September 2004
EPA600/R-04/183
Environmental Technology
Verification Protocol
Water Quality Protection Center
Verification Protocol for the Verification of
Grouting Materials for
Infrastructure Rehabilitation
Prepared by
NSF International
Under a Cooperative Agreement with
U.S. Environmental Protection Agency
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
PROTOCOL FOR THE VERIFICATION OF GROUTING
MATERIALS FOR INFRASTRUCTURE REHABILITATION
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:
Center for Innovative Grouting Materials and Technology (CIGMAT)
University of Houston
Houston, Texas 77204-4003
713-743-4278
Copyright 2004 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 Grouting Materials
Foreword
The U.S. Environmental Protection Agency (EPA) is charged by Congress with protecting the
Nation's land, air, and water resources. Under a mandate of national environmental laws, the
Agency strives to formulate and implement actions leading to a compatible balance between
human activities and the ability of natural systems to support and nurture life. To meet this
mandate, EPA's research program is providing data and technical support for solving
environmental problems today and building a science knowledge base necessary to manage our
ecological resources wisely, understand how pollutants affect our health, and prevent or reduce
environmental risks in the future.
The 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 Grouting Materials
Acknowledgements
The EPA and NSF International acknowledge those persons who participated in the preparation,
review, and approval of this protocol. 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:
J. Jeffery Fordice, P.E., Assistant City Engineer, City of Saline, Michigan
Ahmad Habibian, Ph.D., P.E., Black & Veatch
Phil Hannan, P.E., Black & Veatch
Steve Henning, Avanti International
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
Table of Contents
Foreword ii
Acknowledgements iii
Table of Contents iv
Tables vi
Figures vi
Acronyms vii
Chapter 1 Introduction 1
1.1 Background 1
1.2 Technical Approach 1
1.3 Roles and Responsibilities 2
1.3.1 Verification Organization 2
1.3.2 EPA 2
1.3.3 Technology Panel 2
1.3.4 Testing Organization 3
1.3.5 Vendor 3
Chapter 2 Test Facility 4
Chapter 3 Experimental Design 5
3.1 Grout and Grouted Sand Physical Property Evaluation 5
3.1.1 Grout and Grouted Sand Specimen Preparation 5
3.1.1.1 Grout Specimens 5
3.1.1.2 Grouted Sand Specimens 8
3.1.2 Grout Curing Properties 10
3.1.2.1 Viscosity 10
3.1.2.2 Setting (Gel) Time 10
3.1.3 Physical and Mechanical Properties 10
3.1.3.1 Unit Weight (Density) 11
3.1.3.2 Water Absorption 11
3.1.3.3 Shrinkage 11
3.1.3.4 Permeability 12
3.1.3.5 Unconfmed Compressive Strength and Stress/Strain Relationship 12
3.1.3.6 Tension Tests 12
3.1.4 Durability Properties 13
3.1.4.1 Wet/Dry Cycle 13
3.1.4.2 Chemical Resistance 13
3.1.5 Environmental Properties—Leaching Test 14
3.2 Grout-Substrate Bonding Strength 14
3.2.1 Cylinder Bonding (CIGMAT GR 5-00) 15
3.2.2 Brick/Prism Bonding (CIGMAT CT 3-00) 15
3.2.3 Wet/Dry Cycle 15
3.3 Model Tests 15
3.3.1 Model Test 1: Leak Control in Pipe Joints 16
3.3.2 Model Test2: Leak Control in Manhole Joints 18
3.3.3 Model Test 3: Leak Control at aLateral Joint 20
3.3.4 Model Test 4: Concrete Leak Repair 22
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3.3.5 Model Test Procedures 23
Chapter 4 Sampling and Analytical Procedures 25
Chapters Quality Assurance Project Plan (QAPP) 27
5.1 Quality Assurance Responsibilities 27
5.2 Data Quality Indicators 27
5.2.1 Representativeness 27
5.2.2 Completeness 28
5.2.3 Precision 28
5.2.4 Accuracy 29
5.2.5 Measurements 30
5.2.6 Analytical Quality Control 30
Chapter 6 Data Reporting, Data Reduction, and Data Validation 31
6.1 Data Documentation 31
6.2 Data Reduction 31
6.3 Data Validation 31
6.4 Verification Report 32
Chapter 7 Assessments 33
7.1 Audit Reports 33
7.2 Corrective Action Plan 33
Chapter 8 Safety Considerations 34
References 35
Glossary 37
Appendix A CIGMAT Procedures 38
Appendix B Vendor Data Sheet 39
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
Tables
Table 3-1. Grout Tests for Various Applications 7
Table 3-2. Grouted Sand and Grout-Substrate Interaction Tests 9
Table 3-3. Shrinkage Test Conditions (Vendor-Selected Based on Application) 12
Table 4-1. Handling Methods and Analyses for Collected Samples 25
Table 4-2. Scheduled Instrument QC Checks and Corrective Actions for Analytical Methods .. 26
Table 5-1. Summary of Analytical Accuracy and Precision Limits 30
Figures
Figure 3-1. Typical models used for preparing grout specimens 6
Figure 3-2. Mold for preparing grouted sand specimens 8
Figure 3-3. Model configuration for testing leak control at pipe joints (Model Test 1) 17
Figure 3-4. Typical calibration of Model Test 1: leak rate versus pressure 18
Figure 3-5. Model configuration for testing leak control in manhole joints (Model Test 2) 19
Figure 3-6. Model configuration for testing leak control at a lateral (Model Test 3) 21
Figure 3-7. Model configuration for testing concrete leak repair (Model Test 4) 23
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AA
ASTM
CIGMAT
cm
cP
EPA
ETV
ft
g
in.
I/I
kPa
Ib
lb/ft3
mL
mm
min
MSDS
NSF
ORD
psi
QA
QAPP
QC
RH
RPD
RSD
sec
SD
SOP
TOC
WQPC
Acronyms
Atomic absorption
American Society for Testing and Materials
Center for Innovative Grouting Materials and Technology
Centimeter
Centi-poise
U.S. Environmental Protection Agency
Environmental Technology Verification
Foot or feet
Gram
Inch
Infiltration and inflow
Kilopascals
Pound
Pounds per cubic feet
Milliliter
Millimeter
Minute
Material safety data sheet
NSF International
EPA Office of Research and Development
Pounds per square inch
Quality assurance
Quality assurance project plan
Quality control
Relative humidity
Relative percent deviation
Relative standard deviation
Second(s)
Standard deviation
Standard operating procedure
Total organic carbon
ETV Water Quality Protection Center
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
Chapter 1
Introduction
1.1 Background
A critical issue facing the nation today involves the increased pollution of waterways, shorelines,
rivers, bays, and streams. A high percentage of infiltration and inflow (I/I) into sanitary sewer
systems is attributable to cracks and leaks from open joints in sewer pipes or service laterals
connected to the sewers. Municipalities are discovering that if I/I problems are not adequately
controlled, they will lead to frequent overflows and undue burden on treatment facilities.
The primary goal of in-situ grouting, the oldest trenchless technology method still used to control
leaks in wastewater systems, is to return the structure to its original working condition. Several
types of grout materials have been used to control I/I problems in wastewater systems and storm
systems (8,9). These materials have been commonly used for leak control in below-grade wet
wells and holding tanks, manholes, sewer and storm lines, and cracked retaining walls and other
underground structures (3,5,6,9,10).
However, there is no systematic method for evaluating the performance of grouts under service
conditions. In a 2002 infrastructure research needs report (7), EPA identified the need to evaluate
the performance of grouts under various environmental conditions, such as humidity,
temperature, pH, and wastewater chemistry. The aim of this protocol is to establish a
comprehensive approach for testing grouts for leak control applications in old and new
wastewater collection systems and other concrete repairs.
1.2 Technical Approach
The overall objective of this protocol is to describe a testing program to systematically evaluate
grouts for controlling infiltration to wastewater systems and leaks in concrete structures. Specific
verification objectives are to:
• Evaluate the properties (working, physical, mechanical, durability, and teachability) of
grouts and grouted sands;
• Characterize the bonding properties of the grout-substrate interaction; and,
• Verify the performance of grouted joints and repaired concrete cracks under hydrostatic
pressure up to 5 psi (10 feet of water) and wet/dry cycles over a period of three months.
Testing will use relevant ASTM and CIGMAT standards. A total of 12 different tests will
characterize the grouts (Table 3-1); several additional tests will evaluate grouted sand specimens
and grout-substrate interaction (Table 3-2). Model tests will be used to evaluate grout
effectiveness under various leak control configurations. All CIGMAT standard methods
referenced herein are included in Appendix A, while the ASTM standard numbers are referenced
in this protocol
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A test plan will be prepared for each grout material to be evaluated. The 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 Roles and Responsibilities
The primary roles and responsibilities of each party involved in the verification process are
described in this section.
1.3.1 Verification Organization
The primary role of the verification organization (VO), NSF, is to:
• Coordinate with CIGMAT, the testing organization (TO), and the vendor to prepare a test
plan, using this protocol as a template, to meet testing requirements;
• Coordinate with the ETV Grouts Technical Panel, as needed, to review the test plan prior
to the initiation of verification testing;
• Review and approve test plan, and sign the test plan signoff sheet;
• Coordinate with the EPA Water Quality Protection Center (WQPC) Project Officer to
approve the test plan prior to the initiation of verification testing;
• Review the quality systems of the TO and qualify them to complete the testing;
• Oversee the technology evaluation and associated laboratory testing;
• Review data generated during verification testing;
• Oversee the development of a verification report and verification statement; and
• Provide quality assurance oversight at all stages in the verification process.
1.3.2 EPA
This protocol 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 approval of the test plan, including the quality assurance project plan
(QAPP);
• Sign the test plan signoff sheet;
• Review and approval of the verification report and verification statement; and
• Posting of the verification report and verification statement on the EPA ETV website.
1.3.3 Technology Panel
A technology panel was formed to assist with the review of this generic grout test plan. Input
from the panel ensures that data generated during verification testing are relevant and that the
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
method of evaluating different technologies is fair and consistent. All grout test plans may be
reviewed by representatives of the technology panel and will be approved by the WQPC
Program Manager and vendor.
1.3.4 Testing Organization
The TO for verifications completed under test plans developed from this protocol is CIGMAT
Laboratories at the University of Houston. The primary responsibilities of the TO are to:
• Coordinate with the VO and vendor relative to preparing and finalizing the test plan;
• Sign the test plan signoff sheet;
• Conduct the technology verification in accordance with the test plan, with oversight by
the VO;
• Analyze all samples collected during the technology verification process, in accordance
with the procedures outlined in the test plan;
• 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 the changes are executed.
1.3.5 Vendor
The vendor's primary responsibilities are to:
• Provide the TO with grout samples for verification;
• Complete a product data sheet (Appendix B) prior to testing;
• Sign the test plan signoff sheet;
• Provide technical assistance to the TO, as requested, during the verification testing
period;
• Provide funding for verification testing;
• Review and concur the test plan, including the QAPP; and
• Review the verification report and verification statement.
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
Chapter 2
Test Facility
Since 1985, CIGMAT researchers at the University of Houston have been investigating the
performance of various grouting materials used in wastewater facilities and sand. The CIGMAT
laboratories and associated facilities are located in the College of Engineering complex at 4800
Calhoun Road, Houston, Texas. Several laboratories at the University are available to perform
the required physical and chemical testing.
The CIGMAT laboratories and affiliated facilities are equipped with devices that can perform all
of the grout, grouted sand, and grout-substrate tests in this test plan. Molds are available to
prepare the specimens for testing. Four types of models are available to perform the model tests
which simulate the behavior of applied grouts in several different applications: leak control in a
pipe joint; leak control in a manhole joint; leak control in a lateral; and concrete leak repair.
Hydrostatic test chambers are available to calibrate the leak rates at the test joints.
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
Chapter 3
Experimental Design
The ETV testing program for grouts will evaluate the performance and characteristics of grout
material in three different testing phases:
• The physical properties of the grout and grouted sand will be tested by utilizing test
specimens created by the TO;
• The interaction of the grout and substrate will be tested by applying the grout to test
substrate material (such as bricks or concrete) and completing a series of performance
tests; and,
• Model tests, where grout is applied to laboratory-simulated leaking pipes, pipe joints,
and/or manholes will be conducted to test for leak control.
Testing details are given in the following sections.
3.1 Grout and Grouted Sand Physical Property Evaluation
Properties of the neat resin (unsolidified grout), grout, and grouted sand specimen samples to be
tested can be grouped as:
• Working properties (resin/grout mix);
• Physical and mechanical properties (grout and grouted sand specimens);
• Durability properties (grout and grouted sand specimens); and,
• Leachability (grout and grouted sand specimens).
The properties to be tested are summarized in Tables 3-1 and 3-2 for grout and grouted sand,
respectively.
The physical property evaluation tests consist of creating grout/grouted sand specimens,
challenging the specimens to a particular test, and measuring the results. For tests where testing
procedures have been developed by the American Society of Testing and Materials (ASTM), the
ASTM test procedure will be used. Where no ASTM test procedures exist, CIGMAT has
developed their own testing protocols, and these protocols will be used. Where applicable, the
ASTM and CIGMAT testing procedures are referenced in the following sections and the
CIGMAT procedures are included in Appendix A of this protocol.
3.1.1 Grout and Grouted Sand Specimen Preparation
3.1.1.1 Grout Specimens
ASTM Standard Method C31/C-31M-96 shall be used for making and curing test specimens for
cement, acrylic, or acrylamide-based grouts (which typically do not expand while curing).
Standard Practice CIGMAT GR 4-00 shall be used for making and curing test specimens for
polyurethane-based grout (which may expand while curing). Figure 3-1 shows the molds that
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will be utilized to create the test specimens. Specimens to be cured under water shall be
completely submerged in a water bath of tap water at room temperature. If a specimen floats, a
small amount offeree will be applied to keep it submerged. Multiple specimens of the same type
of grout or grouted sand material may be placed in the same water bath. After solidification,
specimens shall be removed from the mold and stored in labeled, sealed plastic bags for
identification, protection, and to prevent moisture loss. The specimens shall be stored in a
temperature- and humidity-controlled room at 23 ± 2°C (room temperature) and 50 ± 5 percent
humidity.
PVC
Model
Rubber
Stopper
Grout
1.5 in.
4.5 in.
(a) Cement Grouts
Upper Plate
Load Cell
Upper Cap
Teflon Mold
Steel Sleeve
Cylinder
Thermocouple
Lower Cap
Lower Plate
(b) Polyurethane Grouts
Figure 3-1. Typical models used for preparing grout specimens.
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Table 3-1. Grout Tests for Various Applications
Leak Control Applications
Properties
Working
Properties
Physical and
Mechanical
Properties
Durability
Properties
Environment.
Properties
Tests Conditions
Viscosity 23°C
Setting (Gel)
Time ^
Unit Weight 23°C
Water
Absorption
Shrinkage Temp, humidity
Permeability Water
Compressive _ „ „„ ,
o* ^u 3, 7, 28 days
Strength ' ' J
Tensile _ „ „„ ,
o* ~*u 3, 7, 28 days
Strength ' ' J
Elongation 3, 7, 28 days
Wet-Dry Cycle Number of cycles
Chpmical
^nemicdi = ? 1Q
Resistance
Leaching Water
Test Method to be Used
CIGMAT GR 6-02
ASTM C 191-04 (cement-based) or
method defined in 3.1.2.1.2 (chem.)
CIGMAT GR 1-00
CIGMAT GR 3-00
Method defined in 3. 1.3.3
CIGMAT GR 7-02
CIGMAT GR 2-02
CIGMAT PC 2-99 (Specimen
preparation by CIGMAT CH 2-01)
CIGMAT PC 2-99 (Specimen
preparation by CIGMAT CH 2-01)
CIGMAT GR 3-00
CIGMAT CH 2-01
Method defined in 3 . 1 . 5 . 1
Pipe
Joint
X
X
X
NA
NA
NA
NA
NA
NA
NA
NA
X
A/T u i T ^ i Concrete
Manhole Lateral „
Repair
XXX
XXX
XXX
NA NA X
NA NA X
NA NA X
NA NA X
NA NA X
NA NA X
NA NA X
NA NA X
XXX
Number
of Specimens
or Tests
3
6
3
3
3
3
9
9
9
3
9
3
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3.1.1.2 Grouted Sand Specimens
Grouted sand specimens shall be prepared according to CIGMAT GS 1-02. The mold to be used
to create them is shown in Figure 3-2. Each specimen shall be made in a separate mold and the
amount of grout permeated will be recorded by measuring the amount of grout injected. The
molds shall be constructed of Plexiglas™ that can be split longitudinally into three equal pieces
so that the specimen can be removed after it has been prepared. One edge of each piece of the
split tube shall be coated with silicon rubber to form a seal when the three pieces are clamped
together with hose clamps. Plexiglas filters with nylon mesh shall be used at the inlet and outlet
ends. A half-inch sand filter, separated from the specimen by nylon mesh, shall be used at the
inlet to distribute the grout uniformly. The mold shall be filled with sand and another sand filter
with nylon mesh shall be used in the outlet (similar to inlet). The sand shall have a particle size
in the range of 0.3 to 7 mm, a unit weight in the range of 120 to 130 pounds per cubic foot and a
relative density prior to grouting of 85 to 92 percent. Six specimens shall be grouted in parallel at
an injection pressure of 2 psi.
After solidification, specimens shall be removed from the mold and stored in sealed, labeled
plastic bags in a temperature- and humidity-controlled room (23 ± 2°C and 50% ± 5% RH).
Grout Outlet
to PVC Mold
Top Reaction
Plate
Filters
Plexiglass or
Teflon Mold
SS3 \. • .".".".". U88i
Bottom Reaction
Plate
1/2 in. Grout Inlet from
Distribution System
Figure 3-2. Mold for preparing grouted sand specimens.
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Table 3-2. Grouted Sand and Grout-Substrate Interaction Tests
Test Method to be
Materials Tests Conditions Used
Leak Control Applications
Pipe Concrete Number of
Joint Manhole Lateral Repair Tests
GROUTED SAND
Physical and
Mechanical
Properties
Durability
Properties
Unit weight
Water absorbance
Shrinkage
Permeability
Compressive strength
Tensile strength
Wet-dry cycle
Chemical Resistance
Cured
23°C
Temp, humidity
Water
3, 7, 28 days
3, 7, 28 days
Number of cycles
pH = 2, 7,10
GROUT-SUBSTRATE INTERACTION
Concrete, clay brick,
Bonding Wet condition cured under water
Strength
Wet-dry cycle
Number of cycles
CIGMAT GR 1-00
CIGMAT GR 3-00
Method defined in 3 . 1 . 3 . 3
CIGMAT GR 7-02
CIGMAT GR 2-02
CIGMAT PC 2-99
CIGMAT GR 3-00
CIGMAT CH 2-01
CIGMAT GR 5-00 or
CIGMAT CT 3-00
CIGMAT GR 3-00
X
X
X
X
X
X
X
X
NA
NA
X
X
X
X
X
X
X
X
NA
NA
X
X
X
X
X
X
X
X
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
X
X
o
J
o
J
o
J
3
9
9
3
9
12
12
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3.1.2 Grout Curing Properties
3.1.2.1 Viscosity
Grout viscosity will be evaluated using the procedures described in this section. The viscosity of
grouted sand will not be evaluated. Grout viscosity will be evaluated using a procedure outlined
in CIGMAT GR 6-02. Using a cylindrical spindle-type viscometer (Brookfield Viscometer with
8 speeds, LVT model with four spindles or equivalent), the initial viscosity and changes in
viscosity during the gelling process shall be measured at room temperature at selected strain rates
(up to 180 sec"1). The specific strain rates at which viscosity will be measured shall be
determined in advance of testing by the TO, with the consent of the vendor. Once the material
performs consistently at different viscometer speeds, the test shall be complete. A minimum of
three replicate tests shall be conducted.
3.1.2.2 Setting (Gel) Time
Grout setting or gel time will be evaluated using the procedures described in this section. The
setting time of the grouted sand will not be evaluated.
For cement-based grouts, ASTM C 191-04, "Standard Test Method for Time of Setting of
Hydraulic Cement by Vicat Needle," shall be used. The room temperature and relative humidity
(23 ± 2°C, 50% ± 5% RH) shall be adjusted as necessary to comply with the ASTM standard.
No ASTM standard method is currently available to determine the gel time for acrylamide,
acrylic, or polyurethane-based grouts. Hence it shall be determined by the elapsed time from
grout preparation until the grout no longer flows 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 shall be poured into a container. At
periodic intervals to be specified in the test plan, the container shall be slowly tipped to
approximately 45 degrees, and the analyst shall determine if the grout exhibits liquid flow
properties or if the grout sample has gelled and the specimen can no longer flow from the
container.
A total of six replicates of each grout shall be analyzed.
3.1.3 Physical and Mechanical Properties
To obtain initial characterization information on the grout and grouted sand specimens, all
specimens shall be 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. Measurements shall be taken at
the top, middle, and bottom of the specimen, with two measurements taken at 90 degrees from
each other at each location to obtain consistent data.
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3.1.3.1 Unit Weight (Density)
Solidified grout and grouted sand specimens shall be used to determine the unit weight (density)
of the grout. The determination shall be completed per CIGMAT GR 1-00 for both grout and
grouted sand specimens. Unit weight shall be calculated using the weight and volume of the
specimens. A minimum of three replicates will be evaluated for unit weight. Based on the unit
weight, the grout shall be reported as lighter or heavier than water.
3.1.3.2 Water Absorption
Water absorption characteristics shall be evaluated on both grout and grouted sand specimens as
outlined in standard procedure CIGMAT 3-00. A minimum of three solidified grout and grouted
sand specimens shall be immersed in tap water (initial pH in the range of 7 to 8) and changes in
weight and volume (determined by measuring specimen diameter and height) of the specimens
shall be recorded a minimum of once every working day (Monday through Friday, excluding
holidays) until the changes in weight and volume become negligible (less than 0.5 percent of the
previous weight and volume), or for one week, whichever occurs first. The report for this testing
shall include the time of immersion, the initial characteristics of the specimens, the weight and
volume change with time, water absorption as a percentage of the initial weight, and volume of
grout.
3.1.3.3 Shrinkage
This test determines specimen weight and shape changes under various temperature and
humidity conditions (Table 3-3) generally encountered during service (16,19). The vendor shall
choose one or more of four test conditions (parts), based on the anticipated applications for the
grout (crack in wall, sewer, or pipes). For example, Parts A and B specify 10 ± 2°C, similar to
the temperature of soils around sewer lines in cooler northern climates, while Parts C and D
specify a temperature of 27 ± 2°C, more typical of sewer conditions in warmer southern climates.
The vendor may select a different temperature more representative of the application in which
the grout is to be used. A controlled temperature chamber shall be used to maintain the specific
conditions of temperature, while humidity shall be maintained by enclosing specimens in a
sealable plastic bag or glass bottle, or leaving them uncovered. Humidity will be measured using
a digital humidity meter. At the onset of the test, specimens shall be prepared in a mold with
inner dimensions of 1.5 in. (38 mm) in diameter and 3.5 in. (90 mm) in length. It is anticipated
that the grout specimens will shrink during the initial curing. Grout specimens that shrink to a
length of 2.6 in. (65 mm) or less shall be rejected and new grout specimens shall be made. A
minimum of three specimens shall be tested under each selected test condition. The weight and
dimensions of the specimens shall be reported before and after 28 days of conditioning.
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Table 3-3. Shrinkage Test Conditions (Vendor-Selected Based on Application)
Parts Temperature, Duration, and Relative Humidity
Part A
PartB
PartC
PartD
10°C ± 2°C for 28 days @ 90% ± 5% RH
10°C ± 2°C for 28 days @ 50% ± 5% RH
27°C ± 2°C for 28 days @ 90% ± 5% RH
27°C ± 2°C for 28 days @ 50% ± 5% RH
3.1.3.4 Permeability
Solidified grout and grouted sand specimens shall be used to determine their permeability.
Specimens shall be prepared in 2-in. diameter Plexiglas/glass cylinders and permeated with
water under a hydraulic gradient of 100, per CIGMAT GR 7-02. Testing shall be completed at
room temperature and humidity unless otherwise specified by the vendor. A minimum of three
replicate tests shall be run on both grout and grouted sand specimens. The report for this testing
shall include the temperature and humidity at which testing was completed, any changes in the
specimens during the testing, and the permeability obtained during the testing.
3.1.3.5 Unconfined Compressive Strength and Stress/Strain Relationship
CIGMAT GR 2-02 has been developed for testing grouts and grouted sand specimens in
compression under monotonically increasing load (load increasing linearly), based on test
methods ASTM D 3574-03 (polyurethane) and ASTM C 109-02 (cementitious materials).
Compression tests shall be performed using screw-type machines with capacities up to 5,000 Ibs.
Specimens shall be loaded at specified rates based on the type of grout or grouted sand, and the
loading rate may be determined based on trial tests conducted outside of the ETV test. Cement,
acrylic, or acrylamide-based grout and grouted sand specimens 1.5 in. (38 mm) in diameter and
2.6 to 3.5 in. (65 to 90 mm) in length shall be tested. For polyurethane-based grout and grouted
sand, the specimens shall be 1.2 to 1.4 in. (30 to 35 mm) long. The specimens shall be trimmed
and capped (if necessary, using a sulfur compound commonly used for capping cement concrete)
to ensure smooth and parallel surfaces. Specimens shall be tested in triplicate at 3, 7 and 28 days
following specimen preparation. The reported data shall include compressive strength, modulus
and failure strain, where the modulus is determined from the initial slope of the stress/strain
relationship and the failure strain is the maximum loading point before the specimen fails.
3.1.3.6 Tension Tests
Direct tension and indirect tension tests shall be performed on grout and grouted sand specimens.
Special "dumbbell-shaped" Teflon®-lined molds, as described in CIGMAT CH 2-01, shall be
used to prepare the direct tension specimens. Direct tension testing shall be conducted on the
prepared specimens using the dumbbell-shaped molds, following the procedures outlined in
CIGMAT PC 2-99. (Note: CIGMAT PC 2-99 specifies dumbbell-shaped molds with different
dimensions than those outlined in CIGMAT CH 2-01. The correct dumbbell-shaped mold
dimensions for the ETV test are outlined in CIGMAT CH 2-01.) For the indirect splitting tension
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test, specimens 1.5 in. (38 mm) in diameter and 2.6 to 3.5 in. (65 to 90 mm) in length shall be
used (ASTM C-496). A screw-type machine shall be used for both the direct and indirect tension
tests. Following one or two trial tests, the rate of loading by the machine shall be adjusted to
cause failure of the specimens within 20 minutes. The selected test speed shall be included in the
final verification report. A minimum of three specimens shall be tested after each curing period
of 3, 28, and 180 days for a minimum total of nine replicates for each tension test. The reported
data shall include the maximum loads carried by the specimens, the average cross-sectional area,
and the calculated direct and indirect tensile strengths, to the nearest 10 psi (69 kPa).
3.1.4 Durability Properties
3.1.4.1 Wet/Dry Cycle
During its service life, the grout or grouted sand could be subjected to a number of wet/dry
cycles. This test is designed to determine the impact of repeated wetting and drying on the
performance of grouts and grouted sand. A minimum of three replicate specimens shall be used
for this test. The specimens shall be subjected to 10 wet/dry cycles for a total test time of 140
days, or until failure (unconsolidation). One wet/dry cycle shall be 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% RH). The water exposures shall be completed as
described in Section 11 of CIGMAT GR 3-00, using tap water having a pH between 7 and 8.
Changes in length, diameter, weight, and volume of the specimens shall be measured daily per
Sections 9 and 11 of CIGMAT GR 3-00. At the end of the 10-wet/dry cycles, specimens shall be
tested to determine the compressive and/or tensile strengths of the grout, as described in sections
3.1.3.5 and 3.1.3.6. The reported data shall include weight and dimension data collected for the
specimens, as well as the data to be reported described in sections 3.1.3.5 and 3.1.3.6.
3.1.4.2 Chemical Resistance
This test will evaluate the resistance of grouts and grouted sands when exposed to chemical
conditions representing various sand and groundwater environments. The test results will help
when selecting suitable grouts for use in various chemical environments. Cylindrical grout
specimens shall be prepared as described in Section 3.1.1.1, and the initial weight, dimensions,
color, and surface appearance of the specimens shall be recorded. Nine specimens at each pH
shall be fully immersed in solutions with pH 2, 7, and 10 maintained at room temperature (23 +
2°C) for the entire exposure period. The solutions shall consist of tap water with hydrochloric
acid or sodium hydroxide added to achieve the pH required for the tests. The vendor may specify
a different temperature, depending on the application. The weight, volume, color, and surface
appearance of the specimens shall be 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. The pH, clarity,
and color of the exposure solution shall also be recorded at each evaluation time. During the
evaluation, if the pH changes by more than ± 2 units, additional hydrochloric acid or sodium
hydroxide shall be added to the solution to return it to its original pH. The analyst shall note in
the project logbook the quantity of chemical and revised pH during each adjustment. At each
evaluation, compression testing shall be completed for the specimens in accordance with Section
7.4 of CIGMAT CH 2-01. All data and observations shall be reported, along with the
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calculations described in sections 8.1, 8.3, and 8.4 of CIGMAT CH 2-01. The appearance of
specimens and immersion solutions shall be reported as described in sections 9.2 and 9.3 of
CIGMAT CH 2-01.
3.1.5 Environmental Properties—Leaching Test
Potential contaminant leaching from solidified grout shall be determined by analyzing water
exposed to the grout for total organic carbon (TOC) and lead. A minimum of three test replicates,
using cylindrical grout specimens, will be prepared as described in Section 3.1.1.1. The
specimens will be immersed in three individual exposure jars, each containing tap water (pH = 8
± 0.5; TOC < 1 mg/L; total lead < 0.3 mg/L). One blank container containing only the exposure
water shall be prepared and held under the same conditions as the specimen exposure jars. The
exposure jars and blank jar will be held at room temperature for seven days.
The test shall be conducted with the appropriate number of grout specimens and water volume so
that there is an adequate volume of exposure water to conduct the required analyses. A liquid-to-
solid ratio of 1:1 (by volume) shall be selected as the default, but other ratios may be used, as
requested by the vendor and approved by the TO. If a different liquid-to-solid ratio is used, it
shall be reported in the verification report.
At the beginning and end of the exposure period, samples of the exposure water will be analyzed
to determine the presence of organic compounds or metals that have leached from the grout. The
samples will be analyzed for total lead and TOC. Other analyses may be included, as determined
by the testing organization, based on the MSDS sheet provided by the grout manufacturer. If
other analyses are included, the concentration of the analyte in the exposure water shall not be
greater than the method detection limit.
The water in the blank container shall be sampled at the beginning and end of the exposure
period, and analyzed for the same constituents as the grout specimen exposure water. This will
provide a baseline concentration of constituents in the tap water.
Details of the analytical methods, required sample volumes, and sample holding are provided in
Section 4.
3.2 Grout-Substrate Bonding Strength
Interaction between the grout and a concrete substrate shall be evaluated by testing the bonding
strength and type of failure (bonding failure, substrate failure, or a combination) under different
service conditions, as specified in sections 3.2.1 through 3.2.3. Testing of wet grout/concrete
substrate specimens shall be conducted over a period of six months in accordance with CIGMAT
GR 5-00 (where two cylinders are bonded with grout) or CIGMAT CT 3-00 (where the area
between concrete bricks/prisms is grouted), as selected by the vendor prior to the ETV
verification. In addition, bonded configurations prepared according to either CIGMAT GR 5-00
or CIGMAT CT 3-00 shall be subjected to wet/dry cycle testing, as described in Section 3.1.4.1.
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3.2.1 Cylinder Bonding (CIGMAT GR 5-00)
This test configuration may be used to determine the bonding strength of various grout materials
(15,23). The test consists of sandwiching a layer of grout between flat surfaces of concrete (the
ends of concrete cylinders) and then loading the test specimen in tension. Details of specimen
preparation are in CIGMAT GR 5-00. The Grout-Rock (Soil) Test outlined in Section 7.2 of
CIGMAT GR 5-00 will not be conducted as part of the ETV testing. The reported data shall
include all collected data, the bonding strength, and the type of bonding failure.
3.2.2 Brick/Prism Bonding (CIGMAT CT 3-00)
Although CIGMAT CT 3-00 was developed for coating materials, it may be adopted for grouts.
As described in CIGMAT CT 3-00, the grout shall be sandwiched between a pair of rectangular
concrete block and clay brick 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 ETV testing,
wet specimens shall be used to simulate extreme grouting conditions. The bonded wet specimens
shall be immersed in water until testing begins. The reported data shall include the type of brick
used, number of specimens tested, age of specimen at time of test, average bond strength,
standard deviation, type of failure, and the bond strength.
3.2.3 Wet/Dry Cycle
During its service life, a grouted concrete joint could be subjected to a number of wet/dry cycles.
Hence, each bonded configuration will be tested for performance by subjecting it to 10 wet and
dry cycles, where one wet/dry cycle takes 14 days, for a total test time of 140 days, or until
failure. Changes in the length, diameter, weight, and volume shall be measured daily, as
described in Section 3.1.4.1. Following the wet/dry cycles, a minimum of three test specimens
shall be retested to determine the compressive strength of the grout to quantify possible changes.
Compressive strength will be determined using the apparatus and procedure described in
Sections 5 and 10 of CIGMAT GR 2-02. The reported data shall include testing conditions,
number of specimens tested, individual and average compressive strength and modulus, and/or
tensile strength.
3.3 Model Tests
Since water leaks can occur under different conditions, four model tests are available to represent
different field situations. Depending on the application for the grout, the vendor shall select one
or more of these model tests to be completed:
• Model Test 1: Leak Control in Pipe Joint
• Model Test 2: Leak Control in Manhole Joint
• Model Test 3: Leak Control at a Lateral Joint
• Model Test 4: Concrete Leak Repair
The tests are fully explained in the following sections, and details of the model test procedures
are provided in Section 3.3.5.
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3.3.1 Model Test 1: Leak Control in Pipe Joints
This model test simulates a situation in which grout is applied to an 8-in. (20-cm) diameter
leaking pipe joint (Figure 3-3). The leaking pipe joint is placed in a cylindrical steel chamber
filled with sand. The sand shall have the same specifications as described for the preparation of
grouted sand specimens in Section 3.1.1.2. The steel chamber is 22.5 in. (57 cm) in diameter and
34 in. (86 cm) long, and both ends of the chamber have an opening of 8.5 in. (22 cm) for holding
the pipe. This allows access to the leaking pipe joint from either end of the chamber. Valves on
the outside of the test chamber enable the TO to saturate the sand and bleed the air from the
system.
Procedure for preparing a pipe joint for Model Test 1:
• The chamber is placed vertically and the bottom end is sealed using a rubber gasket with
one section of the pipe in place.
• The chamber is filled approximately halfway by freely dropping and lightly compacting
sand. The spigot part of the pipe is put in place and the rest of the chamber is filled with
sand.
• Once the chamber is filled with sand, the top cover is placed on the chamber using a
rubber gasket to make the end watertight.
• The chamber is placed horizontally for the test. A calibration curve of the joint leak rate
versus pressure shall be developed, as shown in Figure 3-4.
• The vendor has the choice of grouting the joint or having CIGMAT grout the joint per
vendor instructions. The grouted joint is then tested for performance as detailed in
Section 3.3.5.
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Water
20 in.
Dia.
Pressure
Gage
Bleed Valve
(a) Elevation View
Inflow
Measurement
(b) Plan View
Figure 3-3. Model configuration for testing leak control at pipe joints (Model Test 1).
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£2
4*
4*
4200
4000
3800
3600
3400
3200
3000
2800
2600
1.5
2.5 3 3.5
Pressure (psi)
4.5
Figure 3-4. Typical calibration of Model Test 1: leak rate versus pressure.
3.3.2 Model Test 2: Leak Control in Manhole Joints
In order to simulate a leaking manhole joint, this model test (Figure 3-5) uses a 10- or 12-in. (25-
or 30-cm) diameter vertical pipe. The pipe is enclosed in a cylindrical steel chamber 22.5 in. (57
cm) in diameter and 34 in. (86 cm) long, filled with sand. The only opening in the chamber
(other than the valves) shall be from the top, leading into the vertical pipe. Valves on the outside
of the test chamber enable the TO to saturate the sand and bleed the air from the system.
Procedure for preparing a manhole joint for Model Test 2:
• The chamber is filled by freely dropping and lightly compacting sand. The spigot part of
the pipe is put in place in the test chamber and the rest of the chamber is filled with sand.
• The chamber remains in the vertical position for the test. A calibration curve of joint leak
rate versus pressure shall be developed, as shown in Figure 3-4.
• The vendor has the choice of grouting the joint or having CIGMAT grout the joint per
vendor instructions. The grouted joint is then tested for performance as detailed in
Section 3.3.5.
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Water
Pressure
Gage
Bleed Valve
12 in. Dia.
\\X\X\X\\V\\]
(a) Elevation View
(b) Plan View
Figure 3-5. Model configuration for testing leak control in manhole joints (Model Test 2).
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3.3.3 Model Test 3: Leak Control at a Lateral Joint
In order to simulate a leaking lateral joint, this model test (Figure 3-6) uses an 8-in. (20-cm)
diameter main pipe with a 4-in. (10-cm) diameter lateral pipe. Both pipes are enclosed in a
cylindrical steel chamber 22.5 in. (57 cm) in diameter and 34 in. (86 cm) long, filled with sand.
Both ends of the chamber have a circular opening 8.5 in. (22 cm) in diameter for the main pipe,
and the top of the chamber has a circular opening for the lateral, allowing access to the leaking
joint from the main pipe and the lateral. Valves on the outside of the test chamber enable the TO
to saturate the sand and bleed air from the system and to apply water under pressure to evaluate
the effectiveness of the grout application.
Procedure for preparing a lateral joint for Model Test 3:
• The chamber is placed vertically and the bottom end sealed using a rubber gasket with
part of the pipe in place.
• The chamber is filled approximately halfway by freely dropping and lightly compacting
sand. The lateral pipe is then inserted in the main pipe and the rest of the chamber shall
be filled with sand.
• Once the chamber is filled with sand, the top cover is placed on the chamber with a
rubber gasket to make the end watertight.
• The chamber remains in the vertical position for the test. A calibration curve of joint leak
rate versus pressure shall be developed, as shown in Figure 3-4.
• The vendor has the choice of grouting the joint or having CIGMAT grout the joint per
vendor instructions. The grouted joint is then tested for performance as detailed in
Section 3.3.5.
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Water
Bleed Valve
Inflow
Measurement
(a) Elevation View
20 in.
Dia.
0
0
(b) Plan View
Figure 3-6. Model configuration for testing leak control at a lateral (Model Test 3).
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3.3.4 Model Test 4: Concrete Leak Repair
In order to simulate a leak in a concrete structure, this model test (Figure 3-7) shall use 10-in.
(25-cm) diameter circular concrete disks with 6-in. (15-cm) openings at the center (each disk is
donut-shaped). As a default, the two disks shall be placed one inch apart and grouted by the
vendor. The vendor may, however, select the opening size. After the vendor-specified curing
period, the grouted joint shall be subjected to hydrostatic pressure testing to determine the leak
rate, as detailed in 3.3.5.
Procedure for preparing a concrete leak repair joint for Model Test 4:
• The gap between the concrete rings on the testing rig is set at the appropriate dimension,
(one inch or as specified by the vendor).
• The vendor or CIGMAT applies the grout in the gap in accordance with the vendor's
standard procedures.
• After the grout has cured, testing will commence using the procedures outlined in Section
3.3.5.
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Supporter
i
3 in
^
Concrete Ring
Steel Pipe
lin.
(a) Elevation View
Grout
10 in.
(b) Plan View
Figure 3-7. Model configuration for testing concrete leak repair (Model Test 4).
3.3.5 Model Test Procedures
The testing procedure will be essentially the same regardless of the model test selected. Each
model test shall be conducted in duplicate. Prior to grouting, each joint to be tested shall be
calibrated in order to develop a characteristic leak rate versus pressure relationship (see
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Figure 3-4). The grout shall be applied to wet sand (models 1 through 3) or wet concrete disks
(model 4) by the vendor. CIGMAT personnel shall supervise the grouting procedures and
pictures shall be taken of the joint/concrete disks prior to and after grouting. The time elapsed
and volume of grout used during the grouting process shall be recorded. The time period
following the application of the grout before testing is initiated shall be determined from the
manufacturer's literature and is dependent on the penetrability and setting time of grout. During
the grouting of the joints/cracks, at least ten grout samples shall be collected to test the setting
time (Section 3.1.2.2), unit weight (Section 3.1.3.1), and compressive properties (Section 3.1.3.5)
of the grouts. These analyses are in addition to those specified in Section 3.1.
Once the grouted joint(s)/concrete disks have cured per the manufacturer's instructions, they
shall be subjected to the following regimen:
1. Apply hydrostatic pressure of 3 psi 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.
3. Repeat Step 1 at a hydrostatic pressure of 5 psi.
4. Maintain saturated conditions for a period of one week. For model tests 1, 2, and 3, fill
the chambers with water with no hydrostatic pressure. In model test 4, soak the joint with
water.
5. Drain all water from the test chambers and allow them to stand for one 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 shall include the characteristic leak rate versus pressure for each ungrouted
joint; lapsed time and volume of grout used during the grouting process; lapsed time between
grouting and commencement of testing; data for grout (setting time, unit weight, and
compressive properties); initial leak rates at the three hydrostatic pressures; and the leak rates at
the three hydrostatic pressures following the saturated/drained cycles.
At the end of each model test, the test chamber shall be emptied, any loose sand shall be
carefully removed with a brush, and the grouted region shall be inspected and documented.
During the inspection, the distribution of grout around the leaking joint/concrete crack shall be
mapped. Photographs shall be taken of the grouted joints during and upon completion of this
activity.
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Chapter 4
Sampling and Analytical Procedures
Verification of grouts under ETV primarily consists of physical tests performed on prepared
specimens as described in Chapter 3, "Experimental Design." The outlined procedures identify
the sampling locations and frequency required for each test.
Further sample preparation and analysis is required only for the leaching test, which is outlined
in Section 3.1.5. Exposure water samples will be collected and analyzed, at a minimum, for total
lead and TOC. Other analyses may be conducted based on the chemical composition of the tested
grout. Tables 4-1 and 4-2 will be modified in the test plan prepared for each grout verification
based on the analyses to be completed. The exposure water samples shall be representative grab
samples collected from the exposure jar.
The sample handling, analysis and reporting shall be as outlined in Table 4-1.
Table 4-1. Handling Methods and Analyses for Collected Samples
Preservation, Reporting
Analysis
Lead
TOC
Method1
SM3310
SM5310
(B or C)
Bottle Type and Size
Plastic, one 125-mL
bottle
Glass, two 40-mL
bottles
Holding Time Detection Limit
Cool to 4°C, pH<2
H2SO4, 28 days
Cool to 4°C, pH<2
HNOs, six months
0.3 mg/L
1 mg/L
1 Standard Methods for the Examination of Water and Wastewater, 20th Edition.
Samples shall be delivered to the analytical laboratory following appropriate chain of custody
procedures, including use of chain of custody forms. Samples shall be logged in and refrigerated
by the laboratory, as described in Table 4-1.
Table 4-2 describes the specific QC checks required for the analytical methods for total lead and
TOC used in this project. These checks shall determine when corrective action is needed.
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Table 4-2. Scheduled Instrument QC Checks and Corrective Actions for Analytical
Methods
QC Procedure Frequency
Acceptance Criteria
Corrective Action
Calibration curve Every batch
Analyze blank Every batch
(deionized water)
Analyze standard Every batch
Dilute over range When needed
samples
Matrix spike
Every batch
±10% of known sample Find cause, repair, rerun before
sample analysis
±10% of calibration blank Find cause, repair, rerun before
sample sample analysis
±10% of known sample Find cause, repair, rerun before
sample analysis
±10% of original
Find cause, repair, rerun previous
samples
80-120% recovery of spike Find cause, repair, rerun previous
samples
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Chapter 5
Quality Assurance Project Plan (QAPP)
The QAPP, which is part of the test plan, specifies procedures that shall be used to ensure data
quality and integrity arising from the testing. Careful adherence to these procedures will ensure
that the data generated from the testing will provide sound analytical results that will indicate the
true performance of the grout, and form the basis for the report on the testing.
5.1 Quality Assurance Responsibilities
The TO, in preparing the test plan, shall be responsible for ensuring that the test plan and the
QAPP properly implement the requirements of this protocol. The VO is responsible for review of
the test plan to assure that all elements required by this protocol are properly addressed.
During testing, the TO shall be responsible for assuring that the elements contained in the test
plan are complied with. Written or electronic records shall be maintained for calibrations, sample
collection, and data manipulation. In grout testing, sources of error may include instrumentation
drift or miscalibration; variations in the grout, sand, and/or substrate; systematic bias of
measurements; and/or intrinsically inaccurate instruments. The quality of reference
measurements is ensured by frequent instrumentation calibration in accordance with the
manufacturer's instructions. The TO shall maintain documentation of instrument calibration.
5.2 Data Quality Indicators
The data obtained during verification testing must be sound for accurate conclusions to be
drawn. For all measurement and monitoring activities conducted for grout verification, the VO
and EPA require that the data quality parameters be established based on the proposed end-users
of the data. Data quality parameters include four indicators of data quality: representativeness,
completeness, precision, and accuracy.
5.2.1 Representativeness
Representativeness refers to the degree to which data accurately and precisely reflect the
conditions or characteristics of the parameters. In verifications following this protocol,
representativeness will be ensured by consistent data acquisition and sample collection
(including sample numbering, timing of sample collection, sampling procedures, sample
preservation, sample packaging, and sample shipping). Representativeness will also be ensured
by using each method at its optimal capability to provide results representing the most accurate
and precise measurements possible. Representativeness also implies collecting sufficient data
during each operation to be able to detect changes in operation. To achieve this, the following
actions will be taken:
Test Materials:
• Test Sand: The test sand batch shall be rejected if the particle-size distribution of the sand
exceeds ±20% of the mean particle-size distribution value.
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• Test Concrete: The test concrete batch shall be rejected if the unit weight and/or water
absorption properties exceed ±20% of the mean values.
Laboratory Conditions:
• Temperature and Humidity: For those tests where temperature and humidity requirements
are specified, temperature and humidity readings shall be recorded daily to ensure that
laboratory conditions have not changed.
Equipment:
• Proper operation: This shall be verified every morning of active testing.
5.2.2 Completeness
Completeness refers to the amount of data collected from a measurement process compared to
the expected amount to be obtained. For this ETV test plan, completeness refers to the proportion
of valid, acceptable data generated using each method. The completeness objective for data
generated following this protocol is 85%, as calculated by Equation 5-1.
(n \
,~, j valid and acceptable -, „ „ /r i \
Completeness = x 100 (5-1)
I "total j
5.2.3 Precision
Precision refers to the degree of mutual agreement among individual measurements and provides
an estimate of random error. Analytical precision is a measurement of how far an individual
measurement may deviate from a mean of replicate measurements. Precision is evaluated from
analysis of field and laboratory duplicates and spiked duplicates. Duplicates will be collected at a
frequency of one duplicate for every ten samples collected for the laboratory analyses discussed
in Chapter 4. The laboratory will run duplicate samples as part of its QA program. The data
quality objective for precision is based on the type of analysis performed.
The standard deviation (SD), relative standard deviation (RSD), and/or relative percent
difference (RPD) recorded from sample analyses are ways to quantify precision. SD is calculated
by:
y (xt-
Standard Deviation = J—— — (5-2)
V n- 1
Where:
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x = sample mean
x; = /'th data point
n = number of data points
Relative percent difference (RPD) is calculated by:
RPD = l- 2 x 100% (5-3)
\ ^ J
Where:
Q = Concentration of the compound or element in the sample
C2 = Concentration of the compound or element in the duplicate
C = Arithmetic mean of the sample and the duplicate
As specified in Standard Methods (Method 1030-C), precision is specified by the standard
deviation of the results of replicate analyses. For the various tests to be conducted by CIGMAT
at its testing facility, precision will be measured by performing duplicate tests and evaluating the
resultant data by calculating the SD, RSD, and RPD. Tables 3-1 and 4-1 provide the required
number of duplicate tests for the various testing methods.
In situations where the testing procedures specify precision objectives (such as ASTM or
Standard Methods), the specific precision objectives must be achieved in order for the test to be
considered valid. For other situations where specific precision objectives are not required, the
precision values shall be reported in the verification report.
5.2.4 Accuracy
For measurements that will be recorded as part of this study, accuracy refers to the difference
between the measured reading and an established reference. In order to report accuracy, the
instruments used during testing shall be calibrated as required by the analytical method, and the
calibration records, which are maintained as a hard copy maintained in the laboratory, shall be
made available.
Spiking a sample matrix with a known amount of a constituent and measuring the recovery
obtained in the analysis is a method of determining accuracy. Using laboratory performance
samples with a known concentration in a specific matrix can also monitor the accuracy of an
analytical method for measuring a constituent in a given matrix. Accuracy is usually expressed
as the percent recovery of a compound from a sample. The following equation will be used to
calculate percent recovery:
Percent Recovery = [( AT-A; ) / As ] x 100 (5-4)
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Where:
AT = Total amount measured in the spiked sample
A; = Amount measured in the un-spiked sample
As = Spiked amount added to the sample
During verification testing, the laboratory will run matrix spike samples at a frequency of one
spiked sample for every 10 samples analyzed. The laboratory will also analyze liquid and solid
samples of known concentration as lab control samples.
5.2.5 Measurements
Leaks in the model tests will be measured accurate to ± 2 mL. The weight and dimension during
the grout and grouted sand tests will be measured to an accuracy of 0.1 g and 0.01 mm,
respectively. The unit weight and strength will be measured to an accuracy of 0.5 Ib/ft3 and 2 psi,
respectively.
5.2.6 Analytical Quality Control
The quality control procedures for blanks, spikes, duplicates, calibration of equipment, standards,
reference check samples and other quality control measurements will follow the guidance of
EPA methods and CIGMAT SOPs. Table 5-1 shows the quality control limits that will be used
by the laboratory for these analyses to ensure compliance with the data quality indicators for
accuracy and precision. Field and laboratory duplicate analyses will be performed at a frequency
of one duplicate per ten samples collected. Samples will be spiked for accuracy determination at
a frequency of one per fifteen samples analyzed by the laboratory. Accuracy and precision will
be calculated for all data using the equations presented in sections 5.2.2 and 5.2.3.
Table 5-1. Summary of Analytical Accuracy and Precision Limits
Analysis
Lead
TOC
Accuracy
(% recovery)
70-130
80-120
Precision
(RPD)
0-30
0-20
Note: If additional analytical parameters are added to the testing procedures, accuracy
and precision limits shall be specified in the test plan.
RPD: Relative percent deviation
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
Chapter 6
Data Reporting, Data Reduction, and Data Validation
The TO (CIGMAT) is responsible for managing all the data and information generated during
the testing program. To maintain quality data, specific procedures shall be followed during data
reporting, reduction, and validation. These procedures are discussed below.
6.1 Data Documentation
All field and laboratory activities shall be thoroughly documented by the use of field logbooks,
project approval/chain of custody sheets, laboratory notebooks and bench sheets, and instrument
records.
A field logbook shall be maintained at the test facility. Daily activity entries shall be made in the
logbook documenting operating conditions, observations, and maintenance activities, if any.
Each sample collected shall be noted in the logbook and any other pertinent information shall be
recorded. Completed pages in the logbook shall be signed and dated.
Original project approval and chain of custody forms shall accompany all samples sent to the
analytical laboratory and will be maintained by the TO. The laboratory shall produce a final data
report that includes all chemical test results, physical measurements, QA/QC data for blanks,
accuracy (recovery), precision (percent difference), and lab control or matrix check samples.
Any deviation from standard protocol shall be discussed in a narrative and any data that does not
meet the QA/QC requirements shall be flagged. A narrative shall be prepared discussing the
findings of any corrective action.
The laboratory shall maintain all logbooks, bench sheets, instrument printouts, and similar
materials. The TO shall make these records available for inspection by the VO or EPA upon
request.
6.2 Data Reduction
Data reduction refers to the process of converting raw test results into useful data for selecting
grout material for wastewater system maintenance and concrete repair. Data shall be obtained
from logbooks, data sheets, and computer outputs. While reduced data will be officially reported
to the VO upon completion of each evaluation, all raw data shall also be made available to the
VO for the QA review of the project and for record keeping.
6.3 Data Validation
The person performing each test shall verify the completeness of the appropriate data forms. The
TO Director shall review laboratory logbooks and data sheets on a regular basis to verify
completeness. The TO technical staff shall regularly inspect testing equipment and keep it in
working order.
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
6.4 Verification Report
All the data collected during the testing shall be reported as indicated in Chapter 3, processed
and analyzed as outlined in Chapter 5, and summarized in a verification report and verification
statement following ETV Water Quality Protection Center guidelines.
The verification report shall thoroughly present and discuss the findings of the verification test. It
shall contain all raw and analyzed data, all QA/QC data sheets, a description of all types of data
collected, a detailed description of the testing procedure and methods, results and QA/QC results.
The verification statement shall present a condensed summary of the testing procedure and
findings. It is expected that the verification report will contain the following main sections.
• Verification Statement
• Notice
• Forward
• Contents
• Abbreviations and Acronyms
• Introduction and Background
• Testing Procedures and Methods
• Testing Results
• Quality Assurance/Quality Control Summary
• Glossary
• References
• Appendices
o Raw Data and Testing Logs
o Laboratory Standard Operating Procedures
o Test Plan
o O&M Manual
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
Chapter 7
Assessments
7.1 Audit Reports
The TO Director or designee shall perform at least one QA inspection of the test facility
laboratories during the evaluation of a grout and shall document any and all findings in an audit
report, which will be submitted to the EPA Project Officer, EPA Program Quality Assurance
Manager, and VO Program Manager for review. The VO Program Manager, Manager, QA and
Safety, or other VO designee shall also 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.
7.2 Corrective Action Plan
The 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; and
• Technical systems audits.
Ultimate responsibility for project QA/QC during implementation of this test plan rests with the
verification organization, specifically with the VO Project Manager, with appropriate input from
the VO 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. The VO Project Manager will coordinate oversight and/or audits of
these tasks with the TO 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.
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
Chapter 8
Safety Considerations
Grouting the joints for the model tests shall be done at the covered test facility at the University
of Houston, which has adequate ventilation. Grout and grouted sand specimens for testing shall
also be prepared in CIGMAT laboratories. 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 the health and safety plan shall be ensured throughout the
duration of the project.
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
References
1. American Water Works Association. Standard Methods for the Examination of Water
and Wastewater, 20th Edition. Washington, DC: American Public Health Association,
1998.
2. Annual Book of ASTM Standards. Section 4, "Construction" and Section 8, "Plastics."
Philadelphia, PA: ASTM, 1999.
3. Center for Innovative Grouting Materials and Technology (CIGMAT), University of
Houston. CIGMATNews and Literature Review 1 (3). , http://geml.uh.cive.edu
4. Test Methods for Evaluating Solid Waste (SW 846): Physical/Chemical Methods.
Washington, DC: EPA, 1986.
5. Henn, R. W. Practical Guide to Grouting of Underground Structures. New York: ASCE
Press, 1996
6. Karol, R. H. Chemical Grouting. New York: Marcel Dekker Inc., 1990.
7. Tafuri, A., and A. Selvakumar. "Wastewater Collection System Infrastructure Research
Needs." Report No. EPA/600/JA-2/226, 2002.
8. Vipulanandan, C., V. Jasti, D. Magill, and D. Mack. "Shrinkage control in acrylamide
grouts and grouted sands." In Proceedings, Materials for the New Millennium.
Washington DC: ASCE, 1996, pp.840-50.
9. Vipulanandan, C., and V. Jasti. Characterization of Polymer and Cellular Cement Grouts
for Sewer Rehabilitation, Research Report No. CIGMAT/UH 96-3. Houston, TX:
University of Houston, 1996.
10. Vipulanandan, C., Y. Mattey, D. Magill, and D. Mack. "Characterizing the behavior of
hydrophilic polyurethane grout." In Proceedings, Advances in Grouting Technologies., ,
GSP 104. Denver, CO: ASCE, 2000, pp. 234-45.
Additional Sources of Information
1. Ata, A., and C. Vipulanandan. "Factors affecting mechanical and creep properties of
silicate-grouted sands." Journal of'Geotechnical and GeoenvironmentalEngineering 125.
(10): 868-76.
2. Ata, A., and C. Vipulanandan. "Cohesive and adhesive properties of silicate grout on the
grouted sand behavior." Journal of Geotechnical and Geoenvironmental Engineering 124
(1): 38-44.
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
3. Bodocsi, A., and M. T. Bowers. "Permeability and acrylate, urethane and silicate grouted
sands with chemicals." Journal of Geotechnical Engineering 111 (8): 1227-244.
4. Repair, protection and rehabilitation. Concrete Construction (October 1998): 898-90.
5. Krizek, R. J., and C. Vipulanandan. "Evaluation of adhesion in chemically grouted
geomaterials." ASTM Geotechnical Testing Journal. 8 (4): 184-90.
6. Lowther, J., and M. A. Gabr. "Permeability and strength characteristic of urethane-
grouted sand." Proceedings: Grouting, Geotechnical Special Publication, No. 66.
Washington, DC: ASCE, 1997, pp. 197-211.
7. Tonyan, T. D., and L. J. Gibson. "Structure and mechanics of cement foams." Journal of
Materials Science 27 (1992): 6272-378.
8. Vipulanandan, C., and R. J. Krizek. "Mechanical behavior of chemically grouted sand."
ASCE Journal of 'GeotechnicalEngineering 112 (9): 869-87.
9. Vipulanandan, C., S. and Shenoy. "Properties of cement grouts and grouted sands with
additives." In Proceedings, Grouting, Soil Improvement and Geosynthetics. Washington,
DC: ASCE, 1992, pp. 500-11.
10. Vipulanandan, C., and V. Jasti. "Development and characterization of cellular grouts for
sliplining." Proceedings, Materials for New Millennium. Washington, DC: ASCE, 1996,
pp. 829-39.
11. Vipulanandan, C., and V. Jasti, V. Behavior of Acrylamide and N-methylolacrylamide
(NMA) Grouts and Grouted Sands, Research Report No. CIGMAT/UH 96-2. Houston,
TX: University of Houston, 1996.
12. Vipulanandan, C., and V. Jasti. "Behavior of lightweight cementitious cellular grouts." In
Proceedings, Grouting, Geotechnical Special Publication No. 66. Washington, DC:
ASCE, 1997, pp. 197-211.
13. Vipulanandan, C. and M. Neelam Kuma. "Properties of fly ash-cement cellular grouts for
sliplining and backfilling applications." In Proceedings, Advances in Grouting and
Ground Modification, GSP 104. Denver, CO: ASCE, 2000, pp. 200214.
14. Vipulanandan, C., M. W. O'Neill, and Y. Weng. "Mechanical properties and chemical
resistance of auger grouts." In Proceedings, Advances in Foundation Technologies, GSP
100. Denver, CO: ASCE, 2000, pp. 433-46.
15. Weaver, K. Dam Foundation Grouting. New York: ASCE Press, 1991.
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Environmental Technology Verification Water Quality Protection Center Grouting Materials
Glossary
Accuracy—A measure of the closeness of an individual measurement or the average of a
number of measurements to the true value and includes random error and systematic error.
Batch—The number of samples analyzed during a period in which an instrument was operated
continuously.
Bias—The systematic or persistent distortion of a measurement process that causes errors in one
direction.
Comparability—A qualitative term that expresses confidence that two data sets can contribute
to a common analysis and interpolation.
Completeness—A qualitative term that expresses confidence that all necessary data have been
included.
Precision—A measure of the agreement between replicate measurements of the same property
made under similar conditions.
Quality Assurance Project Plan—A written document that describes the implementation of
quality assurance and quality control activities during the life cycle of the project.
Representativeness—A measure of the degree to which data accurately and precisely reflect a
characteristic of a population parameter at a sampling point, or for a process or environmental
condition.
Room Temperature—23°C ±2°C. Relative humidity under room temperature conditions is
expected to be 50% ±5%. This definition of room temperature shall be used for all testing
conducted under the ETV Test Plan for the Verification of Grouts, even if a referenced SOP or
standard defines the term differently.
Standard Operating Procedure—A written document containing specific procedures and
protocols to ensure that quality assurance requirements are maintained.
Technology Panel—A group of individuals with expertise and knowledge in grouts.
Test Plan—A written document that describes the procedures for conducting an evaluation for
the application of a grout material; the quality assurance project plan is an important part of the
test plan.
Verification—To establish the evidence on the performance of grouts under specific conditions,
following a predetermined test plan.
Verification Report—A written document containing all raw and analyzed data, all QA/QC
data sheets, descriptions of all collected data, a detailed description of all procedures and
methods used in the verification testing, and all QA/QC results. The test plan shall be included as
part of this document.
Verification Statement—A document that summarizes the verification report reviewed and
approved by the verification organization and EPA.
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Appendix A
CIGMAT Procedures
CIGMATCH2-01
CIGMAT CT 3-00
CIGMAT GR 1-00
CIGMAT GR 2-02
CIGMAT GR 3-00
CIGMAT GR 4-00
CIGMAT GR 5-00
CIGMAT GR 6-02
CIGMAT GR 7-02
CIGMAT GS 1-02
CIGMAT PC 2-99
(Questions about CIGMAT procedures may be directed to CIGMAT at the University of
Houston)
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Appendix B
Vendor Data Sheet
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Environmental Technology Verification Water Quality Protection Center
Grouting Materials
GROUT VENDOR DATA SHEET (Attach Additional Sheets if Necessary)
Grout Product Name:
Grout Product Manufacturer Name and Address:
Grout Type:
Chemical Formula:
TESTING METHOD
Type of Resin, Initiator and or Promotor
Grout Mix (by weight 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 - VOC's
(ASTM )
MANUFACTURER'S RESULTS
WORKER SAFETY
Flammability Rating
Known Carcinogenic Content
Other hazards (corrosive)
MSDS Sheets Availability
RESULT/REQUIREMENT
ENVIRONMENTAL
CHARACTERISTICS
Heavy Metal Content (w/w)
Leaching from Cured Grouts
Disposal of Cured Grouts
RESULT/REQUIREMENT
September 2004
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Environmental Technology Verification Water Quality Protection Center
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/REQUIREMENT
VENDOR EXPERIENCE
Length of Time the Grout in Use
Applicator Training & Qualification
Program
QA/QC Program for Grouts in the Field
COMMENTS
ADDITIONAL COMMENTS (Including Case Studies on Performance)
September 2004
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