1 Determination of Lead in Dust Wipes using Field Analytical Technology Presented by U.S. Environmental Protection Agency’s (EPA) Office of Superfund Remediation and Technology Innovation (OSRTI) and Office of Research and Development (ORD) and the Department of Energy’s (DOE) Oak Ridge National Laboratory (ORNL) Determination of Lead in Dust Wipes using Field Analytical Technology Presented by U.S. Environmental Protection Agency’s (EPA) Office of Superfund Remediation and Technology Innovation (OSRTI) and Office of Research and Development (ORD) and the Department of Energy’s (DOE) Oak Ridge National Laboratory (ORNL) 1 1
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Determination of Lead in Dust Wipes using Field Analytical Technology 1 Determination of Lead in Dust Wipes using Field Analytical Technology Presented by U.S. Environmental Protection
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Determination of Lead in Dust Wipes using Field Analytical Technology
Presented by
U.S. Environmental Protection Agency’s (EPA) Office of SuperfundRemediation and Technology Innovation (OSRTI) and
Office of Research and Development (ORD)
and the Department of Energy’s (DOE) Oak Ridge National Laboratory (ORNL)
Determination of Lead in Dust Wipes using Field Analytical Technology
Presented by
U.S. Environmental Protection Agency’s (EPA) Office of Superfund Remediation and Technology Innovation (OSRTI) and
Office of Research and Development (ORD)
and the Department of Energy’s (DOE) Oak Ridge National Laboratory (ORNL)
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Background Environmental Technology
Verification Program
¾ Early 1990s - Need for environmental technology verification identified� Slow rate of innovation; poor U.S. markets� Lack of credibility of new technologies� Inertia of system, risk aversion of purchasers and
permitters� Burgeoning international market
¾ EPA initiates ETV in October, 1995
Background Environmental Technology
Verification Program
¾ Early 1990s - Need for environmental technology verification identified � Slow rate of innovation; poor U.S. markets � Lack of credibility of new technologies � Inertia of system, risk aversion of purchasers and
permitters
� Burgeoning international market¾ EPA initiates ETV in October, 1995
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ETV Objectives¾ Provide credible performance data for
commercial en a e ologiesto aid � vendors in selling innovative technologies,� purchasers in making decisions to
� regulators in making permitting decisions
ETV Objectives¾ Provide credible performance data for
commercial e vironment l t chvironment l t chnologiesa e to aid � vendors in selling innovative technologies, � purchasers in making decisions to
purchase innovative technologies, andpurchase innovative technologies, and� regulators in making permitting decisions
ETV Successes� 240 Verifications, 78 protocols to date � Vendor demand continues – over 100 technologies
in testing/evaluation, over 100 applications pending � Increasing funding from vendors and others � 805 Stakeholders in 21 groups � Commendations from EPA science and policy
advisory boards � Supports regulatory and voluntary Agency, other
Federal and state programs � Growing international interest � New role in homeland security verifications
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ETV Verifies only
¾ Definition: Verify is to determine performanceunder test� No winners or losers� No approvals � No certification� No pass or fail � No guarantees
¾ Responsibility rests with the technology user toy
ETV Verifies only
¾ Definition: Verify is to determine performanceunder test plan defined conditionsplan defined conditions � No winners or losers � No approvals � No certification � No pass or fail � No guarantees
¾ Responsibility rests with the technology user to correctlcorrectly choose and apply technologieschoose and apply technologies
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Stakeholder Roles
¾ Help set verification priorities¾ Review protocols and operating
procedures¾ Review other important documents¾ Assist in designing and conducting
outreach activities¾ Serve as information conduits to
their constituencies
Stakeholder Roles
¾ Help set verification priorities ¾ Review protocols and operating
procedures ¾ Review other important documents ¾ Assist in designing and conducting
outreach activities ¾ Serve as information conduits to
their constituencies
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ETV Centers¾ ETV Air Pollution Control Technology Center
� Research Triangle Institute¾ ETV Drinking Water Systems Center
� NSF International¾ ETV Greenhouse Gas Technology Center
� Southern Research Institute¾ ETV Advanced Monitoring Systems Center
� Battelle¾ ETV Water Quality Protection Center
� NSF International¾ ETV- Building Decontamination Center
� Battelle¾ ETV P2 Coatings and Coating Equipment Pilot
� Concurrent Technologies Corporation
ETV Centers¾ ETV Air Pollution Control Technology Center
� Research Triangle Institute ¾ ETV Drinking Water Systems Center
� NSF International ¾ ETV Greenhouse Gas Technology Center
� Southern Research Institute ¾ ETV Advanced Monitoring Systems Center
� Battelle ¾ ETV Water Quality Protection Center
� NSF International ¾ ETV- Building Decontamination Center
� Battelle ¾ ETV P2 Coatings and Coating Equipment Pilot
� Concurrent Technologies Corporation
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46 Verifications in 2003¾AMS: 5 Arsenic Detection; 5 Mercury CEMs; 1 Onboard Mobile
Emission Monitor; 1 Gas Emission Monitor;2 Multi-Parameter Water Probes; 6 Cyanide Detection Kits
¾SCMT: 1 Lead in Dust; 2 Groundwater Sampling Devices ¾APCT: 3 Mobile Source Devices¾GHG: 1 Fuel Cell; 2 Micro-turbine CHP; 1 Vehicle Axle
Anodic Stripping Voltammetry for Determination of Lead
Anodic stripping voltammograms for thesample a o standa s of 50
Deposition potential = -600 = 1 n.; quiet time =
ec. frequency = Hz; steppot a
S.W. amplitude = 25 mV26
Anodic Stripping Voltammetry for Determination of Lead
Anodic stripping voltammograms for the nd tw rd additionsample and two standard additions of 50
ppbppb Pb(IIPb(II).). Deposition potential = -600 mV; deposition time mimV; deposition time = 1 min.; quiet time =
10 s S.W. 1510 sec. S.W. frequency = 15 Hz; stepenti l = 4 mV;potential = 4 mV;
S.W. amplitude = 25 mV
Pb(II) is reduced to Pb(0) by holding potential at cathodic value for brief period; Pb quantified with anodic potential sweep, measuring current for oxidizing Pb(0) to Pb(II) and stripping it from solid electrode.
Electrochemical cell uses a working (W), reference (R), and auxillary (A) electrodes in cylindrical tube with teflon cap.
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Anodic Stripping Voltammetry
¾ Advantagesz Low capital costz Disposable materialz Very high sample throughput
¾Disadvantagesz Generates small amounts of chemical waste
Anodic Stripping Voltammetry
¾ Advantages z Low capital cost z Disposable material z Very high sample throughput
¾ Disadvantages z Generates small amounts of chemical waste
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X-Ray Fluorescence
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X-Ray Fluorescence Exposing metallic materials to high energy x-rays stimulates ejection of electrons the energies of which provide information concerning the identity of the metal in
question.
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X-Ray Fluorescence
¾ Advantagesz Non-destructive analysisz Produces no chemical wastez Good sample throughput
¾Disadvantagesz High capital costz May need radiation source license
X-Ray Fluorescence
¾ Advantages z Non-destructive analysis z Produces no chemical waste z Good sample throughput
¾ Disadvantages z High capital cost z May need radiation source license
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NITON XL300
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NITON XL300
0
5
10
15
20
25
l
Precision
75
80
85
90
95
Accuracy
l
ELP A T Sam ples UC Samp es
N IT ON 300 R ef Lab
100
105
110
115
120
125
ELP A T Samples UC Samples
N IT ON 300 R ef Lab
Less is better
Idea
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NITON XL300
303346400
213224250
423940
ELPATSamples,µg/wipe
UC Samples,µg/wipe
ClearanceLevel
µg/wipe
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NITON XL300
303346400
213224250
423940
ELPAT Samples,
ipe
UC Samples,
ipeipe
30 40 45
(
µg/wµg/w
Clearance Level
µg/w
Reported Concentrations at Clearance Levels
True Pb Concentration (ug/wipe) 35 50
PrR
epor
t < 4
0 gi
ven
True
Pb)
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
DataChem Niton XL-300
Probabilities of False Negatives
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NITON XL300NITON XL300
Comparability: R = 0.999 (ELPAT samples); R = 0.999 (UC samples)
False positive results (relative to clearance levels): 0% (0 of 12 ELPATSamples); 0% (0 of 30 UC samples)
False negative results (relative to clearance levels): 54% (15 of 38 ELPAT); 70% (21 of 30 UC samples) [25% and 77% for Reference Laboratory]
Reporting limit: 15 µg/wipe
Throughput (1 analysts): 40 samples/12 hr day
Statistically significant negative bias (“penalty” for high precision) but within acceptable bias range.
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NITON XL700
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NITON XL700
75
80
85
90
95
110
115
0
5
10
15
20
25
Accuracy
Precision
l
100
105
120
125
ELP A T Sam ples UC Sam ples
N IT ON X L700 R ef Lab
ELP A T S amples UC Sam ples
N IT ON XL 700 R ef Lab
Less is better
Idea
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NITON XL700
372431400
272276250
494240
ELPATSamples,µg/wipe
UC Samples,µg/wipe
ClearanceLevel
µg/wipe
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NITON XL700
372431400
272276250
494240
ELPAT Samples,
ipe
UC Samples,
ipeipe
) 35 40 45
)
µg/wµg/w
Clearance Level
µg/w
True Pb Concentration (ug/wipe30 50
Pr(R
epor
t < 4
0 gi
ven
True
Pb
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
DataChem Niton XL-700
Reported Concentrations at Clearance Levels
Probabilities of False Negatives
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NITON XL700
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NITON XL700
Comparability: R
: ;
7]
Reporting limit
Throughput (1 analyst):
= 0.999 (ELPAT samples); R = 0.999 (UC samples)
False positive results (relative to clearance levels) 50% (6 of 12 ELPAT Samples) 62% (21 of 34 UC samples)
False negative results (relative to clearance levels): % ( 2 of 28 ELPAT); 8% (2 of 26 UC samples) [25% and 77% for Reference Laboratory
: 15 µg/wipe
30 - 60 samples/12 hr day
Statistically significant positive bias (“penalty” for high precision) but within acceptable bias range.
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NITON XLt 700
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75
80
85
90
95
110
115
0
5
10
15
20
25
Accuracy Precision
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NITON XLt 700
100
105
120
125
ELP A T Sam ples UC Sam ples
N IT ON X L700 R ef Lab
ELP A T S amples UC Sam ples
N IT ON XL 700 R ef Lab
Less is better Idea
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NITON XLt 700
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Comparability: R
: ;
29]
Reporting limit
Throughput (2 analysts):
NITON XLt 700
= 0.999 (ELPAT samples); R = 0.999 (UC samples)
False positive results (relative to clearance levels) 8% (1 of 12 ELPAT Samples) 22% (8 of 37 UC samples)
False negative results (relative to clearance levels): % ( 8 of 28 ELPAT); 43% (10 of 23 UC samples) [25% and 77% for Reference Laboratory
: 10 µg/wipe
45 - 50 samples/10 hr day
Statistically significant negative bias (“penalty” for high precision) but within acceptable bias range.
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NITON XLt 700
361371400
234232250
424240
ELPATSamples,µg/wipe
UC Samples,µg/wipe
ClearanceLevel
µg/wipe
NITON XLt 700
Reported Concentrations at Clearance Levels
Clearance Level
µg/wipe
UC Samples, µg/wipe
ELPAT Samples, µg/wipe
40 42 42
250 232 234
400 371 361
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/ ) 10 15 20 25 30 40 45 55
(i
)
True Pb Concentration (ug wipe35 50
PrR
epor
t < 4
0 g
ven
True
Pb
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
NITON XLt 700
DataChem
Probabilities of False Negatives
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Keymaster Pb-Test XRF
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75
95
ug/
0
5
10
15
20
25
Accuracy Precision
l
Keymaster Pb-Test XRF
115
135
155
175
195
ELP A T Samples
UC Samples
Keym aster P b T est R ef Lab
Keym aster >200 wipe
ELP A T S amples UC Sam ples
Keym aster P b T est R ef Lab
Less is better Idea
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Keymaster Pb Test XRF
248365400
254275250
9911840
ELPATSamples,µg/wipe
UC Samples,µg/wipe
ClearanceLevel
µg/wipe
40
) 35 40 45 50
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
248365400
254275250
9911840
ELPAT Samples,
ipe
UC Samples,
ipeipe
l l
/wi
True Pb Concentration (ug/wipe
Pr(R
epor
t < 4
0 gi
ven
True
Pb)
DataChem
Pb-Test
Keymaster Pb Test XRF
µg/wµg/w
Clearance Level
µg/w
Reported Concentrations at Clearance Levels
Probabilities of False Negatives
Due to the positive bias at low ead evels, there was no chance of a false negative Response at the 40 µg pe level
False positive results (relative to clearance levels) 25% (3 of 12 ELPAT Samples) 14% (4 of 29 UC samples)
False negative results (relative to clearance levels): 43% ( 12 of 28 ELPAT); 59% (17 of 29 UC samples) [25% and 77% for Reference Laboratory
: < 20 µg wipe
Throughput (2 analysts and 1 instrument): 80 samples/10 hr day
Statistically significant negative bias; less precise than typically acceptable levels; strong linear relat onship between PDV 5000 response and that of comparable lab method.
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PalintestScanning Analyzer SA-5000
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Palintest Scanning Analyzer
75
80
85
90
95
0
1
2
3
4
5
6
7
8
9
10
Accuracy Precision
l
SA-5000
100
105
110
ELP A T Samples UC Samples
SA -5000 R ef Lab
ELP A T Sam ples UC Sam ples
SA -5000 R ef Lab
Less is better Idea
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PalintestScanning Analyzer SA-5000
372308400
221189250
363540
ELPATSamples,µg/wipe
UC Samples,µg/wipe
ClearanceLevel
µg/wipe
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) 45 50 55
()
Palintest Scanning Analyzer
372308400
221189250
363540
ELPAT Samples,
ipe
UC Samples,
ipeipe
True Pb Concentration (ug/wipe35 40 60
Pr R
epor
t < 4
0 gi
ven
True
Pb
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
DataChem Palintest
SA-5000
µg/wµg/w
Clearance Level
µg/w
Reported Concentrations at Clearance Levels
Probabilities of False Negatives
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PalintestScanning Analyzer SA-5000
Palintest Scanning Analyzer SA-5000
Comparability: R = 1.00 (for UC samples ); R = 0.995 (for ELPAT samples);
False positive results (relative to clearance levels): 0% (0 of 12 ELPATSamples); 0% (0 of 38 UC samples)
False negative results (relative to clearance levels): 61% ( 17 of 28 ELPAT); 100% (22 of 22 UC samples) [25% and 77% for Reference Laboratory]
Reporting limit: < 25 µg/wipe
Throughput (1 analyst and 1 instrument): 80 samples/10 hr day
Statistically significant negative bias; very precise; strong linear relationship between SA-5000 response and that of comparable lab method; no false positives, high number of false negatives.
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ETV Program does NOT make Head to Head comparisons of
technologies, because there are needs for a variety of tools in the environmental technology toolbox
ETV Program does NOT make Head to Head comparisons of
technologies, because there are needs for a variety of tools in the environmental technology toolbox
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Asking: “What is the Best Technology?” is Like Asking “What is the Best Vehicle to Purchase?”
It depends on what you need!
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Asking: “What is the Best Technology?” is Like Asking “What is the Best Vehicle to Purchase?”
It depends on what you need!
Sports car vs. MiniVan
PS: Your mileage may vary
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Upcoming Technology Verifications by the Advance Monitoring Systems
Center¾ More rounds of arsenic test kits for water¾ Multi-parameter water monitors¾ Ambient ammonia monitors for animal feed