Baltelle
Business of Innovation
Environmental Technology
Verification Program
Environmental and Sustainable
Technology Evaluations
Test/QA Plan for Verification of
Qualitative Spot Test Kits for Lead in
Paint
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Verification of
Qualitative Spot Test Kits for Lead in Paint
March 30, 2010
Prepared by
Battelle
505 King Avenue
Columbus, OH 43201-2693
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TABLE OF CONTENTS
Section
SECTION A PROJECT MANAGEMENT 7
Al Verification Test Organization 7
A2 Background 12
A3 Verification Test Description and Schedule 13
A4 Quality Objectives And Criteria for Measurement Data 15
A5 Special Training/Certification 17
A6 Documentation and Records 19
SECTION B MEASUREMENT AND DATA ACQUISITION 21
Bl Experimental Design 21
B2 Sampling Requirements 31
B3 Sample Handling and Custody Requirements 32
B4 Laboratory Reference Method 32
B5 Quality Control 33
B6 Instrument/Equipment Testing, Inspection, And Maintenance 34
B7 Calibration/Verification of Test Procedures 34
B8 Inspection/Acceptance of Supplies And Consumables 34
B9 Non-Direct Measurements 35
BIO Data Management 35
SECTION C ASSESSMENT AND OVERSIGHT 37
Cl Assessments and Response Actions 37
C2 Reports to Management 39
SECTION D DATA VALIDATION AND USABILITY 40
Dl Data Review, Validation, and Verification Requirements 40
D2 Validation and Verification Methods 40
D3 Reconciliation With User Requirements 41
SECTION E REFERENCES 42
El References 42
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List of Figures
Figure 1. Organization Chart for the Verification Test [[[ 8
List of Tables
Table 1. Planned Verification Test Schedule [[[ 14
Table 2. DQIs and Criteria for Critical Measurements for Reference Method ........................... 17
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ETV ESTE
Test/QA Plan for Verification of
Qualitative Spot Test Kits for Lead in Paint
March 30, 2010
APPROVAL:
Name
Company
Date
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DISTRIBUTION LIST
Julius Enriquez
Evelyn Hartzell
Michelle Henderson
U.S. Environmental Protection Agency
National Risk Management Research
Laboratory
USEPA Facilities
26 West Martin Luther King Drive
Mail Code: MS207
Cincinnati, OH 45268
Amy Dindal
Stephanie Buehler
Timothy Pivetz
Katherine Mitchell
Warren Strauss
Zachary Willenberg
Battelle
505 King Ave.
Columbus, OH 43201
Participating Lead Paint Test Kit Vendors
(TBD)
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SECTION A
PROJECT MANAGEMENT
Al VERIFICATION TEST ORGANIZATION
The verification test will be conducted under the auspices of the U.S. Environmental
Protection Agency (EPA) through the Environmental Technology Verification (ETV) Program.
It will be performed by Battelle, which is serving as the verification organization under the
Environmental and Sustainable Technology Evaluations (ESTE) arm of ETV.
The day to day operations of this verification test will be coordinated and supervised by
Battelle, with the participation of the vendors who will be having the performance of their
technologies for detecting lead in paint verified. Testing will be conducted at Battelle in
Columbus, Ohio. Each vendor will provide Battelle with their respective technology and will
train the Battelle staff in their technology use. Battelle technical staff as well as non-technical
operators will operate the technologies during verification testing.
The organization chart in Figure 1 identifies the responsibilities of the organizations and
individuals associated with the verification test. Roles and responsibilities are defined further
below. Quality Assurance (QA) oversight will be provided by the Battelle Quality Manager and
also by the EPA Quality Manager, at her discretion.
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Battelle
Management
Zachary Willenberg
Battelle
Quality Manager
Julius Enriquez
EPA ESTE
Project Officer
Michelle Henderson
EPA
Quality Manager
Dr. Stephanie Buehler
Battelle
Verification
Test Coordinator
Lead Paint Test Kit
Vendor
Representatives
Battelle
Technical Staff
Figure 1. Organization Chart for the Verification Test
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Al.l Battelle
Dr. Stephanie Buehler is Battelle's Verification Test Coordinator for this test. In this role,
Dr. Buehler will have overall responsibility for ensuring that the technical, schedule, and cost
goals established for the verification test are met. Specifically, Dr. Buehler will:
• Prepare the draft test/QA plan, verification reports, and verification statements.
• Establish a budget for the verification test and manage staff to ensure the budget is
not exceeded.
• Revise the draft test/QA plan, verification reports, and verification statements in
response to reviewers' comments.
• Assemble a team of qualified technical staff to conduct the verification test.
• Direct the team in performing the verification test in accordance with this test/QA
plan.
• Hold a kick-off meeting approximately one week prior to the start of the verification
test to review the critical logistical, technical, and administrative aspects of the
verification test. Responsibility for each aspect of the verification test will be
confirmed.
• Serve as the primary point of contact for vendor representatives.
• Ensure that confidentiality of sensitive vendor information is maintained.
• Assist vendors as needed during verification testing.
• Become familiar with the operation and maintenance of the technologies through
instruction by the vendors, if needed.
• Review and approve internal QA reviews and assessment reports.
• Review independent QA document reviews and assessment reports by EPA quality
manager.
• Respond to any issues raised in assessment reports, audits, or from test staff
observations, and institute corrective action as necessary.
• Coordinate distribution of the final test/QA plan, verification reports, and verification
statements.
Technical staff from Battelle will support Dr. Buehler in planning and conducting the
verification test. The responsibilities of the technical staff will be to:
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• Assist in planning for the test, and making arrangements for the receipt of and
training on the technologies.
• Attend the verification test kick-off meeting.
• Assist vendor staff as needed during technology receipt and training.
• Conduct verification testing using the vendor's technology and per the final test/QA
plan.
• Conduct reference testing.
• Perform statistical calculations specified in this test/QA plan on the technology data
as needed.
• Provide results of statistical calculations and associated discussion for the verification
reports as needed.
• Support Dr. Buehler in responding to any issues raised in assessment reports and
audits related to statistics and data reduction as needed.
Mr. Zachary Willenberg is Battelle's Quality Manager. Mr. Willenberg will:
• Review and approve the draft and final test/QA plan.
• Attend the verification test kick-off meeting.
• Conduct a technical systems audit at least once during the verification test, or
designate other Q A staff to conduct the audit.
• Audit at least 10% of the verification data or designate other QA staff to conduct the
data audit.
• Prepare and distribute an assessment report for each audit.
• Verify implementation of any necessary corrective action.
• Request that Battelle' s Verification Test Coordinator issue a stop work order if audits
indicate that data quality is being compromised.
• Provide a summary of the QA/QC activities and results for the verification reports.
• Review and approve the draft and final verification reports and verification
statements.
A1.2 Technology Vendors
The responsibilities of the technology vendors are as follows:
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• Review and provide comments on the draft test/QA plan.
• Accept (by signature of a company representative) the final test/QA plan prior to test
initiation.
• Provide adequate units of their technology for evaluation during the verification test.
• Provide all other equipment/supplies/reagents/consumables needed to operate their
technology for the duration of the verification test.
• Supply training on the use of the technology, and provide written consent and
instructions for test staff to carry out verification testing, including written
instructions for routine operation of their technology.
• Provide maintenance and repair support for their technology, on-site if necessary,
throughout the duration of the verification test.
• Review and provide comments on the draft verification report and statement for their
respective technology.
A1.3 EPA
EPA's responsibilities are based on the requirements stated in the "Environmental
Technology Verification Program Quality Management Plan" (EPA QMP).1 The roles of specific
EPA staff are as follows:
Ms. Michelle Henderson is EPA's Quality Manager for the verification test.
Ms. Henderson will:
• Review the draft test/QA plan.
• Approve the final test/QA plan.
• Perform at her option one external technical systems audit during the verification test.
• Notify the EPA ESTE Project Officer of the need for a stop work order if the external
audit indicates that data quality is being compromised.
• Prepare and distribute an assessment report summarizing results of the external audit.
• Review draft verification reports and verification statements.
• Approve final verification reports and statements.
Mr. Julius Enriquez is EPA's ESTE Project Officer. Mr. Enriquez will:
• Review the draft test/QA plan.
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• Approve the final test/QA plan.
• Review independent QA document reviews and assessment reports by EPA quality
manager.
• Review Battelle QA reviews and assessment reports and initiate corrective actions.
• Review the draft verification reports and verification statements.
• Oversee the EPA review process for the test/QA plan, verification reports, and
verification statements.
• Approve final verification reports and statements.
• Coordinate the submission of verification reports and verification statements for
signature by laboratory director and posting on the ETV website.
A1.4 Subcontract Laboratory
Any laboratory providing reference measurements will follow the requirements of the
reference methods as well as the QC requirements as stated in this test/QA plan. A subcontract
laboratory will provide reference measurements for the paint chip samples from each PEM. The
responsibilities of this laboratory will include:
• Proper receipt and handling of sample material.
• Accurate measurement of the target analyte(s) or target parameter(s).
• Submission of data and any supporting documents to Battelle.
• Participation in audit by Battelle Quality Manager and/or EPA's Quality Manager, if
requested.
• Submission of QC limits/criteria used by the laboratory for inclusion in this
document.
A2 BACKGROUND
The ETV Program conducts third-party performance testing of commercially available
technologies. The purpose of ETV is to provide objective and quality assured performance data
on environmental technologies, so that users, developers, regulators, and consultants can make
informed decisions about purchasing and applying these technologies. Stakeholder committees
of buyers and users of such technologies provide input on technology verifications.
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Lead-based paints were commonly used in houses in both interior and exterior
applications prior to 1978, when the US government banned the use of lead-based paint in
residential applications. The term lead-based paint means paint or other surface coatings that
contain lead at contents that equal or exceed a level of 1.0 milligrams per centimeter squared
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(mg/cm ) or 0.5 percent by weight. This paint still exists in many of these houses across the
country. The accurate and efficient identification of lead-based paint in housing is important to
the Federal government as well as private individuals living in residences containing such paints.
Renovation, Repair, and Painting (RRP) activities may disturb painted surfaces and produce a
lead exposure hazard. Such disturbances can be especially harmful to children and pregnant
women as lead exposure can cause neurological and developmental problems in both children
and fetuses. In fact, because of the large amount of pre-1978 housing stock, a report by the
President's Task Force on Environmental Health Risks and Safety Risks to Children found that
r\
approximately 24 million US dwellings were at risk for lead-based paint hazards .
A3 VERIFICATION TEST DESCRIPTION AND SCHEDULE
A3.1 Summary of Technology Category
There are lead-based paint test kits available to help home owners and contractors
identify lead-based paint hazards before any RRP activities take place so that proper health and
safety measures can be enacted. However, many of these test kits have been found to have high
rates of false positives3. The Renovation, Repair, and Painting rule4 calls for an EPA evaluation
and recognition program for test kits that are candidates to meet the goal of a 5% false negative
rate and 10% false positive rate. As stated in the Preamble to the rule, the test kit performance
must be validated by a laboratory independent of the kit manufacturer, using ASTM
International's El 828, Standard Practice for Evaluating the Performance Characteristics of
Qualitative Chemical Spot Test Kits for Lead in Paint5 or an equivalent validation method. EPA
will then only recognize those kits that have been verified through this process. ETV will
coordinate the testing and supply the data that will be used in the recognition process. This plan
incorporates ASTM Method El828 guidelines5.
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A3.2 Verification Test Schedule
Table 1 shows the planned schedule of testing and data analysis/reporting activities to be
conducted in this verification test. The planned dates for conducting verification tests of lead
paint test kits are December 2009 - April 2010 at Battelle's laboratories in Columbus, Ohio. A
final verification test schedule with specific test dates will be provided to participating vendors
once those details are known. It will be necessary for participating vendors to provide their
technologies to Battelle by the specified date so testing staff may become familiar with operating
the kits before testing begins. Vendor staff will provide training in operating the technologies
either in person or by teleconference. The period of operation for verification testing will be
approximately four to six weeks. The test procedures are described in Section B of this test/QA
plan.
Subsequent to the verification test, a separate verification report will be drafted for each
participating technology. These reports will be reviewed by the respective vendor and by peer
reviewers, and submitted to EPA for final signature and subsequent publication. Technologies
and associated equipment (but not consumables) will be returned to the vendors at the
completion of report writing, unless other arrangements have been made with Battelle.
Table 1. Planned Verification Test Schedule
Dates
December 2009
December 2009
-April 20 10
February - May
2010
May -July 20 10
July-
September2010
Testing Activities
Training of verification testing staff on
technology use
Conduct verification testing
Data Analysis and Reporting
Review and compile test data and records as they
become available.
Review and summarize verification testing staff
observations.
Prepare report templates and complete common
sections of reports.
Evaluate and analyze data generated during testing
Complete draft reports and submit for vendor, EPA,
and peer reviews.
Revise draft reports and submit final reports for
EPA approval.
A3.3 Test Site
Testing will be conducted in Battelle laboratories in Columbus, Ohio. There will be no
field testing, i.e., testing at an offsite location outside of the laboratory, such as a house,
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conducted during this technology verification. EPA is considering the possibility of a future
verification test involving real-world field environments.
A3.4 Health and Safety
Battelle will conduct all verification testing and reference lead paint spot test kit
measurements following the safety and health protocols in place for the laboratory and facilities.
This includes maintaining a safe work environment and a current awareness of handling
potentially toxic chemicals. Exposure to potentially toxic chemicals will be minimized, personal
protective equipment will be worn, and safe laboratory practices will be followed, as necessary.
Health and Safety will be reviewed with Battelle's Safety Officer once the specific technologies
to participate in the test are known.
A4 QUALITY OBJECTIVES AND CRITERIA FOR MEASUREMENT DATA
In performing the verification test, Battelle will follow the technical and QA procedures
specified in this test/QA plan and will comply with the data quality requirements in the EPA-
approved QMP6 for the Advanced Monitoring Systems (AMS) Center, except where differences
are noted for ESTE per the EPA ETV Program QMP.1 The objective of this verification test is to
evaluate the performance of test kits for the detection of lead in paint. This evaluation will assess
the capabilities of the lead paint spot test kits against laboratory prepared performance evaluation
material (PEM) samples, and will include a comparison between the lead paint test kit results and
those of a standard technique as described in Section B4. Additionally, this verification test will
rely upon verification testing staff observations to assess other performance characteristics of the
lead paint test kits. Only qualitative results (e.g., detect/non-detect of lead at specified levels)
will be considered for each technology. Below is a discussion of the quality objectives and the
criteria for measurement data that have been established to assure that the test objectives are met.
A4.1 Quality Objectives
Data quality objectives indicate the minimum data quality required to meet the lead paint
spot test kits verification objectives. Data quality objectives for this verification test include
those related to the reference method performance and those related to the test kit performance.
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Data quality objectives for the reference method (see Section B4) are presented in terms of data
quality indicator (DQI) criteria for the critical measurements associated with the reference
method and are listed in Table 2 and discussed in Section A4.2. The quality of the reference
measurements will be monitored using QC samples and procedures, as described in the testing
laboratory's procedures or the method. These requirements are further discussed in Section B.
Method blanks, positive control samples, and negative control samples are expected to be
included as QC samples for each technology. Method blank samples will include performance
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evaluation materials (PEMs) with 0.0 mg/cm lead paint as well as each PEM substrate (wood,
metal, drywall, and plaster) with no paint. Positive and negative control samples, if provided
with a test kit, will be analyzed according to the kit's instructions.
The EPA Quality Manager will perform a technical systems audit (TSA) of the
subcontract laboratory conducting reference analyses. The Battelle Quality Manager or his
designee will perform a TSA of the actual evaluation of the test kits at least once during this
verification test and will audit at least 10% of the verification data acquired, including the data
packages received from the subcontract reference laboratory. The EPA Quality Manager also
may conduct an independent TSA of the verification test, at her discretion.
A4.2 Criteria for Measurement Data
Reference measurements will be conducted by an NLLAP-accredited laboratory using
inductively coupled plasma-atomic emission spectrometry (ICP-AES) on paint chip samples
from each PEM used in the verification test. Table 2 presents the minimum DQIs and criteria for
the reference method critical measurements. These DQIs and criteria are based on NLLAP
guidelines and are consist with the selected NLLAP-accredited laboratory's criteria and
procedures. The method detection limit for the reference analyses will be determined based on
the criteria provided by the subcontract laboratory selected to perform the reference analyses.
The reference method measurement quality will be assured by adherence to these DQI criteria.
For batches of less than 20 samples, at least one sample will be analyzed for each applicable
DQI. Recommendations for appropriate positive and negative controls and their critical
measurements for the lead paint spot test kits will be provided by each vendor, as appropriate.
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SPECIAL TRAINING/CERTIFICATION
Documentation of training related to technology testing, data analysis, and reporting is
maintained for all Battelle technical staff in training files at their respective Battelle location. The
Battelle Quality Manager may verify the presence of appropriate training records prior to the
start of testing. The technology vendor will be required to train Battelle technical staff in the
operation of his/her technology prior to the start of testing. Battelle will document this training
with a consent form, signed by the vendor, which states which specific Battelle staff have been
trained and determined by the vendor to be competent in operation of the vendor's technology.
Table 2. DQIs and Criteria for Critical Measurements for Reference Method
DQI
Precision
Bias and Accuracy of
Instrument
Bias and Accuracy of
Sample
Measurements
Method of
Assessment
Replicate (duplicate)
analyses of test sample
extract
Instrument
calibration/performance
verification using
matrix-matched
reference standard
materials of the same
matrix as the samples
Independent
Calibration Verification
(ICV) - lead standard
at concentration in the
range of lead levels
tested
Initial Calibration
Blank (ICB) - contains
no lead and is used for
initial calibration and
zeroing instrument
response. The ICB
must be matrix
matched to acid content
present in sample
digestates.
Frequency
One per 20
samples or batch
(min. 5%
frequency)
Verified daily or
prior to analyzing
samples
Once per day
after calibration
Once per run at
the beginning of
the run
Minimum
Acceptance
Criteria
Within ±25% relative
percent difference
(RPD)
Per most stringent
instrument,
laboratory, or method
guidelines
Within ±10% of
known value
Absolute value not
more than 20% of the
regulatory limit or the
level of concern
Corrective Action
Flag data; reanalyze QC
samples; if these QC
samples are out of range,
then repeat entire analysis
including recalibration
and all QC samples
Recalibrate instrument
Recalibrate instrument
Prepare new calibration
curves
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DQI
Method of
Assessment
Continuing Calibration
Verification (CCV) -
independent reference
standards or the same
standards used to
prepare the instrument
calibration curve
Interference Check
Sample (ICS) - A
standard solution (or
set of solutions) used to
verify accurate analyte
response in the
presence of possible
interferences from
other analytes present
in samples. The ICS
must be matrix
matched to the reagent
content present in
sample digestates.
Continuing Calibration
Blank (CCB) - A
standard solution which
has no lead and is used
to verify blank
response and freedom
from carryover
Laboratory Control
Sample (LCS) - same
matrix as test samples
with lead concentration
near the level of
concern or regulatory
level; wherever
possible shall not
require extensive
pretreatment dilution or
concentration prior to
Frequency
At the beginning
and end of a
sample run, as
well as every 12
hours, or
according to
instrument
manufacturer's
recommendations,
or according to
instrument
Performance
Characteristic
Sheet, or at a
predetermined
SOP frequency
(once every 10
samples),
whichever is
more frequent
At the beginning
and end of each
run or twice every
12 hours
After each ICS
and CCV
1 per 10-20
samples or batch
(minimum 5%)
Minimum
Acceptance
Criteria
Within ±20% of
known value
Within 20% of known
value
Absolute value not
more than 20% of the
regulatory limit or
level of concern
Within ±20% of
known value
Corrective Action
Establish new calibration
curve and reanalyze
samples; sample analysis
shall not continue or be
restarted until a new
calibration curve is
established and verified
Apply correction factors
to sample results as
appropriate
Flag data; attempt to
determine source of
contamination; reanalyze
QC samples; if these QC
samples are out of range,
then repeat entire analysis
including recalibration
and all QC samples
Flag data; reanalyze QC
samples; if these QC
samples are out of range,
then repeat entire analysis
including recalibration
and all QC samples
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DQI
Method of
Assessment
analysis; shall be either
NIST Standard
Reference Materials or
commercially available
certified reference
materials
Matrix Spike Sample -
prepared using split
sample (before any
digestion when
possible); lead level
spiked shall be enough
to result in final lead
concentration of the
prepared sample of 5x
the sample's observed
lead concentration, or
5x the method
detection limit,
whichever is greater
Duplicate Samples - of
test sample extract only
Method Blank -
mixture of all reagents
used for digestion but
without the matrix; is
carried through all
steps of the analysis
starting with digestion
Frequency
1 per 20 samples
or batch
(minimum 5%)
1 per 20 samples
or batch
(minimum 5%)
1 per 20 samples
or batch
(minimum 5%)
Minimum
Acceptance
Criteria
Within ±25% of
calculated value
Within ±25% of RPD
Absolute value not
more than 20% of the
regulatory limit or
level of concern
Corrective Action
Flag data; reanalyze QC
samples; if these QC
samples are out of range,
then repeat entire analysis
including recalibration
and all QC samples
Flag data; reanalyze QC
samples; if these QC
samples are out of range,
then repeat entire analysis
including recalibration
and all QC samples
Flag data; attempt to
determine source of
contamination; reanalyze
QC samples; if these QC
samples are out of range,
then repeat entire analysis
including recalibration
and all QC samples
A6 DOCUMENTATION AND RECORDS
The records for this verification test include the test/QA plan, the protocols, laboratory
record books (LRB), data collection forms, electronic files (both raw data and spreadsheets), and
the final verification report and statement. All of these records will be maintained in the
Verification Test Coordinator's office or at the testing locations during the test and will be
transferred to permanent storage at Battelle's Records Management Office at the conclusion of
the verification test. All Battelle LRBs are stored indefinitely, either by the Verification Test
Coordinator or Battelle's Records Management Office. The EPA ESTE project officer or
appropriate EPA ETV management will be notified before disposal of any files. The results from
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the reference measurements made by the subcontractor laboratory will be submitted to Battelle
after making the measurement and obtaining the results of the analyses. Table 3 provides further
details the data recording practices and responsibilities. QA documents generated over the course
of this verification test include audit and assessment reports and will be maintained by the
Battelle Quality Manager. Copies of audit and assessment reports will be downloaded into the
ETV web database so that EPA may access it if needed.
All written records must be in ink. Any corrections to notebook entries, or changes in
recorded data, must be made with a single line through the original entry. The correction is then
to be entered, initialed, and dated by the person making the correction. In all cases, strict
confidentiality of the raw data from each vendor's technology, and separation of data from
different technologies, will be maintained throughout the verification test. Separate files
(including manual records, printouts, and/or electronic data files) will be kept for each
instrument.
Table 3. Summary of Data Recording Process
Data to Be
Recorded
Dates, time, and
details of test events
Sample (PEMs) used
(IDs, dates, etc.)
Test kit procedures
and sample results
Reference method
sample preparation
Reference method
procedures,
calibrations, QA, etc.
Where Recorded
LRBsordata
recording forms
LRBsordata
recording forms
Data sheets and LRB
LRB
LRB or data
recording forms
How Often
Recorded
Start/End of test
procedure, and at
each change of test
parameter
When each PEM is
used, throughout test
duration
Throughout test
duration
Throughout sample
preparation
Throughout sampling
and analysis
processes
By Whom
Battelle
Battelle
Battelle
Battelle or
subcontract
laboratory
NLLAP -accredited
laboratory
Disposition of
Data
Used to organize and
check test results;
manually
incorporated
in data spreadsheets
as necessary
Incorporated into
verification report as
necessary
Manually
incorporated into
data spreadsheets for
statistical analysis
and comparisons
Used to demonstrate
validity of samples
submitted for
reference
measurements
Retained as
documentation of
reference method
performance
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SECTION B
MEASUREMENT AND DATA ACQUISITION
Bl EXPERIMENTAL DESIGN
This verification test will specifically address verification of spot test kits for the
detection of lead in paint. This test follows procedures described in ASTM E18285. The lead
paint test kits will be tested only in a laboratory under controlled conditions; no field testing will
take place during this verification test. This will allow comparison of the technology results to a
reference method using a specified set of performance evaluation materials (PEMs). PEMs will
be 3 inch by 3 inch squares of wood, metal, plaster, or drywall coated with paint of various
colors containing a range of lead concentrations. PEM samples will be analyzed in at least
duplicate by the test kits and also analyzed by the reference method (ICP-AES). The lead paint
test kits participating in this test will be evaluated based on qualitative results, indicating only the
presence or absence of lead in the paint at specified concentrations (see Section B 1.1). Some test
kits may provide quantitative results. In the instance where quantitative measures are used in
determining the results for a particular technology, a qualitative result will be reported (i.e.,
presence or absence of the contaminant of interest) as with the other technologies, and the
quantitative measure used to determine that result will also be reported for that sample but will
not be used in any other data analyses as described in Section B1.2. The performance of the lead
paint test kits will be verified based on sensitivity, precision, false positive/negative rates, matrix
effects, and operational factors. These parameters are discussed in detail in Section Bl.l and
B1.2.
The analyses will be performed according to the vendor's recommended procedures as
described in the user's instructions or manual, which should be consistent with training provided
to Battelle staff. Similarly, calibration and maintenance of the technologies will be performed as
specified by the vendor. Results from the technologies being verified will be recorded manually
by the operator on appropriate data sheets or captured in an electronic data system and then
transferred manually or electronically for further data workup. Qualitative characteristics of each
technology such as ease of use will be assessed through observations made by the Test
Coordinator and operators throughout the verification test. The results from each technology will
be reported individually. No direct comparison will be made between technologies, but each
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technology will undergo similar testing so it is convenient for end users to evaluate the ETV
testing results.
Bl.l Test Procedures
Qualitative spot test kits for lead in paint will be evaluated against a range of lead
concentrations in paint on various substrates through the use of PEMs. PEMs are 3 inch by 3
inch square panels of wood (pine and poplar), metal, drywall, or plaster that will be prepared by
Battelle7. Table 4 shows the PEMs to be tested for each test kit. Each PEM will be coated with
the same thickness of either white lead or lead chromate paint. The paint will contain lead at 0.4,
9
0.6, 1.0, 1.4, 2.0, and 6.0 mg/cm . These lead concentrations were chosen based on guidelines
provided in EPA's lead RRP rule4 as well as to represent potential lead levels in homes.
After production of the 6.0 mg/cm2 PEMs, reference analyses results indicated that actual
lead levels for these PEMs were outside of the anticipated 6.0 mg/cm2 target level. For lead
chromate PEMs at 6.0 mg/cm2, 18 reference panels dispersed throughout the PEMs during
production7 indicated that actual concentrations ranged from 4.8 - 6.2 mg/cm2 with a mean of 5.2
9
mg/cm and a CoV of 9.6%. The 18 reference panels coated during the production of 6.0
9 _
mg/cm PEMs using white lead indicated that actual concentrations ranged from 5.6 to 18.4
9 _
mg/cm . Four white lead reference PEMs were considered to be "outliers" (18.4, 12.8, 11.3, and
9 fj
11.1 mg/cm ). Excluding these panels results in an average concentration of 8.0 mg/cm with a
CoV of 12% for this level. Though both the lead chromate and white lead PEMs are outside of
the expected 6.0 mg/cm2 concentration, it was determined that these PEMs were acceptable for
use. The purpose of the 6.0 mg/cm2 lead level is to evaluate the test kit's response at a level well
above the action level of 1.0 mg/cm2. Both the lead chromate and white lead PEMs satisfy this
need and will be used in this verification test. Some modifications will be made, however, for
the use of the white lead PEMs at this level. Because there were four reference panels with quite
high lead levels, PEMs produced within the range of these four reference panels, and thus
thought to have the same lead levels, will be distributed evenly amongst all participating test kits,
to the extent possible. When analyzing the results from this lead level, consideration will be
given to conducting analyses with all data for this lead level as well as without data from PEMs
with >10 mg/cm2.
Paint containing no lead (0.0 mg/cm2) will also be applied to each substrate and tested.
Two different layers of paint will be applied over the leaded paint. One will be a primer
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designed for adhesion to linseed oil-based paint and the second coat will be a typical interior
modern latex paint tinted to one of three colors: white, red-orange, or grey-black. These colors
were chosen by EPA based on the potential of certain colors to interfere or not with lead paint
test kit operations. The top-coat paint manufacturers' recommended application thickness will
be used. Two coats at the recommended thickness will be applied. Each substrate will be tested
without paint, in the same manner as all other PEMs (i.e., per the test kit instructions), to
determine if the substrate material itself is causing any effects on the performance of the test kits.
Two unpainted PEMs of each substrate will be evaluated using each test kit.
Each spot test kit for lead paint will be operated by a technical operator. This operator
will be a Battelle staff member with laboratory experience. The technical operator will be
trained by the vendor in the operation of the vendor's test kit. The same technical operator will
operate a given test kit throughout the course of testing. Multiple technical operators may
operate different lead paint test kits. Because these test kits are anticipated to be used by
certified remodelers, renovators and painters, the test kits will also be evaluated by a non-
technical operator depending on the operational and potential safety issues surrounding each test
kit. Because this verification test will involve the evaluation of lead-based paint, any disturbance
of that paint could pose a potential health hazard. If a test kit's operation does involve disturbing
the paint on the PEM and thus pose a health risk to the operator, then it may not be feasible to
evaluate that test kit using a non-technical operator. In such an instance, any technical operator
from Battelle would have to undergo specific health and safety training to operate the test kit and
all appropriate health and safety practices would have to be followed during testing. If a non-
technical operator is used, the non-technical operator will be a certified renovator with little to no
experience with lead. The non-technical operator will be trained in the use of the lead paint test
kit by a Battelle staff person who has experience operating test kits in general, but not by the
technical operator who was trained by the vendor. This scenario will approximate the training
renovators are expected to receive under the RRP rule3.
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Table 4. PEMs Testing Scheme for Each Test Kit
Lead Type
Control Blank
White Lead
Lead Chromate
Lead Level
(mg/cm2)
0
0.4
0.6
1.0
1.4
2.0
6.0
0.4
0.6
1.0
1.4
2.0
6.0
Substrate
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Wood
Metal
Dry wall
Plaster
Painted PEMs Subtotal
PEMs Analyzed Per Test Kit by Topcoat Color
White
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
156
Red-Orange
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
156
Grey-Black
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
156
Unpainted PEMs Subtotal (2 per each substrate)
Total
Total
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
9
468
8
476
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Tests will be performed in at least duplicate on each PEM by each operator, technical and
non-technical, depending on available space and test kit operation requirements. Replicates will
be tested in succession by each operator on a given PEM. PEMs will be analyzed blindly by
each operator in that the PEMs used for analysis will be marked with a non-identifying number.
Test kit operators will not be made aware of the paint type, lead level, or substrate of the PEM
being tested. PEMs will be tested in no particular order.
Paint chip samples from each PEM will be analyzed by a National Lead Laboratory
Accreditation Program (NLLAP) accredited laboratory using ICP-AES to confirm the lead level
of each PEM used for testing. The paint chip samples for reference analyses will be collected by
Battelle according to ASTM E17298. The reference analyses will confirm the lead level of each
PEM to ensure an accurate understanding of each test kit's performance. Lead levels determined
through the reference analysis will be used for reporting and statistical analyses.
The technologies will be evaluated for the following parameters:
Bl. 1.1 False Positive and False Negative Rates
A false positive response will be defined as a positive result when regulated lead-based
paint is not present. For this test, false positive rates will be assessed on panels with target lead
levels at 0.6 mg/cm2 and lower. Per the guidelines set forth in EPA's April 22, 2008 RRP rule4,
panels with an ICP-AES confirmed lead level greater than 0.8 mg/cm2 will not be used in the
false positive analysis.
A false negative response will be defined as a negative response when regulated lead-
based paint is present. For this test, false negative rates will be assessed on panels with target
lead levels at 1.4 mg/cm2 and higher. Per the guidelines set forth in EPA's April 22, 2008 RRP
rule4, panels with an ICP-AES confirmed lead level less than 1.2 mg/cm2 will not be used in the
false negative analysis
False positive and negative rates will be grouped by paint type (lead chromate vs. white
lead). Results will also be grouped across paint types by PEM substrate and by color. Results
will also be examined by operator type (i.e., technical vs. non-technical).
9
Based on stakeholder input, the EPA lead paint action level of 1.0 mg/cm lead was
included for analysis as part of the verification test. Though evaluations of test kit performance
based on this level is not within the guidelines of the EPA RRP rule4, false positive and negative
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rates, in addition to those stated above, will also be calculated for each test kit based on 1.0
mg/cm2 lead. Thus, false positive rates will be assessed on panels with lead levels at 1.0 mg/cm2
or lower and false negative rates will be assessed on panels with lead levels at 1.0 mg/cm2 or
higher. For panels that measure 1.0 mg/cm2, positive results will be considered "correct" and
negative results will be considered false negative. If the lead concentration of the PEM is
9 9
actually greater than 1.0 mg/cm (e.g., 1.1 mg/cm ), then negative results will be considered false
9
negatives. If the lead concentration of the PEM is actually less than 1.0 mg/cm (e.g., 0.9
r\
mg/cm ), then positive results will be considered false positives.
B'1.1.2 Precision
Precision will be measured by the reproducibility of responses for replicate samples
within a group of PEMs. Groups of PEMs to be evaluated for precision will include lead
concentrations and substrate material at a specific lead concentration.
Bl. 1.3 Sensitivity
The sensitivity or lowest detectable lead level will be identified based on the detection
results across all PEM lead levels.
Bl.1.4 Modeled Probability of Test Kit Response
Logistic regression models will be used to determine the probabilities of positive or
negative responses of the test kit at the 95% confidence level, as a function of lead concentration
and other covariates, such as substrate type.
B 1.1.5 Matrix Effects
Covariate adjusted logistic regression models will be used to determine whether any of
the PEMs parameters (color, substrate, etc) affects the performance of the test kit. Type III
Statistics and comparison of Likelihoods from logistics regression models will be used to
determine the statistical significance of these factors.
Bl.1.9 Operational Factors
Operational factors such as ease of use, operator bias, and helpfulness of manuals, will be
evaluated based on Operator and Verification Test Coordinator observations. Sustainability
metrics such as volume and type of waste generated from the use of each test kit, toxicity of the
chemicals used, and energy consumption will also be evaluated. These metrics will be discussed
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by detailing how much waste is generated and what the waste is composed of, providing
information on how the waste should be properly handled, presenting a summary of the pertinent
MSDS information, when available, and noting whether the test kit used batteries, a power
supply, or no energy source is needed. Information on how many tests each kit can perform as
well as the shelf life of the test kit and chemicals used as part of the test kit will also be reported.
B1.2 Statistical Analysis
The statistical methods and calculations used for evaluating quantitative performance
parameters are described in the following sections. ICP-AES reference analyses will confirm the
lead level of each PEM to ensure an accurate understanding of each test kit's performance. Lead
levels determined through the reference analysis will be used for reporting and statistical
analyses.
B1.2.1 False Positive and False Negative Rates
A false positive response will be defined as a detect from the lead paint test kit when
9 9
evaluated on PEMs with target lead levels at and below 0.6 mg/cm (i.e., 0, 0.4, and 0.6 mg/cm
levels). Per the guidelines set forth in EPA's April 22, 2008 RRP rule4, panels with an ICP-AES
confirmed lead level greater than 0.8 mg/cm2 will not be used in the false positive analysis. A
false negative response will be defined as a non-detect from the lead paint test kit when
evaluated on PEMs with target lead levels at and above 1.4 mg/cm2 (i.e., 1.4, 2.0, 6.0 mg/cm2).
Per the guidelines set forth in EPA's April 22, 2008 RRP rule4, panels with an ICP-AES
r\
confirmed lead level less than 1.2 mg/cm will not be used in the false negative analysis
False positive and negative rates will be grouped by paint type (lead chromate vs. white
lead). Results will also be grouped across paint types by PEM substrate and by color. Results
will also be examined by operator type (i.e., technical vs. non-technical, where applicable).
Based on stakeholder input, the EPA lead paint action level of 1.0 mg/cm2 lead was
included for analysis as part of the verification test. Though evaluations of test kit performance
based on this level is not within the guidelines of the EPA RRP rule4, false positive and negative
rates, in addition to those stated above, will also be calculated for each test kit based on 1.0
9 9
mg/cm lead. Thus, false positive rates will be assessed on panels with lead levels at 1.0 mg/cm
r\
and lower and false negative rates will be assessed on panels with lead levels at 1.0 mg/cm and
higher.
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False positive and negative rates will be evaluated as the number of positive or negative
results, respectively, out of the total number of PEM samples evaluated without or with regulated
lead-based paint, per the concentration levels stated above.
„ , „ „ # of positive results ,,^
False Positive Rate = -^- (1)
total # of PEMs without regulated lead - based paint
# of negative results
False Negative Rate = (2)
total # of PEMs with regulated lead - based paint
B'1.2.2 Precision
Precision will be measured by the reproducibility of responses for replicate samples
within a group of PEMs. Groups of PEMs to be evaluated for precision will include individual
9
lead concentration levels (e.g., all PEMs at 0.4 mg/cm ) and substrate material at a specific lead
9
concentration (e.g., all metal PEMs at 1.4 mg/cm ). Responses will be considered inconsistent if
25% or more of the replicates differ from the response of the other samples in the same group of
PEMs. An overall precision for each test kit will be assessed by paint type by calculating the
overall number of consistent responses for all the sample sets of either white lead or lead
chromate-painted PEMs. The results will be reported as the percentage of consistent responses
out of all replicate sets for those paint types (see Equation 3).
. . . , . # of consistent responses of replicate sets ,.x
Precision (% consistent results) = xlOO (3)
total number of replicate sets
B 1.2.3 Sensitivity
The sensitivity or lowest detectable lead level for each test kit will be identified based on
the detection results across all PEM lead levels. The lowest PEM lead level with consistent
positive or "detect" responses will be considered the lowest detectable level. The identified
lowest detectable lead level will be reported and discussed.
Bl.2.4 Modeled Probability of Test Kit Response
Logistic regression models will be used to determine the probabilities of positive or
negative responses of the test kit at the 95% confidence level, as a function of lead concentration
and other covariates, such as substrate type. An evaluation of the bivariate relationship between
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the response variable and each individual candidate explanatory variable will be performed by
fitting single covariate logistic models to assess the predictive ability of each of the PEM
parameters. Using the results from these bivariate analyses a parsimonious multivariate model
will be developed including a set of explanatory variables which are most predictive of the
probability of the test kit response variable. The potential logistic regression model will take the
form as below:
where Yt is the outcome of the test kit, Xt is a vector of explanatory variables associated with Y;
and ft represent a vector of unknown parameters which will be estimated with the model.
Candidate independent variables associated with the response variable are operator type, lead
type, lead level, substrate type, and topcoat color. Interactions between these predictor variables
will also be assessed. Each level of the covariates can also be included using indicator
variables. SAS procedures GENMOD or LOGISTIC will be used to fit the logistic model
B 1.2. 5 Matrix Effect
The covariate-adjusted logistic regression model described in section B 1.2. 4 will be used
to assess the significance of PEM parameters and the interactions among them on the
performance of the test kits. PEM parameters are included in the model as explanatory variables
associated with the Ypi response variable.
Comparison of the observed values of the response variable to predicted values obtained
from models with and without the predictor variable in question will be the guiding principle in
logistic regression model. The likelihood function is defined as
where x(YiJU)is the conditional probability of Y;jki=l and [l-x(YiJU)] is the conditional
probability of Ypi =0 given the vector of explanatory variables (X). For purposes of assessing
the significance of a group of p predictor variables (where p can be 1 or more), we compute the
likelihood ratio test statistic, G, as follows:
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G = -2 logs [likelihood without the p variables / likelihood with the p variables] (6)
Under the null hypothesis, this test statistic will follow a chi-square distribution with p
degrees of freedom. If the test statistic is greater than the 95* percentile of the chi-square
distribution, then the group of variables, taken together, are statistically significant.
B1.2.6 Operational Factors
There are no statistical calculations applicable to operational factors. Operational factors
such as ease of use, operator bias, average cost, average time for kit operation, and helpfulness of
manuals, will be determined qualitatively based on Operator (both technical and non-technical)
and Verification Test Coordinator observations. The non-technical operator will not receive any
vendor support on the operation of the test kit throughout the test. Descriptions of observations
made throughout testing will be reported and discussed. Sustainability metrics such as volume
and type of waste generated from the use of each test kit, toxicity of the chemicals used, and
energy consumption will be discussed. This discussion will be based on how much waste is
generated and what the waste is composed of, information on how the waste should be properly
handled, a summary of the pertinent MSDS information, when available, and noting whether the
test kit used batteries, a power supply, or no energy source is needed. Information on how many
tests each kit can perform as well as the shelf life of the test kit and chemicals used as part of the
test kit will also be reported.
B1.3 Reporting
The data obtained in the verification test will be compiled separately for each vendor's
technology, and the data evaluations will be applied to each technology's data set without
reference to any other. At no time will data from different vendor's technology be intercompared
or ranked. Following completion of the data evaluations, a draft verification report and
verification statement will be prepared for each vendor's technology, stating the verification test
procedures and documenting the performance observed. Each report will briefly describe the
ETV Program and the procedures used in verification testing. The results of the verification test
will then be stated, without comparison to any other technology tested, or comment on the
acceptability of the technology's performance. Each draft verification report will be submitted
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for review by the respective technology vendor and by EPA and other peer reviewers. Comments
on the draft report will be addressed in revisions of the report. The peer review comments and
responses will be tabulated to document the peer review process. The reporting and review
process will be conducted according to the requirements of the ETV QMP1. All final verification
reports and statements will be made 508 compliant and will be posted on the ETV website
(www.epa.gov/etv).
B2 SAMPLING REQUIREMENTS
B2.1 Sample Collection, Storage and Shipment
PEM samples will be produced and stored prior to the beginning of the verification test
and in accordance with the Revised Plan For Development And Production Of Performance
Evaluation Materials For Testing Of Test Kits For Lead In Paint under the Environmental
Technology Verification Program1. The film thickness, homogeneity, and lead levels of the
paint applied to the PEMs will be verified prior to full-scale PEMs production via spray or draw
down application on quality-controlled metal panels7. This process will test the paint
formulation and application to ensure that the desired lead level can be achieved during full PEM
production. PEMs will be measured for film thickness using a Positector 6000 coating thickness
gauge. Subsequently, paint chip samples corresponding to the locations of the film thickness
measurements will be obtained following ASTM El 729, Standard Practice for Field Collection
of Dried Paint Samples for Subsequent Lead Determination.^ These samples will be shipped to
the NLLAP-accredited laboratory for analysis. This process will not verify the lead levels of
individual PEMs used for verification testing and will take place prior to the production of PEMs
for this verification test. Details on this process can be found in the PEMs development plan7.
The PEMs development plan, along with a summary of the homogeneity and lead level analyses,
can be found in Appendix A.
As part of the verification test, the lead level of paint from each PEM used in the
verification test will be verified through ICP-AES analysis by an independent NLLAP-accredited
laboratory. Paint chip samples from unused portions of each PEM will be collected by Battelle
using guidelines set forth in ASTM E1729 Standard Practice for Field Collection of Dried Paint
o
Samples for Subsequent Lead Determination. Paint chips will be collected into small glass vials
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according to a procedure to be prepared by Battelle (see Appendix B). This procedure will detail
paint chip sampling guidelines for each substrate to ensure consistent paint chip collection
throughout the verification test. These paint chips will be supplied to the subcontract laboratory
for analysis. ICP-AES reference analyses will confirm the lead level of each PEM to ensure an
accurate understanding of each test kit's performance. Lead levels determined through the
reference analysis will be used for reporting and statistical analyses. The lead concentrations
expected across a batch of PEMs will be evaluated prior to their use in the ETV test through the
use of reference PEMs during the production phase7. This process should help ensure that large
deviations in concentrations do not exist across a particular lead level.
B3 SAMPLE HANDLING AND CUSTODY REQUIREMENTS
Sample custody will be documented for the shipping and analysis of paint chip samples
to the subcontract laboratory using standard chain-of-custody (COC) forms provided by Battelle
or supplied by the laboratory, as appropriate. Samples transferred within Battelle may be
documented in bound sample login LRBs. Each COC form will summarize the analyses
requested. The COC forms will track sample release from Battelle to the NLLAP laboratory.
Each COC form will be signed by the person relinquishing the samples once that person has
verified that the COC form is accurate. The original sample COC forms will accompany the
samples; the shipper will keep a copy. Any discrepancies will be noted on the form and the
sample receiver will immediately contact the Verification Test Coordinator to report missing,
broken, or otherwise compromised samples. Copies of all COC forms will be delivered to the
Verification Test Coordinator, and maintained with the test records.
B4 LABORATORY REFERENCE METHOD
Paint chips from an unused portion of each PEM will be analyzed by ICP-AES by an
independent NLLAP-accredited laboratory. Paint chip samples will be collected by Battelle
o
using guidelines set forth in ASTM El729 and supplied to the subcontract laboratory for
analysis. Because PEMs will be assumed to be homogenous, based on pre-production testing7,
the specific place of paint chip collection will not matter, as any spot on the PEM should be
representative of the entire panel. However, to the extent practicable, based on space needed for
individual test kit operation on each PEM, varying places on each PEM will be selected for
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collection of paint ships for reference analyses. The NLLAP-accredited laboratory will use
ASTM 16459 or equivalent for paint digestion and EPA method 601 OB10 or equivalent, along
with their own laboratory SOPs for ICP-AES analysis. The subcontract laboratory will be
responsible for providing calibrated instrumentation, performing all method QA/QC, and
providing calibration records for any instrumentation used. ICP-AES reference analyses will
confirm the lead level of each PEM to ensure an accurate understanding of each test kit's
performance. Lead levels confirmed through the reference analysis shall have a percent error of
less than ±15 percent of expected values. Reference measurements outside this range will be
used in place of expected lead concentrations for reporting and statistical analyses.
B5 QUALITY CONTROL
Steps will be taken to maintain the quality of data collected during this verification test.
When confirmation analyses of the lead levels of the PEMs are performed, QC measures as
noted in the subcontract laboratory's operating procedures or the reference method and provided
in Table 2 will be followed. The QC measures for the reference method will at least include the
analysis of a method blank sample. Method blank samples will be analyzed to ensure that no
sources of contamination are present. If the analysis of a method blank sample indicates a
concentration above the minimum acceptance criteria provided in Table 2, contamination will be
suspected. Any contamination source(s) will be corrected, and proper blank readings will be
achieved, before proceeding with the analyses. A matrix spike sample as well as calibration
verification standards will also be analyzed. Average acceptable recoveries for these samples are
between 75-125%. Initial calibration standards will be run at the beginning of each set of
analyses or at least once daily. The calibration coefficient must be at least 0.995. If this criteria
is not met, the analysis will be stopped and recalibration will be performed. A continuing
calibration verification will be run once every 10 samples. Duplicate samples will be run once
every 10-20 samples.
If quality control samples as provided with each lead paint test kit (e.g., positive/negative
controls), then they will also be run per the vendor's instructions. Painted PEMs containing no
lead as well as each of the PEMs substrates containing no paint will also be run as part of the
verification test.
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B6 INSTRUMENT/EQUIPMENT TESTING, INSPECTION, AND MAINTENANCE
The instruments used for the reference analyses will be tested and inspected as per the
standard operating procedures or instrument manuals of the subcontract laboratory or per the
standard methods being used to make each measurement. Any discovered deficiencies with a
particular instrument will be resolved per the protocol of the laboratory in a timely manner.
When technical staff operate and maintain technologies undergoing testing, those activities will
follow directions provided by the technology vendor. Any maintenance required on components
of the lead paint test kits will be the responsibility of the vendor.
B7 CALIBRATION/VERIFICATION OF TEST PROCEDURES
The TCP instrument used for the reference analyses will be calibrated per the standard
reference method or the standard operating procedures of the analysis laboratory. A calibration
will be run at the beginning of each set of analyses or at least once daily. The calibration
coefficient must be at least 0.995 or higher. An independent calibration verification (ICV)
standard will be run once a day after calibration and a continuous calibration verification (CCV)
standard will be run at the beginning and end of each sample run. The ICV and CCV must be
within ±10% and ±20%, respectively, of known values. If these evaluation criteria are not met,
analysis must be stopped and recalibration performed. If the recalibration fails, the standards
must be re-made and/or the equipment must be evaluated. If any component of a lead paint test
kit requires calibration, the vendor will provide Battelle technical staff with instructions on how
to properly maintain such components.
B8 INSPECTION/ACCEPTANCE OF SUPPLIES AND CONSUMABLES
PEMs used for verification testing will be made prior to the initiation of this test by
Battelle in accordance with the Revised Plan For Development And Production Of Performance
Evaluation Materials For Testing Of Test Kits For Lead In Paint under the Environmental
Technology Verification Program7. The film thickness, homogeneity, and lead levels of the
paint applied to the PEMs will be verified prior to full-scale PEMs production7. This process
will test the paint formulation and application to ensure that the desired lead level is being
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achieved during full PEM production. PEMs will be measured for film thickness using a
Positector 6000 coating thickness gauge. Subsequently, paint chip samples corresponding to the
locations of the film thickness measurements will be obtained following ASTM E1729.8 These
samples will be shipped to the NLLAP-accredited laboratory for analysis. This process will not
verify the lead levels of individual PEMs used for verification testing and will take place prior to
the production of PEMs for this verification test. Details on this process can be found in the
PEMs development plan7.
B9 NON-DIRECT MEASUREMENTS
No non-direct measurements will be used during this verification test.
BIO DATA MANAGEMENT
Various types of data will be acquired and recorded electronically or manually by
Battelle during the verification test. Table 2 summarizes the types of data to be recorded. All data
and observations for the operation of the test kits will be documented by Battelle technical staff
on data sheets or in laboratory record books. Results from the subcontract laboratory reference
instruments will be compiled by the subcontractor's staff in electronic format and submitted to
Battelle upon obtaining the results.
Records received by or generated by any technical staff during the verification test will
be reviewed by a Battelle staff member within two weeks of generation or receipt, before the
records are used to calculate, evaluate, or report verification results. If a Battelle staff member
generated the record, this review will be performed by a Battelle technical staff member involved
in the verification test, but not the staff member who originally generated the record. The review
will be documented by the person performing the review by adding his/her initials and date to the
hard copy of the record being reviewed. In addition, any calculations performed by technical
staff will be spot-checked by Battelle QA and/or technical staff to ensure that calculations are
performed correctly. Calculations to be checked include any statistical calculations described in
this test/QA plan. The data obtained from this verification test will be compiled and reported
independently for each technology. Results for technologies from different vendors will not be
compared with each other.
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Among the QA activities conducted by Battelle QA staff will be an audit of data quality.
This audit will consist of a review by the Battelle Quality Manager (or his designee) of at least
10% of the test data. During the course of any such audit, the Battelle Quality Manager will
inform the technical staff of any findings and any need for immediate corrective action. If serious
data quality problems exist, the Battelle Quality Manager will request that Battelle's Verification
Test Coordinator issue a stop work order. Once the assessment report has been prepared, the
Verification Test Coordinator will ensure that a response is provided for each adverse finding or
potential problem, and will implement any necessary follow-up corrective action. The Battelle
Quality Manager will ensure that follow-up corrective action has been taken.
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SECTION C
ASSESSMENT AND OVERSIGHT
Cl ASSESSMENTS AND RESPONSE ACTIONS
Every effort will be made in this verification test to anticipate and resolve potential
problems before the quality of performance is compromised. One of the major objectives of this
test/QA plan is to establish mechanisms necessary to ensure this. Internal quality control
measures described in this test/QA plan, which is peer reviewed by a panel of outside experts,
implemented by the technical staff and monitored by the Verification Test Coordinator, will give
information on data quality on a day-to-day basis. The responsibility for interpreting the results
of these checks and resolving any potential problems resides with the Verification Test
Coordinator. Technical staff have the responsibility to identify problems that could affect data
quality or the ability to use the data. Any problems that are identified will be reported to the
Verification Test Coordinator, who will work with the Battelle Quality Manager to resolve any
issues. Action will be taken to control the problem, identify a solution to the problem, and
minimize losses and correct data, where possible. Independent of any EPA QA activities,
Battelle will be responsible for ensuring that the following audits are conducted as part of this
verification test.
Cl.l Performance Evaluation Audits
A Performance Evaluation (PE) audit will be conducted to assess the quality of the
reference method measurements made in this verification test. The reference method PE audit
will be performed by supplying an independent, NIST-traceable lead paint standard, to the
subcontract laboratory. The PE audit samples will be analyzed in the same manner as all other
samples and the analytical results for the PE audit samples will be compared to the nominal
concentration. The target criterion for this PE audit is agreement of the analytical result within
20% of the nominal concentration. If the PE audit result does not meet the target criterion, the PE
audit will be repeated. If the outlying results persist, the source of error will be investigated and
corrective action taken as necessary until successful PE audit results are obtained. This audit will
be performed once at the start of the test, and will be the responsibility of the Verification Test
Coordinator or designee.
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C1.2 Technical Systems Audits
The Battelle Quality Manager or designee will perform a TSA of the actual evaluation of
the test kits at least once during this verification test. The purpose of this audit is to ensure that
the verification test is being performed in accordance with the AMS Center and ETV Program
QMPs1'6, this test/QA plan, any published reference methods, and any Standard Operating
Procedures (SOPs) used. In the TSA, the Battelle Quality Manager, or a designee, may review
the reference methods used, compare actual test procedures to those specified or referenced in
this plan, and review data acquisition and handling procedures In the TSA, the Battelle Quality
Manager will observe testing in progress, observe the reference method sample preparation and
analysis (when available), inspect documentation, and review technology-specific record books.
He or she will also check standard certifications and technology data acquisition procedures, and
may confer with technical staff. A TSA report will be prepared, including a statement of findings
and the actions taken to address any adverse findings. The EPA Quality Manager will receive a
copy of Battelle's TSA report. An initial, draft TSA report, not including verification of
corrective actions, will be submitted to EPA within 2 weeks of completion of the audit. At
EPA's discretion, EPA QA staff may also conduct an independent on-site TSA during the
verification test. The TSA findings will be communicated to technical staff at the time of the
audit and documented in a TSA report.
C1.3 Data Quality Audits
The Battelle Quality Manager or his designee will audit at least 10% of the verification
data acquired in the verification test, including any data packages received from the subcontract
reference laboratory. Data packages will conform to ADQ guidelines provided by EPA. The
Battelle Quality Manager will trace the data from initial acquisition, through reduction and
statistical comparisons, to final reporting. All calculations performed on the data undergoing the
audit will be checked. An initial, draft TSA report, not including verification of corrective
actions, will be submitted to EPA within 2 weeks of completion of the audit. Data packages
received from the subcontract laboratory will be briefly reviewed by Battelle for completeness
and then provided to EPA within three days of receipt of the data package. The packages will
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not have gone through any data quality audits at this time, as these audits will be ongoing at the
time of submission of the data to EPA.
C1.4 QA/QC Reporting
Each assessment and audit will be documented in accordance with the AMS Center and
1,6
ETV Program QMP. The results of the technical systems and data quality audit will be
submitted to EPA. Initial, draft reports, not including verification of corrective actions, will be
submitted to EPA within 2 weeks of completion of the audit. Assessment reports will include
the following:
• Identification of any adverse findings or potential problems
• Response to adverse findings or potential problems
• Recommendations for resolving problems
• Confirmation that solutions have been implemented and are effective
• Citation of any noteworthy practices that may be of use to others.
C2 REPORTS TO MANAGEMENT
The Battelle Quality Manager, during the course of any assessment or audit, will identify
to the technical staff performing experimental activities any immediate corrective action that
should be taken. If serious quality problems exist, the Battelle Quality Manager will notify the
Battelle Management to authorize a stop work order. Once the assessment report has been
prepared, the Verification Test Coordinator will ensure that a response is provided for each
adverse finding or potential problem and will implement any necessary follow-up corrective
action. The Battelle Quality Manager will ensure that follow-up corrective action has been taken.
The test/QA plan and final report are reviewed by EPA QA Manager and the EPA ESTE Project
Officer. Upon final review and approval, both documents will then be posted on the ETV
website (www.epa.gov/etv).
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SECTION D
DATA VALIDATION AND USABILITY
Dl DATA REVIEW, VALIDATION, AND VERIFICATION REQUIREMENTS
The key data review requirements for the verification test are stated in Section BIO of
this test/QA plan. In general, the data review requirements specify that the data generated during
this test will be reviewed by a Battelle technical staff member within two weeks of data
generation. The reviewer will be familiar with the technical aspects of the verification test, but
will not be the person who generated the data. This process will serve both as the data review
and the data verification, and will ensure that data have been recorded, transmitted, and
processed properly. Furthermore, this process will ensure that the lead paint test kit data and the
reference method data are collected under appropriate testing conditions and that the reference
method data meet the reference method specifications.
The data validation requirements for this test involve a data quality assessment relative to
the DQIs and audit acceptance criteria specified for this test. The DQIs listed in Section A 4.2
and B5 will be used to validate the data quality. The QA audits described within Section C of
this document, including the performance evaluation audit and data quality audit, are designed to
validate the data quality.
D2 VALIDATION AND VERIFICATION METHODS
Data verification is conducted as part of the data review, as described in Section BIO for
this test/QA plan. A visual inspection of handwritten data will be conducted to ensure that all
entries were properly recorded or transcribed, and that any erroneous entries were properly noted
(i.e., single line through the entry with an error code and the initials of the recorder and date of
entry). Data manually incorporated into spreadsheets for use in calculations will be checked
against handwritten data to ensure that transcription errors have not occurred. All calculations
used to transform the data will be reviewed to ensure the accuracy and the appropriateness of the
calculations. Calculations performed manually will be reviewed and repeated using a handheld
calculator or commercial software (e.g., Excel). Calculations performed using standard
commercial office software (e.g., Excel) will be reviewed by inspecting the equations used in
calculations and verifying selected calculations by handheld calculator. Calculations performed
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using specialized commercial software (i.e., for analytical instrumentation) will be reviewed by
inspection and, when feasible, verified by handheld calculator, or standard commercial software.
To ensure that the data generated from this test meet the goals of the test, a number of
data validation procedures will be performed. Section C of this test/QA plan provides a
description of the validation safeguards employed for this verification test. Data validation and
verification efforts include the completion of QC activities and the performance of TSA audits as
described in Section C. The data from this test will be evaluated relative to the measurement
DQIs described in Section A7.1 and B5 of this test/QA plan. Data failing to meet these criteria
will be flagged in the data set and not used for evaluation of the technologies, unless these
deviations are accompanied by descriptions of their potential impacts on the data quality.
A data quality audit will be conducted by the Battelle Quality Manager to ensure that data
review, verification, and validation procedures were completed, and to assure the overall data
quality.
D3 RECONCILIATION WITH USER REQUIREMENTS
This purpose of this verification test is to evaluate the performance of qualitative spot test
kits for lead based paint. To meet the requirements of the user community, the data obtained in
this verification test should include thorough documentation of the performance of each lead
paint test kit during the verification test. The data review, verification, and validation procedures
described in previous sections will assure that data meet these requirements, are accurately
presented in the verification reports generated from this test, and that data not meeting these
requirements are appropriately flagged and discussed in the verification reports. Additionally, all
data generated using the reference method, which are used to evaluate technology results during
the verification test, should meet the QA requirements of any applicable standard operating
procedures or instrumentation instruction manuals.
The data from this verification test will be compiled into an ETV verification report. The
report will be submitted to EPA in Word and Adobe pdf format and subsequently posted on the
ETV website. This test/QA plan and the resulting ETV verification report(s) will be subjected to
review by the lead paint test kit vendors, Battelle staff, EPA, and expert peer reviewers. The
reviews of this test/QA plan will assure that this verification test and the resulting reports meet
the needs of potential users of the qualitative spot test kits for lead based paint.
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SECTION E
REFERENCES
El REFERENCES
1. "Environmental Technology Verification Program Quality Management Plan", December
2002, EPA/600/R-03/021.
2. President's Task Force on Environmental Health Risks and Safety Risks to Children.
Eliminating Childhood Lead Poisoning: A Federal Strategy Targeting Lead Paint
Hazards. 2000. Washington, DC.
3. NISTIR 6398, "Spot Test Kit for Detecting Lead in Household Paint: A Laboratory
Evaluation," NIST, May 2000.
4. "Lead; Renovation, Repair, and Painting Program Final Rule", Federal Register, 73:78
(April 22, 2008), p.21692.
5. ASTM E1828, "Standard Practice for Evaluating the Performance Characteristics of
Qualitative Chemical Spot Test Kits for Lead in Paint," ASTM International.
6. Quality Management Plan (QMP) for the ETV Advanced Monitoring Systems Center,
U.S. EPA Environmental Technology Verification Program, prepared by Battelle,
Columbus, OH, Version 7.0, 2008.
7. Revised Plan For Development And Production Of Performance Evaluation Materials
For Testing Of Test Kits For Lead In Paint Under The Environmental Technology
Verification Program, Battelle, Columbus, Ohio, September 2008.
8. ASTM E1729, "Standard Practice for Field Collection of Dried Paint Samples for
Subsequent Lead Determination," ASTM International.
9. ASTM E1645, "Standard Practice for Preparation of Dried Paint Samples by Hotplate or
Microwave Digestion for Subsequent Lead Analysis," ASTM International.
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10. U.S. EPA, EPA Method 6010B, "Inductively Coupled Plasma-Atomic Emission
Spectrometry, Revision 2 (December 1996)." In Test Methods for Evaluating Solid
Wastes: Physical/Chemical Methods, EPA SW-846, Third Ed., U.S. Environmental
Protection Agency, Office of Solid Waste and Emergency Response, Washington, D.C.
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Appendix A
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REVISED PLAN FOR
DEVELOPMENT AND PRODUCTION OF
PERFORMANCE EVALUATION MATERIALS FOR
TESTING OF TEST KITS FOR LEAD IN PAINT UNDER THE
ENVIRONMENTAL TECHNOLOGY VERIFICATION PROGRAM
July 2009
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1.
Overview of Problem
The accurate and efficient identification of lead-based paint in housing is important to the
Federal government and to private individuals living in residences containing such paints,
especially when renovation, repair or painting work is planned. Renovation, repair and painting
(RRP) may disturb painted surfaces and produce a lead exposure hazard. According to a recent
report by the President's Task Force on Environmental Health Risks and Safety Risks to
Children, approximately 24 million U.S. dwellings were at risk for lead-based paint hazards in
1999. The term lead-based paint means paint or other surface coatings that contain lead at
contents that "equal or exceed a level of 1.0 milligram per centimeter squared or 0.5 percent by
weight."
The Preamble for the proposed EPA rule for RRP activities mentions the development of an
improved test kit for paint that has a false negative rate of no more than 5 percent and a false
positive rate of no more than 10 percent vis-a-vis the federal standards for lead-based paint. The
Preamble also refers to an EPA evaluation and recognition program for test kits, initially for kits
that are candidates to meet the goal of a 5 percent false negative rate, and then for kits that are
candidates to meet the joint goals of a 5 percent false negative rate and a 10 percent false positive
rate. As stated in the Preamble, test kit performance would have to be "validated by a laboratory
independent of the kit manufacturer, using ASTM International's El 828, Standard Practice for
Evaluating the Performance Characteristics of Qualitative Chemical Test Kits for Lead in Paint
(Ref. 50) or an equivalent validation method. The instruction for use of any particular kit would
have to conform to the results of the validation, and the certified renovator must follow the
manufacturer's instructions when using the kit."
This effort includes the development and production of Performance Evaluation Materials
(PEMs) for use in the evaluation of the performance characteristics of qualitative test kits for
lead in paint. These PEMs will be used by independent laboratories for the verification of
existing and new test kits under the Environmental Technology Verification (ETV) program.
This effort includes the development and production of as many as 6,600 PEMs measuring
approximately 3 inches by 3 inches. Note that estimates of the number of test panels needed
assume that multiple tests can be conducted on each panel.
2. Study Objectives
The EPA requires a sufficient number of PEMs to evaluate up to 14 different test kits. Although
a formal power study was not conducted, it is assumed that this number of panels should be
sufficient to thoroughly test the kits, given that multiple tests can be conducted on each panel.
How many tests can be conducted on each panel will depend on the specific requirements of
each test kit.
In comparison to the NISTIR 6398 study "Spot Test Kits for Detecting Lead in Household Paint:
A Laboratory Evaluation", this effort will include many of the same variables. Table 1
highlights the differences and similarities to both studies. Neither the NISTIR 6398 study nor
the current PEM production effort described here claims to produce Certified Reference
Materials (CRM's) as defined by ISO Guides 31, 34 and 35. Meeting that certification requires
storage and transportation stability studies which can take up to 36 months. These PEMs are
expected to be utilized within 18 months of production. The PEMs produced for this study will
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each be labeled and individually wrapped and sealed to minimize surface abrasions during
storage and transport.
Table 1: NISTIR 6398 vs. PEM Production
Category
Certified Reference
Materials per ISO
Guides 31, 34 & 35
Lead Types
Lead Levels
(mg/cm2)
Substrates
Application methods
Leaded Paint Type
Fineness of Lead
Dispersion Test
Topcoats
Verification Study
Homogeneity
Analysis
NISTIR 6398 (2000)
no
Lead Carbonate & Lead
Chromate
1 0 levels (0 up to 3. 5)
depending on lead type
and Coefficient of
Variation results after
production
Metal - Mylar and release
paper then glue applied to
wood and plaster
Drawdown and roller
Linseed Oil/ Lead paste
added to alkyd paint
None
2 = Alkyd and latex
Originally 37 different
paints were produced and
applied, once analyzed,
results from only 19 total
paints were actually
included in the test
After panel production
was completed a
Coefficient of Variation
was determined using ICP
analysis and a variation of
less than 20% was
accepted
PEM Production
(2008)
no
Lead Carbonate & Lead
Chromate
Seven levels (0, 0.3, 0.6,
1.0, 1.4,2.0,6.0)
Apply directly to wood,
metal, drywall and
plaster
Spray for zero lead
panels and topcoats;
Drawdown for all others
Linseed Oil Based
ASTMD1210
2 = Primer and latex
Verification of lead level
applied with a given film
thickness on a small
number of panels prior
to full production
Independent
homogeneity study
planned prior to and
throughout full PEM
production using ICP
analysis
Comments
See note below
Application directly to the
substrates closely simulates
real-world scenario
Drawdown allows for
direct contact between
leaded paint and substrate
and better consistency of
film thickness
Historically accurate
linseed oil paint
formulation
Ensure lead pigment
agglomerates are
adequately pulverized and
sufficiently dispersed
through paint
3. Study Design Options
The EPA specified four main design factors of interest - paint speciation, substrate, paint lead
level, and overcoat color. These are discussed below along with topcoat color, number of
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topcoats, and panel size. Table 2 presents a simple design that would yield 468 panels per test
kit for the ETV evaluation. Across the nine kits originally planned for this adds up to 4,212
panels and across 14 test kits this adds up to 6,552 panels. This number of PEMs should allow
for sufficient replicates of each design factor of interest for the ETV tests.
3.1 Paint types
A typical interior paint formulation containing either white lead (lead carbonate) or lead
chromate will be prepared. The binder composition will be linseed oil based. The preparation of
linseed oil-based paint PEMs is substantially longer due to the increased drying time required for
this type of chemistry.
3.2 Substrates
We will use wood (both poplar and pine), metal (zinc phosphated cold-rolled steel), drywall, and
plaster (limestone base) applied over drywall. The two types of wood are proposed in order to
better represent potential substrates across the range of pre-1978 housing. These represent
typical substrates to which leaded paint was originally applied.
3.3 Lead Levels
This plan proposes producing panels at seven lead levels: 0.0 mg/cm2, 0.3 mg/cm2, 0.6 mg/cm2,
1.0 mg/cm2, 1.4 mg/cm2, 2.0 mg/cm2, and 6.0 mg/cm2. These levels represent two levels
containing lead below the current lead based paint standard of 1.0 mg/cm , one level at the
standard, two levels slightly above the standard, and additional higher level (6.0 mg/cm2) to
investigate differences in performance at significantly higher lead levels as well as represent
potential lead levels on exterior surfaces, which are higher than those found on interior walls.
The level of the current standard, 1.0 mg/cm , is included to allow for the evaluation results to
provide a smoother performance evaluation curve. In addition, blank samples with no lead paint
applied will also be produced for testing and quality control purposes.
3.4 Paint Colors
Three colors of topcoats will be applied randomly across the panels. The following paint colors
will be used: white, reddish-orange, and grayish-black. These colors were chosen based on
potential for certain colors to cause interferences with the performance of some kits.
3.5 Layers of paint on top of lead paint (Topcoats)
Two different layers of paint will be applied over the leaded paint. One will be a primer
designed for adhesion to linseed oil-based paint and the second coat will be a typical interior
modern latex paint tinted to one of three colors. The thickness of each topcoat is not a design
variable. The manufacturers' recommended application thickness will be used. Two coats at the
recommended thickness will be applied.
3.6 Panel Size
3 inch by 3 inch PEMs will be produced. The assumption is that multiple tests (up to four
replicates) can be conducted per panel.
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Table 2: PEMs Produced for ETV Test
Lead Type
Control Blank
White Lead
Lead Chromate
Lead Level
0
0.3
0.6
1.0
1.4
2.0
6.0
0.3,0.6, 1.0,
1.4,2.0,6.0
Substrate
Wood-Poplar
Wood-Pine
Metal
Drywall
Plaster
Wood-Poplar
Wood-Pine
Metal
Drywall
Plaster
Wood-Poplar
Wood-Pine
Metal
Drywall
Plaster
Wood-Poplar
Wood-Pine
Metal
Drywall
Plaster
Wood-Poplar
Wood-Pine
Metal
Drywall
Plaster
Wood-Poplar
Wood-Pine
Metal
Drywall
Plaster
Wood-Poplar
Wood-Pine
Metal
Drywall
Plaster
Wood-Poplar
Wood-Pine
Metal
Drywall
Plaster
Subtotal - Per Test Kit
# Samples Produced Per Test Kit by Topcoat Color
White
2
1
3
3
3
2
1
3
3
3
1
2
3
3
3
2
1
3
3
3
1
2
3
3
3
2
1
3
3
3
1
2
3
3
3
Red-Orange
1
2
3
3
3
1
2
3
3
3
2
1
3
3
3
1
2
3
3
3
2
1
3
3
3
1
2
3
3
3
2
1
3
3
3
Grey-Black
2
1
3
3
3
2
1
3
3
3
1
2
3
3
3
2
1
3
3
3
1
2
3
3
3
2
1
3
3
3
1
2
3
3
3
2 panels per cell for Wood substrates, 4
panels per cell for other substrates (same
design as White Lead panels)
156
156
156
Total
5
4
9
9
9
5
4
9
9
9
4
5
9
9
9
5
4
9
9
9
4
5
9
9
9
5
4
9
9
9
4
5
9
9
9
27
27
54
54
54
468
9 Test Kits
45
36
81
81
81
45
36
81
81
81
36
45
81
81
81
45
36
81
81
81
36
45
81
81
81
45
36
81
81
81
36
45
81
81
81
243
243
486
486
486
4,212
14 Test Kits
70
56
126
126
126
70
56
126
126
126
56
70
126
126
126
70
56
126
126
126
56
70
126
126
126
70
56
126
126
126
56
70
126
126
126
378
378
756
756
756
6,552
4.
Production Plan
4.1 Materials
Nine different paint formulations will be produced as dictated by the two lead pigments (lead
carbonate and lead chromate) and the six different lead levels in addition to the zero lead level
control. The formulations will be designed to consistently achieve the lead levels required when
applied at typical wet film builds. The paint samples will be produced using standard painting
production procedures in the Battelle laboratories including pre-mixing, media grinding of
pigment and binder resin, and paint letdown with resin and solvents. This procedure has been
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used for paint production both in the laboratory and in commercial paint manufacturing for over
50 years. Battelle staff members completing this task have many years of direct industry
experience in commercial and laboratory paint production. The paint formulations are shown
below on Tables 3 and 4. Since the molecular compositions of the two lead pigments are
different, the formulations have accounted for this by adjusting the load levels. Additional
formulation changes will be investigated and implemented as necessary during production of the
paints for the ETV evaluation.
The lead pigment fineness of dispersion will be monitored throughout the grinding process and
once a Hegman grind of 5-6 has been achieved (ASTM D1210), the paint will be let-down with
additional turpentine and Japan drier.
Table 3: Lead Carbonate Paint Formulations
0% Zero Lead Paint Formulation
Materials
ZnO
PbCO3
TiO2
Linseed Oil
Boiled Linseed Oil
Turpentine
Japan Drier
Supplier
The Carry Co.
American Elements
DuPont
Recochem Inc.
Recochem Inc.
Recochem Inc.
Barr
% by wt.
59.67
0.00
24.86
5.97
0.60
8.70
0.20
100.00
Gram wt
1491.75
0.00
621.56
149.18
14.92
217.55
5.04
2500.00
0.3% Lead Carbonate Paint Formulation
Materials
ZnO
PbCO3
TiO2
Linseed Oil
Boiled Linseed Oil
Turpentine
Japan Drier
silica (TS 100)
Supplier
The Carry Co.
American Elements
DuPont
Recochem Inc.
Recochem Inc.
Recochem Inc.
Barr
Degussa
% by wt.
59.08
5.91
19.69
5.91
0.59
8.62
0.20
1.00
101.00
Gram wt
1477.08
147.71
492.36
147.71
14.77
215.41
4.97
25.00
2525.00
1.0% Lead Carbonate Paint Formulation
Materials
ZnO
PbCO3
TiO2
Linseed Oil
Boiled Linseed Oil
Turpentine
Japan Drier
silica (TS 100)
Supplier
The Carry Co.
American Elements
DuPont
Recochem Inc.
Recochem Inc.
Recochem Inc.
Barr
Degussa
% by wt.
55.53
11.57
18.51
5.55
0.56
8.10
0.19
1.50
101.50
Gram wt
1388.14
289.20
462.71
138.81
13.88
202.44
4.82
37.50
2537.50
This formulation will be used to produce 0.6% and 1.4% lead levels at different coating thickness.
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2.0% Lead Carbonate Paint Formulation
Materials
ZnO
PbCO3
TiO2
Linseed Oil
Boiled Linseed Oil
Turpentine
Japan Drier
silica (TS 100)
Supplier
The Carry Co.
American Elements
DuPont
Recochem Inc.
Recochem Inc.
Recochem Inc.
Barr
Degussa
% by wt.
48.16
22.73
15.41
5.28
0.53
7.70
0.19
1.50
101.50
Gram wt
1204.04
568.31
385.29
132.00
13.20
192.50
4.67
37.50
2537.50
6.0% Lead Carbonate Paint Formulation
Materials
ZnO
PbCO3
TiO2
Linseed Oil
Boiled Linseed Oil
Turpentine
Japan Drier
silica (TS 100)
Supplier
The Carry Co.
American Elements
DuPont
Recochem Inc.
Recochem Inc.
Recochem Inc.
Barr
Degussa
% by wt.
16.73
64.49
5.58
5.09
0.51
7.43
0.18
2.00
102.00
Gram wt
418.16
1612.23
139.39
127.34
12.73
185.70
4.45
50.00
2550.00
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Table 4: Lead Chromate Paint Formulations
0.3% Lead Chromate Paint Formulation
Materials
ZnO
PbCrO4
TiO2
Linseed Oil
Boiled Linseed Oil
Turpentine
Japan Drier
silica (TS 100)
Supplier
The Carry Co.
American Elements
DuPont
Recochem Inc.
Recochem Inc.
Recochem Inc.
Barr
Degussa
% by wt.
60.03
4.40
20.01
6.00
0.60
8.75
0.20
0.70
100.70
Gram wt
1500.74
110.05
500.25
150.07
15.01
218.86
5.01
17.50
2517.50
1.0% Lead Chromate Paint Formulation
Materials
ZnO
PbCrO4
TiO2
Linseed Oil
Boiled Linseed Oil
Turpentine
Japan Drier
silica (TS 100)
Supplier
The Carry Co.
American Elements
DuPont
Recochem Inc.
Recochem Inc.
Recochem Inc.
Barr
Degussa
% by wt.
55.53
11.57
18.51
5.55
0.56
8.10
0.19
1.00
101.00
Gram wt
1388.14
289.20
462.71
138.81
13.88
202.44
4.82
25.00
2525.00
This formulation will be used to produce 0.6% and 1.4% lead levels at different coating thickness.
2.0% Lead Chromate Paint Formulation
Materials
ZnO
PbCrO4
TiO2
Linseed Oil
Boiled Linseed Oil
Turpentine
Japan Drier
silica (TS 100)
Supplier
The Carry Co.
American Elements
DuPont
Recochem Inc.
Recochem Inc.
Recochem Inc.
Barr
Degussa
% by wt.
42.32
27.83
14.81
5.80
0.58
8.46
0.19
1.00
101.00
Gram wt
1058.12
695.72
370.34
145.00
14.50
211.46
4.85
25.00
2525.00
6.0% Lead Chromate Paint Formulation
Materials
ZnO
PbCrO4
TiO2
Linseed Oil
Boiled Linseed Oil
Turpentine
Japan Drier
silica (TS 100)
Supplier
The Carry Co.
American Elements
DuPont
Recochem Inc.
Recochem Inc.
Recochem Inc.
Barr
Degussa
% by wt.
5.99
77.84
2.00
5.47
0.55
7.98
0.18
1.00
101.00
Gram wt
149.69
1946.00
49.90
136.75
13.68
199.43
4.54
25.00
2525.00
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The applied lead levels will be verified prior to full-scale PEM production via drawdown
application on quality-controlled metal panels. Dried paint chip samples will be obtained and
evaluated by an independent NLLAP-accredited laboratory using ICP-AES or equivalent
analysis.
Quadrant #1
Film
Thickness
Test
Area
ICP
Lead Level
Test
Area
Quadrant #3
Film
Thickness
Test
Area
ICP
Lead Level
Test
Area
Quadrant #2
Film
Thickness
Test
Area
ICP
Lead Level
Test
Area
Quadrant #4
Film
Thickness
Test
Area
ICP
Lead Level
Test
Area
This lead level verification study
will test the formulation and
application to ensure that the
desired lead level can be achieved
during full PEM production. The
test map in Figure 1 describes how
each panel will be divided and
where each test will be performed.
Figure 2. PEM Lead Level Verification Step Test Map
One panel of each film thickness will be prepared using the previously manufactured paints.
After drying, the panel will be measured once in each quadrant for film thickness using a
Positector 6000 coating thickness gauge. Subsequently, paint chip samples corresponding to the
locations of the film thickness measurements will be obtained following ASTM El 729,
"Standard Practice for Field Collection of Dried Paint Samples for Subsequent Lead
Determination." These samples will be shipped to the NLLAP-accredited laboratory for
analysis. The laboratory will prepare the paint chip samples for analysis following ASTM 1656
and analyze the samples according to the ASTM 1613 method, "Standard Test Method for
Determination of Lead by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-
AES), Flame Atomic Absorption Spectrometry (FAAS), or Graphite Furnace Atomic Absorption
Spectrometry (GFAAS) Techniques." Results will be provided electronically along with
relevant QA/QC data on calibration samples, analytical duplicates, and analytical spikes.
Since the thickness of the paint film will determine the final lead level per unit area, the purpose
of this verification step is to identify the approximate film thickness that will result in the
targeted lead level for each paint. The ICP lead level measurements will be used to determine
the film thickness that led to the desired lead level. If average lead levels of the nearest
measurements differ from the target by more than 10 percent for target lead levels of 1.0 mg/cm2
and higher and 15 percent for target lead levels <1.0 mg/cm , corresponding adjustments will be
made to the targeted film thickness measurements prior to the homogeneity testing to follow.
Once the desired film thicknesses are determined from the verification step, panels will be coated
for a Homogeneity Study consisting of producing three additional panels at each of the six lead
levels for both types of lead pigments, obtaining four paint chip samples from each panel (one
from each quadrant), and conducting ICP-AES analysis on those paint samples to determine
precise lead measurements. The results from this process will confirm the ability to apply
consistent and accurate lead levels across each panel. Prior to paint chip sampling, film
thickness measurements also will be obtained to verify the desired film thickness for each leaded
paint. Table 5 provides an example of the data that will be collected for the Homogeneity study.
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Table 5: Lead Level Verification/Homogeneity Study for ETV Panels
Lead Type
none
White Lead
Lead
Chromate
Lead
Level
0
0.3
0.6
1.0
1.4
2.0
6.0
0.3, 0.6,
1.0, 1.4,
2.0, 6.0
Replicate
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Film Thickness Measurements - 1 per
Quadrant
Q-1
Q-2
Q-3
Q-4
ICP Testing - 1 per Quadrant
Q-1
Q-2
Q-3
Q-4
Same testing scheme as the White Lead paints
The ICP lead level measurements obtained will be analyzed to establish accuracy of the lead
levels in reference to target lead levels as well as the variability across and within panels.
Variability will be measured using the Coefficient of Variation (i.e., the standard deviation
divided by the mean). A Coefficient of Variation (CoV) less than 15 percent will be deemed
acceptable.
4.2 Facilities
Battelle laboratories include a walk-in spray booth capable of this type of production as well as
air handling equipment and monitors to ensure staff safety.
4.3 Painting Process
Some substrates, such as wood and drywall will be cut down into 3" by 3" panel dimensions.
The plaster panels will be prepared by applying plaster to pre-cut drywall panels via hand trowel
application. All drywall and drywall/plaster panels will require edge treatment to minimize
dusting of the interior gypsum. This treatment will be performed by spray applying a latex
primer to the edge surfaces only to encapsulate the inner core. All substrate preparations will
take place prior to the application of any leaded paints.
The linseed oil-based paints will be applied via drawdown bar directly to the surface of the
substrates. The drawdown method, although somewhat less efficient for applying coatings to a
large number of panels, will allow more precise film builds to be achieved as the application
device will be set to the previously determined target film build level. The drawdown paint
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application method will be utilized for both the white lead and lead chromate paints at the three
specified lead levels. The substrates will be lined up in sets of either two or four, depending on
the substrate type (2 drywall, 2 plaster. 4 metal or 4 wood panels next to each other). The paint
will be applied across the two or four PEMs in the set at the same time. The order of application
for each set will be assigned randomly using a random number generator in MS Excel. For
example, the order of application could be drywall, metal, wood, wood, plaster, metal, etc. The
PEMs will be placed on a horizontal board to dry overnight. Using the same randomization
process, a metal reference panel will be coated in the same fashion (same drawdown bar, same
paint formulation). Reference panels will be inserted as one of the four metal panels in a set,
with the location within the set randomly determined. Within Table 6, which provides an
example drawdown scenario for 56 panels targeted for the same lead paint application and same
topcoat color, three reference panels are inserted into the application process to verify the lead
levels applied to surrounding panels. The first and second reference panels are randomly placed
among the first eight and second eight sets, respectively, while the third reference panel is
randomly placed among the last seven sets of PEMs. The position of the reference panel within
the set of metal panels is also randomly determined.
Table 6. Illustration of Reference Panel Location within Set of 56 Production Panels
Drawdown Positions
#1
drywall
wood
drywall
plaster
plaster
drywall
metal
plaster
plaster
metal
wood
metal
drywall
drywall
wood
plaster
metal
plaster
REF
plaster
drywall
wood
drywall
#2
drywall
wood
drywall
plaster
plaster
drywall
metal
plaster
plaster
REF
wood
metal
drywall
drywall
wood
plaster
metal
plaster
metal
plaster
drywall
wood
drywall
#3
wood
REF
metal
wood
metal
wood
metal
#4
wood
metal
metal
wood
wood
metal
Order
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
The reference PEMs will be tested for film thickness during application and for lead level
verification by TCP analysis after the paint has dried. This test procedure will check that the
application process is resulting in appropriate lead levels. Metal panels will serve as the
reference panels since the metal panels yield the most accurate measurements of film thickness
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and lead levels. Previous work found that the metal panels provided the best film thickness
measurements and also provided a better surface for extracting a complete paint chip sample for
TCP analysis. Despite the use of metal reference panels, the lead levels and paint thickness on
the reference panels will be representative of the coatings applied to all wood, drywall, plaster,
and metal substrate panels that will be randomly scattered throughout each area.
Once reference panel results have undergone review and are determined to have met all target
specifications, the PEMs will then be mounted onto 4 foot by 8 foot drying racks for the
application of topcoat layers and conditioned in constant temperature and humidity rooms to
ensure consistent curing for all samples. All substrates will be attached to the drying racks for
painting using double stick tape. Following application of the topcoat layers, the PEMs will be
removed for packaging and shipping. Packaging will involve attaching a label to each panel,
covering the panel with a chem-wipe for protection, inserting the panel in a plastic, sealable bag,
and attaching a matching label to the exterior of the bag. Separate boxes will be prepared
containing full sets of PEMs.
5. Quality Assurance/Quality Control
Lead levels will be verified prior to full panel production by an independent NLLAP-accredited
laboratory. This detailed testing of initial batches of samples during the PEMs verification step
will establish that specified lead levels can be achieved. As part of the verification step, TCP
analysis will also be conducted in multiple locations on initial batches of panels to confirm lead
levels and homogeneity across panels. During production application of the leaded paints, a
subset of reference panels for each set of PEMs (unique lead level, lead pigment combinations)
will be tested to monitor the paint application process and ensure that targeted lead levels are
achieved with acceptable variability. As noted above, the average lead level across the reference
panels should be within 10% of the targeted value for panels at 1.0 mg/cm2 and higher and
within 15% for panels below 1.0 mg/cm . The tolerance for an acceptable level of variability in
film thickness and lead level is <15% Coefficient of Variation (CoV). One reference panel will
be inserted into the production process for every 18 to 20 production panels.
The laboratory will be required to provide QA/QC data from each batch of paint samples
analyzed on calibration samples, analytical duplicates, and analytical spikes. Percent recovery
for analytical spike samples must be within 20 percent of the actual value. The relative percent
difference for analytical duplicates (i.e., the absolute value of the difference between the two
samples divided by their average) must be less than 20 percent. If any QC samples are found to
be outside of these tolerance limits, the laboratory will be asked to reanalyze the affected batch
of samples.
6. Environmental Safety and Health Issues
Battelle has a safety and health plan related to producing lead-based paint and PEMs coated with
these paints. The plan was approved by appropriate environmental safety and health personnel.
Environmental monitoring during paint mixing and spraying activities determined that lead
exposure levels were below OSHA standards. During development of the PEMs for the ETV
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evaluation, Battelle staff will continue to comply with the safety and health plan. Some of the
components of the safety plan include:
• All staff (and any visitors) will need hazard communication training on lead.
• Baseline and post-work blood-lead levels will be obtained on those that will be
conducting the paint mixing and spray painting.
• Respirators will be used during leaded paint production and the spray application
operation by staff that have undergone the required physical, training and fit test
• The interior of the spray booth will be covered with plastic or other material that can be
easily removed and disposed as hazardous waste.
• The area in front of the booth will be set up as a change out area where the coveralls, etc,
can be removed without spreading lead outside of the area.
Warning signs at the paint booth door and restricting access will be posted.
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Summary of Homogeneity and Lead Levels Analyses for
PEMs Development
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Table A-l. Results from Final Homogeneity Testing for each set of ETV PEMs
Lead
Type
No Lead
White
Lead
Lead
Chromate
Target Lead
Level
0.0
0.3
0.6
1.0
1.4
2.0
6.0
0.3
0.6
1.0
1.4
2.0
6.0
Mean Levels
ICP (mg/cm2)
0.00
0.30
0.65
1.00
1.56
1.85
5.97
0.30
0.62
1.07
1.42
1.92
6.88
FT (mils)
0.73
0.79
0.95
1.18
1.72
1.48
1.94
1.16
0.98
2.7
1.89
1.38
1.81
CoV*
ICP
22.9
13.3
7.1
7.0
7.2
5.6
14.2
9.6
4.1
11.0
4.1
10.1
5.2
FT
12.3
6.1
5.7
4.3
3.5
7.0
8.3
4.0
9.1
6.0
6.8
2.4
3.3
* Coefficient of Variation (Standard Deviation/Mean x 100)
Table A-2. Reference Panel Results from Final Production for each set of ETV PEMs
Lead
Type
No Lead
White
Lead
Lead
Chromate
(Yellow
Lead)
Target Lead
Level
0.0
0.3
0.6
1.0
1.4
2.0
6.0
0.3
0.6
1.0
1.4
2.0
6.0
Lead Levels
Mean (mg/cm2)
0.00
0.40
0.64
1.00
1.48
2.29
9.18
0.32
0.57
1.00
1.41
2.03
5.15
CoV
8.2
17.8
13.5
5.1
8.0
5.6
31.2
13.1
16.6
7.1
11.0
9.4
9.6
Range
Min
0.002
0.234
0.425
0.918
1.322
2.018
5.65
0.252
0.511
0.879
1.194
1.483
3.929
Max
0.003
0.505
0.761
1.095
1.748
2.525
18.4
0.428
0.920*
1.148
1.601
2.314
6.247
* Next highest measurement was 0.659
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Appendix B
Standard Operating Procedure (SOP)
For Collection of Dried Paint Samples for Lead Determination
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I. Scope
This Standard Operating Procedure (SOP) describes the manner to which dried paint
samples should be collected for the determination of lead on substrates such as metal,
wood, plaster and dry wall.
II. Purpose
The purpose of this SOP is to create a reproducible sampling technique that minimizes
variability between samples and to accurately represent a lead level for a specific
substrate.
III. References
A. ASTM E 1729-05 Standard Practice for Field Collection of Dried Paint Samples
for Subsequent Lead Determination.
B. SOP AMA1-006-02 Standard Operating Procedure for the Safe Handling of Lead,
Lead-Spiked Paint, and Lead-Spiked Samples
C. OSHA Standards for Lead-1910.1025
D. Battelle Safety and Industrial Hygiene Program Plan (#ESHQ-Sffl-PP-005)
E. ETV ESTE Test/QA Plan For The Verification Of Qualitative Spot Test Kits For
Lead In Paint
IV. Definitions
A. Paint collection tray-any clean, dry, lead-free container for use in catching paint
scrapings.
B. PPE-Personal protective equipment
C. Lead worker-Training for any person physically handling lead powders or lead-
containing materials such as paints.
V. Procedures
A. Equipment and Materials
i. PPE
1. Disposable Coveralls/Scrubs
2. Disposable Gloves
3. Disposable Shoe Covers
4. Safety Glasses with Side Shields
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ii. Equipment
1. glass vials and lids
2. labels
3. tape
4. Sampling template - one inch square reusable aluminum or steel
template with accurately known dimensions
5. disposable wipes-for cleaning off sampling equipment
6. sharp-edged knives/blades/chisels for cutting and scraping
7. tweezers
8. Paint collection tray
9. small brushes-for brushing off powder to weighing paper for
transfer
B. Lead workers with full PPE in a dedicated lead hazard area with lead disposal will
be used to minimize exposure to other persons or areas.
C. Label vial for collection using the number on the back of the panel
D. Place the 1 inch square template as close to the tested area as possible, without
including any disturbed areas.
i. There are two types of templates, a one inch square and a punch-out of
one inch square. See Picture 1.
Picture 1: Templates
E. Metals
i. While holding the template in place, score an outline of the area using a
sharp edge.
ii. Remove square template and clean the template with a wipe. Set aside
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iii. Using tweezers, remove square latex topcoat and place in vial. See
Picture 2.
iv. Using a blade, scrape the lead off the exposed one inch area and brush on
to a collection tray. Make sure to brush all remaining lead and do not
disturb adjacent area. See Picture 3.
v. Put contents of tray into the same vial, close lid tightly and label
appropriately.
Picture 2: Metal with latex topcoat removed
Picture 3: Metal with lead scraped and brushed on to collection tray
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F. Dry wall
i. While holding the template in place, score an outline of the area using a
sharp edge.
ii. Remove template and clean template with a wipe, set aside.
iii. Using tweezers remove latex topcoat. See Picture 4
iv. Using a blade, scrape the lead off the exposed one inch area, minimizing
any drywall paper within the area.
v. Brush all remaining lead off the panel onto the collection tray without
disturbing the adjacent area.
vi. Place all material into a vial, close tightly and label properly.
Picture 4: Drywall with latex topcoat removed
G. Plaster
i. While holding the template in place, score an outline of the area using a
sharp edge.
ii. Remove template and clean template with a wipe, set aside.
iii. Using tweezers remove latex topcoat. See Picture 5
iv. Using a blade, scrape the lead off the exposed one inch area, minimizing
the collection of any plaster with the sample.
v. Brush on to a collection tray without disturbing the adjacent area. See
Picture 6
vi. Place all material into a vial, close tightly and label appropriately
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Picture 5: Latex topcoat removed from plaster sample
Picture 6: Scraping of lead from plaster
H. Pine and Poplar
i. While holding the template in place, score an outline of the area using a
sharp edge.
ii. Remove template and clean template with a wipe, set aside.
iii. Using tweezers remove latex topcoat. See Picture 7
iv. Using a blade, scrape the lead off the exposed one inch area, minimizing
the collection of any wood with the sample.
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v. Brush on to a collection tray without disturbing the adjacent area. See
Picture 7
vi. Place all material into a vial and close tightly
Picture 7: Latex topcoat removed from wood panel
VI. Safety
A. Project staff who work with lead or lead products must complete lead worker
training. Visitors are not permitted in the lead contaminated areas without prior
approvals and proof of required medical surveillance and training.
B. Staff will be on a Battelle Medical Monitoring Program, and will have had an
annual physical, etc., as required for working with lead, and will be approved to
work on projects using lead
C. Staff working with lead will be kept to the minimum number required to do the
project.
D. Clothing or equipment will not be blown, shaken, etc. to remove dust.
E. Waste (such as filters, liners, PPE, wipes, ETC.) will be disposed of as per
Battelle policies/procedures for lead contaminated items.
F. MSDS for Lead and Paint used in projects are in Room 5148
G. Battelle has strict policies that no food or beverages be present or consumed, nor
any cosmetics applied within the laboratory area. Contact lenses will not be
handled in or around the area
H. Any known or suspected exposure to lead outside of the engineering controls will
be reported to Battelle Health Services or Safety Health/Emergency Response
(SH/ER) representative as soon as possible
I. Refer to Battelle Safety and Industrial Hygiene Program Plan (ESHQ-Sffl-PP-
005) for additional guidance
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Verification of Qualitative Spot Test Kits for Lead in Paint
Test/QA Plan
Page 67 of 67
Version DRAFT
Date: 3/30/2010
VII. Shipping
A. Lead-containing painted samples will be analyzed further at a different location
B. Samples will be protected from possibly contaminating the shipping route by
enclosing the vials in an additional plastic bag and securing the bag with tape.
C. Sample custody will be documented for the shipping and analysis of PEMs to the
subcontract laboratory using standard chain-of-custody (COC) forms provided by
the laboratory performing the analysis.
D. The original sample COC forms will accompany the samples; the shipper will
keep a copy.
E. Copies of all COC forms will be delivered to the Verification Test Coordinator
and maintained with the verification test records.
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