United States     Atmospheric Research and Exposure
Environmental Protection Assessment Laboratory
Agency       Research Triangle Park, NC 27711
                                            June 1993
          Research and Development
                                 EPA600/R-93/130
&EPA
Workshop Report:
Identification of Performance
Parameters for Portable X-Ray
Fluorescence Measurement of
Lead in Paint

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                                                   June 1993
      WORKSHOP REPORT:  IDENTIFICATION OF
PERFORMANCE PARAMETERS FOR PORTABLE X-RAY
 FLUORESCENCE MEASUREMENT OF LEAD IN PAINT
                Research Triangle Park, NC
                   January 11-12,1993
                        Prepared by

                        E. D. Estes
                      W. F. Gutknecht

      Center for Environmental Measurements and Quality Assurance
                   Research Triangle Institute
          Research Triangle Park, North Carolina 27709-2194

                  EPA Contract No. 68D10009
                   RTI Project No. 5960-167
           Mr. Warren Loseke, Work Assignment Manager

      Atmospheric Research and Exposure Assessment Laboratory
               Office of Research and Development
               U.S. Environmental Protection Agency
                Research Triangle Park, NC 27711

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                                DISCLAIMER

      The Workshop described in these proceedings was sponsored by the United States
Environmental Protection Agency.  The opinions, conclusions and recommendations are
solely those of the various participants and therefore, the contents of this document do
not necessarily  reflect the views  of the  Agency.   No official  endorsement should  be
inferred.

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                          ACKNOWLEDGEMENTS

     This document  was  prepared under the direction  of  Mr.  Warren Loseke,
Atmospheric  Research  and  Exposure  Assessment  Laboratory   (AREAL),  U.S.
Environmental Protection Agency, Research Triangle Park, N.C.
     Special acknowledgement is given to Ms. Sharon Harper and Mr. Michael E. Beard
(AREAL/EPA), for their careful review.
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                            EXECUTIVE SUMMARY

      The potential impact on health from environmental lead has resulted in increased
interest in lead exposure by Federal, State and local government agencies. As a result,
programs committed to sampling and analysis of lead are increasing nationwide.  Public
housing authorities are required, by 1994, to randomly inspect ail their housing projects
for lead-based  paint  [Lead-Based Paint Poisoning Prevention Act,  42,  U.S.C. 4:22
(d)(2)(A),  1971].  Currently, the most common approach to screening housing for the
presence  of lead in paint is the use of the portable X-ray fluorescence (XRF) detector,
which gives rapid results and is non-destructive.  More than six different portable XRF
instruments are commercially available.   The  EPA  has sponsored studies of the
performance of each of several of these instruments.
      To review the  status of  portable XRF  technology,  the U.S. Environmental
Protection Agency  sponsored a  1-1/2 day  workshop limited, to Federal and State
government personnel and government contractors. The goal of the workshop was to
identify problems and limitations that could result in measurement error and to develop
a  set  of  performance parameters to generate or verify figures of merit  that are
comparable across the technology.
      The workshop  was attended by 32 persons with experience  in portable XRF
measurements. The morning session of the workshop began with a brief overview of the
purpose and goals of the workshop and was followed by presentations on the following
topics:
                   fundamentals
                   specific studies
                   future needs
                   a proposed test design
                   manufacturer's input

      In the afternoon, the attendees discussed spectral and  physical problems and
limitations of portable XRF and began to identify specific parameters or areas that need
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to be evaluated.  On the second day, the attendees continued to identify parameters that
are experimentally verifiable and to discuss general approaches to the experimental
measurement of these parameters that would allow direct comparisons of portable XRF
instruments. Details of the experiments were not determined and will require consultation
with a statistician. The parameters judged to be the most important by consensus of the
workshop participants are the manufacturer's calibration, precision, accuracy, detection
limit, substrate effects and other interferences, and ruggedness.  Other parameters that
should be  considered  in evaluating  a portable  XRF but are difficult to  measure
experimentally include training, cost, safety features, physical configuration, portability,
data retention/storage capabilities, and manufacturer's support.
                                      IV

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                            Table of Contents

DISCLAIMER	i

ACKNOWLEDGEMENTS 	  ii

EXECUTIVE SUMMARY	iii

TABLE OF CONTENTS 	  v

SECTION 1 INTRODUCTION	  1

      1.1   Goals of the Workshop 	  1

      1.2   Structure of the Workshop	 2

SECTION 2 SUMMARY OF PRESENTATIONS	:	 6

SECTION 3 GENERAL DISCUSSION	  19

SECTION 4 PERFORMANCE PARAMETERS	  23

      4.1   Introduction	  23

      4.2   Manufacturer's Calibration	  23

      4.3   Precision 	  23

      4.4   Accuracy 	  24

      4.5   Detection Limit  	  25

      4.6   Substrate Effects and Other Interferences	  25

      4.7   Ruggedness	  26

      4.8   Other Parameters 	  26

APPENDIX A  Letter of Invitation and Note of Thanks

APPENDIX B  Questionnaire Sent to XRF Manufacturers

APPENDIX C  Lists of Attendees and Manufacturers

APPENDIX D  Papers/Information Distributed by Speakers
             and Manufacturers

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                                  SECTION 1
                                INTRODUCTION

1.1   Goals of the Workshop
      Numerous programs involving research on the toxicity and bioavailability of lead,
the environmental monitoring of lead, and the abatement of lead in and clearance testing
of housing are currently active. Examples of past projects include the Housing and Urban
Development (HUD) National Survey, the Three City Study and method evaluation studies
sponsored by the U.S. Environmental Protection Agency (EPA), and abatement programs
carried out by Maryland, Massachusetts, and many other active groups.
      Public housing authorities are required, by 1994, to  randomly inspect all their
housing projects for lead-based paint [Lead-Based Paint Poisoning  Prevention Act, 42,
U.S.C. 4:22  (d)(2)(A),  1971].   That statute specifies the  use of an  on-site  X-ray
fluorescence (XRF) analyzer for measurement of lead and denominates a reading of 1.0
mg/cm2 as  a positive finding of lead-based paint.  The HUD  Interim Guidelines
(September 1990) use the XRF analyzer and the  1.0 mg/cm2 standard, but also specify
that atomic absorption analysis (AAS) or another comparable testing  technique will be
used  as a backup  or  confirmatory test  when the XRF reading  is inconclusive.
Alternatively, AAS may be used without first using  on-site XRF. The HUD Guidelines set
the level of hazard for lead as 1.0 mg/cm2 (area basis) or 5000 |ig/g (weight basis).
      Currently, the most common approach to screening housing  for the presence of
lead in paint is the use of the portable X-ray fluorescence (XRF) detector, which gives
rapid results and is non-destructive. More than six  different portable XRF instruments are
commercially available. The EPA has sponsored  studies of the performance of each of
several of these instruments.
      The U.S. Environmental Protection Agency sponsored a 1 -112 day workshop limited
to Federal and State government personnel and  government contractors to review the
status of portable XRF technology.  The goal of the workshop was to identify problems
and  limitations  that  could  result in measurement error and to develop  a set  of
performance parameters to generate or verify figures of merit that are comparable across
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the technology.   Parameters to be  included  are  detection limits, precision, bias,
interferences, productivity, safety, and  use or generation of hazardous materials.

1.2   Structure of the Workshop
      Following planning efforts by EPA and EPA-contractor staff, letters of invitation
were mailed to representatives from Federal and State governmental agencies and a
number of EPA contractors with experience in the use of portable XRF methods for
measurement of lead in paint. The intent was to invite recognized experts in the field,
while keeping the size of the workshop manageable and productive. Manufacturers of
portable XRF instruments were not invited to the workshop but were asked to complete
a questionnaire and to supply any additional information that they judged to be of value
to the workshop.
      Thirty-two representatives accepted  the invitation to  attend the workshop (see
Appendix C for list). Upon arrival, attendees received a notebook containing the following
information:
            Workshop Program
                 Agenda
                 List of Attendees
            XRF Reports
                 "First  Preliminary  Draft   Recommendation  on  Portable  and
                 Transportable  X-Ray   Fluorescence  Spectrometers   for  Field
                 Measurements  of  Hazardous  Elemental  Pollutants  (International
                 Organization  of Legal  Metrology,  OIML  Reporting Secretariat
                 PS17/RS5: USA, October, 1992)
                 "Evaluation  of  Portable  X-Ray  Fluorescence  Spectrometer  for
                 Measurement of Lead in Paint, Soil and Dust," Hardison, D. L, C. O.
                 Whitaker, J.  D.  Neefus,  E.  D. Estes  and  W.  F. Gutknecht,
                 Proceedings of 1992 EPA and AWMA International Symposium on
                 Measurement of Toxic  and Other Related Air Pollutants. Durham,
                 NC, May 1992.

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      The workshop began with a morning session of presentations on the current status
of portable XRF technology including fundamentals, specific studies, future needs, a
proposed test design, and manufacturers' input (see workshop agenda presented on page
4).   In the afternoon, the attendees discussed spectral and physical  problems and
limitations of portable XRF and began to identify specific parameters or areas that need
to be evaluated.  On the second day, the attendees continued to identify parameters that
are experimentally verifiable and to suggest experiments that would allow evaluation and
direct comparisons of portable XRF instruments.

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               GENDA
                                   FOR
            PORTABLE XRF SPECTROMETER WORKSHOP
                          JANUARY 11 - 12, 1993
               EPA Environmental Research Center, RTP, NC
      Time
    Topic
   Speaker
 Day 1 - January 11

 9:00 a.m.

 9:15 a.m.

 9:30 a.m.

 9:45 a.m.

 10:00 a.m.

 10:15 a.m.

 10:30 a.m.

 10:50 a.m.

 11:05 a.m.

 11:20 a.m.

 11:35 a.m.

 11:50 a.m.

 1:00 p.m.

1:15 p.m.
 Welcome and Overview
 Presentation by Attendees
Break
Presentation by Attendees
Lunch

Manufacturers' Input

Discussion of spectral and
physical problems/limitations
 M. Beard/S. Harper

 B. Gutknecht

 B. Clickner

 S. Weitz/M. McKnigJit

 J. Pesce

 J. Zilka



 R. Petre

 C. Papanicolopoulos

 T. Spittler

 Open



B. Gutknecht

Attendees

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     Time
    Topic
  Speaker
Day 1 - January 11

2:40 p.m.

3:00 p.m.
4:30 p.m.

Day 2 - January 12

9:00 a.m.


10:30  a.m.

10:50  a.m.
Break

Development of prototype
performance tests (spectral,
physical and statistical aspects)

Adjourn
Discussion/revision of
performance tests

Break

Continuation of discussion/
revision of performance tests
Attendees
Attendees
Attendees
12:00 p.m.
Adjourn

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                                   Section 2
                        SUMMARY OF PRESENTATIONS

       Presentations were made to provide a background for the development of a set
 of performance parameters that would be used to generate or verify figures of merit that
 are  comparable across  portable  XRF technology.   The presentations covered the
 fundamentals of the XRF method, specific studies and comparisons, future needs, and
 manufacturers' input.  Summaries are given below.

 William Gutknecht/RTI - "A Comparison of the Scitec, Warrington and Princeton
 Gamma-Tech Portable XRFs"

       The preliminary (draft)  results  of a limited evaluation  of three  portable XRF
 instruments (Scitec MAP-3, Warrington Microlead 1, and Princeton Gamma-Tech XK-3)
 were presented. The evaluation was carried out using standard films prepared from oil-
 based paint  spiked with  white lead and verified  by acid digestion/atomic absorption
 analysis.  The lead concentration of the standard films ranged from 0 to 6 mg/cm2. The
 films were placed on eight different substrates and analyzed by portable XRF, using the
 manufacturer's calibration and following the manufacturer's instructions. The substrates
 tested were 3/4" plasterboard, 3/4" plywood, 5" concrete, 4" cinderblock, 1/8" aluminum,
 1/8"  steel, brick and solid cinderblock. According to the manufacturer, no  substrate
 correction is necessary for the Scitec.  Warrington and Princeton Gamma-Tech  (PGT)
 data were substrate corrected.
      The Scitec was evaluated using two different "universal" calibrations installed by
the manufacturer.  The first  calibration covered the range 0.6 to 2.64  mg/cm2.  The
standard paint films yielded correlation coefficients of 0.98 to 0.99 and standard  errors
of estimate of x from y of -0.5  mg/cm2 for  the five substrates tested  (plasterboard,
plywood, 4" cinderblock, aluminum and brick).  Biases ranged from + 0.13 mg/cm2 for 3/4"
plasterboard to -0.29 mg/cm2 for 3/4" plywood.  The second calibration covered the  range
from  0 to 6 mg/cm2. The standard films yielded correlation coefficients ranging from 0.93

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for solid cinderblock to 0.995 for steel.  The standard error of the estimate ranged from
0.30 mg/cm2 for steel to 1.1  mg/cm2 for solid cinderblock. The bias ranged from  0.1
mg/cm2 for plasterboard to 4.4 mg/cm2 for solid cinderblock.  The bias was found to be
concentration dependent for plasterboard, aluminum, and concrete (i.e., there is a change
in the value of the bias with a change in the value of the concentration) and constant for
plywood, steel, brick and 4" and  solid cinderblock.
       The Warrington was evaluated with all eight substrates.  Correlation coefficients
were consistent, ranging from 0.990 for concrete to 0.998 for plasterboard, plywood  and
steel.  The standard error of estimate ranged  from 0.2 mg/cm2 for plasterboard, plywood
and steel to 0.4 mg/cm2 for concrete. The bias ranged from -0.04 mg/cm2 (at 1.6 mg/cm2)
for plasterboard to 1.2 mg/cm2 (at 0.3 -  0.8 mg/cm2) for concrete and was found to be
concentration dependent for all substrates.
       The PGT also was evaluated with all eight substrates. The correlation coefficients
were consistent, ranging from 0.977 for brick to 0.988 for 4" cinderblock.  The standard
error of estimate ranged from 0.39 mg/cm2 for 4" cinderblock to 0.63 mg/cm2 for brick.
The bias ranged from  0.1 mg/cm2 (at 0.3 mg/cm2) for plasterboard and cinderblock to
-1.0 to -1.1  mg/cm2 (at 1.6 mg/cm2)  for concrete, aluminum and steel. Bias was found
to be concentration  dependent for all substrates, with the greatest dependency found for
concrete and 4" cinderblock.
       To determine whether Scitec results could be improved by applying a substrate
correction, the Scitec was used to measure the substrate only  for wood, sheetrock, 4"
cinderblock, brick, aluminum siding and  steel. All substrates gave readings very close to
0 mg/cm2 (0.00 to 0.03 mg/cm2). When real-world painted boards were measured before
and after scraping, however, a different result was obtained. A board that measured 13
to 15 mg Pb/cm2 before scraping appeared to contain 1 to 3 mg Pb/cm2 after scraping;
a board that measured 6 to 7 mg Pb/cm2 before scraping yielded results of 0.1  to 3 mg
Pb/cm2 after scraping; and a board that  measured 1.7 to 2.2 mg Pb/cm2 before scraping
measured 0.0 to 0.1 mg Pb/cm2 after scraping.  One explanation for these observations
is that  lead  migrates or is driven into the substrate by the removal process. Variables
that  must be considered  in evaluating a  portable XRF  are  the calibration, substrate

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 correction, lead in the substrate, and paint variability.

 Robert Clicknef/WESTAT - "On the Performance of the Scitec MAP/XRF in the
 National Survey of Lead-Based Paint in Housing"

       Dr. Clickner discussed the performance of the  Scitec MAP-3 XRF used in the
 National Survey of Lead-Based Paint in Housing from January to March, 1990.  Scitec
 delivered eight nominally identical MAPs, each containing a fresh 40 mCi Co57 radioactive
 source and the  "universal automatic substrate correction" software.  Each MAP was
 calibrated by the manufacturer over the range 0.0 to 2.64 mg/cm2.   During the survey,
 381 housing units across the United States were tested and thousands of 60-second XRF
 measurements were  made on dozens of different substrates.
       Shims (standard paint films) from NIST with lead paint levels of 0.6 ± 0.02 and
 2.99 ± 0.3 mg/cm2 and four substrates (wood, drywall, steel and concrete) were used to
 continually check the  MAPs' performance.  Daily validation measurements were made for
 each MAP/shim/substrate combination. Regression analyses on the validation data were
 performed to estimate the precision and accuracy of the readings and to relate readings
 to  substrate  and lead loading  level.  A different equation was obtained for  each
 machine/substrate.
       For a wood substrate, readings generally were lower than the actual lead levels
 (NIST certified levels) when the levels were <2.0 mg/cm2 and higher than the actual levels
 when the levels were  >2.0 mg/cm2. Eighty-eight percent of the validation readings of the
 0.6 mg/cm2 shim on wood were <0.6  mg/cm2 and 52 percent were equal to  0.0 mg/cm2.
 (The MAP will not give a negative reading.) For the 2.99 mg/cm2 shim, 60 percent of the
 readings were >3.0  mg/cm2.  The standard deviation  of  repeated readings was 0.25
 mg/cm2.
      The performance of the MAP on drywall or plaster was similar to the performance
on wood, with readings lower than the actual levels when  the levels were <2.5 mg/cm2
and higher than the actuallevels when the levels were >2.5 mg/cm2.  Eighty-two percent
of the validation readings of the 0.6 mg/cm2 shim on drywall or plaster were <0.6 mg/cm2

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and 52 percent were equal to 0.0 mg/cm2.  At 2.99 mg/cm2, 44 percent of the readings
were <3.0 mg/cm2 and 45 percent were >3.0 mg/cm2. The standard deviation of repeated
readings was 0.25 mg/cm2.
      For a steel substrate, the readings were higher than  the actual levels for all
observed levels of lead,  and there were substantial  differences among  the eight
instruments.  Eighty-eight percent of the validation readings of the 0.6 mg/cm2 shim on
steel were >0.6 mg/cm2. At 2.99 mg/cm2, 60 percent of the readings were >3.0 mg/cm2
although one machine had  no readings above 3.0  mg/cm2.  The standard deviation of
repeated readings was 0.21  mg/cm2.
      For concrete, brick, and other related substrates, the MAP had difficulty detecting
low to moderate levels of lead, and there was much variation both among and within
instruments.  Ninety-five percent of the validation readings of the 0.6 mg/cm2 shim were
equal to 0.0 mg/cm2, and only one  machine had more than one non-zero  reading.  At
2.99 mg/cm2,  95 percent of the readings  were  <3.0 mg/cm2 and 11  percent of the
readings were equal to 0.0  mg/cm2.  The standard  deviation of repeated readings was
0.49 mg/cm2.
      In summary, the MAP readings were found to be systematically different from the
amounts of lead in the paint film standards with the direction and magnitude of the
differences being related to  the substrate material and the lead levels in the paint. The
precision of the readings also was found to be dependent upon the substrate.  On the
basis of this survey, WEST AT concluded that a substrate  correction is necessary to
accurately determine the presence  and amount of  lead-based paint on surfaces when
using XRFs similar to the Scitec MAP-3 used in the national survey of lead-based paint
in housing.

Steve Weitz/HUD - "HUD Needs"
      Mr. Weitz briefly presented the needs of the Department of Housing and Urban
Development (HUD) with respect to  portable XRF technology. The HUD Guidelines are
to be revised totally by October 1993. HUD expends considerable funding on testing and
is dedicated to producing data of the highest quality.  Because lead-in-paint data are the

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 basis for important decisions, improved instruments are needed to obtain better data. To
 develop improved instruments, a method for evaluating the current instruments is needed.

 Mary McKnight/NIST - "Evaluation of Methods for Field Measurement of Lead in
 Paint Films"

       Dr. McKnight presented a plan for evaluating field methods for measurement of
 lead in  paint.  The first step is to characterize the problem by establishing performance
 criteria, observing field practices and identifying key factors that could affect field results.
 A limited simulated field study  and a limited field study will  then  be designed.   The
 simulated field study will be carried out in a test chamber using real walls and  painted
 boards  that closely represent field samples.  The field study will be carried out in actual
 housing units. If the results of the simulated field study are consistent with the results of
 the actual field study, an expanded simulated field study will be conducted over a range
 of field possibilities (lead concentrations, environmental conditions, substrate types, etc.)
 and a knowledge-based system will be developed for assessment of equipment or field
 measurement procedures.  The data obtained in the simulated field study will be  used to
 develop a standard method or protocol for assessing equipment or other measurement
 procedures for lead in  paint.  Other benefits of a study such as this include  gaining
 precision and  bias data for the  measurements and improved  understanding  of factors
 affecting measurement  quality.

 John Pesce/Star Environmental - "An Examination of Substrate Effect on Portable
 X-Ray Fluorescence Instrumentation"

      Mr. Pesce presented the results of an investigation of substrate effect on portable
 X-ray fluorescence (XRF) instrumentation. The data presented were derived from both
 actual field use and round-robin  information.
      Princeton Gamma-Tech (PGT) XK-3 XRF analyzers were used to test  421 units
 in an apartment complex for lead in  paint.  More than 20,000 readings were taken. The
testing protocol included measurement of substrate effect levels (SELs) on all  surfaces.
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The SEL  was subtracted  from  the Apparent  Lead Concentration (ALC)  to obtain a
Corrected Lead Concentration (CLC). Sodium sulfide solution was used for confirmation
when the ALCs were 1.2 mg/cm2, and samples were taken for atomic absorption analysis
when CLCs were  0.8 - 1.5 mg/cm2.  The SEL locations also  were tested with the
Warrington and Scitec XRFs, using a "shoe" or template to fix the orientation of each
instrument.
      A variety of unpainted substrates was tested,  including masonry, cinder block,
plaster, brick, sheetrock,  concrete, wood and metal.   The PGT and  Warrington
instruments showed significant variability forthese building materials. PGT values ranged
from 0.0 mg/cm2 for pressed board to  1.9 mg/cm2 for a metal window sill. Warrington
values ranged from -1.1 mg/cm2 for a metal window sill and mailbox to 1.7 mg/cm2 for a
plaster  column and a concrete  column.   The  Scitec measured  0.0 mg/cm2 for  most
substrates.  The Scitec response was 0.3 - 0.4 mg/cm2  for metal, 0.3 mg/cm2 for a
concrete column and oak, and 0.2 mg/cm2 for sheetrock. It should be noted that the PGT
and Warrington instruments can  give a negative reading, but the Scitec cannot.
      For metals, the PGT and Warrington respond to substrate effects differently, with
the elevated  (+)  readings  of the PGT similar  in absolute value to the depressed  (-)
readings of the Warrington. All XRFs appear to work well on less dense materials such
as wood.
      Substrate  effects also were  examined as a part  of the round-robin study
established by a group of private lead inspectors in Massachusetts. Experiments were
performed using steel channel, red brick, poplar, belly casing, and sheetrock substrates.
The SEL was measured for a piece of each substrate containing no lead paint.  The
apparent lead concentration  (ALC) was measured for the  same substrate painted with
lead paint. The SEL was  subtracted to give a corrected lead concentration (CLC)  for
each substrate. For steel channel, the CLCs of the PGT and Scitec showed some lead;
the CLC of the Warrington showed no lead. For red brick, the CLCs of the PGT and
Warrington showed some lead; the Scitec detected no lead on the painted or unpainted
brick, indicating that a false negative reading can be observed.  All three XRFs identified
lead on poplar wood surfaces  although  the  quantitative results were  not in  good
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 agreement, ranging from 0.5 mg/cm2 for the Scitec to 1.2 mg/cm2 for the PGT.  A convex
 wood molding called belly casing was used to test the effects of an air gap between the
 XRF probe and the sample. Results were consistent with the results for the poplar wood
 sample.  Sheet rock samples produced consistent results with the three XRFs.
       To test for read-through effects, measurements were made on lead flashing under
 1-1/2" of wood.  The PGT appeared less susceptible to detect this type of lead, giving a
 reading of 1.7  mg/cm2.  The Warrington and  Scitec measured 10.8  and 4.6 mg/cm2,
 respectively.
       Based upon this study, it was concluded that portable XRFs can be used with a
 reasonable amount of confidence for a wide variety of substrates, assuming that the
 operator has the experience to know what the substrate is and to  make the appropriate
 corrections.  The operator must know when to doubt the  XRF and use secondary and
 tertiary screening methods.  Neither automatic or manual correction can compensate for
 all possible substrates, and the correction values vary from instrument to instrument from
 the  same manufacturer as  well as from different manufacturers.  Confirmatory testing
 should be performed prior to making abatement decisions.

 John Zilka/Applied Systems - "XRF Problems and Applications"
       Mr. Zilka presented some problems and needs with respect to use of field portable
 XRFs. Applied  Systems uses instruments manufactured by PGT, Scitec and Warrington
 and  has observed variances and reliability problems in the field, particularly with the
 Scitec. The manufacturers have provided little  support in the way of standard  operating
 procedures (SOPs) and validation.
      Two major areas of concern that Mr. Zilka would target for study are the reliability
 of the instrument and the reliability of the inspector.  Currently, Applied Systems runs
 validation checks at the  beginning of the day, hourly, and at the end of the day, but
 detailed validation procedures are needed to determine that the instrument is operating
 properly.  Training field personnel also is a big  problem. To do the job correctly, a field
tester needs  the proper tools  including  a reliable  instrument, site specific  standard
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operating procedures (SOPs) and a basic knowledge of construction materials. Currently,
there are considerable differences in what is required for an inspection and in what is
being done to meet these requirements.  For example, it is unclear how many inspectors
are actually doing  substrate corrections.
       Finally, there is a need for auditing an inspector's work to give  the client some
degree of confidence  in the results.
Roy  Petre/State  of Massachusetts Department  of  Public  Health  -  "General
Concerns"
       Mr.  Petre discussed some policy issues with respect to current standards and
future  needs.  In the past a health-based standard for lead expressed in mass/area was
used because children eating paint chips was the focus of concern.  Currently, dust is
considered to be the major source of exposure. The Childhood Lead Prevention standard
of 0.5  percent by weight for paint is high relative to  dust.   Mr. Petre suggests that the
current standards be examined carefully with respect to exposure models, animal studies,
and total dust exposure from future disturbances.
       Mr.  Petre also expressed a need for a cost-effective method for testing on-site.
Laboratory testing is expensive  and requires considerable delay  and detailed chain-of-
custody procedures.  In some  cases, it may be cheaper to replace the architectural
elements than to test them.  Taking representative field samples  for laboratory analysis
is also a problem, and scraping creates a potential hazard by putting the lead in its most
ingestible form.  One on-site method is portable XRF.  For a portable XRF to be used
with confidence, however, it should have an accuracy and precision of 0.1 to 0.2 mg/cm2.
A "wand" for testing ceilings would be a useful design feature.  A self-correction for
substrate effects  is also a  consideration  since scraping  creates dust.   It would be
desirable to design a machine that can read by layer to eliminate the read-through effect.
For example, an XRF will sometimes detect leaded paint on a plaster surface that has
been covered with wood panelling. On the other hand, thin paint films containing 2 to  4
percent lead may be cleared when an XRF is used for testing because of the  thin  layer

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 effect.  Since the portable XRF reads in concentration units of mass/area, painted
 surfaces containing high percentages of lead by weight may show lead concentrations
 below the regulatory limit if the paint is spread thinly enough.  Theoretically, a correction
 can be made for this effect. The State of  Massachusetts currently uses sodium sulfide
 for confirmatory testing, with good results, when concentrations  below the abatement
 threshold are obtained with the portable XRF.
      Mr. Petre stressed that operator effect must be addressed. Massachusetts has
 been training and licensing lead paint inspectors since 1990. An inspector must complete
 an apprenticeship under a master inspector. In addition, Massachusetts is considering
 a program to certify individual XRFs.

 Chris Papanicolopoulos/Georgia Tech Research Institute - "XRF Instrumentation"
      Dr. Papanicolopoulos presented the results of an investigation of portable XRF
 instruments. From 1987 through 1989, three Princeton Gamma Tech XK-3s were tested,
 and in 1990 some comparisons of the XK-3s, the Scitec  MAP, and the Warrington
 Microlead instruments were made. Many combinations of sample  substrates and paints
 were analyzed in the field.  A goal of the study was to identify problems and to determine
 whether they are instrument specific or generic.
      The Microlead, which has a scintillation counter detector, uses a grease between
the scintillation tube and photomultiplier tube that breaks  down after repeated use and
also in the summer (i.e., at high ambient temperature), causing inconsistent results. Also,
a  design problem was  discovered in the  electronics of the Microlead.  When it was
corrected, measurements were more reliable.
      The PGT XK-3's detector is a proportional counter that is temperature sensitive.
When the sample substrate is a dense material, backscatter can  saturate the counter.
Dr. Papanicolopoulos stated that proportional counters have "reached their limit" and
cannot be improved.
      The Scitec  detector is a semiconductor crystal that must  be "quiet" to operate
properly.  The detector can get very hot when subjected to large numbers of X-rays in a
                                      14

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short period of time and should be cooled in some way such as using the Peltier method.
Large numbers of X-rays can arise from a large amount of lead present in the sample
and/or a very dense substrate causing backscatter of a large percentage of the incident
or excitation X-rays.
      One of the major problems with the portable XRF is substrate interference.  The
PGT XK-3 does not adjust the peak height for backscatter.   If the backscatter goes up
or down,  it will be reflected in the  measured lead concentration.  The Scitec has a
proprietary formula for correcting for backscatter, but it is not appropriate for the soil
method. A better method for handling the backscatter problem is needed.
       Dr. Papanicolopoulos suggested that instruments be certified two times a year with
the resulting data forwarded to the EPA. He also suggested that there be an independent
quality assurance person to see that the instrument is being used to obtain valid results.

Thomas Spittler/EPA Region I - "Laboratory XRF"
       Dr. Spittler presented the results of analysis of paint chips by laboratory XRF.
Peeling paint chips are usually multilayered, with the inner layers containing more lead.
The outer layers frequently are newer paints containing titanium, zinc, and iron that will
absorb lead X-rays from the inner layers.  Spectra from a laboratory XRF were presented
to demonstrate that significantly different lead concentrations could result when front and
back sides of paint chips were measured independently.
      Dr. Spittler stated that paint on walls is not a threat to children unless it is  peeling
or on chewable surfaces.  Attempting to remove and analyze paint that is intact could
generate another "asbestos situation."  However, he is not convinced that portable XRFs
will give reliable results. Data from an alternative method using a  laboratory XRF were
presented.  Three standards were prepared using different weight ratios of  National
Institute of Standards and Technology (NIST) Standard Reference  Material (SRM) 1579
and somar mix (an inert material) to cover a range of from 2.00 to 9.38 percent lead. An
actual  paint  sample  then  was  ground and  blended with  somar  mix in  a  dental
amalgamator.  The standards and samples were analyzed by laboratory XRF with peak
                                       15

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 height used for quantitation.  A measured value of 23.1  percent  lead was obtained
 compared to the "true" value of 24 percent obtained by a more rigorous XRF method.
 The somar  dilution procedure (three standards and one sample) was performed in
 approximately five minutes.  Dr. Spittler stated that the cost of a good laboratory XRF is
 -40,000 (down from -$100,000) and that it can be  operated by a trained high school
 student.
       Dr. Spittler also emphasized that to determine what is poisoning a child, house
 dust and soil samples should be taken in addition to paint samples that might be posing
 a threat.

 William Gut knee ht/RTI - "Portable XRF Manufacturers' Input"

       Prior to the workshop, questionnaires were mailed to six manufacturers of portable
 XRF instruments that were identified by RTI through contacts with a variety of  people
 working on lead studies (see Appendix C). The questionnaire was designed to obtain
 information  on detection  limit, sensitivity, accuracy, calibration procedure,  operating
 procedure,  analysis time,  substrate correction  procedures,  safety  considerations,
 problems/limitations, and any envisioned improvements.  Responses were received from
 the manufacturers of the Scitec MAP-3, the Spectrace 9000 and the Princeton Gamma
 Tech XK-3.  The responses and other information can be found in Appendix  D.
      The manufacturers approached the various performance parameters  (detection
 limit, accuracy, precision) in different ways. The PGT XK-3's detection  limit of 0.5 mg
 Pb/cm2  is taken as the single-reading standard deviation of a series of readings.  The
 Spectrace 9000's detection limit of 0.01 to 0.1 mg Pb/cm2 (depending upon substrate) for
 a 200 sec assay is determined as three  times the standard deviation of repeated blank
 analyses. The Scitec manufacturer pointed out that for XRF analysis of lead-based paint,
the detection limit is a function of measurement condition, measurement time, confidence
 level, and source strength. For a 60 sec measurement, K-shell detection limits of 0.10 and
0.43 mg Pb/cm2 were found for paint on wood and concrete, respectively, based on data
from 46 different instruments with 25 repeated  measurements each.

                                      16

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      Sensitivity  is generally defined  as the change in  response that results from a
specified change in concentration. Only the Spectrace manufacturer reported sensitivity
in this form as ~50(PbJ,  ~4(PbK) cts/sec/mg Pb/cm2/mCi.  Also, only the Spectrace
manufacturer reported an accuracy; the Spectrace literature states the accuracy of their
instrument to be  +. 0.12 mg Pb for < 1 mg Pb/cm2 on  wood using a 60 sec assay.
Measurement times for a test are 60 seconds for the Scitec MAP-3 and Spectrace 9000,
and 12 seconds for the PGT.
      The Scitec and PGT instruments are pre-calibrated by the manufacturer and there
are no plans to allow  for direct user calibration or recalibration.  The PGT XK-3 is
calibrated using 10 readings each of the 0 and 1.53 mg/cm2 HUD standards. The Scitec
is calibrated using NIST 2759 standard paint films on different substrates. The Spectrace
9000 is pre-calibrated by the manufacturer using several pure element standards, various
substrates, and at least one NIST 2759 reference material. However, the calibration may
be modified by  user accessible routines via either the keyboard or the RS232 port. The
port may be protected to ensure only approved access. Keyboard changes are indicated
on the printed (or stored) record and default values can be restored.
      The portable XRFs  also use different approaches for substrate correction.  The
PGT XK-3 manufacturer recommends manual substrates  correction in accordance with
the HUD Guidelines. The Scitec MAP comes with a general or "universal" compensation
for K  and L shell X-rays that is built into the system's software.  Scitec also provides a
"dedicated" substrate correction for high density substrates such as steel, brick, concrete
and thin metals. If lead is suspected to be present in the substrate, Scitec recommends
use of NIST SRMs over the painted  surface to characterize the  substrate.  For the
Spectrace 9000, problems with overlapping X-ray  peaks or signals are identified and
characterized when  the instrument  is  calibrated  and correction factors  are applied
automatically to the spectral data to obtain a substrate corrected readout.
      All three  manufacturers  reported some type of instrument check for satisfactory
operation. A calibration check sample is provided with the PGT XK-3. The Scitec MAP
system conducts a "self test" during a 15 sec warm-up immediately after the instrument
is turned on to  determine  if all system  components are operating within specification.
                                       17

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Scitec software  used to download  measurement values verifies both  measurement
integrity and instrument performance and evaluates the calibration check readings.  The
Spectrace 9000 sounds an alarm if 1) peaks are not in the correct position; 2) the battery
is low; 3) there is unusual electronic noise; or 4) there is loss of signal. All alarms are
accompanied by a descriptive message on the screen.
      Neither PGT nor Scitec released information on planned improvements. Spectrace
envisions 1) increasing the detector area; 2) using a battery with a longer life; 3) reducing
the size of the probe for easier access to narrow spaces; and 4) more sophisticated
substrate corrections.
                                     18

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                                   SECTION 3
                             GENERAL DISCUSSION

       Following the presentations, there was a general discussion of current needs for
 portable XRF  and the spectral  and physical  problems/limitations  that  need to be
 addressed.
       Public housing authorities  are required, by 1994, to randomly inspect  all  their
 housing projects for lead-based paint.  There is, therefore, an urgent need for a reliable
 method for taking representative samples and for producing defensible data with  no false
 negatives.   The  workshop attendees generally  agreed  that an on-site,  real-time,
 nondestructive lead measurement method such as the portable XRF is of value for a
 number of reasons. Use of a reliable portable XRF would result in a considerable  savings
 of time and would not require "touching up" sampling sites after destructive  sample
 collection.
       Jim Hayes of the State  of N.C. Environmental Health Services is conducting an
 epidemiological evaluation of lead poisoned children.  Two  of the  goals of the program
 are to teach parents  the  reason  for concern and to identify potential sources of the
 contamination.  Mr. Hayes pointed out  that it is of real value  to have  an  on-site
 measurement method that can give the parents a lead concentration at the time of the
 visit without causing  damage  to  painted surfaces.   Susan Guyaux of the Maryland
 Department of the Environment  stated  that day-care  center personnel  may  react
 negatively to taking paint scrapings, and that a hazard is actually created by taking
 samples .in this way. She stressed the need for an on-site, non-destructive lead analysis
 method with appropriate laboratory confirmation. Both the field and laboratory methods
 need to be the best that they can  be.
       Dr. William Gutknecht of the Research Triangle Institute stated that portable XRFs
 "are a  reality" and that their sales are increasing.  It is anticipated that they will be used
 more in the future for soil and dust analysis.  With this in mind, the workshop attendees
turned their attention to answering questions such as:
            How "good" are the portable XRFs that are currently on the market?
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            Where and/or under what conditions can portable XRFs be used reliably?
            When is laboratory confirmation necessary?
            What are the problems and limitations of portable XRF technology?
            Is the technology improvable?
            What are the critical parameters needed to evaluate and compare portable
            XRFs?
            How can these parameters be tested?
            It  is sufficient to certify  manufacturers  or is certification of  individual
            instruments needed?

       Several groups represented at the workshop had conducted studies to compare
 lead  measurement results  obtained by  portable XRF and  by atomic  absorption
 spectrometry (AAS).   Bill Gutknecht reported that RTI found  that the XRF and AA
 generally agree although  occasional significant differences  were found.  David  Cox of
 David Cox and Associates reported that in a data base of approximately 4000 AAS vs.
 XRF measurements examined by his company, only 5 to 10 percent were serious outliers
 and there were  ~4 percent false positive results using the portable XRF.  The problem
 is that there is no way to identify the outliers when only one measurement method  is used
 and there is no way  to predict when they will occur.  John Zilka of Applied Systems
 emphasized the need for defensible data.  From his experience, hourly checks indicate
 that the portable XRF generally gives consistent readings, and he  is usually able to tell
 if the equipment is not operating properly.  However, Chris Papanicolopoulos of Georgia
 Tech Research  Institute cautioned that a portable XRF can  be consistently inaccurate.
      Based upon their  experience and expertise,  workshop attendees expressed
 opinions concerning where and under what conditions portable XRFs could  be used.
 Kevin Ashley of NIOSH stated that the portable XRF is a useful screening tool but that
the data obtained are not defensible in court. Merrill Brophy of the Maryland Department
of the Environment supported Dr. Ashley's comment and added that "for a vast majority
                                      20

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of housing," portable XRF is a first step.  However, more confidence in the XRF data is
needed.  Bob Clickner of Westat reported that the portable XRF works "fairly well" for
measurement of paint  on wood and drywall, but generally gives a high reading for paint
on steel.  Sharon Harper of the Office of Research and Development (ORD) EPA agreed
that results were good for paint on wood and drywall. David Cox warned against focusing
too much attention on a single XRF measurement.  He suggested that a better approach
is to take a set of measurements on an aggregate  to answer questions such as "Do the
doors contain lead?" and he has found that portable XRF technology works well for this.
      Much  of  the discussion  centered  upon  the  "gray  area"  where laboratory
confirmation of  an XRF measurement  is needed.  John Scalera of Office of  Pollution
Prevention and Toxics (OPPT), EPA posed two questions to the group: 1) "Is there a
definable concentration limit for XRF at which there is 95 percent confidence in the XRF
data?" and 2) "Is the  XRF useful at this concentration?"  For example, if there is  95
percent confidence in the XRF at 6 or 7 mg/cm2 and this lead concentration is commonly
found, the XRF will be a useful screening tool.  Bob Clickner reported that few  readings
above 6 mg/cm2 were found in the national Survey of Lead-Based Paint in Housing.  If
the confirmation limit was set at 6 mg/cm2 but most levels were <6 mg/cm2, almost every
measurement would require laboratory confirmation. John Zilka, however, stated that he
finds levels far in  excess of 5 or 6 mg/cm2, especially in building exteriors.
      Another factor to be considered in determining the utility of portable XRFs is the
concentration level of  lead that is  considered  dangerous.  John Pesce of Star
Environmental pointed out that there is a difference in philosophy about how much lead
is dangerous and that more data are needed to determine the capabilities of the XRF.
John Zilka stated that we need to answer the question "Is there a safe level of lead, and
is it  tied  in with the accuracy, precision, etc.  of the XRF?"   Chris  Papanicolopoulos
cautioned that the  regulatory levels will probably go lower and lower.   Since XRF
technology is already struggling, inspectors may be forced to use laboratory analyses for
all measurements.
      Jim DeVoe of NIST stated that there is a problem with the design of the portable
XRF and that more sensitivity is needed. John  Pesce reported that he sees differences
                                      21

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in day-to-day field use of the XRF, that the XRF still has trouble with the simplest (non-
real-world) samples and that substrate effects should be more closely examined.  Jim
DeVoe expressed a need for the development and availability of "reference walls" with
different substrate layering orders to simulate wall types that are encountered in the field.
Chris Papanicolopoulos stated that the instrument should have a feedback mechanism
to alert the user to improper operation or an automatic shutoff.  Kenn White of T. C.
Analytics said that, rather than asking manufacturers their capabilities, users should tell
manufacturers their needs and ask if they can be met.
                                     22

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                                  SECTION 4
                        PERFORMANCE PARAMETERS

4.1   Introduction
      After the individual presentations and the general group discussion, the workshop
attendees developed a list  of performance parameters that  could be used to make a
direct  comparison  of  portable  XRFs.   General  approaches  to  the  experimental
measurement of these  parameters were  also  discussed.  However, details of the
experiments were not determined and will require consultation with a statistician.  The
parameters judged to be the most important by a consensus of the workshop participants
are discussed in the following sections.

4.2   Manufacturer's Calibration
      Proper calibration is essential for obtaining reliable results  using any instrumental
method for analysis. Most portable XRFs currently on the market are calibrated by the
manufacturer and have no  provision for user interaction or recalibration.   Much of the
workshop discussion focused on procedures for checking the manufacturer's calibration.
The general agreement among workshop attendees is that calibration checks should be
performed at the beginning and end of each testing day and at  hourly intervals during
use. Suggested standards are the NIST films at 0.0,1.0 and 3.5 mg Pb/cm2 on both low
and high density materials representing site specific substrates. The periodic calibration
checks can be used to evaluate the stability of the calibration and to test for drift.  The
accuracy of the calibration is tested as described in Section 4.4.

4.3   Precision
      One performance parameter that can be experimentally measured is precision,
which is generally defined as the scatter of a group of measurements, made under the
same specific conditions, about their average value.  Precision may be expressed as the
standard deviation (a) or the coefficient of variation (100a/x where  x is the  average
value). Before precision can be used to directly compare portable XRFs, an experiment
                                      23

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 must be carefully designed in terms of the number of tests to be performed and the
 equation used for the calculation of precision. The workshop attendees agreed that a
 "test" should be performed as described by the manufacturer.  For the Scitec, a test is
 defined as a single 60 second reading.  For the PGT XK-3, a test is defined as the
 average of three cycles collected manually. For the Warrington, a test is defined as the
 average of three cycles collected automatically.   For both the PGT XK-3 and the
 Warrington, an initial single reading is taken at the beginning of each test but is not used.
 Test were not defined for other brands of portable XRFs.
       It was decided that NIST films at concentrations of 0.0, 1.0, 2.0, and 3.5 mg/cm2
 should be used for the precision tests. Suggested substrates for precision testing are a
 low density material such as  pine  or plastic foam, a high  density material  such  as
 concrete, and a layered substrate containing both high and low density materials such as
 wood over concrete. The latter has been found to be a major problem for some portable
 XRFs.
      The attendees agreed that the precision tests should be performed both on new
 (off  the shelf) instruments  and  on  instruments  that  have been   used  for field
 measurements for several months. In terms of source depletion, a new instrument would
 be defined as one whose source is less than 10 percent depleted and an old instrument
 as one whose source depleted  beyond 1-1/2 half lives of the excitation source. In all
 cases, a "blind" process should  be used for selection of instruments to be tested.

 4.4   Accuracy
      Another performance  parameter that  can  be measured experimentally  is the
 accuracy or bias.  Bias (B) is defined as the signed  difference between the average  (x)
 of a set of measurements of a reference material and the "true" value (T) of the reference
 material and is calculated in the units of measurement using the equation

                                     B  = X-T

or as a percentage of the true value using the equation
                                      24

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                                     %B = 100 (X-T)/T

       Bias can  be determined from the precision test data since NIST SRMs will be
used.  The data will be examined to determine whether the bias is a function of lead
concentration.
       Of concern  is the need to describe clearly the chances of making an improper
decision when an X-ray measurement result for lead in paint is compared to a decision
level.  This involves characterizing the random and systematic error components of the
method at or near the decision level. Determination of an acceptable accuracy figure for
each instrument will be possible after a definitive field study has been conducted.

4.5    Detection Limit
       Because  the regulatory limit for lead may be lowered as environmental  lead
programs continue, it is important to determine the limits of detection and quantitation.
Again, this involves characterizing the random and  systematic error components at or
near the limit of  detection.  Estimation of each instrument's detection  limit over various
substrates is expected to be possible using field study data.

4.6    Substrate Effects and Other Interferences
       The buildings to be tested under the HUD Guidelines contain  a wide variety of
building materials that can be painted with lead-based paint. Typical materials that are
encountered include wood, plaster, gypsum, concrete, brick, metal, sheetrock, and cinder
block,  and often  these materials are in tandem.  Wood over concrete and plaster over
metal mesh pose major problems for some portable XRFs.  Some instruments will give
readings higher than the regulatory limit for certain substrates when no lead is present.
Other  substrates may yield  negative readings  that will result in a lead concentration
reading that is lower than the true value.
       The different manufacturers of portable XRFs treat substrate effects (background)
in  different ways.  To determine whether a portable XRF is suitable for  a particular
purpose, the effects of various substrates should be evaluated. The workshop attendees
                                       25

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 suggested that experiments be performed using NIST films and a variety of substrates
 that cover a range of densities and thickness.  The effects of "read-through" should also
 be tested by placing an NIST film between two substrates and measuring the apparent
 lead concentration using the portable XRF.

 4.7   Ruggedness
       Because of the enormous number of lead measurements to be made and the wide
 variety of environmental conditions that are likely to be encountered, the  portable XRF
 must be field-rugged.  Workshop participants discussed a number of parameters that
 should be tested to evaluate the ruggedness of portable XRFs.
       Experiments should be performed to determine the temperature range over which
 an XRF operates satisfactorily and to determine the necessary temperature equilibration
 time.  A range of -20 °F to 120 °F was suggested.  The International Organization of
 Legal Metrology (VOIML) recommends that the instrument  be placed in an environmental
 chamber  and  warmed or  cooled  until  it is in thermal equilibrium at the  desired
 temperature.  Tests  should then  be carried out to  determine  the relative  standard
 deviation of  the output signal.
       The XRF should also be  able to withstand a reasonable mechanical shock to the
 control box such as a bump against a door facing. A "bump test" was discussed, but the
 specific procedure is yet to be determined.  The OIML describes a mechanical shock test
 that involves tilting the instrument about one bottom edge to a height of at least 50 mm
 and allowing it to fall once to the surface.
      A third  parameter  for  ruggedness  is  susceptibility to  interference  from
 electromagnetic  fields.    The OIML  recommends exposing  the  instrument  to
 electromagnetic fields at a field strength of 10 V/m and determining the relative standard
 deviation of the output signal during this exposure.
4.8   Other Parameters
      Other parameters that should be considered in evaluating a portable XRF but are
                                      26

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difficult to measure experimentally are as follows:
                   Ease of operation
                   Training  (level required; usefulness of the manufacturer's manual)
                   Cost
                   Safety features/radiation leakage/operator exposure
                   Physical configuration (handle; shutter; probe size and weight; cord)
                   Data retention/storage capabilities
                   Manufacturer's support (licensing; availability of a user "hot line;"
                   training)
                   Portability/weight of detector/probe assembly
                                        27

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           APPENDIX A
Letter of Invitation and Note of Thanks

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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
               RCH AND EXPOSURE ASSE
                ESEARCH TRIANGLE PAR
                NORTH CAROLINA 277 11
 ~*         ATMOSPHERIC RESEARCH AND EXPOSURE ASSESSMENT LABORATORY
l"*^                        RESEARCH TRIANGLE PARK
                                                            November 24, 1992
Dear          :
      Numerous programs involving research on the toxitity and bioavailability of lead,
the environmental monitoring of lead, and the abatement and clearance of lead in
housing are currently active.   Examples of past projects include the HUD National
Survey, the EPA Three City Study, method evaluation studies sponsored by EPA and
abatement programs carried out by Maryland, Massachusetts and many other groups.
      Public housing  authorities are required, by 1994, to randomly inspect all their
housing projects  for lead-based paint.  Currently, the most  common approach to
screening housing for the presence of lead in paint is the use of the portable X-ray
fluorescence (XRF) detector, which gives rapid results and is non-destructive. Currently,
more than six different portable XRF instruments are commercially available. The U. S.
Environmental Protection Agency has sponsored studies of the performance of several
of these instruments.
      The U.S. Environmental Protection Agency is sponsoring a 1-1/2 day workshop
limited  to Federal and State government personnel and government contractors to
review the status of portable XRF technology, to identify problems and limitations that
could result in measurement error, and to develop  a  matrix of performance  parameters
to generate or verify figures of merit that  are comparable across the technology.
Parameters to be included in the matrix are detection limits, precision, bias, interferences,
productivity, safety, and use or generation of hazardous materials.

-------
      As one of the recognized experts in this field, you are invited to attend  this
workshop, which is scheduled for January 11-12, at the EPA Environmental Research
Center in Research Triangle Park, NC. Unfortunately, funds are not available to pay for
attendance at the workshop.  However, this workshop offers an opportunity to make a
contribution to solving what has been called  the nation's number one preventable
childhood health problem, and it also offers an opportunity to identify future research
needs.
      If you are able to attend, please inform Dr. Eva Estes at (919) 541-5926 at your
earliest convenience.  Thank you, and  we  hope to  see  you at the portable XRF
Workshop.

                                                      Sincerely,
                                                      Warren Loseke

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     '       UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
 ^tt/      ATMOSPHERIC RESEARCH AND EXPOSURE ASSESSMENT LABORATORY
                           RESEARCH TRIANGLE PARK
                            NORTH CAROLINA 2771 1


                                         January 26, 1993
Dear         :

      Thank you  for  attending  the  Portable  XRF  Workshop held  at  the  EPA
Environmental Research Center on January 11 -12, 1993 and for presenting the results
of your work in this area. As a result of the workshop we have begun to develop a matrix
of performance parameters to generate figures of merit that are comparable across the
portable XRF technology. Your hands-on experience, knowledge of methodologies, and
real-world data were  instrumental in its success.  We  appreciate not only  your
contributions, but also the preparation and effort required for attending.
      In approximately one month you will receive a draft report of the workshop for your
comments. We look forward to continuing to work with you on this important issue.
      Again, thank you for your contributions and for your interest in lead measurement
programs.
                                         Warren Loseke

:acp

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            APPENDIX B
Questionnaire Sent to XRF Manufacturers

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              UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
             ATMOSPHERIC RESEARCH AND EXPOSURE ASSESSMENT LABORATORY
                             RESEARCH TRIANGLE PARK
                              NORTH CAROLINA 27711
                                                            December 8, 1992
Dear         :
      Numerous programs involving research on the toxicity and bioavailability of lead,
the environmental monitoring of lead,  and the abatement and clearance of lead in
housing  are currently active.   Examples of past projects include the HUD  National
Survey, the EPA Three City Study, method evaluation studies sponsored by EPA and
abatement programs carried out by Maryland, Massachusetts and many other groups.
      Public housing  authorities are required, by 1994, to randomly inspect all their
housing  projects for lead-based paint.   Currently, the most common approach to
screening housing  for the presence of lead in paint is the use of the portable X-ray
fluorescence (XRF) detector, which gives rapid results and is non-destructive. Currently,
more than six different portable XRF instruments are commercially available. The U. S.
Environmental Protection Agency has sponsored studies of the performance of several
of these instruments.
      The U.S. Environmental Protection Agency is sponsoring a 1-1/2 day workshop
                           \
limited to Federal  and State government personnel  and government contractors to
review the status of portable XRF technology, to identify problems and limitations that
could result in measurement error, and to develop  a matrix of performance parameters
to generate  or verify  figures of merit  that  are comparable across the  technology.
Parameters to be included in the matrix are detection limits, precision, bias, interferences,
productivity, safety, and  use or generation of hazardous materials.

-------
      Such discussions would be of limited productivity without input from the people
who actually  develop and  provide  portable  XRF spectrometers.  As one  of  the
recognized suppliers of these instruments, your input is crucial to the success of this
workshop. Consequently, a questionnaire has been enclosed in an attempt not only to
address the  issues described above but also to provide a means for introduction of
additional topics you may wish to see discussed.  Your timely response is needed in
order to incorporate your input into the workshop agenda.  I ask that responses be
returned by  December 31.
      A self-addressed envelope has been included for your convenience. If you have
any questions please call Eva Estes at (919) 541-5926. Thank you in advance for your
cooperation.

                                                Sincerely,

                                                Warren Loseke

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                   Portable  XRF Spectrometer
Name or Model # of spectrometer
      'Please reproduce this form if other models are available.
Applications	
                       (Paint, Soil, Dust, etc.)
Detection Limit	How is the detection limit
determined?
Sensitivity	How is the sensitivity
determined?	
Accuracy	How is the accuracy
determined?            	
Briefly describe the calibration procedure
Are there any plans to allow for direct user calibration or recalibration?

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 Are you aware of the new MIST paint film SRMs?
 Have they been of any value to you in calibrating or testing your instruments?
 Briefly describe the procedure for use of your instrument
Approximate analysis time

Interferences	
What substrate correction procedures are used?
Are their any new developments or guidelines for using substrate correction procedures?
Describe.
Are there any built-in instrument checks to test for satisfactory operation?  Describe. __

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Briefly describe safety procedures/considerations
Are there any problems/limitations with the instrument at present?
Are improvements to the current instruments envisioned?
When might an improved instrument be available?
What improvements will be implemented?
What do you view as the future needs of the public and/or lead testing organizations
regarding portable XRF spectrometers?	
What topics should be added to the XRF workshop agenda?

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Please provide any standard operating procedures, Instrumentations or other literature
you believe would be informative. :	

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           APPENDIX C
Lists of Attendees and Manufacturers

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                  Portable XRF Workshop Attendees

                         January 11 - 12, 1993
 1.   Mr. Michael E. Beard
     USEPA/AREAL
     MD-78
     RTF, NC 27711
     Phone:  (919) 541-2623
     FAX:  (919)541-0239

 2.   Dr. David A. Binstock
     Research Triangle Institute
     P.O. Box 12194, Bldg. 6
     RTF, NC 27707
     Phone:  (919) 541-6896
     FAX:  (919)541-8778

 3.   Ms. Merrill Brophy
     Maryland Department of Environment
     Lead Program
     2500 Broening Highway
     Baltimore, MD 21224
     Phone:  (410) 631-3820
     FAX:  (410)631-4112

 4.   Mr. Bob Clickner
     Westat
     1650 Research Blvd.
     Rockville, MD 20850-3129
     Phone:  (301) 294-2815
     FAX:  (301)294-2829

5.   Mr. David Cox
     David Cox and Associates
     1511 K Street, NW, Suite 738
     Washington, DC 20005
     Phone: (202) 347-3090
     FAX:  (202)347-3106

6.   Dr. Jim DeVoe
     National Institute of Standards and Technology
     Inorganic Analytical Research Division
     U.S. Department of Commerce
     Gaithersburg, MD 20899
     Phone: (301) 975-4144
     FAX:  (301) 926-6182

-------
 7.    Dr. Robert Elias
      USEPA
      ECAO
      MD-72
      RTP, NC  27711
      Phone:  (919)541-4167
      FAX: (919)541-0245

 8.    Dr. Eva Estes
      Research  Triangle Institute
      P.O. Box 12194, Bldg. 6
      RTP, NC  27707
      Phone:  (919)541-5926
      FAX: (919)541-8778

 9.    Ms. Nancy Friederich
      Midwest Research Institute
      425 Volker Blvd.
      Kansas City, MO 64110
      Phone:  (816)753-7600
      FAX: (816)753-8420

10.    Dr. William F. Gutknecht
      Research Triangle Institute
      P.O. Box 12194, Bldg. 6
      RTP, NC  27707
      Phone:  (919) 541-6883
      FAX: (919)541-8778

11.    Ms. Susan Guyaux
      Maryland Department of Environment
      Lead Program
      2500 Broening Highway
      Baltimore, MD 21224
      Phone:  (410)631-3824
      FAX: (410)631-4112

12.    Ms. Sharon L. Harper
      USEPA/AREAL
      MD-78
      RTP, NC 27711
      Phone: (919) 541-2443
      FAX:  (919)541-3527

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13.   Mr. Jim Hayes
      N.C. State Government
      Environmental Health Services Section
      P. O. Box 27687
      Raleigh, NC  27611-7687
      Phone: (919) 733-2884
      FAX:  (919)733-0488

14.   Mr. Lynn  Hill
      356 Amhurst Blvd.
      Dayton, OH 45440
      Phone: (513)427-1499

15.   Mr. Jon Lathers
      Wayne County Environmental Health Dept.
      5454 Venoy Street
      Wayne, Ml  48184
      Phone: (313) 326-4900
      FAX:  (313)326-7221

16.   Mr. Warren A. Loseke
      USEPA/AREAL
      MD-78
      RTP, NC  27711
      Phone: (919)541-2173
      FAX:  (919)541-3527

17.   Dr. Mary McKnight
      National Institute of Standards of Technology
      Building 226, Room B348
      Gaithersburg, MD 20899
      Phone: (301) 975-6714
      FAX:   (301)975-4032

18.   Dr. John D. Neefus
      Research Triangle Institute
      P.O. Box 12194, Bldg.  7
      RTP,  NC  27707
      Phone: (919)541-6578
      FAX:  (919)541-8778

19.   Dr. Chris Papanicolopoulos
      Georgia Tech Research Institute
      Environmental Sciences and Technology Laboratory
      O'Keefe Building, Room 107
      Atlanta, GA  30332-0800
      Phone: (404) 894-3617
      FAX:  (404) 894-3906

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20.   Mr. John Pesce
      Star Environmental Services, Inc.
      P. O. Box 1027
      Melrose, MA 02176
      Phone: (617)662-2220
      FAX:  (617)979-0060

21.   Mr. Roy Petre
      Childhood Lead Poisoning Prevention Program
      Massachusetts Dept. of Public Health
      305 South Street
      Jamaica Plain, MA 02130
      Phone: (617) 522-3700
      FAX:  (617)522-8735

22.   Ms. Angel C. Price
      Research Triangle Institute
      P.O. Box 12194, Bldg.  6
      RTP, NC  27707
      Phone: (919)541-6555
      FAX:  (919)541-8778

23.   Mr. John Scalera
      USEPA
      Mail Code TS-798
      401 M. Street, SW
      Washington, DC  20460
      Phone: (202) 260-6709
      FAX:  (202)260-0001

24.   Mr. Brad Schultz
      USEPA
      Mail Code TS-798
      401 M. Street, SW
      Washington, DC  20460
      Phone:  (202) 260-3896
      FAX:  (202)260-0001

-------
25.    Mr. John Schwemberger
      USEPA
      Mail Code TS-798
      401  M. Street, SW
      Washington, DC  20460
      Phone:  (202) 260-7195
      FAX: (202) 260-0001

26.    Dr. Jim Simpson
      Center for Disease Control
      4770 Buford Highway, NE
      Mail Stop F-42
      Atlanta, GA  30341-3724
      Phone:  (404) 488-7330
      FAX: (404) 488-7335

27.    Dr. Tom Spittler
      U.S. Environmental Protection Agency
      60 Westview Street
      Lexington, MA  02173
      Phone:  (617) 860-4334
      FAX: (617) 860-4397

28.    Ms.  Cynthia (Cindy) R. Stroup
      USEPA
      Mail Code TS-798
      401  M. Street, SW
      Washington, DC  20460
      Phone:  (202) 260-3886
      FAX: (202) 260-0001

29.    Mr. Steve Weitz
      Department of Housing and Urban Development
      Room 8136
      451  Seventh Street, SW
      Washington, DC  20410
      Phone:  (202) 755-1805
      FAX: (202) 1000

-------
30.   Mr. Kenn White
      T.C. Analytics
      1200 Boissevain Avenue
      Norfolk, VA 23507
      Phone: (804) 627-0400
      FAX:  (804)627-1118

31.   Ms. Emily E. Williams
      Research Triangle Institute
      P.O. Box 12194, Bldg. 7
      RTP, NC  27707
      Phone: (919) 541-6217
      FAX:  (919)541-8778

32.   Mr. John Zilka
      Applied Systems
      2003 Sheffield Road, Suite B
      Aliquippa, PA 15001
      Phone: (412) 378-3066
      FAX:  (412) 378-8324

-------
               Suppliers of Portable/Transportable XRF Instruments

                                   May 1992
1.    MAP
      Scitec Corporation
      2000 Logston Blvd.
      Richland, WA 99352

      TEL (509) 375-5000
      FAX (509) 375-4931

      Larry Lynott
2.    Spectrace 9000
      Spectrace Instruments
      (Corporate Office)
      345 East Middlefield Road
      Mountain View, CA  94043

      TEL (415) 967-0350
      FAX (415) 967-6316

      Todd Rhea
      (Regional Office)
      2401 Research Blvd.
      Suite 206
      Fort Collins, CO 80526

      TEL (303) 493-2219
      FAX (303) 493-2520
3.     X-MET 880
      Outokumpu Electronicxs
      1900 N.E. Division St., #204
      Bend, OR  97701

      TEL (800) 229-9209
      FAX (503)  385-6750

      Stan Piorek

-------
4.    PGT XK-3
      Princeton Gamma-Tech, Inc.
      1200 State Road
      Princeton, NJ 08540

      TEL (609) 924-7310
      FAX (609) 924-1729
5.    Microlead I
      Warrington, Inc.
      2113 Wells Branch Parkway
      Suite 6700
      Austin, TX 78728

      TEL (512) 251-7771
      FAX (512) 251-7744

      Gary Stafford
6.     Model SEFA-P
      HNU Systems, Inc.
      160 Charlemont St.
      Newton, MA  02161-9987

      TEL (617) 964-6690
      FAX  (617) 965-5812

      Robert Petitti

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                      APPENDIX D
Papers/Information Distributed by Speakers and Manufacturers

-------
Data Presented by



Dr. Robert Clickner

-------
                                 January 6. 1993
   On the Performance of
     the Scitec MAP/XRF
            in the
      National Survey of
Lead-Based Paint in Housing
              by
 Robert Clickner and John Rogers
           WESTAT
        January 11,1993


      This work was sponsored by
Department of Housing and Urban Development
  and the Environmental Protection Agency.
              -1-

-------
                                                  January 8, 1993
     National Survey of Lead Paint in Housing

o   381 housing units across the United States
o   January to March, 1990
o   Scitec MAP-3 spectrum analyzer X-ray fluorescence devices
o   Used 8 nominally identical MAPs
o   Each MAP delivered from Scitec with
    o  Fresh 40 mci Co57 radioactive source
    o  Calibrated to lead in paint standards of 0.0, 0.22,
        1.20, and 2.64 mg/cm2
    o  "Automatic substrate correction" software
o   Scitec claim: automatic substrate correction eliminates
    the need for substrate corrections
o   Thousands of 60-second XRF measurements on
    dozens of different substrates
                           -2-

-------
                                                  Januarys, 1993
   Validation Measurements in National Survey
o   Continual check of MAPs' performance
o   Shims (from NIST) with lead paint loadings:
        0.6 + 0.02 mg/cm2
        2.99 + 0.3 mg/cm2.
o   Four substrates:
     Wood, drywall, steel, and concrete
o   Daily validation measurements for each MAP/shim/substrate
o   Regression analyses on the validation data
    o   Estimate the precision and accuracy of the readings
    o   Relate readings to
        o   Substrate
        o   Lead loading level
o   Different equation for each machine/substrate
o   Equations inverted to calibrate readings for analyses.
                            -3-

-------
                                                   Januarys, 1993
     Scitec MAP Performance Characteristics

o   Readings are systematically different from the amount
    of lead in the paint.
o   The direction and magnitude of the differences are related to

    o   Substrate  material

    o   Lead loading in the paint

o   Two nominally identical MAPs may exhibit
    significantly different performance characteristics

D   Precision of the readings depends on the substrate
    Therefore, in contrast to the Interim Guidelines and
    Scitec's claims, substrate correction is in fact a
    necessary step in the accurate determination of the
    presence and amount of lead-based paint on surfaces.
o   Findings apply only to XRF devices like the Scitec MAP-3s
    described above and to closely related XRF devices.

-------
                                                 Januarys, 1993
                         Wood
o   Readings < actual loadings when loadings < 2.0 mg/cm2
    Readings > actual loadings when loadings > 2.0 mg/cm2
o   At 0.6 mg/cm2
    a  88% of the readings were < 0.6 mg/cm2
    o  52% of the readings were equal to 0.0 mg/cm2.
    o  (MAP never produces a negative reading.)
o   At 2.99 mg/cm2
    a  60% of the readings were > 3.0 mg/cm2.
o   Standard deviation of repeated readings is 0.25 mg/cm2.
o   7 of the 8 MAPs performed similarly
                           -5-

-------
                                                 January 8, 1993
                  Drywall or Plaster
a   Performance is similar to the performance on wood
o   Readings < actual loadings when loadings < 2.5 mg/cm2
    Readings > actual loadings when loadings > 2.5 mg/cm2
o   At 0.6 mg/cm2
    o  82% of the readings were < 0.6 mg/cm2
    o  52% were equal to 0.0 mg/cm2
o   At 2.99 mg/cm2
    o  44% of the readings < 3.0 mg/cm2
    o  45% were > 3.0 mg/cm2.
o   Standard deviation of repeated readings is 0.25 mg/cm2
o   6 of 8 MAPs exhibited similar performance characteristics
                           -6-

-------
                                                  January 8, 1993
                          Steel
o   Readings > actual loadings, for all observed levels of lead
o   At 0.6 mg/cm2
    o   88% of the readings were > 0.6 mg/cm2
o   At 2.99 mg/cm2
    o  60% of the readings were > 3.0 mg/cm2
    o  1 machine had no readings above 3.0 mg/cm2
a   Substantial differences among the 8 machines
a   Standard deviation of repeated readings is 0.21 mg/cm2
                            -7-

-------
                                                 Januarys, 1993
   Concrete, brick, and other related substrates
o   MAP has difficulty detecting low/moderate levels of lead
o   At 0.6 mg/cm2
    o  95% of the readings were equal to 0.0 mg/cm2
    o  Only 1 machine had more than one non-zero reading
o   At 2.99 mg/cm2
    o  95% of the readings were < 3.0 mg/cm2
    o  11 % of these were equal to 0.0 mg/cm2
o   Standard deviation of repeated readings is 0.49 mg/cm2
a   There is much variation, both among and within machines.
                           -8-

-------
                                             WESTAT
     MAP Validation Readings on 0.6
               mg/sq cm Shim
                                    Concrete

                                 Steel

                               Plaster, Drywall

                            Wood         Substrate
Reading, mg/sq cm
                                              178/93

-------
                                                WESTAT
          MAP Validation Readings on
              2.99 mg/sq cm Shim
                                   Concrete

                              // Steel

                                Plaster, Drywall Substrate

                              Wood
       Reading, mg/sq cm
MAP299.XLC
M

-------
                                                                                    WESTAT
                Estimating Lead Concentrations on Wood:  Calibration Equations

                                for 8 Spectrum Analyzer XRFs.
      3.50
      3.00  —
      2.50  	
    u

    o-
    •)



    I 2.00
      0.00
               Bold Line: Reading = Concentration
           0.00
0.50
1.00       1.50        2.00


  XRF Reading, mg./sq. cm.
2.50
3.00
PBWOOD.XLC
                                                                                     1/8/93

-------
                                                                                    WESTAT
               Estimating Lead Concentrations on Plaster or Dry wall:  Calibration
                           Equations for 8 Spectrum Analyzer XRFs.
       4.50
       4.00 	
       3.50 —
       3.00 -+-
    u

    I  2-50
       0.00
      -0.50
                      Bold Line:  Reading = Concentration

                       0.50       1.00        1.50       2.00        2.50        3.00
                                     XRF Reading, mg./sq. cm.
PBPLASTR.XLC
                                                                                      1/8/93

-------
                                                                                    WESTAT
                Estimating Lead Concentrations on Steel:  Calibration Equations
                                 for 8 Spectrum Analyzer XRFs.
       5.00  -i—
       4.50  —
       4.00  4-
                      Bold line:  Reading = Concentration
                                      1.50     2.00     2.50     3.00     3.50    4.00
      -1.00  -*-
                                     XRF Reading, mg./sq. cm.
PBSTEEL.XLC
                                                                                      1/8/93

-------
                                                                                    WESTAT
                   Estimating Lead Concentrations on Concrete:  Calibration
                           Equations for 8 Spectrum Analyzer XRFs.
      5.00
        4p f\	_.
       .50  	
      4.00
      3.50  —	          	
u
CT

"Si



o

'€
      3.00  	
      2.50  -1—
    u

    o
   u

   Q.

   »*
    •>
      0.00
                                            Bold Line: Reading = Concentration
   2.00  H-
      1.50  		•+-)
      1.00  --
      0.50 —
           0.00     0.50     1.00     1.50     2.00     2.50     3.00     3.50     4.00

                                     XRF Reading, mg./sq. cm.
PBCONCRT.XLC
                                                                                      1/8/93

-------
Figure D-18   Validation XRF  Readings versus Shim Lead Concentration
                     for XRF Instrument #36  on Wood
Lead concentration (mg/sq cm) - 0.5779 + 0.6977*XRF reading + 0.00069*(Days  since 2/2/90)
    5 T
    4 3-
    3 *
o
•
XRF Reading Histogram
Outliers (not used)
Calibration Equation
XRF & 1 mg/sq cm
XRF - Lead Concentration
Shim Concentration
                                                                      XRF @ 1 mg/sq cm Is approximately  0.59
                                                                      Median used for 0.6 shim
                       Lead  Concentration (mg/sq  cm)

-------
Figure D-34   Validation XRF Readings versus Shim  Lead Concentration
                    for  XRF Instrument #36  on Drywall
 Lead concentration (mg/sq  cm)  • 0.1694 + 0.8220'XRF reading 4 0.00081 "(Days  since  2/2/90)
    4.5 T
                                                                           o     XRF Reading Histogram
                                                                           •     Outliers (not used)
                                                                                 Calibration Equation
                                                                                 XRF @ t mg/sq cm
                                                                           	XRF - Lead Concentration
                                                                                 Shim  Concentration
                                                                     XRF @ 1 mg/sq cm Is approximately 0.99
   -0.5 -1-
                        Lead Concentration (mg/sq cm)

-------
Figure D-35   Validation XRF Readings versus  Shim  Lead  Concentration
                    for  XRF Instrument #37 on  Drywall
 Lead concentration (mg/sq  cm)  - 0.2311  + 0.9186*XRF reading + 0.00091*(Days since 2/2/90)
     4 -r
                                                                                 XRF Reading Histogram

                                                                                 Outliers (not used)

                                                                                 Calibration  Equation

                                                                                 XRF @ 1 mg/sq cm

                                                                                 XRF - Lead Concentration

                                                                                 Shim Concentration
                                                                     XRF @ 1 mg/sq cm Is approximately 0.81
                        Lead Concentration (mg/sq cm)

-------
Figure  D-10   Validation XRF Readings versus  Shim  Lead  Concentration
                     for XRF Instrument #36 on Steel
Lead concentration (mg/sq  cm) • -1.0265 + 1.0580'XRF reading  + 0.00105*(Days  since 2/2/90)
    5  T
   4.5 --
              0.5
1      1.5      2      2.5      3
 Lead  Concentration (mg/sq  cm)
                                                                           o
                                                           XRF Reading Histogram

                                                           Outliers (not used)

                                                           Calibration Equation
                                                                        	XRF 9 1 mg/sq cm

                                                                        	XRF - Lead Concentration

                                                                        	Shim  Concentration
                                                                      XRF @ 1 mg/sq cm Is approximately  1.90

-------
Figure  D-13   Validation XRF Readings versus Shim Lead Concentration
                     (or XRF  Instrument  #39  on Steel
Lead concentration (mg/sq  cm)  - -0.9832 +  1.1274'XRF reading + 0.00112*(Days since 2/2/90)
   4.5 T
                  r i i
               0.5      1       1.5      2     2.5     3
                        Lead Concentration (mg/sq cm)
3.5
                                                                                 XRF Reading Histogram
                                                                                 Outliers (not used)
                                                                                 Calibration Equation
                                                                                 XRF <8> 1 mg/sq cm
                                                                                 XRF • Lead Concentration
                                                                                 Shim Concentration  .
                                                                      XRF @ 1 mg/sq cm Is approximately  1.73

-------
Figure  D-26   Validation XRF  Readings versus Shim Lead  Concentration
                   for XRF Instrument  036 on Concrete
 Lead concentration (mg/sq cm) - 0.5692 + 1.5546'XRF reading + 0.00154*(Days since 2/2/90)
    3.5  T
                                                                                 XRF Reading Histogram
                                                                                 Outliers  (not used)
                                                                                 Calibration  Equation
                                                                        	XRF® 1 mg/sq cm
                                                                        	XRF - Lead Concentration
                                                                        	Shim Concentration
                                                                      XRF @ 1 mg/sq cm Is approximately  0.26
                                                                      Median used for 0.6 shim
                        Lead Concentration (mg/sq cm)

-------
Figure D-28   Validation XRF Readings versus  Shim Lead  Concentration
                   for XRF Instrument  #38 on Concrete
 Lead concentration (mg/sq cm) » 0.5753 + 1.1586'XRF reading + 0.00115*(Days since 2/2/90)
                                                                           o
XRF Reading Histogram

Outliers (not used)

Calibration  Equation

XRF @ 1 mg/sq cm

XRF - Lead Concentration

Shim Concentration
                                                                   •I   XRF @ 1 mg/sq cm Is approximately  0.34
                                                                   4  Median used for 0.6 shim
                        Lead Concentration (mg/sq cm)

-------
Flow Diagram Presented by



    Dr. Mary McKnight

-------
Evaluation  of Methods for Field Measurement of Lead In Paint  Films
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-------
Data Presented by



 Mr. John Pesce

-------
                      AN EXAMINATION OF SUBSTRATE
                       EFFECT ON PORTABLE X-RAY
                     FLUORESCENCE INSTRUMENTATION
Pesce, J., Star Environmental Services, Inc. P.O. Box 1027,
Melrose, MA 02176;  Martin, K.P., Massachusetts Institute of
Technology, 77 Mass. Ave., Cambridge, MA 02139;  Straub, W.E.,
Straub Industrial Hygiene, 250 Grove St., Melrose, MA 02176;
Edwards, R.,  Massachusetts Institute of Technology, 77 Mass. Ave.,
Cambridge, MA 02139.
                            ABSTRACT

     Mobile,  hand held X-ray fluorescence analyzers (XRF)  are
     used to measure concentrations of lead in paint.   The
     three manufacturers of the instruments treat background
     readings in different ways.  The same surface can give
     significantly different readings from using different
     instruments.  Some instruments will give readings in
     excess of legal standards for substrate materials when
     there is no lead present.  Others will give a negative
     reading for a substrate which will lower the true lead
     concentration reading.  Readings can be corrected by
     taking readings from bare substrate surfaces, but this is
     an expensive and time consuming process.  Surfaces can
     also be checked by other confirmatory techniques.  This
     paper examines problems in the use of X-ray analyzers
     when measuring lead concentrations in painted surfaces.
     It also demonstrates the need for confirmatory methods.

     Test results are presented on the effects of over twenty
     different substrate materials and conditions.  Materials
     were tested at several lead concentrations.  A testing
     protocol using XRF with confirmatory testing of surfaces
     using sodium sulfide and atomic absorption spectroscopy
     is presented with the experience of using it in six
     buildings containing over four hundred apartment units.

     X-ray analyzers alone are not adequate to determine lead
     concentrations in painted surfaces.  Substrate effects
     and confirmatory testing should be considered.
     Government regulators should not exclude techniques that
     are adjunct to the use of the XRF.

-------
                          INTRODUCTION

 The purpose of this presentation  is to  share  our  experiences  of how
 various substrates effect the hand held X-ray fluorescent  analyzers
 designed to measure lead  in paint.  The substrate effect is usually
 called substrate effect level and sometime referred  to as  substrate
 equivalent lead, and abbreviated SEL.   Our data is derived from
 both  actual field use and recently developed  Round Robin
 information.  The Round Robin encompassed over thirty different
 instruments that are being used in the  fields daily.

 The mobile X-ray fluorescent  (XRF) analyzers  to be discuss are
 those frequently used for in-situ for lead in paint.

 The first to be discussed is that Princeton Gamma  Tech,
 specifically the model XK3,  This device uses  a cobalt 57  source of
 approximately 10 millicuries.  The instrument  counts the X-ray
 events using a krypton filled proportional tube.   Background
 effects are compensated by monitoring a single lower X-ray
 frequency, which changes  the high voltage in  the tube.

 The second type is the Warrington Microlead I, Revision 4.   The
 Microlead also uses a cobalt 57 source of approximately 10
 millicuries.  This instrument uses a high and  low  band pass
 screening with a two filter system.   The filters are alternated
 during the reading cycle.  The filtered X-rays are then
 scintillated and counted  by a photomultiplier tube.  The counts at
 the high and low frequencies are referenced by computer logic to
 adjust the voltage of the dynodes in the photomultipier tube.

 The third type of XRF to  be talked about is the SCITEC Metal
 Analysis Probe analyzer.  This instrument almost always uses a 40
 millicurie cobalt 57 source.  The detector used is a crystal.  The
 analyzer uses an algorhithem based upon information received from
 five  reference channels at different frequencies.  The algorhithem
 is designed to correct for most substrate effects.  Although the
 SCITEC has the ability to be spectrum read,  most of time it is
 operating in the direct read mode.

                              FIELD DATA

 The broad base of building materials that can be painted with lead
based paint,  and consequently must be tested,  is staggering.
Residential wood frame construction poses many wood and plaster
 items inside,  many times these materials are in tandem.  Exteriors
of these types of buildings also often have various types of
coverings over wood,  including wood over wood.  Larger buildings
both residential and commercial generally favor more concrete,
brick, and denser plaster.  These buildings also have a tendency to
contain more metal architectural features and less wood millwork.

-------
     *
     *

     *
     *
                  FIGURE 1

                 FIELD TESTING

421 units tested in an apartment complex
All interior and exterior surfaces were tested/
resulting in over 20/000 readings
PGT-XX3/ XRF instruments were used
32 substrate effect levels (SEL) were measured
A comprehensive lead inspection of 421 units in high-rise apartment
building were performed using all PGT's. The inspection was
conducted to examine surfaces for lead on 100% of all interior,
common and exterior surfaces.

The protocol used for testing included SEL's on all surfaces and
confirmatory use of both sodium sulfide solution (6-8%)  and atomic
absorption.  Confirmation techniques were engaged when certain
levels were found by XRF.  Sodium sulfide solution was used when
Apparent Lead Concentrations were 1.2 mg/cm2 and samples,  taken for
AA analysis when Corrected Lead Concentrations were between 0.8
mg/cm2 to 1.5 mg/cm2. Consequently SEL's had to be take on ceilings,
walls, windows, etc.  Having this significant amount of data on the
SEL's for the building, we took the opportunity to test the SEL
locations with the PGT, Warrington and the SCITEC.   The following
is the data collected:
FIGURE 2
ALL

Masonry
Cinder Block
Plaster type A
Plaster column
Red Brick
Cinder Block
Sheet Rock
Concrete Column
Wood
Pressed Board
Hollow Door
Oak
Metal
Window Sill
Radiator Cover
Vent Duct
Mail Box
TYPES OF
PGT
1.1
0.6
1.2
1.1
1.1
0.2
0.9

0.0
0.4
0.2

1.9
1.6
1.1
1.5
SUBSTRATES
WAR
1.2
-0.1
1.7
1.3
1.2
-0.3
1.7

-0.1
-0.3
-0.2

-1.1
-1.0
-0.7
-1.1

SCI
0.0
0.0
0.0
0.0
0.0
0.2
0.3

0.0
0.0
0.3

0.4
0.3
0.3
0.3

-------
 Since  it is expected that these instruments will be  used  over a
 wide variety of materials, we selected representative  samples.
 The tremendous variability of the XRF's SEL on groups  within  the
 same type of building materials such as plaster/masonry,  cause us
 to take a more microscopic view of the SEL's within  similar
 building components.
FIGURE 3
MASONRY

Cinder Block
Plaster type A
Plaster column
Plaster type B
Red Brick
Cinder Block
Sheet Rock
Concrete Column
TYPES OF
PGT
1.1
0.6
1.2
0.6
1.1
1.1
0.2
0.9
SUBSTRATE
WAR
1.2
-0.1
1.7
0.1
1.3
1.2
-0.3
1.7

SCI
0.0
0.0
0.0
0.0
0.0
0.0
0.2
0.3
Note the variability of the PGT and Warrington with respect to
these type of building materials.  Also note how the SCITEC almost
seems to have a flat response to most of these substrates.  It will
also be interesting to note that both the PGT and Warrington can
give negative readings and the SCITEC cannot.   This list
demonstrates how important it is to know which type of wall or
c.eiling that is being tested before any final determination can be
stated about its lead content.  That is, if the wall is a
supporting concrete wall as opposed to a dividing wall, significant
differences of substrate effect occur.

FIGURE 4


METAL SUBSTRATES

Window Sill
Radiator Cover
Vent Duct
Mail Box
PGT
1.9
1.6
1.1
1.5
WAR
-1.1
-1.0
-0.7
-1.1
SCI
0.4
0.4
0.3
0.3
As shown in figure 4, for metals both the PGT and Warrington seem
to treat the substrate effects completely opposite.  The elevated
readings for the PGT are similar in absolute values as the
depressed readings of the Warrington.  Again the SCITEC seems only
modestly influenced by the substrate.

-------

FIGURE 5


WOOD SUBSTRATES

Pressed Board
Hollow Door
Oak
PGT
0.0
0.4
0.2
WAR
-0.1
-0.3
-0.2
SCI
0.0
0.0
0.3
As shown in figure 5 the XRFs apparently work on less dense
materials.  The standard deviations reported by the manufactures of
.3 mg/cm2 can usually be depended upon for wood type substrates.

                     ROUND ROBIN INFORMATION

Over the past year, a group of private lead inspectors in
Massachusetts have established and participated in a voluntary
Round Robin testing procedure for portable X-ray fluorescence
instruments.  As part of this Round Robin program, substrate
effects were examined.  A detailed presentation of this Round Robin
program will be presented on Wednesday by another author of this
paper.
ALC
SEL
CLC
FIGURE 6
STEEL CHANNEL
PGT ( 9 )
1.8
0.9
0.9
WAR (5)
-0.8
-0.8
0.0
SCI(l)
1.2
0.4
0.8
In this slide the Substrate Effect Level, called the SEL, is a
piece of steel channel, with no lead paint.  The Apparent Lead
Concentration, called the ALC, is the same steel channel with lead
paint.  To make a substrate effect correction to the steel channel
with lead paint, the reading for the steel channel without lead
paint is subtracted.  This gives a Corrected Lead Concentration
called the CLC.  All readings are expressed in mg/cm2.  For the
steel channel samples prepared for the Round Robin the CLC of PGT
and SCITEC showed some measure of lead while the Warrington's CLC
showed there to be no lead.

-------



ALC
SEL
CLC
FIGURE 7
RED BRICK
PGT ( 9 )
1.8
1.2
0.6


WAR (5)
1.4
0.3
1.2


SCI(l)
0.0
0.0
0.0
Red bricks were also prepared with and without lead paint on their
surfaces.  What is shown in figure 7 is obvious that the SCITEC did
not pick up any amount of lead.  While the zero readings of the
SCITEC on substrates is, at first, comforting, it can be seen from
this slide that like the Warrington on metals, a false negative
reading can result.



ALC
SEL
CLC
FIGURE 8
POPLAR
PGT (9)
1.2
0.0
1.2


WAR (5)
0.9
-0.1
1.0


SCI(l)
0.6
0.1
0.5
Poplar wood samples prepared for the Round Robin and shown in
figure 8 indicates that the XRF's were able to identify leaded
surfaces, although quantification are not in good agreement.

FIGURE 9


BELLY CAS I KG

ALC
SEL
CLC
PGT (9)
1.0
O.O
1.0
WAR(5)
1.2
0.3
0.9
SCI(l)
0.7
0.0
0.7
A decorative wood molding called belly casing was also used during
a Round Robin test.  This was done to check the effects of an air
gap between the XRF probe and the sample.  The results shown in
figure 9 are consistent with the flat wood sample shown previously.
This type of belly casing has a convexed fluted surface that would
allow only direct contact with a partial portion of the instrument
probe area.

-------



ALC
SEL
CLC
FIGURE 10
SHEET ROCK
PGT ( 9 )
1.4
0.2
1.2


WAR (5)
0.8
0.1
0.7


SCI(l)
1.2
0.4
0.8
 The  Round Robin  sheetrock  samples  also  produced  a  consistent  result
 for  the  three different XRF's.




ALC
SEL
CLC
FIGURE 11
READ-THROUGH EFFECTS
Lead Flashing under 1 1/2" of wood
PGT (13) WAR (11)
1.7 10.7
0.0 -0.1
1.7 10.8



SCI(l)
4.7
0.1
4.6
The penetration of the gamma ray and consequently the ability of
the K shell X-ray to also penetrate materials, can produce a
reading on the XRF's when lead  is deep beneath the surface.  It is
interesting to notice that in figure 11 the PGT is less susceptible
to detect this type of lead.

The instruments seem to do well over most of the less dense
materials, those which would most likely be found in wood frame
houses with less than four families.  Higher density materials and
metals pose a problem for the XRF's and provide a need to correct
for the type of substrate being examined.  This would indicate that
buildings with construction components of higher density would
require a more keen attention to substrate effect on the lead X-ray
frequency.

At present most of the level driven lead abatement is based upon
XRF reading of around 1.0 mg/cm2.  This is well within a range for
which substrate effects alone can be contained.  It is possible to
read above this level and not have any lead present.

In an effort to reduce the error resultant from XRF testing alone, we
used secondary and tertiary screening methods.  The secondary
screening method used was AA.  The tertiary screening was done with
the use of sodium sulfide solution (6-8%).  (The fact that this
testing procedure is currently only accepted by the Commonwealth of
Massachusetts should not mitigate it usefulness as a confirmatory
method.)

-------
                              CONCLUSIONS

It is our conclusions that for a wide variety of substrates the
instruments can be used with a reasonable amount of confidence.
This can be aided by using substrate corrections but assumes the
operator has the experience to know what the substrate is and how to
make appropriate corrections.  For example structural concrete walls
and those simply that divide rooms can look deceptively similar, yet
the XRF can have profoundly different readings.  Lead/lead paint
behind even one inch thick wood can be mistaken as surface lead.  The
operator of the XRF must have enough knowledge to know when to doubt
the XRF and refer back to secondary and tertiary screening methods.

The XRFs are also not able to compensate for all possible
substrates.   Substrate correction values can be different from
instruments of the same manufacturer as well as  differ from those
of each manufacturer.

Someone's mistaken perception about the level of lead on a surface
could indicate that no lead  is present when dangerous levels of lead
are present,  or could affect the cost of abatement significantly by
indicating abatement when none is needed.   Although it is possible to
use SEL's to correct for these effects to  some extent,  the degree of
correction has limited  accuracy.  Confirmatory testing should be used
on certain substrates when lead levels that could influence the
abatement decision are marginal.

-------
ROUND ROBIN	ROUND NUMBER ONE
DATE 	 10/03/91 AND 10/04/91
SAMPLE ID CODE — A
 SAMPLE DESCRIPTION
This sample consisted of three layers:
   -Top layer> two pieces of unpainted, 3/4" thick, wood.
   -Middle layer> lead roofing flashing.
   -Bottom layer> 1/4" plywood.
   >»The flashing was the only lead in the sample.
PGT
ID Code
watch
dvblt
cegbm
gblam
mkcfx
mejsc
adlwz
walzj

gapcu
pwfal
bdfhj
kmprt
acegi
mean
aviation
Reading
2
.3
2.4
1
1
1
1,
1.
2.

1.
1.
1.
1.
1.

1.
0.
.4
.0
.5
.1
.5
1

7
9
8
4
6

7
42














Warrington
ID Code
tolpk
Iqrom
azbyc
notrl
dfdce
hcdjr
npxtc
andkm

baino
dyzag
fbcps




Reading
10.
11.
9.
11.
10.
10.
10.
11.

12.
10.
10.



9
5
8
3
5
7
5
6

3
1
3

















10.7
0.74

SciTec
ID Code
Ingbv















Reading
4.68







i




















4.68
	

-------
ROUND ROBIN 	 ROUND NUMBER ONE
DATE 	 10/03/91 AND 10/04/91
SAMPLE ID CODE — B
 SAMPLE DESCRIPTION
This sample consisted of four layers:
   -Top layer> one sheet of heavy paper.
   -Second layer> lead paint.
   -Third layer>  two inch thick concrete (from cinder block)
   -Bottom layer> 1/4" plywood.
PGT
ID Code
watch
dvblt
cegbm
gblam
mkcfx
mejsc
adlwz
walzj
qapcu
pwfal
bdfhj
kmprt
acegi
mean
aviation
Reading
2
2
2
1
1
1
3
2
2
2.
2
2
1,

2.
0.
.6
.2
.3
.5
.3
.5
.0
.7
.2
.2
.8
.0
.9

2
54













Warrington
ID Code
tolpk
Igrom
azbyc
notrl
dfdce
hcdjr
npxtc
andkm
baino
dyzag
fbcps




Reading
1
1,
1.
1.
1.
2.
1.
2.
1.
2.
1.



1.
0.
.6
.4
9
7
4
2
4
3
4
0
7
















7
33

SciTec
ID Code
Ingbv














Reading
0.13


























0.13
	

-------
ROUND ROBIN 	 ROUND NUMBER ONE
DATE 	 10/03/91 AND 10/04/91
SAMPLE ID CODE — C
 SAMPLE DESCRIPTION
This sample consisted of two layers;
   -Top layer> lead paint.
   -Bottom layer> wood door, 1 3/4 " thick.
PGT
ID Code
watch
dvblt
cegbm
gblam
mJccfx
mejsc
adlwz
walzj
qapcu
pwfal
bdfhj
kmprt
acegi
mean
aviation
Reading
2.
2.
1,
1
2
1
2
2
2
2.
3.
2.
2.

2.
0.
.3
.6
.4
.9
.1
.6
.3
.7
7
7
1
0
5

3
.48













Warrington
ID Code
tolpk
Igrom
azbyc
notrl
dfdce
hcdjr
npxtc
andkm
baino
dyzag
fbcps




Reading
1.
1.
0.
1.
2.
2.
1.
2.
1.
1.
1.



1.
0.
2
6
7
9
0
5
5
0
6
7
7
















,7
46

SciTec
ID Code
Inqbv














Reading
2.13


























2.13
	

-------
ROUND ROBIN	ROUND NUMBER ONE
DATE 	 10/03/91 AND 10/04/91
SAMPLE ID CODE — D
 SAMPLE DESCRIPTION
This sample consisted of two layers:
   -Top layer> non-lead paint.
   -Bottom layer> wood door,  1 3/4 " thick.
PGT
ID Code
watch
dvblt
cegbm
qblam
mkcfx
mejsc
adlwz
walzj
qapcu
pwfal
bdfhj
kmprt
acegi
mean
aviation
Reading
0.3
0.1
-0.3
0.2
-0.1
0.0
0.0
'0.2
0.3
0.0
0.4
0.8
-0.2

0.1
0.29













Warrington
ID Code
tolpk
Iqrom
azbyc
notrl
dfdce
hcdjr
npxtc
andkm
baino
dyzag
fbcps




Reading
-0.1
-0.2
2.2
0.1
-0.4
0.9
0.6
0.4
0.0
0.0
0.8
SciTec
ID Code Reading
Inqbv 0 . 04








.




0.4
0.73













0.04
	

-------
ROUND ROBIN 	 ROUND NUMBER ONE
DATE 	 10/03/91 AND 10/04/91
SAMPLE ID CODE — E
 SAMPLE DESCRIPTION
This sample consisted of two layers:
   -Top layer> lead paint.
   -Bottom layer> wood door, 1 3/4 " thick.
PGT
ID Code
watch
dvblt
cegbm
qblam
mkcfx
mejsc
adlwz
walzj
gapcu
pwfal
bdfhj
Jonprt
acegi
mean
aviation
Reading
1.3
1.4
0.2
0.5
0.2
0.3
0.6
1.3
0.8
1.0
1.0
0.3
0.6

0.7
0.43













Warrington
ID Code
tolpk
Igrom
azbyc
notrl
dfdce
hcdjr
npxtc
andkm
baino
dyzag
fbcps


•

Reading
0.6
0.7
1.0
0.9
0.6
1.5
0.8
1.0
0.5
0.5
1.2
SciTec
ID Code Reading
Inqbv 0.63








_




0.9
0.31













0.63
	

-------
ROUND ROBIN 	 ROUND NUMBER ONE
DATE 	 10/03/91 AND 10/04/91
SAMPLE ID CODE — F
 SAMPLE DESCRIPTION
This sample consisted of three layers:
   -Top layer> lead paint.
   -Middle layer> two layers of cedar shingles.
   -Bottom layer> 3/4 " wood.
PGT
ID Code
watch
dvblt
cegbm
qblam
mkcfx
mejsc
adlwz
walzj
gapcu
pwfal
bdfhj
kmprt
acegi
mean
aviation
Reading
0.6
0.9
0.4
0.4
0.6
0.5
0.6
0.9
0.9
0.6
1.2
0.4
0.6

0.7
0.25













Warrington
ID Code
tolpk
Igrom
azbyc
notrl
dfdce
hcdjr
npxtc
andkm
baino
dyzag
fbcps




Reading
1.4
1.8
1.5
1.8
1.4
1.8
1.3
2.0
1.7
1.4
1.5
SciTec
ID Code Reading
Ingbv 1.102













1.6
0.23













1.10
	

-------
ROUND ROBIN 	 ROUND NUMBER ONE
DATE 	 10/03/91 AND 10/04/91
SAMPLE ID CODE — G
 SAMPLE DESCRIPTION
This sample consisted of three layers:
   -Top layer> one sheet of heavy paper.
   -Middle layer> non-lead paint primer.
   -Bottom layer> metal door jam.
PGT
ID Code
watch
dvblt
cegbm
gblam
mkcfx
mejsc
adlwz
walzj
qapcu
pwfal
bdfhj
kmprt
acegi
mean
Aviation
Reading
0.
0.
0.
0.
0.
0.
1,
1.
1.
0.
1,
0.
0.

0.
0.
.5
9
.2
.2
1
5
0
3
2
6
0
5
6

7
38













Warrington
ID Code
tolpk
Igrom
azbyc
notrl
dfdce
hcdjr
npxtc
andkm
baino
dyzag
fbcps




Reading
-0.
-1.
-0.
7
1
6
-0.8
-1.
-0.
-1.
-1.
-1.
-0.
-1.



-0
0
2
5
1
3
0
5
3
















.9
.31

SciTec
ID Code
Inqbv














Reading
0.34


























0.34
	

-------
ROUND ROBIN	ROUND NUMBER ONE
DATE 	 10/03/91 AND 10/04/91
SAMPLE ID CODE. — H
 SAMPLE DESCRIPTION
This sample consists of four  layers:
   -Top layer> anodized aluminum metal house siding.
   -Middle layer> lead paint (painted on bottom layer.
   -Bottom layer> 3/4 " wood.
PGT
ID Code
watch
dvblt
cegbm
gblam
mkcfx
mejsc
adlwz
walzj
gapcu
pwfal
bdfhj
kmprt
acegi
mean
Aviation
Reading
1.3
1.5
1.1
1.0
0.6
0.4
1.3
1.9
1.5
1.5
1.&
1.5
1.3

1.3
0.42













Warrington
ID Code
tolpk
Igrom
azbyc
notrl
dfdce
hcdjr
npxtc
andkm
baino
dyzag
fbcps




Reading
1.2
1.1
0.9
1.5
1.0
1.1
0.7
1.4
0.3
1.0
0.7
SciTec
ID Code Reading
Ingbv 1.15













1.0
0.34













1.15
	

-------
ROUND ROBIN 	 ROUND NUMBER ONE
DATE 	 10/03/91 AND 10/04/91
SAMPLE ID CODE — I
 SAMPLE DESCRIPTION
This sample consisted of two layers;
   -Top layer> lead paint.
   -Bottom layer> 3/8 " sheetrock.
PGT
ID Code
watch
dvblt
cegbm
gblam
mkcfx
mejsc
adlwz
walzj
gapcu
pwfal
bdfhj
kmprt
acegi
mean
aviation
Reading
1,
2.
1.
1.
1.
0
1.
1.
1,
1.
.4
.0
.0
.2
.0
.9
.3
8
5
8
1.4
1.
1.

1.
0.
2
1

3
36













Warrington
ID Code
tolpk
Iqrom
azbyc
notrl
dfdce
hcdjr
npxtc
andkm
baino
dyzag
fbcps




Reading
0.
0.
0.
1.
0.
0.
0.
0.
0.
1.
0.



0.
0.
7
9
8
5
8
9
8
9
4
1
5
















.9
.29

SciTec
ID Code
Ingbv














Reading
1.14


























1.14
	

-------
ROUND ROBIN 	 ROUND NUMBER ONE
DATE 	 10/03/91 AND 10/04/91
SAMPLE ID CODE — J
 SAMPLE DESCRIPTION
This sample consists of two layers:
   -Top layer> non-lead paint.
   -Bottom layer> 3/8 " sheetrock.
PGT
ID Code
watch
dvblt
cegbm
gblam
mkcfx
mejsc
adlwz
walzj
qapcu
pwfal
bdfhj
kmprt
acegi
mean
iviation
Reading
0.2
0.5
-0.9
0.3
0.1
0.1
0.0
0.1
0.0
0.1
0.2
-0.1
0.0

0.1
0.32













Warrington
ID Code
tolpk
Igrom
azbyc
notrl
dfdce
hcdjr
npxtc
andkm
baino
dyzag
fbcps




Reading
-0.1
0.0
0.0
0.2
-0.2
0.0
-0.3
0.2
-0.4
-0.2
-0.3
SciTec
ID Code Reading
Inqbv 0.12













-0.1
0.2













0.12
	

-------
Data Presented by
 Dr. Tom Spittler

-------
    COUNTS
16260-X-4
 1DOSEC
1000-
       16360   VS   16260    (REVERSE   SIDE)    I
 80°"  DOT   MODE   -   0.7%   PAINT   CHIP
 600T
 4004
 200-
                                                                 S R
                                     XES
                                                                            KEY

-------
     COUNTS
18282-X-4
 100SEC
2000 >
1600--   DOT   MODE   -   9.6*   PB   PAINT   CHIP
1200-
 800'
 400-
                                                              "XT
        16262   VS    16262    (REVERSE   SIDE)    IM
                                                                               KEV
                                      XES

-------
COUNTS X 1000
     14620-X-4
      100SEC
   14620   VS   14620CREVERSE   SIDE
   DOT   MODE
4 8 %   P B   PAINT   CHIP
           0
                                                                        KEY
                                 XES

-------
  COUNTS X 1000
                             14135-X-4
                               88SEC
8
 1-4135    VS   1413
\ '•"*,
 DOT   MODE
                            2 4
REVERSE    SID
B   PAINT    CHI
                                                                    I N
                                      <	PB	>
                                                                             KEV
                                    XES

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DATA      FOR      SOMAR      DILUTION      TEST
    SAMP.       #
MG      1579         +      SOMAR      MIX
                                                    7   8
                                            2  1   0
                                                    3   6
                                            2  1  5
                                                    1   6  9
                                            2  1   6
                                             M  G      14135
                                                    6   5
                                            209

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     COUNTS
                                    3-X-4
4000
3300 •
2900-
2000-
1500-
lOOOf
 SOOr
       BAVS    1.2    &    4    (IN   DOT    MODE)
                                                                             KEY
                                                             u
                                     XES

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-------
SAMP.      #        PEAK      H         WT.  RATIO         %      PB
N  B  S     1
46     MM
0.371
4.45
N  B  5      2
2  0   -  M  M
0.167
2.00
N B  S      3
89     MM
0,782
9.38
14153
68     MM
0.311
23.1

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Data Presented by
Scitec Corporation

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                                                       April 27, 1993
        Warren Loseke
        U.S. EPA
        Atmospheric Research and Exposure
            Assessment Laboratory
        Research Triangle Park, NC  27711

        Dear Mr. Loseke:

               During the 12 years which the MAP technology has been in existence, we've found that
        the use of X-ray fluorescence for field measurements is often misunderstood, oversimplified, or
        even disregarded. We appreciate your efforts to bring government and state personnel and their
        contractors together to accurately identify and resolve the questions, concerns, and confusion
        which exists.

               The purpose of the use of portable XRF is the identification of lead hazards quickly and
        economically, and in  sufficient detail for cost effective abatement strategies to be implemented.
        Policy makers and government agencies seem to focus their attention on the performance of the
        XRF instrument  as though the device alone is responsible for the valid identification of lead
        hazards.

               However,  a majority of  the errors  that occur in the identification of lead hazards are
        attributable to  the sampling design used, the operator, the  customer, and a lack of effective
        quality control practices—not the sampling device.  Attention must be given to determining how
        to  control  and minimize errors and bias from  all  sources;  sampling designs; operators;
        instruments; laboratories; record keeping; report generation; and customers.

              As the single largest customer for lead paint testing  services, the Department of Housing
        and Urban Development has significant influence over how  lead paint testing and reporting is
        accomplished.  However, the objectives, goals, roles, and responsibilities in HUD's LBP testing
        program are inconsistent and not aligned properly with incentives and control measures.  This
        accounts for most of the errors and data quality problems  which  result.
                                                                                        WI993L.2
2000 Logston Blvd.     Telephone: 1-800-4-NO-Lead
FAX: 509-375-4931
Richland, WA 99352

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       The customer should know what to specify in  requests for bids  and proposals to do
 testing work, they need to know how  to evaluate bids, how to oversee testing, and how to
 evaluate the test data.  Unfortunately most PHA customers today do not have the knowledge or
 skills to  handle these responsibilities.  Without fundamental knowledge and skills, they lack the
 ability to effectively let and administrate contracts.  This deficiency is a major reason for the
 poor quality of test data that is received by HUD.

       Few HUD lead paint testing contracts even deal with the issue of "quality," or even
 specify that the contractor is to provide  accurate and verifiable test data!  Many PHA's assume
 they are  tasked only with turning in test data to HUD, they have no feeling of obligation to make
 sure the test data is good.  Most PHA's believe they've done their job when they've awarded
 a contract to the low bidder...as though their only job is to get  a test report at a low price.

       The sampling design and protocol required by HUD will not generate highly axurate
 data nor result in identification  of lead hazards 95% of the time.  HUD's Guidelines for testing
 by XRF require only the minimum level of testing.  The apparent objective of the Guidelines
 is to satisfy  HUD's legislative directive to  test...not necessarily to locate and determine the
 presence and extent of lead hazards.

       The Guidelines fail to recognize the  fact that lead paint is heterogeneous, instead they
 assume that paint is homogeneous and  don't even require that such a critical assumption be
 checked  or verified.

       A trained inspector will test painted  surfaces in  a way that will reveal the presence of
 lead. Current HUD Guidelines reduce inspection  requirements to the lowest possible standards
 and thereby restrict inspectors'  ability to utilize their skills and knowledge.

       A well trained operator will know how to use the XRF instrument to generate statistically
 valid data.  The instruments are capable of generating valid test data if they are operating
 properly and used properly.  The current HUD testing guidelines don't even require an inspector
 to prove that he/she conducted  any testing, let alone prove that testing was accomplished with
 a properly working instrument!

       The current testing protocols underutilize existing XRF technology and worker skills
 thereby causing total testing costs to be substantially higher than necessary.  The full benefits
 of XRF instruments are ignored and expensive backup laboratory testing required much more
 frequently than is necessary.   Alarmingly, this  expensive backup  testing  is not controlled,
 checked, monitored, or regulated!

       Effective testing protocols would standardize the way dwellings and structures are tested
and test data reported so contractors are required to test  in a similar manner, check instrument
                                                                                  041993L.2

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performance regularly, and report test data in a consistent format. Most importantly, contractors
should be required to prove that they checked instrument performance, tested surfaces,  and
followed protocols.

       Housing authorities should be made responsible for the quality of test data, released from
their  obligation to award  contracts  to  the  low  bidder,  and trained  in how to  write  bid
specifications and  administrate contracts.

       Policy makers need to focus their attention on  all of the issues related to lead paint
testing: The objectives of testing need to be clearly stated and protocols developed to meet the
objectives.   Housing  authorities need their role defined,  responsibilities  identified, and  the
training to carry them out so they can be held accountable.

       Most of all, if HUD  wants high quality test data they need to specify and require
inspectors to provide and prove the quality of the data, AND, HUD must be willing to pay for
it.
                                                                                   041993L.2

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       In response to your survey we submit the following:
PORTABLE XRF SPECTROMETER

       Metals Analysis Probe ("MAP") Model 3B, used with the Ambient Scanner 310B for lead
in paint and soil analysis.

       MAP 3 - FA2C PS

Detection Limit

       Detection limit is defined as the  lowest quantity of total lead detectable  in optimum
conditions with a reasonable measurement time. Detection limits are quantified in terms of Pb
K-line X-ray detection.

       With XRF used for LBP analysis, the detection limit is a function of:

       1.     Measurement conditions
       2.     Measurement time
       3.     Confidence level desired
       4.     Source strength.

       In LBP analysis the detection limit varies with the density of the substrate, the length of
the measurement or number of repeated measurements,  and the source strength.

       Generally, as measurement conditions worsen (substrate density increases), the detection
limit deteriorates, and, as measurement time increases or lengthens, the detection limit improves
(gets lower in real terms).

       Detection limits for soil vary as a function of measurement time, matrix  structure, and
the elements contained in the sample.

       For  lead based paint measurement, the following detection limits are stated in terms of
K- and L-line precision levels at  1  standard  deviation on various substrates or combinations of
building materials.
                                                                               041993L.2

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DETECTION LIMITS - LEAD IN PAINT

       The detection limits for lead in paint on low, medium, and high density substrates are
stated  in terms  of precision  at 15, 60,  and 240 seconds  with a 40 mCi Co" radioisotope.
Precision is stated as one standard deviation of a series of consecutive measurements.
Substrate
(density)

Thin wood (low)
Wallboard (medium)
Concrete (high)
K-Shell Detection Limits in mg/cm2 at
Preprogrammed Measurement Times
15 sees
0.2
0.3
0.8
60 sees
0.1
0.1
0.4
240 sees
0.05
0.1
0.2
       The above stated K-shell detection limits were derived from data recently and randomly
collected from 46 different instruments with 25 repeated measurements each on plaster wallboard
backed with 2x4 (nominal) wood, a hollow core door, and concrete block. The average scatter
for stud backed wallboard for all 46 MAP  instruments was 0.1938, with one standard deviation
of 0.307 mg/cm2.
Substrate
(density)

Thin wood (low)
Wallboard (medium)
Concrete (high)
L-Shell Detection Limits in mg/cm2 at
Preprogrammed Measurement Times
15 sees
0.1
0.2
0.6
60 sees
0.05
0.1
0.3
240 sees
0.025
0.075
0.15
Q.     Are there any plans to allow for direct user calibration or recalibration?

A.     Scitec's policy does not allow for premature announcement of new products,  features,
       or services.  However, in general, our product strategy has not included user calibration
       or recalibration features for three important reasons:

       1.      Accurate field calibration  requires highly skilled, trained,  and  experienced
              technicians, which are short  in supply, difficult  to get to do fieldwork, and
              relatively expensive. This type of person is usually not willing to do paint testing
              on a regular basis.
                                                                                  0419WL.2

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       2.    It is difficult to design parameters  that would allow  quality control of field
             calibrations.  Allowing user calibration would allow users to set up instruments
             to produce biased measurements, e.g., "control" data output if desired.
Q.    Are you aware of the new MIST paint film SRM's?

A.    Yes. Scitec has purchased several sets of these new standards.


Q.    Have they been of any value to you in calibration or testing your instruments?

A.    No, not yet.  Only a small percentage of the XRF instruments in use are calibrated with
       the new standards.  Recalibration requires instrument downtime and expense.  It will be
       some time before all instruments are returned from the field and recalibrated.  Many
       contractors are not  willing to purchase the  MIST standards at the price NIST is asking
       nor pay for recalibration of their instruments.
Q.    Briefly describe the procedure for use of your instrument.

A.    1.     Turn it on
       2.     Enter current date
       3.     Enter calibration check ID code
       4.     Make calibration checks
       5.     Plot cal check results on graph
       6.     Verify instrument performance
             If OK,
       7.     Enter sample reference "ID" number
       8.     Make a  "TEST"  type measurement (@ 60 seconds)
       9.     When apparently homogeneous surfaces show patterns of either no lead or high
             lead, a shorter "SCREEN" type measurement is sometimes used to reduce labor
             time.

       The results of the measurement(s), the length of the  measurement(s),  the sample ID
       number, and the  raw spectral data are all stored in the system's on board  memory,
       automatically. The operator cannot select or control which measurements are stored or
       manipulate the data during transfer to a computer.
Q.     Approximate analysis time.

A.     User selected. Actual measurement time varies as a function of the source size and the
       level of precision the operator chooses.
                                                                               W1993L..2

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       The instrument allows the operator to choose one of three levels of precision, which
       equate to measurement time,  which with a 40 mCi source, are:  15, 60, 240 seconds
       (adjusted automatically by the instrument for source decay).  The actual measurement
       time is a combination of "SCREEN" and "TEST" type readings.  Contractors report an
       average of about  1 minute (includes source decay  time) per sample point.  This time
       includes screen and test mode measurements and source decay.
Q.    Interferences

A.    With K-shell X-rays no known interferences exist. With L-shell X-rays interferences can
       occur from zinc and copper.
Q.    What substrate correction procedures are used?

A.    The  MAP LBP  system  comes with a general or "universal" substrate compensation
       intrinsic in the system's software. Substrate correction is achieved through measurement
       of the  substrate effects during calibration.   Proprietary algorithms installed  in  the
       instrument during manufacture correct for substrate effects before the measurement result
       is displayed by the instrument.
Q.     Are there any new developments or guidelines for using substrate correction procedures?

A.     Substrate  characterization   using  NIST  SRM's,   dedicated  calibrations,  longer
       measurements.  We do not recommend using bare substrate measurements unless the
       operator suspects there is lead in the substrate.
Q.     Are there any built-in instrument checks to test for satisfactory operation?

A.     Yes. During a 15 second warm up immediately after the instrument is turned on, the
       system conducts a "self test" to determine if all system components are operating within
       specification.

       After any measurement the operator can view the actual spectrum of energies detected
       and measured during the analysis.  Operators are trained how to evaluate the spectrum
       to determine if the instrument was functioning properly during the analysis.

       Software used to download measurements verifies both measurement integrity and
       instrument performance. The software analyzes the spectrum to determine measurement
       validity (total counts, source strength, algorithm calculation, date, etc.).  The software
       also evaluates  the calibration  check  readings,  calculates their average and  standard

                                          7                                      W1993L.2

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       deviation and  compares the daily  data  with  the same performance criteria for  the
       instrument when it was manufactured.

       Measurements  which do not meet valid criteria or which are taken with an instrument out
       of calibration are not transferred from the console but rather are shown as "invalid."
Q.     Briefly describe safety procedures/considerations.

A.     100% positive visual and manual safety shutter with locking ON-OFF key.  A "passive-
       OFF" or dead man OFF feature provides secondary shielding independent of the ON-
       OFF key.   The operator controlled key provides positive off.  Since any/all  safety
       ultimately relies on the operator, emphasis is placed on operator training. Operators are
       required to use dosimetry monitoring and keep observers ten feet from  the XRF device
       when in use.
Q.     Are there any problems/limitations with the instrument at present?

A.     Problems:  Policy makers do not allow for proper or optimum use of the instrument.

       Limitations'.

             1.    Calibrations are based on the use of "representative" substrate standards
                   which may not always represent every material encountered in the field.

             2.    Precision of measurements on curved, profiled, or contoured surfaces is
                   variable and unknown.

             3.    Instrument should not be used in extreme heat (>  110°F).
                                                                               041993L.2

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Related Issues:
       Some "influence centers"  claim that a "limitation" of the instrument is  that negative
       readings are "truncated to zero."  Therefore, results "must be biased high."

       This claim is indicative of the lack of understanding of the practical implications of field
       work, a lack of understanding of XRF technology, and a fundamental understanding of
       statistics.

       First of all, it is impossible to have less than zero mg/cm2 lead in a paint film, therefore,
       negative readings are confusing to most inspectors.  In order for an  XRF operator to
       fully understand a negative value they must be taught basic statistics. Few field workers
       have the time, money, or inclination to learn statistics.

       When the detection limit of one reading from an instrument is larger than the "target or
       action  level,"  negative numbers can occur, but are useful  or  meaningful only if an
       averaging  process is  used, that is,  if a series of repeated readings are taken on the
       identical spot and averaged together (typical for direct readers but not for the Spectrum
       Analyzer).

       However,  if the detection limit of one reading is less than the action level,  and  multiple
       readings are not used, negative values are meaningless and add confusion to many.  Since
       a negative value is  confusing to  most people, and the action level is well above the
       detection limit for the Spectrum Analyzer, we do not normally display a negative reading
       because there is no need to do so.

       If the "action  level"  was at or  near zero (0 mg/cm2), or  the precision of a  group of
       measurements at or near zero was being determined, indication of negative results would
       be useful for the Spectrum Analyzer.

       It is not a problem  for us to display negative  readings.  We offer our customers the
       option of having the instrument display negative values.
Q.     Are improvements to the current instruments envisioned?

A.     Yes.  Scitec's  policy is to not  release new development  information prematurely.
       However, we can indicate that we spend a sizeable portion of our operating budget on
       research and development, all directed at improving instrument performance and reducing
       sources of bias-whether instrument or operator generated.

       We recently introduced a new data download software program called "AcuTransfer0"
       which checks and verifies measurement integrity and instrument performance during the
       data download process.
                                                                                 M1W3L.2

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       We also offer "Advanced Report Manager0" (ARM0) software which produces complete
       HUD type reports and analysis.

       These programs  provide a complete field testing "system" that  includes a number of
       quality control features.

       1.     Minimization  of operator bias  or  influence.   All  measurement data  are
              automatically  recorded  by  the  instrument.    That is,  the  measurement
              time/precision, test  location,  component,  paint  conditions,  substrate,  and
              calibration checks are  automatically  recorded,  analyzed, and  reported by  the
              system. The operator cannot bias test data by selecting which measurements to
              report.

       2.     Standardized testing  and sample numbering protocols allow for fast and easy
              (accurate) QC oversight during the data transfer and evaluation process.

       3.     Elimination of field notetaking errors.

       4.     Elimination of typing, transposing, and analytical errors.


Q.     When might an improved instrument be available?

A.     We regularly upgrade and enhance our product and software. The version we currently
       offer is the second model and fifth overall version of the LBP system.  All performance
       related changes are systematically made to older versions during source replacement or
       service.  The current model  is adequate for lead based  paint  testing, but  current
       guidelines do not allow for optimum use of its capabilities.


Q.     What do you view as the future needs of the public and/or lead testing organizations
       regarding portable XRF spectrometers?

A.     1.     Training of housing authorities.

       2.     Clear, concise testing protocols/guidelines with logical objectives.

       3.     Uniform bidding information.

       The major problem contractors have to deal with is the lack of knowledge the PHA has
       concerning lead testing.  Bid requests  and requests for proposals are incomplete and
       poorly written. This  does not allow contractors to compete on an equal basis.
                                          10
                                                                                041993L.2

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       Since the  Guidelines  do  not  require  contractors to  provide proof  of testing and
       compliance with  protocols, contractors regularly  cheat.  Housing authorities are not
       trained or equipped to deal with these problems.
Q.     What topics should be added to the workshop agenda?

A.     We suggest emphasis be placed on:

       1.      Ways of eliminating sources of errors and bias from:

              a.     Operator influence
              b.     Bid requests,  contract awards, contract  administration
              c.     Data handling, recording, reporting.

       2.      Optimizing the use of XRF for field testing.  Current,  and even the proposed
              Guidelines do not allow for or provide incentives for use of the full capabilities
              of XRF  instruments. The Guidelines are written to accommodate the oldest form
              of technology rather than the most advanced form of technology. Therefore HUD
              receives poor quality data at very high total costs.

              Attention should be given to:

              a.     Limited use of L-Shell XRF Analysis.   This type of XRF analysis  has
                    been overlooked, or not even allowed.  However, we believe there is a
                    potential  for  the  use of L-shell  analysis in conjunction  with K-shell
                    analysis.

                    L-line X-rays  can be detected only  if there is lead on the immediate
                    surface coats of paint (i.e., the top 1 or 2 layers).  Because of this many
                    people think that L-shell analysis is not  useful since most lead paint is on
                    the bottom,  or lowest layers,  and therefore only K-line X-rays are useful.
                    However, if lead is  on the surface, 1)  it is a more immediate potential
                    hazard and 2) it can  be measured more  accurately.

                    In some  cases use  of  an  L-shell reading can  reduce  the  need  for
                    confirmatory sampling by AA.

                    L-shell lead  X-ray measurement provides lower detection limits and better
                    precision than K-shell lead X-ray measurement. This is due to the higher
                    yield achievable and the reduced effects from substrate conditions.
                                           11                                     041993L.2

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             We do not propose that L-shell measurement be a substitute for K-shell
             measurement,  but an allowable  alternative  in some cases...if there is
             greater than 1.10 mg/cm2 of lead on the surface coat of paint the condition
             is positive!

             In addition,  L-shell  analysis can be  used to help determine  whether
             detected lead is  behind an outer substrate (e.g., a  pipe, painted wall,
             flashing, etc.), or in the substrate.

       b.     Use  of short and/or long XRF  readings.   The current and proposed
             Guidelines limit  the  usefulness of XRF by limiting the number of,  or
             length of readings allowed and fixing a single inconclusive range where
             chip sampling/lab  analysis  are  required.   This policy unnecessarily
             increases the total testing costs incurred by HUD.

             With the Spectrum Analyzer, a longer, or "CONFIRM" type reading will
             provide a measurement  with  twice  the  precision  of the  "TEST"
             measurement which  is specified by HUD.  Use of a "CONFIRM"  type
             measurement only when the apparent lead concentration is at or near the
             action level would reduce the amount of lab sampling by 50%.

             On the other hand, allowing inspectors to use shorter "SCREEN"  type
             measurements when  lead concentrations are at or near zero, or very  high
             (above 1.5 mg/cm2)  will reduce field testing costs by 60%.

3.      Operator, EPA,  HUD Training.  The current XRF operator training provided
       during EPA courses by the universities is not focused on the most important  field
       issues-how to generate statistically valid test results.  The training is often
       provided by scholastic types who have little or no field experience, or by selected
       contractors  whose  technical  experience is  limited, and  sometimes  biased.
       Training often includes  special interest sub-agendas as the  EPA has no policy
       regarding trainers having conflicts of interest.

       We've found that public housing  authorities and contract administrators lack a
       fundamental understanding of XRF, sampling, and/or statistics.

       Public housing authorities, for the most part,  do not fully understand what it is
       they are tasked to do,  so their requests for proposals  and/or requests for bids are
       poorly worded, structured, and contain inadequate information for contractors to
       respond to in a  meaningful way.   Many  contractors do  not respond to bid
       invitations simply because of the lack of information.
                                   12
                                                                          OU993L.2

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       Most often bids are awarded to the "low bidder," without regard to the technical
       skills of the bidding firm or the total testing costs.  By awarding contracts in this
       way,  public housing   authorities and government  agencies are  providing
       contractors with the means  to rip them off.  Many bids allow,  even  require
       conflict of interests to take place!

       Most contract administrators do not know  how to evaluate, inspect or interpret
       lead testing  reports once  they get them.  Contractors  can  turn  in just about
       anything,  call it a test report, swear to its  authenticity (with several disclaimers
       thrown in throughout the report) and get paid!

       Standardized bid requests, evaluation methods and testing contracts are needed.
       Fundamental training in how to administrate and supervise testing work is needed,
       and standardized test report and data handling methods will reduce the burden on
       housing agencies and improve the quality of the test data.

       Most  of all, testing contractors  should provide  proof that  statistically valid
       random testing  was conducted, and  conducted  with an instrument which was
       working properly.

4.     Laboratory confirmation.  HUD's Guidelines require laboratory confirmation of
       all "inconclusive" and "positive" XRF test results in spite of an absence of any
       study  or  data about the accuracy  and quality of the chip sampling/lab  analysis
       method of sampling.

       Our informal surveys  and evaluation  of  test  data  from contractors and labs
       indicates that the chip sampling/lab analysis method tends to produce results with
       a low  bias, thus providing "false negatives" on inconclusive XRF tests.

       This method is expensive and very time consuming, and  does not necessarily
       provide suitable back-up or "confirmatory" defensible data.

       The main issue here is not the ability of laboratory  instruments and technicians
       to accurately measure lead in paint films  (although there is concern about this
       from one  lab to another), but the ability  of the contractor to remove a good,
       representative sample.

       We recommend:

       a.     A study of the accuracy and cost of  the chip sampling/lab analysis method
              be conducted.

       b.     Quality control methods need to be developed for the chip samplingAab
              analysis procedure.

        c.     Alternative methods of dealing with preliminary "inconclusive" XRF tests
              be investigated, and/or allowed.
                                     13                                      041993L.2

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       We hope our response is helpful to you and will further your efforts to develop effective
evaluations of XRF instruments and guidelines for their use.  We urge you to involve instrument
manufacturers in all processes; we're a source of expertise and experience! Everyone has their
biases, or preferences and prejudices, so you should at least hear and take all input.  Scitec is
willing to participate openly in any and all discussions.  We're looking forward to working with
you.

                                               Sincerely,

                                               Larry T.  Lynott
                                               President

encl:   HAD

cc:    Jim Baugh
      Darren Small
                                          14
                                          i^                                      041993L.2

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  Data Presented by
TN Technologies, Inc.

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                Portable XRF Spectrometer

 Name or Model # of spectrometer Spectrace 9000 (Pb Analyzer)

 Applications Several applications are provided for; with the primary one
 being an optimized configuration for the in-situ measurement of Pb in
 paint film via its "K" and "L " x-ray excitation. This is a mass per unit area
 analysis which reports the values of both the PbL and PbK results on the
 same screen. Other unit area analyses provided include an application for
 dust wipes and filtered  (air/water) particulates. An application for the
 determination of Pb by mass concentration (in ppm. %, or other units) in
 bulk materials such as  soil, dust,  water, etc. is  also contained.  The
 analyses are not limited to Pb; elements such as Hg, As, and many other
 metal pollutants can  be quantified in the same measurement. This
 response relates only to  the Pb-paint application.

 Detection Limit For a single 60 sec measurement the approximate MDLs
 are as follows; « 0.002mgPb/cm2 for the PbL analysis on any substrate,
 and in the range  0.04  to  0.12 mgPb/cm2 for the PbK analysis for
 substrates ranging from thin wood to thick concrete. It will be ~ 0.06 on
 gypsum-over-wood. On thick steel the PbK MDL will be = 0.2mgPb/cm2.

 How is the detection limit determined? It is equated to THREE TIMES the
 standard deviation  (3o) in the results of a measurement (expressed in
 calibrated concentration units) performed on a blank, or low metal content
paint film in contact with a defined substrate. (J-values may be derived
 from the results of repetitive measurement (negative values can be
displayed or printed) or obtained directly from the  analysis report. The
latter reports the o-value of each result according to the conditions of the
measurement (i.e. time, signal strength, source decay etc) and taking into
account  the accumulative statistical errors of all aspects of the data
processing including the  spectrum  strip and the substrate correction
mathematics.

Sensitivity In terms of the net (less substrate) counts/sec/mgPb/cm2, the
sensitivity for PbL analysis is ~ 300, and that for the PbK is ~ 5. In units
of "per millicurie of exciting source radiation" the respective numbers
would be 60 and 5. A Cd-109 source  with the emission equivalent of
5mCi x-rays and 1mCi gamma is used in the instrument.

-------
 How is the sensitivity determined?  By measurement on a series of known
 mgPb paint films and calculation of the initial slope of the source-decay-
 corrected (SDC) countrate/mgPb response.  The NIST 2759 Pb standards
 present  a suitable range.  SDC countrate values can be viewed on the
 instrument screen.

 Accuracy  For a single 60 sec the accuracy of a PbK determination will
 be   ~ ±0.125mgPb/cm2   at  a   loading   of  0.5mgPb/cm2   and
 « ±0.16mgPb/cm2 at a loading of 1.0mbPb/cm2. The influence of paint
 thickness on the PbL measurement makes it difficult to assess  the
 accuracy of that analysis.

 How is the accuracy determined? From the magnitude of the difference
 between the x-ray results and the  "mass/area " chemical analyses  of a
 representative range of samples on a variety  of substrates comprising
 wood, plaster and concrete. The expected accuracies (listed) are based
 on the  2-standard  deviation criteria  and  include  no allowance  for
 knowledge of the substrate. In reality the accuracy is slightly better on a
 wood substrate and that can be evaluated on an individual results basis
 since  the  statistical uncertainties  are  always  reported with  each
 measurement. For example an accuracy of ~ 0.1mgPb could be expected
 on wood.

 Briefly  describe  the calibration  procedure.  The primary  calibration
performed at the factory entails measurement of several pure elements,
 various bare substrates and at least one NIST 2759 standard reference
sample.  A  secondary calibration using an  equivalent of the  substrate
material and a Pb reference sample can be performed in  the field. All
calibration constants are retained in a non-volatile on-board memory. They
are also importable from a floppy disk.

Are there any plans to allow for direct user calibration or recalibration?
As indicated there is provision for user recalibration.

Are you aware of the new NIST paint film SRMs? Yes.

Have  they  been  of  any value to  you in  calibrating  or  testing  your
instruments?  Yes. They are used in the primary calibration and will be an
essential part of the calibration maintenance.

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 Briefly describe the procedure for use of your instrument.  Operation is
 menu driven so all steps are shown on the screen. Measurement can
 begin  ~5min after turn-on. It is push-button  initiated and program
 controlled so that the source shutter will automatically close at the end
 of a short period of measurement. The probe (of ~ 4 Ibwt) must be held
 steady but there is no need to maintain any pressure against the surface.
 The result's display of both PbK and PbL,  together with their error level
 is self-explanatory. A menu choice will automatically store the results, as
 well  as  the spectrum  if  desired.  Prior to beginning  a series  of
 measurements the operator will perform a check for ~ WOsec. If an error
 condition is detected the screen will direct the operator to perform  an
 adjustment.  Several automatic checks, such as the spectrum calibration,
 are also performed during measurement and the operator is alerted to any
 problem.  The need for battery renewal will be indicated with enough
 warning to protect stored results.

 Approximate analysis time  The time (in  real clock seconds) is  user
 selectable from 1 sec up. Recommended time is  ~ 15 sees for an initial
 check.  This should provide for a reliable (95% confidence) x-ray based
 assessment  at  the  1mgPb level on all results except  for those in  an
 "uncertain" zone of 0.75 to  1.25 mgPb. Results within that zone will
 require additional time.

 Interferences  The  main  interference on the analysis  is that of the
 substrate scattered radiation  in the spectral window of the Pb x-rays.
 Other element fluorescent x-rays are excluded by the high resolution of
 the x-ray detector.
                                                      \
 What substrate  correction procedures are used?  The spectrum overlap
 from  the substrate is relatively small, due to the choice of source and
good detector resolution.  It must stiff be  corrected for however and this
is accomplished by a special stripping algorithm that is applied to  each
spectrum  as it is acquired in the measurement. The coefficients of the
stripping algorithm  are maintainable by the  operator  using  a set  of
substrate-equivalent standards.

Are there  any  new developments  or  guidelines for using substrate
correction procedures? Describe. None are known at this time however

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 there is a/ways room for improvement in this area.  The ability to store the
 entire,  high resolution spectrum for further evaluation should prove useful
 in this  direction.
 Are there any built-in instrument checks to test for satisfactory operation?
 Describe.  Yes as described earlier.  The spectrum is continuously checked
 for gain calibration and the operator has a CHECK procedure to conduct
 periodically.  Other continuous checks are made on the signal quality and
 any malfunction will be indicated on the screen.

 Briefly describe safety procedures/considerations. The main concern must
 always be over the chance of accidental exposure to the source. On the
 9000 the source gamma ray emission is only 1/35 of that used in other
 spectrum analyzers and is also of lower gamma ray energy. Adequate
 shielding is built-in for the source closed position.

 Are there any problems/limitations with the instrument at present? The
 probe face may be considered wide f~3") for some situations.

 Are improvements to the  current instruments envisioned?  Yes. For
 example more efficient larger detectors could become available to allow
 even lower activity source usage or shorter measurement times. A smaller
 footprint, lighter probe may also be possible in the near future.

 When might  an improved instrument be available? Some improvements
 could be achieved within a 12 month time frame.

 What  improvements will be  implemented?  Possibly a lighter,  smaller
 footprint measurement probe

 What do you view as the future  needs of the public and/or lead testing
 organizations regarding portable XRF spectrometers?  Better procedures
 for sampling  in regard to XRF instrument verification of the mass/unit
 analysis and a resolution of the % wt versus mgPb dilemma in the current
 code.

What topics  should  be added to the XRF workshop agenda?   Other
analytical  techniques.  Standardization  progress  reports  of other
committees.  Opinions on the "% " vs "mg" dilemma.

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Please provide  any standard operation procedures, instrumentations or
other literature you believe would be informative. Copies of the standard
instrument manual were provided.  The attached pictorial comparison of
current PbK analysis based instruments shows a wide range of values of
the "net signal to background" parameter as a result of the source choice
and the system spectral resolution. A high signal to background reduces
the effect of the background variation, i.e. the substrate problem,  and
allows one to expect accuracies that are limited only by the statistical
factors imposed by the analysis time.

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    SCINTILLATION
     plus FILTERS
                          GAS
                      PROPORTIONAL
      T   I
~iIII "  I
111
     SILICON
                      90
          ENERGY (keV)

             110
Comparison of "NET-to-BACKGROUND" Ratio at
  15mgPb/cm2 on Wood for Various Detectors
          ENERGY (keV)
                  110

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  Data Presented by
Princeton Gamma-Tech

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                    Portable XRF Spectrometer
 Name or Model # of spectrometer      PCT Model XK-3
      'Ptaeae reproduce this form {f other rtwf&s are available.
 APPficaik>n&         Painted surfaces	
                        (Paint, Soil, Dust, etc.)
 Detection Limit	0.5 mg FWtac2	How is the detection Rmit
 determined?   It is taken as the single-reading standard deviation of a series
  of readings.		
 Sensitivity	0.5 majpb/ca2                     How is the sensitivity
 determined?	It la taken as  the single-reading standard deviation of
 	   a. aeries of readincfi.	
Accuracy	How is the accuracy
determined?    Accuracy is  determined by comparing instrument  readings with
U.S. Pqpt.  of HUD lead standards  of  CL60. \t'ft pftd 2.99 mp/r-m2 ^.traceable
to HBS standards.  ROTE:  Precision can be increased by averaging 9. number of
readings.
Briefly describe the Cafbratioa procedure   A series of IP readings  are  taken on
 0 and 1.53 Bg/ca^ HUD  standards.  Internal adjustments are  Chen ma'de to brine
 the unit into calibration  and the procedure repeated until  both readings
 vlthln  -f/- 0.1
Are there any plans to allow for direct user caffbration or recafibration?     NO.

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 Are you aware of the new NIST pair* film SRMs?  Yes
 Have they been of any value to you in cafibrating or testing your instalments?.
   No.   We were  lucky  enoagb to have old HDD standards.   	
 Briefly describe the procedure for use of your instalment  After checking calibration and
 stabilisation (varmup), the face of the XK-3 is placed against the surface to be testet

 and the  handle pushed in_to. the stop.  The hoodie ia held infirmly until a reading  ->
 appears  on  the display, signaled by an audible beep.  The reading remains displayed
 uctll a  new ateagareaent is Initiated.  We attach an Operator'a Maonal for your
 further  information.

 Approximate analysis time     About 12 seconds for a fresh source.


 Interferences   Only backscattered gamma rays.	__	


 What SUbStraie Correction procedures are Used?    Manual substrate corrections
 arc -oa.de, in accordance vlth the recommendations of the BUD guidelines.	
Are their any new developments or guidelines for using substrate correction procedures?
Describe.^	»o.         	
Are there any built-in instalment checks to test for satisfactory operation? Describe,	
Only the calibration check block provided with  the instrument.	

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 Briefly describe safety proceduresAjonskterafions  The XK-3. is unique,  its radiation
source shutter cannot be opened unless  the face of the  XK-3 is against a solid surface.
This prevents anyone from being exposad by the gamma-ray beam, which is possible with
other available inscrircenta.   Specific  safety practices are covered In detail la our
User School, attendance at which Is  strongly recommended for anyone using the instrunei

 Are there any problems/Hmftations with the instrument at present?	
         See cqyer letter.
 Are improvements to the current instruments envisioned?.
         Sae cover letter.
When might an improved instrument be available?.
         See cover  letter.	
What improvements will be implemented?
         See cover  letter.	
What do you view as the future needs of the pubic and/or lead testing organizations
regarding portable XRF spectrometers?	
         See cover letter.       	   	
What topics should be added to the XRF workshop agenda?
         See cover letter.	•  	

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Pfease provide any standard operating procedures, Instrumentations or other literature
you believe would be informative. __	
            attached
                                                         **  TOTAL  PAGE.006 **

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