update on manual method for sampling and analysis of ...update on manual method for sampling and...
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Update on Manual Method for Update on Manual Method for Sampling and Analysis of Sampling and Analysis of Condensable ParticulateCondensable Particulate
Ray Merrill Ray Merrill –– ERGERGRon Myers Ron Myers –– EPAEPA
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OverviewOverviewMethods backgroundMethod 202 performance (bias)Methods Comparison– Hardware & preparation– Sampler operation– Recovery requirements– Analytical finish
Dry Impinger Method performance– Bias– precision
Schedule
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BackgroundBackgroundWhat is Condensable PM ?What is Condensable PM ?
Vapors and gases at stack temperature that form liquid or solid aerosols upon coolingAll condensable PM <1μM
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BackgroundBackgroundHow was Condensable PM Measured?How was Condensable PM Measured?
Existing Method 202– Promulgated in 1991– Over 6 options in method– Artifact issue
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BackgroundBackgroundWhatWhat’’s Changing with Condensable PM Measurement?s Changing with Condensable PM Measurement?
Dry Impinger Method (OTM-28)– Originally proposed by John Richards
(Method 202 variant)– Single standard procedure (no options)– Minimizes SO2 artifact– Low level blank management– Will replace EPA Method 202
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Method 202 Artifact (bias)Method 202 Artifact (bias)
Artifact Mass (mg)SO2
ppmTest
durationH2O
volume No Purge Purge
300 1 Hr 400 ml 180 ± 6 10 ± 0.5
300 3 Hr 800 ml 400 ± 25 20 ± 5
50 6 Hr 1400 ml 200 ± 10 20 ± ??
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OTMOTM--28 Sampling Train28 Sampling TrainDry Impinger GlasswareDry Impinger Glassware
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OTMOTM--28 CPM Filter Media28 CPM Filter Media
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Method Comparison:Method Comparison:Glassware PreparationGlassware Preparation
Existing Method 202 Dry Impinger MethodSoap & Tap Water WashTap Water Rinses
Acetone RinseMeCl Rinse
Soap & Tap Water WashTap Water RinsesUltrafilter water rinseAcetone RinseMeCl RinseHeat @ 300 Heat @ 300 °C C –– 6 Hrs6 Hrs
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Method Comparison:Method Comparison:Glassware Set UpGlassware Set Up
Existing Method 202 Dry Impinger MethodMethod 23 Condenser
2 G/S Impingersw/ tipped stems100ml DI water
G/S Impinger w/ short stem, no water
1 G/S Impinger w/ 100 ml DI water
G/S Impinger w/ stem w/o water
Optional filter Filter
G/S Impinger w/ 100 ml water
G/S Impingerw/ Silica Gel
G/S Impinger w/ Silica Gel
Opt
ion
#1
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Method Comparison:Method Comparison:Sampling TemperatureSampling Temperature
Existing Method 202 Dry Impinger Method
Maintain ALL four impingers in ice water bath
First two impingers in ≈ 85° F water bath
Filter Gas @ ≤ 85° F
Last two impingers in ice water bath
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Method Comparison:Method Comparison:Post Test RecoveryPost Test Recovery
Existing Method 202 Dry Impinger MethodNitrogen PurgeAir PurgeNo Purge
Mandatory Purge with filtered UHP NitrogenOptional}
Option #2
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Recovery Requirements:Recovery Requirements:Reagent Quality RequirementsReagent Quality Requirements
Existing Method 202 Dry Impinger MethodDI Water – ASTM Type II
Acetone – not usedMeCl – ACS Grade
<0.001% residueNH4OH – 14.8 Molar
DI Water –Ultra filteredASTM Type II
Acetone - < 1 ppm residueMeCl – ACS Grade
< 1 ppm residueNH4OH – NIST traceable
0.1 Normal
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Dry Impinger MethodDry Impinger MethodSampling
Verify Sample Validity
Valid? Discard
Measure sample
volumes Dry &
W eigh filters
Extract samples
Evaporate organic
W eigh Residue
No
Yes
Organic Fraction
Oven & ambient evap
Reconst. 100 mL
Titrate w/NH 4OH
Correct M ass for NH 4 Added
Oven & ambient evap
W eigh pan & measure Inorganic
CPM
Inorganic Fraction
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Method OTMMethod OTM--28 Comparisons28 Comparisons
OTM – 28 Compared to– Method 202– Controlled Condensate– Low Temperature Filter Train
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OTM OTM –– 28 to Method 202 Comparison28 to Method 202 Comparison(EPA Laboratory Study)(EPA Laboratory Study)
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OTM OTM -- 28 vs. M202 28 vs. M202 (Gravimetric Comparison)(Gravimetric Comparison)
Source: Electric Power Research Institute, 2008Source: Electric Power Research Institute, 2008
0 .0
2 .0
4 .0
6 .0
8 .0
1 0 .0
1 2 .0
1 4 .0
1 6 .0
1 2 3 4 5 6 7 8 9 1 0 1 1 1 2
mg/
DSC
M
1 5 0 p p m S O 2
~ 1 5 % H 2 02 1 3 - 2 1 6 OF
5 0 0 p p m S O 2
~ 1 5 % H 2 02 4 8 - 2 8 6 O F
A v e B la n k
5 0 0 p p m S O 2
~ 1 0 % H 2 0
3 0 0 - 3 4 0 O F
2 5 p p m S O 2
~ 1 5 % H 202 0 5 - 2 1 5 O F
M - 2 0 2 D r y Im p in g e r
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OTM OTM -- 28 vs. M202 28 vs. M202 (Titration for Acid Artifact)(Titration for Acid Artifact)Source: Electric Power Research Institute, 2008Source: Electric Power Research Institute, 2008
0 .0
5 .0
1 0 .0
1 5 .0
2 0 .0
2 5 .0
1 2 3 4 5 6 7 8 9 1 0 1 1 1 2R u n N u m b e r
mg/
dscm
Sul
fate
~ 1 5 % H O2 5 p p m S O 2
2 0 5 - 2 1 5 F O
~ 1 0 % H O5 0 0 p p m S O 2
3 0 0 - 3 4 0 FO
~ 1 5 % H O1 5 0 p p m S O 2
2 1 3 - 2 1 6 F
~ 1 5 % H O5 0 0 p p m S O 2
2 4 8 - 2 8 6 FO
M -2 0 2 O T M 2 8
O
2
2 2
2
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OTM OTM –– 28 Method Performance28 Method Performance
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OTM OTM –– 28 Method Performance28 Method Performance(EPA Laboratory Replicate Study)(EPA Laboratory Replicate Study)
Run Organic (mg/dscm)
Inorganic (mg/dscm)
Filter (mg/dscm)
Total(mg/dscm)
1 0.12 2.36 -0.36 2.342 0.16 2.99 -0.06 3.033 0.09 1.44 0.00 1.464 0.31 1.98 0.00 2.225 0.17 1.65 0.07 1.776 0.39 2.58 -0.20 2.527 0.08 1.24 0.31 1.568 0.02 1.94 0.18 2.06Blank -0.02 mg 0.21 mg 0.00 mg 0.68 mgAverage 0.17 2.02 -0.01 2.18Std Dev 0.12 0.59 0.21 0.53MDL 0.37 1.78 0.63 1.60
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OTM OTM –– 28 Method Performance28 Method PerformanceAmmonia and Sulfur DioxideAmmonia and Sulfur Dioxide
(EPA Laboratory Replicate Study)(EPA Laboratory Replicate Study)
Phase I Test Run
Method 5 filter
(160 °C) (μg)
Low-temp filter
(71 °C) (μg)
Aqueous (μg)
Organic (μg)
Ambient filter
(30 °C) (mg) Total (μg)
NH3 16 ND ND ND NA ND** ND 17 ND ND ND NA ND** ND 18 ND ND ND NA ND** ND
Train Blank 1 ND NA ND NA NR ND Train Blank 2 ND NA ND NA NR ND Train Blank 3 ND NA ND NA NR ND Reagent Blank NA NA ND NA NR ND
SO4 16 180 160 ND NA ND* 340 17 146 201 ND NA ND* 347 18 181 156 ND NA ND* 337
Train Blank 1 147 142 ND NA NR 289 Train Blank 2 147 102 ND NA NR 249 Train Blank 3 150 NA ND NA NR 150*
Reagent Blank NA NA ND NA NR ND ND = Not detectable above 27.6 total micrograms ND** = Not detected in gravimetric analysis of filter NR = Not run
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OTM OTM -- 28 vs. Controlled Condensate28 vs. Controlled CondensateSOSO44 RecoveryRecovery
Source: Electric Power Research Institute, 2008Source: Electric Power Research Institute, 2008
0 .0
5 .0
10 .0
15 .0
20 .0
25 .0
30 .0
35 .0
40 .0
45 .0
31 32 33 19 2 0 21 34 35 36 22 23 24
mg/
dscm
150 ppm S O 2
0 ppm S O 2 150 ppm S O 2
0 ppm S O4
6 .9 m g /dscm S O 3 S p ike
34 .4 m g/dscm S O 3 S p ike
C on tro lled C ondensa te S OO T M -28 S O by ICO T M -28 C P M res idue w e igh t
24
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Dry Impinger Method RecapDry Impinger Method Recap
No OptionsMinor glassware changesNo water at start of testShort stem impinger insert replaced with tipped insert for purgingDegassed Type III water added if neededBoth organic & inorganic evaporations at room temperatureSignificant reduction of sulfate artifact
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Schedule UpdateSchedule Update
FR Proposal – April 2009Comment Period Close – June 2009FR Promulgation – December 2009
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QUESTIONSQUESTIONS