Environmental Technology Verification Water Quality Protection Center
Coatings for Wastewater Collection Systems
VERIFICATION TEST PLAN
PROTECTIVE LINER SYSTEMS
For
EPA/NSF Environmental Technology Verification Program
Water Quality Protection Center
Joseph Trevino
Protective Liner Systems
6691 Tribble Street
Lithonia, Georgia 30058
Phone: 770-482-5201
Dr. C. Vipulanandan
University of Houston, CIGMAT
4800 Calhoun
Houston, Texas 77004
Phone: 713-743-4278
Thomas Stevens
NSF International
Proj. Mgr., Water Quality Protection Center
789 N. Dixboro Road
Ann Arbor, Michigan 48105
Phone: 734-769-5347
Raymond Frederick
U.S. Environmental Protection Agency
Proj. Offer, Water Quality Protection Center
NRMRL
2890 Woodbridge Ave. (MS-104)
Edison, New Jersey 08837
Phone: 732-321-6627
Carolyn Esposito
U.S. Environmental Protection Agency
Quality Assurance Officer, UWMB,WSWRD
National Risk Management Research Laboratory
2890 Woodbridge Ave. (MS-104)
Edison, New Jersey 08837
Phone: (732) 906-6895
Protective Liner Systems Test Plan This document is for review only and shall not be
8/4/2008 distributed without the written permission of NSF International.
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Environmental Technology Verification Water Quality Protection Center Coatings for Wastewater Collection Systems
TEST PLAN FOR VERIFICATION OF PROTECTIVE LINER SYSTEMS
COATINGS FOR WASTEWATER COLLECTION SYSTEMS
Prepared for:
NSF International
P.O. box 130140
Ann Arbor, MI 48113-0140
734-769-8010
800-673-6275
With support from the
U.S. Environmental Protection Agency
Prepared by:
C. Vipulanandan, Ph.D., P.E.
Center for Innovative Grouting Materials and Technology (CIGMAT)
University of Houston
Houston, TX 77204-4003
713-743-4278
Copyright 2008 NSF International 40CFR35.6450
Permission is hereby granted to reproduce all or part of this work, subject to the limitation that
users may not sell all or any part of the work and may not create any derivative work there from.
Contact the ETV Water Quality Protection Center Manager at 800-NSF-MARK with any
questions regarding authorized or unauthorized uses of this work.
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Environmental Technology Verification Water Quality Protection Center Coatings for Wastewater Collection Systems
Foreward
The U.S. Environmental Protection Agency (EPA) is charged by Congress with protecting the
Nation's land, air, and water resources. Under a mandate of national environmental laws, the
Agency strives to formulate and implement actions leading to a compatible balance between
human activities and the ability of natural systems to support and nurture life. To meet this
mandate, EPA's research program is providing data and technical support for solving
environmental problems today and building a science knowledge base necessary to manage our
ecological resources wisely, understand how pollutants affect our health, and prevent or reduce
environmental risks in the future.
The National Risk Management Research Laboratory (NRMRL) is the Agency's center for
investigation of technological and management approaches for preventing and reducing risks
from pollution that threaten human health and the environment. The focus of the Laboratory's
research program is on methods and their cost-effectiveness for prevention and control of
pollution to air, land, water, and subsurface resources; protection of water quality in public water
systems; remediation of contaminated sites, sediments, and ground water; prevention and control
of indoor air pollution; and restoration of ecosystems. NRMRL collaborates with both public
and private sector partners to foster technologies that reduce the cost of compliance and to
anticipate emerging problems. NRMRL's research provides solutions to environmental
problems by: developing and promoting technologies that protect and improve the environment;
advancing scientific and engineering information to support regulatory and policy decisions; and
providing the technical support and information transfer to ensure implementation of
environmental regulations and strategies at the national, state, and community levels.
This publication has been produced as part of the Laboratory's strategic long-term research plan.
It is published and made available by EPA's Office of Research and Development to assist the
user community and to link researchers with their clients.
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Environmental Technology Verification Water Quality Protection Center Coatings for Wastewater Collection Systems
Acknowledgements
EPA and NSF International acknowledge those persons who participated in the preparation,
review and approval of this Test Plan. Without their hard work and dedication to the project, this
document would not have been approved through the process that has been set forth for this ETV
project.
Author:
Dr. C. Vipulanandan, Director of CIGMAT - Center for Innovative Grouting Materials and
Technology, University of Houston
Technical Panel Reviewers:
Mr. Stephen A. Gilbreath, P.E.
Lockwood, Andrews & Newman, Inc.
Mr. Robert Lamb, P.E.
City of Austin, Texas
Mr. Raghavender Nednur, P.E.
City of Houston, Texas
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Environmental Technology Verification Water Quality Protection Center Coatings for Wastewater Collection Systems
Table of Contents
Foreward 3
Acknowledgements 4
Table of Contents 5
Acronyms 8
Glossary of Terms 8
1 Introduction 9
1.1 Background (City of Houston-University of Houston Study) 9
1.2 Technical Approach 9
1.3 Test Plan Schedule and Milestones 9
1.4 Roles and Responsibilities 10
1.4.1 Verification Organization (NSF) 10
1.4.2 U.S. Environmental Protection Agency (EPA) 10
1.4.3 Technology Panel 11
1.4.4 Testing Organization (CIGMAT Laboratories at UH) 11
1.4.5 Vendor ([Technology Name]) 12
2 Test Facility 12
3 Experimental Design 12
3.1 Preparation of Test Specimens 12
3.1.1 Concrete Specimens 13
3.1.1.1 Preparation of specimens 13
3.1.1.2 Number of specimens to be prepared 13
3.1.2 Clay Brick Specimens 13
3.1.2.1 Preparation of Specimens 13
3.1.2.2 Number of specimens to be prepared 14
3.1.3 Coating Specimens 14
3.1.3.1 Preparation of Specimens 14
3.1.3.2 Number of specimens to be prepared 14
3.2 Evaluation of specimens 14
3.3 Coating Application 15
3.4 Evaluation of coated specimens 15
3.4.1 Preparation of Exposure Vessels 15
3.4.2 Placement of specimens in vessels 16
3.4.3 Conditions for storage of vessels 16
3.5 Analytical Procedures 16
3.5.1 Holiday Test 16
3.5.2 Bonding Strength Tests (Sandwich Method and Pull-Off Method) 17
3.5.2.1 Sandwich Method 18
3.5.2.2 Pull-Off Method 19
4 Data Evaluation and Reporting 22
4.1 Data Reporting 22
4.2 Data Reduction 22
4.3 Data Validation 22
5 Quality Assurance Project Plan (QAPP) 23
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5.1 Quality Control Indicators 23
5.1.1 Representativeness 23
5.1.2 Completeness 23
5.1.3 Precision 24
6 Assessments 24
6.1 Audit Reports 24
6.2 Corrective Action Plan 24
7 Safety Considerations 25
8 References 26
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Environmental Technology Verification Water Quality Protection Center Coatings for Wastewater Collection Systems
Tables
Table 3.1 Mix Proportions for Concrete 13
Table 3-2. Test Names / Methods 14
Table 3-3. Number of Specimens Used for Each Characterization Test 15
Table 3-4. Sample of Holiday Test Results (Liquid Phase) for Coated Concrete (Dry) After One
(1) Month of Immersion 17
Table 3-5. Failure Types in CIGMAT CT 2 Test and CIGMAT CT 3 Tests 19
Table 3-6. Sample of Test Results for Bonding Strength of Coating with Dry Concrete 21
Table 3.7. Total Number of Tests with Coated Concrete 22
Tables Al & A2 28
Figures
Figure 3-1. Test configuration for the Holiday Test 16
Figure 3-2. Sandwich Test configuration 18
Figure 3-3. Pull-Off Test Method Configuration 20
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Environmental Technology Verification Water Quality Protection Center Coatings for Wastewater Collection Systems
Acronyms
ASTM ASTM International
CIGMAT Center for Innovative Grouting Materials and Technology
EPA United States Environmental Protection Agency
ETV Environmental Technology Verification
NSF NSF International
ORD Office of Research and Development
QA quality assurance
QAPP quality assurance project plan
QC quality control
UH University of Houston
WQPC Water Quality Protection Center
Glossary of Terms
Bonding Test - Tests performed to determine the bonding strength of coatings to selected
substrates.
Coatings - Materials applied to protect substrate the substrate against corrosive environment.
Holiday Test - Testing coated materials with pinholes in the coating, which penetrate into the
substrate.
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Environmental Technology Verification Water Quality Protection Center Coatings for Wastewater Collection Systems
1 INTRODUCTION
1.1 Background (City of Houston-University of Houston Study)
University of Houston (UH)/CIGMAT researchers have been investigating the performance of
various coatings for use in the City of Houston's wastewater facilities. Performance of each
coating has been studied with wet (representing rehabilitation of existing wastewater collection
systems) and dry (representing new construction) concrete and clay bricks. The studies have
been focused on (1) applicability and performance of the coating under hydrostatic pressure
(with an evaluation period between six to nine months) (2) chemical exposure with and without
holidays in the coating (initial evaluation period of six months) and (3) bonding strength (initial
evaluation period of twelve months). Chemical tests and bonding tests on over twenty coating
materials are being continued at UH. The long-term data collected on each coating can further
help engineers and owners to better understand the durability of coated materials in wastewater
environments.
1.2 Technical Approach
The overall objective of this test plan is to describe a testing program for systematically evaluate
coating materials used in wastewater systems to control the deterioration of cementitious
materials. Specific testing objectives are to:
evaluate the acid resistance of coated concrete specimens and clay bricks, with and
without holidays; and
determine the bonding strength of coating materials to concrete and clay bricks.
Testing will use relevant ASTM and CIGMAT standards. Specimens made from the coating
material, in addition to uncoated concrete and clay specimens will first undergo characterization
testing to determine if they are suitable for use during the acid resistance and bonding strength
tests. The coating manufacturer will then be responsible for coating the concrete and clay
specimens, under the guidance of CIGMAT staff members. Finally, the coated specimens will
be evaluated over the course of six months.
A coating-specific test plan will be prepared, using this base document as a template, for each
coating material to be evaluated through the ETV Water Quality Protection Center (WQPC).
Each plan will include specific testing procedures and a quality assurance project plan (QAPP)
describing the quality systems to be used during the evaluation.
1.3 Test Plan Schedule and Milestones
The tests described herein will be completed within six months from the start date. The data will
be compiled and summarized in a report to NSF International within two months of the
conclusion of testing.
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1.4 Roles and Responsibilities
This section defines the participants in this technology verification and their roles and
responsibilities.
1.4.1 Verification Organization (NSF)
Coordinate with CIGMAT, the Testing Organization, and the Vendor to prepare and
approve a product-specific test plan using this generic test plan as a template and meeting
all testing requirements included herein;
Coordinate with the ETV Coatings Technical Panel, as needed, to review the product-
specific test plan prior to the initiation of verification testing;
Coordinate with the EPA Water Quality Protection Center Project Officer to approve the
product-specific test plan prior to the initiation of verification testing;
Review the quality systems of the testing organization and subsequently, qualify the
testing organization;
Oversee the coatings evaluations and associated laboratory testing;
Review data generated during verification testing;
Oversee the development of a verification report and verification statement;
Print and distribute the verification report and verification statement; and
Provide quality assurance oversight at all stages of the verification process.
Primary contact: Mr. Thomas Stevens
NSF International
789 North Dixboro Road
Ann Arbor, MI 48105
Phone: 734-769-5347
Email: stevenst@nsf.org
1.4.2 U.S. Environmental Protection Agency (EPA)
This test plan has been developed with financial and quality assurance assistance from the ETV
Program, which is overseen by the EPA's Office of Research and Development (ORD). The
ETV Program's Quality Assurance Manager and the WQPC Project Officer will provide
administrative, technical, and quality assurance guidance and oversight on all ETV WQPC
activities, and will review and approve each phase of the verification project. The primary
responsibilities of EPA personnel are to:
Review and approve test plans, including the quality assurance project plans (QAPPs);
Sign the test plan signoff sheet;
Review and approve the verification report and verification statement; and
Post the verification report and verification statement on the EPA ETV website.
Primary contact: Mr. Ray Frederick
U.S. Environmental Protection Agency, NRMRL
Project Officer, Water Quality Protection Center
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Environmental Technology Verification Water Quality Protection Center Coatings for Wastewater Collection Systems
2890 Woodbridge Ave. (MS-104)
Edison, New Jersey 08837
Phone: 732-321-6627
Email: frederick.ray@epamail.epa.gov
1.4.3 Technology Panel
A Technology Panel was formed to assist with the review of the coatings test plan. Input from
the panel ensures that data generated during verification testing are relevant and that the method
of evaluating different technologies is fair and consistent. All product-specific grout test plans
are subject to review by representatives of the Technology Panel and will be approved by the
WQPC Program Manager, the WQPC Project Officer, and the vendor.
1.4.4 Testing Organization (CIGMAT Laboratories at UH)
The Testing Organization for verifications conducted under this test plan is CIGMAT
Laboratories at the University of Houston. The primary responsibilities of the Testing
Organization are:
Coordinate with the Verification Organization and Vendor relative to preparing and
finalizing the product-specific Test Plan;
Sign the test plan signoff sheet;
Conduct the technology verification in accordance with the Test Plan, with oversight by
the Verification Organization;
Analyze all samples collected during the technology verification process, in accordance
with the procedures outlined in the Test Plan and referenced SOPs;
Coordinate with and report to the Verification Organization during the technology
verification process;
Provide analytical results of the technology verification to the Verification Organization;
and
If necessary, document changes in plans for testing and analysis, and notify the
Verification Organization of any and all such changes before changes are executed.
CIGMAT supports faculty, research fellows, research assistants and technicians. The CIGMAT
personnel will work in-groups to complete the tests described in this test plan. All the personnel
report to the Group Leader and the CIGMAT Director. The CIGMAT Director is responsible for
appointing Group Leaders, who, with his approval, are responsible for drawing up the schedule
for testing. Additionally, a Quality Assurance (QA) Engineer, who is independent of the testing
program, will be responsible for internal audits.
Primary contact: Dr. C. Vipulanandan
University of Houston, CIGMAT
4800 Calhoun
Houston, Texas 77004
Phone: 713-743-4278
Email: cvipulanandan@uh.edu
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1.4.5 Vendor (Protective Liner Systems)
Provide the Testing Organization with coating samples for verification (this includes
applying the coating materials to test specimens at the CIGMAT facilities);
Complete a product data sheet prior to testing. (Refer to Appendix B);
Provide start-up services and technical support as required during the period prior to the
evaluation;
Provide technical assistance to the Testing Organization during verification testing period
as requested; and
Provide funding for verification testing.
Primary contact: Mr. Joseph Trevino
Protective Liner Systems
6691 Tribble Street
Lithonia, GA 30058
Phone: 770-482-5201
Email: Joseph@ProtectiveLinerSystems.com
2 TEST FACILITY
The testing will be performed in the CIGMAT Laboratories at the University of Houston,
Houston, Texas. The CIGMAT Laboratories are located in the Central Campus of UH at 4800
Calhoun Road (off interstate highway 1-45 South toward Galveston).
The CIGMAT laboratories and affiliated facilities are equipped with devices that can perform all
of the coatings tests in this test plan. Molds are available to prepare the specimens for testing,
and all acid resistance and bonding strength test procedures are documented in standard
operating procedures.
3 EXPERIMENTAL DESIGN
The test plan includes characterization of coating materials used on concrete and clay brick
surfaces. In addition, holiday tests and bonding strength tests on the coated/lined materials will
be performed.
3.1 Preparation of Test Specimens
Testing will be completed using both concrete and clay brick specimens. The concrete
specimens will be prepared in the CIGMAT laboratory by CIGMAT personnel prior to
application of the coating. The clay brick specimens will be obtained from a local brick supplier
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and prepared to the proper specifications by CIGMAT staff. The source of materials for all
specimens will be identified in the final report.
3.1.1 Concrete Specimens
3.1.1.1 Preparation of specimens
Mix proportions for the concrete are summarized in Table 3-1. The cylindrical specimens will be
cast in 3-in (diameter) x 6-in (length) plastic molds. Wooden molds will be used to cast the 1.5-
in x 2-in x 6-in prism specimens. The concrete specimens will be cured for at least 28 days at
room conditions.
Table 3.1 Mix Proportions for Concrete
Materials
Cement
Sand
Coarse Aggregate
Water
Amount
6 bags
1400-1500 Ibs
1600 -1700 Ibs
320 -330 Ibs
The materials used for making the specimens shall meet the following specifications:
Cement - ASTM C150 Type 1, purchase in 94 Ib bags
Sand-ASTMC33
Coarse aggregate - ASTM C33, ranging in size from No.4 to 1.5 in sieves
The concrete shall be prepared by combining proportional amounts of cement, sand, and coarse
aggregate in a container and mixing the materials with a standard concrete mixer until the
mixture is uniform in appearance. The specimen molds shall be filled with the mixture and shall
be mechanically vibrated until the concrete in the molds is the appropriate consistency.
3.1.1.2 Number of specimens to be prepared
A total of 20 concrete cylinders and 36 concrete prisms shall be prepared. This number of
specimens is sufficient for testing replicate and control samples.
3.1.2 Clay Brick Specimens
3.1.2.1 Preparation of Specimens
Clay bricks will be purchased new from a brick supplier. The bricks shall be standard sewer
bricks. The source and characteristics of the bricks shall be recorded and the information
included in the final report. The bricks shall be cut at the CIGMAT laboratory into 1.5-in x 2-in
x 6-in prism specimens using a diamond-tipped saw blade. The prepared specimens shall be
stored at room conditions.
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3.1.2.2 Number of specimens to be prepared
A total of 56 clay brick prisms shall be prepared. This number of specimens is sufficient for
testing replicate and control samples.
3.1.3 Coating Specimens
3.1.3.1 Preparation of Specimens
Specimens made only of the coating material shall also be prepared in 1.5-in (diameter) x 3-in
(length) plastic molds. This information is retained and reported to verify the coating in any
future applications. It can be used to determine if the coating material tested through the ETV
WQPC is the same as that is being applied.
3.1.3.2 Number of specimens to be prepared
A total of 6 coating specimens shall be prepared for characterization testing.
3.2 Evaluation of specimens
The concrete cylinders and prisms, clay brick prisms, and raw coating material cylinders shall be
evaluated as described in this section to determine if they meet the required properties for use in
the verification testing. The specimens shall be characterized using the following tests, as
specified in Table 3-2:
Table 3-2. Test Names / Methods
Test Name
Pulse Velocity
Holiday Test (Chemical Resistance)
Bonding Strength
Test Method
ASTM C 597
ASTM G20 / CIGMAT CT-1-99
ASTM C 32 11 CIGMAT CT3 (Sandwich Method)
ASTM D 4541/CIGMAT CT2 (Pull-Off Strength)
The pulse velocity and unit weight of all the specimens will be determined for quality control
purposes. Additional specimens will be used to determine the compressive (3 specimens) and
flexural strength (3 specimens) of concrete and flexural strength of clay bricks (3 specimens)
(Table 3-3). The average values of the strengths will be reported in the final report. Note that
the strength tests are done for completeness and not for quality control.
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Table 3-3. Number of Specimens Used for Each Characterization Test
Material
Coating
Concrete Cylinders
Concrete Prisms
Clay Prisms
Number of Specimens Used in Test
Unit
weight
6
20
36
56
Pulse
velocity*
6
20
36
56
Water
absorption**
6
10
None
10
Flexure***
None
None
3
3
Compression***
None
O
None
None
*Unit weight measurement taken on specimens prior to this test.
** Specimens used after the Pulse Velocity test.
*** Flexure and compression tests are performed for informational purposes only.
The unit weight of concrete and clay brick will be in the range of 140-160 pcf and 120-140 pcf,
respectively. The pulse velocity of concrete and clay brick will be in the range of 15000-16000
ft/sec and 7500-8500 ft/sec, respectively. The water absorption of concrete and clay brick will
be in the range of 0.5-2 % and 18-30% respectively. The flexural strength of concrete and clay
brick will be in the range of 900-1300 psi and 700 -1100 psi, respectively. The compressive
strength of concrete and clay brick will be in the range of 4000-5000 psi.
3.3 Coating Application
The concrete and clay specimens shall be coated by the coating supplier or their representative in
the CIGMAT laboratory at the UH. Wet specimens are immersed in water for at least 7 days
before coating the specimens. The manufacturer of the coating will select the method to prepare
the specimens. The details will be summarized in the final report.
3.4 Evaluation of coated specimens
Coated concrete and clay brick specimens will be tested for chemical resistance and bonding
strength after the coating is cured in accordance with the coating manufacturer's specifications.
3.4.1 Preparation of Exposure Vessels
Typical sizes of the clean vessels that will be used in the holiday tests are shown in Fig. 3-1. In
each bottle there will be only one coated specimen. Once the vessels are closed, they shall be
airtight. No venting of the vessels is required.
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Plastic Lid (Air Tight)
Liquid Le\ el
Coated Concrete
or C lav Brick
Holiday
210
A I*2 mm ;ft u sn height cocciete peeimen ;rclay brick
B 33 nun 11 5 la i hoUtb" location
C ^6 uuu i ? in 1 Ji^inetc: vuncsste c^lsniei
O 152 x 3- x 4:" tumble'.- .ecticc ;>£ d;n bii;l:
Figure 3-1. Test configuration for the Holiday Test.
3.4.2 Placement of specimens in vessels
The specimens will be placed in water or 1% sulfuric acid solution as shown in Fig. 3-1. Half
the specimen will be submerged in the test liquid (CIGMAT CT 1).
3.4.3 Conditions for storage of vessels
The specimens will be stored at room temperature (72°F).
3.5 Analytical Procedures
3.5.1 Holiday Test
In this test (CIGMAT CT 1-99), the changes in (1) diameter/dimension at the holiday level (2)
weight of specimen and (3) appearance of specimen will be monitored at regular intervals. The
test reagents selected for this study are (1) deionized (DI) water (pH = 5 to 6) and (2) 1% sulfuric
acid solution (a pH of 1 represents a long-term, worst-case condition in a wastewater collection
system, arising from formation of hydrogen sulfide). Control tests will be performed with no
holidays.
Dry and wet concrete and clay brick specimens will be coated. Dry specimens are dried at room
condition for at least seven days before coating the specimens.
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Specimens will be prepared by stripping the molds from the concrete cylinders completely. Clay
bricks will be cut to a size of 2-in. x 1.5-in. x 6-in. for this test. Dry and wet specimens shall be
coated on all sides. For the test, two radial holidays of different diameters will be drilled into
each specimen approximately 0.5-in. deep (Fig. 3-1). The diameter of the drill bits used shall not
be less than three times the coating thickness, and they shall be selected from the following
standard diameters: 3 mm (1/8"), 6 mm (1/4"), and 13 mm (1/2"). Both holidays shall lie in the
same axis.
In order to study the chemical resistance of coated concrete and clay brick materials, as shown in
Fig. 3-1, the specimens will be immersed in a selected test reagent to half the specimen height in
a closed vessel so that the specimens are exposed to both the liquid phase and vapor phase. This
method is intended for use as a relatively rapid test to evaluate the acid resistance of coated
specimens under anticipated service conditions.
The specimens shall be inspected after 1 and 6 months to determine if there are blisters, cracking
of the coating, and /or erosion of the coating in the immersed solution. The results will be
summarized as shown in Table 3-4.
All observations shall be recorded at the time of observation and reported in the final report.
Table 3-4. Sample of Holiday Test Results (Liquid Phase) for Coated Concrete (Dry) After
One (1) Month of Immersion
Concrete
Dry
Total No.
%(P/B/F)
Remarks
Holiday
No Holiday
1/8 inch
1/2 inch
After one (1)
month of
immersion
Medium (No. of Specimens)
DI Water
N(2)
N(2)
4
(100/0/0)
None
1% H2SO4
N(2)
N(2)
N(2)
6
(100/0/0)
None
Total No.
%(N/B/C)
4 (100/0/0)
3 (100/0/0)
2 (100/0/0)
10
(100/0/0)
None
Remarks
None
None
None
Total of 10
specimens tested
No damage
N=No blister or crack; B=Blister; C=Cracks.
3.5.2 Bonding Strength Tests (Sandwich Method and Pull-Off Method)
These tests will be performed to determine the bonding strength between concrete/clay brick
specimens and the coating material over a period of six months. The number of specimens to be
used for testing is summarized in Tables A-l and A-2. A total of twelve sandwich and twelve
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pull-off tests shall be performed on coated concrete samples. The same number of tests shall be
conducted with coated clay bricks.
3.5.2.1 Sandwich Method
In this test (CIGMAT CT 3-00), the coating will be sandwiched between a pair of rectangular
concrete block and clay brick specimens and then tested for bonding strength (Fig. 3-2). The
bonding strength of the coating will be the failure load divided by the bonded area. Also the
failure type (see Table 3-5) will be identified.
In the sandwich method test, the coating will be sandwiched between a pair of rectangular
concrete block and clay brick specimens and then tested for bonding strength (Fig. 3-2). Both
dry and wet specimens will be used to represent the extreme coating conditions. Dry specimens
are dried at room conditions for at least seven days before coating the specimens. Wet specimens
are immersed in water for at least seven days before coating the specimens. The manufacturer of
the coating will select the method to prepare the specimens and also coat them. The details will
be summarized in the final report. All the bonded specimens will be cured under water up to the
point of testing. A total of twenty-four concrete and twenty-four clay brick prisms will be used
in this test.
The sandwich method bonding strength tests will be performed to determine the bonding
strength between the concrete/clay brick and the coating material over a period of six months. A
total of 12 tests with concrete and 12 tests with clay bricks are planned.
Figure 3-2. Sandwich Test configuration.
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Table 3-5. Failure Types in CIGMAT CT 2 Test and CIGMAT CT 3 Tests
Failure
Type
TypeBl
Type B2
Type B3
Type B4
Type B5
Description
Substrate Failure
Coating Failure
Bonding Failure
Bonding and
Substrate Failure
Bonding and
Coating Failure
CIGMAT CT 2 Test
(Modified ASTM D4541)
metal ^ |~~|
fixture ~~*1 .Coating
*^r
1 LJ^J |
Concrete/Clay Brick
metal ^|~~|
fixture ~~*1 Coating
UU^
1 LJ LJ |
Concrete/Clay Brick
fixture ~~^| | ^^, Coating
1 U LJ 1
Concrete/Clay Brick
metal »^l~~l
fixture~H Coating
UM^
1 \ PI i [
Concrete/Clay Brick
metal »^l~~l
fixture~n Coating
LJ-*-"^
1 1
Concrete/Clay Brick
CIGMAT CT 3
(ASTM C321 Test)
Concrete/Clay Brick
X
1 \\ 1
> 1
Concrete/Clay Brick
X
* \ \
Concrete/Clay Brick
i i
* \ \
Concrete/Clay Brick
X
1 1
i ^ s\
Coating 1 1
Concrete/Clay Brick
X
1 1
* 1 -= 1
Coating 1 1
3.5.2.2 Pull-Off Method
In this test (CIGMAT CT 2-00), a 2-in. diameter circular area will be used for testing (Fig. 3-3).
Coated concrete prisms and clay bricks will be cored using a diamond core drill bit to a
predetermined depth to isolate the coating and a metal fixture will be glued to the isolated
coating section using a rapid setting epoxy.
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C-" d'30,11 e c tint
' P*rt*
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Table 3-6. Sample of Test Results for Bonding Strength of Coating with Dry Concrete
Concrete
Dry
Total No.
(% Failure)
Remarks
Curing
Time
(days)
10
10
90
90
180
180
Up to twelve
(12) months
Failure Modes
Typel
0%
None
Type 2
0%
None
TypeS
X
X
X
X
67%
Dominant
failure
mode
Type 4
X
X
33%
TypeS
0%
None
Failure
Strength (psi)
192
260
174
217
156
267
Total no. of
successful lab.
tests is 6
Average
strength is 211
psi.
Type 1 = Concrete failure
Type 2 = Coating failure
Type 3 = Bonding failure
Type 4 = Combined concrete and bonding failure
Type 5 = Combined coating and bonding failure
3.3 Sampling Events
3.3.1 General Description
Tables Al and A2 summarize the samples needed for each test condition (dry versus wet;
concrete and clay bricks). Bonding tests are planned after two weeks (or at the earliest time
specified by the coating manufacturer), 3 months and 6 months after coating. The planned tests
with coated concrete are summarized in Table 3.7.
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Table 3.7. Total Number of Tests with Coated Concrete
Exposure
Time
2 Weeks
1 Month
3 Months
6 Months
Holiday Test*
DI Water
8
8
1% H2SO4
12
12
Bonding Strength Test
Sandwich
4
4
4
Pull-Off
4
4
4
* The same specimens are monitored for 6 months.
4 DATA EVALUATION AND REPORTING
CIGMAT is responsible for managing all the data and information generated during the testing
program. To maintain good quality data, specific procedures shall be followed during data
reduction, validation, and reporting. These procedures are discussed below.
4.1 Data Reporting
All the data collected during the testing will be processed and analyzed as outlined in Section 5.
All data will be processed and reported in hard copy. The report will include the main text with
summary of the test results. The appendix will include sections on material tests, hydrostatic
test, chemical-holiday test and bonding test. Photographs on the coated surfaces and bonding
test specimens will be included in the report. Also the information provided by the
coating/lining manufacturer will be included in the appendix.
After discussions with NSF and EPA, appropriate information will be posted on their web sites.
4.2 Data Reduction
Data reduction refers to the process of converting the raw results from the equipment into data
that of use in selecting the material for wastewater system maintenance and rehabilitation. The
data will be obtained from logbooks, data sheets, and computer outputs.
4.3 Data Validation
The person performing the test shall verify the completeness of the appropriate data forms. The
CIGMAT Director will review laboratory logbooks and data sheets on a regular basis to verify
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completeness. The CIGMAT technical staff will inspect the testing equipment and keep them in
working condition.
5 QUALITY ASSURANCE PROJECT PLAN (QAPP)
The QAPP for this testing plan specifies procedures that shall be used to ensure quality and
integrity. Careful adherence to these procedures will ensure that the data generated from the
verification testing will provide sound analytical results that can serve as the basis for
performance testing.
The qualified testing organization, Center for Innovative Grouting Materials and Technology
(CIGMAT), with oversight from NSF, should ensure the QAPP is implemented during all the
testing activities. For each batch of concrete and clay brick purchased to perform the laboratory
tests, 5% of the specimens will be tested to ensure the quality. The testing will include unit
weight, pulse velocity and water absorption of the specimens. If the maximum or minimum
value of the batch exceeded +20% of the mean value the batch will be rejected.
CIGMAT researchers and technical personnel will perform the tests. Primary responsibility for
ensuring that the sampling and testing activities comply with the accepted QA/QC requirements
shall rest with the Director of CIGMAT with oversight by NSF. If problem arises or any test data
appear unusual, they shall be thoroughly documented.
5.1 Quality Control Indicators
5.1.1 Representativeness
As specified by NSF, representativeness of samples for the ETV will be ensured by executing
consistent sample collection procedures, including sample locations, timing of sample collection,
sampling procedures, sample preservation, sample packaging, and sample transport.
5.1.2 Completeness
Completeness refers to the amount of data collected from a measurement process compared to
the amount that was expected. For this ETV test plan, completeness refers to the proportion of
valid, acceptable data generated using each method. The completeness objective for data
generated through this test plan is 85 percent.
In
valid and acceptable \ i rvrv
x 100 (Equation I)
Yl
"total
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5.1.3 Precision
As specified in Standard Methods (Method 1030 C), precision is specified by the standard
deviation of the results of replicate analyses. The overall precision of a study includes the
random errors involved in sampling as well as the errors in sample preparation and analysis.
\ Standard Deviation = J - (Equation 2)
J V w-1
Where:
x = sample mean
x; = /th data point
n = number of data points
6 ASSESSMENTS
6.1 Audit Reports
Any QA inspections will be formally documented in an Audit Report and submitted to the EPA
Pilot Manager, EPA Pilot Quality Manager, and NSF Partner Manager for review. The NSF
Partner Manager, Project Coordinator, Manager, QA and Safety, or other qualified NSF designee
will conduct a technical system audit and a performance evaluation audit of measurement
systems used in testing at least once during the verification testing period for a given technology.
6.2 Corrective Action Plan
This test plan shall include the predetermined acceptance limits, the corrective action to be
initiated whenever such acceptance criteria are not met, and the names of the individuals
responsible for implementation. Routine corrective action may result from common monitoring
activities, such as:
Performance evaluation audits
Technical systems audits
Ultimately, responsibility for project quality assurance/quality control (QA/QC) during
implementation of this Test Plan rests with the Verification Organization, specifically the
Verification Organization Project Manager, with appropriate input from the Verification
Organization QA/QC Manager. However, immediate QA/QC for individual tasks (e.g. sample
collection, handling, preparation, and analysis) rests with the individuals and organization
performing the task at hand, as described this Test Plan. The Verification Organization Project
Manager will coordinate oversight and/or audits of these tasks with the Testing Organization
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Project Manager to ensure that the Test Plan is being executed as written, and that
nonconformances are appropriately reported and documented.
Corrective action shall be taken whenever a nonconformance with the Test Plan occurs.
Nonconformances can occur within the realm of sampling procedures, sample receipt, sample
storage, sample analysis, data reporting, and computations.
7 SAFETY CONSIDERATIONS
Coating the specimens for the tests will be done at the covered test CIGMAT facility at UH,
which as adequate ventilation. The research personnel and technicians on-site will take all
necessary precautions to ensure safety and compliance with local and federal regulations.
CIGMAT maintains a health and safety plan, which shall be made available to personnel
involved in this project. Adherence to health and safety plan shall be ensured throughout the
duration of the project.
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8 REFERENCES
[1] Annual Book of ASTM Standards (1998), Vol. 06.01, Paints-Tests for Formulated
Products and Applied Coatings, ASTM, Philadelphia, PA.
[2] Annual Book of ASTM Standards (1998), Vol. 04.05, Chemical Resistant Materials;
Vitrified Clay, Concrete, Fiber-Cement Products; Mortar; Masonry, ASTM,
Philadelphia, PA.
[3] EPA (1974), "Sulfide Control in Sanitary Sewerage System", EPA 625/1-74-005,
Cincinnati, Ohio.
[4] EPA (1985), "Odor and Corrosion Control in Sanitary Sewerage System and Treatment
Plants", EPA 625/1-85/018, Cincinnati, Ohio.
[5] Islander, R. L., Devinny, J.S. Mansfield, F. aPostyn, A. and Shih, H. (1991)," Microbial
Ecology of Criown Corrosion In Sewers," Journal of Environmental Engineering, Vol.
117, No. 6, p. 751-770.
[6] Kienow, K. and Cecil Allen, H. (1993). "Concrete Pipe for Sanitary Sewers Corrosion
Protection Update," Proceedings, Pipeline Infrastructure II, ASCE, pp. 229-250.
[7] Liu, J. and Vipulanandan, C. (1999)," Testing Epoxy Coating for Protecting Dry and Wet
Concrete Wastewater Facilities," Journal of Protective Coatings and Linings, p. 26-37.
[8] Liu, J., and Vipulanandan, C. "Tensile Bonding Strength of Epoxy Coatings to Concrete
Substrate," Cement and Concrete Research. Vol. 35, pp. 1412-1419, 2005.
[9] Liu, J., and Vipulanandan, C. "Long-term Performance of Epoxy Coated Clay Bricks in
Sulfuric Acid," Journal of Materials in Engineering, ASCE, Vol. 16, No. 4, pp.349-355,
2004.
[10] Liu, J. and Vipulanandan, C "Modeling Water and sulfuric Acid Transport Through
Coated Cement Concrete," Journal of Engineering Mechanics, ASCE, Vol. 129(4), pp.
426-437,2003.
[11] Liu, J. and Vipulanandan, C. "Evaluating a Polymer Concrete Coating for Protecting
Non-Metallic Underground Facilities from Sulfuric Acid Attack," Journal of Tunnelling
and Underground Space Technology, Vol. 16, pp. 311-321, 2001.
[12] Nixon, R. (1997)," Future Material Selection Guidelines for Coatings on Concrete for
Changing Exposure Conditions in Large Municipal Wastewater Collection/Treatment
Systems," Proceedings, Corrosion 97, Paper No.379, 19 p.
[13] Redner, J.A., Randolph, P. Hsi, and Edward Esfandi (1992), "Evaluation of Protective
Coatings for Concrete" County Sanitation District of Los Angeles County, Whittier, CA.
Protective Liner Systems Test Plan This document is for review only and shall not be Page 26 of 34
8/4/2008 distributed without the written permission of NSF International.
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Environmental Technology Verification Water Quality Protection Center Coatings for Wastewater Collection Systems
[14] Redner, J.A., Randolph, P. Hsi, and Edward Esfandi (1994), "Evaluating Coatings for
Concrete in Wastewater facilities: Update," Journal of Protective Coatings and Linings,
December 1994, pp. 50-61.
[15] Soebbing, J. B., Skabo, Michel, H. E., Guthikonda, G. and Sharaf, A.H. (1996),
"Rehabilitating Water and Wastewater Treatment Plants," Journal of Protective Coatings
and Linings, May 1996, pp. 54-64.
[16] Vipulanandan, C., Ponnekanti, H., Umrigar, D. N., and Kidder, A. D. (1996), "Evaluating
Coatings for Concrete Wastewater Facilities," Proceedings, Fourth Materials Congress,
American Society of Civil Engineers, Washington D.C., November 1996, pp. 851-862.
[17] Vipulanandan, C. and Liu, J. "Performance of Polyurethane-Coated Concrete in Sewer
Environment," Cement and Concrete Research, Vol. 35, pp. 1754-1763, 2005.
[18] Vipulanandan, C. and Liu, J. "Film Model for Coated Cement Concrete," Cement and
Concrete Research. Vol. 32(4), pp. 1931-1936, 2002.
[19] Vipulanandan, C. and Liu, J. "Glass-Fiber Mat Reinforced Epoxy Coating for Concrete in
Sulfuric Acid Environment," Cement and Concrete Research, Vol. 32(2), pp. 205-210,
2002.
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ATTACHMENT I
Tables Al & A2
Laboratory Tests for Coating Materials with Concrete & Clay Bricks
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Table Al. Planned Laboratory Tests for Coating Materials with Concrete
ASTM
/CIGMAT
Standard
ASTM
G20/
CIGMAT
CT1
ASTM
C321/
CIGMAT
CT3
ASTM
D4541/
CIGMAT
CT2
Name of test
Chemical
Resistance of
Pipeline Coatings
3%H2SO4
D.I. Water
Bond Strength of
Coating/ Mortars
Pull-Off
Strength of
Coatings Using
Portable
Adhesion Testers
Number of
specimens
(Dry)
WITH
HOLIDAYS
4
2
Number of
specimens
(Dry)
WITHOUT
HOLIDAYS
2
2
6
6
Number of
specimens
(Wet)
WITH
HOLIDAYS
4
2
Number of
specimens
(Wet)
WITHOUT
HOLIDAYS
2
2
6
6
Type of
specimens
Concrete
Cylinder
3 in. diameter
and 6 in. height
Concrete
Rectangular
Blocks
2 1/4 in. X
3 3/4 in. X
Sin.
Concrete
Rectangular
Blocks
2 1/4 in. X
3 3/4 in. X
Sin.
Remarks
20 specimens
must be coated
and tested over a
period of six
months
12 pairs of
bonding
specimens
12 blocks must
be coated
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Table A2. Planned Laboratory Tests for Coating Materials with Clay Bricks
ASTM/
CIGMAT
Standard
ASTM
G20/
CIGMAT
CT1
ASTM
C321/
CIGMAT
CT3
ASTM
D4541/
CIGMAT
CT2
Name of test
Chemical
Resistance of
Pipeline Coatings
1%H2SO4
D.I. Water
Bond Strength of
Coatings/
Mortars
Pull-Off
Strength of
Coatings Using
Adhesion Testers
Number of
specimens
(Dry)
WITH
HOLIDAYS
4
2
Number of
specimens
(Dry)
WITHOUT
HOLIDAYS
2
2
6
6
Number of
specimens
(Wet)
WITH
HOLIDAYS
4
2
Number of
specimens
(Wet)
WITHOUT
HOLIDAYS
2
2
6
6
Type of
specimens
Clay bricks
Clay bricks
Clay bricks
Remarks
20 specimens
must be coated
and tested over a
period of one
year
12 pairs of
bonding
specimens
12 blocks must
be coated
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APPENDIX A
CIGMAT Test Methods
CIGM AT CT 1-99 Standard Test Method of Coated or Lined Concrete and Clay Bricks
CIGMAT CT 2 - 00 Standard Test Method for Pull-Off Strength of Coatings or Linings:
Laboratory Test and Field Test
CIGMAT CT 3-00 Standard Test Method for Bonding Strength of Coatings and Mortars:
Sandwich Method
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APPENDIX B
Vendor Data Sheet
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VENDOR DATA SHEET
PHYSICAL PROPERTIES OF COATING
Coating Product Name:
Coating Product Vendor Name and Address
Coating Type:
Testing Method
Tensile Adhesion to Concrete
(ASTMD4541)
Chemical Resistance (ASTM D 543)
(3 % H2 SO4)
Water Vapor Transmission
(ASTMD 1653/E 1907)
Bending Strength or Tensile Strength
(ASTM D 790)
Hardness- Shore D (ASTM D 2240)
Impact Resistance (ASTM G 14)
Volatile Organic Compounds - VOC's
(ASTM D 2832)
Vendor Results
Worker Safety
Flammability Rating
Known Carcinogenic Content
Other hazards (corrosive)
Result/Requirement
Environmental
Characteristics
Heavy Metal Content (w/w)
Leaching of Cured Coating (TCLP)
Disposal of Cured Coating
Result/Requirement
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Application
Characteristics
Primer Requirement
Number of Coats and Thickness
Minimum Application Temperature
Minimum Cure Time Before Handling
Maximum Application Temperature
Minimum Cure Time before Immersion
into Service
Type of Surface Preparation Before
Coating
Result/Requirement
Vendor
Experience
Length of time the Coating in Use
Applicator Training & Qualification
Program
QA/QC Program for Coating/Lining
Comments
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