Environmental Technology Verification Coatings and
Coating Equipment Program (ETV CCEP)
High Transfer Efficiency Spray Equipment - Generic
Verification Protocol (Revision 0)
September 30, 2006
Distribution Statement "A" applies
Approved for public release; distribution is unlimited
Requests for this document shall be referred to:
Office of the Assistant Secretary of the Army
for Installations and Environment
ASA (I&E) - ESOH
1235 Clark Street
Crystal Gateway 1, Suite 307
Arlington, VA 22202-3263
Contract No. W74V8H-04-D-0005
Task No. 0428
CDRL No. A004
Prepared by
National Defense Center for Environmental Excellence (NDCEE)
Submitted by
Concurrent Technologies Corporation
100 CTC Drive
Johnstown, PA 15904
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1. AGENCY USE ONLY (Leave blank)
2. REPORT DATE 3. REPORT TYPE AND DATES COVERED
30 September 06 Generic Verification Protocol / Sep. 2005 - Jun. 2007
4. TITLE AND SUBTITLE
ETV CCEP, High Transfer Efficiency Spray Equipment - Generic Verification Protocol (Revision 0)
6. AUTHOR(S)
Principal Author/PMt: Robert J. Fisher, CTC
1. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES)
National Defense Center for Environmental Excellence
Operated by Concurrent Technologies Corporation
100 CTC Drive
Johnstown, PA 15904
9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES)
NDCEE Program Office (Office of the Assistant Secretary of the Army for Installations and Environment)
1235 Clark Street, Suite 307
Arlington, VA 22202-3263
Program Manager: Dr. Chuck Lecher, NDCEE Program Manager, 703-602-5538
5. FUNDING NUMBERS
Contract: W74V8H-04-D-0005
Task: NDCEE Task No. 0428
8. PERFORMING ORGANIZATION
REPORT NUMBER
10. SPONSORING/MONITORING
AGENCY REPORT NUMBER
NDCEE-CR-2006-082
10 SUPPLEMENTARY NOTES
12a. DISTRIBUTION/AVAILABILITY STATEMENT
Distribution authorized to the DoD and DoD contractors only.
12b. DISTRIBUTION CODE
13. ABSTRACT (Maximum 200 words)
The Environmental Technology Verification (ETV) Program has been established by the U.S. Environmental Protection Agency (EPA) to verify the
performance characteristics of innovative environmental technologies across all media and report this objective information to the states, buyers, and users of
environmental technology; thus, accelerating the entrance of these new technologies into the marketplace. Verification organizations oversee and report verification
activities based on testing and quality assurance protocols developed with input from major stakeholders and customer groups associated with the technology area. ETV
consists of six technology centers. Information about each of these centers can be found on the Internet at http://www.epa.gov/etv/.
EPA's ETV Program, through the National Risk Management Research Laboratory (NRMRL), Air Pollution Prevention and Control Division (APPCD) has
partnered with Concurrent Technologies Corporation (CTC), through the National Defense Center for Environmental Excellence (NDCEE), to verify innovative
coatings and coating equipment technologies for reducing air emissions from coating operations. Pollutant releases to other media are considered in less detail.
The following protocol outlines the basis for completing an ETV verification test of High-Transfer Efficiency Spray Guns.
14. SUBJECT TERMS
15. NUMBER OF PAGES
59
16. PRICE CODE
17. SECURITY CLASSIFICATION 18. SECURITY CLASSIFICATION 19. SECURITY CLASSIFICATION 20. LIMITATION OF ABSTRACT
OF REPORT OF THIS PAGE OF ABSTRACT None
Unclassified Unclassified Unclassified
NSN 7540-01-280-5500
Standard Form 298 Rev. 12/00
Prescribed by ANSI ST. 239-18
880922
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Section No. i
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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 High Transfer Efficiency Spray Equipment GVP 1
1.2 Quality Assurance for the ETV CCEP 1
1.3 Organization of the High-TE GVP 1
1.4 Formatting 2
1.5 Approval Form 2
2.0 PROJECT DESCRIPTION 4
2.1 General Overview 4
2.1.1 Demonstration Factory Testing Site 5
2.1.2 Laboratory Facilities 6
2.2 Technical/Experimental Approach and Guidelines 7
2.2.1 Test Approach 8
2.2.2. Verification Test Objectives 8
2.2.3 Large Target Description 8
2.2.4 Small Target Description 9
2.2.5 Coating Specification 11
2.2.6 Standard Apparatus 12
2.2.7 Process Standards 12
2.2.8 Design of Experiment 13
2.2.9 Performance Testing 13
2.2.10 Quantitative Measurements 14
2.2.11 Participation 14
2.2.12 Critical and Non-Critical Factors 14
2.3 Schedule 19
3.0 PROJECT ORGANIZATION AND RESPONSIBILITIES 20
4.0 QUALITY ASSURANCE OBJECTIVES 23
4.1 General Objectives 23
4.2 Quantitative Quality Assurance Objectives 23
4.2.1 Accuracy 25
4.2.2 Precision 26
4.2.3 Completeness 26
4.2.4 Impact and Statistical Significance Quality Objectives 26
4.3 Qualitative QA Objectives: Comparability and Representativeness 26
4.3.1 Comparability 26
4.3.2 Representativeness 27
4.4 Other QA Objectives 27
4.5 Impact of Quality 27
5.0 SITE SELECTION AND SAMPLING PROCEDURES 28
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5.1 Site Selection 28
5.2 Site Description 28
5.3 Sampling Procedures and Handling 28
5.4 Sample Custody, Storage and Identification 29
6.0 ANALYTICAL PROCEDURES AND CALIBRATION 30
6.1 Facility and Laboratory Testing and Calibration 30
6.1.1 Facility Testing and Calibration 30
6.1.2 Laboratory Testing and Calibration Procedures 30
6.2 Product Quality Procedures 31
6.3 Standard Operating Procedures and Calibration 31
6.4 Non-Standard Methods 33
7.0 DATA REDUCTION, VALIDATION, AND REPORTING 34
7.1 Raw Data Handling 34
7.1.1 Variables Used In Analysis 34
7.1.2 Error in Mass of Coating Sprayed 34
7.1.3 Error in Solids Content 35
7.1.4 Error in Mass Deposited 35
7.1.5 Calculation of Transfer Efficiency 35
7.2 Preliminary Data Package Validation 36
7.3 Final Data Validation 36
7.4 Data Reporting and Archival 37
7.4.1 Calculation of DFT 37
7.4.2 Interpretation of the Numerical Results 37
7.4.3 Evaluation of the High-TE Spray Gun 37
7.5 Verification Statement 38
8.0 INTERNAL QUALITY CONTROL CHECKS 39
8.1 Guide Used for Internal Quality Program 39
8.2 Types of QA Checks 39
8.3 Basic QA Checks 39
8.4 Specific Checks 40
9.0 PERFORMANCE AND SYSTEM AUDITS 41
10.0 CALCULATION OF DATA QUALITY INDICATORS 42
10.1 Precision 42
10.2 Accuracy 42
10.3 Completeness 42
10.4 Project Specific Indicators 42
11.0 CORRECTIVE ACTION 43
11.1 Routine Corrective Action 43
11.2 Nonroutine Corrective Action 43
12.0 QUALITY CONTROL REPORTS TO MANAGEMENT 44
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LIST OF TABLES
Table 1. Testing and Laboratories and Representative Laboratory Equipment Holdings 7
Table 2. Overall Guidelines and Procedures Applied to this Test/QAPlan 7
Table 3. Critical Control Factors 16
Table 4. Non-Critical Control Factors 17
Table 5. Critical Response Factors 18
Table 6. Estimated Schedule as of 9/27/06 19
Table 7. Summary of ETV CCEP Experience and Responsibilities 21
Table 8. Frequency and Mechanisms of Communications 22
Table 9. Responsibilities During Testing 22
Table 10. QA Objectives for Precision, Accuracy and Completeness for All Non-Critical
Control Factor Performance Analyses 24
Table 11. QA Objectives for Precision, Accuracy and Completeness for All Critical
Response Factor Performance Analyses 25
Table 12. Process Responsibilities 29
Table 13. Non-Critical Control Factor Testing and Calibration Criteria 32
Table 14. Critical Response Factor Testing and Calibration Criteria 33
Table 15. CTC Laboratory QA/QC Format Sources 39
LIST OF FIGURES
Figure 1. Test/QAPlan Approval Form 3
Figure 2. Demonstration Factory Layout 5
Figure 3. Demonstration Factory Organic Finishing Line 6
Figure 4. Large Target Application Diagram 9
Figure 5. Small Target Application Diagram 10
Figure 6. Test Panel Measurement Locations 11
Figure 7. Project Organization Chart 20
LIST OF APPENDICES
A
ASTM International Methods
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SI to English Conversions
Multiply SI
by factor to
SI Unit English Unit obtain English
°C °F (1.80 E +00), then add 32
L gal. (U.S.) 2.642 E-01
m ft 3.281 E + 00
kg Ibm 2.205 E + 00
kPa psi 1.4504 E-01
cm in. 3.937 E-01
mm mil (1 mil = 1/1000 in.) 3.937 E + 01
m/s ft/mm 1.969 E + 02
kg/L Ibm/gal (U.S.) 8.345 E + 00
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List of Abbreviations and Acronyms
%C percent completeness
%R percent recovered
%S percent solids
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
CCEP Coatings and Coating Equipment Program
CTC Concurrent Technologies Corporation
CS coating sprayed
DFT dry film thickness
DOI distinctness-of-image
EP empty pan
EPA U.S. Environmental Protection Agency
ES empty syringe
ETF environmental technology facility
ETV environmental technology verification
FS full syringe
GVP generic verification protocol
HVLP high-volume, low-pressure
IR infrared
ISO International Standardization Organization
NDCEE National Defense Center for Environmental Excellence
NIST National Institute for Standards and Technology
OFL organic finishing line
P2 pollution prevention
PLC programmable logic controller
PS pan solids
QA/QC quality assurance/quality control
QMP quality management plan
RPD relative percent difference
RSD relative standard deviation
SD solids deposited
srm standard reference material
SS solids sprayed
TE transfer efficiency
VOC volatile organic compound
WBS work breakdown structure
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1.0 INTRODUCTION
1.1 Purpose of the High Transfer Efficiency Spray Equipment GVP
The primary purpose of this document is to establish the generic verification
protocol (GVP) for high transfer efficiency (TE) spray equipment, to which
reference will be made frequently throughout this document as the High-TE GVP.
The secondary purpose is to establish the generic format and guidelines for
product specific Testing and Quality Assurance Plans (test/QA plans) that relate
to this GVP.
Environmental Technology Verification Coatings and Coating Equipment
Program (ETV CCEP) project level test/QA plans 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 High-TE test/QA
plans to facilitate independent reviews of project plans and test results, and to
provide a standard platform of understanding for 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. This GVP will ensure that project
results are compatible with and complementary to similar projects. All ETV
CCEP High-TE test/QA plans are adapted from this standard and the ETV
Program Quality Management Plan (QMP). These test/QA plans will contain
sufficient detail to ensure that measurements are appropriate for achieving project
objectives, that data quality is known, and that the data are legally defensible and
reproducible.
1.3 Organization of the High-TE 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.
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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
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
. Test/QA Plan 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 test/QA
plan 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. AEC/
NDCEE
Contract No.:
Task No.
APPROVALS
ETV CCEP Project Manager
Signature
Date
ETV CCEP QA Manager
Signature
Date
ETV EPA Project Officer
Signature
Date
ETV EPA Project QA Manager
Signature
Date
EPA - U.S. Environmental Protection Agency
DCC-W - Defense Contracts Command - Washington
AEC - Army Environmental Center
Figure 1. Test/QA 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. Coating application equipment
is continually being developed or redesigned to reduce any detrimental effects to
the environment. This is primarily accomplished by increasing the TE of the
coating operation and, therefore, reducing the amount of coating used, (i.e., less
overspray) and VOCs released into the environment. Often these coating
equipment technologies are slow to penetrate the market because potential users,
especially an ever-growing number of small companies, do not have the resources
to test the new equipment in their particular application and may be constructively
skeptical of the equipment provider's claims. If an unbiased, third-party facility
could provide pertinent test data, environmentally friendly coating equipment
technologies would penetrate the industry faster and accelerate environmental
improvements.
The ETV CCEP, a joint venture of the U.S. Environmental Protection Agency
(EPA) and CTC of Johnstown, Pennsylvania, in conjunction with the National
Defense Center for Environmental Excellence (NDCEE) Program, has been
established to provide unbiased, third-party 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 will
verify the performance of high-TE spray equipment.
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 Pollution Prevention (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.
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2.1.1 Demonstration Factory Testing Site
CTC has been tasked under the NDCEE Program to establish a
demonstration factory capable of prototyping processes that will reduce or
eliminate environmentally harmful materials used or produced in
manufacturing. To accelerate the transition of environmentally friendly
processes to the manufacturing base, CTC offers the ability to test
processes and products on full-scale, commercial equipment. It includes a
combination of organic finishing, cleaning, stripping, inorganic finishing,
and recycle/recovery equipment. The organic finishing equipment in the
demonstration factory will be available for the ETV CCEP testing
performed in this project. A layout of the CTC Demonstration Factory is
shown in Figure 2. A schematic of the organic finishing line (OFL) is
shown in Figure 3.
Demonstration
Factory
Organic Finishing
Powder Coat
Conventional Spray
Electrocoat (E-Coat)
CO2
2 I Inorganic Finishing
Advanced Electroplating
Ion Plating
Ion Implantation
Plasma Spray
High Velocity 02 Fuel
Ion Beam Assisted
Deposition
| 3 | Advanced Cleaning
Power Washer
Dual-Use Ultrasonic
Advanced Immersion
Supercritical CO2
Honeycomb Cleaning
| 4 | Coatings Removal
Solid Media Blast
Wet/Dry Blast
High-Pressure Waterjet
CO2 Pellet/Turbine Wheel
Ultrahigh-Pressure
Waterjet
Laser
Building
Support System
Shipping
&
Receiving
Process Water Reuse/Recycle
Cross-Flow Microfiltration
Diffusion Dialysis
Electrowinning
Ion Exchange
Membrane Electrolysis
Reverse Osmosis
Vacuum Evaporation
Figure 2. Demonstration Factory Layout
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POWDER COAT
SUBSYSTEM
CLEANING PRETREATMENT
Figure 3. Demonstration Factory OFL
In the event that a particular technology demonstration or laboratory
analysis cannot be performed at CTC, arrangements will be made to
ensure the requirements of the test/QA plan and all associated QA
procedures are completed.
2.1.2 Laboratory Facilities
In support of the demonstration factory coating processes, CTC maintains
extensive, state-of-the-art laboratory testing facilities. These laboratory
facilities are used for the measurement and characterization of processes
and specimens, as well as for bench-scale coating technology evaluations.
Table 1 lists the various testing and evaluation laboratories and the
representative equipment holdings that are relevant to ETV CCEP
equipment projects.
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Table 1. Testing and Laboratories and Representative Laboratory Equipment Holdings
Laboratory
Environmental Testing
Destructive and
Nondestructive Evaluation
Materials and Mechanical
Testing
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.
Calibration of equipment, sensors,
and components to nationally
traceable standards.
Laboratory Equipment
Hewlett Packard 5 972 A GC/MS
P-E Headspace GC/ECD/FID
Magnetic/Eddy Current Thickness
Salt Spray Corrosion Chamber
Microhardness/Tensile/Fatigue/Wear
Noran and CAMScan Electron Microscopes
Nikon and Polaroid Light Optical Microscopes
EDAX Energy Dispersive Spectrometer
Impact Testers
Transmation Signal Calibrator (milliamps,
millivolts)
Thermacal Dry Block Calibrator (Temperature)
Druck Pressure Calibrator (Pressure)
Fluke Digital Multimeter (Voltage)
2.2 Technical/Experimental Approach and Guidelines
The following tasks are proposed for tests completed according to this GVP:
Develop product-specific test/QA plan
Conduct verification and baseline (as needed) tests
Prepare Verification Report and Data Notebook
Prepare Verification Statement for approval and distribution
Table 2 describes the general guidelines and procedures that will be applied to
each test/QA plan.
Table 2. Overall Guidelines and Procedures Applied to Test/QA Plans
A detailed description of each part of the test will be given.
Critical and non-critical factors will be listed. Non-critical 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 test/QA plans 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.
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2.2.1 Test Approach
The following approach will be used for this GVP:
The vendor will select the performance parameters to be verified
and recommend the optimum equipment settings for application
and curing;
The ETV CCEP will obtain enough test panels and foil for the
verification and baseline tests;
The ETV CCEP will obtain enough coating to complete the
verification and baseline tests;
The vendor will provide the high-TE spray gun and all necessary
accessories to be verified;
The ETV CCEP will obtain the baseline spray equipment;
Data such as foil or panel weight (before coating and after curing),
quantity of sprayed coating, quantity of supplied coating, and mil
thickness of coating will be collected, following the ASTM
International methods, or equivalent;
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 test performed per this GVP are to verify
the transfer efficiency and the finish quality achieved by the candidate
technology and determine the technology's P2 benefits relative to a
baseline. During the coating application phase, parameters such as: inlet
air pressure, outlet air pressure, and airflow will be measured. During the
laboratory analysis phase, coated test panels and foils will be used to
measure TE. At a minimum, coated test panels will also be used to
measure parameters such as: dry film thickness (DFT), gloss, distinctness-
of-image (DOT), and visual appearance. The vendor may request
additional performance tests to verify a specific claim.
2.2.3 Large Target Description
The large target will consist of an uncoated steel plate backboard
measuring 91.4 cm by 91.4 cm (36 in. x 36 in.) attached to a stationary
stand in the middle of the spray booth. The backboard will be covered
with heavy gage (approximately 50 |j,m (0.002 in.)) aluminum foil by
wrapping the excess foil around the edges of the backboard. Clean pre-
weighed foil will be used to determine TE. In addition, cold-rolled steel
panels will be coated to determine finish quality.
Each spray gun will utilize multiple passes per coat on the finish quality
panels and foils using 50% overlap. The pattern for applying the coats
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will typically follow passes 1, 2, 3, then 4 (see Figure 4). If a second coat
is necessary, the pattern of the first coat will be repeated after a
predetermined flash time. All passes will begin and end on the backboard
(i.e., no lead or lag overspray). Also, there will be no overspray above or
below the backboard. All guns will travel the same horizontal distance
while spraying for each pass. All guns will be operated at the same
distance from the target. The fan pattern heights will vary depending on
the characteristics of the gun-coating interaction. The spray guns will
typically be operated with the fluid and fan adjustments set at full open.
However, the maximum variation between the fan patterns for each
coating will be no greater than 2.5 cm (1 in.). In other words, assuming
the smallest fan pattern is 25.4 cm (10 in.) for a particular coating, no
spray gun shall have a fan pattern greater than 27.9 cm (11 in.) for that
coating.
For each large target combination, a minimum of four (4) samples will be
collected per gun, per coating. First, three TE (foil only) samples will be
collected. Then, the backboard will be covered with a clean piece of
aluminum foil. A cold-rolled steel finish quality panel, meeting SAE 1008
specifications, measuring 30.5 cm tall by 45.7 cm wide (12 in. by 18 in.),
and treated with zinc phosphate at CTC, will be attached to the center of
the foil-covered backboard. The spray guns will coat the finish quality
panels using the same application pattern as the TE foils. A minimum of
one finish quality panel will be collected for each test combination. The
finish quality panels must be prepared under conditions representative of
those used to obtain the TE data.
Figure 4. Large Target Application Diagram
2.2.4 Small Target Description
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The small target will not use aluminum foil. The TE and finish quality
analyses will be conducted on the same type of panel. Therefore, only
three samples will be coated per gun per coating. The small panels will
measure approximately 12.7 cm by 30.5 cm (5 in. x 12 in.) and will be
made of 22-gauge cold-rolled steel meeting SAE 1008 specifications. The
small panels will be obtained and will be treated with a zinc phosphate
pretreatment at CTC.
Each spray gun will typically make 2 passes per coat on the small panels
using 50% overlap. The pattern for applying the coats will be passes 1
then 2 (see Figure 5). If a second coat is necessary, the pattern of the first
coat will be repeated after a predetermined flash time. Both the top and
bottom passes will lose 50% of their fan pattern to overspray above and
below the small panels. All passes will begin/end 6.4 cm (2.5 in.) from
the leading/trailing edges of the fan pattern to the beginning/ending edges
of the small panels (i.e., the spray guns will be triggered while in motion
and when the center of the air cap is 6.4 cm plus half the horizontal width
of the fan pattern away from the edge of the small panel). The guns will
maintain a fan pattern height of 25.4 cm (10 in.) by varying the gun-to-
target distance. The spray guns will be operated with the fluid and fan
adjustments set at full open. Three small panels will be coated for each
test combination and at least one of those panels will be randomly selected
and evaluated for finish quality.
Figure 5. Small Target Application Diagram
The small panels will be manually transported into and out of the spray
booth. A stand will be placed in the booth to hold the large backboard and
the small panels. Figure 6 is a schematic of the small panels and the large
finish quality panels showing the measurement locations for DFT and
gloss.
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12.7cm
30.5 cm
0 A 0 A 0
0 A 0 A 0
E
o
in
Small TE/Finish Quality Panels °
| Wet Film Fbints
O DFT Fbints
A Gloss Fbints
45.7cm
0 0
000
A A
000
A ° ° ° A
A A
O O O
0 0
Large Target Finish Quality Panels
Figure 6. Test Panel Measurement Locations
The test will consist of a number of test combinations. Each test
combination will consist of a spray gun (high-TE, high-volume, low-
pressure (HVLP) #1, or HVLP #2), a coating (e.g., primer, basecoat, or
topcoat), and a test panel (large combination foil, large combination finish
quality panel, or small combination TE/fmish quality panel). The large
foils will not be used for finish quality and the large finish quality panels
will not be used for TE analysis. The small panels will be used for both
TE and finish quality analysis.
2.2.5 Coating Specification
The vendor will choose the test coating(s) based on its use in the target
industry. The ETV CCEP will obtain a quantity of the test coating(s) to
complete the verification and baseline tests. The test coating(s) will be
prepared following the coating manufacturer's recommendations. The
exact coating preparation procedures will be recorded. For comparison,
the test coating(s) used during the verification test will be prepared the
same as the coating batches prepared for the baseline test. Coating
samples will be taken just prior to coating the test panels or foils to
measure the coating temperature, viscosity, percent solids, volatile content
and density. The coating measurements will be recorded on the coating
batch worksheet.
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2.2.6 Standard Apparatus
Figure 3 shows the testing location of the wet spray booth relative to the
OFL. All testing will be performed in the same wet spray booth.
The test panels and foils will be attached to a stand in the spray booth. A
programmable logic controller (PLC) will activate the motors that drive
the linear motion translators. The translator can move the spray gun
horizontally and vertically. The translator set-up could potentially cover
an area approximately 1.37 m by 1.37 m (4.5 ft x 4.5 ft). The test panels
and foils will be automatically sprayed using vertical overlap of the fan
pattern. The spraying mechanism's PLC will control the triggering of the
spray guns by way of pneumatically actuated clamp. During dwell time
between passes, coating flow will be interrupted to minimize coating
usage. Once the spray application is complete, the next rack or target will
be moved into position.
The spray booth air filters will be changed prior to setting up the standard
apparatus for the verification test. The pressure drop across the filters will
be checked prior to each run and at the end of the test. The pressure drop
is monitored in the event that the filter bank system malfunctions. A
pressure drop across the filter bank greater than 1 cm (0.4 in.) of water
shall indicate that the system requires service. As a comparison, the spray
booth air filters will also be changed before the baseline spray guns are set
up and tested as part of the TE baseline. This will minimize the difference
in the initial air booth velocity between the guns. The air booth velocity
will be measured in close proximity to the test panels or foils. Although
the air velocity through the booth will exceed 0.5 m/s (100 ft/min), the
velocity measured near the test panels or foils will be lower due to the
disruption of the air currents by the test panel or foil.
After a target is coated, the next target in that test combination will be
moved into position. After the test panels or foils have been cured, they
will be transferred to the laboratory for analysis.
2.2.7 Process Standards
The cold-rolled steel panels will consist of two sizes (see Figure 6). The
pretreatment method will be the same for all steel panels. The preparation
of the test coatings used for the verification test will be the same as the
HVLP tests. The TE analysis will follow Procedure A of ASTM D 5286.
The environmental (ambient) conditions of the demonstration factory will
be monitored, both inside the booth near the test panels or foils and near
the outside of the curing oven. The curing process for the verification test
will be similar to the baseline tests. Operating parameters during the
verification test will be held relatively constant and will be comparable to
the HVLP tests.
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2.2.8 Design of Experiment
This GVP provides procedures used to determine the performance
characteristics of high-TE spray equipment. A mean value and variance
(or standard deviation) will be reported for each critical response factor.
A confidence and specification limit of 95% will be applied to these tests.
Several test combinations will be used for each gun (multiple coating
types, two target sizes). The order in which the combinations will take
place will be randomized. This will enable both coating-to-coating and
gun-to-gun variations to be determined for each response factor. The
statistical analyses for all response factors will be performed using a
statistical software package.
2.2.9 Performance Testing
The ETV CCEP will consult the manufacturers' recommendations for key
operating factors to be used for testing, including the coating
specifications: viscosity, weight % solids, etc. Recommended equipment
settings for the coating will be obtained from the vendor. The ETV CCEP
will test these conditions prior to starting the verification test. These
conditions may be modified during the start-up phase to ensure proper gun
performance. During the actual tests, no attempt will be made to optimize
the equipment.
The high-TE spray equipment will be evaluated for both inlet and outlet
air pressures and airflow. Test panels and foils will be used to measure
equipment performance. The small panels and large finish quality panels
will be used for DFT, gloss, DOT, and visual appearance. The small
panels and large foils will be used for TE analysis. The coating
characteristics may be affected by other parameters of the testing process,
such as pretreatment, apparatus setup, and cleanup methods. The
pretreatment process will be the same for all test panels; therefore, the
variability of the pretreatment process should not be a significant factor.
Non-critical control factors will be monitored or held relatively constant
for the verification test. DFT measurements will be used to determine the
variations in film thickness. Gloss, DOT, and visual appearance tests will
be used to analyze the quality of the coating finish. TE measurements will
be used to determine the quantitative difference between the high-TE
spray equipment and a HVLP baseline. The TE test will follow Procedure
A of ASTMD5286.
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The small panels and large foils will be weighed and the weights recorded
prior to being placed in the spray booth. The weight of the gun, cup,
coating, and coating container will be recorded on the worksheets
immediately before applying the coating to each test panel. After each test
panel or foil has been coated, the spray gun, cup, coating, and coating
container will be re-weighed and the weights will be recorded. After the
panels or foils are cured, they will be re-weighed.
2.2.10 Quantitative Measurements
In order to evaluate the TE and the finish quality obtained by using the
high-TE and baseline spray guns, several measurements will be taken
from the non-coated and coated test panels and foils. In the case of the
non-coated panels or foils, the area in square feet and the weight of the TE
foils or panels will be measured. For the coated panels or foils, weight of
the TE foils and panels will be measured and DFT will be measured on the
finish quality panels. This procedure will follow ASTM D 5286 whenever
practical.
The uniformity of the coating applied can be determined by measuring
DFT at several specified locations on the test panels. Measurements will
be taken fifteen (15) locations on the large panels and at nine (9) locations
on the small panels. Figure 6 displays the test panels with their respective
locations of the film thickness and gloss measurements. Gloss
measurements will be taken at five (5) locations on both the large and
small panels. These sites will be numbered and measurements will be
taken accordingly. The recorded measurements will be correlated to a
specific site on each test panel for each test.
In addition to the performance analyses, the ETV CCEP will evaluate the
potential environmental benefits associated with using the high-TE spray
gun. Therefore, TE values will be quantitatively measured for each test
combination using nearly identical test conditions as the HVLP baseline.
A qualitative comparison will then be made to determine if the high-TE
spray gun exhibits a comparable or higher TE than the HVLP baseline.
2.2.11 Participation
The vendor of the technology being verified is welcome to participate in
the start-up phase and observe the verification and baseline testing. The
ETV CCEP personnel will be responsible for performing all necessary test
and demonstrations required for performance evaluation and full-scale
validation.
2.2.12 Critical and Non-Critical Factors
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For the purpose of this GVP, the following definitions will be used for
critical control factors, non-critical control factors, and critical response
factors. A critical control factor is a factor that is varied in a controlled
manner within the design of the experiment to determine its effect on a
particular outcome of a system. Non-critical control factors are all the
factors that are to be held relatively constant or randomized throughout the
testing for each specific piece of equipment (some non-critical factors may
vary from equipment to equipment). Critical response factors are the
measured outcomes of each combination of critical and non-critical
control factors given in the design of experiments.
In this context, the term "critical" does not convey the importance of a
particular factor (that can only be determined through experimentation and
characterization of the total process), but its relationship within the design
of experiments. In the case of the verification testing of a particular piece
of coating equipment, the only critical control factors are the pieces of
coating equipment themselves. All other processing factors will be held
relatively constant (or randomized) and are non-critical 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 this GVP, the critical control factors, non-critical factors, and critical
response factors are identified in a table format along with acceptance
criteria (where appropriate), data quality indicators, measurement
locations, and measurement frequencies, broken down by each run. For
example, parameters associated with the test panel pretreatment will
remain constant and thus be non-critical control factors, while a parameter
such as DFT is identified as a critical response factor.
The only critical control factors are the high-TE and HVLP spray guns
themselves (see Table 3). Examples of the non-critical control factors are
shown in Table 4, and examples of the critical response factors to be
measured are shown in Table 5.
For finish quality targets, the pretreatment process provides a continuous
surface on which the test coating can then be applied. To verify that these
panels have been pretreated properly, coating weights will be determined
on three (3) large panels and three (3) small panels prior to the coating
application phase.
Where appropriate, the output air pressure will be measured using a
pressure gauge obtained from the spray gun manufacturers. The ETV
CCEP will check the accuracy of these gauges before and after testing.
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The airflow requirements of the high-TE and baseline spray guns will be
determined during this test. The airflow will be measured using a
calibrated flow meter. Data will be recorded in m3/min.
The DFT measurements will follow ASTM B 499 (Magnetic), and will be
taken on all coated test panels. The gloss analysis will follow ASTM D
523, and will be taken on all coated test panels. DOT analysis will follow
ASTM D 5767 Test Method B (except that an eight-bladed rotating disc
will be used instead of the sliding combed shutter). The visual appearance
analysis will use normal lighting to examine the surface of the coated
panel. The panels will be examined for fish-eyes in the finish, the
presence of orange peel, the evenness of the coating, and the difference in
the visual gloss caused by sandpaper finish, drips, runs, and inclusions
(such as dirt, fuzz, and fibers).
The TE test will follow ASTM D 5286. An average TE value will be
determined for each combination.
The values in the total number column reflect the experimental design of
coating eighty test panels.
Table 3. Critical Control Factors
Critical
Control
Factor
High-TE
HVLP#1
HVLP#2
Air Cap
TBE
TBE
TBE
Fluid
Nozzle
TBE
TBE
TBE
Fan
Adjustment
TBE
TBE
TBE
Fluid
Adjustment
TBE
TBE
TBE
Fan
Pattern at
the Target
TBE
TBE
TBE
TBE - To be established in each product specific test/QA plan
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Table 4. Non-Critical Control Factors
Non-Critical
Factor
Product Involved in
Testing
Pretreatment Analysis
Surface Area of Test
Panels
Ambient Factory
Relative Humidity
Ambient Factory
Temperature
Spray Booth Relative
Humidity
Spray Booth
Temperature
Spray Booth Air
Flow
Temperature of Panels as
Coated
Distance from Gun to
Panels
Horizontal Gun
Traverse Speed
Vertical Drop
Between Passes
Volatile Content of
Applied Coating
Density of Applied
Coating
Wt.% Solids of Applied
Coating
Coating Temperature, as
Applied
Coating Viscosity as
Applied (#4 Ford)
Cure Time
Cure Temperature
Set Points/
Acceptance
Criteria
Two sizes of test
panels
Varies < 1.2 g/m2
Varies <10% within
and between tests
Varies < 10%
during test
Varies <5 °C during
test
Varies < 10%
during test
Varies <5 °C during
test
0.4-0.6 m/s
(80-120 ft/min)
Varies <5 °C during
test
Varies < 1.3 cm
(<0.5 in.) during test
TBE
TBE
Varies <5% for each
coating
Varies <50 g/L for
each coating
Varies <5% for each
coating
Varies <5 °C during
test
Varies <5 seconds for
each coating
1 hour
110°C
(230 °F)
Measurement
Location
Factory floor
Random panels
removed prior to
start-up
Factory floor
Factory floor
Factory floor
Factory floor
Factory floor
Factory floor
Center of test panel
Factory floor
Factory floor
Factory floor
Sample from
coating pot
Sample from
coating pot
Sample from
coating pot
Sample from
coating
Sample from
coating pot
Factory floor
Factory floor
Frequency
TBE based on the
number of test
coatings chosen
3 large and 3 small
from initial lot of
panels
Once per test
combination
Once per test
combination
Once per test
combination
Once per test
combination
Once per test
combination
Once per test
combination
Once per test
combination
Once per test
combination
Once per test
combination
Once per test
combination
1 sample per test
combination
1 sample per test
combination
1 sample per test
combination
1 sample per test
combination
1 sample per test
combination
Once per test
combination
Once per test
combination
Total Number
for the Test
TBE
6
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE - To be established in each product specific test/QA plan
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Table 5. Critical Response Factors
Critical Response Factor
Dynamic Inlet Air
Pressure
Dynamic Outlet Air
Pressure (Air Cap)
Air Consumption
DFT
(Magnetic method)
Gloss
DOI
Visual Appearance
Transfer Efficiency
Measurement Location
Factory Floor
Factory Floor
Factory Floor
Figure 6 shows location
of measurement points.
From ASTMD 523
ASTMD 5767 Test
Method B2
Entire test panel
From ASTM D 5286
Frequency
Once per test combination
Once per test combination
Once per test combination
1 5 points on each large panel
9 points on each small panel
5 points on each panel
1 point on one random panel
per test combination
1 per panel
One per test combination
(average of all panels in
combination)
Total Number for
the Test
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE
TBE - To be established in each product specific test/QA plan
1 See Sections 2.1.3 and 2.2 for the environmental basis to which these factors relate.
2 Will follow the ASTM International method except that an eight-bladed rotating disc will be used instead of the combed
shutter. This is an optional test, dependent on the types of coatings chosen.
Some target factors that may be used to test high-TE spray equipment include:
Overlap
Number of passes
Number of coats
Target dry film thickness
50%
Established in test/QA plan
Established in test/QA plan
Established in test/QA plan
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2.3 Schedule
ETV CCEP uses standard tools for project scheduling. Project schedules are
prepared in Microsoft Project, which is an accepted industry standard for
scheduling. 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 high-TE spray equipment.
Table 6. Estimated Schedule as of 9/27/06
ID
Taskl
Task 2
TaskS
Task 4
TaskS
Task 6
Name
Approval of Test/Q A Plan
Verification Testing
Complete Data Analyses
Prepare Verification Report
Approval of Verification Report
Issue Verification Statement
Duration
30d
20d
20d
30d
60d
15d
Start Date
TBE
TBE
TBE
TBE
TBE
TBE
Finish
Date
TBE
TBE
TBE
TBE
TBE
TBE
TBE - To be established in each product specific test/QA plan
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i .0 PROJECT ORGANIZATION AND RESPONSIBILITIES
CTC employs a matrix organization, with program and line management, to perform
projects. The laboratory supports the ETV CCEP project manager 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
manager on testing schedules. The ETV CCEP project manager will be responsible for
preparing the test/QA plans and Verification Report and Statement for each test.
The ETV CCEP QA manager, who is organizationally independent of both the laboratory
and the program, is responsible for administering CTC policies developed by the 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 manager
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 7. A summary of the
responsibilities of each ETV CCEP 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 Manager
Robert Fisher
_L
ETV CCEP Laboratory
Leader
Lynn Summerson
ETV CCEP Organic
Finishing Leader
Stephen Kendera
Figure 7. Project Organization Chart
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Table 7. Summary of ETV CCEP Experience and Responsibilities
Key CTC Personnel and Roles
Heather Moyer
NDCEE Program Manager
Shannon Miller - ETV CCEP
QA Manager
Rob Fisher Staff Process
Engineer/ ETV CCEP Project
Manager
Lynn Summerson - ETV CCEP
Laboratory Leader/ Statistical
Support Staff
Stephen Kendera - ETV CCEP
Organic Finishing Leader
Responsibilities
Manages NDCEE Program
Accountable to CTC Technical Services
Manager and CTC Corporate Management
Responsible for overall project QA
Accountable to NDCEE Program Manager
Technical project support
Process design and development
Accountable to NDCEE Program
Manager
Laboratory analysis
Accountable to ETV CCEP Project
Manager
QC Analysis
Accountable to ETV CCEP Project
Manager
Applicable Experience
Project Manager
(10 years)
Quality Mgmt. /ISO 9000 (6 years)
Environmental Compliance and ISO
14000 Management Systems (6 years)
ISO Internal Auditor (5 years)
Organic Finishing Regulations
(10 years)
Organic Finishing Operations
(10 years)
Registered Professional Engineer
Industrial and Environmental
Laboratory Testing (22 years)
Organic Finishing Operations
(25 years)
Education
B.S., Chemical
Engineering
B.A.,
Communications
M.S.,
Manufacturing
Systems
Engineering
B.S., Chemical
Engineering
M.S., Chemistry
B.S., Chemistry
N/A
Time
Dedication
1%
5%
60%
15%
5%
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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.
Table 8. Frequency and Mechanisms of Communications
Initiator
NDCEE Program Manager,
ETV CCEP Project
Manager
ETV CCEP Project
Manager
ETV CCEP Laboratory
Leader
ETV CCEP QA Manager
EPA ETV CCEP Project
Officer
Recipient
EPA ETV CCEP Project
Officer
NDCEE Program Manager
ETV CCEP Project
Manager
NDCEE Program Manager
CTC
Mechanism
Written Report
Verbal Status Report
Written or Verbal Status
Report
Data Reports
Quality Review Report
Onsite Visit
Frequency
Monthly
Weekly
Weekly
As Generated
As Required
At Least Once per
Year
Special Occurrence
Schedule or Financial
Variances
Major (will prevent
accomplishment of
verification cycle testing)
Quality Objective Deviation
Initiator
NDCEE Program Manager
or ETV CCEP Project
Manager
NDCEE Program Manager
or ETV CCEP Project
Manager
Recipient
EPA ETV CCEP Project
Officer
EPA ETV CCEP Project
Officer
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 Manager
Statistical Support
Responsibility
Overall coordination of project
Audits of verification testing operations and laboratory analyses
Coordinates interpretation of test results
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4.0 QUALITY ASSURANCE OBJECTIVES
4.1 General Objectives
The overall objectives of this ETV CCEP GVP are to verify the performance of
high-TE spray equipment spray by establishing the TE improvement and by
documenting finish quality. These objectives will be met by controlling and
monitoring the critical and non-critical factors, which are QA objectives for each
technology-specific test/QA plan based on this GVP. Tables 3 and 4 list the
critical and non-critical control factors, respectively.
The analytical methods that will be used for coating evaluations are adapted from
ASTM International 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 A (ASTM International 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 non-critical control factors. 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 and/or spikes and must fall within the
values found in the specific methods expressed.
The ETV CCEP will coordinate efforts to statistically evaluate test results and QA
objectives.
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Table 10. QA Objectives for Precision, Accuracy and Completeness for All Non-Critical
Control Factor Performance Analyses
Measurement
Product Involved in Testing
Pretreatment Analysis
Surface Area of Test Panels
Ambient Factory Relative
Humidity
Ambient Factory Temperature
Booth Relative Humidity
Booth Temperature
Spray Booth Air
Flow
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
Wt.% Solids of Applied Coating
Coating Temperature, as
Applied
Coating Viscosity as Applied
(Ford #4 Cup)
Cure Time
Cure Temperature
Method
Test panels
ASTM B 767
Ruler
Thermal
Hygrometer
Thermal
Hygrometer
Thermal
Hygrometer
Thermal
Hygrometer
per ACGIH
Infrared (IR)
Thermometer
Ruler
Stopwatch
Ruler
ASTM D 3 960
ASTM D 1475
ASTM D 2369
Thermometer
ASTM D 1200
Stopwatch
Thermocouple
Units
N/A
g/m2
cm2
(ft2)
RH
°C
RH
°C
m/s
(ft/min)
°C
cm
(in.)
cm/s
(in./s)
cm
(in.)
g/L
(Ib/gal)
g/L
(Ib/gal)
%
°C
seconds
minutes
°C
Precision
N/A
±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)
±0.5%
±0.15
(±0.06)
±5%
±0.15
(±0.06)
±0.6%
±0.6%
±1.5%
±0.5 °C
±10%
±5%
±0.5 °C
Accuracy
N/A
±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)
±1.0%
±0.15
(±0.06)
±5%
±0.15
(±0.06)
±1.8%
±1.8%
±4.7%
±0.2 °C
±10%
±5%
±0.2 °C
Completeness
100%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
ACGIH - American Conference of Governmental Industrial Hygienists, Inc.
* Accuracy and Precision stated by the manufacturer for velocities ranging from 20-100 ft/min
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Table 11. QA Objectives for Precision, Accuracy and Completeness for All Critical Response
Factor Performance Analyses
Measurement
Dynamic Inlet Air Pressure
Dynamic Outlet Air Pressure
(Air Cap)
Air Consumption
DFT - Magnetic
Gloss
DOI
Visual Appearance
Transfer Efficiency
Method
Pressure Gauge
Pressure Gauge
Flow Meter
ASTMB499
ASTM D 523
ASTM D 5767
Method B
N/A
ASTM D 5286
Units
psig
psig
nrVmin
mils(1)
gloss units
DOI units
N/A
%
Precision
+0.5 psig
+0.5 psig
+0.5%
RPD
20%
20%
20%
N/A
25%
Accuracy
+0.5%
+0.5%
+0.5%
10% true
thickness
+0.3
+3 DOI units
N/A
RSD<
20%(2)
Completeness
90%
90%
90%
90%
90%
90%
N/A
90%
(1) 1 mil = 0.001 in.
(2) Unknown according to ASTM D 5286
RPD = relative percent difference
RSD = relative standard deviation
N/A = Not Applicable
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, 80-120
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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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
per the specified test method. The degree of precision will be assessed
based on the agreement of all replicates within a property analysis group.
4.2.3 Completeness
The OFL and laboratory strive for at least 90% completeness.
Completeness is 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 OFL 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 non-conformance 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 non-conformance from test/QA plan QA objectives
occurs, the cause of the deviation will be determined by checking
calculations, verifying the test and measurement equipment, and re-
analysis. If an error in analysis is discovered, re-analysis 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/or
measurement system accuracy checks are valid, the nature of any non-
conformance may be beyond the control of the laboratory. If, given that
laboratory quality control data are within specification, any non-
conforming 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 test/QA plan. Coating and environmental performance
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will be evaluated using EPA, ASTM International, 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.
Test panels used in these tests will be compared to the performance
characteristics of the HVLP baseline guns 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 suppliers' literature and verified by setup testing. If the test data
meets the quantitative QA criteria (precision, accuracy, and completeness)
then the samples will be considered representative of the technology under
evaluation 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.
4.5 Impact of Quality
Due to the highly controllable nature of the test panel evaluation methods and
predictability of factors affecting the quality of the laboratory testing of panels,
the quality control of test panel performance characteristics is expected to fall
within acceptable levels. Comparison of response factors will be checked for run-
to-run process variations.
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5.0 SITE SELECTION AND SAMPLING PROCEDURES
5.1 Site Selection
Where possible, this project will be conducted at CTC, in Johnstown, PA, and
ETV CCEP personnel will perform all processing and testing, when possible.
The site for application and evaluation will be at the NDCEE demonstration
factory in the environmental technology facility (ETF) under the direct control of
the Engineering, Statistical Support, and OFL Groups. Application of the coating
involves transporting test panels in and out of the spray booth. The test panel will
be coated in the first of the two wet spray booths. Test panels will be evaluated
prior to application and after curing.
The experimental design involves applying coatings according to the
manufacturers' recommended optimum conditions. The test panels will be
sampled and analyzed to generate performance data.
5.2 Site Description
Figure 2 illustrates the overall layout of the NDCEE demonstration factory and
the location of the process equipment that will be used for this project. This
project may involve the use of the pretreatment line, the wet spray booths, and the
wet cure oven. Other equipment or testing sites may be used, as necessary.
5.3 Sampling Procedures and Handling
Test panels and foils will be used in this project. These will be pre-labeled by
marking their ID (identification) number with permanent marker on the untreated
side of the test panels or foils. The number of test panels and foils processed
during the testing depends on the experimental design, which in turn, depends on
any equipment provider's claim(s) about performance and the respective
confidence levels given in the responses to the Request for Technology. If no
specific performance characteristics are requested for verification by the high-TE
equipment providers, the default experimental design of three TE targets and one
finish quality target per test combination will be used.
A factory operations technician and laboratory analysts will process the test
panels according to a pre-planned sequence of stages, which includes those
identified in Table 12.
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Table 12. Process Responsibilities
Procedure
Visual inspection of test panels or foils
Numbering of test panels or foils
Initial weight of test panels or foils
Arrange test panels or foils in the spray booth
Prepare the coating
Setup the high-TE gun or baseline guns
Take coating samples and measurements
Load coating & prime gun
Perform setup trials (before first run only)
Initial weight of gun, pump, and coating container
Apply coating to test panels or foils
Take process measurements
Cure test panels or foils
Final weight of gun, pump, and coating container
Wrap/stack/transfer test panels or foils to lab
Operations
Technician
X
X
X
X
X
X
X
X
X
Laboratory
Analyst
X
X
X
X
X
X
X
X
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. The laboratory analyst will process the test panels through the
laboratory login prior to performing the required analyses.
5.4 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 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
The NDCEE shall maintain a record of calibrations and certifications for all
applicable equipment used during ETV CCEP testing. Testing and measuring
equipment shall be calibrated prior to the verification test and after the
verification test analyses are complete.
6.1.1 Facility Testing and Calibration
Calibration procedures the ETV CCEP within the OFL 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. All equipment used within the OFL
during ETV CCEP testing will be calibrated according to relevant portion
of Tables 13 and 14.
6.1.2 Laboratory Testing and Calibration Procedures
The analytical methods performed at CTC are adapted from standard
ASTM International, MIL-SPEC, EPA, Association of Official Analytical
Chemists and/or 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 are calibrated
before use and are verified during use and/or immediately after each
sample batch. Standard solutions are purchased from reputable chemical
supply houses in neat 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, are outside method performance standards. As needed,
equipment will be sent off-site for calibration or certification.
The listing of ASTM International Methods for dry film thickness, gloss,
DOI, and transfer efficiency can be found in Appendix A. All equipment,
used for these analyses, is calibrated according to Tables 13 and 14.
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Like the test panels and foils, the solids pans will be prepared as specified
by the ASTM International standard for determining volatile content of
coatings (ASTM D 2369). The solids pans will be labeled with an
identification number and letter. Two separate solids pans will be used for
each batch of coating and the values obtained will be averaged. The data
required for the solids test is recorded on the coating batch worksheet.
The percent of solids is calculated as:
N = [(W2-Wl)/S]x 100
where: Wl = the weight of the dish
W2 = weight of dish plus specimen after heating
S = Specimen weight (Syl - Sy2)
Syl = Syringe before dispensing coating
Sy2 = Syringe after dispensing coating
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, and/or the
published reference method's, instructions. Actual sample analysis will take place
only after setup is verified per 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 dry
film thickness instrument. Applicable ASTM International methods are listed in
Appendix A.
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 International and EPA,
and from accepted protocols provided by industrial suppliers.
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Table 13. Non-Critical Control Factor Testing and Calibration Criteria
Non-Critical
Factor
Products Involved
in Testing
Pretreatment
Analysis
Surface Area of
Test Panels
Ambient Factory
Relative
Humidity
Ambient Factory
Temperature
Spray Booth
Relative
Humidity
Spray Booth
Temperature
Spray Booth Air
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
Wt. % Solids of
Applied Coating
Coating
Temperature, as
Applied
Coating
Viscosity, as
Applied
Cure Time
Cure
Temperature
Method
Test panels
ASTMB767
Ruler
Thermal
Hygrometer
Thermal
Hygrometer
Thermal
Hygrometer
Thermal
Hygrometer
perACGIH
IR Thermometer
Ruler
Stopwatch
Ruler
ASTMD3960
ASTMD1475
ASTMD2369
Thermometer
ASTMD1200
Stopwatch
Thermocouple
Method
Type
N/A
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
Thermocouple/
(controllers)
Calibration
Procedure
N/A
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
Sent for calibration
or certification
Comparison to
NIST-traceable
standard
Calibration
Frequency
N/A
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
Six months
Semi-annually
Calibration
Accept. Criteria(l)
N/A
80-120%
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%
N/A
±1°C
(1) As a percent recovery of a standard
N/A = Not Applicable
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Table 14. Critical Response Factor Testing and Calibration Criteria
Critical
Measurement
Dynamic Inlet Air
Pressure
Dynamic Outlet Air
Pressure (Air Cap)
Air Consumption
DFT
Gloss
DOI
Visual Appearance
Transfer Efficiency
(product and coating
weights)
Method
Number(1)
Manufacturer's
recommendation
Manufacturer's
recommendation
Manufacturer' s
recommendation
ASTM B 499
ASTMD523
ASTM D 5767
Method B
N/A
ASTM D 5286
Method
Type
Pressure
gauge
Test cap
Flow Meter
Magnetic
Glossmeter
Image
analyzer
Visual
Weight
Calibration
Procedure
Comparison to
NIST-traceable
standard
Manufacturer' s
recommendation
Comparison to
NIST-traceable
standard
Comparison to
NIST-traceable
standard
Comparison to
NIST-traceable
standard
Manufacturer's
recommendation
N/A
Comparison to
NIST-traceable
standard
Calibration
Frequency
Annually
Manufacturer' s
recommendation
Six months
Verify calibration
after each run
Verify calibration
after each run
Manufacturer's
recommendation
N/A
Verify calibration
prior to each use
Calibration
Accept. Criteria
±5 psig
Manufacturer' s
recommendation
±1% of full scale
90-110%
90-110%
Manufacturer's
recommendation
N/A
±3.0 g
(1) Listing of ASTM International methods to be used is provided in Appendix A.
(2) As a percent recovery of a standard
N/A = Not Applicable
6.4 Non-Standard Methods
CTC will not use any non-standard methods for this project. However, for
methods that are non-standard (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 in-house developed protocols. 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 non-standard quantitative chemical procedure is
being performed, it should produce replicate results of+/- 25 relative percent
difference 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 non-standard 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
and/or process level. Process data is 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
signal or processed signal, and/or qualitative observations will be
recorded. Comments to document unusual or non-standard observations
also will be included on the forms as necessary. Raw data will be
processed manually by the analyst, 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 kept together for each
sample batch. From the documented procedures and the raw data bench
files, the steps leading to a final result may be traced.
7.1.1 Variables Used In Analysis
CS - The mass of (wet) coating sprayed
%S - The percent of the coating which is non-volatile (solids)
SS - The mass of coating solids sprayed is equal to (CS x %S) /100%
SD - The mass of solids deposited
TE - Transfer efficiency is equal to (SD / SS) x 100%, expressed as a
percentage
The accuracy of the TE values can be calculated based on the accuracy of
each of the measurements involved. Random errors propagate as follows.
7.1.2 Error in Mass of Coating Sprayed.
The coating sprayed (CS) is the difference between two masses, the mass
of the coating pot prior to and after applying the coating to the foils. The
scale has an accuracy of+/- 0.01 g. The mass of coating sprayed on each
foil should be on the order of 50 g. Since two weight measurements must
be made, and each contains an uncertainty of 0.01 g, the total uncertainty
in a worst-case scenario is 0.02 g. The uncertainty in the mass sprayed, is
+/- 0.04%.
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7.1.3 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
pan solids (PS).
%S = (PS - EP) / (FS-ES) x 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 x 0.0005 g. Since between 0.2 and 0.3 g of coating is used in the test,
this uncertainty becomes negligible compared to the numerator
uncertainty. Only about 0.05-0.1 g of solids 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.
7.1.4 Error in Mass Deposited.
The mass of the solids deposited on the foils is measured by weighing the
foils before and after spraying. The scale used has an accuracy of+/-
0.001 g. The mass of solids typically deposited on each foil is on the
order of 20 g. A control foil is also weighed to determine whether the
foils gain or lose weight during the curing process, which results in two
additional weight measurements. Since four weight measurements must
be made, and each contains an uncertainty of 0.001 g, the total uncertainty
in a worst-case scenario is 0.004 g. The uncertainty in the mass deposited,
is +/- 0.02 %.
7.1.5 Calculation of Transfer Efficiency.
SD is the weight of the product after spraying and curing, minus the
weight of the bare product. SS is the product of CS and %S divided by
100. The transfer efficiency is calculated as below:
TE% = (SD/SS)xlOO%
The method for calculating %TE has been redefined (per ASTM D 5286)
to consider the TE per run. By this method, the formula is as follows:
TE (%) = (average weight gain of test panels in a run) x 100%
(weight of paint solids sprayed) / (number of panels per run)
An example calculation is included below:
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TE (%) = 0.8 gx 100%
(4.8 g)/3
TE (%) = 80%
1.6
TE (%) = 50%
The relative TE improvement is determined using the equation below:
TERI (%) = (TEHirf.-TF. - TEHVT.P Ave) X 100%
TEHVLP_Ave
T£RI - the relative improvement over the HVLP baseline average
TEniph-TF, - the average TE for the High-TE system
TEHVLP Ave - the average TE for all three HVLP guns
For example, for the TE data (High-TE = 60%, HVLP average = 50%):
TEm(%)= (60% - 50%) x 100% = 20%
50%
7.2 Preliminary Data Package Validation
The generating operation technician and analyst will assemble a preliminary data
package. 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 to the ETV CCEP laboratory manager.
7.3 Final Data Validation
The ETV CCEP laboratory manager shall be ultimately responsible for all final
data released from this project. The ETV CCEP laboratory manager will review
the final results for adequacy to project QA objectives. If the manager suspects
an anomaly or non-concurrence 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 and the ETV CCEP laboratory leader about the non-
conformance. Also, he will request specific corrective action. If suspicion about
data validity still exists after internal review of laboratory records, the ETV CCEP
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Laboratory manager may authorize a re-analysis. If sufficient sample is not
available for re-testing, a re-sampling will occur. If the sampling window has
passed, or re-sampling is not possible, the ETV CCEP laboratory manager will
flag the data as suspect and notify the ETV CCEP project manager. The ETV
CCEP laboratory manager will sign and date the final data package.
7.4 Data Reporting and Archival
7.4.1 Calculation of DFT
The DFT gauge has a stated accuracy of 0.1 mil. NIST traceable thickness
standards will be used to calibrate the DFT gauge. DFT measurements
will be made at several locations on each product. The location of each
measurement is indicated in Figure 6.
7.4.2 Interpretation of the Numerical Results
The overall accuracy of the test data will allow calculation of TE to within
a few percent. The largest uncertainty lies in the mass-used values, which
contain a random error of about 2%, due to the solids calculation. The
mass-deposited values are estimated to be within 1% and an overall
accuracy of 3% leaves a reasonable margin.
7.4.3 Evaluation of the High-TE Spray Gun
A report signed and dated by the ETV CCEP laboratory manager will be
submitted to the ETV CCEP project manager, the ETV CCEP QA
manager, the EPA QA manager, and other technical principals involved in
the project. 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 manager 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 staff, the vendor, 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.
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7.5 Verification Statement
The ETV CCEP will also prepare a 3-7 page Verification Statement summarizing
the information contained in the Verification Report. After receiving the results
and conclusions from the ETV CCEP project manager or the NDCEE program
manager, 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
8.1 Guide Used for Internal Quality Program
The ETV CCEP uses the NDCEE facility and its QA system to verify coating
technologies. The NDCEE has established an International Organization for
Standardization (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. The ETV CCEP
verifications adhere to the ETV Program QMP, the ETV CCEP QMP, and the
ANSI/ASQC standards.
Table 15. NDCEE Environmental 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 ETF Environmental Laboratory and OFL used by ETV CCEP
follow published methodologies, wherever possible, for testing protocols.
Laboratory methods are adapted from Federal Specifications, Military
Specifications, ASTM International Test Methods, and supplier instructions. The
laboratory adheres to the QA/QC requirements specified in these documents. In
addition, where QA/QC criteria are not specified, or where the laboratory
performs additional QA/QC activities, these protocols are explained in the
laboratory's work instructions. Each NDCEE facility that uses supplied products
implements its own level of QA/QC. During ETV CCEP testing, the NDCEE
laboratory at ETF 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 OFL staff to ensure the appropriate parts, panels, samples, and
operating conditions are used. The laboratory also monitors its reagent deionized
water to ensure it meets purity levels consistent with analytical methodologies.
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The filters are replaced quarterly before failures are encountered. Samples are not
processed until the filters are replaced when failures do occur. 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.
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 International 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 International Class 1 weights.
Reagents purchased directly by the laboratory are American Chemical Society
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 meet hazardous waste handling requirements.
8.4 Specific Checks
The NDCEE Environmental Laboratory will analyze uncoated panels for dry film
thickness 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/or the project-specific QA/QC objectives. Laboratory records
are maintained with the sample data packages and/or in centralized files, as
appropriate. To ensure comparability, the laboratory 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 International, Federal, and Military methods that are accepted in
industry for product evaluations and supplier-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 A.
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9.0 PERFORMANCE AND SYSTEM AUDITS
The 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 is consistent with the audit
requirements specified in the ETV Program 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.
On-Site Visits
The EPA ETV CCEP project officer and EPA ETV CCEP QA manager may visit the
ETV CCEP for an on-site visit during the execution of this project. All project, process,
quality assurance, and laboratory testing information will be available for review.
Performance Evaluation 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 listing 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 manager. The ETV CCEP QA
manager will conduct an initial audit, and additional audits thereafter according to the
ETV CCEP QMP, of verification and testing activities. The results of this activity will be
forwarded to EPA in reports from the NDCEE program manager or the ETV CCEP
project manager.
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) x 100%] / [(Cl + C2) / 2]
where: C1 = larger of the two observations
C2 = smaller of the two observations
Relative Standard Deviation (RSD) = (s/y) x 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% x [(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%x(Cm/Csrm)
where: Cm = observed concentration of reference material
Csrm = theoretical value of srm.
10.3 Completeness
Percent Completeness (%C) = 100% x (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 supplier 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 and/or accuracy indicators.
Such nonconformances will be documented on a process or laboratory 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 and/or sample analyses are completed. These types of
nonconformances are typically detected at the laboratory manager level of data
review. In all cases of nonconformance, the laboratory manager 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 NDCEE will contact
the EPA ETV CCEP project officer. In cases of routine nonconformance, EPA
will be notified in the NDCEE program manager's or ETV CCEP project
manager's regular reports to the EPA ETV CCEP project officer. 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
manager, and on-site visits by the EPA ETV CCEP project officer, 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 7, the ETV CCEP QA manager is
independent from the project management team. It is the responsibility of the ETV
CCEP QA manager to monitor ETV CCEP verifications for adherence to the ETV CCEP
QMP. The laboratory manager monitors the operation of the laboratory on a daily basis
and provides comments to the ETV CCEP QA manager to facilitate their activities. The
ETV CCEP QA manager 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 manager. The ETV CCEP project manager will ensure
these reports are included in the report to the EPA. The laboratory manager 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 objectives in
Section 4.1
. Specific assessment of data quality in terms of quantitative and qualitative
indicators listed in Sections 4.2 and 4.3
Listing and summary of all nonconformances and/or 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 the ETV CCEP in relation
to current projects
Limitations on conclusions, use of the data
Planned QA activities, open items for next reporting period
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APPENDIX A
ASTM International Methods
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ASTM International Methods
ASTM B 499 Standard Test Method for Measurement of Coating Thickness by the
Magnetic Method: Nonmagnetic Coatings on Magnetic Basis Metals
ASTM B 767 Standard Guide for Determining Mass per Unit Area of Electodeposited and
Related Coatings by Gravimetric and other Chemical Analysis Procedures
ASTM D 523 -- Standard Test Method for Specular Gloss
ASTM D 1200 -- Standard Test Method for Viscosity by Ford Viscosity Cup
ASTM D 1475 -- Standard Test Method for Density of Liquid Coatings, Inks, and Related
Products
ASTM D 2369 -- Standard Test Method for Volatile Content of Coatings
ASTM D 3960 -- Standard Practice for Determining Volatile Organic Compound (VOC)
Content of Paints and Related Coatings
ASTM D 5286 Standard Test Method for Determination of Transfer Efficiency Under
General Production Conditions for Spray Application of Paint.
ASTM D 5767 Standard Test Methods for Instrumental Measurement of Distinctness-of-
Image Gloss of Coating Surfaces
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