 differences
27 differences
No differences
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Table D15. Multiple comparison adjusted p-values between test method for bleach (HD on Paint Coupon Surfaces)
Summary of
Significant
Bonferroni-Holm
Differences
Base < Mod 2A
Base < Mod2B
Mod 1 < Mod 2A
Mod 1 < Mod 2B
Mod 2A< Mod 2B
Mean Total
Bleach
Agent
Material
Sample
Type
Decontaminants
Mass
Recovery
(^g) '
Testing
Method
Similarity
Designation
Mod 1
Mod 2
(Chem A)
Mod 2
(Chem B)
HD
Paint
Wipe
Bleach
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Table D17. Multiple comparison adjustedp-values between test method for bleach (HD in SPE Disks)
Sample
Type
Mean Total
Mass
Recovery
(**g) "
Testing
Method
Similarity
Designation
Bleach
Summary of
Significant
Agent
Material
Decontaminants
Mod 1
Mod 2
(Chem A)
Mod 2
(Chem B)
Bonferroni-
Holm
Differences
HD
Paint
SPE
Bleach
1030
Baseline
A
1.0000
1.0000
1.0000
HD
Paint
SPE
Bleach
1174
Mod 1
A
0.9566
0.9019
No significant
HD
Paint
SPE
Bleach + Chem A
1004
Mod 2
A
1.0000
differences.
HD
Paint
SPE
Bleach + Chem B
998
Mod 2
A
Table D18. Multiple comparison adjusted p-values between test methods for bleach (HD on Sealant Coupon Surfaces)
Agent Material
HD
HD
HD
HD
Sealant
Sealant
Sealant
Sealant
Sample
Type
Wipe
Wipe
Wipe
Wipe
Mean Total
Mass
Recovery
(**g) "
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Table D19. Multiple comparison adjusted p-values between test methods for bleach (HD in Sealant Coupons)
Mean Total
Bleach
Summary of
Significant
Bonferroni-
Holm
Differences
Agent
Material
Sample
Type
Mass
Recovery
(Hg) "
Decontaminants
Testing
Method
Similarity
Designation
Mod 1
Mod 2
(Chem A)
Mod 2
(Chem B)
HD
Sealant
Extracted
Coupon
188
Bleach
Baseline
A
0.3549
0.0048
0.2883
HD
Sealant
Extracted
Coupon
134
Bleach
Mod 1
AB
0.2382
0.8529
Mod 2A <
HD
Sealant
Extracted
Coupon
68.2
Bleach + Chem A
Mod 2
B
0.3549
Baseline
HD
Sealant
Extracted
Coupon
126
Bleach + Chem B
Mod 2
AB
Table D20. Multiple comparison adjusted p-values between test methods for bleach (HD in SPE Disks)
Sample
Type
Mean Total
Mass
Recovery
(Hg) "
Testing
Method
Similarity
Designation
Bleach
Summary of
Significant
Agent
Material
Decontaminants
Mod 1
Mod 2
(Chem A)
Mod 2
(Chem B)
Bonferroni-
Holm
Differences
HD
Sealant
SPE
1136
Bleach
Baseline
A
0.8229
1.0000
1.0000
HD
Sealant
SPE
1307
Bleach
Mod 1
A
0.7945
0.2470
No significant
HD
Sealant
SPE
1130
Bleach + Chem A
Mod 2
A
1.0000
differences.
HD
Sealant
SPE
1075
Bleach + Chem B
Mod 2
A
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Table D21. Multiple comparison adjusted p-values between test methods for bleach (VX on Paint Coupon Surfaces)
Agent Material Sample Decontaminants
Type
VX
VX
VX
VX
Paint
Paint
Paint
Paint
Wipe
Wipe
Wipe
Wipe
Bleach
Bleach
Bleach + Chem A
Bleach + Chem B
Mean Total
Mass
Recovery
(Hg) "
141
14.7
353
175
Testing
Method
Baseline
Similarity
Designation
Mod 1
Mod 2
Mod 2
B
C
Mod 1
Bleach
Mod 2
(Chem A)
Mod 2
(Chem B)
Summary of
Significant
Bonferroni-Holm
Differences
Base < Mod 2 A
Mod 1 < Base
Mod 1 < Mod 2A
Mod 1 < Mod 2B
Mod 2B< Mod 2A
Table D22. Multiple comparison adjusted p-values between test methods for bleach (VX in Paint Coupons)
Agent Material
VX
VX
VX
VX
Paint
Paint
Paint
Paint
Sample
Type
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Decontaminants
Bleach
Bleach
Bleach + Chem
A
Bleach + Chem
B
Mean Total
Mass
Recovery
(Hg) "
230
157
121
83.S
Testing
Method
Baseline
Similarity
Designation
Mod 1
Mod 2
Mod 2
Mod 1
Bleach
Mod 2
(Chem A)
Mod 2
(Chem B)
Summary of
Significant
Bonferroni-
Holm
Differences
No significant
differences.
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Table D23. Multiple comparison adjusted p-values between test methods for bleach (VX in SPE Disks)
Table D24. Multiple comparison adjusted p-values between test methods for bleach (VX on Sealant Coupon Surfaces)
Sample
Mean Total
Mass
Testing
Similarity
Bleach
Summary of
Significant
Agent
Material
Type
Decontaminants
Recovery
(^g) "
Method
Designation
Mod 1
Mod 2
(Chem A)
Mod 2
(Chem B)
Bonferroni-Holm
Differences
VX
Sealant
Wipe
Bleach
1.14
Baseline
A
1.0000
<0.0001
<0.0001
Base < Mod 2 A
Base < Mod 2B
VX
Sealant
Wipe
Bleach
0.0049
Mod 1
A
<0.0001
<0.0001
VX
Sealant
Wipe
Bleach + Chem A
364
Mod 2
B
0.4798
Mod 1 < Mod 2A
Mod 1 < Mod 2B
VX
Sealant
Wipe
Bleach + Chem B
294
Mod 2
B
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D25. Multiple comparison adjustedp-values between test methods for bleach (VX in Sealant Coupons)
Agent
Material
Sample
Type
Decontaminants
Mean Total
Mass
Recovery
(^g) "
Testing
Method
Similarity
Designation
VX
Sealant
Extracted
Coupon
Bleach
417
Baseline
AB
VX
Sealant
Extracted
Coupon
Bleach
513
Mod 1
A
VX
Sealant
Extracted
Coupon
Bleach + Chem A
247
Mod 2
C
VX
Sealant
Extracted
Coupon
Bleach + Chem B
327
Mod 2
BC
Mod 1
Bleach
Mod 2
(Chem A)
Mod 2
(Chem B)
Mod 2A < Base
Mod 2 A < Mod
1
Mod 2B < Mod
1
Table D26. Multiple comparison adjusted p-values between test methods for bleach (VX in SPE Disks)
Sample
Type
Mean
Total
Testing
Method
Similarity
Designation
Bleach
Summary of
Significant
Agent
Material
Decontaminants
Mass
Recovery
(us)
Mod 1
Mod 2
(Chem A)
Mod 2
(Chem B)
Bonferroni-
Holm
Differences
VX
Sealant
SPE
Bleach
9.92
Baseline
A
1.0000
1.0000
1.0000
VX
Sealant
SPE
Bleach
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D27. Multiple comparison adjusted p-values between test methods for Dahlgren Decon (HD on Paint Wipes)
Agent
Material
Sample
Type
Decontaminants
Mean Total
Mass
Recovery
(Mg)
Testing
Method
Similarity
Designation
Dahlsren Decon +
Chem A
Mod 3
Summary of
Significant
Bonferroni-Holm
Differences
HD
Paint
Wipe
Dahlgren Decon
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D30. Multiple comparison adjustedp-values between test methods for Dahlgren Decon (HD on Sealant Coupon Surfaces)
Agent
Material
Sample
Type
Decontaminants
Mean Total
Mass
Recovery
(Mg)
Testing
Method
Similarity
Designation
Dahlsren Decon +
Chem A
Mod 3
Summary of
Significant
Bonferroni-Holm
Differences
HD
Sealant
Wipe
Dahlgren Decon
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D33. Multiple comparison adjustedp-values between testing methods for Dahlgren Decon (VX on Paint Coupon Surfaces)
Agent
Material
Sample
Type
Decontaminant
Mean Total
Mass
Recovery
(fig)
Testing
Method
Similarity
Designation
VX
Paint
Wipe
Dahlgren Decon
46.4
Baseline
A
VX
Paint
Wipe
Dahlgren Decon
18.1
Mod 1
A
VX
Paint
Wipe
Dahlgren Decon +
Chem A
250
Mod 3
B
Dahlgren Decon
Mod 1
Mod 3
(Chem A)
Summary of
Significant
Bonferroni-Holm
Differences
Baseline < Mod 3
Mod 1 < Mod 3
Table D34. Multiple comparison adjusted p-values between testing methods for Dahlgren Decon (VX in Paint Coupons)
Summary of
Significant
Bonferroni-Holm
Differences
Agent
Material
Sample
Type
Decontaminant
Mean Total
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
VX
Paint
Extracted
Coupon
Dahlgren Decon
230
Baseline
A
VX
Paint
Extracted
Coupon
Dahlgren Decon
201
Mod 1
A
VX
Paint
Extracted
Coupon
Dahlgren Decon +
Chem A
80.0
Mod 3
A
Dahlgren Decon
Mod 1
Mod 3
(Chem A)
1.0000
0.0530
0.1767
No significant
differences.
Table D35. Multiple comparison adjusted p-values between testing methods for Dahlgren Decon (VX in SPE Disks)
Summary of
Significant
Bonferroni-Holm
Differences
Agent
Material
Sample
Type
Decontaminant
Mean Total
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
VX
Paint
SPE
Dahlgren Decon
317
Baseline
A
VX
Paint
SPE
Dahlgren Decon
273
Mod 1
A
VX
Paint
SPE
Dahlgren Decon +
Chem A
233
Mod 3
A
Dahlgren Decon
Mod 1
Mod 3
(Chem A)
1.0000
0.4837
1.0000
No significant
differences.
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D36. Multiple comparison adjustedp-values between testing methods for Dahlgren Decon (VX on Sealant Coupon Surfaces)
Summary of
Significant
Bonferroni-Holm
Differences
Baseline < Mod 3
Mod 1 < Mod 3
Agent
Material
Sample
Type
Decontaminant
Mean Total
Mass
Recovery
(fig)
Testing
Method
Similarity
Designation
VX
Sealant
Wipe
Dahlgren Decon
0.97
Baseline
A
VX
Sealant
Wipe
Dahlgren Decon
0.37
Mod 1
A
VX
Sealant
Wipe
Dahlgren + Chem A
524
Mod 3
B
Dahlgren Decon
Mod 1
Mod 3
(Chem A)
1.0000
<0.0001
<0.0001
Table D3 7. Multiple comparison adjusted p-values between testing methods for Dahlgren Decon (VX in Sealant Coupons)
Summary of
Significant
Bonferroni-Holm
Differences
Agent
Material
Sample
Type
Decontaminant
Mean Total
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
VX
Sealant
Extracted
Coupon
Dahlgren Decon
730
Baseline
A
VX
Sealant
Extracted
Coupon
Dahlgren Decon
683
Mod 1
A
VX
Sealant
Extracted
Coupon
Dahlgren + Chem
A
251
Mod 3
B
Dahlgren Decon
n/r i 1 Mod •
Mod 1
Mod 3
(Chem A)
Mod 3 < Base
Mod 3 < Mod 1
Table D38. Multiple comparison adjusted p-values between testing methods for Dahlgren Decon (VX in SPE Disks)
Agent Material Sample Decontaminant
Type
Mean Total
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
Dahlgren Decon
ivr i 1 Mod *
Mod 1
Mod 3
(Chem A)
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
SPE
Dahlgren Decon
23.3
Baseline
A
1.0000
1.0000
No significant
differences.
VX
Sealant
SPE
Dahlgren Decon
5.65
Mod 1
A
1.0000
VX
Sealant
SPE
Dahlgren Decon +
Chem A
3.28
Mod 3
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D39. Multiple comparison adjustedp-values between testing methods for D7 (HD on Paint Wipes)
Agent
Material
Sample
Type
Decontaminants
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
D7
Modi
Summary of
Significant
Bonferroni-
Holm
Differences
HD
Paint
Wipe
D7
2.18
Baseline
A
0.4851
No significant
differences.
HD
Paint
Wipe
D7
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D42. Multiple comparison adjustedp-values between testing methods for D7 (HD on Sealant Wipes)
Agent
Material
Sample
Type
Decontaminants
Mean
Total
Mass
Recovery
fog)
Testing
Method
Similarity
Designation
D7
Mod 1
Summary of
Significant
Bonferroni-
Holm
Differences
HD
Sealant
Wipe
D7
2.96
Baseline
A
0.1696
No significant
differences.
HD
Sealant
Wipe
D7
3.78
Mod 1
A
Table D43. Multiple comparison adjusted p-values between testing methods for D7 (HD in Sealant Coupons)
Agent
Material
Sample
Type
Decontaminants
Mean
Total
Mass
Recovery
(M)
Testing
Method
Similarity
Designation
1)2
Modi
Summary of
Significant
Bonferroni-
Holm
Differences
HD
Sealant
Extracted
Coupon
D7
266
Baseline
A
0.0486
Mod 1 < Base
HD
Sealant
Extracted
Coupon
D7
176
Mod 1
B
Table D44. Multiple comparison adjusted p-values between testing methods for D7 (HD in SPE Disks)
Agent
Material
Sample
Type
Decontaminants
Mean
Total
Mass
Recovery
(M)
Testing
Method
Similarity
Designation
1)2
Modi
Summary of
Significant
Bonferroni-
Holm
Differences
HD
Sealant
SPE
D7
1050
Baseline
A
1.0000
No significant
HD
Sealant
SPE
D7
1210
Mod 1
A
differences.
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D45. Multiple comparison adjusted p-values between decontaminants for Baseline method (HD on Paint Coupon Surfaces)
Agent Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Baseline
Dahlgren
Summary of
Significant
Bonferroni-Holm
Differences
HD
Paint
Wipe
Baseline
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D48. Multiple comparison adjustedp-values between decontaminants for Baseline method (HD on Sealant Coupon
Surfaces)
Summary of
Significant
Bonferroni-Holm
Differences
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
HD
Sealant
Wipe
Baseline
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D51. Multiple comparison adjusted p-values between decontaminants for Baseline method (VX on Paint Coupon Surfaces)
Agent Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Baseline
Dahlgren
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
Wipe
Baseline
141
Bleach
A
0.0086
0.0007
D7 < Bleach
Dahlgren Decon <
Bleach
VX
Paint
Wipe
Baseline
70.3
D7
B
0.4472
VX
Paint
Wipe
Baseline
46.4
Dahlgren Decon
B
Table D52. Multiple comparison adjusted p-values between decontaminants for Baseline method (VX in Paint Coupons)
Agent Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Baseline
Dahlgren
Decon
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
Extracted
Coupon
Baseline
229
Bleach
A
1.0000
1.0000
VX
Paint
Extracted
Coupon
Baseline
187
D7
A
1.0000
No significant
differences.
VX
Paint
Extracted
Coupon
Baseline
230
Dahlgren
A
Table D53. Multiple comparison adjusted p-values between decontaminants for Baseline method (VX in SPE Disks)
Agent Material
VX
VX
VX
Paint
Paint
Paint
Sample
Type
SPE
SPE
SPE
Testing
Method
Baseline
Baseline
Baseline
Mean Total
Mass
Recovery
(MS)
148
326
317
Decontaminant
Bleach
D7
Similarity
Designation
Dahlgren Decon
B
B
Baseline
Dahlgren
Decon
Summary of
Significant
Bonferroni-Holm
Differences
Bleach < D7
Bleach < Dahlgren
Decon
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D54. Multiple comparison adjustedp-values between decontaminants for Baseline method (VX on Sealant Wipes)
Agent Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Baseline
Dahlgren
Decon
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
Wipe
Baseline
1.14
Bleach
A
1.0000
1.0000
VX
Sealant
Wipe
Baseline
42.1
D7
A
1.0000
No significant
differences.
VX
Sealant
Wipe
Baseline
0.97
Dahlgren
A
Table D55. Multiple comparison adjusted p-values between decontaminants for Baseline method (VX in Sealant Coupons)
Agent Material
VX
VX
VX
Sealant
Sealant
Sealant
Sample
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Testing
Method
Baseline
Baseline
Baseline
Mean Total
Mass
Recovery
(MS)
417
572
730
Decontaminant
Bleach
D7
Similarity
Designation
Dahlgren Decon
B
C
Baseline
0.0324
Dahlgren
Decon
<0.0001
0.0324
Summary of
Significant
Bonferroni-Holm
Differences
Bleach < D7
Bleach < Dahlgren
Decon
D7 < Dahlgren
Decon
Table D56. Multiple comparison adjusted p-values between decontaminants for Baseline method (VX in SPE Disks)
Agent Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Baseline
Dahlgren
Decon
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
SPE
Baseline
9.92
Bleach
A
1.0000
1.0000
VX
Sealant
SPE
Baseline
15.3
D7
A
1.0000
No significant
differences.
VX
Sealant
SPE
Baseline
23.3
Dahlgren Decon
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D57. Multiple comparison adjusted p-values between decontaminants for Mod 1 method (HD on Paint Wipes)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Mod 1
D7
Summary of
Significant
Bonferroni-Holm
Differences
HD
Paint
Wipe
Mod 1
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D60. Multiple comparison adjusted p-values between decontaminants for Mod 1 method (HD on Sealant Surfaces)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Mod 1
D7
Summary of
Significant
Bonferroni-Holm
Differences
HD
Sealant
Wipe
Mod 1
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D63. Multiple comparison adjusted p-values between decontaminants for Mod 1 method (VX on Paint Coupon Surfaces)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Mod 1
D7
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
Wipe
Mod 1
14.7
Bleach
A
0.8555
No significant
differences.
VX
Paint
Wipe
Mod 1
18.1
Dahlgren
A
Table D64. Multiple comparison adjusted p-values between decontaminants for Mod 1 method (VX in Paint Coupons)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Mod 1
D7
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
Extracted
Coupon
Mod 1
157
Bleach
A
1.0000
No significant
differences.
VX
Paint
Extracted
Coupon
Mod 1
201
Dahlgren
A
Table D65. Multiple comparison adjusted p-values between decontaminants for Mod 1 method (VX in SPE Disks)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Mod 1
D7
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
SPE
Mod 1
210
Bleach
A
1.0000
No significant
differences.
VX
Paint
SPE
Mod 1
273
Dahlgren
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D66. Multiple comparison adjustedp-values between decontaminants for Mod 1 method (VX on Sealant Wipes)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery (jug)
Decontaminant
Similarity
Designation
Mod 1
D7
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
Wipe
Mod 1
0.0049
Bleach
A
1.0000
No significant
differences.
VX
Sealant
Wipe
Mod 1
0.37
Dahlgren Decon
A
Table D67. Multiple comparison adjusted p-values between decontaminants for Mod 1 method (VX in Sealant Coupons)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Mod 1
D7
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
Extracted
Coupon
Mod 1
513
Bleach
A
0.0226
Bleach < Dahlgren
VX
Sealant
Extracted
Coupon
Mod 1
683
Dahlgren Decon
B
Table D68. Multiple comparison adjusted p-values between decontaminants for Mod 1 method (VX in SPE Disks)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Mod 1
D7
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
SPE
Mod 1
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D69. Multiple comparison adjustedp-values between decontaminants for Mod 2 method (HD on Paint Coupon Surfaces)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
HD
Paint
Wipe
Mod 2
15.3
Bleach + Chem A
A
0.0298
Mod 2A < Mod 2B
HD
Paint
Wipe
Mod 2
17.1
Bleach + Chem B
B
Table D70. Multiple comparison adjusted p-values between decontaminants for Mod 2 method (HD in Paint Coupons)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
HD
Paint
Extracted
Coupon
Mod 2
73.7
Bleach + Chem A
A
1.0000
No significant
differences.
HD
Paint
Extracted
Coupon
Mod 2
88.0
Bleach + Chem B
A
Table D71. Multiple comparison adjusted p-values between decontaminants for Mod 2 method (HD in SPE Disks)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery (pg)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
HD
Paint
SPE
Mod 2
1000
Bleach + Chem A
A
1.0000
No significant
differences.
HD
Paint
SPE
Mod 2
998
Bleach + Chem B
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D72. Multiple comparison adjusted p-values between decontaminants for Mod 2 method (HD on Sealant Surfaces)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
HD
Sealant
Wipe
Mod 2
9.15
Bleach + Chem A
A
<0.0001
Mod 2A < Mod 2B
HD
Sealant
Wipe
Mod 2
12.6
Bleach + Chem B
B
Table D73. Multiple comparison adjusted p-values between decontaminants for Mod 2 method (HD in Sealant Coupons)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
HD
Sealant
Extracted
Coupon
Mod 2
68.2
Bleach + Chem A
A
0.3549
No significant
differences.
HD
Sealant
Extracted
Coupon
Mod 2
126
Bleach + Chem B
A
Table D 74. Multiple comparison adjusted p-values between decontaminants for Mod 2 method (HD in SPE Disks)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
dig)
Decontaminant
Similarity
Designation
Mod 2
Bleach +
Chem B
Summary of
Significant
Bonferroni-
Holm
Differences
HD
Sealant
SPE
Mod 2
1130
Bleach + Chem A
A
1.0000
No significant
differences.
HD
Sealant
SPE
Mod 2
1070
Bleach + Chem B
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D75. Multiple comparison adjustedp-values between decontaminants for Mod 2 method (VX on Paint Coupon Surfaces)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
Wipe
Mod 2
353
Bleach + Chem A
A
<0.0001
Mod 2B < Mod 2A
VX
Paint
Wipe
Mod 2
175
Bleach + Chem B
B
Table D76. Multiple comparison adjusted p-values between decontaminants for Mod 2 method (VX in Paint Coupons)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
Extracted
Coupon
Mod 2
121
Bleach + Chem A
A
1.0000
No significant
differences.
VX
Paint
Extracted
Coupon
Mod 2
83.8
Bleach + Chem B
A
Table D77. Multiple comparison adjusted p-values between decontaminants for Mod 2 method (VX in SPE Disks)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
SPE
Mod 2
253
Bleach + Chem A
A
1.0000
No significant
differences.
VX
Paint
SPE
Mod 2
209
Bleach + Chem B
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D78. Multiple comparison adjustedp-values between decontaminants for Mod 2 method (VXon Sealant Coupon Surfaces)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
Wipe
Mod 2
364
Bleach + Chem A
A
0.4798
No significant
differences.
VX
Sealant
Wipe
Mod 2
294
Bleach + Chem B
A
Table D79. Multiple comparison adjusted p-values between decontaminants for Mod 2 method (VX in Sealant Coupons)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
Extracted
Coupon
Mod 2
247
Bleach + Chem A
A
0.4255
No significant
differences.
VX
Sealant
Extracted
Coupon
Mod 2
327
Bleach + Chem B
A
Table D80. Multiple comparison adjusted p-values between decontaminants for Mod 2 method (VX in SPE Disks)
Agent
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(fig)
Decontaminant
Similarity
Designation
Mod 2
Bleach + Chem B
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
SPE
Mod 2
2.15
Bleach + Chem A
A
1.0000
No significant
differences.
VX
Sealant
SPE
Mod 2
0.041
Bleach + Chem B
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D81. Multiple comparison adjustedp-values between decontaminants for Chem A (HD on Paint Coupon Surfaces)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
(fig)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
HD
Paint
Wipe
15.3
Mod 2
Bleach + Chem A
A
0.4851
No significant
differences.
HD
Paint
Wipe
14.2
Mod 3
Dahlgren + Chem A
A
Table D82. Multiple comparison adjusted p-values between decontaminants for Chem A (HD in Paint Coupons)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
HD
Paint
Extracted
Coupon
73.8
Mod 2
Bleach + Chem A
A
1.0000
No significant
differences.
HD
Paint
Extracted
Coupon
132
Mod 3
Dahlgren Decon +
Chem A
A
Table D83. Multiple comparison adjusted p-values between decontaminants for Chem A (HD in SPE Disks)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
(fig)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
HD
Paint
SPE
1000
Mod 2
Bleach + Chem A
A
1.0000
No significant
differences.
HD
Paint
SPE
1060
Mod 3
Dahlgren Decon +
Chem A
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D84. Multiple comparison adjusted p-values between decontaminants for Chem A (HD on Sealant Coupon Surfaces)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
dig)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
HD
Sealant
Wipe
9.15
Mod 2
Bleach + Chem A
A
0.0182
Bleach < Dahlgren
Decon
HD
Sealant
Wipe
10.5
Mod 3
Dahlgren Decon +
Chem A
B
Table D85. Multiple comparison adjusted p-values between decontaminants for Chem A (HD in Sealant Coupons)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
HD
Sealant
Extracted
Coupon
68.2
Mod 2
Bleach + Chem A
A
0.0565
No significant
differences.
HD
Sealant
Extracted
Coupon
155
Mod 3
Dahlgren Decon +
Chem A
A
Table D86. Multiple comparison adjusted p-values between decontaminants for Chem A (HD in SPE Disks)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
HD
Sealant
SPE
1130
Mod 2
Bleach + Chem A
A
1.0000
No significant
differences.
HD
Sealant
SPE
1140
Mod 3
Dahlgren Decon +
Chem A
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D87. Multiple comparison adjustedp-values between decontaminants for Chem A (VX on Paint Coupon Surfaces)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
dig)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
Wipe
353
Mod 2
Bleach + Chem A
A
0.0003
Dahlgren Decon <
Bleach
VX
Paint
Wipe
250
Mod 3
Dahlgren Decon +
Chem A
B
Table D88. Multiple comparison adjusted p-values between decontaminants for Chem A (VX in Paint Coupons)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
Extracted
Coupon
121
Mod 2
Bleach + Chem A
A
1.0000
No significant
differences.
VX
Paint
Extracted
Coupon
80.0
Mod 3
Dahlgren Decon +
Chem A
A
Table D89. Multiple comparison adjusted p-values between decontaminants for Chem A (VX in SPE Disks)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
SPE
253
Mod 2
Bleach + Chem A
A
1.0000
No significant
differences.
VX
Paint
SPE
233
Mod 3
Dahlgren Decon +
Chem A
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D90. Multiple comparison adjusted p-values between decontaminants for Chem A (VX on Sealant Coupon Surfaces)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
(fig)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren + Chem
A
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
Wipe
364
Mod 2
Bleach + Chem A
A
0.0027
Bleach < Dahlgren
Decon
VX
Sealant
Wipe
524
Mod 3
Dahlgren Decon +
Chem A
B
Table D91. Multiple comparison adjusted p-values between decontaminants for Chem A (VX in Sealant Coupons)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery (pg)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
Extracted
Coupon
247
Mod 2
Bleach + Chem A
A
0.9311
No significant
differences.
VX
Sealant
Extracted
Coupon
251
Mod 3
Dahlgren Decon +
Chem A
A
Table D92. Multiple comparison adjusted p-values between decontaminants for Chem A (VX in SPE Disks)
Agent
Material
Sample
Type
Mean Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Similarity
Designation
Mod 3
Dahlgren Decon +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
VX
Sealant
SPE
2.15
Mod 2
Bleach + Chem A
A
1.0000
No significant
differences.
VX
Sealant
SPE
3.28
Mod 3
Dahlgren Decon +
Chem A
A
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Positive Control Results: Within-Test Comparisons
Table D93. Multiple comparison adjusted p-values for between decontaminants and positive
controls with testing methods (HD on Paint Coupon Surfaces)
Agent
Material
Sample
Type
Mean
Total
Mass
Recovery
(US)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
HD
Paint
Wipe
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D94. Multiple comparison adjusted p-values for between decontaminants and positive
controls with testing methods (HD in Paint Coupons)
Agent
Material
Sample
Type
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test
Direction
HD
Paint
Extracted
Coupon
109
Baseline
Bleach
0.0775
No significant
differences.
HD
Paint
Extracted
Coupon
235
Baseline
D7
0.5798
No significant
differences.
HD
Paint
Extracted
Coupon
308
Baseline
Dahlgren Decon
0.8316
No significant
differences.
HD
Paint
Extracted
Coupon
325
Baseline
Positive
Control
HD
Paint
Extracted
Coupon
46.6
Mod 1
Bleach
<0.0001
Bleach < PC
HD
Paint
Extracted
Coupon
82.4
Mod 1
D7
<0.0001
Mod 1 < PC
HD
Paint
Extracted
Coupon
467
Mod 1
Positive
Control
HD
Paint
Extracted
Coupon
73.7
Mod 2 +
Chem A
Bleach +
Chem A
0.0310
Mod 2 A < PC
HD
Paint
Extracted
Coupon
308
Mod 2 +
Chem A
Positive
Control
HD
Paint
Extracted
Coupon
88.0
Mod 2 +
Chem B
Bleach +
Chem B
0.0068
Mod 2B < PC
HD
Paint
Extracted
Coupon
383
Mod 2 +
Chem B
Positive
Control
HD
Paint
Extracted
Coupon
132
Mod 3 +
Chem A
Dahlgren +
Chem A
0.0271
Mod 3A < PC
HD
Paint
Extracted
Coupon
366
Mod 3 +
Chem A
Positive
Control
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D95. Multiple comparison adjusted p-values between decontaminants and positive
Agent
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
controls with testing methods (HD in SPE Disks)
Material
Paint
Sample
Type
SPE
Mean
Total
Mass
Recovery
0*8)
1030
Testing
Method
Baseline
Decontaminant
Bleach
Comparison
vs.
Positive
Control (PC)
0.6495
Test
Direction
No significant
differences.
Paint
SPE
1030
Baseline
D7
0.6495
No significant
differences.
Paint
SPE
1010
Baseline
Dahlgren Decon
0.6495
Paint
SPE
881
Baseline
Positive
Control
Paint
SPE
1170
Mod 1
Bleach
1.0000
No significant
differences.
No significant
differences.
Paint
SPE
1120
Mod 1
D7
Paint
SPE
1140
Mod 1
Positive
Control
Paint
SPE
1000
Mod 2 +
Chem A
Bleach +
Chem A
Paint
SPE
1190
Mod 2 +
Chem A
Positive
Control
Paint
SPE
997
Mod 2 +
Chem B
Bleach +
Chem B
Paint
SPE
1090
Mod 2 +
Chem B
Positive
Control
Paint
SPE
1060
Mod 3 +
Chem A
Dahlgren +
Chem A
Paint
SPE
1140
Mod 3 +
Chem A
Positive
Control
1.0000
No significant
differences.
No significant
differences.
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D96. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (HD on Sealant Coupon Surfaces)
Agent
Material
Sample
Type
Mean
Total
Mass
Recovery
0*8)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test
Direction
HD
Sealant
Wipe
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D97. Multiple comparison adjusted p-values between decontaminants and positive
Agent
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
controls with testing methods (HD in Sealant Coupons)
Material
Sealant
Sample
Type
Extracted
Coupon
Mean
Total
Mass
Recovery
(MS)
1878
Testing
Method
Baseline
Decontaminant
Bleach
Comparison
vs.
Positive
Control (PC)
1.0000
Test
Direction
No significant
differences.
Sealant
Extracted
Coupon
266
Baseline
D7
0.2799
No significant
differences.
Sealant
Extracted
Coupon
209
Baseline
Dahlgren Decon
1.0000
No significant
differences.
Sealant
Extracted
Coupon
188
Baseline
Positive
Control
Sealant
Extracted
Coupon
134
Mod 1
Bleach
Sealant
Extracted
Coupon
176
Mod 1
D7
Sealant
Extracted
Coupon
250
Mod 1
Positive
Control
Sealant
Extracted
Coupon
68.2
Mod 2 +
Chem A
Bleach +
Chem A
Sealant
Extracted
Coupon
207
Mod 2 +
Chem A
Positive
Control
Sealant
Extracted
Coupon
126
Mod 2 +
Chem B
Bleach +
Chem B
Sealant
Extracted
Coupon
201
Mod 2 +
Chem B
Positive
Control
Sealant
Extracted
Coupon
155
Mod 3 +
Chem A
Dahlgren +
Chem A
Sealant
Extracted
Coupon
203
Mod 3 +
Chem A
Positive
Control
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D98. Multiple comparison adjusted p-values between decontaminants and positive
Agent
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
HD
controls with testing methods (HD in SPE Disks)
Material
Sealant
Sample
Type
SPE
Mean
Total
Mass
Recovery
0*8)
1140
Testing
Method
Baseline
Decontaminant
Bleach
Comparison
vs.
Positive
Control (PC)
1.0000
Test
Direction
No significant
differences.
Sealant
SPE
1050
Baseline
D7
1.0000
No significant
differences.
Sealant
Sealant
Sealant
SPE
1130
Baseline
Dahlgren Decon
1.0000
SPE
1070
Baseline
Positive
Control
SPE
1310
Mod 1
Bleach
0.1714
No significant
differences.
No significant
differences.
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
SPE
1210
Mod 1
D7
SPE
1100
Mod 1
Positive
Control
SPE
1130
Mod 2 +
Chem A
Bleach +
Chem A
SPE
1130
Mod 2 +
Chem A
Positive
Control
SPE
1070
Mod 2 +
Chem B
Bleach +
Chem B
SPE
1040
Mod 2 +
Chem B
Positive
Control
SPE
1140
Mod 3 +
Chem A
Dahlgren +
Chem A
SPE
1090
Mod 3 +
Chem A
Positive
Control
0.3073
No significant
differences.
No significant
differences.
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D99. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (VX on Paint Coupon Surfaces)
Agent
Material
Sample
Type
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
VX
Paint
Wipe
141
Baseline
Bleach
0.2001
No significant
differences.
VX
Paint
Wipe
70.4
Baseline
D7
0.3700
No significant
differences.
VX
Paint
Wipe
46.4
Baseline
Dahlgren Decon
0.2001
No significant
differences.
VX
Paint
Wipe
92.1
Baseline
Positive
Control
VX
Paint
Wipe
14.7
Mod 1
Bleach
0.0002
Bleach < PC
VX
Paint
Wipe
18.1
Mod 1
Dahlgren Decon
0.0002
Dahlgren < PC
VX
Paint
Wipe
87.9
Mod 1
Positive
Control
VX
Paint
Wipe
353
Mod 2 +
Chem A
Bleach +
Chem A
0.9140
No significant
differences.
Mod 2 +
Chem A
Positive
Control
VX
Paint
Wipe
357
VX
Paint
Wipe
175
Mod 2 +
Chem B
Bleach +
Chem B
0.2322
No significant
differences.
VX
Paint
Wipe
148
Mod 2 +
Positive
Chem B
Control
VX
Paint
Wipe
250
Mod 3 +
Chem A
Dahlgren Decon
+ Chem A
0.4855
No significant
differences.
VX
Paint
Wipe
270
Mod 3 +
Chem A
Positive
Control
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D100. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (VX in Paint Coupons)
Agent
Material
Sample
Type
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test
Direction
VX
Paint
Extracted
Coupon
230
Baseline
Bleach
0.2725
No significant
differences.
VX
Paint
Extracted
Coupon
187
Baseline
D7
0.0772
No significant
differences.
VX
Paint
Extracted
Coupon
230
Baseline
Dahlgren Decon
0.2725
No significant
differences.
VX
Paint
Extracted
Coupon
295
Baseline
Positive
Control
VX
Paint
Extracted
Coupon
157
Mod 1
Bleach
0.0387
Bleach < PC
VX
Paint
Extracted
Coupon
201
Mod 1
Dahlgren Decon
0.1299
No significant
differences.
VX
Paint
Extracted
Coupon
256
Mod 1
Positive
Control
VX
Paint
Extracted
Coupon
121
Mod 2 +
Chem A
Bleach +
Chem A
0.0631
No significant
differences.
VX
Paint
Extracted
Coupon
274
Mod 2 +
Chem A
Positive
Control
VX
Paint
Extracted
Coupon
83.8
Mod 2 +
Chem B
Bleach +
Chem B
0.0593
No significant
differences.
VX
Paint
Extracted
Coupon
148
Mod 2 +
Chem B
Positive
Control
VX
Paint
Extracted
Coupon
80.0
Mod 3 +
Chem A
Dahlgren +
Chem A
0.3353
No significant
differences.
VX
Paint
Extracted
Coupon
109
Mod 3 +
Chem A
Positive
Control
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D101. Multiple comparison adjusted p-values between decontaminants and positive
Agent
vx
vx
vx
vx
vx
vx
vx
vx
vx
vx
vx
vx
controls with testing methods (VX in SPE Disks)
Material
Paint
Sample
Type
SPE
Mean
Total
Mass
Recovery
(US)
148
Testing
Method
Baseline
Decontaminant
Bleach
Comparison
vs.
Positive
Control (PC)
0.3412
Test
Direction
No significant
differences.
Paint
SPE
326
Baseline
D7
0.3412
No significant
differences.
Paint
SPE
Paint
SPE
Paint
SPE
317
Baseline
Dahlgren Decon
0.3412
233
Baseline
Positive
Control
210
Mod 1
Bleach
No significant
differences.
No significant
differences.
Paint
SPE
Paint
SPE
Paint
SPE
Paint
SPE
Paint
SPE
Paint
SPE
Paint
SPE
Paint
SPE
273
Mod 1
Dahlgren Decon
277
Mod 1
Positive
Control
253
Mod 2 +
Chem A
Bleach +
Chem A
350
Mod 2 +
Chem A
Positive
Control
209
Mod 2 +
Chem B
Bleach +
Chem B
169
Mod 2 +
Chem B
Positive
Control
233
Mod 3 +
Chem A
Dahlgren +
Chem A
202
Mod 3 +
Chem A
Positive
Control
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D102. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (VX on Sealant Coupon Surfaces)
Mean Total
Comparison
Agent
Material
Sample
Type
Mass
Recovery
(M)
Testing
Method
Decontaminant
vs.
Positive
Control (PC)
Test Direction
VX
Sealant
Wipe
1.14
Baseline
Bleach
<0.0001
Bleach < PC
VX
Sealant
Wipe
42.1
Baseline
D7
0.0005
PC < D7
VX
Sealant
Wipe
0.97
Baseline
Dahlgren Decon
<0.0001
Dahlgren < PC
VX
Sealant
Wipe
30.8
Baseline
Positive
Control
VX
Sealant
Wipe
0.0049
Mod 1
Bleach
<0.0001
Bleach < PC
VX
Sealant
Wipe
0.37
Mod 1
Dahlgren Decon
<0.0001
Dahlgren < PC
Positive
Control
VX
Sealant
Wipe
35.8
Mod 1
VX
Sealant
Wipe
364
Mod 2 +
Chem A
Bleach +
Chem A
0.5128
No significant
differences.
VX
Sealant
Wipe
416
Mod 2 +
Positive
Chem A
Control
VX
Sealant
Wipe
294
Mod 2 +
Chem B
Bleach +
Chem B
0.5841
No significant
differences.
VX
Sealant
Wipe
321
Mod 2 +
Chem B
Positive
Control
VX
Sealant
Wipe
524
Mod 3 +
Chem A
Dahlgren Decon
+ Chem A
0.5382
No significant
differences.
VX
Sealant
Wipe
505
Mod 3 +
Chem A
Positive
Control
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table D103. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (VX in Sealant Coupons)
Agent
Material
Sample
Type
Mean
Total
Mass
Recovery
0*8)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test
Direction
VX
Sealant
Extracted
Coupon
417
Baseline
Bleach
0.0003
Bleach < PC
VX
Sealant
Extracted
Coupon
572
Baseline
D7
0.0046
D7 < PC
VX
Sealant
Extracted
Coupon
730
Baseline
Dahlgren Decon
0.1466
No significant
differences.
VX
Sealant
Extracted
Coupon
821
Baseline
Positive
Control
VX
Sealant
Extracted
Coupon
513
Mod 1
Bleach
0.0003
Bleach < PC
VX
Sealant
Extracted
Coupon
683
Mod 1
Dahlgren Decon
0.0036
Dahlgren <
PC
VX
Sealant
Extracted
Coupon
893
Mod 1
Positive
Control
VX
Sealant
Extracted
Coupon
246
Mod 2 +
Chem A
Bleach +
Chem A
0.0782
No significant
differences.
VX
Sealant
Extracted
Coupon
197
Mod 2 +
Chem A
Positive
Control
VX
Sealant
Extracted
Coupon
327
Mod 2 +
Chem B
Bleach +
Chem B
0.6037
No significant
differences.
VX
Sealant
Extracted
Coupon
340
Mod 2 +
Chem B
Positive
Control
VX
Sealant
Extracted
Coupon
251
Mod 3 +
Chem A
Dahlgren Decon
+ Chem A
0.0522
No significant
differences.
VX
Sealant
Extracted
Coupon
180
Mod 3 +
Chem A
Positive
Control
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Table D104. Multiple comparison adjusted p-values between decontaminants and positive
Agent
vx
vx
vx
vx
vx
vx
vx
vx
vx
vx
vx
vx
controls with testing methods (VX in SPE Disks)
Material
Sealant
Sample
Type
SPE
Mean
Total
Mass
Recovery
0*8)
9.92
Testing
Method
Baseline
Decontaminant
Bleach
Comparison
vs.
Positive
Control (PC)
1.0000
Test
Direction
No significant
differences.
Sealant
SPE
15.3
Baseline
D7
1.0000
No significant
differences.
Sealant
Sealant
Sealant
SPE
23.3
Baseline
Dahlgren Decon
1.0000
SPE
*.74
Baseline
Positive
Control
SPE
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Positive Controls: Across-Test Method Comparisons
Table D105. Multiple comparison adjusted p-values between testing methods for positive controls (HD on Paint Coupon Surfaces)
Agent Material
HD
HD
HD
HD
HD
HD
HD
HD
HD
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Sample
Type
Wipe
Wipe
Wipe
Wipe
Wipe
Wipe
Wipe
Wipe
Wipe
Mean
Total
Mass
Recovery
(^g) "
6.09
13.5
10.0
11.2
20.1
12.3
20.4
i.62
21.6
Testing
Method
Baseline
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
Baseline <
Mod 2 + Chem A
Baseline <
Mod 2 + Chem B
Baseline <
Mod 3 + Chem A
Mod 1 <
Mod 3 + Chem A
Mod 3 - Chem A <
Mod 2 + Chem A
Mod 3 - Chem A <
Mod 2 + Chem B
Mod 3 - Chem A <
Mod 3 + Chem A
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Table D106. Multiple comparison adjusted p-values between testing methods for positive controls (HD in Paint Coupons)
Agent Material
HD
HD
HD
HD
HD
HD
HD
HD
HD
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Sample
Type
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Mean
Total
Mass
Recovery
(^g) "
325
520
467
615
308
492
383
424
365
Testing
Method
Baseline
Fate and
Transport
Mod 1
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
Mod 2 -
Chem A
Mod 2
+ Chem
A
1.0000
1.0000
1.0000
0.6121
Mod 2 -
Chem B
1.0000
1.0000
1.0000
1.0000
1.0000
Mod 2
+ Chem
B
1.0000
1.0000
1.0000
1.0000
1.0000
1.0000
Mod 3 -
Chem A
1.0000
1.0000
1.0000
1.0000
1.0000
1.0000
Mod 3
+ Chem
A
1.0000
1.0000
1.0000
1.0000
1.0000
1.0000
Summary of
Significant
Bonferroni-
Holm
Differences
No significant
differences.
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Table D107. Multiple comparison adjusted p-values between testing methods for positive controls (HD in SPE Disks)
Agent Material
HD
HD
HD
HD
HD
HD
HD
HD
HD
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Sample
Type
SPE
SPE
SPE
SPE
SPE
SPE
SPE
SPE
SPE
Mean
Total
Mass
Recovery
(^g) "
881
1520
1140
1060
1190
1120
1090
1110
1140
Testing
Method
Baseline
Fate and
Transport
Modi
Mod 2 -
Chem A
Mod 2
+ Chem
A
Mod 2 - Mod 2 + Mod 3 - Mod 3 +
Chem B Chem B Chem A Chem A
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
Baseline <
Fate and
Transport
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Table D108. Multiple comparison adjusted p-values between testing methods for positive controls (HD on Sealant Coupon Surfaces)
Agent
Material
Sample
Type
Mean
Total
Mass
Recovery
(Hg) "
Testing
Method
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
Summary of Significant
Bonferroni-Holm
Differences
HD
Sealant
Wipe
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Table D109. Multiple comparison adjustedp-values between testing methods for positive controls (HD in Sealant Coupons)
Agent Material
Sample
Type
Mean
Total
Mass
Recovery
(^g) "
Testing
Method
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2
+ Chem
A
Mod 2 -
Chem B
Mod 2
+ Chem
B
Mod 3 -
Chem A
HD
Sealant
Extracted
Coupon
188
Baseline
HD
Sealant
Extracted
Coupon
384
Fate and
Transport
HD
Sealant
Extracted
Coupon
250
Mod 1
HD
Sealant
Extracted
Coupon
212
Mod 2 -
Chem A
HD
Sealant
Extracted
Coupon
207
Mod 2 +
Chem A
HD
Sealant
Extracted
Coupon
253
Mod 2 -
Chem B
HD
Sealant
Extracted
Coupon
201
Mod 2 +
Chem B
HD
Sealant
Extracted
Coupon
276
Mod 3 -
Chem A
HD
Sealant
Extracted
Coupon
203
Mod 3 +
Chem A
Mod 3
+ Chem
A
Summary of
Significant
Bonferroni-Holm
Differences
Base < Fate
Mod 2 - Chem A <
Fate
Mod 2 + Chem A <
Fate
Mod 2 + Chem B <
Fate
Mod 3 + Chem A <
Fate
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Table DUO. Multiple comparison adjusted p-values between testing methods for positive controls (HD in SPE Disks)
Agent Material
HD
HD
HD
HD
HD
HD
HD
HD
HD
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sample
Type
SPE
SPE
SPE
SPE
SPE
SPE
SPE
SPE
SPE
Mean
Total
Mass
Recovery
(^g) "
1070
1470
100
1080
1130
1160
1040
1120
1090
Testing
Method
Baseline
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
Mod 2
+ Chem
A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
Summary of
Significant
Bonferroni-Holm
Differences
Mod 2 + Chem B <
Fate and Transport
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Table Dill. Multiple comparison adjusted p-values between testing methods for positive controls (VX on Paint Coupon Surfaces)
Agent
Material
Sample
Type
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Fate and
Transport
Modi
Mod 2 -
Chem A
Mod 2
+ Chem
A
Mod 2
- Chem
B
Mod 2
+ Chem
B
Mod 3
- Chem
A
Mod 3
+ Chem
A
Summary of
Significant
Bonferroni-Holm
Differences
VX
Paint
Wipe
92.0
Baseline
0.0010
1.0000
1.0000
0.0154
1.0000
1.0000
1.0000
0.2860
Baseline < (Fate,
Mod 2 + Chem A)
VX
Paint
Wipe
440
Fate and
Transport
0.0009
0.0172
1.0000
0.0017
0.0062
0.0013
0.2860
Mod 1 < (Fate and
Transport, Mod 2 +
VX
Paint
Wipe
87.9
Mod 1
1.0000
0.0137
1.0000
1.0000
1.0000
0.2706
Chem A)
Mod 2 - Chem A <
Fate and Transport
VX
Paint
Wipe
180
Mod 2 -
Chem A
0.2706
1.0000
1.0000
1.0000
1.0000
VX
Paint
Wipe
357
Mod 2 +
Chem A
0.0260
0.0967
0.0193
1.0000
Mod 2 - Chem B <
(Fate and Transport,
Mod 2 + Chem A)
Mod 2 + Chem B <
VX
Paint
Wipe
110
Mod 2 -
Chem B
1.0000
0.4541
VX
Paint
Wipe
148
Mod 2 +
Chem B
1.0000
1.0000
Fate and Transport
Mod 3 - Chem A <
VX
Paint
Wipe
100
Mod 3 -
Chem A
0.3476
(Fate and Transport,
Mod 2 + Chem A)
VX
Paint
Wipe
266
Mod 3 +
Chem A
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Table D112. Multiple comparison adjusted p-values between testing methods for positive controls (VX in Paint Coupons)
Agent
Material
Sample
Type
Mean
Total
Mass
Recovery
(Hg) "
Testing
Method
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
Summary of
Significant
Bonferroni-
Holm
Differences
VX
Paint
Extracted
Coupon
295
Baseline
<0.0001
1.0000
1.0000
1.0000
1.0000
1.0000
1.0000
0.5610
VX
Paint
Extracted
Coupon
1020
Fate and
Transport
<0.0001
<0.0001
<0.0001
<0.0001
<0.0001
<0.0001
<0.0001
VX
Paint
Extracted
Coupon
256
Mod 1
1.0000
1.0000
1.0000
1.0000
1.0000
1.0000
VX
Paint
Extracted
Coupon
368
Mod 2 -
Chem A
1.0000
0.8226
0.2370
0.2370
0.0776
All conditions <
VX
Paint
Extracted
Coupon
274
Mod 2 +
Chem A
1.0000
1.0000
1.0000
0.9332
Fate and
Transport
VX
Paint
Extracted
Coupon
196
Mod 2 -
Chem B
1.0000
1.0000
1.0000
VX
Paint
Extracted
Coupon
148
Mod 2 +
Chem B
1.0000
1.0000
VX
Paint
Extracted
Coupon
147
Mod 3 -
Chem A
1.0000
VX
Paint
Extracted
108
Mod 3 +
Coupon
Chem A
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Table D113. Multiple comparison adjusted p-values between testing methods for positive controls (VX on Paint with SPE Disks)
Agent Material
VX
VX
VX
VX
VX
VX
VX
VX
VX
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Paint
Sample
Type
SPE
SPE
SPE
SPE
SPE
SPE
SPE
SPE
SPE
Mean
Total
Mass
Recovery
(^g) "
233
288
277
394
350
231
169
217
202
Testing
Method
Baseline
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 + Mod 2 - Mod 2 + Mod 3 - Mod 3 +
Chem A Chem B Chem B Chem A Chem A
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
No
significant
differences.
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Table D114. Multiple comparison adjusted p-values between testing methods for positive controls (VX on Sealant Coupon Surfaces)
Agent Material
VX
VX
VX
VX
VX
VX
VX
VX
VX
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sample
Type
Wipe
Wipe
Wipe
Wipe
Wipe
Wipe
Wipe
Wipe
Wipe
Mean
Total
Mass
Recovery
(^g) "
30i
69.2
35.5
28.8
416
31.9
321
38.1
505
Testing
Method
Baseline
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
Fate and
Transport
Mod 1
Mod 2- Mod 2+ Mod 2- Mod 2 + Mod 3- Mod 3 +
Chem A Chem A Chem B Chem B Chem A Chem A
Summary of
Significant
Bonferroni-Holm
Differences
Baseline <
(Mod 2 + Chem A,
Mod 2 + Chem B,
Mod 3 + Chem A)
Fate and Transport <
(Mod 2 + Chem A,
Mod 2 + Chem B,
Mod 3 + Chem A),
Mod 1 <
(Mod 2 + Chem A,
Mod 2 + Chem B,
Mod 3 + Chem A)
Mod 2 - Chem A <
(Mod 2 + Chem A,
Mod 2 + Chem B,
Mod 3 + Chem B)
Mod 2 - Chem B <
(Mod 2 + Chem A,
Mod 2 + Chem B,
Mod 3 + Chem A)
Mod 2 + Chem B <
(Mod 2 + Chem A,
Mod 3 + Chem A)
Mod 3 - Chem A <
(Mod 2 + Chem A,
Mod 2 + Chem B,
Mod 3 + Chem A)
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Table D115. Multiple comparison adjusted p-values between testing methods for positive controls (VX in Sealant Coupons)
Agent Material
VX
VX
VX
VX
VX
VX
VX
VX
VX
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sample
Type
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Extracted
Coupon
Mean
Total
Mass
Recovery
(^g) "
821
653
893
551
197
715
340
646
180
Testing
Method
Baseline
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
Mod 2 + Mod 2 — Mod 2 + Mod 3 — Mod 3 + Summary of Significant
Chem A Chem B Chem B Chem A Chem A Bonferroni-Holm Differences
Fate and Transport <
(Baseline, Mod 1)
Mod 2 - Chem A <
(Baseline. Mod 1.
Mod 2 - Chem B)
Mod 2 + Chem A <
(Baseline, Fate and Transport,
Mod 1.
Mod 2 - Chem A,
Mod 2 - Chem B,
Mod 3 - Chem A)
Mod 2 + Chem B <
(Baseline, Fate and Transport,
Mod 1.
Mod 2 - Chem A,
Mod 2 - Chem B,
Mod 3 - Chem A)
Mod 2 - Chem B < Mod 1
Mod 3 - Chem A < (Baseline.
Mod 1)
Mod 3 + Chem A <
(Baseline, Fate and Transport,
Mod 1.
Mod 2 - Chem A,
Mod 2 - Chem B,
Mod 2 + Chem B,
Mod 3 - Chem A)
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Table D116. Multiple comparison adjustedp-values between testing methods for positive controls (VX in SPE Disks)
Agent Material
VX
VX
VX
VX
VX
VX
VX
VX
VX
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sealant
Sample
Type
SPE
SPE
SPE
SPE
SPE
SPE
SPE
SPE
SPE
Mean
Total
Mass
Recovery
(^g) "
1.7
199
1.66
2.70
20.6
0.58
1.00
0.80
101
Testing
Method
Baseline
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 + Mod 2 - Mod 2 + Mod 3 - Mod 3 +
Chem A Chem B Chem B Chem A Chem A
Fate and
Transport
Mod 1
Mod 2 -
Chem A
Mod 2 +
Chem A
Mod 2 -
Chem B
Mod 2 +
Chem B
Mod 3 -
Chem A
Mod 3 +
Chem A
No
significant
differences.
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REFERENCES
[Dl] See, e.g., https://itl.nist.gov/div898/handbook/eda/section3/eda35a.htm. Last accessed
March 15, 2022.
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APPENDIX E
Pesticide Statistical Analysis
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The objective of this analysis was to compare total fipronil and malathion mass recovered from
each of two different materials (paint and sealant) and on each of three different sample types
(wipes, extracted Coupon, and SPE disks) using four different combinations of one of two
decontaminants applied under one of three testing methods (see Table El). Three replicates were
tested for each condition. Table E2 summarizes the study design.
Additional evaluation was performed using positive control tests. The positive control tests
excluded application of the target decontaminant. The decontamination test conditions were
compared to their analogous positive control tests to determine if statistically significant
decontamination occurred. One set of positive controls was tested for the Baseline, and one set
was tested for both Mod 1 and Mod 2. Positive controls were also compared between testing
methods to evaluate whether the differences between methods might be attributable to external
factors other than the decontamination process.
Table El. Description of Testing Methods and Decontaminant Combinations
Testing
Method
Decontaminant
Dwell Time
Water Rinse?
Decontaminant
Application
Baseline
0 minutes
No
lOx Diluted Bleach or
D7
Mod 1
60 minutes + Rinse/
Reapplication + 60 minutes
Yes
D7
Mod 2
120 minutes
No
D7
Observations below the method quantification limit (MQL) were set equal to the MQL, which
ranged from 0.001 to 0.01 pg for fipronil and ranged from 1.0 pg to 11 pg for malathion
dependent on sample type and required sample dilutions. Table E3 displays the percentage of
observations below the MQL in each test condition, as well as the overall percentage of < MQL
observations within each pesticide/material/sample type analysis. Many substitutions at the MQL
value likely bias the estimates high and using a single substitution value artificially reduces the
variance associated with the estimates. The reduction in variance may make the estimates more
likely to be significantly different from other estimates when a real difference is not present.
For Mod 1 where the decontaminant was applied, rinsed, and applied again, the mass recovery
from the rinse data was added to the mass recovery from the wipe data to obtain the total mass
recovered for each replicate. The counts of data below the MQL in the wipe conditions reflect
whether either the rinse or the wipe extraction mass was < MQL, so that samples with both rinse
and wipe values below the MQL and samples with only one of the rinse or wipe values below the
MQL were counted similarly.
All SPE disk replicates across both pesticides and materials and for both test samples and
positive controls were measured to be below the MQL. Therefore, no comparisons could be
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conducted between testing method and decontaminant conditions for SPE disks. Similarly, only
one observation for wipe replicates in each of the paint or sealant conditions with malathion was
above the MQL; therefore, no comparisons were conducted between testing method and
decontaminant conditions for wipes with malathion.
Table E2. Study Design for Testing Method and Decontaminant Comparison
Number of Replicates
Pesticide
Material
Testing
Method
Decontaminant
Wipe
Samples
Extracted
Coupon
Samples
SPE Disk
Samples
Fipronil
Paint
Baseline
lOx Diluted Bleach
3
3
3
Fipronil
Paint
Baseline
D7
3
3
3
Fipronil
Paint
Mod 1
D7
3
3
3
Fipronil
Paint
Mod 2
D7
3
3
3
Fipronil
Sealant
Baseline
lOx Diluted Bleach
3
3
3
Fipronil
Sealant
Baseline
D7
3
3
3
Fipronil
Sealant
Mod 1
D7
3
3
3
Fipronil
Sealant
Mod 2
D7
3
3
3
Malathion
Paint
Baseline
lOx Diluted Bleach
3
3
3
Malathion
Paint
Baseline
D7
3
3
3
Malathion
Paint
Mod 1
D7
3
3
3
Malathion
Paint
Mod 2
D7
3
3
3
Malathion
Sealant
Baseline
lOx Diluted Bleach
3
3
3
Malathion
Sealant
Baseline
D7
3
3
3
Malathion
Sealant
Mod 1
D7
3
3
3
Malathion
Sealant
Mod 2
D7
3
3
3
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Table E3. Percent of Observations < MQL in Each Test Condition
Percent of Replicates
Pesticide
Material
Testing
Method
Decontaminant
Wipe
Samples
Extracted
Extracted
Coupon
Samples
SPE
Disk
Samples
Fipronil
Paint
Baseline
lOx Diluted
Bleach
0%
0%
100%
Fipronil
Paint
Baseline
D7
0%
0%
100%
Fipronil
Paint
Mod 1
D7
100%
33.3%
100%
Fipronil
Paint
Mod 2
D7
0%
0%
100%
Fipronil
Paint
Total
25%
8.33%
100%
Fipronil
Sealant
Baseline
lOx Diluted
Bleach
0%
0%
100%
Fipronil
Sealant
Baseline
D7
0%
0%
100%
Fipronil
Sealant
Mod 1
D7
0%
0%
100%
Fipronil
Sealant
Mod 2
D7
0%
0%
100%
Fipronil
Sealant
Total
0%
0%
100%
Malathion
Paint
Baseline
lOx Diluted
Bleach
66.7%
0%
100%
Malathion
Paint
Baseline
D7
100%
0%
100%
Malathion
Paint
Mod 1
D7
100%
0%
100%
Malathion
Paint
Mod 2
D7
100%
0%
100%
Malathion
Paint
Total
91.7%
0%
100%
Malathion
Sealant
Baseline
lOx Diluted
Bleach
100%
100%
100%
Malathion
Sealant
Baseline
D7
100%
0%
100%
Malathion
Sealant
Mod 1
D7
100%
0%
100%
Malathion
Sealant
Mod 2
D7
66.7%
0%
100%
Malathion
Sealant
Total
91.7%
25%
100%
Pesticide ANOVA
Comparison of Test Sample Results
A fixed effects ANOVA model was fitted to the pesticide total mass recovery data over all
testing method and decontaminant combinations separately for each pesticide, material, and
sample type condition. The models contained an effect for the combination of testing method and
decontaminant and a residual error term. No random effect of trial was fitted due to only one trial
being run for all replicates of each pesticide and material condition.
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The assumptions of normally distributed errors with approximately equal variances were better
met with untransformed data than with natural logarithm-transformed data, so data were left
untransformed for the analysis. The models were fitted using SAS (version 9.4, 64-bit). The form
of the model is presented in Equation El.
Mass (Jag) = (30+ (31}+ eijk
Equation El
where:
• /?0 = intercept or overall mean total mass collected.
• Pij = the fixed effect for the 7th testing method and/h decontaminant.
• £ijk = random error for the k'h replicate from the i'h testing method, and/h decontaminant.
The random error is assumed to be N{0,
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The Bonferroni-Holm multiple comparisons procedure was performed to adjust the ^-values of
the pairwise comparisons so that a familywise error rate of 0.05 was maintained over all 4
comparisons of interest within a pesticide/material/sample type condition. This procedure limits
the probability of a difference being falsely identified as statistically significant when no true
difference exists, and the difference is due to sampling variability. The familywise error rate
means that the chance of a sampling-based falsely significant result is no more than 1 in 20 for
the entire set of 4 comparisons. The Bonferroni-Holm procedure was selected due to its power in
detecting true differences when performing a restricted number of pairwise comparisons.
Comparison of Test Sample Results with Positive Controls
A fixed effects ANOVA model was fitted to the total mass recovery data for decontaminants and
positive controls results within each pesticide/material/sample type/testing method condition.
The models contained an effect for the combination of decontaminant/positive control status and
a residual error term. No random effect of trial was fitted due to only one trial being run for all
replicates of each pesticide and material condition.
The assumptions of normality and equality of variances were better met with untransformed data
than with natural logarithm-transformed data, so data were left untransformed for the analysis.
The models were fitted using SAS (version 9.4, 64-bit). The form of the model is presented in
Equation E2.
Mass (jig) = (10 + /?,• + £tj
Equation E2
where:
• /?0 = intercept or overall mean total mass collected.
• /?,• = the fixed effect for the z'th decontaminant / positive control condition.
• E[j = random error for the jh replicate from the z'th decontaminant / positive control
condition. The random error is assumed to be N{0,
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Comparison of Positive Control Results
A fixed effects ANOVA model was fitted to the total mass recovery data for positive controls
results under each testing method within each pesticide/material/sample type condition. The 72-
Hour Fate and Transport data for each pesticide/material/sample type were also included as a test
method condition in this analysis. The models contained an effect for the combination of testing
method under which the positive control was collected and the chemical application, and a
residual error term. No random effect of trial was fitted due to only one trial being run for all
replicates of each pesticide and material condition. Data were left untransformed for the analysis
to remain consistent with analyses of test samples and test samples vs positive controls. The
models were fitted using SAS (version 9.4, 64-bit). The form of the model is presented in
Equation E3.
Mass (jug) = (10 + /% + eijk
Equation E3
where:
• /?0 = intercept or overall mean total mass collected.
• Pij = the fixed effect for the positive controls from the z'th testing method and jth chemical
application condition.
• Eijk = random error for the kh positive control from the z'th testing method / jth chemical
application condition. The random error is assumed to be N{0,
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Pesticide ANOVA Results
Table E5 through Table E7 displays the potential outliers identified by examining the externally
studentized residuals in each study condition. Probable cause was not identified for any of the
listed outliers. Thus, all replicates were included in the final analysis.
Table E5. Potential Outliers Identified from Test Samples
Analysis
Pesticide
Material
Sample
Type
Test
Method
Decontaminant
Replicate
Number
Total
Mass
Recovery
(MS)
Externally
Studentized
Residual
Fipronil
Paint
Extracted
Coupon
Baseline
lOx Diluted
Bleach
1
3.04
3.21
Fipronil
Paint
Wipe
Baseline
lOx Diluted
Bleach
1
5.43
19.21
Fipronil
Sealant
Extracted
Coupon
Mod 2
D7
1
0.63
3.5
Test
Samples
Fipronil
Sealant
Extracted
Coupon
Mod 2
D7
3
0.41
-3.65
Fipronil
Sealant
Wipe
Mod 2
D7
3
0.84
-3.59
Malathion
Paint
Extracted
Coupon
Mod 2
D7
3
6.01
-3.9
Malathion
Sealant
Extracted
Coupon
Mod 2
D7
1
7.63
-4.42
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Table E6. Potential Outliers Identified from Test Samples v.s Positive Controls
Analysis
Pesticide
Material
Sample
Type
Test
Method
Decontaminant
or Positive
Control (PC)
Replicate
Number
Total
Mass
Recovery
(fig)
Externally
Studentized
Residual
Test
Samples vs
Positive
Control
Comparison
Fipronil
Paint
Extracted
Coupon
Baseline
Positive controls
2
2.29
-3.27
Fipronil
Paint
Extracted
Coupon
Mod 1/
Mod 2
Positive controls
2
4.48
6.98
Fipronil
Paint
Wipe
Baseline
Bleach
1
5.43
3.90
Fipronil
Paint
Wipe
Mod 1/
Mod 2
Positive controls
2
6.13
-13.7
Fipronil
Sealant
Extracted
Coupon
Baseline
Positive controls
2
1.67
5.18
Fipronil
Sealant
Extracted
Coupon
Mod 1/
Mod 2
Positive controls
2
1.96
10.3
Malathion
Sealant
Extracted
Coupon
Baseline
D7
3
4.64
-3.92
Malathion
Sealant
Extracted
Coupon
Mod
1/Mod 2
Positive controls
1
15.4
6.71
Malathion
Sealant
Wipe
Baseline
D7
3
11.0
4.41
Malathion
Sealant
Wipe
Mod 1/
Mod 2
Positive controls
1
1.64
-4.27
Malathion
Sealant
Wipe
Mod 1/
Mod 2
Positive controls
3
8.49
3.36
Table E7. Potential Outliers Identified from Positive Controls Analysis
Analysis
Pesticide
Material
Sample
Type
Test Method
Replicate
Number
Total
Mass
Recovery
(fig)
Externally
Studentized
Residual
Fipronil
Paint
Extracted
Coupon
Mod 1/Mod 2
2
4.48
3.24
Positive
Fipronil
Sealant
Extracted
Coupon
Mod 1 / Mod 2
2
1.96
3.88
Controls
Malathion
Paint
Wipe
Fate and
Transport
1
1.25
-10.6
Malathion
Sealant
Extracted
Coupon
Mod 1/Mod 2
1
15.4
7.34
Figure El to Figure E4 display the total mass recoveries for the replicates in each
pesticide/material/sample type condition. Statistical summaries including arithmetic means and
95% confidence intervals are presented in Table E8 to Table El 1 and are sorted in order of
estimated mean total mass recovery within each pesticide, material, and sample type. Confidence
bounds were not adjusted for multiple comparisons between test conditions, and thus should not
be used to evaluate significant differences between test conditions.
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Figure El. Total recovery mass of test samples for all testing method and decontaminant combinations over all sample types for
Fipronil on Paint Coupon
SampleType = Coupon
SampleType = SPE
SampleType = Wipe
@
+ * *
OOO +++ +++ +++
O O
*
£
+
Baseline Mod 1 Mod 2 Baseline Mod 1 Mod 2 Baseline Mod 1 Mod 2
Testing Method
Decontaminant O Bleach + D7
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Figure E2. Total recovery mass of test samples for all testing method and decontaminant combinations over all sample types for
Fipronil on Sealant Coupon
SampleType = Coupon
SampleType = SPE
SampleType = Wipe
O + +H- +
OOO +++ +H- +++
o * * *
Baseline Mod 1 Mod 2 Baseline Mod 1 Mod 2 Baseline Mod 1 Mod 2
Testing Method
Decontaminant O Bleach + D7
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Figure E3. Total recovery mass of test samples for all testing method and decontaminant combinations over all sample types for
Malathion on Paint Coupon
SampleType = Coupon
SampleType = SPE
SampleType = Wipe
20 -
+
++
+
15 -
+ +
+
O
I | |
10 -
0
+
+
+++
5 -
CCO +++ +++ +++
GED +++
0 -
Baseline Mod 1 Mod 2 Baseline Mod 1 Mod 2 Baseline Mod 1 Mod 2
Testing Method
Decontaminant O Bleach + D7
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Figure E4. Total recovery mass of test samples for all testing method and decontaminant combinations over all sample types for
Malathion on Sealant Coupon
SampleType = Coupon
SampleType = SPE
SampleType = Wipe
20 -
15 -
10 -
*
+
+
+
+
+++
5 -
*
++
ooo
CCO +++ +++ +++
OOO -ft-
0 -
Baseline Mod 1 Mod 2 Baseline Mod 1 Mod 2 Baseline Mod 1 Mod 2
Testing Method
Decontaminant O Bleach + D7
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Table E8. Sorted Arithmetic Means and Unadjusted 95% Confidence Intervals (Fipronil-Paint
Coupons)
Pesticide
Material
Sample
Type
Test
Method
Decontaminant
Mean Total
Mass
Recovery
(fig)
Lower 95%
Confidence
Bound
Upper 95%
Confidence
Bound
Fipronil
Paint
Wipe
Baseline
D7
0.057
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Table E9. Sorted Arithmetic Means and Unadjusted 95% Confidence Intervals (Fipronil-Sealant
Coupons)
Pesticide
Material
Sample
Type
Test
Method
Decontaminant
Mean Total
Mass
Recovery
(fig)
Lower 95%
Confidence
Bound
Upper 95%
Confidence
Bound
Fipronil
Sealant
Wipe
Baseline
lOx Diluted
Bleach
0.068
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Table E10. Sorted Arithmetic Means and Unadjusted 95% Confidence Intervals (Malathion-Paint
Coupons)
Pesticide
Material
Sample
Type
Test
Method
Decontaminant
Mean Total
Mass
Recovery
(fig)
Lower 95%
Confidence
Bound
Upper 95%
Confidence
Bound
Malathion
Paint
Wipe
Baseline
D7
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Table Ell. Sorted Arithmetic Means and Unadjusted 95% Confidence Intervals (Malathion-Sealant
Coupons)
Pesticide
Material
Sample
Type
Test
Method
Decontaminant
Mean Total
Mass
Recovery
(fig)
Lower 95%
Confidence
Bound
Upper 95%
Confidence
Bound
Malathion
Sealant
Wipe
Baseline
lOx Diluted
Bleach
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D7 comparisons:
• Mod 1 paint and sealant extracted coupon samples resulted in lower fipronil values
(lower fipronil recovery) compared to Baseline and Mod 2.
• Baseline sealant extracted coupon samples resulted in lower malathion values compared
to Mod 1 or Mod 2. Note that for malathion there was no difference for Baseline, Mod 1,
or Mod 2 paint coupon samples.
Baseline comparisons:
• D7 resulted in lower fipronil values for both paint coupon wipes and paint extracted
coupons compared to lOx diluted bleach.
• D7 resulted in lower fipronil values for sealant coupons compared to bleach.
• lOx diluted bleach resulted in lower malathion values only for sealant coupons.
Table E38 to Table E49 display the results of the Bonferroni-Holm-adjusted pairwise
comparisons between the test samples and positive controls (within-test comparisons). A
summary of these results showing the significant differences for the four pairwise comparisons
between test samples to positive controls for each pesticide/material/sample combination is
shown in Table E12. Recall that SPE results were all nondetects, as were most malathion paint
wipes, so comparisons could not be made. For D7 in Baseline, Mod 1, and Mod 2 tests, all
fipronil extracted coupon and wipe samples for paint and sealant coupons were less that the
positive controls. For lOx diluted bleach (used only for Baseline tests) all fipronil coupon and
wipe samples for paint and sealant were less that the positive controls except for paint coupons,
which were not different from the positive controls. No differences from the positive controls
were observed for malathion testing, aside from the D7 baseline sealant coupon where the
Baseline result was actually higher than the positive control due to required sample dilutions that
resulted in elevated nondetect results.
Table El2. Summary of Test Sample to Positive Control Comparisons
Chemical
Material
Wipe
Extracted
Coupon
SPE
Fipronil
Paint
4 differences
3 differences
Not Applicable
Sealant
4 differences
4 differences
Not Applicable
Malathion
Paint
Not Applicable
No differences
Not Applicable
Sealant
No differences
1 difference
Not Applicable
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Table E50 to Table E61 display the results of the Bonferroni-Holm-adjusted pairwise
comparisons between the positive control conditions (across-test method comparisons). A
summary of these results showing significant differences for the three pairwise comparisons
between positive controls for each pesticide/material/sample combination is shown in Table E13.
Note that comparisons for the SPE data were not possible as all results were nondetects. The
three differences that were observed were associated with comparisons to the Fate and Transport
data; the reason for these differences is not apparent.
Table El 3. Summary of Positive Control Comparisons
Chemical
Material
Wipe
Extracted
Coupon
SPE
Fipronil
Paint
No differences
1 difference
Not Applicable
Sealant
No differences
No differences
Not Applicable
Malathion
Paint
2 differences
No differences
Not Applicable
Sealant
No differences
No differences
Not Applicable
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Table E14. Multiple comparison adjustedp-values between test methods for D 7 (Fipronil on Paint Coupon Surfaces)
Summary of
Significant
Bonferroni-
Holm
Differences
Pesticide
Material
Sample
Type
Decontaminant
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
Fipronil
Paint
Wipe
D7
0.057
Baseline
A
Fipronil
Paint
Wipe
D7
0.089
Mod 1
A
Fipronil
Paint
Wipe
D7
0.12
Mod 2
A
Dahlgren
Mod 1 Mod 2
Table El 5. Multiple comparison adjusted p-values between test methods for D 7 (Fipronil in Paint Coupons)
Pesticide
Material
Sample
Type
Decontaminant
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
Fipronil
Paint
Extracted
Coupon
D7
0.69
Baseline
A
Fipronil
Paint
Extracted
Coupon
D7
0.15
Mod 1
B
Fipronil
Paint
Extracted
Coupon
D7
0.79
Mod 2
A
Dahlgren
Mod 1 Mod 2
Summary of
Significant
Bonferroni-
Holm
Differences
Mod 1 <
Baseline
Mod 1 < Mod 2
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Table El 6. Multiple comparison adjusted p-values between test methods for D7 (Fipronil in SPE Disks)
Mean
Total
D7
Summary of
Significant
Pesticide
Material
Sample
Type
Decontaminant
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
Modi
Mod 2
Bonferroni-
Holm
Differences
Fipronil
Paint
SPE
D7
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Table E19. Multiple comparison adjusted p-values between test methods for D7 (Fipronil in SPE Disks)
Pesticide
Material
Sample
Type
Decontaminant
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
Fipronil
Sealant
SPE
D7
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Table E22. Multiple comparison adjusted p-values between test methods for D7 (Malathion in SPE Disks)
Mean
Total
D7
Summary of
Significant
Pesticide
Material
Sample
Type
Decontaminant
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
Modi
Mod 2
Bonferroni-
Holm
Differences
Malathion
Paint
SPE
D7
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Table E25. Multiple comparison adjusted p-values between test methods for D7 (Malathion in SPE Disks)
Mean
Total
D7
Summary of
Significant
Pesticide
Material
Sample
Type
Decontaminant
Mass
Recovery
(MS)
Testing
Method
Similarity
Designation
Modi
Mod 2
Bonferroni-
Holm
Differences
Malathion
Sealant
SPE
D7
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Table E28. Multiple comparison adjustedp-values between decontaminants for Baseline testing method
(Fipronil in SPE Disks)
Pesticide
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Baseline
D7
Summary of
Significant
Bonferroni-Holm
Differences
Fipronil
Paint
SPE
Baseline
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Table E31. Multiple comparison adjustedp-values between decontaminants for Baseline testing method
(Fipronil in SPE Disks)
Pesticide
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Baseline
D7
Summary of
Significant
Bonferroni-Holm
Differences
Fipronil
Sealant
SPE
Baseline
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Table E34. Multiple comparison adjustedp-values between decontaminants for Baseline testing method
(Malathion in SPE Disks)
Pesticide
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Baseline
D7
Summary of
Significant
Bonferroni-Holm
Differences
Malathion
Paint
SPE
Baseline
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Table E3 7. Multiple comparison adjustedp-values between decontaminants for Baseline testing method
(Malathion in SPE Disks)
Pesticide
Material
Sample
Type
Testing
Method
Mean Total
Mass
Recovery
(MS)
Decontaminant
Similarity
Designation
Baseline
D7
Summary of
Significant
Bonferroni-Holm
Differences
Malathion
Sealant
SPE
Baseline
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Within-Test Comparisons
Table E38. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (Fipronil on Paint Coupon Surfaces)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(Mg)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
Fipronil
Paint
Wipe
4.16
Baseline
Bleach
0.0007
Bleach < PC
Fipronil
Paint
Wipe
0.057
Baseline
D7
<0.0001
D7 < PC
Fipronil
Paint
Wipe
7.96
Baseline
Positive
Control
Fipronil
Paint
Wipe
0.089
Mod 1
D7
<0.00001
D7 (Mod 1) < PC
Fipronil
Paint
Wipe
0.12
Mod 2
D7
<0.00001
D7 (Mod 2) < PC
Fipronil
Paint
Wipe
7.38
Mod 1 /
Mod 2
Positive
Control
Table E39. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (Fipronil in Paint Coupons)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(Mg)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
Fipronil
Paint
Extracted
Coupon
2.76
Baseline
Bleach
0.7698
Not significantly
different
Fipronil
Paint
Extracted
Coupon
0.69
Baseline
D7
0.0004
D7 < PC
Fipronil
Paint
Extracted
Coupon
2.84
Baseline
Positive
Control
Fipronil
Paint
Extracted
Coupon
0.15
Mod 1
D7
0.0002
D7 (Mod 1) < PC
Fipronil
Paint
Extracted
Coupon
0.79
Mod 2
D7
0.0004
D7 (Mod 2) < PC
Fipronil
Paint
Extracted
Coupon
3.57
Mod 1/
Mod 2
Positive
Control
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Table E40. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (Fipronil in SPE Disks)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
Fipronil
Paint
SPE
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Table E42. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (Fipronil in Sealant Coupons)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
0*8)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
Fipronil
Sealant
Extracted
Coupon
0.039
Baseline
Bleach
<0.0001
Bleach < PC
Fipronil
Sealant
Extracted
Coupon
0.15
Baseline
D7
<0.0001
D7 < PC
Fipronil
Sealant
Extracted
Coupon
1.49
Baseline
Positive
Control
Fipronil
Sealant
Extracted
Coupon
0.015
Mod 1
D7
0.0037
D7 (Mod 1) < PC
Fipronil
Sealant
Extracted
Coupon
0.52
Mod 2
D7
0.0162
D7 (Mod 2) < PC
Fipronil
Sealant
Extracted
Coupon
1.36
Mod 1 /
Mod 2
Positive
Control
Table E43. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (Fipronil in SPE Disks)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
Fipronil
Sealant
SPE
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table E44. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (Malathion on Paint Coupon Surfaces)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
Malathion
Paint
Wipe
1.13
Baseline
Bleach
N/A
N/A
Malathion
Paint
Wipe
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table E46. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (Malathion in SPE Disks)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(MS)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
Malathion
Paint
SPE
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table E48. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (Malathion in Sealant Coupons)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
0*8)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
Malathion
Sealant
Extracted
Coupon
1.00
Baseline
Bleach
0.6890
Not significantly
different
Malathion
Sealant
Extracted
Coupon
4.98
Baseline
D7
<0.0001
PC < Baseline
Malathion
Sealant
Baseline
Coupon
1.07
Control
Malathion
Sealant
Extracted
Coupon
7.29
Mod 1
D7
1.0000
Not significantly
different
Malathion
Sealant
Extracted
Coupon
9.66
Mod 2
D7
1.0000
Not significantly
different
Malathion
Sealant
Extracted
Coupon
7.60
Mod 1/
Mod 2
Positive
Control
Table E49. Multiple comparison adjusted p-values between decontaminants and positive
controls with testing methods (Malathion in SPE Disks)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
0*8)
Testing
Method
Decontaminant
Comparison
vs.
Positive
Control (PC)
Test Direction
Malathion
Sealant
SPE
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Across-Test Method Comparisons
Table E50. Multiple comparison adjusted p-values between testing methods for positive
controls (Fipronil on Paint Coupon Surfaces)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(us) "
Testing Method
Fate and
Transport
Mod 1/
Mod 2
Summary of
Significant
Bonferroni-Holm
Differences
Fipronil
Paint
Wipe
7.96
Baseline
0.9113
0.9113
Fipronil
Paint
Wipe
7.24
Fate & Transport
0.9113
No significant
differences
Fipronil
Paint
Wipe
7.38
Mod 1 / Mod 2
Table E51. Multiple comparison adjusted p-values between testing methods for positive
controls (Fipronil in Paint Coupons)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(us) "
Testing Method
Fate &
Transport
Modi/
Mod 2
Summary of
Significant
Bonferroni-Holm
Differences
Fipronil
Paint
Extracted
Coupon
2.84
Baseline
0.0181
0.1573
Fipronil
Paint
Extracted
Coupon
4.71
Fate and Transport
0.0892
Baseline < Fate and
Transport
Fipronil
Paint
Extracted
Coupon
3.57
Mod 1 / Mod 2
¦
Table E52. Multiple comparison adjusted p-values between testing methods for positive
controls (Fipronil in SPE Disks)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(us) "
Testing Method
Fate and
Transport
Modi/
Mod 2
Summary of
Significant
Bonferroni-Holm
Differences
Fipronil
Paint
SPE
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table E53. Multiple comparison adjusted p-values between testing methods for positive
controls (Fipronil on Sealant Coupon Surfaces)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(us) "
Testing Method
Fate and
Transport
Modi/
Mod 2
Summary of
Significant
Bonferroni-Holm
Differences
Fipronil
Sealant
Wipe
9.63
Baseline
0.5422
0.4212
Fipronil
Sealant
Wipe
9.43
Fate and Transport
0.2596
No significant
differences
Fipronil
Sealant
Wipe
10.05
Mod 1/Mod 2
Table E54. Multiple comparison adjusted p-values between testing methods for positive
controls (Fipronil in Sealant Coupons)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(us) "
Testing Method
Fate and
Transport
Mod 1/
Mod 2
Summary of
Significant
Bonferroni-Holm
Differences
Fipronil
Sealant
Extracted
Coupon
1.49
Baseline
0.0671
0.6549
Fipronil
Sealant
Extracted
Coupon
2.27
Fate and Transport
0.0548
No significant
differences
Fipronil
Sealant
Extracted
Coupon
1.36
Mod 1 / Mod 2
Table E55. Multiple comparison adjusted p-values between testing methods for positive
controls (Fipronil in SPE Disks)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(^g) "
Testing Method
Fate and
Transport
Mod 1/
Mod 2
Summary of
Significant
Bonferroni-Holm
Differences
Fipronil
Sealant
SPE
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table E56. Multiple comparison adjusted p-values between testing methods for positive
controls (Malathion on Paint Coupon Surfaces)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(Hg) "
Testing Method
Fate and
Transport
Mod 1/
Mod 2
Summary of
Significant
Bonferroni-Holm
Differences
Malathion
Paint
Wipe
-------
EPA/600/R-22/037 | July 2022
www.epa.gov/emergency-response-research
Table E59. Multiple comparison adjusted p-values between testing methods for positive
controls (Malathion on Sealant Coupon Surfaces)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(us) "
Testing Method
Fate and
Transport
Modi/
Mod 2
Summary of
Significant
Bonferroni-Holm
Differences
Malathion
Sealant
Wipe
3.24
Baseline
0.8333
0.7271
Malathion
Sealant
Wipe
2.84
Fate and Transport
0.7271
No significant
differences
Malathion
Sealant
Wipe
5.17
Mod 1 / Mod 2
Table E60. Multiple comparison adjusted p-values between testing methods for positive
controls (Malathion in Sealant Coupons)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(**g) "
Testing Method
Fate and
Transport
Mod 1/
Mod 2
Summary of
Significant
Bonferroni-Holm
Differences
Malathion
Sealant
Extracted
Coupon
1.07
Baseline
0.1767
0.1962
Malathion
Sealant
Extracted
Coupon
8.83
Fate and Transport
0.7242
No significant
differences
Malathion
Sealant
Extracted
Coupon
7.60
Mod 1 / Mod 2
Table E61. Multiple comparison adjusted p-values between testing methods for positive
controls (Malathion in SPE Disks)
Pesticide
Material
Sample
Type
Mean
Total
Mass
Recovery
(**g) "
Testing Method
Fate and
Transport
Modi/
Mod 2
Summary of
Significant
Bonferroni-Holm
Differences
Malathion
Sealant
SPE
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