United States
Environmental
Protection Agency
Office of
Pollution Prevention
and Toxics
EPA 747-R-97-004
September 1997
Archive Operations and Protocols
PROTOCOL DEVELOPMENT
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EPA 747-R-97-004
September 1997
Archive Operations and Protocols
Technical Branch
National Program Chemicals Division
Office of Pollution Prevention and Toxics
Office of Prevention, Pesticides, and Toxic Substances
U.S. Environmental Protection Agency
401 M Street, S.W.
Washington, D.C. 20460
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DISCLAIMER
The material in this document has been subject to Agency technical and policy review
and approved for publication as an EPA report. Mention of trade names, products, or
services does not convey, and should not be interpreted as conveying, official EPA
approval, endorsement, or recommendation.
This report is copied on recycled paper.
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CONTRIBUTING ORGANIZATIONS
The methodology described in this Operations Manual is part of a task funded by the
U.S. Environmental Protection Agency (EPA) and the U.S. Department of Housing and
Urban Development. The task was managed by EPA and was conducted collaboratively by
three organizations under contract to EPA: Midwest Research Institute, Battelle Memorial
Institute, and QuanTech. Each organization's responsibilities are listed below.
Battelle Memorial Institute
Battelle Memorial Institute (Battelle) was responsible for oversight of archive sample
maintenance and archive testing.
Midwest Research Institute
Midwest Research Institute (MRI) was responsible for the development of this
operations manual, sample maintenance, collection of paint samples, laboratory analysis,
and supervision of testing.
QuanTech
QuanTech (formerly David C. Cox & Associates) was responsible for testing design,
data management, development of statistical methods, and the writing of the methodology
report and the associated XRF Performance Characteristic Sheets.
U.S. Environmental Protection Agency
The U.S. Environmental Protection Agency (EPA) co-funded the task, managed the
task, reviewed task documents, and managed the peer review of this report. The EPA
Project Leader was John Schwemberger. The EPA Work Assignment Managers were Sam
Brown, John Seal era, and John Schwemberger. The EPA Project Officers were Sam
Brown, Jill Hacker, Phil Robinson, and Sineta Wooten.
U.S. Department of Housing and Development
The Department of Housing and Urban Development (HUD) co-funded the task and
was responsible for reviewing the XRF Performance Characteristic Sheets and for contacts
with the manufacturers of lead-based paint testing technologies. The key HUD staff
member was Bill Wisner.
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ACKNOWLEDGMENTS
Special thanks are due to Mary McKnight of the National Institute of Standards and
Technology (NIST) for operating XRF instruments during archive testing and for her advice
and comments.
IV
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CONTENTS
1.0 Background 1
1.1 Purpose of the EPA/HUD Lead-Based Paint Archive 1
1.2 Purpose of the Operations Manual 2
1.3 History of the Archive Components 2
1.4 Quality of Data 2
1.5 Report Organization 2
1.6 Peer Reviews 3
2.0 Description of Facility 3
2.1 Location 4
2.2 Archive Design/Layout 4
2.3 Security 7
2.4 Component Description 7
2.5 Control Block Information 8
3.0 Staff and Responsibilities 9
4.0 Archive Sample Management 10
4.1 Maintaining Archive Samples 10
4.2 Securing Archive Samples 10
4.3 Managing Testing with Archive Samples 11
5.0 Facility Operations 11
5.1 Order of Testing 11
5.2 Personnel and Radiation Safety 12
5.3 Testing Protocols 12
5.4 XRF Contractor/Operator Responsibilities and Orientation: 13
5.5 Archive Testing 13
6.0 Statistical Analysis of Data 14
7.0 Deliverables and Reports 14
8.0 Audits 15
9.0 References 16
Appendices
A QAPjP Addendum 17
B XRF Testing Protocols 18
C Supplemental Protocols for Sampling, Characterization, and Analysis
of Lead-Based Paint Samples 19
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1.0 Background
Archive operations, which this manual addresses, were preceded by the U.S.
Environmental Protection Agency (EPA) and U.S. Department of Housing and Urban
Development (HUD) field study of portable X-ray fluorescence (XRF) instruments and
chemical test kits.1'2 The results of the EPA field study are presented in the reports A Field
Test of Lead-Based Paint Testing Technologies: Technical Report, (EPA 747-R-95-0026,
May 1995) and A Field Test of Lead-Based Paint Testing Technologies: Summary Report,
(EPA 747-R-95-002a, May 1995). The predecessors to this document are the Quality
Assurance Project Plans for the pilot3 and full4 EPA/HUD Field Study. The results of the
Field Study, which was conducted at various housing units throughout several U.S. cities,
were used to develop a comprehensive performance database of commercially available
XRF instruments and field test kits.
In conjunction with the Field Study, samples of painted housing components were
collected for two purposes: first, to perform data verification and quality assurance after
completion of the Field Study and, second, to have a way to evaluate a new XRF
instrument or test kit that might enter the market after the end of the Field Study.
The samples collected from the Field Study have become an archive of materials that is
being used as the basis for an interim testing program for new portable XRFs, while a
protocol for laboratory testing of new portable XRFs is being developed by National
Institute of Standards and Technology (NIST) for HUD. At this point, no destructive
technologies are being tested at the archive in order to preserve the integrity of the samples.
The archive facility is maintained under secure and controlled conditions to assure the
integrity of the samples.
This document contains the operating procedures for the archive for testing that took
place between December 1994 and September 1996. This document also contains
protocols for testing and sample collection that were used during this period of time. This
report is being released to provide documentation of these operating procedures and
protocols for the time period from December 1994 to September 1996.
1.1 Purpose of the EPA/HUD Lead-Based Paint Archive
The EPA/HUD Lead-Based Paint Archive was developed to evaluate new portable
XRF instruments and to produce instrument-specific information necessary for the
instruments to be used to conduct lead-based paint inspections as specified in the HUD
Guidelines. The instrument-specific information is embodied in the XRF Performance
Characteristic Sheets (PCSs), which are an extension of Chapter 7 in the HUD Guidelines.
PCSs are XRF instrument model-specific documents intended to provide up-to-date
performance information on XRF instruments. Data from the EPA/HUD Field Test of
Lead-Based Paint Testing Technology study1 have been used to develop the first set of
PCSs. The EPA/HUD Lead-Based Paint Archive is a collection of real-world samples that
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were assembled to test XRF instruments not available for evaluation during this study.
Results from analysis of data collected from XRF testing at the archive site are used to
produce PCSs for these instruments.
The archive is not currently being used to test chemical test kits for lead because of the
destructive nature of the analysis. Portable XRF instruments are essentially non-
destructive.
1.2 Purpose of the Operations Manual
The purpose of this Operations Manual is to document the general procedures used to
maintain and operate the facility and describe the quality assurance and specific test
procedures for testing the XRF instruments.
1.3 History of the Archive Components
The components in the EPA/HUD Lead-Based Paint Archive consist of sections of
painted building components that are commonly encountered in residential housing, such as
doors, walls, baseboards, gutters, and window frames. Samples in the archive represent a
subset of the 1,290 samples tested in the above-referenced study. During this study,
selected testing locations on architectural components were targeted for collection from
housing units in three different cities: 10 single-family units in Denver, Colorado;
4 multifamily units in Louisville, Kentucky; and 8 multifamily units in Philadelphia,
Pennsylvania. In addition, four additional samples were sent by the EPA's Office of
Research and Development and are included in the archives. Some of the samples that were
collected in Louisville were obtained after they had been removed from units in the
development and placed in receptacles for removal; therefore, the specific housing units that
these samples came from are unknown. Building materials that contained the selected
measurement locations were removed and later assembled into the Lead-Based Paint
Archive.
1.4 Quality of Data
As with any environmental measurement project, the quality of the data is important to
assure that the data are appropriate for the intended use. To assure that the data collected
in the archive testing are of sufficient quality, a Quality Assurance Project Plan (QAPjP)
Addendum (Appendix A) was prepared. The QAPjP Addendum addresses data quality
objectives for the archive testing, the experimental design, and the data collection and
analysis procedures and protocols. The QAPjP ensures that the data collected are accurate
and of appropriate quality for the intended use.
1.5 Report Organization
This report presents the historical background of the archive facility, a physical
description of the facility, and general operating procedures relative to staff
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responsibilities, sample management, testing procedures, reporting of data, and quality
assurance/quality control. The report has an appendices section, which includes the
QAPjP, historical XRF Testing Protocols, and Supplemental Protocols used at the archive.
1.6 Peer Reviews
This report was reviewed by five subject area experts prior to its publication.
Comments on the document were largely editorial. In response, changes were made to
clarify certain points and to make the report easier to read.
One reviewer commented on the relationship between this report and the EPA report
Methodology for XRF Performance Characteristic Sheets. This report describes the
operation of the archive facility in the period December 1994 to September 1996 and
includes detailed protocols that were used for archive testing and sample collection. Data
collected from the archive were used to develop XRF Performance Characteristic Sheets
that have been released to the public through the National Lead Information Center
Clearinghouse. (The phone number of the Clearinghouse is 1-800-424-LEAD.) The report
Methodology for XRF Performance Characteristic Sheets describes the statistical
methodology used to develop the information in the XRF Performance Characteristic
Sheets. In effect, this report describes how data for the XRF Performance Characteristic
Sheets were collected, and the report Methodology for XRF Performance Characteristic
Sheets describes how those data were analyzed to produce the XRF Performance
Characteristic Sheets.
Other reviewer comments concerned the representativeness of the archived samples
and maintaining the integrity of samples over time. Most of the samples came from an
EPA/HUD field study conducted in three separate cities. The selection of samples for the
archives were selected on a random basis within specific substrate and lead concentration-
range categories. The archived samples are regularly inspected and the storage conditions
are controlled as described in this report to help extend the integrity of the samples for
testing as long as possible.
Another recurring comment involved the purpose and intent of the appended protocols
in this report. The XRF testing protocols represent a historical record of testing, and the
supplemental protocols provide detailed instructions that were used for operation of the
archive and for sample characterization purposes.
2.0 Description of Facility
Building No. 1, the facility housing the archive samples, is a 1,380 ft2 concrete block
building accommodating the design and layout used for archive materials.
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2.1 Location
The building used for the EPA/HUD Lead-Based Paint Archive is located at the MRI
Deramus Field Station in Grandview, Missouri. Deramus Field Station is a rural 78-acre
site with 17,500 ft2 of laboratory space in six special-purpose buildings.
2.2 Archive Design/Layout
The archive components consist of building materials, with the selected measurement
locations indicated, vertically mounted into testing walls that are constructed from sheets of
plywood bolted to a wood frame. The walls are arranged in a rectangular configuration
approximately 32 feet long by 20 feet wide by 8 feet high.
The archive testing facility (see Figure 1) consists of 158 archive components. The
components are mounted in a manner to minimize interferences during XRF testing.
Mounting characteristics include the following:
Separation of at least 4 feet between the testing wall containing the components
and any objects behind the targeted area.
Removal of plywood from the back side of most sample locations. For a few
components, including all brick and concrete components, the components are
mounted within a plywood box that is attached to the wall.
• Exclusion of materials used for mounting, with the exception of plywood or
Styrofoam for a few components, from positions lying directly behind XRF test
areas on the components.
In a few cases, the statistical test design includes XRF measurements on both the
front- and backside of an individual component. The backside measurements are treated as
separate and unique measurements and do not coincide with the front-side measurements
of the archived sample during the XRF test sequence.
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External Concrete
Block Wall
Computer and
Work Bench
Archiving Exterior Covered
Components Windows Control Blocks
Minimum Separation
Between Walls 4'
4' x 8' Framed Component
Holding Panels
Figure 1. Archive Testing Facility
95-43 SEV bal scm 062895
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P3
Alternate
measurement
location where
paint has been
scraped off of
substrate.
2x2 in
X3 Tertiary XRF
Measurement
Location
PI
Primary
measurement
location where
paint has been
scraped off of
substrate.
•I
f-
ys
4x4 in
XI Primary
XRF Test
Location.
Test Kit Measurement Locations
(previously used during field testing)
X2
Secondary
XRF Test
Location.
Figure 2. Example Template Used for Testing Archived Components
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2.3 Security
The Deramus Field Station is within a limited access/entry area that is controlled by
locked gates. Each of the laboratory buildings are under separate locks and can be
accessed only by authorized MRI personnel. All of the keys for the locks at the field
station are in the custody of MRI Security, which issues keys to personnel that are
authorized access to specific buildings.
The archive samples are secured by double lock entry on the building. Access is
controlled by keys issued by MRI. Only the MRI Program Manager, Task Leader, and QA
Officer have been issued keys to the building. MRI Buildings and Grounds has a key to the
building for access in cases of structural maintenance, emergencies, and general safety
inspections. Subcontractors, visitors, or non-project personnel are not allowed access to
this facility without being escorted by the MRI Program Manager, Task Leader, or QA
Officer.
2.4 Component Description
The 158 archive components are normally tested once in a random order. XRF
measurement locations have been marked on each archive sample using a dark colored
marking pen. The markings are in the form of squares and rectangles labeled with the
letters "X" or "P," followed immediately by the numbers "1", "2", or "3." An example of
the template used for testing the components is shown in Figure 2. The template is
modified for some samples due to space limitations, etc. XI is the primary painted XRF
testing location, and X2 and X3 are secondary and tertiary painted testing locations,
respectively. PI is a testing location on each component that has been scraped of its paint;
the PI area is used in measurements involving "bare" or substrate-only testing. Some
samples have P2, P3, or P4 areas, which are secondary testing locations that have also been
scraped of paint, but these secondary locations are not typically used during XRF testing.
XRF testing areas on samples mounted on the testing wall are identified according to
the study protocols. Each testing location has an assigned unique number that is used for
identification purposes. Lead levels have been determined from laboratory analysis of
paint chip samples collected from at least two areas at each sampling location. Up to three
separate painted XRF testing areas are identified on each sampling location using
designations XI, X2, and X3 (as noted above). The testing walls contain 158 archive
components from various locations and a variety of substrates. A summary of the type of
component substrates is presented in the table below.
The development of the PCSs are based on XRF measurement data from the XI
primary painted XRF testing location and the PI nonpainted substrate of each component.
The secondary test locations on each component (e.g., X2, P2, etc.) were not used for
developing the PCSs.
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Summary of
Substrate Type
Wood
Plaster
Metal
Drywall
Brick
Concrete
Samples in the EPA/HUD Lead-Based Paint Archive
No. of Samples Range
63
38
38
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3
2
of Lead Levels (mg/cm2)
0.0003-30.11
0.0024-16.07
0.0032- 3.97
0.0002- 0.90
0.0035-17.50
0.0009- 0.10
2.5 Control Block Information
Control substrate blocks are part of the test design to record instrument variability
relative to changes in substrates and sensitivity "drift" with time. The control blocks are a
series of six quality control (QC) blocks consisting of different materials (metal, wood,
brick, drywall, concrete, and plaster). Each of the QC blocks has been tested by chemical
analysis (ICP-AES) of representative core samples to characterize the concentration of lead
and potential interfering elements.
At the beginning and end of each day, a series of three quality control measurements
will be performed on each of the six control blocks. The three QC measurements that will
be taken on each control block are with the yellow NIST standard film (3.53 mg/cm2)
covering the QC block, followed by the red NIST standard film (1.02 mg/cm2), followed by
one reading taken without a NIST film. This set of measurements will be repeated at the
end of the day.
Two sets of continuing QC measurements are performed after the standard readings
are completed on every fifteenth archive component. The first set of continuing control
readings is performed on the QC block that is composed of material similar to the last
archive component tested. The second set of continuing control readings is performed on
the QC block that is composed of material similar to the next archive component to be
tested.
In a few cases, archive components were added to the archive measurement sequence
and designated by the letter "A" followed by the number of the preceding component. In
these cases, the inserted archive component was not counted as one of the 15 readings for
the purpose of the continuing QC measurement in order to keep continuity with previous
tests. At a later date, the entire archive component series was statistically re-randomized
and renumbered so that all inserted components were fully integrated into the test
sequence.
For the wood control block only, two additional consecutive readings are taken with
the red NIST standard film (1.02 mg/cm2) over the bare wood substrate during the
beginning of day QC measurement series, continuing calibration QC checks during archive
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testing, and at the end-of-the-day QC checks. The purpose of these replicate measurements
on wood is to establish precision of the instrument throughout each testing period and for
subsequent calculation of the calibration check values for the PCS documents.
3.0 Staff and Responsibilities
For this study, the staffing necessary to conduct the operations are the Program
Manager, Testing Supervisor, Testing Monitor, and XRF Contractor/Operator.
The Program Manager will:
• Ensure that all necessary resources are available.
• Ensure that all personnel are informed of the project QA requirements.
• Ensure that all personnel conduct the work in a safe manner.
• Ensure that the project and financial status are reported to the OPPT Work
Assignment Manager.
The Testing Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Assure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI,
NIST, and QuanTech.
• Assure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Complete a new set of SAMPLE LOCATION CONDITION forms for:
o Locations on the components previously identified as being in poor
condition, which already have completed records from the spring 1995
testing.
o Any additional sample locations that are observed to be in poor condition.
• Provide the following forms:
o Archive XRF Information
o Source Age Adjustment Table
o Testing Order List
o Control Readings
o Standard Readings
o Sample Location Condition
• Take radiation emission measurements on the XRF instrument.
• Assure that everyone who enters the facility during XRF testing is wearing a
dosimeter badge and collect the badges at the end of each day.
• Arrange for testing of the dosimeter badges at the appropriate time interval.
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The Testing Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Contractor/Operator to help assure the protocols are followed.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
The XRF Contractor/Operator will:
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help assure that protocols are followed and
any deviations are properly documented.
• Download data to a computer and verify that the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed
during testing.
4.0 Archive Sample Management
The integrity of the components are ensured by maintaining the archived samples
within controlled environment and by protecting the samples against damage from the XRF
instruments during testing.
4.1 Maintaining Archive Samples
The archive facility at MRI's Deramus Field Station has been set up to provide an
environment that will help preserve the components as long as possible to assure the
collection of comparable data. To ensure this, the building is temperature controlled
throughout the year.
The conditions of the archive components are monitored during and after each XRF
activity to assure that no damage has been caused by the instrument. If any damage is
observed either to the component or the painted surface, the damage will be documented
on the sample condition records and reported to the Program Manager and the EPA Work
Assignment Manager. A joint decision will be made as to the corrective action to be taken.
The repairs to the archive samples are generally performed by the Testing Supervisor.
4.2 Securing Archive Samples
The building itself is located on MRI property, which is fenced and posted as restricted
access. The front gate is locked and restricted to MRI personnel only. This MRI property
also has a custodian living on-site for security and maintenance purposes. The Archive
facility is equipped with its own phone line with direct access to MRI Security and Safety
officers.
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4.3 Managing Testing with Archive Samples
All testing activities on the archived samples are carried out using approved protocols
under supervision of the MRI Testing Supervisor. Normally, the Project Task Leader
performs these duties. The specific responsibilities of the Testing Supervisor was
described in Section 3 of this document and these responsibilities are carried out each time
the archives are used for testing.
XRF testing using subcontracted, independent operators is performed in compliance
with the appropriate protocol. Subcontractors are restricted to the operation of the
instruments only and are not involved with technical or procedural decisions during the
tests.
5.0 Facility Operations
All testing of the archives must be done using pre-approved protocols specific for the
XRF instrumentation being used. The protocol provides the calibration requirements
(usually cited from the manufacturer's manual), the number and sequence of QC samples,
and the sequence for the archive components. In addition, the specific protocols specify
the length of timed readings, if appropriate, or the test mode (which usually varies in time
based on the lead concentration of the paint). The testing for most XRF operations should
be accomplished in two to two-and-a-half days. The measurements taken for XRF testing
on the archive components are:
• Initial (beginning of the day) control measurements
• Standard measurements
• Continuing control measurements
• Ending (end of the day) control measurements
5.1 Order of Testing
Randomization of the testing order was assured by the following steps in the design of
the Archive test facility. First, the placement and order of the components on the boards
was assigned in a randomized order. Second, the sequential order of testing was also
randomized to make the XRF operators walk and move about the facility, as they would
during a lead-based paint inspection.
Four additional plaster samples were added to the sample test series after the archive
facility was built. The samples were physically added to the facility by mounting all four
on a separate board. In order to maintain the randomness of the sequential testing order,
the four additional samples were statistically "remixed" with the pool of samples and
assigned random numbers in the test series. The samples were inserted into the original
sequential order of testing by adding the letter "A" after the component number it
followed; for example, if one of the added samples came after 100, it would be given the
identification of 100A and the test sequence would become: 99, 100, 100A, 101, 102, etc.
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Continuing calibration checks on the XRF instruments were performed at the normal 15
sample intervals, except when the added plaster samples were encountered. For
consistency, the "A" samples did not count as one of the 15 samples separating the
continuing calibration checks; this allowed the QC checks to be performed after the same
samples as before the 4 plaster samples were added. At a later date, the entire archive
component series was statistically rerandomized and renumbered so that all inserted
components were fully integrated into the test sequence.
When it is necessary to change the Archive Testing Order, the procedure starting on
page C-39 of the Supplemental Protocols is used to renumber the samples.
5.2 Personnel and Radiation Safety
Although safety and operational instructions are the responsibility of the study
Supervisor, safety is the collective responsibility of everyone and requires the unqualified
support and cooperation of each person involved with the archive operations. In
conducting tests at the MRI archives, each person must be aware and participate in general
safe work and radiation safety practices. Since many accidents are the result of
indifference, failure to use common sense, or failure to follow instructions, those involved
in the study must always be aware of what coworkers are doing in the immediate area,
especially with the XRF instrument.
Since the effects of radiation exposure are not immediately apparent, all XRF
instrumentation will be monitored during use with a survey meter (Geiger-Mueller counter)
equipped with a beta-gamma detector. Any XRF instrument having counts (mR/hr) above
the manufacturer radiation safety specifications will not be tested. In addition to the
monitoring of the instruments, each person will have and wear, during the archive testing
process, a personal film dosimeter to measure and evaluate his or her exposure.
5.3 Testing Protocols
Testing protocols (Appendix B) for each XRF instrument under evaluation are
developed from manufacturer-supplied documents, such as the manufacturers' instrument
operating manuals. Efforts are exerted to perform testing in a manner consistent with
manufacturer guidance subject to the restriction that no destructive testing can be permitted
on samples within the archive. Sampling locations are tested using extensive before,
during, and after QC checks on NIST Standard Reference Material paint films (SRM 2579)
placed over blocks of representative substrates (control blocks). Testing at each sampling
location includes measurements on each painted area (XI, X2, and X3) and measurements
on a bare substrate area both with and without being covered by the 1.02 mg/cm2 NIST
SRM.
Other testing protocols developed for this project that are not a part of XRF testing but
are part of the overall project requirements are found in Appendix C.
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5.4 XRF Contractor/Operator Responsibilities and Orientation
The XRF Contractor/Operator is responsible for his or her training on the equipment
being tested. The contracted instrument operators are required to have a backup instrument
on-site so that testing could be continued with the backup instrument if necessary. Both
the primary and backup instrument should preferably have sources no more than 6 months
old. At the end of the test day, all test data are downloaded to the facility computer and
backup diskettes; then the electronic data files are purged from the operator's instrument
before the instrument is taken off-site. The XRF Contractor/Operator also is responsible
for following all federal and state licensing requirements in handling and using radioactive
material. The contractor/operator is responsible for self monitoring of radiation exposure
using an appropriate film dosimeter.
If the full test round cannot be completed using the primary instrument, the backup
instrument may be used to continue the testing only after demonstrating that manufacturer
and protocol calibration/QC checks are acceptable on the backup instrument. If both the
primary and backup instruments fail before completing the full test series, the testing is
stopped, all causes and actions are documented, and all recoverable data are collected as
normal. Testing does not resume until instruments that can pass all applicable warm-up,
calibration, and quality control checks are available.
5.5 Archive Testing
The general procedure for performing the test is given below.
1. Receive beginning-of-day instructions from Testing Supervisor.
2. Perform manufacturer's initial calibration checks. Perform additional
manufacturer's calibration checks at intervals as required by the manufacturer's
specifications.
3. Perform initial control block measurements on all six blocks. Record temperature
and humidity data.
4. Perform standard set measurements (15 archive components).
5. After the completion of the first 15 archive components, and following every 15
archive components thereafter, perform continuing control readings on the two
control blocks with the same substrates as the last and next substrates tested.
Intermittent delays (such as lunch breaks, etc.) are taken at the continuing
calibration check points.
6. Record temperature and humidity data approximately halfway through the day.
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7. At various times during the day, record in the field notebook the time required by
the XRF instrument to actually display the lead measurement result. The data
recorded during the day for this purpose should include the start and end times for
20 measurements. The start time is the time of day when the XRF probe face-
plate is placed on the surface to be tested and testing commences. The end time is
the time of day when the result is displayed on the XRF readout area.
8. At the end of the first day of testing, perform ending control block measurements
on all six blocks. Record temperature and humidity data.
9. Perform end-of-day activities, which include: performing final manufacturer-
specified calibration checks, reviewing data forms for completeness, downloading
electronically stored data to the on-site computer, and ensuring that all
electronically stored data is erased from the XRF instrument.
6.0 Statistical Analysis of Data
Data collected from the archive are analyzed using statistical methods similar to those
that were developed in the above-referenced study. A model is used to estimate the bias
and precision of an XRF instrument as a function of the amount of lead present in paint.
Estimates are also derived for substrate-corrected XRF results, in cases where such
correction is demonstrated to improve performance. Inconclusive ranges and thresholds
for the XRF readings are derived using bias and precision estimates.
Detail on the methodology for developing the XRF Performance Characteristic Sheets
is available in the report Methodology for XRF Performance Characteristic Sheets5
7.0 Deliverables and Reports
Deliverables and reports for this project include:
• Testing Protocols
• Revisions to the XRF Operations Manual
• Revisions to the Quality Assurance Project Plan
• XRF Data Reports
• Radiation Monitoring Report
• Component Monitoring Report
• Component Repair Report
• Performance Characteristic Sheets
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8.0 Audits
Quality assurance activities associated with the Archive Operations include audits
performed on work in progress and on completed XRF test data sets. Because the quality
and completeness of the data set are vital to accurately evaluate the individual XRF
instruments, QA audits are focused on data collection, transfer, and verification.
Prior to XRF testing, protocols and data forms are reviewed by QA staff to assure that
the data set will include all available data produced by a particular instrument. For
example, the forms are "customized" to assure that all appropriate modes of operation,
time displays, precision indicators, and other readouts are included in the data recording
process.
During the XRF testing, instrument displays are randomly checked by visual
verification (in addition to voice communication between the instrument operator and data
recorder) by either the recorder himself, the supervisor, or the QA officer. These
verification checks are noted on the forms. For any situation in which the monitor's
reading differs from the operator's reading, the testing will be temporarily stopped until the
cause of the discrepancy is determined and the actions taken will be noted on the data
collection forms.
Throughout the test day and after each day's recordings are complete, the data forms
are checked for completeness and clarity by either the supervisor or the QA officer. The
forms are checked for proper page numbering, clarity of notes, appropriate strike-outs of
nonusable data, signatures, dates, and instrument identifications.
After electronic data transfers from the instrument to the facility computer and backup
diskettes, the electronic files are audited by verifying correct dates and file names, checking
consistency of byte numbers between original and copied files, and inspecting the data files
to see if beginning and ending data (sequence numbers, lead concentrations, etc.) are
consistent with the recorded forms.
Care is taken to ensure adequate backups of the data exist in case of accidental loss.
Originals of the completed data forms are photocopied and electronic files are copied onto
the facility computer, then backed up on two sets of diskettes. Exact copies or the originals
are provided for the statistical analysis study, and the originals are retained or transferred
back to the project files for archiving.
QA audits during statistical analysis are conducted to assure the accuracy of derived
results. These audits include double-entry checks during transfer of the recorded data into
the database files and cross-checks between the hand-recorded (primary) data set and the
electronically captured (secondary) instrument data files.
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9.0 References
1. A Field Test of Lead-Based Paint Testing Technologies: Technical Report., EPA 747-
R-95-002b, May 1995.
2. A Field Test of Lead-Based Paint Testing Technologies: Summary Report., EPA 747-
R-95-002a, May 1995.
3. MRI Report, Quality Assurance Project Plan for the Pilot Study: Comprehensive
Field Study ofXRFs, Lead Paint Test Kits, and Laboratory Analyzed Paint Chip
Samples, EPA Contract No. 68-DO-0137, MRI Project 9801-A-57, March 15, 1993.
4. Quality Assurance Project Plan for Comparative Field Study of Methodologies Used
to Detect Lead in Paint, dated November 30,1993.
5. Methodology for XRFPerformance Characteristic Sheets, EPA 747-R-95-008,
September 1997.
16
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Appendix A
QAPjP Addendum
Contents
Quality Assurance Project Plan (QAPjP) Addendum for Comparative
Field Study of Methodologies Used to Detect Lead in Paint A-l
QAPJP Addendum Attachment A-12
QAPjP Clarifications and Additions A-14
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QAPjP ADDENDUM
Revision No. 1
Effective Date: December 14, 1994
QUALITY ASSURANCE PROJECT PLAN (QAPjP) ADDENDUM FOR
COMPARATIVE FIELD STUDY OF METHODOLOGIES
USED TO DETECT LEAD IN PAINT
Work Assignment No. 5-24
Contract No. 68-DO-0137
Work Assignment No. 3-02
Contract No. 68-D3-0004
A-l
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QAPjP ADDENDUM
Revision No. 1
Effective Date: December 14, 1994
This document is an addendum to the QAPjP of July 8, 1993, titled "Quality
Assurance Project Plan for Comparative Field Study of Methodologies Used to Detect
Lead in Paint."
1.0 SUMMARY
In 1993, the Environmental Protection Agency (EPA) initiated a field evaluation of
XRF instruments and lead paint test kits. These two technologies were tested on samples
of painted components in vacant housing units. As stated in the QAPjP (section 3.3.3),
samples from certain (specific) locations were collected and archived for future use.
Since there are XRF instrument manufacturers whose instruments were not in the
study, these manufacturers are requesting an evaluation of their products. The Department
of Housing and Urban Development (HUD) has been the recipient of these requests, and
HUD has asked EPA to provide a limited evaluation based on the archive materials from
the field evaluation. In addition, two questions that have arisen from the study results
should be resolved. One of these involves spatial variation in painted building components
and the other involves the order of substrates when taking XRF measurements.
EPA proposes to initiate its testing of the new instruments and other XRF instruments
in January 1995. The funding will be derived from money earmarked for the completion of
the field evaluation.
2.0 DESIGN
2.1 GENERAL OBJECTIVES AND DESIGN
Approximately 150 samples of painted housing components are available for testing of
new instruments. The range of lead levels in these samples is approximately as follows:
50% less than 0.4 mg/cm2, 25% between 0.4 and 1.7 mg/cm2, and 25% greater than 1.7
mg/cm2. Most of the samples consist of metal, plaster, wood, and drywall. Brick and
concrete substrates have only token representation due to physical limitations in collecting
samples of such substrates.
The first and primary objective is to provide a limited evaluation of new XRF
instruments that were not in the full study and to report the results to HUD.
The second objective is to deal with spatial variability in the paint samples. This will
be done by taking a second sample for ICP analysis so as to better characterize the lead in
the paint in the XRF test area, by using this second sample to validate interpolation models,
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and by taking XRF readings at additional locations on the archived material to determine
the impact of additional areas on XRF measurement.
The third and last objective is to determine if the order of substrate materials has an
effect on XRF readings.
Methods and approaches will be the same as in the field evaluation study, except
where results of the field study indicated a change was desirable.
For the XRF instruments in this study addendum, a source that is no more than 6
months old is required, as was the case in the full field study. Testing will be done by
personnel from XRF testing firms under subcontract to MRI or by personnel from the
National Institute of Standards and Technology (NIST). New instruments will be included
that are being sold and delivered to testers in this addendum study. The new instruments
that are expected to be included in this study are: the revised XL by Niton Corporation, the
SEFA manufactured by HNU Corporation, the LPA-1 manufactured by Radiation
Monitoring Devices, and the LeadStar manufactured by Xsirius Corporation. In general, a
reading with one of these instruments will be nominally 15 seconds long, but manufacturer
instructions will be examined to determine each instrument's standard reading mode, and a
reading will be redefined to fit the manufacturer's standard reading mode unless this is not
practical.
The other instrument to be used in this addendum to the study is the Lead Analyzer.
The Lead Analyzer will be used to determine the impact of laboratory-setting versus field
measurements, providing a common element between the field and archive phases of the
study, and to pilot test the archive layout. The ML-1, the XK-3, or the MAP-3 will be
considered for use if a suitable Lead Analyzer is not available for this study.
For each of the new instruments, two instruments will be used: one by a testing firm
under subcontract to MRI and one owned and operated by NIST. For the Lead Analyzer
(or the ML-1, the XK-3, or the MAP-3), a single instrument will be used, either from a
testing firm under subcontract to MRI or from NIST. However, each subcontractor will be
requested to bring a back-up instrument in case the primary instrument fails to operate.
NIST will be requested to ensure that their instruments are operating properly before
traveling to the testing site.
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2.2 STUDY OBJECTIVES
The study objectives for the first objective are:
1) Estimate the bias of the new XRF instruments at 0 and 1 milligrams per square
centimeter to within plus or minus 0.2 with 95% confidence, overall and to within plus
or minus 0.4 with 95% confidence on wood, metal, and plaster.
2) Estimate the precision of the new XRF instruments at 0 and 1.0 milligrams per
square centimeter to within plus or minus 3 times what was in the full study (with 95%
confidence), overall and on wood, metal, and plaster.
3) Develop an operating characteristic curve over all substrates and on wood, metal,
and plaster for each new XRF. Estimate the threshold probability and 50% point with
precision no more than three times the standard errors of similar parameter estimates
in the full study. [Note: The 50% point is defined as the lead level at which the
probability of receiving a positive indication for lead is 50%.]
4) Estimate the inconclusive region for each XRF using order statistics, overall and on
wood, metal, and plaster. Compute misclassification rates and inconclusive rates
overall and for wood, metal, and plaster substrates.
5) Estimate the bias and precision of each new XRF on the NIST SRMs and develop
control limits for usage of these instruments in the field.
6) Estimate time for a nominal reading using the standard operating protocol for each
new instrument.
7) Determine the influence of paint thickness on XRF measurements.
8) Assess the performance of auxiliary indicators of XRF performance, such as the
"absorption index" of the Niton XL.
The study objectives for the second objective are:
1) Estimate the lead in the paint in the primary XRF testing area using an average of
samples near the primary XRF testing area.
2) Investigate interpolation models for spatial variation in paint using paint chip
samples at varying distances.
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3) Characterize differences between XRF testing at one area versus XRF testing at
three areas on a sample.
The study objective for the third objective is to determine if substrate order has an
impact on XRF readings.
2.3 DATA QUALITY OBJECTIVES
[NOTE: The TCP data refers to the chemical analyses performed in the
characterization and lead-level determination of the archived test samples.]
For the TCP data generated, the data quality objectives (DQOs) for the archive phase
are the same as for the full study, as stated in Chapter 4 of the "Quality Assurance Plan for
Comparative Study of Methodologies Used to Detect Lead in Paint" (July 8, 1993).
For the archive phase, NIST Powdered Paint SRM 2582, if available, will be used in
each batch in addition to the NIST SRM 1579 used in the full study (1 per batch) and the
AIHA materials. The recovery accuracy for reference materials will remain + 25 percent.
Based on the full study data, it is anticipated laboratory split subsamples will demonstrate a
standard deviation of less than 15 percent.
The DQOs for representativeness, comparability, and completeness are relevant to
sampling activities and the layout of the archive testing room.
Efforts to obtain representativeness include the use of the exact same testing locations
identified in the field for the archive samples that were also tested in the full study. These
test locations were distinctly marked with a template as to where the XRF was to be
positioned for testing. Samples selected to be archived were taken to obtain desired levels
of lead over all substrates; however, because of the difficulty and resulting damage
associated with the removal of certain substrates, the archive consists of a limited number
of samples, such as brick and concrete.
In an effort to demonstrate correlation of the field study with the archive phase, initial
instrument testing of the archive will include, if possible, one of the exact same
instruments used in the field, a model of the Lead Analyzer manufactured by TN
Technologies. An effort is also being made to obtain the same Lead Analyzer operator as
was contracted for in the full study.
All of the paint chip sample data generated from the archive phase will be provided in
mass/mass as well as mass per area units for direct comparison to the full study data. All
XRF readings will be reported in mass per area units unless another type of unit is peculiar
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to an XRF. Where applicable, both L-shell and K-shell readings will be recorded.
Important auxiliary variables, such as the "absorption index" of the Niton XL that reflect
instrument performance will also be recorded.
As to completeness, every XRF instrument being evaluated must generate
measurements for each primary XRF test location. The total number of primary testing
locations is anticipated to be approximately 150.
As a part of the evaluation, 100% of the archive test samples must be tested by XRFs
on the bare substrate without the NIST Red Film (1.02 mg/cm2). The goal for
measurement of bare substrate with the NIST Red Film is also 100%.
Micrometer readings to determine the thickness of paint will be taken whenever
possible by measuring a paint chip.
3.0 SAMPLE COLLECTION
Sample collection will be discussed in chronological order.
The first step will be the marking of sample locations. There are three types of
samples in the archive: those marked with the full study template, those marked with the
pilot template, and those marked by a partial template from the full study.
For samples marked by the full study template (completely or partially), the second
paint chip sample will be located adjacent to the left side of the template or the top of the
template, just outside the XRF testing area. A measured area will be marked off, using
lead-free markers. Whenever possible, the measured area will be 2" by 2". The measured
area will be placed catty-corner to the primary paint chip sample, if possible. The distance
from the center of the second paint chip sample to the center of the primary paint chip
sample will be approximately 6" or 8". Records will be kept to determine which samples
have 6" samples and which have 8" samples. If circumstances dictate a different distance,
records will be kept to reflect that.
For samples marked by the pilot template, there were two paint chip samples taken
inside the template. In this case the centroid of the two initial samples will be computed.
An additional area, 2" by 2", for paint chip collection will be marked off near the primary
XRF testing area and approximately catty-corner to the centroid, but not in an area where
duct tape was previously applied. Records will be kept so the location of the three areas
for paint chip collection are known and distances between them can be computed.
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Two additional XRF testing locations will be marked on as many samples as possible.
Their centers will be located and marked at distances which are as far apart as possible,
under the constraint that newly marked locations will be on a line with the original XRF
testing area. Records will be kept of the coordinates.
After all marking has been completed, primary paint chip XRF test components will be
collected from samples for which there is no current primary paint chip sample. Bare
substrate areas for XRF testing will also be cleared for these samples. [NOTE: These bare
areas will be provided for these samples by scraping the paint from the substrate.] Extra
paint chips from the bare areas will be stored in labeled containers and saved for possible
future use. The paint chips will be stored in their recovered state, with no homogenization,
and labeled as to where collection took place by sample number and location. Records will
be kept of the size of the area from which the paint chips were collected. Collection of
secondary paint chip samples will take place after XRF testing is completed if there is a
concern over loss of samples. [NOTE: The concern is loss or deterioration of lead-based
paint from the sample surface.] If there is no such concern and if adherence to schedule is
important, secondary paint chip samples can be collected when primary paint chip samples
are collected.
The next step will be collection of XRF data.
QuanTech will develop a standard order of testing samples. The order will be random
and designed to force the operator to walk around the room during the course of testing.
The testing order will not be identical to the order the samples are mounted in the facility.
The standard collection procedure for the Lead Analyzer and the new instruments is as
follows.
Follow the manufacturer's procedures for start-up and quality control. Start each day's
testing by testing the NIST films on the control blocks, using the same procedures as used
in the full study, with the exception that only a single reading is to be made with the
3.52 mg/cm2 NIST SRM (yellow) and on a bare block. After completion of control block
testing, start testing the archive samples. Follow the order of testing samples developed by
QuanTech. At each sample, take three readings on the primary XRF paint area. Then take
three readings with the NIST 1.02 mg/cm2 red standard over the bare area. Next take one
reading over the bare area (no NIST standard). Finally take a single reading at each of the
two additional XRF areas marked as associated with that sample. This completes the
testing at the sample. Move on to the next sample and continue to test until all sample
locations in the archive have been completed.
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Take a continuing control reading every 15 samples. Take a standard set of control
readings on the last substrate tested, and then a standard set of control readings on the next
substrate to be tested. Use procedures followed in the full study for the continuing control
block readings, with the exception that only a single reading is to be taken on the yellow
NIST SRM and a bare block.
After completion of all the samples in the archive, test the "comparison set" by taking
a single nominal 15 second reading on each sample in the comparison set in the order
specified. The "comparison set" will be selected by QuanTech to test the effect of
substrate changes on XRF readings. Since the standard order will be random, the
"comparison set" order will be grouping by substrate, with a suitable ordering within
substrate groups. Comparisons will be made between the readings on the standard order
set and the "comparison set" to determine the effect of taking readings on randomly
ordered substrates and grouped substrates. Do not take continuing control readings during
"comparison set" testing unless specified in the QuanTech design.
At the end of each day's testing, take readings on the control blocks as was done in the
full study, with the exception that only a single reading is to be taken on the yellow NIST
SRM and a bare block.
See Attachment I to this addendum for an outline of the XRF testing plan that is
described above.
The Lead Analyzer would ideally be used first to test out the archive in early January
1995. The Lead Analyzer will go through the standard testing procedure described above.
The new instruments would ideally be tested next and would go through the same standard
testing procedure. One of the three older instruments would be tested if a Lead Analyzer
could not be obtained in a timely fashion.
After all XRF testing is completed, secondary paint chip samples will be collected if
not already collected. Micrometer readings to determine thickness of paint will be
collected where possible.
4.0 ANALYSES AND MEASUREMENTS
Analyses and measurements will be conducted using the methods and approaches in
Chapter 4 of the QAPjP.
NIST paint SRM 2582, if available, will be included as a QC sample in the batches for
laboratory analysis.
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5.0 DATA PROCESSING AND STATISTICAL ANALYSIS PROCEDURES
All XRF operators will be assigned a monitor who will record all data on forms. Data
will be recorded on forms developed by MRI in consultation with QuanTech and EPA.
Forms from the full study will be used where possible. Attention will be paid to recording
the correct serial number and other identifying numbers so as to be able to identify the
instrument that was tested in the archive phase.
A set of identification numbers that uniquely identify each XRF reading will be
developed. These identification numbers will be recorded by the monitors on the forms to
accurately identify each XRF reading. The XRF operators of instruments that have an
electronic data capture capability will be given instructions in the insertion of identification
codes. These codes will be designed to provide enough information to ease matching
between data on forms and electronically captured data without impending XRF testing.
All data will be double key entered as the primary quality assurance step in data
management. The data forms from the monitors will be the primary source of XRF data.
However, comparisons will be made to electronic data from the XRFs where possible.
Obvious data collection errors will be corrected. To the extent possible, examples of
listings from the instruments will be obtained prior to their use in the archive to aid
planning.
For the first study objective, statistical approaches that were used in the full study to
estimate bias and precision of XRF instruments, to estimate operating characteristic curves
and their key parameters, and to estimate bias, precision, and control limits for the NIST
SRMs will be used for the archive testing. Inconclusive regions will be estimated by order
statistics. Misclassification and inconclusive rates will be calculated. Average time of a
nominal reading will be computed, as well as other descriptive statistics of reading time.
The results of the thickness of paint [NOTE: the thickness values] from the micrometer
readings will be brought into the regression models as a covariate, and the significance of
the covariate will be estimated. Paint thickness variability in the samples will be assessed
using methods developed in the full study. Auxiliary variables will be examined by
scatterplots, correlation estimates, and, where applicable, regression approaches.
For the second study objective, averages of paint chip sample results will be computed
to serve as a more accurate baseline for testing on a sample. Ratios and differences of
secondary to primary paint chip sample results will be examined and characterized by
distributional approaches to determine if there are any unusual pairs of results. Paint chip
sample results from different distances will be compared, and interpolation approaches will
be examined in light of the new data. XRF results from testing a single area will be
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compared to XRF results from testing three areas by using approaches developed in the full
study for analyzing results from laboratory and field duplicates.
For the third objective, comparisons between readings from the standard order and the
"comparison set" will be made by scatterplots, control chart plots, non-parametric tests,
and (paired) t-tests.
6.0 AUDITS
MRI's QA unit will audit all data that is sent to QuanTech following practices that were
used in the full study.
QuanTech will identify sources of error in data and estimate the error rate from each
source using methods that were used in the full study. This includes reconciliation of
handwritten forms and electronically captured data.
EPA will audit the archive facility, the data at MRI and QuanTech, and the statistical
software at QuanTech.
7.0 REPORTS
MRI will report data from laboratory batches following practices used in the full study.
MRI will report XRF data on data collection forms to QuanTech and, if requested, to EPA
no later than six working days after collection of the data. Where applicable, MRI will
furnish to QuanTech data disks with electronically captured data from the XRF testing.
A standard analysis procedure will be set up. The archive data from the Lead Analyzer
will be used to test out the standard analysis procedure.
QuanTech will submit a report on the analysis of the data and an XRF Performance
Characteristic Sheet no later than four weeks from the receipt of the data for a particular
instrument, given that the laboratory analysis has been completed. When data from a
second instrument from the same manufacturer is received, the analysis and XRF
Performance Characteristic Sheet will be updated.
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Revision No. 1
Effective Date: December 14, 1994
8.0 REFERENCES
Quality Assurance Project Plan for the Comparative Field Study of Methodologies
Used to Detect Lead in Paint, July 8, 1994, Midwest Research Institute, EPA Contract
Number 68-DO-0137.
9.0 HEALTH AND SAFETY
Health and safety steps in Chapter 9 of the QAPjP of July 8, 1993, will be followed.
Only one XRF instrument at a time will be allowed in the archive testing facility.
Manufacturers will be required to have proper licensing of instruments completed
before testing is carried out. Operators of the instruments must have completed appropriate
safely training from the manufacturer.
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QAPjP ADDENDUM ATTACHMENT
Effective Date: December 14, 1994
QAPJP ADDENDUM ATTACHMENT I
XRF Testing Plan as Proposed in QAPjP Addendum Revision Number 1
Dated 12/14/1994
Note: A "15-sec reading" refers to a single reading from an XRF instrument following
the manufacturer's standard protocol. Based on past experience, such a reading for
new instruments is expected to be, on average, about 15 seconds in length with a fresh
source.
I. Beginning of Day Control Block Testing
1. On each of the six substrate control blocks, using order of substrates from the full
study (metal, wood, brick, drywall, concrete, and plaster):
A. One 15-sec reading with Yellow NIST Film overlay;
B. Three 15-sec readings using Red NIST Film overlay;
C. One 15-sec reading on bare substrate control block.
II. XRF Readings Per Sample Location
1. Three 15-sec readings on XI;
2. Bare Substrate Area:
A. Three 15-sec Using Red NIST Film overlay;
B. One 15-sec on Bare Substrate Area;
3. One 15-sec reading on X2;
4. One 15-sec reading on X3;
III. Continuing Control Block Check
1. Every 15 Sample Locations
A. On Substrate Control Block Type Reflective of Most Recent Location
Tested:
a. One 15-sec using Yellow NIST Film overlay;
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Effective Date: December 14, 1994
b. Three 15-sec using Red NIST Film overlay;
c. One 15-sec on bare substrate control block.
B. On Substrate Control Block Type Reflective of Next Location to be
Tested:
a. One 15-sec using Yellow NIST Film overlay;
b. Three 15-sec using Red NIST Film overlay;
c. One 15-sec on bare substrate control block.
NOTE: B is optional in situations where there is no change in substrate at the
continuing control block check.
IV. Comparison Set (30 Test Locations Grouped By Substrate)
1. Take one 15-sec reading for:
A. XI
V. End of Day Control Block Testing
1. On each of the 6 substrate control blocks, using the order from the full study
(metal, wood, brick, drywall, concrete, and plaster):
A. One 15-sec reading with Yellow NIST Film overlay;
B. Three 15-sec readings using Red NIST Film overlay;
C. One 15-sec reading on bare substrate control block.
VI. XRF data base download as necessary and hard copy review.
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QAPjP CLARIFICATIONS AND ADDITIONS
Effective Date: August 22, 1997
QAPjP CLARIFICATIONS AND ADDITIONS
Section 2.1 Definition of ICP Analysis
"ICP Analysis" refers to inductively coupled plasma atomic emission spectroscopy
(ICP-AES) analysis for lead. For archive paint samples, a method similar to the EPA
SW-846 Method 6010 was used. The method for the archive paint samples is described in
detail in Appendix G of the report "A Field Test of Lead-Based Paint Testing
Technologies: Technical Report (EPA 747-R-95-002b)."
Section 3.0 Testing Order Used After Addition of Four Additional Components to
the Archives
Four additional plaster samples were added to the sample test series after the archive
facility was built. The samples were physically added to the facility by mounting all four
on a separate board. In order to maintain the randomness of the sequential testing order,
the four additional samples were statistically "remixed" with the pool of samples and
assigned random numbers in the test series. The samples were inserted into the original
sequential order of testing by adding the letter "A" after the component number it
followed; for example, if one of the added samples came after 100, it would be given the
identification of 100A and the test sequence would become: 99, 100, 100A, 101, 102, etc.
Continuing calibration checks on the XRF instruments were performed at the normal 15-
sample intervals, except when the added plaster samples were encountered. For
consistency, the "A" samples did not count as one of the 15-samples separating the
continuing calibration checks; this allowed the QC checks to be performed after the same
samples as before the 4 plaster samples were added. At a later date, the entire archive
component series was statistically rerandomized and renumbered so that all inserted
components were fully integrated into the test sequence.
Section 4.0 Time Measurements
The time of day each component is measured by XRF test is recorded from a clock or
watch to ±1 min precision from local standard time. Actual durations of the XRF
measurement are recorded to the nearest second and are generally recorded directly from
the instrument display, if available.
Section 4.0 Performance Criteria for Temperature and Relative Humidity
Measurements
The digital meter used to record the relative humidity and temperature at the time of
the XRF test measurements is calibrated to be traceable to NIST standards within
accuracies of ±1 °C for temperature and ±5% RH for relative humidity.
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Effective Date: August 22, 1997
Section 7.0 Disk Formatting for XRF Test Data
In general, no special formatting of computer disks is required for the XRF testing.
File formats and downloading procedures vary by XRF instrument and are described on the
data forms at the time of the testing.
Section 9.0 Radiation Safety Certification of XRF Operators
Before any XRF testing is performed, the XRF operator is required to show evidence
of current certification and applicable licenses in radiation safety and the operation of XRF
test equipment.
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Appendix B
XRF Testing Protocols
Contents
General XRF Measurement Protocols [Effective date: January 10, 1995,
used during January 1995 testing of TN Lead Analyzer by a subcontractor] B-l
Clarifications and Additions to General XRF Measurement Protocols B-l5
Testing Protocols for the RMD LPA-1 [Effective date: March 1, 1995, used for
March 1995 testing by M.E. McKnight] B-16
Testing Protocols for the XL [Effective date: March 1, 1995, used for
March 1995 testing by M.E. McKnight] B-22
Testing Protocols for the Leadstar [Effective date: June 1, 1995, used for
June 1995 testing by M.E. McKnight] B-30
Supplemental Protocols for the XL: Plaster Sample Additions [Effective date:
June 9, 1995, used for June 1995 testing by M.E. McKnight] B-36
Supplemental Protocols for the LPA-1: Plaster Sample Additions [Effective date:
June 9, 1995, used for June 1995 testing by M.E. McKnight] B-39
Supplemental Protocols for the LPA-1 and XL: Control Blocks [Effective date:
June 9, 1995, used for June 1995 testing by M.E. McKnight] B-42
Testing Protocols for the LPA-1 [Effective date: July 1, 1995, for use in
July 1995 for testing by subcontractor] B-45
Testing Protocols for the Leadstar [Effective date: July 25, 1995, used for
August 1995 testing by subcontractor] B-51
Testing Protocols for the LPA-1 [Effective date: September 5, 1995, used for
September 1995 testing by NIST] B-57
Testing Protocols for the Pb Analyzer [Effective date: September 5, 1995,
used for September 1995 testing by NIST] B-65
Testing Protocols for the Warrington Microlead I [Effective date:
September 5, 1995, used for September 1995 testing by NIST] B-74
Testing Protocols for the Princeton Gama-Tech (PGT) XK-3
[Effective date: February 5, 1995, used for testing by NIST] B-82
Testing Protocols for the SCITEC MAP 4 [Effective date: February 5, 1995,
used for testing by NIST and subcontractor] B-91
Testing Protocols for the Leadstar with Software Version 4.1 or higher
[Effective date: August 9, 1996, used for August/September 1996
testing by subcontractor] B-102
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
GENERAL XRF MEASUREMENT PROTOCOLS
1.0 SUMMARY
This document describes the standard protocol for collecting XRF measurement data
on painted surfaces and corresponding substrate surfaces of the archived samples. This
document also includes instructions for recording the measurements and making quality
control (QC) measurements during this study. In general, XRF operators will be requested
to make measurements and to electronically store and download testing results according to
the manufacturer's general operating procedures. It is the responsibility of the data monitor
to record as much information as possible about the operation of each XRF instrument
participating in this study.
For purposes of this study, an XRF reading is defined as a single measurement event
that generates a single lead measurement value. Furthermore, XRF instruments are
classified into one of the following two categories:
1) XRF instruments with an operator adjustable measurement time where the reading
time, with a new source, is to be set to one of the following:
a. Reading time with a new source is to be set to 15 seconds. Fifteen
seconds is the minimum reading time to be used for this study. If the
XRF instrument cannot automatically increase this 15 second nominal
reading time as the source ages then manual reading time adjustments are
to be made taking into account the half-life of the source.
b. Reading time to be set to manufacturer's specifications as indicated in
SOP's provided by the manufacturer or set to 15 seconds, whichever is
longer.
2) XRF instruments that do not permit measurement time to be adjusted by the
operator. The reading time is to be that which is programmed by the manufacturer
into the XRF instrument.
In situations where the study protocol given herein differs dramatically from the
manufacturer's protocol, or when this study protocol cannot be followed because of
operational limitations, the XRF operator is required to discuss the situation with the field
supervisor to resolve the problems. Operators should not contact the manufacturer of the
XRF instrument unless approved by the field supervisor. Any deviations from this
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
protocol must be agreed to by the field supervisor and fully documented before
implementing the deviation. In any case, each XRF must be operated in a safe and
consistent manner throughout this study.
2.0 MATERIALS AND EQUIPMENT
• One primary and one back-up portable field XRF instrument with any extra required
supporting equipment. (To be provided by XRF contractor.)
• One set of NIST paint films (SRM 2579); contains five films of different lead
levels. (To be provided by XRF contractor.)
• Dosimeter badges; one for each XRF operator and one for each individual working
within the same room where XRF testing takes place. (Operator badges will be
provided by XRF contractor, badges for QuanTech personnel will be provided by
QuanTech, and badges for MRI personnel will be provided by MRI).
• Forms for recording data and the "Archive Testing Order" sheet; see exemplars in
this protocol. (To be provided by MRI; will be available at site.)
• Waterproof (indelible) permanent marking pen. (To be provided by MRI; will be
available at site.)
• Watch, clock, or other equivalent timepiece for reporting the testing times on the
data forms. (To be provided by MRI; will be available at site.)
• Device(s) to measure temperature and relative humidity. (To be provided by MRI;
will be available at site.)
• Bound field notebooks. (To be provided by MRI; will be available at site.)
• Pre-moistened wipes for cleaning of tools, hands, etc. (To be provided by MRI; will
be available at site.)
• Quality control (QC) blocks, each approximately 4 inch by 4 inch. The thicknesses
given are approximate: 3U inch wood (pine), 2 inch concrete (with aggregate),
lh inch drywall, 20 to 25 gauge metal, 2lh inch brick, and 1 inch plaster. (To be
provided by MRI; will be available at site)
• One 12-inch thick styrofoam block for supporting QC control blocks under
measurement. (To be provided by MRI; will be available at site.)
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
Computer equipment including an IBM compatible CPU (preferably with an INTEL
386 or 486 processor), monitor, printer and a supply of3lh inch formatted diskettes.
(To be provided by MRI; will be available at site.)
Radioactive decay tables that list the half-life of the radioactive sources used by the
XRF instruments participating in this study. (To be provided by MRI; will be
available at the site.)
3.0 MEASUREMENT PROCEDURES
The archive testing program utilizes 158 archive samples. These 158 archive samples
will be tested in random order. The same order of testing is to be used for all instruments,
for all test rounds. (With two exceptions, the order for testing has been the same for all
testing of instruments. The two exceptions are the changes resulting from adding addi-
tional plaster samples to the archive and the occurrence of a single test round with an
ordering based on grouping similar substrates. The testing based on the similar substrates
grouping has not been used for PCS development.) The marking is in the form of squares
and rectangles labeled with the letters "X" or "P" followed immediately by the numbers
"1", "2", or "3". XI is the primary painted XRF testing location, X2 and X3 are secondary
painted testing locations. PI is a secondary testing location that has been scraped of its
paint.
All testing should be accomplished in a two day period. If in the event that testing is
not completed after the second day, perform the testing protocol on the third day as
described for day two. XRF testing on the archived samples can be summarized into the
following:
• INITIAL control measurements, as described in Section 3.3.
• STANDARD measurements as described in Section 3.4.
• CONTINUING control measurements as described in Section 3.5.
• COMPARISON SET measurements as described in Section 3.6.
• ENDING control measurements as described in Section 3.3.
The two day general work plan is given below.
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
Day 1 General Work Plan:
1. Receive beginning-of-day instructions from field supervisor as described in
Section 3.1.
2. Perform manufacturer's initial calibration checks. Perform additional
manufacturer's calibration checks at intervals as required by the manufacturer's
specifications. Both are discussed in Section 3.2.
3. Perform initial control block measurements on all six blocks as described in
Section 3.3. Record temperature and humidity data.
4. Perform standard set measurements as described in Section 3.4.
5. After the completion of the first fifteen archive samples, and following every
fifteen archive sample thereafter, perform continuing control readings on the two
control blocks with the same substrates as the last and next substrates tested as
described in Section 3.5.
6. Record temperature and humidity data approximately half-way through the day.
7. At various times during the day, record in the field notebook the time required by
the XRF instrument to actually display the lead measurement result. The data
recorded during the day for this purpose should include the start and end times for
twenty measurements. A start time is the time of day when the XRF probe face-
plate is placed on the surface to be tested and testing commences. The end time is
the time of day when the result is displayed on the XRF readout area. These data
should be collected for each reading time.
8. At the end of the first day of testing, perform ending control block measurements
on all six blocks as described in Section 3.3. Record temperature and humidity
data.
9. Perform end-of-day activities as described in Section 3.7 which includes review of
data forms for completeness, downloading electronically stored data, and
transferring data forms to the field supervisor.
Day 2 General Work Plan:
10. At the start of the second day, receive beginning-of-day instructions from field
supervisor as described in Section 3.2.
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
11. Perform manufacturer's initial calibration checks. Perform additional
manufacturer's calibration checks at intervals as required by the manufacturer's
specifications. Both are discussed in Section 3.2.
12. Perform initial control block measurements on all six blocks as described in
Section 3.3. Record temperature and humidity data.
13. Perform the standard measurements (Section 3.4) not completed on the previous
day of testing. Begin with the testing location immediately following the last
tested location from the day before.
14. Record temperature and humidity data approximately half-way through the day.
15. After the completion of the first fifteen archive samples on this day, and following
every fifteen archive sample thereafter, perform continuing control readings on the
two control blocks with the same substrates as the last and next substrates tested
as described in Section 3.5.
16. Upon completion of all 154 standard testing locations, re-test the locations as
described in Section 3.6. This testing is known as the "comparison set" testing.
17. At every change of substrate, perform continuing control measurements on the
two control blocks with the same substrate as the last and next substrate tested as
described in Section 3.5.
18. At the end of this day of testing, perform ending control block measurements on
all six blocks. Record temperature and humidity data as described in Section 3.3.
19. Perform end-of-day activities as described in Section 3.7 which includes review of
data forms for completeness, download electronically stored data, and transfer
data forms to the field supervisor.
3.1 INITIAL XRF TESTING PROCEDURE
XRF operators and monitors will receive detailed overview instructions from the field
supervisor on the first day of XRF testing that will include the following topics:
General safety instructions.
Definitions of testing locations, measurements, testing time, and types of data.
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
• Completion of the "Archive XRF Instrument Information" form.
• Specific site issues and description of marked locations and what markings signify.
• Order of performing measurements.
• Use of each data form and placement of data on forms.
• Responsibilities of the XRF operator to inform the field supervisor when the
determination of the duration of the reading time is being made.
• Responsibilities of the XRF operator to enter all information necessary for the
electronic storage of testing results.
• Responsibilities of the XRF operator to call out all readings real-time.
• Responsibilities of the monitor to record information about the manufacturer's
calibration or warm-up protocols in the field notebooks.
• Responsibilities of the monitor to record all data real-time and use verbal feedback
to verify data. (No reading is to be discarded; however additional data can be taken
if insisted on by the XRF operator. Additional readings should be recorded in the
"Comments" column of the appropriate form.)
• Responsibilities of the monitor to periodically observe the actual instrument
readout (particularly for recording both K- and L-shell readings). The monitor
should observe about 10% of the readings and should place a check mark on the
data form next to each observed reading.
• Responsibilities of the monitor to record temperature and humidity data in the field
notebook three times a day.
3.2 BEGINNING OF EACH DAY ON-SITE PROCEDURES
The XRF operator and monitor will receive initial instructions from the acting field
supervisor at the beginning of each testing day. Items will generally include a brief
overview of those listed under Section 3.1 plus any additional items that are dictated by
variable field conditions.
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
At the beginning of each day, the XRF operator will perform tests and instrument
checks that are required by the manufacturer of the XRF to prepare the instrument for
taking lead measurements. The operator is to enter "99999" into the XRF instrument for
the location identification during these procedures. The XRF operator must inform the
monitor that a manufacturer-recommended procedure is being performed and the nature of
the procedure.
The monitor will record the time and nature of all such manufacturer-recommended
procedures in the field notebook. This information should include but not be limited to: 1)
what is being done, 2) the displayed result if any, and 3) the consequence, representation,
or definition of the result. The monitor will also record temperature and humidity data in
the field notebook.
3.3 CONTROL BLOCK READINGS — BEGINNING AND ENDING
At the beginning and end of each day, each XRF operator will perform a set of
measurements on control blocks covered separately with two NIST SRM 2579 standards
(red, 1.02 mg/cm2; and yellow, 3.53 mg/cm2) and without any NIST film covering. These
QC readings will be taken on six substrate blocks: metal, wood, brick, drywall, concrete,
and plaster. Before the start of each testing day five readings will be taken on each control
block. The first reading will be taken through a yellow NIST (3.53 mg/cm2) film covering,
followed by three readings taken through a red NIST (1.02 mg/cm2) film covering,
followed by one reading taken without any NIST film covering. This same procedure will
be repeated at the end of the day. Data from these beginning and end control readings will
be recorded on the "ARCHIVE XRF TESTING DATA - CONTROL READINGS" form.
A step-by-step description is provided below:
At the beginning of each testing day, perform the following procedures:
1. For each new "ARCHIVE XRF TESTING DATA - CONTROL READINGS"
form needed, the monitor will complete the header of the form. Be sure to
indicate in the appropriate space if the beginning control block measurements
precede STANDARD set or COMPARISON set readings. Likewise, indicate in
the appropriate space if the ending control block measurements follow
STANDARD set or COMPARISON set readings.
2. If not already done, perform whatever normal instrument checks are required by
the XRF manufacturer to prepare the instrument for taking lead measurements.
The entered location identification number for these readings should be "99999".
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
The XRF operator will inform the monitor what the procedure is and why it is
being done. The monitor will write this information in the field notebook.
For each control block, the monitor will fill in the "QC Type", "Block Type",
"Time of Measurement," and "XRF Shell" columns. The location identification
will be a two character code: a number and a letter. For the beginning of the day
control block readings, the number will always be "1". The letter depends on the
substrate of the control block and is the block type code shown in the table below.
XRF instruments incapable of storing alpha characters should use the number
codes given in the table below.
CONTROL
BLOCK TYPE
metal
wood
brick
drywall
concrete
plaster
BLOCK
TYPE CODE
M
W
B
D
C
P
NUMBER
CODE
1
2
3
4
5
6
4. Perform control block measurements for all six control blocks using the procedure
outlined below.
a. Perform the measurements on the control blocks in the following
substrate order: metal, wood, brick, drywall, concrete, and plaster.
b. Place the control block within the marked area on the styrofoam support.
c. Enter into the XRF instrument the location identification information, as
described above.
d. Center the yellow NIST film on each control block. Take one reading by
placing the XRF probe face-plate on the NIST film and taking readings
through the NIST film into the center of the control block. The XRF
operator will call out the reading(s) from the instrument's display. The
monitor will record each reading on the "ARCHIVE XRF TEST DATA -
- CONTROL READINGS" form, verbally verifying the value written.
e. Repeat this procedure with the red NIST film and take three readings.
When the three readings are being taken, any movement of the XRF
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
probe face-plate should be avoided so that the three readings are taken on
the same exact spot.
f Repeat this procedure on bare substrate. Place the XRF probe face-plate
on the control block without any NIST film covering and take one
reading into the center of the control block.
g. The monitor will record any other information in the "Comments" column
as necessary.
At the end of the testing day perform all of the above control measurements exactly as
they were performed at the beginning of the day with one exception: the first character of
the two character identification code to be entered into the XRF instrument and to be
recorded on the form is the number "3" for control block readings taken at the end of the
day.
3.4 PROCEDURE FOR STANDARD MEASUREMENTS AT EACH TESTING
LOCATION
On each archive sample, standard measurements are to be taken. The order in which
standard measurements are to be taken is the sequential order of the numbers on the white
cards located in the plastic sleeve near each archive sample. The monitor may use the
"Archive Testing Order Sheet" to locate archive samples. Standard measurements consist
of nine XRF readings and are summarized as follows:
• One XRF reading taken on the painted surface of the primary area labeled XI.
• One XRF reading on the bare substrate area covered with the red NIST standard
(1.02 mg/cm2) labeled PI.
• One XRF reading taken on the surface of the bare substrate area without any NIST
standard covering labeled PI.
• One XRF reading taken on the surface of the area labeled X2. Note that on a few
archive samples, the X2 area is not present.
• One XRF reading taken on the surface of the area labeled X3. Similar to above, on
a few archive samples, the X3 area is not present.
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
A step-by-step description of taking standard set XRF measurements follows:
1. For each new "ARCHIVE XRF TEST DATA - STANDARD READINGS" form
needed, the monitor will complete the header of the form.
2. For each archive sample, the monitor will record the testing location identification
number located on the white card in the "Location ID" column on the "ARCHIVE
XRF TEST DATA - STANDARD READINGS" and record the "Time of
Measurement" and "XRF Shell". The XRF operator will enter the white card
location identification number into the instrument.
3. Perform measurements on the painted and bare substrate surfaces as follows:
a. Take one reading on the painted surface marked as XI. The three
readings should be taken on the same exact spot, so any movement of the
XRF probe face-plate should be avoided when taking these readings.
The XRF operator will call out the reading(s) from the instrument's
display. The monitor will record each reading on the "ARCHIVE XRF
TEST DATA - STANDARD READINGS," verbally verifying the value
written. The monitor will also record other information in the
"Comments" column as necessary.
b. Take one reading on the bare substrate surface covered with the
1.02 mg/cm2 NIST standard red film at the testing location labeled PI.
This area is adjacent to the XI testing area described above and has
approximate dimensions of either four inches by four inches or four
inches by two inches. The three readings should be taken on the same
exact spot, so any movement of the XRF probe face-plate should be
avoided when taking these readings. If difficulties are encountered
holding the NIST film against the substrate surface, use a small piece of
masking tape to hold it in place. Be sure the tape is placed such that it
adheres only to areas outside the marked location. The XRF operator
will call out the reading(s) from the instrument's display. The monitor
will write each reading value on the "ARCHIVE XRF TEST DATA -
STANDARD READINGS," verbally verifying the value written. The
monitor will record any other information in the "Comments" column as
necessary.
c. Take one reading on the bare substrate surface without any NIST film
covering. The XRF operator will call out the reading(s) from the
instrument's display. The monitor will write each reading value on the
"ARCHIVE XRF TEST DATA - STANDARD READINGS," verbally
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
verifying the value written. The monitor will record any other
information in the "Comments" column as necessary.
d. Take one reading at the painted surface marked as X2. The XRF
operator will call out the reading(s). The monitor will write this value on
the "ARCHIVE XRF TEST DATA - STANDARD READINGS,"
verbally verifying the value written. The monitor will record any other
information in the "Comments" column as necessary. Note that in a
small number of cases, the X2 area will not be present.
e. Take one reading at the painted surface marked as X3. The XRF
operator will call out the reading(s). The monitor will write this value on
the "ARCHIVE XRF TEST DATA - STANDARD READINGS,"
verbally verifying the value written. The monitor will record any other
information in the "Comments" column as necessary. Like the X2 area,
the X3 area will not be present on every archive sample.
4. Continuing control readings are performed after every fifteenth archive sample as
outlined in Section 3.5.
3.5 PROCEDURES FOR CONTINUING CONTROL READINGS
Two sets of continuing control readings are performed after every fifteenth archive
sample for standard readings and at every substrate change when taking "comparison set"
readings. The procedure for continuing control readings is the same for either standard
testing or "comparison set" testing. The first set of continuing control readings is
performed on the control block that is composed of similar material as the last archive
sample tested. The second set of continuing control readings is performed on the control
block that is composed of similar material as the next archive sample to be tested. For
each set of control readings, use the following steps:
1. For each new "ARCHIVE XRF TESTING DATA -- CONTROL READINGS"
form needed, the monitor will complete the header of the form. Be sure to
indicate in the appropriate space if these are STANDARD or COMPARISON
control readings.
2. For each control block, the monitor will fill in the "QC Type", "Block Type",
"Time of Measurement," and "XRF Shell" columns and the XRF operator will
enter the location identification into the instrument. The location identification
will be a two character code: a number and a letter. For continuing control block
readings the number will always be "2". The second character, a letter, depends
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
on the substrate of the control block and is the block type code shown in the table
below. XRF instruments incapable of storing alpha characters should use the
number codes given in the table below.
CONTROL
BLOCK TYPE
metal
wood
brick
drywall
concrete
plaster
BLOCK
TYPE CODE
M
W
B
D
C
P
NUMBER
CODE
1
2
3
4
5
6
3. Take the continuing control readings using two NIST films and the bare control
block without any NIST film covering as follows:
a. Place the control block within the marked area on the styrofoam support
block.
b. Center the yellow NIST film on the control block. Take one reading
through the NIST film and into the center of the control block.
c. Repeat the procedure using the red NIST film and take three readings.
The three readings should be taken on the same exact spot, so any
movement of the XRF probe face-plate should be avoided when taking
these readings.
d. Take one reading on the bare control block without any NIST covering.
The XRF operator will call out the reading(s) from the instrument's
display. The monitor will write each reading on the "ARCHIVE XRF
TEST DATA - CONTROL READINGS" form, verbally verifying the
value written. The monitor will record any other information in the
"Comments" column as necessary.
3.6 PROCEDURE FOR COMPARISON SET READINGS
After completion of all the archive samples in the standard set, XRF testing of the
"comparison set" follows. Comparison set readings are to be taken on all 158 archive
samples. The comparison set is ordered such that the archive samples are grouped by
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
substrate in the following order: metal, wood, brick, drywall, concrete, and plaster. The
monitor should exchange the relative positions of the white and pink cards located in the
plastic sleeve near each archive sample so that the pink card is visible prior to comparison
set testing. Comparison set readings are to be taken in the sequential order of the numbers
on the pink cards. The monitor may use the "Archive Testing Order Sheet" to locate
archive samples. Comparison set readings are taken on the surface of the area labeled XI;
readings are not taken at any of the other marked areas. At each testing location labeled XI
perform the following steps:
1. For each new "ARCHIVE XRF TEST DATA -- COMPARISON READINGS"
form needed, the monitor will complete the header of the form.
2. For each archive sample, the monitor will record the pink card location
identification number in the "Location ID" column on the "ARCHIVE XRF TEST
DATA - COMPARISON READINGS" and will also record the "Time of
Measurement" and the "XRF Shell". The XRF operator will enter the pink card
location identification number into the XRF instrument.
3. The XRF operator will take one XRF reading on the painted surface of the area
labeled XI and call out the reading(s) from the instrument's display. The monitor
will write each reading value on the "ARCHIVE XRF TEST DATA -
COMPARISON READINGS," verbally verifying the value written. The monitor
will record other information in the "Comments" column as necessary.
4. Continuing control readings are performed at every substrate change as described
in Section 3.5. Five different pairs of continuing control measurements will be
made during XRF testing of the comparison set.
Note: This "comparison set" with substrate-by-substrate ordering was used once during
the course of archive testing and was subsequently dropped from future testing, as
testing with random ordering met the primary goals of the project.
3.7 END-OF-DAY ACTIVITIES
The XRF operator and monitor will ascertain that all form headers are completed,
including the appropriate page numbering so that the forms of the same type are
numbered in chronological order for that day of testing only, starting with page 1.
The last page number should also be written on every page.
• XRF operator and monitor will verify that all required XRF readings were taken at
each testing location as specified in this protocol. Verification will be performed
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GENERAL XRF MEASUREMENT PROTOCOLS
Effective date: January 10, 1995
Used during January 1995 testing of TN Lead Analyzer by a subcontractor
by reviewing the data forms and checking the appropriate box in the "Archive End
of Day Data Checklist" form.
The XRF operator will download (transfer) electronically stored data and purge
the data that is currently stored in the instrument after the download is completed.
The electronically stored data should be downloaded at the test site to the 3lh inch
diskettes and backup copies on a second set of diskettes should be made. The
computer equipment provided at the site may be used for this purpose. The
monitor should verify that the download was successful prior to instructing the
XRF operator to purge the data stored in the XRF instrument. The monitor will
record the procedure used to download and purge the electronically stored data in
the field notebook.
XRF data forms will be transferred to the acting field supervisor at the end of each
day. The acting field supervisor will check the data forms for completeness and
conduct other end-of-day activities before releasing workers for the day.
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CLARIFICATIONS AND ADDITIONS TO GENERAL
XRF MEASUREMENT PROTOCOLS
Effective Date: May 17, 1996
CLARIFICATIONS AND ADDITIONS TO GENERAL
XRF MEASUREMENT PROTOCOLS
Section 3.0 Order of Testing
Sample testing on the archived lead-based painted components is performed in the
same sequence for all testing rounds and for all XRF instruments. Briefly, the testing order
was established by random spatial distribution of the samples throughout the facility and by
predetermining a random test sequence by random number generation from all substrate
types and lead concentration levels.
Section 3.1 Reading Verifications by Monitor
For any situation in which the monitor's reading differs from the operator's reading, the
testing will be temporarily stopped until the cause of the discrepancy is determined and the
actions taken will be noted on the data collection forms.
With the following exception, the sequence order is the same for all XRF testing. Four
additional plaster samples were added to the sample test series after the archive facility was
built. The samples were physically added to the facility by mounting all four on a separate
board. In order to maintain the randomness of the sequential testing order, the four
additional samples were statistically "remixed" with the pool of samples and assigned
random numbers in the test series. The samples were inserted into the original sequential
order of testing by adding the letter "A" after the component number it followed; for
example, if one of the added samples came after 100, it would be given the identification of
100A and the test sequence would become: 99, 100, 100A, 101, 102, etc. Continuing
calibration checks on the XRF instruments were performed at the normal 15 sample
intervals, except when the added plaster samples were encountered. For consistency, the
"A" samples did not count as one of the 15 samples separating the continuing calibration
checks; this allowed the QC checks to be performed after the same samples as before the 4
plaster samples were added.
Section 3.6 Comparison Set Readings
The procedure indicated in Section 3.6 was discontinued early in the program and
replaced with a single unified ordering system.
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TESTING PROTOCOLS FOR THE RMD LPA-1
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
TESTING PROTOCOLS FOR THE LPA-1
General Responsibilities
The XRF Operator will:
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
• Download data to a computer and verify that the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed
during testing.
The Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help assure the protocols are followed.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Assure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI,
NIST, and QuanTech.
• Assure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Complete a new set of SAMPLE LOCATION CONDITION forms for:
a. Sample locations previously identified as being in poor condition which
already have completed records from the early spring 1995 testing.
b. Any additional sample locations that are observed to be in poor condition.
• Provide the following forms:
• Testing order list • Sample location condition
• Standard readings • Control readings
• Archive XRF information • Source age adjustment table
B-16
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TESTING PROTOCOLS FOR THE RMD LPA-1
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR RMD
Perform warmup
and self-calbratlon
Complete new
INFORMATION
form
Perform BOD QC
Checks (all six
substrates)
Instructions to include: safety issues, field form use, archive
layout and testing order, Sample ID numbering for electronic
data capture, and voice-call back verification of data
recording by monitor.
See form for needed information.
1. Enter date and time.
2. Allow to warmup at least 20 minutes to assure that the
auto self-calibration occurs (automatically done every
15 minutes).
3. Perform calibration check using STD Mode set to 20
seconds: Test both bare and painted sides of factory
supplied wood substrate. Record results on
INFORMATION form.
4. Set Quick Mode Testing using an action level of 1.0
mg/cm2.
BOD (or EOD) QC checks: test a total of 6 pre-placed
blocks on a minimum of 12 inches of styrofoam support.
Please do not move blocks.
For each block, using a 20-sec STD Mode reading, test in
the following order:
a. 1 reading, yellow NIST on block
b. 1 reading, red NIST on block
c. 1 reading, no NIST on block
Record the data on the CONTROL READINGS form (RMD).
If possible key In ID code as Indicated on the form for
electronic data capture.
B-17
-------
TESTING PROTOCOLS FOR THE RMD LPA-1
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR RMD
Move to first or
next location and
take readings
(follow TESTING
ORDER list)
the\. Yes
n r^y ^-, •,
verT?^^
Record temp &
humidity data
the
testing day
within 30 minutes
of the end?
Stop testing, record
temp & humidity
data, perform the
EOD QC Checks
HAVE 15
locations been
tested since
lastQC
heck
Perform
continuing QC
checks
Test all of the samples at each testing location first in
the Quick mode, then repeat using the STD Mode set
to 20 seconds.
For each testing location, In each mode, test In the
following order:
a. 1 reading, on X1
b. 1 reading, on bare (P1) + red NIST
c. 1 reading, on bare (P1)
d. 1 reading, on X2
e. 1 reading, on X3.
Record data on the STANDARD READINGS form
(RMD).
Periodically measure the time required to take a
reading from start to data display and record It In the
field notebook.
EOD QC checks are the same as BOD QC checks:
follow same procedure as for BOD QC Checks.
Record temp and humidity in a field notebook.
Download any electronically stored data, verify
successful transfer before clearing the memory to
make room for more data.
Start next day at top of flow chart using the next
sample to be tested as the first location.
Continuing QC checks, total of 2 blocks tested on a
minimum of 12 inches styrofoam support. Use blocks
matching same type as the last and next locations (If
same type for both, test same block twice).
Follow same testing order and reading times as that
used for BOD testing.
Record on CONTROL READINGS form (RMD). If
possible, key in ID code as indicated on the form for
electronic data capture for these readings.
B-18
-------
TESTING PROTOCOLS FOR THE RMD LPA-1
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
Archive XRF Instrument Information
Date
Testing Site
Testing Dates
Contractor
Manufacturer
Model No.
Serial No.
XRF Operator (Printed name)
XRF Operator (Signature)
Source Material _
Source Serial No.
Source Age or Date
Detector Type
Operating Parameters Used
Open shutter sampling time? (fixed or variable)
If fixed, what Is the duration time?
Dally warm-up and calibration check used? (Briefly discuss)
Regulatory level value used for setting the XRF Instrument? (Yes or No)
If yes, enter the value used
Other XRF parameters under operator control used? (Briefly discuss)
| | Check here to hdlcate the presence of additional comments on the back of this form.
B-19
-------
TESTING PROTOCOLS FOR THE RMD LPA-1
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
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B-20
-------
TESTING PROTOCOLS FOR THE RMD LPA-1
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
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B-21
-------
TESTING PROTOCOLS FOR THE XL
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
TESTING PROTOCOLS FOR THE XL
General Responsibilities
The XRF Operator will:
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
• Download data to a computer and verify that the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed
during testing.
The Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help assure the protocols are followed.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Assure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI,
NIST, and QuanTech.
• Assure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Complete a new set of SAMPLE LOCATION CONDITION forms for:
a. Sample locations previously identified as being in poor condition which
already have completed records from the early spring 1995 testing.
b. Any additional sample locations that are observed to be in poor condition.
• Provide the following forms:
• Testing order list • Sample location condition
• Standard readings • Control readings
• Archive XRF information • Source age adjustment table
B-22
-------
TESTING PROTOCOLS FOR THE XL
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR NITON
Beginning of Day
(BOD) Instruction
Perform warmup
and self-calibration
Complete new
INFORMATION
form
Perform BOD QC
Checks (all six
substrates)
Instructions to include: safety issues, field form use, archive
layout and testing order, Sample ID numbering for electronic
data capture, and voice-call back verification of data
recording by monitor.
See form for needed information.
1. Perform self-calibration.
2. Allow to warm-up for 20 minutes.
3. Perform self-calibration - perform every 4 hours. Record
any results on the XRF INSTRUMENT INFORMATION
form.
4. Perform calibration check using a 20 second reading
(2nd beep):
Test both sides on the supplied 5 standard films against
wood substrate.
IF lead value is outside displayed window by greater than
10% or 0.1 mg/cm2 (whichever is higher),
THEN, repeat calibration check using a 1 minute check,
IF OK, then go back to step 2.
IF not, contact THE SUPERVISOR TO ADVISE.
BOD (or EOD) QC checks: test a total of 6 pre-placed
blocks on a minimum of 12 Inches of styrofoam support.
Please do not move blocks.
For each block, using a 20-sec mode, test in the following
order:
a. 1 reading, yellow NIST on block
b. 1 reading, red NIST on bbck
c. 1 reading, no NIST on block
Record the data on the CONTROL READINGS form
(NITON). If possible key In ID code as Indicated on the form
for electronic data capture.
B-23
-------
TESTING PROTOCOLS FOR THE XL
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR NITON
Move to first or
next location and
take readings
(follow TESTING
ORDER list)
HAV
4 hours
passed since
last self-
calibration ?
Perform self-
calibration of
Instrument
the
testing day
If over ??
Record temp &
humidity data
Stop testing, record
temp & humidity
data, perform the
EOD QC Checks
within 30 minutes
HAVE1
locations been
tested since
lastQC
heck
Perform
continuing QC
checks
For each testing location, using 20-second mode test
In the following order:
a. 1 reading, on X1
b. 1 reading, on bare (P1) + red NIST
c. 1 reading, on bare (P1)
d. 1 reading, on X2
e. 1 reading, on X3.
Record data on the STANDARD READINGS form.
For first testing day, at least, determine using X1 data,
whether a longer testing time is needed based on the
attached NITON truth table. If Indicated, collect a 120
second reading on X1 after completion of a-e using
the 20 second mode.
Periodically measure the time required to take a
reading from start to data display, and record it in the
field notebook.
EOD QC checks are the same as BOD QC checks:
follow same procedure as for BOD QC Checks.
Record temp and humidity In a field notebook.
Download any electronically stored data, verify
successful transfer before clearing the memory to
make room for more data.
Start next day at top of flow chart using the next
sample to be tested as the first location.
Continuing QC checks, total of 2 blocks tested on a
minimum of 12 Inches styrofoam support. Use blocks
matching same type as the last and next locations (If
same type for both, test same block twice).
Follow same testing order and reading times as that
used for BOD testing.
Record on CONTROL READINGS form (NITON). If
possible key In ID codes as Indicated on the form for
electronic data capture for these readings.
B-24
-------
TESTING PROTOCOLS FOR THE XL
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
NITON TRUTH TABLES FOR DETERMINATION OF LONGER TESTING TIMES
Summarized from NITON operating procedures update dated 12/21/94
DEFINITION OF DISPLAYED LEAD RESULTS:
L Interval H 1 h
x-u
x+u
K interval -f-
KL
Ku
where: x = mean L shell result
u = L shell uncertainty
KL = K shell lower result
Ku = K shell upper result
DECISION FLOWCHART (version A):
TestXI using
maximum reading
time (approx 120-
sec).
B-25
-------
TESTING PROTOCOLS FOR THE XL
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
DECISION FLOWCHART (version B):
TestXI using
maximum reading
time(approx 120-
sec).
Do not test using
longer time.
NOTE: Truth tables are based on supplemental documentation received from NITON
(12/21/94). Testing duration decisions based on the depth index were missing
from the supplemental documentation. However, decisions based on the depth
index were the only clearly identified directive in the XL manual. Therefore, this
conditional branch was included into the truth table flow-charts. Differences
between truth table versions reflect only the placement of this depth index check
within the flow-chart. All samples were tested using version B.
B-26
-------
TESTING PROTOCOLS FOR THE XL
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
Archive XRF Instrument Information
Date
Testing Site
Testing Dates
Contractor
Manufacturer
Model No.
Serial No.
XRF Operator (Printed name)
XRF Operator (Signature)
Source Material _
Source Serial No.
Source Age or Date
Detector Type
Operating Parameters Used
Open shutter sampling time? (fixed or variable)
If fixed, what Is the duration time?
Dally warm-up and calibration check used? (Briefly discuss)
Regulatory level value used for setting the XRF Instrument? (Yes or No)
If yes, enter the value used
Other XRF parameters under operator control used? (Briefly discuss)
| | Check here to hdlcate the presence of additional comments on the back of this form.
B-27
-------
TESTING PROTOCOLS FOR THE XL
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
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B-28
-------
TESTING PROTOCOLS FOR THE XL
Effective Date: March 1, 1995
Used for March 1995 testing by M.E. McKnight
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B-29
-------
TESTING PROTOCOLS FOR THE LEADSTAR
Effective date: June 1, 1995
Used for June 1995 testing by M.E. McKnight
TESTING PROTOCOLS FOR THE LEADSTAR
General Responsibilities
The XRF Operator will:
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
• Download data to a computer and verify that the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed
during testing.
The Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help assure the protocols are followed.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Assure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI,
NIST, and QuanTech.
• Assure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Complete a new set of SAMPLE LOCATION CONDITION forms for:
a. Sample locations previously identified as being in poor condition which
already have completed records from the early spring 1995 testing.
b. Any additional sample locations that are observed to be in poor condition.
• Provide the following forms:
• Testing order list • Sample location condition
• Standard readings • Control readings
• Archive XRF information* Source age adjustment table
B-30
-------
TESTING PROTOCOLS FOR THE LEADSTAR
Effective date: June 1, 1995
Used for June 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR XSIRIUS
Perform warmup
and self-calibration
Record temp &
humidity data
Complete new
INFORMATION
form
Perform BOD QC
Checks (all six
substrates)
Instructions to include: safety issues, field form use, archive
layout and testing order, Sample ID numbering for electronic
data capture, voice-call back verification of data recording by
monitor, a blank display for negative lead results, and the
use of a 30-sec reading adjusted for source age.
See form for needed information.
1. Allow to warm-up for 5 minutes.
2. Enter or verify:
a. the selected file names to store the data
b. the action level Is set to 1.0 mg/cm2
c. any other user entered parameters.
3. Perform self-calibration as per the manual and
manufacturer training directives using the manufacturer
supplied calibration sample(s).
Summarize any user entered Information and the
calibration procedure on the Instrument INFORMATION
form.
BOD (or EOD) QC checks: test a total of 6 pre-placed
blocks on a minimum of 12 inches of styrofoam support.
Please do not move blocks.
For each block, using a nominal 15-sec reading, test In the
following order:
a. 1 reading, yellow NISI on block
b. 1 reading, red NIST on block. IF the block is wood,
THEN collect 2 more readings using the red NIST on
the block. Record extra readings on subsequent lines
of the data form placing a diagonal line through the
unused yellow and no NIST data blocks.
c. 1 reading, no NIST on block
Before moving to the next control block repeat a-c above
using a nominal 30-sec reading adjusted for source age.
Record the data on the CONTROL READINGS form.
B-31
-------
TESTING PROTOCOLS FOR THE LEADSTAR
Effective date: June 1, 1995
Used for June 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FORXSIRIUS
Move to first or
next location and
take readings
(follow TESTING
ORDER list)
thefblbwhg
rred skice th
lastser-cafcratb
Perform self-
calibration and
verification
XRF on standby /
> 30 mlns ? /
4 hours past V
XRF shut/
off?,/
the
testing day
If over
Record temp &
humidity data
the
testing day \ Yes
within 30 minutes
of the end?
Stop testing, record
temp & humidity
data, perform the
EOD QC Checks
HAVE 15
locations been
tested since
lastQC
heck?
Perform
continuing QC
checks
For each testing location, using a nominal 15-sec
reading, test In the following order:
a. 1 reading, on X1
b. 1 reading, on bare (P1) + red NIST
c. 1 reading, on bare (P1)
d. 1 reading, on X2
e. 1 reading, on X3.
Record data on the STANDARD READINGS form.
IF during any of the a-e testing above, the density is
£ 4 THEN:
- complete all a-e testing using the nominal
15-sec reading time
- Change the testing mode to a nominal 30-sec
reading adjusted for source age and repeat
a-e testing above recording the data on the
STANDARD READINGS form using a new row.
1. IF XRF off, allow to warmup for 5 minutes.
2. Enter or verify:
a. the selected file names to store the data
b. the action level is set to 1.0 mg/cm2
c. any other user entered parameters.
3. Perform self-calibration as per the manual and
manufacturer training directives using the
manufacturer supplied calibration sample(s).
Summarize changes to any user entered
Information on the Instrument INFORMATION form.
EOD QC checks are the same as BOD QC checks:
follow same procedure as for BOD QC Checks.
Record temp and humidity in a field notebook.
Download any electronically stored data, verify
successful transfer before clearing the memory to
make room for more data.
Start next day at top of flow chart using the next
sample to be tested as the first location.
Continuing QC checks, total of 2 blocks tested on a
minimum of 12 inches styrofoam support. Use blocks
matching same type as the last and next locations (if
same type for both, test same block twice).
Follow same testing order and reading times as that
used for BOD testing (I.e.: First, use the nominal
15-sec reading for testing a-c. Second, before
moving to the next control block, repeat a-c testing
using a nominal 30-sec reading.)
B-32
-------
TESTING PROTOCOLS FOR THE LEADSTAR
Effective date: June 1, 1995
Used for June 1995 testing by M.E. McKnight
Archive XRF Instrument Information
Date Testing Site.
Contractor Manufacturer.
Model No. Serial No.
XRF Operator (Printed name)
XRF Field Monitor (Printed name)
Source Material Source Age or Date
Source Serial No. Detector Type
Operating Parameters Used
Open shutter sampling tlme(s)? (fixed or variable)
If fixed, what Is the duration tlme(s)?
Dally warm-up and calibration check used? (Briefly discuss)
Regulatory level value used for setting the XRF Instrument? (Yes or No)
If yes, enter the value used
Other
Data File Names and Descriptions
| | Check here to hdlcate the presence of additional comments on the back of this form.
B-33
-------
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TESTING PROTOCOLS FOR THE LEADSTAR
Effective date: June 1, 1995
Used for June 1995 testing by M.E. McKnight
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B-34
-------
TESTING PROTOCOLS FOR THE LEADSTAR
Effective date: June 1, 1995
Used for June 1995 testing by M.E. McKnight
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B-35
-------
SUPPLEMENTAL PROTOCOLS FOR THE XL
Effective date: June 9, 1995
Used for June 1995 testing by M.E. McKnight
al. Wood
a2. Plaster
b. Sample 155
SUPPLEMENTAL PROTOCOLS FOR THE XL: PLASTER SAMPLE ADDITIONS
The following protocols are to be used for testing of plaster samples additions assigned
to testing ID positions of 155-158.
NOTE: Record data on relevant data forms (see attached).
1. Warmup for 20 minutes.
2. Calibration checks, using 20-second mode, test both sides of factory samples (5). If
value differs by 10% or 0.1 (whichever is greater, then go back to 1). Record results
on back of data form.
3. Testing (Use 20-second mode for QCs, follow truth table for samples)
a. QC-Control Blocks:
3-red over bare
3-bare
3-red over bare
3-bare
1-X1
1-red over bare
1-bare
1-X2
1-X3
1-X1
1-red over bare
1-bare
1-X2
1-X1
1-red over bare
1-bare
1-X2
1-X3
1-X1
1-red over bare
1-bare
1-X2
1-X3
c. Sample 156
d. Sample 157
e. Sample 158
QC-Control Blocks
al. Plaster
a2. Wood
3-red over bare
3-bare
3-red over bare
3-bare
B-36
-------
SUPPLEMENTAL PROTOCOLS FOR THE XL
Effective date: June 9, 1995
Used for June 1995 testing by M.E. McKnight
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B-37
-------
SUPPLEMENTAL PROTOCOLS FOR THE XL
Effective date: June 9, 1995
Used for June 1995 testing by M.E. McKnight
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B-38
-------
SUPPLEMENTAL PROTOCOLS FOR THE LPA-1
Effective Date: June 9, 1995
Used for June 1995 testing by M.E. Mcknight
b. Sample 155
SUPPLEMENTAL PROTOCOLS FOR THE LPA-1: PLASTER SAMPLE ADDITIONS
The following protocols are to be used for testing of plaster samples additions assigned
to testing ID positions of 155-158.
NOTE: Record data on relevant data forms (see attached).
1. Warmup for 20 minutes to assure self calibration occurs.
2. Calibration checks, using 20-second mode, test both sides of factory block. Record
results on back of data form.
3 Testing: First use Quick Mode at a single block or sample,
then use STD mode (20 seconds)
a. QC-Control Blocks
al. Wood 3-red over bare
3-bare
a2. Plaster 3-red over bare
3-bare
1-X1
1-red over bare
1-bare
1-X2
1-X3
1-X1
1-red over bare
1-bare
1-X2
1-X1
1-red over bare
1-bare
1-X2
1-X3
1-X1
1-red over bare
1-bare
1-X2
1-X3
QC-Control Blocks
al. Plaster 3-red over bare
3-bare
a2. Wood 3-red over bare
3-bare
c. Sample 156
d. Sample 157
e. Sample 158
B-39
-------
s «
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SUPPLEMENTAL PROTOCOLS FOR THE LPA-1
Effective Date: June 9, 1995
Used for June 1995 testing by M.E. Mcknight
a.
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B-40
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SUPPLEMENTAL PROTOCOLS FOR THE LPA-1
Effective Date: June 9, 1995
Used for June 1995 testing by M.E. Mcknight
B-41
-------
SUPPLEMENTAL PROTOCOLS FOR THE LPA-1 AND XL
Effective date: June 9, 1995
Used for June 1995 testing by M.E. McKnight
SUPPLEMENTAL PROTOCOLS FOR THE LPA-1 AND XL: CONTROL
BLOCKS
The following protocols are to be used for gathering independent sets of additional
wood control block data on these instruments. Record data on Supplemental QC data form
(see attached). Perform supplemental testing for each instrument using the indicated
protocols for a total of 9 days.
Supplemental PC Testing - LPA-1
1. Warmup for 20 minutes to assure self calibration occurs. Record results on back of
data form.
2. Calibration checks, using 20-second mode, test both sides of factory block.
3. Testing: First use Quick Mode at a single block,
then use STD mode (20 seconds) on that block
QC-Control Blocks
al. Wood 3-red over bare
3-bare
a2. Plaster 3-red over bare
3-bare
Supplemental QC Testing - XL
1. Warmup for 20 minutes.
2. Calibration checks, using 20-second mode, test both sides of factory samples (5). If
value differs by 10% or 0.1 (whichever is greater, then go back to 1). Record results
on back of data form.
3 Testing: Use 20-second mode
QC-Control Blocks:
al. Wood 3-red over bare
3-bare
a2. Plaster 3-red over bare
3-bare
B-42
-------
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SUPPLEMENTAL PROTOCOLS FOR THE LPA-1 AND XL
Effective date: June 9, 1995
Used for June 1995 testing by M.E. McKnight
a.
o.
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B-43
-------
SUPPLEMENTAL PROTOCOLS FOR THE LPA-1 AND XL
Effective date: June 9, 1995
Used for June 1995 testing by M.E. McKnight
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B-44
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective date: July 1, 1995
For use in July 1995 for testing by subcontractor
SUBCONTRACTER TESTING PROTOCOLS FOR THE LPA-1
General Responsibilities
The XRF Operator will:
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
• Download data to a computer, verify that the transfer was successful, and delete all
data files containing archive data from the XRF electronic memory.
• Report to the Testing Supervisor any indications of deteriorating samples observed
during testing.
• Set the STD mode of operation to a nominal 30-second measurement time when
using this mode.
The Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help assure the protocols are followed.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Assure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI, and
QuanTech.
• Assure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Provide the following forms:
• Testing order list
• Standard readings • Control readings
• Archive XRF information • Source age adjustment table
B-45
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective date: July 1, 1995
For use in July 1995 for testing by subcontractor
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR RMD
Beglnnhg of Day
(BOD) Instruction
Complete new
INFORMATION
form
Perform warmup
and self-calbratlon
Perform BOD QC
Checks (alls*
substrates)
Instructions to Include: safety Issues, field form use, archive
layout and testing order, sequence numbering for electronic
data capture, and voice-call back verification of data
recording by monitor.
See form for needed Information.
1. Enter date and time.
2. Allow to warmup at least 20 minutes to assure that the
auto self-calbratlon occurs (automatically done every
15 minutes).
3. Perform calibration check using STD Mode set to a
nominal 30 seconds: Test both bare and painted sides
of factory supplied wood substrate. Record results on
INFORMATION form.
4. Set Quick Mode Testing using an action level of 1.0
mg/cm2.
BOD (or EOD) QC checks: test a total of 6 pre-placed
blocks on a minimum of 12 inches of styrofoam support.
Perform testtig In order 1-6 as Indicated on the styrofoam
support using a 30-sec STD Mode reading, and record the
sequence number for each reading on the form to Identify
electronic data entries.
For each block, excluding wood, test In the following order
and record data In the appropriate columns using a single
row of the Control Readings form:
a. 1 reading, yellow NIST on block
b. 1 reading, red NIST on block
c. 1 readtig, no NIST on block
NOTE: For all control blocks except wood, fill In all three
data entries In each row. The wood exception Is
explained below.
For the wood substrate, test In the following order and record
data In the appropriate columns using three rows of the
Control Readings form:
a. 1 reading, yellow NIST on the control block
b. 3 consecutive readings, red NIST on the control block
c. 1 readtig, no NIST on the control block
NOTE: slice 3 readings with red NIST on wood control
blocks are taken consecutively, it is necessary to blank
out 4 data entries t\ the 3 rows of the form as follows:
for row 1 blank out the "No NIST SRM" entry, for row 2
blank out the 'yellow NIST" and the "No NIST SRM"
entries, and for row 3, blank out the 'Yellow NIST" entry.
B-46
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective date: July 1, 1995
For use in July 1995 for testing by subcontractor
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR RMD
the
testing day
within 30 minutes
the end?
Stop testkig, record
temp & humidity
data, perform the
EOD QC Checks
Test all of the samples at each testing location first In
the Quick mode, then repeat using the STD Mode set
to a nominal 30 seconds.
For each testing location, In each mode, test In the
following order:
a. 1 reading, on X1
b. 1 reading, on bare (P1) + red NIST
c. 1 reading, on bare (P1)
d. 1 reading, on X2
e. 1 reading, on X3.
Record data on the STANDARD READINGS form.
Periodically measure the time required to take a
reading from start to data display and record It li the
field notebook.
Download all electronically stored data and verify
successful transfer before clearing memory to make
room for more data.
EOD QC checks are the same as BOD QC checks:
follow same procedure as for BOD QC Checks.
Record temp and humidity ki a field notebook.
Download any electronically stored data, verify
successful transfer before clearing memory.
Start next day at top of flow chart using the next
sample to be tested as the first location.
Continuing QC checks, total of 2 blocks tested on a
mlntnum of 12 Inches styrofoam support. Use blocks
matching same type as the last and next locations (If
same type for both, test same block twice).
Follow the same testing order, reading times and data
recording directives as described for BOD QC checks.
B-47
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective date: July 1, 1995
For use in July 1995 for testing by subcontractor
Archive XRF Instrument Information
Date Testing Site.
Contractor Manufacturer.
Model No. Serial No.
XRF Operator (Printed Name)
Source Material Source Age or Date_
Source Serial No. Detector Type
Operating Parameters Used
Open shutter sampling tlme(s)? (fixed or variable)
If fked, what Is the duration tlme(s)?
Dally warm-up and calibration check used? (Briefly discuss)
Regulatory level value used for setting the XRF Instrument? (Yes or No)
If yes, enter the value used
Other
Data File Names and Descrlptbns
| | Check here to hdlcate the presence of additional comments on the back of this form.
B-48
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective date: July 1, 1995
For use in July 1995 for testing by subcontractor
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TESTING PROTOCOLS FOR THE LPA-1
Effective date: July 1, 1995
For use in July 1995 for testing by subcontractor
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B-50
-------
TESTING PROTOCOLS FOR THE LEADSTAR
Effective Date: July 25, 1995
Used for August 1995 testing by subcontractor
SUBCONTRACTOR TESTING PROTOCOLS FOR THE LEADSTAR
General Responsibilities
The XRF Operator will:
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
• Download data to a computer and verify that the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed
during testing.
The Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help assure the protocols are followed.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Assure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI and
QuanTech.
• Assure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Provide the following forms:
• Testing order list • Archive XRF information
• Standard readings • Control readings
B-51
-------
TESTING PROTOCOLS FOR THE LEADSTAR
Effective Date: July 25, 1995
Used for August 1995 testing by subcontractor
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR XSIRIUS
Perform warmup
and self-calibration
Record temp &
humidity data
Complete new
INFORMATION
form
Perform BOD QC
Checks (all six
substrates)
Instructions to include: safety issues, field form use, archive
layout and testing order, Sample ID numbering for electronic
data capture, voice-call back verification of data recording by
monitor, a blank display for negative lead results, and the
use of a 30-sec reading adjusted for source age.
See form for needed information.
1. Allow to warm-up for 5 minutes.
2. Enter or verify:
a. the selected file names to store the data
b. the action level Is set to 1.0 mg/cm2
c. any other user entered parameters.
3. Perform self-calibration as per the manual and
manufacturer training directives using the manufacturer
supplied calibration sample(s).
Summarize any user entered Information and the
calibration procedure on the Instrument INFORMATION
form.
BOD (or EOD) QC checks: test a total of 6 pre-placed
blocks on a minimum of 12 inches of styrofoam support.
Please do not move blocks.
For each block, using a nominal 15-sec reading, test In the
following order:
a. 1 reading, yellow NISI on block
b. 1 reading, red NIST on block. IF the block is wood,
THEN collect 2 more readings using the red NIST on
the block. Record extra readings on subsequent lines
of the data form placing a diagonal line through the
unused yellow and no NIST data blocks.
c. 1 reading, no NIST on block
Before moving to the next control block repeat a-c above
using a nominal 30-sec reading adjusted for source age.
Record the data on the CONTROL READINGS form.
B-52
-------
TESTING PROTOCOLS FOR THE LEADSTAR
Effective Date: July 25, 1995
Used for August 1995 testing by subcontractor
FLOW CHART SUMMARY
DESCRIPTION DETAILS FORXSIRIUS
Move to first or
next location and
take readings
(follow TESTING
ORDER list)
Perform self-
calibration and
verification
the\. Yes
ri rfoy ^*b \
verrj^^
Record temp &
humidity data
Stop testing, record
temp & humidity
data, perform the
EOD QC Checks
HAVE1
locations been
tested since
lastQC
eck?
For each testing location, using a nominal 15-sec
reading, test In the following order:
a. 1 reading, on X1
b. 1 reading, on bare (P1) + red NIST
c. 1 reading, on bare (P1)
d. 1 reading, on X2
e. 1 reading, on X3.
Record data on the STANDARD READINGS form.
IF during any of the a-e testing above, the density is
£ 4 THEN:
- complete all a-e testing using the nominal
15-sec reading time
- Change the testing mode to a nominal 30-sec
reading adjusted for source age and repeat
a-e testing above recording the data on the
STANDARD READINGS form using a new row.
1. IF XRF off, allow to warmup for 5 minutes.
2. Enter or verify:
a. the selected file names to store the data
b. the action level is set to 1.0 mg/cm2
c. any other user entered parameters.
3. Perform self-calibration as per the manual and
manufacturer training directives using the
manufacturer supplied calibration sample(s).
Summarize changes to any user entered
Information on the Instrument INFORMATION form.
EOD QC checks are the same as BOD QC checks:
follow same procedure as for BOD QC Checks.
Record temp and humidity in a field notebook.
Download any electronically stored data, verify
successful transfer before clearing the memory to
make room for more data.
Start next day at top of flow chart using the next
sample to be tested as the first location.
Continuing QC checks, total of 2 blocks tested on a
minimum of 12 Inches styrofoam support. Use blocks
matching same type as the last and next locations (If
same type for both, test same block twice).
Follow same testing order and reading times as that
used for BOD testing (i.e.: First, use the nominal
15-sec reading for testing a-c. Second, before
moving to the next control block, repeat a-c testing
using a nominal 30-sec reading.)
B-53
-------
TESTING PROTOCOLS FOR THE LEADSTAR
Effective Date: July 25, 1995
Used for August 1995 testing by subcontractor
Archive XRF Instrument Information
Date Testing Site.
Contractor Manufacturer.
Model No. Serial No.
XRF Operator (Printed Name)
Source Material Source Age or Date
Source Serial No. Detector Type
Operating Parameters Used
Open shutter sampling tlme(s)? (fixed or variable)
If fixed, what Is the duration thne(s)?
Dally warm-up and calibration check used? (Briefly discuss)
Regulatory level value used for setting the XRF Instrument? (Yes or No)
If yes, enter the value used
Other
Data File Names and Descriptions
Check here to hdlcate the presence of additional comments on the back of this form.
B-54
-------
TESTING PROTOCOLS FOR THE LEADSTAR
Effective Date: July 25, 1995
Used for August 1995 testing by subcontractor
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B-55
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TESTING PROTOCOLS FOR THE LEADSTAR
Effective Date: July 25, 1995
Used for August 1995 testing by subcontractor
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B-56
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
General Responsibilities
The XRF Operator will:
• Perform all manufacturer-recommended warm-up procedures and quality control
checks, and work with the Testing Monitor and the Testing Supervisor to document
that the procedures and checks were done, what the outcomes were, and, if
appropriate, what actions were taken.
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help assure that protocols are followed and
any deviations are properly documented.
• Download data to a computer and verify that the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed.
The Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help assure the protocols are followed.
• Work with the Testing Supervisor to help assure that protocols are followed and
any deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Assure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI,
QuanTech, and NIST.
• Assure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Make sure that all testing is done safely, that all personnel on site wear dosimeter
badges during testing, that dosimeter badges are collected and analyzed after testing
is completed, and that results of dosimeter badge analysis are relayed to the badge
wearers.
• Take radiation measurements periodically around each instrument being used for
testing.
• Provide blank forms to the Testing Monitor (blank forms to be delivered to the
Testing Supervisor by QuanTech) and review forms filled out by the Testing
Monitor for completeness. The forms for the following will be used during testing:
• Testing order list • Archive XRF information
• Standard readings • Control readings
B-57
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
Beginning of Work Session
At the beginning of the work session, be sure that there is a fresh battery pack in the
Analyzer. It is good practice to transfer previous data to the personal computer before
beginning the day's work. If the previous data have not been transferred, refer to the
"Downloading" section below. If the data have been transferred, reset the Analyzer
memory by pressing the RESET button. The SET button confirms the reset.
Verify Keypad Settings
Before taking any measurements, a few system configuration checks should be made:
1. Check that the Manual Shutter Lock and Keylock (if provided) are unlocked.
2. Check that any old data in the LPA-1 has been downloaded if a Memory Reset is
to be performed.
3. Check that the Abatement Level is properly set. The Abatement Level setting can
be checked by turning on the LPA-1 with the Trigger, then pressing the SET key.
The LPA-1 will then display ABATE AT XX mg. If the setting is not correct, the
value can be incremented with the SET key.
4. Verify that the LPA-1 is in the desired operating mode. When in Standard Mode,
the display will show STD MODE XX Sec, where XX is the number of seconds
previously programmed for the length of the measurement. If a Quick Mode
measurement is desired, change operating modes by pressing the SELECT MODE
button.
5. Verify the setting of the LPA-1 system clock by allowing the LPA-1 to power
down, then pressing the NEW UNIT key for two seconds. Press the SET key to
confirm. The display is formatted as month-day-year-time. The time should be
accurate within 15 minutes. To exit this mode, press the NEW UNIT key again
and allow the LPA-1 to shut off.
Check Calibration Sample
Before and after each job, it is good quality control practice to do a system
performance check. It is recommended that this be done by taking three readings on the
Calibration Test Block provided with the instrument and on another lead-free wood block.
The tested value of the yellow test pad is recorded on the back of the block. A reading of
appropriate length (see below) should be taken on both the Calibration Block and also on
any block of unpainted wood or drywall that the user has at hand to provide a zero lead
reference. Note: The back side of the calibration is not a good zero reference because
some amount of the lead on the front of the block is liable to be detected through the thin
wood block.
B-58
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
Use the Date of Receipt of the LPA-1 from the factory as a starting point to correct the
Performance Test reading for half-life decay as follows:
0 to 120 days (4 mos.)—Test at 30 seconds
121 to 175 days (6 mos.)—Test at 40 seconds
176 to 270 days (9 mos.)—Test at 50 seconds
270 to 455 days (15 mos.)—Test at 60 seconds
Beyond 15 months—Time to replace the Source
Ninety-five percent of the time, the value of any single calibration reading should be
the value of the calibration block ±0.3 mg/cm2.
Alternately the user may wish to perform 60-second measurements throughout the life
of the source. This eliminates guesswork and keeps field procedures simple. In this case,
the user should expect to see readings that are the value of the calibration block
±0.2 mg/cm2.
If the Lead Readings were outside of the correct range, wait at least 5 minutes for the
Analyzer's automatic Calibration Check to occur. After the Check is completed, reread the
Standard Block. Should the readings again fall outside the acceptable range, call RMD
before continuing with the inspection.
B-59
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR LPA-1
Beglnntig of Day
(BOD) Instruction
Complete new
INFORMATION
form
Perform warm-up
and self-calibration
Perform BOD QC
Checks (all six
substrates)
Instructions to Include: safety Issues, field form use, archive
layout and testing order, sequence numbering for electronic
data capture, and voice-call back verification of data
recording by monitor.
See form for needed Information.
1. Enter date and time.
2. Perform warm-up and calibration check procedure as
specified by the manufacturer (see attachment).
3. Set Quick Mode Testing using an action level of 1.0
mg/cm2.
BOD (or EOD) QC checks: test a total of 6 pre-placed blocks
on a mlnknum of 12 Inches of styrofoam support. Perform
testing in order 1-6 as indicated on the styrofoam support.
Record the sequence number for each reading on the form to
Identify electronic data entries as described below.
For each block, excluding wood, test using the nominal 30
second STD mode In the following order and record data In the
appropriate columns using a single row of the Control Readings
form:
a. 1 reading, yellow NIST on block
b. 1 reading, red NIST on block
c. 1 reading, no NIST on block
NOTE: For all control blocks except wood, fill In all three
data entries In each row. The wood exception Is explained
below.
For the wood substrate, test using two modes In the order
a-c below. First, test using the Quick mode. Second, test using
a nominal 30 second mode. Record data In the appropriate
columns using three rows of the Control Readings form for each
test mode:
a. 1 reading, yellow NIST on the control block
b. 3 consecutive readings, red NIST on the control block
c. 1 reading, no NIST on the control block
NOTE FOR EACH MODE: since 3 readings with red NIST
on wood control blocks are taken consecutively, it is
necessary to blank out 4 data entry column blocks In 3
consecutive rows of the form as follows: for row 1, blank
out the "No NIST SRM" entry block, for row 2, blank out the
"yellow NIST" and the "No NIST SRM" entry blocks, and for
row 3, blank out the "yellow NIST" entry block.
B-60
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR LPA-1
Move to first or
next location and
take readings
(follow TESTING
ORDER list)
the
testing day
If over
Record temp &
humidity data
ISXRF ^ Yes
ata storage almos
full ??
Download testing
data
the
testing day \ Yes
within 30 minutes
the end??
Stop testing, record
temp & humidity
data, perform the
EOD QC Checks
HAVE 15
locations been
tested since
lastQC
heck n
Perform
continuing QC
checks
Perform testing at each testing location first In the
Quick mode, then repeat using the STD Mode set to a
nominal 30 seconds.
For each testing location, In each mode, test In the
following order:
a. 1 reading, on X1
b. 1 reading, on bare + red NIST
c. 1 reading, on bare
Record data on the STANDARD READINGS form.
Periodically measure the time required to take a
reading from start to data display and record it in the
field notebook.
Download all electronically stored data and verify
successful transfer before clearing memory to make
room for more data.
EOD QC checks are the same as BOD QC checks:
follow same procedure as for BOD QC Checks.
Record temp and humidity in a field notebook.
Download any electronically stored data, verify
successful transfer before clearing memory.
Start next day at top of flow chart using the next
sample to be tested as the first location.
Continuing QC checks, total of 2 blocks tested on a
minimum of 12 Inches styrofoam support. Use blocks
matching same type as the last and next locations (If
same type for both, test same block twice).
Follow the same testing order, reading times and data
recording directives as described for BOD QC checks.
B-61
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
Date
Archive XRF Instrument Information
Testing Site.
Contractor
Model No.
. Manufacturer.
. Serial No.
XRF Operator (Printed Name)_
Source Material
Source Serial No.
Source Age or Date
Detector Type
Software Version No.
Operating Parameters Used
Open shutter sampling tlme(s)? (fixed or variable)
If fixed, what Is the duration tlmefe)?
Dally warm-up and calibration check used? (Briefly discuss)
Regulatory level value used for setting the XRF Instrument? (Yes or No)
If yes, enter the value used
Other
Data File Names and Descriptions
Check here to hdlcate the presence of additional comments on the back of this form.
B-62
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
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B-63
-------
TESTING PROTOCOLS FOR THE LPA-1
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
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B-64
-------
TESTING PROTOCOLS FOR THE Pb ANALYZER
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
General Responsibilities
The XRF Operator will:
• Perform all manufacturer recommended warm-up procedures and quality control
checks, and work with the Testing Monitor and the Testing Supervisor to document
that the procedures and checks were done, what the outcomes were, and, if
appropriate, what actions were taken.
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
• Download data to a computer and verify that the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed.
The Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help assure the protocols are followed.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Assure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI,
QuanTech, and NIST.
• Assure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Make sure that all testing is done safely, that all personnel on-site wear dosimeter
badges during testing, that dosimeter badges are collected and analyzed after testing
is completed, and that results of dosimeter badge analysis are relayed to the badge
wearers.
• Take radiation measurements periodically around each instrument being used for
testing.
• Provide blank forms to the Testing Monitor (blank forms to be delivered to the
Testing Supervisor by QuanTech) and review forms filled out by the Testing
Monitor for completeness. The forms for the following will be used during testing:
• Testing order list • Archive XRF information
• Standard readings • Control readings
B-65
-------
TESTING PROTOCOLS FOR THE Pb ANALYZER
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
Energy Calibration and Standard Operating Check
Complete both of these procedures:
• at the beginning of each work day
• if the Analyzer has been off for more than one hour
• if the Analyzer has been exposed to a temperature change of > 10°C/20°F
• if the unit has been subjected to shock or been damaged
At the end of the day, perform the Standard Operating Check (without running the
Energy Calibration) to verify that the Analyzer performed properly using that day's energy
calibration.
Energy Calibration Procedure
Perform the Energy Calibration before the Operating Check (unless you are running
the "end of work day" check). This procedure will automatically calibrate the spectrometer
function.
Lay the flat safety cover on a level, stable surface and carefully set the probe in the
cover.
1. Choose your application.
2. From the Ready screen press 5, "Options."
3. Press 1, "Energy Calibration."
4. Follow the screen prompts.
Standard Operating Check
The two-part standard operating check verifies the Analyzer's operation with respect to
element X-ray response and analytical background. The operating check is discussed in
detail in Chapter 2.
X-Ray Response
X-ray response is checked by making a 50-second measurement on a pure Pb sample,
then viewing Pb intensity data (Pb intensity should be between 0.95 and 1.05). See
Chapter 2 for detailed instructions on how to conduct the x-ray response check. If intensity
is not > 0.95 and < 1.05, check the probe window for contamination and make sure the Pb
sample is centered over the aperture, then rerun the check. If intensity is still off, turn to
Chapter 8 of the Operator's Manual and run a spectrum energy calibration check.
B-66
-------
TESTING PROTOCOLS FOR THE Pb ANALYZER
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
Note: The x-ray response check may result in an "Algorithm did not converge"
message in the Pb in Paint Chips and Pb in Soil applications. This should be
expected, since the pure Pb intensity is very different from that produced by a
"normal" paint chip or soil sample. For the x-ray response check, we are only
interested in the intensity data—not the analysis result.
Analytical Background Check
The background check verifies proper operation of the spectrometer and can alert you
to dirt or contamination on the probe window. Always protect the probe window since
dirt, moisture, or contamination on it can compromise your analysis.
The check for Pb in paint chips is run on the "blank," which is a sample cup
containing SiO2. To conduct the check, set up the Uniblock in the lab configuration
(steps 1-4) and present the sample as described. Analysis results on this sample should
show a Pb value within ±5 standard deviations of zero (if your results are in units rather
than standard deviations, press 5, "OPTS" on the Results screen and then 3, "Show STD").
If results are not within ±5 standard deviations of zero, you must run the "Acquire
Background" procedure. If you don't see any results, you have Display Thresholds enabled.
To disable thresholds, go to the Ready screen, select 5, "Options," then 6, "More Options,"
then 5, "Disable display thresholds."
Warning: During any analysis, there is a minimal risk of radiation exposure. While an
analysis is in progress,
• Do not remove the probe from the Uniblock (or other
measurement surface)
• Do not look at or touch the probe window.
To abort any analysis in progress, press CONT or the red button on the
probe.
1. Lay the Uniblock flat-side up so that you can read the words "Aluminum" and
"Steel."
2. Slide the probe clamp into the cutout end of the Uniblock.
3. Place the probe in the Uniblock with the probe window facing up and the probe
handle cable pointing away from the probe clamp.
4. Carefully tighten the clamp knob until the probe is secure. Do not force the knob
to turn since this can damage the clamp. Verify that the probe is secure.
B-67
-------
TESTING PROTOCOLS FOR THE Pb ANALYZER
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
5. Set the sample shield on the probe. The cutout should be centered over the probe
window. If the cutout is off center, turn the shield around and recheck the
position of the probe window.
6. Secure the sample shield on the probe with the bungee cord.
7. Place the 30mm sample positioning ring over the probe aperture.
8. Visually inspect the sample and verify that surfaces which will be presented to the
probe are clean.
9. Place the SiO2 sample in the positioning ring on the probe. Close the shield
cover.
10. Measure the sample for at least 60 seconds (adjusted for source decay). Use
Table 1 in Chapter 2 to determine adjusted analysis time.
11. Label and store the result. This is discussed in detail in Chapter 2.
When you accept the label (press CONT from the label screen), the analysis results
will be displayed. Compare the Pb assay value with its standard deviation (STD) value. It
must be < 5 standard deviations above or below "zero." If it is not, check for
contamination on the probe window or the sample cup. If contamination does not appear
to be the problem, run the "Acquire Background" procedure.
Acquire Background
If your analysis showed a Pb value of more than ±5 standard deviations from zero on
the SiO2 sample, you should acquire the background.
1. Go to the Ready screen
2. Press 5, "More."
3. Press 2, "Acquire a Background."
4. Place the SiO2 and then the Teflon sample on the probe as requested.
After you have acquired the background, run the background check again to verify the
acquisition was successful. If the Analyzer still does not check out, contact TN
Technologies at 800-736-0801 (U.S. only) or 512-388-9100.
Known Standard Check
We suggest that you run (and store) at least one analysis on a known standard before
beginning your actual sample measurement. For the Pb in Paint Chips application, this
check should be run on the Fisher SRS 013 sample, for 200 live seconds, adjusted for
source decay. Results should be .07% ± 0.01%.
B-68
-------
TESTING PROTOCOLS FOR THE Pb ANALYZER
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR Pb ANALYZER
Perform warmup
and self-calibration
Complete new
INFORMATION
form
Perform BOD QC
Checks (all six
substrates)
Instructions to include: safety issues, field form use, archive
layout and testing order, sequence numbering for electronic
data capture, and voice-call back verification of data
recording by monitor.
See form for needed Information.
1. Enter date and time.
2. Allow to warmup as specified by the manufacturer.
3. Perform calibration check as specified by the
manufacturer (see attachment).
BOD (or EOD) QC checks: test a total of 6 pre-placed
blocks on a minimum of 12 inches of styrofoam support.
Perform testing in order 1-6 as indicated on the styrofoam
support using a nominal 15 second real time reading, and
record the sequence number for each reading on the form to
identify electronic data entries.
For each block, excluding wood, test in the following order
and record data in the appropriate columns using a single
row of the Control Readings form:
a. 1 reading, yellow NIST on block
b. 1 reading, red NIST on block
c. 1 reading, no NIST on block
NOTE: For all control blocks except wood, fill in all three
data entries in each row. The wood exception is
explained below.
For the wood substrate, test in the following order and record
data in the appropriate columns using three rows of the
Control Readings form:
a. 1 reading, yellow NIST on the control block
b. 3 consecutive readings, red NIST on the control block
c. 1 reading, no NIST on the control block
NOTE: since 3 readings with red NIST on wood control
blocks are taken consecutively, It Is necessary to blank
out 4 data entry column blocks In 3 consecutive rows of
the form as follows: for row 1, blank out the "No NIST
SRM" entry block, for row 2, blank out the 'yellow NIST"
and the "No NIST SRM" entry blocks, and for row 3,
blank out the "yellow NIST" entry block.
B-69
-------
TESTING PROTOCOLS FOR THE Pb ANALYZER
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR Pb ANALYZER
Move to first or
next location and
take readings
(follow TESTING
ORDER list)
the
testing day
If over
Record temp &
humidity data
ISXRF ^ Yes
ata storage almos
full ??
Download testing
data
the
testing day \ Yes
within 30 minutes
the end??
Stop testing, record
temp & humidity
data, perform the
EOD QC Checks
HAVE 15
locations been
tested since
lastQC
heck n
Perform
continuing QC
checks
For each testing location, using a nominal 15 second
real time reading, test in the following order:
a. 1 reading, on X1
b. 1 reading, on bare + red NIST
c. 1 reading, on bare
Record data on the STANDARD READINGS form.
Periodically measure the time required to take a
reading from start to data display and record it in the
field notebook.
Download all electronically stored data and verify
successful transfer before clearing memory to make
room for more data.
EOD QC checks are the same as BOD QC checks:
follow same procedure as for BOD QC Checks.
Record temp and humidity in a field notebook.
Download any electronically stored data, verify
successful transfer before clearing memory.
Start next day at top of flow chart using the next
sample to be tested as the first location.
Continuing QC checks, total of 2 blocks tested on a
minimum of 12 Inches styrofoam support. Use blocks
matching same type as the last and next locations (If
same type for both, test same block twice).
Follow the same testing order, reading times and data
recording directives as described for BOD QC checks.
B-70
-------
TESTING PROTOCOLS FOR THE Pb ANALYZER
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
Date
Archive XRF Instrument Information
Testing Site.
Contractor
Model No.
. Manufacturer.
. Serial No.
XRF Operator (Printed Name)_
Source Material
Source Serial No.
Source Age or Date
Detector Type
Software Version No.
Operating Parameters Used
Open shutter sampling tlme(s)? (fixed or variable)
If fixed, what Is the duration tlmefe)?
Dally warm-up and calibration check used? (Briefly discuss)
Regulatory level value used for setting the XRF Instrument? (Yes or No)
If yes, enter the value used
Other
Data File Names and Descriptions
Check here to hdlcate the presence of additional comments on the back of this form.
B-71
-------
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TESTING PROTOCOLS FOR THE Pb ANALYZER
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
B-72
-------
TESTING PROTOCOLS FOR THE Pb ANALYZER
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
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B-73
-------
TESTING PROTOCOLS FOR THE WARRINGTON MICROLEAD I
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
General Responsibilities
The XRF Operator will:
• Perform all manufacturer recommended warm-up procedures and quality control
checks, and work with the Testing Monitor and the Testing Supervisor to document
that the procedures and checks were done, what the outcomes were, and, if
appropriate, what actions were taken.
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
• Download data to a computer and verify that the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed.
The Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help assure the protocols are followed.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Assure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI,
QuanTech, and NIST.
• Assure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Make sure that all testing is done safely, that all personnel on site wear dosimeter
badges during testing, that dosimeter badges are collected and analyzed after testing
is completed, and that results of dosimeter badge analysis are relayed to the badge
wearers.
• Take radiation measurements periodically around each instrument being used for
testing.
• Provide blank forms to the Testing Monitor (blank forms to be delivered to the
Testing Supervisor by QuanTech) and review forms filled out by the Testing
Monitor for completeness. The forms for the following will be used during testing:
• Testing order list • Archive XRF information
• Standard readings • Control readings
B-74
-------
TESTING PROTOCOLS FOR THE WARRINGTON MICROLEAD I
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
Calibration Check Procedure for MicroLead I—Revision 4
I. Diagnostics and Source Dating
A. Press power switch to turn on analyzer. Verify that no FAULT codes are
displayed after diagnostic countdown is completed.
B. Check TODAY'S DATE. Check SOURCE DATE. If you are going to store field
readings, press the CLEAR MEMORY function key for 3 seconds to erase the
operator's memory space.
II. Set Zero Reference to Remove Bias
A. Press the ZERO STANDARD function key (verify "PROBE" is shown on the
display).
B. With the probe centered on the Gypsum Zero Standard, pull the probe trigger and
hold until at least four Read Cycles are completed (nine is better). Verify that the
display is showing 0.0 mg/cm2.
III. Recording Calibration Check Data
A. Verify Accuracy (Bias) for Zero Lead Level.
1. With the probe centered on the Gypsum Zero Standard, take at least five
replicate 1st Read Cycle measurements (ten is better). Record readings
in logbook. Compute average (x) and standard deviation (a).
2. If x does not equal 0.0 mg/cm2, ±0.1 mg/cm2, start over at II.
B. Verify Precision for Zero Lead Level.
If a does not equal 0.3 mg/cm2 or less, take additional measurements to
improve your statistical database. Recalculate x and a. If a still does
not meet factory specification, call Warrington's service department at
512-251-7771.
B-75
-------
TESTING PROTOCOLS FOR THE WARRINGTON MICROLEAD I
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
Repeat step III at least every 2 hours throughout the day and at the very end of the day.
Record calibration check readings in your logbook each time. Also, approximately twice
per month verify that the "Radiation Density" of the (black) Concrete Zero Standardly
reading "22".
C. Verify Accuracy (Bias) for Positive Lead Level.
1. Place a calibrated Lead Standard on the Gypsum Zero Standard. With the
probe centered, take five replicate 1st Read Cycle measurements (ten is
better). Record readings in logbook. Compute x and a.
2. If x does not equal the stated lead (Pb) value, ±0.1 mg/cm2, take
additional measurements to improve your statistical database.
Recalculate x and a. If x still does not equal the stated lead (Pb) value,
±0.1 mg/cm2, follow manufacturer's instructions for LEAD
STANDARD Note: Do not press the LEAD STANDARD function
key unless you have received specific instructions on how to properly
use this function.
D. Verify Precision for Positive Lead Level.
If a does not equal 0.3 mg/cm2 or less, take additional measurements to
improve your statistical database. Recalculate x and a. If a still does
not meet factory specification, call Warrington's service department at
512-251-7771.
B-76
-------
TESTING PROTOCOLS FOR THE WARRINGTON MICROLEAD I
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR MICROLEAD I
Beginning of Day
(BOD) Instruction
Complete new
INFORMATION
form
Perform warm-up
and self-calibration
Instructions to Include: safety Issues, field form use, archive
layout and testing order, and voice-call back verification of
data recording by monitor.
Perform BOD QC
Checks (all six
substrates)
See form for needed Information.
Perform warm-up and calibration check procedures as specified
by the manufacturer (see attachment).
BOD (or EOD) QC checks: test a total of 6 pre-placed blocks
on a minimum of 12 Inches of styrofoam support. Perform
testing In order 1-6 as Indicated on the styrofoam support.
Record the sequence number for each reading on the form to
identify electronic data entries as described below.
For each block, excluding wood, test in the following order and
record data in the appropriate columns using a single row of the
Control Readings form:
a. 1 reading, yellow NIST on block
b. 1 reading, red NIST on block
c. 1 reading, no NIST on block
NOTE: For all control blocks except wood, fill in all three
data entries In each row. The wood exception Is explained
below.
For the wood substrate, test In the order a-c below. Record data
In the appropriate columns using three rows of the Control
Readings form:
a. 1 reading, yellow NIST on the control block
b. 3 consecutive readings (3 Independent trigger pull events),
red NIST on the control block
c. 1 reading, no NIST on the control block
NOTE: since 3 readings with red NIST on wood control
blocks are taken consecutively, It Is necessary to blank
out 4 data entry column blocks In 3 consecutive rows of
the form as follows: for row 1, blank out the "No NIST
SRM" entry block, for row 2, blank out the "yellow NIST"
and the "No NIST SRM" entry blocks, and for row 3, blank
out the "yellow NIST" entry block.
B-77
-------
TESTING PROTOCOLS FOR THE WARRINGTON MICROLEAD I
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
FLOW CHART SUMMARY
DESCRIPTION DETAILS FOR MICROLEAD I
Move to first or
next location and
take readings
(follow TESTING
ORDER list)
strument beep
quickly during
read
Complete reading,
discard, and re-test
etwo
ours passed skice
last cafcratbn
ec
Repeat step III of
Manufacturers calibration
check procedure
the
testing day
half over?
Record temp &
humidity data
the
testing day
within 30 minutes
of the end?
Stop testing, record
temp & humidity
data, perform the
EOD QC Checks
HAVE
15 locations
been tested
since last QC
check?
Perform
continuing QC
checks
Perform testing at each testing location using a single
nominal 15 second trigger pull event.
For each testing location, test in the following order:
a. 1 reading, on X1
b. 1 reading, on bare + red NIST
c. 1 reading, on bare
Record data on the STANDARD READINGS form.
Periodically measure the time required to take a
reading from start to data display and record it in the
field notebook.
If instrument beeps quickly during a reading, a major
density change has been detected. Under these
conditions, complete the reading and record the value
In the comments column of the form (do not record In
the normal data entry block). Then, re-test and record
the result in the normal manner.
EOD QC checks are the same as BOD QC checks:
follow same procedure as for BOD QC Checks.
Record temp and humidity In a field notebook.
Start next day at top of flow chart using the next
sample to be tested as the first location.
Continuing QC checks, total of 2 blocks tested on a
minimum of 12 inches styrofoam support. Use blocks
matching same type as the last and next locations (If
same type for both, test same block twice).
Follow the same testing order, reading times and data
recording directives as described for BOD QC checks.
B-78
-------
TESTING PROTOCOLS FOR THE WARRINGTON MICROLEAD I
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
Archive XRF Instrument Information
Date Testing Site.
Contractor Manufacturer.
Model No. Serial No.
XRF Operator (Printed Name)
Source Material Source Age or Date
Source Serial No. Detector Type
Software Version No.
Operating Parameters Used
Open shutter sampling tlme(s)? (fixed or variable)
If fixed, what Is the duration tlmefe)?
Dally warm-up and calibration check used? (Briefly discuss)
Regulatory level value used for setting the XRF Instrument? (Yes or No)
If yes, enter the value used
Other
Data File Names and Descriptions
Check here to hdlcate the presence of additional comments on the back of this form.
B-79
-------
TESTING PROTOCOLS FOR THE WARRINGTON MICROLEAD I
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
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B-80
-------
TESTING PROTOCOLS FOR THE WARRINGTON MICROLEAD I
Effective Date: Septembers, 1995
Used for September 1995 testing by M.E. McKnight
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B-81
-------
TESTING PROTOCOL FOR THE PRINCETON GAMMA-TECH (PGT) XK-3
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
TESTING PROTOCOLS FOR THE XK-3
General Responsibilities
The XRF Operator will:
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help ensure that protocols are followed and
any deviations are properly documented.
• Download data to a computer and verify that the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed
during testing.
The Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help ensure the protocols are followed.
• Work with the Testing Supervisor to help ensure that protocols are followed and
any deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Ensure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI,
NIST, and QuanTech.
• Ensure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Complete a new set of SAMPLE LOCATION CONDITION forms for:
a. Sample locations previously identified as being in poor condition which
already have completed records from the early spring 1995 testing.
b. Any additional sample locations that are observed to be in poor
condition.
• Provide the following forms:
• Testing order list • Sample location condition
• Standard readings • Control readings
• Archive XRF information • Source age adjustment table
B-82 Version 2.0
-------
TESTING PROTOCOL FOR THE PRINCETON GAMMA-TECH (PGT) XK-3
Effective date: February 5,1996
Used for February 1996 Testing by M.E. McKnight
Testing Protocols for the
PGT XK-3 Lead-in-Paint Analyzer
Flow Chart Summary
Description Details for PGT XK-3
Beginning of Day\
(BOD) Instruction\)
Complete New
INFORMATION Form
Perform Warm-up
& Calibration Check
Record Temperature
& Humidity Data
Perform BOD
QC Checks
(all six substrates)
W-53 SEV Mt IU I12WS
Instructions to include: safety issues, field form use,
archive layout and testing order, sample ID numbering
for electronic data capture, voice-call back verification of
data recording by monitor, and a blank display for
negative lead results.
See form for needed information.
1. Connect the battery pack to the XK-3 unit
2. Find the lock switch underneath the handle and push
it forward.
3. Allow to warm-up (stabilize) for 10 minutes.
Note: The larger the temperature difference between
where the XK-3 has been stored and where the testing
is to be done, the longer it may take to stabilize.
4. Perform calibration check as per the manual and
manufacturer training directives using the
manufacturer supplied calibration sample(s).
Summarize any user entered information and the
calibration procedure on the instrument INFORMATION
form.
BOO (or EOD) QC checks: test a total of 6 pre-placed
blocks on a minimum of 12 inches of StyrofoamTM
support. Please do not move blocks.
For each block test in the following order
a. 1 reading, yellow NIST on block
b. 1 reading, red NIST on block. IF the block is
wood, THEN collect 2 more readings using the
red NIST on the block. Record extra readings
on subsequent lines of the data form placing a
diagonal line through the unused yellow and no
NIST data blocks.
c. 1 reading, no NIST on block.
Record the data on the CONTROL READINGS form.
B-83
Version 2.0
-------
TESTING PROTOCOL FOR THE PRINCETON GAMMA-TECH (PGT) XK-3
Effective date: February 5,1996
Used for February 1996 Testing by M.E. McKnight
Testing Protocols for the
PGT XK-3 Lead-in-Paint Analyzer
Flow Chart Summary
Move to First or Next
Location and Take
Readings (follow
TESTING ORDER list)
Has
any of
the Following
Occurred?
The Lock Switch has
been turned on
Two Hours after Last Calibration
Check
The First Reading of 10 mg/cm2
• Indication of that Calibration
is Suspect
• Temperatures A > 10° C
• Right before the
instrument is shut
off at the end
of the
day.
Is the
Testing Day Half
Over?
Record Temperature
& Humidity Data
Is the
Testing Day
Within 30 Minutes of
the End?
Stop Testing, Record X
Temperature & Humidity )
Data, Perform the EOD./
QC
Have 15
Locations Been
Tested Since Last
QC Check?
Perform Continuing
QC Checks
Description Details for PGT XK-3
For each testing location, test and record the
measurements in the following order:
a. 1 reading, on X1
b. 1 reading, on bare (P1) + red NIST
c. 1 reading, on bare (P1)
d. 1 reading, on X2
e. 1 reading, on X3.
Note: If insufficient time is available during NIST testing,
X2 and X3 readings may be deleted.
1. IIXRF off, allow to warm up for 10 minutes.
2. Perform calibration checks as per the manual and
manufacturer training directives using the
manufacturer-supplied calibration sample
-------
TESTING PROTOCOL FOR THE PRINCETON GAMMA-TECH (PGT) XK-3
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
USING THE XK-3
Operating Instructions
1. Remove the battery case, coiled cable, and XK-3 unit from the carrying case. Connect
the battery pack to the XK-3 unit, using the coiled cable. Do not operate the XK-3
unless the battery pack is connected to the unit with the coiled cable, or a rapid power
drain of the handle batteries will result.
2. Find the lock switch underneath the handle (toward the rear of the unit) and push it
forward. A red light over the display will glow to indicate that the instrument is now
ready to perform analysis as soon as the shutter is opened. The XK-3 may require
approximately 10 minutes of operation to stabilize after first being turned on. The
larger the temperature difference between where the XK-3 has been stored and where
it's being used, the longer it will take for it to stabilize. The stabilization process can
best be carried out and observed by using the Calibration Check procedures as
described.
3. Depress the red reset button on the back plate of the unit (just above the coiled cable
connection) for 10 seconds.
4. Grasping the rear of the wooden handle, position the faceplate of the instrument
against the surface to be measured and press down firmly and quickly so that a
mechanical click occurs. This action will open the shutter, and the red light over the
window will blink to indicate the shutter is no longer completely closed. As soon as
the shutter is completely open, the previous readout in the window vanishes, leaving
the display blank except for a single decimal point.
5. When the new reading appears, an audible beep will be heard to indicate completion of
the reading. Release the handle. The display window will retain the reading until the
handle is again depressed to begin another measurement.
6. The XK-3 is self-correcting for the decay of the source. As the source ages, the
instrument automatically extends its counting time.
7. Readings with a negative sign (-) may be normal. It depends on the statistical
variations of the readings or could indicate a substrate with negative substrate
contribution; that is substrate equivalent lead (SEL) as defined in the HUD lead
abatement guidelines. It may be necessary to correct for the effect of different
substrate materials on the readings. This subject is covered in detail in the XK-3 User
Schools.
B-85 Version 2.0
-------
TESTING PROTOCOL FOR THE PRINCETON GAMMA-TECH (PGT) XK-3
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
8. The first time a reading of 10.0 mg/cm2 is seen during a testing sequence, the XK-3
should be reset and its calibration checked (see Calibration Check, below). Each
subsequent reading of 10.0 mg/cm2 should be followed by use of the reset button.
Calibration should be checked only after the first reading of 10 mg/cm2 in a series. If
the XK-3 checks out, just reset after subsequent 10.0 mg/cm2.
9. Push the lock switch to the LOCK position when testing has been completed.
NOTE: If the safety shutter is not completely closed, the red light flashes to show that
radiation may be coming from the instrument. The red light will flash any time the shutter
is not completely closed. If the red light is flashing with the lock switch ON and the
operating handle in the UP position, it indicates a possibility of the shutter being open.
If the red power safety light is not lit after the locking switch in ON, and there is no
indication of low battery level or absence of power, treat the unit according to the sticky
shutter procedure (as described in the Operator's Manual).
Calibration Check
To perform the calibration check, follow this procedure:
1. Assemble the XK-3 and turn the lock switch ON, as outlined in the preceding section.
2. Place the calibration check board on a lead-free surface, yellow lead sample side up.
3. Depress the red reset button (on the back of the XK-3 just above the cable connection)
all the way in with a ball-point pen and hold it in for 10 seconds. The reset button
activates an internal circuit that resets the electronics.
4. Put the XK-3 on the check board with the yellow lead sample toward the heel of the
XK-3. Align the XK-3 on the board with the white arrows on the sides of the XK-3 at
least ll/2 inches away from the yellow sample.
5. Depress the safely handle all the way in as described in the Operating Instructions until
a new reading appears on the display.
6. Take at least 10 readings and average them. The average should fall within
±0.5 mg/cm2 of 0.0 mg/cm2. If the XK-3 has only just been turned ON, it may be
necessary to repeat this test several times before it meets the requirements. This is
B-86 Version 2.0
-------
TESTING PROTOCOL FOR THE PRINCETON GAMMA-TECH (PGT) XK-3
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
normal; the XK-3 is stabilizing, as mentioned in Section 1 of the Operating
Instructions.
7. If the XK-3 still doesn't meet the ±0.5 mg/cm2 criterion, use the reset button and repeat
the test.
8. Turn the check board around so that the arrows on the XK-3 sides are aligned with the
arrows on the yellow lead side.
9. Repeat Steps 5 through 7, using the value on the lead sample as the criterion, instead
of 0.0 mg/cm2. With new XK-3s, the check sample lead value is 1.5 mg/cm2.
10. If the averages obtained in these tests are not within the ±0.5 mg/cm2 of the value on
the lead sample, the instrument should be returned for service.
B-87 Version 2.0
-------
TESTING PROTOCOL FOR THE PRINCETON GAMMA-TECH (PGT) XK-3
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
ARCHIVE XRF INSTRUMENT INFORMATION
Date Testing Site
Contractor Manufacturer.
Model No. Serial No.
XRF Operator (Printed Name)
Source Material Source Age or Date.
Source Serial No. Detector Type
Software Version No.
Operating Parameters Used
Open shutter sampling time(s)? (fixed or variable)
If fixed, what is the duration time(s)?
Daily warm-up and calibration check used? (Briefly discuss).
Regulatory level value used for setting the XRF Instrument ? (Yes or No).
If yes, enter the value used
Other
Data File Names and Descriptions NA—The PGT does not store or download electronic
data files.
NOTE: The PGT instrument does not store or download electronic data files.
| | Check here to indicate the presence of additional comments on the back of this form.
Version 2.0
-------
TESTING PROTOCOL FOR THE PRINCETON GAMMA-TECH (PGT) XK-3
Effective date: February 5,1996
Used for February 1996 Testing by M.E. McKnight
-------
TESTING PROTOCOL FOR THE PRINCETON GAMMA-TECH (PGT) XK-3
Effective date: February 5,1996
Used for February 1996 Testing by M.E. McKnight
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B-90
Version 2.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
General Responsibilities
The XRF Operator will:
• Perform all manufacturer recommended warm-up procedures and quality control
checks, and work with the Testing Monitor and the Testing Supervisor to document
that the procedures and checks were done, what the outcomes were, and, if
appropriate, what actions were taken.
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help ensure that protocols are followed and any
deviations are properly documented.
• Download data to a computer and verify that the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed.
The Monitor will:
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help ensure the protocols are followed.
• Work with the Testing Supervisor to help ensure that protocols are followed and any
deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Ensure that the data are collected as described in the protocol.
• Collect all forms and electronic data.
• Ensure that resources are available to achieve planned testing.
• Oversee testing activities.
• Provide beginning-of-day and end-of-day instructions.
• Make primary decisions regarding any testing difficulties that may arise.
• Make sure that all testing is done safely, that all personnel on site wear dosimeter
badges during testing, that dosimeter badges are collected and analyzed after testing
is completed, and that results of dosimeter badge analysis are relayed to the badge
wearers.
• Take radiation measurements periodically around each instrument being used for
testing.
• Provide blank forms to the Testing Monitor (blank forms to be delivered to the
Testing Supervisor by QuanTech) and review forms filled out by the Testing
Monitor for completeness. The forms for the following will be used during testing:
• Testing order list • Archive XRF information
• Standard readings • Control readings
B-91 Version 3.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5,1996
Used for February 1996 Testing by M.E. McKnight
Testing Protocols for the
SCITEC MAP 4 Spectrum Analyzer
Flow Chart Summary Description Details for MAP 4
Beginning of Day
(BOD) Instruction
Yes
Complete New
INFORMATION Form.
Record the lead level(s)
ot the manufacturer
supplied painted wood
block.
Perform Warm-up
Validation Check
Record Temperature
& Humidity Data
Perform BOD QC Checks
(all six substrates).
Change to the appropriate
calibration before taking a reading
and use the calibration displayed to
fifl in the form. Verify that the
displayed calibration was
appropriate for the sample.
T
1
x>
M-Sl SEV bib lib 11209S
Instructions to include: safety issues, field form use, archive layout
and testing order, sample ID numbering for electronic data capture,
and voice-call back verification of data recording by monitor.
Modes of Operation
• Manufacturer Validation Checks: use TEST mode, use CONFIRM
mode if called for by check procedure.
• Control Blocks (BOD, EOD. and CC): use TEST mode only.
• X1: use SCREEN and TEST modes, use CONFIRM if TEST is
inconclusive.use UNLIMITED until a light goes on.
• BARE and RED NIST: TEST mode only
• BARE: TEST mode only
• X2: TEST mode only
• X3: TEST mode only
Note: "STOPPING RULE" for the unlimited mode is discussed in the
Addendum on page 7 of this protocol.
See form for needed information.
Note: The manufacturer's supplied painted wood block will be
used for all manufacturer's specified validation checks.
1. Allow to warm-up (stabilize) for 5 minutes.
2. Enter or verify:
a. the selected file names to store the data
b. the action level is set to 1.0 mg/cm'
c. any other user entered parameters.
3. Perform validation check as per the manual and manufacturer
training directives using the manufacturer supplied calibration
sample(s).
Summarize any user entered information and the calibration
procedure on the instrument INFORMATION form.
BOD (or EOD) QC checks: test a total of 6 pre-placed blocks on a
minimum of 12 inches of Styrofoam™ support. Please do not move
blocks.
Note: Per the manufacturer's instructions, the "Steer calibration
mode will be used for all metal substrates except aluminum. The "K &
L Gen" calibration mode will be used for the other test substrates.
For each block, using the precision Test" setting, test in the following
order:
a. 1 reading, yellow NIST on block
b. 1 reading, red NIST on block. IF the block is wood, THEN
collect 2 more readings using the red NIST on the block.
Record extra readings on subsequent lines ot the data form
placing a diagonal line through the unused yellow and no NIST
data blocks.
c. 1 reading, no NIST on block.
Record the data on the CONTROL READINGS form.
B-92
Version 3.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5,1996
Used for February 1996 Testing by M.E. McKnight
Testing Protocols for the
SCITEC MAP 4 Spectrum Analyzer
Flow Chart Summary
Description Details for MAP 4
Move to First or Next
Location and Take
Readings (follow
TESTING ORDER list)
Has
any of
the Following
Occurred Since the
Last Validation Check?
• Temperature A> 20°C
• XRF on Standby
> 30 Minutes?
2 Hours Past?
XRF Shut
Off?
Is the
Testing Day Half
Over?
Record Temperature
& Humidity Data
Is the
Testing Day
Within 30 Minutes of
the End?
Have 15
Locations Been
Tested Since Last
QC Check?
Stop testing, record
temperature & humidity
data, perform the EOD QC
checks, perform validation
check on instrument as final
measurement at
end of day.
Perform Continuing QC Checks.
Whichever of the two calibration
checks is not covered in the
particular calibration check, add
one more check with appropriate
blocks, as necessary, so that both
calibrations are checked in every
CC check.
The calibration mode should be selected based on the apparent
top substrate.
Modes of Operation
• XI: use SCREEN and TEST modes, use CONFIRM if TEST Is
inconclusive, use UNLIMITED until a light goes on.
• BARE and RED NIST: TEST mode only
• BARE: TEST mode only
• X2: TEST mode only
• X3: TEST mode only
Note: See forms for specific data recording instructions.
Note: If insufficient time is available during NIST
testing, X2 and X3 readings may be deleted.
1. If XRF off, allow to warm up.
2. Enter or verify:
a. the selected filenames to store the data
b. the action level is set to 1.0 mg/cm:
c. any other user entered parameters.
3. Perform validation check as per the manual and
manufacturer training directives using the
manufacturer-supplied calibration sample(s).
Summarize changes to any user entered information on
the instrument INFORMATION form.
Perform and record a final validation check as the last
measurement before leaving the site at end of day.
EOD QC checks are the same as BOD QC checks; follow same
procedure as for BOD QC checks.
Record temperature and humidity in a field notebook.
Download any electronically stored data, verify successful
transfer before clearing the memory to make room for more data.
Start next day at top of flow chart using the next sample to be
tested as the first location.
Continuing QC checks, total of 2 blocks tested on a
minimum of 12 inches Styrofoam™ support. Use blocks
matching same type as the last and next locations
(If same type for both, test same block twice).
Follow same testing order and reading times as that used
for BOD testing.
«-S3 sev iMtoiut>tiaras
B-93
Version 3.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
Morning Validation Checks
Each morning, perform a validation check on your MAP 4 instrument following these
steps. The morning validation check is performed at the test site. Record all specified
calibration/validation checks on both paper and electronic data storage; also, note when the
TEST setting was used and when the CONFIRM setting was used for all the manufacturer-
required validation checks and record the results.
1. Using rubber bands, attach the painted block of wood included with your instrument to
MAP 4's faceplate. Make sure the painted side faces the instrument. Make sure the
orientation of the painted block to the faceplate is the same for all tests.
2. Position MAP 4 so that there are at least 3 feet open air between the instrument front
and the nearest surface. Maintain this distance for the duration of each measurement.
Do not point the instrument near another person or where a person is likely to
approach.
3. Take 5 measurements at Test precision. Be sure to use appropriate codes to identify
these as validation checks. This will be important for your records.
4. Using the forms supplied by SCITEC, record the results as follows:
a. Record the results of each individual measurement, and so on. Also record the time
and date the measurements were taken.
b. Average together the results of the tests and record this number.
c. On the Calibration Check Graph write the average on the first available line under
Recorded Averages.
d. On the graph, plot the location of the average as it compares to SCITEC's average
(written on the Average line). For example, if your average is .3 higher than
SCITEC's, place an "x" at .3 above the Average line.
5. Repeat these steps each morning and carefully monitor the location of the "x'"s on the
graph. Any of the following trends could indicate that your instrument is not
functioning properly:
• A trend of eight or more readings above or below the Average line,
• A trend going from high to low (or low to high).
B-94 Version 3.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
• A consistent pattern of "too high" or "too low" readings, random, but widely
scattered.
6. If you notice any of the above trends, contact SCITEC at 1-800-4NO-LEAD.
Continuing Validation Checks
Frequent validation checks should be made at the worksite while you are testing, following
these steps:
1. Take 1 measurement at Test precision on a NIST standard backed by a sample of
substrate material.
2. Write the results of each individual Daily Calibration Check.
3. If the result of any of these individual checks is off of SCITEC's average by more than
±.2 mg/cm2:
a. Take a Confirm measurement.
b. If you're off by more than ±.1 of SCITEC's average, take one more Confirm
measurement.
c. If you're still off by more than ±.1, contact SCITEC.
Validation Check Codes
The code entered for a validation check measurement should indicate the date, time, who
was using the instrument, and which instrument was used. We suggest the following
coding system.
Date
02255
T
Feb. 25,
1995
Time
0745
T
7:45 a.m.
Operator
No.
7240
T
From
Operator's
Certificate
MAP 4
Serial No.
177
T
Last 3 digits in
your instrument
serial No.
B-95 Version 3.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
Date A five-digit date is used.
• The first two digits indicate the month, e.g., 02 = February.
• The second two digits indicate the day, e.g., 09 = the ninth.
• The final digit indicates the year, e.g., 5 = 1995.
Time Military time is used. Four digits must be entered.
• 0700 = 7.00 a.m.
• 1200 = noon
• 1345 = 1.45p.m.
Operator This is the four-digit number on your Operator's Spectrum Analyzer
Number Training Certificate
Serial These are the last three digits in the serial number assigned to your MAP 4
Number instrument.
Taking a Measurement
The standard assay command on the ASSAY menu allows you to take measurements using
the selected precision, calibration, and action level. Before taking measurements be sure
that these are set appropriately (see Section 3: MAP 4 Operation's Manual).
To Take a Measurement
1. Display the Standard assay command. You can do this by pressing Go To from
any command.
2. Press ENTER/YES. MAP 4 asks for a code to identify this measurement. The
prompt varies depending on ARM mode. If ARM mode is ON, you are asked for an
ARM code. If ARM mode is OFF, you are asked for an ID code.
3. Type a code and press ENTER/YES. If ARM mode is off you are also asked for a
sequence number.
Sequence number indicates the order of measurements under a code. #1 indicates
this is the first measurement taken under code 1234567. To accept the sequence
B-96 Version 3.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
number, press ENTER/YES. To change it, press Esc No and enter the desired
number.
4. Once you've entered a code, you receive a prompt similar to start.
5. Place MAP 4's faceplate flat against the sample surface.
6. Insert the key into the lock located on the front left side of the instrument. Turn the
key clockwise into the ON position (so that the arrow on the key points up).
7. Pull the trigger and hold MAP 4 in place. After the "beep," release the trigger. A
light indicates the level of lead contamination (related to the K-Shell reading):
• Positive = lead is above the selected level.
• Negative = lead is below the selected level.
• Retest = inconclusive results. Further testing is required.
Your measurement results are displayed, similar to this:
Code Precision
01110231-1 Scrn I Note: Assay values greater
K0«10 L0«01 I than 4.99 mg/cm2 will
^^^^^^^^^^^™ be truncated
K-shel! results L-shell result to 5.00 mg/cm2.
NOTE: Record the indicator readings on the data forms as:
P (positive),
N (negative), or
I (inconclusive)
8. Turn the key to OFF position, and remove MAP 4 from the surface.
B-97 Version 3.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
9. To take another measurement press ENTER/YES.
• If ARM mode is on, you are returned to the "Enter ARM code" prompt. You
can either enter a new code or press Enter/Yes to bring up the last code used.
• If ARM mode is off, you are returned to the "TRIGGER to strt" prompt. MAP 4
has automatically assigned an ID code to the next measurement using the last
code entered and next sequence number (e.g., if the last measurement was 555-1,
this measurement will be 555-2). To take a measurement under this code, simply
position the instrument and pull the trigger. To enter a different ID start typing it;
this takes you to the "Enter ID code" prompt.
Addendum: Measurement Time for the Unlimited Mode
The stopping rule for the UNLIMITED mode will be: Test until either a light goes on, or the
displayed precision reaches ±0.1 mg/cm2 or 2 minutes have elapsed since the trigger was
pulled.
The 2-minute time limit is for a source of 11.5 millicuries (mCi). If the source strength of
the instrument is less than 11.5 mCi, the 2-minute time limit will be increased
proportionately to account for the lower source strength. For example, if an instrument
with a source strength of 9 mCi is used, the time limit for that instrument would be
2 minutes and 30 seconds (120 seconds x 11.5/9 =153 seconds, or approximately
2 minutes and 30 seconds). The time limit would never be less than 2 minutes, even if a
source stronger than 11.5 mCi is used.
B-98 Version 3.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5, 1996
Used for February 1996 Testing by M.E. McKnight
ARCHIVE XRF INSTRUMENT INFORMATION
Date Testing Site
Contractor Manufacturer.
Model No. Serial No.
XRF Operator (Printed Name)
Source Material Source Age or Date
Is instrument automatically adjusted
for source decay
Source Serial No. Detector Type.
Software Version No.
NOTE: Adjust clock time to Central Time Zone before starting tests.
Operating Parameters Used
Open shutter sampling time(s)? (fixed or variable)
If fixed, what is the duration time(s)?
Daily warm-up and calibration check used? (Briefly discuss).
Regulatory level value used for setting the XRF Instrument ? (Yes or No).
If yes, enter the value used
Other
Manufacturer's supplied painted wood block lead level(s):
Data File Names and Descriptions
| | Check here to indicate the presence of additional comments on the back of this form.
B-99 Version 3.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5,1996
Used for February 1996 Testing by M.E. McKnight
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B-100
Version 3.0
-------
TESTING PROTOCOLS FOR THE SCITEC MAP 4
Effective date: February 5,1996
Used for February 1996 Testing by M.E. McKnight
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B-101
Version 3.0
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
SUBCONTRACTOR TESTING PROTOCOLS FOR THE LEADSTAR
General Responsibilities
The XRF Operator will:
• Provide a backup instrument, to be made available on site.
• Provide the necessary serial cable (supplied with the LeadStar) to connect the
analyzer serial port on the LeadStar electronics module to the serial port on the host
computer.
• Handle the instruments and make the measurements.
• Work with the Testing Monitor to see that the appropriate data are recorded.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
• Download data to a computer provided by the Testing Supervisor, and verify that
the transfer was successful.
• Report to the Testing Supervisor any indications of deteriorating samples observed
during testing.
• Provide extra set of charged batteries to extend the testing day beyond 8 hr.
Batteries should be replaced whenever the XRF instrument indicates that the "time
remaining is less than 10%."
• Certify in writing that all test data are erased (non-accessible, non-recoverable) from
the instrument memory (as directed by the supervisor) before taking the instrument
off-site and after each day's testing.
The Monitor will:
• Record the results of the manufacturer's warmup and calibration procedures on the
appropriate form.
• Record all relevant data on the appropriate data forms or field notebooks.
• Work with the XRF Operator to help ensure that the protocols are followed.
• Work with the Testing Supervisor to help assure that protocols are followed and any
deviations are properly documented.
The Supervisor will:
• Verify ID assignments on sample locations on the archive components.
• Assure that the data are collected as described in the protocol.
• Collect all forms and electronic data and make appropriate distributions to MRI and
QuanTech.
B-102
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
Ensure that resources are available to achieve planned testing.
Oversee testing activities.
Provide beginning-of-day and end-of-day instructions.
Ensure that host computer is configured to automatically load the interlink interface
by including the following line in the config.sys file: device=c: \dos\interlink.exe
/drives :2/noprinter/com: 1
Make primary decisions regarding any testing difficulties that may arise.
Provide the following forms:
a. Testing order list d. Control readings
b. Standard readings e. Instrument calibration/calibration
c. Archive XRF information check data
f General observations and other field data
Provide the EPA Work Assignment Manager with a status report (via phone) at the
end of each day of testing.
Provide the EPA Work Assignment Manager with an oral report of deviations from
the testing protocol as soon as possible during the course of the testing, with a
written report to follow no later than one working day after the completion of
testing.
Ensure that all personnel who enter the archive facility during XRF testing wear
dosimeter badges, and will arrange for the testing of the badges and reporting of
results after completion of testing.
Take radiation measurements near the instrument periodically during the course of
the testing, compare the measured values to the corresponding values in the
instrument Operator Manual. If radiation levels significantly exceed the values
listed in the operator's manual, testing will be stopped and the EPA Work
Assignment Manager will be notified. The radiation measurement instrument will
be calibrated for the energy range of 57Co and appropriate window thickness.
B-103
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
Flow Chart Summary
Description Details for Advanced Detectors
Beginning of DayN
(BOD) Instruction )
Complete New
INFORMATION
Form
Successfully Complete
Warm-up & Calibration
Yes
Perform a Manufacturer
Calibration Check
(Section lll-A-5 of Manual)
Stop and Consult
Manual
Does the
calibration check
pass?
Turn Off
Automatic Averaging
I
Record Temperature
& Humidity Data
Perform BOD
QC Checks
(all six substrates)
I
1
NX
Instructions to include: safety issues, field form use, archive
layout and testing order, Sample ID numbering for electronic data
capture, voice-call back verification of data recording by monitor.
The Fixed Mode will be used with a setting of 15 (nominal)
seconds, and the Brief Mode will be used to test X1 only with a
maximum setting of 30 (nominal) seconds. Both modes make
adjustments for source decay.
See form for needed information.
1. Allow to warm-up for 5 minutes.
2. Enter or verify:
a. the selected file names to store the data
b. the action level is set to 1.0 mg/cm2
c. any other user entered parameters
3. Perform calibration as per the manual and manufacturer
training directives using the manufacturer supplied calibration
sample(s). (Instrument Operation Instructions, Section III-A,
of the LeadStar Operator Manual, dated March 1996,
specifically: Subsection 4 - calibration.)
4. Perform calibration check as per the manual (Section III-A,
Subsection 5). The calibration checks are to be performed on
the RED NIST (1.02 mg/cm2) standard film over the wood
control block over styrofoam.
Summarize any user entered information and the calibration
procedure on the instrument INFORMATION form.
Note: The instrument calibration and calibration check readings
are separate and distinct form the test series QC controls -
Record each on separate forms provided. Determinations as to
whether the instrument is in calibration will be made based on the
results of the calibration and calibration checks. Results of the
BOD, EOD, and continuing QC control checks will not in
themselves be used to determine if an instrument is or is not in
calibration, but may be used as grounds to call for a calibration
check by the operator.
BOD (or EOD) QC checks: test a total of 6 pre-placed blocks on a
minimum of 12 inches of Styrofoarrv™ support. Please do not
move blocks.
For each block, using a nominal 15-second reading (Fixed Mode),
test in the following order:
a. 1 reading, yellow NIST on block
b. 1 reading, red NIST on block. IF the block is wood, THEN
collect 2 more readings using the red NIST on the block.
Record extra readings on subsequent lines of the data form
placing a diagonal line through the unused yellow and no
NIST data blocks.
c. 1 reading, no NIST on block.
Record the data on the CONTROL READINGS form.
M-38 hoot/tata oeorae
B-104
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
Flow Chart Summary
Move to First or Next
Location and Take
Readings (follow
TESTING ORDER list)
Has
any of the
following occurred
since the last successful
calibration check?
• XRF shut off
Temperature change >10°C
1 XRF on standby > 30 min
• One hour passed
Operator suspects
instrument
malfunction
Perform a
Calibration Check
(Section lll-A-5
of Manual)
es the
calibration check
pass?
Yes
Stop and Consult
Manual
Is the
testing day half
over?
Record Temperature
& Humidity Data
Stop testing,
record temperature
& humidity data,
perform the EOD QC
checks, THEN perform a
manufacturer calibration
check as last reading
of the day.
Is the
testing day
within 30 minutes of
the end?
Have 15
locations been
tested since last QC
check?
Perform Continuing
QC Checks
Description Details for Advanced Detectors
For each testing location (158 samples), using a
nominal 15-second (Fixed Mode) reading, test in the
following order:
a. 1 reading, on X1
b. 1 reading, on bare (P1) + red NIST
c. 1 reading, on bare (P1)
d. 1 reading, on X2
e. 1 reading, on X3.
f. Set nominal (max.) time to 30 seconds and read
x1 only in Brief mode.
Record the length of time it takes to measure X1 in the
Brief mode only.
IF XRF off, allow to warm up for 5 minutes.
Enter or verify:
a. the selected filenames to store the data
b. the action level is set to 1.0 mg/cmz
c. any other user-entered parameters
Summarize changes to any user-entered information
on the instrument INFORMATION form.
Note: Sample data must be preceded by a successful
calibration and bracketed by successful calibration
checks. If there is a failure in a calibration check
(failure means two successive tries at a calibration
check both of which are outside the interval of 0.82 to
1.12), sample measurements from the point of the last
successful calibration check must be redone with a
recalibrated instrument.
B-105
EOD QC checks are the same as BOD QC checks; follow
same procedure as for BOD QC checks.
Record temperature and humidity in a field notebook.
Download any electronically stored data, verify successful
transfer before clearing the memory to make room for more
data.
Start next day at top of flow chart using the next sample to
be tested as the first location.
Continuing QC checks, total of 2 blocks tested on a
minimum of 12 inches Styrofoam™ support. Use blocks
matching same type as the last and next locations (If same
type for both, test same block twice).
Follow same testing order and reading times as that used
for BOD testing (i.e., use the nominal 15-second reading
for testing a-c).
06-38 hoot/Ult K (MOMS
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
Archive XRF Instrument Information
Date Testing Site
Contractor Manufacturer
Model No. Serial No.
XRF Operator (Printed Name)
Source Material Source Age or Date
Source Serial No. Detector Type
Operating Parameters Used
Open shutter sampling time(s)? (fixed or variable)
If fixed, what is the duration time(s)?
Daily warm-up, calibration, and calibration check use? (Briefly discuss).
Regulatory, level value used for setting the XRF instrument? (Yes or No)
If yes. enter the value used
Other
Data File Names and Descriptions
| | Check here to indicate the presence of additional comments on the back of this form.
Supervisor Date
96-34 ichel Irm 072SM
B-106
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
GENERAL OBSERVATIONS AND OTHER FIELD DATA
Date of testing:
XRF instrument:
Recorded by (name and date):
Temperature and Humidity Data
Time of
measurement
Temperature
%RH
Instrument ID:
Start of testing
Mid-test
End of testing
Radiation Measurements
Time of
measurement
Orientation
Reading
Instrument ID:
B-107
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
GENERAL OBSERVATIONS AND OTHER FIELD DATA, cont.
General comments and observations on XRF instrument performance during testing,
exceptions to the protocol, etc.:
Describe the data file downloading and XRF instrument file deletion procedures used:
Statement of Confidentiality by operator attached.
B-108
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
STATEMENT OF DATA CONFIDENTIALITY
(to be signed by the XRF Instrument operator)
It is understood and agreed by , representing
(printed name)
_, that for the XRF tests performed on
(company name)
, the data are not to be disclosed or discussed
(dates of testing)
with any manufacturer or vendor or any outside party other than the U.S. EPA or its
representatives.
Furthermore, by my signature below, I certify that all the data files generated by these
tests and recorded in the XRF instrument's electronic memory have been deleted, purged,
and made non-accessible prior to removing the instrument off-site from the archive test
facility. I understand that I and the company I represent will be liable for any fraudulent
use or disclosure of these data.
Signed
Date
B-109
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
Page
of
Archive XRF Test Data
Calibration Data for LeadStar XRF Instrument
Date
Standard used
Recorder
XRF Device Advanced Detectors. Inc.. LeadStar Serial number
Time of
measurement
K-shell
(mg/cm2)
K-shell
(mg/cm2)
uncertainty
L-shell
(mg/cm2)
L-shell
(mg/cm2)
uncertainty
Density
Seq No.
Was the instrument warm-up successful? Dyes D no If no, stop and consult manual.
Does the measurement meet the K-shell tolerance range? D yes D no If no, stop and consult manual.
and tolerance range =
Nominal value =
General observations or exceptions to the protocol:
for the calibration standard.
NOTES:
a The calibration procedure is specified in Section 111-4 of the instrument Operator manual, dated March 1996.
Calibration and calibration checks are performed using a nominal 15-sec fixed mode.
b Per Section lll-A-2,3 of the Operator's Manual: The "warm-up" period of ~ 5 min is automatically performed when the
instrument is turned on; after this step is completed, the instrument prompts the operator to run the calibration.
c Record K-shell data on control charts during testing; the tolerance range for calibration is specified on back of
the calibration standard.
B-110
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
Page
Archive XRF Test Data
Calibration Check Data for LeadStar XRF Instrument
of
Date
Standard used
Recorder
XRF Device Advanced Detectors. Inc.. LeadStar Serial number
Time of
measure-
ment
AV3
K-shell
(mg/cm2)
K-shell
(mg/cm2)
uncertainty
L-shell
(mg/cm2)
L-shell
(mg/cm2)
uncertainty
Density
Seq
No.
Indicate
Pass (P) or
Fail (F)
General observations or exceptions to the protocol:
NOTES:
The calibration procedure is specified in Section 111-5 of the instrument Operator manual, dated March 1996. Automatic
averaging is turned on, 3 readings are taken, and the average of the 3 readings should be within or equal to 1.12 to
0.82 mg/cm2 for the calibration check to be successful. (Use the AV3 reading for this determination.)
Per Section lll-A-2,3 of the Operator's Manual: The "warm-up" period of - 5 min is automatically performed when the
instrument is turned on; after this step is completed, the instrument prompts the operator to run the calibration.
Record K-shell data on control charts during testing; the tolerance for the calibration check is +0.1 to 0.2mg/cm2 of
the theoretical standard level, that is, 1.12 to 0.82 for the 1.02 mg/cm2 NIST standard.
Calibration and calibration checks are performed using a nominal 15-sec fixed mode.
If calibration check fails criteria, stop and consult protocol and manual for corrective actions.
B-lll
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
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-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
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B-113
-------
TESTING PROTOCOLS FOR THE LEADSTAR
with Software Version 4.1 or higher
Effective Date: August 9, 1996
Used for August/September 1996 testing by subcontractor
References:
The following table lists XRF operation manuals used for protocol development.
List of XRF Operator Manuals Used in Protocol Development
Company name
Advanced Detectors, Inc.
1220 Avenida Acaso
Camarillo, CA 93012
NITON Corp.
Bedford, MA 01 730
NITON Corp.
Bedford, MA 01 730
Princeton Gamma-Tech, Inc.
1200 State Road
Princeton, NJ 08540
RMD, Inc.
44 Hunt Street
Watertown, MA 01 721
SCITEC Corp.
415 N. Quay
Kennewick, WA 99336
SCITEC Corp.
415 N. Quay
Kennewick, WA 99336
TN Technologies, Inc.
P.O. Box 800
Round Rock, TX 78680-0800
Warrington, Inc.
21 13 Wells Branch Pkwy
Austin, TX 78728
Xsirius, Inc.
1220 Avenida Acaso
Camarillo, CA 93012
Title
Lead Star Operator Manual
(Software Version 4.1 or higher)
Operating Procedures for the NITON XL Lead
Detector
User Manual, XL Spectrum Lead Detector
PGT XK-3
Lead-in Paint Analyzer Instruction
Manual
User's Guide to the LPA-1 Lead Paint Analysis
System
MAP 3 — Standard Operating Procedures for
Lead-based Paint Testing with the MAP XRF
Specimen Analyzer
MAP 4 — Operations Manual
The MAP XRF Specimen Analyzer
Pb Analyzer Users' Guide
(Revision 1.01)
Microlead I Instruction Manual
(Revision 4)
LeadStar Operator Manual
Date
March 1996
December 21,
1994
Not specified
January 4,
1993
June 1995
print date
August 7, 1995
Not specified
October 1994
Not specified
May 30, 1995
B-114
-------
Appendix C
Supplemental Protocols for
Sampling, Characterization, and Analysis of
Lead-based Paint Samples
Contents
Collection of Paint Chip Samples from Archive Materials C-l
The Measurement of Paint Thickness on the Archive Samples—Protocol C-9
Sampling Procedure for Control Blocks [Revised 5/17/95] C-29
Density Measurement Procedure for Control Blocks [5/17/95] C-33
Microwave Assisted Acid Digestion of Environmental Samples (SW-846
Method 3052) C-37
Procedure for Changing the Archive Testing Order (August 12,1996) C-51
-------
Collection of Paint Chip Samples
from Archive Materials
c-i
-------
PAINT CHIP COLLECTION PROTOCOLS
Effective Date: December 22, 1994
COLLECTION OF PAINT CHIP SAMPLES FROM ARCHIVE MATERIALS
SUMMARY
This document describes the standard protocol for obtaining a single paint chip sample
from a painted substrate. This standard also includes instructions for sample storage and
transport requirements.
MATERIALS AND EQUIPMENT
ITEM
No. per pair of collectors
Safety goggles
Leather gloves
Disposable gloves
Respirator with organic vapor filters
Razor blade holder
Razor blades
Wood chisel
Hammer
Tweezers
Micrometer
White paper, 8.5 x 11
Masking tape
Duct tape
Marking pens
Clip board with timepiece
"Paint Chip Collection" data forms
Sample containers (plastic centrifuge tubes, plastic
resealable bags)
Resealable plastic bags
Extra shipping container for paint chip samples
Trouble lights and spare bulbs or equivalent lighting
Extension cords
2 + 1 extra
2 pair
1 bag 100 pair
2 - one fitted to each collector
2 + 1 extra
25
2
1
2
1 per team
300 sheets
20 rolls, 1-inch
8 rolls, 2-inch
6
2 + 1 extra
Enough for 200 samples
a minimum of 200 tubes
a minimum of 200 1 qt bags
4
2
200 ft.
C-2
-------
PAINT CHIP COLLECTION PROTOCOLS
Effective Date: December 22, 1994
ITEM No. per pair of collectors
Power HOVatsite
Pocket knife 2+1 extra
Metal marking template 2
Heat gun 2
Replacement heat gun element 2
Tool pouch with belt 1 per tester
Fire extinguisher 1 at site
Note: Other items as needed.
COLLECTION PROCEDURE
At each sampling location, perform the following steps (See Note 1):
NOTE 1: A regular sample will be collected at all locations. Some locations will
require collection of an additional sample called a side-by-side sample. Locations that
require a side-by-side sample are identified by the presence of an individual 2 in x 2 in
square placed at one end of the marked location. For locations having a side-by-side
sample, follow steps 1 through 9 below for collection of the regular sample first. After
completing this sample collection, collect the side-by-side sample using the same
procedure using different bar code number as described in step 2.
1.0 FILL OUT FORM:
1.1 For each new "Paint Chip Collection Reporting" form needed (see attached),
complete the header of the form.
1.2 Record the sampling location identification number in the appropriate column and
row on the form.
2.0 LABEL PAINT COLLECTION CONTAINER:
Label a paint collection container with the sampling location number and the sample ID
type separated by "-" (for example; 905507-P3).
C-4
-------
PAINT CHIP COLLECTION PROTOCOLS
Effective Date: December 22, 1994
3.0 SCORE SAMPLING AREA:
Using a metal template and a cutting tool, score the perimeter of the designated area to
be removed. Collect nominal 2 inch by 2 inch samples whenever possible unless
otherwise indicated on the sample. If it is impractical to use the template, the score
can be made using the outside edge of the template as a guide. The area scored using
the alternative method should be done in a manner that maintains right angle corners
as close as possible. Avoid using pencil or pen to mark the sample outline.
4.0 SETUP COLLECTION TRAY:
Affix a closed bottom paper funnel (or other appropriate collection shape) made from
a clean white sheet of paper or equivalent collection device directly below the
sampling location. The collection device should be located as close as possible to the
sampling site but should not interfere with the removal procedure. Avoid placing tape
on any surface targeted for XRF testing.
5.0 REMOVE PAINT:
Remove paint from the scored areas using the methods described below:
5.1 PRIMARY PAINT REMOVAL METHOD: Using a heat gun, heat the sample
area. Extreme caution should be exercised when using the heat gun. Be sure to
have a fire extinguisher nearby during heat gun use. Do not overheat the sample
area, heat only until the paint becomes soft and supple. If working in teams of
two persons, have one collector heat the area while the other removes the sample
with a paint scrapper. Remove all paint down to the bare substrate. If the paint
does not become soft and supple in a minute or two, discontinue the use of heat
and try the alternative paint removal method.
Avoid the inclusion of the substrate in the collection device. If substrate does fall
into the collection device, remove only that substrate that can be easily removed
without losing any of the paint sample. Do not remove any substrate that cannot be
separated from the paint sample. The laboratory will remove extraneous substrate if
possible, under laboratory conditions.
C-5
-------
PAINT CHIP COLLECTION PROTOCOLS
Effective Date: December 22, 1994
5.2 ALTERNATIVE PAINT REMOVAL METHOD: Using the appropriate
cutting tool for a particular substrate or condition of the sample site, begin
removing the paint from the substrate. If possible, peel the paint off of the
substrate by sliding the blade along the score and underneath the paint. Remove
all paint down to the bare substrate.
6.0 MEASURE ESTIMATED PAINT THICKNESS
After completing removal of all the paint within the collection area, examine the paint
chips contained within the collection tray for appropriate intact pieces large enough to
perform a check on the paint thickness using a micrometer. If possible, use a clean
pair of tweezers to handle the paint chips. An appropriate intact piece is one that
appears to contain all paint layers with little or no substrate and has a minimum of a
1/4 by 1/4 inch surface area. If possible, perform and record with units of measure on
the form, up to three thickness measurements using appropriate intact pieces. If one
large appropriate piece is available, all three measurements can be made on that piece
in different spreadout locations. If not, attempt to use more that one appropriate intact
piece. Make a relevant entry in the comments column describing how many chips
were used to make the measurements. Care must be taken to perform the
measurement directly over the collection tray to ensure that no loss of paint occurs.
7.0 TRANSFER THE PAINT TO THE LABELED SAMPLE CONTAINER
Transfer the collected paint sample from the collection tray to the sample container,
seal the container, and place it in a plastic bag. Exercise care to ensure that all paint
taken from the recorded area is placed into the sample container. Use the Styrofoam
holder that comes with the sample containers to aid in holding the container during
transfer.
8.0 MEASURE AND RECORD THE SAMPLING AREA
Carefully and accurately measure the sampling area dimensions. Do not attempt to
calculate areas in the field. Record the data and dimensions including units used (e.g.,
5.1 cm x 5.0 cm) on the data form using a permanent marker. Try to use only
centimeters for recording data. Avoid making measurement in inches. Any
irregularities or problems that arise in the process should be noted in the Comments
column of the form.
C-6
-------
PAINT CHIP COLLECTION PROTOCOLS
Effective Date: December 22, 1994
9.0 PERFORM FINAL CHECKS AND STORE SAMPLE
Verify the record keeping on the sample just collected by examining the data form
entries and sample container just filled. Place the collected sample into a designated
box until shipment can be made back to the laboratory. Return all completed forms
and samples by the end of each sampling day to the field supervisor.
SUBSTRATE CLEARING PROCEDURE
For sample locations that have no cleared XRF bare area, paint must be cleared down to the
substrate adjacent to the PI sample area. At these locations, after collection of the PI
sample, collect sample from the XRF bare area down to the substrate in the same manner
as collecting other paint samples. If possible, collect paint to enlarge the exposed substrate
area to approximately the same width as the adjacent painted XRF testing area. All
locations are to be collected into one sample collection container and labeled as a "-P4"
sample. More than one set of area dimensions may be required to identify the total area
collected for "-P4" samples.
C-7
-------
PAINT CHIP COLLECTION PROTOCOLS
Effective Date: December 22, 1994
Archive Paint-Chip Collection Reporting Form Page of
Date Paint thickness units of measure
Field Sampler (Prhted name)
Sample Type: PI _ OrfchaL P2 _ Orfehal FbB D upfcate, P3 . Nsw FbH Repfcate, P4 -PI Complement
Location ID
Sample Type
Dfnensbns of Area
Sampled (cm x cm)
Paint Thickness
Comments
-------
The Measurement of Paint Thickness
on the Archive Samples
C-9
-------
The Measurement of Paint Thickness
on the Archive Samples
Protocol
For U.S. Environmental Protection Agency
Office of Pollution Prevention and Toxics
Battelle Task Order 1-08
Subcontract No. 103639-G002421
MRI Work Assignment No. 5020-08
C-ll
-------
Protocol Approval
Protocol Title: The Measurement of Paint Thickness on the Archive Samples
Origin Location: Battelle Memorial Institute and Midwest Research Institute
WA Leader(s): Tom Kelly and Paul Constant
Organization WA Leaders(s)
and Program Managers
EPA/OPPT WA Manager(s)
Tom Kelly, Battelle
Date
Samuel Brown
Date
Bruce Buxton, Battelle
Date
John Schwemberger Date
Jack Balsinger, MRI
Date
Paul Constant, MRI
Date
Richard Schmehl
QuanTech
Date
Distribution
EPA: S. Brown
J. Scalera
J. Schwemberger
MIST: M. McKnight
Battelle: B. Buxton
T. Kelly
MRI: J. Balsinger
P. Constant
C-12
QuanTech: R. Schmehl
G. Dewalt
-------
Tooke Protocol
Revision 3.0
November 3, 1995
1 of 10
Protocol for the Measurement of Paint Thickness
on the Archive Samples
Introduction
This document provides a testing protocol for measuring the paint thickness on the
Lead-based Paint Archive samples using an OG202 Tooke Paint Inspection Gauge
(Figure 1). This testing protocol is divided into three sections. Section 1 outlines the
procedure to select the measurement locations; Section 2 provides the procedure for the
calibration of the Tooke gauge, and Section 3 provides the procedure for the paint
thickness measurements.
Figure 1. OG202 Tooke Paint Inspection Gauge
(approximately actual size)
C-13
-------
Tooke Protocol
Revision 3.0
November 3, 1995
2 of 10
1 Measurement Location Selection Procedure
The measurement location selection procedure describes the selection, identification,
and labeling of the two test locations used for performing the thickness measurements
with a Tooke gauge. Section 1.1 provides the operational criteria, Section 1.2 provides
procedures for classifying the archive sample test areas, and Section 1.3 gives the
documentation requirements for the location.
1.1 Operational Criteria
Following area operational criteria for the Tooke gauge:
• Paint layers must be sufficiently intact to permit a small v-groove (~ V32 in wide
by V4 in long) to be cut through the paint down just into the underlying base
substrate.
• A small mark called a "benchmark" must be drawn, using a contrasting color,
across the surface of the paint prior to making the v-groove. This mark is used
to identify the top of the paint surface when the paint layers are viewed with the
microscopic portion of the Tooke gauge.
Following are the criteria for the archive project:
• Avoid potential damage to XRF areas or destabilization of any of the
measurement areas of an archive sample.
• Do not measure where the paint is likely to be damaged in testing due to the
presence of textured or paper surfaces.
• Collect normal spatial variability data by:
a. Measuring the paint thickness on each sample at two (2) separate locations
whenever possible. If more measurements are needed, the EPA WAM and
the WAL/Supervisor will decide if there are enough painted areas on the
sample to do more measurements without having a significant impact on the
use of the sample for XRF measurements.
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b. Measuring the paint thickness on each sample to ensure that the chosen area
for measurement is representative of the normal paint thickness and not of a
step-wise progression of different paint layers where one layer is partially
peeled off and repainted leaving several visible layers of paint.
1.2 Archive Sample Substrate Considerations
When the Tooke gauge is used on different substrates, the nature of the substrate
must be evaluated and the samples must be assessed for the possibility of causing
excessive damage to painted surface. Therefore, before the archive sample is marked,
the following must be considered:
• On wood or other directional material, incisions must be made in the grain or
"machine" direction to avoid ragged cuts.
• With some coatings, improved cuts can be achieved by speeding or slowing the
cutting rate.
• Coatings with poor adhesion qualities, even though not apparent during visual
inspection, exhibit a ragged line at the substrate interface.
1.3 Selection of Measurement Location and Documentation
An undamaged surface in the test kit area should be used to perform thickness
measurements because these areas are already partially damaged and cannot be used for
other nondestructive type testing. The decision as to which location to select for
performing thickness measurements depends on the test kit area and the type of
classification.
Archive samples are classified by one of five types identified below and presented
in Attachment 1 for individual archive samples.
• Type A samples: Archive samples, where the test kit area is in good condition
and two (2) locations are selected, one in the test kit area closest to the XRF
bare substrate area and the other farthest away from the XRF bare substrate area.
• Type B samples: Archive samples, where the test kit area is in poor condition
and the usable areas must be carefully selected. Two locations are selected to
maximize the distance between the two measurement locations, as indicated for
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Revision 3.0
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type A samples. In addition, care should be taken to ensure that all layers of
paint are present and that paint adhesion is sufficient to measure the thickness.
• Type C samples: Archive samples, where the test kit area is in bad condition
and one location can selected within the test kit block area. If necessary, a
location could be placed just outside the test kit area, provided that the
operational criteria are met.
• Type D samples: Archive samples, where the test kit area is unusable or does
not exist, but ample area is available outside of the XRF areas for measurements.
Two locations are selected, one each on opposite sides of the primary XRF test
area (XI).
• Type E samples: Archive samples, where the test kit area is unusable, or does
not exist, and there is little or no area available outside the XRF area. The
archive sample is reviewed for possible measurement locations. If no area is
acceptable for the measurements after the review, the samples are not measured
for paint thickness.
The documentation for each measurement location includes:
• Applying operational criteria (Section 1.1) to the sample test area and evaluating,
classifying, and documenting them in a project notebook.
• Identifying the thickness measurement location by:
a. Writing a small number (1, 2, 3, etc.) next to the selected location using an
indelible ink pen. Cartesian coordinates will be recorded, in inches, to the
closest 1/4 in for each thickness measurement. Record these coordinates in
appropriate columns of the thickness data form (Attachment 2). Cartesian
coordinates will be measured starting from the 0,0 ordinate which is indicated
on each archive samples location with a "0." This "0" is located on the
lower, left-most corner of the archive template with a few exceptions that are
generally limited to those samples that have no test kit areas. For all
samples, the 0,0 ordinate is located at a corner of a testing area. Use the
following procedure to measure the coordinates:
(1) Using the inch grid plastic overlay sheet, place the sheet on the sample
and line-up the 0,0 point on the sheet with the 0,0 ordinate on the
sample.
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(2) Align the x and y axis on the overlay sheet to coincide with the edges
of the template.
(3) It is important to record cartesian coordinates in the same manner as
was done for the other testing areas to ensure consistency of the data
within the database for this project Therefore, using a copy of the
originally completed cartesian coordinates data for the other testing
areas as a tool, verify proper alignment of the overlay sheet by
comparing the coordinates of center of the XI testing area to the
originally recorded coordinates. Shift the overlay sheet slightly, as
needed, to ensure that the new x and y coordinates match the originals
for the XI testing area. Care should be taken when shifting the
overlay sheet to maintain the axis alignments of the overlay sheet
parallel with the template reference lines.
(4) Holding the template in place, record the x and y coordinates of the
center of the thickness v-groove. Be sure to circle the negative signs
for negative coordinate data entries to ensure accurate communication
of the coordinates.
b. Circling the number.
c. Drawing a line from the circled number to the area where the thickness
measurement is to be performed. This line is drawn so that it will serve as
the "benchmark" line that is required to use the Tooke gauge.
v-groove to be cut
here with the Tooke
gauge
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Recording data for each sample including: the archive location, the ID
numbering convention of "Sample ID No."—"Thickness Location No." (for
example: 81711-1), and the paint thickness reading.
2 Calibration and Check Procedure for the Tooke Gauge
The original calibration at KTA-Tator, Inc., was performed by setting the guide
studs in a precise geometric alignment with the cutting tips. The calibration was
verified using precision-applied film standards. The geometric alignment of the Tooke
gauge will not change unless it is physically damaged; therefore, the manufacturer
recommends that calibration be verified periodically using film thickness standards
within the normal working range of the materials being tested.
Since a procedure for the preparation and calibration of the Tooke gauge is
necessary to ensure reliable measurements, the following procedure for instrument
preparation and calibration will be conducted. The use of the procedure will ensure that
the gauge is ready to use, that the calibration has been verified, and that a system is in
place to check the consistency of readings during the paint thickness measurements of
the archive samples.
2.1 The Tooke gauge is prepared for use by checking that:
• there is no physical damage to the gauge
• the gauge is clean
• the batteries are working, and replacement batteries are available
• the light is operational
• the three cutting tips are in good condition and locked in place in the gauge
2.2 Initial and continuing calibration checks:
The calibration of the Tooke gauge is verified using the NIST Certified Coating
Thickness Calibration Standards (Table 1). The range for the three sets of SRM 1362a
(1362a-91.179, 1359-92.233, and 1363a-93.116) is from 1.57 mils (40.0 Mm) to
30.80 mils (782 um). Each of the NIST Certified Coating Thickness Calibration
Standards consists of four (4) coupons (standards) on a card. The coupons measure
30 mm x 30 mm, which is enough area to accommodate 8 cuts in the practical usable
area. Since change in the readings occurs only when the gauge or cutting tip is
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Revision 3.0
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damaged, new cuts are made in the SRMs only if the gauge or tip has been damaged or
if the cutting tip shows significant wear.
Table 1. Certified Coating Thickness Calibration Standards
SRM No.
1362a-91.179
1359-92.233
13623-91.179
1359-92.233
13623-91.179
13623-91.179
13633-93.116
13633-93.116
13633-93.116
1359-92.233
13633-93.116
1359-92.233
Film Thickness
(urn)
40.0
48.3
77.9
138.0
146.0
207.0
256
399.0
492.0
513.0
617.0
782.0
Film Thickness
(mils)
1.57
1.90
3.07
5.45
5.75
8.15
10.08
15.69
19.37
20.20
24.30
30.80
Calibration
initial/final continue
Xa
b
b
b
b
b
X
b
b
b
b
X
X
b
b
X
b
b
X
b
b
X
b
X
a SRMs used (X).
b These calibration standards will be reserved for future measurements.
When the archive samples are being measured for paint thickness, a minimum of
three (3) initial calibration thickness measurements are made on the newly cut (grooved)
NIST standards. A continuing calibration check is made on previously scribed grooves.
Since different coupons are selected for the continuing calibration than for the initial
calibration, there will be at least two new scribes out of the 10 continuing calibrations
during the measurement process. After every 15 archive samples, a continuing
calibration measurement is made that is the closest to the thickness of the last measured
archive sample. These NIST SRMs encompass the expected range of paint thickness
found in the archive samples. The three (3) cutting tips used to scribe the NIST SRM
are given in Table 2. Newly cut grooves in the NIST SRMs for continuing calibration
checks will be made after every 30 measurements of the archive samples and at the end
of the measurement activity. Newly cut grooves also will be made, with the approval
of the supervisor, if there is perceived damage to the cutting tip.
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Tooke Protocol
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Table 2. Cutting Tip Selection Guide
Cutting tip
1x
2x
10x
Maximum coating
thickness
50 mil
20 mil
3 mil
Uncertainty of thickness
determination
±0.25 mil
±0.13 mil
±0.025 mil
1 Division on the reticle
scale represents
1.0 mil
0.5 mil
0.1 mil
The procedure for the initial calibration is as follows:
• Select the NIST coupon card (4 standards) and place in a holder designed to
assist in properly scribing the measurement groove.
• Using a black or blue marker, draw a short horizontal line (= V4") on the selected
NIST calibration standard (Table 1).
• Select a cutting tip that provides the lowest uncertainty, but for which the film
thickness does not exceed the maximum coating thickness (Table 2).
• Place the Tooke gauge with the selected tip against the SRM surface slightly
above the horizontal marked line to form a tripod with the cutting tip and the
guide studs.
• Maintain moderate pressure but continuous three point contact and draw the
gauge down against the SRM surface, starting with the cutting tip slightly above
the horizontal marked line. Cut a short (= V4 in) v-groove across the horizontal
marked line.
• Using the microscopic portion of the gauge, view the intersection of the
horizontal marked line and the v-groove. If the image of the groove is unclear,
focus the image using the thumb screw located on the body of the gauge below
the microscope. If the reticle (scale) image is unclear, sharpen the reticle image
by adjusting the eyepiece of the microscope.
• Using the wall of the groove with an angle of > 45°, align the top edge of the
paint with one of the major divisions of the reticle image and count the number
of units (marks) between the top and the bottom of the paint layer. Record the
clock time, the cutting tip used, and the measurement reticle image on a copy of
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Tooke Protocol
Revision 3.0
November 3, 1995
9 of 10
the report form "Calibration Measurements for the Tooke Gauge"
(Attachment 2). Also indicate in the comment column if a new scribe was used
for the measurement.
• Calculate the paint film thickness by dividing the number of units read on the
reticle image by the cutting tip designation.
Example: The reading of 12 units using cutting tip 2x
12
mil = — = 6 mils paint thickness
^
or for um, the conversion is mils x 25.4
(12)(25.4) ,„.
um = _—_ '- = 152.4 um
NOTE: The precision of individual observations of a uniform coating on a smooth
substrate has been determined to be within ± 10 % (ASTM D4138-94 "Standard
Test Methods for Measurement of Dry Film Thickness of Protective Coating
Systems by Destructive Means").
3 Paint Thickness Measurement Procedure
Following is a summary of the testing procedure for the thickness measurement
activities. The order in which the measurements are taken is the same as the XRF
measurement order.
3.1 Using a black or blue marker, draw a short horizontal line (= V4 in) at the selected
thickness measurement location.
3.2 Determine the cutting tip to be used according to Table 2. Select a cutting tip that
provides the lowest uncertainty, but for which the likely paint thickness does not
exceed the maximum coating thickness. If the paint thickness can not be estimated,
use the 2x tip.
3.3 Place the Tooke gauge with the selected tip against the painted surface slightly
above the horizontal marked line to form a tripod with the cutting tip and the guide
studs.
3.4 Maintain moderate pressure, but continuous three point contact, and draw the gauge
down against the painted surface starting with the cutting tip slightly above the
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Tooke Protocol
Revision 3.0
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10 of 10
horizontal marked line. Cut a short (~ V4 in) v-groove across the horizontal marked
line.
NOTE: Care must be taken to avoid damaging any of the painted surface areas
when using the Tooke gauge in cutting the grooves. Avoid sliding the gauge across
existing paint edges.
3.5 Using the microscopic portion of the gauge, view the intersection of the horizontal
marked line and the v-groove. If the image of the groove is unclear, focus the
image using the thumb screw located in the body of the gauge below the
microscope. If the reticle (scale) image is unclear, sharpen the reticle image by
adjusting the eyepiece of the microscope.
3.6 Using the wall of the groove with an angle of > 45°, align the top edge of the paint
with one of the major divisions of the reticle image and count the number of units
(marks) between the top and the bottom of the paint layer. Record the
measurement from the reticle image using a copy of the report form "Measurement
of Paint Thickness" (Attachment 2).
3.7 The paint film thickness is calculated by dividing the number of units read on the
reticle image by the cutting tip designation.
Example: The reading of 12 units using cutting tip 2x
12
mil = — = 6 mils paint thickness
2*
or for |jm, the conversion is mils x 25.4
(12)(25.4) .„,
= _ — _ - L = 152.4
3.8 If the cutting tip is found to be inappropriate for the measured thickness, select a
different cutting tip and mark a new area immediately adjacent to the first cut with
the next number and identify the location (Section 3. la). Make a new cut and
measure the paint film thickness (3.3-3.7).
C-22
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Attachment 1
C-23
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Testing Order Numbers of Archive Samples for Each Board Classified by Type for
Use for Paint Thickness Sample Selection
BOARD
A
B
C
D
E
F
G
H
1
J
K
L
M
N
O
P
Q
R
S
Back
Sides
(All
Boards)
TYPE (see page 3 of 10)
A
65, 91
127, 132, 140,
143
15, 96, 153
76, 138
44, 78, 99
93
25
20
6, 67, 90
81
10, 16, 48, 149
36, 83
84, 123, 135, 145
18,29,39, 108,
136
60
B
80
62, 70, 103, 104,
150
54, 112
92
40, 47, 121
12,28,45, 117
49,68
98, 124, 146
11,61, 131
23,52, 106, 129,
142
1, 8, 130, 144
42
17,55
82, 139
46,58, 113
74, 95, 154
72, 122
2,59, 107, 118
C
75, 137
22,38
9, 120, 125
3, 33, 87, 94
105, 128
85, 100
13, 119
34, 50, 64, 79,
152
88
14,41, 114,
133
27,35, 116
21 , 26, 30, 37,
43, 102
73A, 113A,
115A
77
D
51
115
109
24
56
63, 134
7
5,4
31 , 32, 53, 69,
71 , 73, 86, 89,
97, 126, 141,
148
E
66
101, 151
111, 147
110
57
8A
19
C-24
1-1
-------
Attachment 2
C-25
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Date:
Measurements taken bv:
Calibration Measurements for the
Cal.
type*
Testing
clock
time
SRM ID
Cutting
tip
Measurement
(scale
units)
Tooke Gauge
Calculated
thickness
(mils)
Comments
* Calibration type—1 = beginning of the day; 2 = continuing; 3 = end of the day.
Pg Of
C-26
2-1
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a
00
ed
U
hickness
H
e
2
*M
1
V
=
s
1
E
o
O
Calculated
thickness
(mils)
t .
(D »
EC
(D 3
3 (D
II
Q.
_C
0
•E ^
0
o
•c
eo „
0 x
Q
^
(0
CO
c -
ffl O
C-27
2-2
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Sampling Procedure for Control Blocks
[Revised 5/17/95]
C-29
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Sampling Procedure for Control Blocks Revised 05/17/95
EPA Contract No. 68-DO-0137
1. Background
There is need to determine the lead content of each of the six
control blocks used in the test of portable XRF devices. The
control blocks are of the following material: brick, concrete,
plaster, metal, drywall, and wood. An important step to this end
is to obtain a representative sample from each type control block.
The principal assumption made is that the material of each block is
homogenous throughout.
2. Equipment
1 Adjustable speed drill press
1 Drill press vise
1 High-speed, % metal drill bit for metal, wood, plaster, and
drywall control blocks
1 Carbide-tip, % masonry drill bit for brick and concrete
control blocks
1 8-in x 10-in plastic photo-developing tray
2 Wood blocks (2-in x 4-in x %-in) for keeping the jaws of
the vise from damaging the control blocks
1 Funnel
Gloves and safety eye glasses
baby wipes and laboratory wipes
6 Centrifuge tubes
Labels for the centrifuge tubes
3. Sampling procedure
3.1 Place each control block in a clean Ziploc bag and seal.
3.2 Adjust the drill press so that its angular velocity is slow
enough for the material drilled to stay on top of the control
block.
3.3 Don safety glasses and blow down the drill press and the
drill press vise. Don a pair of gloves, and then wipe down
the drill press, vise, and drill bit, using baby wipes
followed by laboratory wipes. Be sure all parts are dry.
Place drill bit in chuck and tighten chuck.
3.4 Place the clean plaastic photo-developing tray on the drill
press table.
3.5 Remove and dispose of gloves. Don a new pair of gloves.
C-31
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3.6 Remove control block from plastic bag and place in vise.
Place a wood block on either side of the block and secure the
block in vise.
3.7 Place vise into photo-developing tray. Adjust drill press so
that drill bit will penetrate the block but will not break
the bottom surface of the block.
3.8 Drill at least three holes to the depth desired to obtain
sufficient sample, carefully retracting drill bit from each
hole.
3.9 Carefully remove block from vise and transfer drilled material
from the top of the block into a clean centrifuge tube via a
clean funnel. Secure top onto centrifuge tube. Label the
tube using indelible ink with the control block set number,
substrate type, date, and collector's name. Remove gloves and
dispose of them.
3.10 Repeat steps 3.2 through 3.9 until samples required have been
acquired.
3.11 When ready to digest sample, shake centrifuge tube to
thoroughly mix the particulate material... Subsample to obtain
the amount of material needed, and proceed with weighing and
other necessary steps in preparing the sample for analysis.
Note: One of the peer reviews of the report commented that collected material should be
ground before subsampling, as drilling may produce large particles or pieces. The
protocol above was found to provide adequate samples; however, this step recom-
mended by the reviewer will be added to the above protocol if this protocol is used
in future work.
C-32
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Density Measurement Procedure for Control Blocks
[5/17/95]
C-33
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Density Measurement Procedure for Control Blocks 05/17/95
EPA contract No. 68-DO-0137
Density measurements of each control block (brick, concrete,
plaster, metal, drywall, and wood) will be made by the following
procedure:
For metal, drywall, and wood control blocks -
1. Weigh the control block and record mass measurement in
grams.
2. Measure the width, length, and depth of the control block
and record each measurement in cm.
3. Calculate the volume of the control block in cm3.
4. Calculate the density of the control block by dividing the
mass by the volume. Record the density determined.
For brick, concrete, and plaster -
Since these control blocks are not of uniform shape, cut out a
uniform sub-block, and then follow the following procedure:
1. Weigh the control block sub-block and record the mass
measurement in grams.
2. Measure the width, length, and depth of the control block
sub-block and record each measurement in cm.
3. Calculate the volume of the sub-block in cm3.
4. Calculate the density of the subunit by dividing the mass
by the volume. Record the density determined.
C-35
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Microwave Assisted Acid Digestion of
Environmental Samples
(SW-846 Method 3052)
C-37
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Title of Method: Microwave Assisted Acid Digestion of Environmental Samples
(SW-846 Method 3052)
1 Summary of Method
1.1 A representative sample of up to 0.5 g is digested in 9 mL of concentrated nitric
acid and 3 mL hydrofluoric acid for 15 min using microwave heating with a suitable
laboratory microwave unit. The sample and acid are placed in a fluorocarbon heavy
duty microwave vessel (HDV). The vessel is capped and heated in the microwave unit.
After cooling, the vessel contents are transferred to volumetric flasks, diluted to volume,
and analyzed by the appropriate SW-846 method (ASF-601, ASF-602). The method is
based upon EPA draft Method 3052, Revision 0, January 1995.
1.2 This method is applicable to the microwave assisted acid digestion of ash and other
siliceous wastes. Sludges, sediments, soils, and oil contaminated soils may be digested
using this method if a total decomposition (relative to the target analyte list) analysis is
required. This method is applicable for the following elements:
Aluminum Bismuth Gold Molybdenum Strontium
Antimony
Arsenic
Boron
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Titanium
Vanadium
Zinc
1.3 This method is provided as a rapid multielement, total acid digestion prior to
analysis protocol so that decisions can be made about the site or material. Digests and
alternative procedures produced by the method are suitable for analysis by flame atomic
absorption (FLAA), graphite furnace atomic absorption (GFAA), inductively coupled
plasma optical emission spectroscopy (ICP-OES) and inductively coupled plasma mass
spectrometry (ICP-MS) (see Appendix A, Table A-l for estimated detection limits).
2 Required Information
To perform this procedure, the following minimum amount of information is
required:
1. Project charge number
2. List of all samples to be processed
3. Sample matrix type
C-39
1-1
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4. List of analytes
5. Assessment of sample hazard level and any special safety precautions
6. Required QC information including a list of samples to be spiked and/or
prepared in duplicate, required spiking analytes, spike levels, and spiking
procedure
7. Copies of relevant analysis plans, quality assurance plans, interoffice memos,
etc.
3 Apparatus and Materials
All glassware and plasticware should be cleaned according to SOP ASF-201.
Microwave vessels should be cleaned according to manufacturer's specifications.
3.1 Heavy duty microwave vessels (Figure 1)
3.2 Graduated cylinders: 100 mL
3.3 Analytical balance capable of weighing to an accuracy of 0.0001 g
3.4 Analytical balance capable of weighing 1 kg to an accuracy of 0.01 g
3.5 Volumetric flasks with stoppers: 100 mL, Class A or polypropylene if hydrofluoric
acid is used.
3.6 Centrifuge
3.7 Centrifuge tubes: polyethylene with screw caps, 50-mL capacity
3.8 Food service towels
3.9 Kimwipes
3.10 Filter paper, Whatman 541, or equivalent
3.11 Plastic or glass funnels
3.12 Gloves: disposable, powderless, vinyl
3.13 Funnels: plastic or glass sized to fit into the 100-mL volumetric flasks and
Whatman 541 filter paper
C-40 2
1-2
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3.14 Centrifuge tubes: plastic, sized to fit available centrifuge, minimum volume of
20 mL
3.15 Microwave apparatus requirements (CEM Model MDS 2100)
3.15.1 The microwave unit provides programmable power with a minimum of 600 W,
which can be programmed to within ±12 W of the required power. Typical units
provide a nominal 600 to 1200 W of power. Temperature and pressure monitoring and
controlling the microwave unit is desirable. The temperature performance requirements
necessitate the microwave decomposition system to sense the temperature to within
±2.5°C and automatically adjust the microwave field output power within 2 seconds of
sensing. Temperature sensors should be accurate to ±2°C; verification at two points
> 50°C apart should be determined periodically. Temperature feedback control provides
the primary control performance mechanism for the method.
3.15.2 The microwave unit cavity is corrosion resistant and well ventilated.
3.15.3 All electronics are protected against corrosion for safe operation.
3.15.4 The system requires fluorocarbon (HDV) lined digestion vessels (80- to
120-mL capacity) capable of withstanding pressures up to 40 atm (580 psi) and capable
of controlled pressure relief at pressures exceeding 40 atm (580 psi).
3.15.5 A rotating turntable is employed to ensure homogeneous distribution of
microwave radiation within the unit. The speed of the turntable should be a minimum
of 4 rpm.
CAUTION: A safety concern relates to the use of sealed containers without pressure
relief valves in the unit. Temperature is the important variable controlling the reaction.
Pressure is needed to attain elevated temperatures but must be safely contained. How-
ever, many digestion vessels constructed from certain fluorocarbons may crack, burst, or
explode in the unit under certain pressures. Only fluorocarbon (such as PFA or TFM)
lined containers with pressure relief mechanisms or container with PFA-fluorocarbon
liners and pressure relief mechanisms are considered acceptable at present.
4 Reagents
4.1 Milli-Q reagent water: minimum resistance of 16.67 M£i-cm or equivalent
4.2 Concentrated nitric acid (HNO3)—70% to 71%: Baker Instra-Analyzed or
equivalent
4.3 Concentrated hydrochloric acid (HC1): 35% to 38%: Baker Instra-Analyzed or
equivalent
C-41 3
1-3
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4.4 Concentrated hydrofluoric acid (HF): 48% to 51%: Baker Instra-Analyzed or
equivalent
5 Quality Control
Quality control samples to be prepared along with submitted samples are discussed
in the following sections and summarized in Table 1. Not all of the QC samples listed
may be required for every project. QC samples may be added or deleted from the sug-
gested list for other projects. Project specific QC requirements with be outlined by the
appropriate person: facility manager, project leader, or designee prior to starting this
procedure.
Table 1. Quality Control Samples
QC samples
Definition
Typical frequency
Method blanks
Spiked samples
Duplicates (either
duplicate of samples
or spikes)
Laboratory control
spike (LCS) (spiked
method blank)
Reference material
(standard reference)
Milli-Q reagent water—digest as a sample with addition 1 per 20 samples, a
of all reagents. Should reflect the maximum treatment minimum of 1 per
given any one sample. batch
A portion of a sample is fortified with all the target 1 per 20 samples per
analytes before preparation. Analytes, standards, and matrix type, a minimum
spike levels are specified by the facility manager, of 1 per batch
project leader, or designee.
Two equal portions of a homogenized sample are
prepared and analyzed independently, or two spiked
samples are prepared at the same spike level from the
same sample.
A blank is fortified with all target analytes before
preparation. Analytes, standards, and spike levels are
specified by the facility manager, project leader, or
designee.
A material of known composition, where the analyte
levels are certified by the manufacturer (e.g., lead paint
dust from NIST).
1 per 20 samples per
matrix type, a minimum
of 1 per batch
2 per 20 samples, a
minimum of 1 per
batch
As required by project,
usually 1 per batch of
samples
A batch of samples is defined as a group of samples which are prepared together in
a specified time period (see Appendix A, Table A-2 for a complete list of samples to be
processed along with QC sample).
5.1 For each batch of samples, a method blank (Milli-Q water and reagents), a spike, a
spike duplicate, and two LCS are typically carried throughout the entire sample prepara-
tion and analytical process. The inclusion of a reference material and the choice of
either a duplicate sample or a duplicate spike is specified in the quality assurance
project plan. Any questions must be directed to the Work Assignment Leader.
C-42
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5.2 Spiked samples are processed on a routine basis with each sample batch to estimate
method accuracy expressed as percent recovery, relative to the true spiked value. A
spiked sample is a sample aliquot (split from an original sample) which is spiked with a
known amount of analyte. All standard stock sources and concentrations used for
spiking are recorded in the laboratory notebook. The facility manager, project leader, or
designee will provide directions on the analytes and spiking levels to be used for each
specific project. Spiked samples are typically processed at a frequency of 1 for every
20 actual samples per matrix type. A minimum of 1 spike is required for each batch
processed.
5.3 Duplicates of samples and/or spikes will be prepared to provide precision data on
sample batch processing. At least one duplicate should be processed at a frequency of
1 for every 20 samples per matrix type. A minimum of 1 duplicate and/or spike
duplicate is required for each batch processed.
5.4 An LCS (a spiked method blank) is not required in SW-846 Method 3052;
however, it is recommended. An LCS is a method blank which is spiked with the
analytes of interest and is digested. Two LCSs should be processed with each batch of
samples. The LCS is used to verify sample preparation efficiency in the absence of
sample matrix effects. If spiked sample recovery data do not meet data quality objec-
tives, then the LCS will be used to determine whether this is a result of losses during
the sample digestion procedure or is likely due to sample matrix effects.
6 Interferences
6.1 Very reactive or volatile materials that may create high pressures when heated may
cause venting of the vessels with potential loss of sample and analytes. The complete
decomposition of either carbonates, or carbon-based samples, may cause enough pres-
sure to vent the vessel if the sample size is greater than 0.25 g when used in the 80- to
120-mL vessels with a pressure relief device capable of withstanding pressures up to
40 atm (580 psi).
6.2 Most samples will be totally dissolved by this method with judicious choice of the
acid combinations used. A few refractory compounds, such as TiO2, alumina, and other
oxides may not be totally dissolved.
7 Procedure
7.1 Preliminary Activities
Before samples are prepared, the following information must be provided:
1. Samples to be prepared
C-43 5
1-5
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2. QC samples:
• Number of blanks
• Number of spikes
• Number of duplicates
• Number of LCSs
• Number and type of reference materials
3. All spiking levels including:
• Level in sample
• Stock standards
• Any dilutions of standards
• Spike volumes
7.2 Temperature control of closed vessel microwave instruments provides the main
feedback control performance mechanism for the method. Control requires a tempera-
ture sensor in one or more vessels during the entire decomposition. The microwave
decomposition system should sense the temperature to within ±2.5°C and permit adjust-
ment of the microwave output power within 2 seconds.
7.3 All volumetric ware must be carefully acid washed and rinsed with reagent water
according to ASF-201. Microwave vessels are cleaned according to the manufacturer's
specifications.
7.4 Sample Digestion
7.4.1 Balance Calibration Check
The balance calibration should be checked at a minimum of one level, equal to
approximately the tare and actual weight of the sample or microwave vessel. Standard
weights should be Class S.
• For sample weights, the observed mass of the calibration weight (not including
the tare weight) must be within 0.5% of the reference mass. Since a 500-mg
sample is to be weighed into a vessel: an empty vessel is tared, and then a
500-mg calibration weight is added, and it must give an observed mass of 500
±2.5 mg. This check should be done before and after sample weighing.
• For vessel weights, the observed mass of the calibration weight must be within
the tolerance of the balance. Since the balance tolerance is ±0.01 g, the observed
mass of the weight should be within 0.01 g of a reference mass.
• If the balance calibration does not pass this test at the beginning of weighing, the
balance should be repaired or another balance should be used.
C-44 6
1-6
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• If the balance calibration does not pass this test at the end of weighing, the
samples or standards should be reweighed using a balance that can meet these
requirements.
• Balance calibration results and the MRI number of the calibration weights should
be recorded in the project records documenting the preparation of samples.
7.4.2 Calibration of Microwave Equipment
Since the microwave unit uses temperature feedback control to follow performance
specifications of the method, only the temperature probe is calibrated once every
6 months using the manufacturer's recommended procedure. The temperature of the
system is checked by immersing a thermowell containing the fiber optic probe in a
beaker of water at room temperature. The temperature is compared to a thermometer
that is NIST traceable. If the temperature of the system and the NIST traceable
thermometer drops by more than 1.5°C, recalibrate the system. Record in a notebook
the system temperature and the thermometer readings.
7.4.3 Weigh a well-mixed sample to the nearest 0.001 g into the fluorocarbon sample
vessel liner. For soils,, ash, sediments, and sludges use no more than 0.5 g. For oil-
contaminated soils use no more than 0.2 g.
7.4.4 Add 9 mL concentrated nitric acid and 4 mL concentrated hydrofluoric acid in a
fume hood. Either a repipettor or Eppendorf pipet may be used. If a vigorous reaction
occurs, allow the reaction to stop before continuing. The hydrofluoric acid content may
be varied by ±2 mL as the method is a performance-based method and optimal concen-
trations of hydrofluoric acid depends on the silicon dioxide content of the sample.
Samples with higher concentrations of silicon dioxide > 70% may require higher con-
centrations of hydrofluoric acid. Alternatively, samples with smaller concentrations of
silicon dioxide < 10% may require much less hydrofluoric acid.
7.4.5 Add 4 mL concentrated hydrochloric acid in a fume hood If a vigorous reaction
occurs, allow the reaction to stop before capping the vessel. Cap the vessel and torque
the cap according to the unit manufacturer's directions. Weigh the closed vessels to the
nearest 0.01 g. Place the vessels in the microwave carousel. This alternative acid addi-
tion is appropriate for the stabilization of Sb and Ag and high concentrations of Fe and
Al. It will, however, limit the analysis to flame atomic absorption (FLAA), and induc-
tively coupled plasma emission spectroscopy (ICP-ES) and eliminate the analysis by
both graphite furnace atomic absorption (GFAA), and inductively coupled plasma mass
spectrometry (ICP-MS).
7.4.6 OPTION 1. If the samples still retain undigested organic matter, hydrogen
peroxide may be added prior to capping the vessels. Peroxide (30%) may be added in
small and catalytic quantities 0.1 to 2 mL with an Eppendorf if the pressure capabilities
and equipment specifications permit. Alternative and variable reagent concentrations
C-45 7
1-7
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must be implemented on equipment capable of monitoring and controlling such
reactions and demonstration of safe operation must precede its use.
CAUTION: Only one acid mixture may be used in a single batch in the microwave
to permit monitoring to uniformly be representative.
CAUTION: Toxic nitrogen oxide fumes may be evolved, therefore all work must be
performed in a properly operating ventilation system. The analyst should also be aware
of the potential for a vigorous reaction. If a vigorous reaction occurs, allow to cool
before capping the vessel.
CAUTION: Toxic hydrogen fluoride fumes may be evolved, therefore all work must
be performed in a properly operating ventilation system. The analyst should wear
protective gloves and face protection and must not at any time permit a solution
containing hydrofluoric acid come in contact with skin or lungs.
CAUTION: When adding hydrochloric acid, toxic chlorine fumes may be evolved,
therefore all work must be performed in a properly operating ventilation system. The
addition of hydrochloric acid must be from concentrated acid and not from a premixed
combination of acids as a buildup of chlorine gas will result from a premixed acid solu-
tion. The analyst should also be aware of the potential for a vigorous reaction. If a
vigorous reaction occurs, allow to cool before capping the vessel.
CAUTION: When digesting samples containing volatile or easily oxidized organic
compounds, initially weigh no more than 0.10 g and observe the reaction before capping
the vessel. If a vigorous reaction occurs, allow the reaction to cease before capping the
vessel. If no appreciable reaction occurs, a sample weight up to 0.25 g can be used.
CAUTION: The addition of peroxide should only be done when the reactive
components of the sample are known. It may react rapidly and violently on easily
oxidizable materials and should not be added if unknown organic constituents are
present.
7.4.7 Properly place the carousel in the microwave unit and connect appropriate
temperature and pressure sensors to the monitoring vessels. When temperature feedback
control is being used, six vessels either with samples and reagents or just reagents are
loaded in the carousel. The temperature of the monitoring vessel should rise to 180 ±
5°C in less than 5.5 min and remain between 180 ± 5°C for 9.5 min. The pressure
should peak between 5 and 15 min for most soil, fly ash, sludge, and sediment
samples.7'8*5 The pressure may exceed these limits in the case of high concentrations of
carbonate or organic compounds. In those cases the pressure will be limited by the
relief pressure of the vessel. All vessels should be sealed according to the
manufacturer's recommended specifications.
C-46
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7.4.7.1 For reactive substances, the heating profile may be altered for safety purposes.
The samples may be heated at a slower rate to prevent potential uncontrollable exo-
thermic reactions. The time to reach 180 ± 5°C may be increased to 10 min provided
that 180 ± 5°C is subsequently maintained for 9.5 min.
7.4.8 If calibration control is being used any vessels containing acids for analytical
blank purposes are counted as sample vessels and when fewer than the recommended
number of samples are to be digested, the remaining vessels should be filled with the
same nitric and hydrofluoric acid mixture (with HC1 also optional) to achieve the full
complement of vessels. This provides an energy balance since the microwave power
absorbed is proportional to the total mass in the cavity.4 Irradiate each group of sample
vessels.
7.4.9 If the hydrofluoric acid concentration is a consideration in the analysis technique
such as with ICP methods, a hydrofluoric acid resistant torch may be used. Alterna-
tively, boric acid at a concentration of 0.0125M H3BO3 may be added to permit the
complexation of the fluoride to protect the quartz plasma torch.
7.4.10 At the end of the microwave program, allow the vessels to cool for a minimum
of 5 min before removing them from the microwave unit. When the vessels have
cooled to room temperature, weigh and record the weight of each vessel assembly. If
the weight of acid plus sample has decreased by more than 1.0% from the original
weight (= 0.25 g), discard the sample. Determine the reason for the weight loss. These
are typically attributed to loss of vessel seal integrity, use of a digestion time longer
than 15 min, too large a sample, or improper heating conditions. Once the source of
the loss has been corrected, prepare a new sample or a set of samples for digestion
beginning at 7.3.2.
Weight difference = (Initial-digested) vessel weight
7.4.11 Complete the preparation of the sample by carefully uncapping the venting
each vessel in a fume hood. Vent the vessel using the procedure recommended by the
vessel manufacturer. Transfer the sample into a 100-mL volumetric polypropylene flask
and dilute the digest to volume with Milli-Q water. If the digested sample contains
particulates which may clog nebulizers or interfere with injection of the sample into the
instrument, the sample may be centrifuged, allowed to settle, or filtered.
7.4.11.1 Settling: If undissolved material remains such as TiO2, or other refractory
oxides, allow the sample to stand until the supernatant is clear. Allowing a sample to
stand overnight will usually accomplish this. If it does not, centrifuge or filter the
sample.
7.4.11.2 Centrifugation: Centrifugation at 2,000 to 3,000 rpm for 10 min is usually
sufficient to clear the supernatant.
C-47 9
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7.4.11.3 Filtering: If necessary the filtering apparatus must be thoroughly cleaned and
prerinsed with dilute (approximately 10% v/v) nitric acid. Filter the sample through
qualitative filter paper into a second acid-cleaned container. Samples may be
acrodisced prior to analysis.
7.5 Transfer 50 mL of the diluted digest to a centrifuge tube and analyze by ICP or
GFAA.
7.6 Obtain a printout of the digestion performance and place in the batch file for
verification of the digestion parameters.
8 References
1. Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, 3rd Ed.,
U.S. Environmental Protection Agency, Office of Solid Waste and Emergency
Response, U.S. Government Printing Office, Washington, D.C., 1986; SW-846.
2. Kingston, H. M. and L. B. lassie, "Safety Guidelines for Microwave Systems
in the Analytical Laboratory," in Introduction to Microwave Acid
Decomposition: Theory and Practice, Kingston, H. M. and lassie L. B., eds.,
ACS Professional Reference Book Series, American Chemical Society,
Washington, D.C., 1988.
3. 1985 Annual Book of ASTM Standards, Vol. 11:01, "Standard Specification for
Reagent Water, ASTM, Philadelphia, Pennsylvania, 1985, Dl 193-77."
4. Introduction to Microwave Sample Preparation: Theory and Practice,
Kingston, H. M. and lassie, L. B., eds., ACS Professional Reference Book
Series, American Chemical Society, Washington, D.C., 1988.
5. Kingston, H. M., EPA IAG #DWI-393254-01-0 January 1-March 31, 1988,
quarterly report.
6. Binstock, D. A., W. M. Yeager, P. M. Grohse, and A. Gaskill, Validation of a
Method for Determining Elements in Solid Waste by Microwave Digestion,
Research Triangle Institute Technical Report Draft, RTI Project Number 321U-
3579-24, November 1989, prepared for the Office of Solid Waste, U.S.
Environmental Protection Agency, Washington, D.C. 20460.
7. Kingston, H. M. and P. J. Walter, "Comparison of Microwave Versus
Conventional Dissolution for Environmental Applications," Spectroscopy,
Vol. 7, No. 9,20-27, 1992.
C-48 10
1-10
-------
8. Kingston, H. M. and S. Haswell, Microwave Enhanced Chemistry, ACS
Professional Reference Book Series, American Chemical Society,
Washington, D.C., 1995 (in press).
9. Kingston, H. M., P. J. Walter, E. M. L. Lorentzen, and G. P. Lusnak, Report to
NIST Office of Standard Reference Materials, "The Performance of Leaching
Studies on Soil SRMs 2170 and 2711," Duquesne University, 1994.
C-49
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Liner
Ferrule Nut
Rupture Membrane
Cover
Sleeve
Heat Shield
•Body
Figure 1. Standard Heavy Duty Vessel
C-50
1-12
12
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Procedure for Changing the Archive Testing Order
(August 12,1996)
C-51
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PROCEDURE FOR CHANGING THE ARCHIVE TESTING ORDER
August 12, 1996 page 1 of 2
NEEDED SUPPLIES and INTRODUCTION
A copy of this procedure, which is presented in two steps. The first step (A)
should be done by a different person than the second step (B).
One set of Archive Testing Order Change Forms (hereafter referred to as the
Forms).
Cards: i) business size cards (2" x 3.5");
ii) either pink or white (different in color from the cards with the current
testing order numbers);
ill) labeled 1 through 158 using large numbers so that the cards are
placed vertically (i.e., long side up and down) in their holders.
Note 1: This procedure assumes that the current testing order cards are white.
STEP A: PLACE THE NEW ORDER NUMBER CARDS
A.1 Complete the appropriate lines in the header on each page of the Forms.
A.2 Starting with Board A and moving sequentially through Board S, perform the
following at each test board:
A.2.1 Using the Forms as a worksheet, locate the first white card with the
current order number without a corresponding entry in the 1st CK column.
Pull out a pink card with the new order number and place this card in-front-
gf the white card with the current order number. Do not remove the white
card.
A.2.2 Using the Forms, place an "X" in the 1st CK column on the appropriate
row to indicate that a pink card has been placed over the white card with
the current order number.
A.2.3 Repeat steps A.2.1 and A.2.2 until all samples on the board show only pink
cards (no white cards showing). Before moving to then next board, verify
that an "X" has been entered in the 1st CK column on all rows of the
Forms for this board letter. If not, then investigate, make corrections, and
note any needed corrective action in the comments column of the Forms
before moving on to A.3.
A.3 Go to the next board letter and repeat A.2 until all samples on all boards show
only pink cards.
C-53
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PROCEDURE FOR CHANGING THE ARCHIVE TESTING ORDER
August 12, 1996 page 2 of 2
STEP B: VERIFY CARD PLACEMENT AGAINST FIELD SAMPLE ID NUMBERS
B.1 Obtain the Forms used during Step A. No entries should have been made under
the 2nd CK column.
B.2 Starting with Board A and moving sequentially through Board S, perform the
following at each test board:
B.2.1 Using the Forms, identify the first new order number without an entry in
the 2nd CK column. On the board, locate the pink card with the matching
new order number and lift the plastic sleeve holder enough to view the field
sample identification number written on the board underneath the sleeve.
To verify that the field identification number on the board matches that
shown on the Forms do the following.
i) If the numbers match, then place an "X" in the 2nd CK column on
the appropriate row on the Forms to indicate that the numbers
match.
ii) If the numbers do not match, then
a) record all three numbers in the comments column of the
appropriate row: Pink = xxx, White = xxx, Field ID - xxxxxx
(where x's are the actual numbers found at that test location);
b) make corrections as needed to fix the problem noting in the
comments column what corrective actions were taken;
c) place an "X" in the 2nd CK column on the Forms,' after
corrective action was taken.
B.2.2 Repeat B.2.1 until all numbers on the board have been verified and have
"X" entries in the 2nd CK column on all rows of the Forms for this board
letter. If not, then investigate, make corrections, and note any needed
corrective action in the comments column of the Forms before moving on
to the next step.
B.3 Go to the next board letter and repeat B.2 until all samples on all boards have
been verified.
C-54
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ARCHIVES TESTING ORDER CHANGE FORM
page 1 of 8
Name of person performing 1st
Date
check
Name of person performing 2nd check
BOARD
LETTER
CURRENT
ORDER No.
NEW
ORDER
No.
1st
CK
FIELD
SAMPLE
ID
2nd
CK
COMMENTS
C-55
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50272-101
REPORT DOCUMENTATION
PAGE
1. REPORT NO.
EPA 747-R-97-004
3. Recipient's Accession No.
4. Title and Subtitle
Archive Operations Manual
5. Report Date
September 1997
6.
7. Author(s)
Dennis Hooton, Jack Balsinger, Paul Constant
8. Performing Organization Rept. No.
9. Performing Organization Name and Address
Midwest Research Institute
425 Volker Boulevard
Kansas City, MO 64110
10. Project/Task/Work Unit No.
11. Contract(C) or Grant(G) No.
68-W6-0048
12. Sponsoring Organization Name and Address
U.S. Environmental Protection Agency
Office of Prevention, Pesticides and Toxic Substances
Office of Pollution Prevention and Toxics
Washington, D.C. 20460
13. Type of Report & Period Covered
Final Report
14.
15. Supplementary Notes In addition to the authors listed above, the following people contributed to this report: B. Diel, G. Wester,
R. Friesen, and S. Cogbill; G. Dewalt and R. Schmehl of QuanTech, Inc. Also, the authors want to thank and acknowledge
Dr. Thomas Kelly of Battelle Memorial Institute for his technical guidance and administrative support, and Dr. Mary McKnight of the
NIST for her technical advice, comments, and support.
16. Abstract (Limit: 400 words)
An archive of selected housing components were collected during a multi-city field study on lead-based paint
technologies (Report No. EPA 747-R-95-002a). The archived housing components represent a variety of substrates
(drywall, concrete, brick, metal, plaster, and wood) which were found to have both high and low-level lead contamination
in the paint as determined by chemical analysis of paint chip samples. The archive has been used to study the
technical performance of different portable X-ray fluorescence (XRF) instruments by statistical evaluation and
comparison to laboratory analysis data and quality control samples. This report documents the operation of the archive
facility and the testing protocols used during its operation. Based on the archive testing, technical performance of the
XRF instruments is measured in terms of bias and precision relative to the amount of lead contamination and category
of substrate. The results of the XRF testing are published as XRF Performance Characteristic Sheets (PCS) which are
available from the National Lead Information Center by calling 1-800-424-LEAD.
17. Document Analysis a. Descriptors
lead-based paint, lead-based paint testing, archive facility, evaluation testing, testing new instruments
b. Identifiers/Open-Ended Terms
X-ray fluorescence instruments, XRF instruments, portable XRF, XRF testing protocols,
XRF Performance Characteristic Sheets, PCS
c. COSATI Field/Group
18. Availability Statement
19. Security Class (This
Report)
UNCLASSIFIED
20. Security Class (This
Page)
UNCLASSIFIED
21. No. of Pages
208
22. Price
(SeeANSI-Z39.18)
See Instructions on Reverse
OPTIONAL FORM 272 (4-77)
(Formerly NTIS-35)
Department of Commerce
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