&EPA
EPA/600/R-13/233 j November 2013 | www.epa.gov/ord
United States
Environmental Protection
Agency
Development of Standard Test
Methods and Evaluation of the
Shelf Life and Weatherability of
Fixative Coatings for Control of
Radiological Contamination
Office of Research and Development
National Homeland Security Research Center
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Development of Standard Test Methods and
Evaluation of the Shelf Life and Weatherability of
Fixative Coatings for Control of Radiological
Contamination
November 2013
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
RESEARCH TRIANGLE PARK, NC 27711
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DISCLAIMER
The U.S. Environmental Protection Agency (EPA), through its Office of Research and Development's National Homeland
Security Research Center (NHSRC), funded and managed this method development through Contract No. EP-C-09-027
with ARCADIS-US. This report has been peer and administratively reviewed and has been approved for publication as an
EPA document. The views expressed in this report are those of the authors and do not necessarily reflect the views or
policies of the Agency,_Mention of trade names or commercial products does not constitute endorsement or
recommendation for use of a specific product.
Questions concerning this document or its application should be addressed to:
John Drake
National Homeland Security Research Center
Office of Research and Development
U.S. Environmental Protection Agency
26 West Martin Luther King Dr.
Cincinnati, OH 45268
513-569-7164
drake.iohn@epa.gov
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ACKNOWLEDGMENTS
Contributions of the following individuals and organizations to the development of this document are gratefully
acknowledged.
U.S. Environmental Protection Agency (EPA)
John Drake, Office of Research and Development (ORD)/NHSRC
Shannon Serre, ORD/NHSRC
Terry Stilman, Region 4
Paul Kudarauskas, Office of Emergency Management (OEM), Consequence Management Advisory Team (CMAT)
ARCADIS-US
iv
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CONTENTS
DISCLAIMER Ill
ACKNOWLEDGMENTS IV
ACRONYMS AND ABBREVIATIONS 3
1.0 INTRODUCTION 5
2.0 LITERATURE AND INDUSTRY SEARCH 6
3.0 REVIEW OF EXISTING TEST METHODS 9
4.0 TEST METHOD DEVELOPMENT 10
5.0 VERIFICATION OF DRAFT TEST METHODS 12
6.0 TESTS OF ADDITIONAL COATINGS USING THE VERIFIED TEST METHODS 14
7.0 QUALITY ASSURANCE AND QUALITY CONTROL (QA/QC) 16
7.1 Quantitative acceptance criteria for QA objectives 16
7.2 Data Quality Indicators 17
7.3 Assessment of DQI Goals 17
8.0 SUMMARY OF TEST DATA 19
8.1 Summary 19
8.2 Adhesion 19
8.3 TABER ABRASION RESISTANCE 21
8.4 Tensile strength 22
8.5 STORMER VISCOSITY 22
8.6 BROOKFIELD VISCOSITY 24
8.7 Density 27
9.0 SUMMARY OF RESULTS 28
1
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TABLES
Table 2-1. Previously tested sequestration coatings 7
Table 2-2. Selection of sequestration coatings identified as potential candidates for method
VERIFICATION 8
Table 4-1. Existing test methods selected for incorporation into the shelf life test method 10
Table 4-2. Existing test methods selected for incorporation into the weatherability test method ..10
Table 5-1. Changes made following verification testing 12
Table 5-2. Final shelf life and weatherability methods 13
Table 7-1. Critical measurement properties for testing of shelf life 16
Table 7-2. Critical measurement properties for testing of weatherability 17
Table 7-3. DQIs for critical measurements 18
Table 8-1. Adhesion - concrete initial 20
Table 8-2. Adhesion - concrete after 200-hr humidity 20
Table 8-3. Adhesion - steel initial 21
Table 8-4. Adhesion - steel after 200-hr humidity 21
Table 8-5. Taber abrasion resistance 23
TABLE 8-6. TENSILE STRENGTH 23
Table 8-7. Stormer viscosity (Krebs Units) 24
Table 8-8. ALARA1146 Brookfield viscosity (centipoises [cps]) 25
Table 8-9. CC Strip/CC Fix Brookfield viscosity (cps) 25
Table 8-10. CC Strip/SBR-10 Brookfield viscosity (cps) 26
Table 8-11. Intergard 10220 Brookfield viscosity (cps) 27
Table 8-12. Density 27
Table 9-1. Summary of results for shelf life 28
Table 9-2. Summary of results for weatherability 29
FIGURES
Figure 6-1. Intergard 10220 being applied to concrete coupons 14
Figure 8-1. Adhesion test coupon 19
Figure 8-2. Brookfield viscosity measurement of SBR-10 24
APPENDICES
Appendix A - Shelf Life Test Method A
Appendix B - Weatherability Test Method B
Appendix C - KTA Test Report - ALARA 1146 C
Appendix D - KTA Test Report - Instacote CC Strip/CC Fix D
Appendix E - KTA Test Report - Instacote CC Strip/SBR-1 0 E
Appendix F- KTA Test Report - Intergard 10220 Test Report F
Appendix G - Data Quality Indicators G
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Acronyms and Abbreviations
ASTM American Society for Testing and Materials
CBRN chemical, biological, radiological, nuclear
cm centimeters)
CMAT Consequence Management Advisory Team
COTS commercial-off-the-shelf
cps centipoises(s)
DOE U.S. Department of Energy
DQI Data Quality Indicator
EPA U.S. Environmental Protection Agency
gal gallon(s)
g gram(s)
h hour(s)
HSRP Homeland Security Research Program
kg kilogram(s)
KU Krebs Unit(s)
lb pound(s)
MIL-PRF Military Performance Standard
Mg milligram(s)
N/A not available
NHSRC National Homeland Security Research Center
OEM Office of Emergency Management
ORD Office of Research and Development
psi pounds per square inch
QA quality assurance
QAPP quality assurance project plan
QC quality control
QMP Quality Management Plan
RH relative humidity
rpm revolutions per minute
RSD relative standard deviation
UV ultra violet
3
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Executive Summary
The U.S. Environmental Protection Agency's (EPA's) Homeland Security Research Program (HSRP) is
helping to protect human health and the environment from adverse impacts resulting from Chemical,
Biological, Radiological and Nuclear (CBRN) contamination whether it results from an intentional act (for
instance, terrorism), a criminal act, or an unintentional act (such as a natural disaster or industrial accident).
One way HSRP helps to protect human health and the environment is by developing performance
requirements and test methods for evaluating the performance of technologies relevant to homeland
security. Through its involvement with the American Society for Testing and Materials (ASTM) the HSRP led
the effort which developed ASTM E-2731-09 Standard Specification for Materials to Mitigate the Spread of
Radioactive Contamination after a Radiological Dispersion Event. ASTM E-2731-09 articulates eighteen
different material performance requirements (e.g., tear strength, abrasion resistance, weatherability, shelf
life, etc.) for coatings which could be used to sequester contamination (particles) and fix them in place,
thereby limiting the spread of contamination (and associated health/exposure impacts) and making future
decontamination and recovery efforts more effective. Test methods for verifying the performance of any
particular coating against the requirements in ASTM E-2731-09 exist for some parameters such as tensile
strength or abrasion resistance. However, test methods for some of these requirements do not currently
exist, including methods for assessment of weatherability and shelf life. ASTM E-2731-09 defines
weatherability as the capability of the coating to remain stable (maintain film integrity) under a variety of
outdoor environmental conditions for a minimum of one year. The environmental conditions specified in
ASTM E-2731-09 include exposure to ultraviolet (UV) light, water immersion, high and low temperatures,
and common bacteria. Similarly, the performance requirement for shelf life given in ASTM E-2731-09 is
defined as the ability of the coating to be applied successfully and to meet the performance requirements as
otherwise specified in the standard, after a specified period of climate-controlled storage (five years per
ASTM E-2731-09).
The EPA HSRP, led by the EPA's National Homeland Security Research Center (NHSRC), has produced a
set of test methods to verify performance of coatings intended to meet the ASTM E-2731-09 performance
standards for shelf life and weatherability. These test methods were drafted, verified by laboratory exercise
using a commercially available coating product widely used in the radiological industry, ALARA 1146
(Carboline Co., St. Louis, MO, USA), and then used to evaluate the shelf life and weatherability performance
of three additional currently commercially available coatings selected as potential candidates for use as
sequestration coatings to immobilize radioactive contamination. Selection of the three coatings to be tested
was based primarily on material availability, reasonable deployment requirements, and past EPA
experience. The three products selected included the two systems (a) CC-STRIP followed by CC Fix
(Instacote, Erie, Ml, USA); (b) CC Strip followed by SBR-10F (Instacote, Erie, Ml, USA); and (c) Intergard
10220 (AkzoNobel, Strongsville, OH, USA).
4
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1.0 Introduction
Research indicates that if a radioactive dispersal device (dirty bomb) is detonated, immediate action may be
necessary to treat urban surfaces. For some radioactive particles migration and chemical binding are rapid,
and after some period of time, significant decontamination may not be feasible. Thus, immediate treatment
of surfaces (within hours) with a sequestrating compound that can be applied easily in large quantities could
alleviate much difficulty in subsequent decontamination. Additionally, loose radioactive particles may be
further dispersed into the environment (blown by wind or washed by rain), making decontamination even
more challenging. The use of sequestrating compounds could immobilize these particles preventing their
dispersion into the environment and increasing the effectiveness of subsequent decontamination efforts.
One type of sequestration compound considered for deployment in the aftermath of a dirty bomb event
would consist of a coating that would likely be a polymeric, paint-like substance. Such a coating would be
capable of encapsulating and immobilizing radioactive particles deposited on outdoor construction surfaces
such as steel, concrete, or asphalt.
Performance specifications for such a sequestration coating were previously developed and promulgated as
ASTM E-2731-09 Standard Specification for Materials to Mitigate the Spread of Radioactive Contamination
after a Radiological Dispersion Event. ASTM E-2731-09 articulates eighteen different performance
requirements (e.g., tear strength, abrasion resistance, weatherability, shelf life, etc.). Test methods for
verifying the performance of any particular coating against these requirements exist for some parameters
such as tensile strength or abrasion resistance. However, test methods for some of these requirements do
not currently exist, for example, methods for assessment of weatherability and shelf life. ASTM E-2731-09
defines weatherability as the capability of the coating to remain stable (maintain film integrity) under a variety
of outdoor environmental conditions for a minimum of one year. The expectation is that the coating will
maintain its mechanical properties during that exposure period. The environmental conditions specified in
ASTM E-2731-09 include exposure to ultraviolet (UV) light, water immersion, high and low temperatures,
and common bacteria. Similarly, the performance requirement for shelf life given in ASTM E-2731-09 is
defined as the ability of the coating to be applied successfully and to meet the performance requirements as
otherwise specified in the standard, after a specified period of climate-controlled storage (five years per
ASTM E-2731-09).
The Environmental Protection Agency's (EPA) Homeland Security Research Program (HSRP), led by the
EPA's National Homeland Security Research Center (NHSRC), has produced a set of test methods to verify
performance of coatings intended to meet the ASTM E-2731-09 performance standards for shelf life and
weatherability. These test methods were drafted, verified by laboratory exercise, and then used to evaluate
the shelf life and weatherability performance of three commercially available coatings selected as potential
candidates for use as sequestration coatings to immobilize radioactive contamination.
5
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2.0 Literature and industry search
An extensive search of available literature and industrial sources was undertaken to identify potential
coating test methods applicable to weatherability and shelf life, and to identify candidate sequestration
coatings that could be used for verification of the test methods being developed. The material standards
community and the coatings industry were canvassed to determine how industry evaluates coating
weatherability and shelf life. Multiple vendors were contacted based on the literature search. Not
unexpectedly, the majority of the manufacturers contacted were focused primarily on marketing and sales
issues and potential sales volume. Technical information, especially with regards to weatherability and shelf
life, was sparse to non-existent. Most manufacturers did not have a method for evaluating shelf life other
than leaving the coating on a shelf (i.e., in storage) for some period of time and testing either the viability of
the coating or the viability of the chemical components of their products. In addition, only very limited
information was available on the ability of any of the commercial coatings to withstand various weather-
related elements. Limited testing or performance data were obtained during this search process. Table 2-1
lists sequestration coatings that have been tested in the past where results have been reported in publicly
available literature.
Several potential candidate coatings were identified as a result of the literature and industrial sources search
and are listed in Table 2-2. Table 2-2 is intended to illustrate only the availability of the potential
sequestration coatings found during the search and is not intended as a complete list of coatings that may
be offered by the industry.
One coating, ALARA 1146 (Carboline Co., St. Louis, MO, USA), was initially selected for verification of the
test methods derived during this project. Verification of an analytical procedure is the demonstration that a
laboratory is capable of replicating, with an acceptable level of performance, a standard method. Following
further consideration and discussions with various coatings manufacturers, three additional coatings were
selected for further testing using the verified test methods. Selection was based primarily on material
availability, deployment requirements, and past EPA experience. Two multiple-component coating systems
were selected from Instacote, Inc. (Erie, Ml, USA), and one from AkzoNobel (Strongsville, OH, USA). The
Instacote coating systems require a two-step application protocol. Although a two-step application was not
considered most desirable from a field deployment perspective, these coating systems were selected due to
their reported durable nature and removability. The three products selected included the Instacote systems
(a) CC-STRIP followed by CC Fix and (b) Instacote CC Strip followed by SBR-10F; and (c) AkzoNobel's
Intergard 10220 (all three in green in Table 2-2).
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Table 2-1. Previously tested sequestration coatings
Product Name
Manufacturer
Literature Source
ALARM 146
Carboline Co.
(St. Louis, MO, USA)
Cleaning and Decontamination using Strippable and Protective Coatings at the
Idaho National Engineering and Environmental Laboratory, INEEL/CON-98-
00797
ALARA™ 1146 Strippable Coating, DOE OST/TMS ID 2314, April 2000
Bartlett TLC
Bartlett Services, Inc.
(Plymouth, MA, USA)
Cleaning and Decontamination using Strippable and Protective Coatings at the
Idaho National Engineering and Environmental Laboratory, INEEL/CON-98-
00797
Bartlett TLC Free
Bartlett Services, Inc.
(Plymouth, MA, USA)
Assessment of Strippable Coatings for Decontamination and Decommissioning,
DOE/EW/55094—32, January 1998
Bartlett Services Inc. StripcoatTLC Free Radiological Contamination Strippable
Coating, EPA/600/R-08/099, September 2008
InstaCote ML
Instacote
(Erie, Ml, USA)
Assessment of Strippable Coatings for Decontamination and Decommissioning,
DOE/EW/55094—32, January 1998
Orion
Isotron Corp.
(Seattle, WA, USA)
Isotron Corp. Orion Radiological Decontamination Strippable Coating,
EPA/600/R-08/100, September 2008
Tech Sol 8001
Technical Solutions &
Systems, Inc.
(Elizabethton, TN, USA)
Assessment of Strippable Coatings for Decontamination and Decommissioning,
DOE/EW/55094—32, January 1998
Tech Sol 8002
Technical Solutions &
Systems, Inc.
(Elizabethton, TN, USA)
Assessment of Strippable Coatings for Decontamination and Decommissioning,
DOE/EW/55094—32, January 1998
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Table 2-2. Selection of sequestration coatings identified as potential candidates for method verification
Coating
Company
Web Address
Application
Advertised
Shelf Life
Notes
ORION
Isotron Corporation
Seattle, WA, USA
www.isotron.net
Brush, airless
spray, roller
10 months
at 75 °F
Produced in Japan under trade name "Extract'
Stripcoat TLC
Bartlett Services, Inc
Plymouth, MA, USA
www.bartlettnuclear.com
Spray
7 to 30 days
Not applicable in subfreezing
temperatures (water-based)
ALARA1146
Carboline
St. Louis, MO, USA
www.carboline.com
Spray
recommended
n/a
Licensed for production in Japan by Carboline
Water-based
RADBLOCK
Isotron Corporation
Seattle, WA, USA
www.isotron.net
...
10 months
at 75 °F
Coming soon (website checked 8/13/12) Gemini. Electrosorb, and WaterDecon
CC-STRIP
InstaCote
Erie, Ml, USA
www.instacote.com/cc-
strip.htm
Sprayers and
rollers
n/a
Does not penetrate pores; CC Wet is required as the first step,
CC Wet is water-based
Other products: CC Wet, CC Fix, CC Fix LV, CC Epoxy SP
Only CC Strip is strippable
Spray Poly
Foster Specialty Construction
Brands, Inc
St. Aurora, IL, USA
www.fosterDroducts.com
...
6 months
UV sensitive: used for asbestos remediation
Multisurface
Protectapeel
Corby, Northamptonshire.
NN174AR, UK
www.DrotecaDeel.co.uk
Airless gun
or roller
12 months
between 5-25 °C
Not tested for radiological contamination
Other products: SC1074, Sc1090, E105NF, E106
Proprietary
Process
Salvarem-The Nuvia Group Z.A.
Beaumont CEDEX-France
www.nuvia-india.com
Various surfaces,
wet application
n/a
Nuvia Group France
Three processes: FORAL, Forac, FORNET for radioactive cleanup
Contrad 70
Decon Labs, Inc.
Prussia, PA, USA
www.deconlabs.com
Wet rinse
n/a
Also Decon 90 surface wash
RDS 2000
Karcher Futuretech GmbH
Schwaikheim Germany
www.rkb.us
n/a
n/a
Two component liquid agent, foaming unit required, foam applied to surfaces
KATS 9500 OPC
Kats Coatings
Rockwall, TX, USA
www.katscoatinas.com
Sprayers
n/a
Non-porous surfaces,
Not tested for radiological contamination, three products: 9501,9502,9503
Intergard 10220
AkzoNobel
Sassenheim, The Netherlands
httD://www.akzonobel.com
n/a
n/a
Water-based polyurethane
Cooperation with DSTL (UK) for absorptive coating
Red Shading - Shelf life inadequate
Purple Shading - Application conditions unacceptable
Green Shading - Selected for testing
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3.0 Review of existing test methods
To determine if there were any existing test methods that could potentially be applicable to
weatherability and shelf life determination, an extensive review of industry (primarily ASTM) methods
and military specifications was conducted, focused on paints and coatings. Initial results indicated that
potential candidates would likely be polymeric, paint-like substances. The review was focused on
identifying methods used for paint testing that might be useful to evaluate shelf life and weatherability of
sequestration coatings. In addition to shelf life and weatherability, ASTM E2731-09 specifies the
following physical/mechanical parameters for a sequestration coating:
• Tensile Strength 35 kg/cm2 (500 psi)
• Adhesion >3.5 kg/cm2 (>50 psi) on concrete
• Abrasion <50-mg (0.002-oz) loss
• Tear Strength 14 kg/cm2 (200 psi)
• Flammability - does not burn.
ASTM E2731-09 specifies a required shelf life of a minimum of five years. In addition, the coating must
meet the above physical parameters for a period of one year under weathering conditions described as
exposure to a variety of outdoor environmental conditions such as ultraviolet (UV) exposure,
precipitation, high and low temperatures, and common bacteria.
It became apparent that performance in terms of weatherability and shelf life are inextricably tied to the
measurable physical/mechanical requirements such as those listed above. Essentially, to evaluate
weatherability performance, the coating must continue to exhibit its physical/mechanical attributes after
being exposed to the weathering environment. Similarly, to evaluate the ability of a coating to meet the
shelf life requirement, the coating must, after storage for the specified five-year period, continue to
exhibit these same physical/mechanical attributes.
While some test methods require removal of the coating from the test substrate, other methods require
that testing to be performed on the test substrate. In addition, both accelerated and non-accelerated test
methods were used to identify potential degradation of a coating.
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4.0 Test method development
The shelf life and the weatherability test methods were produced by incorporating selected portions of
existing coating and paint test methods with some modification to suit the particularities of a capture
coating. Table 4-1 provides a list of six properties initially selected for evaluating the potential shelf life of
a coating. Table 4-1 lists a preferred method as well as alternate methods, if available. Table 4-2
provides a list of five properties initially selected for evaluating the potential weatherability of a coating.
Table 4-1. Existing test methods selected for incorporation into the shelf life test method
Property Describing Shelf Life
Preferred Method
Alternate Methods
Freeze/Thaw Resistance of Organic Coatings
ASTM D2337/
MIL-PRF-32239
N/A
Settling Properties
ASTM D1309/869
N/A
Freeze/Thaw Resistance of Aqueous-Based Coatings
ASTM D2243
N/A
Accelerated Storage Stability
MIL-PRF-32239
N/A
Density
ASTM D1475
N/A
Viscosity
ASTM D1200
ASTM D4287;
ASTM D7395
N/A = not applicable
Table 4-2. Existing test methods selected for incorporation into the weatherability test method
Property Describing
Weatherability
Preferred Method
Alternate Methods
Water resistance at 100% RH
ASTM D2247-02
ASTM D4585-07
Tensile strength
ASTM D2370-98
(organic-based coatings)
ASTM D6083-05e1
(water-based coatings)
N/A
Abrasion resistance
ASTM D4060-07
ASTM D968a
Natural sunlight and soak-freeze-
thaw tolerance
ASTM D5722-08
ASTM D660 and/or D662 and/or D714
and/or D772 and/or D4214 and/or
D610b
ASTM D6695-08 or
MIL-PRF-32239C
Adhesion strength
(on concrete)
ASTM D7234-05
ASTM D4541 -09e1d
N/A= Not Applicable
a For organic coatings only
b As a follow up to D5722-08; not meant to replace D5722-08
c Only for the concentrated natural light part of D5722-08
d Only for surfaces other than concrete
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For the purpose of developing the shelf life test protocol, successful weatherability performance was not
considered to be a prerequisite. Likewise, weatherability of a coating can be tested whether or not the
coating meets the shelf life requirements.
The two draft test methods were subjected to an internal peer review process, performed by subject
matter experts in related fields, as well as personnel with experience in the field of materials testing and
protocol development. Comments received from the review were addressed and the final methods
developed prior to method verification. The final test methods were submitted for verification to an
outside testing subcontractor (KTA-Tator Laboratories, Pittsburgh, PA, USA) with the requirement that
they be strictly followed, to capture any weaknesses or errors. Communications were maintained
between the test crew and the procedure writing crew during the entire verification process to assure
communication of errors/omissions and changes. In addition, two visits were made to the laboratory to
observe the testing of the coatings in progress and to facilitate further refinement of the test methods.
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5.0 Verification of draft test methods
One containment coating, ALARA 1146, was selected for verification of the shelf life and weatherability
test methods. The tests identified in Tables 4-1 and 4-2 were performed using this coating. ALARA 1146
was applied according to manufacturer's recommended procedures to both concrete and steel coupons
forthe purposes of method verification. These coupons were specifically manufactured to replicate two
types of building materials commonly found in the urban environment. The coupons were clean and
were not contaminated. As a result of these verification tests and observations, various changes were
required for both test methods, as shown in Table 5-1. Final modified methods are shown in Table 5-2.
Following method verification, both test methods were finalized and are incorporated into this report as
Appendix A, Shelf Life Test Method and Appendix B, Weatherability Test Method. The results of the
verification tests using ALARA 1146 are presented in Appendix C.
Table 5-1. Changes made following verification testing
Method Changed
Property
Method
Reason for Change
1
Shelf Life Method
Freeze/Thaw
Resistance of
Organic Coatings
D2337
These methods are
essentially identical (one
hour difference in cycle
duration). Method D2243 for
aqueous coatings has been
deleted, and Method D2337
will be used for all coatings.
Freeze/Thaw
Resistance of
Aqueous-Based
Coatings
D2243
2
Shelf Life Method
Viscosity
D1200
D2196
Method 1200 requires use
of a #4 Ford cup, and the
coating would not flow
through this device. This
method was replaced with
Method D2196, which uses
a Brookfield viscometer.
3
Weatherability
Method
Water Resistance at
100% Relative
Humidity (RH)
D2247
This method evaluates
durability of a coating to
water degradation at 100%
RH. We had specified
duration of 300 hours.
However, the laboratory
noted degradation by 200
hours. The required
duration was changed to
200 hours for future tests.
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Table 5-2. Final shelf life and weatherability methods
Property Describing Shelf Life
Method Selected
Freeze/Thaw Resistance of Organic Coatings
ASTM D2337
Settling Properties
ASTM D1309/869
Accelerated Storage Stability
MIL-PRF-32239
Density
ASTM D1475
Viscosity
ASTM D2196
Property Describing Weatherability
Method Selected
Water resistance
D2247-02 a
Tensile strength
D2370-98 (organic-based coatings)
D6083 - 05e1 (water-based coatings)
Abrasion resistance
D4060-07
Natural sunlight and soak-freeze-thaw tolerance
D5722-08
Adhesion strength
D7234-05
a modified per Table 5-1.
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6.0 Tests of additional coatings using the verified test methods
Three additional coatings were identified and tested using the verified test methods. The coatings
identified and tested included (1) Instacote CC Strip (base coat) followed by CC Fix, (2) CC Strip (base
coat) followed by SBR-10F, and (3) AkzoNobel Intergard 10220. All three coatings were applied to both
concrete and steel coupons and allowed to cure for seven days prior to testing. The application of the
coatings, as well as all testing was conducted at ambient laboratory temperature and humidity levels.
The Instacote coatings were used as two-part coatings due to the durability of the CC Fix and SBR-10F
(as top coat) and the removability of CC Strip (as base coat). CC Strip is a flexible, strippable (peelable),
protective coating used in various industries. This combination of applying a durable coating on top of a
strippable coating was suggested to achieve the removability characteristics desired in these candidate
coatings, as well as the durability of the coating surface. After simple laboratory tests at Instacote, Inc.,
the manufacturer reported that the coating system was still both strippable and durable.
The base coats of CC Strip were applied to the metal and concrete coupons in a horizontal orientation
and allowed to cure. The recommended cure time for CC Strip is 24 hours at standard temperature and
humidity. Higher humidity will require a longer cure time. The coupons and panels were allowed to dry
for a minimum of 24 hours before application of the top coats. After curing, the CC Fix and SBR-10F top
coats were applied to the coupons and allowed to dry. The Instacote coatings were brushed on (per the
manufacturer) using a commercial-off-the-shelf (COTS) paint brush for both the base coat and the
durable top coat.
coating (per the manufacturer) onto the coupons
in a horizontal orientation. Intergard 10220 required a 20% dilution with de-ionized (Dl) water to facilitate
spraying. The appearance of the cured Intergard 10220 was as a smooth, well-flowed liquid on both the
metal and concrete coupons. Some small air bubbles appeared on the concrete coupons as the coating
was curing. To assure a more uniform coating these bubbles were manually deflated. The cured
Intergard coated coupons showed minor imperfections. In addition, the Intergard metal panels showed
After curing, both Instacote systems appeared t<
cover the substrate completely and were smooti
and well-flowed, despite the base coat of CC
Strip having some slight imperfections or ridges
The Instacote SBR-10 is a two-part resin and
isocyanate with solvent. When mixed together
and allowed to stand, this combination appeare<
to produce a slightly exothermic reaction. The
pot life for SBR-10 is approximately 10 minutes
with a cure time of 1.5 hours. Drying time
increases with cooler temperatures.
The Intergard 10220 was applied by spraying the
Figure 6-1. Intergard 10220 being applied to
concrete coupons
14
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micro-cracking at the voids that remained from the bubbles in the film. AkzoNobel was willing to provide
only very limited information on the characteristics and previous uses of Intergard 10220, citing as
reason that it was originally developed for the U.S. military.
The detailed test results for Instacote CC Strip/CC Fix are presented in Appendix D, for Instacote CC
Strip/SBR-10F in Appendix E, and for Intergard 10220 in Appendix F.
15
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7.0 Quality Assurance and Quality Control (QA/QC)
This project was performed according to an approved Quality Assurance Project Plan (QAPP) titled
Identification and Development of Standard Methods for Evaluation of the Performance of Sequestration
Coatings (August 2012). The QAPP was developed according to the NHSRC Quality Management Plan
(QMP).The objective as stated in the QAPP was to verify the test methods for shelf life and
weatherability and test three commercial coatings for shelf life and weatherability performance.
Development of the test methods assumed the following efforts would be required:
(a) Revision of the draft test protocols for clarity, omissions, etc., which might occur before and/or
after the testing.
(b) Potential revisions to the specific methods specified within each draft test protocol, based on
laboratory feedback and how well the accuracy, precision, and completeness criteria would be met.
The QA/QC checks described in this section pertain to step (b) above and include quantitative
acceptance criteria for shelf life and weatherability. These critical measurements are summarized in
Section 7.1 and discussed in detail in Appendix G. The acceptance criteria for determining whether or
not they meet the QA objectives of this study are summarized in Section 7.2 and discussed in detail in
Appendix G.
7.1 Quantitative acceptance criteria for QA objectives
The test results will be used to identify any deficiencies of a tested containment coating to be applied as
intended and will establish and verify the ability of a coating to possess successful shelf life and
weatherability performance. Tables 7-1 and 7-2 provide the critical measurement properties for testing
the shelf life and weatherability of a coating, respectively.
Table 7-1. Critical measurement properties for testing of shelf life
Property Describing Shelf Life
Preferred Method
Alternate Methods
Freeze/Thaw Resistance of
Organic Coatings
ASTM D2337
N/A
Settling Properties
ASTM D1309 and ASTM D869
N/A
Accelerated Storage Stability
MIL-PRF-32239
N/A
Density
ASTM D1475
N/A
Viscosity
ASTM D2196
ASTM D4287 or ASTM D7395
N/A=Not Applicable
16
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Table 7-2. Critical measurement properties for testing of weatherability
Property Describing
Weatherability
Preferred Method
Alternate Methods
Water resistance
ASTM D2247-02
ASTM D4585-07
Tensile strength
ASTM D2370-98 (organic-based
coatings)
ASTM D6083-05e1 (water-based
coatings)
N/A
Abrasion resistance
ASTM D4060-07
ASTM D968a
Natural sunlight and soak-freeze-
thaw tolerance
ASTM D5722-08
ASTM D660 and/or D662 and/or
D714 and/or D772 and/or D4214
and/or D610b
ASTM D6695-08 or
MIL-PRF-322390
Adhesion strength
ASTM D7234-05
ASTM D4541 -09e1d
N/A = Not Applicable
a For organic coatings only.
b As a follow up to D5722-08; not meant to replace D5722-08.
c Only for the concentrated natural light part of D5722-08; MIL-PRF = Military Performance Standard
d For surfaces other than concrete.
7.2 Data Quality Indicators
Data quality indicators (DQIs) for the critical measurements were used to determine if the collected data
met the QA objectives. The mean value of at least four replicate tests was used to assess pass/fail for
that portion of the test. A list of the DQIs is given in Table 7-3. The DQIs established in the QAPP were
selected without specific knowledge of the coatings and their characteristics. One objective of the
verification of the test methods was to verify that these were realistic goals for the coatings being tested.
The equipment used to make the critical measurements was calibrated as per the requirements of the
respective ASTM methods.
7.3 Assessment of DQI Goals
The representativeness of the experiments was ensured by the careful selection of the concrete and
steel coupons and experimental conditions. The parameters that were used to assess whether the data
met the quality assurance objectives (as detailed in Table 7-3) include precision, accuracy, and
completeness of the collected data. A detailed discussion of these measures is included in Appendix G.
17
-------
Table 7-3. DQIs for critical measurements
Measurement
Parameter
Test Method
Pass Value
Accuracy
Precision/
Repeatability
Completeness
%
Shelf Life
Freeze/Thaw
Resistance of
Organic Coatings
ASTM D2337
Less than 10%
difference in viscosity
±15%
±20%
90
Settling Properties
ASTM D1309 or
ASTM 869
At least 8 on the
scale from 10 to 0*
N/A
N/A
90
Accelerated Storage
Stability
MIL-PRF-32239
Less than 10%
difference in viscosity
and density
compared to before
accelerated test
±15%
±20%
90
Density
ASTM D1475
Less than 10%
difference
±15%
±20%
90
Viscosity
ASTM D2196
Less than 10%
difference
±15%
±20%
90
Weatherability
Water resistance
ASTM D2247-02
<10% adhesion loss
N/A
N/A
90
Tensile Strength
ASTM D2370-98
(organic-based
coatings)
ASTM D6083-05e1
(water-based
coatings)
>35 kg/cm2
(kilograms/centimeter
squared)
(500 psi)
±15%
±20%
90
Abrasion resistance
ASTM D4060-07
<10% weight loss
±15%
±20%
90
Natural sunlight and
soak-freeze-thaw
tolerance
ASTM D5722-08
Note surface
blemishes
N/A
N/A
90
Adhesion strength
ASTM D7234-05
>3.5 kg/cm2 (>50 psi)
±15%
±20%
90
* "8" signifies a definite feel of settling; no resistance to sidewise movement. This is a very subjective test and the
ratings are listed as word expressions; there are no units.
N/A=Not Applicable
18
-------
8.0 Summary of test data
8.1 Summary
Each of the four coatings was subjected to the individual test methods recommended for each material
property within both the shelf life and weatherability test methods. These tests were performed by KTA-
Tator Laboratories. The data resulting from each of these tests are shown in the tables within each of
the following sections.
8.2 Adhesion
Adhesion (pull-off strength) was measured in accordance with
ASTM D7234, "Standard Test Method for Pull-Off Adhesion
Strength of Coatings on Concrete Using Portable Pull-Off
Adhesion Testers", or ASTM D4541, "Pull-Off Strength of
Coatings Using Portable Adhesion Testers", Annex A4, "Self-
Aligning Adhesion Tester Type IV". Per the shelf life test method,
either adhesion test method is acceptable. However ASTM
D7234 is listed as the preferred method. For verification
purposes since both methods are listed as acceptable, both
methods were exercised. Both methods use the same
equipment to remove the pull stubs and the results were reported
as pounds per square inch (psi). However, the size of the pull
stub differs. ASTM D7234 for concrete specifies a 2" pull stub.
Coatings on the steel panels were evaluated per ASTM 4541
using a %" pull stub. Both of these methods include initial
performance under nominal laboratory conditions of temperature
and humidity (72 ± 5 °F and 50 ± 5 %RH) and under exposure to Figure 8-1. Adhesion test coupon
high humidity conditions (72 ± 5 °F and 95 ± 5 %RH) for 200
hours. Figure 8-1 shows a concrete coupon and pull stubs following the adhesion test.
The results shown in Tables 8-1 through 8-4 are presented in the following sequence: concrete-initial,
concrete after 200 hours humidity, steel, and steel after 200 hours humidity.
19
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Table8-1. Adhesion -concrete initial
Stub ID
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
ALARA 1146
CC Strip/CC Fix*
CC Strip/SBR 10*
Intergard 10220*
1
209
324
203
496
2
204
191
242
254
3
193
401
216
455
4
178
375
229
471
5
204
*
*
*
6
188
*
*
*
7
204
*
*
*
8
214
*
*
*
Average
199
323
223
419
Criteria
>50 psi
Result
Pass
Pass
Pass
Pass
* Per QAPP only four replicates were used
Table 8-2. Adhesion -concrete after 200-hr humidity
Stub ID
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
ALARA 1146
CC Strip/CC Fix**
CC Strip/SBR 10**
Intergard 10220**
1
178
71
168
433
2
115
46
117
407
3
229
*
163
445
4
159
*
137
344
5
38*
**
N/A
**
6
127
**
**
**
7
121
**
**
**
8
127
**
**
**
Average
151
29
146
407
Criteria
>50 psi
Result
Pass
Fail
Pass
Pass
* pull stub removed as test started
** Per QAPP only four replicates were used
20
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Table 8-3. Adhesion - steel initial
Stub ID
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
ALARA 1146
CC Strip/CC Fix
CC Strip/SBR 10
Intergard 10220
A
2522
1141
610.7
1670
B
2522
1161
610.7
1874
C
2382
1141
610.7
1711
D
2100
1182
610.7
1711
E
2382
1059
569.9
2038
F
2522
1059
488.3
1874
Average
2405
1124
584
1813
Criteria
>50 psi
Result
Pass
Pass
Pass
Pass
Table 8-4. Adhesion -steel after 200-hr humidity
Stub ID
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
Pull-Off
Strength (psi)
ALARA 1146
CC Strip/CC Fix
CC Strip/SBR 10
Intergard 10220
A
<200*
284.2
**
1386
B
<200*
**
508.7
1631
C
<200*
**
569.9
1631
D
<200*
202.6
549.5
1018
E
<200*
202.6
529.1
1345
F
1397
202.6
406.7
1549
Average
a
223b
513°
1427
Criteria
>50 psi
Result
-
Pass
Pass
Pass
* pull stub removed as test started; due to rusted panel
** pull stub removed as test started
a not able to calculate average
b average calculated using stubs A,D,E,F
c average calculated using stubs B,C,D,E,F
8.3 Taber abrasion resistance
Taber abrasion resistance was determined in accordance with ASTM D4060, "Test Method for Abrasion
Resistance of Organic Coatings by the Taber Abraser." Four 4" x 4" panels were weighed and then
21
-------
subjected to 1000 cycles using a 1000 g load and CS-17 abrasion wheel. Post-abrasion weights were
acquired for the samples and the weight loss (in mg) reported. The test results for the four coatings are
shown in Table 8-5.
8.4 Tensile strength
Tensile strength was determined in accordance with ASTM D2370, "Standard Test Method for Tensile
Properties of Organic Coatings." The resulting samples were maintained at ambient laboratory
conditions (72 ± 5 °F and 50 ± 5 %RH) for a minimum of 40 hours before testing. The samples were cut
to a width of 1/4" using a double blade cutter and were tested for tensile strength using a Tinius-Olsen
Universal Testing Machine (Tinius Olsen, Inc. Horsham, PA, USA). The results of the testing are shown
in Table 8-6 for each of the four coatings.
8.5 Stormer viscosity
Stormer viscosity was determined in accordance with ASTM D562, "Standard Test Method for
Consistency of Paints Measuring Krebs Unit (KU) Viscosity using a Stormer-Type Viscometer." Stormer-
Type viscometers are produced by various manufacturers and are used to determine the viscosity of
paints, similar to the coatings tested. The Stormer viscometer measurements were taken to satisfy the
requirements of the freeze/thaw resistance testing in ASTM D2337 for organic coatings in the shelf life
test method and also for aqueous coatings in ASTM D2243. Both ASTM methods, D2337 and D2243
were used only during the verification, using ALARA 1146. The remaining coatings were tested using
only ASTM D 2337. The results of the Stormer-Type viscometer measurements are shown in Table 8-7
for all four coatings.
22
-------
Table 8-5.
Taber abrasion resistance
Replicate
ID
ALARA 1146
CC Strip/CC Fix
CC Strip/SBR-10
Intergard 10220
Initial
Weight
(g)
Final
Weight
(g)
Weight
Loss
(mg)
Initial
Weight
(g)
Final
Weight
(g)
Weight
Loss
(mg)
Initial
Weight
(g)
Final
Weight
(g)
Weight
Loss
(mg)
Initial
Weight
(g)
Final
Weight
(g)
Weight
Loss
(mg)
A
70.6396
70.5242
115.4
65.0575
64.9883
69.2
66.3012
66.2403
60.9
65.1257
65.1182
7.5
B
71.1786
71.0676
111.0
65.4911
65.4199
71.2
65.2493
65.1860
63.3
64.9805
64.9667
13.8
C
70.6337
70.5195
114.2
65.3762
65.3066
69.6
66.5958
66.5353
60.5
65.3345
65.3189
15.6
D
70.9035
70.7887
114.8
64.8932
64.8194
73.8
66.5056
66.4495
56.1
65.1114
65.1027
8.7
Average
114
71
60
11
Criteria
<50 mg
<50 mg
<50 mg
<50 mg
Result
Fail
Fail
Fail
Pass
Table 8-6. Tensile strength
Replicate
ID
ALARA 1146
CC Strip/CC Fix
CC Strip/SBR-10
Intergard 10220
Force
(pounds
[lb])
Tensile
Strength
(psi)
Percent
Elongation
(%)
Force
(lb)
Tensile
Strength
(psi)
Percent
Elongation
(%)
Force
(lb)
Tensile
Strength
(psi)
Percent
Elongation
(%)
Force
(lb)
Tensile
Strength
(psi)
Percent
Elongation
(%)
1
13.28
1451
230
3.00
211
1144
12.56
581
1144
11.82
1876
764
2
13.43
1476
206
3.34
246
1358
13.01
602
1065
13.13
1945
696
3
13.31
1471
202
2.71
206
1704
11.55
531
1065
12.26
1946
658
5
14.51
1603
214
2.99
251
1022
13.05
585
1200
12.37
1918
668
8
11.96
1429
206
3.62
296
1201
14.32
663
1124
12.26
1916
628
Average
1486
242
592
1920
Criteria
>500 psi
>500 psi
>500 psi
>500 psi
Result
Pass
Fail
Pass
Pass
-------
Table 8-7. Stormer viscosity (Krebs Units)
Sample ID
Initial
After
Freeze/Thaw
(Cycle 1)
After
Freeze/Thaw
(Cycle 2)
Avg
%
Diff
Criteria
Result
ALARA
1146
ALARA 1146
105
93.7
72.4
99.33
11%
< 10%
Fail
CC
Strip/CC
Fix
CC VIS-Strip
102.9
Solid
--
-
-
-
-
CC Fix
67.2
Solid
--
-
-
-
-
CC
Strip/SBR-
10
VIS-Strip
102.9
Solid
-
-
-
-
--
SBR-10 Part A
49.6
50.9
-
50.2
2.6%
< 10%
Pass
SBR-10 Part B
90.7
87.5
-
89.1
3.6%
< 10%
Pass
SBR-10 Mixed
55.6
55.0
--
55.3
1.1%
< 10%
Pass
Intergard
10220
Intergard 10220
138
Solid
-
-
-
-
-
* Cycle 2 performed for Alara 1146 only
8.6 Brookfield viscosity
The viscosity was determined using a Brookfield
Viscometer (Brookfield Engineering Laboratories, Inc
Middleboro, MA, USA) (preferred method) in
accordance with ASTM D2196, "Standard Test Method
for Rheological Properties of Non-Newtonian Materials
by Rotational (Brookfield-Type) Viscometer." The
spindle type and speed used are largely a trial and error
process with the objective being to choose a
combination that will produce a display reading
between 10% and 100% torque. The two spindles and
speeds shown were used during the method verification
and were, therefore, used for all subsequent coatings
tested. The results for all four coatings are shown in
Tables 8-8 through 8-11. Figure 8-2 shows SBR-10
being measured for viscosity using a Brookfield
Viscometer.
Figure 8-2. Brookfield viscosity measurement
of SBR-10
24
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Table 8-8. ALARA1146 Brookfield viscosity (centipoises [cps])
Sample ID
Spindle 4
Speed-20 rpm**
Spindle 5
Speed-20 rpm
ALARA 1146-lnitial
7175
7400
ALARA 1146-After Storage
Stability
3400
3450
Viscosity Change (%)
71%
73%
Viscosity Change Criteria
<10%
<10%
Result
Fail
Fail
"""Revolutions per minute = rpm.
Table 8-9. CC Strip/CC Fix Brookfield viscosity (cps)
Sample ID
Spindle 4
Speed -20 rpm
Spindle 5
Speed -20 rpm
Initial
Post
Initial
Post
CC Strip
16950
No Reading*
10300
No
Reading*
Sample ID
Spindle 4
Speed -100 rpm
Spindle 5
Speed -100 rpm
Initial
Post
Initial
Post
CC Fix
865
820
425
380
Viscosity Change (%)
9.9%
11.2%
Viscosity Change
Criteria
<10%
<10%
Result
Pass
Fail
* Sample solidified after evaluation using MIL-PRF-32239
25
-------
Table 8-10. CC Strip/SBR-10 Brookfield viscosity (cps)
Sample ID
Spindle 4
Speed -20 rpm
Spindle 5
Speed -20 rpm
Initial
Post Cycle 3
Initial
Post Cycle 3
CC Strip (Initial)
16950
No Reading*
5000
No Reading*
Sample ID
Spindle 2
Speed -50 rpm
Spindle 2
Speed -100 rpm
Initial
Post Cycle 3
Initial
Post Cycle 3
SBR-10 Part A - After Storage
Stability (Cycle 3)
60
48
60
62
Viscosity Change(%)
12(22.2%)
2 (3.3%)
Viscosity Change Criteria
<10%
<10%
Result
Fail
Pass
Sample ID
Spindle 3
Speed -50 rpm
Spindle 4
Speed -50 rpm
Initial
Post Cycle 3
Initial
Post Cycle 3
SBR-10 Part B - After Storage
Stability (Cycle 3)
1190
1085
1180
1040
Viscosity Change (%)
5 (9.2%)
40(12.6%)
Viscosity Change Criteria
<10%
<10%
Result
Pass
Fail
Sample ID
Spindle 3
Speed -100 rpm
Spindle 4
Speed -100 rpm
Initial
Post Cycle 3
Initial
Post Cycle 3
SBR-10 Mixed - After Storage
Stability (Cycle 3)
710
230
760
200
Viscosity Change (%)
480 (102%)
560 (117%)
Viscosity Change Criteria
<10%
<10%
Result
Fail
Fail
* Sample solidified after evaluation using MIL-PRF-32239
26
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Table 8-11. Intergard 10220 Brookfield viscosity (cps)
Sample ID
Spindle 5
Speed -10 rpm
Spindle 6
Speed - 20 rpm
Initial
Post Cycle 3
Initial
Post Cycle 3
Intergard 10220
30000
(Too thick to read*)
24000
41250
Viscosity Change (%)
-
[17,250] 52.9%
Viscosity Change Criteria
<10%
<10%
Result
-
Fail
* Spindle and speed adjustments did not lead to a comparable result
8.7 Density
Density was determined in accordance with ASTM D1475, "Standard Test Method for Density of Liquid
Coatings, Inks, and Related Products." The instrument used was a Gardco U.S. Standard Cup (Paul N.
Gardner Company, Inc., Pompano Beach, FL, USA). The liquid material was tested prior to any
exposure and after the storage stability tests. The replicate average results for all four coatings are
shown in Table 8-12; results are reported as pounds per gallon (lb/gal).
Table 8-12. Density
Sample ID
Initial
(lb/gal)
After Storage
Stability (Cycle 3)
(lb/gal)
Density
Change
(%)
Density
Change
Criteria (%)
Result
ALARM 146
ALARA 1146
8.65
9.095
5.1
Pass
CC Strip/CC Fix
CC Strip
8.978
8.988
0
Pass
CC Fix
8.668
8.668
0
Pass
CC Strip
8.718
8.715
0
<10%
Pass
CC Strip/SBR-
SBR-10 Part A
8.874
8.880
0
Pass
10
SBR-10 Part B
8.836
8.806
0
Pass
SBR-10 Mixed
8.978
8.988
0
Pass
Intergard 10220
Intergard 10220
9.082
8.650
[4.8]
Pass
-------
9.0 Summary of results
Tables 9-1 and 9-2 present a summary of the test results for each coating in pass/fail format. None of
the four products tested passed all of the performance requirements successfully to meet both the five-
year shelf life and weatherability requirements. As specified in ASTM E-2731, the overarching
sequestration coating performance specification, the inability to pass all performance requirements does
not necessarily eliminate a particular product from consideration as a potential deployable asset. More
importantly, the data derived from subjecting potential products to the test methods described herein, as
well as those listed in the larger E-2731 specification, can be helpful to assist emergency planning and
response organizations as they make decisions regarding preparation for and response to a radiological
contamination event. A summary of the results for testing under the Shelf Life Test Method is presented
in Table 9-1 with results for Weatherability testing in Table 9-2. Some of the performance requirements
may prove difficult for any given product to meet. However, as mentioned in ASTM E-2731-09, a
product that meets some, but not all, of the performance requirements may have value for a particular
response and recovery scenario. The data derived from this testing may be used as a guide by which to
evaluate such products.
Table 9-1. Summary of results for shelf life
Freeze/Thaw
Resistance
Settling
Accelerated Storage
Stability
Density
Viscosity
ASTM D2337
ASTM D1309
D869
MIL-PRF-32239
ASTM
D1475
ASTM
D2196
ALARA 1146
Fail
Pass
Fail-Viscosity
Pass-Density
Pass
Pass
CC Strip/CC Fix
Fail
Fail-CC Strip,
Pass-CC Fix
CC Strip: Fail-Viscosity
Pass-Density
CC Fix: Pass-Viscosity
Pass-Density
Pass
Pass
CC Strip/SBR-10
Fail-CC Strip
Pass-SBR-10
Fail-CC Strip
Pass-SBR-10
CC Strip: No Viscosity
Pass-Density
SBR-10: Fail-Viscosity
Pass-Density
Pass
Pass
Intergard 10220
Fail
Fail
Fail-Viscosity
Pass-Density
Pass
Pass
28
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Table 9-2. Summary of results for weatherability
Water
Resistance
Tensile
Strength
Abrasion
Resistance
Natural Sunlight
Soak-Freeze-Thaw
Tolerance*
Adhesion
Strength
ASTM D2247
ASTM
D2370
ASTM D4060
ASTM D5722
ASTM D7234
ALARM 146
Pass-
Concrete
Fail-Steel
Pass
Fail
-
Pass-
Concrete
Pass-Steel
CC Strip/CC Fix
Pass-
Concrete
Pass-Steel
Fail
Fail
-
Pass-
Concrete
Pass-Steel
CC Strip/SBR-10
Pass-
Concrete
Pass-Steel
Pass
Fail
-
Pass-
Concrete
Pass-Steel
Intergard 10220
Pass-
Concrete,
Pass-Steel
Pass
Pass
-
Pass
* Testing not conducted
29
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Appendix A - Shelf Life Test Method
-------
Testing Procedure for Assessing Shelf Life of Containment Coatings
1. Scope
1.1 This specification is intended to provide a basis for testing of materials used to immobilize
radioactive contamination and facilitate subsequent decontamination. These materials are
herein named containment coatings (CCs).
1.2 This specification provides a set of test methods to be used to evaluate properties of CCs
intended for use to prevent the spread of radioactive contamination. Some of the test
procedures are provided as accelerated methods. However, other test procedures are available
to evaluate the candidate coating on a non-accelerated basis.
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses
are mathematical conversions that are provided for information only and are not considered
standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with
its use. It is the responsibility of the user of this standard to establish appropriate safety and
health practices and to determine the applicability of regulatory limitations prior to use. A CC
must be qualified nonhazardous as defined by US EPA and US DOT. CC must also be nontoxic as
an aerosol, vapor, liquid, or solid after application and curing.
1.5 User should refer to ASTM E2731-09: Standard Specification for Materials to Mitigate the
Spread of Radioactive Contamination after a Radiological Dispersion Event
2. Referenced Documents
2.1 ASTM Standards:
E2731-09 Standard Specification for Materials to Mitigate the Spread of Radioactive
Contamination after a Radiological Dispersion Event
D562-01(2005) Standard Test Method for Consistency of Paints Measuring Krebs Unit (KU)
Viscosity Using a Stormer-Type Viscometer
D869-85R04 Standard Test Method for Evaluating Degree of Settling of Paints
D1309-93R04 Settling Properties of Traffic Paints During Storage
D1475-98R08 Density of Liquid Coatings, Inks, Related Products
D2196-10 Viscosity by Brookfield viscometer
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D2337-01R05 Freeze-Thaw Stability of Multicolor Lacquers
D4287-00R05 High-Shear Viscosity Using a Cone/Plate Viscometer
D7395-07 Cone/Plate Viscosity at a 500 s-1 Shear Rate
2.2 Military Standards
MIL-PRF-32239 Coating System, Advanced Performance - Accelerated Storage Stability
3. Terminology
3.1 Definitions:
containment coating—film-forming product used to physically or chemically hold or bind
radioactive particulates; containment does not mean affecting the radioactivity or the decay
process of the radioactive contamination
containment coating film—material that results from the application of the containment
coating
immobilize—to fix in place; to prevent movement or re -formation of aerosol of particulates
due to mechanical or environmental forces such as by tracking, precipitation, or wind
weatherability - the ability of a containment coating to withstand weathering without
degradation of performance. Weathering is defined as exposure to a variety of outdoor
environmental conditions; for example, ultraviolet (UV) exposure, water, high and low
temperatures, and common bacteria
4. Significance and Use
4.1 This specification establishes test methodology for a CC that is intended to immobilize
dispersible radioactive contamination deposited on buildings and equipment as might result
from a radiological dispersal device (RDD) event.
4.2 The intended use of this the CC addressed in this specification is primarily in an urban
environment; however, it may be used in other environments such as suburban or rural areas.
4.3 The CC is intended to be removable during subsequent decontamination and recovery
operations. It is intended to prevent the radioactive contamination from further migration, re-
suspension into the air; and spreading as a result of external forces.
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5.0 Minimum Performance Criteria
Minimum performance criteria for CCs have been established by E2731-09 Standard
Specification for Materials to Mitigate the Spread of Radioactive Contamination after a
Radiological Dispersion Event. E2731-09 specifies the following physical parameters for a CC:
Tensile Strength 35 kg/cm2 (500 psi), Adhesion >3.5 kg/cm2 (>50 psi) on concrete, Abrasion <50-
mg (0.002-oz) loss, Tear Strength 14 kg/cm2 (200 psi), Flammability - does not burn. E2731-09
also specifies a required shelf life of a minimum of 5 years and the CC, or stabilizer film, must
meet the above physical parameters for a period of one year under weather conditions as
described in 3.1. Any CC being evaluated for approval which meets some, but not all, of these
performance criteria may still be considered to have value. However, all CCs must meet the
requirements as specified in E2731-09 before being considered for the tests as stated in this
protocol.
6.0 Shelf Life
The following six test methods, or a combination of, shall be used to simulate and evaluate the
effect of shelf life on properties of the CC. Test methods for viscosity shown in 6.6 and 6.7 are
offered as alternatives to 6.5 depending upon shear tolerance. If an uncontrolled climate
storage facility is used, the CC must meet the requirements of 6.2. This would be used for
organic coatings. If a climate-controlled facility is used, the CC must meet the requirements of
6.3. This would be used for aqueous-based coatings. It should be noted that some of the tests
require the coating to be tested on the substrate, whereas, other tests require the coating to be
tested attached to the substrate. However, the CC must meet the applicable tests chosen in
addition to the other tests as presented below. These test methods will be used to identify
potential degradation of a coating by performing the accelerated and non-accelerated test(s).
The test method results will identify any deficiencies of a coating to be applied as intended and
will establish and verify the ability of a coating to possess successful shelf life performance. For
each test method below, the equipment needed is listed first followed by the methodology of
the test. Table 1 below provides a menu of properties for testing the shelf life of a CC. For each
property, the table gives a preferred method as well as alternate methods, when available.
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Property Describing Shelf Life
Preferred Method
Alternate Methods
Freeze/Thaw Resistance of
Coatings
ASTM D2337/l
N/A
Settling Properties
ASTM D1309/869
N/A
Accelerated Storage Stability
MIL-PRF-32239
N/A
Density
ASTM D1475
N/A
Viscosity
ASTM D2196
ASTM D562; ASTM D4287;
ASTM D7395
A Although ASTM D2337 is titled "Freeze/Thaw Resistance of Organic Coatings", this method will be
used for both lacquers or organic coatings as well as aqueous-based coatings.
6.1 Freeze-Thaw Resistance of Coatings1 -modified
To be used for all coatings (lacquers or organic coatings as well as aqueous-based
coatings).
6.1.1 Equipment Needed
Cold box capable of -3.9 °C (25 °F); Brooksfield viscometer, accurate timer
6.1.2 Methodology
ASTM D2337-01R05 will be modified as stated. Perform thirty cycles of 16 hours at -3.9 ± 5 °C
(25 ± 5 °F) followed by 8 hours at room temperature, 22.2 ± 3 °C (72 ± 5 °F). Following the
completion of above described thirty cycles, perform ASTM D2196 or other suitable method to
check viscosity (see 6.5 below). CC manufacturer shall specify the recommended viscosity
range when tested in accordance with 6.5.
6.2 Settling Properties2
Accelerated method (modified) that simulates in 2 weeks the settling that might occur
during 12 months of storage.
6.2.1 Equipment Needed
Freezer capable of -15 to -12.2 °C (5 to 10 °F) temperature range , oven capable of up to at least
71.1 °C (160 °F), spatula
1 D2337-01R05 Freeze-Thaw Stability of Multicolor Lacquers
2 D1309-93R04 Settling Properties of Traffic Paints During Storage
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6.2.2 Methodology
Accelerated test with a 14 day cycle; Freezer, set to -13 °C (8.6 °F) -8 AM; Oven-10 AM; Freezer-
12 PM; Oven-2 PM, followed by a 16-hr cycle at room temperature for five days. From 4 PM
Friday until 8 AM Monday, leave at room temperature. Freezer-8 AM Monday and repeat cycle
for 7 more days. Each time can of coating is removed from the oven, tap sharply on bench-top.
At completion of exposure, allow to cool at room temperature and determine degree of settling
per ASTM D8693.
Use a standard 500-ml (1 pint) friction top paint container. Prepare a spatula with square-end
blade 12.1 cm (4 % in) length and approximately 2.1 cm (13/16 in) width weighing 45 ± 1 g (1.6
oz) will be used to examine the paint for settling. Drop spatula in coating to determine degree
of settling per ASTM D869. The conditions of the CC should be designated as following:
Rating Description of Paint Condition
10 Perfect suspension. No change from the original condition of the paint.
8 A definite feel of settling and a slight deposit brought up on spatula. No significant
resistance to sidewise movement of spatula.
6 Definite cake of settled pigment. Spatula drops through cake to bottom of container
under its own weight. Definite resistance to sidewise motion of spatula. Coherent
portions of cake may be removed on spatula.
4 Spatula does not fall to bottom of container under its own weight. Difficult to move
spatula through cake sidewise and slight edgewise resistance. Paint can be remixed
readily to a homogeneous state.
2 When spatula has been forced through the settled layer it is very difficult to move
spatula sidewise. Definite edgewise resistance to movement of spatula. Paint can be
remixed to a homogeneous state.
0 Very firm cake that cannot be reincorporated with the liquid to form a smooth paint
by stirring manually.
6.3 Accelerated Storage Stability4
6.3.1 Equipment Needed
Oven capable of 60 °C (140 °F)
6.3.2 Methodology
3 D869-85R04 Standard Test Method for Evaluating Degree of Settling of Paint
4 MIL-PRF-32239 Coating System, Advanced Performance - Accelerated Storage Stability
-------
Store at 60 °C (140 °F) for seven days, cool to room temperature 22.2 °C (72 °F) and check
density (D1475) and viscosity (D2196). Compare density and viscosity to values before
subjecting to accelerated test. See 6.4 and 6.5. below, respectively. Any difference in values
before and after accelerated test could indicate degraded CC during extended storage
conditions.
6.4 Density5
6.4.1 Equipment Needed
Standardized cup, balance, Type II water
6.4.2 Methodology
Use standardized cup, fill with water and determine volume; fill with liquid and weigh to
determine density
6.5 Viscosity6
6.5.1 Equipment Needed
Brookfield viscometer, spindles, Brookfield reference chart (spindle/speed), thermometer
6.5.2 Methodology
Use a quart can or a large beaker (600 ml or greater) that will accommodate the spindle guard.
Add sufficient coating to cover the 'mark' on the spindle. The spindle and speed are selected
such that the generated value is between 20 and 80 on the dial. If the value is lower than 20 or
higher than 80, disregard and select a different spindle/speed until the generated value falls
between 20 and 80 on the dial.
6.6 High-shear Viscosity7
To be used with liquids that can stand high shear rate
6.6.1 Equipment Needed
Cone/plate viscometer
6.6.2 Methodology
Evaluate flow properties (viscosity) of CC under high shear conditions similar to brushing,
spraying, or roll coating. Repeat viscosity determination with two specimens. If the two
viscosity determinations differ by less than 7 %, calculate the mean and report as the high-
5 D1475-98R08 Density of Liquid Coatings, Inks, Related Products
6 D2196-10 Viscosity by Brookfield viscometer.
7 D4287-00R05 High-Shear Viscosity Using a Cone/Plate Viscometer
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shear viscosity for the material. If the values differ by more than 7 %, make a third
determination. If no two readings are within 7 % of each other, the material is not suitable for
testing by this method. For CCs that cannot withstand shear in D4287, use D7395.
6.7 Low Shear Viscosity - Cone/Plate Viscosity8
To be used with liquids at a shear rate of 500 s"1; liquids that cannot stand shear rate as
prescribed in D4287
6.7.1 Equipment Needed
Cone/plate viscometer
6.7.2 Methodology
Evaluate flow properties (viscosity) of CC under low shear conditions similar to procedure used
in 6.6. Repeat viscosity determination with two specimens. If the two viscosity determinations
differ by less than 7 %, calculate the mean and report as the high-shear viscosity for the
material. If the values differ by more than 7 %, make a third determination. If no two readings
are within 7 % of each other, the material is not suitable for testing by this method.
8 D7395-07 Cone/Plate Viscosity at a 500 s-1 Shear Rate
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Appendix B - Weatherability Test Method
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Testing Procedure for Assessing Weatherability of Containment
Coatings
1. Scope
1.1 This specification is intended to provide a basis for testing of materials used to immobilize
radioactive contamination and facilitate subsequent decontamination. These materials are
herein named containment coatings (CCs).
1.2 This specification provides a set of test methods to be used to evaluate properties of CCs
intended for use to prevent the spread of radioactive contamination. At this time this
specification describes a test method to evaluate the weatherability of CCs. Some of the test
procedures are provided as accelerated methods. However, other test procedures are available
to evaluate the candidate coating on a non-accelerated basis.
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses
are mathematical conversions that are provided for information only and are not considered
standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with
its use. It is the responsibility of the user of this standard to establish appropriate safety and
health practices and to determine the applicability of regulatory limitations prior to use. A CC
must be qualified nonhazardous as defined by US EPA and US DOT. CC must also be nontoxic as
an aerosol, vapor, liquid, or solid after application and curing.
1.5 User of this specification should refer to ASTM E2731 - 09: Standard Specification for
Materials to Mitigate the Spread of Radioactive Contamination after a Radiological Dispersion
Event.
2. Referenced Documents
2.1 ASTM Standards:
E2731 - 09 Standard Specification for Materials to Mitigate the Spread of Radioactive
Contamination after a Radiological Dispersion Event
D610 Standard Practice for Evaluating Degree of Rusting on Painted Steel Surfaces
D660 Standard Test Method for Evaluating Degree of Checking of Exterior Paints
D662 Standard Test Method for Evaluating Degree of Erosion of Exterior Paints
D714 Standard Test Method for Evaluating Degree of Blistering of Paints
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D772 Standard Test Method for Evaluating Degree of Flaking (Scaling) of Exterior Paints
D2247-02 Standard Practice for Testing Water Resistance of Coatings in 100% Relative Humidity
D2370-98 Standard Test Method for Tensile Properties of Organic Coatings
D4060-07 Standard Test Method for Abrasion Resistance of Organic Coatings by the Taber
Abraser
D4214 Standard Test Methods for Evaluating the Degree of Chalking of Exterior Paint Films
D4585-07 Standard Practice for Testing Water Resistance of Coatings Using Controlled
Condensation
D5722-08 Standard Practice for Performing Accelerated Outdoor Weathering of Factory-
Coated Embossed Hardboard Using Concentrated Natural Sunlight and a Soak-Freeze-Thaw
Procedure
D6083-05 Standard Specification for Liquid Applied Acrylic Coating Used in Roofing
D6695-08 Standard Practice for Xenon-Arc Exposures of Paint and Related Coatings
D7234-05 Adhesion Strength of Coatings on Concrete
2.2 Military Standards
MIL-PRF-32239 Coating System, Advanced Performance, for all Aerospace Applications
Weather Resistance: Xenon Arc vs. UV
3. Terminology
3.1 Definitions:
containment coating—film-forming product used to physically or chemically hold or bind
radioactive particulates; containment does not mean affecting the radioactivity or the decay
process of the radioactive contamination
containment coating film—material that results from the application of the containment
coating
-------
immobilize—to fix in place; to prevent movement or re -formation of aerosol of particulates
due to mechanical or environmental forces such as by tracking, precipitation, or wind
weatherability - The ability of a containment coating to withstand weathering without
degradation of performance. Weathering is defined as exposure to a variety of outdoor
environmental conditions; for example, ultraviolet (UV) exposure, water, high and low
temperatures, and common bacteria
4. Significance and Use
4.1 This specification establishes test methodology for a CC that is intended to immobilize
dispersible radioactive contamination deposited on buildings and equipment as might result
from a radiological dispersal device (RDD) event.
4.2 The intended use of this the CC addressed in this specification is primarily in an urban
environment; however, it may be used in other environments such as suburban or rural areas.
4.3 The CC is intended to be removable during subsequent decontamination and recovery
operations. It is intended to prevent the radioactive contamination from further migration, re-
suspension into the air; and spreading as a result of external forces.
5. Minimum Performance Criteria
Minimum performance criteria for CCs have been established by E2731 - 09 Standard
Specification for Materials to Mitigate the Spread of Radioactive Contamination after a
Radiological Dispersion Event. E2731 - 09 specifies the following physical parameters for a CC:
Tensile Strength 3447 kPa (500 psi), Adhesion >345 kPa (>50 psi) on concrete, Abrasion <50-mg
loss (<0.002-oz), Tear 1379 kPa (200 psi), Flammability - does not burn. E2731 - 09 also
specifies a required shelf life of a minimum of 5 years and the CC, or stabilizer film, must meet
the above physical parameters for a period of one year under weather conditions as described
in 3.5. Any CC being evaluated for approval which meets some, but not all, of these
performance criteria may still be considered to have value. The CC will be applied per the
manufacturer's recommendations. It is assumed that the thickness of the coating will be
adequate enough to allow for removal from the surface to facilitate testing and perform as a
film as indicated in E-2731-09. It should be pointed out that while some test methods require
removal of the CC from panel, other methods allow for testing to be performed on a panel. All
materials to be tested will be performed on a standardized block of concrete prepared
according to Quality Assurance Project Plan, Revision 2 "Assessment of Water Wash Down for
Mitigation for Cesium Chloride Contamination Part II Pressure Washing", November 24, 2008
unless the test method specifies otherwise.
6.0 Weatherability
Weatherability tests as specified below shall be conducted with the CC that has been tested
according to E2731-09 and meets its requirements with regard to shelf life, working life, cure
time, immobilization of radioactive particles, and non-flammability. Specifically, weatherability
of the CC will be tested following its guaranteed shelf life time. The guaranteed shelf life time
prior to weatherability testing will be accomplished by either the actual storage time on the
-------
shelf or by accelerated shelf life tests as prescribed by the Shelf Life Method. For each
weatherability test method below, the equipment needed is listed first followed by the
methodology of the test. The weatherability testing will be comprised of the following:
• Water Resistance at 100% RH
• Tensile Properties
• Abrasion Resistance
• Natural Sunlight and Soak-Freeze-Thaw Procedure
• Adhesion strength of coatings on concrete
For a CC to be considered passing the weatherability test, it must satisfy the requirements of
each of the five methods above. Table 1 below provides a menu of properties for testing of
weatherability of a CC. For each property to be tested, the table gives a preferred method as
well as alternate methods, where available.
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Property Describing
Weatherability
Preferred Method
Alternate Methods
Water resistance
D2247-02
D4585-07
Tensile strength
D2370-98 (organic-based
coatings)
D6083 - 05el (water-based
coatings)
N/A
Abrasion resistance
D4060-07
D968 *
Natural sunlight and soak-
freeze-thaw tolerance
D5722-08
D660 and/or D662 and/or
D714 and/or D772 and/or
D4214 and/or D610 **
D6695-08 or MIL-PRF-32239
***
Adhesion strength
D7234-05
D4541 - 09el ****
N/A= Not Applicable
* for organic coatings only
** as a follow up to D5722-08; not meant to replace D5722-08
*** only for the concentrated natural light part of D5722-08
**** for surfaces other than concrete
6.1 Water Resistance1
Useful service of a CC may be predicted by knowing its resistance to water degradation. This
test method evaluates durability of a CC at 100% RH.
6.1.1 Equipment Needed
Enclosed fog chamber, thermostatically controlled heated water tank, thermometer
6.1.2 Methodology
Coated samples and control panel with known durability are placed at 15 degrees from vertical
in an enclosed fog chamber maintained at 38°C (100 °F) for a period of 300 hours. Color change,
blisters, loss of adhesion, softening, and embrittlement are observed after no less than 5 min
and no more than 10 min after removal from test. The CC shall be considered to be water
1 D2247-02 Standard Practice for Testing Water Resistance of Coatings in 100% Relative Humidity. Alternatively,
D4585-07 Standard Practice for Testing Water Resistance of Coatings Using Controlled Condensation may be used.
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resistant if no more than 10% loss of adhesion is measured following the water resistance test
and utilizing procedures described in D7234-05 Standard Test Method for Pull-Off Adhesion
Strength of Coatings on Concrete Using Portable Pull-Off Adhesion Testers. The remaining 90%
(or more) of the original adhesion strength following water resistance tests as prescribed by
D2247-02 will be sufficient to maintain the integrity of the CC on the coated surface.
6.2 Tensile Properties2
To determine tensile properties of organic coatings when tested as free films, D2370-98
Standard Test Method for Tensile Properties of Organic Coatings shall be used. However, for
water-based coatings, D6083-05 shall be used. D6083-05 clarifies test conditions regarding
testing tensile strength of water-dispersed protective roof coatings. The tensile strength
determined by D2370-98 (organic coatings) or by D6083 (water-based coatings) shall be at least
20% more than the adhesion strength as determined by D7234-05 Standard Test Method for
Pull-Off Adhesion Strength of Coatings on Concrete Using Portable Pull-Off Adhesion Testers.
Tensile strength at least 20% larger than the adhesion strength is necessary to assure efficient
removal of the CC from the coated surface.
6.2.1 Equipment Needed for D2370-98
Stationary micrometer, tensile tester with load capacities from 100 to 2000 g (3.5 to 70.5 oz),
precision specimen cutter, dental tin foil, sheet of polyethylene
6.2.2 Methodology for D2370-98
Free unsupported films of uniform thickness of the CC to be tested are prepared. Thickness of
films is measured and samples are conditioned for at least 24 hours at 22.2 ± 3 °C (72 ± 5 °F)
and 50 % RH. Next, samples are mounted in the tensile tester with pre-set target elongation
and with preset load application rate. Pull in kg (lb.) needed to rupture the film is measured.
6.2.3 Equipment Needed for D6083-05
The same equipment as for the D2370-98 above.
6.2.4 Methodology for D6083-05
Film measuring 75 mm (2.9 in) long by 13 mm (0.5 in) wide tested according to D2370-98 at
22.2 ± 3 °C (72 ± 5°F) at 50 % relative humidity.
6.3. Abrasion Resistance3
2 D2370-98 Standard Test Method for Tensile Properties of Organic Coatings and D6083 - 05Standard Specification
for Liquid Applied Acrylic Coating Used in Roofing
3 D4060-07 Standard Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser
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D4060-07 shall be used for testing of organic coatings applied at uniform thickness to plane,
rigid surface and properly cured. D4060-07 shall be also used for testing of water-based
coatings. D4060 was used in the past to determine abrasion resistance of water-based coatings
as well.4 To pass the test, the sample shall not lose more than 10% of its original weight. It is
assumed that weight loss of up to 10% will not compromise integrity of the CC.
6.3.1 Equipment needed
Taber abraser, revolutions counter, abrasive wheels, resurfacing medium, vacuum suction
6.3.2 Methodology
Samples coated with a CC are conditioned, weighted, then abrased on a revolving wheel for a
number of cycles. Following abrasion, sample is weighted again. Alternatively, D968 Test
Methods for Abrasion Resistance of Organic Coatings by Falling Abrasive, may be used for
organic coatings only.
6.4. Natural Sunlight and Soak-Freeze-Thaw Procedure5
Note: The method was originally developed for performing accelerated outdoor weathering of
factory-coated embossed hardboard.
6.4.1 Equipment Needed
Fresnel reflecting concentrator accelerated weathering machine described in G90, freezer
capable of sustaining minus 20 °C (minus 4 °F) temperature
6.4.2 Methodology
Sample and control panel with known durability are exposed to concentrated natural sunlight in
Fresnel machine (with periodic daytime surface water spray). Following this exposure to
concentrated natural sunlight, the soak-freeze-thaw procedure is implemented. The soak-
freeze-thaw cycle is comprised of immersion in Dl water at 25 °C (77 °F) for 1 hour, freezing at
minus 20 °C (minus 4 °F) for 12-15 hours, and thawing at room temperature for a minimum of 1
hour; 30 cycles are applied.
The following test methods may be used to determine changes in samples exposed to the soak-
freeze-thaw cycles:
• D660 (Standard Test Method for Evaluating Degree of Checking of Exterior Paints)
• D662 (Standard Test Method for Evaluating Degree of Erosion of Exterior Paints)
4 WATER-BASED ACRYLIC FLOOR COATING K0500 Series, Product Data Sheet by Krylon Industrial Coatings
5 D5722-08 Standard Practice for Performing Accelerated Outdoor Weathering of Factory- Coated Embossed
Hardboard Using Concentrated Natural Sunlight and a Soak-Freeze-Thaw Procedure
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• D714 (Standard Test Method for Evaluating Degree of Blistering of Paints)
• D772 (Standard Test Method for Evaluating Degree of Flaking (Scaling) of Exterior
Paints)
• D4214 (Standard Test Methods for Evaluating the Degree of Chalking of Exterior Paint
Films)
• D610 (Standard Practice for Evaluating Degree of Rusting on Painted Steel Surfaces)
For the above six test methods, the CC will be deemed as passing the test method only if less
than 5% of surface is affected. The 5% rate is considered to not significantly deteriorate the
integrity of the CC.
Xenon Arc6 Method D6695
This method may be used alternatively to the procedure involving exposure of the sample to
concentrated natural sunlight only as described above in D5722-08 Standard Practice for
Performing Accelerated Outdoor Weathering of Factory- Coated Embossed Hard board Using
Concentrated Natural Sunlight and a Soak-Freeze-Thaw Procedure. The D6695 method is used
to test accelerated exposure of general coatings which is associated with sunlight, moisture,
and heat.
Equipment Needed
Xenon-arc apparatus (conforming to requirements of G151 and G155), humidity chamber.
Methodology
After coating has been applied to a flat panel, the sample is conditioned at 23 °C (73.4 °F) and
50 %RH for at least 7 days. Exposure to xenon-arc light for specified time is described in Table 1
of D6695-08 (for general coatings, Cycle 1 is used with continuous light for 102 min at 50% RH).
Corresponding typical irradiances are given in Table 1 of D6695-08. The test methods listed
above in 6.4.2 above may be used to determine changes in exposed samples.
Another alternative to the concentrated natural light part of D5722-08 only may be Xenon Arc
testing described by MIL-PRF-322397. Equipment needed for this test is Xenon-arc weather-o-
meter type Q-Sun/3000 or Q-Sun/1000. In this method, test panels are exposed for 3000 hours
in a Xenon-arc weather-o-meter cycling between 102 minutes of light only and 18 minutes of
light and Dl water spray. After the exposure samples are examined for conformance to 3.6.9
Flexibility, Class 2: High Flexibility Coating System. For the CC to pass this test, it will exhibit no
cracking when tested according to 4.6.15.2 Low Temperature Flexibility of the MIL-PRF-32239.
6 D6695-08 Standard Practice for Xenon-Arc Exposures of Paint and Related Coatings
7 MIL-PRF-32239 Performance Specification-Coating System, Advanced Performance, for Aerospace Applications
Weather Resistance: Xenon Arc vs. UV
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6.5 Adhesion strength of coatings on concrete8
This test method describes procedures for evaluating the pull-off adhesion strength of a coating
applied to concrete. The test determines the greatest perpendicular force (in tension) that a
surface of coating can bear before a plug of coating is detached from the surface. This greatest
perpendicular force determined by D7234-05 must be at least 345 kPa (50 psi), as required by
E2731-09.
Alternatively, ASTM D4541-09el Standard Test Method for Pull-Off Strength of Coatings Using
Portable Adhesion Testers may be used for substrates other than concrete. The method
consists of several "sub-methods" (B through F) applicable to various substrates, e.g., plastic,
wood, etc. Sub-method A, previously addressing concrete substrate has been withdrawn.
According to ASTM D4541-09el, the standard was developed for metal substrates, but may be
appropriate for other rigid substrates such as plastic and wood. This test method uses a
portable pull-off adhesion tester capable of applying a concentric load and counter load to a
single surface so that coatings can be tested even though only one side is accessible.
6.5.1 Equipment Needed
Pull-off adhesion tester, force applicator, and timer for control of the rate of stress application.
6.5.2 Methodology
CCs thicker than 0.5 mm (0.02 in) must be scored in the direction normal to the surface of the
CC. The adhesive is then applied between the surface of the CC to be tested and the fixture.
After the adhesive has cured, adhesion tester is applied to the fixture. The load is applied in a
smooth and gradual manner until the failure (separation of the CC from the surface). The force
attained at failure is recorded and pull-off adhesion strength is calculated. Finally, the substrate
failure or other modes of failure are classified.
8 D7234-05 Standard Test Method for Pull-Off Adhesion Strength of Coatings on Concrete Using Portable Pull-Off
Adhesion Testers
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Appendix C - KTA Test Report - ALARA 1146
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August 8, 2013
Via Email: brent.hall@arcadis-us.com
Mr. Brent Hall
ARCADIS U.S., Inc.
4915 Prospectus Drive, Suite F
Durham, NC 27713-4408
SUBJECT: Laboratory Testing of Strippable Coating; KTA-Tator, Inc. Project No. 320715-R2
Dear Mr. Hall:
In accordance with KTA Proposal PN120083 and ARCADIS U.S. Inc. (ARCADIS)
Work Authorization No. D12-0178, KTA-Tator, Inc. (KTA) has tested a coating material to
several different requirements to determine the resulting physical properties. This report
describes the laboratory techniques used and contains the results of the testing.
SAMPLES
The samples listed in Table 1, "Samples" were received from ARCADIS on the dates
listed. It should be noted that at no time did KTA personnel witness the acquisition or
manufacturing of the samples.
Table 1 - Samples
Sample
ID
Sample Description
Date Received
KTA-1
Three 1-gallon cans of Alara 1146, Lot # L787-072, Blue 0100.
Arrived damaged and leaking.
October 31,2012
KTA-2
Two 1-gallon cans of Alara 1146, Lot #L787-161, Blue 0100.
Not damaged or leaking.
November 20,2012
KTA-3
Thirteen concrete panels for application of coating and testing
measuring 6"x6".
October 31,2012
LABORATORY INVESTIGATION
The laboratory investigation consisted of exposure of the liquid material to different
thermal cyclic conditions to simulate storage and freeze/thaw possibilities followed by
evaluations of viscosity, density and settling. The coating film was tested to determine the
resistance to humidity and abrasion. The film was also tested to determine the tensile adhesion
KTA-Tator, Inc.
115 Technology Drive
Pittsburgh, PA 15275
412.788.1300
wwiv.Ma.com
-------
value and the tensile strength. Since the first shipment of material was leaking, the cans were not
used for testing. All of the testing was performed using Lot #L787-161.
Thermal Cycling
Four different conditions of thermal cycling or exposure were evaluated for this testing
protocol. Each condition is described in a paragraph below. The coating was evaluated by
different methods at the conclusion of the exposure. The results are addressed in the sections
explaining the test methods employed for the evaluations. Each of the cyclic tests was assigned
a number and a short designation for each is referenced in the correspondence results tables.
Cycle 1 - Freeze/Thaw of Solvent based materials
Thermal cycling was performed in accordance with ASTM D2337-01(10), "Standard
Test Method for Freeze-Thaw Stability of Multicolor Lacquers". This test method was
performed to determine the resistance of the solvent based liquid coating material to cycles of
freezing and thawing. The duration of the test was 30 cycles. The cycles occurred on weekdays.
The can remained in the freezer during the weekends. The thermal cycling conditions for this
test consisted of sixteen hours at 25 ± 3°F and eight hours at room temperature (72 ± 5°F). The
liquid material was evaluated by Stormer viscosity after exposure. A visual examination of the
coating revealed that the coating was lumpy initially, but could be mixed to a consistent fluid. A
%" to V" layer of material at the base of the can remained thick and did not mix in well during
hand mixing of the coating.
Cycle 2 - Freeze/Thaw of Water based materials
Thermal cycling was performed in accordance with ASTM D2243-95(08), "Standard
Test Method for Freeze-Thaw Resistance of Water-Borne Coatings". This test method was
performed to determine the resistance of the water based liquid coating material to cycles of
freezing and thawing. The duration of the test was 30 cycles. The cycles occurred on weekdays.
The can remained in the freezer during the weekends. The thermal cycling conditions for this
test consisted of seventeen hours at 25 - 30°F and seven hours at room temperature (72 ± 5°F).
The liquid material was evaluated by Stormer viscosity after exposure. The visual examination
of the coating revealed that there was some separation of a yellow translucent material. Mixing
incorporated the liquid, but the resulting material was not as thick as the original coating material
and had a sandy appearance.
Cycle 3 - Storage Exposure
Thermal cycling was performed in accordance with ASTM D1309-93(10), "Standard
Test Method for Settling Properties of Traffic Paints During Storage". This test method was
performed to determine the resistance of the liquid coating material to cycles of freezing and
heating. The duration of the test was 14 cycles. The cycles occurred on weekdays. The can
remained in the at room temperature in the evenings and on the weekends. The thermal cycling
conditions for this test consisted of two hours at 5 - 10°F, followed by two hours at 160°F.
These cycles were repeated twice, then followed by 16 cycle at room temperature. The 8 hour
cycle was completed during work hours. The liquid was evaluated for settling after exposure.
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The immediate visual evaluation revealed skinning of the coating material that had been in
contact with the interior surface of the lid and the sides of the can until the top surface of the
liquid material (about Vi" to 3A" down the side of the can). The liquid material was examined for
settling and the results are included below
Cycle 4 - Storage Stability
Thermal cycling was performed in accordance with military specification MIL-PRF-
32239, "Standard Method for Accelerated Storage Stability". This test method was performed to
determine the resistance of the water based liquid coating material to extended heat exposure.
The can remained in the oven set at 140°F for the 7 day duration of the test. The liquid material
was requested to be evaluated for changes in viscosity using the Ford Cup, but the initial coating
was too viscous for evaluation using the Ford Cup # 4. Subsequently, the viscosity was
evaluated by Brookfield viscosity after exposure. Additionally, the density of the material was
evaluated after exposure. A visual examination of the material reveals a slight separation of a
translucent layer. Mixing revealed that the layer was incorporated and the resulting material
appeared much like the unexposed coating material.
Stormer Viscosity
Stormer viscosity was determined in accordance with ASTM D562-10, "Standard Test
Method for Consistency of Paints Measuring Krebs Unit (KU) Viscosity Using a Stormer-Type
Viscometer." Readings were taken once the samples were brought to 25 ± 0.2°C, and recorded in
Krebs units (KU). Baseline viscosity readings were obtained on liquid material that was not
exposed to any of the conditions listed above. The results can be found in Table 2, "Results of
Stormer Viscosity."
Table 2 - Results of Stormer Viscosity Evaluation
Sample ID
Initial
After Freeze/Thaw
(Cycle 1)
After Freeze/Thaw
(Cycle 2)
Alara 1146
105 KU
93.7 KU
72.4 KU
Ford Cup Viscosity
Ford cup viscosity was requested for the sample that was scheduled to undergo Cycle 4,
storage stability. The initial sample was set for testing in accordance with ASTM D1200-10,
"Standard Test Method for Viscosity by Ford Viscosity Cup." For this type of viscosity
measurement, the liquid sample was stirred and its temperature was brought to 25 ± 0.2°C. Ford
Cup #4 was filled with the prepared sample with the orifice at the bottom of the cup plugged
with the analyst's finger. The finger was removed and a timer was simultaneously started. The
viscosity is determined by the time of the first break in the stream, using a stopwatch. The liquid
coating supplied for this testing did not flow through the orifice, leading to continual breaks in
the stream. The coating material did not empty from the cup in less than 20 minutes and the
testing was discontinued. ARCADIS was contacted and a mutual decision to evaluate the
viscosity using the Brookfield viscometer was accepted.
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Brookfield Viscosity
The Brookfield viscosity was determined in accordance with ASTM D2169-10,
"Standard Test Method for Rheological Properties of Non-Newtonian Materials by Rotational
(Brookfield type) Viscometer." The temperature of the sample was raised to 25 ± 0.2°C. No
spindle number or speed was specified for this product, so spindle 4 and 20 RPM speed were
selected. The second set of tests was performed using spindle 5 and a speed of 20 RPM, for
confirmation. For this testing, the spindle was lowered into the sample until the immersion mark
on the spindle shaft touched the sample. The viscometer was turned on and the pointer was
allowed to make several rotations until it had stabilized. Once the pointer stabilized, the
viscometer was stopped by simultaneously pressing down on the power and hold switches. The
viscosity reading was multiplied by the spindle factor, and recorded in centipoise (cps) units.
The same procedure was used for the second set of conditions. The average result is value
reported. The results can be found in Table 3, "Results of Brookfield Viscosity."
Table 3 - Results of Brookfield Viscosity Evaluation
Sample ID
Spindle 4
Speed - 20 rpm
Spindle 5
Speed - 20 rpm
Alara 1146 - Initial
7175 cps
7400 cps
Alara 1146 - After Storage Stability
(Cycle 4)
3400 cps
3450 cps
Density
Density was determined in accordance with ASTM D1475-98(08), "Standard Test
Method for Density of Liquid Coatings, Inks, and Related Products." A calibrated cup was
weighed empty and then weighed full of liquid coating. The air bubbles were eliminated from
the coatings as much as feasible by gently tapping the cup. The liquid material was tested prior
to any exposure and then after the storage stability described in Cycle 4. Calculations were
performed, and the results of the testing are listed in Table 4, "Density Results."
Table 4 - Density Results
Sample ID
Initial
After Storage Stability
(Cycle 4)
Alara 1146
8.65 lb/gal
9.095 lb/gal
Degree of Settling
The degree of settling was evaluated in accordance with ASTM D869-85(ll), "Standard
Test Method for Evaluating Degree of Settling of Paint. This method requires that the coating
material not be shaken or stirred after exposure, prior to the settling evaluation. In this case, the
coating had skinned over where it had been in contact with the interior surface of the lid. The
skin was removed and a blunt tipped spatula was dropped into the coating. The spatula hit the
base of the can with a metallic sound, indicating that no settling had occurred in the 14 days of
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cyclic exposure represented in Cycle 3 - Storage Exposure. This testing would receive a
settling value of 10.
Humidity Resistance
The coating was applied over both concrete and steel panels and permitted to dry for a
minimum of 7 days prior to testing. The resulting panels were tested for humidity resistance in
accordance with ASTM D2247-11, "Standard Practice for Testing Water Resistance of Coatings
in 100% Relative Humidity." The coated panels were placed on the exterior of an enclosed
chamber containing a heated, saturated mixture of air and water vapor. At an internal condition
of 100°F and 100% relative humidity, the temperature difference between the specimen surface
and the surrounding vapor causes the formation of condensation on the interior (painted surface)
of the panels. The samples were subjected to 200 hours of humidity exposure. Initially, the
exposure was scheduled for a duration of 300 hours, but the panels were displaying cracks and
discoloration. The exposure was discontinued at the request of ARCADIS. After the exposure
time has elapsed, the coated panels were evaluated for loss of tensile adhesion. The results are
listed in the section titled Tensile Adhesion Strength.
Tensile Adhesion Strength
Tensile adhesion (pull-off strength) was measured in accordance with ASTM D4541-
09el, "Pull-Off Strength of Coatings Using Portable Adhesion Testers," Annex A4, "Self-
Aligning Adhesion Tester Type IV" or ASTM D7234-12, "Standard Test Method for Pull-Off
Adhesion Strength of Coatings on Concrete Using Portable Pull-Off Adhesion Testers." Both of
the methods use the same equipment to remove the pull stubs. The main difference between the
test methods is the size of the pull stubs. The ASTM D7234-12 for concrete specifies the 2" pull
stub. The coating on the steel panels was evaluated using the Vi" pull stub.
For both methods, the testing surfaces were wiped clean and abraded gently using fine
sandpaper. Pull stubs with an abraded test surface were attached to the coating using a two
component epoxy adhesive (Araldite 2011), which was allowed to cure for a minimum of
twenty-four hours at ambient laboratory conditions (70 ± 2°F and 50 ± 5% relative humidity).
The 2" pull-stubs were then detached using a self-aligning pneumatic adhesion tester (PATTI-
Pneumatic Adhesion Tensile Testing Instrument) employing the F8 piston (range: 25-255 psi).
The Vi" pull stubs were detached using the F4 piston, which has a range of 202-2039 psi for the
small diameter pull stub. The pressure required to remove each pull-stub was recorded along
with the location of break and approximate percentage of each. The location of break is defined
as adhesive (a split between layers), cohesive (within a layer), or glue failure (coating strength
exceeds glue strength). The results of the testing can be found in Table 5, "Results of Tensile
Adhesion Testing."
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Table 5 - Results of Tensile Adhesion Testing
Coating
System
Pull
Stub
ID
Pull-Off
Strength
(psi)
Location of Break
Average
Pull-Off
Strength (psi)
Alara 1146
to Concrete
1
209
100% adhesive at the concrete interface
199
2
204
100% adhesive at the concrete interface
3
193
100% adhesive at the concrete interface
4
178
100% adhesive at the concrete interface
5
204
100% adhesive at the concrete interface
6
188
100% adhesive at the concrete interface
7
204
100% adhesive at the concrete interface
8
214
100% adhesive at the concrete interface
Alara 1146
to Concrete
(After 200 hours
humidity)
1
178
80% adhesive to concrete, 20% cohesive
151*
2
115
85% adhesive to concrete, 15% cohesive
3
229
90% adhesive to concrete, 10% cohesive
4
159
60% adhesive to concrete, 40% cohesive
5
38
95% adhesive to concrete, 5% cohesive
6
127
95% adhesive to concrete, 5% cohesive
7
121
90% adhesive to concrete, 10% cohesive
8
127
95% adhesive to concrete, 5% cohesive
Alara 1146
to Steel
A
2522
100% adhesive at the steel interface
2405
B
2522
100% adhesive at the steel interface
C
2382
100% adhesive at the steel interface
D
2100
100% adhesive at the steel interface
E
2382
100% adhesive at the steel interface
F
2522
100% adhesive at the steel interface
Alara 1146
to Steel
(After 200 hours
humidity)
A
<200**
100% adhesive at the steel interface, rusted
< 1397
(only 1 value
reported)
B
<200**
100% adhesive at the steel interface, rusted
C
<200**
100% adhesive at the steel interface, rusted
D
<200**
100% adhesive at the steel interface, rusted
E
<200**
100% adhesive at the steel interface, rusted
F
1397
100% adhesive at the steel interface, rusted
Value from pull stub #5 not usedfor average. ** Pull stub removed as test started.
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Taber Abrasion Resistance
Taber abrasion resistance was determined in accordance with ASTM D4060-10, "Test
Method for Abrasion Resistance of Organic Coatings by the Taber Abraser." Four replicate 4" x
4" panels were weighed then subjected to 1000 cycles using a lOOOg load and CS-17 abrasion
wheels. Post weights were acquired for the samples, and the weight loss (in mg) reported. The
results of the testing are contained in Table 6, "Taber Abrasion Resistance Results."
Table 6 - Taber Abrasion Resistance Results
Coating
Replicate
Initial
Final
Weight Loss
Average Weight Loss
System
ID
Weight
Weight
(mg)
(mg)
A
70.6396
70.5242
115.4
Alara 1146
B
71.1786
71.0676
111.0
113.8
C
70.6337
70.5195
113.9
D
70.9035
70.7887
114.8
Tensile Strength
Tensile strength was determined in accordance with ASTM D2370-98(10), "Standard
Test Method for Tensile Properties of Organic Coatings." The samples were cut to a width of Vi"
using a double blade cutter. The resulting samples were maintained at ambient laboratory
conditions (70 ± 2° F and 50 ± 5% RH) for a minimum of 40 hours before testing. The samples
were tested for tensile strength using a Tinius Olsen Universal Testing Machine. The cross-head
speed used for testing was 2.0 in/min. The gage length of 1 - 2" was evaluated for three
samples. A gage length of 1" was selected due to the strength and elongation of the material.
The force (in pounds) required to break the sample and the sample dimensions were used to
calculate the tensile strength of each free film of coating in pounds per square inch (psi). The
ultimate length at break was used to calculate the elongation. The method requires testing of 10
specimens. The five specimens with the highest combination of properties were selected for
reporting. The results of the testing can be found in Table 7, "Results of Tensile Strength
Testing."
Table 7 - Results of Tensile Strength Testing
Sample
ID
Replicate
ID
Force
(lbs)
Tensile
Strength
(psi)
Average
Tensile
Strength
(psi)
Percent
Elongation
(%)
Average Percent
Elongation (%)
1
13.28
1451
230
Alara
1146
2
13.43
1476
206
3
13.31
1471
1486
202
212
5
14.51
1603
214
8
11.96
1429
206
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If you have any questions or comments regarding this report, please contact me by
telephone at 412-788-1300, extension 183, or by email at vsherbondy@kta.com.
Sincerely,
KTA-TATOR, INC.
A
Valerie D. Sherbondy
Senior Chemist
VDS/RNR:jsc
JN320715-R2
CIN: 205716
cc: Ms. Kim Egler of ARCADIS
R2 - A revision was issued to reference the four replicate taber panels in the text of the report.
(320715-R2 Arcadis.doc)
NOTICE: This report represents the opinion of KTA-TATOR, INC. This report is issued in conformance with generally
accepted industry practices. While customary precautions were taken to verify the information gathered and presented is
accurate, complete and technically correct, this report is based on the information, data, time, materials, and/or samples afforded.
This report should not be reproduced except in full.
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Appendix D - KTA Test Report - Instacote CC Strip/CC Fix
-------
June 6, 2013
Via Email: brent.hall@arcadis-us.com
Mr. Brent Hall
ARCADIS U.S., Inc.
4915 Prospectus Drive, Suite F
Durham, NC 27713-4408
SUBJECT: Laboratory Testing of Strippable Coating;
KTA-Tator, Inc. Project No. 320715-A3-R1
Dear Mr. Hall:
In accordance with KTA Proposal PN131249 and ARCADIS U.S. Inc. (ARCADIS)
Work Authorization No. D12-0178, KTA-Tator, Inc. (KTA) has tested a coating material to
several different requirements to determine the resulting physical properties. This report
describes the laboratory techniques used and contains the results of the testing.
SAMPLES
The samples listed in Table 1, "Samples" were received from InstaCote on the dates
listed. It should be noted that at no time did KTA personnel witness the acquisition or
manufacturing of the samples.
Table 1 - Samples
Sample
ID
Sample Description
Date Received
KTA-5
Three 1-gallon cans of InstaCote CC FIX, Batch # 101612100-1
January 30,2013
KTA-6
One 5-gallon pail of InstaCote CC Hi VIS-Strip #1 VIS-Strip,
Batch #012413-4-2
January 30,2013
LABORATORY INVESTIGATION
The laboratory investigation consisted of exposure of the liquid materials to different
thermal cyclic conditions to simulate storage and freeze/thaw possibilities followed by
evaluations of viscosity, density and settling. The applied coating system was tested to
determine the resistance to humidity and the tensile adhesion value (Table 5), while the topcoat
was tested to determine abrasion resistance (Table 6). A free-film sample of the coating system
was also tested to determine the tensile strength (Table 7).
KTA-Tator, Inc.
115 Technology Drive
Pittsburgh, PA 15275
412.788.1300
www.kta.com
-------
Thermal Cycling
Three different conditions of thermal cycling or exposure were evaluated for this testing
protocol. Each condition is described in a paragraph below. The coating was evaluated by
different methods at the conclusion of the exposure. The results are addressed in the sections
explaining the test methods employed for the evaluations. Each of the cyclic tests was assigned
a number and a short designation for each is referenced in the corresponding results tables.
Cycle 1 - Freeze/Thaw Stability
Freeze/ thaw thermal cycling was performed in accordance with ASTM D2337-01(2010),
"Standard Test Method for Freeze-Thaw Stability of Multicolor Lacquers." This test method
was performed to determine the resistance of the liquid coating material to cycles of freezing and
thawing. The duration of the test was 30 cycles. The cycles occurred on weekdays. The can
remained in the freezer during the weekends. The thermal cycling conditions for this test
consisted of sixteen hours at 25 ± 3°F and eight hours at room temperature (72 ± 5°F). The
liquid material was scheduled to be evaluated by Stormer viscosity after exposure. A visual
examination of the coating materials revealed that both coatings were solid and Stormer viscosity
readings could not be obtained.
Cycle 2 - Storage Exposure
Storage exposure was performed in accordance with ASTM D1309-93(2010), "Standard
Test Method for Settling Properties of Traffic Paints During Storage". This test method was
performed to determine the resistance of the liquid coating material to cycles of freezing and
heating. The duration of the test was 14 cycles, which occurred on weekdays. The can
remained at room temperature in the evenings and on the weekends. The thermal cycling
conditions for this test consisted of two hours at 5 - 10°F, followed by two hours at
approximately 160°F. These cycles were repeated twice, then followed by 16 hours at room
temperature (72 ± 5°F). The 8 hour cycle was completed during work hours. The liquids were
scheduled for evaluation of settling after exposure. The CC VIS-Strip had solidified and the
degree of settling could not be evaluated for settling. The CC Fix product remained liquid and
was evaluated for settling.
Cycle 3 - Storage Stability
Storage stability was performed in accordance with military specification MIL-PRF-
32239, "Standard Method for Accelerated Storage Stability". This test method was performed to
determine the resistance of the water based liquid coating material to extended heat exposure.
The can remained in the oven set at approximately 140°F for the 7 day duration of the test. At the
completion of the exposure, the liquid material was scheduled for evaluation of viscosity using a
Brookfield viscometer. Additionally, the density of the materials were to be evaluated after
storage stability exposure. A visual examination of the materials revealed that the majority of
the VIS-Strip material had solidified during the exposure. The small amount of liquid VIS-Strip
product was used to perform density testing. Not enough liquid was present for a viscosity
evaluation. The CC FIX material had remained liquid and fluid enough for testing. A
photograph of the coating material can be found in the Photographic Appendix.
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Stormer Viscosity
Stormer viscosity was determined in accordance with ASTM D562-10, "Standard Test
Method for Consistency of Paints Measuring Krebs Unit (KU) Viscosity Using a Stormer-Type
Viscometer." Readings were taken once the samples were brought to 25 ± 0.2°C, and recorded in
Krebs units (KU). Baseline viscosity readings were obtained on liquid material that was not
exposed to any of the conditions listed above. The results can be found in Table 2, "Results of
Stormer Viscosity Evaluation."
Table 2 - Results of Stormer Viscosity Evaluation
Sample ID
Initial
After Freeze/Thaw (Cycle 1)
CC VIS-Strip
102.9 KU
Solid
CC Fix
67.2 KU
Solid
Brookfield Viscosity
The Brookfield viscosity was determined in accordance with ASTM D2196-10,
"Standard Test Method for Rheological Properties of Non-Newtonian Materials by Rotational
(Brookfield type) Viscometer." The temperature of the sample was raised to 25 ± 0.2°C.
Previous testing was conducted using spindle 4 and 20 RPM speed, so the testing started with
that selection. The second set of tests was performed using spindle 5 and a speed of 20 RPM, for
confirmation. The selection was not appropriate for the CC FIX product and different
combinations were used and are listed in the table. For this testing, the spindle was lowered into
the sample until the immersion mark on the spindle shaft touched the sample. The viscometer
was turned on and the pointer was allowed to make several rotations until it had stabilized. Once
the pointer stabilized, the viscometer was stopped by simultaneously pressing down on the power
and hold switches. The viscosity reading was multiplied by the spindle/speed factor, and
recorded in centipoise (cps) units. The same procedure was used for the second set of
conditions. The average value is reported. The results can be found in Table 3, "Results of
Brookfield Viscosity Evaluation."
Table 3 - Results of Brookfield Viscosity Evaluation
Sample ID
Spindle 4
Speed - 20 rpm
Spindle 5
Speed - 20 rpm
Initial
Post
Initial
Post
CC VIS-Strip
16,950 cps
No reading
10,300 cps
No reading
Sample ID
Spindle 4
Speed -100 rpm
Spindle 5
Speed -100 rpm
Initial
Post
Initial
Post
CC Fix
865 cps
820 cps
425 cps
380 cps
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Density
Density was determined in accordance with ASTM D 1475-98(08), "Standard Test
Method for Density of Liquid Coatings, Inks, and Related Products." A calibrated cup was
weighed empty and then weighed full of liquid coating. The air bubbles were eliminated from
the coatings as much as feasible by gently tapping the cup. The liquid materials were tested prior
to any exposure and then after the storage stability described in Cycle 3. Calculations were
performed, and the results of the testing are listed in Table 4, "Density Results."
Table 4 - Density Results
Sample ID
Initial
After Storage Stability
(Cycle 3)
CC VIS-Strip
8.978 lb/gal
8.988 lb/gal
CC Fix
8.668 lb/gal
8.668 lb/gal
Degree of Settling
The degree of settling was evaluated in accordance with ASTM D869-85(ll), "Standard
Test Method for Evaluating Degree of Settling of Paint." This method requires that the coating
material not be shaken or stirred after exposure, prior to the settling evaluation. The blunt tipped
spatula was dropped into the CC Fix and coating, the spatula hit the base of the can with a
metallic sound, indicating that no settling had occurred in the 14 days of cyclic exposure
represented in Cycle 2 - Storage Exposure, indicating a rating of 10 for the CC Fix product.
Since the CC VIS-Strip product was semi-solid, no ASTM D869 rating could be applied.
Humidity Resistance
The coating system was applied over both concrete and steel panels and permitted to dry
for a minimum of 7 days prior to testing. The resulting panels were tested for humidity
resistance in accordance with ASTM D 2247-11, "Standard Practice for Testing Water
Resistance of Coatings in 100% Relative Humidity." The coated panels were placed on the
exterior of an enclosed chamber containing a heated, saturated mixture of air and water vapor.
At an internal condition of 100°F and 100% relative humidity, the temperature difference
between the specimen surface and the surrounding vapor causes the formation of condensation
on the interior (painted surface) of the panels. The samples were subjected to 200 hours of
humidity exposure. Visually, these samples appeared to be failing. There was discoloration
noted of both coating materials and large areas of lifted coating were apparent (see photographs).
After the exposure time had elapsed, the coated panels were evaluated for loss of tensile
adhesion. The results are listed in the section titled Tensile Adhesion Strength. Photographs of
the panels can be found in the Photographic Appendix.
Tensile Adhesion Strength
Tensile adhesion (pull-off strength) was measured in accordance with ASTM D4541-
09el, "Pull-Off Strength of Coatings Using Portable Adhesion Testers," Annex A4, "Self-
Aligning Adhesion Tester Type IV" or ASTM D7234-12, "Standard Test Method for Pull-Off
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Adhesion Strength of Coatings on Concrete Using Portable Pull-Off Adhesion Testers." Both of
the methods use the same equipment to remove the pull stubs. The main difference between the
test methods is the size of the pull stubs. The ASTM D7234-12 for concrete specifies 2" pull
stubs. The coating on the steel panels was evaluated using Vi" pull stubs.
For both methods, the testing surfaces were wiped clean and abraded gently using fine
sandpaper. Pull stubs with an abraded test surface were attached to the coating using a two
component epoxy adhesive (Araldite 2011), which was allowed to cure for a minimum of
twenty-four hours at ambient laboratory conditions (72 ± 5°F and 50 ± 5% relative humidity).
The 2" pull stubs on the concrete samples were then detached using a self-aligning pneumatic
adhesion tester (PATTI-Pneumatic Adhesion Tensile Testing Instrument) employing the F8
piston (range: 25-255 psi) or the F20 piston (range 63-637 psi). The Vi" pull stubs were detached
using the F4 piston, which has a range of 202-2039 psi for the small diameter pull stub. The
pressure required to remove each pull stub was recorded along with the location of break and
approximate percentage of each. The location of break is defined as adhesive (a split between
layers), cohesive (within a layer), or glue failure (coating strength exceeds glue strength). The
results of the testing can be found in Table 5, "Results of Tensile Adhesion Testing."
Photographs of the panels can be found in the Photographic Appendix.
Table 5 - Results of Tensile Adhesion Testing
Coating
System
Pull
Stub
ID
Pull-Off
Strength
(psi)
Location of Break
Average
Pull-Off
Strength (psi)
CC VIS-
Strip with
CC Fix to
Concrete
(Initial)
1
324
100% adhesive at the concrete interface
323
2
191
100% adhesive at the concrete interface
3
401
100% adhesive at the concrete interface
4
375
100% adhesive at the concrete interface
CC VIS-
Strip with
CC Fix to
Concrete
(After 200 hours
humidity)
1
71
100% adhesive to concrete
58
(average of
2 values)
2
46
100% adhesive to concrete
3
*
100% adhesive to concrete
4
*
100% adhesive to concrete
CC VIS-
Strip with
CC Fix to
Steel
(Initial)
A
1141
100% adhesive at the steel interface
1124
B
1161
100% adhesive at the steel interface
C
1141
100% adhesive at the steel interface
D
1182
100% adhesive at the steel interface
E
1059
100% adhesive at the steel interface
F
1059
100% adhesive at the steel interface
ARCADIS U.S., Inc.
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Coating
System
Pull
Stub
ID
Pull-Off
Strength
(psi)
Location of Break
Average
Pull-Off
Strength (psi)
CC VIS-
Strip with
CC Fix to
Steel
(After 200 hours
humidity)
A
284.2
100% adhesive at the steel interface, rusted
223
(average of
4 values)
B
*
100% adhesive at the steel interface, rusted
C
*
100% adhesive at the steel interface, rusted
D
202.6
100% adhesive at the steel interface, rusted
E
202.6
100% adhesive at the steel interface, rusted
F
202.6
100% adhesive at the steel interface, rusted
* Pull stub removed as test started.
Taber Abrasion Resistance
Taber abrasion resistance of the CC Fix material was determined in accordance with
ASTM D4060-10, "Test Method for Abrasion Resistance of Organic Coatings by the Taber
Abraser." Duplicate 4" x 4" panels were weighed then subjected to 1000 cycles using a lOOOg
load and CS-17 abrasion wheels. Post weights were acquired for the samples, and the weight
loss (in mg) reported. The results of the testing are contained in Table 6, "Taber Abrasion
Resistance Results."
Table 6 - Taber Abrasion Resistance Results
Coating
System
Replicate
ID
Initial
Weight
Final
Weight
Weight Loss
(mg)
Average Weight Loss
(mg)
CC Fix
A
65.0575
64.9883
69.2
71.0
B
65.4911
65.4199
71.2
C
65.3762
65.3066
69.6
D
64.8932
64.8194
73.8
Tensile Strength
Tensile strength was determined in accordance with ASTM D2370-98(10), "Standard
Test Method for Tensile Properties of Organic Coatings." The samples were cut to a width of Vi"
using a double blade cutter. The resulting samples were maintained at ambient laboratory
conditions (72 ± 5° F and 50 ± 5% RH) for a minimum of 40 hours before testing. The samples
were tested for tensile strength using a Tinius Olsen Universal Testing Machine. The cross-head
speed used for testing was 2.0 in/min. A gage length of 1" was selected due to the expected
strength and elongation of the material and previous testing performed using this protocol. The
force (in pounds) required to break the sample and the sample dimensions were used to calculate
the tensile strength of each free-film of coating in pounds per square inch (psi). The ultimate
length at break was used to calculate the elongation. The method requires testing of 10
specimens. The five specimens with the highest combination of properties were selected for
reporting as outlined in the ASTM method. The results of the testing can be found in Table 7,
"Results of Tensile Strength Testing."
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Table 7 - Results of Tensile Strength Testing
Sample
ID
Replicate
ID
Force
(lbs)
Tensile
Strength
(psi)
Average
Tensile
Strength
(psi)
Percent
Elongation
(%)
Average Percent
Elongation (%)
CC
1
3.00
211
1144
VIS-
2
3.34
246
1358
Strip
3
2.71
206
242
1704
1286
with CC
5
2.99
251
1022
Fix
8
3.62
296
1201
If you have any questions or comments regarding this report, please contact me by
telephone at 412-788-1300, extension 183, or by email at vsherbondy@kta.com.
Sincerely,
KTA-TATOR, INC.
Valerie D. Sherbondy
Senior Chemist
Appendix: Photographs
VDS/RNR:kdw
JN320715-A3-R1
CIN: 205716
cc: Ms. Kim Egler of ARCADIS
R1 - A revision was issued to include edits and to add a photographic appendix.
(320715-A3-R1 Arcadis.doc)
NOTICE: This report represents the opinion of KTA-TATOR, INC. This report is issued in conformance with generally
accepted industry practices. While customary precautions were taken to verify the information gathered and presented is
accurate, complete and technically correct, this report is based on the information, data, time, materials, and/or samples afforded.
This report should not be reproduced except in full.
ARCADIS U.S., Inc.
Testing of Strippable Coating
7 of 7
June 6, 2013
JN320715-A3-R1
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APPENDIX
-------
PHOTOGRAPHIC APPENDIX
VIS STRIP Cycle 1 (close) - Freeze/Thaw Stability
CC FIX Panels Humidity on Bottom
ARCADIS U.S., Inc.
Photographic Appendix
1 of 3
June 6, 2013
JN320715-A3-R1
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CC FIX System on Steel (Humidity Top) - Humidity
CC FIX over VIS Strip over Concrete - Adhesion (Humidity Panels on Bottom)
ARCADIS U.S., Inc.
Photographic Appendix
2 of 3
June 6, 2013
JN320715-A3-R1
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CC FIX with VIS Strip Over Steel - Adhesion
ARCADIS U.S., Inc.
Photographic Appendix
3 of 3
June 6, 2013
JN320715-A3-R1
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Appendix E - KTA Test Report - Instacote CC Strip/SBR-10
-------
July 2, 2013
Via Email: brent.hall@arcadis-us.com
Mr. Brent Hall
ARCADIS U.S., Inc.
4915 Prospectus Drive, Suite F
Durham, NC 27713-4408
SUBJECT: Laboratory Testing of Strippable Coating - InstaCote SBR-10F;
KTA-Tator. Inc. Project No. 320715-A2-R2
Dear Mr. Hall:
In accordance with KTA Proposal PN131249 and ARCADIS U.S. Inc. (ARCADIS)
Work Authorization No. D12-0178, KTA-Tator, Inc. (KTA) has tested a coating material to
several different requirements to determine the resulting physical properties. This report
describes the laboratory techniques used and contains the results of the testing.
SAMPLES
The samples listed in Table 1, "Samples" were received from InstaCote on the dates
listed. It should be noted that at no time did KTA personnel witness the acquisition or
manufacturing of the samples.
Table 1 - Samples
Sample
ID
Sample Description
Date Received
KTA-6
One 5-gallon pail of InstaCote CC Hi VIS-Strip #1 VIS-
Strip, Batch #012413-4-2
January 30, 2013
KTA-8
One gallon InstaCote SBR 10F with solvent, Part A, no
batch number
March 6, 2013
One gallon InstaCote SBR 10F with solvent, Part B
Aspartic Ester, Resin, "Clear," no batch number
LABORATORY INVESTIGATION
The laboratory investigation consisted of exposure of the liquid materials to different
thermal cyclic conditions to simulate storage and freeze/thaw possibilities followed by
evaluations of viscosity, density and settling. The applied coating system was tested to
KTA-Tator, Inc.
115 Technology Drive
Pittsburgh, PA 15275
412.788.1300
www.kta.com
-------
determine the resistance to humidity and the tensile strength (Table 5), while the topcoat was
tested to determine the abrasion resistance (Table 6). A free-film sample of the coating system
was also tested to determine the tensile strength (Table 7).
Thermal Cycling
Three different conditions of thermal cycling or exposure were evaluated for this testing
protocol. Each condition is described in a paragraph below. The coatings were evaluated by
different methods at the conclusion of the exposure. The results are addressed in the sections
explaining the test methods employed for the evaluations. Each of the cyclic tests was assigned
a number and a short designation for each is referenced in the corresponding results tables.
Cycle 1 - Freeze/Thaw Stability
Freeze/thaw thermal cycling was performed in accordance with ASTM D2337-01(2010),
"Standard Test Method for Freeze-Thaw Stability of Multicolor Lacquers." This test method
was performed to determine the resistance of the liquid coating material to cycles of freezing and
thawing. The duration of the test was 30 cycles. The cycles occurred on weekdays. The can
remained in the freezer during the weekends. The thermal cycling conditions for this test
consisted of sixteen hours at 25 ± 3°F and eight hours at room temperature (72 ± 5°F). The
liquid material was evaluated by Stormer viscosity after exposure. A visual examination of the
coating revealed that the SBR-10F coating was similar in appearance to the unexposed samples.
The InstaCote CC VIS-Strip was solid after exposure and a Stormer viscosity reading could not
be obtained. A photograph of the coating material can be found in the Photographic Appendix.
Cycle 2 - Storage Exposure
Storage exposure was performed in accordance with ASTM D1309-93(2010), "Standard
Test Method for Settling Properties of Traffic Paints During Storage." This test method was
performed to determine the resistance of the liquid coating material to cycles of freezing and
heating. The duration of the test was 14 cycles, which occurred on weekdays. The can remained
in the at room temperature for the evenings and on the weekends. The thermal cycling
conditions for this test consisted of two hours at 5 - 10°F, followed by two hours at
approximately 160°F. These cycles were repeated twice, then followed by 16 hours at room
temperature (72 ± 5°F). The 8 hour cycle was completed during work hours. The liquids were
scheduled to be evaluated for settling after exposure. The VIS-Strip product was semi-solid after
this exposure and a settling evaluation could not be performed. Components A and B of the
InstaCote SBR 10F were liquid and the settling evaluation was performed.
Cycle 3 - Storage Stability
Storage stability was performed in accordance with military specification MIL-PRF-
32239, "Standard Method for Accelerated Storage Stability." This test method was performed to
determine the resistance of the water based liquid coating material to extended heat exposure.
The can remained in the oven set at 140°F for the 7 day duration of the test. At the completion
of the exposure, the liquid materials were scheduled for evaluation of viscosity using a
Brookfield viscometer. Additionally, the density of the material was to be evaluated after
ARCADIS U.S., Inc.
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exposure. A visual examination revealed that the majority of the VIS-Strip had partially
solidified during this exposure and that the individual components of the SBR 10 appeared
unaffected. There was enough liquid VIS-Strip material to perform the density testing, but not
enough volume for viscosity testing.
Stormer Viscosity
Stormer viscosity was determined in accordance with ASTM D562-10, "Standard Test
Method for Consistency of Paints Measuring Krebs Unit (KU) Viscosity Using a Stormer-Type
Viscometer." Readings were taken once the samples were brought to 25 ± 0.2°C, and recorded in
Krebs units (KU). Baseline viscosity readings were obtained on liquid material that was not
exposed to any of the conditions listed above. Initial readings were reported for the mixed
material. Fifteen minutes after mixing, the viscosity was approximately 65.5 KU both before
and after exposure. The results can be found in Table 2, "Results of Stormer Viscosity
Evaluation."
Table 2 - Results of Stormer Viscosity Evaluation
Sample ID
Initial
After Freeze/Thaw (Cycle 1)
VIS-Strip
102.9 KU
Solid
SBR-10 Part A
49.6 KU
50.9 KU
SBR-10 Part B
90.7 KU
87.5 KU
SBR-10 Mixed
55.6 KU
55.0 KU
Brookfield Viscosity
The Brookfield viscosity was determined in accordance with ASTM D2196-10,
"Standard Test Method for Rheological Properties of Non-Newtonian Materials by Rotational
(Brookfield type) Viscometer." The temperature of the sample was raised to 25 ± 0.2°C. Since
previous testing for a similar protocol had been performed using spindle 4 and 20 RPM speed,
this combination was utilized for the evaluation. These products did not produce acceptable
results with that combination and the various combinations used for evaluation are listed below.
For this testing, the spindle was lowered into the sample until the immersion mark on the spindle
shaft touched the sample. The viscometer was turned on and the pointer was allowed to make
several rotations until it had stabilized. Once the pointer stabilized, the viscometer was stopped
by simultaneously pressing down on the power and hold switches. The viscosity reading was
multiplied by the spindle/speed factor, and recorded in centipoise (cps) units. The same
procedure was used for the second set of conditions. The average value is reported. The results
can be found in Table 3, "Results of Brookfield Viscosity Evaluation."
Table 3 - Results of Brookfield Viscosity Evaluation
Sample ID
Spindle 4
Speed - 20 rpm
Spindle 5
Speed - 20 rpm
Initial
Post Cycle 3
Initial
Post Cycle 3
VIS-Strip (Initial)
16950 cps
no reading
5000 cps
no reading
ARCADIS U.S., Inc.
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Sample ID
Spindle 2
Speed - 50 rpm
Spindle 2
Speed -100 rpm
Initial
Post Cycle 3
Initial
Post Cycle 3
SBR-10 Part A - After
Storage Stability (Cycle 3)
60 cps
48 cps
60 cps
62 cps
Sample ID
Spindle 3
Speed - 50 rpm
Spindle 4
Speed - 50 rpm
Initial
Post Cycle 3
Initial
Post Cycle 3
SBR-10 Part B - After
Storage Stability (Cycle 3)
1190 cps
1085 cps
1180 cps
1040 cps
Sample ID
Spindle 3
Speed -100 rpm
Spindle 4
Speed -100 rpm
Initial
Post Cycle 3
Initial
Post Cycle 3
SBR-10 Mixed - After
Storage Stability (Cycle 3)
710 cps
230 cps
760 cps
200 cps
Density
Density was determined in accordance with ASTM D 1475-98(08), "Standard Test
Method for Density of Liquid Coatings, Inks, and Related Products." A calibrated cup was
weighed empty and then weighed full of liquid coating. The air bubbles were eliminated from
the coatings as much as feasible by gently tapping the cup. The liquid material was tested prior
to any exposure and then after the storage stability described in Cycle 3. Calculations were
performed, and the results of the testing are listed in Table 4, "Density Results."
Table 4 - Density Results
Sample ID
Initial
After Storage Stability
(Cycle 3)
SBR-10 Part A
8.718 lb/gal
8.715 lb/gal
SBR-10 PartB
8.874 lb/gal
8.880 lb/gal
SBR-10 Mixed
8.836 lb/gal
8.806 lb/gal
VIS-Strip
8.978 lb/gal
8.988 lb/gal
Degree of Settling
The degree of settling was evaluated in accordance with ASTM D869-85(ll), "Standard
Test Method for Evaluating Degree of Settling of Paint." This method requires that the coating
material not be shaken or stirred after exposure, prior to the settling evaluation. In this case, the
CC VIS-Strip coating had solidified and no testing could be performed. Testing of the InstaCote
SBR 10F Components A and B was performed. The spatula hit the base of the can with a
metallic sound, indicating that no settling had occurred in the 14 days of cyclic exposure
represented in Cycle 2 - Storage Exposure. The SBR-1 OF Components A and B would each
receive a settling value of 10.
ARCADIS U.S., Inc.
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Humidity Resistance
The coating was applied over both concrete and steel panels and permitted to dry for a
minimum of 7 days prior to testing. The resulting panels were tested for humidity resistance in
accordance with ASTM D2247-11, "Standard Practice for Testing Water Resistance of Coatings
in 100% Relative Humidity." The coated panels were placed on the exterior of an enclosed
chamber containing a heated, saturated mixture of air and water vapor. At an internal condition
of 100°F and 100% relative humidity, the temperature difference between the specimen surface
and the surrounding vapor causes the formation of condensation on the interior (painted surface)
of the panels. The samples were subjected to 200 hours of humidity exposure. The coating on
the concrete panels had lightened and become more opaque in appearance. Visually, the coating
on the steel samples appeared similar to when the samples were placed in exposure. After the
exposure time had elapsed, the coated panels were evaluated for loss of tensile adhesion. The
results are listed in the section titled Tensile Adhesion Strength. Photographs of the panels can
be found in the Photographic Appendix.
Tensile Adhesion Strength
Tensile adhesion (pull-off strength) was measured in accordance with ASTM D4541-
09el, "Pull-Off Strength of Coatings Using Portable Adhesion Testers," Annex A4, "Self-
Aligning Adhesion Tester Type IV" or ASTM D7234-12, "Standard Test Method for Pull-Off
Adhesion Strength of Coatings on Concrete Using Portable Pull-Off Adhesion Testers." Both of
the methods use the same equipment to remove the pull stubs. The main difference between the
test methods is the size of the pull stubs. The ASTM D7234-12 for concrete specifies 2" pull
stubs. The coating on the steel panels was evaluated using Vi" pull stubs.
For both methods, the testing surfaces were wiped clean and abraded gently using fine
sandpaper. Pull stubs with an abraded test surface were attached to the coating using a two
component epoxy adhesive (Araldite 2011), which was allowed to cure for a minimum of
twenty-four hours at ambient laboratory conditions (72 ± 5°F and 50 ± 5% relative humidity).
The 2" pull stubs on the concrete specimens were then detached using a self-aligning pneumatic
adhesion tester (PATTI-Pneumatic Adhesion Tensile Testing Instrument) employing the F8
piston (range: 25 - 255 psi). The Vi" pull stubs were detached using the F4 piston, which has a
range of 202 - 2039 psi for the small diameter pull stub. The pressure required to remove each
pull stub was recorded along with the location of break and approximate percentage of each.
The location of break is defined as adhesive (a split between layers), cohesive (within a layer), or
glue failure (coating strength exceeds glue strength). The results of the testing can be found in
Table 5, "Results of Tensile Adhesion Testing." Photographs of the panels can be found in the
Photographic Appendix.
ARCADIS U.S., Inc.
Testing of Strippable Coating
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Table 5 - Results of Tensile Adhesion Testing
Coating
System
Pull
Stub
ID
Pull-Off
Strength
(psi)
Location of Break
Average
Pull-Off
Strength (psi)
SBR-10/
VIS-Strip
to Concrete
(Initial)
1
203
100% adhesive between coats
223
2
242
70% adhesive primer/topcoat;
30% adhesive to concrete
3
216
90% adhesive primer/topcoat;
10% adhesive to concrete
4
229
100% adhesive between coats
SBR-10/
VIS-Strip
to Concrete
(After 200 hours
humidity)
1
168
80% adhesive to concrete,
20% cohesive in coating
146
2
117
85% adhesive to concrete,
15% cohesive in coating
3
163
90% adhesive to concrete,
10% cohesive in coating
4
137
60% adhesive to concrete,
40% cohesive in coating
SBR-10 to
Steel
(Initial)
A
610.7
100% adhesive at the steel interface
584
B
610.7
100% adhesive at the steel interface
C
610.7
100% adhesive at the steel interface
D
610.7
100% adhesive at the steel interface
E
569.9
100% adhesive at the steel interface
F
488.3
100% adhesive at the steel interface
SBR-10 to
Steel
(After 200 hours
humidity)
A
*
100% adhesive at the steel interface, rusted
513
(average of
5 values)
B
508.7
100% adhesive at the steel interface, rusted
C
569.9
100% adhesive at the steel interface, rusted
D
549.5
100% adhesive at the steel interface, rusted
E
529.1
100% adhesive at the steel interface, rusted
F
406.7
100% adhesive at the steel interface, rusted
* Pull stub removed as test started.
Taber Abrasion Resistance
Taber abrasion resistance of the SBR-10F was determined in accordance with ASTM
D4060-10, "Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser."
Duplicate 4" x 4" panels were weighed then subjected to 1000 cycles using a lOOOg load and CS-
17 abrasion wheels. Post weights were acquired for the samples, and the weight loss (in mg)
reported. The results of the testing are contained in Table 6, "Taber Abrasion Resistance
Results."
ARCADIS U.S., Inc.
Testing of Strippable Coating
6 of 8
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Table 6 - Taber Abrasion Resistance Results
Coating
System
Replicate
ID
Initial
Weight
Final
Weight
Weight Loss
(mg)
Average Weight Loss
(mg)
SBR-10
A
66.3012
66.2403
60.9
60.2
B
65.2493
65.1860
63.3
C
66.5958
66.5353
60.5
D
66.5056
66.4495
56.1
Tensile Strength
Tensile strength was determined in accordance with ASTM D2370-98(10), "Standard
Test Method for Tensile Properties of Organic Coatings." The samples of the two coat system
were cut to a width of Vi" using a double blade cutter. The resulting samples were maintained at
ambient laboratory conditions (72 ± 5° F and 50 ± 5% RH) for a minimum of 40 hours before
testing. The samples were tested for tensile strength using a Tinius Olsen Universal Testing
Machine. The cross-head speed used for testing was 2.0 in/min. A gage length of 1" was
selected due to the strength and elongation of the material and the previous testing performed for
this testing protocol. The force (in pounds) required to break the sample and the sample
dimensions were used to calculate the tensile strength of each free-film of coating in pounds per
square inch (psi). The ultimate length at break was used to calculate the elongation. The method
requires testing of 10 specimens. The five specimens with the highest combination of properties
were selected for reporting as outlined in the ASTM method. The results of the testing can be
found in Table 7, "Results of Tensile Strength Testing."
Table 7 - Results of Tensile Strength Testing
Sample
ID
Replicate
ID
Force
(lbs)
Tensile
Strength
(psi)
Average
Tensile
Strength
(psi)
Percent
Elongation
(%)
Average Percent
Elongation (%)
1
12.56
581
1144
VIS-Strip
with
SBR-10
2
13.01
602
1065
3
11.55
531
592
1065
1135
5
13.05
585
1200
8
14.32
663
1124
ARCADIS U.S., Inc.
Testing of Strippable Coating
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JN320715-A2-R2
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If you have any questions or comments regarding this report, please contact me by
telephone at 412-788-1300, extension 183, or by email at vsherbondy@kta.com.
Appendix: Photographs
VDS/RNR:kdw/j sc
JN320715-A2-R2
CIN: 205716
cc: Ms. Kim Egler of ARCADIS
R2 - A revision was issued to edit the photographic appendix.
(320715-A2-R2 Arcadis.doc)
NOTICE: This report represents the opinion of KTA-TATOR, INC. This report is issued in conformance with generally
accepted industry practices. While customary precautions were taken to verify the information gathered and presented is
accurate, complete and technically correct, this report is based on the information, data, time, materials, and/or samples afforded.
This report should not be reproduced except in full.
ARCADIS U.S., Inc. 8 of 8 July 2, 2013
Testing of Strippable Coating JN320715-A2-R2
Sincerely,
KTA-TATOR, INC.
yffjiAui
Valerie D. Sherbondy U
Valerie D. Sherbondy
Senior Chemist
-------
APPENDIX
-------
PHOTOGRAPHIC APPENDIX
VIS STRIP Cycle 1 - Freeze/Thaw Stability
ARCADIS U.S., Inc.
Photographic Appendix
1 of 4
July 2, 2013
JN320715-A2-R2
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SBR-10F Panels Humidity vs Ambient - Humidity Exposure
SBR-10F Panels Humidity vs Ambient - Humidity Exposure (close view)
ARCADIS U.S., Inc.
Photographic Appendix
2 of 4
July 2, 2013
JN320715-A2-R2
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SBR-10F Steel - Humidity vs Ambient - Humidity Exposure
SBR-10F on Steel - Humidity vs Ambient - Humidity Exposure (Close View)
ARCADIS U.S., Inc.
Photographic Appendix
3 of 4
July 2, 2013
JN320715-A2-R2
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SB R-l OWVIS Strip Over Concrete - Adhesion
SBR-10WVIS Strip Over Steel - Adhesion
ARCADIS U.S., Inc.
Photographic Appendix
4 of 4
July 2, 2013
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Appendix F - KTA Test Report - Intergard 10220 Test Report
-------
June 17, 2013
Via Email: brent.hall@arcadis-us.com
Mr. Brent Hall
ARCADIS U.S., Inc.
4915 Prospectus Drive, Suite F
Durham, NC 27713-4408
SUBJECT: Laboratory Testing of Strippable Coating - International Intergard 10220;
KTA-Tator. Inc. Project No. 320715-A1-R2
Dear Mr. Hall:
In accordance with KTA Proposal PN131249 and ARCADIS U.S. Inc. (ARCADIS)
Work Authorization No. D12-0178, KTA-Tator, Inc. (KTA) has tested a coating material to
several different requirements to determine the resulting physical properties. This report
describes the laboratory techniques used and contains the results of the testing.
SAMPLES
One five-liter can of International Intergard 10220, batch number 031004327, was
received from ARCADIS on January 25, 2013. This sample was designated by KTA as Sample
KTA-4. It should be noted that at no time did KTA personnel witness the acquisition or
manufacturing of the samples.
LABORATORY INVESTIGATION
The laboratory investigation consisted of exposure of the liquid material to different
thermal cyclic conditions to simulate storage and freeze/thaw possibilities followed by
evaluations of viscosity, density and settling. The coating was tested to determine the resistance
to humidity, tensile adhesion (Table 4) and abrasion (Table 5). A free-film was also prepared
and tested to determine the tensile strength (Table 6).
Thermal Cycling
Three different conditions of thermal cycling or exposure were evaluated for this testing
protocol. Each condition is described in a paragraph below. The coating was evaluated by
different methods at the conclusion of the exposure. The results are addressed in the sections
explaining the test methods employed for the evaluations. Each of the cyclic tests was assigned
a number and a short designation for each is referenced in the corresponding results tables.
KTA-Tator, Inc.
115 Technology Drive
Pittsburgh, PA 15275
412.788.1300
www.kta.com
-------
Cycle 1 - Freeze/Thaw Stability
Freeze/thaw thermal cycling was performed in accordance with ASTM D2337-01(2010),
"Standard Test Method for Freeze-Thaw Stability of Multicolor Lacquers." This test method
was performed to determine the resistance of the liquid coating material to cycles of freezing and
thawing. The duration of the test was 30 cycles. The cycles occurred on weekdays. The can
remained in the freezer during the weekends. The thermal cycling conditions for this test
consisted of sixteen hours at 25 ± 3°F and eight hours at room temperature (72 ± 5°F). The
liquid material was scheduled to be evaluated by Stormer viscosity after exposure. A visual
examination of the coating at the conclusion of the cycling revealed that the coating was solid
and Stormer viscosity could not be performed.
Cycle 2 - Storage Exposure
Storage exposure was performed in accordance with ASTM D1309 - 93(2010), "Standard
Test Method for Settling Properties of Traffic Paints During Storage." This test method was
performed to determine the resistance of the liquid coating material to cycles of freezing and
heating. The duration of the test was 14 cycles, which occurred on weekdays. The can remained
in the at room temperature in the evenings and on the weekends. The thermal cycling conditions
for this test consisted of two hours at 5 - 10°F, followed by two hours at 160°F. These cycles
were repeated twice, then followed by 16 hours at room temperature (72 ± 5°F). The 8 hour
cycle was completed during work hours. The liquid was scheduled to be evaluated for settling
after exposure. The immediate visual evaluation after cycling revealed that the coating material
was solid and no settling evaluation could be performed.
Cycle 3 - Storage Stability
Storage stability was evaluated in accordance with military specification MIL-PRF-
32239, "Standard Method for Accelerated Storage Stability." This test method was performed to
determine the resistance of the water based liquid coating material to extended heat exposure.
The can remained in the oven set at approximately 140°F for the 7 day duration of the test. At
the completion of the exposure, the liquid material was evaluated for changes in viscosity using a
Brookfield viscometer. Additionally, the density of the material was evaluated after the storage
stability exposure. A visual examination of the material revealed that the coating was thicker
than the original material, but still fluid.
Stormer Viscosity
Stormer viscosity was determined in accordance with ASTM D562-10, "Standard Test
Method for Consistency of Paints Measuring Krebs Unit (KU) Viscosity Using a Stormer-Type
Viscometer." Readings were taken once the samples were brought to 25 ± 0.2°C, and recorded
in Krebs units (KU). Baseline viscosity readings were obtained on liquid material that was not
exposed to any of the conditions listed above. The sample exposed to the conditions of Cycle 1
was solid and a post evaluation of viscosity could not be performed. The results can be found in
Table 1, "Results of Stormer Viscosity Evaluation."
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Table 1 - Results of Stormer Viscosity Evaluation
Sample ID
Initial
After Freeze/Thaw (Cycle 1)
International 10220
138 KU
Solid
Brookfield Viscosity
The Brookfield viscosity was determined in accordance with ASTM D2196-10,
"Standard Test Method for Rheological Properties of Non-Newtonian Materials by Rotational
(Brookfield type) Viscometer." The temperature of the sample was raised to 25 ± 0.2°C. No
spindle number or speed was specified, so spindle 4 and 20 RPM speed were initially used to
provide consistency with other materials tested under a similar protocol. This selection was not
appropriate for this material, so the initial viscosity values were obtained using spindle 5 and a
speed of 10 RPM, followed by spindle 6 at 20 RPM, for confirmation. For this testing, the
spindle was lowered into the sample until the immersion mark on the spindle shaft touched the
sample. The viscometer was turned on and the pointer was allowed to make several rotations,
until it had stabilized. Once the pointer stabilized, the viscometer was stopped by simultaneously
pressing down on the power and hold switches. The viscosity reading was multiplied by the
spindle/speed factor, and recorded in centipoise (cps) units. The same procedure was used for
the second set of conditions. The average value is reported. The results can be found in Table 2,
"Results of Brookfield Viscosity Evaluation."
Table 2 - Results of Brookfield Viscosity Evaluation
Sample ID
Spindle 5
Speed -10 rpm
Spindle 6
Speed - 20 rpm
International 10220 - Initial
30,000 cps
24,000 cps
International 10220 - After Storage Stability
(Cycle 3)
Too thick to read*
41,250 cps
* Spindle and speed adjustments did not lead to a comparable result.
Density
Density was determined in accordance with ASTM D 1475-98(08), "Standard Test
Method for Density of Liquid Coatings, Inks, and Related Products." A calibrated cup was
weighed empty and then weighed full of liquid coating. The air bubbles were eliminated from
the coatings as much as feasible by gently tapping the cup. The liquid material was tested prior
to any exposure and then after the storage stability described in Cycle 3. Calculations were
performed, and the results of the testing are listed in Table 3, "Density Results."
Table 3 - Density Results
Sample ID
Initial
After Storage Stability
(Cycle 3)
International 10220
9.082 lb/gal
8.650 lb/gal
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Degree of Settling
The degree of settling was evaluated in accordance with ASTM D869-85(ll), "Standard
Test Method for Evaluating Degree of Settling of Paint." This method requires that the coating
material not be shaken or stirred after exposure, prior to the settling evaluation. In this case, the
coating exposed to Cycle 2 conditions had solidified and no ASTM D869 rating could be
applied.
Humidity Resistance
The coating was applied over both concrete and steel panels and permitted to dry for a
minimum of 7 days prior to testing. The resulting panels were tested for humidity resistance in
accordance with ASTM D2247-11, "Standard Practice for Testing Water Resistance of Coatings
in 100% Relative Humidity." The coated panels were placed on the exterior of an enclosed
chamber containing a heated, saturated mixture of air and water vapor. At an internal condition
of 100°F and 100% relative humidity, the temperature difference between the specimen surface
and the surrounding vapor causes the formation of condensation on the interior (painted surface)
of the panels. The samples were subjected to 200 hours of humidity exposure. Visually, the
applications over steel appeared rusted, but did maintain a flat film. The applications to the
concrete panels appeared unchanged. After drying, small cracks were noted in the coating.
After the exposure time had elapsed, the coated panels were evaluated for loss of tensile
adhesion. The results are listed in the section titled Tensile Adhesion Strength. Photographs of
the panels can be found in the Photographic Appendix.
Tensile Adhesion Strength
Tensile adhesion (pull-off strength) was measured in accordance with ASTM D4541-
09el, "Pull-Off Strength of Coatings Using Portable Adhesion Testers," Annex A4, "Self-
Aligning Adhesion Tester Type IV" or ASTM D7234-12, "Standard Test Method for Pull-Off
Adhesion Strength of Coatings on Concrete Using Portable Pull-Off Adhesion Testers." Both of
the methods use the same equipment to remove the pull stubs. The main difference between the
test methods is the size of the pull stubs. The ASTM D7234-12 for concrete specifies 2" pull
stubs. The coating on the steel panels was evaluated using Vi" pull stub.
For both methods, the testing surfaces were wiped clean and abraded gently using fine
sandpaper. Pull stubs with an abraded test surface were attached to the coating using a two
component epoxy adhesive (Araldite 2011), which was allowed to cure for a minimum of
twenty-four hours at ambient laboratory conditions (72 ± 5°F and 50 ± 5% relative humidity).
The 2" pull stubs on the concrete specimens were then detached using a self-aligning pneumatic
adhesion tester (PATTI-Pneumatic Adhesion Tensile Testing Instrument) employing the F8
piston (range: 25 - 255 psi) or the F20 piston (Range 63 - 637 psi). The Vi" pull stubs were
detached using the F4 piston, which has a range of 202 - 2039 psi for the small diameter pull
stub. The pressure required to remove each pull stub was recorded along with the location of
break and approximate percentage of each. The location of break is defined as adhesive (a split
between layers), cohesive (within a layer), or glue failure (coating strength exceeds glue
strength). The results of the testing can be found in Table 4, "Results of Tensile Adhesion
Testing." Photographs of the panels can be found in the Photographic Appendix.
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Table 4 - Results of Tensile Adhesion Testing
Coating
System
Pull
Stub
ID
Pull-Off
Strength
(psi)
Location of Break
Average
Pull-Off
Strength (psi)
International
10220
to Concrete
(Initial)
1
496
100% adhesive at the concrete interface
419
2
254
100% adhesive at the concrete interface
3
455
100% adhesive at the concrete interface
4
471
100% adhesive at the concrete interface
International
10220
to Concrete
(After 200 hours
humidity)
1
433
80% adhesive to concrete,
20% cohesive in coating
407
2
407
85% adhesive to concrete,
15% cohesive in coating
3
445
90% adhesive to concrete,
10% cohesive in coating
4
344
60% adhesive to concrete,
40% cohesive in coating
International
10220
to Steel
(Initial)
A
1670
100% adhesive at the steel interface
1813
B
1874
100% adhesive at the steel interface
C
1711
100% adhesive at the steel interface
D
1711
100% adhesive at the steel interface
E
2038
100% adhesive at the steel interface
F
1874
100% adhesive at the steel interface
International
10220
to Steel
(After 200 hours
humidity)
A
1386
100% adhesive at the steel interface, rusted
1427
B
1631
100% adhesive at the steel interface, rusted
C
1631
100% adhesive at the steel interface, rusted
D
1018
100% adhesive at the steel interface, rusted
E
1345
100% adhesive at the steel interface, rusted
F
1549
100% adhesive at the steel interface, rusted
Taber Abrasion Resistance
Taber abrasion resistance was determined in accordance with ASTM D4060-10, "Test
Method for Abrasion Resistance of Organic Coatings by the Taber Abraser." Duplicate 4" x 4"
panels were weighed then subjected to 1000 cycles using a lOOOg load and CS-17 abrasion
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wheels. Post weights were acquired for the samples, and the weight loss (in mg) reported. The
results of the testing are contained in Table 5, "Taber Abrasion Resistance Results."
Table 5 - Taber Abrasion Resistance Results
Coating
System
Replicate
ID
Initial
Weight
Final
Weight
Weight Loss
(mg)
Average Weight Loss
(mg)
International
10220
A
65.1257
65.1182
7.5
11.4
B
64.9805
64.9667
13.8
C
65.3345
65.3189
15.6
D
65.1114
65.1027
8.7
Tensile Strength
Tensile strength was determined in accordance with ASTM D2370-98(10), "Standard
Test Method for Tensile Properties of Organic Coatings." The samples were cut to a width of Vi"
using a double blade cutter. The resulting samples were maintained at ambient laboratory
conditions (72 ± 5° F and 50 ± 5% RH) for a minimum of 40 hours before testing. The samples
were tested for tensile strength using a Tinius Olsen Universal Testing Machine. The cross-head
speed used for testing was 2.0 in/min. A gage length of 1" was selected due to the strength and
elongation of the material and to provide consistency with other test results from a similar testing
protocol. The force (in pounds) required to break the sample and the sample dimensions were
used to calculate the tensile strength of each free-film of coating in pounds per square inch (psi).
The ultimate length at break was used to calculate the elongation. The method requires testing of
10 specimens. The five specimens with the highest combination of properties were selected for
reporting, as outlined in the ASTM method. The results of the testing can be found in Table 6,
"Results of Tensile Strength Testing."
Table 6 - Results of Tensile Strength Testing
Sample ID
Replicate
ID
Force
(lbs)
Tensile
Strength
(psi)
Average
Tensile
Strength
(psi)
Percent
Elongation
(%)
Average
Percent
Elongation (%)
1
11.82
1876
764
International
10220
2
13.13
1945
696
3
12.26
1946
1920
658
682
5
12.37
1918
668
8
12.26
1916
628
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If you have any questions or comments regarding this report, please contact me by
telephone at 412-788-1300, extension 183, or by email at vsherbondy@kta.com.
Appendix: Photographs
VDS/RNR:kdw
JN320715-A1-R1
CIN: 205716
cc: Ms. Kim Egler of ARCADIS
R1 - A revision was issued to correct the table reference in the Laboratory Investigation
paragraph.
(320715-A1-R1 Arcadis.doc)
NOTICE: This report represents the opinion of KTA-TATOR, INC. This report is issued in conformance with generally
accepted industry practices. While customary precautions were taken to verify the information gathered and presented is
accurate, complete and technically correct, this report is based on the information, data, time, materials, and/or samples afforded.
This report should not be reproduced except in full.
ARCADIS U.S., Inc. 7 of 7 June 17, 2013
T esting of Strippable Coating JN320715- A1-R2
Sincerely,
KTA-TATOR, INC.
Akkitt t) JJiuM&idif
Vnlerie I). Sherbondy (J
Vrilerie I). Sherbondy
Senior Chemist
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APPENDIX
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PHOTOGRAPHIC APPENDIX
International 10220 Humidity vs Not - Humidity Exposure
International 10220 Surface - Humidity Exposure
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Photographic Appendix JN320715- A1-R2
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International Cracks from Humidity - Humidity Exposure
International 10220 Steel Humidity vs Not - Humidity Exposure
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Photographic Appendix JN320715- A1-R2
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International 10220 Over Concrete - Adhesion
International 10220 Over Concrete - Adhesion
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Appendix G - Data Quality Indicators
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Appendix G - Data Quality Indicators
1.1 Data Quality Indicators
DQIs forthe critical measurements were used to determine if the collected data met the QA objectives. The
mean value of at least four replicate tests was used to assess pass/fail for that portion of the test. A list of
the DQIs was given in Table 7-3. The DQIs established in the QAPP were selected without specific
knowledge of the coatings and their characteristics. One objective of the validation of the test methods was
to verify that these were realistic goals forthe coatings being tested.
The equipment used to make the critical measurements was calibrated as per the requirements of the
respective ASTM methods.
1.2 Assessment of DQI goals
The representativeness of the experiments was ensured by the careful selection of the concrete and steel
coupons and experimental conditions. The parameters that were used to assess whether the data met the
quality assurance objectives (as detailed in Table 7-3) include precision, accuracy, and completeness of the
collected data.
Precision describes the closeness of data obtained using the same procedure over multiple experiments.
There are three functions which are used to describe precision: standard deviation, variance, and coefficient
of variance. The precision of a data set can be defined using the following equation:
where
N = the number of replicates in the data set,
Xj = the measured value in the data set, and
|j = the data set mean.
When applied to a smaller data set, a sample standard deviation is calculated which changes equation G-1
to the following:
(G-1)
(G-2)
where
s = the sample standard deviation, and
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X
= the mean of the smaller data set.
Accuracy describes the closeness of the data to the true value. There are two functions frequently used to
describe accuracy: absolute and relative error. Absolute error is the measured value minus the actual value,
while the percent relative error is the same difference divided by the actual value and multiplied by 100.
The percent completeness of the data is simply the ratio of the number of valid data points taken to the total
number of data points planned, multiplied by 100.
1.3 Shelf life DQI goals
All of the DQI goals related to shelf life, with the exception of settling properties, were based on viscosity
and density DQI goals. These were the only measurements that had actual standards or instrument
calibrations that could be used for the DQI assessment.
1.3.1 Density
Accuracy describes the closeness of the individual data point to the true value of the characteristic.
Accuracy of the density measurement on the coatings was verified by determining the density of the ALARA
1146 coating using the specific gravity of the coating supplied by the manufacturer as the reference. As
shown below, the accuracy was 3.0%, well below the DQI goal of a maximum of 15%.
ALARA 1146 calculated density 8.92 lb/gal (sp. gravity 1.07 * 8.34 lb/gal)
KTA-Tator measured density 8.65 lb/gal
Accuracy = 3.0%
The density cup used by the laboratory is verified every six months.
Precision of the density measurement is demonstrated by performing replicate measurements. The DQI
goal for precision was 20%.. There were four density measurements performed for each of the four
coatings. These measurements resulted in the following values for precision expressed as relative standard
deviation (RSD), all of which were well within the precision goal of ±20%
ALARA 1146 0.01% RSD
Instacote SBR-10 0.29% RSD
Instacote CC Fix 0.01% RSD
Instacote CC Strip 0.01% RSD
Intergard 10220 0.02% RSD
Density measurements were 100% complete.
1.3.2 Viscosity
The Brookfield viscometer was calibrated January 26, 2011, and is accurate to within 1 % of its full scale
range when operated according to calibration conditions as specified in the Brookfield viscometer instruction
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manual. The calibration is verified every six months by KTA-Tator with a reference material with a known
viscosity of 4960 cps. The most recent verification associated with these tests was performed in February
2013 and obtained values of 5200 cps and 5150 cps, both within the acceptance range of 5% set by ASTM
D 2196. Precision for this measurement is represented by the percent difference between the replicate
readings and is 1%, well within the DQI goal of 20%. Viscosity measurements were 100% complete for
coatings that were not solidified during the test processes. The laboratory also took baseline readings of
coating viscosity prior to exposure to any conditions.
The Stormer viscometer was verified on February 15, 2013, using a 73 KU (lot# 12201) and a 106 KU
standard (lot# 11301). Verification was performed in duplicate to assess precision. Measured values for the
73.3 KU standard were 74.0 KU and 74.0 KU, well within the acceptance range of 73.3 KU ± 3.7 KU.
Measured values for the 106.3 KU standard were 106.2 KU and 106.3 KU, well within the acceptance range
of 106.3 KU ± 5.3 KU. All values were well within the DQI goals of 15% accuracy and 20% precision for a
completeness of 100%.
1.3.3 Settling properties
No standards are available for determining the accuracy of this method. Precision can be demonstrated by
doing replicate measurements but no DQI goals for precision were established. Settling properties were
determined for all coatings that were not solid or semi-solid after cycles were completed so the
completeness of this measurement was 100%.
1.4 Weatherability DQI goals
There are no standards that can be used to evaluate accuracy of these types of measurements. Evaluation
of precision was limited to three characteristics related to weatherability where replicates are part of the
method. These three characteristics are adhesion strength, abrasion resistance, and tensile strength. The
DQI precision goal for each of these measurement parameters was 20%. Inability to meet this goal does not
necessarily challenge the validity of the DQI goal, but rather sheds light on the potential shortcomings of the
particular coating. This is information that would be taken into account by the end user when evaluating
whether or not this coating is suitable for their intended use.
1.4.1 Water resistance
Panels were subjected to 200 hours of humidity exposure and tested in accordance with ASTM D2247-11.
DQI goals in terms of accuracy and precision for water resistance were not established. This measurement
was performed for all coatings and was 100% complete.
1.4.2 Tensile strength
Tensile strength was determined in accordance with ASTM D 2370-98 using a Tinius Olsen Universal
Testing Machine. The method requires the testing often specimens and the five specimens with the highest
combination of properties were selected for reporting. The accuracy DQI goal could not be assessed
because there is no known standard. Precision between the five replicates has been assessed and
compared to the established goal of 20%. This goal was met for tensile strength for all coatings and was
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therefore, 100% complete. The precision DQI goal was only slightly exceeded (20.5%) for Percent
Elongation on the CC/Strip/CC Fix coating on concrete as can be seen in the assessment below.
• ALARA 1146 coating on concrete - the precision between five replicates for Tensile Strength testing and
Percent Elongation was 4.6% RSD and 5.3% RSD, respectively.
• Intergard on concrete - the precision between five replicates for Tensile Strength testing and Percent
Elongation was 1.5% RSD and 7.5% RSD respectively.
• CC Strip/CC Fix on concrete - the precision for five replicates for Tensile Strength was 15% RSD and
20.5% RSD for Percent Elongation.
• CC Strip/SBR 10 on concrete - the precision for five replicates for Tensile Strength was 8% RSD and
5.1% RSD for Percent Elongation.
1.4.3 Taber abrasion resistance
Taber abrasion resistance was determined in accordance with ASTM D4060-10. No known standards are
available for assessing the accuracy of this method. Precision was assessed through replicate
measurements and was met for three of the four coatings for a 75% completeness. This value does not
meet the completeness goal of 90% established in the QAPP.
• ALARA 1146 coating on concrete - the precision between four replicates was 1.7% RSD.
• Intergard 10220 coating on concrete - the precision between four replicates was 34.3% RSD.
• CC Strip/CC Fix coating on concrete - the precision between four replicates was 2.9% RSD.
• CC Strip/SBR 10 coating on concrete - the precision between four replicates was 5% RSD.
1.4.4 Adhesion strength
Tensile adhesion (pull-off strength) of the coating on concrete and steel was measured in accordance with
ASTM D4541-09 or ASTM D 7234-12. Both of the methods use the same equipment fortesting, the only
difference being the size of the pull stubs. Not standard is available for assessing the accuracy of this
method. Precision was assessed by performing replicate tests and is detailed below. The DQI goal of 20%
was exceeded for several of the coatings and may be an indication that the goal should be extended to
account for the variability inherent in the method.
• ALARA 1146 coating on concrete pull off test for eight replicates was 6% precision initially and for seven
replicates on the concrete after 200 hours in humidity, precision was 27.4% RSD. The pull off test for
the ALARA 1146 on stainless steel panels of six (6) replicates was 6.8% RSD. The test could not be
completed after the 200 hours humidity due to the panels being rusted.
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• Intergard 10220 on concrete for four (4) replicates had a precision of 26.6% RSD. After 200 hours in
humidity, the precision between four (4) replicates was 11.1% RSD. Intergard 10220 on stainless steel
panels, six (6) replicates had a precision of 7.8% RSD and 16.4% RSD after 200 hour humidity for six
(6) replicates.
• CC Strip/CC Fix on concrete for four (4) replicates initially had a 29% RSD precision. After 200 hours of
humidity the precision was 30.2% RSD for duplicate tests. CC Strip/CC Fix on stainless steel panels, six
(6) replicates initially had a precision of 4.7% RSD and for four (4) replicates after 200 hours humidity,
precision was 18.3% RSD.
• CC Strip/SBR 10 on concrete for four (4) replicates initially had a 7.5% RSD precision. After 200 hours
of humidity the precision was 16.3% RSD. CC Strip/SBR 10 on stainless steel panels, six (6) replicates
had a precision of 8.5% RSD initially and five (5) replicates a 12.4% RSD precision.
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SEPA
United States
Environmental Protection
Agency
PRESORTED STANDARD
POSTAGE & FEES PAID
EPA
PERMIT NO. G-35
Office of Research and Development (8101R)
Washington, DC 20460
Official Business
Penalty for Private Use
$300
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