EPA/600/R-12/582
July 2012
10/36/WQPC-SWP
Environmental Technology
Verification Report
Grouts for Wastewater Collection Systems
Warren Environmental, Inc.
301-04 Epoxy GROUT
Prepared by
Center for Innovative Grouting Materials and Technology
University of Houston
RTI International & NSF International
Prepared for:
U.S. Environmental Protection Agency
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Environmental Technology Verification Report
Verification of Grouts for Rehabilitation of
Wastewater Collection Systems
Warren Environmental, Inc.
Prepared by
Center for Innovative Grouting Materials and Technology (CIGMAT)
University of Houston
Houston, TX 77204
RTI International
P.O. Box 12194
Research Triangle Park, NC 27709-2194
and
NSF International
P.O. box 130140
Ann Arbor, MI 48113-0140
Prepared for:
Raymond Frederick, Project Officer
National Risk Management Research Laboratory
Water Supply and Water Resources Division
U.S. Environmental Protection Agency
Edison, New Jersey 08837
2012
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EPA STREAMS 61/ETV Water Quality Protection Center Verification Grouting Materials
NOTICE
The U.S. Environmental Protection Agency (EPA), through its Office of Research and
Development, funded and managed the research described herein under Task Order (TO) 61,
Field Verification of Drinking Water and Wastewater Systems Assessment and Rehabilitation
Technologies, of Contract No. EP-C-05-060, with RTI International. The testing was performed
by the Center for Innovative Grouting Materials and Technology (CIGMAT); NSF International
provided quality assurance and other technical support. This document has been reviewed by
RTI, NSF, and EPA and is recommended for public release.
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CONTENTS
Page
Section 1 Introduction 1
1.1 ETV Purpose and Program Operation 1
1.2 Roles and Responsibilities 1
1.2.1 Verification Organization (RTI International and NSF International) 1
1.2.2 U.S. Environmental Protection Agency (EPA) 2
1.2.3 Testing Organization (CIGMAT Laboratories at the University of Houston) 2
1.2.4 Vendor (Warren Environmental) 3
1.3 Background and Technical Approach 4
1.4 Test Facility 4
1.5 Objectives 4
Section 2 Grout Material Description 6
Section 3 Methods and Test Procedures 7
3.1 Grout Evaluation 7
3.1.1 Grout Specimen Preparation 7
3.1.2 Grout Curing Properties 9
3.1.3 Durability Properties 10
3.1.4 Environmental Properties—Leaching Test 11
3.2 Grout-Substrate Bonding Strength 11
3.3 Model Test 11
3.3.1 Model Test: Concrete Leak Repair 12
Section 4 Results and Discussion 14
4.1 Grout Properties 14
4.1.1 Working Properties 14
4.2 Physical and Mechanical Properties 14
4.2.2 Shrinkage Test 15
4.2.3 Permeability 15
4.2.4 Compressive Strength and Stress-Strain Relationship 15
4.3 Durability Properties 16
4.3.1 Wet-Dry Cycles 16
4.3.2 Chemical Resistance 17
4.4 Environmental Properties—Leaching Study 18
4.5 Grout/Substrate Interactions 18
4.6 Model Test 20
4.5 Summary of Observations 22
Section 5 QA/QC Results and Summary 24
5.1 Requirements for Sample Preparation 24
5.1.1 Specimen Preparation 24
5.1.2 Unit Weight and Pulse Velocity 24
5.1.3 Flexural Strength 24
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5.2 Quality Control Indicators 25
5.2.1 Representativeness 25
5.2.2 Completeness 25
5.2.3 Precision 26
5.2.4 Accuracy 26
5.3 Audit Reports 27
5.4 Data Review 27
Section 6 Suggested Reading 28
Appendix A Behavior of Cement Concrete Bricks 30
Appendix B Characterization of Grout 33
Appendix C Grout-Substrate (Concrete) Interaction 44
Appendix D Grout Vendor Data Sheet 47
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FIGURES Page
2-1. 301-04 Epoxy grout specimen 6
3-1. Typical mold used for preparing grout specimens 7
3-2. Model configuration for testing concrete leak repair 13
4.1. Sandwiched specimens for bonding test (Warren Environmental 301-04 epoxy
grout) 19
4-2. Typical failed specimen (Type 1 failure pattern) 19
4-3. Results of grout-substrate bonding test 20
4-4. Model test setup (a) Cracked concrete and (b) After grout repair 21
4-5. Model 4 test setup 21
TABLES Page
3-1. Grout Tests for Concrete Leak Repair 8
3-2. Grout-Substrate Interaction Tests 8
3-3. Shrinkage Test Conditions 10
3-4. Handling Methods and Analyses for Collected Samples 11
4-1. Summary of Working Properties of Epoxy Grout 14
4-2. Results of Water Absorption 15
4-3. Summary of Compressive Strength Properties with Curing Time 16
4-4. Wet-Dry Cycle Test Results 16
4-5. Chemical Resistance Test Results 17
4-6. Summary of Bonding Strength Tests (CIGMAT CT-3) 20
4-7. Model Test 4 Leak Rate Results (gallons/day) 22
5-1. Typical Properties for Concrete Specimens 24
5-2. Number of Specimens Used for Each Characterization Test 25
5-3. Total Number of Tests on Concrete-Grout Interaction Material 26
5-4. Standard Deviation for Concrete Specimen Physical and Strength Properties and
Grout Unit Weight 26
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Grouting Materials
ASTM
CIGMAT
°F
DI
DQI
EPA
ETV
ft/sec
ft2
gal
g/cm3
g/L/g
gpm
GP
hr
in.
kg
kg/cm2
kg/m3
L
Ibs
min
NRMRL
m/sec
m3
mg/L
mL
mm
MPa
NSF
pcf
psi
QA
QC
RPD
Room conditions
TO
VO
VTP
WQPC
ACRONYMS AND ABBREVIATIONS
American Society for Testing and Materials
Center for Innovative Grouting Materials and Technology, University of
Houston
Celsius degrees
Fahrenheit degrees
Deionized (water)
Data Quality Indicators
U.S. Environmental Protection Agency
Environmental Technology Verification
Feet per second
Square foot (feet)
Gallons
Grams per cubic centimeters
Grams per liter per gram (of grout)
Gallon(s) per minute
Generic Protocol
Hour(s)
Inch(es)
Kilogram(s)
Kilogram(s) per square centimeter
Kilogram(s) per cubic meter
Liter
Pounds
Minute(s)
National Risk Management Research Laboratory
Meter(s) per second
Cubic meters
Milligram(s) per liter
Milliliter(s)
Millimeter(s)
MegaPascal(s)
NSF International
Pounds per cubic foot
Pounds per square inch
Quality assurance
Quality control
Relative Percent Difference
Temperature of 23°C ±2°C and relative humidity of 50% ±5%
Testing Organization
Verification Organization (RTI & NSF)
Verification Test Plan
Water Quality Protection Center
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ABSTRACT
Municipalities are discovering rapid degradation of infrastructures in wastewater collection and
treatment facilities due to infiltration of leaking water from the surrounding environments.
Rehabilitation of these facilities by in situ methods, including the use of grouting, is used to
return structures to their original working conditions. Grouting is the most widely used leak-
control method in small to large wastewater treatment plants and other collection systems.
Application of grouts to leaking joints is considered a challenge, and performance must be
evaluated using model tests representing close to actual field conditions. The grout used for
repairs must be durable enough to withstand the effect of the severe physical and chemical
environmental conditions to which it will be subjected to during the service life.
This verification evaluated Warren Environmental 301-04 grouting material under laboratory
conditions at the Center for Innovative Grouting Materials and Technology (CIGMAT)
Laboratories at the University of Houston. Testing was conducted on grout and grouted sand
over a period of 6 months to evaluate performance under various simulated physical and
chemical environments. Grout was characterized based on setting time, unit weight, and leaching
of organics in water by performing a series of tests. The grout behavior was characterized based
on the unit weight, water absorption, shrinkage, permeability, compressive strength, wet-dry
cycle, and chemical resistance tests. The compressive strength of grout was determined for a
period up to a month of curing time. Also, the changes in length, diameter, volume, and weight
of the grouted sand were studied in up to 10 wet-dry cycles. Finally, two model tests were
performed to determine the effectiveness of grouting in reducing the leakage at the joints.
Testing resulted in the following observations for Warren Environmental's 301-04 grout:
• Model tests showed that grouting with 301-04 significantly reduced or eliminated the
leak in a simulated one-inch open joint (0 to 19.3 gallons/87.7 liters/day water leaks at 5
psi/0.35 kg/cm2 water pressure) immediately after grouting, and after two wet and dry
cycles over period of 1 month (0 to 16.2 gallons/73.6 liters/day water leaks at 5 psi/0.35
kg/cm2 water pressure). Prior to grouting all of the water leaked out of the open pipe
joint.
• The setting time of the grout at room temperature (70°F/21°C) varied from 38 to 40
minutes. The average unit weight of the solid grout was 62.6 pcf (l.OOg/cm3). The
average total organic content (TOC) in the leaching water was 0.0017 g/L/g of grout.
• During the water absorption test (under saturated conditions), the weight change in the
specimens varied from 0.09% to 0.17%, with an average of 0.14%. The volume change in
the specimen varied from 0.03% to 0.05%, with a mean of 0.04%.
• The shrinkage at 90% humidity and 23°C temperature after 28 days of testing resulted in
an average weight and volume change of 0.03% and 0.01%, respectively.
• The grout was impermeable under a hydraulic gradient of 100.
• The average strength, failure strain, and initial modulus after 3 days of curing were 6,591
psi (463 kg/cm2), 9%, and 225,000 psi (1,5819 kg/cm2), respectively. The average
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strength, failure strain, and initial modulus after 28 days of curing were 6,180 psi (434
kg/cm2), 5%, and 195,000 psi (13,709 kg/cm2), respectively.
• After the tenth wet-dry cycle, the average change in weight, length, diameter, and volume
was 0.25%, -0.41%, 0%, and -0.41%, respectively. The unit weight of the specimens
increased by 0.99%. The average strength of the grout after 10 wet-dry cycles was 6,531
psi (459 kg/cm2); hence, the specimen strength was not affected after 10 wet-dry cycles.
• After 6 months in a pH =2 solution (acid), the average change in unit weight and volume
was -0.31% and 1.70%, respectively. After 6 months in a pH =7 solution (neutral tap
water), the average change in unit weight and volume was 0.77% and 0.47%,
respectively. After 6 months in a pH =10 solution (base), the average change in unit
weight and volume was 0.79% and 0.47%, respectively.
• The bonding strength for water cured grout-concrete specimens did not vary significantly
over a 6-month exposure period, with average strengths ranging from 257 to 280 psi
(18.0 to 19.7 kg/cm2); most of the specimen failures were Type 1 (substrate), with others
being Type 4 (substrate failure with the grout intact).
• After 6 months of the grout-substrate test, following 10 wet-dry cycles, the average
bonding strength was 233 psi (16.4 kg/cm2), and all (100%) of the failures were Type 1
(see Appendix C for illustrations of failure types).
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Section 1
Introduction
1.1 ETV Purpose and Program Operation
The U.S. Environmental Protection Agency (EPA) created the Environmental Technology
Verification (ETV) Program to facilitate the deployment of innovative or improved
environmental technologies through performance verification and dissemination of information.
The ETV Program's goal is to further environmental protection by substantially accelerating the
acceptance and use of innovative, improved, and more cost-effective technologies. ETV seeks to
achieve this goal by providing high-quality, peer-reviewed data on technology performance to
those involved in the design, distribution, permitting, purchase, and use of environmental
technologies.
ETV works in partnership with recognized standards and testing organizations (TOs);
stakeholder groups that consist of buyers, vendor organizations, consulting engineers, and
regulators; and the full participation of individual technology developers. The program evaluates
the performance of innovative technologies by developing test plans that are responsive to the
needs of stakeholders, conducting field or laboratory tests (as appropriate), collecting and
analyzing data, and preparing peer-reviewed reports. All evaluations are conducted in
accordance with rigorous quality assurance (QA) protocols to ensure that data of known and
adequate quality are generated and that the results are defensible.
In cooperation with EPA, NSF International (NSF) operates the Water Quality Protection Center
(WQPC), two of six centers under ETV. The WQPC has developed verification testing protocols
and generic test plans that serve as templates for conducting verification tests for various
technologies. Verification of the Warren Environmental 301-04 Epoxy grout was completed
following the Generic Test Plan for Verification of Grouts for Wastewater Collection Systems,
2009 (henceforth referred to as the Generic Test Plan). The Generic Test Plan (GTP) was used to
develop a product-specific verification test plan (VTP) for the Warren Environmental 301-04
Epoxy grout.
1.2 Roles and Responsibilities
This section defines the participants in this technology verification and their roles and
responsibilities.
1.2.1 Verification Organization (RTI International and NSF International)
The Verification Organization (VO) for verifications conducted under this test plan is RTI
International (RTI) and NSF. The primary responsibilities of the VO are the following:
• Coordinate with the Center for Innovative Grouting Materials and Technology
(CIGMAT), the TO, and the Vendor to prepare and approve a product-specific test plan
using the GTP as a template and meeting all testing requirements included herein;
• Coordinate with the EPA WQPC Project Officer to approve the VTP prior to the
initiation of verification testing;
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• Review the quality systems of the TO and, subsequently, qualify the TO;
• Oversee the grout evaluations and associated laboratory testing;
• Review data generated during verification testing;
• Oversee the development of a verification report;
• Provide QA oversight at all stages of the verification process.
Primary contacts: Mr. Richard Marinshaw
RTI International
3040 Cornwall! s Road
Research Triangle Park, NC 27709
Phone: 919-316-3735
Email: rjmarinshaw@rti.org
Mr. Thomas Stevens
NSF International
789 North Dixboro Road
Ann Arbor, MI 48105
Phone: 734-769-5347
Email: stevenst@nsf.org
1.2.2 U.S. Environmental Protection Agency (EPA)
This report has been funded and overseen by the EPA's Office of Research and Development
(ORD). The ETV Program's QA Manager and the WQPC Project Officer provided
administrative, technical, and QA guidance and oversight on all ETV WQPC activities and
reviewed and approved each phase of the verification project. The primary responsibilities of
EPA personnel were the following:
• Review and approve the VTP, including the test/quality assurance plans (T/QAPs);
• Sign the VTP signoff sheet;
• Review and approve the verification report and verification statement; and
• Post the verification report and verification statement on the EPA ETV Web site.
Primary contact: Mr. Ray Frederick
U.S. Environmental Protection Agency, National Risk Management
Research Laboratory
Project Officer, Water Quality Protection Center
2890 Woodbridge Ave. (MS-104)
Edison, New Jersey 08837
Phone: 732-321-6627
Email: frederick.ray@epamail.epa.gov
1.2.3 Testing Organization (CIGMAT Laboratories at the University of Houston)
The TO for verifications conducted under this test plan is CIGMAT Laboratories at the
University of Houston. The primary responsibilities of the TO are the following:
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• Coordinate with the VO and Vendor relative to preparing and finalizing the VTP;
• Sign the VTP signoff sheet;
• Conduct the technology verification in accordance with the VTP, with oversight by the
VO;
• Analyze all samples collected during the technology verification process, in accordance
with the procedures outlined in the VTP and referenced Standard Operating Procedures
(SOPs);
• Coordinate with and report to the VO during the technology verification process;
• Provide analytical results of the technology verification to the VO; and
• If necessary, document changes in plans for testing and analysis, and notify the VO of
any and all such changes before changes are executed.
CIGMAT supports faculty, research fellows, research assistants, and technicians. CIGMAT
personnel worked in groups to complete the tests described in the VTP. All the personnel
reported to the Group Leader and the CIGMAT Director. The CIGMAT Director was
responsible for appointing Group Leaders, who, with his approval, were responsible for drawing
up the schedule for testing. Additionally, a QA Engineer, who is independent of the testing
program, was responsible for internal audits.
Primary contact: Dr. C. Vipulanandan
University of Houston, CIGMAT
4800 Calhoun Road
Houston, Texas 77204
Phone: 713-743-4278
Email: cvipulanandan@uh.edu
1.2.4 Vendor (Warren Environmental)
The Vendor for verifications conducted under the VTP is Warren Environmental Inc. The
primary responsibilities of the Vendor are the following:
• Provide the TO with pre-grout samples for verification;
• Complete a product data sheet prior to testing;
• Provide technical support, as required, during the period prior to the evaluation; and
• Provide technical assistance to the TO during verification testing period, as requested.
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Primary contact: Ms. Jane Warren
Warren Environmental, Inc.
P.O. Box 1206
Carver, MA 02330
Phone: 508-4947-8539
Email: jane@warrenenviro.com
1.3 Background and Technical Approach
The University of Houston/CIGMAT researchers have been investigating the performance of
various grouts for use in wastewater facilities. Performance of grouts has been studied from
setting to injection into various soils. The studies have been focused on (1) developing and
characterizing grouts for various applications; (2) behavior of grout-concrete substrate under
various environmental conditions; and (3) model verification of various grout applications. The
data collected on various grouts can further help engineers and owners to better understand the
durability of grout materials in wastewater environments.
The overall objective of this study was to systematically evaluate a grout material used in
rehabilitation of cracked concrete to control leakage. Specific testing objectives are to:
• Evaluate the effectiveness of the grout to control leakage at a simulated cracked concrete
structure; and
• Determine the relevant grout properties.
Testing was done according to CIGMAT standards. The grout manufacturer was responsible for
grouting the leaking lateral joints under the guidance of CIGMAT staff members. The grout and
grouted sand specimens were evaluated over a period of 6 months.
1.4 Test Facility
The testing was performed in the CIGMAT Laboratories at the University of Houston, Houston,
Texas. The CIGMAT Laboratories are located in the Central Campus of the University of
Houston at 4800 Calhoun Road.
The CIGMAT Laboratories and affiliated facilities are equipped with devices that can perform
all of the grouting tests described in this report. Molds are available to prepare the specimens for
testing, and all the grout and grouted sand test procedures are documented in SOPs.
1.5 Objectives
The objective of this study was to evaluate Warren Environmental 301-04 Epoxy grout for use in
controlling leaks in cracked concrete. Specific objectives are as follows:
• Determine the working properties of the grout material;
• Determine the physical and mechanical properties of the grout material over a period of
time and exposure conditions;
• Evaluate the grout-substrate interaction over a period of 6 months; and
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• Determine the effectiveness of the test grout for controlling leaks in cracked concrete
over a period of time.
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Section 2
Grout Material Description
The grout material evaluated in this verification was the M-301 Epoxy Trowel-On Mastic
System Grout from Warren Environmental. The grout is described on the Warren Environmental
Inc. Web site (http://www.warrenenviro.com/pdf/301-04.pdf) as a two-part, highly thixotropic
(becomes fluid when stirred or shaken) epoxy system formulated specifically for trowel-on
applications.
Based on the information provided by the supplier, 301-04 Epoxy Grout can be used for sealing
leaks in sewer pipe joints, and can also be used to control water seepage in cracks and joints in
subgrade concrete structures. The grout was formulated with special additives and modifiers to
enhance water and chemical resistance, and bond strength to a variety of substrates, as well as its
own internal strength. The high thixotropic index allows for build-ups of up to % in. on vertical
surfaces without sag. It has been designed to be applied to a clean surface free of standing water
with a notched (toothed) trowel similar to stucco. Alternately, it may be applied using heated
tanks, heated lines, and Warren Environmental Inc.'s patented meter, mix, and spray equipment.
This epoxy system utilizes a 2 parts base-to-1 part activator mix ratio by volume. This product is
sold and installed only by technicians specifically trained and licensed in the manufacturer's
patented techniques.
The cured 301-04 epoxy grout is white in color, as shown in Figure 2-1.
Figure 2-1. 301-04 Epoxy grout specimen.
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Section 3
Methods and Test Procedures
The testing involved characterization of grout material and bonding strength to concrete. In
addition, model tests were performed to determine the effectiveness of grouting in controlling
leakage at a horizontal joint. The following is a summary of the methods and test procedures
used in this verification.
3.1 Grout Evaluation
Properties of the grout specimen samples tested are grouped as follows:
• Working properties;
• Physical and mechanical properties;
• Durability properties; and,
• Environmental properties.
More details on the tests are summarized in Tables 3-1 and 3-2.
Since there were no American Society of Testing and Materials (ASTM) test procedures to
determine the grout properties, CIGMAT developed their own testing protocols, which were
used in these evaluations.
3.1.1 Grout Specimen Preparation
3.1.1.1 Grout Specimens
Figure 3-1 shows the mold utilized to make the grout test specimens. Specimens were prepared
with a resin-to-water ratio of 9:1. Specimens were cured under room conditions. After
solidification, specimens were removed from the mold and stored in labeled, sealed plastic bags
for identification, protection, and to prevent moisture loss. The specimens were stored in a
temperature- and humidity-controlled room at 23 ± 2°C (room temperature) and 50% ± 5%
humidity.
PVC
Model
Grout
1.5 in.
Figure 3-1. Typical mold used for preparing grout specimens.
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Table 3-1. Grout Tests for Concrete Leak Repair
Properties
Working
Properties
Physical and
Mechanical
Properties
Durability
Properties
Environmental
Properties
Tests
Setting (Gel)
Time
Unit Weight
Water
Absorption
Shrinkage
Permeability
Compressive
Strength
Wet-Dry Cycle
Chemical
Resistance
Leaching
Conditions
23°C
23°C
23°C
Temp, humidity
Water
3, 7, 28 days
Number of cycles
pH = 2, 7, 10
Water
Test Method Used
Method defined in
Section 3.1.2.
CIGMATGR1-04
CIGMAT GR 3-04
Method defined in
Section 3.1.2
CIGMAT GR 7-04
CIGMAT GR 2-04
CIGMAT GR 3-04
CIGMAT CH 2-04
Method defined in
Section 3.1.2
#of
Specimens
Tested
6
25
3
3
3
11
3
9
3
Table 3-2. Grout-Substrate Interaction Tests
Materials
Tests
Conditions
Grout-Substrate Interaction
Bonding
Strength
Wet condition
Wet-dry cycle
Concrete brick
cured under water
Number of cycles
Test Method Used
CIGMAT CT 3 -00
CIGMAT GR 3 -04 &
CIGMAT CT 3 -00
Number of
Specimens
Tested
12
3
3.1.1.2 Grout-Substrate Interaction Specimens
Although CIGMAT CT 3-00 was developed for coating materials, it can be adopted for grouts.
As described in CIGMAT CT 3-00, the grout was sandwiched between a pair of rectangular
concrete block specimens and then tested for bonding strength and type of failure. Even though
CIGMAT CT 3-00 specifies the use of dry bricks, for the purposes of this grout evaluation, wet
specimens were used to simulate extreme grouting conditions. The bonded wet specimens were
immersed in water until tested. The reported data include the number of specimens tested; the
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age of specimen at the time of the test; the average bond strength with standard deviation; and
the types of failures.
3.1.2 Grout Curing Properties
3.1.2.1 Setting (Gel) Time
No ASTM standard method is currently available to determine the gel time for epoxy grouts.
Hence, it was determined by the elapsed time from grout preparation until the grout no longer
flowed from a plastic cup or beaker inclined slowly (so that if the cup/beaker were filled with
liquid, the surface of the liquid would remain level) to 45 degrees. Approximately 50 mL of
freshly prepared grout was used. At periodic intervals, based on the observed setting of grout, the
container was slowly tipped to approximately 45 degrees to determine if the grout exhibited
liquid-flow properties, or if the grout sample had gelled and the specimen could longer flow from
the container. A total of six replicate samples of grout were analyzed.
3.1.2.2 Physical and Mechanical Properties
To obtain initial characterization information on the grout, all specimens were weighed to 0.1 g
using a calibrated digital balance and measured (diameter and height) using a vernier caliper with
a least count of 0.01 mm.
3.1.2.3 Unit Weight (Density)
Solidified grout specimens were used to determine the unit weight of the grout. The
determinations were completed per CIGMAT GR 1-00 for grout specimens. Unit weights were
calculated using the weight and volume of the specimens. Three replicates were evaluated for
unit weight.
3.1.2.4 Water Absorption
Water absorption characteristics were evaluated for grout specimens as outlined in standard
procedure CIGMAT GR 3-04. Three grout specimens were immersed in tap water (initial pH in
the range of 7), and changes in the weight and volume (determined by measuring specimen
diameter and height) of the specimens were recorded a minimum of once every working day
(Monday through Friday, excluding holidays) until the changes in weight and volume became
negligible (less than 0.5 percent of the previous weight and volume), or for 1 week, whichever
occurred first.
3.1.2.5 Shrinkage
The specimens were placed in zip lock bags and held at room temperature. Humidity was
measured using a digital humidity meter. At the onset of the test, specimens were prepared in a
mold with inner dimensions of 1.5 in. (38 mm) in diameter and 3.5 in. (90 mm) in length. Three
specimens were tested under the selected test conditions. The weight and dimensions of the
specimens were measured before and after the test. The testing conditions are summarized in
Table 3-3 and were selected based on the manufacturer's recommendation.
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Table 3-3. Shrinkage Test Conditions
Parts
PartC
Temperature, Duration, and Storage Condition
23°C ± 2°C for 28 days in zip lock bags (RH = 90%+ 5%)
3.1.2.6 Permeability
Solidified grout specimens were used to determine the grout's permeability. Specimens were
prepared in 1.5 in. (33 mm) diameter Plexiglas/glass cylinders and permeated with water under a
hydraulic gradient of 100, per CIGMAT GR 7-02. Testing of three replicate samples was
completed at room temperature and humidity.
3.1.2.7 Unconfined Compressive Strength and Stress/Strain Relationship
CIGMAT GR 2-02 was developed for testing grout specimens in compression under
monotonically (linearly) increasing load. Compression tests were performed using screw-type
machines. The specimens were trimmed to ensure smooth and parallel surfaces. Several
specimens were tested at 3, 7, and 28 days following specimen preparation. The reported data
include the compressive strength, modulus, and failure strain. The modulus was determined from
the initial slope of the stress/strain relationship, and the failure strain was the maximum strain
before the specimen fails.
3.1.3 Durability Properties
3.1.3.1 Wet/Dry Cycle
During its service life, the grout could be subjected to a number of wet/dry cycles. This test was
designed to determine the impact of repeated wetting and drying on the performance of grouts.
Three replicate specimens were used for this test. The specimens were subjected to 10 wet/dry
cycles for a total test time of 140 days, or until failure (specimen completely deteriorated). One
wet/dry cycle was 14 days in duration, consisting of 7 days of water exposure followed by 7 days
of dry conditions at room temperature and humidity (23 + 2°C and 50% + 5% relative humidity
[RH]). The water exposures were completed as described in Section 11 of CIGMAT GR 3-04,
using tap water having a pH of approximately 7. Changes in length, diameter, weight, and
volume of the specimens were measured daily. At the end of the 10 wet/dry cycles, the
specimens were tested to determine the compressive strength of the grout.
3.1.3.2 Chemical Resistance
This test evaluates the resistance of grouts when exposed to chemical conditions representing
various environmental applications. The test results help when selecting suitable grouts for use in
various chemical environments. A total of nine grout specimens were prepared, and the initial
weight, dimensions, color, and surface appearance of the specimens were recorded. Three
specimens at each pH were fully immersed in solutions, with pH 2, 7, and 10 maintained at room
temperature (23 + 2°C) for the entire exposure period. The solutions consisted of tap water, with
hydrochloric acid or sodium hydroxide added to achieve the pH required for the tests. The
weight and volume change were determined and recorded for three specimens at each pH after
30, 90, and 180 days, as described in Section 7.3 in CIGMAT CH 2-01. After each evaluation,
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compression testing was completed on the specimens in accordance with Section 7.4 of
CIGMATCH2-01.
3.1.4 Environmental Properties—Leaching Test
Potential contaminant leaching from solidified grout was determined by analyzing water exposed
to the grout for total organic carbon (TOC). Lead is an issue with inorganic grout, but is not an
issue with the proposed grout, so no lead evaluation was required. Three test replicates, using
cylindrical grout specimens, were exposed to tap water in individual exposure jars for 7 days.
One blank container containing only the exposure water was prepared and held under the same
conditions as the specimen exposure jars.
The test was conducted with three grout specimens and water volume so that there was an
adequate volume exposed to water to conduct the required analyses. A liquid-to-solid ratio of 1:1
(by volume) was used.
At the end of the exposure period, samples of the exposure water were analyzed to determine the
presence of organic compounds that may have leached out from the grout. The samples were
analyzed for TOC.
Details of the analytical methods, required sample volumes, and sample holding are summarized
in Table 3-4
Table 3-4. Handling Methods and Analyses for Collected Samples
Analysis
TOC
Method1
SM5310
(B or C)
Bottle Type and Size
Glass, two 40-mL
bottles
Preservation,
Holding Time
Cool to 4°C, pH<2
HNOs, 6 months
Reporting
Detection Limit
1 mg/L
1 Standard Methods for the Examination of Water and Wastewater, 20th Edition
3.2 Grout-Substrate Bonding Strength
Interaction between the grout and a concrete substrate was evaluated by testing the bonding
strength and type of failure (i.e., bonding failure, substrate failure, or a combination) under
different service conditions. Testing of wet grout/concrete substrate specimens was conducted
over a period of 6 months, in accordance with CIGMAT CT 3-00 (over the grouted area between
the concrete bricks/prisms, as selected by the vendor prior to the ETV verification. In addition,
bonded configurations prepared according to CIGMAT CT 3-00 were also subjected to wet/dry
cycle test.
3.3 Model Test
For this study, Warren Environmental Inc. selected the model test related to leak control in
cracked concrete.
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3.3.1 Model Test: Concrete Leak Repair
In order to simulate a leak in a concrete structure, this model test (Figure 3-2) uses 10 in. (25
cm) diameter circular concrete disks with 6 in. (15 cm) openings at the center (each disk is
donut-shaped). The two disks were placed lin. apart and the opening was grouted by the vendor.
After the vendor-specified curing period, the grouted joint was subjected to hydrostatic pressure
testing to determine the leak rate, as outlined in Section 3.3.2.
3.3.2 Model Test Procedures
The grouted concrete disks were subjected to the following test procedures:
1. Apply hydrostatic pressure of 3 psi (0.21 kg/cm2) and hold for 5 minutes; then measure the
leak rate using a graduated cylinder and a stopwatch.
2. Repeat Step 1 at a hydrostatic pressure of 4 psi (0.28 kg/cm2).
3. Repeat Step 1 at a hydrostatic pressure of 5 psi (0.35 kg/cm2).
4. Maintain saturated conditions for a period of 1 week by soaking the joint with water.
5. Drain all water from the test chambers and allow them to stand for 1 week.
6. Fill the chambers with water and repeat Step 4.
7. Repeat Step 5.
8. Determine leak rates as described in Steps 1 through 3.
The reported data include the characteristic leak rate versus pressure for each grouted joint.
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Supporter
Concrete Ring
1 in.
Steel Pipe
(a) Elevation View
Grout
o
o
1
1
1
10 in.
i
O
o
(b) Plan View
Figure 3-2. Model configuration for testing concrete leak repair.
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Section 4
Results and Discussion
As previously described in Section 3, a series of tests were completed on the Warren
Environmental 301-04 Epoxy grout to characterize the material and provide information on how
the grout will perform under various conditions of applications. Grout specimens were tested to
identify their working properties, physical and mechanical properties, durability properties, and
environmental properties. In addition, tests were completed to evaluate the grout/substrate
interaction. The results of these tests are presented in this section.
4.1 Grout Properties
4.1.1 Working Properties
The working properties describe the basic characteristics of the grout material and also help with
establishing quality control (QC) procedures for various types of field applications.
4.1.1.1 Viscosity
This is a typical descriptive of the flow characteristics of a grout material. However, as the grout
was a solid at room temperature, the viscosity test was not performed.
4.1.1.2 Setting (Gel) Time
The setting time testing was performed at room temperature and humidity. A total of six samples
were tested, and the results are summarized in Table 4-1. Setting time varied from 38 to 40
minutes, with an average of 39 minutes. The setting time will control the installation time for the
grout.
4.1.1.3 Unit Weight (Density)
A total of 25 cylindrical specimens were tested, and the results are summarized in Table B-2 of
Appendix B. The grout unit weight varied from 0.91 to 1.09 g/cm3, with an average of 1.00
g/cm3, the unit weight of water. The unit weight of the grout could be used as a quality control
measure in the field and will also help with the estimation of changes in weight due to the leak
repairs.
Table 4-1. Summary of Working Properties of Epoxy Grout
Test Completed
Setting Time (min)
Unit Weight (g/cm3)
Number of
Specimens
6
25
Range
38-40
0.91-1.09
Mean
39.5
1.00
Standard
Deviation
0.84
0.05
cv
0.02
0.05
4.2 Physical and Mechanical Properties
4.2.1 Water Absorbance
The water absorption is a representation of the water-diffusion characteristics of the grout. A
total of three specimens were tested, and the results are summarized in Table 4-2. The weight
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change in the three specimens varied from 0.09% to 0.17%, with an average of 0.14%. The
volume change in the specimen varied from 0.03% to 0.06%, with a mean of 0.04%.
Table 4-2. Results of Water Absorption
Exposure
Time
(days)
0
1
2
3
4
Specimen 41
Density
(g/cm3)
0.98
0.98
0.98
0.98
0.98
AW
(%)
0.08
0.15
0.15
0.15
AV
(%)
0.03
0.03
0.05
0.05
Specimen 42
Density
(g/cm3)
0.98
0.98
0.98
0.98
0.98
AW
(%)
0.17
0.17
0.17
0.17
AV
(%)
0.03
0.03
0.03
0.05
Specimen 43
Density
(g/cm3)
0.99
0.99
0.99
0.99
0.99
AW
(%)
0.09
0.09
0.09
0.09
AV
(%)
0.03
0.06
0.06
0.03
4.2.2 Shrinkage Test
A total of three specimens were tested for 28 days. The weight change varied from 0 to 0.09%,
with an average value of 0.06%. The volume change varied from 0 to 0.04%, with an average of
0.01%.
4.2.3 Permeability
Grout specimens that were cured for a period of 7 days were tested for permeability under a
hydraulic gradient of 100. Three specimens were tested, with no observed discharge from any of
the three specimens over the 72 hour test period the gradient was applied. Hence the permeability
of the grout was zero. The results of the test are summarized in Appendix B, Table B-5.
4.2.4 Compressive Strength and Stress-Strain Relationship
The compressive properties (i.e., strength, failure strain, and initial modulus) were measured
over a period of 30 days. A total of 11 specimens were tested, and the results are summarized in
Table 4-3. The average strength, failure strain, and initial modulus after 3 days of curing were
6,591 psi (463 kg/cm2), 9%, and 225,000 psi (15,819 kg/cm2), respectively. The average
strength, failure strain, and initial modulus after 28 days of curing were 6,180 psi (434 kg/cm2),
5%, and 195,000 psi (13,709 kg/cm2), respectively. The complete set of data for this test is
included in Appendix B, Table B-6
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Table 4-3. Summary of Compressive Strength Properties with Curing Time
Number of
Specimens
3
O
5
Cure
Time
(days)
3
7
28
Compressive
Strength
(psi)/(kg/cm2)
Average
6,591
463
6,402
450
6,180
434
Range
6,105-
7,356
429-517
5,304-
7,592
372-533
5,451-
7,022
383-493
Failure Strain
(%)
Average
9
5
5
Range
8-10
3-7
4-5
Avg. Initial Modulus
(psi)/(kg/cm2)
Average
225,000
15,819
227,000
15,959
195,000
13,709
Range
200,000-
250,000
14,061-17,576
215,000-240,000
15,116-16,873
165,000-225,000
11,600-15,819
4.3 Durability Properties
4.3.1 Wet-Dry Cycles
A total of three specimens were tested for 10 wet-dry cycles. Initial weights and dimensions
(length and diameter) were measured and the cycles started with a 1-week wet cycle followed by
a 1-week dry cycle. The changes in weight, length, diameter, and volume were determined
following each wet-dry cycle and are reported in Table 4-4. After the first wet-dry cycle, the
average change in weight, length, diameter, and volume was 0.04%, -0.25%, 0%, and -0.25%,
respectively. The unit weight of the specimens increased over time, while the length of the
specimens decreased. After the tenth wet-dry cycle, the average change in weight, length,
diameter, and volume was 0.25%, -0.41%, 0%, and -0.41%, respectively. The unit weight of the
specimens increased. The average strength of the grout after 10 wet-dry cycles was also
determined and found to be an average of 6,531 psi (459 kg/cm2), approximately equal to the 3-
day compressive strength of the grout, as shown in Table 4-3. The complete data set for these
tests are included in Appendix B, Tables B-7.1 and B-7.2
Table 4-4. Wet-Dry Cycle Test Results
Cycle Number
(i)
1
2
3
4
5
Avg AW ®
(%)
0.04
0.13
0.17
0.13
0.25
Avg A L 0
(%)
-0.25
-0.36
-0.41
-0.41
-0.41
Avg A D
(%)
0.00
0.00
0.00
0.00
0.00
Avg A V 0
(%)
-0.25
-0.36
-0.41
-0.41
-0.41
Avg Density ®
(g/cm3)
0.99
0.99
0.99
0.99
0.99
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Cycle Number
(i)
6
7
8
9
10
Avg AW
(%)
0.30
0.39
0.26
0.25
0.25
Avg A L 0
(%)
-0.41
-0.41
-0.36
-0.37
-0.41
Avg A D
(%)
0.00
0.00
0.00
0.00
0.00
Avg A V 0
(%)
-0.41
-0.41
-0.36
-0.37
-0.41
Avg Density ®
(g/cm3)
0.99
0.99
0.99
0.99
0.99
(1) One cycle consists of 7 days of water exposure, followed by 7 days of dry exposure.
(2) Average value represents conditions at the end of the cycle, compared with the initial condition.
4.3.2 Chemical Resistance.
A total of nine specimens were tested for a period of 6 months. The initial weights and
dimensions of the specimens were determined, and three specimens were exposed to each of
solution of pH 2, 7, and 10. The test results are summarized in Table 4-5, and presented in
Appendix B, Table B-8
pH= 2 solution: After one month, the average change in weight, volume, and unit weight was
0.32%, 0.59%, and -0.27%, respectively After 6 months, the average change in weight, volume,
and unit weight was 1.38%, 1.70%, and -0.31%, respectively. The weight and volume increased
over the 6-month period.
pH= 7 (tap water): After one month, the average change in weight, volume, and unit weight was
0.29%, 0.11%, and 0.18%, respectively After 6 months, the average change in weight, volume,
and unit weight was 1.24%, 0.47%, and 0.77%, respectively. The weight and volume increased
over the 6-month period, as did the unit weight.
pH= 10 solution: After one month, the average change in weight, volume, and unit weight was
0.42%, -0.06%, and 0.48%, respectively After 6 months, the average change in weight, volume,
and unit weight was 1.24%, 0.47%, and 0.79%, respectively. The weight and volume increased
over the 6-month period, as did the unit weight.
Table 4-5. Chemical Resistance Test Results.
Exposure
Time
(days)
Weight
(g)
Avg
%
Chg
Length
(mm)
Avg
%
Chg
Diameter
(mm)
Avg
%
Chg
Volume (cm3)
Avg
%
Chg
Density
(g/cm3)
Avg
%
Chg
pH2:
0
30
90
180
102.9
103.2
104.0
104.3
0.32
1.06
1.38
95.08
94.95
94.90
95.27
-0.14
-0.20
0.18
36.16
36.29
36.34
36.43
0.37
0.52
0.76
97.61
98.18
98.40
99.23
0.59
0.83
1.70
1.06
1.05
1.06
1.05
-0.27
0.23
-0.31
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Exposure
Time
(days)
Weight
(g)
Avg
%
Chg
Length
(mm)
Avg
%
Chg
Diameter
(mm)
Avg
%
Chg
Volume (cm3)
Avg
%
Chg
Density
(g/cm3)
Avg
%
Chg
pH7:
0
30
90
180
104.7
105.0
105.9
106.0
0.29
1.15
1.24
96.74
96.83
96.89
96.95
0.09
0.15
0.21
36.30
36.30
36.30
36.34
0.01
0.01
0.13
100.10
100.22
100.28
100.57
0.11
0.17
0.47
1.05
1.05
1.06
1.05
0.18
0.98
0.77
pHIO:
0
30
90
180
98.4
98.8
99.5
99.6
0.42
1.19
1.24
91.22
91.38
91.45
91.60
0.17
0.26
0.40
36.28
36.23
36.20
36.29
-0.12
-0.21
0.03
94.20
94.16
94.09
94.75
-0.06
-0.16
0.47
1.04
1.05
1.06
1.05
0.48
1.35
0.79
4.4 Environmental Properties—Leaching Study
A total of three specimens, of equal volumes and approximately equal weights, were exposed in
an equal volume of tap water and the total organic carbon (TOC) was determined in each sample
to measure the leaching of chemicals from the grout. The results found from 0.057 to 0.185 g of
TOC/L, which translated to 0.0007 to 0.0023 g TOC/L/g grout, with a mean of 0.0017 g/L/g.
The test results are reported in Appendix B, Table B-9. These data should be considered
estimated values because of data uncertainty arising from incomplete QA/QC, as discussed in
Section 5.4.
4.5 Grout/Substrate Interactions
The interaction between the grout and a concrete substrate was determined using prepared
concrete bricks to which the grout was applied to form a sandwich, which was cured for varying
lengths of time to demonstrate the cure time relationship between the concrete and the grout.
Four sandwich specimens were evaluated at each of 30, 90 and 180 days following water curing,
and three were evaluated after 180 days of wet-dry cycle curing. The cured specimens were
tested on a load frame to determine the break strength of the grout-brick bond. The break type
was evaluated to determine where the failure occurred, as described in Table C-l in
Appendix C.
The failures observed in the specimens were all either Type 1 (i.e., a concrete brick failure,
where the grout brick bond is intact) or a Type 4 (i.e., a bonding and substrate failure, where the
brick fails at location of the applied grout, but the grout material remains intact). Figure 4-1
shows the brick/grout specimen prior to testing, while Figure 4-2 shows a typical Type 1 failure.
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Concrete
Brick
Epoxy
Grout
Figure 4-1. Sandwiched specimens for bonding test
(Warren Environmental 301-04 epoxy grout).
Figure 4-2. Typical failed specimen (Type 1 failure pattern).
The results of the bonding tests are presented in Figure 4-3 and Table 4-6, with a more complete
description of the results provided in Appendix C.
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00
130 Day Exposure
190 Day Exposure
180 Day Exposure
1180 Day Exposure
- Wet/Dry Cycles
Exposure Time
Note: Number at top of bars indicates the type of failure - 1 is a substrate (concrete block) failure,
4 is a bonding and substrate failure.
Figure 4-3. Results of grout-substrate bonding test.
Table 4-6. Summary of Bonding Strength Tests (CIGMAT CT-3)
Exposure
Time
(days)
30
90
180
Exposure
Conditions
Water
Water
Water
Wet-Dry
Cycles
Failure Type 1 - Number of Failures
1
3
2
3
3
2
3
4
1
2
1
5
Failure Strength
(psi)/(kg/cm2)
Range
228-288
16.0-20.2
247-304
17.4-21.4
204-329
14.3-23.1
204-278
14.3-19.5
Average
260
18.3
280
19.7
257
18.1
233
16.4
See Table C-l.
4.6 Model Test
Two replicate model tests were completed to simulate a leak repair for a concrete structure.
Figure 4-4 (a) shows the defect created for evaluation of the grout for a concrete repair. The
concrete rings were separated by spacers to create an open joint through which all of the water
(100%) leaked out. The grout was placed within the ring space (Figure 4-4 (b)) by the grout
supplier and was allowed cure before testing was initiated.
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/
(a) Simulated cracked concrete. (b) Repaired cracked concrete with epoxy grout.
Figure 4-4. Model test set up (a) Cracked concrete and (b) After grout repair.
Figure 4-5. Model 4 test setup.
After the grouted joint had cured, the joint was placed in a Plexiglas chamber (Figure 4-5),
which was sealed to allow water to completely surround the grouted joint. Hydrostatic pressures
of 3, 4, and 5 psi (0.21, 0.28 and 0.35 kg/cm2) were applied through the inlet to the Plexiglas
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enclosure for 5 minutes at each pressure, and the water leaking through the grouted joint was
collected and recorded. After two wet-dry cycles, the hydrostatic pressure tests were repeated.
The results of the model tests are summarized in Table 4-7. The model tests showed that the
grouting with 301-04 was effective in significantly reducing or eliminating the leak in the
cracked concrete (0 to 19.3 gallons/87.7 liters/day water leaks at 5 psi/0.35 kg/cm2 water
pressure) immediately after grouting and after two wet and dry cycles over period of one month
(0 to 16.2 gallons/73.6 liters/day water leaks at 5 psi/0.35 kg/cm2 water pressure).
Table 4-7. Model Test 4 Leak Rate Results (gallons/day)/(liters/day)
Hydrostatic
Pressure (psi)
O
4
5
Replicate 1
Initial
Condition
11.5/52.3
13.9/63.2
19.3/87.7
Wet-Dry Cycle
Condition
7.6/34.5
12.6/57.2
16.2/73.6
Replicate 2
Initial
Condition
0.0
0.0
0.0
Wet-Dry Cycle
Condition
0.0
0.0
0.0
4.5 Summary of Observations
Combinations of laboratory tests, including two model tests, were performed over a six-month
period with Warren Environmental 301-04 Epoxy Grout to determine its effectiveness in
controlling leaks. Findings of the tests include:
• Model tests showed that the grouting with 301-04 was effective in significantly reducing
or eliminating the leak in an open joint (0 to 19.3 gallons/87.7 liters/day water leaks at 5
psi/0.35 kg/cm2 water pressure) immediately after grouting, and after two wet and dry
cycles over period of one month (0 to 16.2 gallons/73.6 liters/day water leaks at 5 psi/
0.35 kg/cm2 water pressure). Before grouting, all of the applied water leaked out of the 1-
inch gap.
• The setting time of the grout at room temperature (70°F/21°C) varied from 38 to 40
minutes. The average unit weight of the solid grout was 1.00 g/cm3. The average TOC in
the leaching water of equal volume to the solid grout was 0.0017 g/L/g of grout.
• During the water absorption test, the weight change in the specimens varied from 0.09 to
0.17%, with an average of 0.14%. The volume change in the specimen varied from
0.03% to 0.05%, with a mean of 0.04%.
• The shrinkage at 90% humidity and 23°C temperature after 28 days of testing resulted in
an average weight and volume change of 0.06% and 0.01%, respectively.
• The grout was impermeable under a hydraulic gradient of 100.
• The average strength, failure strain, and initial modulus after 3 days of curing were 6,591
psi (463 kg/cm2), 9%, and 225,000 psi (15,819 kg/cm2), respectively. The average
strength, failure strain, and initial modulus after 28 days of curing was 6,180 psi (434
kg/cm2), 5%, and 195,000 psi (13,709 Kg/cm2), respectively.
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• After the tenth wet-dry cycle, the average change in weight, length, diameter, and volume
was 0.25%, -0.41%, 0%, and -0.41%, respectively. The unit weight of the specimens
increased by 0.99%. The average strength of the grout after 10 wet-dry cycles was 6,531
psi (459 kg/cm2), similar to the compressive strength at 3 days cure time.
• After six months in a pH =2 solution (acid), the average change in unit weight and
volume was -0.31% and 1.70%, respectively. After 6 months in a pH =7 solution (neutral
tap water), the average change in unit weight and volume was 0.77% and 0.47%,
respectively. After 6 months in a pH =10 solution (base), the average change in unit
weight and volume was 0.79% and 0.47%, respectively.
• The bonding strength for water cured grout-concrete specimens did not vary significantly
over a 6-month exposure period, with average strengths ranging from 257 to 280 psi
(18.0 -19.7 kg/cm2); most of the specimen failures were Type 1 (substrate), with others
being Type 4 (substrate failure with the grout intact).
After 6-months of wet-dry cycle exposure (10 cycles), the average bonding strength of grout-
concrete specimens was 233 psi (16.4 kg/cm2), with all (100%) of the failures being Type 1.
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Section 5
QA/QC Results and Summary
The Verification Test Plan (VTP) included a Quality Assurance Project Plan (QAPP) that
identified critical measurements for this verification. The verification test procedures and data
collection followed the QAPP to ensure quality and integrity. CIGMAT was primarily
responsible for implementing the requirements of the QAPP during testing, with oversight from
NSF.
The QAPP identified requirements for preparation of the concrete specimens that would be
grouted and used during the verification, along with requirements for QC indicators (i.e.,
representativeness, completeness and precision) and auditing.
5.1 Requirements for Sample Preparation
5.1.1 Specimen Preparation
For each batch of concrete made at CIGMAT to perform the laboratory tests, specimens were
tested to ensure their properties were within allowable ranges. The tests included unit weight and
pulse velocity of the concrete prism specimens. Flexural strengths were also measured, where
appropriate, to characterize the specimens. The target values for the unit weights of the
specimens were maximum or minimum value of the batch within +20% of the mean value of the
batch. The property ranges for the concrete prisms are summarized in Table 5-1.
Table 5-1. Typical Properties for Concrete Specimens
Material
Concrete
Unit Weight
(pcf)
138-149
Pulse Velocity (ft/sec)
12,600-15,800
Flexural Strength
(psi)
720-960
5.1.2 Unit Weight and Pulse Velocity
The pulse velocity and unit weight were determined for 84 and 90 concrete prisms, respectively.
For the concrete block specimens, the unit weight varied between 138 pcf ( 2212 kg/m3) and
149 pcf (2,388 kg/m3), with a mean value of 143 pcf (2292 kg/m3). The allowable range (+20%
of the mean value of the batch) is 114 pcf to 172 pcf. The concrete block specimens fell within
this range. Pulse velocities ranged from 12,600 fps (3,840 m/sec) to 15,800 fps (4,845 m/sec),
with a mean of 14,000 fps (4,367 m/sec), within the allowable range of 20% of the mean value of
the batch.
There was no direct correlation between the pulse velocity and unit weight of concrete
(Figure A-l(a)). The variation of pulse velocity was normally distributed (Figure A-l(b)).
5.1.3 Flexural Strength
While not required by the VTP, flexural strengths were determined for the concrete specimens,
under both dry and wet conditions. This information provides further assurance that the
specimens are acceptable for this verification. Two specimens each of dry and wet concrete
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cylinders were tested for flexural strength. All specimens were cured for 28 days. The average
flexural strength for the wet concrete was about 743 psi (52.2 kg/cm2) and was about 939 psi
(66.0 kg/cm2) for the dry concrete. The flexural strengths of dry and wet concrete are
summarized in Table A-l in Appendix A.
5.2 Quality Control Indicators
5.2.1 Representativeness
Representativeness of the samples during this evaluation was addressed by CIGMAT personnel
following consistent procedures in preparing specimens, having the vendor apply grouts to the
specimens, and following CIGMAT SOPs in curing and testing of the grouted specimens.
5.2.2 Completeness
The numbers of substrate and grouting specimens to be evaluated during preparation of the test
specimens, as well as the number of coated specimens to be tested during the verification, were
described in the VTP. The numbers that were completed during the verification testing are
described in this section.
5.2.2.1 Specimen Preparation
The number (per the VTP) of each specimen to be used for characterization of the substrates is
listed in Table 5-2. As there were multiple grouts being evaluated at the same time, CIGMAT
prepared a batch of specimens to be grouted in the tests. The number of specimens characterized
during preparation of the batch of specimens is indicated in parentheses for each material and
test listed in Table 5-2.
Table 5-2. Number of Specimens Used for Each Characterization Test
Material
Concrete Prisms
Number of Specimens Prepared for Use in Test
Unit
weight
90
Pulse
velocity
84
Water
absorption
None
Flexure*
4
Compression*
None
* Flexure and compression tests were performed for informational purposes only.
The number of specimens tested met, or exceeded the VTP requirement except for the pulse
velocity for concrete prism specimens. The unit weight of concrete is the most important
parameter to determine the quality of the concrete specimens, so every sample was tested for unit
weight. The pulse velocity test—a special test not available for routine testing in test
laboratories—was used at CIGMAT to check the quality of the concrete. The pulse velocity test
results on the concrete specimens showed that there was nothing unusual about the specimens.
As summarized in Appendix A, there was no direct correlation between the pulse velocity and
unit weight of concrete, and the variation of pulse velocity was normally distributed.
5.2.2.2 Grout Properties
As described in Section 4.1, the number of properties tests completed during the evaluation were
equal to, or greater than, required in Table 3-1 of the VTP. The exception was the viscosity test,
as the grout is a solid at room temperature. Completeness for the grout properties was 100%.
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5.2.2.3 Grout-Substrate Interaction Testing
The numbers (per the VTP) of grouted specimens to be evaluated for each substrate during the
testing are indicated in Table 5-3. The bonding tests were completed over a period of six months
to determine if there are changes in bonding strength with time. The total number of specimens
for the entire test was the same as indicated in the VTP, resulting in 100% completeness.
Table 5-3. Total Number of Tests on Concrete-Grout Interaction Material
Exposure Time
1 Month
3 Months
6 Months
Bonding Strength Tests
Water Cured
4
4
4
Wet-Dry Cycle
0
0
3
5.2.2.4 Model Tests
Two replicate model tests were completed, meeting the completeness goal in the VTP.
5.2.3 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. The
VTP did not establish objectives for this measure.
For the most part, only three samples were prepared, or exposures were completed under
different conditions, making comparison difficult. In this evaluation, analysis is made using four
different parameters. Comparison of the results for multiple specimens prepared under similar
conditions provides some indication of the variability of the specimen material and grout
application methods, as well as the preparation of grout samples to determine unit weight. The
results are shown in Table 5-4.
Table 5-4. Standard Deviation for Concrete Specimen Physical and Strength Properties
and Grout Unit Weight
Properties
Unit Weight (pcf)/(g/cm3)
Pulse Velocity (fps)/(m/sec)
Bonding Strength -all Type 1
failures (1) (psi)/(kg/cm2)
Grout Unit Weight (g/cm3)
Number of
Samples
90
84
8
25
Average Value
143/2.29
14,000/4,267
256/18.0
1.00
Standard
Deviation
3.2
873
31.7
0.05
(1) Samples were cured for varying periods of time, from 30 to 180 days.
5.2.4 Accuracy
Few of the measurements made during this evaluation have references for measurement of
accuracy. Matrix spike and duplicate samples, called for in the VTP, were not completed for the
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TOC analyses due to test facility oversight. Subsequently, percent recovery and relative percent
difference (RPD) cannot be determined for the TOC analysis.
5.3 Audit Reports
NSF conducted two audits of the CIGMAT Laboratories prior to the verification test. The first
laboratory audit, completed by an independent contractor, found that CIGMAT had the necessary
equipment, procedures, and facilities to perform the verification tests described in the VTP, but
identified a number of improvements that could be made to provide the documentation to support
testing outcomes. In the second audit, NSF personnel found that systems were in place to record
laboratory data and supporting QA data obtained during the tests. Specialized log sheets had
been prepared for each of the procedures, and these data sheets are stored with the Study
Director. This is important because some of these tests are performed over several months, with
extended periods between testing.
One of the primary weaknesses identified in the CIGMAT systems was in documentation of the
calibration and maintenance of the basic equipment. It was quite clear that calibration of the
balances, pH meters, pulse velocity meter, etc. were performed. All of the needed calibration
reference standards and standard materials were available near each piece of equipment.
However, the frequency of calibration and the actual calibration could not be verified because, in
most cases, the information was not recorded either on the bench sheet or in an equipment
calibration notebook.
5.4 Data Review
The documentation submitted by CIGMAT for the working properties, physical and mechanical
properties, and durability properties support the findings as described in this report. The
documentation provided by CIGMAT for the TOC analyses showed that the laboratory did not
produce sufficient QC documentation to provide traceability to back up the TOC analytical
results. Records to support the calibration of the TOC instrument were lacking, such as records
of the standards preparation and use of a second source standard to verify calibration of the
instrument. Matrix spikes and sample duplicates were not completed for the TOC analyses, and
a standard (to verify there was no instrument drift during the analyses) was not run during and at
the end of the specimen exposure sample analysis runs. The tap water analysis, which was
performed for only one of the two days where TOC analyses were completed, showed an
unusually high TOC concentration (10 times typical tap water), which raised questions of
whether there was sample contamination or an error in the analysis. Documentation to make this
determination was not available. Overall, the TOC data does not have the QA/QC support to
validate or refute the reported values.
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Section 6
Suggested Reading
1. American Water Works Association (1998), Standard Methods for the Examination of Water and
Wastewater, 20th Edition, American Public Health Association, Washington, B.C.
2. Annual Book of ASTM Standards (1999), Section 4 (Construction) and Section 8 (Plastics),
ASTM, Philadelphia, PA.
3. Ata, A. and Vipulanandan, C. (1999), "Factors Affecting Mechanical and Creep Properties of
Silicate-Grouted," Journal of Geotechnical and Geoenvironmental Engineering, ASCE, Vol. 125,
No. 10, pp. 868-876.
4. Ata, A. and Vipulanandan, C. (1998), "Cohesive and Adhesive Properties of Silicate Grout on the
Grouted Sand Behavior," Journal of Geotechnical and Geoenvironmental Engineering, ASCE, Vol.
124, No. 1, pp. 38-44.
5. Bodocsi, A. and Bowers, M. T. (1991), "Permeability and Acrylate, Urethane and Silicate Grouted
Sands with Chemicals, Journal of Geotechnical Engineering, Vol. 117, No. 8, pp. 1227-1244.
6. CIGMAT News and Literature Review, Vol. 1, No. 3 (1995), Center for Innovative Grouting
Materials and Technology (CIGMAT), University of Houston, November 1995.
(http: //gem 1 .uh. cive. edu)
7. Concrete Construction (Oct. 1998), "Repair, Protection and Rehabilitation, pp. 898-890.
8. EPA (1986), Test Methods for Evaluating Solid Waste (SW 846): Physical/Chemical Methods,
Washington, B.C.
9. Henn, R. W. (1996), Practical Guide to Grouting of Underground Structures, ASCE Press, New
York, NY, 191 p.
10. Karol, R. H. (1990), Chemical Grouting, Marcel Bekker Inc., New York, NY, 465 p.
11. Krizek, R. J. and Vipulanandan, C. (1985), "Evaluation of Adhesion in Chemically Grouted
Geomaterials," Geotechnical Testing Journal, American Society for Testing Materials, Vol. 8, No.
4, pp. 184-190.
12. Lowther, J. and Gabr, M. A. (1997), "Permeability and Strength Characteristic of Urethane-Grouted
Sand," Proceedings, Grouting, Geotechnical Special Publication No. 66, ASCE , pp. 197-211.
13. Ozgurel, H. G. and Vipulanandan, C. (2005),"Effect of Grain Size Bistribution on Permeability
and Mechanical Behavior of Acrylamide Grouted Sand," Journal of Geotechnical and
Geoenvironmental Engineering. Vol. 131, No. 12, pp.1457-1465.
14. Tonyan, T. B., and Gibson, L.J. (1992), "Structure and Mechanics of Cement Foams, " Journal of
Materials Science, Vol. 27, pp. 6272- 6378.
15. Vipulanandan, C. and Krizek, R. J. (1986), "Mechanical Behavior of Chemically Grouted Sand,"
Journal of Geotechnical Engineering, American Society of Civil Engineers, Vol. 112, No. 9, pp.
869-887.
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16. Vipulanandan, C. and Shenoy, S. (1992)," Properties of Cement Grouts and Grouted Sands with
Additives," Proceedings, Grouting, Soil Improvement and Geosynthetics, ASCE, pp. 500-511.
17. Vipulanandan, C., Jasti, V., Magill, D. and Mack, D. (1996a), "Shrinkage Control in Acrylamide
Grouts and Grouted Sands," Proceedings, Materials for the New Millennium, ASCE, Washington
D.C.,pp.840-850.
18. Vipulanandan, C. and Jasti, V. (1996b), "Development and Characterization of Cellular Grouts for
Sliplining," Proceedings, Materials for New Millennium, ASCE, pp. 829-839.
19. Vipulanandan, C. and Jasti, V. (1996c), Behavior of Acrylamide and N-methylolacrylamide
(NMA) Grouts and Grouted Sands, Research Report No. CIGMAT/UH 96-2, University of
Houston, Houston, Texas.
20. Vipulanandan, C. and Jasti, V. (1996d), Characterization of Polymer and Cellular Cement Grouts
for Sewer Rehabilitation, Research Report No. CIGMAT/UH 96-3, University of Houston,
Houston, Texas.
21. Vipulanandan, C. and Jasti, V. (1997), "Behavior of Lightweight Cementitious Cellular Grouts,"
Proceedings, Grouting, Geotechnical Special Publication No. 66, ASCE, pp. 197-211.
22. Vipulanandan, C. and Neelam Kumar, M. (2000), "Properties of Fly Ash-Cement Cellular Grouts
for Sliplining and Backfilling Applications," Proceedings, Advances in Grouting and Ground
Modification, ASCE, GSP 104, Denver, CO, pp. 200-214.
23. Vipulanandan, C., O'Neill, M. W. and Weng, Y (2000), "Mechanical Properties and Chemical
Resistance of Auger Grouts," Proceedings, Advances in Foundation Technologies, ASCE, GSP
100, Denver, CO, pp. 433-446.
24. Vipulanandan, C. Mattey, Y., Magill, D. and Mack, D. (2000), "Characterizing the Behavior of
Hydrophilic Polyurethane Grout," Proceedings, Advances in Grouting Technologies ASCE, GSP
104, Denver, CO, pp. 234-245.
25. Vipulanandan, C., and Ozgurel, H. G. (2009),"Simplified Relationships for Particle-Size
Distribution and Permeation Groutability Limits for Soils," Journal of Geotechnical and
Geoenvironmental Engineering. Vol. 135, No. 9, pp. 1190-1197.
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Appendix A
Behavior of Cement Concrete Bricks
In order to ensure the quality, samples of concrete bricks used in this study were tested and the
results are summarized.
A.I. Unit Weight and Pulse Velocity
To ensure the quality of the concrete brick specimens used the unit weight and pulse velocity of
the specimens were measured.
The variation of pulse velocity with unit weight is shown in Figure Al. The unit weight of
concrete specimens varied between 138 pcf (2.21 g/cm3) and 149 pcf (2.39 g/cm3). The pulse
velocity varied from 12,600 ft/sec (3,840 m/sec) to 15,800 ft/sec (4,815 m/sec). There was no
direct correlation between the pulse velocity and unit weight of concrete (Figure A-l(a)). The
variation of pulse velocity was normally distributed (Figure Al(b)).
A.2. Strength
Flexural strength of dry and wet concrete bricks are summarized in Table A-l. The flexural
strength of concrete bricks varied from 743 to 939 psi (52.2 to 66.0 kg/cm2) based on wet and
dry condition, respectively.
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01
£
o
o
o
u
_o
01
01
I/)
14
12 -
10 -
8 -
6 -
4 -
2 -
0
120
(a)
130 140
Unit weight (Ib/ft3)
150
§
o
01
01
17
16 -
15 -
14 -
Q. 13 -
12
0 10 20 30 40 50 60 70 80 90 100
% Probability
Figure A-l. Quality control for concrete brick specimens (a) Pulse velocity versus unit
weight and (b) Distribution of pulse velocity.
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Table A-l. Strengths of Concrete Bricks
Materials
Concrete
Block
(No.
Specimens)
Remarks
Curing
Time
(days)
28
Concrete
cured for
28 days.
Compressive
Strength
(psi)
Wet
Not
Applicable
Information
For quality
Control
Compressive
Strength
(psi)
Dry
Not
Applicable
Information
For quality
Control
Flexural
Strength
(psi)/(kg/cm2)
Dry
939/66.0
(2)
Related to
CIGMAT CT-3
(modified
ASTM
C321-94)
Bonding
Test
Flexural
Strength
(psi)/(kg/cm2)
Wet
743/52.2
(2)
Related to
CIGMAT CT-3
(modified
ASTM
C321-94)
Bonding
Test
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Appendix B
Characterization of Grout
Warren Environmental 301-04 Epoxy Grout
Number of Grout Specimens Tested = 15
The grout specimens were tested for their working properties, physical properties, and leaching
characteristics. In addition to the setting time test, several physical and mechanical property tests
were performed on the grout. The leaching test included the measurement of total organic carbon
(TOC) content in the water.
(a) Viscosity
At room temperature, the resin was a solid, and hence, the viscosity test was not performed.
(b) Setting Time
The gelling time testing was performed at room temperature and room humidity. A total of 6
samples were tested, and the results are summarized in Table B-l. The setting time varied from
38 to 40 minutes, with an average of 39 minutes and a coefficient of variation (COV) of 2%.
Table B-l. Summary of Setting Time Results
Specimen #
Gelling Time (min)
It
40
2t
38
3t
40
4t
39
5t
40
6t
40
(c) Unit Weight
A total of 25 cylindrical specimens were tested, and the results are summarized in Table B-2.
The grout unit weight varied from 0.91 to 1.09 g/cm3, with an average of 1.00 g/cm3 and a COV
of 5%.
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Table B-2 - Unit Weight Results for Warren Environmental 301-04 Epoxy Grout
Specimen #
1
2
3
4
5
6
7
8
9
10
11
12
13
Density
(g/cm3)
1.03
0.99
1.09
1.05
0.91
1.07
0.95
0.95
0.93
1.05
1.05
1.01
1.03
Specimen #
14
15
16
17
18
19
20
21
22
23
24
25
Average
SD
COV
Density
(g/cm3)
0.94
0.94
1.00
0.97
1.05
0.95
0.96
1.06
1.06
1.09
1.02
0.96
1.00
0.05
0.05
(d) Water Absorbance
The water absorption is a representation of the water diffusion characteristics of the grout. A
total of 3 specimens were tested, and the results are summarized in Table B-3. The weight
change in the specimens varied from 0.09 to 0.17%, with an average of 0.14%. The volume
change in the specimen varied from 0.03% to 0.05%, with a mean of 0.04%
Table B-3. Water Absorbance Results
Exposure
Time
(days)
0
1
2
3
4
Specimen 41
Density
(g/cm3)
0.98
0.98
0.98
0.98
0.98
AW
(%)
0.08
0.15
0.15
0.15
AV
(%)
0.03
0.03
0.05
0.05
Specimen 42
Density
(g/cm3)
0.98
0.98
0.98
0.98
0.98
AW
(%)
0.17
0.17
0.17
0.17
AV
(%)
0.03
0.03
0.03
0.05
Specimen 43
Density
(g/cm3)
0.99
0.99
0.99
0.99
0.99
AW
(%)
0.09
0.09
0.09
0.09
AV
(%)
0.03
0.06
0.06
0.03
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(e) Shrinkage Test
Total of 3 specimens were tested for 28 days. The weight change varied from 0 to 0.09%, with
an average value of 0.06%. The volume change varied from 0 to 0.04%, with an average of
0.01%.
Table B-4. Shrinkage test results for Warren Environmental 301-04 Epoxy Grout
Specimen #
.2
+j
HH
40
39
38
Weight (g)
116.3
110.9
110.1
Length
(mm)
117.43
106.73
110.23
Diameter
(mm)
36.10
36.63
36.43
Volume
(cm3)
120.19
112.47
114.90
Density
(g/cm3)
0.97
0.99
0.96
90
«s
h ™
*> !>-.
,-M £>
(M R
< 0
40
39
38
116.4
111
110.1
117.43
106.77
110.23
36.10
36.63
36.43
120.19
112.52
114.90
0.97
0.99
0.96
90
«s
h <»
3 >>
<£ «
< Q
40
39
38
Average
AW (%)
0.09
0.09
0.00
0.06
AL (%)
0.00
0.04
0.00
0.01
AD (%)
0.00
0.00
0.00
0.00
AV (%)
0.00
0.04
0.00
0.01
Density
(g/cm3)
0.97
0.99
0.96
0.97
(f) Permeability
Three grout specimens were tested for permeability under a hydraulic gradient of 100. A total of
three specimens were tested, with no observed passage of water over a 72 hour period. The
results of the testing are summarized in Table B-5. Based on these results, the permeability of
the grout was zero.
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Table B-5. Permeability Test Results
Moisture content and
specimen
characteristics
Specimen
Aver. diam.
Init. Height
Area
Total weight
Total volume
Total unit weight
Curing time
Discharge (Q) (mL)
Permeability (K)
Units
(mm)
(mm)
(cm2)
(g)
(cm3)
(g/cm3)
(days)
15 min
30 min
1 hrs
2hrs
4hrs
8hrs
12 hrs
24 hrs
48 hrs
72 hrs
cm/s
Specimen Number
1
38.10
63.50
11.40
72.2
72.39
1.00
7
0
0
0
0
0
0
0
0
0
0
0
2
38.10
63.50
11.40
72.0
72.39
0.99
7
0
0
0
0
0
0
0
0
0
0
0
3
38.10
63.50
11.40
71.4
72.39
0.99
7
0
0
0
0
0
0
0
0
0
0
0
(g) Compressive Strength and Stress-Strain Relationship
The compressive properties (strength, failure strain and initial modulus) were measured over
period of 90 days. A total of 11 specimens were tested, and the results are summarized in
Table B-6. The average strength, failure strain, and initial modulus after 3 days of curing were
6,591 psi (463 kg/cm2), 9%, and 225,000 psi (15,819 kg/cm2), respectively. The average
strength, failure strain, and initial modulus after 28 days of curing were 6,180 psi (434 kg/cm2),
5%, and 195,000 psi (13,709 kg/cm2), respectively.
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Table B-6. Summary of Compressive Strength Properties with Curing Time
Specimen
la
2a
3a
Average
4a
5a
6a
Average
7a
8a
9a
lOa
lla
Average
Curing time
(days)
3
3
3
7
7
7
28
28
28
28
28
Strength
(psi)/(kg/cm2)
6,310/443
7,356/517
6,105/429
6,591/463
5,304/372
7,592/533
6,311/443
6,402/450
5,451/383
6,755/474
6,203/436
7,022/493
5,470/384
6,180/434
Failure
Strain
0.10
0.08
0.10
0.09
0.06
0.07
0.03
0.05
0.04
0.05
0.05
0.05
0.05
0.05
Initial Modulus
(psi)/(kg/cm2)
200,000/14,061
250,000/17,576
225,000/15,819
225,000/15,819
215,000/15,116
240,000/16,873
225,000/15,819
226,667/15,936
175,000/12,303
220,000/15,467
190,000/13,358
225,000/15,819
165,000/11,600
195,000/13,709
(h) Wet-Dry Cycles
A total of three specimens were tested for 10 cycles. The cycles started with a wet cycle first.
The change in weight, length, diameter, and volume are reported in Table B-7. After the first
wet-dry cycle, the average change in weight, length, diameter, and volume was 0.04%, -0.25%,
0%, and -0.25%, respectively. The unit weight of the specimens increased. After the tenth wet-
dry cycle, the average change in weight, length, diameter, and volume was 0.25%, -0.41%, 0%,
and -0.41%, respectively The unit weight of the specimens increased. The average strength of the
grout after 10 wet-dry cycles was 6,531 psi (459 kg/cm2); hence, the specimen strength was not
affected after 10 wet-dry cycles.
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Table B-7.1. Wet-Dry cycle test results for Warren Environmental 301-04 Epoxy Grout
13
=
!§?
'•Z
o
Specimen #
#18
#19
#20
Weight (g)
85.7
68.6
77.8
Length
(mm)
79.33
69.83
79.07
Diameter
(mm)
36.20
36.20
36.20
Volume
(cm3)
81.65
71.87
81.38
Density
(g/cm3)
1.05
0.95
0.96
i-H
—
"w
>>
U
Specimen #
#18
#19
#20
Average
AW (%)
0.00
0.00
0.13
0.04
AL (%)
-0.16
-0.14
-0.43
-0.25
AD (%)
0.00
0.00
0.00
0.00
AV (%)
-0.16
-0.14
-0.43
-0.25
Density
(g/cm3)
1.05
0.96
0.96
0.99
«s
—
"u
>>
U
Specimen #
#18
#19
#20
Average
AW (%)
0.12
0.15
0.13
0.13
AL (%)
-0.25
-0.33
-0.51
-0.36
AD (%)
0.00
0.00
0.00
0.00
AV (%)
-0.25
-0.33
-0.51
-0.36
Density
(g/cm3)
1.05
0.96
0.96
0.99
fO
—
"w
>>
U
Specimen #
#18
#19
#20
Average
AW (%)
0.23
0.15
0.13
0.17
AL (%)
-0.29
-0.43
-0.51
-0.41
AD (%)
0.00
0.00
0.00
0.00
AV (%)
-0.29
-0.43
-0.51
-0.41
Density
(g/cm3)
1.06
0.96
0.96
0.99
•t
—
"u
>>
U
Specimen #
#18
#19
#20
Average
AW (%)
0.12
0.15
0.13
0.13
AL (%)
-0.29
-0.43
-0.51
-0.41
AD (%)
0.00
0.00
0.00
0.00
AV (%)
-0.29
-0.43
-0.51
-0.41
Density
(g/cm3)
1.05
0.96
0.96
0.99
Version 3.1 Warren Grout
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EPA STREAMS 61/ETV Water Quality Protection Center Verification
Grouting Materials
ITJ
—
"u
>,
U
Specimen #
#18
#19
#20
Average
AW (%)
0.23
0.15
0.39
0.25
AL (%)
-0.29
-0.43
-0.51
-0.41
AD (%)
0.00
0.00
0.00
0.00
AV (%)
-0.29
-0.43
-0.51
-0.41
Density
(g/cm3)
1.06
0.96
0.96
0.99
VO
—
"w
>,
U
Specimen #
#18
#19
#20
Average
AW (%)
0.23
0.29
0.39
0.30
AL (%)
-0.33
-0.43
-0.47
-0.41
AD (%)
0.00
0.00
0.00
0.00
AV (%)
-0.33
-0.43
-0.47
-0.41
Density
(g/cm3)
1.06
0.96
0.96
0.99
i^
—
"w
>,
U
Specimen #
#18
#19
#20
Average
AW (%)
0.23
0.44
0.51
0.39
AL (%)
-0.29
-0.47
-0.47
-0.41
AD (%)
0.00
0.00
0.00
0.00
AV (%)
-0.29
-0.47
-0.47
-0.41
Density
(g/cm3)
1.06
0.96
0.97
0.99
90
—
"w
>,
U
Specimen #
#18
#19
#20
Average
AW (%)
0.12
0.29
0.39
0.26
AL (%)
-0.29
-0.33
-0.47
-0.36
AD (%)
0.00
0.00
0.00
0.00
AV (%)
-0.29
-0.33
-0.47
-0.36
Density
(g/cm3)
1.05
0.96
0.96
0.99
c\
—
"w
kl
U
Specimen #
#18
#19
#20
Average
AW (%)
0.23
0.15
0.39
0.25
AL (%)
-0.33
-0.29
-0.51
-0.37
AD (%)
0.00
0.00
0.00
0.00
AV (%)
-0.33
-0.29
-0.51
-0.37
Density
(g/cm3)
1.06
0.96
0.96
0.99
Version 3.1 Warren Grout
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EPA STREAMS 61/ETV Water Quality Protection Center Verification
Grouting Materials
o
i-H
—
"w
>>
U
Specimen #
#18
#19
#20
Average
AW (%)
0.23
0.15
0.39
0.25
AL (%)
-0.29
-0.43
-0.51
-0.41
AD (%)
0.00
0.00
0.00
0.00
AV (%)
-0.29
-0.43
-0.51
-0.41
Density
(g/cm3)
1.06
0.96
0.96
0.99
Table B-7.2. Compressive Strength after Wet-dry Cycles for Warren Environmental
301-04 Epoxy Grout
Specimen #
#18
#19
#20
Average
Compressive Strength
(psi)/(kg/cm2)
6,407/450
6,605/464
6,580/462
6,531/459
(i) Chemical Resistance
A total of 9 specimens were tested for a period of 6 months. A total of 3 specimens were tested
in solutions of pH 2, 7 and 10. The test results are summarized in Table B.8.
pH= 2 solution: After 1 month, the average change in weight, volume, and unit weight was
0.32%, 0.59%, and -0.27%, respectively After 6 months, the average change in weight, volume,
and unit weight was 1.38%, 1.70%, and -0.31%, respectively. The weight and volume increased
and the unit weight decreased over the 6-month period.
pH= 7 -water: After 1 month, the average change in weight, volume and unit weight was 0.29%,
0.11%, and 0.18%, respectively After 6 months, the average change in weight, volume, and unit
weight was 1.24%, 0.47%, andO.77%, respectively. The weight, volume and unit weight
increased over the 6-month period.
pH= 10 solution: After 1 month, the average change in weight, volume, and unit weight was
0.42%, -0.06%, and 0.48%, respectively After 6 months, the average change in weight, volume,
and unit weight was 1.24%, 0.47%, and 0.79%. respectively. The weight, volume and unit
weight increased over the 6-month period.
Version 3.1 Warren Grout
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EPA STREAMS 61/ETV Water Quality Protection Center Verification
Grouting Materials
Table B-8. Chemical Resistance Test Results
p
M M
'C a.
0 <=>
Specimen #
#22
#23
#24
Average
Weight (g)
97.3
100.1
111.3
102.90
Length
(mm)
88.87
89.67
106.70
95.08
Diameter
(mm)
36.20
36.17
36.10
36.16
Volume
(cm3)
91.47
92.14
109.21
97.61
Density
(g/cm3)
1.06
1.09
1.02
1.06
5« /— s
I""*
75 M
SS
#22
#23
#24
Average
% Change
97.6
100.3
111.8
103.2
0.32
88.70
89.43
106.73
94.95
-0.14
36.27
36.43
36.17
36.29
0.37
91.64
93.22
109.67
98.18
0.59
1.06
1.08
1.02
1.05
-0.27
5«
"5 r*
a ii
o hj
S a
f> '""'
#22
#23
#24
Average
% Change
98.3
100.9
112.8
104.0
1.06
88.63
89.37
106.70
94.90
-0.20
36.33
36.50
36.20
36.34
0.52
91.88
93.51
109.82
98.40
0.83
1.07
1.08
1.03
1.06
0.23
G«
•S r?
= II
i a
£ a.
^o '""'
#22
#23
#24
Average
% Change
98.6
101.2
113.2
104.3
1.38
88.60
90.03
107.17
95.27
0.18
36.53
36.53
36.23
36.43
0.76
92.86
94.36
110.48
99.23
1.70
1.06
1.07
1.02
1.05
-0.31
IP
'I*
'C a.
O &
Specimen #
#10
#13
#21
Average
Weight (g)
102.2
106.4
105.6
104.73
Length
(mm)
94.33
99.23
96.67
96.74
Diameter
(mm)
36.33
36.33
36.23
36.30
Volume
(cm3)
97.78
102.86
99.66
100.10
Density
(g/cm3)
1.05
1.03
1.06
1.05
^ , — >
>> r~
-^
3&
#10
#13
#21
Average
% Change
102.6
106.7
105.8
105.0
0.29
94.23
99.47
96.80
96.83
0.09
36.33
36.37
36.20
36.30
0.01
97.68
103.34
99.63
100.22
0.11
1.05
1.03
1.06
1.05
0.18
Version 3.1 Warren Grout
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EPA STREAMS 61/ETV Water Quality Protection Center Verification
Grouting Materials
5«
£p
= II
o hj
S a
fi ^
Specimen #
#10
#13
#21
Average
% Change
Weight (g)
103.6
107.5
106.7
105.9
1.15
Length
(mm)
94.20
99.60
96.87
96.89
0.15
Diameter
(mm)
36.33
36.40
36.17
36.30
0.01
Volume
(cm3)
97.65
103.65
99.54
100.28
0.17
Density
(g/cm3)
1.06
1.04
1.07
1.06
0.98
5«
1?
IS,
ve '""'
#10
#13
#21
Average
% Change
103.5
107.7
106.9
106.0
1.24
94.47
99.37
97.00
96.95
0.21
36.40
36.43
36.20
36.34
0.13
98.31
103.58
99.83
100.57
0.47
1.05
1.04
1.07
1.05
0.77
2®
c —
'**!
•C M
0 &
#6
#11
#12
Average
106.2
105.4
83.5
98.37
96.80
97.93
78.93
91.22
36.20
36.10
36.53
36.28
99.63
100.24
82.72
94.20
1.07
1.05
1.01
1.04
£o
IT
«£
f> &
#6
#11
#12
Average
% Change
106.6
105.7
84.0
98.8
0.42
97.03
98.00
79.10
91.38
0.17
36.20
36.10
36.40
36.23
-0.12
99.86
100.31
82.31
94.16
-0.06
1.07
1.05
1.02
1.05
0.48
11
ii
#6
#11
#12
Average
% Change
107.1
106.5
84.9
99.5
1.19
97.13
98.03
79.20
91.45
0.26
36.20
36.10
36.30
36.20
-0.21
99.97
100.34
81.96
94.09
-0.16
1.07
1.06
1.04
1.06
1.35
5« — .
•s &
"S 'H
II
vo ^
#6
#11
#12
Average
% Change
107.3
106.6
84.8
99.6
1.24
97.30
98.40
79.10
91.60
0.40
36.40
36.23
36.23
36.29
0.03
101.25
101.44
81.55
94.75
0.47
1.06
1.05
1.04
1.05
0.79
Version 3.1 Warren Grout
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EPA STREAMS 61/ETV Water Quality Protection Center Verification
Grouting Materials
(j) Leaching Study
A total of 3 specimens were tested in equal volume of water and total organic carbon (TOC). The
results are reported in Table B.9. The average TOC measured varied from 0.0007 to 0.0023
g/L/g of grout, with a mean of 0.0017 g/L/g grout. These data should be considered estimated
values because of data uncertainty arising from incomplete QA/QC, as discussed in Section 5.4.
Summary: The average TOC in the leaching solution was 0.0017 g/L/g of grout.
Table B-9. Summary of Leaching Test Results
Specimen #
1
2
3
4
Material
Tap Water
Grout
Grout
Grout
Weight
(g)
79.7
75.3
77.7
Volume of
Grout
(mL)
60
60
60
Volume of
Tap water
(mL)
100
60
60
60
TOC
(g/L)
0.026
0.185
0.151
0.057
TOC
(g/L/g
grout)
0.0023
0.0020
0.0007
Average 0.0017
Version 3.1 Warren Grout
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EPA STREAMS 61/ETV Water Quality Protection Center Verification
Grouting Materials
Appendix C
Grout-Substrate (Concrete) Interaction
Number of Tests = 15
Total of 15 sandwiched bonding tests (CIGMAT CT-3) were performed after for 30, 90 and 180
days. The failures were characterized based on the Types of failures identified in Table C-l.
Table C-l. Failure Types for CIGMAT CT-3 Test
Failure
Type
Type 1
Type 2
Type 3
Type 4
Type 5
Description
Substrate Failure
Coating Failure
Bonding Failure
Bonding and
Substrate Failure
Bonding and
Coating Failure
CIGMAT CT 3
(ASTM C321 Test)
Concrete/Clay Brick
X
\\
>l 1
]
Concrete/Clay Brick
X
^_ i
'\ 1
Concrete/Clay Brick
X
i i
jr
Concrete/Clay Brick
X
1
Coating 1 ^
1
Concrete/Clay Brick
X
i
* \ ***!
Coating 1 1
Version 3.1 Warren Grout
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EPA STREAMS 61/ETV Water Quality Protection Center Verification
Grouting Materials
(a) After 1 Month
A total of 4 specimens were tested. The results are summarized in Table C-2 Based on the test
results, 75% of the failures were Type 1, and 25% were Type 4. The bonding strength varied
from 228 to 288 psi (16.0 to 20.2 kg/cm2). The average strength measured was 260 psi (18.3
kg/cm2).
Summary: The average bonding strength was 260 psi (18.3 kg/cm2), and 75% of the failures
were Type 1.
Table C-2. Summary of One Month Bonding Test Results
Specimen #
1
2
3
4
Total No.
(% Failure)
Curing
Time
(days)
30
30
30
30
Failure Modes
Type 1
X
X
X
3
(75%)
Type 2
Type 3
Type 4
X
1
(25%)
Type 5
Max Strength
(psi)/(kg/cm2)
278/19.5
249/17.5
288/20.2
228/16.0
4 successful tests.
(b) 3 Months
A total of 4 specimens were tested. The results are summarized in Table C-3. Based on the test
results, 50% of the failures were Type 1, and 50% were Type 4. The bonding strength varied
from 247 to 304 psi (17.4 to 21.4 kg/cm2). The average strength measured was 280 psi (19.7
kg/cm2).
Summary: The average bonding strength was 280 psi (19.7 kg/cm2), 50% of the failures were
Type 1, and the other 50% were Type 4.
Table C-3. Summary of 3-Month Bonding Test Results
Specimen #
5
6
7
8
Total No.
(% Failure)
Curing Time
(days)
90
90
90
90
Failure Modes
Type 1
X
X
2
(50%)
Type 2
Type 3
Type 4
X
X
2
(50%)
Type 5
Max Strength
(psi)/(kg/cm2)
304/21.4
284/20.0
283/19.9
247/17.4
4 successful tests.
Version 3.1 Warren Grout
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EPA STREAMS 61/ETV Water Quality Protection Center Verification
Grouting Materials
(c) 6 Months
A total of 4 specimens were tested. The results are summarized in Table C-4. Based on the test
results, 75% of the failures were Type 1, and 25% of the failures were Type 4. The bonding
strength varied from 218 to 329 psi (15.3 to 23.1 kg/cm2). The average strength measured was
257 psi (18.1 kg/cm2).
Summary: The average bonding strength was 257 psi (18.1 kg/cm2), and 75% of the failures
were Type 1.
Table C-4. Summary of 6-Month Bonding Test Results
Specimen #
9
10
11
12
Total No.
(% Failure)
Curing Time
(days)
180
180
180
180
Failure Modes
Type 1
X
X
X
3
(75%)
Type 2
Type 3
Type 4
X
1
(25%)
Type 5
Max Strength
(psi)/(kg/cm2)
278/19.5
204/14.3
218/15.3
329/23.1
4 successful tests.
(d) 6 Months (Wet-Dry)
A total of 4 specimens were tested. The results are summarized in Table C-5. Based on the test
results, 100% of the failures were Type 1. The bonding strength varied from 204 to 278 psi (14.3
to 19.5 kg/cm2). The average strength measured was 233 psi (16.4 kg/cm2).
Summary: The average bonding strength was 233 psi (16.4 kg/cm2), and 100% of the failures
were Type 1.
Table C-5. Summary of 6-Month Bonding Test (Wet-dry Cycles) Results
Specimen #
13
14
15
Total No.
(% Failure)
Curing Time
(days)
180
180
180
Failure Modes
Typel
X
X
X
3
(100%)
Type 2
Type 3
Type 4
TypeS
Max Strength
(psi)/(kg/cm2)
278/19.5
204/14.3
218/15.3
3 successful tests.
Version 3.1 Warren Grout
46
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EPA STREAMS 61/ETV Water Quality Protection Center Verification Grouting Materials
Appendix D
Grout Vendor Data Sheet
Version 3.1 Warren Grout 47
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EPA STREAMS 61/ETV Water Quality Protection Center Verification
Grouting Materials
GROUT VENDOR DATA SHEET
Grout Product Name: Warren Environmental Mastic 301-04
Grout Product Manufacturer Name and Address: Warren Environmental Inc.
P.O. Box 1206. Carver. MA 02330
Grout Type: Epoxy Grout
Chemical Formula: 100% Solids Epoxy
TESTING METHOD
Type of Resin, Initiator and/or Promotor
Grout Mix (by weigh or volume)
Resin Viscosity (ASTM )
Flash Point (ASTM D 937 )
Tensile Adhesion to Concrete and Clay Brick
(ASTM )
Chemical Resistance (ASTM )
(NaOH, 3% H2SO4 or others)
Volatile Organic Compounds - VOCs
(ASTM )
MANUFACTURER'S RESULTS
100%
2:1 by volume
150,000- 250,000 cps
> 235 degrees F
400 psi or greater
See manufacturer's data sheet.
None
WORKER SAFETY
Flammability Rating
Known Carcinogenic Content
Other Hazards (Corrosive)
MSDS Sheet Availability
RESULT/REQUIREMENT
Base
resin has passed airline industry standards
None
None
Yes
ENVIRONMENTAL CHARACTERISTICS
Heavy Metal Content (w/w)
Leaching from Cured Grouts
Disposal of Cured Grouts
RESULT/REQUIREMENT
None
Certified to NSF/ANSI Standard 61
Cured material is not hazardous.
Version 3.1 Warren Grout
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EPA STREAMS 61/ETV Water Quality Protection Center Verification
Grouting Materials
DATA SHEET ON PROPERTIES OF GROUT (Continued)
APPLICATION CHARACTERISTICS
Minimum Application Temperature
Maximum Application Temperature
Minimum Cure Time before Immersion into
Service
Type of Preparation Before Grouting
Grouting Pressure
RESULT/REQUIREMENTS
30° F
200° F
See mixing instructions
Not applicable
VENDOR EXPERIENCE
Length of Time the Grout in Use
Applicator Training and Qualification
Program
QA/QC Program for Grouts in the Field
COMMENTS
12 years
Yes
Yes
ADDITIONAL COMMENTS (Including Case Studies on Performance)
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