run 7 · 2020-03-04 · stack axis #1 (meters)= 1.829 stack axis #2 (meters)= 1.829 circular stack...

REPORT

Test Report for Risk Burn No. 2on the Drake Chemical Superfund Site's

Mobile On-site Hazardous Waste Incinerator

Volume 3—Appendices D through O

For OHM Remediation Services Corp.180 Myrtle Street

Lock Haven, PA 17745

Attn: Mr. Gary JonesTechnical Manager

OHM Subcontract No. 292521-02

MRI Project No. 3620-28

September 4,1997

MIDWEST RESEARCH INSTITUTE 425 Voiker Boulevard, Kansas City, MO 64110 2299 • (816) 753-7600A R 3 l 5 0 b b

Appendices

A List of Samples CollectedB Field Sampling DataC Process DataD Modified Method 5 Particulate Data and Modified Method 5 Calculation DataE Calibration Data for Sampling EquipmentF Report on Chemical Analysis Results for Semivolatile OrganicsG Report on Chemical Analysis Results for PCDD/PCDFH Report on Chemical Analysis Results for HerbicidesI Report on Chemical Analysis Results for VOCsJ Report on Chemical Analysis Results for MetalsK Report on Chemical Analysis Results for Hexavalent ChromiumL Report on Chemical Analysis Results from PCBsM Report on Chemical Analysis Results for ChloridesN Continuous Emission Monitoring Data for SO2O Example Calculations

MRI-Apphed'TUMCKS.APP .

AR315056

Appendix D

Modified Method 5 Particulate Dataand

Modified Method 5 Calculation Data forRun 5Run 6Run 7

MRI-AppKed/R362028.APP

A R 3 1 5 Q 5 7

Modified Method 5 Participate Data

MRI-AppfiedyR362028.APP

AR3I5Q58APPENDIX D

FILE NAME - 28PH5 PROG..=VER 02/17/97RUN # - 5 - Method 0050 Train for PM, HC1, and Chlorine

02-25-1997 12:49:39OCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelATE - 02/07/97 Time: 1150:30-1326:30/1420:30-1501:15/1504:15-1559:30PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 791.164Final Meter Volume (Cubic Feet)= 900.331Meter Factor= .. --, - - - 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 107.966Gas Volume (Dry Standard Cubic'Feet)= 104.848

Barometric Pressure (in Hg)= 29.60Static Pressure (Inches H20)= -0.41

Percent Oxygen== ' • . 1 1 . 1Percent Carbon Dioxide= - 1 0 . 2Moisture Collected (ml)= 2924.4Percent Water= -.- - 56.8

Average Meter Temperature (F)= . 79Average Delta H (in H20)= ' > 1.10Average Delta P (in H20)= - 0.259 . . "Average Stack Temperature (F)= 185

Dry Molecular Weight= -30.08et Molecular Weight= • - 23.22 - ~-

Average Square Root of Delta P (inlH20)= 0.5081% Isokinetic= 98.4

Pitot. Coef f icient= . . • - . 0 . 8 4Sampling Time (Minutes)= 192.0Nozzle Diameter (Inches)= 0.371Stack Axis #1 (Inches)= 72.0Stack Axis #2 (Inches)= 72.0Circular StackStack Area (Square Feet)= 28.27

Stack Velocity (Actual, Feet/min)= 2,114Flow Rate (Actual, Cubic ft/min)= 59,773Flow rate (Standard, Wet, Cubic ft/min)= 48,367Flow Rate (Standard, Dry, Cubic ft/min)= 20,905

Particulate Loading - Front Half -

Particulate Weight (g)= 0.0080 Corr. to 7% O2 equivalentParticulate Loading, Dry Std. (gr/scf) = 0.0012 O'.OOIOParticulate Loading, Actual (gr/cu ft)= 0.0004Emission Rate (lb/hr)= 0.21

No Back Half Analysis .

AR3I5059APPENDXX D

* * METRIC UNITS * *FILE NAME - 28PH5 ' PROG.=VER 02/17/97RUN # - 5 - Method 0050 Train for PM, HCl, and Chlorine

02-25-1997 12:49:41LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/07/97 Time:.1150:30-1326:30/1420:30-1501:15/1504:15-1559:30PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Meters)= 22.403Final Meter Volume (Cubic Meters)= 25.494Meter Factor= 0.989Multiple leak checks, see end 6f printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 3.057Gas Volume (Dry Standard Cubic Meters)= 2.969

Barometric Pressure (mm Hg)= 752Static Pressure (mm H20)= -10

Percent Oxygen= , _ 11.1Percent Carbon Dioxide= • - 10.2Moisture Collected (ml)= 2924.4Percent Water= 56.8

Average Meter Temperature (C)= 26Average Delta H (mm H20)= 28.0Average Delta P (mm H20)= . - 6.6Average Stack Temperature (C)= 85

Dry Molecular Weight= * 30.08Wet Molecular Weight= 23.22

Average Square Root of Delta P (mm H20)= 2.5609% Isokinetic= 98.4

Pitot Coefficient= 0.84Sampling Time (Minutes)= 192.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627

Stack Velocity (Actual, m/min)= 644Flow rate (Actual, Cubic m/min)= 1,693Flow rate (Standard, Wet, Cubic m/min)= 1,370Flow rate (Standard, Dry, Cubic m/min)= 592

Particulate Loading - Front Half

Particulate Weight (g)= P. 0080 Corr. to 7% 02 equivalentParticulate Loading, Dry Std. (mg/cu m)= 2.7 2.2Particulate Loading, Actual (mg/cu m)= 0.9Emission Rate (kg/hr)= 0.10

No Back Half Analysis ,

AR3I5060APPENDIX D

FILE NAME - 28PH5 . PROG.=VER 02/17/97RUN # - 5 - Method 0050 Train for PM, HC1, and Chlorine

02-25-1997 12:49:44LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/07/97 Time: 1150:30-1326:30/1420:30-1501:15/1504:15-1559:30PROJECT # - - - ' -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA .

Point # - Delta P Delta H . Stack T Meter T(in. H20) (in. H20) (F) In(F) Out(F)

1 0.290 1.20 185 68 ' 672 0.310 1.30 185 68 663 0.310 1.20 • 186 72 684 0.270 1.10 186 75 695 0.250 1.00 185 77 706 0.240. 0.95 186 80 727 • 0.250 1.10. 185 82 738 0.270 1.20 185 84 759 0.280' 1.20 185 85 7610 0.280 1.30 - 184 " 86 7711 • 0.280 1.30 " . 184 87 7812 0.220 0.98 184 88 7913 0.220 1.00 183 77 76.14 0.240 1.10 184 77 ' 7615 -0.260 1.20 .184 82 7616 0.250 1.10 184 84 7717 0.240 1.00 185 85 781 8 0.240 1.00 1 8 5 8 6 7 9 . . .19 0.230 0.97 185 86 7920 0.240 1.00 185 87 . 80 -21 0.250 ,1.00 186 88 . -8122 0.260 1.10 185' 90 8223 0.270 1.10 186 92 8224 0.260 1.10 185 91 ' 86

Fraction Final Wt. Tare Wt. Blank Wt. Net Wt.(g) (g) ' (g) (g)

DRY CATCH 0.0000 0.0000 O.OQOO 0.0000FILTER 1.0308 1.0253 0.0000 0.0055

Fraction Final Wt. Tare Wt. Vol. Net Wt.(g) (g) (ml) • (g)

PROBE RINSE , 67.'0398 67.0373 219.6 0.0025IMPINGERS 0.0000 0.0000 0.0 0.0000Probe Rinse Blank (mg/ml)= 0.0000Impinger Blank (mg/ml)= 0.0000Multiple leak checks used. Final readings for each segment are listed belowLk Rate (cftn) Time (min)

0.0020 96.0000 ' "0.0050 96.0000 .

AR3I5061APPENDIX D

FILE NAME - 28PHS PROG.=VER 02/17/97RUN # - 6 - Method 0050 Train for PM, HCl, and Chlorine

02-25-1997 12:51:30LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/08/97 Time: 1100:30-1242:30/1330:30-1512:30PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 901.033Final Meter Volume (Cubic Feet)= 1018.095Meter Factor= - 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 115.774Gas Volume (Dry Standard Cubic'Feet)= 112.870

Barometric Pressure (in Hg)= 29.62Static Pressure (Inches H20) = • -0.41

Percent Oxygen= 11.0Percent Carbon Dioxide= ' 10.5Moisture Collected (ml)= ' 3149.2Percent Water= - 56.8

Average Meter Temperature (F) = 77Average Delta H (in H20)= 1.12Average Delta P (in H20)= 0.264Average Stack Temperature (F)= 185

Dry Molecular Weight= 30.12Wet Molecular Weight= 23.24

Average Square Root of Delta P (in H20)= 0.5128% Isokinetic= 98.8

Pitot Coefficient= 0.84Sampling Time (Minutes)= 204.0Nozzle Diameter (Inches)= 0.371Stack Axis #1 (Inches)= 72.0Stack Axis #2 (Inches)^ 72.0Circular StackStack Area (Square Feet)= 28.27

Stack Velocity (Actual, Feet/min)= '2,131Flow Rate (Actual, Cubic ft/min)= 60,267Flow rate (Standard, Wet, Cubic ft/min)= 48,815Flow Rate (Standard, Dry, Cubic ft/min)= 21,094


Particulate Weight (g)= 0.0075 Corr. to 7% 02 equivalentParticulate Loading, Dry Std. (gr/scf)= 0.0010 0.0008Particulate Loading, Actual (gr/cu ft)= 0.0004Emission Rate (lb/hr)= 0.18

No Back Half Analysis

AR315062APPENDIX D

* * METRIC UNITS * *FILE NAME - 28PH6 PROG.=VER 02/17/97RUN # - 6 - Method 0050 Train for PM, HC1, and Chlorine

02-25-1997 12:51:33LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/08/97 Time: 1100:30-1242:30/1330:30-1512:30PROJECT # - .3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Meters)= 25.514 'Final Meter Volume (Cubic Meters)= 28.828Meter Factor= 0,989 'Multiple leak checks, see end 6f printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 3.278.Gas Volume (Dry Standard Cubic Meters)= 3.196

Barometric Pressure (mm Hg)= . 752Static Pressure (mm H20)= -10

Percent Oxygen= 11.0Percent Carbon Dioxide= '10.5Moisture Collected (ml)= 3149.2 .Percent Water= • 56.8 • •

Average Meter Temperature (C) = 25Average Delta H (mm H20)= 28.6Average Delta P .(mm H20)= ' 6.7Average Stack Temperature (C)= .85

Dry Molecular Weight= 30.12Wet Molecular Weight= 23.24 - -

Average Square- Root of Delta P (mm H20)= 2.5844% Isokinetic= 98.8

Pitot Coefficient= .- 0.84Sampling Time '(Minutes) = 204.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627

Stack Velocity (Actual, m/min)= _ 650Flow rate (Actual, Cubic m/min)= 1,707Flow rate (Standard, Wet, Cubic m/min)= 1,382Flow rate (Standard, Dry, Cubic m/min)= 597


Particulate Weight (g)= 0.0075 Corr. to 7% O2 equivalentParticulate Loading, Dry Std. (mg/cu m)= 2.3 1.9Particulate Loading, Actual (mg/cu m)= 0.8Emission Rate (kg/hr) = -. 0.08


AR315063APPENDIX D

FILE NAME - 28PH6 PROG.=VER 02/17/97RUN # - 6 - Method 0050 Train for PM, HC1, and Chlorine


Point # Delta P Delta H Stack T Meter T(in. H20) (in. H20) (F) . In(F) Out(F)

1 0.280 1.20 184 66 652 0.310 1.30 184 66 653 0.300 1.30 • 184 70 664 0.280 1.20 185 75 685 0.250 1.00 185 78 696 0.230 1.00 184 79 707 0.260 1.10 185 80 728 0.290 1.20 185 82 739 0.310 1.30 185 83 7510 0.310 1.40 184 85 7611 0.290 1.20 185 86 7712 0.260 1.10 185 86 7813 0.200. 0.89 184 75 7414 0.240 1.10 184 75 7415 0.260 1.10 185 79 7416 0.260 1.20 184 82 7517 0.270 1.10 185 84 7618 0.260 1.00 185 85 7719 0.250 1.10 185 86 7820 0.240 1.00 185 86 7821 0.250 1.10 185 87 7922 0.270 1.10 185 87 7923 0.250 1.10 185 88 8024 0.210 0.89 185 88 81

Fraction Final Wt. Tare Wt. Blank Wt. Net Wt.(g) (g) (g) (g)

DRY CATCH 0.0000 0.0000 0.0000 0.0000FILTER 1.0458 1.0402 0.0000 0.0056

Fraction Final Wt. Tare Wt. Vol. Net Wt.(g) (g) (ml) • (g)

PROBE RINSE 60.1114 60.1095 191.0 0.0019IMPINGERS 0.0000 0.0000 0.0 0.0000Probe Rinse Blank (mg/ml)= 0.0000Impinger Blank (mg/ml)= 0.0000

Multiple leak checks used. Final readings for each segment are listed below

Lk Rate (cfm) Time (min)0.0100 102.00000.0020 102.0000 ' ,

AR3I5064APPENDIX D

FILE NAME - 28PH7 PROG.=VER 02/17/97RUN # - 7 - Method 0050 Train for PM, HC1, and Chlorine

02-25-1997 12:53:42LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/09/97 Time: 1045:30-1227:30/1255:30-1437:30PROJECT # -3G20.28.30 OHM Remediation Services Corp., Drake Chemical Superfund site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 20.553Final Meter Volume (Cubic Feet)= 136.091Meter Factor= '0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= , 114.267Gas Volume (Dry Standard Cubic'Feet)= 111.621

Barometric Pressure (in Hg)= '29.65Static Pressure (Inches H20)= -0.41

Percent Oxygen= ' 11.3Percent Carbon Dioxide= 10.4Moisture Collected (ml)= 3081.6Percent Water= ' - 56.5

Average Meter Temperature (F)= 77Average Delta H (in H20) = . 1.11Average Delta P (in H20)= 0.255Average Stack Temperature (F)= 185

Dry Molecular Weight= 30.12 •Wet Molecular Weight= 23.27

Average Square Root of Delta P (in H20)= 0.5044. .% Isokinetic= . - • - - • - - 98.7

Pitot Coefficient= 0.84Sampling Time (Minutes)= 204.0Nozzle Diameter (Inches)= 0.371Stack Axis #1 (Inches) = 72.0Stack Axis #2 (Inches)= 72.0Circular StackStack Area (Square Feet).= 28.27

Stack Velocity (Actual, Feet/min)= 2,094Flow Rate (Actual, Cubic ft/min)= 59,205Flow rate (Standard, Wet, Cubic ft/min)= 48,010Flow Rate (Standard, Dry, Cubic"ft/min)= 20,871


Particulate Weight (g)= 0.0066 Corr. to 7% O2 equivalentParticulate Loading, Dry Std. (gr/scf) = 0.000,9 , O.OQ07Particulate Loading, Actual (gr/cu ft)= 0.0003Emission Rate (lb/hr)= 0.16


AR3I5065APPENDIX D

* * METRIC UNITS * *FILE NAME - 28PH7 PROG.=VER 02/17/97RUN # - 7 - Method 0050 Train for' PM, HCl, and Chlorine


Initial Meter Volume (Cubic Meters)= 0.582Final Meter Volume (Cubic Meters)= 3.854Meter Factor= • 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 3.236Gas Volume (Dry Standard Cubic Meters)= 3.161


Percent Oxygen= 11.3Percent Carbon Dioxide= 10.4Moisture Collected (ml)= 3081.6Percent Water= 56.5

Average Meter Temperature (C)= 25Average Delta H (mm H20)= 28.1Average Delta P (mm H20)= 6.5Average Stack Temperature (C)= 85



Pitot Coefficient^ 0.84Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= - 9.42Stack Axis #1 (Meters)= • 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627



Particulate Weight (g)= 0.0066 Corr. to 7% O2 equivalentParticulate Loading, Dry Std. (mg/cu m)= 2.1 1.7Particulate Loading, Actual (mg/cu m)= 0.7Emission Rate (kg/hr)= 0.07


flR315066APPENDIX D 9

FILE NAME - 28PH7 PROG.=VER 02/17/97.UN # - 7 - Method 0050 Train for PM, HCl, and Chlorine

02-25-1997 12:53:47OCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/09/97 Time: 1045:30-1227:30/1255:30-1437:30PROJECT # - - . ..3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Point # Delta P Delta H Stack T Meter T - -(in. H20) (in. H20) (F) In(F) Out(F)

1 0.270 1.20 184 65 . 652 0.310 1.30 . 184 65 643 0.300 1.30 184 69 644 0.270 1.20 184 74 675 '• 0.240 1.10 184 76 686 0.230 0.96 185 78 697 0.250 1.10 185 79 718 0.260 1.20 184 80 729 0.280 1.20 184 82 7310 0.290 1.20 185 83 74 .11 0.280 . 1..30 184 84 7512 . 0.270 1.10 185 85 7613 0.220 1.00 184 76 7514 0:240 1.10 ,184 77 .7415 0.260 1.10 185 80 7516 0.270 1.10 186 83 7517 0.250 1.10 184 84 7618 0.250 1.10 185 85 7719 0.230 1.00 185 86 7820 0.230 1.00 185 86 7821 0.240 1.00 185 86 ' 7922 0.230 1.00 185 87 7923 0.240 1.00 185 88 8024 . 0.210 0.89 185 89 80

Fraction Final Wt. Tare Wt. Blank Wt. Net Wt.(g) ,(g) (g) (g) .

DRY CATCH 0.0000 0.0000 0.0000 0.0000FILTER 1.0981* 1.0932 0.0003 0.0046

Fraction Final Wt. Tare Wt. Vol. Net Wt.(g) (g) (ml) (g)

PROBE RINSE 68.8647 68.8627 191.6 0.0020'IMPINGERS 0.0000 0.0000 0.0 0.0000Probe Rinse Blank (mg/ml)= 0.0000Impinger Blank (mg/ml)= 0.0000


Lk Rate (cfm) Time (min),0.0010 102.00000.0030 102.0000

•RR315067APPENDIX D 1O

PARTICULATE MATTER (FRONT-HALF TRAIN) RINSES ANALYSIS DATA

MRI Project No. 3620.28.30Client/Source: OHM Remediation Services Corp., Drake Chemical Superfund Site

Source Location: Lock Haven, PennsylvaniaSampling Location: Mobile Hazardous Waste Incinerator Stack

Sampling Team Leader: Jim Surman Analyst: U . /rt<- C~\. ^ _____Beaker Size and Type: 1 50-mL borosilicate glass

Acetone Lot No. g/n-7 3 Water Lot No. /?-'£?- 96Sample Treatment: Acetone and water samples evaporated at ambient temperature and pressure in an

enclosure with HEPA-filtered air; then, desiccated and weighed to a constant weight.Weight Unit: grams

Run No. C? _____ Beaker No. • "~7 ____ Sample No. 3>3.3_Sample Volume 4- Acetone Rinses of Bottle Beaker + Sample Residue Weights

start end Gross Wt. Date TimeBeaker + Sample + Rinses Wt. aoo,~1 313..? £?.djf? J.-/d. -71

Beaker Tare Wt. 67.o /Y7.'t 67.O337 2-/7-T7A. - - - - - - - - - - - - - Sample + Rinses Wt.B. - - - - - - Water Wt. from Recovery Data:C. - - - - - - - - - - - - - - Acetone Wt. (A - B):D. - - - - Acetone Wt./0.79 = mLs Acetone:

Beaker + Residue Gross Weight used for data entry: d>~t.05et'XBeaker Tare Weight from Tare Weight Data: (,7.o

Combined Blank = ((Water Blank x B) + (Acetone Blank x D))/(B + D) = — G — mg/mLVolume !B + D) for data entry = &/9,t? mLs

Comments:

Run No. Cz> _____ Beaker No. y Sample No.Sample Volume + Acetone Rinses of Bottle Beaker + Sample Residue Weights

start end Gross Wt. Date TimeBeaker + Sample + Rinses Wt. o;5.o' /'??. ? fea.it/S j-/(> -VI /7/»~

Beaker Tare Wt. &o.f tf?.9 (^a • tt/V .Z-/7-97 JGQ.A. - - - - - - - - - - - - - Sample + Rinses Wt.B. - - - - - - Water Wt. from Recovery Data:C. - - - - - - - - - - - - - - Acetone Wt. (A - B):D. - - - - Acetone Wt./0.79 = mLs Acetone:

Beaker + Residue Gross Weight used for data entry: GO.Beaker Tare Weight from Tare Weight Data: /*

I/

Combined Blank = ((Water Blank x B) + (Acetone Blank x D))/(B + D) = — o — mg/mLVolume (B + D) for data entry = S9S.0 mLs

Comments:

Run No. 7____ Beaker No. /5" Sample No. 7.3Sample Volume -+ Acetone Rinses of Bottle Beaker + Sample Residue Weights

start end Gross Wt. Date TimeBeaker + Sample + Rinses Wt. I1??, 3 /76".Z ^f.y£V7 _?-/&-f7 J7"Q

Beaker Tare Wt. 6?,f /?<...! (.f.?M7 3.-/7'?7 _./oe*A. - - - - - - - - - - - - - Sample + Rinses Wt.B. - - - - - - Water Wt. from Recovery Data:C. - - - - - - - - - - - - - - Acetone Wt. (A - B):D. - - - - Acetone Wt./0.79 = mLs Acetone:

Beaker + Residue Gross Weight used for data entry:Beaker Tare Weight from Tare Weight Data:

Combined Blank = {(Water Blank x B) + (Acetone Blank x D))/(B + D) = — O~ mg/mLVolume (B + D) for data entry = y 4£ mLs

Comments:

NOTE: Control beaker weights, reagent blank weights, and balance check data are on other forms.

PMRINSEX.WPO Ap<il 29. 1996 (rev. PMRINSE3.WPD February 17, 1997)

&R315068APPENDIX D M i» v • ~ ~ .,.,

PARTICULATE MATTER ON FILTER ANALYSIS DATA


.Source Location: Lock Haven, PennsylvaniaSampling Location: Mobile Hazardous Waste Incinerator Stack

Sampling Team Leader: Jim Surman Analyst: <J- /IfIt-Filter Size and Type: 4.9-inch diameter, Whatman QM-A quartz filter

Filter Lot No.Filter Treatment: Heated at 105 °C for 3 hours, desiccated, and weighed to a constant weight.

Weight Unit: grams-y -

Run No. ,j5T _____ Filter No. / 7 Sample No. jS"3

Gross Wt. Date Time Comments:

2-/z -y? //'cu

Filter Gross Weight used for data entry:Filter Tare Weight from Tare Weight Data:

Run No. __£____ Filter No. y6? Sample No. £3.2.3


Filter Gross Weight used for data entry: / .Filter Tare Weight from Tare Weight Data:

Run No. ~~f_ _____ Filter No. <JXO Sample No. ~13


/, g 4 r i

Filter Gross Weight used for data entry: /'Filter Tare Weight from Tare Weight Data: J

NOTE: Control and blank filter weight data and balance check data are on other forms.

PMFILTEX,WPD June 11. 1996 (rev. PMFIUTE3.WPD February 17, 19971

AR315069APPENDIX D 12

PARTICULATE MATTER (FRONT-HALF TRAIN) REAGENT BLANK ANALYSIS DATA



Sampling Team Leader: Jim Surman Analyst: J • /'(<. C—^-.n^_____________Beaker Size and Type: 150-mL borosilicate glass

Acetone Lot No. j&/W7tf3 Water Lot No. SJ~SZ-?6Sample Treatment: Acetone and water samples evaporated at ambient temperature and pressure in an

enclosure with HEPA-filtered air; then, desiccated and weighed to a constant weight.Filter Size and Type: 4.9-inch diameter, Whatman QM-A quartz filter

Filter Lot No. X63V&Filter Treatment: Heated at 105 °C for 3 hours, desiccated, and weighed to a constant weight.

Weight Unit: grams

Acetone Blank Determination: For Run No.(s) -JT-7___ Beaker No. ^___ Sample No. . x3«-2Acetone Reagent Blank Sample Volume Beaker + Sample Residue Weights

Gross Wt. Date TimeBeaker + Acetone Sample Wt. /tt.3 76. 1V/Y_ j-/l>~?7 /?.•<...•

Beaker Tare Wt. lL. 1 7i..3<//y j-n-tl yd-t.'0Acetone Sample Wt. 77-5 71- Ml? z-n -/7 /*•<,

A. - - - - Acetone Wt./0.79 = mLs Acetone: /• _______ _______ _______

Beaker + Residue Gross Weight used for blank determination: 71- 3VBeaker Tare Weight from Tare Weight Data: 7 6 .

B. - - - - - - - - - - - - - - - - - - - - - - - - - - - — Net Weight of Residue in beaker: — Q. PQJ 0Acetone Blank (B x 1000/A) for data entry or for computing Combined Blank: — O — ' mg/mLComments:

Water Blank Determination: For Run No.(s) <J"-7 Beaker No. / v' Sample No. 5~3 3 /Water Reagent Blank Sample Volume Beaker .+ Sample Residue Weights

Gross Wt. Date TimeBeaker + Water Sample Wt. /£5". *?

Beaker Tare Wt. 6il ~ 6r~l. 0<-Jf 2-/7-J7Water Sample Wt. <? / . .2 6> 7. U YS" -?-/f-f7 /o -

A. - - - - - - - - - - - Water Wt. = mLs Water:

Beaker + Residue Gross Weight used for blank determination: d>l ' .Beaker Tare Weight from Tare Weight Data: 67. 6

B. . - - - - - , - - - - - - - - - - - - - - - - - - - - - Net Weight of Residue in beaker: —Water Blank (B x 1000/A) for data entry or for computing Combined Blank: — 0- — mg/mL

Comments:

tfGross Wt. Date Time Comments:

Filter Blank Determination: For Run No. (s) /"%(:•/ 7 / Filter No. 3*f Sample No. 33 Q

A. - - - - - - - - - - - - - - - - - Filter Gross Weight used for blank determination:B. - - - - - - - - - - - - - - - - - - - - - - Filter Tare Weight from Tare Weight Data:

Net Filter Weight Difference (A - B) for data entry: 0,[retain minus sign if value is negative]

NOTE: Control beaker weights, control filter weights, and balance check data are on another form.PMBLANKX.WPD April 29. 1996 (rev. PMBLANK3.WPO February 17, 1997)

RR315070APPENDIX D 13

PARTICIPATE MATTER (FRONT-HALF TRAIN) CONTROLS ANALYSIS DATA



Sampling Team Leader: Jim Surman Analyst: v ' /fit. C - . _____Balance: Mettler AE200, MRI #10586

Weight Unit: grams

Control Filter Weights & Balance Checks:

Filter No. 3. .NIST Weight(s): Filter No. 32— NIST Weight(s):Original Tare Wt.: /, £>f7

Current Wt. Date

/, OFSV .2- /?-?7/.OS15T J-/Y-77

'"3 Oriqinal Tare Wt.: S>t>?6>l>1 I ' ^Time Balanca/Reading Current Wt. Date Time Balance/Reading

/73c I.OOC( t.c75~/ J-M-ri /7Jo / ^<J //.Of-T1? ,?-/fr-77 Jjoo I.OO&O / . o T 'Y JZ-SL-f?' ,22oe /, tlOOO

Comments: — 0. , .- _ . • ~ - l -ro-* Jo*" rJefS-re*" J<r*, -Ve iy. Ptx/frsMt,, •Thi'i

Control Beaker Weights & Balance Checks:

Beaker No. 73 NIST Weight(s): Beaker No. <3£i NIST Weight(s):Original Tare Wt.: {fte,#&/k Original Tare Wt.: & ~7.

Current Wt. Date Time Balance/Reading Current Wt. Date Time Balance Reading

U.~tf -77

Comments: —o.fcoC. —o.c>ec3

Controls are filters and beakers selected from the original prepared lots that are used for sampling and analysis. They areprocessed along with the filters and beakers containing samples during analysis, i.e., they are heated, desiccated, and weighedalong with the filters and beakers containing samples. The results are not used for correcting analytical data, but are useful inmonitoring changes between original tare weights and weights obtained during analysis of samples. Significant changes couldindicate problems in maintaining relatively constant environmental conditions in the laboratory, processing procedures notreplicating those used when tare weights were obtained, instrumentation calibration drift, and desiccant deterioration.

Each time filters or beakers are weighed, the balance is checked for accuracy by weighing NIST certified weights approximatingthe weights of the filters or beakers.

PMCONTRX.WPO April 29. 1996 (rev. PMCONTR3.WPD February 17. 1997)

aR3!507lAPPENDIX D 14

BEAKER TARE WEIGHT DATA

MRI Project No. 3620.28.30

Sampling Team Leader: Jim Surman Analyst: \J- JvLc <—<^»v—_________Beaker Size and Type: 1 50-mL borosilicate glass

Beaker Treatment: Following cleaning according to the test protocol, heat at 105 °C for 3 hours, desiccate,and weigh to a constant weight.

Weight Unit: gramsDate: .3-A2- 77 -2-^3 -?7

Time Started: ; yet)________ •? ' /^______ _____________

Balance Check before beakers are weighed:Balance Used: Mettler AE200, MRI #10586Weight Value: 50 and 20 grams 50 and 20 grams 50 and 20 gramsBalance Reads: ~7O. 6GQZL ~7$.. O

Average Weightor Weight to be

Beaker I.D. No. First Weighing Second Weighing Third Weighing Used as the Tare

7_______ 6,7. 03 73

LL. ll? -&L 22.P4

3C, ______ LI.

Balance Check after beakers are weighed:Balance'Reads: 76.Q606

COMMENTS:

BEAKRTAX.WPD September 25. 1996 (rev. BEAKRTA3.WPO February 17. 1997)

67. 0.3 TV?

£7. C45 ___________ 67.L?. v-d.z7 Cr. 9^2-7 _______ c>y. 43.7

.AR3I5072APPENDIX D 15

FILTER TARE WEIGHT DATA

MRI Project No. 3620.13.30 and 3620.18.30Sampling Team Leader: Jim Surman Analyst: J.//L (C __ , ______. Filter Size and Type: 4.9-inch diameter Whatman QM-A quartz filter

Filter Lot No. &>-£*J 03

Filter Treatment: Heat at 105 °C for 3 hours, desiccate, and weigh to a constant weight.Weight Unit: grams •Date; / -3-fd" A2~V-f6 __________

Time Started: /f~:$7) ______ I(',-H( ___________Balance Check before filters are weighed:

Balance Used: Mettler AE200, MRI #10586

Weight Value: 1 gram . 1 gram 1 gram

Balance Reads: /, O a & / / . aaoo _____ _______________Average Weightor Weight to be

Filter I.D. No. First Weighing Second Weighing Third Weighing Used as the Tare

i. & 7 y a.

_7

/.Q3S3

n

Balance Check after filters are weighed:Balance Reads: /. OQQ I______ /, OOP ICOMMENTS:

FILTRTAX.WPO 11/1S/95 lfev.PILTRTA3.WPO Januuy J*. 19961

,3 . '/.a 307 ____/. o 3 0? _____________ /'0307_2___ /.oaTt /. 03.7-vS~_____ /. O3-5~O ' • t.Q.

/, 03 /3

I. of 03.. /.tiyo3 ___________ I - ri-V° -2-________ /.63f (

flR3i5073APPENDXX D

____Run 5

Modified Method 5 Calculation Data

MRI.AppHed/R362028.APP

.AR3l5Q7t*APPENDIX D 17

FILE NAME - 28PH5 PROG.=VER 02/17/97RUN # - 5 - Method 0050 Train for PM, HCl, and Chlorine

02-25-1997 12:49:39LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelATE - 02/07/97 Time: 1150:30-1326:30/1420:30-1501:15/1504:15-1559:30ROJECT # - - - - -3,620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA . *

Initial Meter Volume (Cubic Feet)= 791.164Final Meter Volume (Cubic Feet)= 900.331Meter Factor= : 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 107.966Gas Volume (Dry Standard Cubic*Feet)= 104.848

Barometric Pressure (in Hg)= • 29.60Static Pressure (Inches H20) = -0.41

Percent Oxygen= ll.lPercent Carbon Dioxide= 1-0.2Moisture Collected (ml)= '2924.4Percent Water= - 56.8

Average Meter Temperature (F)= 79Average Delta H (in H20)= 1.10Average Delta P (in H20)= . 0.259Average Stack Temperature (F)= 185

Dry Molecular Weight= - 30.08'et Molecular Weight= . 23.22

Average Square Root of Delta P (in H20)=- 0.5081% Isokinetic= 98.4 . .

Pitot Coefficient= _ 0.84Sampling Time (Minutes)= 192.0Nozzle Diameter (Inches)= '0.371Stack Axis #1•(Inches)= 72.0Stack Axis #2 (Inches)=. 72.0Circular Stack ' .Stack Area (Square Feet)= 28.27 ,

Stack Velocity (Actual, Feet/min)= . 2,114Flow Rate (Actual, Cubic ft/min)= 59,773Flow rate (Standard, Wet, Cubic ft/min)= 48,367 . 'Flow Rate (Standard, Dry, Cubic ft/min)= 20,905


Particulate Weight (g)= 0.0080 Corr. to 7% O2 equivalentParticulate Loading, Dry Std. (gr/scf)= 0.0012 0.0010Particulate Loading, Actual (gr/cu ft)= 0.0004Emission Rate (lb/hr)= 0.21


AR3I5075APPENDIX D


02-25-1997 12:49:41LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/07/97 Time: 1150:30-1326:30/1420:30-1501:15/1504:15-1559:30PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Meters)= 22.403Final Meter Volume (Cubic Meters)= 25.494Meter Factor= 0.989Multiple leak checks, see end 6f printout Leak Correction 0.0000Net Meter Volume (Cubic Meters)= 3.057Gas Volume (Dry Standard Cubic Meters)= 2.969


Percent Oxygen= 11.1Percent Carbon Dioxide= 10.2 .Moisture Collected (ml)= 2924.4Percent Water= 56.8

Average Meter Temperature (C) = 26Average Delta H (mm H20)= 28.0Average Delta P (mm H20)= 6.6Average Stack Temperature (C) = 85

Dry Molecular Weight= ' 30.08Wet Molecular Weight= 23.22

Average Square Root of .Delta P (mm H20)= 2.5609% Isokinetic= 98'. 4

Pitot Coefficient= 0.84 'Sampling Time (Minutes)= 192.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= • 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627

Stack Velocity (Actual, m/min)= 644Flow rate (Actual, Cubic m/min)= 1,693Flow rate (Standard, Wet, Cubic m/min)= . 1,370Flow rate (Standard, Dry, Cubic m/min)= 592


Particulate Weight (g)= 0.0080 Corr. to 7% 02 equivalentParticulate Loading, Dry Std. (mg/cu m)= ' 2 . 7 2.2Particulate Loading, Actual (mg/cu m)= 0.9Emission Rate (kg/hr)= 0.10


AR315076APPENDIX D

FILE NAME - 28PH5 PROG.=VER 02/17/97RUN # - 5 - Method 0050 Train for PM/HCl, and Chlorine

02-25-1997 12:49:44-OCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelATE - 02/07/97 Time: 1150:30-1326:30/1420:30-1501:15/1504:15-1559:30PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Point •# ' Delta P Delta H Stack T Meter T(in. H20) (in. H20) (F) In(F) Out(F)

1 0.290 . 1.20 185 68 672 0.310 1.30 185 68 663 0.310 1.20 • 186 72 684 - 0.270 1.10 186 75 69 ' .5 "0.250 1.00 185 77 706 0.240 0.95 186 80 727 0.250 1.10 185 82 73 .8 0.270 1.20 185 84 759 0.280 1.20 185 -85 76 .10 ' 0.280 1.30 184 86 7711 0.280 . 1.30 184 87 7812 0.220 0.98 184 88 7913 0.220 1.00 183 77 7614 - -0.240 1.10 184 77 7615 0.260 1.20 184 82 7616 0.250 1.10 184 84 7717 ' 0.240 .1.00 185 85 7818 0.240 1..00 185 86 7919 0.230 0.97 185 86 7920 0.240 1.00 . 185 87 8021 0.250 1.00 186 88 . 8122 0.260 1.10 185 90 8223 0.270 1.10 186 92 8224 0.260 1.10 185 91 86

Fraction Final Wt. Tare Wt. Blank Wt. Net Wt.(g) (g) (g) (g)

DRY CATCH 0.0000 0.0000 0.0000 0.0000FILTER 1.0308 1.0253 .0.0000 0.0055

Fraction Final Wt. Tare Wt. Vol. Net Wt.(g) (g) (ml) (g)

PROBE RINSE 67.0398 67.0373 219.6 0.0025IMPINGERS . 0.0000 0.0000 0.0 0.0000Probe Rinse Blank (mg/ml)= 0.0000Impinger Blank (mg/ml)= 0.0000


Lk Rate (cfm) Time (min)0.0020 96.00000.0050 96.0000

AR3I5077APPENDIX D 20

FILE NAME - 28MM5 /* PROG.=VER 06/27/89RUN # - 5'- Method 29 Train for Multiple Metals 02-17-1997 16:26:43LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/07/97 Time: 1151-1327/1429-1501:30/1503:30-1559PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 645.479Final Meter Volume (Cubic Feet)= 756.208-^Meter Factor= 0.996-'Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 110.286Gas Volume (Dry Standard Cubic Feet)= 106.829

Barometric Pressure (in Hg)= 29.59 /Static Pressure (Inches H20)= -0.41

Percent Oxygen= 11.0 * 0 0Percent Carbon Dioxide= 10.5 JpLiMoisture Collected (ml) = 2988.0 / />« . \Percent Water= 56.8 , 0*1

Average Meter Temperature (F) = 80Average Delta H (in H20)= 1.12Average Delta P (in H20)= 0.274 /Average Stack Temperature (F) = 185 >/


Average Square Root'of Delta P (in H20)= 0.5231% Isokinetic= . 99.2

Pitot Coefficient= 0.82Sampling Time (Minutes)= 192.0Nozzle Diameter (Inches)= 0.371Stack Axis #1 (Inches)= 72.0Stack Axis #2 (Inches)= 72.0Circular StackStack Area (Square Feet)= 28.27

Stack Velocity (Actual, Feet/rain)= 2,139Flow Rate (Actual, Cubic ft/min)= 60,482Flow rate (Standard, Wet, Cubic ft/min)= 48,947Flow Rate (Standard, Dry, Cubic ft/min)= 21,122

AR-315078APPENDIX D 21

* * METRIC UNITS * *FILE NAME - 28MM5 PROG.=VER 06/27/89RUN # - 5 - Method 29 Train for Multiple Metals 02-17-1997 16:26:45LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/07/97 Time: 1151-1327/1429-1501:30/1503:30-1559PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Meters)= 18.277Final Meter Volume (Cubic Meters)= 21.413Meter Factor= - - 0.996Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 3.123Gas Volume (Dry Standard Cubic Meters)= 3.025


Percent Oxygen= - - - - 11.0Percent Carbon Dioxide= 10.5Moisture Collected (ml) = 2988.0Percent-Water= 56.8 •' .

Average Meter Temperature (C)= 27Average Delta- H (mm H20) = 28.4 . . ,Average .Delta P (mm H20) = 7.0Average, Stack Temperature ( C ) = 8 5

Dry Molecular Weight= ' . 30.12Wet. Molecular Weight= • 23.23

Average Square Root of Delta P (mm H20)= 2.6362% Isokinetic= ' ' 99.2

Pitot Coefficient= 0.82Sampling Time (Minutes)= .192.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627

Stack Velocity (Actual, m/min)= 652Flow rate (Actual, Cubic m/min)= 1,713Flow rate (Standard, Wet, Cubic m/mih)= 1,386Flow rate (Standard, Dry, Cubic m/min)= 598

AR3I5079APPENDXX D 22

FILE NAME - 2BMM5 PROG.=VER 06/27/89RUN # - 5 - Method 29 Train for Multiple Metals 02-17-1997 16:26:48LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/07/97 Time: 1151-1327/1429-1501:30/1503:30-1559PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Point # Delta P Delta H Stack T Meter T(in. H20) (in. H20) (F) In(F) Out(F)

1 0.270 1.20 182 70 702 0.260 1.20 182 70 703 0.280 1.30 182 72 704 0.280 1.25 183 75 715 0.270 1.25 182 77 726 0.270 1.20 183 79 747 0.250 1.10 183 82 768 0.250 1.00 185 83 789 0.260 1.05 185 84 7910 0.270 1.10 185 84 8011 0.280 1.10 185 86 8112 0.270 1.10 185 87 8213 0.280 1.10 185 79 7914 0.270 1.10 185 79 7915 0.290 1.15 185 81 7916 0.280 1.10 185 83 7917 0.270 1.10 185 85 8018 0.250 0.95 186 86 8119 0.280 1.05 186 86 8220 0.290 1.10 186 87 8321 0.300 1.10 187 89 8422 0.290 1.10 186 89 8523 0.280 1.05 186 89 8524 0.280 1.05 186 90 86




FILE NAME - 28CR5 PROG.=VER 06/27/89RUN # - 5 - BIF Method Train for Hexavalent Chromium 02-17-1997 16:27:01LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/07/97. Time: 1150-1326/1420-1501:30/1503:30-1558PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Kaven, PA

Initial Meter Volume (Cubic F,eet)= 332.596 • - - -----Final Meter Volume (Cubic Feet)= ' 379.864Meter Factor= 0.989Multiple leak checks, see end of printout . . Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 46.748Gas Volume (Dry Standard Cubic. Feet) = .. .45.299

Barometric Pressure (in Hg) = 29.59Static Pressure (Inches H20)= -0.41

Percent Oxygen= . .11.0Percent Carbon Dioxide= 10.5Moisture Collected (ml)= 1279.2Percent Water= : • 57.1

Average Meter Temperature (F)= ' 79Average Delta H (in H20)= 0.21Average Delta P (in H20)= 0.244Average Stack Temperature (F)= 187

Dry Molecular Weight= 30.12Wet-Molecular Weight= ' 23.20

Average Square Root of Delta P (in H20) = 0.4933% Isokinetic= .94.3

Pitot Coefficient= 0.82Sampling Time (Minutes)= , . 192.0Nozzle Diameter (Inches)= 0.256Stack Axis #1 (Inches)= ' 72.0Stack Axis #2 (Inches)= 72.0Circular Stack . . _ _ ._Stack Area (Square Feet)= 28.27


RR3I508IAPPENDIX D 24

* * METRIC UNITS * *FILE NAME - 28CR5 - PROG.=VER 06/27/89RUN ft - 5 - BIF Method Train for Hexavalent Chromium 02-17-1997 16:27:04LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/07/97 Time: 1150-1326/1420-1501:30/1503:30-1558PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Meters)= 9.418Final Meter "Volume (Cubic Meters)= 10.756Meter Factor= 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 1.324Gas Volume (Dry Standard Cubic Meters)= 1.283


Percent Oxygen= 11.0Percent Carbon Dioxide= . . 10.5Moisture Collected (ml)= 1279.2Percent Water= 57.1

Average Meter Temperature (C)= 26Average Delta .H (mm H20) = 5.2Average Delta P (mm H20)= 6.2Average Stack Temperature (C)= 86



Pitot Coefficient= • 0.82Sampling Time (Minutes) = 192.0Nozzle Diameter (mm)= 6.50Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627


RR315082APPENDIX D 25

FILE NAME - 28CR5 PROG.=VER 06/27/89RUN # - 5 - BIF Method Train -for Hexavalent Chromium. 02-17-1997 16:27-06LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/07/97 Time: 1150-1326/142.0-1501:30/1503:30-1558PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA ' • .

Point # Delta P Delta H Stack T Meter T . . -(in. H20) (in. H20) (F) In(F) Out(F)

1 0.270 0.24 185 69 692 ,0.290 0'.23 187 69 683 0.270 . 0.22 187 70 684 0.260 . 0.22 186 72 705 ' 0.240 0~.20 186 73. 71 '" "6 0.230 0.18 187 75 727 0.240 0.19 187 77 748 ' 0.240 0.20 187 7 9 - 7 59 0.260 0.21 187 79 7710 0.260 0.23 186 .81 7911 0.250 0.21 " 186 82 7912 0.220 0.22 186 83 80 -13 0.210 0 .1,9 185 79 ' 7914 0.220 0.19 186 80 '7915 0.250 0.21 187 81 7916 0.240 0.21 - 186 82 8017 0.250 0.22 186' 83 8018 . 0.250 0.21 187 84 8219 0.210 0.18 186 85 8220 0.220 0.18 187 86 8321 0.230 0.18 . 188 87 84 . .22 0.240 0.19 188 88 8623 ' 0.250 0.20 188 88 8624 0.250 0.21 187 88 87

Multiple leak checks used. Final readings for each segment are listed belowA



FILE NAME - 28SV5 PROG.=VER 06/27/89RUN # - 5 - Method 0010 Train for Semivolatile Organic Compounds

02-17-1997 16:27:19LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/07/97 Time: 1150-1326/1420-1501:15/1504:15-1559PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 876.248Final Meter Volume (Cubic Feet)= 988.086Meter Factor= 0.995Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 111.279Gas Volume (Dry Standard Cubic Feet)= 107.939

•


Percent Oxygen= 10.9Percent Carbon Dioxide= 10.3Moisture Collected (ml)= 2980.8Percent Water= - 56.5

Average Meter Temperature (F) = 80Average Delta H (in H20)= 1.16Average Delta P (in H20)= 0.268Average Stack Temperature (F) = 184



Pitot Coefficient= 0.82Sampling Time (Minutes)= 192.0Nozzle Diameter (Inches) = 0.372Stack Axis #1 (Inches)= 72.0Stack Axis #2 (Inches)= 72.0Circular StackStack Area (Square Feet)= 28.27

Stack Velocity (Actual, Feet/min) = 2,114Flow Rate (Actual, Cubic ft/min)= 59,772Flow rate (Standard, Wet, Cubic ft/min)= 48,426Flow Rate (Standard, Dry, Cubic ft/min)= 21,048

&R3I5081*APPENDIX D 27

* * METRIC UNITS * *FILE NAME - 28SV5 - • PROG.=VER 06/27/89RUN # - 5 - Method 0010 Train for Semivolatile Organic Compounds

02-17-1997 1S:27:22LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/07/97 Time: 1150-1326/1420-1501:15/1504:15-1559PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superf'und Site, Lock Iaven, PA

Initial Meter Volume (Cubic Meters)= 24.812 . 'Final Me;ter Volume (Cubic Meters) = •• 27.979Meter Factor= 0.995Multiple leak checks, see end of printout Leak-Corrections 0.0000Net Meter Volume (Cubic Meters)= 3.151Gas Volume (Dry Standard Cubic Meters)= 3.056


Percent Oxygen= 10.9Percent Carbon Dioxide= • 10.3Moisture.Collected (ml)= 2980.8 . .Percent Water= ' 56.5 ,

Average Meter Temperature (C) = 27Average Delta H (mm H20)= . 29.5Average Delta P (mm H20)= 6.8Average Stack Temperature (C) = 84

Dry Molecular Weight= 30.08Wet Molecular Weight= - - . 23.25 '

Average Square Root of Delta P (mm H20)= , 2.6079% Isokinetic= 100.1

Pitot Coefficient= 0.82Sampling Time (Minutes)= .192.0Nozzle Diameter (mm)= 9.45Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627

Stack Velocity (Actual, m/min)= 644Flow rate (Actual, Cubic m/min)= 1,693 .Flow rate (Standard, Wet, Cubic m/min)= 1,371 , . -Flow rate (Standard, Dry, Cubic m/min)= 596

AR3I5085APPENDIX D

FILE NAME - 28SV5 PROG.=VER 06/27/89RUN # - 5 - Method 0010 Train for Semivolatile Organic Compounds

02-17-1997 16:27:24LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/07/97 Time: 1150-1326/1420-1501:15/1504:15-1559PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA


1 0.230 1.00 183 68 672 0.310 1.40 183 68 673 0.320 ' 1.30 185 72 684 0.300 1.30 184 76 695 0.280 1.20 184 79 716 0.240 1.00 184 82 737 0.260 1.20 183 83 748 0.270 1.20 184 85 769 0.270 , 1.20 184 87 7810 0.280 1.20 184 88 7911 0.290 1.30 184 89 8012 0.260 1.20 184 90 8113 0.230 1.10 183 77 7614 0.250 1.10 183 77 7615 0.260 1.10 184 81 7616 0.260 1.10 184 84 7717 0.260 ' 1.10 184 . 86 7818 0.260 1.10 185 87 7919 0.220 0.97 184 86 8020 0.250 1.00 185 88 8121 0.280 1.10 186 89 8222 0.280 1.20 184 90 8223 0.300 1.30 185 91 8324 0.280 1.20 185 93 84



AR3I5086APPENDIX D

FILE NAME - 28DF5 PROG.=VER 06/27/89RUN # - 5 - Method 23 Train for PCDDs/PCDFs 02-17-1997 16:27:37LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/07/97 Time: 1150-1326/1420-1501: 30/1503 : 30.-1558PROJECT # - . .3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= '490.753Final Meter Volume (Cubic Feet)= 607.176Meter Factor= 0.985Multiple:leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= . ' 114.677Gas Volume (Dry Standard Cubic Feet)= 111.675

Barometric Pressure (in Hg) = 29.59Static Pressure (Inches H20)= -0.41

Percent Oxygen= - • 10.9Percent Carbon Dioxide= 10.5Moisture Collected (ml)= 3104.7Percent Water= 56.7 **Saturated Stack**

Average Meter Temperature (F)= 78Average .Delta H (in H20)= 1.29 -Average Delta P (in H20) = : 0.280Average Stack Temperature (F)= 184


Average Square Root .of Delta P (in H20)= 0.5291% Isokinetic= 100.4

Pitot Coefficient= 0.84Sampling Time (Minutes) = 192.0,Nozzle Diameter (Inches)= 0.371Stack Axis #1 (Inches)= . 72.0Stack Axis #2 (Inches)= , 72.0Circular Stack •Stack Area (Square Feet)= . 28.27

Stack Velocity (Actual, Feet/min)= 2,199Flow Rate (Actual, Cubic ft/min)= 62,174Flow rate (Standard, Wet, Cubic ft/min)= 50,351 .Flow Rate (Standard, Dry, Cubic ft/min)= 21,825

AR3I5087APPENDIX D 3O

* * METRIC UNITS * *FILE NAME - 28DF5 PROG.=VER 06/27/89RUN # - 5 - Method 23 Train for PCDDs/PCDFs 02-17-1997 16:27:39LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/07/97 Time: 1150-1326/1420-1501:30/1503:30-1558PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Meters)= 13.896Final, Meter Volume (Cubic Meters)= 17.193Meter Factor= • - 0.985Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 3.247Gas Volume (Dry Standard Cubic Meters)= 3.162


Percent Oxygen= 10.9Percent Carbon Dioxide= 10.5Moisture Collected (ml)= 3104.7Percent Water= 56.7 **Saturated Stack**

Average Meter Temperature (C) = 25 -Average Delta H (mm H20)= 32.6Average Delta P (mm H20)= 7.1Average Stack Temperature (C) = 85

Dry Molecular Weight= 30.12Wet Molecular Weight= • 23.25

Average Square Root of Delta P (mm H20)= 2.6667.% Isokinetic= • 100.4

Pitot Coefficient= 0.84 •Sampling Time (Minutes)= 192.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627

Stack Velocity (Actual, m/min)= 670Flow ra,te (Actual, Cubic m/min) = 1,761Flow rate (Standard, Wet, Cubic m/min)= 1,426Flow rate (Standard, Dry, Cubic m/min)= 618

flR3J5088APPENDIX D 31

FILE NAME - 28DF5 PROG.=VER 06/27/89RUN # - 5 - Method 23 Train for PCDDs/PCDFs 02-17-1997 16:27:42LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/07/97 Time: 1150-1326/1420-1501:30/1503:30-1558PROJECT # - -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site Lock Haven, PA '

Point # Delta P Delta H Stack T Meter T(in- H20) (in. H20) (F) In(F) Out(F)

1 0.280 1.30 183 . 68 672 0.280 1.25 . 184 68 67 ' .3 0.290 1.25 185 .71 684. 0.290 1.30 184 74 695. 0.270 1.25 184 75 , 706 0.250 1.10 185 79 747 0.270 1.25 184 81 73 . . . .8 0.280 1.30 184 81 759 ' 0 .280 1.30 184 83 .. 7610 0.270 1.30 183 84 7611 0.260 1.20 184 84 7712 0.230 ' '1.10 - 184 85 7813 0.240 1.15 183 75 75 : . '14 0.260 1.20 184 76 7515 0.290 1.35 184 79 . 7616 0.290 1.35 184 81 7617 0.290 1.35 184 82 . 7618 . 0.270 . 1.20 185 83 7719 0.290 . 1.30 185 83 7820 0.300 1-40 184 85 7921 0.320 1".40 185 86 8022. 0.310 1.45 184 87 8023 0.310 1.45 184 '' 88 8124 0.310 1.35 185 88 81



AR3I5089APPENDIX D .32

FILE NAME - 28PCB5 PROG.=VER 06/27/89RUN # - 5- Method 23 Train for PCBs 02-17-1997 16:27:57LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/07/97 Time: 1150-1326/1420-1501:16/1504:16-1559PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Iaven, PA

Initial Meter Volume (Cubic Feet)= 624.252Final Meter Volume (Cubic Feet)= 742.361Meter Factor= 0.977Multiple leak checks, see end of printout Leak Correction^ 0.0000Net Meter Volume (Cubic Feet) = • 115.393Gas Volume (Dry Standard Cubic Feet)= 111.522

Barometric Pressure (in Hg)= 29.60Static Pressure (Inches H20) = -0.41

Percent Oxygen= 11.0Percent Carbon Dioxide= 10.3Moisture Collected (ml)= 3099.8Percent Water= - 54.8 • **Saturated Stack**

Average Meter Temperature (F)= 82Average Delta H (in H20)= 1.28Average Delta P (in H20)= 0.269Average Stack Temperature (F) = 183






* * METRIC UNITS * *FILE NAME - 28PCB5 PROG.=VER 06/27/89RUN # - 5 - Method 23 Train for PCBs 02-17-1997 16:27:59LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/07/97 Time: 1150-1326/1420-1501:16/1504:16-1559PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock taven, PA

Initial Meter Volume (Cubic Meters)= 17.676Final Meter Volume (Cubic Meters)= .21.021 ' ,Meter Factor=- - - - -- . - 0.977Multiple leak checks, see end of printout Leak Correction— 0.0000Net Meter Volume (Cubic Meters)= 3.267Gas Volume (Dry Standard Cubic Meters)= 3.158

Barometric.Pressure (mm Hg)= 752Static Pressure (mm H20) = -10

Percent Oxygen= . _ 11.0Percent Carbon Dioxide= 10.3Moisture Collected (ml)= - • 3099.8Percent Water= 54.8 **Saturated Stack**

Average Meter Temperature (C)= 28Average Delta H (mm H20)= - 32.4Average Delta P (mm H20)= 6.8Average Stack Temperature (C) = 84

•Dry Molecular Weight= 30.09Wet Molecular Weight= 23.46

Average Square Root of Delta P (mm H20)= 2.6130% Isokinetic= • 100.1

Pitot Coefficient= 0.82Sampling Time (Minutes) = , 192.0Nozzle Diameter (mm)= . 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters) = 2.627

Stack Velocity (Actual, m/min)= 642Flow rate (Actual, Cubic m/min) = 1,686 .._Flow rate (Standard, Wet, Cubic m/min)= 1,369Flow rate (Standard, Dry, Cubic m/min)= 619

AR3I509IAPPENDIX D 34

FILE NAME - 28PCB5 PROG.=VER 06/27/89RUN # - 5 - Method 23 Train for PCBs . 02-17-1997 16:28:02LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/07/97 Time: 1150-1326/1420-1501:16/1504:16-1559PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lockaven, PA

Point # Delta P Delta H Stack T Meter T(in. H20) (in. H20) (F) In(F) Out(F).

1 0.240 1.14 182 69 682 0.260 1.24 182 71 683 0.280 - 1.28 183 75 704 0.270 1.35 182 78 715 0.260 1.26 182 81 746 0.250 1.21 183 83 767 0.240 1.17 182 85 788 0.240 1.12 183 87 809 0.250 1.17 183 88 8110 0.250 1.22 182 Q8 8211 0.270 1.33 182 89 8312 0.240 1.18 182 90 8413 0.280 1.36 182 79 7914 0.270 1.31 182 79 7915 0.310 1.51 182 83 7816 0.280 1.36 . 182 85 7917 0.270 1.26 183 88 8118 , 0.270 1.26 183 89 8219 0.280 1.31 183 88 8320 0.280 1.31 183 90 8321 0.300 1.34 184 91 8422 0.290 1.36 . 183 92 8523 0.300 1.34 184 • 93 8624 0.280 1.25 184 93 87


Lk Rate (cfm) Time (min) '0.0040 96.00000.0030 96.0000


Run 6


MRI-AppHed/R362028.APP

BR3I5093APPENDIX D 36

FILE NAME - 28PH6 ' PROG.=VER 02/17/97RUN # - 6 - Method 0050 Train for PM, HC1, and Chlorine

02-25-1997 12:51:30LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower Level'ATE - 02/08/97 Time: 1100:30-1242:30/1330:30-1512:30ROJECT # - ' -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA "

Initial Meter Volume (Cubic Feet)= 901.033Final Meter Volume (Cubic Feet)= 1018.095Meter Factor= 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 115.774Gas Volume (Dry Standard Cubic'Feet)= 112.870

Barometric Pressure (in Hg)= ( 29.62 ' .Static Pressure (-Inches H20)= -0.41

1 ' '

Percent Oxygen= .- . .11.0Percent Carbon Dioxide= . ' 1 0 . 5Moisture Collected (ml)= ,3149.2Percent Water= 56.8

Average Meter Temperature (F)= 77Average Delta H (in H20)= 1.12Average Delta P (in H20)= ' 0.264Average Stack Temperature (F)= 185

Dry Molecular Weight= • 30.12Wet Molecular Weight= 23.24 .

Average Square Root of Delta P (in H20)= 0.5128% Isokinetic= • r 98.8

Pitot Coefficient= 0.84Sampling Time (Minutes)= 204.0Nozzle Diameter (Inches)= 0.371Stack Axis #1 (Inches)= 72.0Stack Axis #2 (Inches)= . 72.0Circular StackStack Area (Square 'Feet)= - 2 8 . 2 7



Particulate Weight (g)= 0.0075 Corr. to 7% 02 equivalentParticulate Loading, Dry Std. (gr/scf)= 0.0010 0.0008Particulate Loading, Actual (gr/cu ft)= 0.0004Emission Rate (lb/hr)= 0.18


.'AR3I5091*APPENDIX D



Initial Meter Volume (Cubic Meters)= 25.514Final Meter Volume (Cubic Meters)= 28.828Meter Factor= 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 3.278Gas Volume (Dry Standard Cubic Meters)= 3.196

Barometric Pressure (mm Hg)= • , 752Static Pressure (mm H20)= -10

Percent Oxygen= " 11.0Percent Carbon Dioxide= - 10.5Moisture Collected (ml)= 3149.2Percent Water= 56.8

Average Meter Temperature (C)= 25Average Delta H (mm H20)= 28.6Average Delta P .(mm H20)= 6.7Average Stack Temperature (C)= 85


Average Square Root of Delta P (mm H20) = 2.5844% Isokinetic= 98.8

Pitot Coefficient= 0.84Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= - 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= '2.627



Particulate Weight (g) = 0.0075 Corr. to 7% 02 equivalentParticulate Loading, Dry Std. (mg/cu m)= 2.3 1.9Particulate Loading, Actual (mg/cu m)= 0.8Emission Rate (kg/hr)= , 0.08



FILE NAME - 28PH6 PROG.=VER 02/17/97RUN # - 6 - Method 0050 Train for PM, HCl, and Chlorine

02-25-1997 12:51:36LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/08/97 Time: 1100:30-1242:30/1330:30-1512:30PROJECT # - -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

• Point # Delta P Delta H Stack T Meter T(in. H20) (in. H20) (F) In(F) Out(F)

1 0.280 1.20 184 66 .652 0.310 1.30 184 66 653 0.300 1.30 • 184 70 664 0.280 1.20 185 75 685 0.250 1.00 .185 78 696 0.230 1.00 184 79 707 0.260 1.10 185 80 728 0.290 1.20 185 82 739 0.310 1.30 185 83 75

• 10 0.310 1.40 184 85 7611 0.290 1.20 . 185. 86 7712 ' 0.260 1.10 185 86 7813 0.200 0.89 184 75 7414 0 .240 - 1.10 184 75 7415 ' 0.260 1.10 185 79 7416 -0.260 1.20 184 82 7517 0.270 1.10 185 84 7618 0.260 1.00 185 85 7719 0.250 1.10 185 86 7820 0.240 1.00 185 86 7821 0.250 1.10 185 87 7922 0.270 1.10 185 87 7923 0.250 1.10 185 88 8024 . 0.210 0.89 185 . 88 81

Fraction Final Wt. Tare Wt. Blank Wt. Net Wt.(g) (g) . (g) (g)

DRY CATCH 0.0000 0.0000 0.0000 0.0000FILTER 1.0458 1.0402 0.0000 0,0056

Fraction Final Wt. Tare Wt. Vol. Net Wt. .(g) (g) (ml) (g)

PROBE RINSE 60.1114 60.1095 191.0 0.0019IMPINGERS 0.0000 0.0000 0.0 0.0000Probe Rinse Blank (mg/ml)= 0.0000 , ,Impinger Blank (mg/ml)= 0.0000



AR3I5096APPENDIX D . 39

FILE NAME - 28MM6 PROG.=VER 06/27/89RUN ft - 6 - Method 29 Train for Multiple Metals 02-17-1997 16:28:34,LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/08/97 Time: 1101-1243/1331-1513PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 757.705Final Meter Volume (Cubic Feet)= 873.652Meter Factor= . 0.996Multiple leak checks, see end of printout . Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 115.483Gas Volume (Dry Standard Cubic Feet)= 112.216


Percent Oxygen= 11.1Percent Carbon Dioxide= 10.5Moisture Collected (ml)= 3132.9Percent Water= . 56.8

Average Meter Temperature (F) = 79Average Delta H (in H20)= 1.07Average Delta P '(in H20)= 0.269Average Stack Temperature (F) = • 186






* * METRIC UNITS * *FILE NAME - 28MM6 . PROG.=VER 06/27/89RUN # - 6 - Method 29 Train for Multiple Metals 02-17'-1997 16:28:36LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/08/97 Time: L101-1243/1331-1513PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA . ..

Initial Meter Volume (Cubic Meters)= 21.455Final Meter Volume (Cubic Meters)= 24.738Meter Factor= 0.996 ---Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 3.270Gas Volume (Dry Standard Cubic Meters)= 3.178

e

Barometric Pressure (mm Hg)= . • 752Static Pressure (mm H20)= -10

Percent Oxygen= . 11.1 . . -Percent Carbon Dioxide=' 10.5Moisture Collected (ml)= 3132.9Percent Water= . 56.8

Average Meter Temperature (C)= 26Average Delta H . (mm H20,)= .27.2Average Delta P (mm H20)= 6.8Average Stack Temperature (C)= 85

Dry Molecular Weight= . 30.12Wet Molecular Weight= 23.24

Average Square Root of Delta P.(mm H20)= 2.6118% Isokinetic= 97.4

Pitot- Coefficient= 0.82Sampling Time (Minutes)= . 204.0Nozzle Diameter (mm) = 9.50 -Stack Axis #1 (Meters)= . . 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627

Stack Velocity (Actual, m/min)= 646Flow rate (Actual, Cubic m/min)= 1,697Flow rate (Standard, Wet, Cubic m/min)= 1,372Flow rate (Standard, Dry, Cubic m/min)= . 593


FILE NAME - 28MM6 PROG.=VER 06/27/89RUN § - 6 - Method 29 Train for Multiple Metals 02-17-1997 16:28:38LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/08/97 Time: 1101-1243/1331-1513PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lockaven, PA


1 0.250 0.95 186 69 692 0.260 1.05 185 69 683 0.280 1.20 184 72 694 0.280 1.15 185 75 705 0.280 1.10 186 78 726 0.260 1.10 185 80 74 - .7 0.260 1.10 185 81 758 • 0.270 1.05 186 82 779 0.300 1.25 185 83 7810 0.270 1.10 185 84 7911 0.270 1.05 186 86 8112 0.270 1.05 186 87 8213 0.250 1.00 185 77 7614 • 0.260 1.05 185 77 7615 0.270 1.10 185 80 7716 0.270 1.05 186 . 81 7717 0.270 1.05 186 83 7918 0.250 1.00 186 83 7919 0.270 1.10 186 84 8020 0.290 1.15 186 85 8121 0.290 1.15 186 86 8122 0.280 1.05 187 , 87 8223 0.260 1.00 186 87 8224 0.240 0.88 187 87 83




FILE NAME - 28CR6 PROG.=VER 06/27/89RUN # - 6 - BIF Method Train for Hexavalent Chromium 02-17-1997 16:28:55LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 382.925Final Meter Volume (Cubic "Feet)= 433.113Meter Factor= ; - -- . 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 49.636Gas Volume (Dry Standard Cubic Feet)= 48.234 , ' .

Barometric Pressure (in Hg)= 29.61Static.Pressure (Inches H20)= ' -0.41

Percent Oxygen= . . - . 11.1 --- -Percent Carbon Dioxide= ' 10.5Moisture Collected, (ml) = 1356.4Percent Water= 57.0

Average Meter Temperature (F)= 78Average Delta H (in H20)= 0.21Average Delta P (in H20)= 0.239Average Stack Temperature (F)= 186

Dry Molecular Weight= . 30.12Wet Molecular-Weight = - - 23.22

Average Square Root of Delta P (in H20)= 0.4889•% Isokinetic= 95.1 "


Stack Velocity (Actual, Feet/min)= 2,002Flow Rate (Actual, Cubic ft/min) = 56', 606Flow rate (Standard, Wet, Cubic ft/min)= - 45,711Flow Rate (Standard, Dry, Cubic ft/min)= 19,665

A R 3 I 5 I O OAPPENDIX D 43

* * METRIC UNITS * *FILE NAME - 28CR6 PROG.=VER 06/27/89RUN # - 6 - BIF Method Train for Hexavalent Chromium 02-17-1997 16:28:57LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lockaven, PA


Barometric Pressure (mm Hg)= 752Static Pressure (mm H20)= . -10


Average Meter Temperature (C) = 25Average Delta H (mm H20)= 5.2Average Delta P (mm H20)= 6.1Average Stack Temperature (C)= 86



•Pitot Coefficient= 0.82Sampling Time (Minutes) =. 204.0Nozzle Diameter (mm)= ' 6.50Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627

Stack Velocity (Actual/ m/min)= 610Flow rate (Actual, Cubic m/min)= 1,603Flow rate (Standard, Wet, Cubic m/min)= 1,294Flow rate (Standard, Dry, Cubic m/min)= 557

A R 3 I 5 I O IAPPENDIX D 44

FILE NAME - 28CR6 - PROG.=VER 06/27/89RUN # -.6 - BIF Method Train for Hexavalent Chromium 02-17-1997 16:29:00LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA


1 0.240 0.22 185 6-8 68 . '"2 0.250 0.24 186 . 69 68'3 . 0.250 0.21 186 71 69 •4 0.240 0.21 186 72 695 0.240 0.20 187 75 726 ' ' 0.220 0.19 186 77 737 0.240 0.21 , 186 78 758 0.250 0.22 186 80 769 0.260 0.23 186 81 7810 0.260 0.23 186 82 7811 0.240 0.21 186 83 8012 0.230 0.20 186 83 8013 0.240 0.21 186 78 7714 . - -Q.240 0.21 -186 78 • 7715 0.240 0.21 186 79 7716 . 0.250 0.21 187 79 . 7717 0.250 0.20 187 80 7718 . 0.250 0.21 187 81 78 . .19 0.230 0.19 187 82 7920 0.210 0.17 187 . 82 8021 0.210 * 0.16 188 83 8122 0.230 0.19 187 84 8223 0.230 0.19 187 85 8324 0.240 0.20 187 85 84


Lk Rate (cfm) Time (min)0.0040 102.0000 ' '0.0010 102.0000

A R 3 I 5 I 0 2APPENDIX D 45

FILE NAME - 28SV6 . PROG.=VER 06/27/89RUN # - 6 - Method 0010 Train for Semivolatile Organic Compounds

02-17-1997 16:29:14LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 991.165Final Meter Volume (Cubic Feet)= 1104.749Meter Factor= 0.995Multiple leak checks., see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 113.016Gas Volume (Dry Standard Cubic Feet)= 110.048


Percent Oxygen= 11.0Percent Carbon Dioxide= - 10.5Moisture Collected (ml)= . 3071.4Percent Water= 56.8

Average Meter Temperature (F)= 78Average Delta H (in H20)= 1.08Average Delta P (in H20)= 0.253Average Stack Temperature (F) = 184

Dry Molecular Weight= . 30.12Wet Molecular Weight= 23.24

Average Square Root of Delta P (in H20)= 0.5028% Isokinetic= . 99.9


Stack Velocity (Actual, Feet/min)= . 2,055Flow Rate (Actual, Cubic ft/min)= 58,101Flow rate (Standard, Wet, Cubic ft/min)= 47,076Flow Rate (Standard, Dry, Cubic ft/min)= 20,339

A R 3 I 5 I Q 3APPENDIX D 46

* * METRIC UNITS * *FILE NAME - 28SV6 . ' PROG.=VER 06/27/89RUN # - 6 - Method 0010 Train for Semivolatile Organic Compounds

02-17-1997 16:29:16LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT #' -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lockaven, PA

Initial Meter Volume'(Cubic Meters)= . • 28.066Final Meter Volume (Cubic Meters)= 31.282Meter Factor= - . 0.995 ;Multiple leak checks, see end of printout Leak Cor'rection= 0.0000Net Meter Volume (Cubic Meters)= 3.200Gas Volume (Dry Standard Cubic Meters) = 3-. 116

Barometric Pressure (mm Hg)= . 752Static Pressure (mm H20)= -10

Percent Oxygen= 11.0Percent Carbon Dioxide= . 10.5Moisture Collected (ml)= 3071.4Percent Water= 56.8.

Average Meter Temperature (C) = 26Average, Delta H (mm H20)'= . 27.3, • "Average Delta P (mm H20)= 6.4Average Stack Temperature (C)= 85

Dry Molecular Weight= 30.12Wet Molecular Weight= . - . 23.24


Pitot Coefficient= • 0.82Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= , 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular Stack ~Stack Area (Square Meters)= 2.627

Stack Velocity (Actual, m/min) = 626Flow rate (Actual,.Cubic m/min)= 1,645Flow rate (Standard, Wet, Cubic m/min)- • 1,333Flow rate (Standard, Dry, Cubic m/min)= 576

APPENDIX D 47

FILE NAME - 28SV6 • PROG.=VER 06/27/89RUN # - 6 - Method 0010 Train for Semivolatile Organic Compounds

02-17-1997 16:29:19LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock I-aven, PA


1 0.260 1.10 184 ' 65 652 0.280 1.20 184 65 643 0.280 1.20 184 70 664 • 0.270 1.10 185 74 675 0.260 1.10 185 77 696 0.230 1.00 184 79 71 .7 0.260 1.10 185 82 738 0.270 1.10 185 83 759 0.290 1.30 184 84 7610 0.270 1.20 184 85 7711 0.260 1.10 185 87 7812 0.240 1.00 184 87 7913 0.220 0.94 184 76 7514 0.230 1.00 184 75 7415 0.250 1.10 184 79 7516 0.250 1.10 184 82 7517 0.260 1.10 184 84 7618 0.250 1.10 184 86 7719 0.200 - 0.82 ' 185 87 7920 0.220 0.91 185 87 8021 0.260 ' 1.10 185 88 8022 0.270 1.10 185 89 8123 0.270 1.10 185 89 8224 0.230 0.95 185 89 82



AR3I5I05APPENDIX D 43

FILE NAME - 28DF6 . - PROG.=VER 06/27/89RUN # - 6 - Method 23 Train for PCDDs/PCDFs 02-17-1997 16:29:32LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= ' 609.200 ' . . _ . _ _ _ ,Final Meter Volume (Cubic Feet)= 730.506Meter Factor= , 0.985Multiple leak checks, see end of printout Leak Corrections 0,0000Net Meter Volume (Cubic Feet)= 119.486 ,Gas Volume (Dry Standard Cubic Feet) = 116.900

Barometric Pressure (in Hg)= 29.61Static Pressure (Inches H20)= - -0..41

Percent Oxygen= 11.1Percent Carbon Dioxide= 10.5Moisture Collected (ml)= 3272.2Percent Water= ' 56.9

Average Meter Temperature (F)= 76Average Delta H (in H20)= . 1.24Average Delta P (in H20)= 0.278Average __Stack Temperature (F) = 185

Dry Molecular Weight= 30.12Wet Molecular Weight= . 23.23 -

Average Square Root of Delta P (in'H20,)= 0.5273% Isokinetic= . 99.7 .

Pitot Coefficients 0.84Sampling Time (Minutes)= 204.0Nozzle Diameter (Inches)= 0.371Stack Axis #1 (Inches)= ' <72 . 0Stack Axis #2 (Inches)= 72.0Circular StackStack Area (Square Feet)= 28.27

Stack Velocity (Actual, Feet/min)= 2,192Flow Rate (Actual,.Cubic ft/min)= 61,981Flow rate (Standard, Wet, Cubic ft/min)= 50,200Flow Rate (Standard, Dry, Cubic ft/min)= 21,653

A R 3 I 5 I Q 6APPENDXX D 49

* * METRIC UNITS * *FILE NAME - 28DF6 PROG.=VER 06/27/89RUN # - 6 - Method 23 Train for PCDDs/PCDFs 02-17-1997 16:29:34LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lockaven, PA

Initial Meter Volume (Cubic Meters)= 17.250Final Meter Volume (Cubic Meters)= 20.685Meter Factor= ' 0.985Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 3.383Gas Volume (Dry Standard Cubic Meters)= 3.310


Percent Oxygen= 11.1Percent Carbon Dioxide- 10.5Moisture Collected (ml)= 3272.2Percent Water= 56.9




Pitot Coefficient= . 0.84Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627

Stack Velocity (Actual, m/min)=- 668Flow rate (Actual, Cubic m/min)= 1,755Flow rate (Standard, Wet, Cubic m/min)= 1,422Flow rate (Standard, Dry, Cubic m/min)- 613

A R 3 I 5 I Q 7APPENDIX D 5O

FILE NAME - 28DF6 ' . PRQG.=VER 06/27/89RUN # - 6 - Method 23 Train for PCDDs/PCDFs . 02-17-1997 • 16:29:37LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA . .


1 0.280 1.25 184 66 652 0.290 1.25 185 68 663 0.280 1.30 184 72 674 0.280 1.30 184 74 68 -5 0.280 1.20 185 76 69 ° -6 0.260 1.20 184 77 717 0.270 ' 1.25 184 79 728 0.300 1.30 185 80 739 0.310 1.40 184 80 7410 0.280 1.30 ' 184 82 7511 - 0.250 1.10 185 83 7612 0.230 1.05 184 83 .76 ' . . --13 0.260"" 1.20 184 72 7114 0.260 1.20 184 73 7215 0.290 1.30 184 76 7216 0.280 1.20 185 79 7317 0.290 1.25 185 80 7318 . 0.270 1.20 185 81 7419 0.250 1.10 . 185 82 7520 0.290 1.25 185 82 7521 0.300 1.30 185 83 7722 0.300 1.30 185 84 7723 0.290 1.25 185 84 77

' 24 0.290 1.35 184 84 77



A R 3 1 5 I 0 8APPENDIX D 51

FILE NAME - 28PCB6 • PROG.=VER 06/27/89RUN # - 6 - Method 23 Train for PCBs . 02-17-1997 16:29:50LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 744.378Final Meter Volume (Cubic Feet)= - 866.479Meter Factor= 0.977Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 119.293Gas Volume (Dry Standard Cubic Feet)= 116.149


Percent Oxygen= 11.1Percent Carbon Dioxide= • 10.5Moisture Collected (ml)= 3224.6Percent Water= 54.7 **Saturated Stack**

Average Meter Temperature (F) = . 78Average Delta H (in H20)= 1.21Average Delta P (in H20) = 0.257Average Stack Temperature (F)= 183


Average Square Root of Delta P (in H20.) = 0.5069% Isokinetic= ' 100.2



flR3l5!09APPENDIX D 52.

* * METRIC UNITS * *FILE NAME - 28PCB6 . PROG.=VER 06/27/89RUN # - 6 - Method 23 Train for PCBs ' 02-17-1997 16:29:53LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower-LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp.,. Drake Chemical Superfund Site, Lock Kaven, PA

Initial Meter Volume (Cubic. Meters)= 21.078Final Meter Volume (Cubic Meters) = 24.535 '• — 'Meter Factor= 0.977Multiple leak checks, see end of printout Leak.Corrections 0.0000Net Meter Volume (Cubic Meters)= 3.378Gas Volume (Dry Standard Cubic Meters) = 3.28.9

Barometric Pressure (mm Hg)= 752Static Pressure (mm H20) = -10

Percent Oxygen= - - . : -- 11.1Percent Carbon Dioxide= 10.5Moisture Collected (ml)= . 3224.6'Percent Water= 54.7 **Saturated Stack**


Dry Molecular Weight= . . 30.12Wet Molecular Weight= . 2 3 . 4 9

Average Square Root of Delta P (mm H20)= 2.5545% Isokinetic= •- - , - 100.2

Pitot Coefficients 0.82Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= 9.42 • -Stack Axis #1 (Meters) = 1..829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627

Stack Velocity (Actual, m/min)= • 627 ' .Flow rate (Actual, Cubic m/min)= 1,647Flow rate (Standard, Wet, Cubic m/min)= 1,338Flow rate (Standard, Dry, Cubic m/min)= 606

SR3I5! J OAPPENDIX D 53

FILE NAME - 28PCB6 . PROG.=VER 06/27/89RUN # - 6 - Method 23 Train for PCBs 02-17-1997 16:29:55LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/08/97 Time: 1100-1242/1330-1512PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA


1 0.220 1.04 182 65 652 0.250 1.24 181 67 653 0.260 1.24 182 71 674 • 0.260 1.24 182 74 685 0.250 1.20 182 77 696 ' 0.250 1.20 182 78 717 0.260 1.20 183 81 738 0.250 1.15 183 83 759 0.260 1.26 182 83 7610 0.260 ' 1.20 183 84 7711 0.270 1.25 183 85 7812 0.240 1.12 183 86 7913 0.240 1.16 182 76 7614 0.260 1.25 182 76 7515 0.270 1.24 183 80 7516 0.260 1.26 182 82 7617 0.270 1.19 184 84 7718 0.260 1.21 183 85 7919 0.250 1.16 183 86 7920 0.260 1.21 183 87 8121 0.280 1.31 183 88 8222 0.280 1.31 183 89 8223 0.270 1.26 183 89 8324 0.240 1.12 183 89 83



A R 3 I 5 I I IAPPENDIX D 54

__________ __ Run 7


MRI.Applied/R36202S.APP

A R 3 I 5 I 1 2APPENDIX D . 55

FILE NAME -. 28PH7 . PROG.=VER 02/17/97RUN # - 7 - Method 0050 Train for PM, HCl, and Chlorine

• . 02-25-1997 12:53:42LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - ,02/09/97 Time: 1045:30-1227:30/1255:30-1437:30PROJECT # -3620.28.30 OHM Remediation Services Corp:, Drake Chemical Superfund Site, Lock.Haven, PA

I

Initial Meter Volume (Cubic Feet)= 20.553Final Meter Volume (Cubic, Feet) = 136.091 -Meter Factor= 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 114.267Gas Volume' (Dry Standard Cubic'Feet)= 111.621

Barometric Pressure (in Hg)= . 29.65Static. Pressure (Inches H20)= -0.41 '

Percent Oxygen= 11.3Percent Carbon Dioxide= • 10.4Moisture Collected (ml)= 3081.6Percent Water= .._.._..._.- 56.5

Average Meter Temperature (F) = 77Average Delta H (in H20)= . 1.11Average Delta P (in H20)= 0.255Average Stack Temperature (F) = 185


Average Square Root of Delta P (in H20) = 0.5,044% Isokinetic= - - 98.7

Pitot Coefficient= - 0.84Sampling Time (Minutes) = 204.0Nozzle Diameter (Inches)= . 0.371Stack Axis #1 (Inches)= 72.0Stack Axis >#2 (Inches)= 72.0Circular StackStack Area (Square Feet)= 28.27



Particulate Weight (g)= . 0.0066 Corr. to 7% 02 equivalentParticulate Loading, Dry Std. (gr/scf)= 0.0009 0.0007Particulate Loading, Actual (gr/cu ft)= 0.0003Emission Rate (lb/hr)= 0.16

No Back Half Analysis .

A R 3 I 5 I I 3APPENDIX D 56



Initial Meter Volume (Cubic Meters)= 0.582Final Meter Volume (Cubic Meters)= 3.854Meter Factor= - 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000 'Net Meter Volume (Cubic Meters)= 3.236Gas Volume (Dry Standard Cubic Meters)= 3.161

Barometric Pressure (mm Hg)= 753Static Pressure (mm H20)= . -10


Average Meter Temperature (C)= 25Average Delta H (mm H20)= 28.1Average Delta P (mm H20)= 6.5Average Stack Temperature (C) = 85

Dry Molecular Weight= , 30.12Wet Molecular Weight= - 23.27

Average Square Root of Delta P (mm H20)= 2.5419% Isokinetic= - - 98.7

Pitot Coefficient= 0.84Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= . 2.627



Particulate Weight (g)= 0.0066 Corr. to 7% O2 equivalentParticulate Loading, Dry Std. (mg/cu m) = 2.1 1.7Particulate Loading, Actual (mg/cu m)= 0.7Emission Rate (kg/hr)= . 0.07


A R 3 I 5 I I UAPPENDIX D 57

i>.

•FILE NAME - 28PH7 PROG.=VER 02/17/97RUN # - 7 - Method 0050 Train for PM, HC1, and Chlorine

; 02-25-1997 12:53:47OCATION - Mobile Hazardous Waste'Incinerator Stack - Lower LevelATE - 02/09/97 Time: 1045:30-1227:30/1255:30-1437:30PROJECT # - •3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Point # Delta P Delta H Stack T Meter T(in. H20) (in. H20) (F) ' In(F) Out(F)

1 0.270 1.20 184 65 652 0.310 1.30 . 184 65 643 0.300 1.30 184 69 644 0.270 1.20 184 74 675 0.240 1.10 184 76 ' 686 . 0.230 0.96 185 78 697 0.250 1.10 185 79, 718 ' 0.260 1.20 184 80 729 0.280 1.20 ' 184 82 7310 ' 0.290 1.20 185 83 7411 0.280 1.30 184 84 7512 ' 0.270 1.10 185 85 7613 0.220 -1.00 184 76 7514 0.240 1.10 184 77 7415 0.260 1.10 185 80 7516 ' 0.270 1.10 186 83 75 '17 0.250 1.10 .. 184 84 76 . :18 0.250 1.10 185 85 77 - ' -19 0.230 1.00 185 86 7820 0.230 1.00 185 86 7821 0.240 1.00 185 86 7922 0.230 1.00 185 87 7923 0.240 - 1.00 185 88 8024 0.210 0.89 185 89 80

Fraction ' Final Wt. Tare Wt. Blank Wt. Net Wt.(.g) (g) -(g) (g)

DRY CATCH 0.0000 . 0.0000 0.0000 0.0000FILTER -1.0981 1.0932 0.0003 0.0046

Fraction Final Wt. Tare Wt. Vol. Net Wt.(g) (g) (ml) , (g)

PROBE RINSE 68.8647 68.8627 191.6 0.0020IMPINGERS 0.0000 0.0000 0.0 0.0000Probe Rinse Blank (mg/ml)= 0.0000Impinger Blank (mg/ml)= 0.0000


Lk Rate (cfm) Time (min)0.0010 102.0,0000.0030 102.0000

B R 3 I 5 I 1 5APPENDIX D 5S

FILE NAME - 28MM7 PROG.=VER 06/27/89RUN # - 7 - Method 29 Train for Multiple Metals 02-17-1997 16:30:34LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/09/97 Time: 1046-1228/1256-1438PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 874.152Final Meter Volume (Cubic Feet)= 988.656Meter Factor= 0.996Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 114.046Gas Volume (Dry Standard Cubic Feet)= 110.870

Barometric Pressure (in Hg)= 29.64Static Pressure (Inches H20}= -0.41




Average Square Root of Delta P (in H20}= 0.5186% Isokinetic= 97.3

Pitot Coefficient= 0.82Sampling Time (Minutes)= 204.0Nozzle Diameter (Inches)= 0.371Stack Axis #1 (Inches)= 72.0Stack Axis #2 (Inches)= 72.0Circular StackStack Area (Square Feet)= • 28.27


A R 3 I 5 I I 6APPENDIX D 59

* *'METRIC UNITS * *FILE NAME - 28MM7 PROG.=VER 06/27/89RUN # - 7 - Method 29 Train for Multiple Metals 02-17-1997. 16:30:35LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/09/97 Time: 1046-1228/1256-1438PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Meters)= -24.752Final Meter Volume (Cubic Meters)= . 27.995Meter Factor= -------- . • ' -. - 0.. 996Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 3.229Gas Volume (Dry Standard, Cubic Meters)= 3.139

Barometric Pressure (mm Hg)= . 753Static Pressure (mm H20)= . -10

Percent Oxygen= - - 11.3Percent Carbon Dioxide= .. - 10.4 . . •Moisture Collected (ml)= 3073.9Percent Water= . .. 56.6 . .

Average Meter Temperature (C)= 26Average Delta H (mm H20)= . 26.6 " . .Average Delta P (mm H20)= 6.8Average Stack Temperature (C)= 85 . -

Dry Molecular Weight= - - • - 30.12Wet Molecular Weight= 23.25

Average Square Root of Delta P (mm H20)= 2.6139% Isokinetic= -- . 97.3

Pitot Coefficient= . 0.82Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= 1.829Stack Axis # 2 (Meters)= 1.829 . . .Circular StackStack Area (Square Meters)= 2.627

;



FILE NAME - 28MM7 PROG.=VER 06/27/89RUN ft - 7 - Method 29 Train for Multiple Metals 02-17-1997 16:30:39LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/09/97 Time: 1046-1228/1256-1438PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA


1- 0.250 1.05 184 69 692 0.260 1,00 185 69 693 0.270 1.05 185 71 694 0.280 1.10 185 74 715 0.270 1.05 185 77 726 0.260 1.05 185 78 747 0.250 0.99 185 80 758 0.250 0.99 185 81 769 0.270 1.10 185 82 7810 0.280 1.10 ' 185 83 7811 0.280 1.10 185 84 7912 0.290 1.15 185 85 8013 0.290 1.15 185 78 7814 0.280 1.10 185 79 7815 0.280 1.20 184 81 7816 0.290 1.10 186 82 7917 0.270 1.00 186 84 8018 0.250 1.00 185 85 8019 0.270 1.00 186 85 8120 0.280 1.05 186 86 8221 0.270 1.00 186 87 8222 0.270 1.00 186 '88 8323 0.250 0.95 . 186 88 8424 0.250 0.90 187 88 84




FILE NAME - 28CR7 PROG.=VER 06/27/89RUN # - 7 - BIF Method Train for Hexavalent Chromium 02-17-1997 16:30:56LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/09/97 Time: 1045-1227/1255-1437'PROJECT # - -3620.2.8.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 436.061Final Meter Volume (Cubic Feet)= 488.229Meter Factor= - • . - - . ' . , . 0.989Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet) = 51.594 . ._.,,.--Gas Volume (Dry Standard Cubic Feet)= 50.147 ' "

Barometric Pr'essure (in Hg) = 29.64 . . - _._ .Static Pressure (Inches H20)= - . -. -0.41

Percent Oxygen= . ... . 11.3Percent Carbon Dioxide= . 1 0 . 4Moisture Collected, (ml)= 1378.6Percent Water= - - . > • . - 56.4 • " "

Average Meter Temperature (F) = 78Average Delta H (in H20)= 0.22 .. _Average Delta P (in H20)= . 0.267 ' :Average Stack Temperature (F)= 187

Dry Molecular Weight= ' 30.12 .Wet Molecular Weight= 23.28 '

Average Square Root of Delta P (in H20)= 0.5162% Isokinetic= " _ . _ _ _ . . - . . . . " . . . 92.6

Pitot Coefficient= - 0.82 .Sampling Time (Minutes)= • 204.0Nozzle Diameter (Inches)= 0.256Stack Axis #1 (Inches)= 72.0 •Stack Axis #2 (Inches)= 72.0Circular StackStack Area (Square Feet)= 28.27

Stack Velocity (Actual, Feet/min) = 2,111Flow Rate (Actual, Cubic ft/min) = 59', 673 'Flow rate (Standard, Wet, Cubic ft/min)= • 48,205Flow Rate (Standard, Dry, Cubic ft/min)= 21,006 -


* * METRIC UNITS * *FILE NAME - 28CR7 PROG.=VER 06/27/89RUN # - 7 - BIF Method Train for Hexavalent Chromium 02-17-1997 16:30:58LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/09/97 Time: 1045-1227/1255-1437PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA



Percent Oxygen= 11.3Percent Carbon Dioxide= - 10.4Moisture Collected (ml)= - . 1378.6Percent Water= - 56.4

Average Meter Temperature (C) = 26Average Delta H (mm H20)= 5.6Average Delta P (mm H20)= 6.8Average Stack Temperature (C) = 86

Dry Molecular Weight= 30.12^Wet Molecular Weight= 23.28


Pitot Coefficient= 0.82Sampling Time (Minutes) = 204.0Nozzle Diameter (mm)= 6.50Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters) = 2.627

Stack Velocity (Actual, m/min)= • 643Flow rate (Actual, Cubic m/min)= 1,690Flow rate (Standard, Wet, Cubic m/min)= 1,365Flow rate (Standard, Dry, Cubic m/min)= 595

A R 3 1 5 1 2 QAPPENDIX D 63

FILE NAME - 28CR7 PROG.=VER 06/27/89RUN # - 7 - BIF Method Train for Hexavalent Chromium 02-17-1997 16:31:01LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/09/97 Time: 1045-1227/1255-1437PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Kaven, PA

Point # Delta P Delta H Stack T Meter T . .(in. H20) (in. H20) (F) In(F) Out(F)

1 0.260 0.21 187 69 682 0.270 0.22 187 68 673 0 .270 0.23 .. 186 69 674 0.250 0.21 187 72 69 , . .5 ' 0.250 0.22 186 73 706 0.230 0.20 186 75 727 0.270 0.22 187 77 738 ' i 0.270 0.22 187 78 759 0.290 0.25 186 ^80 76 . . ' '10 0.290 0.24 187 81 78 .1 1 0.270 0.24 1 8 6 8 1 7 8 ' . ,1 2 0.280 0.25 -186 8 2 - 8 0 ,13 0.270 0.22 187 80 7914 0.260 0.21 187 80 7915 0.270 0.24 186 80 78 -16 .. 0.290 0.24 187 81 7917 0.290 0.23 ' 187 82 8018 0.290 0.24 187. 83 8119 0.270 0.22 187 84 8120 0.250 „ 0.19 188 85 8221 . . . 0.250 0.21 187 85 8322 0.240 0.20 187 86 84 . ' '23 .0.260 0.19 188 87 ' 8524 0.260 0.20 188 87 86 ...

• Multiple leak checks used. Final readings for each segment are listed below

Lk Rate (cfm) Time (min)0.0010 102.0000 -0.0020 102.0000 .. . . .

A R 3 I 5 I 2 IAPPENDIX D 64

FILE NAME - 28SV7X PROG.=VER 06/27/89RUN # -7 - Method 0010 Train for Semivolatile Organic Compounds -- SUMMARY USING VELOCITY HEAD DATA FROM THE PCB TRAIN 02-17-1997 16:31:22LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/09/97 Time: 1045-1227/1255-1437PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 105.591Final Meter Volume (Cubic Feet)= 223.550Meter Factor= - - 0.995Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 117.369Gas Volume (Dry Standard Cubic Feet)= 114.348


Percent Oxygen= 11.2Percent Carbon Dioxide= 10.5Moisture Collected (ml)=- 3134.3Percent Water= 56.4


Dry Molecular. Weight*= 30.13Wet Molecular Weight= 23.29 ' •

Average Square Root of Delta P (in H20)= 0.5114% Isokinetic= - 101.1



R R 3 I 5 I 2 2APPENDIX D 65

* * METRIC UNITS * * ' . . . . _FILE NAME - 28SV7X PROG.=VER 06/27/89RUN # -7 - Method 0010 Train for Semivolatile Organic Compounds -- SUMMARY USING VELOCITY HEAD DATA FROM THE PCB TRAIN 02-17-1997 16:31:25LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/09/97 Time: 1045-1227/1255-1437PROJECT # - , - ' . ".' : ""3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA .


Barometric Pressure (mm Hg)= . 753Static Pressure (mm H20) = -10

Percent Oxygen. = r. 11.2 - .Percent Carbon Dioxide= -10.5Moisture Collected (ml)= 3134.3Percent Water= 56.4 , .

Average Meter Temperature (C)= 26 ' .Average Delta H (mm H2.0) = • 29.2Average Delta P (mm H20)= -. 6.6 .Average Stack Temperature (C)=. 85

Dry Molecular Weight= 30.13 .Wet Molecular Weight =. 23.29 ~

Average Square Root of Delta P (mm H20)= 2.5772% Isokinetic= • 101.1

Pitot Coefficient= 0.82Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= 2.627


A R 3 I 5 1 2 3APPENDIX D

FILE NAME - 28SV7X PROG.=VER 06/27/89RUN # -7 - Method 0010 Train for Semivolatile Organic Compounds -- SUMMARY USING VELOCITY HEAD DATA FROM THE PCS TRAIN 02-17-1997 16:31:27LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/09/97 Time: 1045-1227/1255-1437PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA


1 0.240 1.20 183" 64 642 0.260 1.30 184 65 . 643 0.260 1.30 184 69 654 0.260 1.30 184 74 675 0.260 1.20 184 77 696 0.250 1.00 184 80 717 0.260 1.10 185 81 738 0.250 1.20 184 83 759 0.260 1.30 184 84 7610 0.260 1.20 185 85 7611 0.270 1.20 184 86 7712 0.240 1.20 184 86 7813 0.280 1.00 184 77 7714 0.280 1.10 184 77 76 '15 0.290 1.20 184 81 7616 0.290 1.20 185 84 7717 0.260 1.20 184 85 7818 0.270 1.10 185 86 78.19 0.260 1.00 184 87 8020 0.260 1.00 185 88 81 .21 0.260 1.10 185 88 8122 0.270 1.10 185 89 8223 0.250 1.10 185 89 8224 0.240 1.00 185 90 84


Lk Rate (cfm) Time (rain)0.0020 102.00000.0000 102.0000

APPENDIX D 67

FILE NAME - 28SV7 ' PROG.=VER 06/27/89RUN # - 7 - Method 0010 Train for Semlvolatile Organic Compounds

02-17-1997 16:31:47LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/09/97 Time: 1045-1227/1255-143.7PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 105.591 , ," '•Final Meter Volume (Cubic Feet)= 223.550Meter Factor= . 0.995Multiple leak checks, see end of printout . Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 117.369Gas Volume (Dry Standard Cubic Feet)= 114.348


Percent Oxygen= " " . . . . . 11.2 •Percent Carbon Dioxide= 10.5 . .Moisture Collected (ml)= 3134.3Percent Water= . " . -----' ; 56.4

Average Meter Temperature (F) = 78Average Delta H (in H20)= 1.15Average Delta P (in H20)= .0.272Average -Stack Temperature (F) = 184

Dry Molecular Weight= - 30.13Wet Molecular Weight= .23.29 :

Average Square Root of Delta P (in H20)= 0.5207% Isokinetic= • . 99.3

Pitot Coefficient= '0.82 ..Sampling Time (Minutes)= . 204.0Nozzle Diameter ..(Inches) = -0.371Stack Axis #1 (Inches)= 72.0Stack Axis #2 (Inches)= 72.0Circular StackStack Area (Square Feet)= 28.27


A R 3 I 5 I 2 5APPENDIX D

* * METRIC UNITS * *FILE NAME - 28SV7 PROG.=VER 06/27/89RUN # - 7 - Method 0010 Train for Semivolatile Organic Compounds


Initial Meter Volume (Cubic Meters)= 2.990Final Meter Volume (Cubic Meters)= 6.330Meter Factor= 0.995Multiple leak checks, se'e end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Meters)= 3.323Gas Volume (Dry Standard Cubic Meters)= 3.238




Dry Molecular Weight= 30.13Wet Molecular Weight= ' 23.29

Average Square Root of Delta P (mm H20)= 2.6245% Isokinetic= - - - - - - 99.3

Pitot Coefficient= .0.82Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= . 2.627


A R 3 1 5 1 2 6APPENDIX D 69

FILE NAME - 28SV7 ' PROG.=VER 06/27/89RUN # - 7<- Method 0010 Train for Semivolatile Organic Compounds



1 0.260 1.20 183 64 642 0.310 . 1.30 184 65 643 0.310 1.30 184 69 .654 0.300 1.30 184 74 675 0.280 1.20 184 77 69 .6 0.240 , 1.00 184 80 717 0.270 1.10 185 81 73

. 8 0.280 1.20 184 83 759 0.300 1.30 184 ' 84 7610 - 0.300- 1.20 185 85 7611 0.280 1.20 . 184 86 7712 0.270 1.20 . 184. 86. 78

. 13 . 0.230 1.00 184 77 7714 0.260 1.10 184 77 ' 7615 0.270 1.20 184 81 76 . ___.16 0.290 1.20 185 . . 84 7717 0.270 1.20 184 85 78 : . •18 • 0.270 , 1.10 185' . 8 6 . 7 819 0.220 1.00 184 87 8020 0.250 1.00 185 8 8 - 8 121 0.270 1.10 185 .88 81 .22 0.270 1.10 185 89 8223 0.270 1.10 185 89 8224 6.250 1.00 185 90 . 84



R R 3 I 5 I 2 7APPENDIX D 7O

FILE NAME - 28DF7 PROG.=VER 06/27/89RUN # - 7 - Method 23 Train for PCDDs/PCDFs 02-17-1997 16:32:07LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/09/97 Time: 1045-1227/1255-1437PROJECT # - -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 732.500Final Meter Volume (Cubic Feet)= 859.111Meter Factor= 0.985 - ,.Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 124.712Gas Volume (Dry Standard Cubic Feet)= 121.869


Percent Oxygen= , 11.3Percent Carbon Dioxide= 10..4Moisture Collected (ml)= 3371.2Percent Water= .- 56.6

Average Meter Temperature (F)= 77Average Delta H (in H20)= 1.35Average Delta P (in H20)= 0.295Average Stack Temperature (F) = - 184


Average Square Root of Delta P (in H20)= 0.5434% Isokinetic= - .100.1

Pitot Coefficient= 0.84Sampling Time (Minutes)= 204.0Nozzle Diameter (Inches)= 0.371Stack Axis #1 (Inches)= 72.0Stack Axis #2 (Inches)= 72.0Circular StackStack Area (Square Feet)= 28.27 .

Stack Velocity (Actual, Feet/min)= 2,256Flow Rate (Actual, Cubic ft/min)= 63,784Flow rate (Standard, Wet, Cubic ft/min) = 51,740Flow Rate (Standard, Dry, Cubic ft/min)= 22,467


* * METRIC UNITS * *FILE NAME - 28DF7 ' . PROG.=VER 06/27/89RUN # - 7 - Method 23 Train for PCDDs/PCDFs 02-17-1997 16:32:10LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/09/97 Time: 1045-1227/1255-1437PROJECT # -3620.28.30 OHM'Remediation Services Corp., Drake Chemical Superfund Site, Lock faven, PA

Initial Meter Volume (Cubic'Meters)= 20.741Final Meter Volume (Cubic Meters)= 24.327Meter Factor= 0.985Multiple leak checks, see end of printout . Leak Correction= -0.0000Net Meter Volume (Cubic Meters)= 3.531Gas Volume (Dry Standard Cubic" Meters) = 3.451 .

Barometric Pressure (mm Hg)= 753Static Pressure (mm H20) = -10

Percent Oxygen= . 11.3 . ,Percent Carbon Dioxide= : 10.4Moisture Collected (ml)= ' 3371.2Percent Water= . ' 56.6

Average Meter Temperature (C)= 25Average Delta H (mm H20)= 34.2Average Delta P (mm H20) = 7.5Average Stack Temperature (C)= 85


Average Square Root of Delta P (mm H20)= 2.7386% Isokinetic= ' . 100.1

Pitot. Coefficient= • • '0.84Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters) = 2.. 627

Stack Velocity (Actual, m/min)= 688Flow rate (Actual, Cubic m/min) = ,1,806Flow rate (Standard, Wet, Cubic m/min)= , 1,465 . .Flow rate (Standard, Dry, Cubic m/min)= 636


FILE NAME - 28DF7 PROG.=VER 06/27/89RUN # - 7 - Method 23 Train for PCDDs/PCDFs 02-17-1997 16:32:12LOCATION - Mobile Hazardous Waste Incinerator Stack - Upper LevelDATE - 02/09/97 Time: 1045-1227/1255-1437PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Point # Delta P Delta H .Stack T Meter T(in. H20) (in. H20) (F) In(F) Out(F)

1 0.290 1.30 184 67 662 0.300 1.40 183 67 663 0.290 ' 1.40 183 70 67 , f4 0.280 1.30 184 75 695 0.280 1.30 184 77 716 0.280 1.30 184 78 727 0.290 1.35 184 • 79 738 0.310 1.40 184 80 739 0.310 1.40 184 - - 81 7410 0.290 1.25 185 81 7511 0.270 1.25 184 .82 7612 0.270 1.25 18*4 82 7613 0.290 1.30 184 75 7414 0.310 1.35 185 76 7415 0.300 1.35 184 79 7416 0.320 1.40 185 81 7517 0.310 1.45 184 82 7618 0.300 1.40 184 82 7619 0.300 1.40 184 84 7720 0.300 1.30 185 85 7821 0.310 1.45 184 86 7922 0.300 1.30 185 86 7923 0.300 1.40 184 86 8024 0.290 1.30 185 87 80



A R 3 1 5 1 3 0APPENDIX D 73

FILE NAME - 28PCB7 . ' PROG.=VER 06/27/89RUN # - 1 - Method 23 Train for PCBs . 02-17-1997 16:32:26LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE' - 02/09/97 Time: 1045-1227/1255-1437PROJECT # - - -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA

Initial Meter Volume (Cubic Feet)= 868.087Final Meter Volume (Cubic Feet)= 991.190Meter Factor= . . . . . • . . 0.977Multiple leak checks, see end of printout Leak Correction= 0.0000Net Meter Volume (Cubic Feet)= 120.272Gas Volume (Dry Standard Cubic Feet)= 116.987

Barometric Pressure (in Hg)= 29.65 • . -.Static Pressure (Inches H20)= -0.41 .

Percent Oxygen= . 11.3Percent Carbon Dioxide= . 10.4Moisture Collected (ml)= 3218.2Percent Water= .. 54.8 **Saturated Stack**

Average Meter Temperature (F) = . 79Average Delta H (in H20)= 1.23Average Delta P (i,n H20)=- - - 0.262Average Stack Temperature (F)= 183

Dry Molecular Weight= 30.12 . .Wet Molecular Weight= ,23.48


Pitot Coefficient= " 0.82Sampling' Time (Minutes)= 204.0Nozzle Diameter (Inches)= 0.371Stack Axis #1 (Inches)= 72.0Stack Axis #2 (Inches)= ' 7 2 . 0Circular StackStack Area (Square Feet)= 28.27

Stack Velocity (Actual, Feet/min)= 2,075Flow Rate (Actual, Cubic ft/min)= 58,666Flow rate (Standard, Wet, Cubic ft/min)= 47,715'Flow Rate (Standard, Dry, Cubic ft/min)= 21,585

'. A R 3 I 5 I 3 IAPPENDIX D 74

* * METRIC UNITS * *FILE NAME - 28PCB7 . PROG.=VER 06/27/89RUN # - 7 - Method 23 Train for PCBs 02-17-1997 16:32:29LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/09/97 Time: 1045-1227/1255-1437PROJECT # -3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock Haven, PA



Percent Oxygen= 11.3Percent Carbon Dioxide= 10.4Moisture Collected (ml)= ' 3218.2Percent Water= -------- ' 54.8 **Saturated Stack**

Average Meter Temperature (C)= 26Average Delta H (mm H20)= 31.3Average Delta P (mm H20)= 6.6Average Stack Temperature (C) = 84

Dry Molecular Weight= 30.12Wet Molecular Weight? 23.48

Average Square Root of Delta P (mm H20) = 2.5772% Isokinetic= 100.1

Pitot Coefficient= 0.82Sampling Time (Minutes)= 204.0Nozzle Diameter (mm)= 9.42Stack Axis #1 (Meters)= ' 1.829Stack Axis #2 (Meters)= 1.829Circular StackStack Area (Square Meters)= . 2.627

Stack Velocity (Actual, m/min)= 632Flow rate (Actual, Cubic m/min)= 1,661Flow rate (Standard, Wet', Cubic m/min) = 1,351Flow rate (Standard, Dry, Cubic m/min)= 611


FILE NAME - 28PCB7 PROG.=VER 06/27/89 "~RUN # - 7 - Method 23 Train for PCBs ' 02-17-1997 16:32:31LOCATION - Mobile Hazardous Waste Incinerator Stack - Lower LevelDATE - 02/09/97 Time: 1045-1227/1255-1437PROJECT # - .3620.28.30 OHM Remediation Services Corp., Drake Chemical Superfund Site, Lock H~aven, PA

Point # Delta P Delta H Stack T Meter T. . . -(in. H20) (in. H20) (F) In(F) Out(F)

1 0.240 1.13 182 64 642 0.260 . 1.23 182 65 64 . -3 0.260 1.23 182 68 654 0.260 1.24 182 72 675 . 0.260 1.25 . 182 75 696 0.250' 1.15 183 78 717 0.260 1.20 183 80 73 " •8 0.250 - 1.21 182 82 759 0.260 1.21 " 183 84 7710 . 0..260 1.21 183 85 79 .

-11 0.270 1.26 183 86 80 . . _12 - 0.240 1.12 ' -183 87 8113 0.280 1.36 182 '79 7914 -- 0.280 1.30 183 80 .7915 - 0.290 1.35 " 183 83 7916 0.290 1.35 183 85 8017 0.260 1.27 182 - 87 80 .18 0.270 1.26 183 87 81 ' ' : " ""19 0.260 1.22 183 88 82 .20 ' . 0.260. 1.16 184 ,89 - 8221 0.260 1.28 182 89 8.3 , ' " -22 0.270 1.27 183 90 8423 . 0..250 1.18 183 91 8524 - 0.240 1.13 183 91 85



A R 3 I 5 1 3 3 'APPENDIX D 76

Appendix E

Calibration Data for Sampling Equipment

Note: All calibration data is presented in Appendix E ofRisk Burn No. 1 Report.


Appendix F

Report on Chemical AnalysisResults for Semivolatile Organics

MRI-Appfed/R3 62028. APP

RR3I5I35

Appendix F: Risk Burn 2 Report on Chemical Analysis Results for SemivolatileOrganics including Pesticides in Stack and Ash Samplesby Greg Jungclaus, Principal Chemist

The Risk: Burn 2 samples that were analyzed for semivolatile organics included the combinedMM5-SV sampling train components; bottom ash; fly ash; and waste feed samples. The combinedMM5-SV train extracts were analyzed for a target list of semivolatile and pesticide analytes, while thebottom ash and fly ash were analyzed for a similar target list of semivolatile analytes, and the wastefeeds were analyzed for a smaller list of target compounds,

The stack samples were analyzed by normal sensitivity and by high sensitivity full scan GC/MSanalyses in order to meet the low target practical quantitation limits (PQLs) for these compoundsrequired by the client. In addition the bottom ash and fly ash samples were analyzed by normalsensitivity GC/MS analysis, and by high sensitivity GC/MS.

The full scan GC/MS analysis data for the MM5-SV samples were also used to tentatively identifyand semi-quantify the 20 largest peaks in each sample, i.e., the TICs (tentatively identifiedcompounds).

1.0 Sample Receipt

Risk Burn No. 2 samples were received at MRI on February 11, 1997, at 6:30 pm. All sampleswere received cold and intact. The samples were stored in a cold room at about 4 deg C until theywere relinquished to the sample preparation chemists.

Each of the components of the MM5 train samples were weighed prior to opening the samplecontainer and recovering the samples. The sample weights were recorded on the Sample ConditionForm that accompanied the samples. The weights were found to agree with the original weightsrecorded in the field indicating that none of the samples were lost during transport due to leakage etc.

2.0 Sample Preparation

2.1 Stack Samples

The stack samples were prepared according to Method 0010 from SW-846. The filter/XAD,condensate, front half/back half rinse samples were extracted separately and the extracts combinedprior to analysis. The filter/XAD portion was spiked with the EPA Method 8270 surrogatecompounds prior to extraction. The spike levels were 50 ug for the base/neutral surrogates and 75 ugfor the acidic surrogates.

The surrogate compounds spiked onto the filter/XAD portion of the stack samples are listed inTable F-l.

R£R\r3«20-28.apf

A R 3 I 5 I 3 6APPENDIX F

The filter/XAD combination was extracted with methylene chloride in a Soxhlet extractor for 18hours. Each condensate water and front half/back half rinse sample was extracted with methylenechloride in a separately fimnel. The entire amount of condensate and front half/back half rinse samplewere used for these analyses. The volumes are recorded elsewhere in the report. The condensatesamples were extracted with three separate aliquots of methylene chloride, first at an acidic pH andthen at a basic pH to enhance extraction efficiency of the more water-soluble basic and acidiccompounds. The extracts from the acidic and basic extractions for each sample were combined priorto final concentration.

In order to enhance extraction efficiency, the front half/back half rinse samples were diluted withorganic-free water until the methylene chloride formed a distinct layer in the separatory funnel. Therinses were also extracted under acidic and basic conditions with three separate aliquots of methylenechloride and the extracts combined.

The combined extracts from each sample were concentrated using a combination of Kuderna-Danish evaporation and gentle nitrogen blowdown to a final volume of 1.0 mL.

QC samples were analyzed along with the stack samples. The QC samples included a field trainblank which included all the components of the stack samples. In addition a XAD laboratory controlspike (LCS) was spiked with 25 ug of all the target SVOC compounds and prepared and analyzed inthe same manner as the samples to determine the recovery efficiency of the compounds.

2.2 Ash and Waste Feed Samples

The ash and waste feed samples were extracted in a Soxhlet extractor according to Method 5040from SW-846. The sample size was 30 g for the fly ash, 15 g for the bottom ash, and 5 g for thewaste feeds. The weighed portion of each sample was first placed in a 250-mL beaker and mixedwith enough anhydrous sodium sulfate to yield a granular mixture. The dried samples weretransferred to the Soxhlet extractor and spiked with 100 ug of each of the base/neutral Method 8270surrogates and 150 ug of each of the acidic Method 8270 surrogates. The samples were thenextracted for 16 hours with a 350-mL charge of methylene chloride.

The extracts were dried by passing them through a filter funnel containing anhydrous sodiumsulfate and then transferred into a K-D apparatus. After concentration to a volume of about 5 mL,the extracts were filtered through a 0.45-um filter and adjusted to a volume of 10 mL. The sampleextracts were then subjected to gel permeation cleanup (GPC) cleanup. The color of some of theextracts was so dark that they were diluted and/or split into fractions before loading onto the GPC soas to not overload the GPC column. The amount of the dilution or split was based on previousexperience with these samples from the mini-burn and Risk Burn 1 samples that had been analyzedpreviously.

One half of the original amount of extract injected into the GPC was recovered for chemicalanalysis, i.e., the dilution factor was two for the analyses. The cleaned up extracts were concentratedto a final volume of 1.0 mL and submitted for GC/MS analysis.

RER.U3620-28.jpf

R R 3 I 5 I 3 7APPENDIX F

QC samples were analyzed with the solid samples. The QC samples included a sand method blank,a duplicate of one of the bottom ashes from Run 5 (5237); a duplicate of one of the fly ashes fromRun 5 (5242); a duplicate of one of the waste feeds from Run 5 (5248); a matrix spike and matrixspike duplicate of one of the bottom ashes from Run 5 (5237); a MS/MSD of one of the fly ashesfrom Run 5 (5242); and a MS/MSD of one of the waste feeds from Run 5 (5248).

Samples of the waste feed, bottom ash, and flyash were also sent to Environmental Chemical Corp.(ECC) for analysis of p-Naphthylamine. Those results are included in the Risk Burn No. 2 report(Section 3.10).

3.0 Sample Analysis

The extracts from both the stack samples and ash samples were treated in a special manner in theMass Spectrometry Facility in order to meet the very low detection limit requirements. Upon receiptin the Mass Spectrometry Facility, the 1.0-mL extracts were split. One 500-uL portion was spiked atthe 20-ug/mL level with the Method 8270 internal standards (normal level). The other 500-uLportion was spiked with the same internal standards at the 2.0-ug/mL level (high sensitivity level).

3.1 Calibration Criteria

The first set of extracts were analyzed against a calibration curve with the calibration range of 5.0-80 ug/mL. The initial calibration criteria were that the Method 8270 Calibration Check Compounds(CCCs) yielded <20 percent relative standard deviation (RSD) of the CCCs over the calibration rangeand that the absolute response factors of the System Performance Check Compounds (SPCCs) be atleast 0.05. These criteria were met.

The continuing calibration criteria were that the CCCs yield GC/MS response factors with relativepercent differences (RPDs) of less than 20% from the average of the initial calibration curve and thatthe area counts be within the range of 0.5-2.0 of the average from the initial calibration. Thesecriteria were also met.

Subsequently the extracts were analyzed against a calibration curve that ranged from 0.25-5.0ug/mL. In addition the extracts were analyzed relative to a separate pesticide calibration curve thatranged in concentration from 0.5-10 ug/mL. The calibration criterion that was used for the pesticideanalyses was that the %RSD of the response factors over the calibration range be less than 20%which is the criterion for SVOC analytes in SW-846 Method 8270. This criterion was met.

3.2 GC/MS Analysis Parameters

The GC/MS analysis parameters are listed in Table F-2.

RER\r3«20-28.apf

A R 3 I 5 I 3 8APPENDIX F

4.0 Sample Results

4.1 Stack Samples

4.1.1 Target compounds

Table F-3 lists all the target compounds along with the total ug amounts of each compounddetected in each of the three runs. Both the normal sensitivity and high sensitivity data are shown inthe table. The table also presents the surrogate recoveries for each sample. The surrogate recoverieswill be discussed in Section 5.0 of this appendix.

Very few target compounds were detected in the stack samples that were not detected in the blanktrain sample. The high sensitivity analyses provided a few additional hits for compounds not detectedduring the initial, normal sensitivity analyses.

Table F-4 shows the pesticide analysis results for the same stack sample extracts analyzedseparately along with a pesticide calibration curve. None of the chlorinated pesticides were detectedin the samples.

4.1.2 Non-target Tentatively Identified Compounds (TICs)

Tables F-5 to F-8 summarize the total amounts of the 20 largest TIC compounds in the TrainBlank, Run 5, Run 6, and Run 7, respectively. A large number of compounds were seen, but most ofthe compounds appeared in the Blank Trahi as well as in the stack samples. These data show that thestack gas contained only low levels of a few semivolatile organic contaminants. One compound ofnote is iodobenzene which appeared at consistent levels in all three runs. The source of the iodine isnot known.

4.2 Waste Feed, Bottom Ash, and Fly Ash Samples

The waste feeds were analyzed for a target list of 16 compounds while the bottom ash and fly ashsamples were analyzed for a much larger list of target compounds. Table F-9 summarizes the targetSVOC data in the waste feed samples. There were some hits for chlorinated benzenes and forpolycyclic aromatic hydrocarbon (PAH) compounds. Most of the amounts were between the methoddetection limit (MDL) and the practical quantitation limit (PQL).

Table F-10 shows the analysis results for the much larger list of target compounds analyzed in thebottom ash and fly ash samples. The only compound detected was benzoic acid in the bottom ash.

R£RW«0.2S.«pf

flR3i5!39APPENDIX F

5.0 QC Results and Data Quality Assessment

5.1 Holding Times

Holding times were met for the MRI analyses of the stack gas, waste feed, bottom ash and fly ashsamples. The samples were all extracted within 14 days of collection and the extracts analyzed within30 days of extraction. The condensates were extracted on February 20,1997. The front half and backhalf rinses were extracted on February 20, 1997. The XAD/filter samples were extracted on February18, 1997. The ash samples were extracted on February 17, 1997.

5.2 Background Levels of Analytes

A sampling train blank was analyzed to measure the background levels of analytes that may haveoriginated in the solvents, reagents, glassware, workplace atmosphere, or from contact of the samplesor extracts with gloves or other contaminated surface. The blank train sample results indicated that afew of the target compounds were present. The most abundant compounds were phenol,naphthalene, benzoic acid, dibutyl phthalate, and bis(2-ethylhexyl)phthalate. Eight (8) other targetcompounds were detected in the train blank with amounts less than 1 ug.

The train blank did contain a significant amount of the non-target TIC compounds and the levels inthe train blank were about the same as in the samples. Most of the TIC compounds werehydrocarbons and oxygenated compounds like fatty acids and fatty acid methyl esters. The source ofthe compounds is not known, but they are frequently seen in trial burn blank train samples.

A sand blank was analyzed as the method blank for the waste feed, bottom ash, and fly ashsamples. No reportable level of background contamination was detected in the sand method blankassociated with the solid samples.

/

5.3 Total Method Accuracy

The method accuracy is measured by the recovery of surrogate compounds spiked into eachsample prior to extraction and by recovery of the target compounds spiked onto neutral matrices(laboratory control spike samples) and into field samples (matrix spike samples).

Different data quality objectives (DQOs) were established for the stack samples (combinedXAD/filter, condensates, and rinses) and for the waste feed and ash samples. The stack sample DQOfor the recovery of target analytes spiked into LCS samples was 50-1.50% and likewise the DQO forrecovery of the surrogate compounds spiked into the stack samples prior to extraction was 50-150%recovery in both the field samples and the LCS spike samples.

The waste feed and ash sample DQO for recovery of both the surrogate compounds and the targetcompounds spiked into ash samples (matrix spike/matrix spike duplicates) was 30-130%.

A R 3 I 5 U OAPPENDIX F

5.3.1 Stack Samples

The recovery (accuracy) data for the surrogate compounds was presented on each of the resultstables. For the stack samples, all individual surrogate recovery values met the 50-150% recoveryobjective as shown in Table F-l 1. Note that the surrogates are spiked onto only the XAD/filterportion of the stack samples prior to extraction and combination of the extracts.

A XAD LCS was spiked with 25 ug of all the target analytes to determine the percent recovery.The recoveries are presented in Table F-l 2. Of the compounds spiked, 54 met the DQO of 50-150%recovery and 5 did not meet the DQO. The compounds for which the recovery DQO was not metincluded beta-naphthylamine (36%), pentachlorophenol (41%), 2,4-dinitrophenol (14%), 3,3'-dichlorobenzidine (33%), and hexachlorocyclopentadiene (29%). Most of these compounds are polaracidic or basic compounds that typically yield lower recoveries than the neutral compounds.

The beta-naphthylamine was spiked into a separate LCS sample from the other compounds due toits known degradation by the other compounds as experienced with the Risk Burn 1 samples.

Table F-13 shows the LCS recoveries for a 5-ug spike of the target chlorinated pesticides alongwith the surrogate recovery compounds. All of the chlorinated pesticide recoveries met the 50-150%objective.

5.3.2 Waste Feed, Bottom Ash and Fly Ash Samples

For the ash samples, all the surrogate recoveries met not only the 30-130% DQO but would alsohave met the 50-150% DQO for the stack samples. These surrogate recoveries indicate the samplepreparation and analyses procedures were in control.

Table F-14 shows the matrix spike/matrix spike duplicate spike recoveries for the targetcompounds in the waste feed, bottom ash, and fly ash samples. Except for a measured recovery of27% for benzoic acid in.the MSD sample, the waste feed matrix spike and matrix spike duplicate(MS/MSD) samples met the objective for recovery of the 16 spiked compounds including beta-naphthylamine.

A total of 4 compounds did not meet the recovery objective of 30-130% for the larger list of targetanalytes spiked into the bottom ash and fly ash samples. The compounds that did not meet theobjective included benzyl alcohol (5-6% in bottom ash and in flyash), 2,4-dimethyl phenol (29% inone bottom ash spike), benzoic acid (5% in one bottom ash spike and 16-17% in the flyash), andhexachlorocyclopentadiene (16-18% in the bottom ash).

5.4 Total Method Precision

The reproducibility of the chemical analyses methods is measurable from the percent relativestandard deviation (%RSD) of the surrogate recoveries for a given set of samples and the relativepercent difference (RPD) of the MS and MSD recoveries for each compound.1 The DQO forprecision was <50% RSD for the pooled recoveries of the surrogates in the stack samples and ash

RERW«0-28.»pf

A R 3 I 5 UAPPENDIX F

samples and <35 RPD for the MS and MSD recoveries of target compounds from spiked ashsamples. The actual recoveries achieved are discussed below.

5.4.1 Stack Samples

There were no duplicate values for the stack samples, but the %RSD of the surrogate recoverieswas calculated for the combined stack samples. Table F-15 shows the %RSD for the surrogaterecoveries for the stack gas samples. The data are for four samples, the Train Blank and the samplesfrom Runs 5-7.

5.4.2 Waste Feed, Bottom Ash, and Fly Ash Samples

Table F-16 shows the precision as %RSD of the surrogate recoveries from the waste feed, bottomash, and fly ash samples. The precision vales are based on four (4) values, duplicates from Run 5 andsingle values from Run 6 and Run 7. All %RSD values were less than the 35 objective and all %RSDvalues were 12 or less.

Table F-14 also shows the precision of the MS and MSD recoveries of the target compoundsspiked into the waste feed, bottom ash and fly ash samples as the RPD value for each compound.The data show that the recoveries were quite precise. Only the precision for the benzoic acid in thebottom ash (RPD 184) did not meet the precision objective.

R£R\r3«20-28.apf

&R3I5U2APPENDIX F

Table F-l. Semivolatile Surrogate Compounds

Surrogate Compound

2-Fluorophenol

D5-Phenol

D4-2-Chlorophenol

D4- 1 ,2-Dichlorobenzene

D5-Nitrobenzene

2-Fluorobiphenyl

Tribromophenol

D14-Terphenyl

Spike Level

75 ug/sample

75 ug/sample

75 ug/sample50 ug/sample

50 ug/sample

50 ug/sample

75 ug/sample

50 ug/sample

Type

Acidic

Acidic

Acidic

Neutral

Neutral

Neutral

Acidic

Neutral

Table F-2. GC/MS Analysis Parameters

Parameters

Scan range

Calibration range

GC column

Linear velocity

Scan speed

Column temperature program

Injection volume

Settings |

35-550 amu [

5.0-80 ug/mL and 0.25-5.0 ug/mL

30-m x 0.32-mm ID DB-5 with 1-um film thickness

30 cm/sec helium

100 scans/min

40 deg C for 4 min, then 10 deg C/min to 300 deg C andhold21min

2.0 uL (splitless) |

RER\rM20-28.apf

AR3I5U3APPENDIX F 3

»J

,j*C/3

O2

W"S13sCUrsctfO

1(73

g2*

fo

JU

H

îtr

COcC£

mCC?

CTa.co 3 => =333=1303233 3 ^ 3 3 3 3 3 3 O 3 Z)

ca mto CM o5 ^ "

m-> -> CQ -j -j CQr co oo T— p— (o

3Îj_j_j_jQC,'_j_3:.j _J OID ÔoID^Ô^QÔ ^3 QZ3H)^^DI3r3IDOID

CO COco co en°H <° inf ^ to

_. m m-s -> CQ -5 -a CQ -aOJ U5 CVJ 00 J>~ CO COh- ID r- co t . in CM

3 3 3 3 3 3 2 5 =>0 3 <N 3 33 3 £ 3 3 O 3 =1 O 3 3 3 £ 3 O g p 13 Z) Z> Z) 3

CQ CQOO O> 00T O) CO

«

~3 -O0 r- T- 0h* CO O) CN: co T- co

33333333333 3 3333°333333°"33 3 ^3333333313

CO CN

in 2

O O O O O O O O O O O O 0 O O O ' O O O O O O O O O O O O O O O O O O O O O O O O

CD C> O O O O O O C3 CD O O O O O O O O CD CD O CD O O O O CD O O O O O O O O O O CO O O

0}| 0)

a > c c ~ c S a j ( U " =; (D N c CD x: x; "51 S ^ co ?* oj N p* ca ^ g g f S S gE | Is -8 8- §• «i S g & s&i g § s o £ i Sf|°° I^^S^«<" 1 g g S 1 f i|lll.iu|.§2|li- Ie-i.£|fesn j Q . i ^ t ^ - ^ . Q Q ' U c c V a ) >, .-r=r=2c5o •o-S-^££ccii:"fQO>*^t<Droc?c o. 3 o 5 oi

8-as

A R 3 I 5 I U UAPPENDIX F

CA

"s

^13 S?.S —c e

^ op

§s

r*-cn:

COct§

IOc3te.

"55

cojj

13O

O)

c3

<

c *S>

c 3S e03 §

11§ Cf

5i S

°s

crLU5CO

c8CO

3

.ff5CO

13U_

s5CO

csw3u_

crLU5CO

c13LL.

CQ -> CQ CD —) -OO CQ *~ ^ CO CO O)° S iC c *""'"O ZJQiaZJZJDOQ^ OQ J^

CM r*- h- co^9 >> coto co ^ co

CD —5 CD CD —5 —3CO r*1" T~ O CO CNJO r- tO r- O) CO

O Z> d O 13 13 O O d *~ 3 o* d P

CDin cjj * O)OJ CNJ N. ^m in - co

CQCD CQ — j CQ CD — 5 — jSOJ CN O ^- CO tOm 01 o t— in mCNI3 CN^^^O^ZJ^CMCO ^^ 2^

in • S (Qm m co

-1 —3

^ P1— CO CO CO OJ O)h- co i- co co <o in°9 ^ tN T **! ° r-0-30 =30z3Z3=3Z3000OZ)Z» =3O

o o o o o o o o o o o o o o o o o o od o d d o o o o o d d d o o o o c l o d

1 1-3li ^ S

Htfffcfflfffilji.llf0:"-!?-tlct-IlctQlllxScl?^?!!--"

< O T - C O C O C N J C O O C O

•r-

^ C O r ^ - N - O O O O C O T —

P ^ - C O C O C O C O C O h - C M

C O ^ r - N - C O f ^ - O C ON - C O C O C O C O C O C O T ^

^1ou)§303"o§go> "°

I ' •<• g §1 1 llllls1 i|illlt|C/J CNQ,CNv-"ZCNCMK

*R&

AR3I5U5APPENDIX F 1O

101.22'S3

s

2'5en

i£

|^

^i^

H

"i ll<

"55CD ^c c

5 1"3

in -SC' "c

CH 0

c "Si2 3=i iJO 0

O O5

'" r1S •'SQ -=

^ D D D D D D D D

D D D D D 3 D I D D

I 3 I D D I D D D D D D

o o o o o o o o o000000000

1- •*" CM" --f •*" LU ui

-, -j -, -,

-j -^ — j -j

D D D D

O O O O

0000

0>croX0)

•o o"^ 2CD i_ S

.S .£ co 1i; i= -S £^O T3 LJ rC C 0> iLU HI I ca

O)_Dro

•J= CD

£ "3JS xi

"3 oJ2 <U IB- O) ££ O 2

•g<D T3!- 0)3 tsCO C

og-f s1 1 §O5 </) </JOJ « «

8 S S'CO -3

RER\r3620-28.apf

. A R 3 I 5 I U 6APPENDIX F 11

Table F-5. MM5-SemivoIatile Blank Train Analytes Associated withTwenty Largest Peaks Identifed in Sample Trains

RER\r3620.2S,»pf

ButoxyethoxyethanolBenzoic acidXylenes aEthyl benzaldehydeMethyl benzoateAlkane aBenzaldehydeUnknown aEthyl benzole acid aEthyl acetophenone aDecane + C3 benzeneAlkyl acetophenone abis(2-Ethylhexyl)phthalateEthyl methyl benzoateAcetophenoneDichlorocyclohexaneDimethyl cyclohexanePhenol

Total

TIC660

215684039272323221512

105.84.93.3

amount (u,g)

Z

zZzzzzzzzzzzzz

Targetanalyte

526

10.2

1.09

a This compound represents the sum of several similar compounds withunique mass spectra that cannot be otherwise identified using the massspectral library.

Z Indicates a compound that is only tentatively identified and semiquantitated.

AR3I5U7APPENDIX F 12

Table F-6. Twenty Largest Peaks Identifed in Run 5MM5-SemivolatiIe Train

Benzole acidButoxyethoxyethanolXylenes aBenzaldehydeEthyl benzaldehydeUnknown Alkane aUnknown aMethyl benzoatePhenolEthyl benzole acidDichlorocyclohexaneEthyl acetophenoneDecane + C3 benzeneBromobenzenelodobenzeneMethyl hexenoneHydroxymethyl pentanoneDimethyl cyclohexanebis(2-Ethylhexyl)phthaIateAcetophenone

Total

TIC

250 B243 B120 B120 B5754 B43 B

36 B25 B16 B15 B141211109.1 B

8.1 B

amount (jig)Targetanalyte599 B

36.4

8.38 B

a This compound represents the sum of several similar compounds with• unique mass spectra that cannot be otherwise identified using the mass

spectral library.

B Indicates that measured value is not greater than 5 times the blank value.Z Indicates a compound that is only tentatively identified and semiquantitated.

RER\r3«20-28,apf

AR3I5U8APPENDIX F

RERV3«20-28.«pf


Benzoic acidUnknown aAlkane aXylenes aBenzaldehydebis(2-Ethy!hexyl)phthalateEthyl benzaldehydePhenolMethyl benzoateDichlorocyclohexaneEthyl benzole acid aHydroxymethyl pentanoneMethyl hexenonelodobenzeneBromobenzeneAlkyl acetophenone'8Decane + C3 benzeneAcetophenoneBiphenylEthyl methyl benzoate

Total amount (|ig)

TIC

151 B99 B77 B54 B

34 B

31 B26 B23 B1111109.39 B

8.3 B6.3 B6.26.2 B

Targetanalyte438 B

35 B

32.9



AR3I5U9APPENDIX F 14

RER\l3«0-28.apf


B,enzoic acidEthyl benzaldehyde aXylenes aBenzaldehydeChlorinated unknownDichlorinated unknownAlkane aMethyl benzoateUnknown aPhenolEthyl benzoic acid aEthyl acetophenone abis(2-Ethylhexyl)phthalateAlkyl acetophenone aBromobenzeneC14H2002 Alkyl cyclohexadienedioneEthyl methyl benzoateDecane + C3 benzeneHydroxymethyl pentanonelodobenzene

Total amount (|j.g)

TIC

340 B111 B55 B424238 B37 B37 B

27 B18 B

12 B111111 B10 B1010

Targetanalyte

' 472 B

33.3

13.0 B



A R 3 I 5 1 5 0APPENDIX F 15

Table F-9. Semivolatile Results in Feed SamplesDetection limit

based on 1/5 loweststandard3

(ng/kg)1 ,2-Dichlorobenzene1 ,4-Dichlorobenzene1 ,2,4-TrichiorobenzeneBenzo(k)fluoranthene.Benzo(a)pyreneBenzoic acidNaphthalenePhenanthreneBenzo(a)anthraceneChrysenePhenolPentachlorophenolFluoranthenePyreneBenzo(b)fluoranthene

(3-Naphthylamine (by ECC)b

Surrogate Recoveries (%) - QA2-FluorophenolPhenol-d52-Chlorophenol-d41 ,2-Dichlorobenzene-d4Nitrobenzene-d5c2-Fluorobiphenyl°2,4,6-TribromophenolTerphenyl-d14°

1,0001,0001,0001,0001,0001,0001,0001,0001,0001,0001,0001,0001,0001,0001,000

(550) d

objective

Rep1UUUUUUUU

2,410UUU

1,8301,430U

(2,450)

(30-130%)5155575961(35)65(52)7073(126)

Feed (ng/kg)Run 5

Rep 21,360UUUU

1,090U

1,080J 3,240

UUU

J 1,750J 1,450

U

NA

6871747677798390

Run 6

J 1 ,200UUUU

J UU

J 1 ,280 JJ 2,700 J

UUU

J 1,550 JJ 1 ,250 J

U

(3,430)

6569717473(42)77(46)8289(123)

Run 7

1,570U

1,2801,1601,350UU

5,1303,8101,710UU

4,5503,8001,150

(4,040)

6570727375(44)77(60)8389(118)

J

JJJ

JJ

JJJ

1 Detection limit equal to 1/5th the lowest standard. This is based on the area counts for the lowest standard, which weresufficiently high to enable detection and estimated quantitation of compounds whose area counts are 1/5 as high asthose for the lowest standard.

b Samples of feed were sent to ECC by MRI, and were analyzed within the holding time of 14 days,c Surrogate recoveries shown in parenthesis are for ECC analysis of samples.d ECC detection limit for p-Napthylamine in feed samples.

U Indicates compound was analyzed for but not detected.J Indicates an estimated value; above the MDl but below the PQL.NA - Not analyzed

Note: A method blank was analyzed, but all analytes were non-detect.

RER\r3620-28.apf

A R 3 I 5 1 5APPENDIX F 16

Table F-10. Semivolatile Organic Compounds in Ash Samples

PhenolBis(2-chloroethyl) ether2-Chlorophenol1 ,3-Dichlorobenzene1 ,4-DichlorobenzeneBenzyl alcohol1 ,2-Dichlorobenzene2-MethylphenolBis(2-chloroisopropyl) ether4-Methylpheno!A/-Nitroso-di-n-propylamineHexachloroethaneNitrobenzeneIsophorone2-Nitrophenol2,4-DimethylphenolBenzole acidBis(2-chloroethoxy) methane2,4-Dichlorophenol1 ,2,4-TrichlorobenzeneNaphthalene4-ChloroanilineHexachlorobutadiene4-Chloro-3-methylphenol2-MethylnaphthaleneHexachlorocyclopentadiene2,4,6-Trichlorophenol2,4,5-Trichlorophenol2-Chloronaphthalene2-NitroanilineDimethyl phthalateAcenaphthylene3-NitroanilineAcenaphthene

DetectionLimit:

Based on1/5 loweststandard *(Ma/kg)BottomAsh/Flyash140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70

Bottom ash (pg/kg)

RunS

Rep. 1UUUUUUUUUUUUUUUU

2,060 JUUUUUUUUUUUUUUUUU

Rep. 2UUUUUUUUUUUUUUUU


(continued on

RunS

UUUUUUUUUUUUUUUU


next page)

Run 7 .

UUUUUUUUUUUUUUUU

250 JUUUUUUUUUUUUUUUUU

Fly ash (Mg/kg)

RunS

Rep. 1UUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUUU

Rep. 2UU 'UUUUUUUUUUUu •Uuuuuuuuuu

. uuuuuuu

• uuu

RunS

uuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuuu

Run 7

uuuuuuuuuuuuuuuu'uuU 'uuuuuu ,uuuuuuuuu

RER\r3620-28.apf

A R 3 I 5 1 5 2APPENDIX F

Table F-10 Continued(Semivolatile Organic Compounds in Ash Samples)

2,4-Dinitrophenol4-NitrophenolDibenzofuran2,4-Dinitrotoluene2,6-DinrtrotolueneDiethyl phthalate4-Chlorophenyl phenyl etherFluorene4-Nitroaniline4,6-Dinitro-2-methylphenolA/-N itrosodiphenylamine4-Bromophenyl phenyl etherHexachlorobenzenePentachlorophenolPhenanthreneAnthraceneDi-n-butyl phthalateFluoranthenePyreneButyl benzyl phthalate3,3'-DichlorobenzidineBenz[a]anthraceneBis(2-ethylhexyl) phthalateChryseneDi-n-octyl phthalateBenzo[6]fluorantheneBenzoffcjfluorantheneBenzo[a]pyreneIndeno[1 ,2,3-co]pyreneBenzo[g,/i,;]perylene

(5-Naphthylamine (by ECC)1"

Surrogate Recoveries2-FluorophenolPhenol-d52-chlorophenol-d41 ,2-Dichlorobenzene-d4Nitrobenzene-d5c2-Fluorobiphenyic2,4,6-Tribromopheno)Terphenyt-d14c

DetectionLimit

BottomAsh/Flyash140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70140/70

(16/9)

Bottom ash (ug/kg)

Run

Rep. 1UU

-. UUUUUUUUUUUUUUUUUUUUUUUUUUUU

(U)

5

Rep. 2UUUUUUUUUUUUUUUUUUUUUUUUUUUUUU

(NA)

RunS

UUUUUUUUUUUUUUUUUUUUUUUUUUUUUU

(U)

Run 7 .


(U)

Fly ash (ug/kg)

RunS


(U)


(NA)

Run 6


(U)

Run 7


(U)

(%)-QA Objective 30-130%.7683818686(62)86(68)8682 (94)

6771697377727273

6469687177 (83)72 (90)7669 (90)

6470687278(110)72 (71)7372(97)

6470697077 (82)72 (88)7276 (120)

6066646775707175

6672707378 (53)72 (71)7177(112)

6874737480(66)75 (81)7379(116)

a Detection limit equal to 1/5th the lowest standard. This is based on the area counts for the lowest standard, whichwere sufficiently high to enable detection and estimated quantitation of compounds whose area counts are 1/5th ashigh as those for the lowest standard.

b Samples were sent to ECC after receipt at MRI. Thus, the 14 day holding time was exceeded by 2-4 days.c Surrogate recoveries shown in parenthesis are for ECC analysis of samples.

U Indicates compound was analyzed for but not detected.J Indicates an estimated value, above the detection limit, but below the PQLNA Not analyzedNote: A method blank was analyzed, but all analytes were non-detect.

RERW«20-28.lpf

A R 3 I 5 I 5 3APPENDIX F IS

Table F-ll. Recovery and Precision Results for Combined MM5 Semivolattle TrainFilter/XAD

Surrogate Recoveries (%)

2-FluorophenolPhenol-d52-Chlorophenol~d41 ,2-Dichlorobenzene-d4Nitrobenzene^dS2-Fluorobiphenyl2,4,6-TribromophenolTerphenyl-d14

Blank Train

7384818786

87

80

113

Run 5

79838085

86

85

77

124

Run 6

7681777480

83

84113

Run 7

7681787882

8380118

Precision(RSD)

3

2

2

7

4

244

QA objectives: 50-150% surrogate recovery and 50% RSD for precision.

RERW«20-28.apf AR3I.5I5UAPPENDIX F

Table F-12. Matrix Spike Recoveries (XAD) for SVOCs

NAME

Benzo(a)anthraceneBenzo(a)pyreneBenzo(b)fluorantheneBenzo(k)fluorantheneChryseneDibenz(a,h)anthracene1 ,2-Dichlorobenzene1 ,4-DichlorobenzeneFluorantheneHexachlorobenzenelndeno(1 ,2,3-cd)pyreneNaphthalene

p-Naphthylamine

2-Nitroaniline4-NitroaniIineNitrobenzenePentachlorobenzenePentachlorophenolPyrene1 ,2,4-Trichlorobenzene2,4,5-Trichlorophenol2,4,6-TrichlorophenolAcenaphtheneAcenaphthyleneAnthraceneBenzo(e)pyreneBenzo(g,h,i)peryleneBenzoic acid

% Recovery(for 25 ug spike level)QA Objective 50-1 50%

929294899292767397899483

36a'b

8756809341 a997990839188861079269

a Recovery outside QA objective range of 50-150%.b Recovery result of 36% is for a separate matrix spike of p-Naphthylamine only.

HERVr3620.28.pf A R 3 I 5 I 55APPENDIX F 20

Table F-12 Continued(Matrix Spike Recoveries (XAD) for SVOCs)

NAME

bis(2-Chloroethoxy)methanebis(2-Ethylhexyl)phthalateButylbenzylphthalateCarbazole4-ChIoroaniline4-Chloro-3-methylphenol2-ChloronaphthaIene2-ChlorophenolDibenzofuran1,3-Dichlorobenzene3,3'-Dichlorobenzidine2,4-DichlorophenolDiethylphthalate2,4-DimethylphenolDimethylphthalateDi-n-butylphthalate2,4-DinitrophenolDi-n-octylphthalateFluoreneHexachlorobutadieneHexachlorocyclopentadieneHexachoroethane2-Methylnaphtha!ene2-Methylphenol4-Methylphenol2-Nitrophenol4-NitrophenolPhenanthrenePhenol1 ,2,4,5-Tetrachlorobenzene2,3,4,6-Tetrachlorophenol

% Recovery(for 25 ug spike level)QA Objective 50-1 50%

8497937571848676957433 a819561 ,929114a95897729 a74907675797287788278

3 Recovery outside QA objective range of 50-150%." Recovery result of 36% is for a separate matrix spike of p-Naphthylamine only.

RER\r3«20-28.apf

A R 3 I 5 1 5 6APPENDIX F

Table F-13. Matrix Spike Recoveries (XAD) for Pesticides and Surrogates

RERAr3«20-28.ipf

% Recovery(for 5 (ig spike level)

, QA Objective 50 - 1 50%Aldrina -Chlordaney -Chlordane4,4 -ODD2,4 -DDE4,4 -DDE4,4 -DOTEndosulfan IEndosulfan sulfateEndrinEndrin aldehydeHeptachlorP -Hexachlorocyclohexane

Surrogate Recoveries (%)2-FluorophenolPhenol-d52-Chlorophenol-d41 ,2-Dichlorobenzene-d4Nitrobenzene-d52-Fluorobiphenyl2,4,6-TribromophenolTerphenyl-d14

951111111011081129699961229796101

6876747584838787

A R 3 1 5 I 5 7APPENDIX F 22

Table F-14. Matrix Spike Recoveries and Precision for SVOCs in Bottom Ash and Flyash

RER.Wd20-28.apf

Feed' Bottom ash"% Recovery % Recovery

(QA Objective 30-1 30%) (QA Objective 30-1 30%)Precision Precision

MS MSD RPD MS MSD RPDPhenolBis(2-chloroethyl) ether2-Chlorophenol1 ,3-Dichlorobenzene1 ,4-DichlorobenzeneBenzyl alcohol1 ,2-Dichlorobenzene2-MethylphenolBis(2-chloroisopropyl) ether4-MethylphenolW-Nitroso-di-W-propylamineHexachloroethaneNitrobenzeneIsophorone2-Nitrophenol2,4-DimethyiphenolBenzole acidBis(2-chloroethoxy) methane2,4-Dichlorophenol1 ,2,4-TrichlorobenzeneNaphthalene4-ChloroanilineHexachlorobutadiene4-Chloro-3-methylphenol2-MethylnaphthaleneHexachlorocyclopentadiene2,4,6-Trichlorophenol2,4,5-Trichlorophenol2-Chloronaphthaiene2-NitroanilineDimethyl phthalateAcenaphthylene3-NitroanilineAcenaphthene2,4-Dinitrophenol4-NitrophenolDibenzofuran2,4-Dinitrotoluene2,6-DinitrotolueneDiethyl phthalate

79 63 23 85- 77- 75

- 7781 65 22 78_ 5"88 71 21 79- 65_ 80_ 63_ „ . _ y-j_ .. 76- 83_ 89_ 75

29b35 27" 26 5b- 79

7691 74 21 8193 75 21 89- 48- 79- 83_ 90_ - 16"- - _ _ 65_ 93_ „ _ g3- - - 77_ 90_ 85- - - 76— — — 91_ 36- 75- - - 109_ 86_ 84— — — 97

(continued on next page)

92888384855b877085857582899985401068986899756889310018"731119589102958510149871259792108

81310990107630587111332184b12121091511111112121813141311111031151412911

Fly ash'% Recovery

(QA Objective 30-1 30%)Precision

MS MSD RPD82818179805b8275846773778892824917b81778386598284913774898680898682925467108858294

84848483846b8577908574828595804116b848284896584879535798691849591909758771159287102

2445520437241633218 '64613102446736576957146868

A R 3 I 5 I 5 8APPENDIX F 23

Table F-14 Continued(Matrix Spike Recoveries and Precision for SVOCs in Bottom Ash and Flyash

Feed'% Recovery


MS MSD RPD4-Chlorophenyl phenyl etherFluorene4-Nitroaniline4,6-Dinitro-2-methylphenolW-Nitrosodiphenylamine4-Bromophenyl phenyl etherHexachlorobenzenePentachlorophenolPhenanthreneAnthraceneDi-n-butyl phthalateFluoranthenePyreneButyl benzyl phthalate3,3'-DichlorobenzidineBenz[a]anthraceneBis(2-ethylhexyl) phthalateChryseneDi-/7-octyl phthalateBenzo[i>]fluorantheneBenzo[/t]fluorantheneBenzo[a]pyrenelndeno[1 ,2,3-cd]pyreneBenzo[g,/j,/]perylene

P-Naphthylamine (by ECC)

-

-86115--123127--129-105-959392-—

(30)

-

-7383—-95103--99-86-797676---

(38)

i—1632--2621--26-20-182020-—

(24)

Bottom ash"% Recovery

(QA Objective 30-1 30%) .Precision

MS MSD RPD90929979918891749084981099690699210891898484829189

(83)

10210310891100961008499921091241089980102117102101851029410198

(79)

131110149991310911131210151081113120141010

(4)

Fly ash'% Recovery


MS MSD RPD899310283908890708586951061009067859990918184838783

(20)

94971088894939575909310311310695749311398988597919592

(19)

5466465768866 ,510913975149910

(5)

Surrogate Recoveries (%)-QA Objective 30-130%2-FluorophenolPhenol-d52-chlorophenol-d41 ,2-Dichlorobenzene-d4Nitrobenzene-d52-Fluorobiphenyl2,4,6-TribromophenolTerphenyl-d14

Surrogate Recovery (%) by ECCNitrobenzene-d52-FluorobiphenylTerphenyl-d14

6070707077788389

7689116

5257585966677380

7088105

1421191715151311

8110

6570687075737472

73103111

6975737582808379

82101107

677799129

1424

6772717077707172

8999125

6876747481777878

8491109

654651038

6814

Spike level was 10,000 |jg/kg for feed, 1,000 ug/kg for bottom ash, and 500 pg/kg for flyash.Data are outside the QA objectives.Objectives: 30-130% Recovery; 35% Relative Percent Difference (RPD)

R£RW620-28,ipf

& R 3 I 5 I 5 9APPENDIX F 24

Table F-15. Precision of Surrogate Recoveries for Combined Stack Gas Samples (a)

Surrogate Compound2-Fluorophenol

D5-Phenol

D4-2-ChlorophenolD4- 1 ,2-Dichlorobenzene

D5-Dinitrobenzene

2-Fluorobiphenyl2,4,6-Tribromophenol

D14-Terphenyl

Precision, %RSD, Combined Extracts3

2

2

7

4

2

4

4(a) %RSD based on 4 samples.

Table F-16. Precision of Surrogate Recoveries for Waste Feed, Bottom Ash, and Fly AshSamples

Surrogate Compound

2-Fluorophenol

D5-Phenol

D4-2-Chlorophenol

D4- 1 ,2-Dichlorobenzene

D5-Dinitrobenzene

2-Fluorobiphenyl

2,4,6-Tribromophenol

D14-Terphenyl

Precision, %RSD

Waste Feed

12

11

11

11

10

8.6

8.0

9.6

Bottom Ash

8.4

8.9

8.9

9.3

5.5

9.3

8.4

7.6

Fly Ash

5.3

4.8

5.4 '1

4.5

2.7

2.9

1.4

2.2

RER\rM20-28.apf A R 3 I 5 I 6 0APPENDIX F 25

Appendix G

Report on Chemical Analysis Results for PCDD/PCDF


&R3I516I

Appendix GDioxin and Furan Analytical Report for Risk Burn Number 2

by Rachel A. Rose-Mansfield, Assistant Chemist

1.0 Sample Receipt and Storage

MM5-Dioxin/Furan train samples from three runs, one field blank train and seven ashsamples were received cold and intact on February 11, 1997. Samples were stored in the330-E cold room prior to sample preparation.


The MM5-Dioxin/Furan samples were prepared for Dioxin and Furan analysis accordingto EPA Method 23 for stack and associated QC samples, and according to EPA Method8290 for ash and associated QC samples, with the exceptions noted in the Trial Burn Plan(September 20,1996).

EPA Method 23-Stack Sample PreparationOne method blank and one lab control spike (LCS), consisting of preextracted XAD wereextracted with the XAD trap and filters. Each XAD trap was spiked with field surrogates(4 ng) prior to shipment to the field. Each XATJJ/Filter was spiked with lab surrogates (4ng tetra through hepta and 8 ng octa) prior to extraction. Each toluene rinse was spikedwith lab surrogates (4 ng tetra through^hepta and 8 ng octa) prior to concentration. Thefront and back half rinses were not spiked with lab surrogates.

One soxhlet extraction was performed for the XAD/Filter samples using toluene as thesolvent. The front and back half solvent rinses were concentrated and added to theXAD/Filter prior to the extraction. The toluene rinses were also concentrated but notcombined with the XAD/Filter, and were analyzed as separate samples. All samples,extracts and concentrates, were solvent exchanged into hexane and taken to a volume of10ml. A 5ml portion of each sample was archived. The other 5ml portion of theXAD/Filter and toluene rinse samples were run through two-part columns and a carbon 'column of 18%Carbopak C-Celite for cleanup. At the end of cleanup all XAD/Filter andtoluene rinse were concentrated and spiked with recovery standard. A nitrogenevaporation system was used to achieve a final volume of 20 ul for XAD/Filter andtoluene rinse samples.

A spike check consisting of field and lab surrogates, and native Dioxins and Furans wasprepared for the.XAD/Filter and toluene rinse sample batch.

EPA Method 8290-Ash Sample Preparation 'Two method blanks and one LCS, consisting of precleaned quartz sand, were extractedwith the ash samples. Each ash sample was spiked with lab surrogates ( 2 ng tetra throughhepta and 4. ng octa) prior to extraction.

A R 3 I 5 I 6 2APPENDZX G

Soxhlet extraction was performed on all of the ash samples using toluene as the solvent .The extracts were solvent exchanged into hexane and taken to a volume of 10ml. A 5 mlportion of each sample was archived. The other 5ml of the ash samples were partitionedagainst sulfuric acid and potassium hydroxide, followed by silica, alumina and carboncolumns cleanup. After the cleanup all ash samples were concentrated and spiked withrecovery standard. Nitrogen evaporation system was used to achieve a final volume of 20ul for the ash samples.

A spike check consisting of field and lab surrogates, and native Dioxins and Furans wasprepared, for the ash sample batch.

3.0 Sample Analysis

The samples were analyzed by high resolution gas chromatography/high resolution massspectrometry according to EPA Methods 23 and 8290. The extracts were analyzed on anAutospec-Ultima high resolution mass spectrometer at a resolution of greater than10,000. A DB-5 ( 60 m length, 0.25mm inner diameter, 0.25 film urn thickness) columnwas used to effect separation of 2,3,7,8-TCDD and all other TCDD isomers.Confirmation analyses for 2,3,7,8-TCDF was performed using a DB-Dioxin ( 60 m length,0.25 mm inner diameter, 0.25 |im film thickness) column.

The initial calibration consisted of a series of five calibration standards ranging from 2 to200 ng/ml for Method 23 and ranging from 0.5 to 200 pg/ul for Method 8290(Table G-1AandGl-B). The initial calibration passed the criteria with a %RSD of less than 20% forall compounds. All compounds met the criteria for signal to noise ( ten to one) and massion abundance ratios (+/- 15% of theoretical values).

Continuing calibration using a mid level standard (CS3 for Method 8290 and CS4 forMethod 23), as well as column performance and window defining mixes passed the criteriaas specified in Method 23 and Method 8290. Successful sample analysis were bracketedby passing the calibration standards at the beginning and end of each 12 hour shift. Allcontinuing calibration standards met the above criteria.

Native results were calculated relative to the lab surrogates. Field surrogates werecalculated relative to the lab surrogates. Lab surrogates were calculated relative to therecovery standards.

4.0 Sample Results

The stack sample native results are given in Table G-2, and the ash sample native resultsare given in Table G-3. OCDD and OCDF have been re-listed under the Homolog Groupas well. The matrices are listed above the field IDs. Table G-4 lists the lab and fieldsurrogate recoveries for the stack samples. Lab and field surrogate recoveries for ashsamples are presented in Table G-5. Field surrogate recoveries are not listed for toluenerinses or ash samples since they were not spiked with field surrogates. Recoveries of the

A R 3 I 5 I 6 3APPENDIX G

Laboratory Control Spike for the stack samples are shown in Table G-6 and ash samplesin Table G-7. Table G-8 shows the results of the MS/MSD pair from the bottom ashsamples. Ash sample duplicate recoveries are given in Table G-9.

5.0 Q.C. Results

All samples were extracted and analyzed within holding times as specified in the trial burnplan.

( • * ' • •

The method blank for the XAD/Filter samples showed detectable levels of some isomersincluding 1,2,3,7,8-PeCDD, 1,2,3,6,7,8-HxCDD, 1,'2,3,7,8,9-HxCDD, 1,2,3,4,6,7,8-HpCDD, OCDD, 1,2,3,4,7,8,9-HpCDF and OCDF. However, the total amount ofisomers found in the method blank were considerably lower than the total amount found inthe samples.

The method blank for the ash samples showed detectable levels of OCDD and OCDFbelow the estimated method detection limits specified in Method 8290 (Ippt for tetra,2.5ppt for penta to hepta and 5ppt for octa isomers).

The LCS for the XAD/Filter showed recoveries of 72 and 112%, and the LCS for the Ashshowed recoveries between 85 and 126%. Results are presented in table G-6 and G-7 asthe percent recoveries. There were no recoveries outside of the MRI objective of 50 to150%.

All field surrogates met the recovery criteria of 70 to 130% with the exception of the LCSfor the XAD batch, which had a recovery of l3C-l,2,3,4,7,8,9-HpCDF of 131%. All labsurrogates also met the recovery criteria (40 to 130% for tetra to hexa and 25% to 130%for hepta to octa).

Table G-8 shows the percent recovery and %RPD for the MS/MSD pair done as part ofthe ash batch. No isomers present %RPD greater than the 25% objective from the trialburn plan.

Table G-9 lists the ash sample duplicate recoveries in pg/g. Since no isomers ofdioxin/furan were detected in both the ash and duplicate samples it was not possible tocalculate meaningful averages or %RPDs.

A,R3I5IS*4APPPMnTV ft

Table G-1AMethod 23 CALIBRATION STANDARD CONCENTRATIONS (pg/A/L)

for analysis of stack samplesCOMPOUND

2,3,7,8-TCDF2,3,7,8-TCDD1, 2,3,7, 8-PeCDF2,3,4,7,8-PeCDF1,2,3,7,8-PeCDD1,2,3,4,7,8-HxCDF1,2,3, 6,7, 8-HxCDF2,3,4,6,7,8-HxCDF1, 2,3,7,8, 9-HxCDF1,2,3,4,7,8-HxCDD1,2,3,6,7,8-HxCDD1,2,3,7,8,9-HxCDD1,2,3,4,6,7,8-HpCDF1,2,3,4,7,8,9-HpCDF1,2,3,4,6,7,8-HpCDDOCDFOCDD

Lab Surrogates

13C-2,3,7,8-TCDF13C-2,3,7,8-TCDD13C-1,2,3,7,8-PeCDF13C-1,2,3,7,8-PeCDD13C-1,2,3,6,7,8-HxCDF13C-1,2,3,6,7,8-HxCDD1 3C-1 ,2,3,4,6,7,8-HpCDF1 3C-1 ,2,3,4,6,7,8-HpCDD13C-OCDD

Field Surrogates

37CI-2,3,7,8-TCDD13C-2,3,4,7,8-PeCDF13C-1,2,3,4,7,8-HxCDF13C-1,2,3,4,7,8-HxCDD13C-1,2,3,4,7,8,9-HpCDF

Recovery Standards

13C-1,2,3,4-TCDD13C-1,2,3,7,8,9-HxCDD

CS2

22101010101010101010101010102020

'

100100100100100100100100200

40100100100100

100100

CS3

101050505050505050505050505050100100

100100100100100100100100200

40100100100100

100100

CS4

4040200200200200200200200200200200200200200400400

100100100100100100100100200

40100100100

. 100

100100

CS5

200200100010001000100010001000100010001000100010001000100020002000

100100100100100100100100200

40100100100100

100100

CS6

500500250025002500250025002500250025002500250025002500250050005000

100100100100100100100100200

40100100100100

100100

*


Table G-1BMethod 8290 CALIBRATION STANDARD CONCENTRATIONS (pg///l.)

for analysis of ash samplesCOMPOUND

2,3,7,8-TCDF2,3,7,8-TCDD1,2,3,7,8-PeCDF2,3,4,7,8-PeCDF1,2,3,7,8-PeCDD1,2,3,4,7,8-HxCDF1,2,3,6,7,8-HxCDF2,3,4,6,7,8-HxCDF1,2,3,7,8,9-HxCDF1,2,3,4,7,8-HxCDD1,2,3, 6,7, 8-HxCDD1,2,3,7,8,9-HxCDD1,2,3,4,6,7,8-HpCDF1,2,3,4,7,8,9-HpCDF1,2,3,4,6,7,8-HpCDDOCDFOCDD

Labeled Analog

13C-2,3,7,8-TCDF13C-2,3,7,8-TCDD13C-1,2,3,7,8-PeCDF13C-1,2,3,7,8-PeCDD13C-1,2,3,4,7,8-HxCDF13C-1,2,3,6,7,8-HxCDD13C-1,2,3,4,6,7,8-HpCDF13C-1,2,3,4,6,7,8-HpCDD1 3C-1 ,2,3,4,6,7,8,9-OCDD

Recovery Standard

13C-1,2,3,4-TCDD13C-1,2,3,7,8,9-HxCDD

CS1

0.50.52.52.52.52.52.52.52.52.52.52.52.52.52.555

100100100100100100100100200

100100

CS2

22101010101010101010101010102020

100100100100100100100100200

100100

CS3

101050505050505050505050505050100100

100100'100100100100100100200

100100

CS4

4040200200200200200200200200200200200200200400400

100100100100100100100100200

100100

CS5

200200100010001000100010001000100010001000100010001000100020002000

100100100100100100100100200

100100

A R 3 I 5 I 6 6APPENDXX G

CNcijDjaco

•*•*ucoCD

£ *

CBEEDC/5m13jlT"

toCDQ.EreCOOOT3CD

"Su_

CreoreCOs—

s1-ro03

r-ccr55

CDC

I§mS5

incd5»

cremT30JCZ035

CDQ.ECOCO

CNCOmoT~COin

COmCO

COin

0CNI --

COoCN

35oCN

1CN

oCNCDCOoCNCDo5oCNCD

CNCD

OT —CNmCOoCNin3>oCNin^CNin

CD

O-z.

9T3CDLL

pCQ* — 'mr—CDco

CDCO

COI--CDCO

CN

r-CDCO

rrT*

COCO

COCO

Ql .OCO•%LU

9CNOCNCDr -OTX

CNCN0CNmO5X

<t —

CN0CNmenX

ioCNmo>X

LO

oCNmX

CDErec_CD

ECO2

~.ac"(515HVICOEo10

COr—c*»CM

o"P Q.r*"1- >

o § ino o S

=> S.D

-CD g CNO o O0 o 0

Z)

c\rCO Q O

o c> o0 o 0

5"

o"in j. o3 f 3o o o5"

^_^ _ sO OD. D-5 r^. SLU o LUm o co0 _; O0 ° 0o o5" =>"

QQ g

D O -^Q « xQ CL co1— ob r-~"co r }*r~ co coco CN" CN"CN" t- T-

O'a.

O CD

°§.o.3)

0 0o o

, _ _^O O

LumCN T-O OO, O,:D::>

CN CO

0 O

,

§ 5o o

Q QQ QX XI! XCO 02!*•[ CO"

CO COCN CN

o"cS n " "t }* r*"* * co * co 05 i o J* ^ ^ ^ f- v~ inCN CD f CO C T™" CD f f~ ^ 1 1 1 if) .M -| • ~ *o o o o o o o o o o o o o o oo o o o o" o o o o o o o o o ° °

5" o. o'z)'3)

O t - O O O O O O O i - O O -<4->-CDT-o o o o o o o o o o o o oooo

o?c n 5 c N ^ c O C O c O C N o C N C N § 5§^S

O O O O O O O O o O O O O O O O

5"

Q*

CL oTO5 CO C J OJ T * p - CO 1 1 1 f~* * CO D CO CO O5 CO

o o o o d o o' PJ o ° do do o" o^"1 ' — 'o ^^

O~ '—CL 0MI O5 O O3 LfJ f™i *f"» *j">CO CI5 ' * ' — i- ^ _ i .„ AJ **»t ^^ tjO CO CO n*~ CO ^ft

3 D i* ^ f~j f™j r™ \ f" * /••% to cO CO C? f"*|E CO C3d d g o o o d d d o ° d d d d d

°- ID Z) Z) 3) 13 Z) oS T'D

"oc2

Q LU LL 2Q L L U _ L L U _ Q Q !-*^_ — .U-U-QQQQ^^ Q"f uTooxxx><^""'r 8OO_ Q aj aj X X X _L CO_ O5_ ^rji-~ QD_D-cococooir^co _CD H co_ co_ r«." r-" r-{ co_ co" r~-" o Q Q Q< Q co r-{ r~-_ i <ol «3 K -* •* u_ -3 Q Q Q QCOQI^-CO-*COCO-*COCOCOQ £ Q Q O OCN" O co CN" co CN CN" co" CN" CN" CN" O o o UJ X Q-T-" O CN" v-" CN" T-" -" CN" -r-" -" -r-" O X I- Q- X X

*— .(Q

O CD O • O OC3 O O ^— ' O O

^ $ J^ ?i oo o o o o o

^ * 05 r* * * co O)* oj r * co o} co«f— c f\j CNJ ' — coO O O 0 0 O

m co CN m i- T-co co co r~- m oo o o o o o

T}* CD O

0 0 0 0 0 00 d d o' ° °

zT zT 3

_ LL LL LLQ LL Q Q Q LL

O o LU X 0. CO \- CL X X O

CD

2.c*-E~c00OJOJT3CD.C

coreo> c

2iilE ^5•—- h?1 SIs|3iCD CO to to oCO O O.a a.CD P —to § X0 g O

j: x 9| g 035 E Q11 ?o ca 'mSi E =>CD = TD"O to rnS'V E^"1^™\ ^— • LJ-1 5 yCT-LU coE 0 =

§|2• LU LLjysCD 0 h-

— * — \ CO

<r

/1R3I5I67APPENDXX G

C/5

•" "co

3 COW CO(D /•>

re

CD ca•43 o

o

CD

'Q. ^ COCO W

cu O. O

c ° m§ Z «> PO CD CD£1 co XCD

a>CM£U CMo

<S5gfc g|

1 r- CM5 5 cTcN< in co CQD_ r~- Is*UJ co °2CO T

§ p°5 ^- a«MO

S g K fc PCO 3u r~01 CM ,-.0 ~ o o oCD 05

CQ o M X

CU

c •<& 01

CNfSS

£pi£2cu r- co E:3 V> b>O X

f/j ~ c T CM" co" to" Q- o" o" co" in" Q- Q-CO a —. ™ CMCOc015^_._OTj-Tt-5:_J.5

CUCD ^ CO

§ & CM £ o

«|§S|• o X

CD

" = 'YJbi^co gry „..-*— [ r\lj — v N P"- *—'a: cu r; £: CMc CN CD CQ

CU 10 IN.3 02o X

jB Q - _CUa.E

= O r=T3 ca UL

CD .2 "X !CO U_ UJ 2

CO

COoo

CM COCMT— - T~ T— * Tj* Tj* T~ T™* - CM CM CM f~ " J* " t" " CO CO O5 CD • 1" J" un . O5o o o" o o o o o o o ci o o o o o o o o o o o o ci *" o o

o o o o o o o' o' o' o o o o o o o o o a d o o o o o o'

0~ 0~ CL Q. Q_ cO~ D-

Q § L U U J L L I c O o o g o O i - O T - o i n U J c o

pâ,pqq°°o,ooooooogo 0^0,0.0000000

o"CM r~- r- COCOCM Q-V-CM T^-T-CM COCM

oo0

co fe • d p. d p. d o o d d d o o pi d o o o pi pi pi o pi pi ° ° oDDDD DDD ODD. DDD

o. o, o, g o, o d a, ol o, p °' p! °' °" p ° ° o, o, °' °' o, °' °' ° °

D" 3" D' ' D"

oo" i?T F~~ Q- Q- o" co~ CM* Q- Q- F--- Q- Q- oo" UT" o" o" co" CL

S'D' D'D' D'D'cuE

Q gOC

2oQ U_ U_

Q

QQQO -.___,,,.QQQQ. CJ ^û_u_QQC3Q^ "Q o o o -2" .co. Q Q o o o o -2" -2~ ^

- r - - T - l "-C-JLJ-.-----.--.-II00 ^ ^ - - - - 0 0 °lr^CU-l--*--J-CO pJ^cU-^-^-^-^-ÔOOl /n

IT oo K K « col H co oo i-.; r-: iC'od; co^ r-{ o o n Q u u u_corv--|4-cor~-"tr(~>eor~r~"<frcocQfx-''3''<a'ii ~ u u HH -. u. u.

cococococOQr~co-<tcoco-<i-cococoQC O C M C M C M C M C M O C O C M C O C M C M C O C N C M C M O OCM" t-~ T-" T-" T-" T-" O CM" T-" CM" •«-" T-" CM" T-" T-" r-" O I

QQQQgu.QQQO UJ X Q. O o UJ X 0. O\- Q. X X O (- Q- XI O

A R 3 i 5 1 6 8APPENDIX G

to_CDQ.ECOCO.Cto<

co £ ICOOa

<3 _CO 3~X «CO co -aQ; CD

>, js« <"a:E3COcoCO

5 CD § K< CO S CN- CN g CQO r~ co t*~CQ CD

rf 05 o < CO S CN« SJ S EQ

CO

CD

•§ Tf g £< •* g CN><£ % £rr "* co r-co • -O5

X

CO

CD COCQ CD

CD

f CD O «< CO g CN~ CN § CDO **> CO Is"CQ CD

LUCQ

•O ty g,!0c z r CNrSQgCQ

CO CDco X

Z co

CQ CO

coCO£=.-'o££Z oo

CO CDco X

CDE

Q gQ CD

£2 |ECD •% COa. LU *=

r--CDO o

s oco m *—- ^ rt >. * ,-f •. * * yj

o, p. p. p. T- r - •* r-i P po o o o o'

O

t) CDS C

5 P f3, C3 O O Q' (—i ^ 'r~ S, PLd

COCO ~

'. P COdS2.2-2.CDMd2.2-p'p_dp'p'2-p __S'^131313 5"=> 5"D rTS'5" 5* D =) D D

a" ^ ^ ^ _ .. ^^^^CD ^ o CD *^p T— oocDcDi^^coÔ5 ~ co ;^ CD CD T— r^- in T—

o o o o ^ T— °°. o o o oi o co o CN oi'"! CD *". ai CD °°. oi oi ai oo CD, d, d, 2- § "~ d, d, o, o, d, d, f° d, 2- d, 2- d, d, d, d, d, d,

D" ^ 5"

^ o" o"C? g- CO T ~ co jjj. jq. f if) - T— OO {Q- O5 P CO r~- CD

d2-p'pp'°2T~p2.2-pp,pd,d,f2d 2-§'2-2'T~2'§'2'2-0D='=T3'5'd 3 => => 3 =)" 3 D " ^- —— — ——

Q U. UL gQQQQ LL.LL.LLU.QQ —

QQQQ^J ^ ^ n i i Q Q Q Q ^ ^ QQ O O- CJ 3- S.QQOOOO-S'-S' 3

(jQ-cooocor-" (jQ-CLcocooocnr-'co"h- co r~" t--" co" CD" H cp 06 r-~ r—" r-~" oo" co" r--~coi^-^cDr^-ôcof-~r»-'^'CDCDr^-Ti-T}'|.r-c O C \ I C N C N C N C N l O c O C N C O C N C N C O C N C N ) C N O oCN" T-" T-" T-' T-" T-" O CN" i-" CN" i- •<-" CN" t-~ T-" T-" O I

Q Q Q u, IL. LLO O O O Q n r^rîOLL

OLUXQ.OOLUXCL.C1-Q.XXOh-Q-XXO

CD

2c

co

. coCo "a.

£ S

T3

.C

COCO§1

Q) O cS5 ET3

CD r -2to S oJ§§^§ s|o CD O= =§9^ to CQ3 o Q"2 v g55 x

COo c 'toCD C ÔJ J -oSLU M6Q.

C- LUloi

E

I

ol^~ LU u_:~ § sCD O |—"O O' .CO.

c

CD

APPENDIX G a

if a: %ra (

E

^ %2w •* o LO< - fci CN^, CM O CDc^SS;

SS x

CO I

£ 2: >n •*inoJcocNi--cj-coooT_t-a)coO5ococo - -- « . ^ - ~ >, -, vw^^^ i-TTC O c s ^ o ^ e o c p O q i o i O c o T - c o ^ ; •# «> o r. ca & g> T. r.

w 2: co r«-CD C35CO jT

oo r-CD 5co X

coco

J CN CNoLnsCO"z

O)

CDE

9 CQ _CD

'cr ~o CTJ Li.ca "53 t? CO5 E QJ 5

5" d d, D si, Dr)t£.oo:Dd.D

eo od •* o> o od jo od co c\i cb r-' od •* r- c\i p. co oo" •<- co od~ -

co' co o' eo' od ° t7 o 10' CD' od co' oo ° in r: co CDi !* ° fc o'

O O•c^ ^^r^-OO1^ U^LOOOCO v- £^* '*s OO CO OO

. O O cO O O O O,0000000

r> :D

,— G" ^£^^ ^ _, O* ^

o co °°. fi! CN o in o cq CN § o P W ""> co" co 06 m' "? S o en; q; in

3COfl* T~ _ _ -~^ _ u- Q- ST CL

1-1"" 3 >j « f * * ^ ji ,_ • — ---.._ V) * * " . _ fS CO _ i (••* (~ / ^ __ >. > 1_ rrt rv sr\

: CO ^ T q m. "T. "? S ^! gI q m CN LiJ g cq UJ

- 3 - 3 D - - 3 ci^ T-;5'r-:^ 3 D

CN

Q u_ u_Q Q Q d LLLJLUL11.QQ

Q Q Q Q O ^^ u_u _ Q Q Q C 3 ^ ^ Q

Hp oo I--" h-~ oo" co" h- ab co r~" h~" r~-" oo" co" r-" §. ^- Cj ~ _ - %- - ^T. . U— O

CN" T-~ T-" T-" T-" i-" O CN" T-" CN" T-" T-" CN" T-" T-" T-" O Xi

Q Q Q „ u_ LJL u.QQQQQll.QQQ'J-

CLXXOh-CLXXO

cu vC35 \

CD

O Q.o p

Q)<a.ara

111- ilvX *--.

CO <m ><

c. £

in Q

1

CD ,__• CJ

m Q

IS

m i_Crt)

t •

^ 5

> S

y/

C_coen Q" 3 fO *^pi x"x

to2

0)Q.ECOCO

CNCOinoT—COinT—T—COinCOT—COmoT—

SCO0CN

oCN

V-CN^oCNCDCOOCNCDO5OCNCD^CNCOO-CNincooCNtnO5oCNinT—CNm

COo

Q•oCOii.

pCOas£ is§ s

CNCS1

!§CO ^O5

T—

CO

T.

t—siO5~T~

--^ mCD '^ CN^- °CO DQCD O5CO Jl

COE

Q g^ CDO :=CO- U-T? COuj 2

O)oCOc:<cT3COCOjQCO— '

CO CDCO •*CD 1

v— CDCO T-CD r-

CD OOCD OCD t -

•* O1 CN1 - CO

t O5l*"~ t~"CD 1

U. QQ Q

«££a» «o r- r-^ CO CO

co °V <V-Q O Oco co co

CO OO COr~ m

CD 05o> oCD CO

CD COo oc~- co

CO v-r O5r- co

"* °°.CD m

8-PeCDF

8-PeCDD

r ~ r* "CO COCN CN

™ ""

6 6co co

O CO•* mCO 00

-* CNCO •*OO CO

•* O5•* inCO OO

T- O

CN inO5 O5

O CN1 05'

u_ QQ Q0 0

CO COr-~" i-~Tco" co"CO COCN CN

** "1 1O Oco co

CDj*

inco

COcor>-

CN

CO

.co

U-

0_

COt-~"CD"

COCN~

1Oco

CD COCN CNO5 CO

T- O

f- OOO5 OO

O5 COas mOO CO

CM COO i*,*~ OO

-*• T-CN 1-05 CO

QQ0Q.T.CO

co[^ QCO QCN OT-"O

66co co

CDCNO5

CNinO5

,_

5

ooO5

z.

QQ

03 OTO 7C3) COO j^"i coco CN"lo.92 r-U- CO

l _ CNO |• O5

T- COi- OT— T—

O5 T—o o

o r^•«- 05

< <-z. z

u_

<o a. oo06 r—~h-" •*"•*" co-co CNCN" T -"6 6co co

•* oCO COCO T~

t*- S-co - fOO CO

05 CD

co •«-

O5 u-)0 CNOO "~

-z. .

LLQ Q

0 -g-X d5_OO CO

•*- tfco" co"CN CN~

66co co

^0CO

o

^COct=ocCOCL1m]co, —

oCD;g"3o&COooESiCOO)o^CO

"53il!LS

*A R 3 I 5 1 7 I

APPENDIX G 1O

T33

<£

Q.LU

•»*3

Q.LU

CDc <"'2 2H „,Qj

OCT3 3CQ "o

1-CD|v- <2

§ Ea: CDi 12 "o

CD

<£.!§ o:o; CDi§ CD2 Z3

5 !°0m g

§Sa: £

5 "oh-

CDa.EcaCO

O)CO03

rv.oin

T—COin

CNCN

CMCMCO

CNCNin

QT3CDu.

™ ™0- ooo CDIs*- I**""CD O5

T— Y—

vt Oco &r**" (•••••CO Oco x

. — , o03 CN— oO3 CNjv- QQ

CO C35CO T

05

CO g

CD S~&X

co|v. CM§1

03X

f—

f2 oco CDCO "~oX

EQ siCO 1L.

^ wLU S

CTOCO<t•aCDCDCO_J

03TOO)g

COJ3co— 1

CO IT-CD h-

CN fv.O5 CNCD N-

r " j*oi coco r-

m •*o co'CD CD

•* cooi inco fv.

03 r--oi -<tCO (v-

u. QQ QO Oco_ ab_r~- I*-.CO COCM CNi iO OCO CO

fv- mCN CNiv. CD

O 00r-. coCD in

T— IV-

CM T^JV. CO

•<J- 1-

CD Tfco m

OO COco" CMfv. CD

m o0 CMfv. CO

U_ QQ QO OCD CDQ. Q.CO COIs- r -co" co"CM CM

O Oco co

in coco co

03 COCO O|v- 00

T- O5co' coCO CO

•t COco aifv. (v.

co r—- f rv.'CO CO

oo inco oo'CO CO

U. QQ QO 0X XX X1 1co_ co_

CO_ CD_co" co"CM CN

O 0CO CO

O COO5 COIV. O5

O5 COm CNfv. O3

o coCO 0oo •"-

•* -th- O5

CN CMCO OCO •«-

,co oCO ~

a. QQ Qo oa. a.X Xco co|v-" IV."

co" co"it •*co" co"CM CM

0 Oco co

ococo

COCOoo

os

^aico

•inco"O3

cooiO3

_CD"cc

Q oQ t

O$&T- U_

.

"Z

..•z

^

z-

*

2

*

QQO

i°°-coCN"OCO

~Z "Z

•z -z

<f <f^ ~ZL

n

~z z

•z ~z

LL

,8-PeCDF

7,8-HxCD

Is- •*•<*•" co"CO CMCM" T-"t i0 0CO CO

<C <fz -z

•z -z

<f" <r/z. z.

~z ~z

~z. ~z

•z ~z

u.Q Q8 °-X O)c£ co

•«t •*"co" co"CN CN

1 1O 0CO CO•*- •«-

CNCDencaQ.

in_gjcu co> vO "a.

pi

cu.aca

CO QC_3 *i ^^

cuQ.ECOCO

f _ CO

c ^i-O CN)

Is-CDCO

QQ —— o-a 2E UJ

CO

oCMOQIs-O5X

cuECOtz_cu

CO"S.

en003<3T3CDCD

03_l

o coTl- OOoo r

a. QQ Q„, ° °S H H-g, CO CO

2 - .^ CO COCO <? "n O OCO CO CO__l T- T-

O5 COO v-co r—

•PeCDF

•PeCDD

CO OOIs- Is-CO COCN" CN"

*" ~

O 0CO CO

05.j.

CT>

,8-HxCDF

Is-CDCOCM"~

1OCO

Is- CDCO Is-O5 OO

U-

i -OO Is-Is-" CD"CD -*•CO COCM" CM"_ _

1 iO 0CO CO

co r-o r-.•"- O5

QQOQ.

COIs-"CD"•* QCO QCM" O--"O1 iO OCO CO

CDiriO5

QQ

o O+-> i —CO ~en coi_ r3 CO"CO CM"~o —._ f**.U. CO

- rg•r- OT — ^~

•PeCDF

,8-HxCDF

CO Is-Is-" •>*•"•*f" co"co" CN"CM" TJ-"U 6CO CO"~ T~

05 &in T-CO CO

U_Q gO £•x -rX enoo_ oo]Is-" Is-"•* •*"CO" CO"CM" CM""

i i0 0CO COT— T—

o«0CO

oIs-"ocuo-CU,

o

aa>.•g

o

cuoocu1

"co*s-'

A R 3 I 5 1 7 3APPENDIX G 12

CO T* *"" TT

<3§g

"- °° 0>XO

^ CO <°U. °°

1811oo

o>

^ o> £ < CO g CM•J CM g 00o co prt r-^CO ro

<9_ /o T~C^ « LT)CO S CMS " £Q

m

03 fcCO CDco X

T3 CD S m

IllsSS

o>E

Q <2Q T5 i

525"-CO CD "x WS U. UJ S

o>_oCDC

CO

r^coeq-^cocDcocqcqr o> co o co 10 <o' •«- CN < < <

ojcNcori-oicoouir--

co co N; CD cq in r-~ in ui <f <f <f <f <fCD LO to co cvi co' CM' oi TJ: 77777

C N l T - u n C N T - O T O O O O 777- ^^-^-

>T O3 vU P"1" CN tLJ OJ tJ iN j» -* j- j* j-

O> O5 O CN O CO CN O) CN 77777

eq o CD co ^ o> CD cq <<<<<-OOOCMT-OJOJCO'^-CO 77777

Q u_ u_Q Q a. Q Q u. Q

Q CO-J-OO

S H co r- coCOO) _Or— C O C O C O Q I ^ - C O C O C O

QQ-cor—"oOooQ-coco"

co r- co Tt coco" CM" CN" CM" O co" CM" CM" CN" ,5 °°- f " °°" t " fT3

_CDCD _' ~ o>^ t i i i i i i i i T 3 — i i i i£ 5 O O O O O O O O O ? J O O O O Ococococococococococo.— r«-cocococo

C3503CL

. A R 3 I 5 I 714APPENDIX G 13

o. O 2iin o Q.I CU pO £ fcn

"O_cucu.QCO

Q. "?.£= D T-</3 •**• Q m<C 3" —' CM.,_ CM O CO-2" in CM P-U- CO 05

CO Tco -1--~- CO

•a

co r>-CD 03co X

co X_k co

co' CMrf^SgCO CO o)

CO -r

tn c° v;;111 co 5co XCDE

Q cQ _CD

| 32 2 ca cu •$< C/5S b_ ill 5

•a_O)0)JD03

< < < < <

lf) CO CNl rf CO CO 10 CO CO < < < < <

T- to co a> co CN i- CN < < < < <

Q) 01-9 — --f* /\ _ ^ _ .

CM CO O CO T- O) < < < < <comr^-ocMcot-coo ^^^^^inmcDi^comincoco *-•*.*-*-*-

Q a. LuQ Q u_ Q Q u. Q

QQO u _QO Q u _ Q O

QO^"? u-O-^^f nxux^"QCLcot^ (_)Cl.c6h--"oOc6ll.c6co"

Si— co r CD" 1— co r~-" co" S i t~~" co i~-" i-"g, co r* co •* Q co r>{ co" •*" §* °°. •* r*-" •*" M-"O Is-" CO CO] CO] Q h-" CO" CO" CO" t ^ CO" -5J-" CO" CO"

co CM" CM" CM" O co" CM" CM" CM" . n. CM" co" CM" CM"<g CM r-~ T-" " O CM r-" T-" T-" W 2j a O O O O O O O O o l o O O O Ocacococococococococo;— i-~-cocococo

Table G-6.Lab Control Spike Percent Recovery

for Stack samples

MatrixField ID

Isomer Extract ID

DIOXINS2378TCDD12378PeCDD123478HXCDD123678HXCDD123789HXCDD1234678HpCDDOCDD

FURANS2378TCDF12378PeCDF23478PeCDF123478HxCDF123678HxCDF234678HxCDF123789HxCDF1234678HpCDF1234789HpCDFOCDF

XADLCS36782

% Recovery

88.390.089.585.0103

* 110.111

10592.589.510696.510394.5126122116

&R3I5I76APPENDIX G 15

Table G-7.Lab Control SpikePercent Recovery

for Ash samples

Isomer

DIOXINS2378TCDD12378PeCDD123478HxCDD123678HXCDD123789HxCDD1234678HpCDDOCDD

FURAIMS2378TCDF12378PeCDF23478PeCDF123478HxCDF123678HxCDF234678HxCDF123789HxCDF1234678HpCDF1234789HpCDFOCDF

Matrix SandField ID LCSExtract ID 36815

% Recovery

7281.588.280.6112101107

9496.810199.192.910396.9110106108

Page1 A R 3 I 5 I 7 7APPENDIX G 16

TableG-8. MS/MSD Recoveries (%) for Bottom Ash Batch

*

Isomer

DIOXINS2378TCDD12378P6CDD123478HxCDD123678HxCDD123789HxCDD1234678HpCDDOCDDFURANS2378TCDF12378PeCDF23478P6CDF123478HxCDF123678HxCDF234678HXCDF123789HXCDF1234678HpCDF1234789HpCDFOCDF

Field ID MSExtract ID 36813MS File H97B251-16

7082868295102113

108929172637263108102111

MSD36814

H97B251-17

7586928611296113

1009110172627570106101104

%RPD(a)

6.94.86.74.816.46.10.0

7.71.110.40.01.64.110.5 '1.91.06.5

(a)-Percent Relative Difference=(high-low)average X 100

ftR3'l5l78APPENDXX G " . 17

Table G-9. Duplicate Analysis Resultls for Fly Ash Run 5 (pg/g)

DIOXINS2378TCDD12378PeCDD123478HxCDD123678HxCDD123789HxCDD1234678HpCDDOCDDFURANS2378TCDF12378PeCDF23478PeCDF123478HxCDF123678HxCDF234678HxCDF123789HxCDF1234678HpCDF1234789HpCDFOCDF

Field ID 5244Extract ID 36809MS File H97B251-9

11(0.0671)U(0.141)U(0.110)U(0.0980)U(0.120)3.73

U(6.01EMPC)

U(0.0763)U(0.0884)

U(0.648EMPC)1.190.8370.630

U(0.0669)3.00.46

U(0.161)

5244 DUP36820 Average

H97B251-5 Recovery

U(0.887)U(0.149)

U(0.202EMPC)U(0.478EMPC)

U(0.189)U(4.24EMPC)

5.71

0.925U(0.159)U(0.155)

U(1.15EMPC)U(0.269EMPC)U(0.998EMPC)

U(0.114)U(3.15EMPC)U(0.137)

2.78"

NCNCNCNCNCNCNC

NCNCNCNCNCNCNCNCNCNC

%RPD(a)

NCNCNCNCNCNCNC

NCNCNCNCNCNCNCNCNCNC

(a)-Percent Relative Difference=(high-low)average X 100U(Detection limit)-U Not detected with noise based detection limits in pg/gU(conc. EMPC) EMPC- Est. Max. Possible Concentration given as the detection limit in pg/gNC-Value not calculated due to U or EMPC value

A R 3 I 5 I 7 9APPENDIX G IS

Appendix H

Report on Chemical Analysis Results for Herbicides


aR3i5l80

Appendix H: Report on Chemical Analysis Results for Herbicides inRisk Burn No. 2

Three Flyash, three Bottom Ash, and three Solid Feed samples were analyzed forherbicides from Risk Burn No. 2. (These samples were also sent to EnvironmentalChemical Coloration (ECC) for Fenac analysis. Those Fenac results were included in thereport, Section 3.12).

Sample preparation was performed using ECC, standard operating procedure (SOP)No. 93-26 "Chlorinated Herbicides," dated February 23, 1993 and revised February 19,1996. For analysis, this was supplemented by EPA SW-846 Method 8151 and MidwestResearch Institute (MRI) standard operating procedure (SOP) CS-AMP-23, "Analysis ofFenac in Air Samples by Gas Chromatography/Electron Capture Detector (GC/ECD) forthe Drake Superfund Site." The following sections provide information related to thereceipt, preparation, analysis, results, and quality control (QC) of the samples submittedfor herbicide analysis from Risk Burn No. 2

1.0 Sample Receipt

Risk Burn No. 2 samples were received at MRI on February 11, 1997 at 6:30 P.M.The samples were received in good condition. Evidence tape attached to the samplecoolers and sample boxes was intact upon sample receipt. All samples were cold uponreceipt. Samples were stored in the MRI cold room until relinquished to sampletechnicians for processing.


Samples for Risk Burn No. 2 were prepared on February 20, 1997 using the ECCprocedure. Sample preparation involved weighing 5 grams of each sample and mixing itwith 5 grams of sodium sulfate. This mixture was then added to a chromatographiccolumn. An alkaline acetone/ether solvent mixture was passed through thechromatographic column containing the sample. This removed any herbicides present inthe samples as alkaline salts. Then, acidic ether was passed through the chromatographiccolumn containing the sample. This step removed any herbicides present in the samples asesters or free acids. Four acidic ether washes were performed. Herbicides contained inthe alkaline acetone/ether mixture and the combined acidic ether washes were transferredto an alkaline water solution through a separatory funnel transfer. The alkaline water,containing herbicides as salts, was acidified with hydrochloric acid (HC1) to obtain ahydrogen ion content (pH) of less than 2. The acidic water, containing the herbicides asfree acids, was passed through a C-18 solid phase extraction (SPE) column. The free-acidherbicides, now bound to the SPE C-18 packing, were eluted from the SPE column with 3ether washes. A diazomethane solution was added to the sample extract to convert theherbicides from free-acids to methyl esters. Ethyl ether was removed from the sampleextracts with a nitrogen blow-down apparatus and hexane addition. The sample extractswere brought to a final volume of 10 milliliters (mL) with hexane.

A R 3 I 5 I 8APPENDIX H

3.0 Sample Analysis Method

The ECC procedure describes analysis, but is rather general. Therefore, analyses alsoutilized EPA SW-846 Method 8151 and MRI SOP CS-AMP-23. These methods utilize agas chromatograph (GC) equipped with an electron capture detector (ECD) for herbicideseparation and detection. These procedures do not involve any significant deviations fromthe ECC procedure. Table H-l summarizes the analytical equipment used for herbicideanalysis along with the operating conditions of the equipment.

Table H-l: Analytical Equipment and Operating Conditions

Component or ParameterGas ChromatographCarrier Gas.Make-up GasPrimary Analytical Column

Confirmation Analytical Column

GC Conditions

DetectorAutosamplersInjection volumeData System

Type or SettingHewlett-Packard 5890 Series IIHelium, 7 ml/minute flow rateNitrogen, 60 ml/ minute total flowDB-1701, 30 meters x 0.53 mm I.D.

1,0 |jm film thicknessDB-608, 30 meters x 0.53 mm I.D.

0.83 (jm film thicknessInitial Temp: 70°C hold for 2 minutesRamp 15°C/min to 170°CRamp 4°C/min to 300°C hold for 4 minutesInjector: oncolumn injectionDetector: 325°CDual Electron Capture Detectors (ECD)Two HP-7673 autosamplers2.0 |JLPE Nelson Turbochrome version 3.3

Standards were injected into the GC to determine retention time windows andresponses for each of the herbicides. Sample extracts were then injected into the GC andcompared to the standards to identify and quantify herbicides present in the sample. Thiscomparison was first performed with the primary column. When herbicides wereidentified in samples with the primary column at concentrations exceeding the practicalquantitation limit (PQL), the confirmation column data was evaluated to provide definitiveidentification of the herbicides present in the samples.

4.0 Sample Results

Risk Burn No. 2 samples were analyzed for herbicides on February 24 throughMarch 4, 1997. Results for samples are shown in Table H-2. No herbicides withconcentrations exceeding the PQL were identified in any of the Fly Ash samples. Dalaponwas identified in all three Fly Ash samples at concentrations greater than the MDL.Dalapon also was identified in the method blank sample and these results are discussedlater in Section 5.0. The herbicide 2,4,5-T was identified in the Fly Ash Run 7 sample at a

A R 3 1 5 I 8 2APPENDIX H

1/3«J

"a|GO

u

O^c3

jt/>

P*

J>

"S

r/

Herbicide I

<•.o

1£31/3fM

SC

™"

£

c "- in = S g >

CO V~'

mlo°5c "- in

CO "

j-tO -v

O ^mx:

co to o en= E •* 5 o £ o>Cd t! co 3.o ^

CQ

.Ctoin to 0 'Sc E "* =£=5 O £J CDO ^^m

"if §1

Hif3 >,CM "5)Qi LL u 3_

~ N* -

||l

S~*

Q ^ HL

**~*

(fl

ico

:DCMV

IDinv

I)

v

CO,O)OJ

in'CO

~ 3KO•I™

mCMV

inv

inCMv

inCMv

mCM

Q

CN

CO"*

—3

^

COCO

V

$

^CMV

inCMV

inCMv

mCMv

IDmV

mCM

COQ

CM"

h-.

T~

CM

T"

_jin(Njo>

COCMV

IDcoCMV

r>COCMV

— J

CO

DCOCMV

IDCOCMV

DcoCMV

COCM

SCN

sCM

CO

V

-JCMCO

COCM'v

IDcqCMV

=3<PV

13CD

COCMV

COCMV

IDCOCNV

COCN

O.

CM"

CD _,

04 0l CCO

-3 — J ^CN 0CN m1CO y

|(°. 0

CO

r- COMCO CO"CO .«Q Q

-i ^CN <QCO <M* V

_, DN. «?CO CN^~ V

D =>« SCM CMv V

3 =>« SCM (Nv V

21CM CNV V

-) D•0 ^CM CNV T~v

alv v

s 1v V

2 aCM CMV V

Mv v

« sCM <N"~

Q.SQ.o no SJC 0o cQ Q

raOCOOOCO

a

COoin

"ooCOcoCM

Doom_

DO0ooo"v3Ooooo"<(—V

IDooinCM"v

ID0omCM"v

13ooinCM"v

DooCM"v

ooinCN

<Q.O5

DOOoo_o"T-V

Ooooo"Voooo"V

IDo0oo_

VDOo0oo"V

z>Ooooo"T—V

r>oo0in"v

IDoo0m"v

oooin"v

D0gin"v

oo0m"

0_Q.O5

0) gm °

Q fO° ^

co J2

• - tnCO -*

CO COr co

CM OCO O)

CO •<*•

O O)co co

CO CO

CD COCO CO

$ 2 £> L. S £o §,§ §:g,a:Q 0 0 °gO5 t o fc: oCM" co o: H to cc

COJ3

o

'5 TJ

0) .:S

1" 18 !>> c1 iT) *

1 '" 3u- oS a.

! iO CD" 3 £ss TJ"O CTJ COi -J -fi gg§ as a>> . e c•Jj CO CO

"- w woj a> </></)£ £ — —to c "> wCD co CO CO

'a *- S Sc ^ .® ..g TO CO CO

fillil O o O5 *= o o8 2 m m

illlc o . „(u O c; c"to E E^ -a 3 3S Q) O OJ> *- o o5 CD 2 5>o "S3 co coCD 2 .E .E£ ° Q. Q.CO CO CDco 3 £: TJ^Si•i -2 1 1•sjll.ts 3!. o oE co Si 2£= C CD CDc CO TJ TJO (A CO COv- co co cocu > > >tS "O "D TJ« c e c"333

1 1" 1" °"^-* ci c c

_jQ CQ

O°

=O

0)TJ4O

wCD

TJ3 Co Ec .3I 8<B C"

a or\ l ~c^ csis

£ '•§ cc § -cQ LJZJ •*-*

1 § i"S ni °

C c*"E '•£ c— Q..°O CD CO

co 2 =

£ ° 55^p

HICD .£ w

Ij'sg 2 §* "° TJ^ -C «I 2 o

concentration slightly greater than the MDL. These were the only herbicides identified inthe Fly Ash samples.

No herbicides with concentrations exceeding the PQL were identified in any of theBottom Ash samples. MCPA was identified in the Bottom Ash Run 5 and Run 6, andMCPP was identified in all three Bottom Ash samples at concentrations exceeding thePQL during the primary column analysis of the sample extracts. The confirmation columnanalysis of these sample extracts determined that MCPA and MCPP were not present.The reported MDL values for MCPA and MCPP in these samples were raised to indicatethe MDL of the confirmation column. Dalapon was identified in all three Bottom Ashsamples at concentrations greater than the MDL. Dalapon also was identified in themethod blank sample and these results are discussed later in Section 5.0. The herbicide2,4-D was identified.in all three Bottom Ash samples at concentrations ranging from 29.6micrograms per kilogram (ug/kg) to 107 ug/kg. These values were all greater than theMDL for 2,4-D.

MCPP was identified in all three Solid Feed samples at concentrations exceeding thePQL during the primary column analysis of the sample extracts. The confirmation columnanalysis of these sample extracts determined that MCPP was not present. The reportedMDL values for MCPP in these samples were raised to indicate the MDL of theconfirmation column. No other herbicides with concentrations that exceeded the PQLwere identified in the solid feed samples. A number of herbicides were identified in theSolid Feed samples with concentrations greater than the MDL. Dalapon was identified inSolid Feed Run 5 and Run 7 samples with concentrations of 65.2 ug/kg and 217 ug/kg,respectively. Dalapon also was identified in the method blank sample and these results arediscussed later in Section 5.0. MCPA was identified in all three Solid Feed samples withconcentrations ranging from 28,600 ug/kg to 50,390 ug/kg. Results for MCPA wereobtained from the confirmation column due to interferences present in the primary columnanalysis of the sample extracts. 2,4-DB was identified in all three Solid Feed samples withconcentrations ranging from 369 ug/kg to 467 ug/kg. 2,4,5-T was identified in all threeSolid Feed samples with concentrations ranging from 9.25 ug/kg to 11.7 ug/kg. 2,4,5-TPwas identified in Solid Feed Run 5 and Run 7 at 3.21 ug/kg and 2.64 ug/kg, respectively.Dicamba was identified in all three Solid Feed samples with concentrations ranging from14.6 ug/kg to 20.9 ug/kg. Dichloroprop was identified in Solid Feed Run 6 and Run 7 at167 ug/kg and 43.2 ug/kg, respectively.

5.0 Quality Control (QC) Results and Data Quality Assessmenti

The data quality assessment of Risk Burn No. 2 samples for herbicide analysis includesan evaluation of sample holding time requirements; standard calibration procedures; QCresults for method blank samples, surrogate recoveries, and laboratory control spike(LCS) sample results. The following paragraphs give the results of each of theseevaluations. The end of these section provides a summation of the data quality assessmentof the herbicide data for Risk Burn No. 2 samples.

A R 3 I 5 1 8 1 4APPENDIX H

The herbicide technical holding time requirements are 14 days from sample collectionto sample preparation, and 40 days from sample collection to sample analysis. Samples forRisk Burn No. 2 were collected on February 7 through February 9, 1997. Samples wereprepared on February 20, and analyzed from February 24 through March 4, 1997. Theholding time requirements for the herbicide analysis of Risk Burn No. 2 samples were met.

Standard calibration for the herbicides involved the analysis of eight concentrationlevels of a mixture containing all of the herbicides, with the exception of the surrogate:Triclopyr. This mixture contained the herbicides as methyl esters. The Triclopyr standardcontained Triclorpyr as a methyl ester and included six concentration levels.

Both, the primary and confirmation columns were used for sample quantitation. Theconfirmation column was used to provide a definitive identification for the presence ofherbicides in the samples, and to quantitate herbicides in samples exhibiting interferenceswith the primary column.

An initial calibration (ICAL) was performed by analyzing each of the standards usingthe analytical conditions listed in Table H-l. Retention time windows for each herbicide.were determined by applying a ± 0.05 minute window around the mean retention timedetermined from the ICAL. Calibration curves were generated for each herbicide using acalibration curve with a first order fit. The herbicide concentration was plotted versus thepeak height response obtained from the analysis of the standard. In order to obtaincorrelation coefficients of 0.99 or greater, some of the higher concentration standardswere removed from the curve. For all herbicides, with the exception of Trichlopyr, atleast five standard concentration levels were used to create the calibration curve. Threestandard concentration levels were used to create the Trichlopyr calibration curve.

Independent check standards (ICS) were used to evaluate the accuracy of the workingherbicide standards. The ICSs were prepared from a different source than the herbicideworking standards. MRI SOP CS-AMP-23 requires that the percent accuracy of the ICSsshould be within ±10 percent of the true value. The percent accuracy for all of the ICSstandards was within ±10 percent of the true value when quantified against the ICALstandards, with the exception of 2,4-DB which was within 12.8 percent of the true value.

Continuing calibrations were performed after the analysis of every 10 sample injectionsand at the end of the analytical run. MRI SOP CS-AMP-23 states that the continuingcalibration standards should quantify within 75-125% of the initial calibration. Allcontinuing calibration standards met the 75-125% requirement, with the exception ofDalapon, Dinoseb and Dicamba in one continuing calibration. Dinoseb and Dicamba bothprovided 130 percent recovery from the response in the ICAL. Dalapon provided 128%recovery. These percent recoveries were slightly greater than the 75-125% percentcontrol limit.

A method blank sample was prepared and analyzed along with the Risk Burn No. 2samples. Dalapon was found in the method blank sample at a concentration exceeding theMDL. The Dalapon concentration in the method blank sample was 322 ug/ kg. Samplesfound to contain Dalapon with concentrations less than five times the amount found in the

A R 3 I 5 I 8 5

method blank sample were qualified with a "B" to indicate that the sample result may havebeen affected by positive results found in the method blank sample.

Surrogate standards were added to all of the samples to evaluate the sample extractionand analysis efficiency. Two surrogate standards were added to each sample, 2,4-dichlorophenyl acetic acid (2,4-DCAA) and Trichlorpyr. Surrogate recoveries for each ofthe Risk Burn No. 2 samples are shown in Table H-2. Surrogate recoveries in samplesranged from 37 to 134 percent recovery. The surrogate recovery QA objective is 50 to160 percent. Surrogate recoveries for 2,4-DCAA were less than the control limits for theFly Ash Run 7 sample (37 %) and the Solid Feed Run 6 sample (40 %). Surrogaterecoveries for Trichlopyr were less than the control limit for the Fly Ash Run 7 sample (47%) and for the Bottom Ash Run 7 sample (45 %).

LCS samples were analyzed to evaluate the accuracy of the herbicide analyticalmethod. MRI SOP CS-AMP-23 establishes a 25 to 125 percent recovery control limit forthe LCS. The following list provides the percent recoveries of herbicides in the LCSs.

LCS Percent LCS PercentHerbicide Recovery (%) Herbicide Recovery (%)

2,4-D 63 Dichloroprop 712,4-DB 22 Dinoseb 792,4,5-T 71 MCPA 502,4,5-TP 75 MCPP 70Dalapon 33Dicamba 95

Only 2,4-DB provided a LCS percent recovery outside of the 25 to 125 percentcontrol limit. This compound has historically provided low recovery using this method.

The data quality assessment of the herbicide data was performed based upon sampleholding time criteria,* standard calibration acceptance criteria and the results of QC data.The impact of this assessment on Risk Burn No. 2 sample results are detailed in thefollowing paragraphs.

All of the Risk Burn No. 2 samples for herbicide analysis were extracted and analyzedwithin the technical holding times.

The samples were analyzed with acceptable ICALs. The independent check standard(ICS) for 2,4-DB was outside of the ±10 percent of the true value. 2,4-DB was within12.8 percent of the true value, slightly outside of the control limit. This was not viewed asadversely effecting the quality of the data generated and no corrective action was taken.The percent recoveries for Dinoseb, Dalapon, and Dicamba in one continuing calibrationstandard were outside of the 75-125 percent control limit established in the MRI SOP CS-AMP-23. The percent recoveries for these herbicides in the continuing calibrationstandard were slightly greater than the 75-125% control limit. This was found to have aninsignificant impact on the reported sample results since the concentration of Dicamba

A R 3 I 5 1 8 6APPENDIX H 6

reported in any of the samples never exceeded 20 percent of the PQL. No correctiveaction was taken for these exceedences.

Dalapon was identified in the method blank sample at a concentration greater than theMDL. Samples found to contain Dalapon at a concentration of less than 5 times theamount found in the method blank sample were qualified with a. "B" to indicate that thereported sample amount may have been caused by an artifact or interference present in thesample preparation or analysis methods.

Recovery of herbicides in the LCS sample were within the 25 to 125 percent controllimit established in MRI SOP CS-AMP-23, with the exception of 2,4-DB. 2,4»DB percentrecovery in the LCS was 21 percent, slightly below the 25 percent lower control limit.2,4-DB was not found in the Bottom Ash or Fly Ash samples. It was found in the SolidFeed samples at concentrations ranging from 369 to 467 ug/kg. The low recoveryillustrated in the LCS may indicate that the concentration of 2,4-DB in the Solid Feedsamples may be greater than the reported sample values.

A R 3 I 5 I 8 7APPENDIX H

Appendix I

Report on Chemical Analysis Results for VOCs

MRI-AppEed/R362028.APP

AR3I5I88

APPENDIX I Report on Chemical Analysis Results for VOCs forRisk Burn No.2

Author: Jon Onstot, Senior Mass Spectrometrist, Chemical Sciences Department

This appendix describes the procedures and results for the OHM Risk Burn No. 2 volatileorganic compound (VOC) analysis. The scope of work included purge-and-trap GC/MSof VOST condensate water, waste feed, and fly ash and bottom ash using SW-846Methods 5030/8260, and VOST desorption GC/MS of VOST sorbent cartridges usingMethods 5041/8260. Additional VOST and VOST condensate samples were analyzed forselected volatile analytes using selected ion monitoring (SIM) GC/MS. The list of targetanalytes for the full scan analyses is shown in Table 1-1. The SIM analysis was done forthe same list of compounds except benzene and 2-butanone. Table 1-2 A shows the list oftarget analytes for the feed samples and Table I-2B for the ash samples.

The full scan GC/MS analysis data for the VOST trap samples were also used totentatively identify and semiquantify the 20 largest peaks; i.e., tentatively identifiedcompounds (TICs).

1.0 Sample Receipt

All samples were received from Brad Deck, the MRI Chemical Sciences Departmentsample custodian. Samples were received cold and intact on delivery with the exception ofone SIM VOST condensate sample (Run 5 Train B, Sample No. 5233) which was brokenin shipment. The samples were transferred to a refrigerator in a VOC-free laboratory untilanalysis.


2.1 VOST

No sample preparation was performed on the VOST cartridges prior to analysis.

2.2 VOST condensate

VOST condensate samples were prepared by transferring a 5 ml aliquot of sample to a 40ml Dynatech VOC autosampler vial and spiking with 5 ul of internal standard/surrogatestandard solution (250 total ng per surrogate). The condensate sample from Train A,Run 5 was analyzed by full scan and SIM since the -condensate sample from Train B, Run5 was broken in shipment.

2.3 Ash

Flyash samples were prepared by transferring a 5 g (+/0. Ig) aliquot to a 40 ml DynatechVOC autosampler vial and spiking with 5 ul of internal standard/surrogate standard

A R 3 1 5 I 8 9APPENDIX I

solution (250 total ng per reference analyte). Bottom ash samples were prepared asdescribed above with the exception that 1 g aliquots were used.

2.4 Waste Feed

Waste feed samples were prepared by transferring a 1 g (+/- 0. Ig) aliquot to a 40 mlDynatech VOC autosampler vial and spiking with 5 ul of internal standard/surrogatestandard solution (250 total ng per reference analyte).

3.0 Sample Analysis

All analyses were performed on a Fisons MD800 GC/MS system equipped with an 014560 Purge-and-Trap Concentrator and a Dynatech PTA30 W/S autosampler. VOSTsamples were desorbed using an MRI-designed and fabricated thermal desorption unit.Operating parameters for each of the components listed above are provided in Table 1-3

3.1 VOST full scan

Analyses of VOST samples were performed according to SW-846, 5041 and 8260 asreferenced in 5041. Modifications to those methods used for this work included the use ofa Vocarb 3000 analytical trap for the purge-and-trap step. This trap was madecommercially available after the last promulgated versions of the methods. However, thelatest proposed revision to the methods (5030B, Rev. 2, 1/95) lists Vocarb 3000 as anapproved alternate trap material. This modification was described in the Trial Burn Plan.

A five-point initial calibration curve (50-1000 total ng on-column) was analyzed prior toanalysis of samples. In addition, the following analyses were performed at the beginning ofeach 12-hour shift: instrument performance check standard (25 ng 4-bromofluorobenzene)daily calibration check standard (250 ng on-column) and daily system blank (blank frontand back cartridges with 250 ng IS/surrogate mix spiked onto Tenax front cartridge).

All field samples were analyzed within the 14-day holding time. All samples weresuccessfully analyzed, i.e. reportable data was obtained for all samples.

3.2 VOST SIM

All analytical parameters described above for the VOST full scan analysis were also usedfor the VOST SIM analysis, with the following exceptions: 1) the initial calibration rangewas 0.5-25 ng on-column and 2) the mass spectrometer acquired data for only twocharacteristic masses per analyte during acquisition.

All VOST SIM field samples were successfully analyzed with the 14-day holding timeexcept for samples collected during Run 5B. Those samples were anajyzed one day afterholding times had expired due to unexpected delays in setting up the GC/MS system forSIM analysis.

A R 3 I 5 I 9 0APPENDIX I

i

3.3 VOST condensate

Analyses of VOST condensate samples were performed according to SW-846 Methods5030 and 8260. A modification applied to the work included the use of a Vocarb 3000analytical trap for the purge-and-trap step. This modification was described in the TrialBurn Plan. Also, a surrogate recovery objective of 70-120% was applied for thecondensate purge-and-trap, the same as for ash samples.

VOST condensate samples were analyzed by both full scan and selected ion monitoringGC/MS. For full scan analysis, a six-point initial calibration curve (5-200 total ng/ml) wasanalyzed prior to analysis of samples. In addition, the following full scan analyses wereperformed at the beginning of each 12-hour shift: instrument performance check standard(25 ng 4-bromofluorobenzene) daily calibration check standard (25 ng/ml on-column) anddaily system blank 5 ml VOC-free water spiked with IS/surrogate mix. For SIM analysis, afive-point calibration curve (0.1-5 ng/ml) was analyzed prior to analysis of samples. Inaddition, the following SIM analyses were performed at the beginning of each 12-hourshift: instrument performance check (25 ng BFB) and daily system blank (5 ml VOC-freewater spiked with IS/surrogate mix). A daily calibration check standard was not analyzedfor the SIM analysis since all analyses, including the initial calibration curve and fieldsamples, were performed in a single twelve hour shift.

All VOST condensate field samples were analyzed within the 14-day holding time. Allsamples were successfully analyzed, i.e. reportable data was obtained for all samples.Please note that sample No. 5233 (SIM VOST condensate, Train B) was broken inshipment and was not analyzed. The full scan VOST condensate sample from Train A(No. 5232) was analyzed via SIM in its place.

3.4 Ash

Analyses of ash samples were performed at the same conditions as described for the fullscan VOST condensate samples. All field samples were successfully analyzed within the14-day holding time. However, one sample, No. 7241 (Run 7 bottom ash) had to be rerunbecause the original analysis failed internal standard recovery criteria caused by a leakduring the purge cycle. This was not noted at the time of analysis, as it should have been.The sample was rerun on 3/7/97, 12 days after the sample's holding time had expired.

3 . 5 Waste Feed , . " , . . . .

Analyses of waste feed samples were performed at the same conditions as those describedfor the full scan VOST condensate samples. All field samples were successfully analyzedwithin the 14-day holding time.

4.0 Sample Results

Results for the analysis of VOST and VOST condensate samples are provided in Section3.3 of the Risk Burn Report (including TICs) and results for the analysis of ash samples

A R 3 I 5 I 9 . IAPPENDIX I

are provided in Section 3.9 of the Risk Burn Report. A discussion of observations andproblems encountered during sample analysis is provided below.

Benzene levels in the VOST field samples consistently exceeded the initial calibrationrange and saturated the GC/MS detector. Therefore, the benzene was quantified using asecondary ion m/z 79 (C-13 isotope of the molecular ion) in order to maintain theresulting peak area counts below the instrument saturation level. Since the benzene levelexceeded the calibration range, the reported results should be considered as estimatedvalues.

5.0 QC Results and Data Quality Assessment

Data quality for this work was demonstrated via the following QC parameters:

• initial and continuing calibration standards• daily system blanks• duplicate sample analyses for one run on VOST condensate, waste feed and ash

samples• surrogate recovery for d4-l,2-dichloroethane, bromofluorobenzene and d8-toluene in

all VOC samples

Results for each of the QA parameters listed above are discussed below.

All initial and continuing calibration standards passed Method 8260 performance criteriafor Calibration Check Compounds (CCCs) and System Performance Check Compounds(SPCCs).

Surrogate recoveries for VOST, VOST condensate, waste feed and ash samples aresummarized in Table 1-4. Recoveries which failed the Risk Burn Plan criteria are indicatedin the table as shaded cells (70-120% for ash samples; 75-125% for VOST samples).

Recovery of d8-toluene was biased high for the bottom ash samples and recovery of BFBwas biased high for the waste feed samples. The cause of the high bias was notdetermined. In addition, d4-l,2-dichloroethane showed high recovery in the VOST fieldsamples which was attributed to its coelution with benzene. The levels of benzeneobserved in the VOST field samples (>3000 total ng) resulted in significant interference tothe surrogate quantitation mass response. The VOST field blanks were not exposed tothese benzene levels and thus the d4-DCE surrogate recovery in those samples passedcriteria. Recovery for BFB was low (54%) in one VOST full scan sample and high (153%)in one VOST SIM sample.

Results for the analysis of duplicate sample analyses are shown in Tables 1-5 through 1-9for bottom ash, fly ash, full scan VOST condensate, SIM VOST condensate and wastefeed samples, respectively. All duplicate samples passed the Risk Burn Plan precisionrequirement of <35% relative percent difference, with the exception of toluene in thewaste feed duplicate analysis (41%) attd four analytes in the VOST condensate SIM

duplicate analysis: chlorobenzene,m 2-hexanone, styrene and o-xylene. Please note thatthe RPDs greater than 35% noted above do not include analytes which were below PQL .(J flagged data). Duplicate sample results are not reported for VOST since those samplesare completely expended in a single analysis and thus cannot be analyzed in duplicate. .


Table 1-1. Volatile Organic Compound Analytes inStack Gas Samples (VOST Method 0030)

Compound

Benzene

2-Butanone (MEK)

Carbon tetrachlorideChlorobenzene

Chloroform

1,2-Dichloroethane1,1-Dichloroethene

Tetrachloroethene

Toluene

1,1,1-TrichloroethaneTrichloroethene

Vinyl chloride

Bromodichloromethane

BromoformBromomethane

Carbon disulfide

ChloroethaneDibromochloromethane

frans-1,2-Dichloroethene

Ethylbenzene

2-Hexanone

Methylene chloride

4-Methyl-2-pentanone

Styrene

Trichlorofluoromethane

Vinyl acetate

o-Xylene

m,p-Xylene

Xylenes (total)

A R 3 I 5 I 9 UAPPENDIX I

Table I-2A. Full Scan VOC Analytes(waste feed samples only)

Benzene EthylbenzeneToluene Trichloroethene

cis-l,2-Dichloroethene m-/p-Xylenet-l,2-Dichloroethene o-XyleneTetrachloroethene Chlorobenzene

f l R 3 l 5 i 9 5APPENDIX I

Table 1-2

-

B. Volatile Organic Analytes in Ash SamplesCompoundChloromethaneBromomethaneVinyl ChlorideChloroethaneMethylene ChlorideAcetoneCarbon Bisulfide1,1-Dichloroethene1,1-Dichloroethanefrans-1 ,2-DichloroetheneChloroform1,2-Dichloroethane2-Butanone1,1,1-TrichloroethaneCarbon TetrachlorideVinyl AcetateBromodichloromethane1 ,1 ,2,2-Tetrachloroethane1 ,2-Dichloropropanefrans-1 ,3-DichloropropeneTrichloroetheneDibromochloromethane1 ,1 ,2-TrichloroethaneBenzenec/s-1 ,3-Dichloropropene2-Chloroethyl Vinyl EtherBromoform2-Hexanone4-Methyl-2-pentanoneTetrachloroetheneTolueneChlorobenzeneEthylbenzeneStyreneTotal Xvlenes


Table 1-3. GC/MS Operating Parameters Used for VOC Analysis

1. Mass SpectrometerModel: Fisons MD800S can Range: 35-350amuScan Rate: 0.5 s/scan + 0.1 s InterScan (100 scans/min)Source Temperature: 200 CTransfer Line Temp: 200 C

2. Gas ChromatographModel: Fisons GC8000Column: J&W DB624 30m x 0.53mm; 3um thicknessProgram: 10 C, 4min hold, 10/min to 200 CCarrier/Flow: Helium, 30 cm/sec (5 psi)

3. Purge-and-TrapModel OI Analytical 4560 / Dynatech PTA30 W/SAnalytical Sorbent Trap: Vocarb 3000 (Supelco)Purge Time/Temp.: 11 min, 40 CDesorb Time/Temp.: 4 min, 250 CBake Time/Temp.: 12 min, 250 CTransfer Line Temp.: 150 CCarrier/Flow: Helium, 40 ml/min

4. VOST DesorberModel: MRJ custom designMode: Dual cartridge desorption (front and back traps desorbed

simultaneously)Desorb Temperature: 180 CCarrier/Flow: Helium, 30 cm/min through each cartridge; 60 ml/min total

flow.

A R 3 I 5 I 9 7APPPMHTV T

Table 1-4. OHM Risk Burn No. 2Surrogate Recovery Summary

Sample TypeBottom AshBottom AshBottom AshBottom AshBottom Ash MSBottom Ash MSDFly AshFly AshFly AshFly AshFly Ash MSFly Ash MSDWaste FeedWaste FeedWaste FeedWaste FeedVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST / Full ScanVOST CondensateVOST CondensateVOST CondensateVOST CondensatePurge-and-Trap BlankPurge-and-Trap BlankPurge-and-Trap BlankPurge-and-Trap BlankVOST /SIMVOST /SIMVOST / SIMVOST /SIMVOST /SIMVOST / SIMVOST /SIMVOST / SIMVOST / SIMVOST /SIMVOST /SIMVOST /SIMVOST Cond. / SIMVOST Cond. / SIMVOST Cond. / SIMVOST Cond. / SIM

Sample Description52385238 DUP6238.72385238523852435243 DUP624372435243524352495249 DUP62497249Run 5 / FBRun 5 / Pair 1Run 5 / Pair 2Run 5 / Pair 3Run 5 / Pair 4Run6/FBRun 6 / Pair 1Run 6 / Pair 2Run 6 / Pair 3Run 6 / Pair 4Run7/FBRun 7 / Pair 1Run 7 / Pair 2Run 7 / Pair 3Run 7 / Pair 4523262326232 DUP72321/24/971/28/971/30/971/30/97Run5/FBRun 5 / Pair 1Run 5 / Pair 2Run 5 / Pair 3Run6/FBRun 6 / Pair 1Run 6 / Pair 2Run 6 / Pair 3Run7/FBRun 7 / Pair 1Run 7 / Pair 2Run 7 / Pair 35232*62336233 DUP7233

d4-1 ,2-Dichloroethane11010310290113112113112116120107 ,101116113

:':;i:«i;iii:ii:-::i22:" ",:'.".': ,113109

;;r::::: '••'• 14$;"':'::.: ".:" '.';Ji'i; ;->;::. m^; -\::"h;!«t:h':-'-:;::.154'!::::.. : ;.!fi;:;:::r'.:-.::i :::;:V:'-":"

106::::,:::::•:•. ;V}77-;::::!::::: :- ;.:166::: : ,:::!:':"';:;::-;162:V'" .':. . .; • : ; . . ; : ' : :"181 , • : • • ;

106: 168'

176321

"'•:•.• 178949610196999797101105

':...-:;:f..-l73..'..

:'-":::: •' .215.. "",,'.:•': :.:••;'•'.'.'. '201 . • '•

103.t:;:;;';!::: 18S:'::; ". .

Ti;;:;:;;:n!":!:i89f::. ' '.'..:in::: :: ::189 , '. .I!: ,:

95:!;!:;!;;;;;;:!:;:•: i-:: : .l-::::/':',:,,,.or -ias';,, '

949610196

Surrogate Recovery (%)Bromofluorobenzene

807980

•'•'••• " ,66:: ' •88100

".••:' ' :.)&•'•••:'•• . I ' ! ."'117

, , ^ . . . ^ . . urf)C • • • • • • •!•••; . ; ; : • : ' , : : : • » *v ... : ... ; • :

1208671

:., :. . 134,, A; ^

•.- '•• '.• 131.:.:.:... ...:;.•.;.• '.•129.:::..:.::.'.. .

•/.. ' ' :128:: . • ,:.. . ,._.

1231191201199011811711911693118114541149316311388105106105107981531121049011010310788108931079616311388

d8-Toluene157

' ••'-•-•••139•• ' • - IBS/":

,135;:".,. 142

••" . .124.".:. '..-..:..... 63, ; :: . •:

134- ; . •- •:, ' 13$:, ,.,:•:"..::.:::

7596

; ' - - :.163 :- J-:-:.60, ,.--"-7672'132:.. ,............................

1141111071061051009910298104100961099878100766810710610610610811298981141051029311390103100781007668

Shaded values failed 70-120% surrogate recovery criteria specified in Risk Burn Plan.* Sample 5232 analyzed by SIR in place of 5233 which was recieved broken.

A R 3 I 5 I 9 8APPENDIX I 10

Table 1-5. OHM Risk Burn NO. 2Bottom Ash Duplicate Analysis Summary (jig/kg)

AnalyteChloromethaneBromomethaneVinyl Chloride ,ChloroethaneMethylene ChlorideAcetoneCarbon Disulfide1,1-Dichloroethene1,1-Dichloroethanet-1 ,2-DichloroetheneChloroform1 ,2-Dichloroethane2-Butanone1 ,1 ,1-TrichloroethaneCarbon TetrachlorideVinyl AcetateBromodichloromethane1 ,1 ,2,2-Tetrachloroethane1 ,2-Dichloropropanetrans-1 ,3-DichloropropeneTrichloroetheneDibromochloromethane1 ,1 ,2-TrichloroethaneBenzenecis-1 ,3-Dichloropropene2-Chloroethyl-vinyl ether (1)Bromoform2-Hexanone4-Methyl-2-PentanoneTetrachloroetheneTolueneChlorobenzeneEthylbenzeneStyrenem-/p-Xyleneo-XyleneTotal Xylenes

MDL0.80.91.20.70.820.80.50.30.50.52.50.73.00.50.61.70.82.60.60.70.21.02.00.50.95.01.43.22.90.50.50.40.40.30.40.30.4

523811.9J18.1 J

--

10.8 J-

5.7 J-----

16.1 J--

. --------

19.2------

10.8 J---

2.7 J-

3.9 J

5238 DUP10.6J16.9 J

--

9.8 J-

5.1 J-- •---.----------

16.9------

9.2 J---

2.2 J-

3.0 J

RPD (%)117-.10-11-----a-.--------13------16---.20-25

NotesRPD = Relative Percent Difference (%)a = Only one value was reported above the MDL.

B R 3 I 5 I 9 9APPENDIX I

Table 1-6. OHM Risk Burn No. 2Fly Ash Duplicate Analysis Summary (jj.g/kg)

AnalyteChloromethaneBromomethaneVinyl ChlorideChloroethaneMethylene ChlorideAcetoneCarbon Disulfide1,1-Dichloroethene1,1-Dichloroethanet-1 ,2-DichloroetheneChloroform1 ,2-Dichloroethane2-Butanone1,1,1-TrichloroethaneCarbon TetrachlorideVinyl AcetateBromodichloromethane1 ,1 ,2,2-Tetrachloroethane1 ,2-Dichloropropanetrans-1 ,3-DichloropropeneTrichloroetheneDibromochloromethane1,1,2-TrichloroethaneBenzenecis-1 ,3-Dichloropropene2-Chloroethyl-vinyl ether (1)Bromoform2-Hexanone4-Methyl-2-PentanoneTetrachloroetheneTolueneChlorobenzeneEthylbenzeneStyrenem-/p-Xyleneo-XyleneTotal Xylenes

MDL, 0.80.91.20.70.820.80.50.30.50.52.50.73.00.50.61.70.82.60.60.70.21.02.00.50.95.01.43.22.90.50.50.40.40.30.40.30.4

52432.0 J3.6 J

--

2.0 J-

0.5 J-----

3.4 J------------- '--------

'-

0.4 J

5243 DUP2.1 J4.1 J

--

2.2 J-

0.5 J----3.6------------------

0.8 J-----

0.4 J

RPD (%)1219--25-8---.aa-----------------a-----14

NotesRPD = Relative Percent Difference (%)a = Only one value was reported above the MDL.

ftR3i52QOAPPENDIX I 12

Table 1-7. OHM Risk Burn No. 2VOST Condensate Duplicate Analysis Summary (Full Scan)

AnalyteBenzene2-ButanoneCarbon TetrachlorideChlorobenzeneChloroform1 ,2-Dichloroethane1,1-DichloroetheneTetrachloroetheneToluene1 ,1 ,1-TrichloroethaneTrichloroetheneVinyl ChlorideBromodichloromethaneBromoformBromomethaneCarbon DisulfideChloroethaneDibrdmochloromethanet-1 ,2-DichloroetheneEthylbenzene2-HexanoneMethylene Chloride4-Methyl-2-PentanoneStyreneTrichlorofluoromethaneVinyl Acetateo-Xylenem-/p-XyleneTotal Xylene

MDL0.80.91.20.70.820.80.50.30.50.30.52.50.73.01.70.50.60.80.60.90.21.02.00.50.71.42.93.23.0

Concentration (ng/ml)Train A, Full Scan5232

-2.9 J

--

"---

0.7 J-----

6.0 J0.7 J

---

,0.2 J1.9 J---

1.9J---

5232 DUP-

3.8 J------

0.9 J-----

5.2 J0.6 J

----

0.6 J1.5 J

-

-----

RPD (%).14._.--.16-.---79.---4011---20--

• -

A R 3 I 5 2 0 !APPENDIX I 13

Table 1-8. OHM Risk Burn No. 2VOST Condensate Duplicate Analysis Summary (SIM)

AnalyteBenzene2-ButanoneCarbon TetrachlorideChlorobenzeneChloroform1,2-Dichloroethane1 , 1 -DichloroetheneTetrachloroetheneToluene1,1,1 -TrichloroethaneTrichloroetheneVinyl ChlorideBromodichloromethaneBromoformBromomethaneCarbon DisulfideChloroethaneDibromochloromethanet-1 ,2-DichloroetheneEthylbenzene2-HexanoneMethylene Chloride4-Methyl-2-PentanoneStyreneTrichlorofluoromethaneVinyl Acetateo-Xylenem-/p-XyleneTotal Xylene

MDL0.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.020.02

Concentration (ng/ml)Train B, SIM

62330.08 J0.63-

1.240.03 J

--

0.04 J0.23-

0.03 J-

0.03 J-

0.150.23---

0.160.160.06 J

-0.830.07 J

-0.620.940.04 J

6233 Dup0.08 J0.670.02 J4.330.03 J0.03 J

-0.10 J0.19-

0.09 J-

0.04 J-

0.10 J0.20---

0.115.060,06 J

-1.910.06 J

-0.280.510.10J

RPD (%)32a559a-3811-47-7-235---19941-395-373038

NotesMDLs are defined as PQL / 5 . Experimental MDLs were not determined.a = Only one value was reported above the MDL.

AR3I5202APPENDIX I 14

Table 1-9. OHM Risk Burn No. 2Waste Feed Duplicate Analysis Summary (fig/kg)

AnalyteBenzeneToluenecis-1 ,2-Dichloroethenet-1 ,2-DichloroetheneTetrachloroetheneEthyibenzeneTrichloroethenem-/p-Xyleneo-XyleneChlorobenzene

5249-

19.0---

16.92.6 J110.754.7331 .3

5249 DUP-

45.1--

'18.12.5 J123.559.5386.7

RPD (%)-41---32548

RR315203APPENDIX I 15

Appendix J

Report on Chemical Analysis Results for Metals


AR3.I5201*

*Appendix J:Risk Burn Number 2—Report on Chemical Analysis Results for Metals

1.0 Sample Receipt

Risk Burn Number 2 consisted of MM5-MM stack samples, solid waste feed samples, andbottom ash, fly ash, and scrubber water samples for metals analysis. Reference the Risk BurnNumber 2 complete sample listing in Appendix A.

The samples for Risk Burn Number 2 were received by Midwest Research Institute (MRI)at 6:30 p.m. on February 11, 1997. The boxes and coolers containing the samples had evidencetape which was still intact. All the samples designated for metals analysis were cold and intactupon receipt and were stored in the 330-E cold room until relinquished to Atomic SpectrometryFacility (ASF) personnel on February 19.

Before sample preparation, the weight of each stack sample container (excluding filters)was measured and recorded to verify that sample losses did not occur during shipment. Also, thepH of each front-half (FH) and back-half (BH) stack component (excluding the mercuryimpingers) was measured and found to be less than 2. The samples were stored in an ASFrefrigerator at approximately 4°C until sample preparation.


The samples were prepared for metals analysis according to the Trial Burn Plan for theDrake Chemical Superfund Site's Mobile Hazardous Waste Incinerator (Volume I, datedSeptember 20, 1996). Reference Appendix G of the Trial Burn Plan for the risk burn procedures.

a.

2.1 Stack Sample Preparation Methods

The metals procedures for the stack samples were in accordance with draft EPA Method29, "Determination of Metals Emissions from Stationary Sources" (dated April 1994), and EPASW-846 Method 7470A (Revision 1, November 1990), with the modifications listed in Table 6-2of the Trial Burn Plan. Quality control (QC) samples, including method blanks, simulated trainspikes, and filter reference materials, were also prepared according to Table G7-2C inAppendix G of the Trial Burn Plan.

Method 29 contains the sampling, sample recovery, sample preparation, and analysisprocedures for the determination of metals from stack emissions. For sample preparation, themetals' in the stack samples were solubilized/digested using nitric acid and hydrofluoric acid.

J-l

A.R3I5205APPENDIX J

Following digestion, Type I water was used to dilute the samples to a final volume, as describedin Method 29.

Method 7470A is a digestion and cold-vapor atomic absorption procedure for thedetermination of mercury in liquid samples. Reagents such as sulfuric acid, nitric acid, andpotassium permanganate were used to prepare 1 mL to 10 mL aliquots of the Method 29 stacksamples for mercury analysis. Type I water was used to dilute to a final volume of 200 mL, asindicated in the Trial Burn Plan Table 6-2 modifications to Method 7470A. Method blanks,laboratory control spikes, matrix spikes, and matrix spike duplicates were also digested as QCsamples.

2.2 Solid Waste Feed Preparation Methods

The solid waste feed samples were prepared according to the Trial Burn Plan, using EPA ,SW-846 Method 3050A (Revision 1, November 1990) with the modifications listed in Table 6-2of the Trial Burn Plan. After the digestion of approximately 1-g portions of each sample usingnitric acid and hydrogen peroxide, the samples were diluted to 100 mL with Type I water.Additional QC samples, including a method blank, laboratory control spike, matrix spike, matrixspike duplicate, and a sample duplicate, were prepared according to Table 14-2B of the QualityAssurance Plan portion of the Trial Burn Plan (Volume II, dated September 20, 1996).

These solid waste feed digests were then prepared for mercury analysis using Method7470 A, with the modifications listed in Table 6-2 of the Trial Burn Plan. An aliquot of each solidwaste feed Method 3050A digest (10 mL for the samples and method blank, and 1 mL for thelaboratory control spike and matrix spikes) was prepared; Type I water was used to dilute to afinal volume of 200 mL.

2.3 Ash and Scrubber Water Preparation Methods

The bottom and fly ashes plus an extraction fluid blank were prepared using EPA SW-846Method 1311 (Revision 0, July 1992)—Toxicity Characteristic Leaching Procedure (TCLP). Asper the method, approximately 100 g of each ash sample was extracted with an amount ofextraction fluid equal to 20 times the solid sample weight. After the 18 ± 2 h extraction andsubsequent filtration, the samples and blank were preserved with nitric acid to a pH of less than 2.

The scrubber waters fit into the liquid waste category according to Method 1311 and weretherefore defined as the TCLP extracts. These samples were filtered and preserved to a pH ofless than 2, as per the method.

The filtered and preserved extracts from above were digested using EPA SW-846 Method3010A (Revision 1, November 1990) and Method 3020A (Revision 1, November 1990). Afterthe digestion of 100-mL portions of each sample using nitric acid, the samples were diluted to 100mL with Type I water. Method 3010A also uses hydrochloric acid as part of the digestion

J-2

AR3I5206APPENDIX J

procedure. In addition, each of these digestion methods included the following QC samples: amethod blank, a laboratory control spike, and a matrix spike and matrix spike duplicate of oneextract, as described in Table G7-2A of the Trial Burn Plan.

The TCLP filtrates were also prepared for mercury analysis using Method 7470A,including the QC samples noted in the paragraph above. The initial sample size of each filtratewas 100 mL. The samples were digested and taken to a final volume of 200 mL as described inthe Method 7470 A modifications in Table 6-2 of the Trial Burn Plan.

3.0 Sample Analysis

As per the analysis requirements, the solid waste feed digests were analyzed for the sixmetals listed in Table G4-ld of the Trial Burn Plan (arsenic, beryllium, cadmium, chromium, lead, •and mercury); the ash and scrubber water digests were analyzed for the eight TCLP metalsspecified in Table G4-5 of the Trial Burn Plan (arsenic, barium, cadmium, chromium, lead,mercury, selenium, and silver); and, the stack sample digests were analyzed for the 22 metalslisted in Table G4-7a of the Trial Burn Plan. Analysis was conducted using inductively-coupledplasma atomic emission (ICP), graphite furnace atomic absorption (GFAA), and cold vaporatomic absorption (CVAA) spectrometers. CVAA analysis was for mercury only.

The analysis results were compared to the required practical quantitation limits (PQLs) asbelow: For the stack samples, the PQLs are listed in Table G4-7a of the Trial Burn Plan; for theTCLP extracts, the PQLs are listed in Table G4-5 of the Trial Burn Plan. GFAA analysis wasperformed for the stack sample and TCLP extract analytes (except mercury) that did not meet therequired PQLs by ICP or that contained particular interferences by ICP. For the solid waste feedsamples, no GFAA analysis was required.

3.1 ICP Analysis

A Thermo-Jarrell Ash ICAP 6IE was used for ICP analysis according to EPA SW-846Method 6010A (Revision 1, November 1990). This instrument provides a direct readout ofsolution concentration (ug/mL) in the digested samples. Dilutions of some of the TCLP extractdigests (from the Method 3010A sample preparation) were required to reduce the total dissolvedsolids content for the analysis or to lower selected analytes to within the calibration range of theinstrument.

The QC procedures listed in Method 6010A were employed, including initial calibration,initial and continuing calibration verifications (ICVs and CCVs), initial and continuing calibrationblanks (ICBs and CCBs), high standard verifications, interference check standards (ICSs), andserial dilutions of the sample matrices (to test for matrix interference).

J-3

AR3I5207APPENDIX J

3.2 GFAA Analysis

Two Varian SpectrAA-300Z GFAA spectrometers, with Zeeman background correction,were used for GFAA analysis according to EPA SW-846 Method 7000A (Revision 1, November1990) and the respective 7000-series methods. Dilutions of some of the samples, particularly theTCLP extract digests (from the Method 3020A sample preparation), were required to reduce thetotal dissolved solids content for the analysis or to lower selected analytes to within the calibrationrange of the instrument.

The GFAA instrument responses are in mass units of ng. To convert to a solutionconcentration in the digested samples, the mass response (ng) is divided by the GFAA injectionvolume, 0.01 mL for method of standard additions (MS A) analysis and 0.02 mL for non-MSAanalyses. The units "ng/mL" and "ug/L" are synonymous.

The QC procedures listed in Method 7000A were implemented, including initialcalibration, ICVs, CCVs, ICBs, CCBs, and the analysis of post-digestion spikes on the samplematrices (to test for matrix interference). If the post-digestion spike recovery results were notwithin the 85% to 115% method criterion, that particular matrix or set of samples was thenanalyzed using the method of standard additions (MS A), according to the method.

3.3 CVAA Analysis

The CVAA analysis was performed using a PSA Merlin Plus Mercury Analyzer accordingto Method 7470 A with the modifications listed in Table 6-2 of the Trial Burn Plan. Thisinstrument supplies a direct readout of absorbance and solution concentration (ug/L) in thedigested samples. The QC procedures listed in Method 7000A, including ICVs, CCVs, ICBs, andCCBs, were included in the CVAA analyses.

4.0 Sample Results

The attached tables summarize the Risk Burn Number 2 metals analysis data for the stacksamples, the solid waste feed samples, and the TCLP ash and scrubber water extracts, as follows.

• Table J-l presents the metals analysis results for each component of the stack trains andthe field reagent blanks, in units of total ug. The stack component method blanks (FHBH, and mercury) are also shown in this table for comparison purposes.

• Table J-2 is a summary of the stack sample QC data, including spike recoveries, filterreference material recoveries, and spike duplicate precision results.

• Table J-3 contains the metal concentrations in the solid waste feed samples, in units ofug/g (as received), plus the corresponding sample QC data.^

J-4

AR3I5208APPENDIX J

^ ^ r

• Table J-4 presents the TCLP metal concentrations in the bottom ash, fly ash, and scrubberwater samples as well as in the extraction fluid blank, in units of ng/L. The concentrationsshown are expressed as |ig per liter of extract. This table also summarizes the sample QCdata.

• Table J-5 is a comparison of the estimated stack sample PQLs defined in Table G4-7a ofthe Trial Burn Plan to the PQLs achieved for these samples. The actual PQLs correspondto the instrument used for each particular analyte.

Some of the metal results in Tables J-l, J-3, and J-4 contain data qualifier flags. A "U"flag indicates that the element was analyzed but was not detected; where a "U" flag appears, thecorresponding "<" result is the instrument detection limit corrected for any digestion and dilutionfactors. A "J" flag indicates an estimated value; it appears where a sample result was betweenthe detection limit and 3 times the detection limit.

As shown in Table J-5, the PQLs were met for the analysis of the stack samples. For theTCLP ash extracts, the results were all near or below the required PQLs. However, the PQLs forsilver, chromium, and lead in the scrubber water samples were not met because these samplesrequired dilution to reduce the total dissolved solids content to a level that could be tolerated bythe analysis instruments.

5.0 QC Results and Data Quality AssessmentAll the samples were prepared and analyzed according to the Trial Burn Plan and the

referenced methods, and the required detection limits were met as noted above. The sampleanalysis was completed within the required holding times for the target analytes. The instrumentanalysis and sample analysis QC results (defined in Tables G7-2A and G7-2C of the Trial BurnPlan, Table 14-2B of the QAP, and in the respective EPA SW-846 methods) are discussed below.

5.1 Instrument Analysis Quality Control

The instrument analysis QC specifications were met for all of the target analytes asfollows:

• The ICV recoveries were within 90% to 110% on each of the respective instruments.

For ICP analysis, the CCVs were within 90% to 110% recovery; for GFAA and CVAA,the CCVs were all within 80% to 120% recovery.

• The instrument blanks (ICBs and CCBs) were all near or below their respective detectionlimits.

J-5

AR3I5209APPENDIX J

• The high standard verifications for ICP analysis were within 5% of the target values.

• The ICSs for ICP analysis were within the 75% to 125% recovery criterion of the TrialBurn Plan.

5.2 Sample Analysis Quality Control—Stack Samples

Reference the attached Tables J-l and J-2 for a summary of the stack sample results andanalysis QC. The sample analysis QC specifications were met for the target analytes as follows:

• Several analytes were detected in the method blanks and in the field reagent blanks. Itshould be noted, though, that the FH and BH method blank results were comparable tothose found in the respective field reagent blank samples, with the exception of calciumand sodium in the BH blanks. The BH field reagent blank results for calcium and sodiumwere approximately 10 to 20 times those for the BH method blank; this is not surprisingconsidering the ubiquitous nature of these analytes and that these reagent blanks, unlikethe laboratory method blanks, were sent to the field and back.

• The results from the BH and FH simulated train spikes and spike duplicates were withinthe 65% to 135% recovery specification, with the exception of silver in both FH spikesand in one of the BH spikes. Also, all the spike sets met the 40% relative percentdifference (RPD) criterion except for silver. It should be noted, however, that an excessof hydrochloric acid is typically required to solubilize silver in the samples. Low silverrecoveries and poor RPDs have routinely been observed when using sample preparationmethods that do not use hydrochloric acid, such as Method 29; Table G4-7a of the TrialBurn Plan includes the note that silver typically has low recovery.

• The results from the two filter reference materials were within the 75% to 125% recoverycriterion for each analyte in the filters. The RPDs for each analyte in the filters werewithin the 50% RPD criterion.

• Separate matrix spikes for mercury only were prepared on the FH, BH, and mercuryimpinger samples. The analysis results for mercury were all within 75% to 125% recoverywith RPDs of less than 20%.

• All the serial dilutions for ICP analysis were within the ±10% difference specification ofSW-846 Method 6010A, with the exception of zinc in the FH serial dilution analysis andmagnesium in the BH serial dilution analysis. If the instrument response of the undilutedsample was less than 50 times the detection limit, a percent difference was not calculated.

J-6

A R 3 I 5 2 I OAPPENDIX J

5.3 Sample Analysis Quality Control—Solid Waste Feed Samples

Reference the attached Table J-3 for a summary of the solid waste feed sample results andQC. The sample analysis QC specifications were met for the target analytes as follows:

• The method blank results were below the detection limits for the target analytes.

• A matrix spike and a matrix spike duplicate were prepared for one of the solid waste feedsamples. In addition, a laboratory control spike was also prepared and analyzed. Theresults of these spikes were all within the 70% to 130% recovery criterion. The matrixspike set was also within the 20% RPD specification for the target analytes.

•- One solid waste feed sample was prepared in duplicate. The RPDs between the duplicatesamples were within the 35% RPD criterion for the target analytes except for mercury.However, both the sample and the duplicate sample results for mercury were estimated(i.e., included a "J" flag).

• The serial dilutions for TCP analysis were within the ±10% difference specification ofMethod 6010A for all the target analytes with the exception of chromium. If theinstrument response of the undiluted sample was less than 50 times the detection limit, apercent difference was not calculated.

5.4 Sample Analysis Quality Control—Ash and Scrubber Water TCLP Extracts

Reference the attached Table J-4 for a summary of the sample results and QC in the TCLPextracts. The sample analysis QC specifications were met for the target analytes as follows:

• The extraction fluid blank did not have detectable levels of the target analytes with theexception of barium and lead. The lead blank result was estimated (i.e., included a "J"flag), and the barium concentration was comparable to that of the samples.

• A matrix spike and a matrix spike duplicate were performed on one of the bottom ashextracts. In addition, a laboratory control spike was also prepared and analyzed. Theresults of these spikes were all within the 70% to 130% recovery criterion. The matrixspike set was also within the 20% RPD specification for the target analytes.

• Serial dilutions for ICP analysis were performed on a bottom ash, a fly ash, and a scrubberwater sample. The results were within the ±10% difference specification of Method6010A, except for barium in the bottom ash sample and chromium in the fly ash sample.If the instrument response of the undiluted sample was less than 50 times the detectionlimit, a percent difference was not calculated.

J-7

AR3I52APPENDIX J

DI/]

•I

&

6

2o

5

Q_—

&

a

<o

A«

ii

oIO

3O

^1

21

-•*°" -3

••H

cSJ

Jl

<! "53

Q-s£oto

c

d1cD

D 13•— COIO Ooo' MV V

co rxCN qin' ~CN

o -*•O COd d

10 —IO CN

IO 00tf CS•o d

«d dv

O CN

IO OIX

-P J

00 CN^ ~d dV V

itLL. CQ

o> o

-HJci]§ 2"S "53

U- CO

i

3 Z>

j;00 -<tV V

•— oco_ qco' ~IX

CN •—10 «q

o 1000> IO

•O CN•— COo- d

qS-0 dV

•o -o•o oIO OIX

3

CN CN TCN 0

V

CNCNCN10

CN CNCN CNV) IO

cn?JJl0 CO

&

c

•"• r>r- rxto "•— v

SCNCN

(> CN

K? £"rx rx

•0 0IX CO

— ico -*• r coix d

§8o dv

IO 00

•o oK

J

o CN T_: o

v

CNCNCN•O•— COCN CNCN CNO -O

0)

E '§.-g .iD CO

J T.

•Oc

-1 O

10

c> "V

IO IOq CN* t ~CO

•— O

K t

—

O —— uiK d

00 COO Od dv v

10 Oo ooCN Orx

_3

~o NQ *""""— ' d

v

CNCN

r— COCN CNr1 c4rx rx

D)

11"i ~0 COs °

1

~" D•Og•- -o— V

•<* -ooo " *—•CN

IX 0010 —O O

00 -Oco IxCO ~

CN —

o' d

»"o dV

•O IOCO CO10 dIX

— J

CO 00•o —:d °

V

>o oCN CN10 10

o oCN CN10 10

D)

Jl0= D.

D CO

m £5 7T"

•E12iE

iJ.§3•

Dc.0

1T^o*J*

.£=

i"3-D

-1JJw

D

3J"vs<

•*CO

v

-I «v v

_« §'S-2

g-'-gC O )

nE «

f l R 3 1 5 2 i 2

<2c>

COo

Dto

CN

J

iIm

_JQ.0

5

a

6

j

&

30

&

Q_

A

source

•

to

|>J

•*!

ai

si

<S1

io ~E1

<:-!

4f"5

Q<aEaCO

|•cI1

cC£

cs txCO COCV COcs

CO •—-o —d -*'

"1 00O CDV

•tf CO•— COvi d

§CSCO

co m3N

•f C>

d cV V

o o-X Co "~cs

3

5; Ko dV

m a< "y- *•["

U- CO

g,g_i -c cD 'OQ CD

|JS •*

E 2i

rfz

co cs— IX•d — 'CS CN

-o ow> <ol> COCS COcs

ix qco co'

CO —tx 10-<r d

0 0-q- o** 0oo cscs "

Tf CO• r cs0 OV V

0 **• ccd oCO CO0cs

13 "

£ 30 0V

cscscs•— COcs cscs c>10 "°

g= !I]0 co4)

II

T)cr>

O uiiq IXcs CO —

•o csCO COco -do- cs

—

-o •«»•O CN

tx co"T 0

O COCN tCO OCO "fx —cs

•o- co• cso oV V

o -»00 If•d ocO CO

cs

DC> 0d _V

CNcs-£•~ c*1cs c>cs o-0 -0

cg) 311cj= 'c

D CO4) C

c2 1.

*occ5

o —CM CS

•0 -<t0 0d ^t•— COCM

CS COcs oCO -<f

o —co ir>>o d

o -oCO •—K COr~ COtxCN

•*t CO-<t cs0 OV V

§0-o-<t ooTt COoCN

3-,

o- K0 oV

csCMCNIX

•"-" CO• cs c>tx tx

cr

= sa t« 'c

~zioZ 31

tx§O£

CO <O

<O COCM

CO -O0 Od -d•0

"I COo _:V

IT) O•O CM

8 COCO

*o IXcs

•t CO-if COO 0V V

0 tx<> iq**~ VIin CNocs

=r~ co<> coo _:V

IO -Oo- ti-cs c>x^x

o oCS CNV) V)

D)g> s

J j"i -iD CO

1 IzCQ ^—

1gO£

2in

n§

.S> E~o —^ I13 1? -S

$ §-£•I II

£3'?J:8

1C

A R 3 I 5 2 I 3APPPMPITY .1

&

&

&

a

&

A

£

1O

o

M"!

">-s

z~i

*1

•c "3< D

Qflj-QEJ?

'co1•g5

3

O CNCO •—_tq „—

3 — •

£ f>d ciV

O Tt00 ••»X. CN

o "~IX

-<f oCO CO-d txCN i—

-o coCN O

too—

U. CO

g> gf -*tJJCO CD

Jl5 5:u_ CO

<"2-

>o oCO COCN OCO —

3 -^

0 O (od dV

O Ix•O O10 -<tc> —CO

CN "OCO Oo' co•£> —CN •—

O CO— O^

CNCNCN

•— COCN CNCN CN*O <O

O5D1

£ [?o= '5.-g ED COof Oli

1

CN O"•t COt- CO•t —

-3 -,

0- "O oV

o o-co rxIO COCO CNo —CO

-* oCO Oco' co'CO OCN i—

•o >o— o-*' d

CNCNCN•Or- COCN CNCN CN•O -0

s3

III5= '5

O COJoI

•oc3Ck£

IX CO**• o•M- —

3-,

2: O. 10o dV

o —00 lO"O COCO CN•o —CO

O 00oo oTf CO'CN COCO i—

cSSco' ~

CNCNCNIx— COCN CNCN CNIX IX

sp.•. feJ c?•= Q-

11

Q£ IE

txc3

CO *OtX Tf^ "~

-,_0 °: CNo ,_jV

o <oCM -»

>O CN

O t-CO IX jfx 10•" CNV

O -Otx "OCN O

<f> -Oo oCN CNV) 1O

O- OCM CM<O >O

?

^^

25 '5.

"c * OslioD)OO

ILL.

t»oti

D

|

.25

fe

?

•I

J

= 8-2

II IIEm IE

AR3I52UAPPFNDTX .1 1O

Stack Data Summary, Page 4 of 4

Table J-l. Risk Burn Number 2 - Analysis Results for MM5-MM (Metals) Train

RunNA

Run 5

Run 6

Run 7

Field Reagent

DescriptionFH Method Blank, ugHg Method Blank, ugHg Method Blank, ugHq Method Blank, uq

Rinse and filter, ugHNO3 impinger, ugFourth impinger, ugKMnO4 impinger, ugHCl rinse,1 ug

Rinse and filter, ugHNO3 impinger, ugFourth impinger, ugKMnO4 impinger, ugHO rinse, ug

Rinse and filter, ugHNO3 impinger, ugFourth impinger, ugKMnO4 impinger, ugHCl rinse, ugBlankRinse and Filter, ugHNO3 impinger, ugFourth impinger, ugKMnO4 impinger, ugHd rinse, ug

Sample IDFHMB7470A MB 17470A MB 27470A MB 3

5221/52225223522452255226

6221/62226223622462256226

7221/72227223722472257226

5294/52955294/529652945297/52985299

CVAA

Hg(ug)

1.19 J<0.02 U< 0.02 U< 0.02 U

< 0.40 U< 6.51 U0.38 J9.94

276.95

< 0.40 U6.42 J1.30 J

326.506.23

0.69 j8.39 J

<0.21 U169.15154.75

<0.40 U<6.00 U<0.20 U<0.80 U< 1.00 U

A "<" indicates a result less than the detection limit, corrected for digestion and dilution factors.NA = Not applicableMB = Method blankFH ~ Front half

Flags ——> U: sample result < detection limitJ: detection limit <= sample result < (3 * detection limit)

f i R 3 1 5 2 i 5APPENDIX J 11

g-ct>CT^ :i_ a >; * i - T-cor'-'sr co — I^-ITCD COT-CO^TT- cMinco»-CD coco ^^s'"016

S

10

a:oO«a.rato

5

m

U.

a

CO«>S0CO&II)o:~3.mT3CO(/>

v>cCOrt.£a>O)01£oS-H

'fiCO

a c?g:S

5 §• ^1°8ÔT o:£ ETCF1 1^w a:a s~a. g.a:

=§§•&?^Q I2"o S?w *m ft-

'ro 2?

* 1CO .£CD CK

Q CI"a:2-

m 3" £? g"IQ $£•£ |it Q?

f OO ffi

0 oCO

"co

co r— coCM CM 0

00 T- COo o rCM »- COT~ ~

tf O> T-

M* CO **•CM CD 0)~

T- CM T-

CO T- O

O CO O" — CDO) CO CO

0 Tf 0

CO CO CO

CD T- CMi- *- 0

o m coco co i-O CO CO

o in T-8N- T-

CD CD

< Q- O_<00

O

(0 CO CO< m m

CO CO«- CM

•«- Otf COo o*•" T~

T- •*CM mo oT~ r-

in oo o

o mCD CD

in trgsCO CM0 0

T- CM

Sfe

XTTC

Sfe

Q- Q-O O

So

|x.0

00oCO

CMOCO

o

COCOCO

CO1CO*~

(V,

CO

,3.S

o

Q-

< •<—CO

2 m*fr"

2*>.*- in0*~

Z °

Z °°CD

£*8

CD COT- O

eo 1Sfe

O COT- OO0 CO

§0O

I Z

co r--h- r~

CO Is*CM N-CO CO

CO •*!•CO OCO CO

co inM-T-

CO h-»d- CDCO OO

t- CO

°"

i- oT- OO

CO CDCO COCD

0 0m fCD

a. a.0 0

a o>CO <

< < <Z Z Z

222

< < <Z 2 Z

*- O T-

o ••*••«-

co o r>-CD T- COCO CO CO

r-~ oo r-CO O> CO

l^. o mO CD T-

co in h-in i-~ eoCO O O

co co inr T- inCD O O

D. < a.ogo0

*S3

•* 0CM 0

CO COO CO0 CD

O COCO O)O CO*~

CM CO0 0

o inCO CO

CO •«-ssCO f0 0

*- CMTT inCO CO

Is- OO

CO CO

Q. D-O O

O 3O O

CM < CO•^ Z o

t < •<«••<t Z T-:CO O

0 < COSZ o

0"~

CM CM 1O O O

CO CO 1"-.CM in coCO CO CO

CO T- •*(•

CO CO CO

co in oo o o

in *- coT CO COCO CO CO

h- in coco in coCO CO CO

o_ D- a.O O O

LLS!

< <Z Z

< <2 2

< <z z

•* CMCM i-

'sf coCO CO

CO T-ss

CO COCM i-

h- -<tin ooCO CO

oo coh- COOO CO

a. D-O O

CO\s 9

T— mCM CM

•c- •*ss**• ooCO COO COT~

•* **•O T-

co mCO COCD CO

Is- CMco inCO CO

CO CO0 0

o oCO CMCD CO

l«- CO

CO 8)

a. a.0 0

> <=

~y* tU —I .T» *« '*S *-* V-C .-> 7« N-' V B' V r*- V-*V-/%-/ V-/ %_/*-/ -/ I-/ \~S \-t a\ \Ut- «

Q0. £,OL

•— o ^» *^ a> S* c*»O g>Q §5

f 1- 8^-i 5

tJ _D_ «^CC ~~*

a:

O- 03_ rac $g- '5. g roJ|

OO. «?•EC ~~*

,o .E Q gU_ Q. 5

>S

y «p coQ- &a:

" te g-^c?î-iÎ-ol1 c S

Or' Q) CT«P COrj) CO * .. *

?'H° fe-t D_ Q

QQ. .o:

D:CON-'COin

I ~ * *

TO £Qg

CO

(!)

s~R"3i&zrs SI

co

oo

CM

O

CD

CO|

|

•£(UQ.

tiQa_a:

A OPCMPITY , I

o0)

c?D.2?roE

CO

"8

"oCO

<,1o

Q.o

D-o

Q.O

D.O

Q.O

A

S3OCO3S

*ia

£sa_3_

O a

S|

*i4Sa

QuoEroCO

co.•abCO(DQ

-3 r> -3s3so'°d

CM h- CDi - in o1 CO COCO CO CO

o in N-in o CDCN CM CN

13-5 Din

•c- CO TTCN 0- CN0 0V V

O) T CDco in h-d d d

-3-3-3• CN O>o o rN.' co' co'

T— T— Vin in inCN CM CNin CD r

1u. in CD f-a> c c c"5S => = 3Jg o: o: o:2"6CO

DCN S£ SS ^o' O CD O) 00 COv o' co' co' in Tv r^- o oo oo

Z)^ ^ -S£ ^

oo h- j- co oo in^ rr CN co o' CN

0 O OV T— T- T-

D>C vP sP sP vp

t\J O* 0s 0s O Ooo T- co en oo t-0 d |gg d

ID< ^ ^Jsj Z. CM eo in co

d in T^ r^ d° £°-°-

n^ ^^^ ^

O 't "* 00 h-. T-_(-; v d ai o> d~ o en o

noo o1* cr^oo " T- Q it -<fCsi OO' CN O) T-' CNy o o> o

Q. Q3 3Q Q

m <U Q) "S< JS ^2 'Q. t1- Q-•g COCOCO CO

w — x x x;: o -c ~ —Q. i— *- w3 «^"p CO <0 {D

^ Q oS5 5C Q^SOr-^- ^.(0 t,lnO.QlOlO,_.l<'S? feCNoroCNCNQCNCO QiineB^jt^N-Q.r^•a a t£. t£.2 Q. 0) 0)5 E ^£ ^£fl) flj Q. QS w en en

-ES'c8£33 »i 1o ^5

s Ij 5 TI «t5 J3S =6

1 ! fo o —f- .21 ^••g to o$ s, 'isc» y« 'S %

. =• 0 "Sco *•- *'a "S «5 | VTJ E ±iS t ~ I g j|W O. f-o *H 5 <DS- E ° -S8 - '"6 t! *o ~ v v•D -S i'E- CO- c- 0 y^ SJ5 «51 CO g 0.

S 8 tl A« S&I A0. & *-. <UE -E5CCS r „ " »« V " Q D)I <ife £AR3152I7

oO)D)(D"• ft— T^ ™T rn * •* " •" r"\i m m ^. i i. i T m ... . ^

E Sc? I£ EID UQ CO

O mx:10

IOQ

amco•oawc_ora

Ioo5«Sa.

3ZCk.3m.XM£

o

10IQ.O

U.0

a.o

%0

D.O

A

a>H

1Q

0) *•;CO =!a

S|

£i

o5a

•a 2

<o 2"rr3

"53

C03"3— •

Q(UQE<DCO

0

Descript

3330 0 Ooo oo ooCN CN CNV V V

3D

o ° °2 CM CM•^ V V

333o o oCN CN CM

. O o' O°V V V

333CN CN CMCO CO COV V V

-3 -3o o oh- CO O

CO M" CMO *3- O

3 ~> ~>

CO § §

"* 0 I--V T-

3330 0 0CO* CO CO°V V V

CN CN CMin co N.

m CD r*.c cr c

— 333•gj a: 0:0:

1CO

o o oin o infeS'S

T—

O O Oo o oCM 00° 00°ro m co

333o o oCN CM CNo° o° oV V V

CO (D 00•«— o co

V T- T-

o o o0 0 Oiri iri iri00 CM Ot-~ in oT- CN T-

T- in ooh~ co T-CO 00 CO00 i- O

o o o000o o or- in CNCO CO

33-5P ° eoCO CO T-V V CO

(O CO (OCM CN CN

in co tc: c c333OH (£. OL

1E

o o oo o o0 0 0°eo i- roCO CO CO

333o o o000CM CM CMCN CN CMV V V

co co inCO (O h-iri to T-1

333o o oCN CM CMCO CO COV V V

333o o oo o oiri iri iriV V V

o o oco co inCM CM f»-T- •r- O

8SSCO CO COCN T-

-5-53

00°.T- CO O

CO CO V

t*. 1 - 1 -CN CN CNin co r«-

jj in co »*-£ c c c« 3 3 35 cc oi a

3oCO

3o00CNV

-8CO

3

8oV

3CNcoV

3oin0V

v—CO

3o00

V

3oco"V

•croCD,2yLL

0

1 Extract!

Si O O COiri CM' N" CN0 CM t-

U5 O O OCO CO CO O^^?

01 0 N- N-N T-1 T-' O°CO O O

CO 00 CO OT-' CM -"T CN

^ ^o in in coco co T-: CMCO O CO T-

oq i in o r^" N° CO v-co oo oo

&5 ?-. CN COCO " 00 CO00 CO O T-

^ - ^O 00 ?- TTCO OO CO Ooo r r >

Q. o.3 3O O

a) cu a> "5•5. °5L "5. '5.CO CO CO CO— XX Xo -c -c ~U-. 4. _l rf^ (0(0 (0§55 5

el •? ^

0) Q.OL OLO (U

'5. "a.CO CO

Si 3 CaJ w .£•o £ c<u <u o

N - « « «- 5 « o.'g

U)_2CL

(0U)

SoJO

"•5•ai=(D

OCoI 1D]' T3

S JO

V*- 1 _.P E «t ~ 2

8 Cfl,

.tf = o-E

.u »-*-H Eni ^0) ro4 \ucu in

g • •o II~ V V±i ±i

(0u

in £co SE-g OK~ H " "»V " Q co- < a. J2< 2 K u-

AR3I52I8

D

"5

*~

1

fc-

u " 5

^f-v "ra!|

91

if

CNCOCN

-<to'

0

e0)te i5

c"'o-w. '5-.SD O .= g

- •€ 9 •=Illlui£ OQ a: 2 I

Q.

D10MDo_*sinJt-

0

-o

O.

u

o:<o

j>o

P.S

II

Hi J

352

I 85 8

« • s -s iA .y p. «A ._._....... I g §•OCO — CN

'O'O-O'— COIXOOOUIUItXTOOCOOO-OUIOCN-; — — OlxCNKtxO

•— O CN ~ -t tx CO -O — CO CSCN-— OK — CO —O CO CO ^-t COrx

co — ix "tr >o Z o io CN •— -o o ^: K rx co CN o m CN -od d CD — ~~, —' CN — CN d — d o" d d c> d — d

COCOOOlO-— •—

ooo o —cooooooo orx>ooorx

— coco'— CNncNlxrouilx—o — CS--OCN-OCNCO

O O O O O X O-* C O O O O O O O O - - P J O OO rx

O "8 rf *ol •" CN.o-lr>'r!u?"'. •9r?cNf lf?f>'^*P"~ rxooco.— 10. . . . . . p n .°~. co CN n oO^-CNp~iritx °~. co CN n o od -»'p~B

•i 67

U_ iO Oo o 0 o

e.y E a -I 1 = — i I ° I -= fc s 6 .s e gIJIJJIjjjjjjjjlllfjjjl

E

.Ml-s§ iS--8

.£"o

I .

a Z-

-E -5

3

-

A R 3 I 5 2 I 9APPFNDTX J 15

Appendix K

Report on Chemical AnalysisResults for Hexavalent Chromium

MRI-AppSed/R362028.APP

AR3I5220

Appendix K: Analysis of MM5-CR Train Samples for HexavalentChromium

Three stack train samples and one field blank sample were analyzed in duplicate forhexavalent chromium (Cr+6) from the Risk Burn No. 2 MM5-CR train samples. Sampleanalysis was performed using the EPA BIF method titled "Determination of HexavalentChromium Emissions from Stationary Sources," as specified in 40 CFR 266, Appendix IX,Section 3.2. MRI standard operating procedure (SOP) CS-AMP-14 also was used forsample analysis and follows the guidelines established in the BIF method. This methodutilizes ion chromatography, a post-column reactor and a visible wavelength detector forCr+6 determination.

1.0 Sample Receipt

Risk Burn No. 2 samples were received at MRI on February 11, 1997 at 6:30 P.M.The samples were received in good condition. Evidence tape attached to the samplecoolers and sample boxes was intact upon sample receipt. All samples were cold uponreceipt. Samples were stored in the MRI cold room until relinquished to sampletechnicians for processing.

Weighing of each sample bottle was performed before the sample bottle wasopened, and compared to sample bottle weights recorded in the field before sampleshipment to MRI. This data was recorded on the Sample Condition Form thataccompanied the sample shipment. Sample weights recorded by MRI did not vary bymore than 0.1% of the sample weights recorded in the field. For all samples MRIrecorded a larger sample weight for each sample than was recorded in the field. This wasmost likely caused by vermiculite that adhered to the sample bottle during shipment toMRI being included in the weight recorded by MRI. The small amount of variance in thetwo weights for each sample show that no sample loss occurred during sample shipment.

Hydrogen ion content (pH) was measured at the time of sample preparation.According to the BIF method, the pH of samples could not be less than 8.5. The threeMM5-CR train samples provided pH readings of 9.5. The pH of the field reagent watersample was 7.0. Since the purpose of this sample was to evaluate any positive responsefor Cr"1"6 from the reagent water used in the field, the sample was analyzed as received.The pH of the 1.0 N potassium hydroxide (KOH) field reagent sample was 13.5. Thepurpose of this sample was to evaluate any positive response for Cr+6 attributable to theKOH used in the field. As is discussed later, this sample was diluted one to ten beforesample analysis to provide a blank that was more representative of the KOH concentrationin the actual MM5-CR train samples.


Samples for Risk Burn No. 2 were prepared on February 13, 1997. All containers,flasks, sample containers, and vials were rinsed with 0.1 N KOH before use to prevent loss

4R3I522APPENDIX K

of Cr+6. Sample preparation involved filtering five milliliters (mL) of each sample througha 0.45 micron nylon syringe filter. The 1.0 N KOH field reagent sample was initiallydiluted one to ten before filtering to provide an ionic strength that approximately matchedthat of real samples. Five mLs of the diluted 0.1 N KOH field reagent sample was filteredthrough the 0.45 micron syringe filters. Amber autosampler vials were then filled fromthe collection flasks containing the filtered samples.


The analysis of hexavalent chromium was performed using an ion chromatographwith a post-column reagent. The ion chromatographic columns separate the Cr*6 in itsaqueous form, CraCV2, or chromate ion, from other anions in the sample. A post-columnreagent is mixed with the column effluent which complexes with the chromate to form achromophore which is detected using a visible wavelength detector. The method offersspecificity for chromium two ways, 1) the chromate ion is eluted from thechromatographic column at a specific retention time, and 2) is then complexed to form aunique compound that is detected at a specific wavelength.

Samples from the Risk Burn No. 2 were analyzed using a Dionex DX-2000i ionchromatograph. The chromatographic columns used were supplied by Dionex andincluded a NG1 guard column and a AS-7 chromatographic column. The chromatographiceluant, or mobile phase, was a solution of ammonium sulfate and ammonium hydroxide.Samples were injected into the chromatographic column with an Alcott 728 autosamplerconfigured with a 200 microliter sample loop. Column effluent was mixed with the post-column reagent, an acidic solution containing diphenylcarbazide, before entering thevisible wavelength detector. The post-column reagent reacts with chromate ions in thecolumn effluent to form a chromophore that was detected at 520 nanometers (nm) withthe visible wavelength detector. The data system used to collect and quantitate Cr+6results was a P.E. Nelson Turbochrome Version 4.1 system.

4.0 Sample Results

Risk Burn No. 2 samples were analyzed for Cr+6 on February 13, 1997. The Cr+6results for all samples and field blank samples are less than the lower reporting limit (LRL)of 0.5 micrograms per liter (ug/L). Table K-l shows the Cr+6 results for each of the RiskBurn No, 2 samples.

5.0 Quality Control (QC) Results and Data Quality Assessment

The data quality assessment of Risk Burn No. 2 samples for Cr+6 analysis includesan evaluation of sample holding time requirements, standard calibration procedures, andQC results for blanks, replicate sample analysis, matrix spike (MS) and matrix spikeduplicate (MSD) samples, and performance audit samples. The following paragraphs givethe results of each of these evaluations'and the impact on the sample results.

.AR3I5222APPENDIX K

Table K-l. Risk Burn No. 2 Sample Results for Cr+6

MRT Sample Number52306230723053005301

Sample NameRun 5Run 6Run?

Field reagent blank, 1 .0 N KOHField reagent blank, blank water

Cr+6 found (ug/L)<0.5U<0.5U<0.5U

• <0.5U<0.5U

Notes: ug/L = micrograms per literU = Undetected at concentrations greater than the lower reporting limit (LRL) of

0.5 ug/L

The technical holding time for Cr*6 analysis is 14 days. Samples for Risk Burn No.2 were collected from February 7 through February 9, 1997. Samples were prepared andanalyzed on February 13, 1997. Thus the technical holding time requirements for Cr+6analysis of Risk Burn No. 2 samples was met.

Standard calibration requirements for Cr+6 analysis are: a minimum of fourstandard concentration levels, an initial and a final calibration, responses for duplicateinjections of calibration standards must be within five percent of the average response, andpredicted values from duplicate injections of the calibration standards must be withinseven percent of the actual value when calculated using a linear regression curve of theaverage responses from the duplicate injections of the calibration standards. An initial(ICAL) and a final (FCAL) instrument calibration was performed employing six standardconcentration levels ranging from 0.5 ug/L to 25 ug/L. The linear regression curve forthe average of the initial and final calibrations provided an R2 value of 0.99985. Thestatistical evaluation of the calibrations are shown in Table K-2.

Table K-2. Calibration Standard Statistics

StandardLevel(HE/L)0.51.02.55.01025

ICALPeakHeight15622229714293577183146855348676

FCALPeakHeight15564228924372178573147397355209

AveragePeakHeight15593229324332877878147126351943

ICAL%

Diff.0.20.20.90.90.20.9

FCAL%

Diff.0.20.20.90.90.20.9

ICALPredicted

Cone./ %DiffUg/L / %DifF0.470 / 5.921.01 /0.602.46 71.574.96 70.8710.03/0.3424.74/1.04

FCALPredicted

Cone./ %DifFug/L / %Diff0.466/6.771.00 70.202.52 70.725.06 71.1610.07/0.7325.22/0.87

Table K-2 shows that the responses for all of the duplicate injections of thecalibration standards was within five percent of the average response, and that thepredicted concentration for each standard calculated with the average linear regression

SR3I5223APPENDIX K

curve was within seven percent. All standard calibration requirements were met for theanalysis of Risk Burn No. 2 samples.

The initial and final calibrations included a 0.0 ug/L blank standard to evaluateresponses for Cr"1"6 in reagents used to prepare the standards. The ICAL 0.0 ug/L blankstandard provided a response of 2.99 ug/L for Cr+6. The FCAL 0.0 ug/L blank standardprovided a response of 0.005 ug/L for Cr+6. No definitive cause for the high Cr+6response for the ICAL 0.0 ug/L blank standard can be found. This high response had noimpact on the standard calibrations, nor on the results obtained from any samples.

A method blank sample and two field reagent blank samples were prepared andanalyzed along with the Risk Burn No. 2 samples. No Cr+6 was detected in the methodblank sample at a concentration greater than the LRL of 0.5 ug/L. The field reagent blanksamples, blank water and 1.0 N KOH, also were found to contain no Cr+6 atconcentrations greater than the LRL. The result for the field reagent blank samples areshown in Table K-1.

Replicate injections of each sample are required to be within five percent of theaverage response of the two injections. None of the Risk Burn No. 2 samples were foundto contain reportable concentrations of Cr+6. The replicate criteria was also applied to theMS and MSD samples and the performance audit sample. Table K-3 shows the statisticsfor the replicate injections of these samples.

Table K-3. Replicate Sample Statistics

SampleRun 6 MSRun 6 MSDAudit Sample

Replicate 1Peak Height

6334662584166234

Replicate 2Peak Height6394962685165231

AverageResponse6364862635165733

Replicate 1% Difference

0.470.080.30

Replicate 2% Difference

0.470.080.30

As Table K-3 shows, replicate injections of samples met the five percent criteria.

The Run 6 sample, 6230, was used as the MS and MSD for Risk Burn No. 2samples. The MS and MSD was prepared by adding 5.0 ug/L of Cr+(S to two aliquots ofthe Run 6 sample. The average percent recovery of the MS sample from the replicateinjections way 79.4%, and the average percent recovery of the MSD sample from thereplicate injections was 77.9%. Both the MS and MSD percent recoveries were within the50 to 150% control limit established in the MRICS-AMP-14 SOP. The relative percentdifference (RPD) of the average percent recoveries of the MS and MSD was 1.9%. TheRPD was within the control limit of less than or equal to 30% RPD as is established in theMRI SOP.

A performance audit sample was prepared and analyzed along with the Risk BurnNo. 2 samples. This audit sample was independently prepared by the MRI quality

AR3I5221*A PPCMn TY

assurance personnel. The audit sample was analzed as a single-blind audit sample,meaning that the analyst knew it was an audit sample but did not know the actualconcentration of Cr+6 in the sample. The true value of the audit sample was 11.3 ug/L ofCr+6. The average value reported for the replicate injection of the audit sample was 11.41ug/L. The percent recovery of the audit sample was 101 percent which was within the 90to 110 percent recovery criteria established in the BIF method.

Risk Burn No. 2 samples submitted for Cr+6 analysis were analyzed within thetechnical holding times; were analyzed with an acceptable standard calibration; and metthe QC criteria established in the BIF method and the MRI SOP for blank samples,replicate sample injections, MS and MSD recovery, and performance audit samplerecovery.

AR3I5225APPFNDTY K

Appendix L

Report on Chemical Analysis Results from PCBs

MRI-AppHed/R362028.APP

AR3I5226

Midwest Research InstituteAppendix L

PCB Analytical Reportfor Risk Burn No. 2

by Mark Horrigan — StaffMass Spectrometrist

1.0 Sample Receipt and Storage

MM5 train samples from three runs and one blank train were received cold and intact onFebruary 1 1, 1997. Samples were stored in the 330-E cold room prior to sample preparation.


The samples were prepared for PCB analysis using guidelines from EPA Method 23 and DraftMethod 1668 (October 4, 1995) and Method 680.One method blank and one lab control spike (LCS), consisting of pre-extracted XAD wereextracted with this batch. Each XAD trap was spiked with field surrogates (20 to 92ng) prior toshipment to the field. Each XAD/filter sample was spiked with lab surrogates (20ng) prior toextraction. The front and back half rinses were not spiked with lab surrogates.Two soxhlet extractions were performed for the XAD and filter, one using toluene and then asecond using methylene chloride. The front and back half solvent rinses were concentrated andadded to the XAD/Filter prior to extraction. Both solvent extracts were concentrated, combined,solvent exchanged into hexane and taken to a volume of 10 ml. A 5 ml portion of this sample wassaved as an archive. The other 5ml portion was partitioned against sulfuric acid as a cleanup step,then concentrated and spiked with recovery standards. Nitrogen evaporation was used to achievea final volume of lOOuL in tridecane.

Each MM5 train sample had an associated toluene rinse portion. The toluene rinse was preparedas a separate sample, and therefore spiked with lab surrogates (20ng). Field surrogates were notadded to the toluene rinse. The samples were concentrated, solvent exchanged into hexane andtaken to a volume of 10 ml. A 5 ml portion of this sample was saved as an archive. The other5ml portion was partitioned against sulfuric acid as a cleanup, then concentrated and spiked withrecovery standards. Nitrogen evaporation was used to achieve a final volume of lOOuL intridecane.

A spike check consisting of field and lab surrogates, and native PCBs was prepared with thisbatch as a check standard.

AR3I5227APPENDIX L

3.0 Sample Analysis

The samples were analyzed by high resolution gas chromatography/high resolution massspectrometry following guidelines from Draft Method 1668 (October 4, 1995).The analysis was carried out on a Hewlett-Packard 5890 gas chromatograph using a DB-5MS(60m, 0.25mm ID, .25 micron) column interfaced to a VG70-S mass spectrometer. Massresolution greater than or equal to 10,000 (10% valley definition) was demonstrated for allanalysis.

The initial calibration consisted of a series of five calibration standards ranging from 2 to200ng/mL (Table L-l). The initial calibration passed the criteria of less than 20% rsd for allcompounds. All compounds met the criteria for signal to noise (ten to one) and mass ionabundance ratios ( +/- 15% of theoretical values).Continuing calibration using a mid level standard (CS3) passed the criteria of less than 20%difference from the initial calibration for native analytes, and less than 30% difference for labeledcompounds. A successful continuing calibration may fail no more than four compounds. Tetraand penta substituted isomers must pass.Successful sample analysis were bracketed by passing the calibration standards at the beginningand end of each 12 hour shift. All continuing calibration standards met the above criteria.Native results were calculated relative to the lab surrogates for all 1668 isomers (see Table L-l).Native results for all other isomers (680) were calculated relative to the recovery standards. Fieldsurrogates were calculated relative to the lab surrogates. Lab surrogates were calculated relativeto the recovery standards.

4.0 Sample Results

The sample results are given in Table L-2. The native PCB values are presented first in total ngfor each homolog. Lab and field surrogate recoveries are shown in the lower portion of the tableas percent recovery. Field surrogate recoveries are not given for the toluene rinse samples sincethey were not spiked.

The results in Table L-2 show that the blank train contained a total of 37 ng whereas the totalamount in the sample trains ranged from 181-263 ng. This is opposite to what was found in RiskBurn No.l, where the amount of PCBs in the blank train was higher than the amount in thesample trains for 3 of the 4 runs.

APPFNOT

I I

5.0 Q.C. Results

All samples were extracted and analyzed within holding times as specified in the trial burn plan.

The method blank showed detectable levels of mono through hepta substituted homologs. Thehighest value found was in the tri-PCBs, 2.75ng, but at one fourth the level found in the lowestMM5 train sample.

The lab control spike sample showed recovery results between 59 and 103 %. Results arepresented in Table L-3 as percent recovery. All isomers met the object of 50 to 170% recovery.

Due to a lab error, the toluene rinse sample from run 7 was not spiked with lab surrogates.Therefore surrogate recoveries and native results are not available for this sample. Lab and fieldsurrogates met the recovery criteria in all other samples.

APPPNriTY I

Table L-1. PCB Calibration Standard Concentrations (ng/mL)

680 PCB NativeMono (3)Di(5)Tri (29)Tetra (50)Penta (87)Hexa(154)Hepta(188)Octa (200)Deca (209)1668 PCB NativeTetra (77)Penta (105)Penta (11 4)Penta (11 8)Penta (123)Penta (126)Hexa(156)Hexa(157)Hexa(167)Hexa(169)Hexa(170)Hepta (180)Hepta(189)PCB Field13CMono(3)13CDi(15)13CTetra(52)13CHexa(153)13C Octa (202)13C Deca (209)PCB Lab13Ctetra(77)13C Penta (105)13CPenta(118)13C Penta (126)13CHexa(156)13CHexa(169)13C Hepta (180)PCB Cleanup13C Tetra (81)13C Penta (111)PCB Recovery13CHexa(138)13C Hepta (178)

CS2

2.002.002.004.004.024.026.026.0210.0

2.0010.010.010.010.010.020.020.020.020.020.020.020.0

6.006.0012.512.525.028.5

10210010198.499.0101101

1.9910.1

99.8101

CS3

10.010.010.020.020.120.130.130.150.0

10.050.050.050.050.050.0100100100100100100100

24.024.050.050.0100114

10210010198.499.0101101

9.9550.0

99.8101

CS3.5

25.025.025.050.050.350.375.375.3125

25.0125125125125125250250250250250250250

86.486.4180180360410

10210010198.499.0101101

24.9125

99.8101

CS4

40.040.040.080.080.480.4120120200

40.0200200200200200400400400400400400400

120120250250500570

10210010198.499.0101101

39.8200

99.8101

CS5

2002002004004024026026021000

200iooo10001000100010002000200020002000200020002000

4804801000100020002280

10210010198.499.0101101

1991001

99.8101

AR3I5230

cT"1j»eo128oCCCOzCM

££

Es10 S r-' <0

3 «D > «

CM £OQ f~

M |_CC Q;C CO _îr 12 ** mm co , „ r;2 iv J£> 5— co O

ro CM03 01

tCC

cggi|VCMOQ

H-9s

to g eo ing p2 g SDC o > 5

CMOQ

tCC

m S in inc ™ § S

CMOQ

CM

! ElJj»s*• ^ n irQ CO *£

«= CM 4<U CQ

O

Q 0 * X-o 2 "• "S•« tt c/j roLL m 5 5

'" CD » *T-eoivcncoin{SlflSSoS r - i v c M q i n S e o g g

* — «~ «~ CNJ r- Q OID ID ID

cocMineneoeng}§Jg£e M ^ o q ^ q e M g ? g ^ 5^ c o c o m i v c O Q c J o ^

ÎBwN«logjp!g§oSoJîoS^^S"«- ^^r- «^d66

|vCM«-'*|vr»<Or-|2[^r~cd6ivcMccitvi®<D'-'-CMCMr-eOr-COr-j.J^

C M C M c n e n o O ' - c o l § o J §e ^ ^ r - e n o o c n . i v c n c o'-cocMr-co«-mc5o<:5

X c7 PJôoincocogCfOfOJECM^^^rT-ir-rtOOcJr-CM-r-6dq_:__:

———— " "

3

^

To*;•2wc?•5X®.2? r o 2 r a 2 n ] n 5 < o* s £ f c c X Q - t J c on ° . _ - c : v ( u u o ( uZ 5 Q H I - 0 _ X X O 2 Q

eo «- o en co js.iv eo en ° «- *~oo en r~ *~ en *~

CM it «- »t CM CO CO«- r- t- CM •* CM CM

^ CD — CM «- CM t-co co en ° "" *"co en «-'-'-«-

in ^ CM - co co oTt O i>. O CM O i-cn •- en «-«-«-«-

en o ^ CM en <-eo o co eo eM o r-en •" en en *" "~ r"

co eo i^«-; m eo o«- <t IV CO «~ ên oo en en *~ en *~

"r?a>goa>CCs£yg 2 2 2 <o <o 2S r a c c c x x a .0 3 w V ( U I U V V < Ucnoa.o.a.xxxS'TcbincDcocnoa i v t - o c M i n c o c ocol^r"'~'~'~r"'~jjOOOOOOOeocococococococo

•a TJ 73 T3 -a -a4V CO 0} O Q) COT3 T3 TJ T) 73 73•0 T3 73 T3 T3 T3

O 0 0 O 0 0Z Z Z Z Z Z

in «- |V CM CO r-00 CO 6 T~ CO C5co co oo en rv *-

tt r- «t CM CO enen 6 CD in en oco en co co co *~

* •* en CM coS «o oco iv oo en *~

in co eo co co iv.CD CD Tf eri CD oco rv co iv iv i-

T3 73 73 73 T3 73<l> <D d) 0) (D 4J•0 73 73 . -0 T3 73^

O O O O O OZ Z Z Z Z Z

5go09CC

#*

fo g l s s||5?SS5S,2 i m CM m o O<" eo T- in i- CM CM2 o o o o o o.2 CO CO CO CO CO COL. «-«-«-«- «- t-

O3 d)c "5.2 1o 8c .-c «-• &'01 •-™ "SJ o S gCU+-* (U(U !-? I8 2CO 4-*.n co

3?O !?C ftro 3-c .52

"S |tj oCO "m<u o•O -!-•c o

S §

AR3I523A PPCTMn TV I

3C

o

«=

CMOQ

•Z O) co «C 1^. r- C

CD

t<

CM S« iCM £OQ H

Q ** JJ^ co £ -c > °"55 -K t/3 to

r^mr^t-rs.^-0) co co>-«-6 «> rv! « CM - r- ^ S » •*' 6o5O)ooo>'~'~«~ t o o o o o t n

, , , /-, "O "O "O "O< o C M o - - -m m m ~. . _ _ < < < < < <oo oo oo ^ ^ ^ , . ( . ,. , . ,. , .o o o o o o

Z Z Z Z Z Z

<D•O "O T3 TD TJ T3=000000000 ooooooo 553525022222Z2ZZ 2222222 < < < < < <O O O O O OZ Z Z Z Z Z

o o o o o o

"5 ST £= > g"» § O- * ;

a to a, tog g g 6 8

= S c X Q - S c S jjOOOOOOO 2000000J .«• *CI U 4J fl3 flj O Q Qi jn 00 CO OO 00 00 OO 00 ^ 00 00 OO 00 CO 00

AR3I5232CT MO T V

I I

Table L-3.LCS Recovery (%)

Isomer Amount foundng

Mono (BZ 2)Di (BZ 5)Tri (BZ 29)Tetra (BZ 50)Tetra (BZ 77)Penta (BZ 87)Penta (BZ 1 23)Penta (BZ 118)Penta (BZ 114)Penta (BZ 105)PentatBZ 126)Hexa (BZ 1 54)Hexa (BZ 1 67)Hexa (BZ 1 56)Hexa (BZ 157)Hexa (BZ 1 69)Hepta(BZ 1 88)Hepta(BZ 1 80)Hepta(BZ 1 70)Hepta(BZ 1 89)Octa (BZ 200)Deca (BZ 209)

1.172.041.532.451.773.648.759.099.039.138.383.6614.514.914.218.15.2817.118.318.96.198.54

Amount spikedng

22242410101010104202020206202020610

% Recovery

5910277618991889190918492737571918886929510385

RR315233DDCTMD TV I

Appendix M

Report on Chemical Analysis Results for Chlorides


Appendix M: Analysis of Samples from HCI/CL2 Emission Sampling Trains inRisk Burn No. 2

by M. Thornburg - Associate Chemist

Six samples and two field blanks were analyzed for hydrochloric acid as chloride fromRisk Burn No.2. Sample analysis was performed using a modified version of Method 9057based on ion chromatography (1C) and conductivity detection. The method was performed aswritten except for a modification to dilute the calibration standards in a buffered eluent solutionrather than in 0.1 N NaOH or 0.1 N H2S04 in order to improve chromatographic performance.This modification is discussed in the sample analysis section of this appendix.

1.0 Sample Receipt

The samples were received at MRI on February 11, 1997, in good condition. Thesamples were stored in MRI's sample control facility, under secure and refrigerated conditions(~4 °C) until received by analytical personnel for processing and analysis.

2.0 Sample Preparation Method

Samples for Risk Burn No. 2 were prepared on February 14 and analyzed on February21, 1997. The samples were first weighed to determine if any sample was lost duringtransport, and all samples were found to be intact. All containers, vials, and flasks used forsample handling were rinsed before use with copious amounts of the 1C eluent to removepotential contaminants. The eluent used was modified from the 3.0 millimolar sodiumbicarbonate/2.4 millimolar sodium carbonate recommended in Method 9057. Method 9057allows for the use of other dilute eluents buffered to a similar pH that contain no interferingions with the chromatographic analysis. Therefore the eluent was modifed to 1.8 milli-molarsodium bicarbonate/1.7 millimolar sodium carbonate. The samples were prepared for analysisby diluting two milliliters of sample to ten milliliters with I.C. eluent. This step wasperformed to dilute the sample matrix a factor of 5 to improve the chromatographicperformance of the method. A dilution of the sample matrix with the 1C eluant resulted in morestable and even baselines. This procedure was within the scope of Method 9057 whichsuggests dilution of samples to a final volume appropriate for all samples.

The field blanks provided for analysis consisted of a sodium hydroxide solution and a sulfuricacid solution. These sampling train reagent blank solutions were diluted to match the averagedilution of the field samples. In addition to the 1:5 dilution with eluent, a 1:10 dilution of thecaustic field reagent blank and a 1:40 dilution of the acid field blank were performed in anattempt to more closely match the field matrix. Actual volumes of field sample condensateswere equivalent to a 10 fold dilution of the acid reagent and a 3 fold dilution of the causticreagent. Therefore, the blanks were overdiluted a factor from 3 to 4 compared to fieldsamples.

Quality control samples prepared with the field samples included eluent instrument blanks, alaboratory control spike, an acid field sample matrix spike, and a caustic field sample matrixspike. The field samples used for matrix spike quality control samples were collected duringruris 6 and 7 of the trial burn. Although these samples are different than the risk burnsamples, they are considered representative samples for quality control matrix spikes. Aliquotsof the field samples, field blanks, and quality control samples were transferred to autosamplervials for 1C analysis.

AR3I5235M

The analysis of chloride was performed using a Dionex Model 300 ion chromatograph.The separation of chloride from other anions was performed on Dionex AG4A-SC and AS4A-SC columns. The analytical instrument was operated in the suppressed conductivity detectionmode. The chromatographic eluent was 1.8 millimolar sodium bicarbonate/1.7 millimolarsodium carbonate. Auto-injection of the samples onto the I.C. system was performed using aSpectraPhysics AS3500 autosampler configured with a 50 microliter sample loop. The ionchromatograph was calibrated using a certified Alltech standard, custom anion mixture A,which contained chloride as well as several other common anions. Chromatographicseparation showed good resolution of the chloride peak from other common anions.

The analytical standards used for calibration of the instrument were prepared by serialdilution of the Alltech standard to yield standards over the calibration range of 0.1, 0.2, 0.4,1.0, and 2.0 ug/mL. Although method 9057 specifies preparation of these calibrationstandards in 0.1 N NaOH or 0.1 N H2S04 as appropriate, the standards were diluted in theeluant solution in order to achieve a more stable instrument background. Analysis ofstandards in either 0.1 N NaOH or 0.1 N H2S04 resulted in poor chromatographic separation ofthe chloride peak. This method modification was necessary to achieve instrument performanceto more closely match the diluted samples. Matrix spikes were used to assess the impact ofthis method modification.

A set of four quality control audit samples prepared by MRI's quality assurancecoordinator were analyzed in the same batch as the field samples and quality control samplesprepared by the analyst. All sample analyses were in duplicate as required by the method.

An instrument calibration curve was generated by analyzing the calibration solutionsbefore and after the sample analysis. The average peak area for each calibration level wascompared to the concentration, and linear regression was used to define the calibration curve.The area response for the chloride peak detected in sample chromatograms was used todetermine the concentration of chloride using the linear regression curve. The calibrationcurve was extrapolated below the lowest standard to estimate concentrations below thequantitation limit.

P. E. Nelson Turbochrom software, version 3.1 was used to acquire chromatographicdata and perform the linear regression calculations.

4.0 Sample Results

The sample results are presented in Table M-l. The detection limits for the samplesare reported as < 0.1 ug/mL.

Included in the sample results table are the accompanying acid and caustic field blanks.Although these results are reported < 0.1 ug/mL, the samples were overdiluted compared tothe field samples. The impact of this error is minimal because samples results were all belowthe detection limt. No response for chloride was noted for the quality assurance blanksamples above the 0.1 ug/ml detection limit.

AR3S523GADD CKII-ITV H

Table M-l. Risk Burn No. 2 Sample Results for Chloride

MRI Sample No.

53255327632563277325732753325333

Sample Name

Run5RunSRun 6Run 6Run 7Run 7

Field Blank (H2SO4)Field Blank (NaOH)

crReplU<0.1U<0.1U<0.1U<0.1U<0.1U<0.1U<0.1U<0.1

Found (mg/L)

Rep 2U<0.1U<0.1U<0.1U<0.1U<0.1U<0.1U<0.1U<0.1

Note: Duplicate sample analysis results are shown for all samplesU=Less than 0.1 ug/mL

5.0 Quality Control (QC) Results and Data Quality Assessment

The quality controls that were included with the sample batch were two calibrationcurves (one before sample analysis and one after sample analysis), independently preparedaudit samples, eluent method blanks, a spiked laboratory control sample, an acidic matrixspike, and a basic matrix spike.

5.1 Calibration CurvesThe calibration curve was generated from the average area response at each level of the

curve. The curve was generated using linear regression, and an revalue of 0.9996 wasobtained. Table M-2 summarizes the calibration data. The area response for the calibrationstandards analyzed at the beginning and end of the calibration sequence were consistent withgood precision shown as relative percent difference (RPD) in Table M-2. The accuracy of thevarious points comprising the calibration curve was determined by calculating each individualresponse versus the slope and intercept of the curve, curve. The accuracy for both the initialand end of analysis curves was acceptable.

5.2 Independent Audit SampleMRI's quality assurance unit provided independent audit samples to be analyzed with

the analytical batch. The results for these samples were corrected for the amounts found in thecorresponding quality assurance blanks. The sulfuric acid quality assurance sample wasquantitated as 104 percent of the theoretical amount and the sodium hydroxide sample wasquantitated as 100 percent of the theoretical amount. These results verified the accuracy of theanalytical system including both sample preparation and analysis.

5.3 Method BlanksThe blanks included 1C eluent method blanks prepared with the analytical batch, field

blanks of 0.1N sodium hydroxide and 0.1N sulfuric acid, and two independent audit sample

AR3I5237M

blanks. The eluent method blanks contained no measurable concentrations of chloride,indicating that none of the field samples were contaminated with chloride during the samplepreparation and dilution procedures. Results for field blanks and Quality Assurance blankswere also below the detection limit.

5.4 Laboratory Control Spike and Matrix SpikesThe result for the laboratory control spike sample was 86 % recovery. The acid matrix

spike (MSA) and basic matrix spike (MSB) were prepared in actual field samples to determinematrix affect on recovery. The results of these analyses were 95.6 percent recovery for theacid matrix and 126 percent recovery for the basic matrix. The high bias for the basic matrixwould indicate that the results for the actual caustic samples may be biased slightly high (butall samples were below the detection limit).

Table M-2. Calibration Curve Standard Statistics

Standardlevel

(ug/mL)

0.10

0.20

0.40

1.00

2.00

1st CALCurvePeakArea

133831

267009

506220

1308401

2551720

2nd CALCurvePeakArea126374

342130

505919

1326602

2587192

AverageCurvePeakArea130103

304570

506070

1317502

2569456

RPD(a)

5.7

25

0.06

1.4

1.4

1st CalCurve

Accuracy%(b)100

102

97.3

101

98.9

2nd CalCurve

Accuracy%

94.2

131

97.3

103

100

a- RPD = relative percent difference precision (high value-low value)/average X 100 %b- % Accuracy of individual standard calculated versus the linear regression calibration curve

=(calculated concentration/theoretical concentration) X 100 %

AR3I5238APPENDIX M

Appendix N

Continuous Emission Monitoring Data for SO2

MRI.AppKed'R3S2028.APP

RR315239

Appendix NContinuous Emission Monitoring for Sulfur Dioxide

MRI conducted Sulfur Dioxide (SO2) emission monitoring concurrently with all other MRIsampling methods during Risk Burn 2 for runs 5, 6, and 7. The SO2 monitor wasoperated in accordance with the Code of Federal Regulations, Part 60, Appendix A,Method 6C. A list of equipment used during the Sulfur Dioxide monitoring is providedbelow. Results for the three sample runs can be found in tables N-1, N-2 and N-3. - —Documentation of QA/QC checks, calibration gas certificates of analysis and thecalibration gas dilution system calibration certifications are found at the end of thisappendix.

The MRI SO2 monitor measures sample gas on a dry basis. The sample gas wasdrawn through a stainless steel probe and heated Teflon line to the sample gasconditioner. At the sample conditioner the moisture in the sample was removed beforecontinuing on to the gas distribution manifold. At the distribution manifold sample gasflow was regulated and supplied to the SO2 monitor at 1.5 liters per minute. The analogsignal from the SO2 monitor was collected in 1 second increments for 60 seconds. The60 readings were then averaged and recorded as 1 minute averages. The 1 minuteaverages were stored in an electronic format as well as being logged on the printer.

CEM Equipment

Stainless Steel ProbeHeated Sample Line - Technical Heaters 150 ft. @ 250 degrees FM&C Eclectro Gas Cooler - Type EC/ECSCalibration Gas Dilution System - Environics Model 2020Gas Distribution Manifold - MRI DesignSulfur Dioxide Analyzer - Western Research Model 721 ATMData Logger Software - Labtech NotebookData Logging Computer - WinBook XPPrinter - Panasonic Model KX-P1180

M

Table N-1 SO2 Data for Run 5Project No. 3620-28-30 Drake OHM RSCOperator: Gulick Date: 2/7/97

TIME SO2 TIME SO2 TIME SO2(24 hr) (ppm) (24 hr) (ppm) (24 hr) (ppm)

1150 0.0 1230 0.1 1310 0.01151 0.0 1231 0.0 1311 0.01152 0.0 1232 0.0 1312 0.01153 0.0 1233 0.0 1313 0.01154 0.0 1234 0.0 1314 0.11155 0.0 1235 0.1 1315 0.01156 0.1 1236 0.0 1316 0.01157 0.0 1237 0.0 1317 0.21158 0.0 1238 0.0 1318 0.01159 0.0 1239 0.0 1319 0.01200 0.0 1240 0.0 1320 0.01201 0.0 1241 0.1 1321 0.01202 0.1 1242 0.0 1322 0.01203 0.0 1243 0.4 1323 0.01204 0.0 1244 0.1 1324 0.01205 0.0 1245 0.0 1325 0.01206 0.0 1246 0.0 1326 0.01207 0.0 1247 0.01208 0.0 1248 0.0 1421 0.01209 0.0 1249 0.0 1422 0.01210 0.0 1250 0.0 1423 0.01211 0.0 1251 0.0 1424 0.01212 0.0 1252 0.0 1425 0.01213 0.0 1253 0.0 1426 0.01214 0.0 1254 0.0 1427 0.01215 0.0 1255 0.0 1428 0.01216 0.0 1256 0.0 1429 0.01217 0.0 1257 0.0 1430 0.01218 0.0 1258 0.0 1431 0.01219 0.0 1259 0.0 1432 0.01220 0.0 1300 0.0 1433 0.01221 0.0 1301 0.0 1434 0.01222 0.0 1302 0.0 1435 0.01223 0.0 1303 0.1 1436 0.01224 0.0 1304 0.0 1437 0.01225 0.1 1305 0.0 1438 0.01226 0.0 1306 0.2 1439 0.01227 0.0 1307 0.0 1440 0.01228 0.1 1308 0.1 1441 0.01229 0.0 1309 0.0 1442 0.0

AR3I52UAPPENDIX N

Table N-1 (cont.)

TIME SO2 TIME S02(24 hr) (ppm) (24 hr) (ppm)

1443 0.0 1528 0.01444 0.0 1529 0.01445 0.0 1530 0.01446 0.0 1531 0.01447 0.0 1532 0.01448 0.0 1533 0.01449 0.0 1534 0.01450 0.0 1535 0.01451 0.0 1536 0.01452 0.0 1537 0.01453 0.0 1538 0.01454 0.0 1539 0.01455 0.0 1540 0.01456 0.0 1541 0.21457 0.0 1542 0.01458 0.0 1543 0.01459 0.0 1544 0.01500 0.0 1545 0.01501 0.0 1546 0.0

1547 0.01504 0.0 1548 0.01505 0.0 1549 0.01506 0.0 1550 0.01507 0.0 1551 0.01508 0.1 1552 0.01509 0.0 1553 0.01510 0.0 1554 0.01511 0.0 1555 0.01512 0.0 1556 0.01513 0.0 1557 0.01514 0.0 1558 0.01515 0.0 1559 0.01516 0.0 1600 0.01517 0.01518 0.0 Minimum 0.01519 0.01520 0.0 Maximum 0.41521 0.01522 0.0 Average 0.01523 0.01524 0.01525 0.01526 0.01527 0.3

APPENDIX N

Table N-2 So2 Data for Run 6Project No. 3620-28-30 Drake OHM RSCOperator: Gulick Date: 2/8/97


1100 0.0 1141 0.0 1222 0.01101 0.0 1142 0.0 1223 0.01102 0.0 1143 0.0 1224 0.01103 0.0 1144 0.0 1225 0.01104 0.0 1145 0.0 1226 0.01105 0.0 1146 0.0 1227 0.01106 0.0 1147 0.0 1228 0.01107 0.0 11.48 0.0 1229 0.01108 0.0 1149 0.0 1230 0.01109 0.0 1150 0.0 1231 0.01110 0.0 1151 0.0 1232 0.01111 0.0 1152 0.0 1233 0.01112 0.0 1153 0.0 1234 0.01113 0.0 1154 0.0 1235 0.01114 0.0 1155 0.0 1236 0.01115 0.0 1156 0.0 1237 0.01116 0.0 1157 0.0 1238 0.01117 0.0 1158 0.0 1239 0.01118 0.0 1159 0.0 1240 0.01119 0.0 1200 0.0 1241 0.01120 0.0 1201 0.0 1242 0.01121 0.3 1202 0.0 1243 0.01122 0.0 1203 0.2 1244 0.01123 0.0 1204 0.01124 0.0 1205 0.0 1331 0.01125 0.0 1206 0.0 1332 0.01126 0.0 1207 0.0 1333 0.21127 0.0 1208 0.0 1334 0.01128 0.0 1209 0.0 1335 0.01129 0.0 1210 0.0 1336 0.01130 0.0 1211 0.0 1337 0.01131 0.0 1212 0.2 1338 0.01132 0.0 1213 0.0 1339 0.01133 0.0 1214 0.0 1340 0.01134 0.0 1215 0.0 1341 0.01135 0.0 1216 0.0 1342 0.01136 0.0 1217 0.0 1343 0.01137 0.0 1218 0.0 1344 0.01138 0.0 1219 0.0 1345 0.01139 0.0 1220 0.0 1346 0.01140 0.0 1221 0.0 1347 0.0

APPENDIX N

Table N-2 (cont.)


1348 0.0 1427 0.0 1506 001349 0.0 1428 0.0 1507 001350 0.0 1429 0.0 1508 0.01351 0.0 1430 0.0 1509 001352 0.0 1431 0.0 1510 001353 0.0 1432 0.0 1511 001354 0.0 1433 0.0 1512 001355 0.0 1434 0.0 1513 001356 0.0 1435 0.0 1514 001357 0.0 1436 0.01358 0.0 1437 0.0 Minimum 0.01359 0.0 1438 0.0 Maximum 0.41400 0.0 1439 0.0 Average 001401 0.0 1440 0.01402 0.0 1441 0.01403 0.0 1442 0.01404 0.0 1443 0.01405 0.0 1444 0.01406 0.3 1445 0.01407 0.0 1446 0.01408 0.0 1447 0.01409 0.0 1448 0.01410 0.0 1449 0.01411 0.0 1450 0.01412 0.0 1451 0.01413 0.0 1452 0.01414 0.0 1453 0.01415 0.0 1454 0.01416 0.0 1455 0.01417 0.0 1456 0.01418 0.0 1457 0.01419 0.4 1458 0.01420 0.0 1459 0.01421 0.0 1500 0.01422 0.0 1501 0.01423 0.0 1502 0.01424 0.0 1503 0.01425 0.0 1504 0.01426 0.0 1505 0.0

Table N-3 SO2 Data for Run 7Project No. 3620-28-30 Drake OHM RSCOperator: Gulick Date: 2/9/97

TIME S02 TIME SO2 TIME SO2(24 hr) (ppm) (24 hr) (ppm) (24 hr) (ppm)

1045 0.0 1126 0.0 1207 0.01046 0.0 1127 0.0 1208 0.01047 0.0 1128 0.0 1209 0.01048 0.0 1129 0.0 1210 0.01049 0.0 1130 0.0 1211 0.01050 0.0 1131 -0.0 1212 0.01051 0.0 1132 0.0 1213 0.01052 0.1 1133 0.0 1214 0.01053 0.0 1134 0.0 1215 0.01054 0.0 1135 0.0 1216 0.21055 0.0 1136 0.0 1217 0.01056 0.0 1137 0.0 1218 0.01057 0.0 1138 0.0 1219 0.01058 0.0 1139 0.0 1220 0.01059 0.0 1140 0.0 1221 0.01100 0.0 1141 0.0 1222 0.01101 0.0 1142 0.0 1223 0.01102 0.0 1143 0.0 1224 0.01103 0.0 1144 0.0 1225 0.01104 0.0 1145 0.0 1226 0.01105 0.0 1146 0.0 1227 0.01106 0.0 1147 0.0 1228 0.01107 0.0 1148 0.0 1229 0.01108 0.1 1149 0.01109 0.0 1150 0.0 1256 0.01110 0.0 1151 0.0 1257 0.01111 0.0 1152 0.0 1258 0.01112 0.0 1153 0.0 1259 0.01113 0.0 1154 0.0 1300 0.01114 0.0 1155 0.0 1301 0.01115 0.0 1156 0.0 1302 0.01116 0.0 1157 0.0 1303 0.01117 0.0 1158 0.0 1304 0.01118 0.0 1159 0.0 1305 0.01119 0.0 1200 0.0 1306 0.01120 0.0 1201 0.0 1307 0.01121 0.0 1202 0.0 1308 0.01122 0.0 1203 0.0 1309 0.01123 0.0 1204 0.0 1310 0.01124 0.0 1205 0.0 1311 0.01125 0.0 1206 0.0 1312 0.0

APPPwnry M

Table N-3 (cont.)

TIME S02 TIME S02 TIME SO2(24 hr) (ppm) (24 hr) (ppm) (24 hr) (24 hr)

1313 0.0 1350 0.0 1427 0.01314 0.0 1351 0.0 1428 0.01315 0.0 1352 0.0 1429 0.01316 0.0 1353 0.0 1430 0.01317 0.0 1354 0.0 1431 0.01318 0.0 1355 0.0 1432 0.01319 0.0 1356 0.0 1433 0.01320 0.0 1357 0.0 1434 0.01321 0.0 1358 0.0 1435 0.01322 0.0 1359 0.0 1436 0.01323 0.0 1400 0.0 1437 0.01324 0.0 1401 0.0 1438 0.01325 0.0 1402 0.01326 0.0 1403 0.3 Minimum 0.01327 0.0 1404 0.11328 0.0 1405 0.0 Maximum 0.31329 0.0 1406 0.01330 0.0 1407 0.0 Average 001331 0.0 1408 0.01332 0.0 1409 0.01333 0.1 1410 0.01334 0.0 1411 0.01335 0.0 1412 0.01336 0.0 1413 0.01337 0.0 1414 0.01338 0.0 1415 0.01339 0.0 1416 0.01340 0.0 1417 0.01341 0.0 1418 0.01342 0.0 1419 0.01343 0.0 1420 0.01344 0.0 1421 0.01345 0.0 1422 0.01346 0.0 1423 0.01347 0.0 1424 0.01348 0.0 1425 0.01349 0.0 1426 0.0

APPENDIX N

CEMQA/QC Checks for SO2Span Drifts for Risk Burn 2

Initial Value Final Value Difference as % of Pass/Fail(ppm) (ppm) Instrument Full Scale

Run5 200.8 199.3 0.8 Pass

Run 6 201.1 196.6 2.3 Pass

Run? 201.5 198.6 1.5 Pass

Zero Drifts for Risk Burn 2

Initial Value Final Value Difference as % of Pass/Fail(ppm) (ppm) Instrument Full Scale

Run 5 0.3 0.0 0.2 Pass

Run 6 0.0 0.0 0.0 Pass

Run 7 0.0 0.0 0.0 Pass

Instrument Full Scale Value for SO2 is 200 ppmPass/Fail Criteria for Zero and Span Drift is +/- 3% of Instrument Full Scale

Bias Checks performed on 1/20/97

Cal Gas Instrument Difference as % ofValue Reading Instrument Full Scale Pass/Fail(ppm) (ppm)

SO2 100.00 97.3 1.4 Pass

Instrument Full Scale Value for SO2 is 200 ppm.Pass/ Fail Criteria for all instruments is +/- 5% of Instrument Full Scale.

Response Time

1 Minute, 22 Seconds

APPENDIX N

CEM QA/QC Checks for SO2

for 2/7/97(Risk Burn 2 - Run 5)

Calibration Error Check

Cal Gas Instrument Difference as % ofValue Reading Instrument Full Scale Pass/Fail

SO2 0.0 0.3 0.2 Pass(ppm) 200.0 200.8 0.4 Pass

100.0 98.9 0.6 Pass50.0 48.4 0.8 Pass




SO2 0.0 0.0 0.0 Pass(ppm) 200.0 201.1 0.6 Pass

100.0 100.0 0.0 Pass50.0 49.5 0.3 Pass




SO2 0.0 0.0 0.0 Pass(ppm) 200.0 , 201.5 0.8 Pass

100.0 100.1 0.1 Pass50.0 49.0 0.5 Pass

Instrument Full Scale Value for SO2 is 200 ppmPass/Fail Criteria for All Instruments is +/- 2% of Instrument Full Scale

AR3152U8APPFMnry w

ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET

Mf #: 1, Description: AIR , Size: 10000. SCCM, K-factor: 1.0

SERIAL # *3±s:&JLt.g£.________

This flow controller was calibrated using a Sierra Cal Bench(TM), a traceablePrimary Flow Standard Calibration System. This calibration is referenced todry air at a temperature of &2.F (_C) and a pressure of 29.92 in .Hg (760Torr)

Set. Flow True Flow5 % 500.0 CCM 498.79 CCM13 r; 3000.0 CCM 1009,0 COM20 % 2000.0 CCM 2029.8 CCM30 % 3000.0 CCM 3058.2 CCM40 % 4000.0 CCM 4088.8 CCM50 y. 5000.0 CCM 5121.9 CCM60 % 6000.0 CCM 6143.3 CCM70 % 7000.0 CCM 7178.3 CCM80 * 8000.0 CCM 8206.3 CCM90 % 9000.0 CCM 9224.6 CCM100% 10000. CCM 10252. CCM

Calibration data was last saved on Friday 03 January 97 at 16:22:00

Verified by: j4*rJ>L 4f v ueH**** Date:.

ftR3!52i*9APPENDIX N 1O

I I


Mf #: 2, Description: AIR , Size: 10000, SCCM, K-factcr: 1.0

SERIAL #

This flow controller was calibrated using a.Sierra Cal BenchCTM), a traceablePrimary Flow Standard Calibration System. This calibration is referenced todry air at a temperature of AJLF C_C) and a pressure of 29.92 in.Hg (760Torr)

Set Flow True Flow5 % 500.0 CCM 510.51 CCM3n % 1000.Q CCM 1021.4 CCM20 % kOOO.O CCM k046.9 CC!'.30 % 3000.0 CCM 3074.8 CCM40 % 4000.0 CCM 4103.8 CCM50 % 5000.0 CCM 5136.6 CCM60 H 6000.0 CCM 6156.8 CCM70 % 7000.0 CCM 7182.5 CCM80 % 8000.0 CCM 8203.3 CCM90 % 9000.0 CCM 9219.5 CCMlOOss 10000. CCM 10233. CCM

Calibration data was last saved on Friday 03 January 97 at 17:09:00

Verified by:_M.«jfcjL._ 5 t SZ e ^ Date :__/_-_»3__-_SL2L

AR3I5250APPENDIX N 11

Mf #: 3, Description: AIR , Size: 1000.0 SCCM, K-factor: 1.0

SERIAL #

This flow controller was calibrated using a Sierra Cal Bench(TM), a traceablePrimary Flow Standard Calibration System. This calibration is referenced todry air at a temperature of §2-F ( _ C) and a pressure of 29,92 in .Hg ( 760Tor,r )

Set Flow True Flow5 5s 50.0 CCM 50.515 CCM10 % 100.0 CCM 101.84 CCM20 * 200.0 CCM 204.84 CCM30 X 300.0 CCM 306.67 CCM40 & 400.0 CCM 408.82 CCM50 % 500.0 CCM 510.43 CCM60 % 600.0 CCM 6:M. 44 rr,M70 * 700.0 CCM 713.69 CCM80 % 800.0 CCM 816.61 CCM90 % 900.0 CCM 918.19 CCM

C::;'.Tni.M.l1 ' jn df**,o. />au last savert on I** i'JUy 03 January 57 at 17:55:00

Verified by; X<vJ2- $ e JtLuuv-w Date:,

RR31525IAPPENDIX N 12

Mf #: 4, Description: AIR . , Size; 100.0 SCCM , K-factor: 1.0

SERIAL # /)«?<?*/ a. o«y 9 _________

S flOW C'"""'*'v*'*'11or' U7a c r£> 1 * Vjr-at «=>H uc i rirr a CM arr- a C» 1Primary Flovv Standard Calioraticn Syst&m. This calibre.t i o\ is referenced todry air at a ".eniper *ture cf &£.:•' ( _ C) and a p-essure of 2r/.92 in.Hg ( 760Torr

Set Flow True Flo:3 X 5.0 CCM 5. 2? 6 CC'I10 s 10 0 CCM 10.?6r- CCM20 Si 20 0 CCM TO S4 CCM30 % _ CCM ..u.524 CCM '40 % i.- CCM -I" 606 CCM50 :. . - » ? 0 CCM ;••: 5^C CCMoO ?S iC.O CCM 6C..-:-?3 Cu.M70 "= 7J.u OCh v^."7v? CCMCo °~ ?0.0 CCM DC ?1 7 0.1Mi<0 S5 90.0 CCfi 91.035 C'Ji_Gue, H-:.C CCM 101.1? CCM

ion date, was last s>--v©<a on Fri^-y 03 Janaavy 97 . at 19:11

VP r .<. f. i ed dy:._ 'A> U_ / aCU>_. Dite :__/__-_,2_.._-_jr J?_

AR3I5252A PPPMOTY M

p. 14

LIQUID CARBONICCYLINDER GAS PRODUCTS

STOO SOUTH ALAMEDA STBEET • LOS ANGELES, CA soosa

- -' ' - _'--: ..tv-i;/. t-*~.fj? D'prc'-, •i &KxJkJcifi

, ,» .... ^ ft ' .w ,,•.?.*•*»' r. *»!%•->, . •'•*• «j •; PA ii">i *'»a

CUSTOMER EID

COMPONENTSULFUR DIOXIDE s*»#90-46B

j

tic ^ SKi is iKii ioiMis :•i-7%:-,-. i-v. .: -->j •„:• • :.t£i*f<Z*v&:.i '• !*'$.;<$}*•*'•, , '.s* • : . i-i'-.i-fftw:-:*-.. lAZ™. ; .,•;•',:.. ,:~ ,:. .. .-' :>,n . >- j!; <% ;5.J~;vv,::::«K.» .:.,«.,. • -. •••... ••• -.•i*--. •• •

P.O NUMBER 032295-1

• JM?i?jiT3 j iiri'C'riPJWDi Jtyni •KJ CiiKJ fH Ef jJ BU\4JAJUJ

NiyrSRMNO. CYLINDER NO. '> CONCENTRATTON1696» CLH-004064 , 3125 ppm

•j

wn iKK&m --R^REFERENCE STANDARD Z=ZSROGAS C^GAS CANDIDATE

1. COMPONENT SULFUft DIOXIDE sanWO-468 ANALYZER MAKB-MODEL-S/N Siemens Uttraaat 5E S/H C1-009ANALYTICAL PRINCIPLE NDIR . LAST CALIBRATION DATE 03/22/95

I Y J R S T ANALYSIS DATE 4/06/95 SECOND ANALYSIS DATE 4/13/95Z o R 3125 C 2710 CONC. 2710 ppai Z 0 R 3125 : C 2710 CONC. 2710 ppmR 3125 Z 0 C Z710 CONC. 2710 fp* R 3125 Z 0 C 2710 CONC. 2710 ppnZ o C 2710 R 3125 CONC. 2710 ppm Z 0 C 2710 , R 3130 CONC. 3706 ppnU/M pps MEAN TEST ASSAY 2710 ppm U/M ppm MEAN TEST ASSAY 2709 ppm

I : ' *1

11!1

iI

(

iPROCEWJRE G2 60X DILUTION. GA4 DIVIDER STEC Inc. TYPE SOG-7104/06/95 4516.7 ppm SULFUR DIOXIDE4/13/95 4515. 0 ppm SULFUR DIOXIDE

, )

, lii • •• "" : " •"•" ' i: ! THIS CYLINDER NO. SA13860 CERTIFIED CONCENTRATION! (US BEEN CERTIFIED ACCORDING TO SECTION EPA-400/R93/224 SULFUR DIOXIDE 4516 ppm

OF TRACEABEUTY PROTOCOL NO. Rev. 9/93 NITROCSH BALANCE ;• PROCEDURE 02 :I j CERTU-1K1> ACCURACY ±2 % NIST TRACEABLE •; i CYLINDER PRESSURE 2000 ' PSIG !!: CERTCTtCA-TlON DATE 04/13/95 " .- \: txpcRAtiON DATE 04/13/93 TERM 36 MONTHS •. :|

/ _

ANALYZED BY

r / sf C __ -"'// /S &y S. " !/ -J&~> // AAJ=. DU fC - - ————— —— CERTIFIED BY - j P . % >~X /H-BK- J

VEHAH^STlir '.V iflWM fr-YOWjK! <i ' •

AR3I5253APPENDIX N 14

Appendix OExample Calculations

This appendix presents example calculations for several of the tables presented in thereport to help the reader understand how values in the tables were calculated frommeasured values. An attempt has been made to round all values presented in the tables tothe correct number of significant figures. However, when a calculated value is also used insubsequent calculations in the same table, then one or more extra digits beyond thesignificant figures may be carried with that value.

flR3!5255APPFNDTX O

Example Calculations

Table 3.1-2 Run 5

(g'.O mg) 1 0.01543 1 = 0.123 grains\ ™g )

0.123 grains _ 00(m7 grains104.8 dscf dscf

( oom 17 ST™™} f Sram } ( 35.314 dscf} n 0fiR gra/ws^ <&£/' J 15.43 grains) \ dscm ) dscm

f 0.00117 S™H f 8'5 ) = 0.000956 aim\ dscf ) ( 10.4 J ifec/

fnonoosfi S "5! f ™S } ( 5.314 dscf} _ 0 wg^ <sfec/ / \ 0.01543 grains) \ dscm ) dscm

\

f 000 68 aH fs97 dscm\ ( min ) 00 67 gI V.V/w^«\JO 1 1 «•> ^ .mi.-..-—., i 1 .... ....— 1 \J.\sjb\J 1 •— -^

\^ dscm ) \ min ) \ 60 secy sec

foO"67 *} f3600sec] f lb } -o-l- 7*V secj V AoMr J V 453.59 g) hr

Values Enteredin Table

0.12 grains

0.00096grains/dscf

2.2 mg/dscm

0.027 g/sec

0.21 Ib/hr

AR3I5256

Fable 3.2-1 Run 5 acidic impingers

| 0.05 - 1 (3.183 L) = 0.159 mg\ L )

0.16 x I0-3g _ 00536o Y 10-s g _ 5 30 10-s g2.969 ofcc/w tffcc/H akc/w

(539 x lO'5 8 } (597 dscm] { min ) 5363 x 10'4 *1 -J t^J *V JL w 1 1 <J J 1 11 ——'•"•'«"- i ' +JfJ\JJ A- IV

V dscm) \ min y V 60 sec) sec

(5 363 YlO-4 g] t^-5SffCl] _ 551/|xlo-4 g( sec) ( 35.5g Cl ) sec

f 5 511 x 1C'4 ^ ) f 36°° S6C) f 7* ) - 13 76 x lO'4 7*^ sec ) ( hr ) ( 453.59 g) hr


0.16mg

5.4 x 10'5 g/dscm

5.4 x lO"4 g/secCl

5.5 x 10-4 g/secHC1

4.4 x lO'3 Ib/hrHC1

AR3I5257n

1 I


Table 3.3-1 Benzene Run 5

5261 ng + 5760 ng + 5683 ng + 6413 ng = 23,117 ng

23,117 ng _ ng11. SI L L

Fable 3.3-4 Benzene Run 5

4 ng _ ng56.59 L L

Table 3.3-7 Benzene Run 5

f 0.07 M) + (298 »S\ = 298.07 M1 L) ( L) L

( 298.1 x ID'9 £) f-l i) ( 597 2" V = 0.1780 -J-^ -^/ \ dscm) \ min y min

(0 1 7SO ^ • 1 1 min - 0 OfPQfi? 8 - 'y Q7/r n^ ^v. 1 / O\J 1 1 .1——— i \Jt\J\J y\j 1 ~" j .y / J-J w.J

minj \ 60 secj sec sec

f 000 967 g] f3600 Sec) f 7* ) -00^355 lb( sec) ( hr ) ( 453.59 g) A/-


23,117

298ng/L

0.07 ng/L

298ng/L

2.97E-03 g/sec

2.36E-02 Ib/hr

flR3IS258APPFMDTV O


Table 3.3-11 4,4-DimethyI-2-oxetanone(2-butene?) Run 5

49 ng + 45 ng + 0 ng + 28 ng = 122 ng

122 = 1.574 W^ = 1.574 77.52 L Z, dscm

Fable 3.3-14 Benzene Run 5

(->98 ^ ) fs97 *CW) f """ 1 °65i ^^u — i i _; _^ y .,,„,,..—...... II ' "'" 1 4*^y\JJ

\ dscm) \ min y ^ 60 secj sec

f o n65 T 10-3 ^ ) f 3600 sec] ( 76 \_ Ib{ sec) ( hr ) ( 453.59 g) hr


122ng

1.57ng/L

2.97E-03 g/sec

2.35E-02 Ib/hr

AR3I5259APPENDIX O


Table 3.4-1 2-Nitrophenol Run 5

5-54 \ig _ \ig3.056 dscm dscm

Table 3.4-2 2-Nitrophenol Run 5

fl8 ^ } ( l'g } (597 *C/W) f min } 1791 x IQ-5 g\ dscm) ( 1,000,000 \ig) \ min ) \ 60 sec) sec

f i 7-1 X- io-5 * H /& If 360° sec) - i r r io-4 7*( secj ( 453.6 g) ( hr ) hr

Aldrin, Table 3.4-4 Run 5

0-25 pg _ ^ ug3.056 Ac/w fifec/w

Table 3.4-7

f 00818 ^ ) f ! -) fs97 *CW) f "^ ) - 8 110 x 10'7 ^ dscm) \ 1,000,000 \ig) ( min ) \ 60 sec; sec

f * 110 x IO-7 * H lb H 36°° S6C) - 6 160 r IO-6 lb( secj ( 453.6 g) ( hr ) hr


1.8 jig/dscm

1.8xlO-5g/sec

1.4 x 10 -" Ib/hr

0.082 \ig/dscm

8.1xlO'7g/sec

6.5 x 10 -6 Ib/hr

AR3I5260APPFNDTV o


Butoxyethoxyethanol Table 3.4-10

250 iig3.056 dscm

fo181 V-g } ( 1 g } (507("" dscm) ( 1,000,000 pg)

( 8.140 xKT4 g] { lb }( secj I, 453.6 g)

- 81 81 dscm

dscm\ ( min ^ _ g 1/IO 1Q-4 gmin y V 60 secy sec

( 3600 sec^ , .„ 1A-3 76————— - 6.460 x 10 J —^ hr } hr


82 ng/dscm

S.lxlO^g/sec

6.5 x 10 -3 Ib/hr

AR3I526APPFNDTY O

Table 3.5-1 D/F Run 5

Total DIP = 3.94 ng

3-94 ng _ _j 0/16 ng3.162 <&c/« ffcc/w

fl^6 ng } ( 8'5 ) - 1018 ng\ dscm) \ 10.4) dscm

Table 3.5-3 1,2,3,4,7,8-HxCDD Run 5

[ °-01° "g } (0.1) - 0.000316 "g equivalent\ 3.162 dscm) dscm

Table 3.5-3 Run 5

Total 2,3,7,8 -TCDD equivalent - 0.020 ngdscm

foO^O ng } ( 8'5) - 00163 ngI \J.\J 6*\J - ~ 1 1 »'•-—• • .1 \Jt\Ji\J*J '

\ dscm) \ 10.4) dscm

(oO"Ox ID'9 8 } fs97 dscm] ( min ) 0199x lO'9 8• ^ V^ V ^ JL V - -•-- 1 1 y 1 "" 1 1 ' i™1™1 """•'» i \J . i S J A 1\J ___—

^ dscm) \ min j \ 60 secj sec

f 0 19" * 1C'9 ^ ) f 36°° S6C) f lb 1 - 1 57« r ID'9 7*i^ secj ( /;r J 453.59 g) hr


1.25 ng/dscm

1.02ng/dscm

3.2E-04 ng/dscm

0.016 ng/dscm

2:OE-10 g/sec

1.6E-091b/hr

AR3I5262APPENDIX O 8

Table 3.6-5 MonoPCB Run 5

122 ng _ ,_ ,_ ng3.158 dscm dscm

f3863 "g } (597 dscm] { """I - 3314 ng\ dscm) \ min ) \ 60 secj sec

(3 <M1E-07 * ) f 36°° S6C) f 7* 1 - 3051£ 07 /6V secj ( hr ) ( 453.59 g) hr

Table 3.7-1 Arsenic Run 5

BlankMeasured Correction

Rinse and filter 2.22 ng - 0.58 ng = 1.64 ng

HNO3 Impingers <0.12ng - Ong = 0.06 ig at Yt D.L.

Total =1.70ug

1-70 »g _ 5fft vg3.025 dscm dscm

(o56^0xlO-6 g } (597 CW) f min ) 559^xlQ-6 8\ dscm) \ min ) { 60 secj sec

(55^x 10-6 g } ( 3600 sec i [ 1b } _ 38 1Q-6 lb\ secj ( hr ) \ 453.59 g) hr


38.6 ng/dscm

3.84E-07 g/sec

3.05E-06 Ib/hr

1.70 g

0.562 |xg/dscm

5.59E-06 g/sec

4.44E-05 Ib/hr

AR3I5263o

Fable 3.8-1 Run 5

<0.5 -H£ = 0.25 - at 1/2 D.L.L L

1 0.25 Ml (2.769 L) = 0.692 \ig\ -^ /

0.692 _ 539 ng1.283 dlsc/H afcc/w

fo539r ID'6 g } fso? *cwlf "^n ) - 5 36 x 10-6 g\ dscm) \ min )\ 60 secy sec

f 5 36 Y 10-6 «• 1 f 360° S6C) f /6 ) - r 5 r 10^ /Z>^ secj ( hr j ( 453.59 g) hr


0.25 ng/L

0.69 ng

0.54 (ig/dscm

5.4E-06 g/sec

4.2E-05 Ib/hr

APPPMHTY n 1O


Table 3.1 1-4 1,2,3,4,6,7,8-HpCDD Run 5

I 6.14 - 1 (0.01) = 0.06141 kg)

— equivalentkg


0.0614ng/kg

AR3I5265APPP-MPITY n

run 7 · 2020-03-04 · stack axis #1 (meters)= 1.829 stack axis #2 (meters)= 1.829 circular stack...

Documents