Environmental Technology Verification Coatings and
Coating Equipment Program (ETV CCEP)
UV-Curable Coatings - Generic Verification Protocol
Revision No. 0
September 26, 2003
Distribution Statement "A" applies
Approved for public release; distribution is unlimited
Requests for this document shall be referred to:
Mr. Michael Kosusko
U.S. Environmental Protection Agency
National Risk Management Research Laboratory
Mail Code (E343-02)
Research Triangle Park, NC 27711
Contract No. DAAE30-98-C-1050
Task No. 306
CDRL No. A008
Prepared by
National Defense Center for Environmental Excellence (NDCEE)
Submitted by
Concurrent Technologies Corporation
100 CTC Drive
Johnstown, PA 15904
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TABLE OF CONTENTS
Page
SI TO ENGLISH CONVERSIONS iv
LIST OF ABBREVIATIONS AND ACRONYMS v
1.0 INTRODUCTION 1
1.1 Purpose of the UV-Curable Coatings Generic Verification Protocol 1
1.2 Quality Assurance for the ETV CCEP 1
1.3 Organization of the UV-Curable Coatings GVP 1
1.4 Formatting 2
1.5 Approval Form 2
2.0 PROJECT DESCRIPTION 5
2.1 General Overview 5
2.1.1 Coating Application and Curing Test Location 5
2.1.2 NDCEE Environmental Coatings Laboratory Facilities 6
2.1.3 Statement of Project Objectives 7
2.2 Technical/Experimental Approach and Guidelines 7
2.2.1 Test Approach 7
2.2.2 Verification Test Objectives 8
2.2.3 Test Panels 8
2.2.4 Coating Specification 8
2.2.5 UV Curing Apparatus 9
2.2.6 Coating Baseline Test 9
2.2.7 Design of Experiment 9
2.2.8 Performance Testing 10
2.2.9 Quantitative Measurements 10
2.2.10 Participation 10
2.2.11 Critical and Noncritical Factors 11
2.2.12 Determination of Total Volatile Content of the UV-Curable Coating 14
2.3 Schedule 14
3.0 PROJECT ORGANIZATION AND RESPONSIBILITIES 15
4.0 QUALITY ASSURANCE OBJECTIVES 19
4.1 General Objectives 19
4.2 Quantitative Quality Assurance Objectives 19
4.2.1 Accuracy 19
4.2.2 Precision 22
4.2.3 Completeness 22
4.2.4 Impact and Statistical Significance Quality Objectives 22
4.3 Qualitative QA Objectives: Comparability and Representativeness 22
4.3.1 Comparability 22
4.3.2 Representativeness 23
4.4 Other QA Objectives 23
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5.0 SITE SELECTION AND SAMPLING PROCEDURES 25
5.1 Site Selection 25
5.2 Sampling Procedures and Handling 25
5.3 Sample Custody, Storage and Identification 26
6.0 ANALYTICAL PROCEDURES AND CALIBRATION 27
6.1 Facility and Laboratory Testing and Calibration 27
6.1.1 Facility Testing and Calibration 27
6.1.2 Laboratory Testing and Calibration Procedures 27
6.2 Product Quality Procedures 28
6.3 Standard Operating Procedures and Calibration 28
6.4 Nonstandard Methods 31
7.0 DATA REDUCTION, VALIDATION, AND REPORTING 33
7.1 Raw Data Handling 33
7.1.1 Error in Solids Content 33
7.2 Preliminary Data Package Validation 33
7.3 Final Data Validation 34
7.4 Data Reporting and Archival 34
7.5 Verification Statement 34
8.0 INTERNAL QUALITY CONTROL CHECKS 35
8.1 Guide Used for Internal Quality Program 35
8.2 Types of QA Checks 35
8.3 Basic QA Checks 35
8.4 Specific Checks 36
8.5 Offsite QA Checks 36
9.0 PERFORMANCE AND SYSTEM AUDITS 37
10.0 CALCULATION OF DATA QUALITY INDICATORS 39
10.1 Precision 39
10.2 Accuracy 39
10.3 Completeness 39
10.4 Project Specific Indicators 39
11.0 CORRECTIVE ACTION 41
11.1 Routine Corrective Action 41
11.2 Nonroutine Corrective Action 41
12.0 QUALITY CONTROL REPORTS TO MANAGEMENT 43
13.0 REFERENCES 45
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LIST OF TABLES
Table 1. Testing and Laboratories and Representative Laboratory Equipment Holdings 6
Table 2. Overall Guidelines and Procedures Applied to this GVP 7
Table 3. Critical Control Factors 11
Table 4. Noncritical Control Factors 12
Table 5. Critical Response Factors 13
Table 6. Estimated Schedule as of 9/26/2003 14
Table 7. Summary of Current ETV CCEP Experience and Responsibilities 16
Table 8. Frequency and Mechanisms of Communications 17
Table 9. Responsibilities During Testing 17
Table 10. QA Objectives for Precision, Accuracy and Completeness for All Noncritical
Control Factor Performance Analyses 20
Table 11. QA Objectives for Precision, Accuracy and Completeness for All Critical
Response Factor Performance Analyses 21
Table 12. Process Responsibilities 26
Table 13. Noncritical Control Factor Testing and Calibration Criteria 29
Table 14. Critical Response Factor Testing and Calibration Criteria 30
Table 15. CTC Laboratory QA/QC Format Sources 35
LIST OF FIGURES
Figure 1. Testing and Quality Assurance Project Plan Approval Form 3
Figure 2. Project Organization Chart 15
LIST OF APPENDICES
A Default Standard Test Panel
B ASTM Methods
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SI to English Conversions
Multiply SI
by factor to
SI Unit English Unit obtain English
o
C °F 1.80, then add 32
L gal, liq(U.S.) 0.2642
m ft 3.281
kg Ibm 2.205
kPa psi 0.14504
cm in. 0.3937
mm mil (1 mil = 1/1000 in.) 39.37
m/s ft/min 196.9
kg/L Ibm/gal, liq(U.S.) 8.345
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List of Abbreviations and Acronyms
ACGIH American Conference of Governmental Industrial Hygienists
ACS American Chemical Society
ANSI American National Standards Institute
AOAC Association of Official Analytical Chemists
ASQC American Society for Quality Control
ASTM American Society for Testing and Materials
CCEP Coatings and Coating Equipment Program
CTC Concurrent Technologies Corporation
DFT dry film thickness
DI deionized
DOI distinctness-of-image
EP empty pan
EPA U.S. Environmental Protection Agency
ES empty syringe
ETF Environmental Technology Facility
ETV Environmental Technology Verification
FBO Federal Business Opportunities (FedBizOpps.gov)
FS full syringe
GVP Generic Verification Protocol
HAP hazardous air pollutant
ID identification
IR infrared
ISO International Standardization Organization
MEK methyl ethyl ketone
NDCEE National Defense Center for Environmental Excellence
NIST National Institute for Standards and Technology
P2 pollution prevention
PEA Performance Evaluation Audit
PS mass of pan with deposited solids
QA/QC quality assurance/quality control
QMP Quality Management Plan
RFT Request for Technologies
RPD Relative Percent Difference
RSD Relative Standard Deviation
SOP Standard Operating Procedures
SRM standard reference material
TBD to be determined
TQAPP Testing and Quality Assurance Project Plan
UV ultraviolet
VOC volatile organic compound
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1.0 INTRODUCTION
1.1 Purpose of the UV-Curable Coatings Generic Verification Protocol
The primary purpose of this document is to establish the Generic Verification Protocol
(GVP) for ultraviolet (UV)-curable coatings, to be referred to as the UV-Curable Coatings GVP.
The secondary purpose is to establish the generic format and guidelines for product specific
Testing and Quality Assurance Project Plans (TQAPPs) that relate to this GVP.
Environmental Technology Verification Coatings and Coating Equipment Program (ETV
CCEP) pilot product-specific TQAPPs will establish the specific data quality requirements for all
technical parties involved in each project. A defined format, as described below, is to be used for
all ETV CCEP UV-Curable Coatings TQAPPs to facilitate independent reviews of project plans
and test results, and to provide a standard platform for communicating with stakeholders and
participants.
1.2 Quality Assurance for the ETV CCEP
Projects conducted under the auspices of the ETV CCEP will meet or exceed the
requirements of the American National Standards Institute/American Society for Quality Control
(ANSI/ASQC), Specifications and Guidelines for Quality Systems for Environmental Data
Collection and Environmental Technology Programs, ANSI/ASQC E-4 (1994) standard.1 This
GVP will ensure that project results are compatible with and complementary to similar projects.
All ETV CCEP UV-Curable Coatings TQAPPs are adapted from this standard, the ETV Program
Quality Management Plan (QMP), and the ETV CCEP QMP.2'3 These TQAPPs will contain
sufficient detail to ensure that measurements are appropriate for achieving project objectives, that
data quality are known, and that the data are reproducible and legally defensible.
1.3 Organization of the UV-Curable Coatings GVP
This GVP contains the sections outlined in the ANSI/ASQC E-4 standard. As such, this
GVP identifies processes to be used, test and quality objectives, measurements to be made, data
quality requirements and indicators, and procedures for the recording, reviewing and reporting of
data.
The major technical sections discussed in this GVP are as follows:
Project Description
Project Organization and Responsibilities
Quality Assurance (QA) Objectives
Site Selection and Sampling Procedures
Analytical Procedures and Calibration
Data Reduction, Validation and Reporting
Internal Quality Control (QC) Checks
Performance and System Audits
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Calculation of Data Quality Indicators
Corrective Action
Quality Control Reports to Management
Appendices
1.4 Formatting
In addition to the technical content, this GVP also contains standard formatting elements
required by the ANSI/ASQC E-4 standard and Concurrent Technologies Corporation (CTC)
deliverables. Standard format elements include, at a minimum, the following:
Title Page
TQAPP Approval Form
Table of Contents
Document Control Identification (in the plan header):
Section No.
Revision No.
Date:
Page: of
1.5 Approval Form
Key ETV CCEP personnel will indicate their agreement and common understanding of
the project objectives and requirements by signing the TQAPP Approval Form for each piece of
equipment tested. Acknowledgment by each key person indicates commitment toward
implementation of the plan. Figure 1 shows the Approval Form format to be used.
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APPROVAL FORM
Date Submitted:
QTRAKNo.:
Revision No.:
Project Category:
Title:
Project/Task Officer:
EPA/Address/Phone No.:
U.S. EPA-
U.S. DCC-W
Interagency
Agreement No.:
U.S. ARC/
NDCEE
Contract No.:
Task No.
APPROVALS
ETV CCEP Project Manager
Signature
Date
ETV CCEP QA Officer
Signature
Date
ETV EPA Project Manager
Signature
Date
ETV EPA Project QA Manager
Signature
Date
EPA - Environmental Protection Agency
DCC-W - Defense Contracts Command - Washington
AEC - Army Environmental Center
Figure 1. Testing and Quality Assurance Project Plan Approval Form
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2.0 PROJECT DESCRIPTION
2.1 General Overview
Organic finishing processes are used by many industries for the protection and decoration
of their products. Organic coatings contribute nearly 20 percent of total stationary area source
volatile organic compound (VOC) emissions as well as a significant percentage of air toxic
emissions. Alternatives, such as UV-curable coatings, are continually being developed by many
sources in an effort to reduce any detrimental effects to the environment. Often these UV-
curable coatings are slow to penetrate the market because potential users, especially an ever-
growing number of small companies, do not have the resources to test UV-curable coatings on
their particular application and may be constructively skeptical of the UV-curable coating
provider's claims. If an unbiased, third party facility could provide pertinent test data,
environmentally friendlier coatings would penetrate the industry faster and accelerate
environmental improvements. UV-curable coatings require a specific type of energy (i.e., light
energy with a wavelength of approximately 400 nm, or in the UV spectrum) to initiate chemical
cross-linking of the coatings components. Thermal energy alone may cause any volatiles to
evaporate from the coating, but thermal energy alone will not cause the coating to cure. Typical
curing equipment includes a source of UV light and a mechanism to convey the 'wet' surfaces
past the UV source.
The ETV CCEP is a partnership between the U.S. Environmental Protection Agency
(EPA) and the National Defense Center for Environmental Excellence (NDCEE) Program and is
managed by CTC of Johnstown, PA. It has been established to provide unbiased, third party
environmental performance data. The ETV CCEP has been tasked to develop, and subsequently
utilize, a series of standardized protocols to verify the performance characteristics of coatings and
coating equipment. This GVP enables verification of the performance of UV-curable coatings.
To maximize the ETV CCEP's exposure to the coatings industry, the data from the
verification testing will be made available on the Internet at the EPA's ETV Program website
(http://www.epa.gov/etv/) under the P2 Innovative Coatings and Coating Equipment Pilot as well
as through other sources (e.g., publications, seminars). This will help establish the ETV CCEP's
reputation in the private sector. A long-range goal of this initiative is to become a vital resource
to the industry and, thus, self-sustaining through private support. This is in addition to its
primary objective of improving the environment by rapidly introducing more environmentally
friendly coating technologies into the industry.
2.7.7 Coating Application and Curing Test Location
CTC, through NDCEE, does not currently possess equipment to cure UV-reactive
coatings. The coating application and curing of these materials must be conducted offsite.
Regardless of the test location, arrangements will be made to ensure the requirements of the
TQAPP, ETV CCEP QMP, and ETV Program QMP and all associated QA procedures are
completed. ETV CCEP staff will conduct a site survey and pretest audit of the offsite test
location and equipment to ensure that all the QA/QC requirements are met. The ETV CCEP
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staff will also oversee all coating application and curing procedures, transport the standard test
panels from the test location and CTC as needed, measure all process variables, conduct any
offsite laboratory analyses, and package the standard test panels for transport to the NDCEE
Environmental Coatings Laboratory. The ASTM D 5403 analysis of total volatile content will be
used to determine the environmental impact of the UV-curable coating. The ETV CCEP
personnel will determine processing volatiles at the offsite test location, but the determination of
potential volatiles will be completed at CTC.
2.1.2 NDCEE Environmental Coatings Laboratory Facilities
In support of the ETV CCEP, the NDCEE's extensive state-of-the-art Environmental
Coatings Laboratory facilities will be available to evaluate the cured standard test panels.
Laboratory facilities available from the NDCEE are described in Table 1.
Table 1. Testing and Laboratories and Representative Laboratory Equipment Holdings
Laboratory
Environmental Testing
Destructive and
Nondestructive
Evaluation
Materials and
Mechanical Testing
Powder Metallurgy
Intelligent Processing of
Materials
Risk & Environment
Analysis
Calibration Laboratory
Focus
1) Identification and quantification of
biological, organic, and inorganic
chemicals and pollutants to all media.
2) Industrial process control chemical
analysis.
Evaluation of product and process
performance, and surface cleanliness.
Measurement of service and processing
material and mechanical properties.
Investigation of powder properties.
Development and evaluation of
embedded process sensors.
Management, monitoring, and evaluation
of material and process alternatives from
health and safety perspective.
Calibration of equipment, sensors, and
components to nationally traceable
standards.
Laboratory Equipment
Hewlett Packard 5972A GC/MS
Varian Liberty 110 Sequential ICP
P-E 4100ZL Graphite Furnace
Mitsubishi GT06 Autotitrator
P-E Headspace GC/ECD/FID
TOC/Flashpoint/pH/Conductivity
Graseby 2010 Isokinetic Stack Analyzer
Graseby 2800 VOST Stack Sampler
Questron Q-Wave 1000 Microwave
Leeman PS200/AP200 Mercury Stations
Millipore TCLP/ZHE Extraction Station
Lachat Quickchem Flow Injection Analyzer
Optically Stimulated Electron Emission
X-ray/Magnetic/Eddy Current Thickness
Salt Spray Corrosion Chamber
Microhardness/Tensile/Fatigue/Wear
Noran and CAMScan Electron Microscopes
Leco 2001 Image Analysis System
Nikon and Polaroid Light Optical Microscopes
EDAX Energy Dispersive Spectrometer
Single Crystal Imaging
Metallography Polishing/Grinding/Etching
MTS Machines
Tinius Olsen Testers
Impact Testers
Horiba LA900 Laser Particle Size Analyzer
Autopore II 9020 Mercury Porosimeter
Accupyc 1330 Pycnometer
Gemini II 2370 Surface Area Analyzer
TEC Model 1600 Stress Analyzer
Spectraphysics Argon & ND: YAg Lasers
Resonance Frequency System
Biosym: molecular modeling software
MOP AC, Extend, HSC Chemistry, Riskpro,
Sessoil, and GIS software packages
Transmation Signal Calibrator (milliamps,millivolts)
Thermacal Dry Block Calibrator (Temperature)
Druck Pressure Calibrator (Pressure)
Fluke Digital Multimeter (Voltage)
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2.1.3 Statement of Project Objectives
The overall objective of the ETV CCEP is to verify pollution prevention (P2)
characteristics and performance of coatings and coating equipment technologies, and to make the
results of the verification tests available to prospective technology users. The ETV CCEP aspires
to increase the use of more environmentally friendly technologies in products finishing in an
effort to reduce emissions.
2.2 Technical/Experimental Approach and Guidelines
The following tasks are proposed for tests completed according to this GVP:
Develop product-specific TQAPP
Conduct verification and baseline (as needed) tests
Prepare the Verification Report and Data Notebook
Prepare the Verification Statement for approval and distribution
Table 2 describes the general guidelines and procedures that will be applied to each TQAPP.
Table 2. Overall Guidelines and Procedures Applied to this GVP
A detailed description of each part of the test will be given.
Critical and noncritical factors will be listed. Noncritical factors will be held constant
throughout the testing. Critical factors will be listed as control (process) factors or
response (coating product quality) factors.
The product-specific TQAPPs will identify the testing site.
The testing will be under the control and close supervision of ETV CCEP
representatives to ensure the integrity of the third party testing.
The QA portions of this GVP will be strictly adhered to.
A statistically significant number of samples will be analyzed for each critical response
factor. Variances (or standard deviations) of each critical response factor will be
reported for all results.
2.2.1 Test Approach
The following approach will be used for this GVP:
The vendor will identify the performance parameters to be verified and
recommend the optimum equipment settings for application and curing;
The ETV CCEP will obtain enough test panels for the verification and baseline
tests;
The ETV CCEP will obtain the baseline coatings (as appropriate);
The vendor will provide the UV-curable coating being verified;
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Data such as dry film thickness (DFT), gloss, and visual appearance will be
collected, following American Society for Testing and Materials (ASTM)
methods, or equivalent (see Appendix B);
A statistically valid test program that efficiently accomplishes the required
objectives will then be used to analyze the test results.
2.2.2 Verification Test Objectives
The objectives of the verification tests performed per this protocol are to determine the
total volatile content per ASTM D 5403 and to verify the quality and durability of UV-curable
coatings. The coated test panels will be checked for DFT, visual appearance, and at least three of
the following analyses: gloss, color, distinctness-of-image (DOT), adhesion, corrosion resistance
(salt spray), direct impact resistance, flexibility (mandrel bend), pencil hardness, humidity
resistance, weather resistance, abrasion resistance, and chemical resistance [methyl ethyl ketone
(MEK) rub]. The cost associated with each analysis (except the mandatory DFT and visual
appearance) will be presented to the participating vendors. The coating vendors will then choose
which optional tests they want to have performed on the panels prepared using their coating. The
coating vendor must choose a minimum of three optional tests. The total cost for completing
each verification test and the vendor's share of that cost will depend on the number and type of
analyses chosen. Additional pretreatment processes or tests that are either listed above or
requested by the vendor may be included at the expense of the UV-curable coating vendor.
2.2.3 Test Panels
The actual test panels may be fabricated from steel, stainless steel, glass, plastic, alloys,
wood, or composites based on the UV-curable coating vendor's recommendations. All steel
panels will be commercially available and pretreated with zinc phosphate prior to coating
application unless otherwise specified in the individual TQAPP. Details concerning panel
characteristics, pretreatment, and pretreatment analysis will be identified in each product-specific
TQAPP. The quality of any substrate pretreatment will be evaluated before shipment to the test
site to ensure that the substrate panels meet specifications. However, the default standard test
panel, as is shown in Appendix A, Default Standard Test Panel, will be 30.5 cm (12 in.) long
and 10.2 cm (4 in.) wide with 0.6-cm (0.25-in.) hole punched in one end so that it may be
suspended from a hook. Other parts may be treated and tested at the expense of the UV-curable
coating vendor.
2.2.4 Coating Specification
The UV-curable coatings submitted for verification testing should provide an
environmental benefit over the existing coatings currently in use in each UV-curable coating's
target industry. The stakeholders group will also review the UV-curable coatings to determine
their status as innovative coatings.
Each coating vendor will supply its test coating and respective specifications for the
verification test. In addition, each vendor will supply a sufficient amount of coating to complete
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the verification tests, the exact preparation instructions, and the instructions/parameters for
applying the coating. The application procedures and conditions must be typical of the actual
target industry.
2.2.5 UV Curing Apparatus
A suitable UV curing coating application apparatus, based on suggestions from the UV-
curable coating provider, will be used to apply the UV-curable coating to test panels (and any
other part requested by the coating provider in the TQAPP). A thickness range will be
designated for each UV-curable coating as well as curing conditions.
Before the test, a set of dummy panels will be coated to ensure that the equipment
parameters are set correctly. The fluid delivery pressure will be monitored periodically
throughout the test. The paint usage may be determined through gravimetric means.
To help ensure proper equipment setup and operation, the UV-curable coatings vendors
will be invited to participate in the startup phase of the testing and to observe the testing of their
coatings. Each product-specific TQAPP will provide background to vendors for their test.
2.2.6 Coating Baseline Test
A coating baseline test may be performed for a coating that is submitted for verification
as appropriate. The coating baseline will be used to determine the relative environmental and
performance benefits of the UV-curable coating being verified. The coating baseline panels will
also be evaluated for DFT, visual appearance, and the same optional tests chosen by the coating
vendor for the verification test.
The coating baseline will use an existing coating and application method that is consistent
with the verified technology's target industry. The coating baseline testing will be designed and
performed by the ETV CCEP personnel. Certain operating parameters used for the coating
baseline will be identical to the parameters used for the UV-curable coating verification test.
Other parameters will be developed from the application equipment's or coating manufacturer's
recommendations and experimental trials performed by the ETV CCEP.
2.2.7 Design of Experiment
This test protocol will verify the performance of UV-curable coatings submitted in
response to the associated Federal Business Opportunities (FedBizOpps.gov) (FBO) notice or
Request for Technologies (RFT). A mean value and variance (or standard deviation) will be
reported for each critical response factor. If a UV-curable coating vendor makes a claim about a
particular coating characteristic, the vendor of the coating will be asked to submit a confidence
limit and specification limit (acceptable quality limit) for that claim for verification purposes. If
the vendor does not submit a confidence and specification limit, a default 95% confidence limit
will be applied. Any claims made by the coating vendor regarding particular coating
characteristics will be used in the design of experiments. The appropriate number of test panels
to be coated and analyzed is based on the confidence limit, specification limit, and the
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appropriate statistical test to be applied to the results (i.e., Student's T-Test, Chi Square Test, or
F-Test). Typically, as a default scenario, each verification test will consist of five runs with one
rack of eight panels in a single row per run. The statistical analyses for all response factors will
be carried out using Minitab statistical software.
Prior to the verification test, setup panels will be coated to ensure that the equipment
parameters are correct. In actual verification testing, one panel per run will be removed for
pretreatment analysis, and a predetermined number of panels (five runs with one rack of eight
panels) will be coated to determine the P2 benefit and finish quality. Specifically, the standard
test panels coated during the verification test will be analyzed for their chemical and physical
properties as well as appearance.
If requested in the RFT or FBO response, the coating vendor can supply five additional
parts to be coated during each verification test run. Fixturing of parts will be determined after
the coating vendor submits parts, and vendors are bound by the part size and weight restrictions
of the offsite test facility.
2.2.5 Performance Testing
UV-curable coating vendors will provide the ETV CCEP with coating specifications and
appropriate equipment settings. The ETV CCEP will not attempt to optimize test settings during
the actual test runs; however, the coating vendors will be given the opportunity to do so during
the startup phase of the testing. The ETV CCEP will provide the UV-curable coating vendors
with a list of key noncritical test factors that may affect the test results). Depending on the nature
of the vendor's coating technology, this list may not address all of the factors that could impact
the test results.
All testing will be conducted on the coated standard panels. All such tests will be
performed per ASTM procedures and provide insight to the chemical and physical properties of
the coatings. A comparison will be made from panel to panel and run to run.
2.2.9 Quantitative Measurements
In order to evaluate the environmental benefit and the finish quality obtained by using the
UV-curable coating, several measurements will be taken on the coating, and noncoated and
coated test panels. Coating samples will be analyzed for total volatile content, which includes
VOCs and hazardous air pollutants (HAPs). Noncoated panels will be checked for surface area
and pretreatment. Coated panels will be checked for DFT and visual appearance.
2.2.10 Participation
The vendor of the technology being verified is welcome to participate in the startup
phase and observe the verification testing. The ETV CCEP personnel will be responsible for
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performing all necessary tests and verifications required for performance evaluation. For safety
purposes, the vendor staff may operate the UV curing equipment.
2.2.11 Critical and Noncritical Factors
In a designed experiment, critical and noncritical control factors must be identified. In
this context, the term "critical" does not convey the importance of a particular factor.
(Importance can only be determined through experimentation and characterization of the total
process.) Rather, this term displays its relationship within the design of experiments. For the
purposes of this protocol, the following definitions will be used for critical control factors,
noncritical control factors, and critical response factors.
Critical control factor - a factor that is varied in a controlled manner within a design
of an experiment to determine its effect on a particular outcome of a system.
Noncritical control factors - factors that remain relatively constant or are randomized
throughout the testing.
Critical response factors - the measured outcomes of each combination of critical and
noncritical control factors used in the design of experiments.
In the case of the verification testing of a coating, there is only one critical control factor,
and that is the coating itself. All other processing factors are noncritical control factors;
therefore, the multiple runs and sample measurements within each run for each critical response
factor will be used to determine the amount of variation expected for each critical response
factor. For example, for each coating application, parameters associated with pretreatment would
remain constant, and, thus, be noncritical control factors; however, a parameter, such as
adhesion, would be identified as a critical response factor and could vary from run to run.
Tables 3 through 5 identify the factors to be monitored during testing as well as their
acceptance criteria (where appropriate), data quality indicators, measurement locations, and
measurement frequencies. The values in the "Total Numbers" column are based on the default
test scenarios.
TableS. Critical Control Factors
Critical Control Factor
UV-Curable Coating
Resin Type
TBD
Solvent Type
TBD
Cure Method
TBD
Target Industry
TBD
TBD - To be determined
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Table 4. Noncritical Control Factors
Noncritical
Factor
Application Method
(Manufacturer/Model)
Input Air Pressure to Gun
or Pot
Product Involved in Testing
Coating Delivery Pressure
Pretreatment Analysis
Surface Area of Test Panels
Ambient Factory Relative
Humidity
Ambient Factory
Temperature
Booth Relative Humidity
Booth Temperature
Spray Booth Airflow
(Face Velocity)
Temperature of Panels, as
Coated
Distance to Panels
Horizontal Gun Traverse
Speed
Vertical Drop Between
Passes
Volatile Content of Applied
Coating
Density of Applied Coating
Weight % Solids of
Applied Coating
Coating Temperature, as
Applied
Coating Viscosity, as
Applied
Cure Time
Set Points/
Acceptance
Criteria
From coating and
equipment providers
From coating provider
Standard Test Plan
(material TBD)b
From coating provider
Varies <1 .2 g/m
TBD
Varies <10%
During test
Varies <5 °C during test
Varies <10%
During test
Varies <5 °C during test
0.40.6 m/s
(80-120 ft/min)
Varies <5 °C during test
Varies <1.3 cm
(<0.5 in.) during test
TBD
TBD
Varies <5% for each
coating
Varies <50 g/L during
test
Varies <5% during test
Varies <5 °C during test
Varies <5 seconds during
test
TBD
Measurement Location
Factory floora
Factory floor
Factory floor
Factory floor
Coatings laboratory
Factory floor
Factory floor
Factory floor
Factory floor
Factory floor
Factory floor
Factory floor
Factory floor
Factory floor
Factory floor
Coatings laboratory
Coatings laboratory
Coatings laboratory
Coatings laboratory
Coatings laboratory
Factory floor
Frequency
Once per test
Once per test
Default scenario
in Section 5.2
Once per run
Once per run
Once per test
Once per run
Once per run
Once per run
Once per run
Once per run
Once per run
Once per test
Once per test
Once per test
Once per run
Once per run
Once per run
Once per run
Once per run
Once per run
Total
Number for
the Test
1
1
40 panels
5
5
1
5
5
5
5
5
5
1
1
1
5
5
5
5
5
5
a At offsite test facility
b TBD - To be determined
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Table 5. Critical Response Factors
Critical Response
Factor
Measurement
Location or Method
Frequency
Total Number
for the Test
Environmental
Total Volatile Content
Energy Usage of the UV
Lamps
ASTM D 5403
(offsite and at CTC)
Calculated from total
lamp wattage and total
cure time
5 samples from coating batch
used during test
Once per run
5
5
Quality /Durability (mandatory for all coatings)
Dry Film Thickness (DFT)
(Magnetic Method)
Visual Appearance
ASTM B 499
Entire test panel
TBDa
1 per panel
TBD
40
Quality /Durability (optional)
Gloss
Color"
Distinctness-of-image
(DOI)C
Adhesion4
Pencil Hardness4
Corrosion Resistance
(Salt Spray)
Direct Impact
Mandrel Bend
Chemical Resistance
[Methyl Ethyl Ketone
(MEK) Rub]
Humidity Resistance
Weather Resistance
Abrasion Resistance
ASTM D 523
ASTM D 1729 or
ASTM D 2244
ASTM D 5767 Test
Method B
ASTM D 3359
ASTM D 3363
ASTMB 117
ASTM D 2794
ASTM D 522
ASTM D 5402
ASTM D 1735
ASTM G 26
ASTM D 4060
One random panel per run
One random panel per run
One random panel per run
One random panel per run
One random panel per run
One random panel per run
One random panel per run
One random panel per run
One random panel per run
One random panel per run
One random panel per run
One random panel per run
5
5
5
5
5
5
5
5
5
5
5
5
a TBD - to be determined
b Both color analyses will use the same panel if both are selected.
c The sliding combed shutter is replaced by a rotating eight-bladed disc.
d The adhesion and pencil hardness tests will all be performed on the same panel as the DFT test.
Some target factors that may be used to test UV-curable coatings include:
Equipment preparation
Spray pattern
Number of passes
Dwell time between passes
Number of coats
Flash time between coats
Target dry film thickness (DFT)
TBD
TBD
TBD
TBD
TBD
TBD
TBD
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2.2.12 Determination of Total Volatile Content of the UV-Curable Coating
This verification test will use ASTM D 5403, Test Method A, which will determine the
Total Volatile Content by the following procedure:
Test substrates will be heavy gage aluminum foil
Test substrates will be in the shape of square pans with approximately 2 cm tall sides
Test substrates will measure approximately 10 cm by 30 cm
Weigh prepared test substrate (without coating) [A]
Deposit UV-curable coating onto test substrates to a maximum of 1 mil wet film
thickness using a syringe (minimum of 0.2 g)
Weigh the coated test substrate [B]
Cure coated substrate according to manufacturer's specifications
Weigh the cured test substrate [C]
Heat cured test substrate at 110 ± 5 °C for 60 minutes
Weigh test substrate after cooling [D]
% Processing Volatiles =100 [(B - C) / (B - A)]
% Potential Volatiles = 100 [(C - D) / (B - A)]
Total Volatile Content = % Processing Volatiles + % Potential Volatiles
2.3
Schedule
ETV CCEP uses standard tools for project scheduling. Project schedules are prepared in
Microsoft Project. Project schedules show the complete work breakdown structure of the
project, including technical work, meetings and deliverables. Table 6 shows the estimated
schedule for the testing of UV-curable coatings.
Table 6. Estimated Schedule as of 9/26/2003
ID
Taskl
Task 2
TaskS
Task 4
TaskS
Task 6
Name
Approval of TQAPP
Verification Testing
Complete Data Analyses
Prepare Verification Report
Approval of Verification Report
Issue Verification Statement
Duration
10 days
10 days
20 days
30 days
30 days
15 days
Start Date
TBD
TBD
TBD
TBD
TBD
TBD
Finish Date
TBD
TBD
TBD
TBD
TBD
TBD
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3.0 PROJECT ORGANIZATION AND RESPONSIBILITIES
ETV CCEP, through its agreement with CTC, performs verification testing of
environmentally beneficial technologies. The laboratory supports the ETV CCEP project
manager and the ETV CCEP project leader by providing test data. Laboratory analysts report to
the ETV CCEP laboratory leader. The ETV CCEP laboratory leader and organic finishing
engineer coordinate with the ETV CCEP project leader on testing schedules. The ETV CCEP
project leader is the conduit between the laboratory and the ETV CCEP project manager. The
ETV CCEP project leader answers directly to the ETV CCEP project manager. For the ETV
CCEP, the ETV CCEP project leader will be responsible for preparing the TQAPPs, Verification
Report and Statement, and Data Notebook for each test.
The ETV CCEP QA officer, who is independent of both the laboratory and the program,
is responsible for administering ETV and ETV CCEP QMP policies and CTC policies developed
by its quality committee. These policies provide for, and ensure that quality objectives are met
for each project. The policies are applicable to laboratory testing, factory demonstration
processing, engineering decisions, and deliverables. The ETV CCEP QA officer reports directly
to CTC senior management and is organizationally independent of the project or program
management activities.
The project organization chart, showing lines of responsibility and the specific CTC
personnel assigned to this project, is presented in Figure 4. A summary of the responsibilities of
each CTC participant, his/her applicable experience, and his/her anticipated time dedication to
the project during testing and reporting is given in Table 7.
ETV CCEP Project Leader
Robert Fisher
-Julie Napotnik
ETV CCEP Laboratory
Leader
Lynn Summerson
Organic Finishing
Stephen Kendera
Brian Albright
Figure 2. Project Organization Chart
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Table 7. Summary of Current ETV CCEP Experience and Responsibilities
Key CTC Personnel and Roles
Fred Mulkey
NDCEE Program Director
Brian Schweitzer
Manager, Process Engineering/
ETV CCEP Project Manager
Jacob Molchany - ETV CCEP
QA Officer
Robert Fisher - Staff Process
Engineer/ ETV CCEP Project
Leader
Julie Napotnik - Assistant
Process Engineer/ ETV CCEP
Project Team
Stephen Kendera Sr. Organic
Finishing Technician
Lynn Summerson - ETV CCEP
Laboratory Leader/Statistical
Support Staff
Brian Albright - ETV CCEP
Assistant Laboratory Analyst
Responsibilities
Manages NDCEE Program
Accountable to CTC Technical Services
Manager and CTC Corporate Management
Responsible for overall ETV CCEP
technical aspects, budget, and schedule
issues on daily basis
Accountable to NDCEE Program Director
Responsible for overall project QA
Responsible for establishing the QA audit
checklist.
Accountable to NDCEE Program Director
Technical project support
Process design and development
Accountable to ETV CCEP Project
Manager
Conducts site survey and oversees
coating application / curing procedures.
Technical project support
Process design and development
Accountable to ETV CCEP Project
Manager
Performs day-to-day operations of the
Organic Finishing Line
Accountable to Finishing Engineer
Laboratory analysis / pre-test QA audit
Accountable to ETV CCEP Project
Manager
QC Analysis
Accountable to ETV CCEP Laboratory
Leader
Applicable Experience
Laboratory Chemist and Manager
(15 years)
Project Quality Assurance (15
years)
Project Management (14 years)
Registered Environmental Manager
Process Engineer (14 years)
Project Manager, Organic Finishing
(9 years)
Industrial QA/QC and (14 years)
Quality Mgmt. /ISO 9000 (8 years)
Environmental Compliance and ISO
14000 Management Systems (8 years
Certified Hazardous Materials Mgr.
Organic Finishing Regulations
(9 years)
Organic Finishing Operations
(6 years)
Professional Engineer
Organic Coating Systems (3 years)
Process Engineer (4 years)
Industrial Paint and Coatings
Experience (28 years)
Industrial and Environmental
Laboratory Testing (20 years)
Environmental and QC Testing
(7 years)
Education
M.S., Chemistry
B.S., Chemistry
B.S., Mechanical
Engineering
B.S., Industrial
Engineering
B.S., Chemical
Engineering
B.S., Geo-
Environmental
Engineering
M.S., Chemistry
B.S., Chemistry
B.S., Chemistry
Time
Dedication
5%
25%
5%
50%
50%
10%
20%
10%
The ETV CCEP personnel specified in Table 7 are responsible for maintaining
communication with other responsible parties working on the project. The frequency and
mechanisms for communication are shown in Table 8. In addition, the individuals listed in Table
9 will have certain responsibilities during the testing phase.
Each product-specific TQAPP will document the roles and responsibilities of offsite
personnel.
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Table 8. Frequency and Mechanisms of Communications
Initiator
NDCEE Program Director,
ETV CCEP Project
Manager, or ETV CCEP
Project Leader
ETV CCEP Project
Manager
ETV CCEP Laboratory
Leader
ETV CCEP Project Leader
ETV CCEP QA Officer
EPA ETV CCEP Project
Manager
Recipient
EPA ETV CCEP Project
Manager
NDCEE Program Director
ETV CCEP Project Leader
ETV CCEP Project
Manager
NDCEE Program Director
CTC
Mechanism
Written Report
Verbal Status Report
Written or Verbal Status
Report
Data Reports
Written or Verbal Status
Report
Quality Review Report
Onsite Visit
Frequency
Monthly
Weekly
Weekly
As Generated
Weekly
As Required
At Least Once per
Year
Special Occurrence
Schedule or Financial
Variances
Major Quality Objective
Deviation (will prevent
accomplishment of
verification cycle testing)
Initiator
NDCEE Program Director
or ETV CCEP Project
Manager
NDCEE Program Director
or ETV CCEP Project
Manager
Recipient
EPA ETV CCEP Project
Manager
EPA ETV CCEP Project
Manager
Mechanism/
Frequency
Telephone Call,
Written Follow-up
Report as Necessary
Telephone Call with
Written Follow-up
Report
Table 9. Responsibilities During Testing
Position
ETV CCEP Project Manager
ETV CCEP QA Officer
ETV CCEP Project Leader
Statistical Support
Responsibility
Overall coordination of project
Audits of verification testing operations and laboratory
analyses
Overall coordination of testing, reporting, and data review
Coordinates interpretation of test results
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4.0 QUALITY ASSURANCE OBJECTIVES
4.1 General Obj ectives
The overall objectives of this ETV CCEP GVP are to verify the performance of UV-
curable coatings by establishing their environmental benefit and by documenting the applied
coating's finish quality. These objectives will be met by controlling and monitoring the critical
and noncritical factors, which are QA objectives for each technology-specific TQAPP based on
this GVP. Tables 3 and 4 list the critical and noncritical control factors, respectively.
The analytical methods that will be used for coating evaluations are adapted from ASTM
Standards, or equivalent. The QA objectives of the project and the capabilities of these test
methods for product and process inspection and evaluation are synonymous because the methods
were specifically designed for evaluation of the coating properties under investigation. The
methods will be used as published, or as supplied, without major deviations unless noted
otherwise. The specific methods to be used for this project are attached to this document as
Appendix B (ASTM Methods).
4.2 Quantitative Quality Assurance Objectives
Quality assurance parameters such as precision and accuracy are presented in Tables 10
and 11. Table 10 presents the manufacturers' stated capabilities of the equipment used for
measurement of noncritical control factors typically used by ETV CCEP. Control factors and
equipment will be updated in product-specific TQAPPs should other equipment be used. The
precision and accuracy parameters listed are relative to the true value that the equipment
measures. Table 11 presents the precision and accuracy parameters for the critical response
factors. The precision and accuracy are determined using duplicate analysis and known standards
or spiked samples and must fall within the values found in the specific methods expressed.
The ETV CCEP will coordinate efforts to statistically interpret test results and QA
objectives.
4.2.1 Accuracy
Standard reference materials, traceable to national sources such as the National Institute
for Standards and Technology (NIST) for instrument calibration and periodic calibration
verification, will be procured and utilized where such materials are available and applicable to
this project. For reference calibration materials with certified values, acceptable accuracy for
calibration verification will be within the specific guidelines provided in the method if
verification limits are given. Otherwise, 80 to 120 percent of the true reference values will be
used (see Tables 10 and 11). Reference materials will be evaluated using the same methods as
for the actual test specimens.
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Table 10. QA Objectives for Precision, Accuracy and Completeness for All Noncritical
Control Factor Performance Analyses
Measurement
Input Air Pressure to Gun or Pot
Product Involved in Testing
Coating Delivery Pressure
Pretreatment Analysis
Surface Area of Test Panels
Ambient Factory Relative
Humidity
Ambient Factory Temperature
Booth Relative Humidity
Booth Temperature
Spray Booth Airflow
(Face Velocity)
Temperature of Panels, as
Coated
Distance to Panels
Horizontal Gun Traverse Speed
Vertical Drop Between Passes
Volatile Content of Applied
Coating
Density of Applied Coating
Weight % Solids of Applied
Coating
Coating Temperature, as Applied
Coating Viscosity, as Applied
Cure Time
Method
Pressure gauge
Test panels
Pressure gauge
ASTM B 767
Ruler
Thermal
hygrometer
Thermal
hygrometer
Thermal
hygrometer
Thermal
hygrometer
Per ACGIH
Infrared (IR)
thermometer
Ruler
Stopwatch
Ruler
ASTM D 3960
ASTMD 1475
ASTM D 2369
Thermometer
ASTMD 1200
Stopwatch
Units
psig
N/A
psig
g/m2
cm2
(ft2)
%
°C
%
°c
m/s
(ft/min)
°C
cm
(in.)
cm/s
(in./s)
cm
(in.)
g/L
(Ib/gal)
g/L
(lb /gal)
%
°C
Seconds
(#4 Ford Cup)
s
Precision
+ 0.5 psig
N/A
+ 0.5 psig
±0.005
±0.025
(± 0.0036)
± 3% of
full scale
± 3% of
full scale
± 3% of
full scale
± 3% of
full scale
±0.03*
(±5)
±0.13 °C
±0.15
(± 0.06)
±5%
±0.15
(± 0.06)
± 0.6%
± 0.6%
±1.5%
±0.5°C
± 10%
± 10%
Accuracy
+ 0.5%
N/A
+ 0.5%
±0.01
±0.025
(± 0.0036)
± 3% of
full scale
± 3% of
full scale
± 3% of
full scale
± 3% of
full scale
±0.03*
(±5)
±0.25 °C
±0.15
(± 0.06)
±5%
±0.15
(± 0.06)
±1.8%
±1.8%
± 4.7%
±0.2°C
± 10%
± 10%
Completeness
90%
100%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
ACGIHAmerican Conference of Governmental Industrial Hygienists, Inc.
* Accuracy and Precision stated by the manufacturer for velocities ranging from 20 to lOOft/t
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Table 11. QA Objectives for Precision, Accuracy and Completeness for All Critical Response
Factor Performance Analyses
Measurement
Total Volatile Content
Energy Usage of the U V
Lamps
Dry Film Thickness
(DFT) - Magnetic
Visual Appearance
Gloss
Color
Spectrometer
Spectral Light II
Distinctness-of-Image
(DOI)
Adhesion
Pencil Hardness
Corrosion Resistance
(Salt Spray)
Direct Impact
Mandrel Bend
Chemical Resistance
[Methyl Ethyl Ketone
(MEK) Rub]
Humidity Resistance
Weather Resistance
Abrasion Resistance
Method
ASTM D 5403,
Method A
Calculated
ASTM B 499
N/Ab
ASTM D 523
ASTMD 1729
ASTM D 2244
ASTM D 5767
Method B
ASTMD 3359
ASTMD 3363
ASTMB 117
ASTM D 2794
ASTM D 522
ASTM D 5402
ASTMD 1735
ASTM G 26
ASTM D 4060
Units
g/kg
(Ibm/lbm)
KW
mils3
N/A
Gloss units
AE Values
Visual
DOI units
Pass/Fail
and 0 to 5
rating
H-B scale
Pass/Fail
Pass/Fail
Pass/Fail
Visual
Pass/Fail
Pass/Fail
mg
Precision
2.3% per
ASTM
D5403
+ 10%
20%
N/A
20% RPDC
20% RPD
N/A
20% RPD
All pass or
all fail
N/A
All pass or
all fail
All pass or
all fail
All pass or
all fail
TBDby
ASTMd
All pass or
all fail
All pass or
all fail
46% RPD
Accuracy
Not reported
in ASTM
D5403
+ 10%
10% true
thickness
N/A
+ 0.3
+ 0.2 AE
N/A
+ 3 DOI
units
N/A
N/A
N/A
Ranges
listed in
ASTM
D2794
+ 15%
N/A
N/A
N/A
Not reported
in ASTM
D4060
Completeness
90%
90%
90%
100%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
a 1 mil = 0.001 in.
b N/A - Not applicable
c RPD - Relative Percent Difference
d TBD - to be determined
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4.2.2 Precision
The experimental approach of this GVP specifies guidelines for the number of test panels
to be coated. The analysis of replicate test panels for each coating property at each of the
experimental conditions will occur by design. The degree of precision will be assessed based on
the agreement of all replicates within a property analysis group.
4.2.3 Completeness
The coating facility and laboratory strives for at least 90 percent completeness.
Completeness is defined as the number of valid determinations expressed as a percentage of the
total number of analyses conducted, by analysis type.
4.2.4 Impact and Statistical Significance Quality Objectives
All process/facility measurements and laboratory analyses will meet the accuracy and
completeness requirements specified in Tables 10 and 11. The precision requirements also
should be achieved; however, a nonconformance may result from the analysis of replicates due to
limitations of the coating technology under evaluation, and not due to processing equipment or
laboratory error. Regardless, if any nonconformance from TQAPP QA objectives occurs, the
cause of the deviation will be determined by checking calculations, verifying the test and
measurement equipment, and reanalysis. If an error in analysis is discovered, reanalysis of a new
batch for a given run will be considered and the impact to overall project objectives will be
determined. If the deviation persists despite all corrective action steps, the data will be flagged as
not meeting the specific quality criteria and a written discussion will be generated.
If all analytical conditions are within control limits and instrument and measurement
system accuracy checks are valid, the nature of any nonconformance may be beyond the control
of the laboratory. If, given that laboratory quality control data are within specification, any
nonconforming results occur, the results will be interpreted as the inability of the coating
equipment undergoing testing to produce panels meeting the performance criteria at the given set
of experimental conditions.
4.3 Qualitative QA Objectives: Comparability and Representativeness
4.3.1 Comparability
Participating technologies will be operated per the vendor's recommendations. The data
obtained will be comparable from the standpoint that other testing programs could reproduce
similar results using a specific TQAPP. Coating and environmental performance will be
evaluated using EPA, ASTM, and other nationally or industry-wide accepted testing procedures
as noted in previous sections of this GVP. Process performance factors will be generated and
evaluated according to standard best engineering practices. In addition, vendors will be asked to
provide performance data for their product and the results of preliminary or prior testing relevant
to this GVP, if available.
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The characteristics of test panels coated during these tests will be compared to the
performance criteria and to other applicable end-user and industry specifications. The
specifications will be used to verify the performance of the participating technology. Additional
assurance of comparability comes from the routine use of precision and accuracy indicators as
described above, the use of standardized and accepted methods and the traceability of reference
materials.
4.3.2 Representativeness
The limiting factor to representativeness is the availability of a large sample population.
An experimental design has been developed so that this project will either have sufficiently large
sample populations or otherwise statistically significant fractional populations. The tests will be
conducted at optimum conditions based on the manufacturers' and the coating vendors' literature
and input and verified by setup testing. If the test data meet the quantitative QA criteria
(precision, accuracy, and completeness) then the samples will be considered representative of the
participating technology and will be used for interpreting the outcomes relative to the specific
project objectives.
4.4 Other QA Objectives
There are no other QA objectives as part of this evaluation.
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5.0 SITE SELECTION AND SAMPLING PROCEDURES
5.1 Site Selection
Innovative coatings will be tested on large pilot-scale/small production-scale equipment,
available at either the NDCEE facilities, at appropriate independent facilities, or the technology
vendor's facilities. The following factors will be used to determine whether it is more beneficial
to conduct a verification test at a non-NDCEE facility:
(1) Lack of appropriate equipment at the NDCEE facilities, which also would not be cost-
effective to acquire;
(2) Ease of access to other facilities with proper equipment at reasonable cost;
(3) Cooperative verifications [i.e., with the U.S. Army Environmental Center (USAEC)]
with significant cost sharing; and
(4) An expressed need from potential end users for testing conducted at an actual
manufacturing site.
The necessary equipment for UV-curable coating is not currently available at the
NDCEE. Therefore, an offsite location will be chosen that meets the requirements of this GVP,
the ETV CCEP QMP, and the ETV Program's QMP. ETV CCEP staff will collect all relative
test data during the coating application and curing operations at the offsite facility. Also,
qualified ETV CCEP personnel will conduct any additional laboratory analyses that require the
use of the curing equipment at the offsite facility. Test panels will be evaluated prior to
application and after curing by ETV CCEP using the NDCEE facility.
5.2 Sampling Procedures and Handling
Test panels will be used in this project. These will be prelabeled by marking their
identification (ID) number with permanent marker on the untreated side of the test panels. The
number of test panels processed during the testing depends on the experimental design, which in
turn, depends on any equipment provider's claim(s) about performance characteristics and the
respective confidence levels given in the responses to the RFT. If the UV-curable coating
provider requests no specific performance characteristics for verification, the default
experimental design will then be used. The default experimental design uses 40 panels for the
test (8 panels per rack, 1 rack per run, and 5 runs per test).
A factory operations technician and laboratory analysts will process the test panels
according to a preplanned sequence of stages identified in the product-specific TQAPP, which
includes those identified in Table 12.
A laboratory analyst will record the date and time of each run and the time each
measurement was taken. After curing, the test panels will be removed from the racks, separated
by a layer of packing material, and stacked for transport to the laboratory. Sample custody
documents will need to accompany the panels as they are transferred from the offsite processing
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facility to the laboratory. The laboratory analyst will process the test panels through the
laboratory login prior to performing the required analyses.
Table 12. Process Responsibilities
Procedure
Visual Inspection of Test Panels
Numbering of Test Panels
Arrange Test Panels on the Racks
Prepare the Coating
Setup the Application Equipment
Take Coating Samples and Measurements
Load Coating
Perform Setup Trials (before first run only)
Apply Coating to Test Panels
Take Process Measurements
Cure Test Panels
Wrap/Stack/Transfer Test Panels to Lab
Operations
Technician
X
X
X
X
X
X
X
Laboratory
Analyst
X
X
X
X
X
Samples of the coating will be gathered prior to each run to determine the volatile content
of the material. Samples that are to be transported back to the NDCEE ETF Laboratory will be
packaged separately by run and analyzed as distinct batches. The coating samples will be
packaged in a way that prevents exposure to ambient UV energy.
Panels that have been coated and cured will be packaged and transported to the NDCEE
ETF Laboratory for analyses. All appropriate measures will be taken to assure that the applied
coating is not damaged during transport. All custody changes will require that a custody log be
completed and signed.
5.3 Sample Custody, Storage and Identification
The test panels will be given a unique laboratory ID number and logged into the
laboratory record sheets. The analyst delivering the test panels will complete a custody log
indicating the sampling point IDs, sample material IDs, quantity of samples, time, date, and
analyst's initials. The test panels will remain in the custody of ETV CCEP, unless a change of
custody form has been completed. The change of custody form should include a signature from
ETV CCEP, the test product ID number, the date of custody transfer, and the signature of the
individual to whom custody was transferred.
Laboratory analyses may only begin after each test product is logged into the laboratory
record sheets. The laboratory's sample custodian will verify this information. Both personnel
will sign the custody log to indicate transfer of the samples from the coating processing area or
offsite location to the laboratory analysis area. The laboratory sample custodian will log the test
panels into a bound record book; store the test panels under appropriate conditions (ambient
room temperature and humidity); and create a work order for the various laboratory departments
to initiate testing. The product evaluation tests also will be noted on the laboratory record sheet.
Testing will begin within several days of coating application.
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6.0 ANALYTICAL PROCEDURES AND CALIBRATION
6.1 Facility and Laboratory Testing and Calibration
ETV CCEP, in conjunction with the NDCEE, shall maintain a record of calibrations and
certifications for all applicable equipment. Testing and measuring equipment shall be calibrated
prior to the verification test and checked for accuracy after the verification test analyses are
complete.
6.1.1 Facility Testing and Calibration
Calibration procedures for ETV CCEP within the NDCEE testing facility and laboratory
shall be recorded. Certified solutions and reference materials traceable to NIST shall be obtained
as appropriate to ensure the proper equipment calibration. Where a suitable source of material
does not exist, a secondary standard is prepared and a true value obtained by measurement
against a technical-grade NIST-traceable standard.
After the coating is mixed, the temperature and viscosity of the coating will be measured.
In addition, coating samples will be taken to the lab for density and percent solids analyses. A
listing of ASTM Methods can be found in Appendix B. All equipment used during facility
testing is calibrated according to the appropriate criteria listed in Table 13.
Qualified ETV CCEP personnel will calibrate any equipment owned or operated by the
offsite facility that will be used for these tests. The calibration results will be documented and
incorporated into the laboratory report. An example of offsite equipment is a laboratory balance,
which may be used in the determination of total volatile content of the UV-curable coatings.
6.1.2 Laboratory Testing and Calibration Procedures
The analytical methods performed for ETV CCEP at the NDCEE are adapted from
standard ASTM, MIL-SPEC, EPA, Association of Official Analytical Chemists (AOAC) and
industry protocols for similar manufacturing operations. Initial calibration and periodic
calibration verification are performed to insure that an instrument is operating sufficiently to
meet sensitivity and selectivity requirements. At a minimum, all equipment is calibrated before
use and is verified during use or immediately after each sample batch. Standard solutions are
purchased from reputable chemical supply houses in pure and diluted forms. Where certified and
traceable to NIST reference materials and solutions are available, the laboratory purchases these
for calibration and standardization. Data from all equipment calibrations and chemical standard
certificates from vendors are stored in laboratory files and are readily retrievable. No samples are
reported in which the full calibration curve, or the periodic calibration check standards, is outside
method performance standards. As needed, equipment will be sent offsite for calibration or
certification.
A listing of relevant ASTM Methods can be found in Appendix B. All equipment, used
for these analyses, is calibrated according to Tables 13 and 14.
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The ambient temperature and relative humidity is measured both inside and outside the
spray booth. Also, the temperature of one product per run is measured prior to starting each test
run.
All equipment used for these analyses will be calibrated according to Tables 13 and 14.
6.2 Product Quality Procedures
Each apparatus that will be used to assess the quality of a coating on a test product is set
up and maintained according to each manufacturer's, or the published instructions of the
reference method. Actual sample analysis will take place only after setup is verified against the
reference method and the equipment manufacturer's instructions. As available, samples of
known materials with established product qualities are used to verify that a system is functioning
properly. For example, traceable thickness standards are used to calibrate the DFT instrument.
Applicable ASTM methods are listed in Appendix B.
6.3 Standard Operating Procedures and Calibration
Tables 13 and 14 summarize the methods and calibration criteria that will be used for the
evaluation of the coatings. Each analysis shall be performed as adapted from published methods
and references, such as ASTM and EPA, and from accepted protocols provided by industrial
suppliers.
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Table 13. Noncritical Control Factor Testing and Calibration Criteria
Noncritical Factor
Input Air Pressure
Products Involved in
Testing
Coating Delivery
Pressure
Pretreatment
Analysis
Surface Area of Each
Product
Ambient Factory
Relative Humidity
Ambient Factory
Temperature
Spray Booth Relative
Humidity
Spray Booth
Temperature
Spray Booth Airflow
(Face Velocity)
Temperature of Test
Panels, as Coated
Distance From Gun
to Test Panels
Horizontal Gun
Traverse Speed
Vertical Drop
Between Passes
Volatile Content of
Applied Coating
Density of Applied
Coating
Weight % Solids of
Applied Coating
Coating Temperature,
as Applied
Coating Viscosity, as
Applied
Cure Time
Method
Factory gauge
Test panels
Pressure
gauge
ASTM B767
Ruler
Thermal
hygrometer
Thermal
hygrometer
Thermal
hygrometer
Thermal
hygrometer
Per ACGIHC
Infrared (IR)
thermometer
Ruler
Stopwatch
Ruler
ASTM
D3960
ASTM
D1475
ASTM
D2369
Thermometer
ASTM
D1200
Stopwatch
Method
Type
Pressure gauge
N/Ab
Pressure gauge
Chromate solution
(50g/L Cr03)
Ruler
Thermal
hygrometer
Thermal
hygrometer
Thermal
hygrometer
Thermal
hygrometer
Anemometer
IR thermometer
Ruler
Stopwatch
Ruler
Volatile content
Weight
Weight
Thermometer
#4 Ford Cup
Stopwatch
Calibration
Procedure
Comparison to NIST-
traceable standard
N/A
Comparison to NIST-
traceable standard
Comparison to NIST-
traceable standard
Inspect for damage,
replace if necessary
Sent for calibration or
certification
Sent for calibration or
certification
Sent for calibration or
certification
Sent for calibration or
certification
Sent for calibration or
certification
Sent for calibration or
certification
Inspect for damage,
replace if necessary
Sent for calibration or
certification
Inspect for damage,
replace if necessary
Comparison to NIST-
traceable standard
Comparison to NIST-
traceable standard
Comparison to NIST-
traceable standard
Comparison to NIST-
traceable standard
Comparison to NIST-
traceable standard
Comparison to NIST-
traceable standard
Calibration
Frequency
Six months
N/A
Six months
With each use
With each use
Annually
Annually
Annually
Annually
Annually
Annually
With each use
Six months
With each use
With each use
With each use
With each batch
of coating
Annually
Prior to each test
Annually
Calibration
Acceptance
Criteria3
+ 5 psig
N/A
+ 5 psig
80120%
Lack of damage
Calibration or
certification
documentation
Calibration or
certification
documentation
Calibration or
certification
documentation
Calibration or
certification
documentation
Calibration or
certification
documentation
Calibration or
certification
documentation
Lack of damage
N/A
Lack of damage
+ 0.003 g
+ 0.003 g
+ 0.003 g
+ 1°C
± 10%
± 10%
a As a percent recovery of a standard
b N/A - Not applicable
c ACGIH - American Conference of Governmental Industrial Hygienists, Inc.
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Table 14. Critical Response Factor Testing and Calibration Criteria
Critical
Measurement
Total Volatile
Content
Energy Usage of the
UV Lamps
Dry Film Thickness
(DFT)
Visual Appearance
Gloss
Color
Spectrometer
Spectral Light II
Distinctness-of-
Image (DOI)
Adhesion
Pencil Hardness
Corrosion Resistance
(Salt Spray)
Direct Impact
Mandrel Bend
Chemical Resistance
[Methyl Ethyl Ketone
(MEK) Rub]
Humidity Resistance
Weather Resistance
Abrasion Resistance
Method
Number"
ASTMD5403,
Method A
Calculated
ASTM B 499
N/AC
ASTM D 523
ASTM D 1729
ASTM D 2244
ASTM D 5767
Method B
ASTM D 3359
ASTM D 3363
ASTMB 117
ASTM D 2794
ASTM D 522
ASTM D 5402
ASTM D 1735
ASTM G 26
ASTM D 4060
Method
Type
Volatile
content
Calculated
Magnetic
Visual
Gloss meter
Spectrometer
Visual
Image
analyzer
Tape test
Pencil
Salt fog,
5% NaCl,
neutral pH
2-pound
weight
Conical
mandrel
MEK-
saturated
cheesecloth
100%
Humidity
using fog
apparatus
Xenon arc w/
and w/o
humidity
Taber Abraser
Calibration
Procedure
Comparison to NIST-
traceable standard
N/A
Comparison to NIST-
traceable standard
N/A
Comparison to NIST-
traceable standard
Zero w/ white tile
N/A
Manufacturer's
recommendation
Verify condition of
scribes and freshness
of adhesives
Supplier-graded lead
(use same supplier)
Verify collection rate,
pH, salinity, and bare
steel corrosion rate
Verify weight of
indenter, verify ruler
Verify conical
diameter
Reagent grade MEK
Collection rate, pH
Irradiance,
temperature, black
panel, wet and dry
bulb, wattage, water
quality
Verify load weights
Calibration
Frequency
Each use
N/A
Verify calibration
after each run
N/A
Verify calibration
after each run
Each use
N/A
Manufacturer's
recommendation
Each use
Each use
Weekly chemical
tests, monthly steel
tests
Yearly
Yearly
N/A
Daily collection
rate and pH
Weekly
Each use
Calibration
Acceptance
Criteria11
± 0.003 g
N/A
90110%
N/A
90110%
N/A
N/A
Manufacturer's
recommendation
N/A
N/A
RSDd<20%
among steel
panels, average of
chemical tests
within specific
ranges
80120%
80120%
N/A
Within ASTM
ranges
Within ASTM
ranges
95105%
a Listing of ASTM methods to be used is provided in Appendix B.
b As a percent recovery of a standard
c N/A - Not applicable
d RSD - Relative Standard Deviation
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6.4 Nonstandard Methods
ETV CCEP and the offsite test facility does not plan to use any nonstandard methods for
this project. However, for methods that are nonstandard (i.e., no commonly accepted or specified
method exists or no traceable calibration materials exist), procedures will be performed
according to the manufacturer's instructions or to the best capabilities of the equipment and the
laboratory. This information will be documented. The performance will be judged based on the
manufacturer's specifications, or will be judged based on protocols developed by the testing
organization. These protocols will be similar or representative in magnitude and scope to related
methods performed in the laboratory, which do have reference performance criteria for precision
and accuracy. For instance, if a nonstandard quantitative chemical procedure is being performed,
it should produce replicate results of ± 25 relative percent difference (RPD) and should give
values within ± 20 percent of true or expected values for calibration and percent recovery check
samples. For qualitative procedures, replicate results should agree as to their final evaluations of
quality or performance (i.e., both should either pass or both should fail if sampled together from
a properly functioning process). The intended use and any limitations would be explained and
documented for a nonstandard procedure.
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7.0 DATA REDUCTION, VALIDATION, AND REPORTING
7.1 Raw Data Handling
Raw data will be generated and collected by the analysts at the bench or process level.
Process data are recorded into a process log during factory operations. Bench data will include
original observations, printouts, and readouts from equipment for sample, standard, and reference
QC analyses. Data will be collected both manually and electronically. At a minimum, the date,
time, sample ID, instrument ID, analyst ID, raw or processed signal, and qualitative observations
will be recorded. The sample ID will be traceable from the raw data sheets through the summary
sheets reported in the Data Notebook. Comments documenting unusual or nonstandard
observations will also be included on the forms as necessary. The analyst will process raw data
manually, automatically by an electronic program, or electronically after being entered into a
computer. The analyst will be responsible for scrutinizing the data according to specified
precision, accuracy, and completeness policies. Raw data bench sheets, calculations, and data
summary sheets will be maintained for each sample batch. From the written standard operating
procedures (SOPs) and raw data bench files, the steps leading to a final result may be traced.
7.1.1 Error in Solids Content
The solids content is the difference between two masses, the wet mass and the dry mass
of the coating. The procedure specifies four measurements to be made, mass of the empty pan
(EP), mass of the full syringe (FS), the mass of the empty syringe (ES), and the mass of the pan
with the deposited solids (PS).
%S = (PS - EP) / (FS -ES) 100
Since two measurements are made in the numerator and the denominator, the total uncertainty in
each of these values is the sum of the uncertainties, or 2 0.0005 g. Since between 200 and 300
mg of coating is used in the test, this uncertainty becomes negligible compared to the numerator
uncertainty. Only about 50 to 100 mg of solids are expected to remain in the pan after drying,
making the numerator value uncertain by a maximum of 2%. Therefore, the solids content
reported can be safely reported as within 2% of the actual value.
7.2 Preliminary Data Package Validation
A laboratory analyst will assemble a preliminary data package consisting of the data
generated by the laboratory analysis. This package will contain the QC and raw data results,
calculations, electronic printouts, conclusions and laboratory sample tracking information. The
ETV CCEP laboratory leader will review the entire package and may also check sample and
storage logs, standard logs, calibration logs, and other files, as necessary, to insure that tracking,
sample treatments and calculations are correct. After the package has been peer reviewed in this
manner, a preliminary data report will be prepared. The entire package and final laboratory
report will be submitted by the ETV CCEP laboratory leader to the ETV CCEP project leader for
incorporation into the Data Notebook.
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7.3 Final Data Validation
The ETV CCEP laboratory leader shall be ultimately responsible for all final data
released from this project. The ETV CCEP laboratory leader will review the final results for
adequacy to project QA objectives. If the manager suspects an anomaly or nonconcurrence with
expected or historical performance values, with project QA objectives, or with method specific
QA requirements of the laboratory procedures, he will initiate a second review of the raw data
and query the generating analyst about the nonconformance. Also, he will request specific
corrective action. If suspicion about data validity still exists after internal review of laboratory
records, the ETV CCEP laboratory leader may authorize a reanalysis. If sufficient sample is not
available for retesting, a resampling will occur. If the sampling window has passed, or
resampling is not possible, the ETV CCEP laboratory leader will flag the data as suspect and
notify the ETV CCEP project leader. The ETV CCEP laboratory leader will sign and date the
final data package and deliver it to the ETV CCEP project leader for review and incorporation
into the Data Notebook.
7.4 Data Reporting and Archival
A report signed and dated by the ETV CCEP laboratory leader will be submitted to the
ETV CCEP project manager, the ETV CCEP QA officer, the EPA ETV CCEP QA manager, and
other technical principals involved in the project. The ETV CCEP project leader will incorporate
any additional process information into the report prior to the ETV CCEP project manager's final
review. The ETV CCEP project manager will decide on the validity of the data and will make
any interpretations with respect to project QA objectives. The final laboratory report will contain
the lab sample ID, date reported, date analyzed, the analyst, the procedures used for each
parameter, the process or sampling point identification, the final result and the units. The
NDCEE environmental laboratory will retain the data packages at least 10 years. The ETV
CCEP project manager or the NDCEE program director will forward the results and conclusions
to EPA in their regular reports for final EPA approval of the test data. This information will be
used to prepare the Verification Report, which will be published by the ETV CCEP. The ETV
CCEP, the vendor, the ETV CCEP Stakeholders, EPA technical peer reviewers, and the EPA
Technical Editor will review the Verification Report. The EPA and the ETV CCEP will then
approve the revised document prior to it being published.
7.5 Verification Statement
The ETV CCEP will also prepare a Verification Statement from the information
contained in the Verification Report. After receiving the results and conclusions from the ETV
CCEP project manager or the NDCEE program director, the EPA will approve the Verification
Report and Verification Statement. Only after agreement by the vendor, will the Verification
Statement be disseminated.
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8.0 INTERNAL QUALITY CONTROL CHECKS
U
Guide Used for Internal Quality Program
ETV CCEP uses the NDCEE facility and its QA systems to verify coating technologies.
The NDCEE has established an ISO 9001 operating program for its laboratories and the
Demonstration Factory. The laboratory is currently establishing a formal quality control program
for its specific operations. The format for laboratory QA/QC is being adapted from several
sources as listed in Table 15. This QA system is consistent with the ETV QMP, the ETV CCEP
QMP, and ANSI/ASQC guidelines.
Table 15. CTC Laboratory QA/QC Format Sources
Document
General Requirements for the Competence of
Calibration and Testing Laboratories
Critical Elements for Laboratories
Chapter One, Quality Control
Requirements of 100-300 series of methods
Handbook of Quality Assurance for the
Analytical Chemistry Laboratory, 2nd Ed.
Reference Source
ISO Guide 25, ISO Quality Programs
Pennsylvania Department of Environmental
Protection
SW-846, EPA Test Methods
EPA Test Methods
James P. Dux
8.2 Types of QA Checks
The NDCEE Environmental Technology Facility (ETF) Environmental Laboratory and
Organic Finishing Line used by ETV CCEP follow published methodologies, wherever possible,
for testing protocols. Laboratory and coating process methods are adapted from federal
specifications, military specifications, ASTM Test Methods, and vendor instructions. The
laboratory and finishing line adhere to the QA/QC requirements specified in these documents. In
addition, where QA/QC criteria are not specified, or where the laboratory or finishing line
perform additional QA/QC activities, these protocols are explained in the laboratory or finishing
line's SOPs (Work Instructions). Each NDCEE facility that uses supplied products implements
its own level of QA/QC. During ETV CCEP testing, the NDCEE laboratory and finishing line
personnel will perform the testing and QA/QC verification outlined in Tables 10 and 11
(Precision, Accuracy, and Completeness) and Tables 13 and 14 (Calibration); therefore, these
tables should be referred to for the method-specific QA/QC that will be performed.
8.3 Basic QA Checks
During each test, an internal Process QA Checklist will be completed by the laboratory
and finishing line staff to ensure that the appropriate parts, panels, samples, and operating
conditions are used. The laboratory also monitors its reagent DI water to ensure it meets purity
levels consistent with analytical methodologies. The DI water filters are replaced quarterly
before failures are encountered. The quality of the water is assessed with method reagent water
blanks. Blank levels must not exceed minimum detection levels for a given parameter to be
considered valid for use.
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Thermometers are checked against NIST-certified thermometers at two temperatures.
The laboratory checks and records the temperatures of sample storage areas, ovens, hot plate
operations, and certain liquid baths that use thermometers.
Balances are calibrated by an outside organization using standards traceable to NIST.
The ETF laboratory also performs in-house, periodic verifications with ASTM Class 1 weights.
The ETF laboratory maintains records of the verification activities and calibration certificates.
The laboratory analyst also checks the balances prior to use with ASTM Class 1 weights.
Reagents purchased directly by the laboratory are American Chemical Society (ACS)
grade or better. Reagents are not used beyond their certified expiration dates. Reagents are dated
on receipt and when first opened.
Laboratory waste is segregated according to chemical classifications in labeled containers
to avoid cross-contamination of samples.
8.4 Specific Checks
The NDCEE Environmental Laboratory will analyze uncoated panels for DFT to verify
that the instrument has not drifted from zero, perform duplicate analyses on the same samples,
and perform calibration checks of the laboratory equipment during ETV CCEP testing.
Laboratory personnel will also check any referenced materials and equipment as available and
specified by the referenced methodology and the project-specific QA/QC objectives. Laboratory
records are maintained with the sample data packages or in centralized files as appropriate. To
ensure comparability, laboratory and finishing line personnel will carefully control process
conditions and perform product evaluation tests consistently for each specimen. The specific QA
checks listed in Tables 10, 11, 13, and 14 provide the necessary data to determine whether
process control and product testing objectives are being met. ASTM, federal, and military
methods that are accepted in industry for product evaluations and vendor-endorsed methods for
process control, will be used for all critical measurements, thus satisfying the QA objective. A
listing of the published methods that will be used for this GVP is included in Appendix B.
8.5 Off site QA Checks
Several QA activities will be conducted at the offsite facility, including: a pre-test site
visit, completion of a QA and calibration checklist, collection of calibration certificates, and
performance audits on equipment to be used during the test. This information will be included in
the laboratory report and Data Notebook. Equipment owned by the offsite facility that may be
used during these tests consists of the UV lamps (energy usage), the conveyor system, and
laboratory balances (total volatile analysis).
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9.0 PERFORMANCE AND SYSTEM AUDITS
ETV CCEP uses the NDCEE facility and its QA systems to verify coating technologies.
The NDCEE has developed a system of internal and external audits to monitor both program and
project performance which are consistent with the audit requirements specified in the ETV and
ETV CCEP QMPs. These include monthly managers meetings and reports, financial statements,
EPA reviews and stakeholders meetings, and In-Process Reviews. The ETF laboratory also
analyzes performance evaluation samples in order to maintain Pennsylvania Department of
Environmental Protection Certification.
ISO Internal Audits
The NDCEE has established its quality system based on ISO 9000 and 14000 and
has implemented a system of ISO internal audits. This information will be used
for internal purposes.
Onsite Visits
The EPA ETV CCEP project manager may visit the NDCEE or the offsite test
facility for an onsite visit during the execution of this project. All project,
process, quality assurance, and laboratory testing information will be available for
review.
EPA Audits
The EPA will periodically audit the ETV CCEP during this project. All project,
process, quality assurance, and laboratory testing information will be made
available per the EPA's auditing procedures.
Technical Systems Audits
A list of all coating equipment, laboratory measuring and testing devices, and
procedures, coating procedures, and a copy of the approved ETV QMP and the
approved ETV CCEP QMP will be given to the ETV CCEP QA officer. The
ETV CCEP QA officer will conduct an initial audit, and additional audits
thereafter according to the ETV CCEP QMP, of verification and testing activities.
The NDCEE program director or the ETV CCEP project manager will forward a
summary of the results of this activity to EPA.
Performance Evaluation Audits (PEAs)
The precision and accuracy of the measurement equipment will be examined to
determine compliance with the product-specific TQAPPs. The auditor will
evaluate measurements such as DFT and total volatile content. The ETV CCEP
QA officer will conduct a PEA for each verification test. The NDCEE program
director or the ETV CCEP project manager will forward a summary of the results
of this activity to the EPA.
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Audits of Data Quality
Peer review in the laboratory constitutes a process whereby two analysts review
raw data generated at the bench level. After data are reduced, they undergo
review by laboratory management. For this GVP, laboratory management will
spot check 10 percent of the project data by performing a total review from raw to
final results. This activity will occur in addition to the routine management
review of all data. Records will be kept to show which data have been reviewed
in this manner.
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10.0 CALCULATION OF DATA QUALITY INDICATORS
10.1 Precision
Duplicates will be performed on separate samples as well as on the same sample source,
depending on the method being employed. In addition, the final result for a given test may be the
arithmetic mean of several determinations on the part or matrix. In this case, duplicate precision
calculations will be performed on the means. The following calculations will be used to assess
the precision between duplicate measurements.
Relative Percent Difference (RPD) = [(Cl - C2) 100%] / [(Cl + C2) / 2]
where: Cl = larger of the two observations
C2 = smaller of the two observations
Relative Standard Deviation (RSD) = (s/y) 100%
where: s = standard deviation
y = mean of replicates.
10.2 Accuracy
Accuracy will be determined as percent recovery of a check standard, check sample, or
matrix spike. For matrix spikes and synthetic check samples:
Percent Recovery (% R) = 100% [(S - U)/T]
where: S = observed concentration in spiked sample
U = observed concentration in unspiked sample
T = true value of spike added to sample.
For standard reference materials (srm) used as calibration checks:
%R=100%-(Cm/Csrm)
where: Cm = observed concentration of reference material
Csrm = theoretical value of srm.
10.3 Completeness
Percent Completeness (% C) = 100% (V/T)
where: V = number of determinations judged valid
T = total number of determinations for a given method type.
10.4 Project Specific Indicators
Process control limit: range specified by vendor for a given process parameter.
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11.0 CORRECTIVE ACTION
11.1 Routine Corrective Action
Routine corrective action will be undertaken in the event that a parameter in Tables 10,
11, 13, and 14 is outside the prescribed limits specified in these tables, or when a process
parameter is beyond specified control limits. Examples of nonconformances include, but are not
limited to, invalid calibration data, inadvertent failure to perform method-specific QA tests,
process control data outside specified control limits, and failed precision or accuracy indicators.
Such nonconformances will be documented on a standard laboratory or process/facility testing
form. Corrective action will involve taking all necessary steps to restore a measuring system to
proper working order and summarizing the corrective action and results of subsequent system
verifications on a standard form. Some nonconformances will be detected while analysis or
sample processing is in progress, and can be rectified in real time at the bench level. Other
nonconformances may be detected only after a processing trial or sample analyses are completed.
These types of nonconformances are typically detected at the ETV CCEP laboratory leader level
of data review. In all cases of nonconformance, the laboratory leader will consider repeating the
sample analysis as one method of corrective action. If a sufficient sample is not available, or the
holding time has been exceeded, complete reprocessing may be ordered to generate new samples
if a determination is made by the ETV CCEP project manager that the nonconformance
jeopardizes the integrity of the conclusions to be drawn from the data. In all cases, a
nonconformance will be rectified before sample processing and analysis continues. If corrective
action does not restore the production or analytical system, causing a deviation from the ETV
CCEP QMP, the ETV CCEP will contact the EPA ETV CCEP project manager. In cases of
routine nonconformance, EPA will be notified in the NDCEE program director or ETV CCEP
project manager's regular reports to the EPA ETV CCEP project manager. A complete
discussion will accompany each nonconformance.
11.2 Nonroutine Corrective Action
While not anticipated, activities such as internal audits by the ETV CCEP QA officer, and
onsite visits by the EPA ETV CCEP project manager, may result in findings that contradict
deliverables in the ETV CCEP QMP. In the event that nonconformances are detected by bodies
outside the laboratory organizational unit, as for routine nonconformances, these problems will
be rectified and documented prior to processing or analyzing further samples or specimens.
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12.0 QUALITY CONTROL REPORTS TO MANAGEMENT
As shown on the Project Organization Chart in Figure 4, the ETV CCEP QA officer is
independent from the project management team. It is the responsibility of the ETV CCEP QA
Officer to monitor ETV CCEP verifications for adherence to the ETV CCEP QMP. The ETV
CCEP laboratory leader monitors the operation of the laboratory on a daily basis and provides
comments to the ETV CCEP QA officer to facilitate his activities. The ETV CCEP QA officer
will audit the operation records, laboratory records, and laboratory data reports and provide a
written report of the findings to the ETV CCEP project manager and laboratory leader. The ETV
CCEP project manager will ensure these reports are included in the report to the EPA. The
laboratory leader will be responsible for achieving closure on items addressed in the report.
Specific items to be addressed and discussed in the QA report include the following:
General assessment of data quality in terms of general QA obj ectives in Section 4.1
Specific assessment of data quality in terms of quantitative and qualitative
indicators listed in Sections 4.2 and 4.3
Results of the site surveys and pretest audits of offsite testing locations and
equipment listed in Section 2.1.1
. Listing and summary of all nonconformances and deviations from the ETV CCEP
QMP
Impact of nonconformances on data quality
. Listing and summary of corrective actions
Results of internal Q A audits
Closure of open items from last report or communications with EPA in current
reporting period
. Deviations or changes in the ETV CCEP QMP
. Progress of the NDCEE QA Programs used by ETV CCEP in relation to current
project
. Limitations on conclusions, use of the data
. Planned QA activities, open items for next reporting period
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13.0 REFERENCES
1. American Society for Quality Control. American National Standard Specifications and
Guidelines for Quality Systems for Environmental Data Collection and
Environmental Technology Programs. ANSI/ASQC E4-1994, E4. American Society
for Quality, 1994.
2. U.S. Environmental Protection Agency. Environmental Technology Verification
Program: Quality Management Plan. EPA/600/R-03/021. December 2002.
http://www.epa.gov/etv/pdfs/qmp/00_qmp_etv.html.
3. Concurrent Technologies Corporation. Environmental Technology Verification Coatings
and Coating Equipment Program (ETV CCEP) Pilot: Quality Management Plan.
December 21, 1998. http://www.epa.gov/etv/pdfs/qmp/06_qmp_p2.pdf.
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Section No. A
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APPENDIX A
Default Standard Test Panel
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STANDARD TEST PRODUCT
o
O
7/16"-
HOLE FOR HANGING
TEST PRODUCT (5/16" D!A.)
(il) (311)
(29)
(17) (37)
(23)
(33)
(21)
(0,0 REF.)-
, 12"
TEST POINTS ARE INDICATED
BY THEIR POSITION RELATIVE
TO THE BOTTOM LEFT HAND
CORNER OF THE PANEL.
(ALL VALUES ARE IN INCHES).
Coric^rrent
Technologies
Corporation
EIWIBQNKCNTAL
VEHIF1CATION COATIW6S AW
COATING EQUIPMENT - - - - -
;T PRODUCT
WITH
~<*Smm m*
EIF-Offl-iO?
REV, 0
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APPENDIX B
ASTM Methods
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ASTM Methods
ASTMB 117
ASTM B 499
ASTM B 767
ASTM D 522
ASTM D 523
ASTMD 1200
ASTMD 1475
ASTMD 1729
ASTMD 1735
ASTM D 2244
ASTMD 2369
ASTM D 2794
ASTMD 3359
ASTMD 3363
ASTM D 3960
ASTM D 4060
ASTM D 5402
ASTM D 5403
ASTM D 5767
ASTM G 26
Standard Practice for Operating Salt Spray (Fog) Apparatus
Standard Test Method for Measurement of Coating Thickness by the Magnetic Method:
Nonmagnetic Coatings on Magnetic Basis Metals
Standard Guide for Determining Mass per Unit Area of Electodeposited and Related
Coatings by Gravimetric and other Chemical Analysis Procedures
Standard Test Methods for Mandrel Bend Test of Attached Organic Coatings
Standard Test Method for Specular Gloss
Standard Test Method for Viscosity by Ford Viscosity Cup
Standard Test Method for Density of Liquid Coatings, Inks, and Related Products
Standard Practice for Visual Evaluation of Color Differences of Opaque Materials
Standard Practice for Testing Water Resistance of Coatings Using Water Fog Apparatus
Standard Test Method for Calculation of Color Differences from Instrumentally
Measured Color Coordinates
Standard Test Method for Volatile Content of Coatings
Standard Test Method for Resistance of Organic Coatings to the Effects of Rapid
Deformation (Impact)
Standard Test Method for Measuring Adhesion by Tape Test
Standard Test Method for Film Hardness by Pencil Test
Standard Practice for Determining Volatile Organic Compound (VOC) Content of Paints
and Related Coatings
Standard Test Methods for Abrasion Resistance of Organic Coatings by the Taber
Abraser
Assessing the Solvent Resistance of Organic Coatings Using Solvent Rubs
Standard Test Methods for Volatile Content of Radiation Curable Materials
Standard Test Methods for Instrumental Measurement of Distinctness-of-Image Gloss of
Coating Surfaces
Practice for Operating Light Exposure Apparatus (Xenon-Arc Type) With and Without
Water for Exposure of Nonmetallic Materials
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