United States
Environmental Protection
Agency
Effects of Vapor-Based
Decontamination Systems on
Selected Building Interior Materials:
Vaporized Hydrogen Peroxide
FIRE
National Homeland Security Research Cente
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EPA/600/R-08/074 July 2008 www.epa.gov/ord
Effects of Vapor-Based Decontamination
Systems on Selected Building Interior
Materials: Vaporized Hydrogen Peroxide
Mark D. Brickhouse
Teri Lalain
Philip W. Bartrain
Moiiicia Hall
Zoe Hess
Louis Reiff
Brent Mantooth
Edgewood Chemical Biological Center
Research and Technology Directorate
Aberdeen Proving Ground, MD 21010-5424
Zach Zander
David Stark
Pamela Humphreys
Barry Williams
Science Applications International Corporation
Abingdon, MD 21009
Shawn Ryan
Blair Martin
United States Environmental Protection Agency
Research Triangle Park, NC 27711
Office of Research and Development
National Homeland Security Research Center, Decontamination and Consequence Management Division
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Disclaimer
EPA through its Office of Research and Development partially funded and collaborated in
the research described herein under Interagency Agreement (TAG) DW 939917-01-0 with
the U.S. Army Edgewood Chemical and Biological Center (ECBC). The work performed
in association with this report was conducted from November 2003 to June 2006. The
report lias been subject to an administrative review but does not necessarily reflect the
views of the Agency. No official endorsement should be inferred. EPA does not endorse
the purchase or sale of any commercial products or services.
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Acknowledgments
A program cannot be successfully completed without die contributions of a good team
of people. The authors thank the following individuals for their hard work and assistance
with the execution of this technical program.
The authors thank Mr. David Sorrick (ECBC) for his assistance in acquiring the test
equipment and the design and construction of the circuit breaker test stations.
The authors thank Dr. David Cullinan (SAIC/Geo-Centers, Inc.) for preparing many
coupon run baskets, coupon measurements, and chain-of-custody forms during the time
Ms assigned laboratory was closed.
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Table of Contents
1.0 Background 1
2.0 Summary of Conclusions 3
3.0 Introduction 5
4.0 Experimental Method 7
4.1 Coupon Preparation 7
4.2 Coupon Exposure: Wood. Wallboard. Ceiling Tile, Steel. Carpet.
and Concrete Cinder Block 8
4.3 Coupon Exposure: Circuit Breakers 8
4.4 Visual Inspection 8
4.5 Coupon Aging 8
4.6 Data Review and Technical Systems Audits 8
4.7 Physical Testing 9
4.8 Statistical Analyses 9
4.9 Chemical Testing: FTIR 9
5.0 Post-Fumigation Inspection 11
6.0 Evaluation of Structural Steel 13
6.1 Introduction 13
6.2 Sample Preparation and Testing 13
6.3 Results 14
6.4 Discussion 14
7.0 Evaluation of Gypsum Wallboard 17
7.1 Introduction 17
7.2 Sample Preparation and Testing 17
7.3 Results 18
7.4 Discussion 18
8.0 Evaluation of Acoustical Ceiling Tile 19
8.1 Introduction 19
8.2 Sample Preparation and Testing 19
8.3 Results 20
8.4 Discussion 20
9.0 Evaluation of Carpet 23
9.1 Introduction 23
9.2 Sample Preparation 23
9.3 Results 24
9.4 Discussion 24
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10.0 Evaluation of Concrete Cinder Block 27
10.1 Introduction 27
10.2 Sample Preparation and Testing 27
10.3 Re suits 28
10.4 Discussion 28
11.0 Evaluation of Wood 31
11.1 Introduction 31
11.2 Sample Preparation 31
11.3 Results 32
11.4 Discussion 32
12.0 Evaluation of Electrical Circuit Breakers 35
12.1 Introduction 35
12.2 Sample Preparation 35
12.3 Circuit Breaker Testing Stations 35
12.4 Results and Discussion 36
13.0 FTIR Analysis of Select Wood Samples 39
13.1 Sample Preparation 39
13.2 FTIR 39
13.3 Background and Analysis Methods 39
13.4 Results 40
13.5 Discussion 40
14.0 Quality Assurance Findings 41
15.0 References 43
Appendix A: Coupon Identifier Code A-l
Appendix B: Detailed Coupon Preparation and Inspection Procedures B-l
Appendix C: Wood Coupon Location of Break C-l
Appendix D: Concrete Cinder Block Coupon Break Location D-l
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List of Figures
3.1 The Steris VHP Decontamination Cycle 6
4.1 Samples of the Test Coupons 7
6.1 Photograph- Steel Coupon Test 13
7.1 Photograph - Gypsum Wallboard Coupon Test 17
8.1 Photograph - Acoustical Ceiling Tile Coupon Test 19
8.2 Representative Break - Acoustical Ceiling Tile Coupons 20
9.1 Photograph-Carpet Coupon Test 23
10.1 Photograph - Concrete "Cinder Block" Coupon Test 27
10.2 Representative Concrete Coupon Before and After Testing 28
11.1 Photograph - Wood Coupon Test 31
11.2 Representative Wood Coupon Before and After Testing 32
12.1 Circuit Breaker Test Stations 35
A-l IOPDS04016 Figure 1, "CouponPlacement in Chambers" A-2
A-2 IOP DS04016 Figure 2, "Circuit Breaker Placement in Chambers" A-2
C-l Location of Break, Wood Coupons - VHP Control Set C-l
C-2 Location of Break, Wood Coupons - VHP 125-150 ppm Set C-2
C-3 Location of Break, Wood Coupons - VHP 250-300 ppm Set C-3
D-l Location of Break. Block Coupons - Control Set D-l
D-2 Location of Break, Block Coupons- VHP 125-150 ppm Set D-2
D-3 Location of Break, Block Coupons - VHP 250-300 ppm Set D-3
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List of Tables
4.1 Representative Building Interior Materials 8
4.2 Instron Model 5582 Specifications 9
6.1 VHP Steel Coupon Test Results 15
7.1 Gypsum Wallboard Coupon Test Results for Maximum Load 18
8.1 VHP Coupon Test Results for Tile 21
9.1 Carpet Coupon Test Results for Average Tuft Bind - VHP Control Samples 25
10.1 VHP Coupon Test Results for Concrete Cinder Block 29
11.1 VHP Coupon Test Results for Wood 33
12.1 VHP Circuit Breaker Test Results 36
12.2 Average and Standard Deviation by Group 37
13.1 FUR Analvsis Data 40
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List of Acronyms
APG
ASTM
CB
C1O7
CoC
CT
CW
doc
DS
ECBC
EPA
GSA
H2°2
hr or lirs
IAG
LAW
ID
IOP
ISO 17025
MSDS
NHSRC
QA
QAPP
QMP
R&D
RDECOM
RH
SOPs
TICs
TIMs
UL
V
VHP®, VHP
Aberdeen Proving Groimds
American Society for Testing and Materials
chemical and biological
chlorine dioxide
chain-of-custody
concentration tune
chemical warfare
documentation
Decontamination Sciences
Edgewood Chemical and Biological Center
U.S. Environmental Protection Agency
General Services Administration
hydrogen peroxide
hour or hours
Interagency Agreement
in accordance with
Gant Chart representation for task number (on Gant Chart only)
internal operating procedure
International Standardization Organization Standard 17025
on Laboratory Quality Procedures
Material Safety Data Sheets
National Homeland Security Research Center
quality assurance
Quality Assurance Project Plan (QAPP)
Quality Management Plan
Research and Development
Research, Development, and Engineering Command (formerly SBCCOM)
relative humidity
standing operating procedures ("standard" may also be used in place
of "standing" with the same meaning)
toxic industrial chemicals
toxic industrial materials
Underwriters Laboratories
volt
reference to Steris' registered "vaporized hydrogen peroxide" procedure
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Coupon-Specific Coding
" W" bare wood
"R" carpet
"T" ceiling suspension tile
"G" latex-painted gypsum wallboard
"S" painted structural A572 steel
"C" unpainted concrete cinder block
"A" aluminum coupons
"D" copper coupons
"F" steel coupons
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The material compatibility studies were designed to determine
how decontaminant vapors impact building materials within
an enclosed building interior space. Since building interiors
may contain large surfaces composed of complex materials
and electrical components such as circuit breakers, data are
needed to determine how such materials are affected by
exposure to the vapor. Vaporized hydrogen peroxide (VHP®)
and chlorine dioxide (C1O2) were selected for study since these
decontamination technologies have been used to decontaminate
indoor surfaces contaminated by anthrax and show potential
for use in decontaminating indoor surfaces contaminated by
chemical agents. Representative building interior materials were
tested including unpainted concrete cinder block, standard stud
1.0
Background
lumber (2"x 4" fir), latex-painted !/2-inch gypsum wallboard,
ceiling suspension tile, painted structural steel, and carpet. The
physical properties of the building materials were measured
using American Society for Testing and Materials (ASTM) test
methods. The material compatibility studies also investigated
electrical breakers, using Underwriters Laboratories (UL)
test methods. Specialized chemical testing was conducted to
determine whether chemical changes occurred in select building
materials. In addition, visual appearance was documented.
This report contains the results for the VHP-exposed coupon
material compatibility tests. The C1O2 results are documented in
a separate report.
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VHP-exposed building materials showed no change in
appearance or in integrity compared to nonexposed samples. The
samples were evaluated for outliers using the Dixon's Q-Test in
accordance with (IAW) ASTM Method E 178 and for statistically
demonstrated differences using the Welch's T-Test.
• Painted Structural Steel: The fumigated structural steel
coupons show some minor changes (1-3%) in tensile strength
when compared to the control coupons. All samples were
above the specified tensile strength requirements of the ASTM
test (by 20% or more). There is no obvious change in the
potential for failure of the steel after fumigation using VHP.
• Gypsum Wallboard: Exposure to VHP makes gypsum
wallboard more resistant to penetration by a nail.
• Ceiling Tile: Exposure to VHP causes a small increase in the
breaking force required for the ceiling tile coupons.
• Carpet: Exposure to VHP appears to slightly increase the
force required to pull the carpet tuft bind.
2.0
Summary of Conclusions
• Concrete Cinder Block: The fumigated concrete cinder block
samples did not exhibit any changes from the control samples.
There is no evidence to indicate that fumigation with VHP has
any effect on cinder blocks.
• Wood: The fumigated pine furring strips, prepared from the
stud lumber, exhibit no statistically detectable changes from
the control samples, though a very minor trend of increasing
maximum force and increasing time to break was observed.
Circuit Breaker: Exposure to VHP presents a conflicting
picture of the effects on circuit breakers. Under the 60-amp
challenge, exposed circuit breakers trip more rapidly than the
controls. Under the 30-amp challenge, the circuit breakers trip
more slowly than the controls. Either situation could present
a problem to the user. Failure criteria must be established to
determine whether the changes observed in this test present an
acceptable response.
Visual Inspection: No differences are observed for any of the
coupons after VHP exposure and aging compared to before
VHP exposure.
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3.0
Introduction
To address homeland security needs for decontamination, the
U.S. Environmental Protection Agency (EPA) established an
Interagency Agreement with the U.S. Army Edgewood Chemical
and Biological Center (ECBC) to take advantage of ECBCs
extensive expertise and specialized research facilities for the
decontamination of surfaces contaminated with chemical and
biological (CB) warfare agents. The National Homeland Security
Research Center (NHSRC) fonned a collaboration with ECBC
in a mutual leveraging of resources, expanding upon ECBC's
ongoing programs in CB decontamination to more completely
address the parameters of particular concern for decontamination
of indoor surfaces in buildings following a terrorist attack using
CB agents, or toxic industrial chemicals (TICs) or materials
(TDVIs). In the context of decontamination, the contaminants
of interest are those that can persist on indoor surfaces, leading
to continuing chance of exposure long after the contamination
occurs. VHP® and CIO, are decontamination technologies
that have been used to decontaminate indoor surfaces
contaminated with anthrax spores and show potential for use in
decontaminating indoor surfaces contaminated by some chemical
agents. This program is specifically focused on decontamination
of the building environment, for purposes of restoring a public
building to a usable state after a terrorist contamination episode.
Systematic testing of decontamination technologies generates
objective performance data so building and facility managers,
first responders, groups responsible for building decontamination.
and other technology buyers and users can make informed
purchase and application decisions.
Since building interiors may contain large surfaces composed
of complex materials, material compatibility studies were
designed to determine how the decontaminant vapors impact
building materials within an enclosed building interior space.
The objective of this study was to conduct laboratory test
procedures to determine to what degree building materials were
affected by decontamination using VHP® and CIO,. The building
interior materials used for testing were a subset of die variety
of structural, decorative, and functional materials common to
commercial office buildings regardless of architectural style and
age. The building materials studied encompassed a variety of
material compositions and porosities; they included unpainted
concrete cinder block, standard stud lumber (2"x 4" fir, type-
II), latex-painted '/2-inch gypsum wallboard, acoustical ceiling
suspension tile, primer-painted structural steel, and carpet. The
material compatibility studies also investigated material(s)
related to electrical breaker connections. The physical appearance
was documented by visual inspection of the test material. The
physical properties of the building materials were measured using
standardized ASTM and UL test methods.
The VHP® technology developed by Steris (EPA registration
#58779-4) has been in use for more than a decade. The VHP
fumigant was initially used to sterilize pharmaceutical processing
equipment and clean rooms.1'2 In response to the anthrax
attacks of October 2001, Steris adapted its VHP technology to
perform the decontamination of two U.S. government facilities,
the General Services Administration (GSA) Building 410 at
Anacostia Naval Base, Washington, DC, and the U.S. Department
of State SA-32 Sterling VA mail center.
Decontamination of an interior space using VHP is a four-
phase process involving preparation of the building ulterior
air (dehumidification), achieving a steady-state decontaminant
level (conditioning), performing the decontamination, and then
aerating for safe reentry (Figure 3.1).3
Dehumidification: Hydrogen peroxide vapor can co-condense
with water vapor producing an undesired condensate high in
hydrogen peroxide. High relative humidity (RH) and/or cold
temperatures are likely to permit condensation, but it can be
prevented by circulating dry, heated air through the interior
prior to injection of the hydrogen peroxide vapor. The target
humidity level is determined by the concentration of vapor to
be injected and the desired steady-state concentration for the
decontamination. The lower relative humidity permits a higher
concentration of hydrogen peroxide without reaching a saturation
point. For this study, the maximum RH at start-of-ran (prior to
introducing decontaminant) was 30%.
Conditioning: During the conditioning phase, the injection of
hydrogen peroxide vapor is initiated at a rapid rate to achieve the
desired chamber concentration set point without condensation.
Once the target concentration is achieved, the injection rate is
lowered to maintain the set-point concentration.
Decontamination: Decontamination is a timed process dependent
on the hydrogen peroxide vapor concentration. In actual building
applications, a decontamination tinier counts down from the
preset decontamination time. If the concentrations or temperature
values fall below the set point, the timer stops. This ensures
that during the decontamination phase the building interior is
exposed to at least the minimum decontamination conditions for
the desired exposure tune. For this laboratory-scale study, the
enclosure VHP concentration was maintained within the target
concentration range.
Aeration: After completion of the decontamination phase, the
hydrogen peroxide injection is tenninated. Air is introduced into
the chamber and displaces the hydrogen peroxide. The space is
monitored until the hydrogen peroxide concentration falls to a
safe level for coupon removal.
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Figure 3.1: The Steris VHP® Decontamination Cycle
1. Dehumidification
— 2. Conditioning
3. Decontamination
H2O
4. Aeration
Time
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Material compatibility testing was conducted in compliance with
the Quality Assurance Project and Work Plan4 developed under
the Quality Management Plans5'6 and EPA E4 quality system
requirements.7"9
4.1 Coupon Preparation
Test coupons were prepared in accordance with ASTM testing
requirements for material compatibility testing. The coupons
were cut from stock material IAW the procedure in Appendix
B of the QAPP11, which lias been reproduced as Appendix B of
this report. Coupons were prepared by obtaining a large enough
quantity of material that multiple test samples could be obtained
with uniform characteristics (e.g., test coupons were all cut from
the interior rather than the edge of a large piece of material).
The building materials studied, as well as supplier and coupon
dimensions, are provided in Table 4.1 and shown in Figure 4.1.
4.0
Experimental Method
Chain-of-custody (CoC) cards were used to ensure that the
test coupons were traceable throughout all phases of testing.
The coupons were measured and visually inspected prior to
testing to ensure that they were within the acceptable tolerances
(Appendix B) and were not defective and/or damaged. Coupon
measurements and visual inspection were recorded on the CoC
card. Coupons that were defective, damaged, or not within the
allowable size tolerances were discarded. Each coupon was
assigned a unique identifier code to match it with the sample,
test parameters, and sampling scheme (Appendix A). The code
was also recorded on the CoC cards, which followed each
sample from exposure testing through material compatibility
testing to disposal.
The material compatibility studies also investigated materials
related to electrical breaker connections such as intact one-pole
circuit breakers (HOM120, 2400 watts, 120/240 volts,
20 amperes).
Figure 4.1: Samples of the Test Coupons
'Coupons are not shown to scale
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Table 4.1: Representative Building Interior Materials
Material
Structural Wood, fir
Latex-Painted Gypsum Wallboard
Concrete Cinder Block
Carpet
Painted Structural Steel
Ceiling Suspension Tile, Acoustical
Code
w
G
C
R
S
T
Supplier
Home Depot
Home Depot
York Supply
Home Depot
Specialized Metals
Home Depot
Length
10.0 in
6.0 in
4.0 in
6.0 in
12.0 in
5.3 in
12.0 in
Width
1.5 in
6.0 in
8.0 in
8.0 in
2.0 in
0.8 in
3.0 in
Thickness
0.5 in
0.5 in
1.5 in
0.0 in
0.3 in
0.3 in
0.6 in
4.2 Coupon Exposure: Wood, Wallboard, Ceiling
Tile, Steel, Carpet, and Concrete Cinder Block
The process for exposing the building material samples to VHP
and results for die material demand study are documented in
a separate report titled "Material Demand Studies: Materials
Sorption of Vaporous Hydrogen Peroxide," by Lawrence Procell
et. al. This testing followed the operating procedures specific to
the Steris technology. A brief overview of the exposure process is
provided in this section; the material demand report contains the
detailed test information and results.
The coupons were placed in the exposure chamber. The RH
inside the glove box was regulated below 30% during the
dehumidification phase with dry air added as necessary. The
temperature during the decontamination phase was kept above
the minimum requirement of 30 °C. The vapor generator was
operated to maintain the chamber concentration within specified
ranges. The full-target concentration was 250-ppm VHP for four
hours for a total concentration-time (CT) value of 1000 ppm-
lirs. The half-target concentration was 125-ppm VHP for eight
hours, also for a total concentration-time (CT) value of 1000
ppm-hrs. Air exchange conditions were chosen to maximize the
residence time of the vapor in the chambers, while concurrently
minimizing the background vapor decomposition under baseline
conditions in the absence of materials. The VHP tests were
conducted with a turnover rate of approximately 16 exchanges
per hour to compensate for the higher spontaneous decomposition
of VHP. Aeration of the chamber was conducted following the
decontamination phase (exposure period) and continued until
the vapor concentration fell to^elow the levels required by the
Risk Reduction Office to ensure safe operation for personnel. The
coupons remained in the chamber until aeration was complete.
The standard measuring range of the VHP monitor is 0 to 10.0
ppm H,O2 with a display resolution of 0.1 ppm. Control samples
were prepared using the same procedure as the test runs except
with only air (no fumigant) through the chamber. Three replicate
runs were done for each sample at each condition. The samples
were removed from the chamber, marked with unique sample
identifier codes, and visually examined.
4.3 Coupon Exposure: Circuit Breakers
Like the building materials discussed in Section 4.2, the
circuit breakers (Hom220, Home Depot) were placed in the
exposure chamber and exposed to fumigant. After exposure to
the decontaminant, the circuit breakers were stored hi a fume
hood for two days and then placed in storage under load for
three months. Each set of circuit breakers was inserted into
an electrical box (8 spaces, 16 circuits, 100 amp max from
square D, Home Depot # 577-340). The circuit breaker box
was wired with 12-gauge, 20-amp wire into the 120-volt outlet.
Each circuit breaker was wired in series with an electrical lamp
(s513e) with an outlet box (sllOe) manufactured by Thomas &
Bretts (Home Depot # c214477 and b214426. respectively). The
load in each lamp was a Phillips 40-watt light bulb (Philips and
Sylvania, Home Depot). Current was applied to the circuits and
monitored. At the end of 90 days, the circuit breakers were tested
to determine the effect of VHP.
4.4 Visual Inspection
The coupons were visually inspected and digitally photographed
upon removal from the chamber. Visual inspection of the coupon
surfaces was conducted through side-by-side comparison of
the decontaminated test surface and fresh coupons of the same
test material. The testing staff looked for changes such as
discoloration, blistering, warping, and peeling on die test coupon.
After the visual inspection was completed, the coupon custody
was transferred to the Material Compatibility Technical Leader
for the three-month aging period and material compatibility
testing. The coupons were examined again at the time of the
material testing and the visual appearance recorded on the
data test forms. If the coupon had dramatic changes compared
to a fresh coupon, then the coupon was photographed and
the photograph was included in die report. Representative
photographs of each material type are provided in the report.
4.5 Coupon Aging
The material compatibility studies were conducted using the
coupons from the material demand study. The coupons were
aged for a minimum of 90 days following exposure to the
decontaminant prior to material compatibility testing. The
coupons were placed in open containers and stored under ambient
conditions. The open container arrangement allowed aging of the
coupons in conditions mimicking real-world aging.
4.6 Data Review and Technical Systems Audits
The approved Material Compatibility QAPP specified procedures
for the review of data and independent technical system audits.
All data were peer reviewed within two weeks of collection. The
project quality manager (or designee) was required to audit at
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least 10% of the data collected. Two technical system audits were
performed over the course of testing. A technical system audit is
a thorough, systematic, on-site qualitative audit of the facilities,
equipment, personnel, training, procedures, record keeping, data
validation, data management, and reporting aspects of the system.
4.7 Physical Testing
An Instron Model 5582 was used for the physical property
testing. The Instron is a universal testing machine capable of
performing tensile, compression, shear, peel, and flexural tests
on most materials and components. Each material subsection
contains a photograph of the coupon loaded into the test
apparatus. The Instron model 5582 specifications are listed in
Table 4.2.
4.8 Statistical Analyses
The data from the material compatibility testing phase of
the systematic decontamination program were subjected to a
statistical analysis to determine whether the differences observed
between the various test sets were merely the result of random
variations in test data or represented actual differences in the
performance of the materials as a result of exposure to fumigation
chemicals.
Methods used were from the statistical analysis functions
embedded within both the Microsoft Excel software and
Practical Statistics for Analytical Chemists, by Robert L.
Anderson, © 1987. Van Nostrand Reinhold Company.
First, the individual coupon test sets were tested for statistical
outliers that could be eliminated from the data. The DixorTs
Q-Test for outliers was first used to identify potential outliers
within a test group of coupons that had undergone similar
treatment (controls, half-target, or full-target exposures). If
an outlier was identified in the test group analysis, it was
eliminated and the statistics (averages and standard deviations)
were recalculated.
Once statistical outliers had been eliminated, the test groups
were analyzed to determine whether they were statistically
significantly different - that is. to determine whether the
treatment with the chosen fumigant had a detectable effect
on the sample.
Welch's T-test values were calculated to compare the test groups,
and results are reported for the 95% level of confidence. The
percent level of confidence reported indicates the confidence
that the two sample groups being compared are, in fact, different
and represent truly different samples. A 95% level of confidence
indicates a 5% chance that the two samples are, in fact, subparts
of the same population. If a comparison determines that a sample
is significantly different at the X% level of confidence, it is also
significantly different at any lower level of confidence.
Detection that a control and exposed sample are statistically
different implies that the treatment likely had some detectable
effect on the material. Statistically different results do not
imply that the material will fail as a result of treatment, unless
the material no longer meets specifications. In some cases,
measured values may vary by several percent: however, there is
no statistically detectable difference. It cannot be assumed that
this difference is real unless the difference is statistically detected
(e.g., by a Welch's T-test).
4.9 Chemical Testing: FTIR
The effects of decontaminant vapor on the cellulose and other
polymers in wood at the molecular level were studied using
a diffuse reflectance infrared Fourier transform (DRIFT)
technique. Chemical reactions between the decontaminant vapor
and the wood (i.e., oxidation and cleaving of the polymer chains)
can be evidenced by significant changes in the infrared spectra of
the wood. Fourier Transform Infrared Spectroscopy (FTIR) was
performed on twelve wood coupons to examine the substructural
oxidation effect of VHP and liquid hydrogen peroxide. Results of
these tests are provided in Section 13.0.
Table 4.2: Instron Model 5583 Specifications
Load Capacity:
Maximum Speed:
Minimum Speed:
Maximum Force at Full Speed:
Maximum Speed at Full Load:
Return Speed:
Position Control Resolution:
Total Crosshead Travel:
Total Vertical Test Space:
Height:
Width:
Depth:
Weight:
kN
Kgf
mm/min
mm/min
kN
nun/min
mm/min
(im
mm
mm
mm
mm
mm
kg
100
10000
500
0.001
75
250
600
0.06
1235
1309
2092
1300
756
862
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The coupons were visually inspected prior to fumigation (pre-
fumigation), immediately after fumigation (post-fumigation),
and after storage (post-storage) at the time of material testing.
Carpet coupons were inspected for any frayed tufts, pulled loops,
and other noticeable defects. Concrete coupons were inspected
for cracks, chips—particularly at the comers — any raised
ridge sections, and other noticeable defects. Steel coupons were
inspected for rust, peeling paint, any ridged sections on the small
I-beam cross section, and any other noticeable defects. Tile
5.0
Post-Fumigation Inspection
coupons were inspected for crashed comers and edges, and any
other noticeable defect. Wallboard coupons were inspected for
any damage to the paper section, as well as any other noticeable
defects. Wood coupons were inspected for any knots, missing
knots, splitting, and other noticeable defects. The post-fumigation
and post-storage inspections were compared to the initial (pre-
fumigation) inspections. No differences were observed for any of
the coupons after VHP exposure and aging compared to before
VHP exposure.
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6.0
Evaluation of Structural Steel
6.1 Introduction
The effects of VHP on die physical integrity of steel were
investigated using the tension test as described in ASTM Test
Method A370-03a "Standard Test Methods and Definitions
for Mechanical Testing of Steel Products," Sections 5-13. The
tension test was used to determine the integrity of steel coupons
exposed to vaporous decontaminant compared to unexposed
(control) steel coupons.
6.2 Sample Preparation and Testing
The steel samples were removed from storage, visually inspected,
and measured. The coupons from chamber positions 1, 4, 7,10,
and 16 were selected for testing in order to obtain representation
throughout the test chamber. The samples were used "as is"
without any additional preparation. The testing was conducted in
accordance with the ASTM Test Method A370-03a. The Instron
fixture for the steel test was installed prior to testing. The Instron
universal testing machine operation and calibration verification
was conducted by suspending a certified weight from the fixture
and recording the weight. Three sets of five coupons were tested
for each concentration (full-target and half-target) and four
sets were tested for the controls (0 pprn). The load required to
rupture the steel coupons was measured inNewtons (N). The
tensile strength is the maximum tensile stress that a material is
capable of sustaining and is calculated by dividing the amount
offeree required to rupture a specimen by the specimen cross-
sectional area. The cross-sectional area for the steel, dog bone
shaped coupon is the center width of the coupon multiplied by
the center thickness. No precision or bias requirements have
been established for this test method. The results for control
coupons were compared against the results for decontaminant-
exposed coupons. A statistical analysis of the data was conducted
to determine whether the decontaminant-exposed steel coupon
results were statistically different from the control steel coupon
results. A photograph of a representative steel sample before and
after testing is provided in Figure 6.1.
Figure 6.1 Photograph-Steel Coupon Test
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6.3 Results
The coupons were stored for at least 90 days after fumigation.
The actual number of storage days was based on the arrival
of the Instron fixtures for testing. The coupons for a particular
fumigation were studied after a similar number of days in storage.
Values for the load required to rapture the steel coupons, the
tensile strength results, and the number of days in storage before
testing are provided in Table 6.1.
6.4 Discussion
The steel studied was an A572 Grade 50 high-strength structural
steel. The minimum tensile strength requirement is 450 N/min2.
All coupons met this minimum specification.
A statistical analysis of the test group results was conducted to
detect potential statistical outliers (Q-test) and determine whether
there were any differences between the control and exposed
samples (Welch's T-test). Two test coupons were flagged for
having tensile strength values mat were outliers within their test
sets at the Q=0.99 confidence level: these values are highlighted
in orange in Table 6.1. However, within test groups (control
samples, half-target concentration samples, and full-target
concentration samples), statistical analysis showed that none of
the coupons could be eliminated as statistical outliers. Therefore,
all values were retained for the statistical analysis.
The average values for the maximum load for the test groups
were: 61744 ± 1597 N for the control coupons: 61811 ± 1337
N for the half-target coupons; and 61040 ± 437 N for the full-
target coupons. The average values for the tensile strength of the
steel coupons were as follows: 555 ± 19 N/mm2 for the control
coupons; 545 ± 23 N/imn2 for the half-target coupons; and 549 ±
15 N/rnin2 for the full-target coupons.
For both the half-target concentration and full-target
concentration samples, the average tensile strengths were slightly
lower than the control samples, but all were well over the
minimum acceptable value from the ASTM standard of 450 N/
mm2. The differences were statistically insignificant at the 95%
level of confidence.
-------
Table 6.1 VHP Steel Coupon Test Results
Maximum Load
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Coupon 5
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Tensile Strength
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Coupon 5
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Number of Days
in Storage
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Coupon 5
Test Set Average ±
Standard Deviation
Control Samples (0 ppm)
Tension Test Results, N
Test 1
SN50310
60975
60402
60577
59711
60725
60478
477
Test 2
SSN50622
65766
61079
62921
64075
61732
63115
1874
Test3
SN50228
61284
60997
60848
61109
60600
60968
260
Test 4
SSN50623
60627
62074
64483
61238
63661
62417
1622
61744 ±1597
Control Samples (0 ppm)
Tensile Strength, N/mm2
Test 1
SN50310
565
559
561
524
562
554
17
Test 2
SSN50622
577
509
552
562
542
548
26
Tests
SN50228
538
565
563
566
561
559
12
Test 4
SSN50623
532
545
566
567
589
560
22
555 ±19
Control Samples (0 ppm) Days
Test 1
SN50310
95
95
95
95
95
Test 2
SSN50622
98
98
98
98
98
Test3
SN50228
98
98
98
98
98
Test 4
SSN50623
97
97
97
97
97
97 ±1
Half-Target Concentration
(125-150 ppm) Results, N
Test 1
SV50420
61175
61559
60806
60731
60900
61034
338
Test 2
SV50603
62453
59570
61380
64594
63982
62396
2023
Tests
SV50606
60493
62283
62932
62046
62257
62002
907
61811 ±1337
Half-Target Concentration
(125-150 ppm) Results,
N/mm2
Test 1
SV50420
537
570
563
562
534
553
17
Test 2
SV50603
548
523
511
567
561
542
24
Tests
SV50606
531
577
552
544
494
540
30
545 ± 23
Half-Target Concentration
Days
Test 1
SV50420
107
107
107
107
107
Test 2
SV50603
96
96
96
96
96
Tests
SV50606
93
93
93
93
93
99 ±6
Target Concentration
(250-300 ppm) Results, N
Test 1
SV50405
60393
60655
61793
60245
61148
60847
631
Test 2
SV50517
60430
61194
61180
60959
61401
61033
371
Tests
SV50518
61121
61034
61321
61202
61524
61240
191
61040 ±437
Target Concentration
(250-300 ppm) Results, N/
mm2
Test 1
SV50405
559
562
572
558
566
563
6
Test 2
SV50517
530
537
537
535
539
535
•~i
j
Tests
SV50518
566
565
538
537
540
549
15
549 ±15
Target Concentration Days
Test 1
SV50405
92
92
92
92
92
Test 2
SV50517
104
104
104
104
104
Tests
SV50518
103
103
103
103
103
100 ±6
-------
-------
7.0
Evaluation of Gypsum Wallboard
7.1 Introduction
The effects of VHP on die physical integrity of gypsum wallboard
were investigated using die nail pull-dirough resistance test
method B as described in ASTM Test Method C473-03 "Standard
Test Methods for Physical Testing of Gypsum Panel Products"
Section 13. The test measures the ability of the wallboard to
resist nail pull-dirough by determining the load required to push
a standard nail through the wallboard. The ASTM test was used
to determine die integrity of gypsum wallboard coupons exposed
to vaporous decontaminant compared to unexposed (control)
gypsum wallboard coupons.
7.2 Sample Preparation and Testing
The gypsum wallboard samples were removed from storage,
visually inspected, and measured. The coupons from chamber
positions 1, 2, 4, 5, and 7 were selected for testing in order to
obtain representation throughout the test chamber. The samples
were brought to moisture equilibrium such that the weight of
the sample did not change by more titan 0.2% on successive
weighings at a minimum interval of two hours. The sample
preparation was conducted within a range of 15-25°C and
48-75% PJL The testing was conducted in accordance with
ASTM Test Method C473-03. The Lnstron fixture for the gypsum
wallboard test was installed prior to testing. The Instron universal
testing machine operation was verified by suspending a certified
weight from the fixture and recording the weight. Three coupons
were tested for each concentration (full-target and half-target),
and four sets were tested for the controls (0 ppm). The force
required to drive a nail shank tiirough the wallboard coupons was
measured in N, with five replicate measurements made for each
coupon (i.e., each coupon was punctured five times). The ASTM
method indicates that any coupon measurement in the series
that varies 15% more tiian the average needs to be discarded. If
15% of the coupons deviate from the average, the method states
that the test will be repeated. No additional precision or bias
requirements have been determined for this test by ASTM. The
results for the control coupons are compared against the results
for the decontaminant-exposed coupons. A statistical analysis of
the data was conducted to determine whether the decontaminant-
exposed coupon results were statistically different from the
control coupon results. A photograph of a representative gypsum
wallboard sample before and after testing (i.e., with holes) is
provided in Figure 7.1.
Figure 7.1 Photograph - Gypsum Wallboard Coupon Test
-------
7.3 Results
The coupons were stored for at least 90 days after fumigation.
The actual number of storage days was based on the arrival
of the Instron fixture for testing. The coupons for a particular
fumigation were studied at the same number of days. Values for
the load required to push the nail through the wallboard coupons
and number of days in storage before testing are provided in
Table 7.1.
7.4 Discussion
A statistical analysis of the test group results was conducted to
detect potential statistical outliers (Q-test) and determine whether
there were any differences between the control and exposed
samples (Welch's T-test). Although there was a great deal of
scatter in the data (the standard deviations of the results were
between 14 and 22% of the mean value within the various test
groups), none of the individual coupons was determined to be
outliers at the Q=0.99 confidence level.
The average tension test results were 48.6 ± 7.0 N for the control
group, 56.6 ± 12.8 N for the half-target group, and 63.3 ± 9.5
N for the full-target group. The Welch's T-test was used to
determine whether there were statistically significant differences
among the test groups (control, half-, and full-target). The control
test group was statistically significantly different from the full-
target and the half-target test groups at the 95% confidence level.
However, the half-target and full-target test groups were not
significantly different at the 95% level of confidence.
These test methods show that exposure to VHP has statistically
significant effects on the maximum load of wallboard coupons as
determined by the ATSM test method. Exposure to either VHP
fumigation resulted in an increase in the ability of the wallboard
to resist nail pull-through. However, this test does not indicated
whether this decrease in maximum load would result in failure of
installed wallboard after fumigation.
Table 7.1 Gypsum Wallboard Coupon Test Results for Maximum Load
VHP
Coupon set
Hole 1
Hole 2
Hole 3
Hole 4
Hole 5
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Control Samples (0 ppm)
Tension Test Results, N
Test 1
GN50303
47.2
53.8
64.1
56.6
55.4
7.0
Test 2
GN50401
40.2
42.5
41.3
36.5
45.6
41.2
3.3
Tests
GN50620
59.1
45.3
55.3
47.2
45.0
50.4
6.4
Test 4
GN50621
48.1
47.5
46.0
52.7
54.4
49.7
3.6
48.6 ±7.0
Target Concentrations
(250-300 ppm) Results, N
Test 1
GV50421
71.8
72.7
67.5
60.2
58.8
66.2
6.4
Test 2
GV50526
70.2
62.4
72.8
83.2
70.7
71.8
7.5
Tests
GV50531
56.3
51.0
53.5
54.0
53.3
53.6
1.9
63.3 ±9.5
Half-Target Concentration
(125-150 ppm) Results, N
Test 1
GV50407
60.7
61.6
75.3
78.7
71.4
69.5
8.1
Test 2
GV50505
65.6
64.4
54.5
65.9
52.3
60.5
6.6
Tests
GV50506
46.5
37.1
43.5
48.8
40.9
43.3
4.6
56.6 ±12.8
-------
8.0
Evaluation of Acoustical Ceiling Tile
8.1 Introduction
The effects of VHP on die physical integrity of ceiling tile were
investigated using the transverse strength test as described
in ASTM Test Method C367-99 "Standard Test Methods for
Strength Properties of Prefabricated Architectural Acoustical Tile
or Lay-In Ceiling Panels" Sections 1, 3-5, and 21-29. The test
measures the force required to cause the tile to break. The ASTM
test was used to determine the integrity of ceiling tile coupons
exposed to vaporous decontaniinant compared to unexposed
(control) ceiling tile coupons.
8.2 Sample Preparation and Testing
The acoustical ceiling tile samples were removed from storage,
visually inspected, and measured. The samples were brought to
moisture equilibrium such that die weight of the sample did not
change by more than 1% on successive weighings at a minimum
interval of two hours. The sample preparation was conducted
widiin a range of 18-24 °C and 48-75% RH. The testing was
conducted in accordance with ASTM Test Method C367-99.
The Instron fixture for die ceiling tile test was installed prior
to testing. The Instron universal testing machine operation
was verified by suspending a certified weight from the fixture
and recording die weight. For each test the coupons from
chamber positions 1 through 8 were selected for testing; this
selection resulted in placing all coupons in the chamber during
a single fumigation trial. Ceiling tile coupons were tested in
two directions — witii the mandrel parallel to die axis of die
test machine (hereafter referred to as "machine direction") and
witii die mandrel perpendicular to die axis ("cross-machine
direction"). Three sets of four machine-direction coupons and
four cross-machine direction coupons were tested for each
concentration (0 ppm, target, and half-target). The load required
to break die ceiling tile coupons was measured in N. Figure 8.1
shows a photograph of a coupon loaded into die Instron for the
machine direction and cross-machine direction tests. No precision
or bias requirements have been established for this test method.
The results for the control coupons have been compared to the
results for the decontaminant-exposed coupons. A statistical
analysis of die data was conducted to determine whether the
decontaminant exposed coupon results were statistically different
from die control coupon results.
The Modulus of Rupture (MOR) was calculated according to die
test method, using die following equation:
MOR units N/mm2 (lb/in2) =
3 x P x L
2xbxd2
where P is the maximum load, N (Ibf)
L is die lengdi of span, mm (in.)
b is die specimen width, nun (in.)
d is die specimen tiiickness, mm (in.)
Figure 8.1 Photograph - Acoustical Ceiling Tile Coupon Test
Cross-Machine Direction
-------
8.3 Results
The coupons were stored for at least 90 days after fumigation.
The actual number of storage days was based on the arrival
of the Instron fixture for testing. The coupons for a particular
fumigation were studied at the same number of days. A
photograph of a representative ceiling tile sample before and after
testing is provided in Figure 8.2. Values for the load required to
rupture the ceiling tile coupons, the ceiling tile coupon MOR
results, and number of days in storage are provided Table 8.1.
8.4 Discussion
A statistical analysis of the individual test results was conducted
to detect potential statistical outliers (Q-test) and determine
whether there were any differences between the control and
exposed samples (Welch's T-test). None of the coupons could
be eliminated as statistical outliers from within their individual
test sets or test groups (control, half-target concentration, or full-
target concentration samples) at the Q=0.99 level of confidence.
For the machine-direction tests, the maximum load values were
as follows: 35.23 ± 4.92 N for the controls, 40.76 ± 5.20 N for
the half-target coupons, and 36.63 ± 4.07 N for the full-target
coupons. The moduli of rupture were: 0.82 ± 0.11 N/mm2 for the
controls. 0.97 ± 0.15 N/mm2 for the half-target, and 0.82 ±0.11
N/mm2 for the full-target coupons.
For the cross-machine tests, the maximum load values were as
follows: 28.83 ± 5.02 N for the controls, 32.18 ± 3.22 N for
the half-target coupons, and 27.23 ± 3.69 N for the full-target
coupons. The moduli of rupture were: 0.67 ± 0.12 N/mm2 for the
controls. 0.76 ± 0.07 N/mm2 for the half-target, and 0.62 ± 0.08
N/mm2 for the full-target coupons.
In all cases, the cross-machine test results were lower than those
in the machine direction orientation.
With regard to the individual coupon sets tested, there were
obvious variations among the test groups (control, half-target
exposure, or full-target exposure). In both the machine direction
and cross-machine tests, the half-concentration coupons had
higher maximum loads and moduli of rupture. For the machine
direction tests, the half-target results were significantly different
from the results for both the control test coupons and the full-
target coupons at a 95% confidence level. The control coupons
and full-target coupons were not, however, significantly different
at the 95% confidence level.
For the cross-machine tests, the control coupons were not
significantly different from either the half- or full-target coupons
at the 95% level of confidence.
From these test methods, it is not clear that the VHP fumigation
process has, overall, a statistically significant effect on the
maximum load and the modulus of rupture of acoustic
ceiling tile. The maximum load and modulus of rupture did
increase due to long exposure (8 hours) at the lower concentration
(150 ppm); however, die effect was only significant in the
machine-direction tests.
Figure 8.2 Representative Break - Acoustical Ceiling Tile Coupons
-------
Table 8.1 VHP Coupon Test Results for Tile
Maximum Load
Machine Direction
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Pest Average
Standard Deviation
Test Set Average ±
Standard Deviation
Modulus of Rupture
Machine Direction
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Maximum Load
Cross-Machine
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Modulus of Rupture
Cross-Machine
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Number of Days
in Storage
Coupon set
Test Set Average ±
Standard Deviation
Control Samples (0 ppm)
Tension Test Results, N
Test 1
TN50307
36.00
30.28
32.16
33.62
33.02
2.41
Test 2
TN50610
37.11
41.46
41.72
27.11
36.85
6.83
Tests
TN50613
28.74
40.05
35.61
38.88
35.82
5.08
35.23 ±4.92
Control Samples (0 ppm)
Tensile Strength, N/mm2
Test 1
TN50307
0.83
0.69
0.74
0.78
0.76
0.06
Test 2
TN50610
0.86
0.96
0.97
0.63
0.85
0.16
Test 3
TN50613
0.67
0.93
0.82
0.90
0.83
0.12
0.82 ±0.11
Control Samples (0 ppm)
Tension Test Results, N
Test 1
TN50307
20.08
25.63
23.33
24.38
23.36
2.38
Test 2
TN50610
29.97
30.15
26.17
37.15
30.86
4.58
Test3
TN50613
30.85
34.15
30.07
34.00
32.27
2.11
28. 83 ±5.02
Control Samples (0 ppm)
Tensile Strength, N/mm2
Test 1
TN50307
0.47
0.59
0.54
0.56
0.54
0.05
Test 2
TN50610
0.69
0.70
0.61
0.86
0.71
0.11
Test3
TN50613
0.71
0.79
0.70
0.79
0.75
0.05
0.67 ±0.12
Control Samples (0 ppm) Days
Test 1
TN50307
191
Test 2
TN50610
284
Tests
TN50613
281
252 ± 53
Half-Target Concentration
(125-150 ppm) Results, N
Test 1
TV50418
45.12
44.01
39.09
45.36
43.40
2.93
Test 2
TV50511
48.61
37.78
36.73
34.38
39.38
6.32
Tests
TV50601
45.00
43.26
31.50
38.22
39.50
6.06
40.76 ± 5.20
Half-Target Concentration
(125-150 ppm) Results, N/mm2
Test 1
TV50418
1.05
1.02
0.89
1.05
1.00
0.07
Test 2
TV50511
1.31
0.88
1.00
0.80
0.99
0.22
Tests
TV50601
1.04
1.00
0.73
0.89
0.91
0.14
0.97±0.15
Half-Target Concentration
(125-150 ppm) Results, N
Test 1
TV50418
40.17
30.74
30.98
28.69
32.65
5.12
Test 2
TV50511
34.79
28.86
33.82
33.40
32.72
2.64
Tests
TV50601
31.47
31.06
33. 10
29.08
31.18
1.65
32. 18 ±3.22
Half-Target Concentration
(125-150 ppm) Results, N/mm2
Test 1
TV50418
0.93
0.71
0.72
0.66
0.76
0.12
Test 2
TV50511
0.81
0.78
0.78
0.78
0.79
0.01
Tests
TV50601
0.73
0.72
0.77
0.67
0.72
0.04
0.76 ± 0.07
Half-Target Concentration Days
Test 1
TV50418
184
Test 2
TV50511
183
Tests
TV50601
299
222 ± 67
Target Concentration
(250-300 ppm) Results, N |
Test 1
TV50316
33.27
30.40
40.17
33.52
34.34
4.14
Test 2
TV50427
39.54
33.40
35.46
42.76
37.79
4.18
Test 3
TV50428
41.34
40.98
33.96
34.73
37.75
3.95
36.63 ±4.07
Target Concentration
(250-300 ppm) Results, N/mm2
Test 1
TV50316
0.77
0.70
0.93
0.78
0.80
0.10
Test 2
TV50427
0.92
0.77
0.82
0.99
0.88
0.10
Tests
TV50428
0.96
0.83
0.69
0.69
0.79
0.13
0.82 ±0.11
Target Concentration
(250-300 ppm) Results, N
Test 1
TV50316
25.19
23.17
27.38
31.54
26.82
3.59
Test 2
TV50427
23.80
22.55
34.69
30.17
27.80
5.68
Tests
TV50428
24.86
26.93
26.67
29.84
27.08
2.06
27.23 ±3.69
Target Concentration
(250-300 ppm) Results, N/mm2
Test 1
TV50316
0.58
0.54
0.63
0.73
0.62
0.08
Test 2
TV50427
0.55
0.52
0.80
0.70
0.64
0.13
Test 3
TV50428
0.58
0.62
0.62
0.60
0.60
0.02
0.62 + 0.08
Target Concentration Days
Test 1
TV50316
189
Test 2
TV50427
189
Tests
TV50428
188
189 ± 1
-------
-------
9.1 Introduction
The effects of VHP on die physical integrity of loop pile carpet
fibers were investigated using ASTM Test Method C1335-
03 "Standard Test Method for Tuft Bind of Pile Yam Floor
Coverings." The method determines the force required to pull
out a tuft of a pile yarn from a floor-covering sample. The ASTM
test was used to determine the integrity of loop pile carpet fibers
exposed to vaporous decontaminant compared to unexposed
(control) loop pile carpet fibers.
9.2 Sample Preparation
The carpet samples were removed from storage, visually
inspected, and measured. The coupons from chamber positions
1,3,4, 5, and 7 were selected for testing in order to obtain
representation throughout the test chamber. The samples
were brought to moisture equilibrium such that the weight of
the sample did not change by more than 0.2% on successive
weighings at a minimum interval of two hours. The sample
9.0
Evaluation of Carpet
preparation was conducted within a range of 15-24 °C and
48-75% RH. The testing was conducted in accordance with
ASTM Test Method D1335-03. The Instron fixture for the carpet
test was installed prior to testing. The Instron universal testing
machine operation and calibration verification was conducted
by suspending a certified weight from the fixture and recording
the weight. Three sets of five coupons were tested for each
concentration (full-target and half-target) and four sets were
tested for the controls (0 ppm). The load required to pull a carpet
loop from the binding was measured in N, and five replicate
measurements were made for each coupon. No bias requirements
have been established for this test method. The results for control
coupons were compared to the results for decontaminant-exposed
coupons. A statistical analysis of the data was conducted to
determine whether the decontaminant-exposed coupon results
were statistically different from the control coupon results. A
photograph of a representative carpet sample before and after
testing is provided in Figure 9.1
Figure 9.1 Photograph - Carpet Coupon Test
Direction t
of Force
t
-------
9.3 Results
The coupons were stored for at least 90 days after fumigation.
The actual number of storage days was based on the arrival
of the Instron fixture for testing. The coupons for a particular
fumigation were studied at the same number of days. Values
from the carpet tuft bind results and number of days in storage
are provided in Table 9.1.
9.4 Discussion
A statistical analysis of the individual test results was conducted
to detect potential statistical outliers (Q-test) and determine
whether there were any differences between the control and
exposed samples (Welch's T-test). Although there was a great
deal of scatter in the data (the standard deviations of the results
were 25% of the mean value within the various test groups),
none of the coupons was determined to be outliers at the
Q=0.99 confidence level.
The values for the average tuft bind for the groups of coupons
were as follows: 14.8 ± 3.7 N for the control coupons, 16.8 ±
4.0 N for the half-target coupons, and 15.3 ± 3.7 N for the full-
target coupons.
There are variations among the test groups (control, half-target
exposure, or full-target exposure) at the 95% confidence level.
While the difference between the control group and the full-
target group are statistically insignificant, the half-target values
are statistically different from the controls and full-target groups.
The results suggest that VHP fumigation at the half-target
concentration for long exposure times (8 hours) may have an
effect on the tuft bind tests of carpet coupons as determined by
our test methods. The fumigation made it more difficult, i.e..
greater bind force was necessary, to pull a tuft out of the test
carpet used in this study.
-------
Table 9.1 Carpet Coupon Test Results for Average Tuft Bind - VHP Control Samples
Turf Bind Force
Coupon
Loop 1
Loop 2
Loop 3
Loop 4
jOop 5
lest Average
Standard Deviation
)ays in Storage
Coupon
Loop 1
Loop 2
Loop 3
Loop 4
Loop 5
Test Average
Standard Deviation
Days in Storage
Test Set Average ±
Standard Deviation
Turf Bind Force
Coupon
Loop 1
Loop 2
Loop 3
Loop 4
Loop 5
Test Average
Standard Deviation
Days in Storage
Test Set Average ±
Standard Deviation
Turf Bind Force
Coupon
Loop 1
Loop 2
Loop 3
Loop 4
Loop 5
Test Average
Standard Deviation
Days in Storage
Test Set Average ±
Standard Deviation
Control Sample (0 ppm) Results, N
RN50309
#1
12.5
14.9
10.8
12.7
2.0
#2
15.9
13.1
13.7
14.3
1.5
#3
14.7
8.0
14.1
8.9
19.2
13.0
4.6
#4
11.0
15.9
9.2
14.3
12.6
3.0
#5
9.5
16.2
12.5
14.1
13.1
2.9
147
RN50615
#1
11.9
18.7
10.0
19.2
14.9
14.9
4.1
#2
17.1
10.9
10.6
17.6
10.7
13.4
3.6
#3
13.4
15.4
16.6
15.2
1.6
#4
19.0
13.6
13.0
16.2
15.5
15.5
2.4
#5
18.2
14.1
10.5
11.9
16.1
14.1
3.1
147
RN50309
#1
12.5
14.9
10.8
12.7
2.0
ffl
15.9
13.1
13.7
14.3
1.5
#3
14.7
8.0
14.1
8.9
19.2
13.0
4.6
#4
11.0
15.9
9.2
14.3
12.6
3.0
#5
9.5
16.2
12.5
14.1
13.1
2.9
147
RN50614
#1
21.9
13.7
19.0
15.3
16.9
17.3
3.2
#2
23.1
21.6
20.2
18.3
20.8
2.0
#3
24.4
18.9
16.5
14.1
15.0
17.8
4.1
#4
12.2
8.4
14.3
11.6
3.0
#5
9.6
18.0
13.8
13.1
18.6
14.6
3.7
148
14.8 ±3.7
Target Concentration (250-300 ppm) Results, N
RV50419
#1
11.2
18.0
16.0
19.2
16.2
16.1
3.0
#2
12.5
12.9
11.0
12.1
1.0
#3
15.3
10.0
15.6
11.6
13.1
2.8
#4
19.8
13.0
19.8
20.7
17.7
18.2
3.1
#5
10.4
14.2
16.5
18.4
16.6
15.2
3.1
147
RV50519
#1
10.5
19.1
20.7
23.5
12.5
17.2
5.6
#2
15.1
21.8
15.5
12.8
21.3
17.3
4.0
#3
11.5
8.3
11.6
10.5
1.8
#4
18.0
12.2
14.0
14.7
2.9
#5
21.3
15.8
14.1
16.8
16.2
16.8
2.7
148
RV50520
#1
16.8
12.5
18.0
15.7
2.8
#2
16.5
17.3
14.1
16.0
1.6
#3
16.6
11.9
10.3
10.2
12.2
3.0
#4
10.0
21.7
17.6
11.3
18.4
15.8
5.0
#5
13.1
11.2
14.6
13.0
1.7
147
15.3 ±3. 7
Half-Target Concentration (125-150 ppm) Results, N
RV50321
#1
#2
12.0
20.7
12.2
15.1
19.9
16.0
4.2
#3
14.7
20.7
10.9
16.0
23.6
17.2
5.0
#4
16.5
16.2
19.4
17.4
1.8
#5
12.2
19.1
14.5
18.2
15.0
15.8
2.8
161
RV50429
#1
15.3
18.8
12.3
22.4
16.9
17.1
3.8
#2
16.8
23.7
15.8
26.2
25.5
21.6
4.9
#3
12.7
13.0
19.0
20.7
20.3
17.1
4.0
#4
25.6
16.3
18.3
14.6
21.7
19.3
4.4
#5
15.1
21.2
19.2
15.7
17.8
2.9
152
RV50502
#1
17.7
19.4
13.1
14.0
16.0
3.0
#2
11.0
18.2
7.7
18.5
18.5
14.8
5.1
#3
13.0
10.6
19.0
15.7
11.7
14.0
3.4
#4
13.2
13.5
15.9
14.2
1.5
#5
15.9
14.8
13.8
14.8
1.1
149
16.8±4.0
Note: The cells highlighted in gray are samples that were not required to be analyzed, due to meeting the test method
sampling criteria of ±15%.
-------
-------
10.0
Evaluation of Concrete Cinder Block
10.1 Introduction
The effects of VHP on the physical integrity of concrete cinder
block coupons were investigated using the compression test
as described in ASTM Test Method C140-03 "Standard Test
Methods for Sampling and Testing Concrete Masonry Units
and Related Units." The ASTM test was used to determine
the integrity of the concrete cinder block coupons exposed
to vaporous decontaminant compared to unexposed (control)
concrete cinder block coupons.
10.2 Sample Preparation and Testing
The concrete cinder block samples were removed from storage,
visually inspected, and measured. The coupons from chamber
positions 1, 4, and 7 were selected for testing hi order to obtain
representation throughout the test chamber. The samples were
placed in an environmental range of 16-32 °C and less than
80% RH for 48 hours prior to testing. The testing was conducted
in accordance with ASTM Test Method C140-03. The Instron
fixture for the concrete cinder block test was installed prior to
testing. A photograph of a concrete cinder block coupon loaded
into the Instron test apparatus is shown in Figure 10.1. The
Instron universal testing machine operation and calibration
verification was conducted by suspending a certified weight from
the fixture and recording the weight. Three sets of three coupons
were tested for each concentration (0 pprn, full-target, and half-
target). The load required to rupture the coupons was measured
in kgf/mm2 and can be found in Table 10.1. No precision or bias
requirements have been established for this test method. The
results for control coupons were compared to the results for
decontaminant-exposed coupons. A statistical analysis of the
data was conducted to determine whether the decontaminant-
exposed coupon results were statistically different from the
control coupon results.
Figure 10.1 Photograph - Concrete "Cinder Block" Coupon Test
-------
10.3 Results
The coupons were stored for at least 90 days after fumigation.
The actual number of storage days was based on the arrival
of the Instron fixture for testing. The coupons for a particular
fumigation were studied at the same number of days. A
photograph of a representative concrete cinder block sample
before and after testing is provided in Figure 10.2. The coloring
difference between the samples in the picture is a result of room
lighting and is not real. Both samples were taken on the same
blue color mat. Values for the load required to crush the concrete
cinder block coupons, the coupon gross area compressive
strength results, and number of days in storage are provided in
Table 10.1. The concrete cinder block is a heterogeneous material
sample to sample. The break patterns varied from sample to
sample; a photograph of each sample is provided in Appendix D.
10.4 Discussion
A statistical analysis of the individual test results was conducted
to detect potential statistical outliers (Q-test) and determine
whether there were any differences between the control and
exposed samples (Welch's T-test). None of the coupons could
be eliminated as statistical outliers from within their individual
test sets or test groups (control, half-target concentration, or full-
target concentration samples) at the Q=0.99 level of confidence.
A Welch's T-test evaluation of the data for both maximum load
and gross area compressive strength indicated that there were
no statistically significant differences among die means of the
exposed and control samples at the 95% confidence level. These
test methods indicated that exposure to VHP had no significant
effect on the maximum load or the gross area compressive
strength of cinder blocks.
Figure 10.2 Representative Concrete Coupons Before and After Testing
Before Testing
Coupon 0/5060201
After Testing
-------
Table 10.1 VHP Coupon Test Results for Concrete Cinder Block
Maximum Load
Coupon set
Coupon 1
Coupon 2
Coupon 3
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Gross Area
Compressive
Strength
Coupon set
Coupon 1
Coupon 2
Coupon 3
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Number of Days
in Storage
Coupon set
Coupon 1
Coupon 2
Coupon 3
Test Set Average ±
Standard Deviation
Control Samples (0 ppm) kgf
Test 1
CN50331
4084
4686
4512
4427
310
Test 2
CN50617
3869
4491
4731
4364
445
Tests
CN50616
2905
1932
3432
2757
761
3 849 ±944
Control Samples
(0 ppm) kgf/mm2
Test 1
CN50331
3.2
3.6
4.0
3.6
0.4
Test 2
CN50617
1.8
2.1
2.2
2.0
0.2
Tests
CN50616
1.5
0.9
1.8
1.4
0.4
2.3 ±1.0
Control Sample (0 ppm) Days
Test 1
CN50331
104
104
104
Test 2
CN50617
328
328
328
Tests
CN50616
104
104
104
179 ±112
Half-Target Concentration
(125-150 ppm) Results, kgf
Test 1
CV50524
5094
2634
2993
3574
1329
Test 2
CV50525
5902
4317
4330
4850
911
Tests
CV50602
4583
5026
3988
4532
521
43 19 ±1024
Half-Target Concentration
(125-150 ppm)
Results, kgf/mm2
Test 1
CV50524
2.6
1.3
1.4
1.8
0.7
Test 2
CV50525
2.8
2.2
2.3
2.4
0.3
Tests
CV50602
2.3
2.4
2.1
2.3
0.1
2.2 ±0.5
Half-Target Concentration
Days
Test 1
CV50524
163
163
163
Test 2
CV50525
162
162
162
Tests
CV50602
137
137
137
154 ±13
Target Concentration
(250-300 ppm) Results, kgf
Test 1
CV50404
2800
3598
2614
3004
523
Test 2
CV50503
4378
4165
4050
4197
167
Tests
CV50504
3286
2935
3670
3297
367
3500 ±632
Target Concentration
(250-300 ppm)
Results, kgf/mm2
Test 1
CV50404
2.5
3.7
2.3
2.8
0.8
Test 2
CV50503
2.3
2.1
2.3
2.2
0.1
Tests
CV50504
2.0
2.0
1.9
2.0
0.1
2.3 ±0.5
Target Concentration Days
Test 1
CV50404
100
100
100
Test 2
CV50503
118
118
118
Tests
CV50504
117
117
117
112 ±9
-------
-------
11.1 Introduction
The effects of VHP on the physical integrity of wood were
investigated using the bending edge-wise test as described in
ASTM Test Method D4761-02a "Standard Test Methods for
Mechanical Properties of Lumber and Wood-Base Structural
Material," Sections 6-11. The ASTM test was used to
determine the integrity of wood coupons exposed to vaporous
decontaminant compared to unexposed (control) wood coupons.
11.2 Sample Preparation
The wood samples were removed from storage, visually
inspected, and measured. The coupons from chamber positions
1, 4, 7, 10, and 14 were selected for testing in order to obtain
representation throughout the test chamber. The samples
were brought to moisture equilibrium such that the weight of
the sample did not change by more than 0.2% on successive
11.0
Evaluation of Wood
weighings at a minimum interval of two hours. The sample
preparation was conducted within a range of 15-25 °C and
48-75% RH. The testing was conducted in accordance with
ASTM Test Method D4761-02a. The Instron fixture for the
wood test was installed prior to testing. The Instron universal
testing machine operation and calibration verification was
conducted by suspending a certified weight from the fixture and
recording the weight. Three sets of five coupons were tested
for each concentration (0 ppui, full-target, and half-target). The
load required to rupture the wood coupons was measured in
N. The setup of the Instron for testing the wood furrings can
be seen in Figure 11.1. No precision or bias requirements have
been established for this test method. The results for control
coupons were compared to the results for decontaminant-exposed
coupons. A statistical analysis of the data was conducted to
determine whether the decontaminant-exposed coupon results
were statistically different from the control coupon results.
Figure 11.1 Photograph - Wood Coupon Test
-------
11.3 Results
The coupons were stored for at least 90 days after fumigation.
The actual number of storage days was based on the arrival
of the Instron fixtures for testing. The coupons for a particular
fumigation were studied at the same number of days. A
photograph of a representative wood sample before and after
testing is provided in Figure 11.2. The wood coupon results for
the required load and time to break, moisture content, and number
of days in storage are provided in Table 11.1. The wood samples
vary slightly in knot and grain pattern from sample to sample.
The break patterns varied from sample to sample; a photograph
of each sample is provided in Appendix C.
11.4 Discussion
A statistical analysis of the individual test results was conducted
to detect potential statistical outliers (Q-test) and determine
whether there was a difference between the control and exposed
samples (Welch's T-test). Within the target concentration test
group, two coupons were outliers within their test sets with
respect to both maximum force required to break and time-
to-break values at the Q=0.99 confidence level. Of these two
outliers, only Coupon 5 of Test 2 was an outlier within the entire
test group of 15 coupons. This value was removed from the data
sets before statistical analysis was performed. The moisture
content of Coupon 4 of Test Set 2 for the half-target concentration
test group was also noted as an outlier; however, it was not an
outlier when considering the entire test group. Therefore, this
value was retained.
With regard to the data from the test groups of coupons, the
average maximum load values for the VHP-exposed coupons
increased by 11-18% over the value for the control sets for both
half-target concentration sets and full-target concentration sets.
The time-to-break values for the exposed coupons were also
higher (3-18%), but the moisture content values showed no trend.
The average maximum force value for the control samples was
4006 ± 861 N. The half-target concentration samples had an
average maximum force value of 4431 ± 929 N (an increase
of 10.6%), while the full-target concentration samples had an
average maximum force value of 4725 ± 732 N (an increase of
17.9%).
The average tirne-to-break value for the control coupons was
3.9 ± 0.9 seconds. The half-target concentration coupons had an
average time-to-break of 4.0 ± 0.9 seconds, and the full-target
concentration coupons had an average time-to-break of 4.6 ± 0.7
seconds.
The average change in moisture content for the control samples
after storage was -0.02 ± 0.13%. For the half-target concentration
coupons, the average change in moisture content was +0.48 ±
0.52, and for the full-target concentration coupons the average
change in moisture was -0.06 ± 0.13%.
The differences between the control samples and full-target
concentration coupons with respect to the maximum force and
time-to-break were statistically significant at the 95% confidence
level. The half-target concentration samples were not statistically
different from the controls.
The results suggest that VHP fumigation at the full-target
conditions may have impacted the wood used for this study,
according to the ASTM test method. The fumigation appeared to
increase the force and time required to break the wood.
Figure 11.2 Representative Wood Coupon Before and After Testing
-------
Table 11.1 VHP Coupon Test Results for Wood
Maximum Force
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Coupon 5
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Time to Break
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Coupon 5
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Moisture Content
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Coupon 5
Test Average
Standard Deviation
Test Set Average ±
Standard Deviation
Number of Days in
Storage
Coupon set
Coupon 1
Coupon 2
Coupon 3
Coupon 4
Coupon 5
Test Set Average ±
Standard Deviation
Control Sample (0 ppm) N
Test 1
WN50304
4562
3782
4539
3858
4076
4163
369
Test 2
WN50608
4766
4739
3560
4177
3136
4076
721
Test3
WN50609
2475
2888
3038
5312
5175
3777
1355
4006 ±861
Control Sample
(0 ppm) minutes
Test 1
WN50304
4.6
3.8
4.5
3.9
4.1
4.2
0.4
Test 2
WN50608
4.6
4.5
3.3
3.9
2.7
3.8
0.8
Test3
WN50609
2.4
2.7
2.9
5.3
5.2
3.7
1.4
3.9 ±0.9
Control Sample (0 ppm) %
Test 1
WN50304
0.15
0.09
0.20
0.12
0.18
0.15
0.04
Test 2
WN50608
-0.12
-0.07
-0.18
-0.12
-0.10
-0.12
0.04
Tests
WN50609
-0.12
-0.10
-0. 19
-0.06
0.02
-0.09
0.08
-0.02 ±0.13
Control Sample (0 ppm) Days
Test 1
WN50304
138
138
138
138
138
Test 2
WN50608
145
145
145
145
145
Tests
WN50609
144
144
144
144
144
142 ±3
Half-Target Concentration
(125-150 ppm) Results, N
Test 1
WV50415
3038
4014
3977
5752
4696
4295
1006
Test 2
WV50509
2873
4389
4877
3717
4842
4140
849
Tests
WV50510
6306
4542
4174
3938
5323
4857
965
4431 ±929
Half-Target Concentration
(125-150 ppm) Results, minutes
Test 1
WV50415
3.0
4.0
4.0
5.8
4.7
4.3
1.0
Test 2
WV50509
2.9
3.5
3.8
3.6
4.5
3.7
0.6
Tests
WV50510
5.5
3.6
3.4
3.3
4.9
4.1
1.0
4.0 ±0.9
Half-Target Concentration
(125-150 ppm) Results, %
Test 1
WV50415
-0.10
-0.16
-0.17
-0.05
-0.15
-0.13
0.05
Test 2
WV50509
1.04
0.96
0.91
-0.13
0.93
0.74
0.49
Tests
WV50510
0.83
0.88
0.83
0.75
0.84
0.83
0.05
0.48 ±0.52
Half-Target Concentration, Days
Test 1
WV50415
136
136
136
136
136
Test 2
WV50509
143
143
143
143
143
Tests
WV50510
142
142
142
142
142
142 ± 10
Target Concentration
(250-300 ppm) Results, N
Test 1
WV50406
4730
4951
5045
4862
6428
5203
695
Test 2
WV50425
4400
5153
4919
4287
1305
4013
1556
Tests
WV50426
4202
3023
4715
4394
5040
4275
769
4725 ± 732
Target Concentration
(250-300 ppm) Results, minutes
Test 1
WV50406
4.7
5.0
5.0
4.9
6.4
5.2
0.7
Test 2
WV50425
4.1
4.9
4.6
4.2
1.3
3.8
1.4
Tests
WV 50426
4.1
3.0
4.7
4.3
4.8
4.2
0.7
4.6 ±0.7
Target Concentration
(250-300 ppm) Results, %
Test 1
WV50406
0.12
-0.02
0.14
0.08
0.16
0.10
0.07
Test 2
WV50425
-0.05
-0.19
-0.15
-0.15
-0.19
-0.15
0.06
Test 3
WV50426
-0.22
-0.15
-0.13
-0.02
-0.11
-0.12
0.07
-0.06 ±0.13
Target Concentration, Days
Test 1
WV50406
145
145
145
145
145
Test 2
WV50425
189
189
189
189
189
Tests
WV50426
188
188
188
188
188
176 ±21
Note: The values highlighted in orange were determined to be outliers within their individual test sets but not within their individual
test groups at the Q=0.99 confidence level. The values highlighted in red were determined to be outliers within the test set and test
group and were, therefore, removed from the data set prior to statistical analysis.
-------
-------
12.0
Evaluation of Electrical Circuit Breakers
12.1 Introduction
The impact of fumigant and humidity on die performance of
electrical circuit breakers was also investigated in this study. This
investigation involved circuit breakers prepared as baseline, test,
and control. Baseline circuit breakers are the "as-purchased"
circuit breakers. The test circuit breakers were prepared in the
exposure chambers using fumigant. The control circuit breakers
were prepared in the exposure chambers using a temperature and
relative humidity profile similar to that of the test breakers.
12.2 Sample Preparation
The single-pole, 20-amperes rated circuit breakers were
purchased from Home Depot (model HOM120). All of the circuit
breakers were installed in the testing stations to confirm that
they were operational before exposure testing. All of the circuit
breakers were removed from the stations, numbered, and chain-
of-custody initiated. The baseline circuit breakers were put aside
until needed. The test and control exposure testing was discussed
in Section 4. Each run used seven circuit breakers. After a test or
control circuit breaker set was prepared in the exposure chamber,
the breakers were removed from the exposure chamber and
visually inspected.
12.3 Circuit Breaker Testing Stations
After visual inspection, the breakers were installed in the testing
station and observed for 90 days under load (Figure 12.1). The
testing station is an electrical box containing 8 spaces, 16 circuits,
100 amp max from square D (Home Depot # 577-340). The
circuit breaker box was wired with 12-gauge, 20-amp wire into
the 120-V outlet. Each circuit breaker was wired in series with an
electrical lamp (s513e) with an outlet box (sllOe) manufactured
by Thomas & Bretts (Home Depot # c214477 and b214426,
respectively). Each lamp contained a Phillips 40-watt light bulb
(Home Depot # a356140). The test or control circuit breakers
were installed into slots 1 through 7, and the baseline circuit
breaker was installed in slot 8 (Figure 12.1, upper left corner).
Figure 12.1 Circuit Breaker Test Stations
-------
12.4 Results and Discussion
The circuit breakers were exposed to furnigant and visually
inspected after removal from the exposure chamber. No visual
damage was observed on any of the circuit breakers used in
this program following fumigation. The circuit breakers were
then installed into the testing stations for 90 days. The stations
were observed on each work day and light bulbs replaced as
needed. No breakers failed during the 90-day storage under load.
Following the 90-day storage, the breakers were tested using
current-time measurements done at 150% (30 amp) and 300%
(60 amp) of the breakers' rated value. Tests were done using an
AVO/multi-amp MS-2, available from Advanced Test Equipment
Rentals. The test results are provided in Table 12.1. The circuit
breaker data was statistically analyzed to determine whether the
breaker was compromised after exposure to decontaminant by
comparing the test results obtained with fumigant-exposed circuit
breakers to those obtained with control coupons (not exposed to
fumigant). Each breaker station contained one control breaker
that had not been exposed in the chamber.
The measurement for the analysis was the time for the circuit
breaker to open (Time-to-Open) when experiencing a current
above its rated value. A circuit breaker that trips too quickly will
protect personnel and equipment but can represent a significant
loss of time and productivity for the users. A circuit breaker that
takes too long to trip can result in a heat buildup, and possibly a
fire, and might fail to protect equipment, users, and property.
A statistical analysis of the individual test results was conducted
to detect potential statistical outliers (Q-test) and determine
whether there were any differences (Welch's T-test) between
the control circuit breakers and samples exposed to VHP. No
statistical outliers were found in any of the data at the Q=0.99
level of confidence.
Table 12.2 summarizes the data for the average and standard
deviation for the various test groups. The Welch's T-test was
used with a 95% confidence level in order to determine whether
the changes in the Time-to-Open between the groups were
statistically significant. At the 30-amp challenge level, the slight
Table 12.1 VHP Circuit Breaker Test Results
4-hour VHP Box
Test Control
BN5022401
BN5022405
BN5022402
BN5022406
BN5022403
BN5022407
BN5022404
Baseline Breaker
Test Average
Standard Deviation
8-hour VHP Box
Test Control
BN5030801
BN5030802
BN5030803
BN5030804
BN5030805
BN5030806
BN5030807
Baseline Breaker
Test Average
Standard Deviation
60-Amp
Test Time
5.57
4.90
5.70
6.52
6.31
2.60
4.08
4.96
5.10
1.38
60-Amp
Test Time
5.75
5.92
5.14
6.39
5.90
5.69
5.06
6.12
5.69
0.46
30-Amp
Test Time
65.16
48.26
62.53
62.51
59.24
53.92
44.76
40.94
56.63
7.82
30-Amp
Test Time
67.61
43.72
49.62
70.91
56.40
69.43
57.39
66.65
59.30
10.45
4-hour VHP Test
(250-300 ppm)
BV5051301
BV5051302
BV5051303
BV5051304
BV5051305
BV5051306
BV5051307
Baseline Breaker
Test Average
Standard Deviation
8-hour VHP Test
(125-150 ppm)
BV5051201
BV5051202
BV5051203
BV5051204
BV5051205
BV5051206
BV5051207
Baseline Breaker
Test Average
Standard Deviation
60-Amp
Test Time
5.23
4.23
5.94
5.60
4.51
2.95
5.93
5.01
4.91
1.09
60-Amp
Test Time
2.44
4.28
4.60
3.62
3.30
4.66
2.51
3.03
3.63
0.93
30-Amp
Test Time
60.13
82.72
118.05
65.52
91.55
50.50
59.19
91.06
75.38
23.62
30-Amp
Test Time
64.80
79.00
57.23
55.94
84.22
60.63
58.90
49.96
65.82
11.25
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increases in the Time-to-Open from the control to the VHP-
exposed circuit breakers were not determined to be statistically
significant. In addition, no difference was determined to exist
at die 30-amp challenge between the 4-hour control and die
8-hour control.
However, under the 300% (60-amp) challenge, a statistically
significant decrease in the Time-to-Open due to the 8-hour VHP
exposure was observed. No difference was determined to exist
between die control set and the 4-hour VHP exposed test group.
While no difference was determined to exist between the 4-hour
and 8-hour control groups, the Time-to-Open for die 8-hour VHP
exposed group was statistically significantly different from the
4-hour VHP exposed group.
These results suggest that the longer exposure to the fumigant,
even at lower concentration levels, did result in a statistically
significant effect that became apparent at the higher (300%
of rated value) test challenge. No specification was found to
determine whether this effect was widiin die device failure
criteria.
Table 12.2 Average and Standard Deviation by Group
Exposure
4-Hour Control
4-Hour @ 250 ppm VHP
8-Hour Control
8-Hour (qi 125 ppm VHP
30-Amp Challenge
Time-to-Open (sec)
56.63 ± 7.82
75. 38 ±23.62
59.30 ± 10.45
65.82 ± 11.25
60-Amp Challenge
Time-to-Open (sec)
5. 10 ±1.38
4.91 ± 1.09
5.69 ±0.46
3.63 ±0.93
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13.0
FTIR Analysis of Select Wood Samples
Using a Thermo-Nicolet Model 670 with Compact Parabolic
Concentrator® (CPC) Diffuse Reflectance Accessory and a
Mercury-Cadmium-Telluride Detector (HgCdTe), 12 wood
coupons were tested for substructural oxidation. Samples were
tested in the 5000-650 cm"1 range with 4 cm"1 resolution.
13.1 Sample Preparation
In August 2005, eight wood coupons were collected from the
sample storage room. Coupons were prepared in order to show
the cellular effects of exposure to VHP as compared to unexposed
wood coupons and compared to unexposed coupons treated with
liquid hydrogen peroxide.
Coupons WV5042509, WV5042609, WV5050909, and
WV5051010 were exposed in the VHP chamber and allowed
to age prior to FTIR testing.
Coupons WN5030409 and WN5060809 were not exposed to any
hydrogen peroxide and were allowed to age prior to FTIR testing.
Coupons WN5030417 and WN5060817 were not exposed to
VHP but were spiked with 0.5 mL of liquid hydrogen peroxide on
one end of the coupon. During a 30-minute evaporation period,
the liquid hydrogen peroxide was periodically stirred. After the
30 minutes, the coupons were blotted dry with Kiinwipes®. These
coupons were subsequently transferred to the FTTR for analysis.
13.2 FTIR
Twelve wood coupons were tested for substructural oxidation
using a Thermo-Nicolet Model 670 with a CPC Diffuse
Reflectance Accessory (Figure 1) and a Mercury-Cadmium-
Telluride Detector. Instrument parameters were:
Spectral range
Resolution
Scans
Apodization
Phase correction
Zero fill
Final data spacing
4000-650 cm"1
4 cm"1
64
Happ-Genzel
Mertz
2X
2 cnr1
Following preparation of the coupons, they were further prepared
for analysis on the FTIR. Using 400-grit silicon carbide paper,
the surface of the wood coupon was abraded. Sample sizes of
less than 100 ug were collected. Samples were introduced to the
Thermo-Nicolet Model 670 via the CPC Diffuse Reflectance
Accessory.
13.3 Background and Analysis Method
The cellulose hi wood is a linear polymer of P-(1,4)-D-
glucopyranose (polysaccharide) units. This, as well as other
polysaccharides with similar structures, provide the rigidity to
wood. The effects of VHP on the polymer, if occurring, may
be expected to result in cleavage of the chains at the C-O-C
linkages, oxidation of the O-H functionalities to the respective
carbonyl, and/or opening of the monomer rings. Expected effects
in the infrared spectra of the wood are shifts and/or reductions
in bands related to O-H and C-O-C, as well as increases in
intensities of bands in the region of the spectra arising from C=O
functional groups.
The effect of VHP on wood was investigated at the molecular
level using diffuse reflectance infrared Fourier transform
(DRIFT) spectroscopy. DRIFT is a technique in which the
material to be investigated is diluted, after grinding or powdering,
with a nonabsorbing material, for example, potassium bromide. A
small quantity of the resulting mixture is placed in an accessory
that allows the collimated infrared beam from the spectrometer
to be focused on the surface of the material from above.
Because the surfaces of the particles of analyte and diluent are
oriented randomly, the infrared energy becomes decollimated,
or diffused. The resulting spectrum is treated mathematically
using the "Kubelka-Munk" transformation. The technique is used
extensively in the pharmaceutical industry and in the analysis of
agricultural products.
While a literature search has indicated that DRIFT may be
expected to be useful for elucidating the effects of the VHP on
wood, it may be difficult to prove a negative response of the
wood to the VHP. For this reason, wood samples subjected to a
more aggressive oxidation than would be expected during this
test were also analyzed. Wood specimens (positive controls)
exposed to liquid hydrogen peroxide (35%) and negative controls
(no treatment) were prepared and analyzed in the same fashion as
the test specimens.
The primary assumption of analysis was that the effects of
exposure to hydrogen peroxide would oxidize the -OH in rings
and ether linkages hi the cellulose polymer of the wood. This
would result hi an increase in carbonyl bands noticeable in the
1700 cm"1 region. Normalization of samples were performed by
analyzing the region around 2900 cnr1. The ratio of CH stretching
in this region can be compared to carbonyl stretching regions.
-------
13.4 Results
13.5 Discussion
Table 13.1 shows the integrated area responses for each sample in Using the Welch's T-Test, no statistically significant differences
both the 2900 cm"1 and 1700 cm"1 regions analyzed. The ratio of
the two regions is also provided. A discussion of the results can
be found in section 13.5.
were found between the control. VHP-exposed, or Liquid H,O2-
exposed coupon sets. Analysis by this method did not reveal
any changes to the structure of the wood due to oxidation by
hydrogen peroxide (vapor or liquid).
Table 13.1 FTIR Analysis Data
VHP Exposed Coupons
Sample ID
3025-2800
1824-1689
ratio
WV5042509
15.52
9.93
0.64
WV5042609
15.06
7.18
0.48
WV5050909
17.29
7.86
0.45
WV5051010
19.34
8.89
0.46
Average
16.80
8.47
0.51
SD
1.95
1.20
0.09
Control Coupons
Sample ID
3025-2800
1824-1689
ratio
WN5030409
20.03
8.84
0.44
WN5060809
15.80
7.55
0.48
WN5030417
24.21
10.59
0.44
WN5060817
20.54
8.83
0.43
Average
20.15
8.95
0.45
SD
3.44
1.25
0.02
Liquid H202 Exposed Coupons
Sample ID
3025-2800
1824-1689
ratio
WN5030417
16.06
7.31
0.46
WN5060817
29.44
12.13
0.41
Average
22.75
9.72
0.43
SD
9.46
3.41
0.03
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14.0
Quality Assurance Findings
Two technical audits of the Instron destructive testing process on was conducted on 19 October 2005 and involved ceiling tile
VHP-fumigated coupons were conducted over the course of the coupons. All operations w ere in accordance with the applicable
program. The first, conducted 6 June 2005, covered steel coupons SOPs and lOPs. Data quality audits were conducted on 7 of
from a control run in the VHP chamber. All operations were in the 56 VHP material compatibility tests (13%). All were found
accordance with the SOPs and lOPs. The second technical audit to be acceptable, in accordance with the Quality Assurance
Project Plan.
-------
-------
15.0
References
(1) Jahnke, M.; Lauth, G. Pharm. Eng. 1997,2-12.
(2) McDonnell, G. G.; Gringol, G.; Antloga, K. Dairy, Food Environ. Sanit. 2002, 868-873.
(3) Brickhouse, M. D.; Turetsky, A.; McVey, I. "Decontamination of CBW Agents by mVHP: Demonstration
of die CBW Decontamination of a Building Using mVHP," Edgewood Chemical Biological Center, 2005.
(4) Brickhouse, M. D. "Quality Assurance Project Plan and Work Plan for Deposition Velocity Studies:
Materials Sorption of Vaporized Hydrogen Peroxide or Chlorine Dioxide. Doc. No. DSQAPP2004DV."
2004.
(5) "Quality Management Plan (QMP) for the National Homeland Security Research Center (NHSRC) Office
of Research and Development (ORD)." U.S. Environmental Protection Agency (U.S. EPA). 2003.
(6) "Quality Management Plan for Environmental Programs," Edgewood Chemical Biological Center
Research. Development and Engineering Command, 2003.
(7) "EPA Guidance for Data Quality Assessment, Practical Methods for Data Analysis, EPA QA/G-9,"
U.S. Environmental Protection Agency, 2000.
(8) "EPARequirements for Quality Assurance Project Plans, EPA QA/R-5," U.S. Environmental Protection
Agency, 2001.
(9) "EPA Guidance for Quality Assurance Project Plans. EPA QA/G-5," U.S. Environmental Protection
Agency, 2002.
(10) "EPA Guidance on Environmental Data Verification and Data Validation. EPA QA/G-8."
U.S. Environmental Protection Agency, 2002.
(11) Brickhouse, M. D. "Quality Assurance Project Plan and Work Plan for Effects of Vaporized
Decontamination Systems on Selected Building Interior Materials, Doc. No. DSQAPP2004MC," 2004.
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Appendix A:
Coupon Identifier Code
All coupons were marked with an ID number that consisted of a nine-character alphanumeric code. A description
of the identifier pattern and an example code are shown below.
Code Pattern
Character Explanation
1 Material
W = wood
G = gypsum
S = A572 steel
T = acoustic ceiling tile
C = concrete cinder block
R = carpet
B = circuit breakers
A = aluminum coupons
F = copper coupons
E = steel coupons
2 Fumigant
V = VHP
D = chlorine dioxide
N = no fumigant
4,5
6,7
Test start date
year for example: 4 = 2004
month for example: 06 = June
day for example: 10 = the 10th of a month
Chamber position (see IOP DS04016 Figure 1)
Example GV4101104
Gypsum wallboard with test start date of October 11th, 2004: sample number 4.
-------
Figure A-l: IOP DS04016 Figure 1, "Coupon Placement in Chambers"
a) Concrete
• Steel
b) Carpet
e) Wallboard
c) Tile
rtP-i
Ki)~i K4>i
K«)n
f) Wood
$<»>
Coupons shown on rack shelves from direction of glove box transfer chamber, Pictoral
coupon scaling for length and width is (0.75 * 2 *(cm /10)).
Figure A-2: IOP DS04016 Figure 2, "Circuit Breaker Placement in Chambers"
a) Circuit Breakers
*
Coupons shown on rack shelves from
direction of glove box transfer chamber.
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Appendix B:
Detailed Coupon Preparation and
Inspection Procedures
Coupon Preparation Procedure
The coupon preparation, unless otherwise noted, was conducted at the Edgewood Chemical Biological Center
Experimental Fabrication Shop.
Mechanically Graded Lumber (Bare Wood)
• Stock Item Description: 2 x 4 x 8 KD WW/SPF Stud
• Supplier/Source: Home Depot, Edgewood Maryland
• Coupon Dimensions: 10 in. x 1 !/•> in. x !/2 in.
• Preparation of Coupon:
- The machined ends of the stock were discarded by removing > '/t in. of the machined end.
Coupons were cut from stock, using a table saw equipped with an 80-tooth crosscut blade.
Latex-Painted Gypsum Wallboard
• Stock Item Description: !/•> in. 4 ft. x 8 ft. Drywall
• Supplier/Source: Home Depot. Edgewood Maryland
• Coupon Dimensions: 6 in. x 6 in. x !/2 in.
• Preparation of Coupon:
- The ASTM method requires that the samples be taken from the interior of material rather than from
the edge (machined edge). The machined ends of the stock were discarded by cutting away > 4
inches from each side.
- Coupons were cut from stock, using a table saw equipped with an 80-tooth crosscut blade.
- The 6 in. x 6 in. coupons were painted with 1 mil of Glidden PVA primer and followed by 1-2 mils
of Glidden latex topcoat. The primed coupons were allowed to stand for > 24 hours prior to the
application of the topcoat.
- All six sides of the 6 in. x 6 in. coupon were painted.
Concrete Cinder Block
• Stock Item Description: 8 in. x 16 in. x 1.5 in. concrete cinder block cap
• Supplier/Source: York Supply, Aberdeen Maryland
• Original Coupon Dimensions: 4 in. x 8 in. x 1.5 in.
• Modified Coupon Dimensions: 4 in. x 8 in, x 0.5 in.
• Preparation of Coupon:
- Coupons were cut from stock using a water-jet.
- Four coupons were cut from each stock piece.
- Original dimensions were too large for material testing.
o Each coupon was cut into three sections.
o Two sections were measured at modified coupon dimensions.
o The third section was discarded.
-------
Carpet
• Stock Item Description: 12-ft. Powerhouse 20 Tradewind
• Supplier/Source: Home Depot, Edge wood, Maryland
• Coupon Dimensions: 6 in. x 8 in.
• Preparation of Coupon:
- Coupons were cut from the stock using a utility knife.
- The longer direction (8 in.) was cut parallel to the machine edge.
- The machined edge was discarded by removing > Vi in.
Painted Structural Steel
• Stock Item Description: A572 Grade 50, 4 ft. x 8 ft. x % in.
• Supplier/Source: Specialized Metals
• Coupon Dimensions: 1/4 in. x 12 in. total, dog bone shaped with 2 in. wide at ends,
% in. wide at center
• Preparation of Coupon:
- Coupons were cut from stock using a water-jet.
- A visual observation was conducted on each coupon to determine whether size and shape had
deviated from dimension. If so, the coupon was discarded.
- Coupons were cleaned and degreased following procedures outlined in TTC-490.
- Coupons were prepared for painting per TT-P-645 with red oxide primer.
The Edgewood Chemical Biological Center Experimental Fabrication Shop prepared the materials
in accordance with the standards used for the preparation and painting of steel. TTC-490 is a federal
standard providing cleaning methods and pretreatment for iron surfaces for application of organic
coatings. The pretreatment is the application of a zinc phosphate corrosion inhibitor. TT-P-645 is a
federal standard for the application of alky d paint. These standards were not obtained through this
program but were purchased by the shop for their work.
Ceiling Suspension Tile
• Stock Item Description: Armstrong 954. Classic Fine Textured. 24 in. x 24 in. x 9/16 in.
• Supplier/Source: Home Depot, Edgewood, Maryland
• Coupon Dimensions: 12 in. x 3 hi. x 9/16 in.
• Preparation of Coupon:
- Coupons were cut from stock, using a table saw equipped with an 80-tooth crosscut blade.
- Sixteen samples were removed from each stock item.
Coupon Inspection Procedure
All coupons were inspected prior to testing to ensure that the material being used was in suitable condition.
Coupons were rejected if there were cracks, breaks, dents, or defects beyond what are typical for the type of
material. In addition, coupons were measured to verify' the coupon dimensions. Coupons deviating from the
dimension ranges listed below were discarded.
Mechanically Graded Lumber (Bare Wood) 10 in. ± 1/16 in. x 1.5 in. ± 1/16 in. x 0.5 in. ± 1/32 in.
Latex-Painted Gypsum Wallboard 6 in. ± 1/16 in. x 6 in. ± 1/16 in. x 0.5 in. ± 1/16 in.
Concrete Cinder Block 4 in. ± i/2 in. x 8 in. ± Vi in. x 0.5 in. ± 1/16 in.
Carpet 6 in. ± 1/8 in. x 8 in. ± 1/8 in.
Painted Structural Steel 1/4 in. ± 1/128 in. x 12 in. ± 1/16 in. with 2 in. ± 1/16 in. wide at
ends, 3/4 in. ± 1/16 in. wide at center
Ceiling Suspension Tile 12 in. ± 1/8 in. x 3 in. ± 1/16 in. x 9/16 in. ± 1/16 in.
-------
Appendix C:
Wood Coupon Location of Break
The ASTM test method requires reporting the location of the arrows are used on samples where the photograph contrast may
break for each wood sample. The purpose of this appendix is not clearly show the location of the break.
to provide this reporting information in pictorial form. Yellow
Figure C-l: Location of Break, Wood Coupons - VHP Control Set
-------
Figure C-2: Location of Break, Wood Coupons-VHP 125-150 ppm Set
-------
Figure C-3: Location of Break, Wood Coupons - VHP 250 - 300 ppm Set
Note:direction of foice upwjrds (opposite of others)
-------
-------
Appendix D:
Concrete Cinder Block Coupon Break Location
The location of the break for each concrete sample is reported
here, from the testing using ASTM Test Method C140-03. The
purpose of this appendix is to provide this reporting information
in pictorial fonn. Yellow arrows are used on samples where
the photograph contrast may not clearly show the location of
the break.
Figure D-l: Location of Break, Block Coupons - Control Set
-------
Figure D-2: Location of Break, Block Coupons - VHP 125 - 150 ppm Set
-------
Figure D-3: Location of Break, Block Coupons - VHP 250 - 300 ppm Set
-------
©EPA
United States
Environmental Protection
Agency
PRESORTED STANDARD
POSTAGE & FEES PAID
EPA
PERMIT NO. G-35
Office of Research and Development
National Homeland Security Research Center
Cincinnati, OH 45268
Official Business
Penalty for Private Use
$300
Recycled/Recyclable
Printed with vegetable-based ink on
paper that contains a minimum of
50% post-consumer fiber content
processed chlorine free
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