United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, IMC 27711
EPA-454/R-99-001C
February 1999
AIR
   SEPA
   Final Report - Volume III of
   Emissions Testing of Combustion
   Stack and Pushing Operations at
   Coke Battery No. 2 at Bethlehem
   Steel Corporation's Burns Harbor
   Division in Chesterton, Indiana

-------
                 FINAL REPORT
 EMISSIONS TESTING OF COMBUSTION STACK AND
PUSHING OPERATIONS AT COKE BATTERY NO. 2 AT
       BETHLEHEM STEEL CORPORATION'S
            BURNS HARBOR DIVISION
            IN CHESTERTON, INDIANA

                    Volume III
              Appendices D through G
            EPA Contract No. 68-D-98-004
              Work Assignment No, 2-01


                   Prepared for:

              John C, Bosch Jr. (MD-19)
              Work Assignment Manager
            SCGA, EMC, EMAD, OAQPS
          U.S. Environmental Protection Agency
           Research Triangle Park, NC 27711

                  February 1999
                 p:\sSl I ,QOO\fma!rpt.wp
-------
                                  DISCLAIMER

      This document was prepared by Pacific Environmental Services, Inc. (PES) under EPA
Contract No. 68D98004, Work Assignment No. 2-01. This document has been reviewed
following PES' internal quality assurance procedures and has been approved for distribution.
The contents of this document do not necessarily reflect the views and policies of the U.S. EPA.
Mention of trade names does not constitute endorsement by the EPA or PES.
                                        n

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                       TABLE OF CONTENTS
1.0   INTRODUCTION	1-1

2.0   SUMMARY OF RESULTS  	2-1

     2.1   EMISSIONS TEST LOG	2-1
     2.2   FILTERABLE PARTICULATE MATTER, METHYLENE CHLORIDE
          EXTRACTABLE MATTER (MCEM), AND METALS	2-1
     2.3   POLYCYCLIC AROMATIC HYDROCARBONS (PAHs)	2-22

3.0   PROCESS AND CONTROL EQUIPMENT OPERATION	3-1

     3.1   INTRODUCTION	3-1
     3.2   PROCESS DESCRIPTION	3-1
     3.3   PROCESS AND CONTROL DEVICE MONITORING	3-4

4.0   SAMPLING LOCATIONS	4-1

     4.1   COKE OVEN BATTERYNO. 2	4-1

5.0   SAMPLING AND ANALYTICAL PROCEDURES	 5-1

     5.1   LOCATION OF MEASUREMENT SITES AND
          SAMPLE/VELOCITY TRAVERSE POINTS  	.5-1
     5.2   DETERMINATION OF STACK GAS VOLUMETRIC FLOW RATE 	5-3
     5.3   DETERMINATION OF STACK GAS EMISSION RATE CORRECTION
          FACTORS, DRY MOLECULAR WEIGHT, AND EXCESS AIR  	5-3
     5.4   DETERMINATION OF STACK GAS MOISTURE CONTENT 	5-3
     5.5   DETERMINATION OF PARTICULATE MATTER/METHYLENE
          CHLORIDE EXTRACTABLE MATTER/METALS	 5-3
     5.6   POLYCYCLIC AROMATIC HYDROCARBONS 	5-4
                               in

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                   TABLE OF CONTENTS (Concluded)
6.0   QUALITY ASSURANCE/QUALITY CONTROL PROCEDURES
     AND RESULTS	6-1

     6.1   CALIBRATION OF APPARATUS 	6-1
     6.2   ON-SITE MEASUREMENTS  	6-5
     6.3   LABORATORY ANALYSES  	6-9
APPENDIX A  PROCESS DATA
APPENDLXB  RAW FIELD DATA
APPENDLX C  ANALYTICAL DATA
APPENDIX D  CALCULATIONS
APPENDIX E  QA/QC DATA
APPENDIX F  PARTICIPANTS
APPENDIX G  SAMPLING AND ANALYTICAL PROCEDURES
                              IV

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                                   LIST OF TABLES
                                                                                 Page
Table 2.1     Emissions Test Log, Bethlehem Steel Corporation, Chesterton,
             Indiana	,	2-2
Table 2.2     Particulate Matter/MCEM/Metals Emissions Sampling and Flue Gas
             Parameters - Baghouse Inlet, Bethlehem Steel, Chesterton, Indiana	2-4
Table 2.3     Filterable Particulate Matter Concentrations and Emission Rates -
             Baghouse Inlet, Bethlehem Steel, Chesterton, Indiana	2-5
Table 2.4     Methylene Chloride Extractable Matter Concentrations and Emission
             Rates - Baghouse Inlet, Bethlehem Steel, Chesterton, Indiana	2-6
Table 2.5     Multiple Metals Concentrations and Emission Rates Baghouse Inlet,
             Bethlehem Steel, Chesterton, Indiana  	,	2-7
Table 2.6     Particulate Matter/MCEM/Metals Emission Sampling and Flue  Gas
             Parameters - Baghouse Outlet, Bethlehem Steel, Chesterton, Indiana  ...... 2-12
Table 2.7     Filterable Particulate Matter Concentrations and Emission Rates -
             Baghouse Outlet, Bethlehem Steel, Chesterton, Indiana	 2-13
Table 2.8     Methylene Chloride Extractable Matter Concentrations and Emission
             Rates - Baghouse Outlet, Bethlehem Steel, Chesterton, Indiana	2-14
Table 2.9     Multiple Metals Concentrations and Emission Rates - Baghouse Outlet,
             Bethlehem Steel, Chesterton, Indiana  ,.,......	2-15
Table 2.10    Baghouse Dust Multiple Metals Concentrations, Bethlehem Steel,
             Chesterton, Indiana	2-18
Table 2.11    Filterable Particulate Matter and Methylene Chloride Extractable
             Matter Removal Efficiencies, Coke Oven Battery No. 2 Baghouse,
             Bethlehem Steel, Chesterton, Indiana  	2-20
Table 2.12    Particulate Matter/MCEM/Metals Emissions Sampling and Flue Gas
             Parameters - Underfire Stack, Bethlehem Steel, Chesterton, Indiana	2-21
Table 2.13    Filterable Particulate Matter Concentrations and Emission Rates -
             Underfire Stack, Bethlehem Steel, Chesterton, Indiana		2-23
Table 2.14    Methylene Chloride Extractable Matter Concentrations and Emission
             Rates - Underfire Stack, Bethlehem Steel, Chesterton, Indiana  	2-24
Table 2.15    Multiple Metals Concentrations and Emission Rates - Underfire Stack
             Bethlehem Steel, Chesterton, Indiana	2-25
Table 2.16    PAH Emissions Sampling and Flue Gas Parameters - Baghouse  Inlet
             Bethlehem Steel, Chesterton, Indiana  	2-29
Table 2.17    PAH Concentrations and Emission Rates, Baghouse Inlet,
             Bethlehem Steel, Chesterton, Indiana  	2-30

-------
                            LIST OF TABLES (Concluded)
Table 2,18    PAH Emissions Sampling and Flue Gas Parameters - Baghouse Outlet
             Bethlehem Steel, Chesterton, Indiana	2-34
Table 2.19    PAH Concentrations and Emission Rates, Baghouse Outlet,
             Bethlehem Steel, Chesterton, Indiana	2-35
Table 2.20    PAH Emissions Sampling and Flue Gas Parameters - Underfire Stack
             Bethlehem Steel, Chesterton, Indiana	2-38
Table 2.21    PAH Concentrations and Emission Rates Underfire Stack
             Bethlehem Steel, Chesterton, Indiana	2-40

Table 3.1     Summary of Pushing Process and Control Device Parameters	 3-4
Table 3.2A   Combustion Stack Parameters Test Run No. 1, 8/14/98	3-6
Table 3.2B   Combustion Stack Parameters; Test Run No. 2, 8/14/98	3-7
Table 3.2C   Combustion Stack Parameters: Test Run No. 3,8/15/98	3-8

Table 4.1     Summary of Sampling and Analytical Methods, Bethlehem Steel Corp.,
             Chesterton, Indiana 	4-2
Table 4.2     Summary of Sampling Locations, Test Parameters, Sampling Methods, and
             Number and Duration of Tests, Bethlehem Steel Corp., Chesterton, Indiana .. 4-3
Table 4.3     PAH In-Stack Detection Limits	4-4
Table 4.4     Estimated Metals In-Stack Detection Limits	4-9

Table 5.1     Summary of Sampling Locations, Test Parameters, Sampling Methods,
             and Number and Duration of Tests, Bethlehem Steel Corporation,
             Chesterton, Indiana	5-2

Table 6.1     Summary of Temperature Sensor Calibration Data	6-2
Table 6.2     Summary of Pitot Tube Dimensional Data	6-4
Table 6.3     Summary of Dry Gas Meter and Orifice Calibration Data  	6-6
Table 6.4     Summaryof EPA Method 315 and  CARB Method 429 Field Sampling
             QA/QC Data	6-8
Table 6.5     Summary of EPA Method 315 Analytical QC Data Lab Blank Analysis .... 6-10
Table 6.6     Summary of EPA Method 315 Analytical QC Data Field Blank Analysis ... 6-11
Table 6.7     Summaryof EPA Method 29 Analytical QC Data Lab Control Sample
             (LCS) Recovery and Duplicate Analysis	6-13
Table 6.8     Summary of CARB Method 429 Analytical QC Data Field Blank
             Results	,	6-14
Table 6.9     Summary of CARB Method 429 Analytical QC Data Lab Control
             Sample (LCS)	6-15
Table 6.10    Summary of CARB Method 429 Analytical QC Data Surrogate
             Standard Recoveries	6-17
                                         VI

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                                  LIST OF FIGURES

                                                                                 Page

Figure 1.1     Key Personnel and Responsibility for Testing at Bethlehem Steel Corp.,
              Chesterton, Indiana	1-2

Figure 3.1     Schematic Of Pushing Emission Control For Battery No. 2	 3-2

Figure 4.1     Baghouse Inlet Sample Location, Bethlehem Steel Corp., Chesterton,
              Indiana	4-2
Figure 4.2     Baghouse Inlet Traverse Point Locations, Bethlehem Steel Corp.,
              Chesterton, Indiana	4-3
Figure 4.3     Baghouse Outlet Sample Location, Bethlehem Steel Corp., Chesterton,
              Indiana	4-4
Figure 4.4     Baghouse Outlet Traverse Point Locations, Bethlehem Steel Corp.,
              Chesterton, Indiana  	,	4-5
Figure 4.5     Combustion (Underfire) Sampling Location, Bethlehem Steel Corp.,
              Chesterton, Indiana	4-7
Figure 4.6     Method 1 Calculation Sheet, Combustion Stack, Bethlehem Steel Corp.,
              Chesterton, Indiana	4-8

Figure 5.1     Sampling Train Schematic for EPA Method 315  	5-5
Figure 5.2     Sampling Train Schematic for CARB Method 429	5-7
Figure 5.3     CARB Method 429 Sample Recovery Schematic	5-8
Figure 5.4     CARB Method 429 Analytical Schematic	5-9
                                         VII

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 APPENDIX D




CALCULATIONS

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                    Nomenclature and Dimensions

An   =     Cross-sectional area of sampling nozzle, ft2

As    =     Cross-sectional area of stack, ft2

Bws  =     Proportion by volume of water vapor in the gas stream, dimensionless

Cp   =     Pitot tube coefficient, dimensionless

Cs    =     Concentration of pollutant matter in stack gas-dry basis, grains per dry
            standard cubic foot (gr/dscf)

%CO —     Percent of carbon monoxide by volume, dry basis

%CO2=     Percent of carbon dioxide by volume, dry basis

AH   =     Average pressure drop across the sampling meter flow orifice, inches
            of water (in. H2O)

GCV =     Gross calorific value, Btu/lb

I     =     Percent of isokinetic sampling

La    =     Maximum acceptable leakage rate for either a pretest leak check or for
             a leak check following a component change/ equal to €.020 cubic foot
            per minute or 4% of the average sampling rate, whichever is less

Md   =     Dry molecular weight, Ib/lb-mole

Mn   =     Total amount of pollutant matter collected, milligrams (mg)

Ms   =     Molecular weight of stack gas (wet basis), Ib/lb-mole

%N2  =     Percent of nitrogen by volume, dry basis

%O2  =     Percent of oxygen by volume, dry basis

AP    =     Velocity head of stack gas, inches of water (in. H2O)

Pbar  —     Barometric pressure, inches of mercury (in. Hg)

Ps    =     Absolute stack gas pressure, inches of mercury (in. Hg)

Pstd  =     Gas pressure at standard conditions, inches of mercury (29.92 in. Hg)

-------
pmr  =      Pollutant matter emission rate, pounds per hour (Ib/hr)

Qs    =      Volumetric flow rate - wet basis at stack conditions, actual cubic feet
             per minute (acftn)

Qsstd =      Volumetric flow rate - dry basis at stack conditions, actual cubic feet
             per minute (dscfm)

Tin   =      Average temperature of dry gas meter, °R

Ts    =      Average temperature of stack gas, °R

Tstd  =      Temperature at standard conditions, 528°R

VTc   =      Total volume of liquid collected in impingers, ml

Vsg  =      Volume of moisture collected in silica gel, grams

Vm  =      Volume of dry gas sampled at meter conditions, ft3

Vmstd=      Volume of dry gas sampled at standard conditions, ft3

Vs    =      Average stack gas velocity at stack conditions, ft/s

Vwstd =      Volume of water vapor at standard conditions, scf

y     =      Dry gas meter calibration factor, dimensionless

0     =      Total sampling time, minutes

NOTE: Standard conditions = 68°F and 29.92 in. Hg

-------
          Example Calculations for Pollutant Emissions


1.    Volume of dry gas sampled corrected to standard conditions, ft3.
      Note: Vm must be corrected for leakage if any leakage rates exceed La.
                     Vmstd = 17.647  *  Vm * y * - —
                                                  Tm, °R
2. Volume of water vapor at standard conditions, ft3.


                         Vmstd = 0.04707 * Vic + 0.04715 * Vsg


3. Moisture content in stack gas, dimension less.



                                         Vwstd
                              B\vs =
                                     Vwstd +  Vmstd
4. Dry molecular weight of stack gas, Ib/lb -mole.


                  Md = 0.44 * %CO, + 0.32 * %O2 + 0.28 * (%N2 + %CO)


5. Molecular weight of stack gas, Ib/Ib-mole.


                            Ms = Md (1-Bws) + 18* BWS


6. Stack velocity at stack conditions, f/s.
                     Vs = 85.49 *  Cp * —- /AD  -     ^ °R
                                                  Ps * Ms




7. Stack gas volumetric flow rate at stack conditions, cfm.


                                 Qs = 60 * Vs * As


8. Dry stack gas volumetric flow rate at standard conditions, cfm.
                     Qsstd = 17.647  * Qs *   Ps   * (l-Bws)
                     *              *    Ts,°R

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9.  Concentration in gr/dscf.

                                                 Mn
                                Cs = 0,01543 *
                                                Vmstd



10. Concentration in Ib/dscf.


                                Cs, Ibldscf -
                                              7000


11. Pollutant mass emission rate, Ib/hr.


                             Pmr, Ib/hr = /M&c/* gjrfrf * 60


12. Pollutant mass emission rate, Ib/MMBtu.
                                  m \firo*        ,
                                ,  Ib/MMBtu = *- — -
                                              MMBtu/hr


13. F-factor, Fd.


            10fi*(3.64*%/0 + (1.53*%Q + (0.57*%S) + (0.14*%N) - (0.46*%<92)
                                       GCF {Btullb}




14. F-factor, pollutant mass emission rate, Ib/MMBtu.

                                = lbldscf * F  * 20-9
                                     (20.9 - %<92)




15. Heat imput, MMBtu/hr fuel.

                                 (5ft//ft) * Feed Rate (Ib/hr)
                                          106


16. Heat input, MMBtu/hr, F-factor.
                           * ((20.9 - %<92) + 20.9) * 60
                      Fa

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Summary of Stock Gas Parameters and Test Results
S511.000
Bethlehem Steel -Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Baghouse Inlet
Page 1 of 2


PstaBc
y
Pbar
vm
Dp1*
DH
Tm
T8
vte
CO2
02
N2
CP

As
Q
Dn
Push



An
Vn,(,M)
Vm(sws
Qm
PS
BWS
Bwsjssl)
Vwstd
1-Bv*
Md
M,
VB
A
Qa
Qs
Qs
1
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
Stack Static Pressure, inches H2O
Meter Box Correction Factor
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Square Root Dp, (in. H20}1'2
Avg Meter Orifice Pressure, in. H20
Average Meter Temperature, °F
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pilot Tube Coefficient
Circular Stack? 1=Y,D=N:
Diameter or Dimensions, inches;
Sample Run Duration, minutes
Nozzle Diameter, inches
Tons of Coke pushed
Total Test Time, hours
Tons of Coke per Hour
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, ft3
Standard Meter Volume, m3
Average Sampling Rate, dscfm
Stack Pressure, inches Hg
Moisture, % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), Ib/lb-mole
Molecular Weight (w.b.), Ib/ib-mole
Stack Gas Velocity, ft/s
Stack Area, ft2
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
B-l-315-1
8/11/98
1035-2020

•2.20
1.012
29.70
126.092
0.2980
0.2870
80
153
66.6
0.5
20.05
79.5
0.84
1
114
459
0.215
1,115
9.75
114.4
B-l-315-2
8/12/98
0922-1941

-2.30
1.012
29.80
123.572
0.2964
0.2905
80
158
60.9
0.5
20.0
79.5
0.84
1
114
510
0.215
1,128
10.32
109.3
B-t-315-3
8/13/98
0842-1736

-2.20
1.012
29.80
121.955
0.2926
0.2844
85
170
50.9
0.5
20.0
79.5
0.84
1
114
483
0.215
998
8.90
112.1
Average

-2.23
1.012
29.77
123.873
0.2957
0.2873
82
160
59.5
0.5
20.0
79.5
0.84

114.00
484
0.215
1,080
9.66
111.9
All Calculations are on Time Weighted Average Basis
0.000252
123.890
3.508
0.270
29.54
2.5
27.5
3.135
0.975
28.88
28.61
18.2
70.9
77,509
64.257
1,820
118.1
0.000252
121.824
3.450
0.239
29.63
2.3
31.0
2.867
0.977
28.88
28.63
18.2
70.9
77.263
63,845
1,808
105.2
0.000252
119.125
3.373
0.247
29.64
2.0
41.1
2.396
0.980
28.88
28.67
18.1
70.9
76,952
62,601
1,773
110.8
0.000252
121.613
3.444
0.252
29.60
2.2
33.2
2.799
0.978
28.88
28.64
18.2
70.88
77,242
63,568
1,800
111.4

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Baghouse Inlet
Page 2 of 2





PM
PM @ 7% 0
CPM
PM @ 7% 0
EPM
CPM
CPM
EPM
Push

EOM
EOM @ 7%
CEOM
EOM @ 7%
EEOM
CEOM
CEOM
EEOM
Push
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA
EMISSIONS DATA
Particulate Matter
Total Catch, g
Concentration, gr/dscf @ 7% O2
Concentration, g/dscm
Concentration, g/dscm @ 7% O2
Emission Rate, ug/hr
Concentration, gr/dscf
Concentration, Ib/dscf
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Extractable Organic Matter
Total Catch, g
Concentration, gr/dscf @ 7% 02
Concentration, g/dscm
Concentration, g/dscm @ 7% 02
Emission Rate, pg/hr
Concentration, gr/dscf
Concentration, Ib/dscf
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
B-l-315-1
8/11/98
1035-2020



2.7253
5.5513
0.777
1.27E+01
8.48E+10
0.339
4.85E-05
187.0
1.63

0.0082
0.0167
Z34E-03
3.82E-02
2.55E+08
1.02E-03
1.46E-07
0.563
4.92E-03
B-l-315-2
8/12&8
0922-1941



3.7194
7.2767
1,078
1.67E+01
1.17E+11
0.471
6.73E-05
257.8
2.36

0.0090
0.0176
2.61 E-03
4.03E-02
2.83E+08
1.14E-03
1.63E-07
0.624
5.71 E-03
B-I-315-3
8/13&8
0842-1736



2.7629
5.5279
0.819
1.26E+01
8.71 E+10
0.358
5.11E-05
192.1
1.71

0.0065
0.0130
1.93E-03
2.98E-02
2.05E+08
8.42E-04
1.20E-07
0.452
4.03E-03
Average




3.0692
6.1187
D.891
1.40E+01
9.63E-HO
0.390
5.56E-05
212.3
1.90

0.0079
0.0158
2.29E-03
3.61 E-02
2.48E+08
1.00E-03
1.43E-07
0.546
4.89E-03

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 • EOM/Particulate Matter
Baghouse Inlet
Page 1 of 6




Sb
csb
Cs,, @ 7% 02
ESb
ESb
Push

As
CAS
CSb @ 7% O2
EAS
EA,
Push

Ba
CBa
CBa @ 7% O2
EBa
EBa
Push
RUN NUMBER
RUN DATE
RUN TIME
Antimony
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7%
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Arsenic
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7%
Emission Rate, ug/nr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Bgrium
Target Catch, |jg
Concentration, ug/dscm
Concentration, ug/dscm @ 7%
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
B-l-315-1
8/11/98
1035-2020

4.3
1.23
20.0
133,815
2.94E-04
2.57E-06

62.9
17.9
293
1,957,431
4.31 E-03
3.77E-05

26.6
7.58
124
827,785
1.82E-03
1.59E-05
B-l-315-2
8/12/98
0922-1941

3.7
1.07
16.6
116,345
2.56E-04
2.34E-06

81.8
23.7
366
2,572,166
5.66E-03
5. 18 E-05

34.9
10.12
156
1,09.7,416
2.41 E-03
2.21 E-05
B-t-315-3
8/13/98
0842-1736

3.4
1.01
15.6
107,204
2.36E-04
2.10E-06

92.3
27.4
423
2,910,274
6.40E-03
5.71 E-05

27.6
8.18
126
870,245
1.91 E-03
1.71 E-05
Average



3.8
1.10
17.4
119,121
2.62E-04
2.34E-06

79.00
23.0
361
2,479,957
5.46E-03
4.88E-05

29.70
8.63
136
931,815
2.05E-03
1 .84E-05

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Summary of Stack Gas Parameters and Test Results
S511.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Baghouse Inlet
Page 2 of 6
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA- Continued
Beryllium
Be Target Catch, pg
CBS Concentration, pg/dscm
CBe @ 7% O2 Concentration, pg/dscm @ 7%
EBe Emission Rate, ug/hr
EBB Emission Rate, Ib/hr
Push Pounds per Ton of Coke Pushed
Cadmium
Cd Target Catch, pg
Ccd Concentration, yg/dscm
Gcd @ 7% C>2 Concentration, ug/dscm @ 7%
Ecd Emission Rate, ug/hr
Ecd Emission Rate, Ib/hr
Push Pounds per Ton of Coke Pushed
Chromium
Cr Target Catch, ug
GO Concentration, ug/dscm
CCr @ 7% O2 Concentration, pg/dscm @ 7%
Ecr Emission Rate, ug/hr
Ecr Emission Rate, Ib/hr
Push Pounds per Ton of Coke Pushed
B-l-315-1
08/11/98
1035-2020


1.0
0.274
4.47E+00
29,875
6.57E-05
5.75E-07

1.3
0.371
6.06E+00
40,456
8.90E-05
7.78E-07

6.0
1.71
2.80E+01
186,718
4.11E-04
3.59E-06
B-I-31S-2
08/12/98
0922-1941


1.1
0.310
4.79E+00
33,646
7.40E-05
6.77E-07

2.1
0.609
9.40E+00
66,034
1.45E-04
1.33E-06

9.7
2.81
4.34E+01
305,012
6.71 E-04
6.14E-06
B-l-315-3
08/13/98
0842-1736


1.0
0.302
4.67E+00
32,161
7.08E-05
6.31 E-07

2.6
0.771
1.19E+01
81,980
1.80E-04
1.61E-06

6.8
2.02
3.11E+01
214,408
4.72E-04
4.21 E-06
Average




1.02
0.295
4.65E+00
31,894
7.02E-05
6.28E-07

2.0
0.583
9.12E+00
62,823
1.38E-04
1.24E-06

7.50
2.18
3.42E+01
235,380
5.18E-04
4.65E-06

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulata Matter
Baghouse Inlet
Page 3 of 6





Co
Ceo
Ceo @ 7% O2
ECO
ECO
Push

Cu
Ccu
CCu @ 7% O2
ECU
ECU
Push

Pb
CPb
CPb @ 7% O2
EPb
Epb
Push
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA- Continued
Colbalt
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7%
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Copper
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7%
Emission Rate, ug/hr
Emission Rate, Ibmr
Pounds per Ton of Coke Pushed
Lead
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7%
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
B-l-315-1
08/11/98
1035-2020


3.0
0.855
1.40E+01
93,359
2.05E-04
1 .80E-06

14.0
3.99
6.53E+01
435,676
9.58E-04
8.38E-06

102.3
29.2
4.77E+02
3,183,548
7.00E-03
6.12E-05
B-I-315-2
08/12/98
0922-1941


5.0
1.449
2.24E+01
157,223
3.46E-04
3.16E-06

21.0
6.09
9.40E+01
660,336
1.45E-03
1.33E-05

152.3
44.1
6.82E+02
4,789,009
1.05E-02
9.64E-05
B-i-315-3
08/13/98
0842-1736


3.0
0.889
1.37E+01
94,592
2.08E-04
1.86E-06

20.0
5.93
9.16E+01
630,612
1.39E-03
1.24E-05

127.3
37.7
5.83E+02
4,013,845
8.83E-03
7.87E-05
Average




3.67
1.065
1.67E+01
115,058
2.53E-04
2.27E-06

18.33
5.34
8.36E+01
575,541
1.27E-03
1.13E-05

127.3
37.0
5.81 E+02
3,995,467
8.79E-03
7.88E-05

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel • Chesterton,
US EPA Test Method
Indiana


315 - EOM/Particulate Matter
Baghouse Inlet
Page 4 of 6
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA- Continued
Manganese
Mn Target Catch, ug
CMI Concentration, ug/dscm
CMD @ 7% O2 Concentration, ug/dscm @ 7%
EMH Emission Rate, ug/hr
EMI, Emission Rate, Ib/hr
Push Pounds per Ton of Coke Pushed
|/leroury
Hg Target Catch, ug
^Hg Concentration, ug/dscm
CHS @ 7% O2 Concentration, ug/dscm @ 7%
EHB Emission Rate, ug/hr
Eng Emission Rate, Ib/hr
Push Pounds per Ton of Coke Pushed
Nickel
Ni Target Catch, ug
CNI Concentration, ug/dscm
CNI @ 7% O2 Concentration, ug/dscm @ 7%
ENJ Emission Rate, ug/hr
ENI Emission Rate. Ib/hr
Push Pounds per Ton of Coke Pushed
B-l-315-1
OS/11/98
B-l-315-2
08/12/98
1035-2020 0922-1941


39.0
11.1
1.82E+02
1,213,669
2.67E-03
2.33E-05

0.5
0.14
2.33E+00
15,560
3.42E-05
2.99E-07

87.0
24.8
4.06E+02
2,707,416
5.96E-03
5.21 E-05


43.0
12.5
1.93E+02
1,352,117
2.97E-03
2.72E-05

0.6
0.17
2.69E+00
18,867
4.15E-05
3.80E-07

86.5
25.1
3.87E+02
2,719,956
5.98E-03
5.47E-05
B-l-315-3
08/13/98
0842-1736


41.0
12.2
1.88E+02
1,292,755
2.84E-03
2.54E-05

0.5
0.15
2.29E+00
15,765
3.47E-05
3.09E-07

61.4
18.2
2.81 E+02
1,935,979
4.26E-03
3.80E-05
Average




41.00
11.9
1.87E+02
1,286,180
2.83E-03
2.53E-05

0.53
0.15
2.44E+00
16,731
3.68E-05
3.29E-07

78.30
22.7
3.58E+02
2,454,450
5.40E-03
4.83E-05

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Baghouse Inlet
Page 5 of 6





P
Cp
Cp @ 7% O2
EP
EP
Push

Se
Cse
Ccje @ 7% 02
ESe
Ese
Push

Ag
caa
Cftg @ 7% Oj
EAg
EAg
Push
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA -Continued
Ehosphorys.
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7%
Emission Rate, M9/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Selenium
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7%
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Silver
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7%
Emission Rate, M9/nr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
B-l-315-1
08/11/98
1035-2020


40.0
11.4
1.86E+02
1,244,789
2J4E-03
2.39E-05

14.4
4.10
6.71 E+01
448,124
9.86E-04
8.62E-06

0.3
0.0855
1.40E+00
9,336
2.05E-05
1.80E-07
B-l-315-2
08/12/98
0922-1941


45.0
13.0
2.01 E+02
1,415,006
3.11E-03
2.85E-05

21.1
6.12
9.45E+01
663,481
1.46E-03
1.34E-05

0.6
0.1739
2.69E+00
18,867
4.15E-05
3.80E-07
B-l-315-3
08/13/98
0842-1736


43.0
12.7
1.97E+02
1,355,816
2.98E-03
2.66E-05

19.1
5.66
8.74E+01
602,234
1.32E-03
1.18E-05

0.4
0.1186
1.83E+00
12,612
2.77E-05
2.47E-07
Average




42.67
12.4
1.95E+02
1,338,537
2.94E-03
2.63E-05

18.20
5.29
8.30E+01
571,280
1.26E-03
1.13E-05

0.43
0.1260
1.97E-I-00
13,605
2.99E-05
2.69E-07

-------
Summary of Stack Gas Parameters

S51 1.000
and Test Results



Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter


RUN NUMBER
RUN DATE
RUN TIME
Baghouse Inlet
Page 6 of 6
B-l-315-1
08/11/98
1035-2020


B-l-315-2
08/12/98
0922-1941


B-l-315-3
08/13/98
0842-173S


Average


EMISSIONS DATA- Continued
Thallium
Tl Target Catch, ug
CTI Concentration, ug/dscm
On @ 7% O2 Concentration, ug/dscm
ETI Emission Rate, ug/hr
ETI Emission Rate, Ib/hr
Push Pounds per Ton of Coke
Zinc
Zn Target Catch, ug
Czn Concentration, ug/dscm
Cm @ 7% O2 Concentration, ug/dscm
EZH Emission Rate, ug/hr
Ezn Emission Rate, Ib/hr
Push Pounds per Ton of Coke

3.7
1.05
@7% 1.72E+01
115,143
2.53E-04
Pushed 2.22E-06

167.1
47.6
@7% 7.79E+02
5,200,107
1.14E-02
Pushed 1.00E-04

4.9
1.42
2.19E+01
154,078
3.39E-04
3.10E-06

231.1
67.0
1.03E+03
7,266,841
1.60E-02
1.46E-04

4.6
1.36
2.11E+01
145,041
3.19E-04
2.85E-06

217.1
64.4
9.94E+02
6,845,293
1.51E-02
1.34E-04

4.40
1.28
2.01 E+01
138,087
3.04E-04
2.72E-06

205.10
59.7
9.36E+02
6,437,414
1.42E-02
1.27E-04

-------
Method 315/29 Analytical Results (ug) and Blank Corrections
           Bethlehem Steel - Chesterton, Indiana
                     Baghouse Inlet
Target Cateh, ug/sample
.
Metal
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Colbalt
Copper
Lead
Manganese
Mercury
Nickel
Phosphorus
Selenium
Silver
Thallium
Zinc
B-I-315-1

4,3
62.9
27.4
1.0
3.0
6.0
3.0
14.0
103.0
42.0
0.5
87.0
40.0
14.4
0.3
3.7
178.0
B-I-315-1
Corrected
4.3
62.9
26.6
1.0
1.3
6.0
3.0
14.0
102.3
39.0
0.5
#VALUE!
40.0
14.4
0.3
3.7
167.1
B-I-315-2

3.7
81.8
35.7
l.l
3.8
9.7
5.0
21.0
153.0
46.0
0.6
86.5
45.0
21.1
0.6
4.9
242.0
B-I-315-2
Corrected
3.7
81.8
34.9
1.1
2.1
9.7
5.0
21.0
1513
43,0
0.6
#VALUE!
45.0
21.1
0.6
4.9
231,1
B-I-315-3

3.4
92.3
28.4
1.0
4.3
6,8
3.0
20.0
128,0
44.0
0.5
61.4
43.0
19.1
0,4
4.6
228.0
B-I-315-3
Corrected
3.4
92.3
27.6
1.0
2.6
6.8
3.0
20.0
127.3
41.0
0,5
#VALUE!
43.0
19.1
0,4
4.6
217,1
Filter Blank
0.0
0,0
0.8
0.0
1.7
0.0
0,0
0,0
0.7
3.0
0.0

0.0
0.0
0.0
0.0
10.9

-------
                                    Method 315 Analytical Results (g) and Blank Corrections
                                             Bethlehem Steel - Chesterton, Indiana
                                                       Baghouse Inlet

                                                All Weights are listed in grams
                                                                                                               Corrected Total
               2.5592      0.0008
            0.0022      0.0024       0.0019
 B-l-315-2      3.3744      0.0003       0.3489      0.0012      0.0016       0.0044      0.0036       3.7194
 B-i-315-3     2.6308
0.1360      0.0017       0.0013      0.0006      0.0030      2.7629
Blank Values    0.0017       0.0003      0.0022      0.0001
                          0.00
0.0001      0.0016      0.0039
0.0021

-------
Summary of Stack Gas Parameters and Test Results
Bethlehem Steel-Chesterton, Indiana
CARS Method 429 - PAH's
Baghouse Inlet





i
AH
Ptar
vm
Tra
Pjlrto
T,
vb
COj
°z
N2
S
v2

As
0
Dn




An
Vmbtd)
V.M,
Bw,
Bw,
I

RUN NUMBER
RUN DATE
RUNTIME
MEASURED DATA
Meter Box Correction Factor
Avg. Meter Orifice Pressure, in. H2O
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Meter Temperature, *F
Stack Static Pressure, inches H2O
Average Stack Temperature, "F
Condonsate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pftot Tube Coefficient
Average Square Root Dp, (in, HiO)1/J
Circular Stack? 1=Y,0=N:
Diameter or Dimensions, inches:
Sample Run Duration, minutes
Nozzle Diameter, Inches
Tons of Coke pushed
Total Test Time, hours
Tons of Coke per Hour
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, dscf
Standard Meter Volume, dscm
Moisture, % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft*
Dry Mote Fraction
Molecular Weight (d.b,), Ib/lb-mole
Molecular Weight (w b.), Ib/lb-rnola
Stack Gas Velocity, ft/s
Stack Area, ft2
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
Page 1 of 1
B-M29-1
8/11/33
1030-2016

1.005
0.2642
29.70
88.661
76
-2,20
142
63.3
0.5
20.05
79.45
0.84
0.2716
1
114
453
0.217
1,115
9,77
114.1

0.000257
67.151
2.468
3.3
20.9
2.9BO
0.967
28,88
28.52
16.5
70.9
70,118
58,683
1,662
90.5

B-M29-2
8/12/98
0924-1935

1.005
0.2335
29.80
87.370
79
-2.30
147
64.7
0.5
20.00
79,50
0.84
0,2457
1
114
482
0,215
1,128
10,18
110.8

0.000252
85.686
2.426
3,4
23,7
3.045
0.966
28.8B
28.51
15.D
70,9
63,871
53.111
1.504
94.1

B-M29-3
8/13/99
1332-1934

1.005
0.24S8
29.80
69.18S
80
-2.30
145
59.0
0.5
20.00
79.50
0.84
0.2B68
1
114
362
0.215
660
6.03
109,5

0.000252
67,729
1.918
3,9
22,5
2.777
0,961
23,88
28.45
16.2
70.9
69,027
57,287
1,622
91.8


Average


1.005
0.2505
29.77
81.739
7B
-2.27
145
62,333
0.50
20.02
79.48
0.84
0,2617

114
432
0.216
968
8.66
111.5

0.000254
80.189
2.271
3,6
22.352
2.934
0.964
28,88
28.49
15.9
70.88
67,672
56,361
1,596
92.2

-------
Baghouse Inlet

Naphthalene
Molecular Weight, g/g-mole
Target Catch, ng
ng to fig
Concentration, pg/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
2-Methylnaphthalene
Molecular Weight, g/g-moie
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Acenaphthylene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, ug/hrh
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Acenaphthene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, (Jg/hr b
Emission Rate, Ib/hr *
Pounds per Ton of Coke Pushed
Fluorene
Molecular Weight, g/g-mole
Target Catch, ng
ngto ug
Concentration, u.g/dscrn "
Emission Rate, ng/hr*
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
S-I-429-l

128.16
26,480
26.48
10.7
1,069,819
2.36E-03
2.07E-05

142.20
7,886
7.89
3.20
318,602
7.02E-04
6.I5E-06

154.21
5,500
5.50
2.23
222,206
4.90E-04
4.29E-06

154.21
690.00
0.69
0.280
27,877
6.15E-05
5.39E-07

166.21
2,200
2.20
0.891
88,882
1.96E-04
1.72E-06
B-I-429-2

128.16
34,480
34.48
14.2
1,282,322
2.83E-03
2.55E-05

142,20
6,786
6.79
2.80
252,373
5.56E-04
5.02E-06

154.21
5,900
5.90
2.43
219,423
4.84E-04
4.37E-06

154.21
470.00
0.47
0.194
17,479
3.85E-05
3.48E-07

166.21
1,800
1.80
0.742
66,943
1.48E-04
1.33E-06
B-I-429-3

128.16
28,480
28.48
14.8
1,445,362
3.19E-03
2.91E-05

142.20
2,986
2.99
1.56
151,540
3J4E-04
3.05E-06

154.21
2,600
2.60
1.36
131,950
2.91E-04
2.66E-06

154.21
530.00
0.53
0276
26,898
5.93E-05
5.42E-07

166.21
1,300
1.30
0.678
65,975
1.45E-04
1.33E-06
Average


29,813
29.81
13.3
1,265,834
2.79E-03
2.51E-05


5,886
5.89
2.52
240,838
5.31E-04
4.74E-06


4,667
4,67
2.01
191,193
4.22E-04
3.77E-06


563.33
0.56
0.250
24,085
5.31E-05
4.76E-07


1,767
1.77
0.770
73,933
1.63E-04
1.46E-06

-------

Phenanthrene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ng
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rale, Ib/hr c
Pounds per Ton of Coke Pushed
Anthranccne
Molecular Weight, g/g-roole
Target Catch, ng
ng to ng
Concentration, ug/dscm *
Emission Rate, (ig/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coke Pushed
Fluoranthene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rale, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Pyrene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Benzo (a) anthrancene
Molecular Weight, g/g-mole
Target Catch, ng
ng to fig
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
B-I-429-1

178.22
19,976
20.0
8.09
807,050
1.78E-03
1.56E-05

178.22
730
0.73
0,296
29,493
6.50E-05
5.70E-07

202.26
14,000
14.00
5.67
565,614
1.25E-03
I.09E-05

202.24
2,200
2.20
0.891
88,882
1.96E-04
1.72E-06

228.29
910
0.91
0.3687
36,765
8.11E-05
7.10E-07
B-I-429-2

178.22
24,976
25.0
10.29
928,865
2.05E-03
I.85E-05

178.22
690
0.69
0.284
25,661
5.66E-05
5.11E-07

202.26
18,000
18,00
7.42
669,426
I.48E-03
1.33E-05

202.24
2,500
2.50
1.030
92,976
2.05E-04
1.85E-06

228.29
770
0.77
0.3173
28,637
6.31E-05
5.70E-07
B-I-429-3

178.22
19,976
20.0
10.42
1,013,784
2.24E-03
2.04E-05

178.22
640
0.64
0,334
32,480
7.16E-05
6.54E-07

202.26
6,600
6.60
3.44
334,951
7.38E-04
6.75E-06

202.24
380
0.38
0.198
19,285
4.25E-05
3.88E-07

228.29
130
0.13
0.0678
6,598
1.45E-05
1.33E-07
Average


21,643
21.6
9.60
916,566
2.02E-03
1.82E-05


687
0.69
0.305
29,211
6.44E-05
5.78E-07


12,867
12.87
5.51
523,330
U5E-03
1.03E-05


1,693
1.69
0.707
67,048
1.48E-04
1.32E-06


603
0.60
0.2513
24,000
5.29E-05
4.71E-07

-------

Chrysene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, u.g/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr '
Pounds per Ton of Coke Pushed
Benzo (b) fluoranthene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, u.g/dscm *
Emission Rate, ug/hr
Emission Rate, Ib/hr e
Pounds per Ton of Coke Pushed
Benzo (k) fluoranthene
Molecular Weight, g/g-mole
Target Catch, ng
ng to u.g
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coke Pushed
Benzo (e) pyrene
Molecular Weight, g/g-mole
Target Catch, ng
ng to u.g
Concentration, ug/dscm '
Emission Rate, ug/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coke Pushed
Benzo (a) pyrene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coke Pushed
B-I-429-1

228.28
5,500
5.50
Z23
222,206
4.90E-04
4.29E-06

252.32
7,500
7.50
3.04
303,008
6.68E-04
5.85E-06

252.32
3,000
3.00
1.22
121,203
2.67E-04
2.34E-06

252.30
2,000
2.00
0.810
80,802
1.78E-04
1.56E-06

252.30
620
0.62
0.251
25,049
5.52E-05
4.84E-07
B-I-429-2

228.28
6,000
6.00
2.47
223,142
4.92E-04
4.44E-06

252.32
8,200
8.20
3.38
304,961
6.72E-04
6.07E-06

252.32
3,100
3.10
1.28
115,290
2.54E-04
2.29E-06

252.30
1,900
1.90
0.783
70,662
1.56E-04
1.41E-06

252.30
430
0.43
0.177
15,992
3.53E-05
3.18E-07
B-I-429-3

228.28
1,900
1.90
0.99
96,425
2.I3E-04
1.94E-06

252.32
2,900
2.90
1.51
147,175
3.24E-04
2.96E-06

252.32
830
0.83
0.433
42,123
9.29E-05
8.48E-07

252.30
390
0.39
0.203
19,793
4.36E-05
3.99E-07

252.30
130
0.13
0.068
6,598
1.45E-05
1.33E-07
Average


4,467
4.47
!.90
180,591
3.98E-04
3.56E-06


6,200
6.20
2.64
251,714
5.55E-04
4.96E-06


2,310
2.31
0.975
92,872
2.05E-04
I.83E-06


1,430
1.43
0.599
57,085
1.26E-04
1.12E-06


393
0.39
0.165
15,879
3.50E-05
3.12E-07

-------
                                          B-l-429-1
B-I-429-2
                                                                          B-I-429-3
Average
Perylcne
     Molecular Weight, g/g-mole               202,24          202.24          202.24
     Target Catch, ng                         100.00            ND            ND             33,33
     ngtoug                                   0.10            0.00            0,00              0,03
     Concentration, ug/dscm °                  0.0405            0,00            0.00            0.0135
     Emission Rate, ug/hrb                    4,040             0.00            0.00            1346.7
     Emission Rate, Ib/hrc                   8.91E-06       O.OOE+00       O.OOE+00          2.97E-06
     Pounds per Ton of Coke Pushed          7.80E-08       O.OOE+00       O.OOE+00          2.60E-08
Indeno (1,2,3-cd) pyrene
     Molecular Weight, g/g-mole               290,34          290.34          290.34
     Target Catch, ng                         2,700           2,700             450            1,950
     ngtoug                                   2.70            2.70            0.45              1.95
     Concentration, ug/dscm *                    1.09            1.11           0.235             0,814
     Emission Rate, ug/hr b                  109,083         100,414          22,838           77,445
     Emission Rate, Ib/hre                   2.40E-04        2.21E-04       5.03E-05          1.71E-04
     Pounds per Ton of Coke Pushed          2.11E-06        2.00E-06       4.60E-07          1.52E-06
Dibenz (a,h) anthracene
     Molecular Weight, g/g-mole               278.33          278.33          278.33
     Target Catch, ng                         1,100           1,100             240               813
     ngtong                                   1.10            !.10           0,240             0.813
     Concentration, ug/dscm *                   0.446           0,453           0.125             0,341
     Emission Rate, ug/hr b                   44,441          40,909          12,180           32,510
     Emission Rate, Ib/hr'                   9.80E-05        9.02E-05       2.69E-05          7.17E-05
     Pounds per Ton of Coke Pushed          8.58E-07        8.14E-07       2.45E-07          6.39E-Q7
Benzo (g,h,i) perylene
     Molecular Weight, g/g-mole               276,34          276.34          276.34
     Target Catch, ng                         2,200           2,200             320            1,573
     ngtofig                                   2.20            2,20            0.32              1.57
     Concentration, ug/dscm"                   0.891           0.907           0.167             0.655
     Emission Rate, ug/hrb                   88,882          81,819          16,240           62,314;
     Emission Rate, Ib/hrc                   1.96E-04        1.80E-04       3.58E-05          1.37E-04
     Pounds per Ton of Coke Pushed          1.72E-06        1.63E-06       3.27E-07          1.22E-06
  a Milligrams per dry standard cubic meter at 68° F (20° C) and 1 aim.
    Micrograms per hour.
    Pounds per hour.
 D  Not Detectable - Results are below target anaiyte detection iimil. Values are counted as zero (0) in averages.
{ }   Estimate - Anaiyte results are below the quantitation limit and above the detection limit.

-------
   quantdata
Baghouse Inlet
Trunc'd CMPD
Naphlhal cmpdl
2-Methyl Cmpd2
Acenaph cmpdS
Acenaph cmpd4
Fluorene cmpdS
Phenant cmpd6
Anlhranc cmpd?
Fluorant cmpdS
Pyrene CmpdS
Benzo (a cmpdIO
Chiysen cmpdl 1
Benzo(b cmpdl 2
Benzo(k cmpdl 3
Benzo (e cmpdl 4
Benzo (a cmpdl 5
Paytene cmpd 16
Indeno ( cmp1 7
Dibenz( cmpdl 8
Benza(g cmpd19
Quanterra Compound Name Mol. Wt Method Blank
Naphthalene 1 128.16 520
Z-Melhylnaphthalene 2 142.2 14
Aeenaphthylene 3 154.21 0
Acenaphthene 4 154.21 0
Fluorene 5 166.21 0
Phenanthrene 6 178.22 24
Anthrancene 7 178.22 0
Fluoranihene 8 202.26 0
Pyrene 9 202.24 0
Benzo (a) anthrancene 10 228.29 0
Chrysens 11 228.28 0
Benzo (b) fluoranthene 12 252.32 0
Benzo (k) fluoranthene 13 252.32 0
Benzo (e) pyrene 14 252.3 0
Benzo (a) pyrene 15 252.3 0
Perylene 16 202.24 0
lndano(1,2,3-cd) pyrene 17 290.34 0
Dibenz (a.h) anthracene 18 278.33 0
Benzo (g.h.i) perylene 19 276,34 0
B-l-429-1 Blank Adjusted
27,000 26,480
7,900 7,886
5,500 5,500
690 690
2,200 2,200
20,000 19,976
730 730
14,000 14,000
2,200 2,200
910 910
5,500 5,500
7,500 7,500
3,000 3,000
2,000 2,000
620 620
100 100
2,700 2,700
1,100 1,100
2,200 2,200
B-l-429-2 Blank Adjusted
35,000 34,480
6,800 6,786
5,900 5,900
470 470
1,800 1,800
25,000 24,976
690 690
18,000 18,000
2,500 2,500
770 770
6,000 6,000
8,200 8,200
3,100 3,100
1,900 1,900
430 430
ND ND
2,700 2.700
1,100 1,100
2,200 2,200
B-i-429-3 Blank Adjusted
29,000 28,480
3,000 2.986
2,600 2,600
530 530
1,300 1,300
20,000 19,976
640 640
6,600 6,600
380 380
130 130
1,900 t,900
2,900 2,900
830 830
390 390
130 130
ND ND
450 450
240 240
320 320

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Baghouse Outlet
Page 1 of 2



Pstate
y
Pfaar
vm
Dp"2
DH
Tm
T,
V,e
C02
02
N2
CP

As
Q
Dn
Push



An
Vm(st!f]
Vmjstd)
Q,
PS
Bws
BWs(sat)
V^
1-BWS
Md
Ms
va
A
Qa
Qs
Q,
I
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
Stack Static Pressure, inches r^O
Meter Box Correction Factor
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Square Root Dp, (in, H20)1;2
Avg Meter Orifice Pressure, in. H2O
Average Meter Temperature, "F
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pitot Tube Coefficient
Circular Stack? 1 =Y,0=N:
Diameter or Dimensions, inches:
Sample Run Duration, minutes
Nozzle Diameter, inches
Tons of Coke Pushed
Total Test Time, hours
Tons of Coke per Hour
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, ft3
Standard Meter Volume, m3
Average Sampling Rate, dscfm
Stack Pressure, inches Hg
Moisture, % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), lb/lb*mole
Molecular Weight (w.b.), Ibflb-mole
Stack Gas Velocity, ft/s
Stack Area, ft2
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
B'0-315-1
8/11/98
1037-195S

-0.43
0.979
29.70
132.109
0.4220
0.5003
77
134
69.8
0.45
20.50
79.1
0.84
1
108
368
0.220
1,115
9.35
119.3
B-0-315-2
8/12/98
0929-1935

-0.43
0.979
29.80
188.898
0.4106
0.5859
77
135
87.0
0.5
20.0
79.5
0.84
1
108
480
0.235
1,128
10.10
111.7
B-O-315-3
8/13/98
0840-1749

-0.50
0.979
29.80
190,238
0.4171
0.6154
80
135
83.1
0,5
20.0
79.5
0.84
1
108
481
0.235
1,047
9.15
114.4
Average


-0.45
0.979
29.77
170.415
0.4166
0.57
78
135
80.0
0.5
20.2
79.4
0.84

108.00
443
0.230
1,097
9.53
115.1
All Calculations are on Time Weighted Average Basis
0.000264
126.338
3.577
0.343
29.67
2.5
16.9
3.285
0.975
28.89
28.62
25.3
63.6
96,755
83,087
2,353
99.6
0.000301
181.292
5.134
0.378
29.77
2.2
17.3
4.095
0.978
28.88
28.64
24.6
63.6
94.024
81,147
2,298
98.3
0.000301
181.577
5.142
0.377
29.76
2.1
17.3
3.912
0.979
28.88
28.65
25.0
63.6
95,502
82,493
2,336
96.7
0.000289
163.069
4.618
0.366
29.73
2.3
17.2
3.764
0.977
28.83
28.64
25.0
63.62
95,427
82,242
2,329
98.2

-------
Summary of Stack Gas Parameters and Test Results
5511.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Baghouse Outlet
Page 2 of 2





PM
PM @ 7% O
CPU
PM @ 7% O
EPM
CPM
CPM
EPM
Push

EOM
EOM @ 7%
CEOM
EOM @ 7%
EEOM
CEOM
CEOM
EEOM
Push
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA
EMISSIONS DATA
Participate Hatter
Total Catch, g
Concentration, gr/dscf @ 7% 02
Concentration, g/dscm
Concentration, g/dscm @ 7% O2
Emission Rate, pg/hr
Concentration, gr/dscf
Concentration, Ib/dscf
Emission Rale, Ib/hr
Pounds per Ton of Coke Pushed
Extractable Organic Matter
Total Catch, g
Concentration, gr/dscf @ 7% O2
Concentration, g/dscm
Concentration, g/dscm @ 7% O2
Emission Rate, pg/hr
Concentration, gr/dscf
Concentration, Ib/dscf
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
B-O-31S-1
8/11/98
1037-1958



0.0047
0.0200
1.31E-03
4.57E-02
1.85E+08
5.74E-04
8.20E-08
0.409
3.43E-03

0,0042
0.0178
1.17E-03
4.08E-02
1.66E+D8
5.13E-04
7.33E-08
0.365
3.06E-03
B-O-315-2
8/12M8
0929-1935



0.0044
0.0058
8.57E-D4
1.32E-02
1.18E+08
3.75E-04
5.35E-08
0.261
2.33E-03

0.0046
0.0060
8.96E-04
1.38E-02
1.24E+08
3.92E-04
5.59E-08
0.272
2.44E-03
B-Q-315'3
8/13/98
0840-1749



0.0053
0,0070
1.03E-03
1.59E-02
1.44E+08
4.50E-04
6.43E-08
0.319
2.78E-03

0.0052
0.0068
1.01E-03
1.56E-02
1.42E+08
4.42E-04
6.31 E-08
0.312
2.73E-03
Average




0.0048
0.0109
1.07E-03
2.49E-02
1.49E+08
4.66E-04
6.66E-08
0.329
2.85E-03

0.0047
0.0102
1.03E-03
2.34E-02
1.44E+08
4.49E-04
6.41 E-08
0.317
2.74E-03

-------
Summary of Stack Gas Parameters and Test Results
S511.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Baghouse Outlet
Page 1 of 6
RUN NUMBER
RUN DATE
RUN TIME



Sb






Sb






Ba




Sb
CSb
@ 7% O
ESb
ESb
Push

As
CAs
@ 7% O
EAs
EAs
Push

Ba
CBa
@7%0
EBa
EBa
Push
Antimony

B-0-315-1
8/11/98
1037-1958

Target Catch, |jg
Concentration,
Concentration,
Emission Rate
Emission Rate
ug/dscm
ug/dscm @ 7% 02
ug/hr
Ib/hr
Pounds per Ton of Coke Pushed
Arsenic

0


0
0

Target Catch, ug
Concenfration,
Concentration,
Emission Rate,
Emission Rate,
ug/dscm
ug/dscm @ 7% O2
ug/hr
Ib/hr
Pounds per Ton of Coke Pushed
Barium


0.0
.OOE+00
0,0000
0.000
.OOE+00
.OOE+00

0.0
O.OOE+00


0.000
0.000
O.OOE+00
O.OOE+00

Target Catch, ug
Concentration,
Concentration,
Emission Rate,
Emission Rate,
pg/dscm
pg/dscm @ 7% 02
ug/hr
Ib/hr
Pounds per Ton of Coke Pushed
1

0.4
.12E-01
3.89E+00

15,784
3.47E-05
2.91 E-07
B-O-315-2
8/12/98
0929-1935


0


0
0



0.0
.OOE+00
0.0000
0.000
.OOE+00
.OOE+00

0.0
O.OOE+00


0.000
0.000
O.OOE+00
O.OOE+00


1

0.7
.36E-01
2.11E+00

18,799
4.14E-05
3.70E-07
B-0-315-3
8/13/98
0840-1749


0


0
0



0.0
.OOE+00
0.0000
0.000
.OOE+00
.OOE+00

0.0
O.OOE+00


0.000
0.000
O.OOE+00
O.OOE+00



0.0
O.OOE+00
O.OOE+00

0
0
OOE+00
O.OOE+00
Average


0

0.0
.OOE+00
0.0000

0
0.000
.OOE+00
O.OOE+00


0


0
0


8
2

0.00
.OOE+00
0.000
0.000
.OOE+00
.OOE+00

0.37
.27E-02
.OOE+00
11,528
2
2
.54E-05
.21 E-07

-------
Summary of Stack Gas Parameters and Test Results
S511.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Partlculate Matter
Baghouse Outlet
Page 2 of 6





Be
CBe
Be @ 7% O
EBe
EBe
Push

Cd
CCd
Cd @ 7% O
ECd
ECd
Push

Cr
CCr
CCr @ 7% O
ECr
ECr
Push
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA - Continued
Beryllium
Target Catch, (jg
Concentration, pg/dscm
Concentration, ug/dscm @ 7% O2
Emission Rate, jjg/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Cadmjum
Target Catch, \ig
Concentration, pg/dscm
Concentration, ug/dscm @ 7% 02
Emission Rate, pg/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Chromium
Target Catch, (jg
Concentration, jjg/dscm
Concentration, (jgftjscm @ 7% O2
Emission Rate, jjg/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
B-O-315-1
08/11/98
1037-1958


0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.1
2.80E-02
9.71E-01
3,946
8.68E-06
7.28E-08

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
B-O-315-2
08/12/98
0929-1935


0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
B-O-315-3
08/13/98
0840-1749


0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
Average




0.00
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.0
9.32E-03
3.24E-01
1,315
2.89E-06
2.43E-08

0.00
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Bag ho use Outlet
Page 3 of 6
RUN NUMBER
RUN DATE
RUN TIME
B-O-315-1
08/11/98
1037-1958
B-0-315-2
08/12/98
0929-1935
B-O-315-3
08/13/98
0840-1749
Average
EMISSIONS DATA - Continued
Colbalt


Co






Cu






Pb



Co
CCo
@ 7% O
ECo
ECo
Push

Cu
Ccu
@ 7% O
ECu
ECU
Push

Pb
CPb
© 7% 0
EPb
EPb
Push
Target Catch, ug
Concentration,
Concentration,
Emission Rate,
Emission Rate,
ug/dscm
ug/dscm @ 7% 02
pg/hr
Ib/hr
Pounds per Ton of Coke Pushed
Copper

0
0

0
0.0
.OOE+00
.OOE+00
0
.OOE+00
O.OOE+00

Target Catch, ug
Concentration,
Concentration,
Emission Rate,
Emission Rate,
ug/dscm
ug/dscm @ 7% 02
ug/hr
Ib/hr
Pounds per Ton of Coke Pushed
Lead

0
0


0.0
.OOE+00
.OOE+00
0
O.OOE+00
O.OOE+00

Target Catch, ug
Concentration,
Concentration,
Emission Rate,
Emission Rate,
ug/dscm
ug/dscm @ 7% 02
ug/hr
ib/hr
Pounds per Ton of Coke Pushed

0.0
O.OOE+00
O.OOE+00

0
0
OOE+00
O.OOE+00
0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

2.0
3.90E-01
6.02E+00
53,713
1.18E-04
1.06E-06

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0
0

0.0
.OOE+00
.OOE+00
0
O.OOE+00
O.OOE+00


0
0


0.0
.OOE+00
.OOE+00
0
O.OOE+00
O.OOE+00



0,0
O.OOE+00
0

.OOE+00
0
O.OOE+00
O.OOE+00
0.00
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.67
1.30E-01
2.01 E+00
17,904
3.94E-05
3.53E-07

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steei - Chesterton, Indiana
US EPA Test Method 315 - EOM/Partlculate Matter
Baghouse Outlet
Page 4 of 6



Mn







Mn
CMn
@ 7% O
EMn
EMn
Push

Hg
CHg
Hg @ 7% O






CNi



EHg
EHg
Push

Ni
CNi
@ 7% 02
ENi
ENi
Push
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA- Continued
Manganese
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7% O2
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Mercury
Target Catch, |jg
Concentration, ug/dscm
Concentration, ug/dscm @ 7% 02
Emission Rate, pg/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Nickel
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7% O2
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
B-O-315-1 B-O-315-2
08/11/98 08/12/98
1037-1958 0929-1935
0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
4.0
7.79E-01
1.20E+01
107,425
2.36E-04
2.12E-06

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.9
1.75E-01
2.71 E+00
24,171
5.32E-05
4.76E-07
B-0-315-3
08/13/98
0840-1749

0
0

0
0.0
.OOE+00
.OOE+00
0
.OOE+00
O.OOE+00



0.0
O.OOE+00
0

0
0


0
.OOE+00
0
.OOE+00
.OOE+00

0.0
.OOE+00
O.OOE+00

0
0
0
.OOE+00
.OOE+00
Average

1.33
2.60E-01
4.01 E+00
35,808
7
7


.88E-05
.05E-07

0.00
O.OOE+00
O.OOE+00

0
O.OOE+00
O.OOE+00


5
9

1
1

0.30
.84E-02
.03E-01
8,057
J7E-05
.59E-07

-------
Summary of Stack Gas Parameters and Test Results
S511.000
Bethlehem Steel - Chesterton, Indiana
U S EPA Test Metho d 31 5 - EOM/Partlculate Matter
Baghouse Outlet
Page 5 of 6

RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA - Continued
Phosphorus
P Target Catch, ug
CP Concentration, ug/dscm
CP @ 7% O2 Concentration, ug/dscm @ 7% O2
EP Emission Rate, ug/hr
EP Emission Rate, Ib/hr
Push Pounds per Ton of Coke Pushed
Sejenjurn
Se Target Catch, ug
CSe Concentration, ug/dscm
Se @ 7% O Concentration, ug/dscm @ 7% 02
ESe Emission Rate, ug/hr
ESe Emission Rate, Ib/hr
Push Pounds per Ton of Coke Pushed
Silver
Ag Target Catch, ug
Cag Concentration, ug/dscm
Ag @ 7% O Concentration, ug/dscm @ 7% 02
EAg
EAg
Push
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
8-0-3*5-1
08/11/98
1037-1958
0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
B-O-315-2
08/12M8
0929-1935
0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
0.5
9.74E-02
1.50E+DO
13,428
2.95E-05
2.65E-07
2.1
4.09E-01
6.32E+00
56,398
1.24E-04
1.11E-06
B-O-315-3
08/13/98
0840-1749
0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
0.0
O.OOE+00
O.OOE+00
0
O.OOE+OD
O.OOE+00
0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
Average
0.00
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
0.17
3.25E-02
5.01E-01
4,476
9.85E-06
8.82E-08
0.70
1.36E-01
2.11E+00
18,799
4.14E-05
3.70E-07

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Partlculate Matter
Baghouse Outlet
Page 6 of 6





Tl
CTI
CTI @ 7% O2
ETI
ETI
Push
Zn
CZn
Zn @ 7% O
EZn
EZn
Push
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA- Continued
Thallium
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7% O2
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
Target Catch, ug
Concentration, ug/dscm
Concentration, pg/dscm @ 7% O2
Emission Rate, ng/hr
Emission Rate, Ib/hr
Pounds per Ton of Coke Pushed
B-O-315-1
08/11/98
1037-1958


0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
B-O-315-2
08/12/98
0929-1935


0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
0.8
156E-01
2.41 E+00
21,485
4.73E-05
4.23E-07
B-O-375-3
08/13/98
0840-1749


0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
Average




0.00
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
0.27
5.19E-02
8.02E-01
7,162
1.58E-05
1.41E-07

-------
Method 315 Analytical Results (ug) and Blank Corrections
         Bethlehem Steel - Chesterton, Indiana
                   Baghouse Outlet
Target Catch, ug/sample

Metal
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Colbalt
Copper
Lead
Manganese
Mercury
Nickel
Phosphorus
Selenium
Silver
Thallium
Zinc
B-O-315-i

0.0
0.0
1.2
0.0
1.8
0.0
0.0
0.0
0.5
3.0
0.0
0.0
0.0
0.0
0.0
0.0
8.3
B-O-315-1
Corrected
0.0
0.0
0.4
0.0
0.1
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0,0
0.0
0.0
B-O-31S-2

0.0
0.0
1.5
0.0
1.4
0.0
0.0
2.0
0.5
7.0
0.0
0.9
0.0
0.5
2.1
0.0
11.7
B-O-315-2
Corrected
0.0
0.0
0.7
0.0
0.0
0.0
0.0
2.0
0.0
4.0
0.0
0.9
0.0
0.5
2.1
0.0
0.8
B-O-315-3

0.0
0.0
0.8
0.0
1.7
0.0
0.0
0.0
0.5
3.0
0.0
0.0
0.0
0.0
0.0
0.0
7.8
B-O-315-3
Corrected
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Filter Blank
0.0
0.0
0.8
0.0
1.7
0.0
0.0
0.0
0.7
3.0
0.0
0.0
0.0
0.0
0.0
0.0
10.9

-------
                                    Method 315 Analytical Results (g) and Blank Corrections
                                            Bethlehem Steel - Chesterton, Indiana
                                                     Baghouse Outlet

                                               All Weights are listed in grams
  Run No.
      Filters
                                                                    Corrected Total
                PM
            MCEM
PM
MCEM
MCEM
MCEM
MCEM
PM
MCEM
 B-O-315-1
0,0011       0.0003       0.0061       0,0019      0.0006       0.0000      0.0026      0.0047        0.0042
 B-O-315-2    0.0028      0,0006      0.0041       0.0009      0,0013       0.0002       0.0028      0.0044
 B-O-315-3     0.0004       0.000
                        0.0074      0.0026      0.0008       0.0026      0.0004      0.0053
Blank Values    0,0011      0.0002      0.0014      0.0009
                                                0.0000       0.0000       0.0001      0.0025
                                                                        0.0012

-------
Summary of Stack Gas Parameters and Test Results
Bethlehem Steel-Chesterton, Indiana
CARS Method 429 - PAH's
Baghouse Outlet





T
AH
Pfcar
vm
Tm
Pflallc
T.
vte
CO*
°z
N2
Cp
Ap"1

As
e
Dn




An
VnfcW)
Vm^d)
B«
Bvn(..t»
V«,j
1-Bw,
Md
M.
v.
A
Q.
Q.
Q,(cnw)
1

RUW NUMBER
RUN DATE
RUN TIME
MEASURED DATA
Meter Box Correction Factor
Avg. Meter Orifice Pressure, in. H2O
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Meter Temperature, 'F
Stack Static Pressure, inches H2O
Average Stack Temperature, *F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pilot Tube Coefficient
Average Square Root Dp, (in. H2O)ia
Circular Stack? 1=Y,0=N:
Diameter or Dimensions, inches:
Sample Run Duration, minutes
Nozzle Diameter, inches
Tons of Coke pushed
Total Test Time, hours
Tons of Coke per Hour
CALCULATED DATA
Nozzle Area, ft1
Standard Meter Volume, dscf
Standard Meter Volume, dscm
Moisture, % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft5
Dry Mole Fraction
Molecular Weight (d.b.), Ib/tb-mole
Molecular Weight (w.b.), Ib/lb-mote
Stack Gas Velocity, ft/s
Stack Area, ft*
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinotic Sampling Ratio, %
Page 1 of 1
B-O-429-1
8/11/98
103T-1958

1,002
0.5292
29,70
150.008
79
-0.65
132
93,8
0.45
20.50
79.05
0.84
0.4351
1
108
367
0.220
1,115
9.35
119.3

0.000264
146.291
4.142
2.9
16.1
4.415
0.971
28.89
28.57
26.1
63.6
99,693
85,504
2,421
112.4

B-O-429-2
emras
0928-1934

1.002
0.6925
29.80
200.695
80
-0.49
137
118.0
0.5
20.00
79.50
0.84
0.4607
1
108
478
0.235
1,128
10.10
111.7

0.000301
196.291
5.556
2.6
18.2
5.554
0.972
28.88
28.58
27.7
63.6
105,790
90,478
2,562
95.9

B-O-429-3
Bm/98
OB40-174B

1.002
0.6581
29,80
201.093
83
-0.50
136
95.8
0.5
20.00
79.50
0.84
0.4357
1
108
480
0.235
1,047
9.13
114.7

0.000301
195.382
5.533
2.3
17.8
4.509
0.977
28.88
28.63
26.2
63.6
99,873
85,994
2,435
100.0


Average


1.002
0.6266
29.77
183.999
81
-0.55
135
102.533
0.48
20.17
79.35
0.84
0.4438

108
442
0.230
1,097
9.53
115.2

O.D00289
179.321
5.078
2.6
17.363
4.826
0.974
28.88
28.60
26.7
63.62
101 ,785
87.325
2,473
102.7

-------
Bag house Outlet

Naphthalene
Molecular Weight, g/g-raole
Target Catch, ng
ng to ug
Concentration, ng/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
2-MethyInaphthaIene
Molecular Weight, g/g-mole
Target Catch, ng
ngtojig
Concentration, ug/dscm *
Emission Rate, u.g/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coke Pushed
Acenaphthylene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ]ig
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Acenaphthene
Molecular Weight, g/g-mole
Target Catch, ng
ng to n_g
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Fluorene
Molecular Weight, g/g-mole
Target Catch, ng
ng to jig
Concentration, ug/dscm "
Emission Rate, ng/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
B-Q-419-l

128.16
7280,00
7,28
1.76
255,300
5.63E-04
4.72E-06

142.20
1586.00
1.59
0.383
55,619
1.23E-04
1.03E-06

154,21
300.00
0.300
0.0724
10520.61
2.32E-05
1.94E-07

154.21
140.00
0.140
0,0338
4,910
1.08E-05
9.08E-08

166.21
300.00
0.30
0.0724
10520.61
2.32E-05
1.94E-07
B-Q-429-2

128.16
8780.00
8.78
1,58
242,822
5.35E-04
4.79E-06

142.20
2486.00
2.49
0.447
68,754
1.52E-04
IJ6E-06

154,21
280.00
0.280
0.0504
7743.76
1.71E-05
1.53E-07

154.21
120.00
0.120
0.0216
3,319
7.32E-06
6.55E-08

166.21
270,00
0.27
0.0486
7467,20
1.65E-05
1.47E-07
B-Q-429J

128.16
9180.00
9.18
1.66
242,426
5.34E-04
4.66E-06

142.20
1686.00
1.69
0.305
44,524
9.82E-05
8.56E-07

154.21
340.00
0.340
0.0615
8978.73
1.98E-05
1.73E-07

154.21
97.00
0.097
0.0175
2,562
5.65E-06
4.92E-08

166.21
200.00
0.20
0.0361
5281.61
1.16E-05
1.02E-07
Average


8413.33
8.41
1.67
246,849
5.44E-04
4.721-06


1919.33
1.92
0.378
56,299
1.24E-04
1.08E-06


306.67
0.307
0.0614
9081.03
2.00E-05
1.73E-07


119.00
0.119
0,0243
3,597
7.93E-06
6.85E-08


256.67
0.26
0.0524
7756.47
1.71E-05
1.4SE-07

-------

Phenanthrene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, u.g/dscm *
Emission Rate, u.g/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Anthrancene
Molecular Weight, g/g-mole
Target Catch, ng
ng to |ig
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr '
Pounds per Ton of Coke Pushed
Fluoranthene
Molecular Weight, g/g-mole
Target Catch, ng
ng to u.g
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Pyrene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ng/dscm *
Emission Rate, ng/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Benzo (a) anthrancene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr °
Pounds per Ton of Coke Pushed
B-O-429-1

178.22
1,176.00
1.18
0.284
41240.79
9.09E-05
7.62E-07

178.22
84,00
0.08
0,02028
2,946
6.49E-06
5.45E-08

202.26
480.00
0.48
0.1159
16,833
3.71E-05
3.11E-07

202,24
280.00
0.28
0.0676
9819.24
2.16E-05
1.82E-07

228.29
55.00
0.06
0.01328
1,929
4.25E-06
3.57E-08
B-Q-429-2

178.22
946.00
0.95
0.170
26162.84
5.77E-05
5.16E-07

178,22
38.00
0.04
0.00684
1,051
2.32E-06
2.07E-08

202,26
240.00
0.24
0.0432
6,638
1.46E-05
1.31E-07

202.24
180.00
0.18
0.0324
4978.13
1.10E-05
9.83E-08

228.29
43.00
0.04
0.00774
1,189
2.62E-06
2.35E-08
B-O-429-3

178.22
606.00
0.61
0.110
16003.27
3.53E-05
3.08E-07

178.22
20.00
0,02
0.00361
528
1.16E-06
L02E-08

202.26
150.00
0.15
0.0271
3,961
8.73E-06
7.62E-08

202.24
96.00
0.10
0.0174
2535.17
5.59E-06
4.87E-08

228.29
23.00
0,02
0.00416
607
1.34E-06
1.17E-08
Average


909.33
0.91
0.188
27802,30
6.13E-05
5.29E-07


47.33
0,05
0.01024
1,508
3.33E-06
2.85E-08


290,00
0.29
0.0621
9,144
2.02E-05
1.73E-07


185.33
0.19
0.0391
5777.51
1.27E-05
1.10E-07


40.33
0.04
0.00839
1,242
2.74E-06
2.36E-08

-------

Chrysene
Molecular Weight, g/g-mole
Target Catch, ng
ng to pg
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coke Pushed
Benzo (b) fluoranthene
Molecular Weight, g/g-mole
Target Catch, ng
ngtoug
Concentration, ug/dscm *
Emission Rate, jig/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Benzo (k) flnoranthene
Molecular Weight, g/g-mole
Target Catch, ng
ngto ug
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Benzo (e) pyrene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coke Pushed
Benzo (a) pyrene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
B-O-429-1

228.28
110,00
0.1 1
0,0266
3,858
8.50E-06
7.13E-08

252.32
73.00
0,07
0.01762
2,560
5.64E-06
4.73E-08

252,32
68.00
0.07
0.01642
2,385
5.26E-06
4.41E-08

252.30
48,00
0.05
0.01159
1,683
3.71E-06
3.11E-08

252.30
48.00
0.05
0.01159
1,683
3.71E-06
3.11E-08
B-O-429-2

228.28
140.00
0.14
0.0252
3,872
8.54E-06
7.64E-08

252.32
63.00
0.06
0,01133
1,742
3.84E-06
3.44E-08

252.32
32.00
0.03
0.00576
885
1.95E-06
1.75E-08

252.30
33.00
0.03
0.00594
913
2.01E-06
1.80E-08

252.30
27.00
0,03
0.00486
747
1.65E-06
1.47E-08
B-Q-429-3

228.28
63.00
0.06
0.0114
1,664
3.67E-06
3.20E-08

252.32
38.00
0.04
0.00687
1,004
2.21E-06
1.93E-08

252.32
25.00
0.03
0.00452
660
1.46E-06
1.27E-08

252.30
24.00
0.02
0.00434
634
1.40E-06
1.22E-08

252.30
20,00
0.02
0.00361
528
1.16E-06
1.02E-08
Average


104.33
0.10
0.0210
3,131
6.90E-06
5.99E-08


58.00
0.06
0.01194
1,769
3.90E-06
3.37E-08


41.67
0.04
0.00890
1,310
2.89E-Q6
2.47E-08


35,00
0.04
0.00729
1,077
2.37E-06
2.04E-08


31.67
0,03
0.00669
986
2.17E-06
L87E-08

-------

Perylene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ng
Concentration, ug/dscm *
Emission Rate, ng/hrb
Emission Rate, Ib/hr *
Pounds per Ton of Coke Pushed
Indeno (1,2,3-cd) pyrene
Molecular Weight, g/g-raole
Target Catch, ng
ng to |jg
Concentration, (ig/dscm "
Emission Rate, ng/hrh
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
Dibenz (a,h) anthracene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm *
Emission Rate, jig/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coke Pushed
Benzo (g,h,i) perylene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coke Pushed
B Milligrams per dry standard cubic meter at 68°
Micrograms per hour.
e Pounds per hour,
B-O-429-1

202.24
11.00
0.01
0.00266
386
8.50E-07
7.13E-09

290.34
63.00
0.06
0.01521
2,209
4.87E-06
4.08E-08

278.33
14,00
0.01
0.00338
491.0
1.08E-06
9.08E-09

276.34
140.00
0.14
0.03380
4,910
l.OSE-05
9.08E-08
F {20° C) and 1


B-O-J29-2

202.24
13.00
0.01
0.00234
360
7.93E-07
7.10E-09

290.34
30.00
0.03
0.00540
830
1.83E-06
I.64E-08

278.33
ND
0.00
0.00000
0.00
O.OOE+00
O.OOE+00

276.34
45.00
0.05
0.00810
1,245
2.74E-06
2.46E-08
aim.


B=D-429-3

202.24
ND
0.00
0.00000
0.00
O.OOE+00
O.OOE+00

290.34
25.00
0.03
0.00452
660
1.46E-06
1.27E-08

278.33
ND
0.00
0.00000
0.00
O.OOE+00
O.OOE+00

276.34
64.00
0.06
0.01157
1,690
3.73E-06
3.25E-08



Average


8.00
0.01
0.00166
248
5.48E-07
4.74E-09


39.33
0.04
0.00837
1,233
2.72E-06
2.33E-08


4.67
0.00
0.00113
163.65
3.61E-07
3.03E-09


83.00
0.08
0.01782
2,615
5.76E-06
4.93E-08



ND Not Delectable - Results are below target analyte detection limit. Values are counted as zero (0) in averages.
) Estimate - Analyte results are below the quantitation limit and
above the detection limit

-------
    quantdata
Baghouse Outlet
Trunc'd Name CMPD
Naphthalene cmpdl
2-Methylnaphthalene cmpd2
Acenaphthylene cmpd3
Acenaphthene Ctnpd4
Fluorene cmpdS
Phenanthrene cmpdS
Anthrancene cmpd?
Fluoranthene cmpd8
Pyrene cmpd 9
Benzo (a) anthrancene Cmpd 1 0
Chrysene cmpdl 1
Benzo (b) fluoranthene cmpd12
Benzo (k) fluoranthene cmpdl 3
Benzo (e) pyrene cmpd14
Benzo (a) pyrene cmpdl 5
Perylene Cmpd16
Indeno (1 ,2,3-cd) pyren cmpl 7
Oibenz (a,h) anthracen Cmpd18
Benzo (g,ti ,i) perylene cmpdl 9
Quanterra Compound Name Mol. Wt. Method Blank
Naphthalene 1 128.16 520
2-Methylnaphthalene 2 142.2 14
Acenaphthylene 3 154.21 0
Acenaphthene 4 154.21 0
Fluorene 5 166.21 0
Phenanthrene 6 178.22 24
Anthrancene 7 178.22 0
Fluoranthene 8 202.26 0
Pyrene 9 202.24 0
Benzo (a) anthrancene 10 228.29 0
Chrysene 11 228.28 0
Benzo (b) fluoranthene 12 252.32 0
Benzo (k) fluoranthene 13 252.32 0
Benzo (e) pyrene 14 252.3 0
Benzo (a) pyrene 15 252.3 0
Perylene 16 202.24 0
Indeno (1 ,2,3-cd) pyrene 17 290.34 0
Dibenz (a.h) anthracene 18 278.33 0
Benzo 
-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 • EOM/Particulate Matter
Underfire Stack
Page 1 of 2



PdaBc
y
Pbar
vm
Dp1*
DH
Tm
Ts
vte
CO2
02
N2
CP

As
Q
Dn
Charge



An
Vm(5td)
Vmjstd)
Qm
Ps
Bws
Bws(5at]
Vwsw
1-BWS
Md
Ms
vs
A
Qa
Qs
Qs
I
RUN NUMBER
RUN DATE
RUN TIME
0
MEASURED DATA
Stack Static Pressure, inches H2O
Meter Box Correction Factor
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Square Root Dp, (in. HzO)t/2
Avg Meter Orifice Pressure, in. H20
Average Meier Temperature, °F
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pilot Tube Coefficient
Circular Stack? 1=Y,0=N:
Diameter or Dimensions, inches:
Sample Run Duration, minutes
Nozzle Diameter, inches
Tons of Coal Charged
Total Test Time, hours
Tons of Coal per Hour
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, ft3
Standard Meter Volume, m3
Average Sampling Rate, dscfrn
Stack Pressure, inches Hg
Moisture, % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), Ib/lb-mole
Molecular Weight (w.b.), lb/!b-mole
Stack Gas Velocity, ft/s
Stack Area, ft2
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
B-U-315-1
B/14/98
0921-1325


-0.80
0.981
29.80
99.017
0.2067
0.8592
95
444
402.8
4,40
11.30
84,3
0.84
1
177
180
0.442
647
4.07
159.0

0,001065
92.198
2.611
0,512
29.74
17.1
2829.7
18.960
0.829
29.16
27.25
15.7
170.9
160,715
77,362
2,191
106.2
B-U-315-2
8/14/98
1 441-1 B09


-0.81
0.981
29,80
81.886
0.1728
0.5650
103
451
334.2
5,5
9.55
85.0
0.84
1
177
180
0.435
491
3.47
141.5

0.001032
75.109
2.127
0.417
29.74
17.3
3041.3
15,731
0.827
29.26
27.31
13.1
170.9
134,733
64,153
1,817
107.7
B-U-315-3
8/15/98
0838-1203


-0,87
0.981
29.65
135.910
0.2276
1.6520
95
438
534.2
5.0
10.45
84.6
0.84
1
177
185
0.498
550
3.42
160.8

0.001353
126.161
3.572
0.682
29.59
16.6
2671.5
25.145
0.834
29.22
27.35
17.2
170.9
176,514
85,538
2,422
100.7
Average


-0.83
0.9S1
29.75
105,604
0.2024
1.03
93
444
423.7
5.0
10.4
84.6
0.84

177.00
182
0.458
563
3.65
153.8

0.001150
97,823
2.770
0.537
29.69
17.0
2847.5
19.945
0.830
29,21
27.31
15.3
170.87
157,321
75,684
2,143
. 104.9

-------
Summary of Stack Gas Parameters and Test Results
S511.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Underfire Stack
Page 2 of 2
RUN NUMBER
RUN DATE
RUN TIME
B-U-315-1
8/14/98
0921-1325
B-U-315-2
8/14/98
1441-1809
B-U-315-3
8/15/98
0838-1203
Average
EMISSIONS DATA
EMISSIONS DATA
Participate Matter

PM

PM





PM
@7%0
CPM
@7%0
EPM
CPM
CPH
EPM
Push
Total Catch, g
Concentration,
Concentration,
Concentration,
Emission Rate
Concentration,
Concentration,
Emission Rate

gr/dscf @ 7% O2
g/dscm
g/dscm @ 7% O2
pg/hr
gr/dscf
Ib/dscf
Ib/hr
Pounds per Ton of Coal Charged
0.2036
0.0493
0.0780
113E-01
1.03E+10
3.41 E-02
4.87E-06
22.6
1.42E-01
0.2176
0.0548
0.1023
1.25E-01
1.12E+10
4.47E-02
6.39E-06
24.6
1.74E-01



1
0.3258
0.0530
0.0912
.21E-01
1.33E+10
3.99E-02
5.69E-06

1
29.2
.82E-01
0.2490
0.0524
0.0905
1.20E-01
1.16E+10
3.95E-02
5.65E-06
25.5
1.66E-01
Extractable Organic Matter

EOM
EOM @ 7%

CEOM
EOM @ 7%





EEOM
CEOM
CEOM
EEOM
Push
Total Catch, g
Concentration,
Concentration,
Concentration,
Emission Rate,
Concentration,
Concentration,
Emission Rate,

gr/dscf @ 7% 02
g/dscm
g/dscm @ 7% O2
jjg/rir
gr/dscf
Ib/dscf
Ib/hr
Pounds per Ton of Coal Charged
0.0408
0.0099
0.0156
2.26E-02
2.05E+09
6.83E-03
9.76E-07
4.53
2.85E-02
0.0323
0.0081
0.0152
1.86E-02
1.66E+09
6.64E-03
9.48E-07
3.65
2.58E-02



5
0.1379
0.0224
0.0386
.13E-02
5.61 E+09
1
.69E-02
2.41 E-06

7
12.37
.69E-02
0.0703
0.0135
0.0231
3.09E-02
3.11E+09
1.01 E-02
1.44E-06
6.85
4.37E-02

-------
               Summary of Stack Gas Parameters and Test Results
                                   S511.000
                      Bethlehem Steel - Chesterton, Indiana
                US EPA Test Method 315 - EOM/Particulate Matter
                                Underfire Stack
                                  Page 1 of 6
         RUN NUMBER
         RUN DATE
         RUN TIME
B-U-315-1
 8/14/98
0921-1325
B-U-315-2
 8/14/98
1441-1809
                                                              B-U-315-3
                                                               8/15/98
                                                              0838-1203
Average
         Antimony
 Sb      Target Catch, pg
 Csb      Concentration, ug/dscm
@ 7% O2 Concentration, pg/dscm @ 7% 02
 Esb      Emission Rate, (jg/hr
 E$b      Emission Rate, Ib/hr
Push     Pounds per Ton of Coal Charged
 As
 CAS
          Arsenic
          Target Catch, us
          Concentration, ug/dscm
, @ 7% O2 Concentration, (jg/dscm @ 7% O2
  EA$      Emission Rate, ug/hr
  EAS      Emission Rate, Ib/hr
 Push     Pounds per Ton of Coal Charged

          Barium,
  Ba      Target Catch, ug
  Csa      Concentration, ug/dscm
, @ 7% O2 Concentration, ug/dscm @ 7% O2
  EBB      Emission Rate, ug/hr
  EBB      Emission Rate, Ib/hr
 Push     Pounds per Ton of Coal Charged
      0.0
 O.OOE+00
   0.0000
     0.000
 O.OOE+00
 O.OOE+00
      0.0
 O.OOE+00
   0.0000
     0.000
 O.OOE+00
 O.OOE+00
      4.8        4.0
  2.19E-03   2.20E-03
  3.17E-03   2.70E-03
  630,905    435,987
  6.34E-07   5.28E-07
                                                                    0.0     0.0
                                                               O.OOE+00  O.OOE+00
                                                                 0.0000    0.0000
                                                                   0.000   0.000
                                                               O.OOE+00  O.OOE+00
                                                               O.OOE+00  O.OOE+00
                 5.8     4.87
             2.39E-03  2.26E-03
             3.19E-03  3.02E-03
             842,910   636,601
             7.66E-07  6.42E-07
                                        3.99E-09    3.73E-09    4.76E-09  4.16E-09
                                             0.4         1.8         0.5     0.90
                                        1.83E-04    9.91E-04    2.06E-04   4.60E-04
                                        2.64E-04    1.21E-03    2.75E-04   5.84E-04
                                          52,575     196,194      72,665   107,145
                                        5.28E-08    2.38E-07    6.60E-08   1.19E-07
                                        3.32E-10    1.68E-09    4.10E-10   8.07E-10

-------
                  Summary of Stack Gas Parameters and Test Results
                                    S511.000
                        Bethlehem Steel - Chesterton, Indiana
                   US EPA Test Method 315 - EOM/Particulate Matter
                                 Underflre Stack
                                   Page 2 of 6
         RUN NUMBER
         RUN DATE
         RUN TIME
                                          B-U-315-1   B-U-315-2  B-U-315-3
                                           08/14/98   08/14/98    08/15/98
                                          0921-1325   1441-1809  0838-1203
                                 Average
 Be
         EMISSIONS DATA - Continued
         Beryllium
 Be      Target Catch, pg
 Cfle     Concentration, ug/dscm
@ 7% O2 Concentration, ug/dscm @ 7% 02
 EBS     Emission Rate, ug/hr
 EBB     Emission Rate, Ib/hr
Push     Pounds per Ton of Coal Charged
     Cd
         CjjdnjiutQ
         Target Catch, |jg
   d     Concentration, ug/dscm
   7% O2 Concentration, ug/dscm @ 7% 02
         Emission Rate, ug/hr
         Emission Rate, Ib/hr
Push     Pounds per Ton of Coal Charged
 Cr
 CCr
            Chromium
            Target Catch, ug
            Concentration, ug/dscm
CCr @ 7% O2 Concentration, ug/dscm @ 7% 02
    Ecr     Emission Rate, ug/hr
    Ecr     Emission Rate, Ib/hr
   Push    Pounds per Ton of Coal Charged
     0.0        0.0         0,0     0.00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
       0          0          00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
     0.2        0.0        0.0     0.1
 9.13E-05   O.OOE+00  O.OOE+00  3.04E-05
 1.32E-04   O.OOE+00  O.OOE+00  4.41 E-05
  26,288          0          0    8,763
 2.64E-08   O.OOE+00  O.OOE+00  8.80E-09
 1.66E-10   O.OOE+00  O.OOE+00  5.54E-11
     0.0        0.0        0.0     0.00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
       0          0          00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Underfire Stack
Page 3 of 6





Co
Ceo
CCo @ 7% O2
ECO
ECO
Push

Cu
Ccu
Ccu @ 7% O2
ECU
ECU
Push

Pb
CPb
CPb @ 7% O2
EPb
EPb
Push
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA- Continued
Colbalt
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7% O2
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coal Charged
popper
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7% O2
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coal Charged
Lead
Target Catch, ug
Concentration, ug/dscm
Concentration, ug/dscm @ 7% O2
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coal Charged
B-U-315-1
08/14/98
0921-1325


0.0
O.OOE+00
0,OOE+00
0
O.OOE+00
O.OOE+00

0.0
O.OOE+00
O.OOE+00
0
O.OOE+OO
O.OOE+00

3.4
1.55E-03
2.25E-03
446,891
4.49E-07
2.82E-09
B-U-315-2
08/14/98
1441-1809


0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

3.0
1.65E-03
2.02E-03
326,990
3.96E-07
2.80E-09

2.9
1.60E-03
1.96E-03
316,091
3.83E-07
2.71 E-09
B-U-315-3
08/15/98
0838-1203


0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

2.0
8.26E-04
1.10E-03
290,659
2.64E-07
1.64E-09

2.0
8.26E-04
1.10E-03
290,659
2.64E-07
1.64E-09
Average




0.00
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

1.67
8.26E-04
1.04E-03
205,883
2.20E-07
1.48E-09

2.8
1.32E-03
1.77E-03
351,213
3.65E-07
2.39E-09

-------
                     Summary of Stack Gas Parameters and Test Results
                                       S511.000
                           Bethlehem Steel - Chesterton, Indiana
                      US EPA Test Method 315 • EOM/Partieulate Matter
                                    Underfire Stack
                                      Page 4 of 6
            RUN NUMBER
            RUN DATE
            RUN TIME
                                      B-U-315-1
                                      08/14/98
                                      0921-1325
          B-U-315-2
          08/14/98
          1441-1809
B-U-315-3
 08/15/98
0838-1203
Average
Mn
            EMISSIONS DATA - Continued

            Manganese
            Target Catch, ug
      MD     Concentration, ug/dscm
      7% °z Concentration, pg/dscm @ 7% O2
      wn     Emission Rate, ug/hr
            Emission Rate, Ib/hr
    Push    Pounds per Ton of Coal Charged

            Mercury
     Hg     Target Catch, ug
    CHS     Concentration, ug/dscm
CHg @ 7% O2 Concentration, ug/dscm @ 7% O2
    Eng     Emission Rate, ug/hr
    EHQ     Emission Rate, Ib/hr
    Push    Pounds per Ton of Coal Charged

            Nickel
     Nl     Target Catch, ug
    CNI     Concentration, ug/dscm
CN1 @ 7% O2 Concentration, ug/dscm @ 7% O2
    ENI     Emission Rate, ug/hr
    ENJ     Emission Rate, Ib/hr
    Push    Pounds per Ton of Coal Charged
     0.0        0.0        0.0     0.00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
O.OOE+00   O.OOE-i-00   O.OOE+00  O.OOE+00
       0          0          00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
                                            0.0         0.0        0.0    0.00
                                       O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
                                       O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
                                             0           0          00
                                       O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
                                       O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
                                            0.0         0.0         0.0     0.00
                                       O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
                                       O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
                                             0          0           00
                                       O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
                                       O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00

-------
                  Summary of Stack Gas Parameters and Test Results
                                    S511.000
                        Bethlehem Steel - Chesterton, Indiana
                   US EPA Test Method 315 - EOM/Partlculate Matter
                                 Underfire Stack
                                   Page 5 of 6
         RUN NUMBER
         RUN DATE
         RUN TIME
B-U-315-1
 08/14/98
0921-1325
B-U-315-2
 08/14/98
1441-1809
B-U-315-3
 08/13/98
0838-1203
Average
         EMISSIONS DATA - Continued
         Phosphorus
  P      Target Catch, pg
  Cp     Concentration, ug/dscm
@ 7% O2 Concentration, ug/dscm @ 7% 02
  Ep     Emission Rate, ug/hr
  Ep     Emission Rate, Ib/hr
Push    Pounds per Ton of Coal Charged

         Selenium
  Se     Target Catch, ug
 CSe     Concentration, ug/dscm
@ 7% O2 Concentration, ug/dscm @ 7% 02
 Ese     Emission Rate, ug/hr
 ESB     Emission Rate, Ib/hr
Push    Pounds per Ton of Coal Charged

         Silver
 Ag     Target Calch, ug
 Cag     Concentration, ug/dscm
@ 7% O2 Concentration, M9/dscm @ 7% 02
 l=Ag     Emission Rate, ug/hr
 EAQ     Emission Rate, ib/hr
Push    Pounds per Ton of Coal Charged
      0.0         0.0         0.0     0.00
 O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
 O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
        0          0          00
 O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
 O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
      2.3        2.0         1.0     1.77
  1.05E-03   1.10E-03   4.13E-04  8.55E-04
  1.52E-03   1.35E-03   5.49E-04  1.14E-03
  302,309    217,994    145,329   221,877
  3.04E-07   2.64E-07   1.32E-07  2.33E-07
  1.91E-09   1.87E-09   8.21E-10  1.53E-09
      0.0        0,0         0.0     0.00
 O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
 O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
        0          0          00
 O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00
 O.OOE+00   O.OOE+00   O.OOE+00  O.OOE+00

-------
Summary of Stack Gas Parameters and Test Results
S51 1.000
Bethlehem Steel - Chesterton, Indiana
US EPA Test Method 315 - EOM/Particulate Matter
Underfire Stack
Page 6 of 6





TI
CT.
C-n@7%C
En
En
Push

Zn
C2n
Czn @ 7% C
Ezn
Ezn
Push
RUN NUMBER
RUN DATE
RUN TIME
EMISSIONS DATA- Continued
Thallium
Target Catch, ug
Concentration, ug/dscm
'2 Concentration, ug/dscm @ 7% O2
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coal Charged
Zinc
Target Catch, ug
Concentration, ug/dscm
'2 Concentration, ug/dscm @ 7% 02
Emission Rate, ug/hr
Emission Rate, Ib/hr
Pounds per Ton of Coal Charged
B-U-315-1
08/14/98
0921-1325


0.9
4.11E-04
5.95E-04
118,295
1.19E-07
7.47E-10

1.8
8.22E-04
1.19E-03
236,589
2.38E-07
1.49E-09
B-U-315-2
08/14/98
1441-1809


0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00

0.9
4.95E-04
6.07E-04
98,097
1.19E-07
8.40E-10
B-U-315-3
08/15/98
0838-1203


1.0
4.13E-04
5.49E-04
145,329
1.32E-07
8.21 E-10

0.0
O.OOE+00
O.OOE+00
0
O.OOE+00
O.OOE+00
Average




0.63
2.75E-04
3.81 E-04
87,875
8.36E-08
5.23E-10

0.90
4.39E-04
5.99E-04
111,562
1.19E-07
7.78E-10

-------
Method 315 Analytical Results (ng) and Blank Corrections
         Bethlehem Steel - Chesterton, Indiana
                   Underfire Stack
Target Catch, ug/sample

Metal
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Colbalt
Copper
Lead
Manganese
Mercury
Nickel
Phosphorus
Selenium
Silver
Thallium
Zinc
B-U-315-1

0.0
4,8
1.2
0.0
1.9
0.0
0.0
0.0
4.1
3.0
0.0
0.0
0.0
2.3
0.0
0.9
12.7
B-U-315-1
Corrected
0.0
4.8
0.4
0.0
0.2
0.0
0.0
0.0
3.4
0.0
0.0
0,0
0.0
2,3
0.0
0.9
1.8
B-U-315-2

0.0
4.0
2,6
0.0
1.6
0.0
0.0
3.0
3.6
3.0
0.0
0.0
0.0
2.0
0.0
0.0
11.8
B-U-315-2
Corrected
0.0
4.0
1.8
0.0
0.0
0.0
0.0
3.0
2.9
0.0
0.0
0.0
0.0
2.0
0.0
0.0
0.9
B-U-315-3

0.0
5.8
1.3
0.0
1.1
0.0
0.0
2.0
2.7
1.0
0.0
0.0
0.0
1.0
0.0
1.0
10.1
B-U-315-3
Corrected
0.0
5.8
0.5
0.0
0.0
0.0
0.0
2.0
2.0
0.0
0.0
0.0
0.0
1.0
0.0
1.0
0.0
Filter Blank
0.0
0.0
0.8
0.0
1.7
0.0
0.0
0.0
0.7
3.0
0.0
0.0
0.0
0.0
0.0
0.0
10.9

-------
                                    Method 315 Analytical Results (g) and Blank Corrections
                                            Bethlehem Steel - Chesterton, Indiana
                                                       Underfire Stack

                                               All Weights are listed in grams
  Run No.
Filters
                                                                                              Corrected Total
 B-U-315-1
                                                                                           0.0408
0.0792      0.0003       0.1324       0,0404      0.0001       0.0000       0.0003     0.2036
 B-U-315-3     0.0722       0.000       0.2616       0.1373      0.0005      0.0001       0.0003     0.3258
Blank Values    0.0058      0.0000       0.0022       0.0003      0.0000      0.0000       0.0000     0.0080
                                                                                           0.0003

-------
Summary of Stack Gas Parameters and Test Results
Bethlehem Steel-Chesterton, Indiana
CARB Method 429 - PAH's
Underfire Stack





r
AH
Pb,
vm
Tm
PilaUc
T,
vto
CO2
oz
N2
cp
Ap"2

As
0
Dn
Charge



An
Vmwfl
VBtrt«
B«
&«(,«)
v««
1-Bw,
M,
Ms
V.
A
Q,
Q,
Q^cnm)
1

RUN NUMBER
RUN DATE
RUNTIME
MEASURED DATA
Meter Box Correction Factor
Avg. Meter Orifice Pressure, in. HjO
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Meter Temperature, "F
Slack Static Pressure, inches H2O
Average Stack Temperature, 'F
Condensata Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pilot Tube Coefficient
Average Square Root Dp, (in. HjO)"3
Circular Stack? 1=Y,0=N:
Diameter or Dimensions, inches:
Sample Run Duration, minutes
Nozzle Diameter, inches
Tons of Coal Charged
Total Test Time, hours
Tons of Coal per Hour
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, dscf
Standard Meter Volume, dscm
Moisture, % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft*
Dry Mole Fraction
Molecular Weight (d.b.), Ib/lb-mole
Molecular Weight (w.b.), Ibflb-mole
Slack Gas Velocity, ft/s
Slack Area, ft2
Slack Gas Volumetric flow, acfm
Slack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
IsoMnetic Sampling Ratio, %
Page 1 of 1
B-U-429-1
B/14/98
0921-1326

1,004
0.86
29.80
96.703
115
-0.83
453
395.2
4.4
11.30
84.30
0.84
0.2224
1
177
180
0.442
647
4.07
159.0

0.001066
88.949
2.519
17.3
3104.1
18.649
0.827
29.15
27,22
17.0
170.9
173,886
82,595
2,339
96.0

B-U -429-2
8/14/98
1442-1809

1,004
1.125
29,80
107.900
109
•0.83
448
568.5
5.5
9.55
84.95
0.84
0.2572
1
177
180
0.434
491
3.45
142.3

0.001027
100.360
2.842
21.1
2949.4
26.759
0.789
29.26
26.89
19.7
170.9
201,774
92,035
2,606
100.8

B-U -429-3
B/15/98
0838-1208

1.004
1,25
29.65
119.731
115
-0.85
440
382.8
5.0
10.45
84.55
0.84
0.2220
1
177
180
0.475
550
3.50
157.1

0.001231
109.683
3.106
14.1
2728.1
18.018
0.859
29.22
27.64
16.7
170.9
171,473
85,412
2,419
99.1


Average


1.004
1.08
29.75
108.111
113
-0.84
447
449.167
4.97
10.43
84.60
0.84
0,2339

177
180
0.450
563
3.67
152.8

0.001108
99.664
2.822
17.5
2927.198
21.142
0.825
29.21
27.25
17.8
170.87
182.379
86,681
2,455
98.6

-------
Underfire Stack

Naphthalene
Molecular Weight, g/g-mole
Target Catch, ng
ng to fig
Concentration, ug/dsctn *
Emission Rate, ug/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coal Charged
2-Methylnaphthalene
Molecular Weight, g/g-mole
Target Catch, ng
ngtoug
Concentration, ug/dscm a
Emission Rate, ug/hr b
Emission Rate, Ib/hr *
Pounds per Ton of Coal Charged
Acenaphtliylene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ^g
Concentration, |ig/dscm *
Emission Rate, fig/hr
Emission Rate, Ib/hr *
Pounds per Ton of Coal Charged
Acenaphthene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ng
Concentration, ug/dscm *
Emission Rate, ng/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coal Charged
Fluorene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coal Charged
B-U-429-4

128,16
10,480
10.48
4,16
583,882
1.29E-03
8.10E-06

142.20
5,786
5.79
2.30
322,361
7.11E-04
4.47E-06

154.21
950
0.95
0.377
52,928
1.17E-04
7.34E-07

154.21
190.00
0.19
0.0754
10,586
2.33E-05
1.47E-07

166.21
810
0.81
0.3216
45,128
9.95E-05
6.26E-07
B-U-429-2

128.16
30,480
30.48
10.73
1,677,094
3.70E-03
2.60E-05

142.20
1,986
1.99
0.699
109,275
2.41E-04
1.69E-06

154.21
290
0.29
0.102
15,957
3.52E-05
2.47E-07

154.21
110.00
0.11
0.0387
6,053
1.33E-05
9.38E-08

166.21
230
0.23
0.0809
12,655
2.79E-05
I.96E-07
B-U-429-3

128.16
179,480
179.48
57.79
8,385,796
1.85E-02
1.18E-04

142.20
8,186
8.19
2,64
382,472
8.43E-04
5.37E-06

154.21
2,600
2.60
0.837
121,479
2.68E-04
1.70E-06

154.21
450.00
0.45
0.1449
21,025
4.64E-05
2.95E-07

166.21
1,300
1.30
0.4186
60,740
1.34E-04
8.52E-07
Avejage


73,480
73.48
24.22
3,548,924
7.82E-03
5.06E-05


5,319
5.32
1.88
271,369
5.98E-04
3.84E-06


1,280
1.28
0.439
63,455
1.40E-04
8.9SE-07


250.00
0.25
0.0863
12,554
2.77E-05
1.79E-07


780
0.78
0.2737
39,508
8.71E-05
5.58E-07

-------

Phenanthrene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coal Charged
Anthrancene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coal Charged
Fluoranthene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coal Charged
Pyrem
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coal Charged
Benzo (a) anthrancene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, ug/dscm "
Emission Rate, ug/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coal Charged
B-U-42JJ-1

178.22
1,576
1.58
0,626
87,805
I.94E-04
I.22E-06

178.22
51.00
0.05
0,02025
2,841
6.26E-06
3.94E-08

202.26
430.00
0.43
0,1707
23,957
5.28E-05
3.32E-07

202.24
170,00
0.17
0.0675
9,471
2.09E-05
I.31E-07

228.29
45.00
0.05
0.01787
2,507
5.53E-06
3.48E-08
B-U-429-2

178.22
706
0.71
0,248
38,846
8.56E-05
6.02E-07

178.22
20.00
0.02
0.00704
1,100
2.43E-06
1.70E-08

202.26
220.00
0.22
0.0774
12,105
2.67E-OS
1.88E-07

202.24
80.00
0.08
0.0282
4,402
9.70E-06
6.82E-08

228.29
25.00
0.03
0.00880
1,376
3.03E-06
2.13E-08
B-U-429-3

178.22
1,676
1.68
0.540
78,307
1.73E-04
1.IOE-06

178.22
86.00
0.09
0.02769
4,018
8.86E-06
5.64E-08

202.26
620.00
0.62
0.1996
28,968
6.39E-05
4.06E-07

202.24
220.00
0.22
0.0708
10,279
2.27E-05
1.44E-07

228.29
72.00
0.07
0.02318
3,364
7.42E-06
4.72E-08
Average


1,319
1.32
0.471
68,320
1.51E-04
9.73E-07


52.33
0.05
0.01833
2,653
5.85E-06
3.76E-08


423.33
0,42
0.1493
21,677
4.78E-05
3.09E-07


156.67
0.16
0.0555
8,051
1.77E-05
1.I5E-07


47,33
0.05
0.01661
2,416
5.33E-06
3.44E-08

-------

Chrysene
Molecular Weight, g/g-mole
Target Catch, ng
ngtoug
Concentration, pg/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coal Charged
Benzo (b) flu or a nth ene
Molecular Weight, g/g-mole
Target Catch, ng
ngtoug
Concentration, pg/dscm a
Emission Rate, ug/hr b
Emission Rate, Ib/hr e
Pounds per Ton of Coal Charged
Benzo (k) fluoranthene
Molecular Weight, g/g-mole
Target Catch, ng
ngtoug
Concentration, ug/dscm "
Emission Rate, ng/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coal Charged
Benzo (e) pyrene
Molecular Weight, g/g-mole
Target Catch, ng
ng to ug
Concentration, (ig/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coal Charged
Benzo (a) pyrene
Molecular Weight, g/g-mo!e
Target Catch, ng
ng to ug
Concentration, ug/dscm *
Emission Rate, ug/hr b
Emission Rate, Ib/hr c
Pounds per Ton of Coal Charged
B-U.429-1

228.28
120.00
0.12
0.0476
6,686
1.47E-05
9.27E-08

252.32
76,00
0.08
0.0302
4,234
9.33E-06
5.87E-08

252.32
50.00
0.05
0.0199
2,786
6.14E-06
3.86E-08

252.30
42.00
0.04
0.0167
2,340
5.16E-06
3.25E-08

252.30
47.00
0.05
0.0187
2,619
5.77E-06
3.63E-08
B-U-429-2

228.28
59.00
0.06
0.0208
3,246
7.16E-06
5.03E-08

252.32
45.00
0.05
0.0158
2,476
5.46E-06
3.S4R08

252.32
31.00
0.03
0.0109
1,706
3.76E-06
2.64E-G8

252.30
32.00
0.03
0.0113
1,761
3.88E-06
2.73E-08

252,30
24.00
0.02
0.0084
1,321
2.91E-06
2.05E-08
B-U-42-9-3

228,28
160.00
0.16
0.0515
7,476
I.65E-05
1.05E-07

252.32
64.00
0.06
0.0206
2,990
6.59E-06
4.20E-08

252.32
39.00
0.04
0.0126
1,822
4.02E-06
2.56E-08

252.30
34.00
0.03
0.0109
1,589
3.50E-06
2.23E-08

252.30
32.00
0.03
0.0103
1,495
3.30E-06
2.10E-08
Averaee


113.00
0,11
0.0400
5,803
1.28E-05
8.26E-08


61.67
0.06
0.0222
3,234
7.13E-06
4.63E-08


40.00
0,04
0.0144
2,105
4.64E-06
3.02E-08


36.00
0.04
0.0130
1,896
4.18E-06
2.73E-08


34.33
0.03
0.0125
1,811
3.99E-06
2.59E-08

-------
                                                         MJ-429-2
B-U-429-3
                                                                                        ,Aygrage
Perylene
     Molecular Weight g/g-mole               202.24          202,24           202.24
     Target Catch, ng                          12.00            ND             ND             4.00
     ngtou.g                                  0.01            0.00             0.00             0.00
     Concentration, ug/dscm"                   0,00            0.00             0.00             0.00
     Emission Rate, ng/hrb                      669            0.00             0.00              223
     Emission Rate, Ib/hr"                   1.47E-06       O.OOE+00        O.OOE+00         4.91E-0?
     Pounds per Ton of Coal Charged         9.27E-09       O.OOE+00        O.OOE+00         3.Q9E-09
Indeno (1,2,3-cd) pyrene
     Molecular Weight, g/g-mole               290.34          290.34           290.34
     Target Catch, ng                          44.00           32.00            35.00            37.00
     ngtoug                                  0.04            0.03             0.04             0.04
     Concentration, ug/dscm'                 0.0175          0.0113           0.0113           0.0133
     Emission Rate, ug/hrb                    2,451           1,761            1,635             1,949
     Emission Rate, Ib/hrc                   5.40E-06       3.88E-06        3.61E-06         4.30E-06
     Pounds per Ton of Coal Charged         3.40E-08       2.73E-08        2.29E-08         2.81E-08
Dibenz (a,h) anthracene
     Molecular Weight, g/g-mole               278.33          278.33          278,33
     Target Catch, ng                          12.00            ND             ND             4.00
     ngtop.g                                   0.01            0,00             0.00              0.00
     Concentration, ug/dscm"                 0.00476        0.00000         0.00000          0.00159
     Emission Rate, ug/hrh                      669              0               0             223
     Emission Rate, Ib/hre                   1.47E-06       O.OOE+00        O.OOE+00         4.91E-07
     Pounds per Ton of Coal Charged         9.27E-09       O.OOE+00        O.OOE+00          3.09E-09
Benzo (g,h,i) perylene
     Molecular Weight, g/g-mole               276.34          276.34          276.34
     Target Catch, ng                          81.00           78.00           63.00             74.00
     ngtou.g                                   0.08            0.08             0.06              0.07
     Concentration, ug/dscm *                  0.0322         0.0274          0.0203           0.0266
     Emission Rate, ug/hrb                    4,513           4,292            2,944             3,916
     Emission Rate, Ib/hrc                   9.95E-06       9.46E-06        6.49E-06          8.63E-06
     Pounds per Ton of Coal Charged         626E-08       6.65E-08        4.I3E-08          5.68E-08
  " Milligrams per dry standard cubic meter at 68° F (20° C) and 1 atm.
    Micrograrns per hour.
  c Pounds per hour.
ND Not Detectable - Results are below target anaryte detection limit. Values are counted as zero (0) in averages,
[ }  Estimate - Analyte results are below the quanlitation limit and above the detection limit.

-------
   quantdata
Underfine Stack
Trunrfd CMPD
Naphthal cmpdl
2-Methyi cmpd2
Acenaph cmpd3
Acenaph cmpd4
Fluorene cmpd5
Phenant cmpdS
Anthranc cmpd?
Fluorant cmpdS
Pyrene Cmpd9
Benzo (a cmpdl 0
Chrysen cmpdl 1
Benzo(b cmpdl 2
Benzo(k cmpd 13
Benzo (e cmpdl 4
Benzo (a cmpdl 5
Perylene cmpd16
Indent) { cmp17
Dibenz ( cmpdl 8
Benzo (g cmpd19
Quanterra Compound Name Mol. Wt. Method Blank
Naphthalene 1 128.16 520
2-Methylnaphthalene 2 142,2 14
Acenaphthylene 3 154.21 0
Acenaphlherte 4 154.21 0
Fluorene 5 166.21 0
Phenarrthrene 6 178.22 24
Anthraneene 7 178.22 0
Fluoranlhena 8 202.26 0
Pyrene 9 202.24 0
Benzo (a) anthrancene 10 228.29 0
Chrysene 11 228.28 0
Benzo (b) fluoranthene 12 252.32 0
Benzo (k) fluoranthene 13 252,32 0
Benzo (e) pyrene 14 252.3 0
Benzo (a) pyrene 15 252.3 0
Perylene 16 202.24 0
indeno(1.2,3-cd) pyrene 17 290.34 0
Dibenz (a,h) anthracene 18 278.33 0
Benzo (g,h,i) perylene 19 276.34 0
B-U-429-1 Blank Adjusted
11,000 10,480
5,800 5,786
950 950
190 190
810 810
1,600 1,576
51 51
430 430
170 170
45 45
120 120
76 76
50 50
42 " 42
47 47
12 12
44 44
12 12
81 81
B-U-429-2 Blank Adjusted
31,000 30,480
2,000 1,986
290 290
110 110
230 230
730 706
20 20
220 220
80 80
25 25
59 59
45 45
31 31
32 32
24 24
ND ND
32 32
ND ND
78 78
B-U-429-3 Blank Adjusted
180,000 179,480
8,200 8,186
2,600 2,600
450 450
1,300 1,300
1,700 1,676
86 86
620 620
220 220
72 72
160 160
64 64
39 39
34 34
32 32
ND ND
35 35
ND ND
63 63

-------
APPENDIX E




QA/QC DATA

-------
                        REPORT OF METHOD AUDIT

Laboratory:           Quanterra Environmental Services
                        880 Riverside Parkway
                        West Sacramento, CA 95605

                        Telephone: 916-373-5600

Project: Indiana Coke (Proj #RO 12.000)

Audit Date: September 2,1998

Audit conducted by:  Dennis Becvar of PES, and Robert Weidenfeld of Quanterra

Purpose: The purpose of this audit was to verify if the analytical procedures of
Quanterra Environmental Services (Quanterra) for Polyaromatic Hydrocarbons were
followed in accordance with CARS Method 429 as published August 9, 1996.

Sample Receiving and Log in: Samples are received in a dedicated area (isolated from
the analytical laboratories) of the facility. The client name, description of the samples,
date and time received, requested methods and analytes are recorded on a sample
receiving form directly from the chain of custody form sent with the package containing
the samples. In order to minimize contamination or mixing of samples/clients only one
package is opened at a time.  After the package is opened, each sample is removed from
thepacking material and the sample container is immediately checked for temperature
(the acceptable temperature range is 4+2 °C) with an infrared, unobtrusive, temperature
sensor. In addition to the temperature check, each sample is checked for leakage,
shipping damage, proper labeling, intact-seals, and volume marks on bottles with liquids.
After the samples are logged into the Quanterra sample tracking system, they are stored
in a large cold storage room. The Quanterra sample tracking system is interfaced with
their Laboratory Information Management System (LIMS), and each "logged hi" sample
is identified with a computer generated laboratory control number and the location (rack
and shelf) the sample will be stored in the refrigerator. The temperature in the refrigerator
is maintained at 2-4 °C; also, for documentation purposes, the temperature is
continuously recorded  on a chart recorder.

       If there are any questions regarding the samples the Quanterra project manager is
notified, and if necessary, the client is contacted. It should be noted that for the samples
delivered by PES for the  above project, one of the filters was wet from the ice in the
shipping container.

Sample Extraction and  Concentration: Within a week or less (the method requires
extraction to occur within 21 days of sample collection) the samples are transferred under
chain of custody to the extraction laboratory. The XAD-2 cartridges, front half washes
and filters are transferred to a precleaned Soxhlet apparatus. All of the SoxWets are
cleaned with methylene chloride over a period of 8-12 hours.  The samples are  extracted

-------
with methylene chloride over a period of sixteen hours at a recylce rate of approximately
three cycles per hour. Internal standards are added to the samples before extraction.
After the Soxhlet has been allowed to cool the sample is equally divided with one half of
the sample retained as an archive sample and the second half is prepared for cleanup with
a silica gel column, dried through sodium sulfate, and subsequently concentrated.

Sample Analysis: The extracted and concentrated samples are routed to the high
resolution GC/MS laboratory for analysis. The samples are placed in an autosampler tray
and the samples are injected into the instrument automatically. The sample injector is
purged two times with solvent between sample injections. In addition to internal
standards in each sample, the instrument is restandardized after each fifteen samples.
The instrument in programmed for control limits and the data in the sample set are
flagged if the instrument exceeds the allowable window for drift.

Data Reporting: After the sample analyses are completed the data are checked
manually for completeness. If any matrix effects or sample anomalies are found the
samples are routed through the analytical laboratory for reanalysis. Each data package
sent out by the laboratory is approved by the QA/QC manager and the project manager
for completeness.

General Comments: The laboratory is well organized, extremely well maintained  and
staffed with analysts having many years of experience. Since the analyses are organized
by analytical group, i.e. PAH's, metals, etc. each of the analysts has a very thorough
understanding of the analysis they are performing. The instrumentation is state of the art
and operated by analysts with at least five years of experience. The electronic outputs of
the instruments are connected the LIMS.  Access to the data in the LIMS is restricted to
the analysts, QA/QC staff and project manager, in all cases, the data are in a "read only"
format.  The quality assurance program appears to be very thorough with, sufficient
electronic controls and human reviews to flag any data that is outside the acceptable
quality control criteria for the analysis.  Corrective actions are included in all steps of
Quanterra's quality control process.

       This auditor did not observe any sample handling or analytical procedures outside
the procedures of CARB Method 429 that would result in the invalidation of data for the
above referenced project.  Mr. Weidenfeld of Quanterra mentioned that the sample
matrix for the above samples was expected to be relatively complex and data
interpretation would require a significant amount of data reduction time.  The schedule
for most CARB 429 projects is to issue the laboratory report within 30 days of receiving
the samples.

-------
                    PROCEDURES AUDIT FOR METHOD 315
                            ERG LABORATORIES
       The following is a record of a visit to ERG Labs to evaluate their procedures and
handling of Method 315 samples of emission tests from coke ovens. The work was performed by
ERG chemist Mr. Linh Nguyen under the direction of Dr. Joan T, Bursey, Laboratory Director.

       The first objective was to observe the procedure for weighing the samples. After the
samples were logged in, they were transferred to the weighing room, which is temperature and
humidity controlled. The samples were then put in desiccators to desiccate for twenty-four hours
before being weighed. The samples were then weighed on a laboratory balance.  The balance
was located on a weighing table, which is especially designed to add stability and provide more
accurate weight measurements.

       Because the analysis of Method 315 samples for Methylene Chloride Extractable Matter
(MCEM) is done over a period of about seven to eight working days, it was not possible to
observe the analysis in its entirety. It was decided to observe two segments of the analysis on
separate visits. During the first visit the procedures handling of the filters for MCEM analysis,
were observed to verify that the analyses were done according to section 11.2.1.2 of the method.
The chemist was very meticulate in his work and explained the procedures as they were
occurring and answered questions as they were raised. The second visit was about four days later
or midway into the analysis. This segment included the MCEM analysis of the impinger
solutions. This was done following the procedures in section 11.2.4.1 of the method. This
involved the adding of a known quantity  of methylene chloride to the impinger water in a
separatory funnel and extracting off the phase that had separated. This was done  a total of three
times. The extracts were then heated to near dryness, transferred to an aluminum dish where the
extract was allowed to dry and reach equilibration in the balance room. The sample was then
weighed to the nearest 0.1 mg. After analysis was completed and data computed, the data
wasreviewed by the laboratory director for accuracy and completeness.

      Thus observer did not notice any sample handling or analytical procedures outside the
procedures of Method 315 that would result in the invalidation of data for the above referenced
project.

-------
                                                         Pacific Environmental
                                                         Services, Inc.
Memo
       T«    PES Project File S511.000

       From:  FrankBn Meadows, Project Manager

       CC:

       Date:  11/13/98

       Re:    Rrst Analytical Laboratory Visit
              Trie PM and MCEM sample residues were hand delivered by the PES Project Manager to
       First Analytical Laboratory (FAL) for subsequent analysis for 17 trace metals.  The samples were
       received In a dedicated sample receiving area where they were unpacked and arranged by Run
       Number and sample fraction. The samples were inspected for integrity, damage, and chain-of-custody
       documentation. All of the samples were received in good condition and all were accounted for.

              Once the samples were accounted for, Dr. WilBam A Wadiin,  FAL Laboratory Manager,
       assigned a project number to the PES project and logged  the samples into FAL's sample tracking
       system.  Each sample and sample fraction was assigned a unique identification number and the
       samples were again compared to the sample chain-of-custody document.

              During the sample preparation stage,  each sample digestate was labelled with the original
       sample identification code.  These numbers were used to track the sample through the sample
       preparation and digestion process.  All raw data printouts and calibration curves are labelled with the
       identification number These numbers were used throughout the preparation and analysis to the final
       report of the results, so that a paper trail could be generated for each analytical result that tracks the
       result back to the original sample.

              A walk-through of the laboratory indicated that the laboratory was well organized, clean, and
       well maintained. The samples were prepared and analyzed by Dr. Wadiin.  Standard FAL procedure is
       to analyze the samples progressively first using the procedure having the least analytical sensitivity
       followed by the procedure having the next best analytical  sensitivity.  The laboratory continuously
       monitors instrument performance and makes necessary instrument repairs in advance of instrument
       failure so  that samples do not need to be re-analyzed due to instrument performance outside the
       method QC requirements.

              FAL has been participating in the EPA's quarterly audit for metals analysis (lead) for the past
       three years. FAL is also approved by EPA Region I for EPA Method 29 analyses.
        i Page 1

-------

                        NOZZLE CALIBRATION SHEET
DATE:
- f/
                                        CAUBRATIQN BY:
/
               Nozzie
             Identification
               Number
D 1 , in.
                      D2,in.
D3»in.
                                         6 ,
AD, in.
                                                  ti.OOi,
            avg
                                                          0*117
           Where:
               DI 2 3 =s nozzle diameter measured on a different diameter, in.
                      Tolerance = measure within 0.001 in.

              AD = maximum difftrance in any two measurements, in.
                      Tolerance = 0.004 in.
               Davg= average of DV D2, D3.

-------
            NOZZLE CALIBRATION SHEET
                             CALIBRATION BY:.
    Nozzle
 Identification
   Number
Dvin.
D,ln.
D3,ln.
AD, in.
                            avg
    •
 D ~C'
             0.2*1
                        ,00)
                                      0,802*
Where:
   D.,, „ = nozzle diameter measured on a different diameter, In.
     \tf.,O
           Tolerance = measure within 0.001 in.


   AD = maximum difference in any two measurements, in.
           Tolerance = 0.004 in.
   Davg= average of D1, D2, Dg.

-------
            NOZZLE CALIBRATION SHEET
DATE:
                            CAUBRATION BY:

    Nozzle
 Identification
   Number
                     D2, in.
D3,ln.
AD, in,
            avg
£-.-
X    //> l-r
6  , y? 7
&.(>
                              a,
            4496
                                              0*^3*,
                                     a
Where:
   D, 2 3 = nozzle diameter measured on a different diameter, in.
          Tolerance = measure within 0.001 in.

   AD = maximum difference in any two measurements, in,
          Tolerance = 0.004 in.
    avor
               of Dv D2, D3.

-------
            NOZZLE CALIBRATION SHEET
DATE;
CALIBRATION BY:
Nozzle
Identification
Number
•&-••*• 	 y*y*>


D .j , in.
-,p y»|-r
ftvfl
(Q f 75^

D2,in.
-A-^&_
«.ft?


D3, In.
t/d-7
fcWfl


AD, in.
,
@i®(n
^?*
-------
                                                                                         9/3QT94: CD2-t
                                      CAUBRATtON DATA SHBT I
                                      Type S Phot Tufa* Inspection
Level and Perpendicular?
Obstruction?
OwnBpejdf
*, 1-10" * *, * +10«l
% MO* * % * *l««l
&, K» * fi, S -1-5*1
8, M« * if * +8*1
r
e
t * Atwr 
Yts
}00
po
o
(
\
o
I
c3
,0(71
c.
J/%
\,-t^
f.IC
OA/QCG^ek
                      U0tttHlty
                                         Aosuwey.
Reasonableness
CtftttJcMthn
I certify that the Type S nttot tufae/orotae Of     R. ? ' 1- \
criteria and/or appUcabJe detifln feeture* end Is hereoy assiflned a ptet tube oOlbratlQo factor Cp of 0.84.
                                                                 . RiMt* or MBMte rt «pedfiqBtlonj,
                   Personnel ISionatur«>O«te)
                                                                  Teem Leader (Sionature/Date)

-------
                                                                                    9/30/94:  CD2-1
                                    CALIBRATION DATA SHEET 2
                                     Type S Phot Tub* fcttpectton
Level end Perpendicular?

UliVU UCC1OV"
Damaged?
0, (-10° a «t * +10*1
oj M0**«j* 4>10«l
S, (-8" « St * +B']
5, M««i>S +8-1
r
e
I- Attnr 1 T*V
o
%
/. o J •*»
/- 36,

ConptotanMs
L*glbIUty,
Accuracr.
CtrtOatha
leertfvttiatthaTvp«Sprt«tubi/prob»IOI
Spwrfftarttora
                                          mMt* or «xea*ds ID specfflcatkuu,
criteria md/or •ppUeabla design feature* md ts hereby acsigned a pitot tubt etlbmtlon teeter Cp of 0.84.
                  Personnel
                                         Teem Leader jSignattire/Datel

-------
5B
                         PACIFIC ENVIRONMENTAL SERVICES, INC.
                                                                                              4700 Duke Drive,
                                                                                                     Suite 150
                                                                                             Mason, Obio 45040
                                                                                          Phone:(513)398-2556
                                                                                             Fax (513) 398-3342
                                                                                                 www.pes.com
Pitot Tube Number:

Effective Length:
                           5B
                           64"
          Date:

Calibrated By:
Pitot Tube Openings Damaged?               YES

Pitot Tube Assembly Level?              |  YES  j

       a ,  =                3         °(< 10°)

       p.—                1          ^ ^ 5 j

                Y=         3             e =
                                                                  NO
                                                                  NO
                                                                      a
     2 = A sin Y  —

    w = A sin 6  =
                                0.059
                                0.020
                                                cm (in.)   0.32 cm ( < 1/8 in.)

                                                cm (in.)   0.08 cm ( < 1/32 in.)

                                                0.562                cm (in.)
                          PB =
                          D,
                                                0.562
                                                0.375
                                                                     cm (in.)
                                                                     cm (in.)
                                                fi           ft
                         (a)
                                                                                      12/22/97
                            Flow
                                                                   '"•'•';c;, —•«••--	
                                                                   _^*/"	f Q2(» or-)
                                                                                       S. Simon
                                                                                       1.124
                                                                                        Flow
                                                                                     (<=>
                      ~ 	'"^BKI"	
                                                                   (a)
           The typea o* faiae-opanlng mis alignment shown above will not affect thebaselne value of Cp(s) so
           long as <*,and <*,is less than or equal to 1O*, a,and a, la loss than or equal to 5*, z Is lass than or
           equal to O.32 cm (1/8 In.), and w b lass than orequel to O.OB cm(1&2 frv) {reference 11.O In
                 1SOV	
                                                                                                   '(< 10°)
                                      Pitot Tube Calibration Form
                                                                                        1998 Yearly Calibration

-------
5C
PACIFIC ENVIRONMENTAL SERVICES, INC.
                       4700 Duke Drive,
                              Suite 150
                      Mason, Ohio 45040
                    Phone: (5l3) 398-2556
                      Fax (513) 398-3342
                          www.pes.com
Pilot Tube Number: 5C Date:
Effective Length: 61" Calibrated By:

Pilot Tube Openings Damaged? YES | NO (

Pilot Tube Assembly Level? \" YES | NO
a , . 0 °« 10°) a 2 -
12/23/97
S. Simon
1
P, = 1 °«5°) |32 = l
Y= 1 9 = 1 A =
z = A sin Y = 0.017 cm (in.) 0.32 cm ( < 1/8 in.)
w = A sin 0 = 0.017 cm (in.) 0.08 cm ( < 1/32 in.)
PA = 0.474 cm (in.)
0.948

                                                                                               '(< 10°)
                                              0.474
                         D,
                       0.375
cm (in.)

cm (in.)
                                                                 (0)
           Ths types of face-opening misalignment shown above wit not affect the baseSna value of C£>(s) so
           long as a, and Sis lass tnan or equal to 1O*, a, and a. Is less than or aqua) to 5*. z is less than or
           equal to Q.32 cm (1/S h,), and w Is less than or equal too,OB cm (1/32 in ) (referenoal 1 O In
           Section
                                     Pitot Tube Calibration Form
                                                                                     1998 Yearly Calibration

-------
 5E
PACIFIC ENVIRONMENTAL SERVICES, INC.
                                               4700 Duke Drive,
                                                      Suite 150
                                              Mason, Ohio 45040
                                           Phone: (513) 398-2556
                                              Fax (513) 398-3342
                                                  www.pes.com
Pilot Tube Number:

Effective Length:
   5E
   64"
                              Date:      12/22/97

                   Calibrated By:         S.Simon
                                         YES
Pitol Tube Openings Damaged?

Pilot Tube Assembly Level?               (  YES  |

       a ,  =        	1         °(< 10°)


       Pi  -        	

                 Y =
                                                                    NO
                                                                        a ,  =
                             1
                             0
                  e =
       1
A =
     z = A sin Y —

     w = A sin B =
         0.02
                           PA  =
                           P =
cm (in.)   0.32 cm ( < 1/8 in.)

cm (in.)   0.08 cm ( < 1/32 in.)

0.561                 cm (in.)
                        0.561
                                                 0.375
                      cm (in.)

                      cm (in.)
                                                                             Jua.
                                                                                 =•-)
                                                                      (g)
1.122
            The types of face-opening mis alignment shown above will not affect the baselne value of Q?
-------
 7A
PACIFIC ENVIRONMENTAL SERVICES, INC.
                                               4700 Duke Drive,
                                                      Suite 150
                                             Mason, Ohio 45040
                                           Phone: (513) 398-2556
                                             Fax (513) 398-3342
                                                  www.pes.com
Pilot Tube Number:

Effective Length:
   7A
   86"
Pilot Tube Openings Damaged?               YES

Pitot Tube Assembly Level?               |   YES   j

       a ,  =                0        "(< 10°)
                 Y=
                                           e =
                               1
                             Date:      12/22/97

                   Calibrated By:        S. Simon
                                           NO
                                                                        P2  =

                                         0.996
                                                                             (< 10°)
     z = A sin Y —

     w = A sin 8 =
         	"TTJ
        0.069
        0.017
                           P  ss
cm (in.)   0.32 an ( < 1/8 in.)

cm (in.)   0.08 cm ( < 1/32 in.)

0.498                 cm (in.)
                                                 0.498
                                                 0.375
                                             cm (in.)

                                             cm (in.)
                                                                                          Flow
                                                                                       (c)
                                                                                        I.wl!
            Tha types of face-opening misalignment shown above wlI not affect thebaselne value of Cp(s) so
            long aa Q, and "^ia less than or equal to 1Q-,e,and B2 is less than or equal to ST. z is less than or
            equal to 0,32 cm (1/8 In.), andw is tesa thai or equal too.OS cm (1/32 In.) (reference11 O In
            Sadltn
                                        Pitot Tube Calibration Form
                                                                                          1998 Yearly Calibration

-------
7D
                    PACIFIC ENVIRONMENTAL SERVICES, INC.
                                                                                              4100 Duke Drive,
                                                                                                     Suite 150
                                                                                            Mason, Ohio 45040
                                                                                          Phone: (513) 398-2556
                                                                                            Fax (513) 398-3342
                                                                                                 www.pes.com
Pilot Tube Number:

Effective Length:
                           7D
                          84.5"
Pilot Tube Openings Damaged?

Pilot Tube Assembly Level?

       a j  =       	3

       Pi  -       	

                Y=         1
                            1
                                       YES
                                |   YES  |

                                 °(< 10°)

                                 °«5°)
                                         9=
                                                     0
                                                                             Date:

                                                                   Calibrated By:
                                                              NO  |
                                                                  NO
                                                                     a2  =
                                                                        A =
                                                                                  12/23/97
                                                                                  S. Simon
                                                                                        0.931
                                                                                                   '(< 10°)
 z = A sin Y =

w = A sin 9 =
              QL
                                0.016
                          PA =
                          Pp =
                             —
                           i
                          vfl^S
                                                cm (in.)   0.32 cm ( < 1/8 in.)

                                                cm (in.)   0.08 cm ( < 1/32 in.)

                                                0.466                 cm (in.)
                                           0.465
                                               0.375
                                                                     cm (in.)
                                                                cm (in.)
                                                                              or-)
           TTie types a face-opening misetignmnnt shown abava wll not affect tha baseine value of Cp(s) so
           long as ", and ^is less than or equal lo to*, a, and Q2 Is less than or equal to 5". z is less than or
           equal to O32 cm (1/B in.), and w is less than or equal loO.OS cm{1.<32 In.) (reference! 1 O in
           SecHon
                                      Pitot Tube Calibration Form
                                                                                        1998 Yearly Calibration

-------
 8C
                        PACIFIC ENVIRONMENTAL SERVICES, INC.
                                              4700 Duke Drive,
                                                     Suite 150
                                            Mason, Ohio 45040
                                          Phone:(513)398-2556
                                            Fax (513) 398-3342
                                                 www.pes.com
Pilot Tube Number:

Effective Length:
Pilot Tube Openings Damaged?

Pilot Tube Assembly Level?
                            8C
                           85"
                                        YES
                                          10°)
                             Date:      12/12/97

                   Calibrated By:         S.Simon
                                                                  NO
                                                                      a
                                                   '(< 10°)
                                          9 =
                                                                             A =
                                                                                        0,939
     z = A sin Y =

     w = A sin & =
                                0.016
                              P_
                            A
                           Dt =
cm (in.)   0.32 cm ( < 1/8 in.)

cm (in.)   0.08 cm ( < 1/32 in.)

 0,47                 cm (in.)
                                                0.469
                                                0.375
                     cm (in.)

                     cm (in.)
                                                                    (a)
            Tre types of face-opening misalignment shown abovewll not affect the baseline value of Cp(s) so
            long as ", and c^ls less than or equal to 1O°. a, and tts  is less than or equal to S", z fe lass than or
            equal to O.32 cm (1/8 In.), and w s less than or equal too.OB cm(1/32 In.) (referencal 1.0 In
                                       Pitot Tube Calibration Form
                                                                                         1998 Yearly Calibration

-------
                 PACIFIC ENVIRONMENTAL SERVICESJNC.
                                                 4700 Duke Drive,
                                                      Suite 150
                                                Mason, OH 45040
                                             Phone: (513) 398-2556
                                               Fax: (513) 398-3342
                                                   www.pes.com
               TEMPERATURE SENSOR CALIBRATION DATA FORM
                              FOR SAMPLE HEAD
DATE:
12/19/97
AMBIENT TEMPERATUREfF):

CALIBRATOR:
              77
            S.Simon
THERMOCOUPLE NUMBER:

BAROMETRIC PRES.(ln.Hg):

REFERENCE:
Mercury-in-glass:

Other:
SH-2
29.33
                                                                  ASTM-3
Reference
point
number
1
2
Source3
(Specify)
Ambient Air
Cold Bath
Reference
Thermometer
Temperature,°F
77
40
Thermocouple
Potentiometer
Temperature,°F
76.6
40.6
Temperature
Difference,"
°F
0.4
0.6
''Type of calibration used.

"Allowable tolerance ±2°F


Comments:
                      SAMPLE HEAD CALIBRATION FORM
                                            1998 Yearly Calibration

-------
                 PACIFIC ENVIRONMENTAL SERVICES,INC.
                                                 4700 Duke Drive,
                                                       Suite 150
                                                Mason, OH 45040
                                              Phone: (513) 398-2556
                                                Fax:(513)398-3342
                                                   www.pes.com
               TEMPERATURE SENSOR CALIBRATION DATA FORM
                              FOR SAMPLE HEAD
DATE:
12/19/97
AMBIENT TEMPERATURE(°F):

CALIBRATOR:
              77
            S.Simon
THERMOCOUPLE NUMBER:

BAROMETRIC PRES.(ln.Hg);

REFERENCE:
Mercury-in-glass:

Other:
SH-3
29.33
                                                                  ASTM-3
Reference
point
number
1
2
Source3
(Specify)
Ambient Air
Cold Bath
Reference
Thermometer
Temperature,°F
77
42
Thermocouple
Potentiometer
Temperature,°F
76.6
42.8
Temperature
Difference,"
°F
0.4
0.8
"Type of calibration used.

bAllowable tolerance ±2°F
Comments:
                       SAMPLE HEAD CALIBRATION FORM
                                             1998 Yearly Calibration

-------
DATE:
                 PACIFIC ENVIRONMENTAL SERVICESJNC.
                                                 4700 Duke Drive,
                                                      Suite 150
                                                Mason, OH 45040
                                             Phone: (513) 398-2556
                                               Fax:(513)398-3342
                                                   www.pes.com
               TEMPERATURE SENSOR CALIBRATION DATA FORM
                             FOR SAMPLE HEAD
12H9/97
AMBIENT TEMPERATURE(°F):

CALIBRATOR:
              76
            S.Simon
THERMOCOUPLE NUMBER:

BAROMETRIC PRES.(ln.Hg):

REFERENCE:
Mercury-in-glass:

Other:
29.33
                                                                  ASTM-3
Reference
point
number
1
2
Source*
(Specify)
Ambient Air
Cold Bath
Reference
Thermometer
Temperature,0F
76
39
Thermocouple
Potentiometer
Temperature,°F
76
39.2
Temperature
Difference,"
°F
0
0.2
aType of calibration used,

bAllowable tolerance ±2°F


Comments:
                      SAMPLE HEAD CALIBRATION FORM
                                            1998 Yearly Calibration

-------
                 PACIFIC ENVIRONMENTAL SERVICESJNC.
                                                 4700 Duke Drive,
                                                      Suite 150
                                                Mason, OH 45040
                                             Phone:(513)398-2556
                                               Fax: (513) 398-3342
                                                  www.pes.com
               TEMPERATURE SENSOR CALIBRATION DATA FORM
                             FOR SAMPLE HEAD
DATE:
12/19/97
AMBIENT TEMPERATURE(°F):

CALIBRATOR:
              76
            S.Simon
 THERMOCOUPLE NUMBER:

_ BAROMETRIC PRES.(ln.Hg):

 REFERENCE:
"Mercury-in-glass:

 Other:
SH-5
29.33
                                                                 ASTM-3
Reference
point
number
1
2
Source*
(Specify)
Ambient Air
Cold Bath
Reference
Thermometer
Temperature,°F
76
40
Thermocouple
Potentiometer
Temperature,°F
76
40.8
Temperature
Difference,"
°F
0
0.8
*Type of calibration used.

bAI!owable tolerance ±2°F


Comments:
                      SAMPLE HEAD CALIBRATION FORM
                                            1998 Yearly Calibration

-------
                 PACIFIC ENVIRONMENTAL SERVICES.INC.
                                                 4700 Duke Drive,
                                                       Suite 150
                                                 Mason, OH 45040
                                              Phone: (513) 398-2556
                                                Fax: (513) 398-3342
                                                   www.pes.com
               TEMPERATURE SENSOR CALIBRATION DATA FORM
                              FOR SAMPLE HEAD
DATE:
12/19/97
AMBIENT TEMPERATURE(°F):

CALIBRATOR;
              77
            S.Simon
THERMOCOUPLE NUMBER:

BAROMETRIC PRES.(ln.Hg):

REFERENCE:
Mercury-in-glass:

Other
SH-6
29.33
                                                                   ASTM-3
Reference
point
number
1
2
Source*
(Specify)
Ambient Air
Cold Bath
Reference
Thermometer
Temperature,°F
77
40
Thermocouple
Potentiometer
Temperature,°F
77.4
40.8
Temperature
Difference. b
°F
0.4
0.8
Type of calibration used.

bAllowable tolerance ±2°F


Comments:
                       SAMPLE HEAD CALIBRATION FORM
                                             1998 Yearly Calibration

-------
                 PACIFIC ENVIRONMENTAL SERVICES.INC.
                                                 4700 Duke Drive,
                                                       Suite 150
                                                Mason, OH 45040
                                              Phone: (513) 398-2556
                                                Fax: (513) 398-3342
                                                   www.pes.com
               TEMPERATURE SENSOR CALIBRATION DATA FORM
                             FOR SAMPLE HEAD
DATE:
12/19/97
AMBIENT TEMPERATURE(°F):

CALIBRATOR:
              77
            S.Simon
THERMOCOUPLE NUMBER:

BAROMETRIC PRES.(ln.Hg):

REFERENCE:
Mercury-in-glass:

Other:
SH-7
29.33
                                                                  ASTM-3
Reference
point
number
1
2
Source3
(Specify)
Ambient Air
Cold Bath
Reference
Thermometer
Temperature,*^
77
40
Thermocouple
Potentiometer
Temperature,0 F
78
41.2
Temperature
Difference,"
°F
1
1.2
aType of calibration used.
"Allowable tolerance +2°F
Comments:
                       SAMPLE HEAD CALIBRATION FORM
                                             1998 Yearly Calibration

-------
                 PACIFIC ENVIRONMENTAL SERVICESJNC.
                                                 4700 Duke Drive,
                                                       Suite 150
                                                Mason, OH 45040
                                             Phone:(513)398-2556
                                               Fax:(513)398-3342
                                                   www.pes.com
               TEMPERATURE SENSOR CALIBRATION DATA FORM
                              FOR SAMPLE HEAD
DATE:
12/19/97
AMBIENT TEMPERATURE(°F):

CALIBRATOR:
              76
            S.Simon
THERMOCOUPLE NUMBER:

BAROMETRIC PRES.(ln.Hg):

REFERENCE:
Mercu ry-in-glass:

Other
SH-8
29.33
                                                                  ASTM-3
Reference
point
number
1
2
Source*
(Specify)
Ambient Air
Cold Bath
Reference
Thermometer
Temperature,°F
76
39
Thermocouple
Potentiometer
Temperature,°F
76.4
38.2
Temperature
Difference,11
°F
0.4
0.8
''Type of calibration used.
 Allowable tolerance ±2°F
Comments;
                       SAMPLE HEAD CALIBRATION FORM
                                            1998 Yearly Calibration

-------
                    PACIFIC ENVIRONMENTAL SERVICES.INC.
                                 4700 Duke Drive,
                                       Suite 150
                                     Mason, Ohio
                             Phone: (513) 398-2556
                                Fax:(513)3983342
                                   www.pes.com
                  TEMPERATURE SENSOR CALIBRATION DATA
                         FOR STACK THERMOCOUPLES
THERMOCOUPLE NUMBER:
 5B
 DATE:
12/22/97
BAROMETRIC PRES.(ln.Hg):
AMBIENT TEMP. °F:
29.52
 72
 REFERENCE:
 Mercury-in-glass:

 Other:

"CALIBRATOR:
                                                                  ASTM-3F
                                                                    J.C.
Reference
point
number
1
2
3
4
Source8
(Specify)
Ambient Air
Cold Bath
Hot Bath
Hot Oil
Reference
Thermometer
Temperature,°F
72
44
204
400
Thermocouple
Potentiometer
Temperature,°F
72
44
204
400
Temperature
Difference,"
%
0.00
0.00
0.00
0.00
*Type of calibration used.

b(ref temp.°F+460Wtest thermometer temp.°F+46Cn   X100
           reftemp,°F+460

Comments:
                            100<1.5%
                      STACK THERMOCOUPLE CALIBRATION FORM      1998 Yearly Calibration

-------
                    PACIFIC ENVIRONMENTAL SERVICES.INC.
                                  4700 Duke Drive,
                                       Suite 150
                                     Mason, Ohio
                              Phone:(513)398-2556
                                Fax: (513)3983342
                                   www.pes.com
                  TEMPERATURE SENSOR CALIBRATION DATA
                         FOR STACK THERMOCOUPLES
THERMOCOUPLE NUMBER:
T5B
 DATE:
12/23/97
BAROMETRIC PRES.(ln.Hg):
AMBIENT TEMP. °F:
29,52
 74
 REFERENCE:
 Mercury-in-glass:

 Other:

"CALIBRATOR:
                                                                  ASTM-3F
                                                                    J.C.
Reference
point
number
1
2
3
4
Source8
(Specify)
Ambient Air
Cold Bath
Hot Bath
Hot Oil
Reference
Thermometer
Temperature,°F
74
46
200
318
Thermocouple
Potentiometer
Temperature, °F
74
46
200
318
Temperature
Difference,"
%
0.00
0.00
0.00
0.00
''Type of calibration used,

bf ref. temD.°F+460Wtest thermometer ierm"F-+4601.
      X100
           reftemp,0F+460
Comments;
                 100<1.5%
                      STACK THERMOCOUPLE CALIBRATION FORM
                              1998 Yearly Calibration

-------
                    PACIFIC ENVIRONMENTAL SERV1CES,INC.
                                 4700 Duke Drive,
                                       Suite 150
                                     Mason, Ohio
                             Phone:(513)398-2556
                                Fax: (513)3983342
                                   www.pes.com
                 TEMPERATURE SENSOR CALIBRATION DATA
                        FOR STACK THERMOCOUPLES
THERMOCOUPLE NUMBER:
 7A
 DATE:
12/23/97
BAROMETRIC PRES.(ln.Hg);
AMBIENT TEMP. °F:
29.52
 74
 REFERENCE:
 Mercury-in-glass:

 Other.

"CALIBRATOR:
                                                                  ASTM-3F
                                                                   G.Gay
Reference
point
number
1
2
3
4
Source8
(Specify)
Ambient Air
Cold Bath
Hot Bath
Hot Oil
Reference
Thermometer
Temperature,°F
74
36
198
333
Thermocouple
Potentiometer
Temperature1°F
74
36
199
332
Temperature
Difference, b
%
0.00
0.00
0.15
0.13
aType of calibration used.

b(ref. temp.°F+460)-(test thermometer temp.°F+460)   X100
           reftemp.°F+460

Comments:
                            100
-------
                    PACIFIC ENVIRONMENTAL SERVICES.INC,
                                 4700 Duke Drive,
                                       Suite 150
                                     Mason, Ohio
                              Phone: (513) 398-2556
                                Fax:(513)3983342
                                   www.pes.com
                  TEMPERATURE SENSOR CALIBRATION DATA
                         FOR STACK THERMOCOUPLES
THERMOCOUPLE NUMBER:
 7D
 DATE:
12/23/97
BAROMETRIC PRES.(in.Hg):
AMBIENT TEMP. °F:
29.52
 74
 REFERENCE:
 Mercury-i n-glass:

 Other:

"CALIBRATOR:
                                                                  ASTM-3F
                                                                   G. Gay
Reference
point
number
1
2
3
4
Source8
(Specify)
Ambient Air
Cold Bath
Hot Bath
Hot Oil
Reference
Thermometer
Temperature, °F
74
40
206
340
Thermocouple
Potentiometer
Temperature,°F
74
41
205
341
Temperature
Difference,1"
%
0.00
0.20
0.15
0.13
''Type of calibration used.

b(ref. temp.°F+460Wtest thermometer tempt°F+460)   X100
           ref temp,°F+460
                            100<1.5%
Comments;
                      STACK THERMOCOUPLE CALIBRATION FORM       1998 Yearly Calibration

-------
                    PACIFIC ENVIRONMENTAL SERVICES.INC.
                                 4700 Duke Drive,
                                       Suite 150
                                     Mason, Ohio
                             Phone: (513) 398-2556
                                Fax: (513)3983342
                                   www.pes.com
                 TEMPERATURE SENSOR CALIBRATION DATA
                        FOR STACK THERMOCOUPLES
THERMOCOUPLE NUMBER:
 8C
 DATE:
12/15/97
BAROMETRIC PRES.(ln.Hg):
AMBIENT TEMP. °F:
29.52
 74
 REFERENCE:
 Mercury-in-glass:

 Other:

"CALIBRATOR:
                                                                  ASTM-3F
                                                                   G. Gay
Reference
point
number
1
2
3
4
Source3
(Specify)
Ambient Air
Cold Bath
Hot Bath
Hot Oil
Reference
Thermometer
Temperature, °F
74
38
199
339
Thermocouple
Potentiometer
Temperature,°F
74
38
199
339
Temperature
Difference,b
%
0.00
0.00
0.00
0.00
""Type of calibration used.

brref. temD.QF+460V-ftest thermometer temo.°F+460>
      X100
           ref temp10F+460
Comments:
                 100<1.5%
                      STACK THERMOCOUPLE CALIBRATION FORM       1998 Yearly Calibration

-------
                     TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No.

Ambient Temp. °F
      Reference Temp. Sensor:
                           j  Sensor Type
                                                    -TC.    Length

                                             Barometric Pressure, "Hg
Date
t-zz-«w
"
• •















Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
wS>
M&'
*Sio'















Temp. °F
Ref.
Sensor
•*>t
1^
^10















Test
Sensor
3^
€><{
•L^















Temp.
Diff . %
o
-.c-s
-.-ztv















Within
Limits
Y/N
X
H
4






-•








Calibrated
By
v^
\Ui
\ Wv
0














J
Tentp. Diff =
   ^
                   Temp + 40) " (  Test
                                  f
                                  (Ref. Temp. + 460)
                                                          46Q)
                                                               x 100 s 1.5

-------
              TEMPERATURE SENSOR CALIBRATION FORM
Temperature Sensor No.
Ambient Temp. °F
                     Jl:
                                 Sensor Type
                             ~ <• ^    Length,
                      Barometric Pressure, "Hg J
Reference Temp. Sensor:
Date
^V=iY
I*
"















Ref.
Point
No.
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Temp.
Source
J£5
1TI'
BoYc,















Temp. °F
Ref.
Sensor
^7.
If
-t.o'ii















Test
Sensor
^z~
7S
to^















Temp.
Diff. %
o
,Ul
.\^So















Within
Limits
Y/N
V
V
^y















Calibrated
By
\u&
W
\t3i
u














 % Temp. Diff =
      *^
(Ref*
                             40) " (  Te3t
                           (fief. Temp. + 460)
                                                   46Q)
                                                        x 100 * 1.5 %

-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
        4700 Duke Drive,
              Suite 150
       Mason, Ohio 45040
      Phone:(513)398-2556
       Fax:(513)398-3342
          www.pes.com
Box No.:
Date:
•BBI
DH
inHg
Vw,
Vw2
Vd,
Vd2
Tw
Td
t
MB-1
10-27-97
••••••
Delta H
Vaccum
Initial RIM
Final RTM
Initial DGM
Final DGM
Ave. Temp RTM °F
Ave. Temp DGM "F
Time (rain.)
Bar. Press,(Pb);
Calibrated By :
| RUN1
0.50
10
934.200
951.896
448.724
466.501
70
79
46.000


RUN 2
0.75
10
952.122
962.945
466.737
477.617
72
82
23.000
29.13
TAA
RUN 3
1.00
10
963.339
975.195
478.016
489.970
71
83
22.0
in. Hg

RUN 4
1.50
10
975.415
987.207
490,201
502.081
72
84
18.0


RUNS
2.00
10
987.492
998,114
502.365
513.078
70
85
14.0


RUNS
4.00
10
999.025
1009.583
513.990
524.620
71
87
10.0
Vwj - Vw! Ne, volume RTM
Vd2 - Vd, Ne, volume DGM
Y
dH@
AVERAGE Y = 1.012
Average Y Range =
AVERAGE dH@ 1.954
Average dH@ Range =
17.696 10.823
17.777 10.880
1.011 1.012
1.916 1.925
0.992
1.754
11.856
11.954
1.012
1.946
TO
TO
11.792 10.622 10.558
11.880 10.713 10.630
1.011 1.014 1.013
1.979 1.949 2.013
1.032
2.154
ACCEPT
ACCEPT
Calculations
Y = (Vw
dH@ =
* Pb * (Td + 460}) / (Vd * (Pb +
0.0317 * dHd / (Pb (Td + 460)) *
{dHd / 13.6)) *
(((Tw +460) *
(Tw 4-460))
I) / Vw)"2
       Initial Dry Gas Meter Calibration Form (English Units)
1998 Yearly Calibration

-------
    PACIFIC ENVIRONMENTAL SERVICES, INC.
Box No.:

Date:

Calibrated By:

Plant:


•

DH

inHg

Vw,

Vw2

Vdt

Vd2


Tw

Td
        1

     8-17-98

        gg

  Bethlemem Steel


 •I

Delta H

Vacuum

Initial RTM

Final RTM

Initial DGM

Final DGM

Ave, Temp RTM °F

Ave. Temp DGM °F

Time (min.)
Bar, Press.(Ps):

Pretest Gamma:

 Pretest dH@:



   RUN1

    1,90

    5,00

   69.112

   76,785

   274.034

   281.633

    69.0

    70.0

    10.0
 30.00

 1.012

 1.954



 RUN 2

 1.90

 5.00

 76.785

 84.492

281.633

289,274

 69.0

 76,0

  10.0
AVERAGE Y =                       1.011


% Difference from Yearly Y =            -0.058

AVERAGE dH@ =                     1.812

Calculations

Y = (Vw * Ph * (Td + 460)) ; (Vd * (Pb + (dHd / 13.6)) * (Tw +460))

dH@ = 0.03H * dHd / (Pb (Td + 460)) * (((Tw +460) * time) / Vw)'2
in. Hg
      RUN 3

       1.90

       5.00

      84.492

      91.992

     289.274

     296.735


       69.0

       74.0

       10.0
Vw2 - Vw,
Vdj - Vd,


Net Volume RTM
Net Volume DGM
Y
dH©
7.673
7.599
1.007
1.801
7.707
7,641
1.017
1.765
7.500
7.461
1.010
1.870
                                             ACCEPT
                                                                                       4700 Duke Drive,
                                                                                              Suite 150
                                                                                      Mason, Ohio 45040
                                                                                     Phone:(513)398-2556
                                                                                      Fax: (513)398-3342
                                                                                           www.pes.com
                           Posttest Dry Gas Meter Calibration Form (English Units)
                                                                                 9/18/98

-------
                  PACIFIC ENVIRONMENTAL SERVICES, INC.
        4700 Duke Drive,
              Suite ISO
       Mason, Ohio 45040
      Phoite:(513)398-2556
       Fax: (513)398-3342
           www.pes.com
Box No.:

Dale:
).:

BBO
DH
mHg
Vw,
Vwz
Vd,
Vdj
Tw
Td
t
2
10-17-97
•••••••
Delta H
Vacuum
Initial RTM
Final RTM
Initial DGM
Final DGM
Ave. Temp RTM °F
Ave. Temp DGM °F
Time (min.)
Bar, Press.(Pb)
Calibrated By :
| RUN1
0.50
10
558,612
569.029
108.182
118.634
75
75
25.5


RUN 2
0.75
10
574.095
585.906
123.684
135,517
76
78
24.0
29.50
RJK
RUN 3
1.00
10
586.200
598.741
135.800
148.334
78
80
22.0
in.Hg

RUN*
1.50
10
598.965
6J2.032
148.548
161.596
78
82
19.0


RUNS
2.00
10
612.242
630.414
161.792
179.920
79
83
23.0


RUN 6
4.00
10
630.900
646.492
180.404
195.932
SO
85
14.0
Vw2 - Vw, Ket volume RTM
Vdj - Vd, Ne, volume DGM
Y
dH@
AVERAGE Y= 1.002
Average Y Range =
AVERAGE dH@= 1.797
Average dH@ Range =
10.417 11.811 12.541 13.067 18.172 15.592
10.452 11.833 12.534 13.048 18.128 15.528
0.996 0.999 1.003 1.004 1.006 1.003
1.719 1.779 1.769 1.822 1.839 1.852

0.982 TO 1.022

1.597 TO 1.997

ACCEPT

ACCEPT
Calculations
Y = (Vw
dH@ =
* Pb * (Td + 460)5 / (Vd * (Pb + (dHd / 13.6)) * (Tw +460))
0.0317 * dHd / (Pb (Td + 460)) * ((CTW +460) » t) / Vw)"2
                          Initial Dry Gas Meter Calibration Form (English Units)
1998 Yearly Calibration

-------
    PACIFIC ENVIRONMENTAL SERVICES, INC.
Box No.;

Date:

Calibrated By ;

Plant:

•

DH

hiHg

Vw,

Vwj

Vd,

Vdi

Tw

Td

t
      MB 02

      8-17-98

        sb

   Bethlhem Steel

  •I

Delta H

Vacuum

Initial RTM

Final RTM

Initial DGM

Final DOM

Ave. Temp RTM °F

Ave. Temp DGM °F

Time (inin.)
Bar. Press.(Pb):

Pretest Gamma:

 Pretest dH@:



   RUN1

    l.SO

    5.00

   18.042

   35.622

   382.086

   399.555

    74,0

    73.0

    23.0
Vw2-Vw,     Net Volume RTM         17.580

Vdz-Vd,     Net Volume DGM         17.469

                     Y              1.000

                   dH@             1.742
AVERAGE Y =
  ' Difference from Yearly Y =
                       0.999


                       -0.340


                       1.728
 30.00

 1.002

 1.797



 RUN 2

  1.80

  5.00

 35.622

 53.240

399.555

417.231

  74.0

  77.0

  23.0
                                        17.618

                                        17.676

                                        0.998

                                        1.721
in.Hg
      RUN 3

      1.80

      5.00

      53.240

      68,529

     417.231

     432.629

      74.0

      79.0

      20.0
                                      15.289

                                      15.398

                                      0.998

                                      1.722
                           ACCEPT
AVERAGE dH@ =

Calfulatirms

Y = (Vw » Pb * (Td + 460)) / (Vd * (Pb + (dHd /13.6)) * (Tw +460))

dH@ = 0.0317 * dHd / (Pb (Td + 460)) * (((Tw +460) * time) / Vw)"2
                                                                                         4700 Duke Drive,
                                                                                                Suite 150
                                                                                       Mason, Ohio 45040
                                                                                       Phone:(513)398-2556
                                                                                        Fax: (513)398-3342
                                                                                            www.pes.com
                            Posltcsi Dry Gas Meter Calibration Form (English Units)

-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
                           AM  "
        4700 Duke Drive.
             Suite 150
       Mason, Ohio 45040
      Phone: (513)398-2556
       Fax: (513)398-3342
          www.pes.com
Box No.:
Date;
BBBHI
DH
inHg
Vw,
Vw2
Vd,
Vd2
Tw
Td
t
13
10-16-97

Delta H
Vacuum
Initial RTM
Final RTM
Initial DGM
Final DGM
Ave, Temp RTM "F
Ave. Temp DGM °F
Time (rain.)
Bar, Press.(Pb):
Calibrated By :
| RUN 1
0.50
10
474,707
484.514
70.442
80.267
90
95
24.0


RUN 2
0.75
10
484.860
493.318
80.600
89.087
89
95
17.0
29.59
R. Kolde
RUNS
1.00
10
493,733
505.845
89.500
101 .668
89
94
21,0
in. Hg

RUN 4
1,50
10
506.082
517.191
101.900
113.061
89
95
16.0


RUNS
2.00
10
517.525
527.985
113.405
123.902
90
98
13.0


RUN 6
4.00
10
528.376
539.639
124.306
135.615
91
99
10.0
Vw2 - Vw , Net volume RTM
Vdj - Vd, Ne, volume DGM
Y
dH@
AVERAGE Y = 1 .004
Average Y Range =
AVERAGE 
-------
    PACIFIC ENVIRONMENTAL SERVICES, INC.
Box No.:

Date:

Calibrated By :

Plant:


•

DH

inHg

Vwj

Vw2

Vd,

Vd2


Tw

Td

t
      3(13)

     8-17-98

       gg

  Bethlehem Steel


 Bi

Delta H

Vacuum

Initial RTM

Final RTM

Initial DGM

Final DGM

Ave. Temp RTM °F

Ave. Temp DGM "F

Time (min.)
Bar. Press.(Ps):

Pretest Gamma:

 Pretest dH@:




   RUN1

    1.80

    5.00

   260.644

   276.031

   273.179

   288.826


    88.0
    20.0
AVERAGE Y -
                       0,990
 30.00

 1.004

 1.784




 RUN 2

 1.80

 5.00

276.031

291.405

288.826

304.526


 88.0

 96.0

 20.0
in. Hg
      RUN 3

       1.80

       5.00

     291.405

     307.125

     304.526

     320.620


       88.0


       98.0

       20.5
Vw2 - Vw,
Vd2 - Vd,


Net Volume RTM
Net Volume DGM
Y
dH@
15.387
15.647
0.990
1.742
15.374
15.700
0.989
1.739
15,720
16.094
0.990
1,741
 % Difference from Yearly Y =            -1.422


 AVERAGE dH@ =                     1.740

 Calculations

 Y = (Vw * Pb * (Td + 460)) / (Vd * (Pb -f (dHd / 13.6)) * (Tw +460))

 dH@ - 0.0317 * dHd 1 (Pb (Td + 460)) * (((Tw -f 460) • time) / Vw)'2
                                             ACCEPT
                                                                                        4700 Duke Drive,
                                                                                              Suite 150
                                                                                      Mason, Ohio 45040
                                                                                     Phone: (513)398-255(5
                                                                                      Fax: (513)398-3342
                                                                                           www.pes.com
                           Posttest Dry Gas Meter Calibration Form (English Units)

-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
        4700 Duke Drive,
              Suite ISO
       Mason, Ohio 45040
      Phone:(513)398-2556
       Fax: (513)398-3342
          www.pes.com
Box No.: 14
Date: 11-13-97
B^^M^MHI
DH Delta H
in Hg Vaccura
Vwi Initial RTM
Vwi Final RTM
Vdi Initial DGM
Vda Final DGM
Tw Ave TemP RTM "F
Td . Ave. Temp DGM °F
t Time (rain.)
Bar. Press.(Pb):
Calibrated By :
j RUN1
I
0.50
10
563.413
571.445
840.210
848.429
84
85
20.0
29.20
in. Kg



ggay
RUN 2
0.75
10
571.766
583.529
848.779
860.801
84
85
24.0
RUNS
1,00
10
583.83?
595.101
861.129
872.660
84
85
20.0
RUN 4
1.50
10
595.357
613.720
872.919
891.706
84
85
27.0
RUNS
2.00
10
638.753
646.620
917.245
925.248
75
83
10.0
RUN 6
4.00
10
614.016
638.235
892.031
916.654
84
85
22.0
Vwj - Vw, Ne, volume RTM
Vd2 - Vd, Net volume DGM
Y
dH@
AVERAGE Y = 0.979
Average Y Range =
AVERAGE dH@ 1.872
Average dH@ Range =
8.032 11.763
8.219 12.022
0.978 0.978
1.828 1.840
0.959
1.672
11.262
11.531
0.976
1.859
TO
TO
18.363 7.867 24.219
18.787 8.003 24.623
0.976 0.993 0.976
1.912 1.849 1,946
0.999
2.072
ACCEPT
ACCEPT
Calculations
Y = (Vw
dH@ =
* Pb * (Td + 460)) / (Vd * (Pb +
0.0317 * dHd / (Pb (Td + 460)) *
(dHd/ 13.6))
(((Tw +460)
* (Tw +460))
* t) / Vw)'2
       Initial Dry Gas Meter Calibration Form (English Units)
1998 Yearly Calibration

-------
    PACIFIC ENVIRONMENTAL SERVICES, INC.
                   4(14)

                  8-18-98

                    gg

               Bethlehem Steel
Box No,:

Date:

Calibrated By :

Plant:


•

DH          Delta H

in Hg         Vacuum

Vwi          Initial RTM
Vd,

Vd,


Tw

Td

t
Final RTM

Initial DOM

Final DGM

Ave. Temp RTM °F

Ave. Temp DGM °F

Time (min.)
Bar. Press.(Pb):

Pretest Gamma:

 Pretest dH@:



   RUN1

    1,80

    5,00

   165.419

   181.812

   294.100

   310.663

    72.0

    76.0

    20,0
AVERAGE Y =
                       0.992
 30.00

 0.979

 1.872



 RUN 2

 1.80

 5.00

181.812

198.880

310.663

327.945

 72.0

 78.0

 20.0
                                                   in. Hg
 RUNS

 1.80

 5.00

198.880

213.701

327.945

343.025


 72.0

 78.0

 20.0
Vw, - Vw,
Vdj - Vd,


Net Volume RTM
Net Volume DGM
Y
dH@
16.393
16.563
0.993
1.495
17.068
17.282
0.994
1.374
14.821
15.080
0.990
1.822
% Difference from Yearly Y =             1.352

AVERAGE dH@ =                     1.564

Calculations

Y = (Vw * Pb * (Td + 460)) / (Vd * {Pb + (dHd /13.6)) * (Tw +460))

dH@ = 0.0317 * dHd / (Pb (Td + 460)) * (((Tw +460) * time) / Vw)"2
                                              ACCEPT
                                                                                        4700 Duke Drive,
                                                                                              Suite 150
                                                                                      Mason, Ohio 45040
                                                                                     Phone:(513)398-2556
                                                                                      Fax: (513)398-3342
                                                                                           www.pes.com
                           Posttest Dry Gas Meter Calibration Form (English Units)

-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
                                   -5*
        4700 Duke Drive,
              Suite ISO
       Mason, Ohio 45040
      Phone:(513)398-2556
       Fax: (513)398-3342
          www.pes.com
Box No.:
Date:
BBBB
DH
inHg
Vwi
Vwj
Vd,
Vd2
Tw
Td
t
MB 15
12-29-97
•BBBBBB
Delia H
Vaccum
Initial RTM
Phial RTM
Mtial DOM
Final DGM
Ave. Temp RTM "F
Ave, Temp DGM "F
Time tmin.)
Bar. Press.(Pb):
Calibrated By :
1 RUN1
0.50
10
150.884
157.026
564.125
570.432
73
76
15.000


RUN 2
0.75
10
157.349
164.869
570.758
578.496
75
80
15.000
29.15
GGAY
RUNS
1.00
10
165.074
173.741
578.795
587.643
75
82
15.0
ULHg

RUN 4
1.50
10
173.960
184.259
587.860
598.511
76
84
15.0


RUNS
2.00
10
184.521
196.465
598.779
611.127
76
86
15.0


RUN 6
4.00
10
197.212
214.019
611.999
629.263
78
88
15.0
Vwj - Vw, Ne, volume RTM
V«t2 - Vd, Net volume DGM
Y
dH@
AVERAGE Y = 0.981
Average Y Range =
AVERAGE dH@ 1.770
Average dH@ Range =
6.142 7.520
6.307 7.738
0.978 0.979
1.719 1.720
0.961
1.570
8.667
8.84$
0.990
1.720
TO
TO
10.299 11.944 16.807
10.651 12.348 17.264
0,978 0.980 0.982
1.827 1.805 1.830
1.001
1.970
ACCEPT
ACCEPT
Calculations
Y -(Vw
dH@ =
* Pb * (Td + 460)) / (Vd * (Pb +
0.0317 * dHd / (Pb (Td + 460)) *
(dHd / 13.6))
«(Tw +460)
* (Tw +460))
*t)/Vw)'2
        Initial Dry Gas Meter Calibration Form (English Units)
1998 Yearly Calibration

-------
                 PACIFIC ENVIRONMENTAL SERVICES, INC.
Box No.:

Date:

Calibrated By ;

Plant:

•

DH

inHg

Vw,
Vd,

Vd2


Tw

Td

t
      15(5}

     8-18-98

       gg

  Bethlehem Steel


 Bi

Delta H

Vacuum

Initial RTM

Final RTM

Initial DGM

Final DGM

Ave. Temp RTM "F

Ave. Temp DGM "F

Time (min.)
Bar. Press,(Ps):

Pretest Gamma:

 Pretest dH@:



   RUN1

    1,80

    5.00

   214.453

   230.230

   608.315

   624.400


    72.0

    81.0

    20.6
AVERAGE Y =
 % Difference from Yearly Y =
AVERAGE dH@ =
                       0.994


                       1.296


                       1,728
 30.00

 0.981

 1.710



 RUN 2

 1.80

 5.00

230.230

245.365

624.400

639.854


 72.0

 84.0

 20.0
in.Hg
      RUNS

      1.80

      5.00

     245.365

     260.368

     639.854

     655.294


      73.0

      86.0

      20.0
Vw2 - Vw,
Vd2 - Vdi


Net Volume RTM
Net Volume DGM
Y
dH@
15.777
16.085
0.993
1.696
15.135
15.454
0.997
1.728
15.003
15.440
0.991
1.759
                          ACCEPT
                                                                          4700 Duke Drive,
                                                                                Suite 150
                                                                         Mason, Ohio 45040
                                                                        Phone:(513)398-2556
                                                                         Fax: (513)398-3342
                                                                             www.pes.com
 Y = (Vw * Pb * (Td + 460)) / (Vd * (Pb + (dHd /13.6)) * CTw +460))

 dH@ = 0.0317 * dHd / (Pb CTd + 460)) * (((Tw +460) * time) / Vw)"2
                           Posttest Dry Gas Meter Calibration Form (English Units)
                                                                                9/18/98

-------
PACIFIC ENVIRONMENTAL SERVICES, INC.
                                                        4700 Duke Drive,
                                                              Suite 150
                                                       Mason, Ohio 45040
                                                      Phone:(513)398-255fi
                                                       Fax: (513)398-3342
                                                          www.pes.com
Box No.:
Date:

DH
inHg
Vw,
VW2
Vd,
Vdj
Tw
Td
t
RMB-13
10-17-97
msaammm
Delta H
Vacuum
Initial RTM
Final RTM
Initial DOM
Final DGM
Ave. Temp RTM "F
Ave. Temp DGM "F
Time (min.)
Bar. Press.(Pb):
Calibrated By :
RUN 1
0.50
10
669.271
680.326
23.196
34.289
68.500
73.000
27.000
29.50
R.Kolde
RUN 2 RUN 3
0.75 1.00
to 10
680.835 691.078
690.745 701.245
34.797 45.097
44.775 55.330
67.500 67.000
73.500 75.000
20.000 18.0
in. Kg

RUN 4 RUN 5 RUN 6
1.50 2.00 4.00
10 10 10
701. 61B 713,486 724.113
713.109 723.578 735.099
55.700 67.635 73.300
67.254 77.774 89.309
67.000 67.500 63.500
75.500 76.500 78.000
17.0 13.0 10.0
Vw3 - Vw, Ne, volume RTM
Vd2 - Yd, Net volume DGM
Y
dH@
AVERAGE Y= 1.005
Average Y Range =
AVERAGE dH@ = 1.778
Average dH@ Range =
11.055 9.910 10.167 11.491 10.092 10.986
11.093 9.978 10.233 11.554 10.139 11.009
1.004 1.003 1.006 1.007 1.007 1.006
1.680 1.712 1.748 1.830 1.850 1.849
0.985 TO 1.025
1.578 TO 1.978
ACCEPT
ACCEPT
Calculations
Y = (Vw
dH@ =
* Pb * (Td -I- 460)) / (Vd * (Pb + (dHd / 13.6)) * (Tw +460))
0.0317 * dHd / (Pb (Td + 460)) * (((Tw +460) » t) 1 Vw)'2
Initial Dry Gas Meter Calibration Form (English Units)
                                                        1998 Yearly Calibration

-------
                 PACIFIC ENVIRONMENTAL SERVICES, INC.
Box No.:

Date:

Calibrated By :

Plant:


•

DH

inHg

Vw,
Vd,

Vdz


Tw

Td

t
                6(Rmbl3)

                  8-18-98

                    gg

               Bethlehem Steel


              •1

            Delta H

            Vacuum

            Initial RTM

            Final RTM

            Initial DGM

            Final DOM

            Ave. Temp RTM °F

            Ave. Temp DGM °F

            Time (min.)
Bar. Press,(Ps):

Pretest Gamma:

 Pretest dH@:



   RUN1

    1.80

    5.00

   105.106

   120.425

   749.253

   764.233


    70.0

    78.0

    20.0
 AVERAGE Y =


 % Difference from Yearly Y =

 AVERAGE dH® =
 30.00

 1.005

 1,778



 RUN 2

 1.80

 5.00

120.425

135.120

764.233

779.232


 70.0

 78.0

 20.0
                                    1.005


                                    -0.024


                                    1.793

Calculations

Y = (Vw • Pb • (Td + 460)) / (Vd * (Pb + (dHd / 13.6)) * CTw 4-460))

dH@ = 0.0317 * dHd / (Pb (Td + 460)) * (((Tw +460) * time) / Vw)"2
in.Hg
      RUN 3

       1.80

       5.00

     135.120

     149.771

     779.232

     794.234


       71.0

       81.0

       20.0
Vw2 - Vw,
Vdj - Vd,


Net Volume RTM
Net Volume DGM
Y
dH@
15.319
14.980
1.034
1.693
14,695
14.999
0.990
1.840
14.651
15.002
0.991
1.847
                           ACCEPT
                                                                                        4700 Duke Drive,
                                                                                               Suite ISO
                                                                                       Mason, Ohio 45040
                                                                                      Pfaone:(513)39S-Z556
                                                                                       Fax: (513)398-3342
                                                                                           www.pes.com
                            Posttest Dry Gas Meter Calibration Form (English Units)

-------
11/12/98   07:15
©5134896619
                                             FES CINCINNATI
                                                              •+-»-» UUKH&Jft
                   Pacific Environmental Services VOST Box Calibration
Date: 11 19-93
Vost Box Number: V- 1


Bubble Meter
1012 1007
1010 1007
1010 1008
1009

Average: 1009.00



Bubble Meter
1008 1010
1010 1009
101 1 1007
1003

Average: 1008.29



1009 1005
1008 1003
1006 1005
1008

Average: 1006.29


Flow Rate: 1.0 1/min
Rotameter Setting;
Bubble Meter Temp. :
Runl

Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Y=
Run 2

Initial Volume
Final Volume
Initial Temp.
Final Temp,
Average Temp,
Time:
QDGM=
VTu,
Run 3
Initial Volume
Final Volume
Initial Temp,
Final Temp.
Average Temp.
Time:
QDGM=
Y_
,

1.08
91

Meter Box
9S29
9855
104
104
101
26.25
972.821
1.0372

Meter Box
9855.5
93 SI. 5
104
103
103.5
26,25
968.505
1.0411

9882
9908
104
103
103.5
26.26
968,1358553
1.0394
                                                   Average Y=
                                                  1.0392

-------
11/12/98   07:18
05134896619
                    Pacific Environmental Services VOST Box Calibration
                                            Flow Rate:
                                          1,01/min
Vosi Box Number:


Bubble Meter
1005
1007
1007


Average:



Bubble Meter
1007
1006
1006


Average;



1005
1004
1003


Average:


V-2



1007
1009
1012
1008

1007,86




1008
1009
1010
1012

1008.29



1003
1002
1004
1005

1003.71


Rotameier Setting:
Bubble Meter Temp. :
Run 1

Initial Volume
Final Volume
Initial Temp.
Final Temp,
Average Temp,
Time:
QDGM=
Y=
Run 2
•
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp.
Time:
QDGM=
Y=
Run 3
Initial Volume
Final Volume
Initial Temp.
Final Temp.
Average Temp,
Time;
QDGM=
Y-
0.95
91

Meter Box
8883,5
8903.5
105
104
104.5
18,49
" 1055.798
0.9546

Meter Box
8903.5
8923.5
105
105
105
18.5
1054.293
0.9564

8924
8944
105
105
105
18.6
1048,624988
0.9572
                                                    Average Y=
                                                   0.9560

-------
   PACIFIC  ENVIRONMEKTAL SERVICES. INC.
                                                                                 Central Park West
                                                            5001 South Miami Boulevard, P.O. Box 12077
                                                       Research Triangte Park, North Carolina 27709-2077
                                                                  (919)941-0333 FAX: (919) 941-0234
                          Posttest Dry Gas Meter Calibration Form (English Unite)
Pretest Calibration Factor
System Vacuum Setting, (in Hg)
Reference Meter Correction Factor
Date:    ^'\^-°ci P.*,fnHg
                           Calibrator.   J> \r>
                                 Meter Box No.
      AH
     1.8
   Trial
Duration
 (min)
          Pio6
                       Initial
                       0,0
Final
(ft3)
                       _  Dry
Net
(ft3)
Initial, Inlet
 -=m~-
-MB
J&gJulet-
       T
                                                                               1-b-l
-PfflalrOuMet
                        ffl-
                                                                                CV

Trial
1
2
3
feo<"

ji y
Ayg.
C C/'H i W
— fF)
<\^v»
H^H
n^>5
Meter Box
Correction
Factor
Y
#DIV/01
#DIV/Ot
#DIV/OI
Reference
Orifice Press
AH9
(in. H2O)
#DIV/01
#DIV/01
#DIV/OI
             fpr-
                                                                                                                        v
                                                                                                                         D
                                                                                      lu
                                                                                                            L'"C
                                                                                                            i ,001
master.xls
                                            Posttest
                                                                                8/22/97

-------
                                      LU
Bethlehem Steel Corporation
Coke Oven Emission Test
Chesterton, Indiana
                                  u
Date
»  1998
                                                                 1 of 2
Quality Control Check
Prior to Start of Tests
Ifmmn all r>tMnuiwi otMMUfHUPi *f+\f*l tmtll train flVVMTitilir

Assemble (tains in dust free environment
Visually inspect each train fiar proper assembly


•^ifrtrtf ittn mnm^r •mmninHf fiiULZJfl fltXB

Visually inspect ^fiypitng nozadc for chips
Visually inspect Typo SPitottnbe
Leak check each leg of Type SPitot tube

I^ntr f*hiM*ip Anting mmiiiilig ti'itiii

During Testing

trwciso point
... ,,,_, ^j^ ^ ,
datasheets
Unusual occurrences noted in test tog
Properly mamtain the roll and pitch of axis of Type S
1 O
Leak check train before and after any component
changes during test
Mft'PfBI ^f pt'tt^te ami finer teinpftf mine
**•*,-• • • unrtH-lMtti nHTTinintfl- ' '



accuracy
Data sheets reviewed by •Prf'daily during testing
Observation

Qowe
P« we
Dow«
iDense
0 to /vi ^*
po ^e
O 6 HJ^f
6 o*oe
O e «J e

cl5*'
ir .
•w*
AJ/A
Deioe
Do-f
C^r
^,
-Ko

-------
Date
Page
        ,  1998
2 of 2
Quality Control Cheek
After Testing
Visually inspect sampling nozzle
Visually inspect Type SPitot tube
Leak check each leg of me Type SPitot tube


Record observations if any
Field Log
Project name/ID and location
Sampling personnel (names/position)

Geological observations including map


Simple destiiptions
Description of QC samples
Deviations from QAPP
Difficulties in sampling or unusual conditions
Sample Labels
Sample ID
Date and time of collection
I ah tHrhnioan initials

Analytical parameter
Preservative required

UDservRuon

C^Lov(_»_
JUv^W
cLuv>--*~
cLtfM_A«.
^^

. \ * / ft
ft*4"h{«kA*wi j tct,l v- Mej^TfH \ *JC\
S*-|\^ pcj^ ^tLJuL
SAiLj[hM.U Lw^eJf^J


)iM
VwtK
L

-------
Bethlehem Steel Corporation
Coke Oven Emission Test
Chesterton, Indiana
                               /3 ft.'-in
Pag
1 of 5
I. Teat Run Observations Date
R * Recommended
M » Mandatory
1. Train set up • filter ED
filter weight
filter checked for holes
filter centered
	 • • aoszle" clean'
nozzle 'undamaged
nozzle diameter 
nnai _'_ positive* line \MJ
on manometer for
(15 sec. J negative- line* \1)
	 pxtot* tube* undamaged- • •
M-3 bag initial leak cheek (M)
Tedlar bag: Should hold 2 to 4 in. H^
oressore- for- 10 minutes1 or* 	
zero flow meter reading on
continuous evacuation* or-
Compie'ceiy fill bag and let
stand overnight — no deflation.
<$
Test
Run
1
*>A
Kit A
\s*
t^
iS
t/
,^1^
ts^
\^
•^
• IS'
• -i^ •
• iS • •
yf. . . ,
' L^*** * "
• \^S '
.J/A ,

•*fc*4
iUW^"
/^ */^f '
j-^05/ 1
1 &>9£flL

\
\
\
- 6A5-
/4^V%
^& d^
fi.ft ff4:i
y i
r^ "'f
„ •
/"J <3A
•^iti' 1
'**&cj '
\J
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VJL99C
2  of 5
Date
R " Recommended
M - Mandatory

4. M-3 sampling train check:
initial \M/
(should hold
10 in. vacuum tlnal IMJ 	
for- 1/2' min. ) 	 	 • 	
jPu'ree sample train- with' stack1 gas 	
• Constant rate sampling- 	 1- par 	

. Txme- test scartea - • 	 - -
• Time tear ended 	
6. Dry zas (' * )' port' initial 	 ;
meter ...... f £5^1- 	
volume: ("'•)• port* initial 	 : •
	 final 	
( • }• port- initial 	
• • • final 	
< • 3 • port initial 	
	 final- 	
7. Train operation Nozzle changed
during run during run —
. 11— 	 HOT ALLOWED
pitch- and- yaw of- probe- ow k-. 	 • 	
nozzle- not acraped* on' nipple 	
effective- seal- around- probe 	
probe moved' at* proper* time • 	
probe- .heated* • 	 • • • •
calculator constants or nomograph
changed when TS and /or TH
changes' significantly ...
average time to aet
isokenetica after probe
moved' to* next* point 	 •• 	 • • •
Average values:
inpinger temperature
should DBS 70 F 	
Poac filter gas streamer or
Filter box temperjttu-re-- .^
*5P" Circle one 	
stack* temueratare- • ........
barometric' P taken* and' value •
waa probe ever disconnected
from filter holder while in
stack?
was filter chaneed during run?
f-/a-n
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-------
Page
       3  of
Date
R " Recommended
M - Mandatory

Check on filter holder loosening of
clamping device bolder
was silica gel changed
during run? • •
was any part3.cu.late loot?
Accurate Ap
reading of* AH • ... .
meter temperat*are 	 	 	
stack' temperature 	
meter* vacuum* 	 • •
-j/ t •"»"•»• per- point 	
impinge r- tenuBeratore 	 * 	
iiiter* box tefflperature 	
•^Minimum sample time of * * • •$/' min met
^-Minimum sample volume of *.'*/''_ dacf collected

8. Post teat: -• All- openines- sealed 	
- recovery area* clean- sheltered 	
-- filter handled- with- glovesv forceps- • •
£"petri' dish sealed, labeled 	
- anv' sample lost 	 •
grad eyl.
weighed
water* measured* • mL • • gmB 	
- silica- gel- weighed-,- tier *-*ms- ••••-- • •
" condition •• color* - - /*/fi*|*/>sj *">*'?* * • • • •
	 • 	 *• spent* 	 • 	
- probe' cooled- suf f ieientiy * 	
- noszie' removed* and- brushed 	 	
- probe brushed $• times 	
- nozzle1 brushes- clean 	
- wash bottles clean* 	 	 	
- acetone clean 	 • 	
— M-8 15" minute- surge • • • 	
. ,% - wacer/solucion clean 	
j^r\\i.,,..Cv»i*ui-- - blank "taken: acetone-, water; other*
Ql^ Probe brush and extension clean-, '
Samuie container:* Clean
Canped*
Laoeied
4 Sealed 	
' ' Liauid- level- marked' • •
M«
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                                        Page   4 of
/







Q
Date
R » Recomnended
M - Mandatory
.
9. Post test Orsat Analysis of Initial (Ml
integrated bag sample orsat
analyzer - Analyser leak check
(levels should not fall below Final (M)
cap. tubing and not more than
0.2 ml.- in- barrette for 2" rain-. J
Orsat- samples-: • Each bag anaivzed- 3- tines-
Z CO? agrees- within" Oi2f 	
£'• Qp agrees- within 0-.2I 	
Z- CO- ajgrees- within- 0-.2X 	
Analysis at end of teat. Orsat analyzer
checked against air \zo.y *• Oi3J 	
Qrsat Analysis:
— *fo*_
OjjX- 	 • • • • - fi-&
coi 	
Fo - ZQ-.9- -X-0?'
% GO? 	
Fuel 	 • 	
grange- for- fuel
Orsat- analysis* valid
Orsat solutions changed
when calculated Fo
exceeds fuel type- range-
10. All saraoles locked up
All sampling- coanonents- clean- and* sealed- • •
j£ All data- sheets submitted to- observer* **£
- Orsat 	 • 	 	
- Run- isokenetic- - - Team/Observer- 	
• • - Particoiate- recovery 	
1C, - Process- data- • •••••• -^ 	
• - Charts 	
• -• Calibration sheets 	 • • 	
JP'frft
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-------
                                                               Page
                                                                      5 of 5
J.   NOTES:   Care should be taken, when sampling for organic compounds, to
     follow  stringent quality control  guidelines to avoid contamination of the
     sample  and sampling train.   Take  note of any occurences which could bias
     Che sample in any manner.

     Include:  (1) General comments;  (2) Changes to pretest agreement with
     justification; (3) Identify (manufacturer) and describe condition of
     sampling equipment; (4) any abnormal occurrences during test program.
     (Additional page(s) attached:   Yes   •  , Mo  */•___•)
,ces <
iS'.
£L»;, tlLLJL I
  Signature of Observer           Affiliation of Observer          Dace

-------
                                       0

                                      SL
Bethlehem Steel Corporation
Coke Oven Emission Test
Chesterton, Indiana
   flJfc.sU
            Date    "Jtt±?*   » 1998
             Page    1 of 2
Quality Control Check
Prior to Start of Tests
Keep all cleaned glassware sealed until train assembly
Assemble trains in (but free environment
Visually inspect each train for proper assembly

Level and zero manomeier


Viennlhs munetst fmrmlma nrrrrle fijr COIDS

Visually inspect Type SPitot tube
Leak check each leg of Type SPitot tube
T Mrif rfirvir jPiiiiiB VBiHilfntit ttttin

During Testing


tTAVdsc point

OfflBptt Q2Q1 ADA Qj-Krli Iml v18* IIRAMUKU On pTCXOilUlillCu.
Q&tft jfff^rCEt
Unusual occurrences noted in test log
Property mamtam d^ roll and pitch of axis of Type S

, _, ^
Leak check train before and after any component
changes during test


	 	 . A . . . .

exit tetnperaeure

accuracy
Data sheets reviewed by PM daily during testing
Observation

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-------
Date    JUJL? "   » 1998
Page   2 of 2
Quality Control Check
After Testing
Visually inspect sampling nozzle

Visually inspect Type SPitot tube
Leak check each leg of 1he Type S Phot tube

Leak check tin entire amtiptiag tram
Record observations if any
Field Log
Project name/ID and location

Sampling personnel (names/position)
Geological observations including T"np


Sample ufisct iptions

Description of QC samples
rv_u.ih'j»_ f 	 f*>ADD
LJevianons cram vjArr
Difficuldes in sampling or unusual conditions
Sample Labels
Sample ID
Date and time of collection
I *jb f^^|n'r>'fin Initials

Analytical parameter
Preservative required
Observation

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-------
Bethlehem Steel Corporation
Coke Oven Emission Test
Chesterton, Indiana
Pa8«   1 of 5
I. Teat Run Observations Date
R - Re co-amended
H " Mandatory
...
1. Train set-up- * filter ID
filter might
filter checked for holes
filter centered
	 * • nozzle' clean' • • • • -
nozzle • undamaged
nozzle diameter (inii
probe liner clean
probe markings correct
probe heated along
entire- length 	
	 inpmgers- charged 	
	 lapTuftgers- iced 	 • • • •
	 meter- box leveled 	
•••••• • • 	 	 pitot manometer' zeroed4 • • • • •
	 on.x3.ce- manometer* zeroed 	
	 • 	 f liter* boar or* holder- at- temp*.
all ball joints lightly
greased
• 	 all" openings- canoed- • • • • •
2. Train leak check LC' *
at nozzle: initial' {R-J- • • VAC 	

v'iw* cm i£ ij LW' * * ' * *
in. Hz initial, intermediate (R) VAC •
Intermediate and LC
final at highest intermediate (R) VAC
Vacuum during LC
test run.) intermediate (R) VAC
final Ul) LC
VAC |
3. Pitot lines leak initial positive line (R)
check: negative- line (R)' * '
thold 3 in. H2O> 	 " 	 " 	 	
nnai positive line \MJ
on manometer for
(15 sec. ) 	 nejmtxv*** line- (&•}•
	 picof tnbst* unttamaged* • •
M-3 bag initial leak check (H)
Tedlar bag: Should hold 2 to 4 in. HjO
pressure' for* 10'Tnirrates' or" 	
zero flow meter reading on
continuous evacuation- or-
Completely till bag and let
stand overnight—- no deflation.

«-(Wk
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Run
1

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-------
2 of f
Date
R « Recomoended
M « Mandatory

4. M-3 sampling train check:
initial \wj
(should hold
10 in* vacuum zinai \n/ 	 • 	
for- 1/2- min. )• 	 	
Puree sample train- with* stack* gas 	
Constant- rate- sampling 	 1* psr ••••••
5. Time- test* started* 	
- Time test ended 	
6. Dry gas C* * )* port* initial* 	
meter 	 final 	
volume: (*•*•)• port* initial* • * * • *
• * 	 final 	
1 • •)• port- initial 	 *
'• -final 	 - 	
{• " jjjorr initial 	 • * • * 	
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-------
Page
       3  of
Date
R * Recommended
H - Mandatory

Check on filter holder loosening of
clamping device holder
was silica gel changed
daring run? *
was any part xeu late lost? ' • •
Accurate Ap ' * •
reading of" aH " ..... .
meter temperature- • * • • • .-••*.•
stack temperature- 	
meter* vacuum* - 	 	
_fa£ time- pear point - * 	
* uepinger- temoerature 	
illiter- biox tewoerature 	 	
•^Minimum sample time o£ • • • V* • min met
^Minimum sample volume of •/ • • dscf collected

8. Post teat: -• &|i^O8cninfs* sealed 	 *
- recovery area- clean* sheltered 	
-• filter hand led- with* gloves*,' forceps* •
-petti- dish sealed, labeled* 	
- any sample lost*
grad cyl.
weighed
water* measured* * at, * * gins 	
- silica gel* weighed-, net- BBS- ••••••
- condition - color* - * '/&•#}& 4±f 	
	 £'• spent" 	 -* 	
- probe- cooled* sufficiently 	
- nozzle- removed- and- brushed 	
- probe brushed 6- times 	
- nozzle- brushes* clean* 	 * 	
- wash bottles clean 	
- acetone clean- • 	
- M~I 15' minute- purse • * * * 	
J*L t 1 /if \ - water/solution clean- 	 '
|*Ll*L|L^ L W^nteL - blank taken.* acetone*.'* water*. ' other*
3 Probe brush* and extension clean; *
Samoie container:* Clean
Capped*
Labeled
Sealed 	
Liouid* level* marked*
frJ-K
Test
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-------
Page
                                                                                           4 of
Date
R =• Reconnended
H • Mandatory

9. Post test Orsac Analysis of Initial (MJ
integrated bag sample Qrsat
analyzer - Analyzer leak check
(levels should not fall below Final (Mf
cap. tubing and not more than
0.2 mL in1 bur re tte for 2 -rain'. ) 	
Orsat samples: Each bar analyzed* 3- times-
2- C0«j agrees- vithin- OvlSK 	
£• 5y- agrees- within 0.2X 	
jr. £0. ag'rees- within- Q-.2X 	
Analysis at end of test. Orsat analyzer
checked against air* (20i9- *•• Ch3) 	 •
Orsat Analysis:
CD?*
2?x 	 • 	
coz 	
Fo » 20; §• — Z- Ojj
* CQ

'AJ "ft- ' t A f$ l'r "• ' Ai'fti rt/ft A)/r „/, UA» '<\LtJ ' w^ ^C£ca "^£LA': 'W1*? ' . *p-f^ •JO/A- • ^^ ' A+*t Test Run 2 jft^yr-j <&LK: J "~~r<. VfA' ' ' yCe/) ' " %€i? " • XJy/T" . 1 JL A /\. Tt^U »6jf 0 dQ,ff/to $*/^ ' IA t^) 1 p\ fif/fy ' Ju/'tf' ylA//r */4 M-8^ ' ' ^^ -: w%a" I* ' tfici* • - • •I7pu" "F¥" • wk- " jO/fl~ ' '~y%5' ' " Test Run 3 , . . . . . ! 1 t Test Run 4 • • . . ' . . . . . Q O c»-v—'te^ .


-------
                                                                Page
                                                                      5 of 5
   NOTES:  Care should be taken, when sampling for organic  compounds,  Co
   follow stringent quality control guidelines to avoid contamination  of  the
   sample and sampling train.  Take note of any occurences  which could bias
   the sample in any manner.

   Include: (1) General comments; (2) Changes to pretest agreement with
   justification; (3) Identify (manufacturer) and describe  condition of
   sampling equipment; (4) any abnormal occurrences during  test program.
   (Additional page(s) attached:  Yes '•'  . No  V .)
                                                                 p -
S ignature of Obs erv«r            Affiliation of Observer          Date

-------
Bethlehem. Steel Corporation
Coke Oven Emission Test
Chesterton, Indiana
                                      A-/4
                                       J
                        as/,
          Date
          Page
1998
                                                                1 of 2
Quality Control Check
Prior to Start of Tests
Vf-n nil j-tMnwui ohuMnniiB Denied until train n*c*mklw
ivccp BU cionicu gmawoie amu*** uwtu Uiiiu usscmDIy
Assemble trains in dost fiee environment
Visually inspect each train for proper assembly
LflVfll and TBTO ypmimnetef
•
CTsIculnte prnpcr iwrnpif'iR nozzle size

. i- i f tr

Visually inspect Type SPitot tube
Leak cneck each leg of Type SPftot tube

I rCflk check entire sjnnpling train

During Testing


UaVdaO pOUll
r- i j j i i • • J *
datasheets
Unusual occurrences noted in test log
Properly maintain the roll and piteh of axis of TypeS
Pilots and sampling nozzle

Leak check train before and after any component
changes during test
Maintam me probe and fitter temperature
Maintain ice in ice water bath and maintain impinger
exit temiKratiirc

f*!iiiftrntinfi ^nnnc reviewed for comnletefievi Juirf
accuracy
Data sheets reviewed byJ^daUy during testing
Observation


/?
£/ 8 /w

v<* -T^. •^^6 •••»4-e-a 0^ I CMl*Ml. <3L


-------
                                                            Date
                                                            Page
                      , 1998
               2 of 2
Quality ContrDl Check
After Testing
UimaSftf •naiiM't mtrnflltfllT fifVJTfe

VisuaUy inspect Type SPitot tube
Leak check each leg of the Type SPitot tube



K£COTQ oDscrvonons u any
Field Log
Project name/ID and location


G0ok)gic&i obsetv&tioHS including xnBp


Sample descriptions

Desuipuuu of QC samples
Deviations from QAPP
Difficulties in sampling or unusual conditions
• ~
Sample Labels
Sample ID
Date and time of collection
TL*>\ J
0
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-------
Bethlehem Steel Corporation
Coke Oven Emission Test
Chesterton,  Indiana
1 of 5
I. Test Run Observations Date
R « Recoranended
H - Mandatory
1. Train aef op- " filter ID
filter weight
filter checked for holes
filter centered
• nozzle clean
nozzle 'undamaged
nozzle diameter (inij
probe Liner clean
probe markings correct
probe heated along
entire- length* • • • •
	 inpingers* charted*
• • 	 impingers- iced 	 • * *
	 meter* box leveled* * • * ~ ' *
• • • • • 	 pitot manometer' zeroed 	
• • • 	 orifice* manometer* zeroed* * - • -
	 •-••••• • • filter- boar or- holder* at* teis-r.
all ball joints lightly
	 	 greased • • • 	 	 •
	 all1 openings* capped- • • • • •
Z. Train leak check LC 	
at nozzle: initial  	 VAC 	
KQPZ cfm 1 15 LC 	 j
in. Hg initial, intermediate (R) VAC
Intermediate and LC 	
final at highest intermediate (R) VAC
Vacuum during LC
test run.} intermediate (R) VAC
Final 
-------
                                                           , 199C



                                                           2 of 5
Date
R • Recoaoended
H » Mandatory

4. M-3 sampling train check:
j~2~tl2* V W /
(should hold
LO in. vacuum final* \a,J • 	
for 1/2- min. ) 	
Puree sampie train- with* stack* ESS 	 * *
• • Constant' rate sampling 	 1* pmr 	
5. Time- test- started 	 .......
• Time test* ended 	 * 	
6. Dry gas (* • •)• port* initial* ••••••••
meter ...... fimi 	
volume: (• * * ')jJJ2£t* initial' 	 :•* *
	 final 	
I • )• port* initial* " * 	
• • • * final 	
( • J * port initial 	 "
	 • 	 final 	
7. Train operation Nozzle changed
during run during run. —
	 HOT &LLUNC0 	
pitch* and* yaw of- probe- ovk*. 	
nozzle* not scratoed* on* nipple 	
effective* seal* around- probe 	
probe moved* at* jarooer* time 	
probe .heated* ' * • * 	 • • • • • •
calculator constants or nomograph
changed when TS and /or TM
changes- significantly-
average time Co set
isokenetics after probe
moved* to* next* point 	 * 	
Average values:
impinger temperature
should be s 70 r 	
Post filter gas streamer or
Filter box temper^Jttnrw!8***-«'w
r circle one 	 * *
*****
Test
Run
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stack* temperature*
-1 153"
barometric- P taken* and* value
was probe ever disconnected
from filter holder while in
stack?
was filter ehanj-ced during run I
39. *7 \ *39.^
/U 0
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-
1
	 	 i

-------
                                                                      , 195



                                                                      3 of :
Date
R - Recommended
M « Mandatory

Check on filter holder loosening of
clamping device holder
was silica gel changed
during run?
was any part icul ate lost?
Accurate AP Ais***ui 5k $+ /# ' $*0 "
reading of* AH #•««•% flw* 0**^*^ ffhu&nst^
meter temperature 	 	 	
stack temperature 	
meter- vacuum- 	
tine' per* point 	
impinger' teaoeratare 	
filter- box temperature 	 	
Minimum sample time of ' • ' y^ .nin met
Minimum sample volume of ^ ' y* " dscf collected

8. Post test: — Ail- openings- sealed 	
- recovery- area- clean* sheltered 	 	
- filter handled- with- gloves*,* forceps-
_ gpJUJ. dish sealed, labeled 	
- anv* sample lost 	
grad cyi,
weighed
water- measured* tnL • • gnat 	
- silica gel* weighed", * ner gas- 	
- condition - coior-^-fcj •nCt^*** 	
.... -j gpent* •••••"-•••--••-
- probe* cooled* sufficiently 	
- nozzle removed- and- brushed 	
-jjtrohe brushed- 6* times • • • 	
- nozzle* brushes- clean 	
- vas'h bottles clean* * *
- acetone clean 	 - 	 * 	 ••
— Mro 15' minute' ourge 	
. - water^solution clean- * • * 	
Lu«,LUit/i*cS* - blank taken: acetone; water*, other-
Probe brush' and extension clean; *
Sample container* Clean
Capped*
Labeled
Sealed 	 • ' "
Li-mid- level* marked* •
t-a-18
Test
Run
1
•
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-------
  Page
                            4 of
Date
R « Reeonnended
M " Mandatory

9. Post test Orsat Analysis o£ Initial (M*
integrated bag sample Orsat
analyzer - Analyzer leak check
(levels should not fall below Final (M) •
cap. tubing and not more than
• 2 mL xtt ourrecce ror i. tain.; 	
Orsaf saopieat Each bar analyzed 3' tines-
I' CO-» afrees* within- 0*.2! 	
X- 0? agrees"- within 0*.2X 	
Z- CD- agrees- within- 0;2X 	
Analysis at end of test. Orsat analyser
checked against air- (20-.9- *• 0-.3) 	
Orsat Analysis:
•9ifo_
9-52- 	
C01- •" 	
Fo » Z0i§- -• S 6V
• X GO* 	
Fuel 	
Fftrange- for- fuel
Orsaf analysis' valid'
Or sac solutions changed
when calculated Fo
exceeds fue 1 • type • range •
LO. All satnoies locked up
Ml samoiing- components* clean- and- sealed
-V Ail data- sheets submitted to- observer- 	
f^ - Orsat 	 • 	 	
- Run- isofcenetic- • • Team/Observer 	
• • - particuiate1 recovery • • • - • 	
_*. - Process1 data 	
-• Charts 	
• -• Calibration sheets 	 • 	
SO*
Test
Run
I
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-------
                                                                 Page
                                                                        5 of 5
J.   NOTES:  Care should be taken,  when sampling for organic compounds,  Co
     follow stringent quality control guidelines to avoid contamination  of  the
     sample and sampling train.   Take note of any oceurencea which could bias
     the sample in any manner.

     Include: (1) General comments; (2) Changes to pretest  agreement with
     justification; (3) Identify (manufacturer) and describe condition of
     sampling equipment; (4) any ajrgcmnai oceurrenc§£>during test program.
     (Additional pageCs) attached:   Yes • ••  . No
                                                         J.    SLc
  Signature of Observer
Affiliation of Observer
Date

-------
Bethlehem Steel Corporation
Coke Oven Emission Test
Chesterton, Indiana
                                 R
                                         * T
                 1998
Page
                                                                 1 of 2
Quality Control Check
Prior to Start of Testa
K>*n all elMnwd phtMcwne sealed until train assentfelv

Assemble traina in dnst flee environment
Visually inspect each train for proper assembly
Level and zero manometer



Vfanallu imnpjit mnmthur nnrrfft for chins

VTsuaUy inspect Type SPitot tube
Leak check each leg of Type SPitot tube



During Testing


U&V£iMpOilil

aampie oaDi ano caicuiauuua i^vmusu uu piciorimmeu
data sheets



Pitots and sampltDg noole
1 .writ chffdr train h*^orp mid pfter any component
... . r
cuaugea ouiiiig test




exK icmpu&uire
f^aKI'iral i nti fiitim iwvieimKi for CtliimlcfiCtli^^t smit
accuracy
Data sheets reviewed by PM daily during testing
Observation
'
dUcSTSJ^1
<3 6«o^,
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4«o^ (fy~3lf , 2Jk,J ( /^f*"^»^y/? > JlZ
oU^
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OLtfvi^

Ofr^AJf
^W .
^/
A3 /A
^

-------
         Date
         Page
2 of 2
Quality Control Check
After Testing
Visually inspect sampling nozzle
Visually inspect Type SPitot tube
Leak check each leg of the Type SPitot tube


Record obscrvzitions if any
Field Log
Project name/ID and location
Sampling personnel (names/position)

Geological observations including map
Sample ran tones and dates
Sample dejSCsniiJtiOQS

uescripuon 01 vjv* samples
Deviations from QAPF
Difficulties in sampling or unusual conditions

Sample Labels
Sample ID
Date and time of collection
l^teefam-cian SiiMab

Analytical parameter

Preservative ie<^uueQ.
Observation
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-------
   Bethlehem Steel Corporation
   Coke Oven Emission Test
   Chesterton, Indiana
                                ,     .
                            &?f#t"*X  G
                                >fu »u X
                                                             Pa8«
of 5
     Teat Bun Observations

     R - Recoanended
     H - Mandatory
                                        Date
     Train, set' or " filter ID
                                         /J/|
                    filter weight
                     ilter checked for holes
                    filter centered
                    nozzle- clean-
                    nozzle* undamaged
                    nozzle diameter (in;)
                    probe liner clean
                    probe markings correct
                    probe heated along
                    entire1 length .....
                    impingers- charged
                    impidgers- iced-
                    meter- box leveled
                    pitot manometer1 zeroed'
                    orifice- manometer- zeroed
                                              •  '*XM
                    filter- boar or* holder- at* teimr.
               all ball joints lightly
               greased ••  •	
                                                          *)/&'
                    a 11' openings- capped
                                                      "**3
2.
                 initial-
                                  LC* *
                                       VAC-
                                       LC-
                      intermediate (R) VAC
Train leak check
ac nozzle:
(
-------
/
Date
R • Recommended
M - Mandatory

4. M-3 sampling train check:
initial \MV 	 ......
(should hold
10 in. vacuum final* (M) 	
for- i/2* -Bin. ) 	 • 	
Purge sample train- with- stack* gas 	
• • Constant rate- sampling 	 1' pur 	
5. Time- test- started- •• • • • •• 	
• Time test' ended 	 	
6. Dry eas (• • )• port' initial 	 • 	
meter ...... ff^^ 	 -
volume: ("*}• port' Initial- •••' • :•• •
	 final 	
C }• port' initial 	 •
• • ' final 	 • 	
( • ) • port initial 	
	 final 	 * • *
7. Train operation Nozzle changed
during run during run -

pitch- and- yaw of- probe* o.kv 	
nozzle- not s craned- on- nipple* •••••••••- 	
effective- seal* around- probe 	 • 	
probe moved- af proper- time 	
prone" '.heated* • • 	 • • • • • •
calculator constants or nomograph
changed when TS and /or TM
changes- significantly-
average time to set
isokenetics after probe
moved' to* next" point 	
Average values:
impinger temperature
should* be < 7Q r 	 • 	
Post filter gas streamer or

^mmmmml'- Circle One
stack" temoeratnre- • 	
barometric- P taken- and- value
was probe ever disconnected
from filter holder while in
stack?
was filter chantzed during run!
S,3.f
Test
Run
1

-------
3 of ;
Dace
R *" Recommended
M « Mandatory

deck on filter holder loosening of
clamping device holder
was silica gel changed
during run?
was any partieulate lostf * ' '
Accurate 4P $**$ •?$ ffj st* #*•&
reeding of" AH /$tro. Pitta OA*H*M* ^utOuA*. *
meter temperature 	 ....
stack' temperature- * - * 	
meter- vacuum* 	
•4k time- per* point 	 * 	
inminger- temperature 	
filter* box tenoerature 	 	
Minimum sample time of ^^^ ain met
Minimum sample volume ox ^^^ decf collected

8. lose teat: — All* openings- sealed- 	
- recovery* area- clean* sheltered- ••••••••
- filter handled- with- ztovesv forceps- • •
- petri dish sealed, labeled* 	
- anv* samole lost* - 	
grad cyl.
weighed
water* measured* * n**^ * * inns 	
- silica gel* weighed •„ net* KRIS* ••••••
- condition - color* - -/ fa -ftxi **-*'*" "
- probe* cooled- sufficiently 	
- nozzle- removed* and* brushed* 	
- probe brushed* 6* times 	
- nozzle- brushes- clean* 	
- wash bottles clean* * • • • • • • 	
- acetone clean 	
— M*"8 la- minute* nurse 	

LUx^ UkftM** blank taken: aeetoneV water; other*
. Probe brush* and extension clean*, *
Samole container*: * Clean • *
Capped-
Labeled
1 Sealed 	
Liauid' level* -marked* *
Wt
Test
Run
1
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-------
     J.,
Page
4 of
Date
R « Recoimended
M - Mandatory
• • 	 	 - ......
9. Post teat Orsat Analysis of Initial (MJ
integrated bag sample orsac
analyzer - Analyzer leak check
. (levels should not fall below Final (M)
cap. tubing and not more than
0.2 nli in bnrrctte for 2' Bin-. ) .......
Orsat- samples;- Each bag analyzed- 3* tines-
Z- G0? agrees- within- Qi2! 	
*• 0?- agrees- within 0-.2X 	
I- CD- agrees- within- 0*.2f 	
Analysis at end of test. Orsat analyzer
checked against air (20.9 ±"Q»3-) 	
Orsat Analysis:
«*«_«». . . 	
GU7& 	
2?s 	
CDZ 	 	
FO - Z0i9 -SO*
• z GO.? 	
Fuel1 • 	
j^ujcange- for1 foe!.'
Orsat- analysis- valid-
Orsat solutions changed
when calculated F0
exceeds foe 1 type * range •
10. All saraoles locked up
All sawsiing- components- clean- and- seaied
M. Ail data' sheets submitted' to- observer* 	
"^ - Orsat 	
- Run- isofcenetie- • • • Team/Observer' •••••••
• - - Particuiate- recovery 	
} ^_ - Process- data 	 • 	
- Charts 	 - - - 	
• -• Calibration sheets 	 • •
$«-n
Test
Ron
1
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-------
                                                                         5 of 5

  J.   NOTES:  Care should be taken, when sampling for organic  compounds,  to
      follow stringent quality control guidelines to avoid contamination  of the
      sample and sampling train.  Take note of any occurences  which could bias
      the sample in any manner.

      Include: (1) General comments; (2) Changes to pretest agreement with
      justification; (3) Identify (manufacturer) and describe  condition of
      sampling equipment; (4) any abnormal occurrences, during  test program.
      (Additional page(s) attached:  Yea •••  . Ho
T^,-.  PV
   Signature of Ob^rver            Affiliation of Observer          Date

-------
 APPENDIX F




PARTICIPANTS

-------
PROJECT PARTICIPANTS
Affiliation
USEPA
EMC
BSD

PES











DEECO

ERG
FAL
Quanterra
LabCorp
Name

John C. Bosch, Jr.
Alfred E. Vervaert
Lula H. Melton
John T. Chehaske
Franklin Meadows
Daniel F. Scheffel
Dennis P, Holzschuh
Ron Kolde
Dennis P, Becvar
Dennis D. Holzschuh
Troy A. Abernathy
Gary M. Gay
Jason T. Centers
Steven B. Blaine
Nicky P. Nielsen
Richard Durham
Marc Hamilton
Joan T. Bursey
William H. Wadlin
Robert Weidenfeld

Responsibility

Work Assignment Manager
Group Leader
Process Monitor and Observer
Program Manager
Project Manager
Field Team Leader
QA Coordinator
Sample Recovery
Laboratory Audit
Field Team Member
Field Team Member
Field Team Member
Field Team Member
Field Team Member
Field Team Member
Sample Recovery
QAPP
PM/MCEM Analysis
Metals Analysis
PAH Analysis
NIOSH PAH Analysis

-------
                     PROJECT PARTICIPANTS (Concluded)
   Affiliation
       Name
              Responsibility
RTI
Marvin Branscome
Sandy George
Stacy Molinich
EPA/ESD Contractor
EPA/ESD Contractor (Observer)
EPA/ESD Contractor (Observer)
Bethlehem Steel
Thomas W. Easterly
Larry Mayton
Rich Guerra
Superintendent, Environmental Services Dept,

-------
            APPENDIX G




SAMPLING AND ANALYTICAL PROCEDURES

-------
        EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
                         NSFS TEST METHOD
 Method 1 - Sample and Velocity Traverses for Stationary Sources


1.  PRINCIPLE AND APPLICABILITY

1.1   Principle.   To  aid in  the representative  measurement of
pollutant  emissions  and/or  total  volumetric  flow  rate  from a
stationary source,  a  measurement site where the  effluent stream is
flowing in a known  direction is selected, and the cross-section of
the  stack  is divided into  a  number of equal areas.   A traverse
point is then located within each of these equal areas.

1.2   Applicability.    This method  is  applicable  to  flowing  gas
streams in  ducts,  stacks, and flues.   The method  cannot be used
when:  (1)  flow  is  cyclonic or swirling  (see  Section  2.4),   (2) a
stack is  smaller than about 0.30 meter  (12  in.)  in diameter, or
0.071 mz  (113 in.2)  in cross-sectional area, or (3)  the measurement
site is less than  two stack or duct diameters  downstream or less
than a half diameter upstream from a flow disturbance.

The  requirements  of  this  method  must  be   considered  before
construction  of a  new  facility from which  emissions will  be
measured; failure  to do  so may require subsequent alterations to
the  stack  or   deviation  from  the  standard procedure.    Cases
involving variants are  subject to approval by  the Administrator,
U.S. Environmental Protection Agency.

2.  PROCEDURE

2.1    Selection  of  Measurement Site.    Sampling  or  velocity
measurement  is performed  at a site located at least eight stack or
duct diameters downstream and two diameters upstream from any flow
disturbance  such as a bend, expansion,  or contraction in the stack,
or from a  visible flame.   If necessary,  an alternative location may
be  selected, at a  position at least two  stack  or  duct diameters
Prepared by Emission Measurement Branch              EMTIC TM-001
Technical Support Division, OAQPS, EPA

-------
        EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
                         NSPS TEST METHOD
downstream and a half diameter upstream from any flow disturbance.
For a rectangular cross  section,  an equivalent  diameter (De) shall
be  calculated  from the  following  equation,   to  determine  the
upstream and downstream distances:
                           D -
                            e   (L + W)

                                                       Eq. 1-1

     Where
          L    =    Length and W = width.

An  alternative   procedure   is   available  for  determining  the
acceptability  of  a  measurement  location not meeting the criteria
above.  This procedure,
determination  of gas  flow  angles  at  the  sampling  points  and
comparing the results with acceptability criteria, is described in
Section 2.5.

2.2  Determining the Number of Traverse Points.

2.2.1   Particulate  Traverses.   When the  eight- and two-diameter
criterion can be met, the minimum number of traverse points shall
be: (1) twelve, for circular or rectangular stacks with diameters
(or equivalent diameters)  greater than 0.61 meter  (24 in.);  (2)
eight,  for  circular, stacks with diameters  between  0.30  and 0.61
meter  (12 and  24  in.);  and (3)  nine,  for rectangular stacks with
equivalent diameters between 0.30 and 0.61 meter (12 and 24 in.).

When  the  eight-  and  two-diameter criterion  cannot be  met,  the
minimum number of traverse points  is determined from Figure 1-1.
Before  referring  to the  figure,  however,  determine the distances
from  the chosen  measurement site  to  the  nearest  upstream  and
downstream  disturbances,  and divide  each distance by the stack
Prepared by Emission Measurement Branch              EMTIC TM-001
Technical Support Division, OAQPS, EPA

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EMTIC TM-001          EMTIC NSPS TEST METHOD                Page 3
diameter or equivalent  diameter, to determine the distance in terms
of the number of duct  diameters.  Then, determine  from Figure  1-1
the minimum number  of traverse points that  corresponds:  (1)  to  the
number  of  duct  diameters  upstream;  and   (2)  to  the  number  of
diameters downstream.   Select the higher of the two  minimum numbers
of traverse points,  or  a  greater value,  so that for  circular stacks
the number  is a multiple  of 4,  and for  rectangular stacks,  the
number is one of those shown in Table 1-1.

2.2.2   Velocity (Non-Particulate)  Traverses.   When velocity  or
volumetric  flow rate  is to be  determined  (but  not  particulate
matter),  the same procedure  as that used for particulate traverses
(Section  2.2.1)  is  followed,  except that Figure   1-2 may  be used
instead of  Figure 1-1.

2.3  Cross-Sectional Layout and Location of Traverse Points.

2.3.1    Circular Stacks.    Locate  the  traverse  points  on  two
perpendicular  diameters  according  to  Table  1-2 and the  example
shown in Figure  1-3.  Any equation  (for examples,  see  Citations 2
and 3 in the Bibliography)  that gives the  same  values  as those  in
Table 1-2 may be used  in lieu of Table 1-2.

For particulate traverses, one of the diameters  must  be  in  a plane
containing  the  greatest  expected concentration variation,  e.g.,
after bends, one diameter shall be in the plane  of  the  bend.  This
requirement  becomes  less  critical  as   the   distance  from  the
disturbance increases; therefore, other diameter locations  may  be
used,  subject to the approval of the Administrator.

In addition,  for stacks  having  diameters greater than  0.61  m  (24
in.),  no traverse points  shall be within 2.5 centimeters  (1.00 in.)
of the stack walls; and for stack diameters equal  to or less than
0.61 m (24 in.),  no  traverse points shall be located  within  1.3  cm
(0.50 in.)  of the stack walls.  To meet these criteria,  observe  the
procedures given below.
2.3.1.1   Stacks With Diameters Greater Than  0.61 m  (24  in.).  When
any of the traverse  points as located in Section 2.3.1  fall  within
2.5 cm (1.00 in.) of the
stack walls,  relocate  them away  from  the  stack walls  to:  (1)  a
distance of
2.5 cm  (1.00  in.);  or (2)   a distance equal to the  nozzle  inside
diameter,  whichever  is  larger.  These relocated traverse points  (on
each end of  a  diameter)  shall  be the  "adjusted" traverse  points.

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EMTIC TM-001          ElffTIC NSPS TEST METHOD                Page 4
Whenever  two  successive  traverse  points are  combined to form  a
single  adjusted traverse point, treat  the  adjusted point as  two
separate  traverse  points,   both  in  the  sampling  (or  velocity
measurement) procedure,  and  in  recording the  data.

2.3.1.2   Stacks With Diameters Equal To or Less Than 0.61 m  (24
in.)-   Follow  the  procedure in Section  2.3.1.1, noting  only  that
any "adjusted"  points should  be  relocated away from the stack walls
to: (1)  a distance  of 1.3 cm  (0.50  in.);  or  (2) a distance equal to
the nozzle inside diameter,  whichever is larger.

2.3.2  Rectangular  Stacks.  Determine the number of traverse points
as explained in Sections  2.1  and 2.2 of this method.   From Table 1-
1,  determine  the  grid  configuration.   Divide  the stack cross-
section into as many equal rectangular elemental  areas  as traverse
points,  and then locate a traverse point at  the centroid of  each
equal area according  to  the  example in  Figure 1-4.
If  the  tester  desires  to  use more  than   the  minimum number  of
traverse  points, expand the  "minimum  number of traverse points"
matrix  (see Table  1-1)  by adding the extra traverse points along
one or the other or both  legs  of the matrix;  the  final  matrix  need
not be  balanced.   For  example,  if a  4 x 3 "minimum number  of
points" matrix were  expanded  to 36 points,  the  final matrix could
be 9  x  4  or 12 x 3,  and would  not necessarily have to be 6  x 6.
After constructing  the final matrix, divide the stack cross-section
into as  many equal  rectangular,  elemental areas as traverse points,
and locate a traverse point at the  centroid of each equal  area.  The
situation of traverse points  being  too close to  the  stack walls is
not expected to arise with  rectangular  stacks.   If this problem
should  ever  arise,  the  Administrator must  be  contacted   for
resolution of the matter.

2.4  Verification of Absence of  Cyclonic  Flow.   In most stationary
sources, the direction of stack  gas flow is  essentially  parallel to
the stack walls.  However, cyclonic flow may  exist  (1) after  such
devices  as cyclones  and  inertial  demisters  following venturi
scrubbers, or  (2) in stacks having  tangential  inlets or other  duct
configurations which  tend to  induce swirling;  in these instances,
the presence or absence  of cyclonic flow at the  sampling location
must be determined.   The following techniques are  acceptable  for
this determination. Level and zero the manometer.   Connect a  Type
S pitot tube to the manometer.  Position the  Type S pitot tube at
each traverse point,  in succession, so that  the planes  of the  face
openings  of the  pitot tube  are perpendicular to the stack cross-

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EMTIC TM-001          EMTIC NSPS TEST METHOD                Page  5
sectional plane;  when the  Type S pitot tube is in this  position,  it
is at "0° reference."  Note the differential pressure  (Ap)  reading
at each traverse  point.  If a null  (zero) pitot reading is  obtained
at  0°  reference  at  a given  traverse point,  an acceptable  flow
condition exists  at that  point.  If the pitot  reading is  not  zero
at  0°  reference,  rotate  the  pitot tube  (up  to ±90°  yaw  angle) ,
until a null reading  is obtained.  Carefully determine and record
the value of the  rotation angle  (a) to  the nearest degree.  After
the null technique
has been applied  at each  traverse  point,  calculate the average  of
the absolute values  of a;  assign a  values of 0°  to those points for
which no rotation was required,  and include these in the  overall
average.    If  the average value  of  a  is greater  than  20°,  the
overall  flow  condition   in  the  stack  is   unacceptable,  and
alternative  methodology,  subject   to  the   approval   of  the
Administrator,  must  be used to perform accurate sample  and  velocity
traverses.  The alternative procedure  described in Section  2.5 may
be used to  determine  the  rotation  angles  in lieu of the procedure
described above.
2.5   Alternative Measurement  Site  Selection Procedure.    This
alternative applies  to sources where measurement locations  are  less
than 2 equivalent or duct diameters downstream or less than  one-
half  duct  diameter  upstream  from  a   flow  disturbance.   The
alternative  should  be  limited to ducts larger than 24  in.  in
diameter  where   blockage  and  wall  effects   are  minimal,     A
directional flow-sensing  probe is used  to  measure  pitch  and yaw
angles of the gas  flow at  40 or more traverse points; the resultant
angle is  calculated  and compared with  acceptable  criteria  for mean
and standard deviation.

NOTE:   Both the  pitch  and yaw  angles  are measured  from a  line
passing through the  traverse point  and parallel  to the stack axis.
The pitch angle is the angle of the gas flow component  in the plane
that INCLUDES the  traverse line and is parallel  to the stack axis.
The yaw angle is  the  angle of the  gas flow component  in the plane
PERPENDICULAR  to  the traverse line at  the  traverse  point and  is
measured  from the  line  passing  through  the  traverse  point  and
parallel to the stack axis.

2.5.1  Apparatus.

2.5.1.1  Directional  Probe.  Any directional probe, such as United
Sensor Type DA Three-Dimensional  Directional  Probe,  capable  of
measuring both the pitch and yaw angles of gas flows is acceptable.

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EMTIC TM-001          EMTIC NSPS TEST METHOD                Page  6
 (NOTE:   Mention  of  trade name  or  specific products  does  not
constitute  endorsement  by  the  U.S.  Environmental   Protection
Agency.)   Assign an identification number to the directional  probe/
and  permanently mark  or  engrave the  number on  the  body of  the
probe.  The pressure holes  of directional probes are susceptible to
plugging when used in particulate-laden  gas streams.  Therefore,  a
system  for cleaning  the   pressure  holes  by  "back-purging"  with
pressurized air is  required.

2.5.1.2  Differential Pressure Gauges.  Inclined manometers,  U-tube
manometers, or other differential pressure gauges (e.g.,  magnehelic
gauges)  that meet  the specifications described in Method  2, Section
2.2.

NOTE:  If  the differential pressure gauge produces both  negative
and  positive  readings, then both negative  and positive  pressure
readings  shall be  calibrated  at  a minimum  of  three  points  as
specified  in Method 2, Section 2.2.

2.5.2  Traverse Points.   Use a minimum of 40 traverse  points  for
circular ducts and 42 points for rectangular ducts for the  gas  flow
angle determinations.   Follow Section  2.3 and  Table  1-1  or 1-2  for
the location and layout of  the traverse points.  If the measurement
location is determined to  be acceptable
according  to  the  criteria  in this alternative procedure, use  the
same traverse point number  and locations for sampling and  velocity
measurements.

2.5.3  Measurement  Procedure.

2.5.3.1   Prepare  the directional probe and differential  pressure
gauges as  recommended by  the manufacturer.   Capillary tubing  or
surge tanks  may be used to dampen  pressure  fluctuations.  It  is
recommended,  but  not required,  that  a  pretest  leak  check  be
conducted.  To perform a leak check, pressurize or  use  suction on
the impact opening  until a reading  of  at least  7.6 cm  (3  in.)  H20
registers on the differential pressure gauge,  then plug  the  impact
opening.   The pressure of a leak-free system will remain  stable  for
at least 15 seconds.

2.5.3.2  Level and zero the manometers.  Since the manometer level
and. zero may drift  because of vibrations and  temperature  changes,
periodically check  the level and zero during  the  traverse.

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 EMTIC TM-001         EMTIC NSPS TEST METHOD                Page 7
.2.5.3.3   Position the probe at the appropriate locations in the gas
 stream,  and rotate  until zero deflection is indicated for the yaw
 angle pressure gauge.  Determine and record the yaw angle.  Record
 the pressure gauge readings for the pitch angle,  and determine the
 pitch angle from the calibration curve.   Repeat this procedure for
 each traverse point.  Complete a "back-purge" of the pressure lines
 and  the  impact  openings prior  to measurements  of  each  traverse
 point.

 A post-test check as described in Section 2.5.3.1 is required.  If
 the  criteria  for  a leak-free  system  are  not met,  repair  the
 equipment,  and repeat the flow angle measurements.

 2.5.4   Calculate the resultant  angle at  each  traverse point,  the
 average   resultant  angle, and  the  standard  deviation using  the
 following equations.  Complete the calculations retaining at least
 one  extra  significant  figure beyond that  of the  acquired data.
 Round the values after the final calculations,

 2.5.4.1   Calculate  the resultant angle  at each traverse point:

                R.. = arc cosine [ (cosineY.jJ (cosinePi) ]
                                                        Eq. 1-2
Where:
           Ri    =    resultant angle at traverse point i,  degree.
           Y±    =    yaw angle at traverse point i,  degree.
           P±    =    pitch angle at traverse point i,  degree.

2.5.4.2   Calculate  the  average resultant for the measurements:
                                  n

                                                             Eq. 1-3
Where:
           Ravg   =     average resultant angle,  degree
           n     =     total  number of traverse  points,

2.5,4.3   Calculate  the  standard deviations:

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EMTIC TM-001
                      EMTIC NSFS TEST METHOD
Page 8
                              >
                                  (n-1)
Where:
                    standard deviation, degree.
2.5.5  The  measurement location is acceptable if R
£ 10°.
                                                   avg
                                                            Bj. 1-4
                                                        20° and S
2.5.6   Calibration.   Use a flow  system as described in Sections
4.1.2.1  and  4.1.2.2  of Method  2.   In  addition,  the flow system
shall have the  capacity to generate two test-section velocities:
one  between  365  and 730  m/min  (1200  and 2400  ft/min)  and one
between 730 and 1100 m/min  (2400 and 3600  ft/min) .

2.5.6.1  Cut  two entry ports in the test section.   The axes through
the entry ports  shall be perpendicular to each other  and intersect
in the centroid  of the test section.  The ports  should be elongated
slots parallel  to the  axis of the test section and  of sufficient
length to allow measurement of pitch angles while maintaining the
pitot head position  at  the test-section centroid.   To facilitate
alignment of  the directional probe during calibration,  the test
section  should   be  constructed  of  plexiglass  or some  other
transparent material.  All calibration measurements should be made
at the same point in the test section, preferably at the centroid
of the test section.

2.5.6.2  To  ensure that the gas  flow  is  parallel to the central
axis of the test  section, follow the procedure in Section 2.4 for
cyclonic flow determination to measure the gas flow  angles at the
centroid of the  test section from two test ports  located 90° apart.
The  gas flow  angle measured  in  each  port must be ±2°  of 0°.
Straightening vanes should be installed,  if necessary, to meet this
criterion.

2.5.6.3  Pitch Angle Calibration.  Perform a calibration traverse
according  to  the  manufacturer's  recommended   protocol  in   5°
increments for angles from  -60°  to +60° at one velocity in each  of
the two ranges specified above.  Average the pressure ratio values
obtained  for each  angle  in  the  two  flow ranges,  and plot  a

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EMTIC TM-001          EMTIC NSPS TEST METHOD               Page  9
calibration curve with  the average values of the  pressure ratio  (or
other   suitable  measurement   factor   as   recommended   by   the
manufacturer) versus the pitch angle.  Draw  a smooth line through
the  data points.   Plot also  the  data values  for  each traverse
point.  Determine the  differences between the measured datavalues
and  the  angle  from  the calibration curve  at  the  same pressure
ratio.   The difference at each  comparison  must be within 2°  for
angles between 0° and 40° and within  3° for  angles between 40°  and
60°.

2.5.6.4  Yaw Angle Calibration.  Mark the three-dimensional probe
to allow the determination of the yaw position of the probe.  This
is  usually  a line extending the length  of  the  probe and aligned
with the impact  opening.  To determine the accuracy of measurements
of the yaw angle,  only  the zero or null  position  need be calibrated
as follows:  Place the directional probe in  the test section,  and
rotate  the  probe  until  the   zero  position  is found.   With a
protractor  or other  angle  measuring  device,  measure  the  angle
indicated  by the  yaw  angle indicator on  the  three-dimensional
probe.  This  should  be within  2° of  0°.   Repeat this measurement
for any other points  along the length of the pitot where yaw angle
measurements could be  read  in  order  to account  for variations in
the pitot markings used to indicate pitot head positions.

BIBLIOGRAPHY

!„   Determining  Dust Concentration   in   a  Gas   Stream,   ASME
     Performance Test  Code No.  27.  New York.  1957.

2.   DeVorkin,  Howard,  et al.  Air Pollution Source Testing Manual.
     Air Pollution Control  District.   Los  Angeles,  CA.   November
     1963.

3.   Methods  for Determining  of Velocity,  Volume,  Dust  and Mist
     Content  of Gases.   Western  Precipitation Division of  Joy
     Manufacturing Co.  Los Angeles,  CA.  Bulletin WP-50.  1968.

4.   Standard Method*for Sampling  Stacks for Particulate Matter.
     In: 1971 Book of ASTM Standards,  Part 23.  ASTM Designation D
     2928-71.  Philadelphia, PA.  1971.

5.   Hanson,  H.A.,  et al.   Particulate Sampling  Strategies  for
     Large  Power Plants Including Nonuniform Flow.   USEPA,  ORD,
     ESRL,  Research  Triangle  Park,  NC.   EPA-600/2-76-170.   June

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EMTIC TM-001          EMTIC NSPS TEST METHOD               Page  10
     1976.

6.   Entropy Environmentalists,  Inc.  Determination of  the Optimum
     Number of Sampling Points: An Analysis of Method  1 Criteria.
     Environmental Protection Agency.  Research Triangle Park, NC.
     EPA Contract No. 68-01-3172, Task 7.

7.   Hanson,  H.A.,  R.J.  Davini,  J.K.  Morgan, and  A.A. Iversen.
     Particulate  Sampling  Strategies  for  Large   Power   Plants
     Including Nonuniform  Flow.  USEPA, Research Triangle Park, NC.
     Publication No. EPA-600/2-76-170.  June 1976.   350 p.

8.   Brooks,  E.F.,  and R.L.  Williams.    Flow and  Gas Sampling
     Manual.   U.S.  Environmental  Protection  Agency.   Research
     Triangle  Park,  NC.   Publication No. EPA-600/2-76-203.   July
     1976.  93 p.

9.   Entropy  Environmentalists,  Inc.   Traverse Point  Study.  EPA
     Contract No.  68-02-3172.   June 1977.  19 p.

10.  Brown,  J.  and  K. Yu.    Test  Report:  Particulate Sampling
     Strategy  in Circular  Ducts.   Emission  Measurement Branch.
     Emission   Standards    and  Engineering   Division.      U.S.
     Environmental Protection  Agency,  Research Triangle Park,  NC
     27711.  July 31, 1980.  12 p.

11.  Hawksley, P.G.W.,  S.  Badzioch, and J.H. Blackett.  Measurement
     of Solids in  Flue  Gases.   Leatherhead,  England,  The British
     Coal Utilisation Research Association.  1961.   p.  129-133.

12.  Knapp,  K.T.    The  Number of  Sampling  Points  Needed for
     Representative Source Sampling.  In: Proceedings  of the  Fourth
     National Conference  on Energy and Environment.  Theodore,  L.
     et al. (ed).  Dayton,  Dayton Section of the American Institute
     of Chemical Engineers.  October 3-7,  1976.  p.  563-568.

13.  Smith, W.S.  and D,J.  Grove.   A Proposed Extension  of EPA
     Method 1  Criteria.   Pollution Engineering.   XV  (8):36-37.
     August 1983.

14.  Gerhart,   P.M. and  M.J.  Dorsey.   Investigation  of Field  Test
     Procedures for Large Fans.  University of Akron.  Akron, OH.
     (EPRI Contract CS-1651) .   Final Report (RP-1649-5).  December
     1980.

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EMTIC TM-001          EMTIC NSPS TEST METHOD               Page  11
15.  Smith,  W.S.  and D.J.  Grove.  A New Look at Isokinetic Sampling
        Theory  and  Applications.    Source  Evaluation  Society
     Newsletter.  VIII(3):19-24.  August  1983.

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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 12
               Table  1-1.   CROSS-SECTION  LAYOUT  FOR
                        RECTANGULAR STACKS
                      -Number  of  traverse  points
               Matrix layout
                          9
                         12
                         16
                         20
                         25
                         30
                         36
                         42
                         49
                          3x3
                          4x3
                          4x4
                          5x4
                          5x5
                          6x5
                          6x6
                          7x6
                          7x7

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EMTIC TM-001
EMTIC NSFS TEST METHOD
Page 13
                            TABLE 1-2
          LOCATION  OF  TRAVERSE  POINTS IN CIRCULAR STACKS
             (Percent of stack diameter from inside
                     wall to traverse point)
Traverse
Point
Number on a
Diameter
1 	

2

3 	

4 	

5 	

6 .....

7

8 	

9 .....

10 , . . .
11 . . . .
12 ....
13 ....
Number of traverse points on a diameter
2
14
.6
85
.4











4
6.
7
25
.0
75
.0
93
.3









6
4.
4
14
.6
29
.6
70
.4
85
.4
95
.6







8
3.
2
10
.5
19
.4
32
.3
67
.7
80
.6
89
.5
96
.8





10
2.6
8.2
14.
6
22.
6
34.
2
65.
8
77.
4
85.
4
91.
8
97.
4



12
2.1
6.7
11.
8
17.
7
25.
0
35.
6
64.
4
75.
0
82.
3
88.
2
93.
3
97.
9

14
1.8
5.7
9.9
14.
6
20.
1
26.
9
36.
6
63.
4
73.
1
79.
9
85.
4
90.
1
94.
3
16
1.6
4.9
8.5
12.
5
16.
9
22.
0
28.
3
37.
5
62.
5
71.
7
78.
0
83.
1
87.
5
18
1.
4
4.
4
7.
5
10
.9
14
.6
18
.8
23
.6
29
.6
38
.2
61
.8
70
.4
76
.4
81
.2
20
1.
3
3.
9
6.
7
9.
7
11
2.
9
16
.5
20
.4
25
.0
30
.6
38
.8
61
.2
69
.4
75
.0
22
1.1
3.5
6.0
8.7
11.
6
14.
6
18.
0
21.
8
26.
2
31.
5
39.
3
60.
7
68.
5
24
1.1
3.2
5.5
7.9
10.
5
13.
2
16.
1
19.
4
23.
0
27.
2
32.
3
39.
8
60.
2

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EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 14
14 ....

15 ....

16 ....

17 ....

-L o • • . *

19 ....

20 ....

21 ....

22 ....

23 ....

24 ....





































































































































98.
2




















91.
5
95.
1
98.
4
















85
.4
89
.1
92
.5
95
.6
98
.6












79
.6
83
.5
87
.1
90
.3
93
.3
96
.1
98
.7








73.
8
78.
2
82.
0
85.
4
88.
4
91.
3
94.
0
96.
5
98.
9




67.
7
72.
8
77.
0
80.
6
83.
9
86.
8
89.
5
92.
1
94.
5
96.
8
98.
9

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EMTIC  TM-001
             EMTIC NSPS TEST  METHOD
Page 15
                 so
                 40
                 30
                   0.5
                            Duct Diameters Upstream from Flow Disturbance* (Distance A)

                                  1,0             1.5             2JO
                                                                            2.5
                 10
DLL
  2
                          Higher Numt»r ii for
                          Rectangular Stacks or Ducts
                           or 25
                          * From Point of Any Type of
                          Disturbance (Bend, Expansion, Contractfon, ete.)

                                                                    Uaasuiernen!
                                                                     Si1e
                                                   '6   suck Diamelor > 0.81 rn (24 in 1

                                                        I       12
                                                                    BorO
                                                        Stock Diameter • n.30 to 0,61 m (12-24 In,)


                                                        I	I	I	
                           3      4      5      6      T       8

                            Duct Dlamelera Downstream from Flow Disturbance* (Distance B)
                                                                      S
                                                                            10
           Figure  1-1.  Minimum  number  of  traverse points  for
           particulate  traverses.

-------
EMTIC TM-001
EMTIC N5P5 TEST METHOD
Page 16
          so
            0,5
                     Duct Diameters Upstream from Flow DisUjrbance" (Distance A)

                          1.0            1.5            2,0
          40
          30
          20
           10
i 1 i 1 1 1
a
Higher Number Is fof
Rectangular Slacks or Ducts




IB Stack Die

I

t
1
B
1
±





/Dlstorbariea
I Measurement
[_ Site
^~


Disturbance


-





meter > 0.61 m(24!n.)
_ |

— * From Point of Any Type of
Disturbance (Bend, Expansion, Contraction, etc.)
12
a
8 or 9 —

Stack Diameter - 0.30 to 0.61 m (12-24 in.)
1 1 1 i 1 |
J
                    345678


                     Duct Diameters Downstream from Flow Disturbance* (Distance B)

                                       /
                                       i
                                                                   10
     Figure 1-2.  Minimum number of  traverse points  for  velocity

     (nonparticulate)  traverses.

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EMTIC TM-001
         EMTIC NSPS TEST  METHOD
Page 17
       Traverse
        Point

         1
         2
         3
         4
         5
         6
 Distance
%o< diameter

  4.4
  14.7
  29.S
  70.5
  65.3
  95.8
    Figure  1-3. Example showing circular  stack cross section
    divided  into  12  equal areas,  with location  of  traverse
    points indicated.

-------
EMTIC TM-001
EMTIC NSPS TEST METHOD
Page 18
o

o
	
0
0
,-_: 	 ^
O
	
o
o
	 1
o
	 _l
o
0
— , 	
o
• _««.__»*
0
   Figure  1-4.  Example showing rectangular  stack  cross section
   divided into 12 equal areas,  with  a  traverse point at centroid
   of  each area.

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               EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
                               NSPS TEST METHOD
         Method 2 - Determination of Stack Cas Velocity and Volumetric
                         Flow Rate (Type S Pitot Tube)


1.  PRINCIPLE AND APPLICABILITY

1.1  Principle.   The  average gas velocity  in a  stack is determined from the  gas
density and  from measurement  of  the  average  velocity  head  with  a  Type  S
(Stausscheibe or reverse type) pitot  tube.

1.2  Applicability.   This  method is applicable for measurement of the average
velocity of a gas stream and  for  quantifying gas flow.

This procedure  is not applicable at measurement sites that  fail  to meet  the
criteria of Method 1, Section 2.1.  Also, the  method cannot be  used  for  direct
measurement in cyclonic or swirling gas streams; Section 2.4 of Method 1  shows
how  to determine  cyclonic or  swirling  flow  conditions.    When unacceptable
conditions  exist,  alternative  procedures,  subject  to the  approval  of  the
Administrator,  U.S.  Environmental Protection Agency,  must be employed to make
accurate flow rate  determinations;  examples of  such alternative procedures are:
(1) to  install straightening  vanes;  (2) to calculate the total volumetric flow
rate stoichiometrically, or (3) to move to  another measurement site at  which  the
flow is acceptable.

2.  APPARATUS

Specifications  for  the apparatus are given below.  Any other apparatus that  has
been demonstrated  (subject to approval  of the Administrator)  to be capable of
meeting the specifications will be considered  acceptable.

2.1  Type S  Pitot Tube.  Pitot tube made  of metal tubing  {e.g., stainless steel)
as shown  in Figure  2-1.  It  is  recommended  that the  external tubing diameter
(dimension  Dt, Figure  2-2b)  be  between 0.48 and 0.95  cm  (3/16 and 3/8 inch).
There shall  be  an equal distance from  the base  of each leg of the pitot tube to
its face-opening plane  (dimensions PA and PB,  Figure  2-2b);  it is recommended
that this distance be between  1.05  and 1.50 times the external tubing  diameter.
The face  openings  of the pitot  tube shall,  preferably, be aligned as shown in
Figure  2-2?  however, slight misalignments of the openings are permissible (see
Figure  2-3)  .

The Type S pitot  tube shall have a  known coefficient, determined as outlined in
Section 4,  An identification number  shall be  assigned to the pitot tube; this
number  shall  be permanently  marked  or engraved on the  body of the  tube.    A
standard pitot  tube may be used instead of a Type S, provided that it meets  the
specifications  of Sections 2.7 and 4,2; note, however,  that  the  static  and impact
pressure  holes  of  standard pitot  tubes   are susceptible   to  plugging  in
particulate-laden gas streams.  Therefore,  whenever a standard pitot tube is used
to perform a traverse, adequate proof must  be furnished that the openings of  the
Prepared by Emission Measurement Branch                            EMTIC H-002
Technical Support Division, OAQPS, EPA

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               EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
                               NSPS TEST METHOD
pitot tube have not plugged up during the traverse period; this can be  done  by
taking a velocity  head  (Ap) reading at the final traverse point,  cleaning  out the
impact  and static  holes of  the standard  pitot  tube by  "back-purging" with
pressurized air,  and then taking another Ap reading.   If the Ap readings made
before  and after  the  air purge are the same  (±5 percent),  the  traverse  is
acceptable.  Otherwise,  reject the run.  Note that if Ap at the final traverse
point is unsuitably low,  another point  may  be selected.   If "back-purging"  at
regular intervals is part of  the procedure, then comparative Ap readings shall
be taken,  as above, for the last two  back purges at which  suitably  high  Ap
readings are observed.

2.2  Differential Pressure Gauge.  An inclined manometer or equivalent  device.
Most sampling trains are  equipped with a  10-in.  (water column) inclined-vertical
manometer,  having  0.01-in. H2O divisions  on  the 0- to 1-in. inclined scale, and
0.1-in.  H20 divisions on the 1- to 10-in. vertical  scale.  This type of manometer
(or other gauge of equivalent sensitivity)  is satisfactory for the measurement
of Ap values  as  low as  1.3 mm [0.05 in.)  H20.  However, a differential pressure
gauge of  greater sensitivity shall  be  used  (subject  to the  approval  of the
Administrator),  if any  of  the  following is found to be true:  (1) the arithmetic
average of all  Ap readings  at  the traverse points in the  stack  is less than
1.3 mm  (0.05 in.)  H20;  (2)   for  traverses of 12 or more  points,  more  than  10
percent of the  individual Ap  readings are below  1.3 mm (0.05 in.)  H20;  (3) for
traverses  of fewer than  12  points,  more than one Ap  reading  is  below 1.3  mm
(0.05 in.)  H20.  Citation 18 in the  Bibliography describes commercially available
instrumentation for the  measurement  of low-range gas velocities.

As an alternative to criteria (1)  through (3) above, the following calculation
may  be  performed  to  determine  the  necessity  of  using  a  more  sensitive
differential pressure  gauge:  .
                    T =
Where:
             =    Individual velocity  head reading at a traverse point, ram  (in.)
                  H20.

        n    =    Total number of traverse points.

        K    =    0.13 mm H20 when metric units are used and 0.005 in. H20  when
                  English units are used.
Prepared by Emission Measurement Branch                             EMTIC M-002
Technical Support Division, OAQPS, EPA

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EMTIC TM-002                     NSPS TEST METHOD                        Page  3


If T is  greater than 1.05,  the velocity head data are unacceptable and  a more
sensitive differential pressure gauge must be used.

NOTE:  If differential pressure gauges other than inclined manometers are used
(e.g.,  magnehelic  gauges),  their calibration must be  checked after each test
series.  To check the calibration of a differential pressure  gauge, compare Ap
readings of  the  gauge with those of a gauge-oil manometer at a minimum of three
points, approximately representing the range of Ap values in  the stack.  If, at
each point,  the values  of  Ap as read by the  differential  pressure gauge and
gauge-oil manometer agree to within 5 percent, the differential pressure gauge
shall be considered  to be in proper calibration.   Otherwise, the test  series
shall either be  voided, or procedures  to adjust the measured Ap values and final
results shall be used, subject to the approval of the Administrator.

2.3    Temperature  Gauge.    A thermocouple,  liquid-filled bulb  thermometer,
bimetallic thermometer, mercury-in-glass thermometer, or other gauge capable of
measuring temperature to  within 1.5  percent of  the minimum  absolute stack
temperature.   The temperature gauge shall be  attached to the pitot tube such that
the sensor tip does not touch any metal; the gauge shall be in an interference-
free arrangement with respect to the pitot tube face openings (see Figure  2-1 and
also Figure 2-7 in Section 4).  Alternative positions may be  used if the pitot
tube-temperature gauge system is calibrated according to the procedure of  Section
4.  Provided that a difference of not  more than 1 percent in the average velocity
measurement  is  introduced,  the temperature gauge need  not  be attached  to the
pitot tube;  this alternative is subject to the approval of the Administrator.

2,4  Pressure Probe and Gauge.  A piezometer tube and mercury- or water-filled
U-tube  manometer capable of measuring stack pressure to within 2.5 mm (0.1 in.)
Hg.  The static tap of a standard type pitot tube or one leg  of a Type  S pitot
tube with the face opening planes positioned parallel to the  gas flow may also
be used as the pressure probe.

2.5  Barometer.  A mercury, aneroid, or other  barometer  capable  of measuring
atmospheric  pressure  to within  2.5  mm (0.1 in.) Hg.   See NOTE  in Method 5,
Section 2.1.9.

2.6  Gas Density Determination Equipment.   Method 3 equipment,  if needed (see
Section  3.6), to  determine the stack gas dry  molecular weight, and Reference
Method  4 or  Method 5 equipment for moisture content determination; other methods
may be used subject to approval of the Administrator.

2.7  Calibration  Pitot Tube.   When  calibration  of  the Type S pitot  tube is
necessary (see Section 4), a standard pitot tube for a reference.  The standard
pitot  tube  shall,  preferably, have  a  known coefficient,  obtained either  (1)
directly from the National Bureau of Standards, Route 70 S,  Quince Orchard Road,
Gaithersburg,  Maryland, or (2) by calibration against another standard pitot tube
with an NBS-traceable coefficient. Alternatively, a standard pitot  tube designed
according to the  criteria  given in  Sections 2.7.1  through 2.7,5  below and
illustrated  in Figure 2-4  (see also Citations 7, 8, and 17 in  the Bibliography)
may be used.  Pitot tubes designed according to these specifications will have
baseline coefficients of about 0.99 ± 0.01.

2.7.1  Hemispherical (shown in Figure 2-4} ellipsoidal, or conical tip.

2.7.2   A minimum  of six diameters  straight  run (based upon D,  the external
diameter of the tube) between the tip and the static pressure holes.

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EMTIC TM-002                     NSPS TEST METHOD                        Page 4
2.7.3   A minimum of eight diameters  straight run between the  static  pressure
holes and the centerline of the  external  tube,  following  the 90-degree bend.

2.7.4  Static pressure holes of equal size (approximately 0.1  D),  equally spaced
in a piezometer  ring configuration.

2.7.5  Ninety-degree bend, with  curved  or mitered junction.

2.8  Differential Pressure Gauge for Type S Pitot Tube Calibration.  An  inclined
manometer or  equivalent.    If  the  single-velocity calibration technique  is
employed (see Section 4.1.2.3), the calibration differential pressure gauge shall
be  readable  to the  nearest  0.13  mm  [0.005  in.)  H20.    For  multivelocity
calibrations, the gauge shall be readable to the nearest 0.13 mm  (0.005 in.) H20
for Ap values between 1.3  and 25 mm (0.05 and 1.0 in.) H20,  and to the nearest
1.3 mm  (0.05 in.) H20  for Ap values above 25 mm (1.0 in.)  H20.   A special,  more
sensitive gauge  will be  required to read Ap values below 1.3 mm  (0.05 in.) H20
(see Citation 18 in the Bibliography).


3.  PROCEDURE

3.1   Set up the apparatus as  shown in  Figure 2-1.  Capillary  tubing  or surge
tanks installed  between  the  manometer and pitot tube may be used to dampen Ap
fluctuations.  It is recommended, but not required,  that a  pretest leak-check be
conducted as follows:  (1)  blow through  the  pitot  impact opening until  at least
7.6 cm (3 in.)  H20 velocity pressure registers  on the manometer;  then, close off
the impact opening.  The pressure shall remain  stable  for at least 15  seconds;
(2) do the same for the static pressure side, except using  suction to obtain the
minimum of 7.6  cm  (3  in.) H20.    Other leak-check procedures,   subject  to the
approval of  the Administrator, may be used.

3.2   Level and zero the manometer.   Because the  manometer  level  and  zero may
drift due to vibrations and temperature changes,  make periodic checks during the
traverse.    Record  all  necessary  data as  shown  in  the example  data  sheet
(Figure 2-5) .

3.3  Measure the  velocity head  and temperature at  the traverse points specified
by Method 1.  Ensure that  the  proper differential  pressure gauge is being used
for the range of  Ap values encountered (see Section 2.2).  If  it  is necessary to
change to a  more sensitive gauge, do so, and remeasure the  Ap  and temperature
readings at each  traverse point.  Conduct a post-test leak-check  (mandatory),  as
described in Section 3.1 above,  to validate the traverse  run.

3.4  Measure the  static pressure in the stack.   One reading is usually adequate.

3.5  Determine the atmospheric pressure.

3.6  Determine the stack gas dry  molecular weight.   For combustion processes or
processes that emit essentially C02,  02,  CO, and N2,  use  Method 3.   For processes
emitting essentially air, an analysis need not be conducted; use  a dry molecular
weight of 29.0.   For other  processes, other  methods, subject  to  the approval of
the Administrator, must be used.

3.7  Obtain the moisture content from Reference Method 4 (or equivalent) or from
Method 5.

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EMTIC TM-002                      NSPS TEST METHOD                       Page 5


3.8   Determine the cross-sectional  area of the stack or duct  at  the sampling
location.  Whenever possible, physically measure the stack dimensions rather than
using blueprints.

4.  CALIBRATION

4.1  Type S Pitot Tube.  Before its  initial use,  carefully examine  the Type S
pitot tube  in top,  side,  and end views to verify that  the  face  openings of the
tube are aligned within  the specifications illustrated in Figure 2-2 or 2-3.  The
pitot tube shall not be  used if it fails to meet these alignment  specifications.

After verifying the face opening  alignment,  measure and record the following
dimensions  of the  pitot tube:   (a)  the external tubing diameter (dimension  Dt,
Figure 2-2b); and (b)  the base-to-opening plane distances  (dimensions PA and  PE,
Figure  2-2b) .   If Dt  is between  0.48  and 0.95 cm  (3/16 and 3/8  in.), and if %
and PB are  equal  and  between 1.05 and 1.50 C(.,  there are two  possible options:
(I) the pitot tube may be calibrated  according  to the procedure outlined  in
Sections 4.1.2 through 4.1.5 below, or  (2) a baseline (isolated tube) coefficient
value of 0.84 may be assigned to  the pitot tube.  Note, however, that if the
pitot tube  is part of an assembly, calibration may still be  required,  despite
knowledge of the  baseline coefficient value (see Section 4.1.1).

If  Dt,  PA,  and £  are  outside  the specified limits,  the pitot  tube  must  be
calibrated  as outlined  in Sections  4.1.2 through 4.1.5 below.

4.1.1  Type S Pitot Tube Assemblies.   During sample and velocity traverses,  the
isolated Type S  pitot  tube is not always used; in many instances, the  pitot tube
is  used in  combination with other  source-sampling components  (thermocouple,
sampling probe,  nozzle)  as part of an  "assembly."  The presence of other sampling
components  can  sometimes affect  the  baseline value of  the  Type  S  pitot tube
coefficient (Citation  9  in the Bibliography); therefore  an assigned (or otherwise
known)  baseline  coefficient value may  or may not be valid for  a  given assembly.
The baseline and assembly coefficient  values will be  identical only when the
relative placement of the components in the assembly  is such that aerodynamic
interference effects  are eliminated.    Figures  2-6  through  2-8  illustrate
interference-free  component arrangements for Type  S pitot tubes  having external
tubing diameters between 0.48 and 0.95 cm (3/16 and 3/8  in.).   Type  S  pitot tube
assemblies  that fail to  meet any or  all of the specifications of Figures 2-6
through 2-8 shall  be calibrated according to the procedure  outlined in Sections
4.1.2  through  4.1.5 below,  and  prior  to  calibration,  the  values  of  the
intercomponent spacings (pitot-nozzle,  pitot-thermocouple, pitot-probe sheath)
shall be measured  and recorded.

NOTE:   Do not use  any  Type S pitot  tube  assembly which  is constructed such that
the impact pressure opening plane of the pitot  tube is  below the entry plane  of
the nozzle  (see Figure  2-6B).

4,1.2  Calibration Setup.  If the Type S pitot tube  is to be calibrated,  one leg
of the tube shall  be permanently  marked A,  and the  other, B.   Calibration shall
be done in  a flow  system having  the following  essential design  features:

4.1.2.1   The flowing gas stream must be confined  to a duct of  definite cross-
sectional area,  either circular or rectangular.   For circular cross  sections,  the
minimum duct diameter  shall be 30.5 cm (12 in.); for rectangular  cross sections,
the width  (shorter  side)  shall be  at  least 25.4 cm (10 in.).

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EMTIC TM-002                     NSPS TEST METHOD                        Page 6


4.1.2.2  The cross-sectional area of the calibration duct must  be  constant over
a distance of 10 or more duct diameters.  For  a  rectangular cross section,  use
an equivalent diameter, calculated from the following equation,  to  determine the
number of duct diameters:

                                 D   »
                                  e    (L + W)


                                                                Eq.  2-1
Where:
        De   =    Equivalent diameter.
        L    -    Length.
        W    =    Width.

To  ensure  the presence  of  stable,  fully  developed  flow  patterns  at  the
calibration site,  or "test section," the  site must be  located at  least  eight
diameters downstream and two diameters upstream from the nearest  disturbances.

NOTE:  The eight-  and two-diameter criteria are not  absolute;  other test section
locations may  be used (subject to  approval  of the Administrator),  provided that
the flow at the test  site is stable  and demonstrably parallel  to the duct  axis.

4.1.2.3   The  flow system  shall have the  capacity to generate a test-section
velocity around 915  m/min  (3,000  ft/min).   This velocity must be  constant with
time to guarantee steady flow during calibration.   Note  that  Type S pitot tube
coefficients obtained by single-velocity calibration at 915 m/min  (3,000 ft/min)
will generally be  valid to ±3 percent for the measurement  of velocities above 305
m/min  (1,000 ft/min) and to ±5  to 6 percent for the measurement of velocities
between 180 and 305 m/min  (600 and 1,000 ft/min). If a more precise correlation
between Cp and velocity is desired,   the flow system shall have the capacity to
generate at least  four distinct, time-invariant test-section velocities covering
the velocity range from 180 to 1,525 m/min  (600 to 5,000 ft/min), and calibration
data shall be  taken at regular velocity intervals over this range  (see Citations
9 and  14 in the Bibliography for  details).

4.1.2.4  Two entry ports, one each for the standard  and Type S pitot tubes,  shall
be  cut in  the  test  section; the standard  pitot  entry  port shall  be located
slightly downstream  of the Type S port, so that the standard and  Type S impact
openings  will lie in  the  same cross-sectional plane during calibration.   To
facilitate alignment  of the pitot tubes during calibration, it  is advisable that
the test section be constructed  of plexiglas or some other transparent material.

4.1.3  Calibration Procedure.  Note that this procedure is a general one and must
not be used without  first referring to the special considerations presented in
Section  4.1.5.  Note also that this procedure  applies only  to single-velocity
calibration.   To  obtain calibration data  for the  A and B sides  of  the Type S
pitot  tube, proceed  as follows:

4.1.3.1  Make  sure that the manometer is properly filled and that the oil is free
from contamination  and is of the proper  density.    Inspect and leak-check all
pitot  lines; repair  or replace  if necessary.

4.1.3.2  Level and zero the manometer.  Turn on the fan, and allow the flow to

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EMTIC TM-002                     NSPS TEST METHOD                        Page 7


stabilize.  Seal the Type S  entry port.

4.1.3.3  Ensure that the manometer  is level  and  zeroed.   Position the standard
pitot tube at  the calibration point  (determined as outlined in Section 4.1.5.1),
and align the  tube  so that its tip is pointed  directly into the flow.  Particular
care should be taken in aligning the tube to avoid yaw and pitch angles.   Make
sure that the entry port surrounding the tube is properly sealed.

4.1.3.4  Read  Apstd,  and record its value in a  data table similar to the one  shown
in Figure 2-9.  Remove the standard  pitot tube from the duct,  and disconnect it
from the manometer.  Seal the standard entry port.

4.1.3.5  Connect the Type S pitot tube to the manometer.   Open the Type S  entry
port.   Check  the manometer level and zero.   Insert  and  align the  Type S  pitot
tube so that its A  side impact opening is at  the  same point as was the standard
pitot tube and is pointed directly into the  flow.  Make sure that  the  entry port
surrounding the tube is properly sealed.

4.1.3.6   Read Aps,  and enter its value in the data table.   Remove  the Type S
pitot tube from the duct, and disconnect it  from the manometer.

4.1.3.7   Repeat  Steps 4.1.3.3  through 4.1.3.6  above until three pairs  of Ap
readings have been obtained.

4.1.3.8  Repeat Steps 4.1.3.3 through 4.1.3.7 above  for  the B side of the Type
S pitot tube.

4.1.3.9  Perform calculations,  as described  in Section 4.1.4 below.

4.1.4  Calculations.

4.1.4.1  For each of the six pairs  of Ap readings  (i.e.,  three from  side  A and
three from side B)  obtained  in  Section 4.1.3 above,  calculate the value of
the Type S pitot tube coefficient as follows:
                              C   =C
                               P(s)   p(std),
                                                                         Eq. 2-2
        Where:

        Cpls,       =    Type S pitot tube coefficient.

        Cp(5tdS      =    Standard  pitot  tube   coefficient;   use   0.99   if  the
                       coefficient is unknown  and the tube is designed according
                       to  the  criteria of  Sections  2.7.1  to  2.7.5  of  this
                       method.

        APutd      =    Velocity  head measured by  the  standard pitot tube,  cm
                       (in.) H20.

        Aps       =    Velocity head measured  by the Type S pitot tube,  cm (in.)
                       H20.

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EMTIC TM-002                     NSPS TEST HETHOD                        Page 8


4.1.4.2  Calculate ^, (side A), the mean A-side coefficient,  and C"p (side  B),  the
mean  B-side coefficient;  calculate  the difference between  these two  average
values.

4.1.4.3  Calculate the deviation of  each of  the  three A-side  values  of
CfW from Cp (side A) , and the deviation of each B-side values of Cp(s) from
Cp (side B).  Use the following equation:


                        Deviation = C    -C~(A or B)
                                                                  Eq. 2-3

4.1.4.4  Calculate a, the average deviation  from  the mean,  for  both  the  A and B
sides of the pitot tube.  Use the following equation:
                  a (side A or B)  =
                                                                  Eq. 2-4

4,1.4.5  Use the Type  S pitot tube  only  if  the  values  of  a (side  A)  and o (side
B) are  less than or equal to 0.01 and if  the  absolute value  of  the difference
between C"p (A)  and C~p  (B)  is 0.01 or  less.

4.1.5  Special Considerations.

4.1.5.1  Selection of Calibration  Point.

4.1.5.1.1  When an isolated Type S pitot  tube is calibrated, select a calibration
point at or near  the  center of the duct, and follow the  procedures  outlined in
Sections  4.1.3 and 4.1^4 above.   The Type S pitot coefficients so  obtained,
i.e.,  Cp  (side  A)  and Q  (side  B), will be  valid,  so long as either:  (1)  the
isolated pitot  tube is used; or (2)  the pitot tube  is used with other components
(nozzle,  thermocouple,   sample  probe)  in   an  arrangement  that  is free  from
aerodynamic interference  effects  (see Figures  2-6  through 2-8).

4.1.5.1.2   For  Type  S  pitot  tube-thermocouple  combinations (without  sample
probe),  select  a calibration point at or  near the center of the duct, and follow
the procedures  outlined in Sections 4.1.3 and 4.1.4 above.   The coefficients so
obtained will be valid so  long as the pitot  tube-thermocouple combination is  used
by itself or with other components  in an interference-free arrangement (Figures
2-6 and 2-8),

4.1.5.1.3   For  assemblies with  sample probes,  the calibration point  should be
located at or near the center of the  duct;  however, insertion  of  a probe sheath
into a small duct may  cause significant  cross-sectional area blockage and yield
incorrect  coefficient values  (Citation  9 in the Bibliography).  Therefore,  to
minimize  the blockage effect,  the calibration point  may be a few  inches  off-

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EMTIC TM-002                      NSPS TEST METHOD                       Page 9


center if  necessary.   The  actual  blockage effect will be  negligible when the
theoretical  blockage,  as  determined by  a projected-area  model of  the  probe
sheath, is  2 percent or less  of the duct cross-sectional  area  for assemblies
without external  sheaths (Figure 2-lQa), and 3 percent or  less  for assemblies
with external sheaths  (Figure  2-lOb).

4.1.5.2  For those probe assemblies  in which pitot tube-nozzle interference is
a factor (i.e.,  those in  which  the pitot-nozzle separation distance fails to meet
the specification  illustrated in  Figure 2-6A), the  value of Cp!sl depends upon the
amount of  free-space between the  tube and nozzle, and therefore is a function of
nozzle size.  In these  instances, separate calibrations shall be  performed with
each of the commonly used nozzle  sizes in place.   Note that  the single-velocity
calibration  technique  is acceptable  for  this purpose, even  though the larger
nozzle  sizes (>0.635  cm or 1/4  in.)  are not  ordinarily  used  for isokinetic
sampling at velocities  around 915 m/rain  (3,000 ft/min),  which is the calibration
velocity;  note  also that  it  is  not necessary to draw an isokinetic sample during
calibration  (see  Citation  19 in  the  Bibliography).

4.1.5.3 For a  probe assembly constructed such that its  pitot tube is always used
in the same orientation,  only one side of the pitot tube need be calibrated (the
side which will face the flow).   The pitot  tube  must  still meet the alignment
specifications  of  Figure  2-2 or 2-3, however,  and must have an average deviation
(a) value of 0.01 or less  (see Section 4.1.4.4.1

4.1.6  Field Use and Recalibration.

4.1.6.1  Field Use.

4.1.6.1.1   When a  Type  S  pitot  tube  (isolated or in an assembly)  is used in the
field,  the  appropriate  coefficient  value  (whether  assigned  or  obtained  by
calibration) shall be used to perform velocity calculations.  For calibrated Type
S pitot tubes,  the A side coefficient  shall be used when  the A side of the tube
faces the flow, and the  B  side coefficient shall  be used when the B side faces
the flow;  alternatively,  the arithmetic/average  of the A  and B side coefficient
values may be used, irrespective of  which side  faces the flow.

4.1.6.1.2   When a  probe assembly  is used to sample  a small duct,  30.5 to 91.4 cm
(12 to 36  in.)  in  diameter,  the probe sheath sometimes blocks a significant part
of the duct cross-section,  causing a reduction in the effective  value of Cp(H),
Consult Citation 9 in the Bibliography for details.  Conventional  pitot-sartipling
probe assemblies  are not recommended for use in  ducts having inside diameters
smaller than 30.5 cm (12 in.)  (see Citation 16  in the Bibliography).

4.1.6.2  Recalibration.

4.1.6.2.1   Isolated Pitot Tabes.  After each  field use, the  pitot tube shall be
carefully  reexamined in top, side, and end views.   If the pitot face openings are
still aligned within the  specifications illustrated in Figure 2-2  or 2-3, it can
be assumed that  the baseline coefficient of the pitot tube has not changed.  If,
however,  the tube has been damaged  to the extent that it  no  longer meets the
specifications  of  the Figure 2-2  or 2-3,  the  damage shall either  be repaired to
restore proper alignment of the  face  openings,  or the tube  shall be discarded.

4.1.6.2.2   Pitot Tube Assemblies. After each field use, check the face opening
alignment  of the  pitot  tube,  as in Section 4.1.6.2.1;  also,   remeasure  the
intercomponent  spacings of the  assembly.  If the intercomponent spacings have not

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EMTIC TM-002                     NSPS TEST METHOD                      Page 10


changed and the  face opening alignment is  acceptable, it can be assumed that the
coefficient of the assembly has not changed.  If the face opening alignment is
no longer  within the specifications  of  Figure  2-2 or 2-3,  either  repair the
damage or replace the pitot tube  (calibrating the new assembly, if necessary).
If the intercomponent spacings have changed, restore the original spacings, or
recalibrate the assembly.

4.2  Standard Pitot Tube (if applicable).   If a standard pitot tube is used for
the velocity traverse, the tube shall be constructed according to the criteria
of Section 2.7 and shall be assigned a baseline coefficient value of 0.99.  If
the standard pitot tube is used as part of an assembly, the tube shall be in an
interference-free arrangement (subject to the approval of the Administrator).

4,3   Temperature Gauges.  After  each  field use,  calibrate dial thermometers,
liquid-filled bulb thermometers, thermocouple-potentiometer systems, and other
gauges  at  a  temperature  within  10 percent  of  the  average  absolute  stack
temperature.  For temperatures up to 405"C (761°F), use an ASTM mercury-in-glass
reference thermometer, or equivalent, as a  reference; alternatively, either
a reference thermocouple and potentiometer  (calibrated by NBS) or thermometric
fixed  points,   e.g.,  ice bath  and  boiling water  (corrected  for  barometric
pressure)  may  be used.   For  temperatures above  405°C  (761°F),  use  an NBS-
calibrated  reference  thermocouple-potentiometer  system  or  an  alternative
reference, subject to the approval of the Administrator.

If, during calibration, the absolute temperature measured with the gauge being
calibrated and the reference gauge agree within 1.5 percent,  the temperature data
taken in the field shall be considered valid.  Otherwise, the pollutant emission
test shall either be considered invalid  or  adjustments (if appropriate) of the
test results shall be made, subject to the  approval of the Administrator.

4.4  Barometer.   Calibrate the barometer used against a mercury barometer.

5.  CALCULATIONS
                                       /
Carry out calculations, retaining at least one extra decimal figure beyond that
of the acquired data.  Round off figures after final calculation.

5.1  Nomenclature.

          A    =    Cross-sectional area of stack, m2 (ft2) .

          Bws   =    Water vapor  in the gas stream (from Method 5 or Reference
                    Method 4),  proportion  by volume.

          Cp   =    Pitot tube coefficient, dimensionless.

          Kp   =    Pitot tube constant,
                     34.97
                             sec
                                   (g/g-mole) (nunHg)
(mmH,0)
                                                2
                                                       1/2
for the metric system.

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EMTIC TM-002
             NSPS TEST METHOD
Page 11
                    85.49
       ft
      sec
                                Ib/lb-mole)  (in.Hg)
                                          (in.H20)
                                                        1/2
for the English system.
          Md   •=    Molecular weight of stack gas,  dry basis (see Section 3.6),
                    g/g-mole  (Ib/lb-mole).

          Ms   =    Molecular weight of stack gas,  wet basis,  g/g-mole (Ib/lb-
                    mole).

                            = Md(l-Bws)  +  18.0Bws
                                                                 Eq. 2-5

                    Barometric pressure at measurement site,  mm Hg (in.  Hg)

                    Stack static pressure, mm Hg (in.  Hg).

                    Absolute stack pressure,  mm Hg (in.  Hg),
                                 =  P    + P
                                     bar    g
          t,

          T.
                                             Eq. 2-6
Standard absolute pressure,  760 mm Hg (29.92 in.  Hg) .

Dry volumetric stack  gas  flow rate corrected  to  standard
conditions,  dsmVhr  (dscf/hr) .

Stack temperature,  °C  (8F).

Absolute stack temperature,  °K (°R) .


              = 273 + t.
for metric.
                                  = 460 + t
                                                                 Eq. 2-7
for English.
                                                                 Eq. 2-8
                    Standard absolute temperature,  293°K (528°R).

                    Average stack gas velocity,  m/sec (ft/sec).

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EMTIC TM-002
                            NSPS TEST METHOD
              Page 12
          Ap   =    Velocity head of stack gas, ram HS0 (in.  H20) .

          3,600=    Conversion factor, sec/hr.

          18.0 =    Molecular weight of water, g/g-mole  (Ib/lb-raole).

5.2  Average Stack Gas Velocity.
                          v  = K C
                           s    p p
                                           g»
                                          s(avg)

                                          P M
                                            s s
5.3  Average Stack Gas Dry Volumetric Flow Rate.
                    Qsd = 3,600(l~Bws)vsA  -
                                                std
                                              s (avg)
                                                  "std
                                                                  Eq.  2-9
                                                                  Eq.  2-10
BIBLIOGRAPHY
1.


2.


3.
5.


6.


7.

8.

9.
Mark, L.S.  Mechanical  Engineers'  Handbook.   New York.  McGraw-Hill Book
Co., Inc.  1951.

Perry.  J.H.   Chemical Engineers' Handbook.   New York.  McGraw-Hill Book
Co., Inc.  1960.

Shigehara,  R.T.,  W.F. Todd,  and W.S.  Smith.  Significance  of Errors in
Stack  Sampling  Measurements.    U.S.  Environmental   Protection  Agency,
Research Triangle Park, N.C,   (Presented at the Annual Meeting of the Air
Pollution Control Association, St. Louis, MO., June 14-19, 1970).

Standard Method for  Sampling Stacks for Particulate Matter.  In: 1971 Book
of ASTM  Standards,  Part 23.  Philadelphia,  PA.   1971.  ASTM Designation
D 2928-71.

Vennard,  J.K.   Elementary Fluid Mechanics.  New York.  John Wiley and Sons,
Inc.  1947.
Fluid  Meters  -  Their  Theory  and  Application.
Mechanical Engineers, New York, N,Y.  1959.
American  Society  of
ASHRAE Handbook of Fundamentals.  1972.  p. 208.

Annual Book of ASTM Standards, Part 26.  1974.  p. 648.

Vollaro,  R.F.   Guidelines for Type S Pitot Tube  Calibration.   U.S.
Environmental Protection Agency, Research Triangle Park, N.C.   (Presented
at   1st  Annual   Meeting,    Source   Evaluation  Society,   Dayton,  OH,
September 18, 1975.)

-------
EMTIC TM-002                     NSPS TEST METHOD                      Page 13


10.  Vollaro, R.F.  A Type S Pitot Tube Calibration Study.  U.S. Environmental
     Protection Agency,  Emission Measurement Branch,  Research  Triangle Park,
     N.C.  July 1974.

11.  Vollaro, R.F.  The Effects of Impact Opening Misalignment on the Value of
     the Type S Pitot Tube Coefficient.  U.S. Environmental Protection Agency,
     Emission Measurement Branch, Research Triangle Park, NC.  October 1976.

12.  Vollaro, R.F.  Establishment of a Baseline Coefficient Value for Properly
     Constructed  Type  S Pitot Tubes.  U.S.  Environmental Protection Agency,
     Emission Measurement Branch, Research Triangle Park, NC.  November 1976,

13.  Vollaro, R.F.   An Evaluation of Single-Velocity Calibration Technique as a
     Means of  Determining  Type  S Pitot Tube Coefficients.  U.S. Environmental
     Protection Agency,  Emission Measurement  Branch, Research Triangle Park, NC.
     August  1975.

14.  Vollaro,  R.F.   The Use of Type S Pitot  Tubes  for the Measurement of Low
     Velocities.   U.S.  Environmental  Protection  Agency,  Emission Measurement
     Branch,  Research Triangle Park, NC.  November 1976.

15.  Smith, Marvin L.  Velocity Calibration of EPA Type Source Sampling Probe.
     United Technologies Corporation, Pratt and Whitney Aircraft Division, East
     Hartford, CT.  1975.

16.  Vollaro, R.F.   Recommended Procedure for Sample Traverses in Ducts Smaller
     than 12  Inches  in Diameter.  U.S.  Environmental Protection Agency, Emission
     Measurement Branch, Research Triangle Park,  NC.  November 1976.

17.  Ower,  E. and R.C. Pankhurst.  The Measurement of Air Flow, 4th Ed. London,
     Pergamon Press.  1966.

18.  Vollaro, R.F.  A Survey of Commercially Available Instrumentation for the
     Measurement  of Low-Range Gas Velocities.   U.S.  Environmental Protection
     Agency,    Emission   Measurement  Branch,  Research   Triangle   Park,   NC,
     November 1976. (Unpublished Paper).

19.  Gnyp, A.M.,  C.C.  St.  Pierre, D.S. Smith, D. Mozzon,  and J.  Steiner. An
     Experimental Investigation  of  the Effect of Pitot  Tube-Sampling Probe
     Configurations on  the Magnitude  of the S Type  Pitot Tube Coefficient for
     Commercially Available Source Sampling Probes.  Prepared by the University
     of  Windsor  for  the  Ministry  of  the  Environment,  Toronto,  Canada.
     February 1975.

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EMTIC TM-002
                            NSPS TEST  METHOD
Page  14
   1.90-2.54 cm'
   (0.75-1.0 !n.)

_ 7.62 cm (3 In.)' _
                            Temperature Sensor
                          y
                                Type S PIW Tube
                * Suggested (Interference Free)
                Pilot tube/Thetmocoup^e Spacing
Figure  2-1.   Type S  pitot tube  manometer  assembly.

-------
EMTIC TM-002
NSFS  TEST METHOD
Page  15
                Transverse
                 Tube Axis
         Longitudinal
          Tube Axis
                                                   A-Side Plane
                  T
                                                   B-Sida Plane
                                              (b)
                                                                         (a) end vlaw; faca opening planes perpendicular
                                                                           to transverse arts;

                                                                         (b) lop view; face opening planes parallel la
                                                                         (c) 6lda view: both legs of equal langth and
                                                                           cantertines coinadort. when wowed from
                                                                           both sides. Baseline coefficient values of
                                                                           O.EM may be assigned lo pilot tubes con-
                                                                           struoed Ms way
Figure  2-2.    Properly  constructed  Type  S pitot  tube.

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EMTIC TM-002
NSFS TEST METHOD
Page 16
                                              OL
                         G_
                        — — — — — -C-~J^~~~•    ~\n~^f-"F^T'  ,v^
Figure 2-3.  Types  of  face-opening misalignment that can result  from  field use
or  improper construction  of Type  S pilot tubes.   These will  not affect  the
baseline value of Cp(s) so long as a1 and a? &1Q", p1 and £2 s58, z 50.32  cm {1/8
in.) and w sO.08  cm (1/32  in.)  (citation 11 in Bibliography).

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EMTIC TM-002
NSPS TEST METHOD
Page 17

k 	 \_j


<->
-•c
L
n • ->\
\y 	 i "^Cs
Cmvedcr \
Mitered Junction

Static
Holot
HUD) \^
Hemispherical
Tip N.

1

• *•



_

   Figure 2-4.   Standard pitot tube  design specifications

-------
EMTIC TM-002                     NSPS TEST METHOD                      Page  18

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EMTIC TM-002
                  NSPS TEST METHOD
                                Page 19
PLANT
DATE _
RUN NO.
STACK DIA. OR
DIMENSIONS, m (in.)  	  BAROMETRIC PRESS., mm  Hg
(in. Hg) 	CROSS SECTIONAL AREA, m2 (ft2)	
OPERATORS			
PITOT TUBE I.D. NO. 	
  AVG. COEFFICIENT, Cp =
  LAST DATE CALIBRATED
                                SCHEMATIC  OF  STACK
                                  CROSS  SECTION
Traverse
Pt. No.













Vel. Hd., ap
mm (in. ) H20













Stack Temperature
T,,
°C (°F)













Average
T8,
°K (°R)








/'





p,
mm Hg
(in.Hg)














(^P)1/2














                     Figure 2-5.  Velocity traverse data.

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EMTIC TM-002
NSPS TEST METHOD
Page 20
                          A. Bottom View; showing minimum pilot tube-nozzle separation.
                   Sampling
                    Probe
                  Static Pressure
                  Opening Plane
                         Types
                        Pilot Tube
                          B. Side View; to prevent pitot tube from Interfering with gas
                            flow streamlines approartilng the nozzle, the Impact pressure
                            opening plane of the pitot tube shall be even with or above the
                            nozzle antry plane.
  Figure 2-6.   Proper pitot tube-sampling  nozzle configuration to
  prevent  aerodynamic   interference;  button-hook   type   nozzle;
  centers of nozzle  and  pitot  opening  aligned;  Dt between  0.48  and
  0.95  cm  (3/16 and  3/8  in.).

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EMTIC TM-002
NSPS TEST METHOD
Page 21
               Temperature Sens«f
                                            Temp«rafure
                                                        .
                     Types Pilot Tutm
                                                  Typn S PHol Tube
                                          MI* I
                              z>
   Figure  2-7.     Proper  thermocouple  placement   to  prevent
   interference; Dt between 0.48  and 0.95 cm  (3/16 and 3/8 in.)-

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EMTIC TM-002
NfSPS TEST METHOD
Page  22
                                 Type SPilol TUbe
                      JCL
                       Sampfe Probe
  Figure  2-8.   Minimum pitot-sample probe separation needed to
  prevent interference;  Dt between 0.48 and  0.95  cm (3/16 and 3/8
  in.) .

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EMTIC TM-002
NSPS TEST METHOD
         Page 23
FITOT TUBE IDENTIFICATION NUMBER:
         DATE:
CALIBRATED BY:

RUN NO.
1
2
3
"A" SIDE CALIBRATION
AP«d
cm H2O
(in H20)




aP|->
cm H20
(in H20)



p
wp,avg
(SIDE A)
Cp<»i





Deviation
CDfa, - C0
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EMTIC TM-002
          NSPS TEST METHOD
Page 24
          w
                                                (b)
   Figure  2-10,
   assemblies.
Projected-area models  for  typical  pitot tube

-------
                  EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
                                   NSPS TEST METHOD
                  Method 3B - Gas Analysis for the Determination of
                    Emission Rate Correction Factor or Excess Air
1.  APPLICABILITY AND PRINCIPLE

1.1  Applicability.

1,1.1  This method is applicable for determining carbon dioxide (C02), oxygen  (02).
and carbon monoxide (CO) concentrations of a sample from a gas stream of a fossil -
fuel combustion process for excess air or emission rate correction factor
calculations.

1.1.2  Other methods, as well as modifications to the procedure described herein,
are also applicable for all of the above determinations. Examples of specific
methods and modifications include:  (Da multi-point sampling method using an Orsat
analyzer to analyze individual grab samples obtained at each point,  and  (2) a method
using COZ or 02 and stoichiometric calculations to determine excess air.   These
methods and modifications may be used, but are subject to the approval of the
Administrator, U.S. Environmental Protection Agency (EPA),

1.1.3  Note.  Mention of trade names or specific products does not constitute
endorsement by EPA.

1.2  Principle.  A gas sample is extracted from a stack by one of the following
methods:  (1) single-point, grab sampling; (2) single-point,  integrated  sampling;  or
(3) multi-point, integrated sampling.  The gas sample is analyzed for percent C02,
percent 02,  and,  if necessary,  percent CO.  An  Orsat  analyzer must be  used  for  excess
air or emission rate correction factor determinations.

2.  APPARATUS

The alternative sampling systems are the same as those mentioned in  Section 2 of
Method 3.

2.1  Grab Sampling and Integrated Sampling.  Same as in Sections 2.1 and 2.2,
respectively, of Method 3.

2.2  Analysis.  An Orsat analyzer only.  For low COZ  (less than  4.0  percent) or high
02 (greater  than  15.0  percent)  concentrations,  the measuring burette of the Orsat
must have at least 0.1 percent subdivisions.   For Orsat maintenance  and  operation
procedures,  follow the instructions recommended by the manufacturer, unless
otherwise specified herein.

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Prepared by Emission Measurement Branch                                 EKTIC  TM-003B
Technical Support Division, OAQPS, EPA                                   May 15.  1990
EMTIC TM-003B                  EWTIC NSPS TEST METHOD                          Page 2
3.  PROCEDURES

Each of the three procedures below shall be used only when specified in an
applicable subpart of the standards.  The use of these procedures for other purposes
must have specific prior approval of the Administrator.
Mote:  A Fyrite-type combustion gas analyzer is not acceptable for excess air or
emission rate correction factor determinations, unless approved by the
Administrator.  If both percent C02 and  percent 02 are measured, the analytical
results of any of the three procedures given below may also be used for calculating
the dry molecular weight (see Method 3).

3.1  Single-Point, Grab Sampling and Analytical Procedure.

3.1.1  The sampling point in the duct shall be as described in Section 3.1 of Method
3.

3.1.2  Set up the equipment as shown in Figure 3-1 of Method 3, making sure all
connections ahead of the analyzer are tight.  Leak check the Orsat analyzer
according to the procedure described in Section 6 of Method 3.  This leak check  is
mandatory.

3.1.3  Place the probe in the stack, with the tip of the probe positioned at the
sampling point; purge the sampling line long enough to allow at least five
exchanges.  Draw a sample into the analyzer.  For emission rate correction factor
determinations, immediately analyze the sample, as outlined in
Sections 3.1.4 and 3.1.5, for percent C02  or percent Q2.  If excess air is desired,
proceed as follows: (1) immediately analyze the sample,  as in Sections 3.1.4 and
3.1.5, for percent C02,  02. and CO; (2) determine the percentage of the gas that  is N?
by subtracting the sum of the percent C02,  percent  02,  and percent CO from 100
percent, and (3) calculate percent excess air as outlined in Section 4.2.

3.1.4  To ensure complete absorption of the C02,  02, or if applicable, CO. make
repeated passes through each absorbing solution until  two consecutive readings are
the same.  Several passes (three or four)  should be made between readings.  (If
constant readings cannot be obtained after three consecutive readings, replace the
absorbing solution.)  Note:  Since this single-point,  grab sampling and analytical
procedure is normally conducted in conjunction with a  single-point, grab sampling
and analytical procedure for a pollutant,  only one analysis is ordinarily conducted.
Therefore, great care must be taken to obtain a valid  sample and analysis.  Although
in most cases, only C02 or 02 is required, it is recommended that both COZ and 02 be
measured, and that Section 3.4 be used to validate the analytical data.

3.1.5  After the analysis is completed,  leak check (mandatory) the Orsat analyzer
once again, as described in Section 6 of Method 3.  For the results of the analysis

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to be valid, the Orsat analyzer must pass this leak test before and after the
analysis.
EMTIC TM-003B                   EMTIC  NSPS TEST  METHOD                          Page 3
3.2  Single-Point, Integrated Sampling and Analytical Procedure,

3.2.1  The sampling point in the duct shall be located as specified
in Section 3.1.1.

3.2.2  Leak check (mandatory) the flexible bag as in Section 2.2,6 of
Method 3.  Set up the equipment as shown in Figure 3-2 of Method 3. Just before
sampling, leak check (mandatory) the train as described in Section 4.2 of Method 3.

3.2.3  Sample at a constant rate, or as specified by the Administrator.  The
sampling run must be simultaneous with, and for the same total length of time as,
the pollutant emission rate determination.  Collect at least 30 liters (1.00 ft3)  of
sample gas.  Smaller volumes may be collected, subject to approval of the
Administrator.

3.2.4  Obtain-one integrated flue gas sample during each pollutant emission rate
determination.  For emission rate correction factor determination, analyze the
sample within 4 hours after it is taken for percent C02 or percent 02 (as outlined in
Sections 3.2.5 through 3.2.7). The Orsat analyzer must be leak checked (see Section
6 of Method 3) before the analysis.  If excess air is desired, proceed as follows:
(1) within 4 hours after the sample is taken, analyze it (as in Sections 3.2.5
through 3.2.7) for percent C02,  Oz, and CO; (2) determine the percentage of the gas
that is N2  by  subtracting the sum of  the  percent  C02, percent 02,  and percent CO from
100 percent; and (3) calculate percent excess air, as outlined in Section 4.2.

3.2.5  To ensure complete absorption of the COZ,  02, or if applicable, CO, follow the
procedure described in Section 3.1.4.  Note:   Although in most instances only C02 or
02 is  required,  it is  recommended that  both C02 and Oz be measured, and  that Section
3.4.1 be used to validate the analytical  data.

3.2.6  Repeat the analysis until the following criteria are met:

3.2.6.1  For percent C02,  repeat the  analytical procedure  until  the results  of any
three analyses differ by no more than (a) 0.3 percent by volume when C02  is  greater
than 4.0 percent or (b) 0.2 percent by volume when CO;,  is  less  than or  equal  to 4.0
percent.  Average three acceptable values of percent C02,  and  report the  results  to
the nearest 0.1 percent,

3.2.6.2  For percent 02,  repeat  the analytical procedure  until  the results  of any
three analyses differ by no more than (a) 0.3 percent by volume when Oz is  less than
15.0 percent or (b)  0.2 percent by volume when 02 is  greater than  or equal  to 15.0
percent.  Average the three acceptable values of percent 02. and  report the  results

-------
to the nearest 0.1 percent.

3.2.6.3  For percent CO, repeat the analytical procedure until the results of any
three analyses differ by no more than 0.3 percent.  Average the three acceptable
values of percent CO, and report the results to the nearest 0.1 percent.
EMTIC TM-003B                   EMTIC NSPS TEST METHOD                          Page 4
3.2.7  After the analysis is completed, leak check (mandatory) the Orsat analyzer
once again, as described in Section 6 of Method 3.  For the results
of the analysis to be valid, the Orsat analyzer must pass this leak test before and
after the analysis.

3.3  Multi -Point. Integrated Sampling and Analytical  Procedure.

3.3.1  The sampling points shall be determined as specified in Section 5.3 of Method
3.

3.3.2  Follow the procedures outlined in Sections 3.2.2 through 3.2.7, except for
the following:  Traverse all sampling points, and sample at each point for an equal
length of time.  Record sampling data as shown in Figure 3-3 of Method 3.

3.4  Quality Control Procedures.

3.4.1  Data Validation When Both C02 and 02 Are Measured.  Although in most
instances, only C02 or 02 measurement is required, it is recommended that both C02 and
02 be  measured to provide a  check  on the quality  of the  data.   The  following  quality
control procedure is suggested. Note:  Since the method for validating the C02  and Oz
analyses is based on combustion of organic and fossil fuels and dilution of the gas
stream with air, this method does not apply to sources that (1) remove C02  or 02
through processes other than combustion, (2) add Oz  (e.g..  oxygen enrichment) and N2
in proportions different from that of air, (3) add COZ (e.g.,  cement or  lime  kilns),
or (4) have no fuel factor,  F0.  values  obtainable (e.g., extremely  variable waste
mixtures).  This method validates the measured proportions of C02 and  02 for fuel
type,  but the method does not detect sample dilution resulting from leaks during or
after sample collection.  The method is applicable for samples collected downstream
of most lime or limestone flue-gas desulfurization units as the COZ added or  removed
from the gas stream is not significant in relation to the total COZ concentration.
The C02 concentrations from  other  types of
scrubbers using only water or basic slurry can be significantly affected and would
render the F0 check minimally  useful.

3.4.1.1  Calculate a fuel factor,  F0> using  the following  equation:

                      20.9 - *02
                F0 = - •                                             Eq.  3B-1
where:

-------
        %Qt = Percent 02 by volume,  dry basis,

       2CQ2 - Percent C02 by volume,  dry basis.

      20.9 = Percent 02 by volume in ambient air.
EMTIC TM-003B                   EMTIC NSPS TEST METHOD                         Page 5
If CO is present in quantities measurable by this method, adjust the 02 and C02
values before performing the calculation for F0 as follows:
       3!C02(adj)  =  *C02 + XCO

        TO2(adj)  =  £02 - 0.5

where:

       ECO = Percent CO by volume, dry basis,
3.4.1.2  Compare the calculated F0 factor with the expected FD  values.  The  following
table may be used in establishing acceptable  ranges for the expected F0 if the fuel
being burned is known.  When fuels are burned in combinations, calculate the
combined fuel Fd and Fc factors  (as defined  in Method 19) according  to  the procedure
in Method 19, Section 5.2.3.  Then calculate the F0 factor as  follows:

                       0.209 Fd
                 FD = -                                             Eq. 3B-2
           Fuel type                                       F0 range
   Coal:   Anthracite and lignite 	 ......  1.016-1.130
           Bituminous	1.083 - 1.230

   Oil:    Distillate	1.260 - 1.413
           Residual 	  .....  1.210 - 1.370

   Gas:    Natural. ..................  1.600 - 1.836
           Propane	  1.434 - 1.586
           Butane	  .  1.405 - 1.553

   Wood.  .	1.000  -  1,120
   Wood bark	1.003  -  1.130

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3.4.1.3  Calculated F0  values,  beyond the  acceptable ranges shown in this table,
should be investigated before accepting the test results.   For example,  the strength
of the solutions in the gas analyzer and the analyzing technique should  be  checked
by sampling and analyzing a known concentration,' such  as air;  the fuel  factor should
be reviewed and verified.  An acceptability range of ±12 percent is appropriate for
the F0 factor  of mixed  fuels with  variable fuel  ratios.  The level of the emission
rate relative to the compliance level  should be considered in  determining if a
retest is appropriate,  i.e.;  if the measured emissions are much lower  or much
greater than the compliance limit,

EMTIC TM-003B                  EMTIC NSPS TEST METHOD                          Page 6
repetition of the test would not significantly change the compliance status of the
source and would be unnecessarily time consuming and costly,

4.  CALCULATIONS

4.1  Nomenclature.  Same as Section 5 of Method 3 with the addition of the
following:

         2EA = Percent excess air,

       0.264 - Ratio of Oz to N2 in air, v/v.

4.2  Percent Excess Air.  Calculate the percent excess air (if applicable) by
substituting the appropriate values of percent 02, CO,  and N2 (obtained from Section
3.1.3 or 3.2.4) into Equation 3B-3.

                        %0Z -  0,5  %CQ
          IEA =  -   x 100                        Eq. 3B-3
                  0.264 XN2 -
Note:  The equation above assumes that ambient air is used as  the source of Oz and
that the fuel does not contain appreciable amounts of N2 (as do coke oven or blast
furnace gases).  For those cases when appreciable amounts  of N2 are present  (coal.
oil, and natural gas do not contain appreciable amounts of N2) or when oxygen
enrichment is used, alternative methods,  subject to approval of the Administrator,
are required.

5.  BIBLIOGRAPHY

Same as Method 3.

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        EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
                         NSPS TEST METHOD
           Method 4 - Determination of Moisture Content
                          in Stack Gases
1.  PRINCIPLE AND APPLICABILITY

1.1  Principle.   A gas sample  is extracted at a  constant  rate  from
the  source;  moisture  is  removed  from  the  sample  stream  and
determined  either volumetrically or gravimetrically.

1.2  Applicability.   This  method is applicable for  determining the
moisture content of  stack gas.

I.Z.I  Two procedures are  given.  The first is a reference method,
for accurate determinations of moisture content  (such as are  needed
to  calculate emission data).   The  second  is  an  approximation
method, which  provides estimates of  percent moisture to aid  in
setting isokinetic  sampling  rates prior  to  a  pollutant  emission
measurement run.   The approximation method described herein is  only
a  suggested approach;  alternative means  for  approximating  the
moisture content,  e.g.,  drying tubes,  wet bulb-dry bulb  techniques,
condensation  techniques,   stoichiometric calculations,  previous
experience, etc., are  also acceptable.

1.2.2  The reference  method is often conducted simultaneously  with
a pollutant  emission measurement  run;  when  it  is,   calculation  of
percent isokinetic,  pollutant emission  rate,  etc., for the  run
shall  be  based  upon  the  results  of  the reference method or  its
equivalent;  these  calculations shall not be based upon  the results
of the approximation method, unless the  approximation method  is
shown,  to  the satisfaction of  the Administrator,  U.S. Environmental
Protection  Agency,  to  be  capable of  yielding results  within  1
percent H20 of the reference method.

1.2.3  Note:  The reference method may yield questionable results
Prepared by Emission Measurement Branch              EMTIC TM-004
Technical Support Division, OAQPS, EPA              July 11, 1989

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        EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
                         NSPS TEST METHOD
when applied  to  saturated gas streams or to streams that  contain
water  droplets.   Therefore,  when these conditions  exist or  are
suspected,  a second  determination  of the moisture content  shall be
made simultaneously  with  the reference method, as follows:  Assume
that the  gas stream  is  saturated.   Attach  a  temperature sensor
[capable of measuring  to  within l^C  (2°F) ] to the reference method
probe.   Measure  the stack gas temperature at each traverse point
(see Section 2.2.1}  during the  reference method  traverse; calculate
the average  stack gas temperature.   Next, determine the  moisture
percentage, either by:   (1) using  a psychrometric chart and making
appropriate corrections if stack pressure is different from that of
the chart,  or (2) using saturation vapor pressure tables.   In cases
where  the  psychrometric  chart or the  saturation  vapor  pressure
tables  are not applicable  (based on  evaluation of  the process),
alternative methods, subject to the approval of  the Administrator,
shall be used.

2.  REFERENCE METHOD

The  procedure  described  in  Method  5  for  determining   moisture
content is acceptable as  a reference method.

2.1  Apparatus.   A schematic  of  the  sampling  train used  in  this
reference method is shown in  Figure 4-1.  All components  shall be
maintained and calibrated according to the procedures in Method 5.

2.1.1  Probe.   Stainless  steel  or glass tubing,  sufficiently heated
to prevent water condensation, and equipped with a filter, either
in-stack (e.g., a plug of glass wool inserted into the end of the
probe)   or  heated out-stack (e.g., as described in Method 5),  to
remove  particulate  matter.   When stack conditions permit, other
metals  or plastic tubing  may be used for the probe, subject to the
approval of the Administrator.

2.1.2  Condenser.   See Method  5,  Section 2.1.7, for  a description
Prepared by Emission Measurement Branch              EMTIC TM-004
Technical Support Division, OAQPS, EPA              July  11,  1989

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EMTIC TM-004                     EMTIC NSPS TEST METHOD
                                                            Page  3
of an acceptable type of  condenser and for alternative measurement
systems.

2.1.3  Cooling  System.   An ice bath container and crushed ice  (or
equivalent), to aid  in condensing moisture.

2.1.4  Metering System.   Same as in Method 5,  Section  2.1.8, except
do not  use  sampling systems designed for  flow  rates higher than
0.0283  rrvVmin   (1.0  cfm) .    Other metering  systems,  capable   of
maintaining  a   constant  sampling  rate  to  within 10  percent  and
determining  sample  gas  volume to within 2 percent,  may be  used,
subject to the  approval  of the Administrator.

2.1.5  Barometer.  Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm  (0.1 in.) Hg.   See
NOTE in Method  5, Section 2.1.9.

2.1.6   Graduated Cylinder and/or Balance.   To  measure condensed
water and moisture caught in the silica gel to within 1 ml or  0.5
g.  Graduated cylinders  shall have subdivisions no greater than 2
ml.   Most  laboratory balances  are  capable  of weighing  to  the
nearest 0.5  g or less.   These balances are suitable for use  here.

2.2  Procedure.   The  following procedure  is  written for a condenser
system  (such as the  impinger system described in Section 2.1.7 of
Method  5)   incorporating  volumetric  analysis  to  measure   the
condensed moisture,  and silica  gel  and gravimetric  analysis  to
measure the moisture leaving the condenser.

2.2.1  Unless otherwise  specified by the Administrator, a minimum
of eight traverse points shall be used for circular stacks having
diameters less  than  0.61  m  (24 in.),  a minimum of nine points  shall
be used for  rectangular  stacks
having  equivalent  diameters  less  than  0.61  m  (24  in.),  and  a
minimum of twelve traverse points shall be used in all other cases.
The traverse points  shall  be  located according  to Method 1.   The
use  of   fewer   points   is  subject  to   the  approval  of   the
Administrator.   Select a  suitable probe and probe length such that
all  traverse points can  be  sampled.   Consider sampling  from
opposite sides
of the  stack  (four  total  sampling  ports)  for  large  stacks,   to
permit  use  of  shorter probe  lengths.   Mark  the  probe  with heat
resistant tape  or  by some  other method  to  denote the  proper
distance  into  the  stack  or duct for  each  sampling  point.    Place

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EMTIC TM-004                     1MTIC NSPS TEST METHOD
                                                           Page 4
known  volumes of  water  in the  first  two impingers.   Weigh and
record the  weight of  the  silica gel  to  the nearest  0.5  g, and
transfer the silica gel to the fourth impinger; alternatively, the
silica gel may first be transferred to the  impinger,  and the weight
of the silica gel plus impinger recorded.

2.2.2  Select a total sampling time such that a minimum total gas
volume of 0.60 scm (21  scf) will be collected,  at  a  rate no greater
than  0.021  mVmin (0.75  cfm) .   When  both moisture  content and
pollutant  emission  rate  are  to   be  determined,  the  moisture
determination shall be  simultaneous with,  and for the same  total
length  of  time  as,  the  pollutant  emission  rate  run,  unless
otherwise specified in an applicable subpart of the standards.

2.2.3  Set up the  sampling train as shown in Figure 4-1.  Turn on
the probe heater and (if applicable) the filter heating system to
temperatures of  about 120°C  (248°F), to prevent water  condensation
ahead  of  the  condenser;  allow  time  for  the  temperatures  to
stabilize.   Place  crushed ice in the  ice  bath  container.    It is
recommended,  but  not  required,  that  a  leak  check  be  done,  as
follows:   Disconnect  the  probe from  the  first impinger  or  (if
applicable)  from  the  filter  holder.  Plug the inlet  to the  first
impinger (or filter holder), and pull a 380 mm  (15  in.) Hg vacuum;
a lower vacuum may be used, provided that  it is  not  exceeded during
the test.   A leakage rate in excess of 4  percent of  the average
sampling rate or 0.00057 mVmin  (0.02 cfm), whichever  is less, is
unacceptable.  Following the leak check, reconnect the  probe to the
sampling train.

2.2.4  During the  sampling run, maintain a sampling rate within 10
percent  of  constant  rate, or as specified by the Administrator.
For each run,  record  the  data required on the example data  sheet
shown in Figure 4-2.  Be sure to record the dry gas meter reading
at  the beginning  and  end  of each  sampling time  increment and
whenever sampling  is halted.   Take other  appropriate  readings at
each sample point, at least once during each time  increment.

2.2.5   To  begin  sampling,  position the  probe tip  at the  first
traverse point.  Immediately start the pump,  and adjust the flow to
the desired rate.  Traverse  the cross  section,  sampling  at each
traverse point for an equal length  of  time.  Add more ice and, if
necessary,  salt  to maintain a  temperature  of  less than 20°C  {68°F)
at the silica gel  outlet.

2.2.6  After collecting the sample, disconnect the probe from the

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EMTIC TM-Q04                      EMTIC NSPS TEST METHOD
                                                            Page 5
filter  holder (or from  the  first impinger),  and conduct  a  leak
check  (mandatory) as described  in Section  2.2.3.   Record the leak
rate.   If the leakage rate exceeds the  allowable  rate,  the tester
shall either  reject  the  test results or shall correct  the sample
volume as in Section  6.3  of Method 5.  Next,  measure the volume of
the moisture condensed to the nearest ml.   Determine the increase
in weight of  the silica  gel (or  silica gel  plus  impinger)  to the
nearest 0.5 g.  Record this  information (see example data sheet,
Figure 4-3), and  calculate the moisture percentage, as described in
2.3 below.

2.2.7  A quality  control  check of  the volume metering system at the
field site is  suggested before collecting the sample following the
procedure in Method 5, Section  4.4.

2.3  Calculations.  Carry out the  following calculations, retaining
at least one extra decimal figure  beyond that of the acquired data.
Round off figures after  final calculation.

2.3.1  Nomenclature.

   Bws = Proportion of water  vapor, by volume, in the gas stream.

    Mw = Molecular  weight  of water,  18.0  g/g-mole  (18.0  Ib/lb-
         mole).
                                /
    Pra = Absolute pressure  (for I this method,  same as  barometric
         pressure)      at the  dry gas meter, mm Hg (in. Hg).

   Pstd = Standard absolute pressure,  760 mm Hg (29.92 in. Hg) .

    R = Ideal gas  constant,  0.06236  (mm  Hg) (m3) / (g-mole) (°K)  for
         metric  units  and  21.85  (in.  Hg) (ft3) / (Ib-mole) (°R)  for
         English  units.

    T,,, = Absolute temperature at meter,  °K  (°R).

   TEtd - Standard absolute temperature,  293°K (528°R) .

    Vra = Dry gas  volume measured by dry  gas meter,  dcm  (dcf).

   AVm = Incremental  dry  gas volume measured by  dry gas meter  at
         each  traverse  point,  dcm (dcf).

      - Dry gas volume measured by the dry  gas meter,  corrected  to

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EMTIC TM-004                      EMTTC NSPS TEST METHOD
                                                            Page 6
         standard conditions,  dscm (dscf).

      =  Volume of  water vapor  condensed,  corrected  to  standard
         conditions, scm (scf).

      =  Volume of water vapor collected in  silica gel,  corrected
         to  standard  conditions, scm (scf).

    Vf =  Final  volume of condenser water,  ml.

    VA =  Initial volume, if any,  of condenser water, ml.

    Wf =  Final  weight of  silica gel or silica  gel plus impinger, g.

    Wi =  Initial weight  of  silica gel  or silica gel plus impinger,
g.

    Y as  Dry gas meter calibration factor.

    pw =  Density of water,  0.9982 g/ml  (0.002201 Ib/ml).


2.3.2  Volume  of Water  Vapor  Condensed.

                            RT
           V      = (V -V )D    std
           vwc(std)  *vf  vi"~w p  M
Where:

    K! =  0.001333 mVml for metric units,

      -  0.04707  ftVml for English  units.


2.3.3  Volume of Water Collected in Silica Gel,

                    (Wf - W.) RT3td
           V
            wsg(std)      p  M
                         std w
                  = K2(Wf -W.)

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EMTIC TM-004                      1MTIC NSPS TEST METHOD
                                                            Page  7
Where:


    K2 =  0.001335 inVg  for  metric units,


      =  0.04715  ftVg  for  English units



2.3.4  Sample Gas Volume.
            V     = V Y
             m (std)    in  t p   \ / m \

                        ( stdM m)                           Eq. 4-3
                         vp
                   = K Y
                   ~" i\— J.
                      3

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EMTIC TM-004                     EMTIC NSPS TEST METHOD
                                                            Page 8
Where:

    K3  =  0.3858  °K/mm  Hg  for  metric units,

       =  17.64  °R/in,  Hg  for  English units.
NOTE:   If  the  post-test  leak  rate  (Section  2.2.6)  exceeds  the
allowable  rate,  correct  the  value  of Vm  in Equation  4-3,  as
described in Section  6.3 of Method 5.

2.3.5  Moisture Content.
          B      Vwc(std) +Vwsg(std)                           Eq.  4~4
           ws  V     + V      +V
               wc(std)  wsg(std)  m(std)
NOTE:   In saturated  or moisture  droplet-laden gas  streams,  two
calculations  of  the moisture  content of  the  stack gas  shall be
made, one  using  a  value based upon the  saturated  conditions  (see
Section 1.2),  and  another based upon the  results  of  the impinger
analysis.   The lower of  these two values  of Bws  shall be considered
correct.

2.3.6   Verification  of Constant  Sampling Rate.   For  each time
increment,  determine the AVm.  Calculate the average.  If the value
for  any  time increment  differs  from  the average by more than 10
percent, reject  the results, and repeat  the  run.

3.  APPROXIMATION METHOD

The  approximation  method described below  is presented  only as a
suggested method (see Section  1.2).

3.1  Apparatus.  See  Figure 4-4.

3.1.1  Probe.  Stainless steel  or glass tubing,  sufficiently heated
to prevent water condensation and equipped  with a filter (either
in-stack or heated  out-stack) to remove particulate matter.  A plug
of  glass  wool,  inserted  into  the  end  of  the  probe,  is  a
satisfactory  filter.

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EMTIC TM-004                      EMTIC NSPS TEST METHOD
                                                            Page 9
3.1.2  Impingers.  Two midget  impingers,  each with 30-ml capacity,
or equivalent.

3.1.3  Ice Bath.  Container and  ice,  to aid in condensing moisture
in impingers.

3.1.4  Drying Tube.  Tube packed with new or regenerated 6- to 16-
mesh indicating-type  silica gel (or  equivalent desiccant), to dry
the sample gas  and to protect the  meter and pump.

3.1.5  Valve.  Needle valve, to  regulate the sample gas flow rate.

3.1.6  Pump.   Leak-free,  diaphragm  type, or  equivalent,  to pull the
gas sample through the train.

3.1.7   Volume  Meter.   Dry gas meter,  sufficiently  accurate  to
measure the sample volume to within 2 percent,  and calibrated over
the range of flow rates and conditions actually encountered during
sampling.

3.1.8  Rate Meter.  Rotameter, to measure the flow range from 0 to
3 liters/min  (0  to 0.11  cfm).

3.1.9  Graduated Cylinder.  25-ml.

3.1.10   Barometer.   Mercury,   aneroid,  or  other barometer,  as
described in Section  2.1.5  above.

3.1.11   Vacuum  Gauge.' At  least 760-rom (30-in.)  Hg gauge,  to  be
used for the sampling leak  check.

3.2  Procedure.

3.2.1  Place exactly  5 ml water in each  impinger.   Leak check the
sampling train as follows:   Temporarily insert a vacuum  gauge at  or
near the probe inlet;  then,  plug the probe inlet, and pull a vacuum
of at least  250  mm (10 in.) Hg.  Note the  time rate of change  of
the dry gas meter dial; alternatively, a rotameter (0 to 40  cc/min)
may  be  temporarily  attached  to  the  dry  gas  meter  outlet  to
determine the leakage  rate.  A leak rate not in excess of 2  percent
of the  average  sampling  rate  is  acceptable.   NOTE:    Carefully
release the probe  inlet plug  before  turning off the pump.

3.2.2  Connect the  probe, insert it  into the stack,  and sample  at

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EMTIC TM-004                     EMTIC  NSPS TEST METHOD
                                                           Page 10
a constant  rate  of 2  liters/min  (0.071 cfm).   Continue  sampling
until  the  dry gas  meter registers about  30 liters  (1.1  ft3)  or
until  visible liquid  droplets are  carried over  from the  first
impinger to the second.   Record temperature,  pressure,  and dry gas
meter readings as required by  Figure  4-5.

3.2.3  After collecting the sample, combine the contents of the two
impingers, and measure  the volume  to  the nearest  0.5  ml.

3.3  Calculations.   The calculation method presented is designed to
estimate  the moisture  in  the  stack  gas;  therefore,   other  data,
which are only necessary for  accurate  moisture  determinations,  are
not  collected.   The following equations  adequately  estimate  the
moisture  content,  for  the  purpose  of   determining  isokinetic
sampling rate settings.

3.3.1  Nomenclature.

    B™ = Approximate proportion by  volume of  water vapor in the gas
         stream leaving  the  second impinger, 0.025.

    Bws = Water vapor in  the  gas stream, proportion  by volume.

     Mw - Molecular  weight of  water,  18.0  g/g-mole  (18.0  Ib/lb-
         mole).

     Pra - Absolute  pressure  (for this method,  same as  barometric
         pressure)  at  the dry  gas  meter, mm Hg (in. Hg).

   PHtd = Standard absolute pressure,  760 mm Hg (29.92 in.  Hg) .

     R = Ideal gas  constant, 0.06236  [(mm Hg)  [m3) ] / [ (g-mole) (°K) ]
         for metric units and 21.85 [(in. Hg) (ft3) ] / [ (lb-mole) (°R)]
         for English units.

     Tm = Absolute temperature  at meter, °K  (°R) .

   Tstd - Standard absolute temperature, 293°R  (528°R)  .

     Vf = Final volume  of impinger  contents,  ml.

     Vi = Initial volume  of impinger contents,  ml.

     Vm = Dry gas volume  measured by dry gas meter,  dcm (dcf).

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EMTIC TM-004                      EMTIC NSPS TEST METHOD
                                                           Page 11
       = Dry  gas volume measured  by dry gas meter,  corrected to
         standard conditions,  dscm (dscf ) .

     Y = Dry  gas meter  calibration factor.

     pw = Density of water, 0.9982 g/ml (0.002201 Ib/ml) .

3.3.2  Volume of Water  Vapor Collected.
                      PstdMw                               Eq.  4-5
Where:

     K! = 0.001333 mVml for metric units,

       - 0.04707 ftVml for English units

3.3.3  Gas Volume.
                        IP  I I  T
                       _12L   J_^d
                       r>    IT
                        stpd/ \   m /                         Eq.  4-6

                  = K.  V  -2L
                    i  mm
Where:

     K2 = 0.03858 °K/mm Hg for metric units,

       = 17.64 DR/in. Hg for English units.

3.3.4  Approximate Moisture Content.

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EMTic TM-004                     EJTTIC NSPS TEST METHOD
                                                           Page 12
                      Vwc
             B   = 	—	+B
              MS   y +V       *""
                    wcv m(std)                               Eq.  4-7

                      wc  -+(0.025)
                  V  +-V
                   wc m(std)
4.  CALIBRATION
4.1   For  the reference  method,  calibrate  the metering  system,
temperature gauges, and barometer according  to  Sections 5.3,  5.5,
and 5.7, respectively,  of  Method 5.   The  recommended leak check of
the metering  system  (Section  5.6 of  Method 5) also applies to the
reference method.  For  the approximation method,  use the procedures
outlined  in  Section  5.1.1 of Method 6 to calibrate  the metering
system, and  the  procedure of Method 5, Section 5.7,  to calibrate
the barometer.

5.  BIBLIOGRAPHY

1. Air Pollution Engineering  Manual  (Second  Edition).  Danielson,
   J.A. (ed.).  U.S.  Environmental Protection Agency, Office of Air
   Quality  Planning  and  Standards.   Research Triangle  Park,  NC.
   Publication No. AP-40.  1973.

2. Devorkin,  Howard, et al.   Air Pollution Source  Testing Manual.
   Air Pollution Control  District, Los  Angeles, CA.   November 1963.

3. Methods  for Determination of Velocity,  Volume, Dust  and  Mist
   Content  of  Gases.     Western  Precipitation  Division  of  Joy
   Manufacturing Co.   Los Angeles, CA.  Bulletin WP-50.   1968.

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EMTIC TM-004
EMTIC NSPS TEST METHOD
                                                                 Page 13
                             Condenser-Ice Bath Syslem Including Silica Gel Tute
  method.
                     Figure  4-1.   Moisture  sampling  train reference

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EMTIC TM-004                     EMTIC NSPS TEST METHOD
                                                          Page  14

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                Figure  4-2.   Field Moisture  Determination  Reference  Method.
Plant 	
Location.
Operator,
Date	
Run No. 	
Ambient temperature.
Barometric pressure.
Probe Length	
                                      SCHEMATIC OF STACK CROSS SECTION
Traverse
Pt. No.










Sampling
Time
(9) , min










Stack
Temperature
°C (°F)










Average
Pressure
differential across
orifice meter AH
mm (in.) H20











Meter
Reading gas
sample
volume
m3 (ft3)











AVm
m3
(ft3)











Gas sample
temperature at
dry gas meter
Inlet
Tmin
°C(°F)











Outlet
Tnw
°C{°F)











Temperature
of gas
leaving
condenser or
last
irapinger
°C(°F)












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EMTIC TM-004                          EMTIC NSPS TEST METHOD
                                                                       Page  16
                Figure 4-3.  Analytical data - reference method.

                                   Impinger          Silica gel
               	. volume. ml	weight, a
           Final
           Initial
           Difference

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EMTIC TM-004
EMTIC NSFS TEST METHOD
                                                          Page 17
  Figure  4-4.  Moisture  Samping  Train  - Approximation  Method,

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EMTIC TM-004
      EMTIC  NSPS TEST METHOD
                                                                        Page 18
           Figure 4-5.  Field Moisture Determination - Approximation Method.
Location.
Test	
Date	
Comment s:
Operator	
Barometric pressure_
Clock Time






Gas volume
through
meter, (VJ ,
m3 (ft3)






Rate meter
setting mVmin
(ftVmin)






Meter
temperature
0 C (° F)







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APPENDIX A TO PART 63--TEST METHODS
*  *  * * *
METHOD 315 - DETERMINATION OF PARTICIPATE AND METHYLENE CHLORIDE
EXTRACTABLE MATTER fMCENfl FROM SELECTED SOURCES
AT PRIMARY ALUMINUM PRODUCTION FACILITIES
       NQTE: This method does not include all of the specifications (e.g., equipment and supplies) and
procedures (e.g., sampling and analytical) essential to its performance. Some material is incorporated by
reference from other methods in this part. Therefore, to obtain reliable results, persons using this method
should have a thorough knowledge of at least the following additional test methods: Method lt Method
2, Method 3, and Method 5 of 40 CFRpart 60, appendix A,
1.0    Scope and Application.
       1.1  Analytes.  Particulate matter (PM).  No CAS number assigned. Methylene chloride
extractable matter (MCEM). No CAS number assigned.
       1.2  Applicability. This method is applicable for the simultaneous determination of PM and
MCEM when specified in an applicable regulation.  This method was developed by consensus with the
Aluminum Association and the U.S. Environmental Protection Agency (EPA) and has limited precision
estimates for MCEM; it should have similar precision to Method 5 for PM in 40 CFR part 60, appendix
A since the procedures are similar for PM.
       1.3  Data quality objectives. Adherence to the requirements of this method will enhance the
quality of the data obtained from air pollutant sampling methods.
2T0    Summary of Method.
       Particulate matter and MCEM are withdrawn isokinetically from the source. PM is collected on
a glass fiber filter maintained at a temperature in the range of 120 ± 14°C (248 ± 25°F) or such other
temperature  as specified by an applicable subpart of the standards or approved by the Administrator for a
particular application.  The PM mass, which includes any material that condenses on the probe and is
subsequently removed in an acetone rinse or on the filter at or above the filtration temperature, is
determined gravimetrically after removal of uncombined water. MCEM is then determined by adding a
methylene chloride rinse  of the probe and filter holder, extracting the condensable hydrocarbons
collected in the impinger water, adding an acetone rinse followed by a methylene chloride rinse of the
sampling train components after the filter and before the silica gel impinger, and determining residue
gravimetrically after evaporating the solvents.
3.0.    Definitions.  [Reserved]
4J)    Interferences.  [Reserved]
$&    Safety.
       This method may involve hazardous materials, operations, and equipment.  This method does not
purport to address all of the safety problems associated with its use.  It is the responsibility of the user of
this method to establish appropriate safety and health practices and determine the applicability of
regulatory limitations prior to performing this test method.
6.0 Equipment and Supplies.
       NOTE: Mention of trade names or specific  products does not constitute endorsement by the
EPA.
       6.1  Sample collection. The following items are required for sample collection:
       6.1.1 Sampling train.  A schematic of the sampling train used in this method is shown in Figure
5-1, Method 5,40 CFR part 60, appendix A.  Complete construction details are given in APTD-0581
(Reference 2 in section 17.0 of this method); commercial models of this train are also available. For
changes from APTD-0581 and for allowable modifications of the train shown in Figure 5-1, Method 5,40
CFR part 60, appendix, A see the following subsections,
       NOTE:  The operating and maintenance  procedures for the sampling train are described in
APTD-0576 (Reference 3 in section 17.0 of this  method).  Since correct usage is important in obtaining

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valid results, all users should read APTD-0576 and adopt the operating and maintenance procedures
outlined in it, unless otherwise specified herein. The use of grease for sealing sampling train components
is not recommended because many greases are soluble in methylene chloride. The sampling train
consists of the following components:
       6.1.1.1  Probe nozzle. Glass or glass lined with sharp, tapered leading edge.  The angle of taper
shall be <30°, and the taper shall be on the outside to preserve a constant internal diameter. The probe
nozzle shall be of the button-hook or elbow design, unless otherwise specified by the Administrator.
Other materials of construction may be used, subject to the approval of the Administrator. A range of
nozzle sizes suitable for isokinetic sampling should be available. Typical nozzle sizes range from 0.32 to
1.27 cm (1/8 to 1/2 in.) inside diameter (ID) in increments of 0.16 cm (1/16 in.). Larger nozzle sizes are
also available if higher volume sampling trains are used. Each nozzle shall be calibrated according to the
procedures outlined in section 10,0 of this method.
       6.1.1.2 Probe liner. Borosilicate or quartz glass tubing with a heating system capable of
maintaining a probe gas temperature at the exit end during sampling of 120 ± 14°C (248 ± 25°F), or such
other temperature as specified by an applicable subpart of the standards or approved by the
Administrator for a particular application. Because the actual temperature at the outlet of the probe is
not usually monitored during sampling, probes constructed according to APTD-0581 and using the
calibration curves of APTD-0576 (or calibrated according to the procedure outlined in APTD-0576) will
be considered acceptable.  Either borosilicate or quartz glass probe liners may be used for stack
temperatures  up to about 480°C (900°F); quartz liners  shall be used for temperatures between 480 and
900°C (900 and 1,650°F). Both types of liners may be  used at higher temperatures than specified for
short periods  of time, subject to the approval of the Administrator. The softening temperature for
borosilicate glass is 820°C (1,500°F) and for quartz glass it  is 1,500DC (2,700°F).
       6.1.1.3 Pitot tube.  Type S, as described in section 6.1 of Method 2,40 CFR part 60, appendix A,
or other device approved by the Administrator. The pitot tube shall be attached to the probe (as shown in
Figure 5-1 of Method 5, 40 CFR part 60, appendix A) to allow constant monitoring of the stack gas
velocity. The impact (high pressure) opening plane of the pitot tube shall be even with or above the
nozzle entry plane (see Method 2, Figure 2-6b, 40 CFR part 60, appendix A) during sampling.  The Type
S pitot tube assembly shall have a known coefficient, determined as  outlined in section 10.0 of Method 2,
40 CFR part 60, appendix A.
       6.1.1.4 Differential pressure  gauge. Inclined manometer or equivalent device (two), as described
in section 6.2 of Method 2,40 CFR part 60, appendix A. One manometer shall  be used for velocity head
(Dp) readings, and the other, for orifice differential pressure readings.
       6.1.1.5 Filter holder. Borosilicate glass, with a glass frit filter support and a silicone rubber
gasket The holder design shall provide a positive seal against leakage from the outside or around the
filter. The holder shall be attached immediately at the  outlet of the probe (or cyclone, if used).
       6.1.1.6 Filter heating system. Any heating system capable of maintaining a temperature around
the filter holder of 120 ± 14°C (248 ± 25°F) during sampling, or such other temperature as specified  by an
applicable subpart of the standards or approved by the  Administrator for a particular application.
Alternatively, the tester may opt to operate the  equipment at a temperature lower than that specified. A
temperature gauge  capable of measuring temperature to within 3°C (5.4°F) shall be installed so that the
temperature around the filter holder can  be regulated and monitored  during sampling. Heating systems
other than the one shown in APTD-0581 may be used.
       6.1.1.7 Temperature sensor. A temperature sensor capable of measuring temperature to within
±3°C (5.4°F) shall be installed so that the sensing tip of the temperature sensor is in direct contact with
the sample gas, and the temperature around the filter holder can be regulated and monitored during
sampling.
       6.1.1.8 Condenser. The following system shall be used to determine the stack gas moisture
content; four glass impingers connected in series with leak-free ground glass fittings. The first, third,

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and fourth impingers shall be of (he Greenburg-Smith design, modified by replacing the tip with a 1.3 cm
(1/2 in.) ID glass tube extending to about 1.3 cm (1/2 in.) from the bottom of the flask.  The second
impinger shall be of the Greenburg-Smith design with the standard tip. The first and second impingers
shall contain known quantities of water (section 8.3.1 of this method), the third shall be empty, and the
fourth shall contain a known weight of silica gel or equivalent desiccant. A temperature sensor capable
of measuring temperature to within 1°C (2°F) shall be placed at the outlet of the fourth impinger for
monitoring.
        6.1.1.9 Metering system. Vacuum gauge, leak-free pump, temperature sensors capable of
measuring temperature to within 3°C (5.4°F), dry gas meter (DGM) capable of measuring volume to
within 2 percent, and related equipment, as shown in Figure 5-1 of Method 5,40 CFR part 60, appendix
A. Other metering systems capable of maintaining sampling rates within 10 percent of isokinetic and of
determining sample volumes to within 2 percent may be used, subject to the approval of the
Administrator. When the metering system is used in conjunction with a phot tube, the system shall allow
periodic checks of isokinetic rates.
        6.1.1.10  Sampling trains using metering systems designed for higher flow rates than that
described in APTD-0581 or APTD-0576 may be used provided that the specifications of this method are
met.
        6.1.2  Barometer. Mercury, aneroid, or other barometer capable of measuring atmospheric
pressure to within 2,5 mm (O.I in.) Hg.
        NOTE: The barometric reading may be obtained from a nearby National Weather Service
station. In this case, the station value (which is the absolute barometric pressure) shall be requested and
an adjustment for elevation differences between the weather station and sampling point shall be made at
a rate of minus 2.5 mm (0.1 in) Hg per 30 m (100 ft) elevation increase or plus 2.5 mm (0.1 in) Hg per 30
m (100 ft) elevation decrease.
        6.1.3  Gas density determination equipment.  Temperature sensor and pressure gauge, as
described in sections 6.3 and 6.4 of Method 2,40 CFR part 60, appendix A, and gas analyzer, if
necessary, as described in Method 3, 40 CFR part 60, appendix A,  The temperature sensor shall,
preferably, be permanently attached to the pitot tube or sampling probe in a fixed configuration, such that
the tip of the sensor extends beyond the leading edge of the probe sheath and does not touch any metal.
Alternatively, the sensor may be attached just prior to use in the field. Note, however, that if the
temperature sensor is attached in the field, the sensor must be placed in an interference-free arrangement
with respect to the Type S pitot tube openings (see Method 2, Figure 2-4,40 CFR part 60, appendix A).
As a second alternative, if a difference of not more than 1 percent in the average velocity measurement is
to be introduced, the temperature sensor need not be attached to the probe or pitot tube. (This alternative
is  subject to the approval of the Administrator.)
        6.2 Sample recovery. The following items are required for sample recovery:
        6.2.1 Probe-liner and probe-nozzle brushes. Nylon or Teflon® bristle brushes with stainless
steel wire handles. The probe brush shall have extensions (at least as long as  the probe) constructed of
stainless steel, nylon, Teflon®, or similarly inert material.  The brushes shall be properly sized and
shaped to brush out the probe liner and nozzle.
        6.2.2 Wash bottles.  Glass wash bottles are recommended. Polyethylene or tetrafluoroethylene
(TFE) wash bottles may be used, but they may introduce a positive bias due to contamination from the
bottle. It is recommended that acetone not be stored in polyethylene or TFE bottles for longer than a
month.
       6.2.3  Glass sample storage containers. Chemically resistant, borosilicate glass bottles, for
acetone and methylene chloride washes and impinger water, 500 ml or 1,000 ml.  Screw-cap liners shall
either be rubber-backed Teflon® or shall be constructed so as to be leak-free and resistant to chemical
attack by acetone or methylene chloride. (Narrow-mouth glass bottles have been found to be less prone
to  leakage.) Alternatively, polyethylene bottles may be used.
       6.2.4  Petri dishes. For filter samples, glass, unless otherwise specified by the Administrator.
       6.2.5  Graduated cylinder and/or balance. To measure condensed water, acetone wash and

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methylene chloride wash used during field recovery of the samples, to within 1 ml or 1 g. Graduated
cylinders shall have subdivisions no greater than 2 ml. Most laboratory balances are capable of weighing
to the nearest 0,5 g or less. Any such balance is suitable for use here and in section 6.3.4 of this method.
        6.2.6 Plastic storage containers. Air-tight containers to store silica gel.
        6.2.7 Funnel and rubber policeman.  To aid in transfer of silica gel to container; not necessary if
silica gel is weighed in the field.
        6.2.8 Funnel. Glass or polyethylene, to aid in sample recovery.
        6.3  Sample analysis. The following equipment is required for sample analysis:
        6.3.1 Glass or Teflon® weighing dishes.
        6.3.2 Desiccator. It is recommended that fresh desiccant be used to minimize the chance for
positive bias due to absorption of organic material during drying.
        6.3.3 Analytical balance. To measure to within 0.1 mg.
        6.3.4 Balance. To measure to within 0.5 g.
        6.3.5 Beakers. 250ml.
        6.3.6 Hygrometer.  To measure the relative humidity of the laboratory environment.
        6.3.7 Temperature sensor.  To measure the temperature of the laboratory environment.
        6,3.8 Buchner fritted fiinnel. 30 ml size, fine (<50 micron)-porosity fritted glass.
        6.3.9 Pressure filtration apparatus.
        6.3.10 Aluminum dish. Flat bottom, smooth sides, and flanged top, 18 mm deep and with an
inside diameter of approximately 60 mm.
7.0 Reagents and Standards.
        7.1 Sample collection. The following reagents are required for sample collection:
        7.1.1 Filters. Glass fiber filters, without organic binder, exhibiting at least 99.95 percent
efficiency (<0.05 percent penetration) on 0.3 micron dioctyl phthalate smoke particles. The filter
efficiency test shall be conducted in accordance with ASTM Method D 2986-95A (incorporated by
reference  in § 63.841 of this part).  Test data  from the supplier's quality control program are sufficient for
this purpose. In sources containing S02 or S03, the filter material must be of a type that is unreactive to
S02 or S03. Reference 10 in section 17.0 of this method may be used to select the appropriate filter.
        7.1.2 Silica gel. Indicating type, 6 to 16 mesh. If previously used, dry at 175°C (350°F) for 2
hours. New silica  gel may be used as received. Alternatively, other types of desiccants (equivalent or
better) may be used, subject to the approval of the Administrator.
        7.1.3 Water. When analysis of the material caught in the impingers is required, deionized
distilled water shall be used. Run blanks prior to field use to eliminate a high blank on test samples.
        7.1.4 Crushed ice.
        7.1.5 Stopcock grease. Acetone-insoluble, heat-stable silicone grease.  This is not necessary if
screw-on connectors with Teflon® sleeves, or similar, are used. Alternatively, other types of stopcock
grease may be used, subject to the approval of the Administrator. [Caution: Many stopcock greases are
methylene chloride-soluble.  Use sparingly and carefully remove prior to recovery to prevent
contamination of the MCEM analysis.]
        7.2  Sample recovery.  The following reagents are required for sample recovery:
        7.2.1 Acetone.  Acetone with blank values < I ppm, by weight residue, is required. Acetone
blanks may be run prior to field use, and only acetone with low blank values may be used. In no case
shall a blank value of greater than 1E-06 of the weight of acetone used be subtracted from the sample
weight.
        NOTE:  This is more restrictive than Method 5,40 CFR part 60, appendix A.  At least one
vendor (Supelco Incorporated located in Bellefonte, Pennsylvania) lists <1  mg/1 as residue for its
Environmental Analysis Solvents.
        7.2.2 Methylene chloride.  Methylene chloride with a blank value <1.5 ppm, by weight, residue.
Methylene chloride blanks may be  run prior to field use, and only methylene chloride with low blank
values may be used.  In no case shall a blank value of greater than 1.6E-06  of the weight of methylene
chloride used be subtracted from the sample weight.

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        NOTE:  A least one vendor quotes <1 mg/1 for Environmental Analysis Solvents-grade
methylene chloride,
        7.3  Sample analysis. The following reagents are required for sample analysis:
        7.3.1 Acetone. Same as in section 7.2.1 of this method.
        7.3.2 Desiccant. Anhydrous calcium sulfate, indicating type. Alternatively, other types of
desiccants may be used, subject to the approval of the Administrator.
        7.3.3 Methylene chloride. Same as in section 7.2.2 of this method.
8.0 Sample Collection. Preservation. Storage, and Transport.
        NOTE:  The complexity of this method is such that, in order to obtain reliable results, testers
should be trained and experienced with the test procedures.
        8.1 Pretest preparation. It is suggested that sampling equipment be maintained according to the
procedures described in APTD-0576.
        8.1.1 Weigh several 200 g to 300 g portions of silica gel in airtight containers to the nearest 0.5
g. Record on each container the total weight of the silica gel plus container. As an alternative, the silica
gel need not be preweighed but may be weighed directly in its impinger or sampling holder just prior to
train assembly.
        8.1.2 A batch of glass fiber filters, no more than 50 at a time, should placed in a soxhlet
extraction apparatus  and extracted using methylene chloride for at least 16 hours. After extraction, check
filters visually against light for irregularities, flaws, or pinhole leaks. Label the shipping containers
(glass or plastic petri dishes), and  keep the filters in these containers at all times except during sampling
and weighing.
        8.1,3 Desiccate the filters at 20 ± 5.6°C (68 ± 10°F) and ambient pressure for at least 24 hours
and weigh at intervals of at least 6 hours to a constant weight,  i.e., <0.5 mg change from previous
weighing; record results to the nearest 0.1 mg. During each weighing the filter must not be exposed to
the laboratory atmosphere for longer than 2 minutes and a relative humidity above 50 percent.
Alternatively (unless otherwise specified by the Administrator), the filters may be oven-dried at 104°C
(220°F) for 2 to 3 hours, desiccated for 2 hours, and weighed.  Procedures other than those described,
which account for relative humidity effects, may be used, subject to the approval of the Administrator.
        8.2 Preliminary determinations.
        8.2.1 Select  the sampling site and the minimum number of sampling points according to Method
1,40 CFR part 60, appendix A or as specified by the Administrator. Determine the stack pressure,
temperature, and the  range of velocity heads using Method 2,40 CFR part 60, appendix A; it is
recommended that a leak check of the pitot lines (see section 8.1 of Method 2, 40 CFR part 60, appendix
A) be performed. Determine the moisture content using Approximation Method 4 (section 1,2 of
Method 4,40 CFR part 60, appendix A) or its alternatives to make  isokinetic sampling rate settings.
Determine the stack gas dry molecular weight, as described in  section 8.6 of Method 2, 40 CFR part 60,
appendix A; if integrated Method 3 sampling is used for molecular weight determination, the integrated
bag sample shall be taken simultaneously with, and for the same total length of time as, the particulate
sample run.
        8.2.2 Select a nozzle size  based on the range of velocity heads such that it is not necessary to
change the nozzle size in order to maintain isokinetic sampling rates. During the run, do not change the
nozzle size.  Ensure that the proper differential pressure gauge is chosen for the range of velocity heads
encountered (see section 8.2 of Method 2, 40 CFR part 60, appendix A).
        8.2.3 Select a suitable probe liner and probe length such that all traverse points can be sampled.
For large stacks, consider sampling from opposite sides of the  stack to reduce the required probe length.
        8.2.4 Select a total sampling time greater than or equal to the minimum total sampling time
specified in the test procedures for the specific industry such that: (1) The sampling time per point is not
less than 2 minutes (or some greater time interval as specified by the Administrator); and (2) the sample
volume taken (corrected to standard conditions) will exceed the required minimum total gas sample
volume. The latter is based on an approximate average sampling rate.
        8.2.5 The sampling time at each point shall be the same. It is recommended that the number of

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minutes sampled at each point be an integer or an integer plus one-half minute, in order to eliminate
timekeeping errors.
       8.2.6 In some circumstances (e.g., batch cycles), it may be necessary to sample for shorter times
at the traverse points and to obtain smaller gas sample volumes. In these cases, the Administrator's
approval must first be obtained.
       8.3 Preparation of sampling train.
       8.3.1 During preparation and assembly of the sampling train, keep all openings where
contamination can occur covered until just prior to assembly or until sampling is about to begin.  Place
100 ml of water in each of the first two impingers, leave the third impinger empty, and transfer
approximately 200 to 300 g of preweighed silica gel from its container to the fourth impinger.  More
silica gel may be used, but care should be taken to ensure that it is not entrained and carried out from the
impinger during sampling. Place the container in a clean place for later use in the sample recovery.
Alternatively, the weight of the silica gel plus impinger may be determined to the nearest 0.5 g and
recorded.
       8.3.2 Using a tweezer or clean disposable surgical gloves, place a labeled (identified) and
weighed filter in the filter holder.  Be sure that the filter is properly centered and the gasket properly
placed so as to prevent the sample gas stream from circumventing the filter. Check the filter for tears
after assembly is completed.
       8.3.3 When glass liners are used, install the selected nozzle using a Viton A 0-ring when stack
temperatures are less than 260°C (500°F) and an asbestos string gasket when temperatures are higher.
See APTD-0576 for details.  Mark the probe with heat-resistant tape or by some other method to denote
the proper distance into the stack or duct for each sampling point.
       8.3.4 Set up the train as in Figure 5-1 of Method 5,40 CFR part 60, appendix A, using (if
necessary) a very light coat of silicone grease on all ground glass joints, greasing only the outer portion
(see APTD-0576) to avoid possibility of contamination by the silicone grease. Subject to the approval of
the Administrator, a glass cyclone may be used between the probe and filter holder when the total
particulate catch is expected to exceed 100 mg or when water droplets are  present in the stack gas.
       8.3.5 Place crushed ice around the impingers.
       8.4 Leak-check procedures.
       8.4.1 Leak check of metering system shown in
Figure 5-1 of Method 5,40 CFR part 60, appendix A. That portion of the sampling train from the pump
to the orifice meter should be leak-checked prior to initial use and after each shipment. Leakage after the
pump will result in less volume being recorded than is actually sampled. The following procedure is
suggested (see Figure 5-2 of Method 5,40 CFR part 60, appendix A):  Close the main valve on the meter
box. Insert a one-hole rubber stopper with rubber tubing attached into the orifice exhaust pipe.
Disconnect and vent the low side of the orifice manometer. Close off the  low side orifice tap.  Pressurize
the system to 13 to 18 cm (5 to 7 in.) water column by blowing into the rubber tubing. Pinch off the
tubing, and observe the manometer for 1  minute. A loss of pressure on the manometer indicates a leak in
the meter box; leaks, if present, must be corrected.
       8.4.2 Pretest leak check. A pretest leak-check is recommended but not required. If the pretest
leak-check is conducted, the following procedure should be used.
       8.4.2.1  After the sampling train has been assembled, turn on and set the filter and probe heating
systems to the desired operating temperatures. Allow time for the temperatures to stabilize.  If a Viton A
0-ring or other leak-free connection is used in assembling the probe nozzle to the probe liner, leak-check
the train at the sampling site by plugging the nozzle and pulling a 380 mm (15 in.) Hg vacuum.
       NOTE:  A lower vacuum may be used, provided that it is not exceeded during the test.
       8.4.2.2  If an asbestos string is used, do not connect the probe to the train during the leak check.
Instead, leak-check the train by first plugging the inlet to the filter holder (cyclone, if applicable) and
pulling a 380 mm (15 in.) Hg vacuum.  (See NOTE in section 8.4.2.1 of this method).  Then connect the
probe to the train and perform the leak check at approximately 25 mm (1 in.) Hg vacuum; alternatively,
the probe may be leak-checked with the rest of the sampling train, in one step, at 380 mm (15 in.) Hg

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vacuum. Leakage rates in excess of 4 percent of the average sampling rate or 0.00057 mVmin (0.02
cfm), whichever is less, are unacceptable,
        8.4.2.3 The following leak check instructions for the sampling train described in APTD-0576
and APTD-0581 may be helpful. Start the pump with the bypass valve fully open and the coarse adjust
valve completely closed.  Partially open the coarse adjust valve and slowly close the bypass valve until
the desired vacuum is reached. Do not reverse the direction of the bypass valve, as this will cause water
to back up into the filter holder. If the desired vacuum is exceeded, either leak-check at this higher
vacuum or end the leak check as shown below and start over.
        8.4.2.4 When the leak check is completed, first slowly remove the plug from the inlet to the
probe, filter holder, or cyclone (if applicable) and  immediately turn off the vacuum pump.  This prevents
the water in the impingers from being forced backward into the filter holder and the silica gel from being
entrained backward into the third impinger.
        8.4.3 Leak checks during sample run.  If,  during the sampling run, a component (e.g., filter
assembly or impinger) change becomes necessary, a leak check shall be conducted immediately before
the change is made. The leak check shall be done according to the  procedure outlined in section 8.4.2 of
this method, except that it shall be done at a vacuum equal to or greater than the maximum value
recorded up to that point in the test. If the leakage rate is found to be no greater than 0.00057 mVmin
(0.02 cfrn) or 4 percent of the average sampling rate (whichever is less), the results are acceptable, and
no correction will need to be applied to the total volume of dry gas  metered; if, however, a higher
leakage rate is obtained, either record the leakage rate and plan to correct the sample volume as shown in
section 12.3 of this method or void the sample run.
        NOTE: Immediately after component changes, leak checks are optional; if such leak checks are
done, the procedure outlined in section 8.4.2 of this method should  be used.
        8.4.4 Post-test leak check.  A leak check is mandatory at the conclusion of each sampling run.
The leak check shall be performed in accordance with the procedures outlined in section 8.4.2 of this
method, except that it shall be conducted at a vacuum equal to or greater than the maximum value
reached during the sampling run.  If the leakage rate is found to be no greater than 0.00057 mVmin
(0.02 cfm) or 4 percent of the average sampling rate (whichever is less), the results are acceptable, and
no correction need be applied to the total volume of dry gas metered. If, however, a higher leakage rate
is obtained, either record the leakage rate and correct the sample volume, as shown in section 12.4 of this
method, or void the sampling run.
        8,5  Sampling train operation. During the sampling run, maintain an isokinetic sampling rate
(within 10 percent of true isokinetic unless otherwise specified by the Administrator) and a temperature
around the filter of 120 ± 14°C (248 ± 25"F), or such other temperature as specified by an applicable
subpart of the standards or approved by the Administrator.
        8.5.1 For each run, record the data required on a data sheet such as the one shown in Figure 5-2
of Method 5,40 CFR part 60, appendix A.  Be sure to record the initial reading. Record the DGM
readings at the beginning and end of each sampling time increment, when changes in flow rates are
made, before and after each leak-check, and when  sampling is halted. Take other readings  indicated by
Figure 5-2 of Method 5,40 CFR part 60, appendix A at least once at each sample point during each time
increment and additional readings when significant changes (20 percent variation in velocity head
readings) necessitate additional adjustments in flow rate.  Level and zero the manometer. Because the
manometer level and zero may drift due to vibrations and temperature changes, make periodic checks
during the traverse.
        8.5.2 Clean the portholes prior to the test run to minimize the chance of sampling deposited
material. To begin sampling, remove the nozzle cap and verify that the filter and probe heating systems
are up to temperature and that the pitot tube and probe are properly  positioned. Position the nozzle at the
first traverse point with the tip pointing directly into the gas stream. Immediately start the pump and
adjust the flow to isokinetic conditions. Nomographs are available, which aid in the rapid adjustment of
the isokinetic sampling rate without excessive computations. These nomographs are designed for use
when the Type S pitot tube coefficient (Cp) is 0.85  ± 0.02 and the stack gas equivalent density (dry

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molecular weight) is 29 ± 4.  APTD-0576 details the procedure for using the nomographs. If Cp and Md
are outside the above-stated ranges, do not use the nomographs unless appropriate steps (see Reference 7
in section 17,0 of this method) are taken to compensate for the deviations.
       8.5.3 When the stack is under significant negative pressure (height of impinger stem), close the
coarse adjust valve before inserting the probe into the stack to prevent water from backing into the filter
holder. If necessary, the pump may be turned on with the coarse adjust valve closed.
       8.5.4 When the probe is in position, block off the openings around the probe and porthole to
prevent unrepresentative dilution of the gas stream.
       8.5.5 Traverse the stack cross-section, as required by Method 1,40 CFR part 60, appendix A or
as specified by the Administrator, being careful not to bump the probe nozzle into the stack walls when
sampling near the walls or when removing or inserting the probe through the portholes; this minimizes
the chance of extracting deposited material.
       8.5.6 During the test run, make periodic adjustments to keep the temperature around the filter
holder at the proper level; add more ice and, if necessary, salt to maintain a temperature of less than 20°C
(68°F) at the condenser/silica gel outlet. Also, periodically check the level and zero of the manometer.
       8.5.7 If the pressure drop across the filter becomes too high, making isokinetic sampling
difficult to maintain, the filter may be replaced in the midst of the sample run. It is recommended that
another complete filter assembly be used rather than attempting to change the filter itself. Before a new
filter assembly is installed, conduct a leak check (see section 8.4.3 of this method). The total PM weight
shall include the summation of the filter assembly catches.
       8.5.8 A single train shall be used for the entire sample run, except in cases where simultaneous
sampling is required in two or more separate ducts or at two or more different locations within the same
duct, or in cases where equipment failure necessitates a change of trains.  In all other situations, the use
of two or more trains will be subject to the approval of the Administrator.
       NOTEj: When two or more trains are used, separate analyses of the front-half and (if applicable)
impinger catches from each train shall be performed, unless identical nozzle sizes were used in all trains,
in which case the front-half catches from the individual trains may be combined (as may the impinger
catches) and one analysis of the  front-half catch and one analysis of the impinger catch may be
performed.
       8.5.9 At the end of the sample run, turn off the coarse adjust valve, remove the probe and nozzle
from the stack, turn off the pump, record the final DGM reading, and then conduct a post-test leak check,
as outlined in section 8.4.4 of this method. Also leak-check the pitot lines as described in section 8.1 of
Method 2,40 CFR part 60, appendix A.  The lines must pass this leak check in order to validate the
velocity head data.
       8.6 Calculation of percent isokinetic. Calculate percent isokinetic (see Calculations, section
12.12 of this method) to determine whether a run was valid or another test run should be made. If there
was difficulty in maintaining isokinetic rates because of source conditions, consult the Administrator for
possible variance on the isokinetic rates.
       8.7 Sample recovery.
       8.7.1  Proper cleanup procedure begins as soon as the probe is removed from the stack at the end
of the sampling period. Allow the probe to cool,
       8.7.2 When the probe can be safely handled, wipe off all external PM near the tip of the  probe
nozzle and place a cap over it to prevent losing or gaining PM.  Do not cap off the probe tip tightly while
the sampling train is cooling down. This would create a vacuum in the filter holder, thus drawing water
from the impingers into the filter holder.
       8.7.3 Before moving the sample train to the cleanup site,  remove the probe from the sample
train, wipe off the silicone grease, and cap the open outlet of the probe. Be careful not to lose any
condensate that might be present. Wipe off the silicone grease from the filter inlet where the probe was
fastened and cap it.  Remove the umbilical cord from the last impinger and cap the impinger. If a
flexible line is used between the first impinger or condenser and the filter holder, disconnect the line at
the filter holder and let any condensed water or liquid drain into the impingers or condenser. After

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wiping off the silicone grease, cap off the filter holder outlet and irapinger inlet. Ground-glass stoppers,
plastic caps, or serum caps may be used to close these openings.
        8.7.4 Transfer the probe and filter-impinger assembly to the cleanup area. This area should be
clean and protected from the wind so that the chances of contaminating or losing the sample will be
minimized.
        8.7.5 Save a portion of the acetone and methylene chloride used for cleanup as blanks. Take
200 ml of each solvent directly from the wash bottle being used and place it in glass sample containers
labeled "acetone blank" and "methylene chloride blank," respectively.
        8.7.6 Inspect the train prior to and during disassembly and note any abnormal conditions. Treat
the samples as follows:
        8.7.6.1  Container No. 1. Carefully remove the filter from the filter holder, and place it in hs
identified petri  dish container. Use a pair of tweezers and/or clean disposable surgical gloves to handle
the filter. If it is necessary to fold the filter, do so such that the PM cake is inside the fold.  Using a dry
nylon bristle brush and/or a sharp-edged blade, carefully transfer to the petri dish any PM and/or filter
fibers that adhere to the filter holder gasket  Seal the container.
        8,7.6.2  Container No. 2. Taking care to see that dust on the outside of the probe or other
exterior surfaces does not get into the sample, quantitatively recover PM or any condensate from the
probe nozzle, probe fitting, probe liner, and front half of the filter holder by washing these components
with acetone and placing the wash in a glass container. Perform the acetone rinse as follows:
        8.7.6.2.1  Carefully remove the probe nozzle and clean the inside surface by rinsing with acetone
from a wash bottle and brushing with a nylon bristle brush. Brush until the acetone rinse shows no
visible particles, after which make a final rinse of the inside surface with acetone.
        8.7.6.2.2  Brush and rinse the inside parts of the Swagelok fitting with acetone in a similar way
until no visible  particles remain.
        8.7.6.2.3  Rinse the probe liner with acetone by tilting and rotating the probe while squirting
acetone into its upper end so that all inside surfaces are wetted with acetone. Let the acetone drain from
the lower end into the sample container. A funnel (glass or polyethylene) may be used to aid in
transferring liquid washes to the container. Follow the acetone rinse with a probe brush.  Hold the probe
in an inclined position, squirt acetone into the upper end as the probe brush is being pushed with a
twisting action through the probe, hold a sample container under the lower end of the probe, and catch
any acetone and PM that is brushed from the probe. Run the brush through the probe three times or more
until no visible  PM is carried out with the acetone or until none remains  in the probe liner on visual
inspection. With stainless steel  or other metal probes, run the brush through in the above-described
manner at least six times, since metal probes have small crevices in which PM can be entrapped. Rinse
the brush with acetone and quantitatively collect these washings in the sample container.  After the
brushing, make a final acetone rinse of me probe as described above.
       8.7.6.2.4  It is recommended that two people clean the probe to minimize sample losses.
Between sampling runs, keep brushes clean and protected from contamination.
       8.7.6.2.5  After ensuring that all joints have been wiped clean of silicone grease, clean the inside
of the front half of the filter holder by rubbing the surfaces with a nylon bristle brush and rinsing with
acetone.  Rinse  each surface three times or more if needed to remove visible partlculate. Make a final
rinse of the brush and filter holder. Carefully rinse out the glass cyclone also (if applicable).
       8.7,6.2.6  After rinsing the nozzle, probe, and front half of the filter holder with acetone, repeat
the entire procedure with methylene chloride and save in a separate No. 2M container.
       8.7.6.2.7  After acetone and methylene chloride washings and PM have been collected in the
proper sample containers, tighten the lid on the sample containers so that acetone and methylene chloride
will not leak out when it is shipped to the laboratory, Mark the height of the fluid level to determine
whether leakage occurs during transport. Label each container to identify clearly its contents.
       8.7.6.3  Container No. 3. Note the color of the indicating silica gel to determine whether it has
been completely spent, and make a notation of its condition. Transfer the silica gel from the fourth
impinger to its original container and seal the container. A funnel may make it easier to pour the silica

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gel without spilling. A rubber policeman may be used as an aid in removing the silica gel from the
impinger. It is not necessary to remove the small amount of dust particles that may adhere to the
impinger wall and are difficult to remove. Since the gain in weight is to be used for moisture
calculations, do not use any water or other liquids to transfer the silica gel. If a balance is available in
the field, follow the procedure for Container No. 3 in section 11.2.3 of this method.
       8.7.6.4  Impinger water. Treat the impingers as follows:
       8.7.6.4.1  Make a notation of any color or film in the liquid catch. Measure the liquid that is in
the first three impingers to within 1  ml by using a graduated cylinder or by weighing it to within 0.5 g by
using a balance (if one is available). Record the volume or weight of liquid present This information is
required to calculate the moisture content of the effluent gas.
       8,7.6.4.2  Following the determination of the volume of liquid present, rinse the back half of the
train with water, add it to the impinger catch, and store it in a container labeled 3 W (water).
       8.7.6.4.3  Following the water rinse, rinse the back half of the train with acetone to remove the
excess water to enhance subsequent organic recovery with raethylene chloride and quantitatively recover
to a container labeled 3S (solvent) followed by at least three sequential rinsings with aliquots of
methylene chloride. Quantitatively recover to the same container labeled 3S.  Record separately the
amount of both acetone and methylene chloride used to the nearest 1  ml or 0.5g.
       NOTE: Because the subsequent analytical finish is gravimetric, it is okay to recover both
solvents to the same container.  This would not be recommended if other analytical finishes were
required.
       8.8 Sample transport. Whenever possible, containers should be shipped in such a way that they
remain upright at  all times.
9.0 Quality Control.
       9.1 Miscellaneous quality control measures.

 Section     Quality Control Measure	Effect	

8.4,          Sampling and equipment        Ensure accurate
10.1-10.6    leak check and calibration        measurement of
                                            stack gas flow rate,
	sample volume	
       9.2 Volume metering system checks. The following quality control procedures are suggested to
check the volume metering system calibration values at the field test  site prior to sample collection.
These procedures are optional.                   \
       9.2.1  Meter orifice check.  Using the calibration data obtained during the calibration procedure
described in section 10.3 of this  method, determine the AH@ for the metering system orifice. The AH@ is
the orifice pressure differential in units of in. H20 that correlates to 0.75 cfin of air at 528°R and 29.92 in.
Hg.  The AHa is calculated as follows:
  W        *£»

                                                          T   02
                                  = 0.0319  AH  	m
                                                      P     Y2  V2
                                                      r     J    vm
where
0.0319 = (0.0567 in. Hg/°R)(0.75 cfm)2;
AH       =    Average pressure differential across the orifice meter, in. H20;
Tm        -.    Absolute average DGM temperature, °R;
0        =    Total sampling time, min;
Pbar       =    Barometric pressure, in. Hg;

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Y         =    DGM calibration factor, dimensionless;
Vm        =    Volume of gas sample as measured by DGM, dcf.
        9.2.1.1  Before beginning the field test (a set of three runs usually constitutes a field test),
operate the metering system (i.e., pump, volume meter, and orifice) at the AH@ pressure differential for
10 minutes.  Record the volume collected, the DGM temperature, and the barometric pressure. Calculate
a DGM calibration check value, Ye, as follows:
                                         10
0.0319  T
                                                           m
where
Yc     = DGM calibration check value, dimensionless;
10     = Run time, min.
       9,2.1.2 Compare the Yc value with the dry gas meter calibration factor Y to determine that: 0.97
Y < Yc < 1.03Y. If the Yc value is not within this range, the volume metering system should be
investigated before beginning the test.
       9.2.2 Calibrated critical orifice. A calibrated critical orifice, calibrated against a wet test meter
or spirometer and designed to be inserted at the inlet of the sampling meter box, may be used as a quality
control check by following the procedure of section 16.2 of this method.
10.0 Calibration and Standardization.
       NOTE: Maintain a laboratory log of all calibrations.
        10.1 Probe nozzle. Probe nozzles shall be calibrated before their initial use in the field. Using a
micrometer, measure the ID of the nozzle to the nearest 0.025 mm (0.001 in.). Make three separate
measurements using different diameters each time, and obtain the average of the measurements.  The
difference between the high and low numbers shall not exceed 0.1 mm (0.004 in.). When nozzles
become nicked, dented, or corroded, they shall be reshaped, sharpened, and recalibrated before use.
Each nozzle shall be permanently and uniquely identified.
        10.2 Pitot tube assembly. The Type S pitottube assembly shall be calibrated according to the
procedure outlined in section 10,1 of Method 2, 40 CFR part 60, appendix A.
        10.3 Metering system.
        10.3.1  Calibration prior to use. Before its initial  use in the field, the metering system shall  be
calibrated as follows;  Connect the metering system inlet to the outlet of a wet test meter that is accurate
to within 1 percent. Refer to Figure 5-5 of Method 5, 40 CFR part 60, appendix A. The wet test meter
should have a capacity of 30 liters/revolution (1 frVrev). A spirometer of 400 liters (14 ft3) or more
capacity, or equivalent, may be used for this calibration, although a wet test meter is usually more
practical. The wet test meter should be periodically calibrated with a spirometer or a liquid displacement
meter to ensure the accuracy of the wet test meter. Spirometers or wet test meters of other sizes may be
used, provided that the specified accuracies of the procedure are maintained.  Run the metering system
pump for about 15 minutes with the orifice manometer indicating a median reading, as expected in  field
use, to allow the pump to warm up and to permit the interior surface of the wet test meter to be
thoroughly wetted. Then, at each of a minimum of three  orifice manometer settings, pass an exact
quantity of gas through the wet test meter and note the gas volume indicated by the DGM. Also note the
barometric pressure and the temperatures of the wet test meter, the inlet of the DGM, and the outlet of
the  DGM.  Select the highest and lowest orifice settings to bracket the expected field operating range of
the  orifice. Use a minimum volume of 0.15 m3 (5 cf) at all orifice settings. Record all the data on a form
similar to Figure 5-6 of Method 5,40 CFR part 60, appendix A, and calculate Y (the DGM calibration
factor) and AH@ (the orifice calibration factor) at each orifice setting, as shown on Figure 5-6 of Method
5,40 CFR part 60, appendix A. Allowable tolerances for individual Y and AH@ values are given in

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Figure 5-6 of Method 5, 40 CFR part 60, appendix A.  Use the average of the Y values in the calculations
in section 12 of this method.
        10.3.1.1.  Before cal ibrating the metering system, it is suggested that a leak check be conducted.
For metering systems having diaphragm pumps, the normal leak check procedure will not detect
leakages within the pump. For these cases the following leak check procedure is suggested: make a 10-
minute calibration run at 0.00057 rnVmin (0.02 cfm); at the end of the run, take the difference of the
measured wet test meter and DGM volumes; divide the difference by 10 to get the leak rate. The leak
rate should not exceed 0.00057 mVmin (0.02 cfm).
        10.3 2 Calibration after use. After each field use, the calibration of the metering system shall be
checked by performing three calibration runs at a single, intermediate orifice setting (based on the
previous field test) with the vacuum set at the maximum value reached during the test series. To adjust
the vacuum, insert a valve between the wet test meter and the inlet of the metering system. Calculate the
average value of the DGM calibration factor.  If the value has changed by more than 5 percent,
recalibrate the meter over the full range of orifice settings, as previously detailed.
        NOTE: Alternative procedures, e.g., rechecking the orifice meter coefficient, may be used,
subject to the approval of the Administrator.
        10.3.3 Acceptable variation in calibration. If the DGM coefficient values obtained before and
after a test series differ by more than 5 percent, either the test series shall be voided or calculations for
the test series shall be performed using whichever meter coefficient value (i.e., before or after) gives the
lower value of total sample volume.
        10.4 Probe heater calibration.  Use a heat source to generate air heated to selected temperatures
that approximate those expected to occur in the sources to be sampled. Pass this air through the probe at
a typical sample flow rate while measuring the probe inlet and outlet temperatures at various probe
heater settings. For each air temperature generated, construct a graph of probe heating system setting
versus probe outlet temperature. The procedure outlined in APTD-0576 can also be used. Probes
constructed according to APTD-0581 need not be calibrated if the calibration curves in APTD-0576 are
used. Also, probes with outlet temperature monitoring capabilities do not require calibration.
        NOTE: The probe heating system shall be calibrated before its initial use in the field.
        10.5 Temperature sensors. Use the procedure in section 10.3 of Method 2, 40 CFR part 60,
appendix A to calibrate in-stack temperature sensors. Dial thermometers, such as are used for the DGM
and condenser outlet, shall be calibrated against mercury-in-glass thermometers.
        10.6 Barometer. Calibrate against a mercury barometer.
11.0 Analytical Procedure.
        11.1 Record the data required on a sheet such as the one shown in Figure 315-1 of this method.
        11.2 Handle each sample container as follows:
        11.2.1  Container No. 1.
        11.2.1.1  PM analysis.  Leave the contents in the shipping container or transfer the filter and any
loose PM from the sample container to a tared glass weighing dish. Desiccate for 24 hours in a
desiccator containing anhydrous calcium sulfate.  Weigh to a constant weight and report the results to the
nearest 0.1 mg. For purposes of this section, the term "constant weight" means a difference of no more
than 0.5 mg or 1 percent of total weight less tare weight, whichever is greater, between two consecutive
weighings, with no less than 6 hours of desiccation time between weighings (overnight desiccation is a
common practice). If a third weighing is required and it agrees within ±0.5 mg, then the results of the
second weighing should be used. For quality assurance purposes, record and report each individual
weighing; if more than three weighings are required, note this in the results for the subsequent MCEM
results.
        11.2.1.2  MCEM analysis. Transfer the filter and contents quantitatively into a beaker. Add 100
ml of methylene chloride and cover with aluminum foil.  Sonicate for 3 minutes then allow to stand for
20 minutes. Set up the filtration apparatus. Decant the solution into a clean Buchner fritted funnel.
Immediately pressure filter the solution through the tube into another clean, dry beaker. Continue
decanting and pressure filtration until all the solvent is transferred. Rinse the beaker and filter with 10 to

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20 ml methylene chloride, decant into the Buchner fritted funnel and pressure filter. Place the beaker on
a low-temperature hot plate (maximum 40°C) and slowly evaporate almost to dryness. Transfer the
remaining last few milliliters of solution quantitatively from the beaker (using at least three aliquots of
methylene chloride rinse) to a tared clean dry aluminum dish and evaporate to complete dryness.
Remove from heat once solvent is evaporated. Reweigh the dish after a 30-minute equilibrium in the
balance room and determine the weight to the nearest 0.1 mg. Conduct a methylene chloride blank run
in an identical fashion.
        11.2.2 Container No. 2.
        11.2.2.1 PM analysis. Note the  level of liquid in the container, and confirm on the analysis
sheet whether leakage occurred during transport.  If a noticeable amount of leakage has occurred, either
void the sample or use methods, subject to the approval of the Administrator, to correct the final results.
Measure the liquid in this container either volumetrically to ±1 ml or gravimetricalry to ±0.5 g.  Transfer
the contents to a tared 250 ml beaker and evaporate to dryness at ambient temperature and pressure.
Desiccate for 24 hours, and weigh to a constant weight. Report the results to the nearest 0.1 mg.
        11,2.2.2 MCEM analysis.  Add 25 ml methylene chloride to the beaker and cover with
aluminum foil.  Sonicate for 3 minutes then allow to stand for 20 minutes; combine with contents of
Container No. 2M and pressure filter and evaporate as described for Container 1 in section 11.2.1.2 of
this method.
        NOTES FOR MCEM ANALYSIS:
        1. Light finger pressure only is necessary on 24/40  adaptor.  A Chemplast adapter #15055-240
has been found satisfactory.
        2. Avoid aluminum dishes made with fluted  sides, as these may promote solvent "creep,"
resulting in  possible sample loss.
        3. If multiple samples are being  run, rinse the Buchner fritted funnel twice between samples
with 5 m! solvent using pressure filtration. After the  second rinse, continue the flow of air until the glass
frit is completely dry. Clean the Buchner fritted runnels thoroughly after filtering five or six samples.
        11.2.3  Container No. 3.  Weigh the spent silica gel  (or silica gel plus impinger) to the nearest 0.5
g using a balance.  This step may be conducted in the field.
        11.2.4  Container 3W (impinger water).
        11.2.4.1 MCEM analysis.  Transfer the solution into a 1,000 ml separatory runnel quantitatively
with methylene chloride washes. Add enough solvent to total approximately 50 ml, if necessary. Shake
the funnel for 1 minute, allow the phases to separate,  and drain the solvent layer into a 250 ml beaker.
Repeat the extraction twice.  Evaporate with low heat (less than 40°C) until near dryness.  Transfer the
remaining few milliliters of solvent quantitatively with small solvent washes into a clean, dry, tared
aluminum dish and evaporate to dryness.  Remove from heat once solvent is evaporated. Reweigh the
dish after a 30-minute equilibration in the balance room and determine the weight to the nearest 0.1 mg.
        11.2.5 Container 3S (solvent).
        11.2.5.1 MCEM analysis.  Transfer the mixed solvent to 250 ml beaker(s). Evaporate and weigh
following the procedures detailed for container 3W in section  11.2.4 of this method.
        11.2.6 Blank containers. Measure the distilled water, acetone, or methylene chloride in each
container either volumetrically or gravimetrically. Transfer the "solvent" to a tared 250 ml beaker, and
evaporate to dryness at ambient temperature and pressure. (Conduct a solvent blank on the distilled
deionized water blank in an identical fashion to that described in section 11.2.4.1  of this method.)
Desiccate for 24 hours, and weigh to a constant weight. Report the results to the nearest 0.1 mg.
       NOTE:  The contents of Containers No. 2,3W, and  3M as well as the blank containers may be
evaporated at temperatures higher than ambient.  If evaporation is done at an elevated temperature, the
temperature must be below the boiling point of the solvent; also, to prevent "bumping," the evaporation
process must be closely supervised, and the contents of the beaker must be swirled occasionally to
maintain an  even temperature.  Use extreme care,  as acetone and methylene chloride are highly
flammable and have a low flash point.

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12J) Data Analysis and Calculations.
       12.1 Cany out calculations, retaining at least one extra decimal figure beyond that of the
acquired data.  Round off figures after the final calculation. Other forms of the equations may be used as
long as they give equivalent results.
       12.2 Nomenclature.
A,,     =       Cross-sectional area of nozzle, m3 (ft3).
BWS    =       Water vapor in the gas stream, proportion by volume.
C,     =       Acetone blank residue concentration, mg/g.
C,     =       Concentration of paniculate matter in stack gas, dry basis, corrected to standard
               conditions, g/dscm (g/dscf).
I      =       Percent of isokinetic sampling.
La     =       Maximum acceptable leakage rate for either a pretest leak check or for a leak check
               following a component change; equal to 0.00057 mVmin (0.02 cfin) or 4 percent of the
               average sampling rate, whichever is less.
L;     —       Individual leakage rate observed during the leak check conducted prior to the "i*"
               component change (I = 1,2,3...n), mVmin (cfin).
Lp     =       Leakage rate observed during the post-test leak check, mVmin (cfin).
m,     =       Mass of residue of acetone after evaporation, mg.
mn     =       Total amount of particulate matter collected, mg.
Mw    =       Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb~mole).
Pbar    =       Barometric pressure at the sampling site, mm Hg (in Hg).
Ps     =       Absolute stack gas pressure, mm Hg (in. Hg).
P^    =       Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R     -       Ideal gas constant, 0.06236 [(mm HgXm3)]/[(°K)
               (g-mole)] {21.85 [(in.Hg)(ft3)]/[(0RXlb-mole)]}.
Tm     =       Absolute average dry gas meter (DGM) temperature (see Figure 5-2 of Method 5,40
               CFR part 60, appendix A), °K (°R).
T$     =       Absolute average stack gas temperature (see Figure 5-2  of Method 5, 40 CFR part 60,
               appendix AX °K(°R).
Tstd    =       Standard absolute temperature, 293°K (528°R).
V,     =       Volume of acetone blank, ml.
Vaw    =       Volume of acetone used in wash, ml.
V,     =       Volume of methylene chloride blank, ml.
Vw    =       Volume of methylene chloride used in wash, ml.
V,c     =       Total volume liquid collected In impingers and silica gel (see Figure 5-3 of Method 5,
               40 CFR part 60, appendix A), ml.
Vm     =       Volume of gas sample as measured by dry gas  meter, dcm (dcf)-
Vm(sd)  ~       Volume of gas sample measured by the dry gas meter, corrected to standard conditions,
               dscm  (dscf).
V«(jni)  ~       Volume of water vapor in the gas sample, corrected to standard conditions, scm (scf).
V,     =       Stack gas velocity, calculated by Equation 2-9  in Method 2,40 CFR part 60, appendix
               A, using data obtained from Method 5,40 CFR part 60,  appendix A, m/sec (ft/sec).
W,     =       Weight of residue in acetone wash, mg.
Y     =       Dry gas meter calibration factor,
AH    =       Average pressure differential across the orifice meter (see Figure 5-2 of Method 5, 40
               CFR part 60, appendix A), mm H20 (in H20).
pa     =       Density of acetone, 785.1 mg/ml (or see label on  bottle).
pw     =       Density of water, 0.9982 g/ml (0.002201 Ib/ml).
p,     =       Density of methylene chloride, 1316.8 mg/ml (or see label on bottle).
0     =       Total  sampling time, min.
9|     =       Sampling time interval, from the beginning of a run until the first component change,

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               min.
©i        =   Sampling time interval, between two successive component changes, beginning with the
               interval between the first and second changes, min.
8p        =   Sampling time interval, from the final (n*) component change until the end of the
               sampling run, min.
13.6      =   Specific gravity of mercury,
60        —   Sec/min.
100       =   Conversion to percent,
        12.3 Average dry gas meter temperature and average orifice pressure drop. See data sheet
(Figure 5-2 of Method 5,40 CFR part 60, appendix A).
        12.4 Dry gas volume.  Correct the sample volume measured by the dry gas meter to standard
conditions (20°C, 760 mm Hg or 68°F, 29.92 in Hg) by using Equation 315-1.
                .,. ,,  y  "V       13.6)                                   Eg. 315-1
                       in         _  _
                                              P   +l  AH
                                                bar I """"""~""~~
                                = i/ _  w •' ^      v  13,6
where
K,   =  0.3858 °K/mm Hg for metric units,
     = 1 7.64 °R/inHg for English units.
     MOTE: Equation 315-1 can be used as written unless the leakage rate observed during any of the
mandatory leak checks (i.e., the post-test leak check or leak checks conducted prior to component
changes) exceeds L,. If Lp or Lj exceeds Lw Equation 315-1 must be modified as follows:
     (a) Case I.  No component changes made during sampling run.  In this case, replace Vra in Equation
315-1 with the expression;
     (b) Case II. One or more component changes made during the sampling run. In this case, replace
Vm in Equation
315-1 by the expression:
          IV m  -  (L,  -  L.)  0,  -       (L,  - La) Q,  - (£.,  -  L.)  Qp]
                                        i=2
and substitute only for those leakage rates (Lj or Lp) which exceed L,.
      12.5 Volume of water vapor condensed.

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                                                                                 Eg. 315-2
where
K2     =   0.001333 m3/ml for metric units;
       =   0.04706 ftVml for English units.
       12.6 Moisture content.
                                                                                 Eq.
                                                                                 _*
                          "           v
       MOTE: In saturated or water droplet-laden gas streams, two calculations of the moisture content
of the stack gas shall be made, one from the impinger analysis (Equation 3 1 5-3), and a second from the
assumption of saturated conditions.  The lower of the two values of B^ shall be considered correct. The
procedure for determining the moisture content based upon assumption of saturated conditions is given
in section 4.0 of Method 4, 40 CFR part 60, appendix A. For the purposes of this method, the average
stack gas temperature from Figure 5-2 of Method 5, 40 CFR part 60, appendix A may be used to make
this determination, provided that the accuracy of the in-stack temperature sensor is ±1°C (2°F).
       12.7 Acetone blank concentration.

                                 Ma
        12.8 Acetone wash blank.
                                        W, = CBVawPa                               Eq. 315-5
        12.9 Total particulate weight. Determine the total PM catch from the sum of the weights
obtained from Containers 1 and 2 less the acetone blank associated with these two containers (see Figure
315-1).
       NOTE:  Refer to section 8.5.8 of this method to assist in calculation of results involving two or
more filter assemblies or two or more sampling trains.
        12.10 Particulate concentration.
                                       'c,-KimJV*w                               Eq.315-6
where
K     = 0.001  g/mg for metric units;
       = 0.0 1 54 gr/mg for English units.
        12.11 Conversion factors.
From
ft3
gr
gr/ft3
mg


12.12
Jo.
m3
mg
mg/m3
g
Ib
Isokinetic variation.
Multiply by
0.02832
64.80004
2288.4
0.001
1.429X10-4


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        12.12.1  Calculation from raw data.
             100 T.
        / =
     *4 Vfc
                                     m
                                               ""
                                                    13.6
                                                                Eg. 315-7
                            60 9 vs Ps An
where
K4   -  0.003454 [(mm Hg)(m3)]/[(ml)(°K)] for metric units;
      =  0.002669 [(in HgXft3)HM)C"R)] for English units.
        12.12.2 Calculation from intermediate values.
           ,  ,
                                   PSM 100
std
                          e An Ps 60
                                 = Kc
                                                T   V
                                                      m(std)
where

K5     =  4.320 for metric units;
       =  0.0945 0 for English units.
       12.12.3 Acceptable results. If 90 percent i I <. 110 percent, the results are acceptable.  If the
PM or MCEM results are low in comparison to the standard, and "I" is over 110 percent or less than 90
percent, the Administrator may opt to accept the results. Reference 4 in the Bibliography may be used to
make acceptability judgments.  If "I" is judged to be unacceptable, reject the results, and repeat the test.
       12.13 Stack gas velocity and volumetric flow rate. Calculate the average stack gas velocity and
volumetric flow rate, if needed, using data obtained in this method and the equations in sections 5.2 and
5.3 of Method 2, 40 CFR part 60,  appendix A.
       12.14 MCEM results.  Determine the MCEM concentration from the results from Containers 1,
2, 2M, 3W, and 3.S less the acetone, methylene chloride, and filter blanks value as determined in the
following equation;
13LQ Method Performance.  [Reserved]
14.0 Pollution Prevention. [Reserved]

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15.0 Waste Management.  [Reserved]
16.0 Alternative Procedures.
       16.1 Dry gas meter as a calibration standard. A DGM may be used as a calibration standard for
volume measurements in place of the wet test meter specified in section 16,1 of this method, provided
that ft is calibrated initially and recalibrated periodically as follows:
       16.1.1 Standard dry gas meter calibration.
       16.1.1,1. The DGM to be calibrated and used as a secondary reference meter should be of high
quality and have an appropriately sized capacity, e.g., 3 liters/rev (0.1 fP/rev).  A spirometer (400 liters
or more capacity), or equivalent, may be used for this calibration, although a wet test meter is usually
more practical.  The wet test meter should have a capacity of 30 liters/rev (1 ftVrev) and be capable of
measuring volume to within 1.0 percent; wet test meters should be checked against a spirometer or a
liquid displacement meter to ensure the accuracy of the wet test meter. Spirometers or wet test meters  of
other sizes may be used, provided that the specified accuracies of the procedure are maintained.
       16.1.1.2 Set up the components as shown in Figure 5-7 of Method 5,40 CFR part 60, appendix
A. A spirometer, or equivalent, may be used in place of the wet test meter in the system.  Run the pump
for at least 5 minutes at a flow rate of about 10 liters/min (0.35 cfm) to condition the interior surface of
the wet test meter.  The pressure drop indicated by the manometer at the inlet side of the DGM  should be
minimized (no greater than 100 mm HaO [4 in. H2O] at a flow rate of 30 liters/min [1 cfin]). This can be
accomplished by using large- diameter tubing connections and straight pipe fittings.
       16.1.1.3 Collect the data as shown in the example data sheet (see Figure 5-8 of Method 5,40
CFR part 60, appendix A). Make triplicate runs at each of the flow rates and at no less than five different
flow rates.  The range of flow rates should be between 10 and 34 liters/min (0.35 and 1.2 cfin) or over
the expected operating range.
       16.1.1.4 Calculate flow rate, Q, for each run using the wet test meter volume, VWJ and the run
time, q. Calculate the DGM coefficient, Yds, for each run. These calculations are as follows;


               •Q  =  K       ^ V"                                        a,. 315.9

                             (*v +
                                    Tsd) P
                                     std    baf
                                                       Eq, 319-10
where
K,    =   0.3 858 for international system of units (SI);
           17.64 for English units;
Pto   =   Barometric pressure, mm Hg (in Hg);
Vw   =   Wet test meter volume, liter (ft3);
t,,    =   Average wet test meter temperature, °C (°F);
i,a    -   273°C for SI units; 460°F for English units;
0    =   Run time, min;
t^    =   Average dry gas meter temperature, °C (°F);
Vds   =   Dry 8as meter volume, liter (ft3);
Ap   =   Dry gas meter inlet differential pressure, mm H2O (in H2O).
        16.1.1.5 Compare the three Yj, values at each of the flow rates and determine the maximum and
minimum values.  The difference between the maximum and minimum values at each flow rate should
be no greater than 0.030. Extra sets of triplicate runs may be made in order to complete this requirement.
In addition, the meter coefficients should be between 0.95 and 1.05. If these specifications cannot be

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met in three sets of successive triplicate runs, the meter is not suitable as a calibration standard and
should not be used as such. If these specifications are met, average the three Yds values at each flow rate
resulting in five average meter coefficients, Yds.
        16.1.1.6 Prepare a curve of meter coefficient, Yds, versus flow rate, Q, for the DGM. this curve
shall be used as a reference when the meter is used to calibrate other DGMs and to determine whether
recalibration is required.
        16.1.2  Standard dry gas meter recalibration.
        16.1.2.1 Recalibrate the standard DGM against a wet test meter or spirometer annually or after
every 200 hours of operation, whichever comes first. This requirement  is valid provided the standard
DGM  is kept in a laboratory and, if transported, cared for as any other laboratory instrument Abuse to
the standard meter may cause a change in the calibration  and will require more frequent recalibrations.
        16.1.2.2 As an alternative to full recalibration, a  two-point calibration check may be made.
Follow the same procedure and equipment arrangement as for a full recalibration, but run the meter at
only two flow rates (suggested rates are 14 and 28  liters/min [0.5 and 1.0 cftn]).  Calculate the meter
coefficients for these two points, and compare the values  with the meter calibration curve. If the two
coefficients are within  1.5 percent of the calibration curve values at the same flow rates, the meter need
not be recalibrated until the next date for a recalibration check.
        16.2  Critical orifices as calibration standards.  Critical orifices may be used as calibration
standards in place of the wet test meter specified in section 10.3 of this method, provided that they are
selected, calibrated, and used as follows:
        16.2.1  Selection of critical orifices,
        16.2.1.1 The procedure that follows describes the use of hypodermic needles or stainless steel
needle tubing that has been found suitable for use as critical orifices.  Other materials and critical orifice
designs may be used provided the orifices act as true critical orifices; i.e., a critical vacuum can be
obtained, as described in section 7.2.2.2.3 of Method 5, 40 CFR part 60, appendix A. Select five critical
orifices that are appropriately sized to cover the range of  flow rates between 10 and 34 liters/min or the
expected operating range.  Two of the critical orifices should bracket the expected operating range. A
minimum of three critical orifices will be needed to calibrate a Method 5 DGM; the other two critical
orifices can serve as spares and provide better selection for bracketing the range of operating flow rates.
The needle sizes and tubing lengths  shown in Table 315-1 give the approximate flow rates indicated in
the table.
        16.2.1.2 These needles can  be adapted to a Method 5 type sampling train as follows; Insert a
serum bottle stopper, 13 x 20 mm sleeve type, into a 0.5 in Swagelok quick connect.  Insert the needle
into the stopper as shown in Figure 5-9 of Method  5,  40 CFR part 60, appendix A.
        16.2.2  Critical orifice calibration.  The procedure described in this section uses the Method 5
meter box configuration with a DGM as described  in section 6.1.1.9 of this method to calibrate the
critical orifices. Other  schemes may be used, subject to the approval of the Administrator.
        16.2.2.1 Calibration of meter box. The critical orifices must be calibrated in the same
configuration as they will be used; i.e., there should be no connections to the inlet of the orifice.
        16.2.2.1.1  Before calibrating the meter box, leak-check the system as follows: Fully open the
coarse adjust valve and completely close the bypass valve. Plug the inlet. Then turn  on the pump and
determine whether there is any leakage. The leakage rate shall be zero; i.e., no detectable movement of
the DGM dial shall be seen for 1 minute.
        16.2.2.1.2 Check also for leakages in that portion of the sampling train  between the pump and
the orifice meter. See section 5.6 of Method 5,40 CFR part 60, appendix A for the procedure; make any
corrections, if necessary.  If leakage is detected, check for cracked gaskets, loose fittings, worn 0-rings,
etc. and make the necessary repairs.
        16.2.2.1.3  After determining that the meter box is leakless, calibrate the meter box according to
the procedure given in section 5.3 of Method 5, 40 CFR part 60, appendix A. Make sure that the wet test
meter meets the requirements stated in section 7.1.1.1 of Method 5,40 CFR part 60, appendix A. Check
the water level  in the wet test meter. Record the DGM calibration factor, Y.

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        162.2.2  Calibration of critical orifices.  Set up the apparatus as shown in Figure 5-10 of Method
5, 40 CFR part 60, appendix A.
        16.2.2.2.1 Allow a warm-up time of 15 minutes. This step is important to equilibrate the
temperature conditions through the DGM.
        162.22.2 Leak-check the system as in section 72.2.1.1 of Method 5, 40 CFR part 60, appendix
A. The leakage rate shall be zero.
        16.222.3 Before calibrating the critical orifice, determine its suitability and the appropriate
operating vacuum as follows: turn on the pump, fully open the coarse adjust valve, and adjust the bypass
valve to give a vacuum reading corresponding to about half of atmospheric pressure. Observe the meter
box orifice manometer reading, DH.  Slowly increase the vacuum reading until a stable reading is
obtained on the meter box orifice manometer. Record the critical vacuum for each orifice. Orifices that
do not reach a critical value shall not be used.
        16222.4 Obtain the barometric pressure using a barometer as described in section 6.12 of this
method. Record  the barometric pressure, P^, in mm Hg (in. Hg).
        1622.2.5 Conduct duplicate runs at a vacuum of 25 to 50 mm Hg (1 to 2 in. Hg) above the
critical vacuum.  The runs shall be at least 5 minutes each.  The DGM volume readings shall be in
increments of complete revolutions of the DGM. As a guideline, the times should not differ by more
than 3.0 seconds  (this includes allowance for changes in the DGM temperatures) to achieve ±0.5 percent
in K'. Record the information listed in Figure 5-11 of Method 5,40 CFR part 60, appendix A.
        16.222.6 Calculate K1 using Equation 315-11.
                                               _^
                   tf  • /   *y //•»    .   *-»rj  * -p Z
                                          :) 'a
,_ "i r« '  |r*"    li^1 >am*                               Eq. 315-11
              pk  7  0
              ' bar ' m v
where
K'    =  Critical orifice coefficient, [m3)(°K)w]/
          [(mm Hg)(min)] {[(WR)*)]/[(in. Hg)(min)]};
Tmrt,  -  Absolute ambient temperature, °K (°R).
        16.2.2.2.7 Average the K' values. The individual K' values should not differ by more than ±0.5
percent from the average.
        16.23 Using the critical orifices as calibration standards.
        162.3.1  Record the barometric pressure.
        16.2.3.2  Calibrate the metering system according to the procedure outlined in sections 72.2.2.1
to 72.2.2.5 of Method 5,40 CFR part 60, appendix A. Record the information listed in Figure 5-12 of
Method 5,40 CFR part 60, appendix A.
        162.3.3  Calculate the standard volumes of air passed through the DGM and the critical orifices,
and calculate the DGM calibration factor, Y, using the equations below:
                             =K,Vm[Pbar + (AH/13.6)]/Tm                            Eq. 315-12
                        =K'(Pbare)/Tamb"2                                           Eq. 315-13
              Y             =Va(sld/Vm(stI1)                                          gq. 315-14
where
              Volume of gas sample passed through the
                     critical orifice, corrected to standard conditions, dscm (dscf).
K' =    0.3 85 8 °K/mm Hg for metric units
    =   17.64 °R/in Hg for English units.
        162.3.4  Average the DGM calibration values for each of the flow rates. The calibration factor,
Y, at each of the flow rates should not differ by more than ±2 percent from the average.
        162.3.5  To determine the need for recalibrating the critical orifices, compare the DGM Y

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factors obtained from two adjacent orifices each time a DGM is calibrated; for example, when checking
orifice 13/2,5, use orifices 12/10.2 and 13/5.1. If any critical orifice yields a DGM Y factor differing by
more than 2 percent from the others, recalibrate the critical orifice according to section 7.2.2.2 of Method
5, 40 CFR part 60, appendix A.
17,0 References.
       1.  Addendum to Specifications for Incinerator Testing at Federal Facilities. PHS, NCAPC.
December 6, 1967.
       2. Martin, Robert M. Construction Details of Isokinetic Source-Sampling Equipment.
Environmental Protection Agency. Research Triangle Park, NC. APTD-0581. April 1971.
       3. Rom, Jerome J. Maintenance, Calibration, and Operation of Isokinetic Source Sampling
Equipment. Environmental Protection Agency. Research Triangle Park, NC. APTD-0576. March 1972,
       4. Smith, W.S., R.T. Shigehara, and W.F. Todd. A Method of Interpreting Stack Sampling Data.
Paper Presented at the 63rd Annual Meeting of the Air Pollution Control Association, St. Louis, MO.
June 14-19,1970.
       5. Smith, W.S., et al. Stack Gas Sampling Improved and Simplified With New Equipment.
APCA Paper No.  67-119.  1967.
       6. Specifications for Incinerator Testing at Federal Facilities. PHS, NCAPC. 1967.
       7. Shigehara, R.T. Adjustment in the EPA Nomograph for Different Pitot Tube Coefficients and
Dry Molecular Weights.  Stack Sampling News 2:4-11.  October 1974.
       8. Vollaro, R.F,  A Survey of Commercially Available Instrumentation for the Measurement of
Low-Range Gas Velocities.  U.S. Environmental Protection Agency, Emission Measurement Branch.
Research Triangle Park, NC. November 1976 (unpublished paper).
       9. Annual Book of ASTM Standards.  Part 26. Gaseous Fuels; Coal and Coke; Atmospheric
Analysis.  American Society for Testing and Materials. Philadelphia, PA. 1974. pp. 617-622.
       10. Felix, L.G., G.I. Clinard, G.E. Lacy, and J.D. McCain. Inertial Cascade Impactor Substrate
Media for Flue Gas Sampling.  U.S. Environmental Protection Agency.  Research Triangle Park, NC
27711. Publication No. EPA-600/7-77-060. June 1977. 83 p.
       11. Westlin, P.R., and R.T. Shigehara. Procedure for Calibrating and Using Dry Gas Volume
Meters as Calibration Standards. Source Evaluation Society Newsletter.  3(1):17-30. February 1978.
       12. Lodge, J.P., Jr., J.B. Pate, B.E. Ammons, and G.A.  Swanson,  The Use of Hypodermic
Needles as Critical Orifices in Air Sampling. J. Air Pollution Control Association. 16:197-200. 1966.
18.0 Tables. Diagrams. Flowcharts, and Validation Data
TABLE 315-1. Flow Rates for Various Needle Sizes and Tube Lengths.
Gauge/length
(cm)
12/7.6
12/10.2
13/2.5
13/5.1
13/7.6
13/10.2
Flow rate
(liters/min)
32.56
30.02
25.77
23.50
22.37
20.67
Gauge/length
(cm)
14/2.5
14/5.1
14/7.6
15/3.2
15/7.6
15/10.2
Flow rate
(liters/min)
19.54
17.27
16.14
14.16
11.61
10.48

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Particulate analysis
Plant
Date
Run No.
Filter No.
Amount liquid lost during
transport
Acetone blank volume (ml)
Acetone blank concentration (Eq.315-4) (mg/mg)
Acetone wash blank (Eq.315-5) (mg)

Container
No. 1
Container
No. 2
Final weight
(mg)










Tare weight (mg)


Total
Less Acetone blank
Weight of particulate matter
Weight gain (mg)





Moisture analysis

Impingers
Silica gel
Final volume /
(mg)
Notel

Initial volume (mg)
Note 1

Total
Liquid collected (mg)



FIGURE 315-1.  Particulate and MCEM Analyses




Note 1: Convert volume of water to weight by multiplying by the density of water (1 g/ml).

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                                     MCEM analysis
Container No.
 Final
weight
 Tare of
aluminum
dish (mg)
Weight
 gain
  Acetone
wash volume
    (ml)
Metflrfbmfc
    wash
   volume
    (ml)
  2+2M
  3W
  3S
                  total
                                                   'total
                                                                   aw
  Less acetone wash blank (mg)
  (not to exceed I mg/1 of
  acetone used)
                                          =c
  Less methylene chloride wash
  blank (mg) (not to exceed
  1.5 mg/1 of methylene
  chloride used)
                                       Wt =
  Less filter blank (mg)
  (not to exceed....
  (nig/filter)
  MCEM weight (mg)
                                                         = E
 FIGURE 315-1 (Continued). Particulate And MCEM Analyses

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                    State of California
          California Environmental Protection Agency
                   Air Resources Board
                     Method 429

Determination of Polyeyclfc Aromatic Hydrocarbon {PAH}
           Emissions from Stationary Sources
               Adopted: September 12,1989
            Amended: {insert date of amendment]

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                          TABLE OF CONTENTS
1   INTRODUCTION	    1
1.1  APPLICABILITY	„	    1
1.2  PRINCIPLE	    1
1.3  DEFINITIONS AND ABBREVIATIONS	    1
2   THE PRE-TEST PROTOCOL	 . . ,	    4
2.1  RESPONSIBILITIES OF THE END USER, TESTER, AND ANALYST	    4
2.2  PRE-TEST REQUIREMENTS		............	    5
2.3  REQUIRED PRELIMINARY ANALYTICAL DATA	    6
2.4  EXPECTED RANGE IN TARGET PAH CONCENTRATIONS
     OF INDIVIDUAL PAHs	    7
2.5  SAMPLING RUNS, TIME, AND VOLUME  . .	. . .		    7

3   INTERFERENCES		   10
4   SAMPLING APPARATUS, MATERIALS, AND REAGENTS	   11
4.1  SAMPLING APPARATUS	 .	.   11
4.2  SAMPLING MATERIALS AND REAGENTS	   14
4.3  PRE-TEST PREPARATION  	   18
4.4  SAMPLE COLLECTION	   21
4.5  CALCULATIONS	   26
4.6  ISOKINETIC CRITERIA	,	   30

5   SAMPLE RECOVERY  		,	. . .   31
5.1  SAMPLE RECOVERY APPARATUS		   31
5.2  SAMPLE RECOVERY REAGENTS	   32
5.3  SAMPLE RECOVERY PROCEDURE	,	   32
5.4  SAMPLE PRESERVATION AND HANDLING		   34
6   ANALYTICAL PREPARATION 		   34
6.1  SAFETY .		   34
6.2  CLEANING OF LABORATORY GLASSWARE ..................	. .   35
August 9, 1996                                     Proposed M-429 Page i

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6.3 APPARATUS	  35
6.4 SAMPLE PREPARATION: REAGENTS	  36
6.5 SAMPLE EXTRACTION	  37
6.6 COLUMN CLEANUP	  40

7   GC/MS ANALYSIS	  42
7.1 APPARATUS	  42
7.2 REAGENTS	  43
7.3 INITIAL CALIBRATION	  45
7.4 CONTINUING CALIBRATION	  48
7.5 GC/MS ANALYSIS	  49
7.6 QUALITATIVE ANALYSIS	  50
7.7 QUANTITATIVE ANALYSIS 	  51

8   QUALITY ASSURANCE/QUALITY CONTROL			  52
8.1 QA SAMPLES	  52
8.2 ACCEPTANCE CRITERIA 	  54
8.3 ESTIMATION OF THE METHOD DETECTION LIMIT (MDL)
     AND PRACTICAL QUANTITATION LIMIT JPQL)	  56
8.4 LABORATORY PERFORMANCE	,,.,..  57

9.   CALCULATIONS 	  57
9.1 ANALYST'S CALCULATIONS		  57
9.2 TESTER'S CALCULATIONS		  61

10  REPORTING REQUIREMENTS		  64
10.1 SOURCE TEST PROTOCOL	  64
10.2 LABORATORY REPORT  	  65
10.3 EMISSIONS TEST REPORT	  68
11  BIBLIOGRAPHY	  70
August 9, 1996                                     Proposed M-429 Page ii

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TABLES

   1   Method 429 Target Analytes	   71

   2   Practical Quantitation Limits for Target PAHs	   72

   3   PAH  Analysis by HRMS of Different Lots
        of Cleaned Resin	   73

   4   Composition of the Sample Spiking Solutions	   74

  4A   Composition of Alternative Sample Spiking Solutions	   75

   5   Concentrations of PAHs in Working GC/MS Calibration
        Standard Solutions for Low Resolution Mass Spectrometry 	   76

   6   Concentrations of PAHs in Working GC/MS Calibration
        Standard Solutions for High Resolution Mass Spectrometry	   78

  6A   Concentrations of PAHs in Alternative Working GC/MS Calibration
        Standard Solutions for High Resolution Mass Spectrometry	   80

   7   Spike Levels for Labelled Standards	   82

  7A   Spike Levels for Labelled Standards for Alternative
        HRMS Spiking Scheme		   83

   8   Target Concentrations for  Labelled Standards in Sample Extract	,   84

  8A   Target Concentrations for  Labelled Standards in Sample Extract
        Obtained with Alternative HRMS Spiking Scheme	   85

   9   Concentrations of Compounds in Laboratory Control Spike Sample	   86

  10   Recommended Gas Chromatographic Operating Conditions
        for PAH Analysis	   87

  11   Assignments of Internal Standards for Calculation of RRFs
        and Quantitation of Target PAHs and Surrogate Standards ............   88

11A   Assignments of Internal Standards for Calculation of RRFs
       and Quantitation of Target PAHs and Surrogate
         Standards Using Alternative HRMS Spiking Scheme	   89

  12   Assignments of Recovery Standards for Determination of Percent
       Recoveries of Internal Standards and the Alternate Standard  ..........   90

12A   Assignments of Recovery Standards for Determination of
       Percent Recoveries of  internal Standards and the  Alternate Standard
         Using Alternative HRMS Spiking Scheme	   91

  13   Quantitation and Confirmation  Ions for Selected
        Ion Monitoring of PAHs by HRGC/LRMS  .	   92

  14   Mass Descriptors Used for Selected Ion Monitoring
       Of PAHs by HRGC/HRMS  		   94
August 9, 1996                                           Proposed M-429 Page lit

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FIGURES
   1   Method 429 Flowchart	   96
   2   PAH Sampling Train	   97
   3   Condenser and Sorbent Trap for Collection of Gaseous PAH	 .   98
   4   XAD-2 Fluidized Bed Drying Apparatus	   99
   5   Method 429 Reid Data Record  	  100
   6   Recovery of PAH Sampling Train	  101
   7   Flowchart for Sampling, Extraction and Cleanup for  	  102
       Determination of PAH in a Split Sample
   8   Flowchart for Sampling, Extraction and Cleanup for
       Determination PAH in a Composite Sample	  103
   9   Example of Pre-Test Calculations for PAH Emissions Test	  104
  10   CARB Method 429 (PAHs) Sampling Train Setup Record	  105
  11   CARB Method 429 (PAHs) Sampling Train Recovery Record	  106
  12   Chain of Custody Sample Record	  107
  13   Chain of Custody Log Record	  108
14A   Example of GC/MS Summary Report (HRMS) for
       Initial Calibration Solution #1	  109
14B   Example of Initial Calibration (ICAU RRF Summary 	  110
14C   Example of Continuing Calibration Summary .	  111
15A   Example of Summary Report of LCS Results	  112
15B   UCS Recoveries for Benzo{a)pyrene  	  113
16A   Example GC/MS Summary Report (HRMS) for Sample Run #32  	  114
16B   Example Laboratory Report of PAH Results for Sample Run #32  	  115
17A   Example of Tester's Summary of Laboratory Reports	  116
17B   Field Data Summary for PAH Emissions Test	  117
17C   Example of Emissions Test Report	  118

APPENDIX A
      Determination of the Method Detection Limit	  119
August 9, 1996                                         Proposed M-429 Page iv

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                                    Method 429

              Determination of Polycyclic Aromatic Hydrocarbon (PAH)
                        Emissions From Stationary Sources
 1.       INTRODUCTION

 1.1      APPLICABILITY
         This method applies to the determination of nineteen polycyclic aromatic
         hydrocarbons (PAH) in emissions from stationary sources. These are listed in
         Table 1.  The sensitivity which can ultimately be achieved for a given sample will
         depend upon the types and concentrations of other chemical compounds in the
         sample as well as the original sample size and instrument sensitivity.

         Any modification of this method beyond those expressly permitted shall be
         considered a major modification subject to approval by the Executive Officer  of
         the California Air Resources Board or his or her authorized representative.

 1.2      PRINCIPLE

         Paniculate and gaseous  phase PAH are extracted isokinetically from the stack
         and collected on XAD-2  resin, in impingers, or in upstream sampling train
         components (filter, probe, nozzle).  Only the total amounts of each PAH in the
         stack emissions can be determined with this  method. It has not been
         demonstrated that the partitioning  in the different parts of the sampling train is
         representative of the partitioning in the stack gas sample for particulate and
         gaseous PAH.

         The required analytical method is isotope dilution mass spectrometry combined
         with high resolution gas  chromatography. This entails the addition of internal
         standards to all samples in known  quantities, matrix-specific extraction of the
         sample with appropriate  organic solvents, preliminary fractionation and  cleanup
         of extracts and analysis of the processed extract for PAH using high-resolution
         capillary column gas chromatography coupled with either low resolution mass
         spectrometry (HRGC/LRMS), or high resolution mass spectrometry
         {HRGC/HRMSl.  To ensure comparable results, the same MS method must be
         used for samples collected at all tested locations at those sources where more
         than one  location is tested.

         Minimum performance criteria are specified herein which must be satisfied to
         ensure the quality of the sampling and analytical data.

1.3      DEFINITIONS AND ABBREVIATIONS

1.3.1       Internal Standard

            An internal standard is a 2H-labelled  PAH  which is added to all field  samples,
            blanks and other quality control samples before extraction. It is also present
            in the calibration solutions.  Internal standards are used to measure the
August 9, 1996                                              Proposed M-429 Page 1

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            concentration of the analyte and surrogate compounds. There is one internal
            standard assigned to each of the target analytes and surrogates.
1.3.2       Surrogate Standard
            A surrogate standard is a labelled compound added in a known amount to the
            XAD-2 resin of the sampling train, and allowed to equilibrate with the matrix
            before the gaseous emissions are sampled. The surrogate standard has to be
            a component that can be completely resolved, is not present in the sample,
            and does not have any interference effects.  Its measured concentration in
            the extract is an indication of the how effectively the sampling train retains
            PAH collected on the XAD-2 resin.  The recovery of the surrogate standards
            in the field  blanks can be used to determine whether there are any matrix
            effects caused by time or conditions under which the sample is transported
            and stored  prior to analysis.
1.3.3       Alternate Standard
            An alternate standard is a  2H-labelled PAH compound which is added to the
            impinger contents prior to extraction to estimate the extraction efficiency for
            PAHs in the impinger sample.
1.3.4       Recovery Standard
            A recovery standard is a 2H-labelled PAH compound which is added to the
            extracts of al! field samples, blanks, and quality control samples before
            HRGC/MS analysis. It is also present in the calibration solution. The
            response of the internal standards relative to the recovery standard is used to
            estimate the recovery of the internal standards. The internal standard
            recovery is an indicator of the overall performance of the analysis.
1.3.5       Relative Response Factor
            The relative response factor is the response of the mass spectrometer to a
            known amount of an analyte or labelled compound (internal standard or
            surrogate standard) relative to a known amount of an internal standard or
            another labelled compound (recovery standard or internal standard).

1.3.6       Performance Standard

            A performance standard is a  mixture of known amounts of selected standard
            compounds. It is used to demonstrate continued acceptable performance of
            the GC/MS system.  These checks include system performance checks,
            calibration checks, quality checks, matrix recovery, and surrogate recoveries.

1.3.7       Performance Evaluation Sample

            A performance evaluation sample is one prepared by EPA  or other
            laboratories that contains known concentrations of method analytes, and has
            been analyzed by multiple laboratories to determine statistically the accuracy
            and precision that can be expected when a method is performed by a
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             competent analyst.  Concentrations must be in the same range as typical
             field samples,  Analyte concentrations are not known by the analyst.

 1.3.8        Laboratory Control Sample

             A laboratory control sample is one that contains known concentrations of
             method analytes that is analyzed by a laboratory to demonstrate that it can
             obtain acceptable identifications and measurements with procedures to be
             used to analyze field samples containing  the same analytes. Analyte
             concentrations are known by the analyst. The laboratory must prepare the
             control sample from stock standards prepared independently from those used
             for calibration.

 1.3.9        End User

             The regulating agency shall  be considered the end user if this test method is
             conducted for regulatory purposes, or the regulating agency shall designate
             the  end user for the purposes of this method.  Otherwise the end user shall
             be the party who defrays the cost of performing this  test method. In any
             case, the pre-test protocol (Section 2) must identify the end user.

 1.3.10      Tester

             Usually the tester is a  contract engineering  firm that performs the sampling
             procedures and delegates responsibility for  specific analytical  procedures to
             an analytical group (usually  part of a  subcontracting laboratory firm).  In
             some cases, the  tester may be part of the regulating  agency.  The tester shall
             be the party ultimately responsible for the performance of this test method
             whether directly  or indirectly through the co-ordination of the efforts of the
             analytical group and the efforts of the sampling group.

 1.3.11       Analyst
                                        j
                                        i
             This term refers to the analytical group that performs the analytical
             procedures to generate the required analytical  data.

 1.3.12      Source Target Concentration

             This is the target concentration for each emitted PAH of interest specified by
             the end user of the test results.  The target concentration shall be expressed
             in units of mass of target substance per volume of emissions;  typical units
             are nanograms per dry standard cubic meter or micrograms per dry standard
             cubic meter (ng/dscm or //g/dscm)

 1.3.13       The Method Detection Limit

             The method detection  limit (MDL) is based on the precision of detection of
             the analyte concentration near the detection limit. It  is the product of the
             standard deviation of seven  replicate analyses of resin samples spiked with
             low  concentrations of the analyte and Student's t value for 6 degrees of
             freedom at a confidence level of 99 %.
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1.3.14      The Practical Quantitation Limit

            The practical quantitation limit (PQL) is a limit for each compound at or below
            which data must not be reported.  It is the minimum sample mass that must
            be collected in the sampling train to allow detection during routine laboratory
            operation within the precision limits established by the MDL determination.
            The PQLs will be estimated at 5 times the MDL for those PAH that are not
            contaminants of the resin. The PQL for the remainder will be estimated at 5
            times the blank XAD-2 resin level.

2.       THE SOURCE TEST PROTOCOL

         Every performance  of this test method shall have an identified operator of the
         source to be tested, an identified end user of the test method results, and an
         identified tester who performs this test method.  Figura 1  is a summary of the
         responsibilities of the  parties involved  in the coordination and performance of the
         source test.  The protocol for the entire test procedure should be understood and
         agreed upon by the responsible parties prior to the start of the test.

2.1      RESPONSIBILITIES  OF THE END USER AND THE TESTER

2.1.1       The End User

            Before testing may begin, the end user of the test  results (1.3.9) shall specify
            a source target  concentration for each of the PAH to be determined by this
            method using the  guidelines of Section 2.2.1.

            The end user shall approve the source test protocol only after reviewing the
            document and determining that the minimum pre-test  requirements (Sections
            2.2 to 2.5 } have  been met.

2.1,2       The Tester

            The tester (1.3.10) shall have tKe  primary responsibility for the performance
            of the test method, and shall co-ordinate the efforts of the analytical group
            and the efforts  of the sampling group.

            The tester shall be responsible for the selection of an analyst with
            documented experience in the satisfactory performance of the method. The
            tester shall obtain from the analyst all of the analytical data (Section 2.3)
            that are required for pre-test calculations of sampling parameters.

             Before performing the rest of this method, the tester  shall develop and write
            a source test protocol (Section 2.2) to help ensure that useful test method
            results are obtained.  The tester shall plan the test based on the information
            provided by the end  user, the results of pre-test survsys of the source, and
            the tester's calculations of target source testing parameters (Section 2,2).

            The tester shall be responsible for ensuring that all of the sampling and
            analytical reporting requirements (Section 10)  are met.
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2.1.3        The Analyst

             The analyst snail be responsible for performing all of the required analytical
             procedures described in this test method and reporting the results as required
             by Sections 2.3,4.2.1,4,2.2,  10.1.1, 10.1.2, 10.1.3, and 10.2).

2.2      PRE-TEST REQUIREMENTS

         The source test protocol shall specify the test performance criteria of the end
         user and all assumptions, required  data and calculated targets for the following
         testing parameters:

             (1} source target concentration of each emitted PAH of interest (2.2.1),

             (2) preliminary analytical data (2.3) for each target PAH, and

             (3) planned sampling parameters (2.5.4, 2.5.5, and 2.5.6),

         The protocol must demonstrate that the testing parameters calculated by the
         tester will meet the needs of the end user.  The source test protocol shall
         describe the procedures for all aspects  of the source test including information
         on supplies, logistics, personnel and other resources necessary for an efficient
         and coordinated test.

         The source test protocol shall identify the end user of the results, the tester, the
         analytical group, and the sampling  group, and the protocol shail be signed by the
         end user of the results and the tester.

         The tester shall not proceed with the performance of the remainder of this
         method unless the source test protocol is signed by the tester and tha end user.

2.2.1        Source Target Concentration (STC)

             The tester shall not proceed with the test unless a target concentration has
             been chosen.  This will be the primary reporting objective of the emissions
             test. The  end user shall  select a basis for determining each target
             concentration from: a) regulatory limits, b) environmental risk assessments,
             and (c) the interests of the end user, the tester, and the stationary source.

2.2.1.1          Regulatory Limits

                 The regulatory limit shall be the basis for determining a target
                 concentration for stationary source emissions in those cases where the
                 purpose of the emissions test is to demonstrate compliance with the
                 established regulatory limit.

2.2,1.2          Environmental Risk Assessments

                 In some cases testing is conducted for an environmental risk
                 assessment.  A pre-test estimate of the permissible risk shall  then be
                 used to determine the target concentration for stationary source
                 emissions.

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                                                                                          I
                Note that some risk assessment methodologies wilt assume that a PAH          —
                is present at the detection limit or one half of the detection limit even          _,_•
                when the compound is not detected.  This is inappropriate for planning         ;
                for the performance of the test method because by definition a
                substance cannot be detected at one half of its detection limit.  In such          m
                cases, the target sampling parameter must be the maximum practical            •
                sample volume.
2.2.1.3         Interests of the End User, the Tester and the Stationary Source
                                                                                           I
                In cases where the emissions test is not being performed to demonstrate         •
                compliance with a regulation, nor is it required for a risk assessment,            |
                the end user may use emissions results from previous tests of the
                facility  or from similar facilities.                                              •

                If estimates of the emissions are not availble, the tester must conduct a
                preliminary test at each emissions point of interest.  This target                 «
                concentration is necessary for the calculation of the target sampling             •
                parameters required by Section 2.5. Therefore, the emissions measured
                during the preliminary test must be representative of source operation.
                The tester must document operating conditions, and know from                 I
                historical data, the extent to which the results of this  preliminary run are         •
                representative of emissions from the source. This will require
                documentation of operating conditions during the preliminary test, and a         I
                knowledge of the potential variability in emissions with differences in            I
                source operation.

                As an alternative to conducting a preliminary test, the end user may             " |
                specify,  as a sampling target, the longest  practical sampling time so as
                to obtain the lowest practically achievable source reporting limit                  •
                (Section 2.5.6).                                                             j

2.3      REQUIRED PRELIMINARY ANALYTICAL DATA                                         •

2.3.1        Results of Blank Contamination Checks

            The tester must obtain from the analyst the results of the PAH contamination
            checks. The analytical report must satisfy the reporting  requirements of
            Sections 10 and 10.1.
                                                                                             i
            The analyst shall use the procedures described in Sections 4.2.1 and 4.2.2 to
            clean the sampling media (filters and XAD-2 resin) and check for PAH
            contamination.

            Table 3 shows the results  of analyses of different lots of re-cleaned XAD-2
            resin. The purpose of this table is to show typical variability. Actual results
            may vary from one test to another.
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2.3.2        The Method Detection Limit

             The method detection limit (MDLJ must be determined by the same analyst
             (1.3.11) that will perform the analyses subsequent to sampling.  Before
             estimating the method detection limit { MDL), the analyst shall identify those
             PAH that are contaminants of the XAD-2 resin using the procedures
             described in Sections 4,2,2.1 to 4.2.2.4. The analyst shall determine the
             MDL as described in Section 8.3  and Appendix A.

2.3.3        The Practical Quantitation Limit

             The analyst shall calculate the practical quantitation limits (PQLs) for the
             target  PAH.  This value will be 5 times the MDL or  5 times the XAD-2
             background level for those compounds that have been identified  by the
             analyst as contaminants.

             Table 2 lists practical quantitation limits obtained during ARB's development
             of this method. The values for the PQLs will vary with the performance of
             individual laboratories. Therefore, the tester must obtain PQL values for all  of
             the target analytes from the analyst.

2.4      EXPECTED RANGE IN TARGET CONCENTRATIONS OF INDIVIDUAL PAHs

         The PAH compounds in a source test sample can show large differences in
         concentrations.  A sample that might provide sufficient analyte for the detection
         and quantitation of the lowest concentration PAH could contain levels of other
         PAHs that exceed the upper limit of the method.

         In some cases the solution is two GC/MS injections - first with the undiluted
         extract, and then again  after appropriate dilution of the extract. At other times
         the required minimum dilution might be so large as to result in the reduction of
         the internal standard response below the minimum required by the method.  With
         prior notification of expected levels of the target analytes, the analyst can modify
         the preparation of the samples so that useful results might be obtained.  All
         major modifications must be approved by the Executive Officer.

2.5      SAMPLING RUNS, TIME, AND VOLUME

2.5.1        Sampling Runs

             A test  shall include at least three sampling runs in series and a blank
             sampling train.

2.5.2        Minimum Sample Volume {MSVJ

             This is the minimum sample volume that must be collected in the sampling
             train to provide the minimum  reportable mass of PAH for quantitation. It
             must be based on a) the practical quantitation limit (2.3.3), b) the source
             target concentration (2,2.1),  and c) sampling limitations.  Use Equation
             429-1  to calculate the target MSV for each PAH analyte.
August 9, 1996                                             Proposed M-429  Page 7

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                                                  !                  429-1
                            MSV(dscm)  =PQL x   '
            Where:
            PQL  =  The practical quantitation limit, ng/sample (Section 2.3.3)
            STC  =  The source target concentration, ng/dscm (Section 2.2,1)

2.5.3       Minimum Sampling Time (MST)

            This is the minimum time required to collect the minimum sample volume at
            the expected average volumetric sampling rate (VSR). Use Equation  429-2
            to calculate the minimum sampling time (MST) required to collect the
            minimum sample volume calculated in Section 2.5.2. The tester must use an
            average volumetric sampling rate (VSR) appropriate for the source to be
            tested.

                                   MSV       1         1          429-2
                                 -
            Where:

            VSR   =  Expected average volumetric sampling rate, dscfm
             60    =  Factor to convert minutes to hours
         0.02831 7 =  Factor to convert dscf to dscm

            The end user must decide whether the MSTs are all practically feasible and
            whether they can be increased to allow for any deviation from the sampling
            and analytical conditions assumed by the test plan.  Based on this decision,
            the tester must use either Section 2.5.4 (a) or  2.5.4 (b) to calculate a
            planned sample volume (PSV).

2.5.4       Planned Sample Volume [PSV)

            This is the volume of emissions that must be sampled to provide the target
            analytes at levels between the PQL and the limit of linearity. The planned
            sample volume is the primary sampling target whenever practically feasible.
            The PSV is calculated according to either 2.5.4 (a) or 2.5.4 (b).

            (a)     If the end user has decided that the MSTs can be increased, the
                   tester must use  Equation 429-3 to calculate the PSV using the largest
                   of the 19 MSV values calculated in Section 2.5.2.  and the largest
                   value for F that will give a practically achievable sample volume that
                   provides the target analytes at levels between the PQL and the limit
                   of linearity. Use this PSV to calculate the planned sampling time
                   (Section 2.5.5 a) and Equation 429-6.

            (b)     If the MSTs are  not all practically achievable, the tester and the end
                   user must agree on a maximum practical sampling time
                   (Section 2.5.5b). This value must then be used for the PST in
                   Equation 429-4 to calculate the PSV. Tha tester must identify in the

August 9, 1996                                             Proposed M-429  Page 8

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                    source test protocol the target analytes for which the PSV is lower
                    than the MSV,  The primary reporting objective of the test cannot  be
                    achieved for those analytes.  If the primary reporting objective cannot
                    be achieved for all of the target analytes, it must be discussed in the
                    protocol and the alternative reporting objective (Section 2.5.6) must
                    be approved by the end user  of the results.

                    The volume of sample that is actually collected will be determined  by
                    practical sampling limitations, the intended use of the data and the
                    level of uncertainty that the end user can tolerate in the measurement
                    of the target concentrations.  This uncertainty will decrease as the
                    value of F {Equation 429-5) increases.

                                                                   429-3
                              PSV(dscm) =MSV  x F
                                                                   429-4
                             PSV(dscm)  =PST x VSR
                                     F - PSV
                                         MSV

            Where:

            PST    = Planned sampling time  from Section 2.5.5
            F       = A safety factor (> 1) that allows for deviation from ideal sampling
                      and analytical conditions


2.5.5       Planned Sampling Time {PSTJ

            Two options are available for calculating the planned sampling time
            depending on whether the primary objective can be achieved for all of the
            target analytes.

            (a)     The planned sampling time (PST) shall be long enough to 1) collect
                   the planned sample volume with reportable levels of the target
                   analytes and 2) sample representative operating conditions of the
                   source.  If the average sampling rate  (VSR) used to estimate the
                   planned sampling time cannot be achieved in the field
                   (Section 4.4.4.1), the sampling time must be recalculated using the
                   actual VSR and the target PSV in equation 429-6.

            (b)     The planned sampling time shall be a practical maximum approved by
                   the end user and it shall be long  enough to sample representative
                   operating conditions of the source.

                                                1         i        429-6
                                         ><  0028317*^
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2.5.6       Preliminary Estimate of Source Reporting Limit (SRL)

            Before the test proceeds, the end user and the tester shall agree on a
            preliminary estimate of the source reporting limit for each target PAH. The
            SRL shall be calculated using Equation 429-7. The planned sample volume
            will contain reportable levels of a given anaiyte if that analyte is present in
            the emissions at a concentration that is equal to or greater than the
            calculated SRL.

                                                POL                429-7
                               SRL(ng/dscm) =• -Lh
            Where:

            SRL  =   Preliminary estimate of source reporting limit, ng/dscm
            PQL  =   Practical quantitation limit, ng
            PSV  =   Planned sample volume, dscm

2.5.7    Example Calculations

         Figure 9 B is an example of the minimum required calculations of sampling
         parameters for the source test protocol.

3.       INTERFERENCES

         Interferences may be caused by contaminants in solvents, reagents, sorbents,
         glassware, and other sample processing hardware that lead to discrete artifacts
         and/or elevated backgrounds at the ions monitored.  All of these materials must
         be routinely demonstrated to be free from interferences under the conditions of
         the analysis by running laboratory reagent blanks as described in Section 6.1 ,1.

         The use of high purity reagents and solvents helps to minimize interference
         problems.  Purification of solvents by distillation in all-glass systems may be
         required.

         Transformation of PAH and the formation of artifacts can occur in the sampling
         train.  PAH degradation and transformation on sampling train filters have been
         demonstrated. Certain reactive PAH such as benzofalpyrene,
         benzo[a]anthracene, and fluoranthene when trapped on filters can readily react
         with stack gases. These PAH are transformed by reaction with low levels of
         nitric acid and higher levels of nitrogen oxides, ozone, and sulfur oxides.

         PAH degradation may be of even greater concern when they are trapped in the
         impingers. When stack gases such as sulfur oxides  and nitrogen  oxides come in
         contact with the impinger water they are converted  into sulfuric acid and nitric
         acid respectively. There is evidence that under such conditions certain PAH will
         be degraded.  It is recommended that the PAH levels in the impingers be used  as
         a qualitative tool to determine if breakthrough has occurred in the resin.
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4.       SAMPLING APPARATUS, MATERIALS AND REAGENTS

4,1      SAMPLING APPARATUS

         The sampling train components listed below are required. The tester may use an
         alternative to the required sampling apparatus only if, after review by the
         Executive Officer, it is deemed equivalent for the purposes of this test method.

         Mention of trade names or specific products does not constitute endorsement by
         the California Air Resources Board, In all cases, equivalent items from other
         suppliers may be used.

         A schematic of the sampling train is shown in Figure 2.  The train consists of
         nozzle, probe, heated paniculate  filter, condenser, and sorbent module followed
         by three impingers and a silica gel drying cartridge.  An in-stack filter may not be
         used because at the in-stack temperatures the filter material must be of a
         material other than the Teflon required by the method,  A cyclone or similar
         device in the heated filter box may be used for sources emitting a large amount
         of particufate matter.

         For sources with a high moisture  content, a water trap may be placed between
         the heated filter and the sorbent module.  Additional impingers may  also  be
         placed after the sorbent module.  If any of these options are used, details must
         be provided in the test report.  The train may be constructed by adaptation of  an
         ARB Method 5  train.  Descriptions of the train components are contained in the
         following sections.

4.1.1       Probe  Nozzle

            Quartz, or borosilicate glass with sharp, tapered leading edge. The angle of
            taper shall be 30° and the taper shall be on the outside to preserve a
            constant internal diameter. The probe nozzle shall be of the button-hook or
            elbow design, unless otherwise approved  by the Executive Officer.

            A range of sizes suitable for isokinetic sampling  should be available, e.g.,
            0.32 to 1.27 cm (1/8 to 1/2 in.) - or larger if higher volume sampling trains
            are used - inside diameter (ID) nozzles In increments of 0.16 cm  (1/16 in.).
            Each nozzle shall be calibrated according to the procedures outlined in
            Section 5.1  of ARB method 5.

4.1.2       Probe

            The probe should be lined  or made of Teflon, quartz, or borosilicate glass.
            The liner or  probe is to provide an inert surface for the PAH in the stack gas.
            The liner or  probe extends past the retaining nut into the stack.  A
            temperature-controlled jacket  provides protection of the liner or probe. The
            liner shall be equipped with a  connecting fitting that is capable of forming a
            leak-free, vacuum tight connection without the use of sealing greases.
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4.1.3        Preseparator
             A cyclone, a  high capacity impactor or other device-may be used if
             necessary to remove the majority of the partides before the gas stream is
             filtered. This catch must be used for any subsequent analysis. The device
             shall be constructed of quartz or borosilicate glass. Other materials may be
             used subject to approval by the Executive Officer.
4.1.4        Filter Holder
             The filter holder shall be constructed of borosilicate glass, with a Teflon frit
             or Teflon coated wire support and glass-to-glass seal or Teflon gasket.  The
             holder design shall provide a positive seal against leakage from the outside or
             around the filter. The holder shall be attached immediately at the outlet of
             the probe, cyclone, or nozzle depending on the configuration used. Other
             holder and gasket materials may be used subject to approval  by the Executive
             Officer.
4.1.5        Sample Transfer Line
             The sample transfer line shall be Teflon (1/4 in. O.D. x 1/32 in. wall) with
             connecting fittings that are capable of forming leak-free, vacuum tight
             connections without using sealing greases. The line should be as short as
             possible.
4.1.6        Condenser
             The condenser shall be constructed of borosilicate glass and shall be
             designed to allow the cooling of the gas stream to at least 20°C before it
             enters the sorbent module.  Design for the normal range of stack gas
             conditions is shown in Figure 3.
4.1.7        Sorbent Module
             The sorbent module shall be made of glass with connecting fittings that are
             able to form leak-free, vacuum tight seals without the use of sealant greases
             (Figure 3).  The vertical resin trap is preceded by a coil-type condenser, also
             oriented vertically, with circulating cold water.  Gas entering the sorbent
             module must have been cooled to 20 °C (68°F) or less.  The gas temperature
             shall be monitored by a thermocouple placed either at the inlet or exit of the
             sorbent trap.  The sorbent bed must be firmly packed and secured in place to
             prevent settling or channeling during sample collection.  Ground glass caps
             (or equivalent) must be provided to  seal the sorbent-filled trap both prior to
             and following sampling.  All sorbent modules must be maintained in the
             vertical position during sampling.
4.1.8        Impinger Train
             Connect three or more impingers in series with ground glass fittings able to
             form leak-free, vacuum tight seals without sealant greases.  All impingers
             shall be of the Greenburg-Smith design modified by replacing the tip with a
August 9, 1996                                             Proposed M-429  Page 12

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             1.3 cm (1/2 in.) I.D, glass tube extending to 1.3 cm (1/2 in.(from the bottom
             of the flask.

             The first impinger may be oversized for sampling high moisture streams. The
             first and second impingers shall contain  100 mL of 3 mM sodium bicarbonate
             (NaHC03l and 2.4 rnM sodium carbonate Na2C03) (Section 4.2.5).  This is
             intended to neutralize any acids that might form in the impingers. The third
             impinger shall be empty. Silica gel shall be  added to the fourth impinger.
             A thermometer which measures temperatures to within 1°C (2°F), shall be
             placed at the outlet of the third impinger.
4.1.9       Silica Gel Cartridge
            This may be used instead of a fourth impinger.  It shall be sized to hold 200
            to 300 gm of silica gel.

4.1.10      Pilot Tube

            Type S, as described in Section 2.1 of ARB Method 2 or other devices
            approved by the Executive Officer.  The pitot tube shall be attached to the
            probe extension to allow constant monitoring of the stack gas velocity as
            required by Section 2.1.3 of ARB Method 5. When the pitot tube occurs
            with other sampling components as part of an assembly, the arrangements
            must meet the specifications required by Section 4.1.1  of ARB Method 2.
            Interference-free arrangements are illustrated in Figures 2-6  through 2-8 of
            ARB Method 2 for Type S pitot tubes having external tubing diameters
            between 0.48 and 0.95 cm (3/16 and 3/8 in.}.

            Source-sampling assemblies that do not meet these minimum spacing
            requirements (or the equivalent of these requirements)  may be used only if
            the pitot tube coefficients of such assemblies have been determined by
            calibration procedures approved by the Executive Officer.

4.1.11      Differential Pressure Gauge

            Two inclined manometers or equivalent devices, as described in Section 2.2
            of ARB Method 2. One manometer shall be used for velocity head (AP)
            readings and the other for orifice differential pressure readings.

4.1.12      Metering System

            Vacuum gauge, leak-free  pump, thermometers accurate to within 3°C
            (5.4°F), dry gas meter capable of measuring volume to within 2 percent, and
            related equipment, as shown in Figure 2. Other metering systems must meet
            the requirements stated in Section 2.1.8 of ARB Method 5.

4.1.13      Barometer

            Mercury, aneroid, or other barometer capable of measuring atmospheric
            pressure to within 2.5 mm Hg (0.1 in. Hg).  In many cases, the barometric
            reading may be  obtained from a nearby national weather service station, in
            which case the  station value (which is the absolute barometric pressure) shall

August 9, 1996                                             Proposed M-429  Page 13

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             be requested and an adjustment for elevation differences between the
             weather station and sampling point shall be applied at a rate of minus 2.5
             mm Hg (0,1 in. Hg) per 30 m (100 ft) elevation increase or vice versa for
             elevation decrease.

4.1.14       Gas Density Determination Equipment

             Temperature sensor and pressure  gauge, as described in Section 2.3 and 2.4
             of Method 2, and gas analyzer, if  necessary, as described in Method 3.  The
             preferred configuration and alternative arrangements of the temperature
             sensor shall be the same as those described in Section 2.1.10 of ARB
             Method 5.

4.1.15       Filter Heating System

             The heating system must be capable  of maintaining a temperature around the
             filter holder during sampling of (120 ± 14°C) (248±25°F). A temperature
             gauge capable of measuring temperature to within 3°C (5.4°F) shall be
             installed so that the temperature around the filter holder can be regulated and
             monitored  during  sampling.

4.1.16       Balance

             To weigh the impingers and silica  gel cartridge to within 0.5 g.

4.2      SAMPLING MATERIALS AND REAGENTS

4.2.1        Filters

             The filters shall be Teflon coated glass fiber filters without organic binders, or
             Teflon membrane filters, and shall exhibit at least 99.95 percent efficiency
             (0.05 percent penetration) on 0.3  micron  dioctyl phthalate smoke particles.
             The filter efficiency test shall be conducted in accordance with ASTM
             standard Method  D 2986-71.  Test data from the supplier's quality control
             program are sufficient for this purpose. Record the manufacturer's lot
             number.

4.2.1.1           Contamination Check of Filter

                 The tester must have the filters cleaned by the analyst and checked for
                 contamination prior to use in the field.  The contamination check must
                 confirm that  there are no PAH contaminants present that will interfere
                 with the analysis of the sample PAHs of interest at the target reporting
                 limits.  The analyst must record the date the filter was cleaned.

                 The filters shall be cleaned in batches not to exceed 50 filters. To clean
                 the filters, shake for one hour in  methylene chloride in a glass dish that
                 has been cleaned according to Section 6.2. After extraction, remove
                 the filters and dry them under a clean N2 stream.  Analyze  one filter
                 using  the same extraction, clean-up and analysis  procedures to be used
                 for the field samples {Sections 6.5.1.2, 6.6, and  7.5).
August 9, 1996                                            Proposed M-429  Page 14

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                       Blank value _ Total mass (ng) of anaiyte      429-8
                        per filter   "    NO, filters extracted

                 The acceptance criteria for filter cleanliness depends on t) the method
                 reporting limit, 2} the expected field sample volume and 3J the desired
                 reporting limit for the sampled emissions stream.   Filters with PAH
                 levels equal to or greater than the target reporting limit for the analyte(s)
                 of concern shall be rejected for field use.

                 If the filter does not pass the contamination check, re-extract the batch
                 and analyze a clean filter from the re-extracted batch. Repeat the re-
                 extraction and analysis until an acceptably low background level is
                 achieved.  Store the remainder tightly wrapped in clean hexane-rinsed
                 aluminum  foil as described in Section 4.3.3.

                 Record the date of the last cleaning of the filters and the date of the
                 PAH analysis, and prepare a laboratory report of the analytical results
                 that includes  all of the information required by Section 10.2.

                 The tester shall obtain this laboratory report with the date of cleaning of
                 the filters, and the date of the filter contamination check from the
                 analyst, and report them in the source test protocol and  the test report
                 as required by Sections 10.1 and 10.3.

4.2.2        Amberlite XAD-2 Resin

             The XAD-2 resin must be purchased precleaned and then cleaned again as
             described below before use in the sampling train.

4.2.2.1          Cleaning XAD-2 Resin

                 This procedure must be carried out in a giant Soxhlet extractor which
                 will hold enough XAD-2 for several sorbent traps, method blanks and QC
                 samples.  Use an all glass thimble containing an extra coarse frit for
                 extraction of the XAD-2. The frit is recessed 10 to 15 mm above a
                 crenelated ring at the bottom of the thimble to facilitate drainage.  The
                 resin must be carefully retained in the extractor cup with a glass wool
                 plug and stainless steel screen to prevent floating on the methyiene
                 chloride.

                 Clean the resin by two sequential 24 hour Soxhlet extractions with
                 methyiene chloride. Replace with fresh methyiene chloride after the first
                 24 hour period.

4.2.2.2          Drying Cleaned XAD-2 Resin

                 The adsorbent must be dried with clean inert gas.  Liquid nitrogen from a
                 standard commercial liquid nitrogen cylinder has proven to be a reliable
                 source of large volumes of gas free from organic contaminants. A
                 10.2 cm ID Pyrex pipe 0.6 m long with suitable retainers as shown in
                 Figure 4 will serve as a satisfactory column.  Connect the liquid nitrogen

August 9, 1996                                              Proposed M-429 Page 15

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                cylinder to the column by a length of cleaned 0.95 cm ID copper tubing,
                coiled to pass through a heat source.  A convenient heat source is a
                water bath heated from  a steam line.  The final nitrogen temperature
                should only be warm to  the touch and not over 40 °C.

                Continue the flow of nitrogen through the adsorbent until all the residual
                solvent is removed. The rate of flow should be high enough that the
                particles are gently agitated but not so high as to causa  the particles to
                break up.

4.2.2.3         Residual Methylene Chloride Check.

                Extraction: Weigh a 1.0 g sample of dried resin into a small vial, add 3
                rnL of hexane, cap the vial and shake it well.

                Analysis: Inject a 2 //L sample of the extract into a gas chromatograph
                operated under the following conditions:

                Column:         6 ft x  1/8 in stainless steel containing 10% OV-101
                                 on 100/120 Supelcoport.

                Carrier Gas:      Helium at a rate of 30 rnL/min.

                Detector:        Flame ionization detector operated at a sensitivity of 4
                                 X 10'11 A/mV.

                Injection Port
                Temperature:     250 °C.

              .  Detector
                Temperature:     305 °C.

                Oven                   /
                Temperature:     30 °C for 4 min; programmed to rise at 40 °C per min
                                 until it reaches 250 °C; return to 30 °C after 1000
                                 seconds.

                Compare the results of the analysis to the results from a reference
                solution prepared by adding 2.5 fiL of methylene chloride into  100  ml of
                hexane.  This corresponds to 100 yg of methylene chloride per g of
                adsorbent. The maximum acceptable concentration is 1000^/g/g of
                adsorbent. If the methylene chloride in the adsorbent exceeds this level,
                drying must be  continued until the excess methylene chloride is
                removed.

4.2.2.4         Contamination Check of XAD-2 Resin

                The cleaned, dried XAD-2 resin must be checked for PAH contamination.
                Analyze a sample of the resin equivalent in size to the amount required
                to charge one sorbent cartridge for a sampling train. The extraction,
                concentration, cleanup and GC/MS analytical procedures shall be the
August 9, 1996                                            Proposed M-429  Page 16

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                 same for this sample as for the field samples (Sections 6.5.1.2, 6,6, and
                 7.5).

                 The acceptance limit will depend on the PQL, the expected
                 concentration in the sampled gas stream,  and the planned sample
                 volume.  The contamination level must be less than the PQL or no more
                 than 20 percent of the expected sample level.

                 If the cleaned resin yields a value for a target analyte which is not
                 acceptable for the end user's intended application of the test results,
                 repeat the extraction unless the analyst has historical data that
                 demonstrate that  re-extraction cannot reasonably be expected to further
                 reduce the contamination levels.  The tester must obtain these data from
                 the analyst and include them in both the source test protocol and the
                 emissions test report.

                 The contamination check shall be repeated if the analyst does not have
                 such historical data.  The analyst shall reclean and dry the resin
                 (4.2.2.1, 4.2.2.2, and 4.2.2.3) and repeat the PAH analysis of the re-
                 cleaned resin. If the repeat analysis yields a similar result to the first,
                 record the contamination level for both the initial cleaning and the re-
                 cleaning.

                 The analyst shall record the dates of the cleaning and extraction of the
                 resin, and prepare a laboratory report of the analytical results that
                 includes all of the information required by  Section 10.2.

                 The tester shall obtain the dates of cleaning and the laboratory report of
                 the results of the  contamination check from the analyst, and report them
                 in both the source test protocol and the emissions test report as required
                 by Sections 10.1  and 10.3.

                 The tester shall identify the analytes for which the PQLs wiil be based
                 on a  blank contamination value, and calculate the PQLs as required by
                 Section 2.3.3.
4.2.2.5          Storage of XAD-2 Resin
                 After cleaning, the resin may be stored in a wide mouth amber glass
                 container with a Teflon-lined cap, or placed in one of the glass adsorbent
                 modules wrapped in aluminum foil and capped or tightly sealed with
                 Teflon film at each end. The containers and modules shall then be
                 stored away from light at temperatures 4 °C or lower until the resin is
                 used in the sampling train.

                 The adsorbent must be used within twenty one (21) days of cleaning. If
                 the adsorbent is not used within 21 days, it must be  re-checked for
                 contamination before use.
August 9, 1996                                             Proposed M-429 Page 17

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4.2.3        Silica Gel
             Indicating type, 6 to 16 mesh. If previously used, dry at 175°C (350°F) for 2
             hours. New silica gel may be used as received. Alternatively, other
             desiccants (equivalent or better)  may be used, subject to approval by the
             Executive Officer.
4.2.4        Reagent Water
             Deionized, then glass-distilled, and stored in hexane- and methylene chloride-
             rinsed glass containers with TFE-lined screw caps.

4.2.5        Impinger Solution

             Sodium bicarbonate 3 mM, and sodium carbonate 2.4 mM.  Dissolve
             1.0081 g sodium bicarbonate (NaHC03) and 1.0176 g of sodium carbonate
             {Na2C03) in reagent water (4.2.4), and dilute to 4 liters.

4.2.6        Crushed Ice

             Place crushed ice in the water bath around the impingers.

4.2.7        Glass Wool

             Cleaned by sequential rinsing in three aliquots of hexane, dried in a 110 °C
             oven, and stored in a hexane-washed glass jar with TFE-lined screw cap.

4.2.8        Chromic Acid Cleaning Solution

             Dissolve 200 g of sodium dichromate in 15 ml of reagent water, and then
             carefully gdd 400 mL of concentrated sulfuric acid.

4.3      PRE-TEST PREPARATION

         The positive identification and quantitation  of PAH in an emissions test of
         stationary sources are strongly dependent on the integrity of the samples
        ' received and the precision and accuracy of all analytical procedures employed.
         The QA procedures described in Sections 4.3.7 and 8 are to be used to monitor
         the performance of the sampling methods,  identify problems, and take corrective
         action.

4.3.1        Calibration

             All sampling train components shall be maintained and calibrated according to
             the procedure described in APTD-0576  (Section 11.7), unless otherwise
             specified herein. The tester shall maintain a record  of all calibration data.

4.3.1.1      Probe Nozzle

             Probe nozzles shall be calibrated according to the procedure described in
             ARB Method 5.
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 4.3.1.2     PitotTube
             Calibrate the Type S pilot tube assembly according to the procedure
             described in Section 4 of ARB Method 2.
 4.3.1.3      Metering System
             Calibrate the metering system before and after use according to the
             requirements of Section 5.3 of ARB Method 5.

4.3.1.4      Temperature Gauges

             Use the procedure in Section 4.3 of ARB Method 2 to calibrate in-stack
             temperature gauges.  Dial thermometers, such as those used for the dry gas
             meter and condenser outlet, shall be calibrated against mercury-in-giass
             thermometers.

4.3.1.5      Leak Check of Metering System Shown in Figure 1

             The tester shall use the procedure described in Section 5.6 of ARB Method 5

4.3.1.6      Barometer

             Calibrate against a mercury barometer.

4.3.2        Cleaning Glassware for Sampling and Recovery

             All glass parts of the train upstream of and including the sorbent module and
             the first impingers shall be cleaned as described in Section 3A of the 1974
             issue of Manual of Analytical Methods for Analysis of Pesticide Residues in
             Human and Environmental Samples (Reference 11.4). Take special care to
             remove residual silicone grease sealants on ground glass connections of used
             glassware.  These greasy  residues shall be removed by soaking several hours
             in a chromic acid cleaning solution (4.2.8)  prior to  routine  cleaning as
             described above. Other cleaning procedures may be used as long as
             acceptable blanks are obtained.  Acceptance criteria for blanks  are stated in
             Section 8.2.

             Rinse all glassware with acetone, hexane,  and methylene  chloride prior to use
             in the PAH sampling  train.

             Glassware used in sample recovery procedures must be rinsed as soon as
             possible after use with the last solvent used in it. This must be followed by
             detergent washing with hot water, and rinses with tap water, deionized
             water, acetone, hexane, and methylene chloride. Other cleaning procedures
             may be used as long as acceptable blanks are obtained. Acceptance criteria
             for blanks are stated in Section 8.2.

4.3.3        Preparation of Filter

             The clean dry filter (4.2.1) must be kept tightly wrapped in hexane-rinsed
             aluminum foil and stored at 0 to 4°C in a container away from light until

August 9, 1996                                             Proposed M-429  Page 19

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            sampling. Before inserting the filter in the sampling train, check visually
            against light for irregularities and flaws or pinhole leaks.

4.3.4       Preparation of Sorbent Cartridge, Method Blank, and
            Laboratory Control Samples

            Sorbent Cartridge

            Use a sufficient amount (at least 30 gms or 5 gms/m3 of stack gas to be
            sampled) of cleaned resin to  completely fill the glass sorbent cartridge which
            has been thoroughly cleaned as prescribed (4.2.2).

            Add the required surrogate standards  (Table 7) to the sorbent cartridges for
            all of the sampling and blank trains for each series of test runs.  Follow  the
            resin with hexane-rinsed glass wool, cap both ends, and wrap the cartridge In
            aluminum foil. Store the prepared cartridges as required by Section 4.3.5.

            The sorbent cartridges must  be loaded, and the surrogate standards must be
            added to the resin in a clean  area in the laboratory.  There  must be no
            turnaround of a used cartridge in the field.

            The analyst shall record the date that the surrogate standards were added to
            the resin and the amount of each compound.  The tester shall obtain these
            data from the analyst and report them in the source test protocol and the
            test report.

            The appropriate levels for the surrogate standards are given in Table 7 which
            shows the spiking plan for surrogate standards, internal standards, alternate
            standards, and recovery standards. All of these required compounds are
            generally available. Additional labelled PAH may also be used if available.
            The labelled compounds used as surrogate standards must be different from
            the internal standards used for quantitation, and from the alternate and
            recovery standards.  If the spiking scheme (Table 7} is modified, the tester
            must demonstrate that the proposed modification will generate data of
            satisfactory quality.  Table 7A shows an approved modification that has been
            used in ARB's method development.  All modifications must be approved by
            the Executive Officer before  the emissions test is performed.

            Laboratory Method Blank

            Take a sample of XAD-2 resin from the  same batch used to prepare the
            sampling cartridge. This will serve as the laboratory method blank
            (Section 8.1.1).  The mass of this sample must be the same as that used  in
            the sampling train. Spike with the same surrogate standards at the same
            levels used in the sampling cartridges.

            Laboratory Control Sample

            Set aside two  samples of XAD-2 resin from the same batch used to prepare
            the sampling cartridge. These will serve as the  laboratory control samples.
            (Section 8.1.3).  The mass of each sample must be the same as that used in
            the sampling train.

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4.3.5        Storage of Prepared Cartridges, Method Blank and Laboratory Control Sample

             Store the aluminum foil wrapped sorbent cartridges away from light at 4 °C
             or lower until they are fitted into the sampling trains.  Do not remove the
             caps before the setup of the sampling train.

             The maximum storage time from cleaning of the resin to sampling with the
             spiked resin cartridge must not exceed 21 days (4.2.2.5).

             Store the laboratory method blank and laboratory control samples in amber
             glass jars with Teflon lined lids at temperatures no higher than 4 °C.

4.4      SAMPLE COLLECTION

         Because of the complexity of this method, testers must be experienced with the
         test procedures in order to ensure  reliable results.

4.4.1        Preliminary Field Determinations

             Select the sampling site and the minimum number of sampling points
             according to ARB Method  1 or as specified by the Executive Officer.

             Determine the stack pressure,  temperature, and the range of velocity heads
             using ARB Method 2.  Conduct a leak-check of the pilot lines according to
             ARB Method 2, Section 3.1.

             Determine the moisture content using ARB Method 4 or its alternatives for
             the purpose of making isokinetic sampling rate settings.

             Determine the stack gas dry molecular weight, as described in ARB
             Method 2, Section 3.6. If integrated sampling (ARB Method 3} is used for
             molecular weight determination, the integrated bag sample shall be taken
             simultaneously with, and for the same total length of time as, the sample
             run.

             Select a nozzle size based  on the range of velocity heads, such that it is not
             necessary to change the nozzle size in order to maintain isokinetic sampling
             rates.  Do not change the nozzle size during the run.  Ensure that the proper
             differential pressure gauge is chosen for the range of velocity heads
             encountered (see Section 2.2 of ARB Method 2).

             Select a probe extension length such that all traverse points can be sampled.
             For large stacks, consider sampling from opposite sides of the stack to
             reduce the length of probes.

             The target sample volume  and  sampling time must already have been
             calculated for the source test protocol and approved by the end user as
             required by Sections 2.2 and 2.5. The total sampling time must be such that
             (1)  the sampling  time per point is not less than 2 minutes (or some greater
             time interval as specified by the Executive Officer), and (2) the total gas
             sample volume collected (corrected to standard conditions) will not be less
             than the target value calculated for the source test protocol (Section 2.5.5).

August 9, 1996                                             Proposed M-429 Page 21

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             To avoid timekeeping errors, the number of minutes sampled at each point
             should be an integer or an integer plus one-half minute.

4.4.2        Preparation of Collection Train

             Keep ail openings where contamination can occur covered until just prior to
             assembly or until sampling is about ta begin.

             Caution:  Do not use sealant greases in assembling the sampling train.

             Record the performance of the setup procedures for the sampling train.
             Figure 10 is an example of a form for recording the sampling train setup data.
             The tester must record af! of the routine information indicated on this form as
             well as any additional data which are necessary for documenting the quality
             of any reported results.

             Race 100 ml of the impinger solution (4-2.5) in  the first impinger and weigh.
             Record the total weight.  Repeat the procedure for the second impinger.
             Leave the third impinger empty.  Weigh the empty third impinger and record
             the weight.

             Weigh 200  to 300 g of silica gel to the nearest 0.5 g directly into a tared
             impinger or  silica gel cartridge just prior to assembly of the sampling train.
             The tester may optionally measure and record in advance of test time the
             weights of several portions of silica gel in air-tight containers. One portion of
             the preweighed silica gel must then be transferred from its container to the
             silica gel cartridge  or fourth impinger.  Place the container in  a clean place for
             later use in the sample recovery.

             Using tweezers or clean disposable surgical gloves, place a filter in the filter
             holder.  Be sure that the filter is properly centered and the gasket properly
             placed so as to prevent the sample gas stream from circumventing the filter.
             Check the filter for tears after assembly of the filter holder is completed.

             Mark the probe extension with heat resistant tape or by some other method
             to denote the proper distance into the stack or duct for each  sampling point.

             Assemble the train as in Figure 2. Place crushed ice around the impingers.

4.4.3        Leak Check Procedures

4.4.3,1          Pretest Leak Check

                 After the sampling train has been assembled, turn on and set the filter
                 and probe heating systems at the desired operating temperatures.  Allow
                 time for the temperature to stabilize.   Leak-check the train at the
                 sampling site by plugging the nozzle with a  TFE plug and pulling a
                 vacuum of at least 380 mm Hg (15 in. Hg).

                 Note:     A lower vacuum may be used, provided that it is not
                           exceeded during the test.
August 9, 1996                                            Proposed M-429  Page 22

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                 The following leak-check instructions for the sampling train are
                 described in Section 4.1.4.1 of ARB Method 5.  Start the pump with by-
                 pass valve fully open and coarse adjust valve completely closed.
                 Partially open the coarse adjust valve and slowly close the by-pass valve
                 until the desired vacuum is reached. Do not reverse the direction of the
                 by-pass valve. This will cause water to back up into the filter holder.  If
                 the desired vacuum is exceeded, either leak-check at this higher vacuum
                 or end the leak-check as described below and start over.

                 Determine the leakage rate. A leakage rate in excess of 4 percent of the
                 average sampling rate or 0.00057 m  per min. (0.02 cfm), whichever is
                 less, is unacceptable. Repeat the leak check procedure until an
                 acceptable leakage rate is obtained.  Record the leakage rate on the field
                 data sheet (Figure 5).

                 When the leak-check is completed,  first slowly remove the plug from the
                 inlet to the probe nozzle and immediately turn off the vacuum pump.
                 This prevents water from being forced backward and keeps silica gel
                 from being entrained backward.
4.4.3.2          Leak Checks During Sample Run
                 If, during the sampling run, it becomes necessary to change a
                 component (e.g., filter assembly or impinger), a leak check shall be
                 conducted  immediately before the change is made. The leak-check
                 shall be done according to the procedure described in Section 4.4.3.1
                 above, except that it shall be done at a vacuum equal to or greater than
                 the maximum value recorded up to that point in the test. If the leakage
                 rate is found to be no greater than 0.00057 m3/min (0.02 cfm) or 4
                 percent of the average sampling rate (whichever is less), the results are
                 acceptable, and no correction will need to be applied to the total  volume
                 of dry gas metered.  If, however, a higher leakage rate is obtained, the
                 tester shall either (1) record the leakage rate and correct the volume of
                 gas sampled since the last leak  check as shown in Section 4.4.3.4
                 below, or (2) void the sampling  run. Record the leakage rate.

                 Immediately after component changes, leak-checks must be conducted
                 according to the procedure outlined in Section 4.4.3.1 above.  Record
                 the leakage rate on the field data sheet (Figure 5).
4.4.3.3          Post Test Leak Check
                 A leak-check is mandatory at the conclusion of each sampling run.  The
                 leak-check shall be done in accordance with the procedures outlined in
                 Section 4.4.3.1  except that it shall be conducted at a vacuum equal to
                 or greater than the maximum value recorded during the sampling run.
                 Record the leakage rate on the field data sheet (Figure 5). If the leakage
                 rate is found to be no greater than 0.00057 m3/min (0.02 cfm)  or 4
                 percent of the average sampling rate (whichever is less),  the results are
                 acceptable, and no correction need be applied to the total volume of dry
                 gas metered.  If, however, a higher leakage rate is obtained, the tester
August 9, 1996                                             Proposed M-429  Page 23

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                shall either, (1) record the leakage rate and correct the sample volume as
                shown in Section 4.4.3.4 below, or (2) void the sampling run.

4.4.3.4         Correcting  for Excessive Leakage Rates

                If the leakage rate observed during any leak-check after the start of a
                test exceeds the maximum leakage rate La (see definition below),
                replace Vm in Equation 429-9 with the following expression,

                         Vm -{Lj -La)8j  -  (L   -La)6          429-9
                           m   2^t |l-'  '-a'^i    »"-p  '-a'*?


                Where:

                Vm =    Volume of gas sampled as measured by the dry gas meter
                         (dscf).

                La  =    Maximum acceptable leakage rate equal to 0.00057 m^/min
                         (0.02 ft3/min) or 4% of the average sampling rate, whichever is
                         smaller.

                Lp  =    Leakage rate observed  during the post-test leak-check, m3/min
                         (ft3/min).

                Lj   =    Leakage rate observed  during the leak-check performed prior to
                         the "ith" leakcheck (i = 1,2,3...n), m3/min (ft3/min).

                0j   =    Sampling time interval between two successive leak-checks
                         beginning with the interval between the first and second leak-
                         checks, min.

                0p  =    Sampling time interval between the last (n*) leak-check and the
                         end of the test, min.

         Substitute only for those leakage rates (Lj or Lp) which exceed La.

4.4.4    Train Operation

4.4.4.1     Sampling Train

            During the sampling run maintain a sampling rate within 10 percent  of true
            isokinetic, unless otherwise specified or approved by the Executive Officer.
            The actual sampling rate must be at or abova the VSR (Equation 429-4) to
            collect the target sample mass in the estimated sampling time.  If the target
            sampling rate cannot be achieved, adjust the planned sampling time to
            achieve the target sample volume (PSV).

            For each run, record the data required on the sample data sheet shown in
            Figure 5. The operator must record the dry gas meter reading at the
            beginning of the test, at the beginning and end of each sampling time


August9, 1996                                            Proposed M-429 Page 24

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             increment, when changes in flow rates are made, before and after each leak
             check, and when sampling is halted.

             Record other readings required by Figure 5 at least once at each sample point
             during each time increment and additional readings when significant changes
             (20 percent variation in velocity head readings) necessitate additional
             adjustments in flow rate.

             Level and zero the manometer.  Because the manometer level and zero may
             drift due to vibrations and temperature changes, make periodic checks during
             the traverse.

             Clean the portholes prior to the test run to minimize the  chance of sampling
             the deposited material. To  begin sampling, remove the nozzle cap and verify
             that the pitot tube and probe extension are properly positioned.  Position the
             nozzle at the first traverse point with  the tip pointing directly,into the gas
             stream.

             Immediately start the pump and adjust the flow to isokinetic conditions.
             Nomographs are available, which aid  in the rapid adjustment of the isokinetic
             sampling rate  without excessive computations. These nomographs are
             designed for use when the Type S pitot tube coefficient (Cp) is 0.85±0.02,
             and the stack gas equivalent density  (dry molecular weight) (Md) is equal to
             29 ±4.  APTD-0576 (Reference 11.7) details the procedure for using the
             nomographs.  If  Cp and Md are outside the above stated  ranges, do not use
             the nomographs unless appropriate steps (see Reference 11.8) are taken to
             compensate for the deviations.

             When the stack  is under significant negative pressure (height of impinger
             stem), take care to close  the coarse adjust valve before  inserting the probe
             extension assembly into the stack to  prevent water from being forced
             backward. If necessary, the pump may be turned on with the coarse adjust
             valve closed.

             When the probe  is in position, block off the openings around the probe and
             porthole to prevent unrepresentative dilution of the gas stream.

             Turn on the recirculating pump for the adsorbent module and the condenser,
             and begin monitoring the temperature of the gas entering the adsorbent trap.
             Ensure that the temperature of the gas is 20 °C or lower before sampling is
             started.

             Traverse the stack cross section, as required by ARB Method 1 or as
             specified by the Executive Officer, being careful not to bump the probe
             nozzle into the stack walls when sampling near the walls or when  removing
             or inserting the probe extension through the portholes. This minimizes the
             chance of extracting deposited material.

             During the test run, take appropriate steps  (e.g., adding crushed ice to the
             impinger ice bath) to maintain the temperature at the condenser outlet below
             20°C (68°F). Also, periodically check the level and zero of the manometer.
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             If the pressure drop across the filter becomes too high, making isokinetic
             sampling difficult to maintain, the filter may be replaced during a sample run.
             Another complete filter assembly must be used rather than changing the filter
             itself.  Before a new filter assembly is installed, conduct a leak-check as
             outlined-in Section 4.4.3.2. The total PAH analysis shall include the
             combined catches of all filter assemblies.

             A single train shall be used for the entire sample  run, except in cases where
             simultaneous sampling is required in two or more separate ducts or at two or
             more different locations within the same duct, or, in cases where equipment
             failure necessitates a change of trains.  In all other situations, the use of two
             or more trains will be subject to approval by the Executive Officer.

             Note that when two or more trains are used, a separate analysis of each train
             shall be performed, unless identical nozzle sizes were used on all trains, in
             which case the catches from the individual trains may be combined and a
             single analysis performed.

             At the end of the sample run, turn off the  pump, remove the probe extension
             assembly from the stack,  and record the final dry gas meter reading. Perform
             a leak-check, as outlined in Section 4.4.3.3. Also, leak-check the pitot lines
             as described in ARB Method 2; the lines must pass this leak-check, in order
             to validate the velocity head data. Record leakage rates.

             Record any unusual events during the sampling period.

4.4.4.2      Blank Train

             There shall  be at least  one blank train for each series of three or fewer test
             runs.  For those sources at which emissions are sampled at more than one
             sampling location, there shall be at least one blank train assembled at each
             location for each set of three or fewer runs.

             Prepare and set up the blank train in a manner identical to that described
             above for the sampling trains. The blank train shall be taken through all of
             the sampling train preparation steps including the leak check without actual
             sampling of the gas stream.  Recover  the blank train as described in
             Section 5.3. Follow all subsequent steps specified for the sampling  train
             including extraction, analysis, and data reporting.

4.4.5        Calculation of Percent Isokinetic

             Calculate percent isokinetic {Section 4.5.7) to determine whether the run
             should  be repeated.  If there was difficulty in maintaining isokinetic rates
             because of  source conditions, consult with the Executive Officer for possible
             variance on the isokinetic  rates.

4.5      CALCULATIONS

         Carry out calculations retaining at least one extra decimal  figure beyond that of
         the acquired data.  Round  off  figures after the final calculation.
August 9, 1996                                             Proposed M-429 Page 26

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 4.5.1    Nomenclature

         A      =   Cross-sectional area of stack, ft2.

         An     =   Cross-sectional area of nozzle, ft2.

         BWS     =   Water vapor in the gas stream, proportion by volume.

         Cs      =   Concentration of PAH in stack gas, ng/dscm, corrected to standard
                     conditions of 20°C, 760 mm Hg (68°F, 29.92 in. Hg) on dry basis.

         Gs      =   Total mass of PAH in stack gas sample, ng.

         AH     =   Average pressure differential across the orifice meter, mm H20 (in.
                     H20).

         I        =   Percent isokinetic sampling.

         La      =   Maximum acceptable leakage rate for either a pretest leak-check or
                     for a leak check following a component change; equal to 0.00057
                     m3/min (0,02 cfm) or 4 percent of the average sampling rate,
                     whichever is less.

         Lj      =   Individual leakage rate observed during the leak-check conducted
                     prior to the "ith" component change (i  = 1 , 2, 3, ...n), m3/min
                     (cfm).

         Lp      =   Leakage rate observed during  the post-test leak check,  m3/min
                     (cfm).

         Md     =   Molecular weight of stack gas, dry basis, Ib/lb-mole {g/g-mole).

         Mw     =   Molecular weight of water,  18.0 g/g-mole (18.0 Ib/lb-mole).
                                       s
         Ms      =   Molecular weight of stack gas, wet basis, Ib/lb-mole (g/g-mole).

         Pbar     =   Barometric pressure at the sampling site, mm Hg (in, Hg).

         Ps      =  Absolute stack gas pressure, mm Hg (in Hg).

         pstd     =  Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
                        volumetric stack gas flow rate corrected to standard conditions,
                    dscf/min (dscm/min).

         pw      =  Density of water, 0.9982 g/mL (0.002201 Ib/mL).

         R       =  Ideal gas constant 0.06236 mm Hg-m3/°K-g-mole (21.85 in Hg-
                    ft3/R-lb-mole).
August 9, 1996                                            Proposed M-429  Page 27

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         Tm     =  Absolute average dry gas meter temperature, °K (°R).

         Ts      =  Absolute average stack gas temperature °K (°R),

         T«d     -  Standard absolute temperature, 293°K (528°R).

         V1c     =  Total volume of liquid collected in impingers and silica gel, mL.

         Vm     =  Volume of gas sample as measured by dry gas meter, dcm (dcf).

         Vmistdi  =  Volume of gas sample measured by the dry gas meter, corrected to
                    standard conditions, dscm (dscf).

         VW(Std)  =  Volume of water vapor in the gas sample, corrected to standard
                    conditions, dscm (dscf).

         vs      =  Stack gas velocity, calculated by ARB Method 2, Equation 2*9,
                    ft/sec (m/sec).

         Y       =  Dry gas meter calibration factor.

         9       ss  Total sampling time, min.

         61      =  Sampling time interval, from the beginning of  a run until the first
                    component change, min.

         9j       «=  Sampling time interval between two successive component
                    changes, beginning with the interval between the first and second
                    changes, min.

         6p      =  Sampling time interval, from the final  (n*) component change  until
                    the end of the sampling run, min,
                                        1              th
         
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                                   -   Tfg                 >'  TTl
             »/       »/  v  ' s         lo.b/    !>•  i,  v  \       lo.b
             vm(std) =vm " -s=— J - 5 - L  = Kl vm Y
                            1 m       rstd
            Where:
                        Tstd
                 K1  =  	      =  0.3858 °K/mm Hg for metric units
                        Pstd
                                  =  17.65 °R/in Hg for English units

             NOTE:  Equation 429-10 may be used as written unless the leakage rate
             observed during any of the mandatory leak-checks (i.e., the post-test leak-
             check or leak-checks conducted prior to component changes) exceeds La.  If
             Lp or Lj exceeds La, Vm in Equation 429-10 must be modified as described in
             Section 4.4.3.4.

4.5.4        Average Stack Gas Velocity

             Calculate the average stack gas velocity, vs, as specified in ARB Method 2,
             Section 5.2,

4.5.5        Volume of Water Vapor

             Calculate the volume of water vapor using Equation 429-11 and the weight
             of the liquid collected during sampling (Sections 5.3.6 and 5.3.8).
                        /      —  \/    rw   '"5Ui  _ ix  ••
                        /wwd)  -  Vlc _  _  - K2
            Where:
                 K2  —  0.001333 m3/mL for metric units, or
                     =  0.04707 ft3/mL for English units. .
4.5.6       Moisture Content
            Calculate the moisture content of the gas, Bws.
                              •'WS
                                          Vwistd)                     429-12
                                     vm|stdj  * vw{stdl
         NOTE:  In saturated or water-droplet laden streams, the procedure for
                 determining the moisture content is given in the note to Section 1.2 of
                 Method 4.  For the purpose of this method, the average stack-gas
                 temperature from Figure 5 may be used for this determination, provided
                 that the accuracy of the in-stack temperature sensor is ± 1°C (2°FJ
August 9, 1996                                            Proposed M-429  Page 29

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4.5,7       Isokinetic Variation


4.5.7.1          Calculation from Raw Data
                         100Ts[K3V1c  *  Vpl (Pbar *  *")]        429-13
                                           Tm  \       J3.b/
                        	[	Jm	
                                    60 0 vs P, An


            Where:


                K3  = 0.003454 mm Hg-m3/mL-°K for metric units


                    = 0.002669 in Hg-ft3/mL-°R for English units


4.5.7.2         Calculation from Intermediate Values



                                  100TsVm(std, P^
                             Tstd vs 9 An P5 60 ( 1 - Bws)            429-14
                            -
                              4
                                   VSB An(1 -Bws)


            Where:


                K4  =  4.320 for metric units.


                    =  0.09450 for English units.


4.5.8       Average stack gas dry volumetric flow rate


            Use Equation 429-1 5 to calculate the average dry volumetric flow rate of the
            gas.

                                                    f P \            429-1 5
                         Qstd =60K, (1  -B^s) vsAMj



            Where;

                        Tstd
                K,  =  —     =  0.3858  °K/mm Hg for metric units

                        pstd
                                 =   17.65 °R/in Hg for English units


4.6      ISOKINETIC CRITERIA


         If 90 percent <  I < 1 10 percent, the isokinetic results are acceptable. If there
         is a bias to the results because I  <  90  percent or I > 110 percent, then the
         results must be rejected and the test repeated, unless the test results are
         accepted by the Executive Officer.





August 9, 1996                                            Proposed M-429 Page 30

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5        SAMPLE RECOVERY

5.1      SAMPLE RECOVERY APPARATUS

5.1.1        Probe Nozzle Brush

             Inert bristle brush with stainless steel wire handle.  The brush shall be
             properly sized and shaped to brush out the probe nozzle.

5.1.2        Wash Bottles

             Teflon wash bottles are required; Teflon FEP*.

5,1.3        Glass Sample Storage Containers

             Precleaned narrow mouth amber glass bottles, 500 mL or 1000 ml.  Screw
             cap liners shall be Teflon.

5.1.4        Filter Storage Containers

             Sealed filter holder or precleaned, wide-mouth amber glass containers with
             Teflon lined screw caps.

5.1.5        Balance

             To measure condensed water to within 0.5 g.

5.1.6        Silica Gel Storage Containers

             Air tight  metal containers to store silica gel.

5.1.7        Funnel and Rubber Policeman

             To aid in transfer of sifica gel to container; not necessary if silica gel is
             weighed  in the field.

5.1.8        Funnel

             To aid in sample recovery.  Glass or Teflon* must be used.

5.1.9        Ground Glass Caps or Hexane Rinsed Aluminum Foil

             To cap off adsorbent tube and the other sample-exposed portions of the
             aluminum foil.

5.1.10       Aluminum Foil

             Heavy-duty, precleaned with methylene chloride.
August 9, 1996                                             Proposed M-429 Page 31

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5.2      SAMPLE RECOVERY REAGENTS

5.2.1        Reagent Water

            Deionized (Dl), then glass distilled, and stored in hexane and methylene
            chloride-rinsed glass containers with TFE-lined screw caps.
5.2.2       Acetone
            Nanograde quality.  "Distilled in Glass" or equivalent, stored in original
            containers.  A blank must be screened by the analytical detection method.
5.2.3       Hexane
            Nanograde quality-  "Distilled in Glass" or equivalent, stored in original
            containers.  A blank must be screened by the analytical detection method.

5.2.4       Methylene Chloride

            Nanograde quality or equivalent.  A blank must be screened by the analytical
            detection method.

5.3      SAMPLE RECOVERY PROCEDURE

         Proper cleanup procedure begins as soon as the probe is removed from the stack
         at the end of the sampling period and a post test leak check has been performed
         (4.4.3.3).  Allow the probe to cool.

         When the probe can be safely handled, wipe off all external particulate matter
         near the tip of the probe nozzle. Conduct the post test leak check as described
         in Section 4.4.3.3. Remove the probe from the train and close off both ends of
         the probe with precleaned aluminum  foil (5.1.10). Seal off the inlet to the train
         with a ground glass cup or precleaned aluminum foil.

         Transfer the probe and impinger assembly to the cleanup area. This  area must
         be clean, and enclosed so that the chances of contaminating the sample will be
         minimized.

         No smoking is allowed.

         Inspect the train prior to and during disassembly and note any abnormal
         conditions, broken filters, color  of the impinger liquid, etc.  Figure 6 summarizes
         the recovery procedure described in Sections 5.3.1 to 5.3.8.

         Figure 11 is an example of a form for recording the performance of the sample
         recovery procedure. The tester must record all of the routine information
         indicated on this form as well as any additional data which are necessary for
         documenting the quality of any  reported results.
August 9, 1996                                             Proposed M-429 Page 32

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 5.3.1        Sample Container No. 1 {front half rinses]

             Quantitatively recover material deposited in the nozzle, probe, the front half
             of the filter holder, and the cyclone, if used, first by brushing and then by
             sequentially rinsing with acetone, hexane, and methylene chloride three times
             each. Place all these rinses in Container No. 1. Mark the liquid level.

 5.3.2        Cyclone Catch

             If the optional cyclone is used, quantitatively recover the particulate matter
             by sequentially rinsing the cyclone with acetone, hexane, and methylene
             chloride.  Store in a clean sample container and cap,

 5.3.3        Sample Container No. 2 (filter)

             Carefully remove the filter from  the fitter holder and place it in its identified
             container. Use a pair of precleaned tweezers to handle the filter.  Do not
             wrap the filter in aluminum foil.  If it is necessary to fold  the filter, make sure
             that  the particulate cake is inside the fold.  Carefully transfer to the container
             any particulate matter and/or  filter fibers which adhere to the filter holder
             gasket by using a dry inert bristle brush and/or a sharp-edged blade.  Seal the
             container.

 5.3.4        Sorbent Module

             Remove the sorbent module from the train  and cap it.

 5,3.5        Sample Container No. 3 (back half rinses)

             Rinse the back half of the filter holder, the  transfer line between the filter and
             the condenser, and the condenser (if using the separate condenser-sorbent
             trap) three times each with acetone, hexane and methylene chloride, and
             collect all rinses in Container Mo. 3.  If using the combined condenser/sorbent
             trap, the rinse of the condenser  shall be performed in the laboratory after
             removal of the XAD-2 portion. If the optional water knockout trap has been
             employed, the contents and rinses shall be placed in Container No. 3. Rinse
             it three times each with acetone, hexane, and methylene chloride. Mark the
             liquid level.

             The back half rinses may also be combined in a single container with the
             front half rinses (Section 5.3,1).

 5.3.6        Sample Container No. 4 (Impinger contents)

             Wipe off the outside of each of the first three impingers to remove excess
             water and other material. Weigh the impingers and contents to the nearest
             ±0.5 g using a balance. Record the weight, Calculate and then record the
             weight  of liquid collected during sampling.  Use this weight and the weight of
             liquid collected in the silica gel (Section 5.3.8) to calculate the moisture
             content of the effluent gas (Sections 4.5.5 and 4.5.6). Pour the impinger
             catch directly into Container No, 4. Mark the liquid level.
Augusts, 1996                                             Proposed M-429  Page 33

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                                                                                          I
5.3.7       Sample Container No. 5 (Impinger rinses)
            Rinse each impinger sequentially three times with acetone, hexane, and           '
            methytene chloride and pour rinses into Container No. 5. Mark the liquid             •
            level. These rinses may be combined with the previously weighed impinger          I
            contents in Container No. 4.

5.3.8       Weighing Silica Gel                                                              I

            Weigh the spent silica gel to the nearest 0.5 g using a balance.  Record the
            weight.  Calculate and then record the weight of liquid collected during              I
            sampling. Use this weight and the weight of liquid collected in the impingers         "
            (Section 5.3.6} to calculate the moisture content of the  effluent gas
            (Sections 4.5.5 and 4.5.6). .                                                     j

5.4      SAMPLE PRESERVATION AND HANDLING

         From the time of collection to extraction, maintain all samples (Sections 5.3.1  to
         5.3.7) at 4°C or lower and protect from light.  All samples must be extracted as
         soon as practically feasible, but within 21  days of collection; and all extracts
         must be analyzed as soon as practically feasible, but within  40 days of
         extraction.  Success in meeting the holding time requirement will depend on pre-
         test planning by the tester and the laboratory.

6        ANALYTICAL PREPARATION

         This method is restricted to use only by or under the supervision of analysts
         experienced in the use of capillary column gas chromatography/mass
         spectrometry and skilled in the  interpretation of mass spectra.  Each analyst
         must demonstrate the ability to generate acceptable results  with this method
         using the procedures described in Sections 7.3, 8.2.6, and 8.3.1.

6.1      SAFETY

         The toxicity or carcinogenicity of each reagent used in this method has not been
         precisely defined.  Nevertheless, each chemical compound should be treated as a
         potential health  hazard and exposure to these chemicals must be reduced to the
         lowest possible  level  by whatever means available.  The laboratory is responsible
         for maintaining a current file of OSHA regulations regarding  the safe handling of
         the chemicals specified in this method.  A reference file of material data handling
         sheets should also be made available to all personnel involved in the chemical
         analysis.  Reference 11.9 describes procedures for handling  hazardous chemicals
         in laboratories.

         The following method analytes  have been classified as known or suspected
         human or mammalian carcinogens:  benzo(a)anthracene and dibenzo-
         (a,h,(anthracene. A guideline for the safe handling of carcinogens can be found
         in Section 5209 of Title 8 of the California Administrative Code.
August 9, 1996                                             Proposed M-429 Page 34

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6.2      CLEANING OF LABORATORY GLASSWARE

         Glassware used in the analytical procedures (including the Soxhlet apparatus and
         disposable bottles) must be cleaned as soon as possible after use by rinsing with
         the last solvent used in it. This must be followed by detergent washing with hot
         water, and rinses with tap water, deionized water, acetone, hexane, and
         methylene chloride.  Other cleaning procedures may be used as long as
         acceptable blanks are obtained.  Acceptance criteria for blanks are given in
         Section 8.2.

         Clean aluminum foil with acetone followed by hexane and methylene chloride.

6.3      APPARATUS

6.3.1        Grab Sample Bottle

             Amber glass, 125-mL and 250-mL, fitted with screw caps lined with Teflon.
             The bottle and cap liner must be acid washed and solvent rinsed with
             acetone and methylene chloride, and dried before use.

6.3.2        Concentrator Tube, Kuderna-Danish

             10-mL, graduated (Kontes-K-570050-1025 or equivalent).  Calibration must
             be checked at the volumes employed in the test.  A ground glass stopper
             must be used to prevent evaporation of extracts.

6.3.3        Evaporation Flask, Kuderna-Danish

             500-mL (Kontes K-570001-Q500 or equivalent). (Attached to concentrator
             tube with springs).

6.3.4        Snyder Column, Kuderna-Danish

             Three-ball macro (Kontes K-569001-0121  or equivalent).

6.3.5        Snyder Column, Kuderna-Danish

             Two-ball micro (Kontes K-569001-0219 or equivalent).

6.3.6        Mini vials

             1.0 mL vials; cone-shaped to facilitate removal of very small samples; heavy
             wall borosilicate glass; with Teflon-faced rubber septa and screw caps.

6.3.7        Soxhlet Apparatus

             1 liter receiver, 1 heating mantle, condenser, Soxhlet extractor.

6.3.8        Rotary Evaporator

             Rotovap R (or equivalent), Brinkmann Instruments, Westbury, NY.


August 9, 1996                                            Proposed M-429  Page 35

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6.3.9       Nitrogen Slowdown Apparatus

            N-Evap Analytical Evaporator Model 111 (or equivalent), Organomation
            Associates Inc., Northborough, MA.

6.3.10      Analytical Balance

            Analytical. Capable of accurately weighing to the nearest 0.0001 g.

6.3.11      Disposable Pipet

            5 3/4 inch x 7.0 mm  OD.,

6.4      SAMPLE PREPARATION REAGENTS

6.4.1       Reagent water

            Same as 5.2.1.

6.4.2       Acetone

            Same as 5.2.2.

6.4.3       Hexane

            Same as 5.2.3.

6.4.4       Methylene Chloride

            Same as 5.2.4.

6.4.5       Sulfuric Acid

            ACS. Reagent grade. Concentrated, sp. gr. 1.84.

6.4.6       Sodium Sulfate

            ACS. Reagent grade. Granular, anhydrous. Purify prior to use by extracting
            with methylene chloride and oven drying for 4 or more hours in a shallow
            tray. Place the cleaned material in a glass container with a Teflon lined screw
            cap, and store in a desiccator.

6.4.7       Silica Gel

            For column chromatography, type 60, EM reagent, 100-200 mesh, or
            equivalent. Soxhlet extract with methylene chloride, and activate by heating
            in a foil covered glass container for longer than 16 hours at 130 °C, then
            store in a desiccator.  The storage period shall not exceed two days.

            NOTE:  The performance of silica geJ in the column cleanup procedure varies
            with manufacturers and with the method of storage. The analyst shall
            establish a procedure that satisfies the performance criteria of Section 6.6.1.

Augusta, 1996                                            Proposed M-429 Page 36

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6.4.8       Alumina: Acidic

            Soxhlet extract with methylene chloride, and activate in a foil covered glass
            container for 24 hours at 190 °C.

            NOTE:  The performance of alumina in the column cleanup procedure varies
            with manufacturers and with the method of storage.  The analyst shail
            establish a procedure that meets the performance criteria of Section 6.6.1.

6.4,9       Nitrogen

            Obtained from bleed from liquid nitrogen tank.

6.5      SAMPLE EXTRACTION

         WARNING: Stack sampling will yield both liquid and solid samples for PAH
         analysis. Samples must not be split prior to extraction even when they appear
         homogeneous as in the case of single liquid  phase samples.  Solid samples such
         as the resin are not homogeneous and particulate matter may not be uniformly
         distributed on the filter. In addition, filter samples are generally so small that the
         desired detection limit might not be achieved if the sample were split.

         The recovered samples may be combined as follows:

         1) Particulate filter and particulate matter collected on the filter (Section 5.3.3),
            cyclone catch (Section 5.3.2) and sample container No. 1 (Section 5.3.1).

         2) Sample container No. 3 (Section 5.3.5), resin (Section 5.3.4) and rinse of
            resin cartridge.

         3) Sample container No.4 (Section 5.3.6) and sample container No.5 {Section
            5.3.7)

         Two schemes for sample preparation are described in Sections 6.5.1 and 6.5.2
         below. One of these must be used.

         Section  6.5.1 describes sample preparation  procedures for separate GC/MS
         analyses of impingers and the remainder of the sampling train. Figure 7 is a
         flowchart of the extraction and cleanup procedures.

         Section  6.5.2 describes sample preparation  procedures for GC/MS analysis of a
         single composite extract from each sampling train. The recovered samples are
         combined as shown in Figure 8.

6.5.1       Separate Analysis of Impingers

            A separate analysis of the impingers can be used to determine whether there
            has been breakthrough  of PAHs past the resin.
August 9, 1996                                             Proposed M-429  Page 37

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6.5.1.1           Extraction of Liquid Samples

                 A.  Sample Container No. 1 (Front half rinses}

                    Concentrate the contents of sample container No. 1 (Section 5.3.1)
                    to a volume of about 1-5 ml using the nitrogen blowdown
                    apparatus. Rinse the sample container three times with small
                    amounts of methylene chloride and add these rinses to the
                    concentrated solution. Concentrate further to about 1-5 ml. This
                    residue will likely contain particulate matter which was removed in
                    the rinses of the probe and nozzle. Transfer the residue {along  with
                    three rinses of the final sample vessel) to the Soxhlet apparatus with
                    the filter and particulate catch and proceed as described under
                    Section 6.5.1.2 below.

                 B.  Sample Container No. 3 (Back half rinses}

                    Concentrate the contents of sample container No. 3 (Section 5.3.5)
                    to a volume of about 1-5 ml using the nitrogen blowdown
                    apparatus. Rinse the sample container three times with small
                    amounts of methylene chloride and add these rinses to the
                    concentrated solution. Concentrate further to about 1 -5 mL.
                    Combine this residue (along with three rinses of the final"sample
                    vessel) in the Soxhlet apparatus with the resin sample, and proceed
                    as described under Section 6.5.1.2 below.

                 C.  Containers No.  4 and No. 5 (Impinger contents and rinses)

                    Place the contents of Sample Containers No. 4 and No. 5 (Sections
                    5.4.6 and 5.4.7) in a separatory funnel. Add the appropriate
                    amount of 2H-labelled alternate standard solution (Section 7 and
                    Table 7 or 7A) to achieve the final extract concentrations indicated
                    in Table 8 or 8A.  The amounts required by Section 7.2.4 are based
                    on a final volume  of 500 fjL for analysis (450 fjl of sample extract
                    and 50 /A. of recovery standard solution).  Extract the  sample three
                    times with 60 ml aliquots of methylene chloride.  Combine the
                    organic fractions. Divide the extract in two - one half  to be
                    archived, and the other for cleanup and GC/MS  analysis.  Store the
                    archive sample  at 4°C away from light.

                    Pour the remaining extract through Na2SO4 into a round bottom
                    flask.  Add 60 to  100 ml hexane and evaporate to about 10 ml.
                    Repeat three times or less if the methylene chloride can be removed
                    with less hexane. Add the appropriate amount of alternate standard
                    (Section 7.2.7)  to achieve the final extract concentrations shown in
                    Table 6 or 6A.  This standard must be used to monitor the efficiency
                    of the  cleanup procedure.

                    Concentrate the remaining sample to 2 ml with a Kuderna-Danish
                    concentrator or rotary evaporator, then transfer the extract to a 8-
                    mL test tube with hexane.  Proceed with sample cleanup procedures
                    below  (Section  6.6).

August 9, 1996                                             Proposed M-429  Page 38

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6,5.1.2     '     Extraction of Solid Samples

                     Filter, Particulate matter, and .Resin
                    The Soxhlet apparatus must be large enough to allow extraction of
                    the sample in a single batch.  Clean the Soxhlet apparatus by a 4 to
                    8-hr Soxhlet with methylene chloride at a cycling rate of 3 cycles
                    per hour.  Discard the solvent. Add 20 g Na2S04to the thimble.
                    Combine the filter, resin, glass wool, and concentrated front and
                    back half rinses (6,5.1.1 A and 6.5.1.1B) and place on top of the
                    Na2SO4. Add the appropriate amount of internal  standard (Section
                    7.2.4 and Table 7) to achieve the final extract concentrations
                    indicated in Table 8.

                    Place the thimble in the Soxhlet apparatus, and add about 700 ml
                    of methylene chloride to the receiver.  Assemble the Soxhlet, turn
                    on the heating controls and cooling water, and allow to reflux for 16
                    hours at a rate of 3 cycles per hour. After extraction, allow  the
                    Soxhlet to cool.  Divide the sample in two - one half to be archived,
                    and the other for cleanup and  GC/MS analysis.  Store the archive
                    sample at 4°C away from light.
                    Exchange the remaining extract to hexane. Add 60 to 100 mL
                    hexane and evaporate to about 10 mL.  Repeat three times or as
                    necessary to remove the methylene chloride. Add the appropriate
                    amount of alternate standard (Section 7.2.7 and Table 7 or 7A) to
                    achieve the final extract concentrations shown in Table 8 or 8A.
                    This alternate standard must be used to monitor the efficiency of
                    the cleanup procedure when the impingers are analyzed separately
                    from the remainder of the sampling train.

                    Concentrate the remaining sample to about 2 ml with a Kuderna-
                    Danish concentrator or rotoevaporator, then transfer the extract to a
                    8-mL test tube  with hexane. Proceed with sample cleanup
                    procedures below (Section 6.6).

6.5.2       Single Composite Extract For Analysis

6.5.2.1          Extraction of Aqueous Samples

                    Containers No.  4 and No. 5 (Impinger contents and rinses)

                    Pour the contents of Sample Containers No. 4 and No. 5 (Sections
                    5.3.6 and 5.3.7) into an appropriate  size separatory funnel. Do  not
                    add internal standards. Instead, add the appropriate amount of
                    alternate standard spiking solution (Section 7 and Table 7 or 7A) to
                    achieve the final extract concentrations indicated in Table 8 or 8A,

                    Extract the sample three times with 60 ml aliquots of methylene
                    chloride.  Combine the organic fractions with the solid samples and
                    concentrated rinses (6.5.2.2) in a Soxhlet extractor.

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6.5.2.2         Extraction of Solid Samples

                Concentrate the front and back half rinses as described in Sections
                6.5.1.1A and 6.5.1.1B. Clean the Soxhlet apparatus as in Section
                6.5.1.2. Place the filter and resin in the Soxhlet apparatus along with
                the concentrated front and back half rinses and the imptnger extract.
                Add the internal standards, extract the sample, and concentrate the
                extract as described in Section 6.5.1.2.  Divide the extract into two
                equal portions.  Store one of these, the archive sample, at 4 °C away
                from light.  The remaining extract must be exchanged to hexane as
                described in Section 6.5.1.2. Do not add the alternate standard to this
                composite extract. It has already been added to the impinger sample
                (6.5.2.1).

                Concentrate the extract to 2 mL with a Kuderna-Danish concentrator or
                rotary evaporator, then transfer to a 8-mL test tube with hexane or
                equivalent non-polar solvent  such as isooctane.  Proceed with sample
                cleanup procedures below (Section 6.6)

6.6      COLUMN CLEANUP

         Several column chromatographic cleanup options are available. Either of the two
         described below may be sufficient. Before using a procedure for the cleanup of
         sample extracts, the analyst must demonstrate that the requirements of Sections
         8.1.3.1 and 8.2.6 can be met using the cleanup procedure. Acceptable
         alternative cleanup  procedures may also be used provided that the analyst can
         demonstrate that the performance requirements of Sections 8.1.3.1 and 8.2.6
         can be met.  Compliance with the requirements of Sections 8.1.1.1  and 8.2.6
         must also be demonstrated whenever there is a change in the column cleanup
         procedure used for the initial demonstration.

         The sample extract obtained as described in Sections 6.5.1C and  6.5.1.2 or
         6.5.2.2 is concentrated to a volume of about 1 mL using the nitrogen blowdown
         apparatus, and this is transferred quantitatively with hexane rinsings to at least
         one of the columns described below.

6.6.1        Column Preparation

            A.  Silica Gel Column

                Pack a glass gravity column (250 mm x 10 mm) in the following
                manner;

                Insert a clean glass wool plug (Section 4.2.7) into the bottom of the
                column and add 10 grams of activated silica gel (Section 6.4.7) in
                methylene chloride. Tap the column to settle the silica gel, and then add
                a 1 cm layer of anhydrous sodium sulfate (Section 6.4.6)

                Variations among batches of silica gel may affect the elution volume of
                the various PAH.  Therefore, the volume of solvent required to
                completely elute all of the PAH must be verified by the analyst. The
                weight of the silica gel can then be adjusted accordingly.  Satisfactory

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                 recovery (as defined in Section 6.6) of each native PAH in the LCS
                 (8.1.3) must be demonstrated whenever there is a change in the method
                 of preparing the silica gel columns.

             B.   Acid Alumina Column

                 Pack a 250 mm x 10 mm glass gravity column as follows:

                 Insert a clean glass wool plug (Section 4.2.7) into the bottom of the
                 column. Add 6 g of acid alumina prepared as described in
                 Section 6.4.8. Tap the column gently to settle the alumina, and add 1
                 cm of anhydrous sodium suifate to the top.

                 Satisfactory recovery (as defined in Section 6.6} of each native  PAH in
                 the LCS (8.1.3) must be demonstrated whenever there is a change in
                 the method of preparing the acid alumina columns.

6.6.2    Column Chromatography Procedure

             A.   Silica Gel Column

                 Elute the column with 40 mL of hexane.  The rate for all elutions should
                 be about 2 mL/min,  Discard the eluate and Just prior to exposure of the
                 sodium suifate layer to the air, transfer the 1 ml sample extract onto the
                 column using  two additional 2 ml rinses of hexane to complete  the
                 transfer. Just prior to exposure of the sodium suifate layer to the air,
                 begin elution of the column with 25 mL of hexane followed by 25 mL of
                 methylene chloride/hexane (2:3)(v/v).  Collect the entire eluate.
                 Concentrate the collected fraction to about 5 mL using the  K-D
                 apparatus or a rotary evaporator. Do not allow the extract to  go to
                 dryness.

                 Transfer to a minivial using a hexane rinse and concentrate to 450//L
                 using a gentle stream of nitrogen. Store the extracts in a refrigerator at
                 4 °C or lower away from light until  GC/MS analysis (Section 7).

             B.   Alumina Column

                 Elute the column with 50 mL of hexane.  Let the solvent flow  through
                 the column until the head of the liquid in the column is just above the
                 sodium suifate layer. Close the stopcock to stop solvent flow.

                 Transfer 1 mL of the sample extract onto the column. Rinse out extract
                 vial with two  1 mL rinses of hexane and add it to the top of the  column
                 immediately.  To avoid overloading  the column, it is suggested that no
                 more than 300 mg of extractable organics be placed on the column.

                 Just prior to exposure of the sodium suifate to the air, elute the  column
                 with a total of 15 mL of hexane.  If the extract is in 1 mL of hexane,
                 and if 2 mL of hexane was used as a rinse, then  12 mL of additional
                 hexane should be used.  Collect the effluent and concentrate to  about 2
                 mL using the K-D apparatus or a rotary evaporator.

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                Transfer to a minivial using a hexane rinse and concentrate to 450 //L
                using a gentle stream of nitrogen.  Store the extracts at 4°C or lower
                away from light until GC/MS analysis.

7        GC/MS ANALYSIS

7.1      APPARATUS

7.1.1       Gas Chromatograph

            An  analytical system complete with a temperature programmable gas
            Chromatograph and all required accessories including syringes, analytical
            columns, and gases. The GC injection port must be designed for capillary
            columns.  Splitless injection is recommended.

7.1.2       Column

            Fused silica columns are required.

            A.  30 M long x 0.32 mm ID fused silica capillary column coated with a
                crossMnked phenyl methyl silicone such as DB-5.

            B.  Any column equivalent to the DB-5 column may be used as long as it
                has the same separation capabilities as the DB-5.

7.1.3       Mass Spectrometer

7.1.3.1          Low Resolution

                A  low resolution mass spectrometer (LRMS) equipped with a 70 eV
                (nominal) ion source operated in the electron impact  ionrzation mode,
                and capable of monitoring all of the ions in each Selected Ion Monitoring
                (SIM) group (Table 13)  with a total cycle time of 1 second or less.

7.1.3.2          High Resolution

                The high resolution mass spectrometer (HRMS) must be capable of
                operation in the SIM mode at a resolving power of 8,000. Electron
                impact ionization must be used. The mass spectrometer must  be
                capable of monitoring all of the ions listed in each of the three SIM
                descriptors (Table 14} with a total cycle time of 1 second or less.

7.1.4       GC/MS Interface

            Any gas Chromatograph to mass spectrometer interface may be used as long
            as it gives acceptable calibration response  for each analyte of interest at the
            desired concentration and achieves the  required tuning performance criteria
            (Sections 7.3.5 and  7.3.6). AH components of the interface must be glass
            or glass-lined materials. To achieve maximum sensitivity, the exit end of the
            capillary column should be placed in the mass spectrometer ion source
            without being exposed to the ionizing electron beam.
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 7.1.5        Data Acquisition System

             A computer system must be interfaced to the mass spectrometer.  The
             system must allow the continuous acquisition and storage on machine-
             readable media of all data obtained throughout the duration of the
             chromatographic program. The computer must have software that can
             search any GC/MS data file for ions of a specific mass and plot a Selected
             Ion Current Profile or SICP (a  plot of the abundances of the selected ions
             versus time or scan number).  Software must also be able to integrate, in any
             SICP, the abundance between specified time or scan-number limits.

             The data system must provide hard copies of individual ion chromatograms
             for selected gas chromatographic time intervals.

             The data system must also be able to provide hard copies of a summary
             report of the results of the GC/MS runs. Figures 14A to 14C show the
             minimum data that the system must be available to provide.

 7.2      REAGENTS

 7.2.1        Stock Standard Solution (1 .00 fjgtfJl)

             Standard solutions can be prepared from pure standard materials or
             purchased as  certified solutions.

 7.2.2        Preparation of Stock Solutions

             A.  Calibration standards. Prepare stock calibration standard solutions of
                 each of the PAH analytes by accurately weighing the required amount of
                 pure material. Dissolve the material in isooctane and dilute to volume.
                 When compound purity is assayed  to be 96% or greater, the weight may
                 be used without correction to calculate the concentration of the stock
                 standard.

                 Commercially prepared stock standards may be used at any
                 concentration if they  are certified by the manufacturer or by an
                 independent source.

             B=   Internal standards.  Prepare stock solutions in isooctane of the fourteen
                 internal standards listed in Table 4 or 4A at concentrations of 1000
             C.   Recovery standards.  Prepare stock solutions in isooctane of the three
                 recovery standards listed in Table 4 or 4A at concentrations of
                 1000 ng/^L.

             D.   Alternate standard.  Prepare a stock solution in isooctane of the
                 alternate standard listed in Table 4 or 4A at a concentration of
                 1000 ng/^L.
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             E.   Surrogate standards. Prepare stock solutions in isooctane of the
                 surrogate standards listed in Table 4 or 4A at a concentration of
                 1000 ng//;L,

             Store stock standard solutions in Teflon*-sealed screw-cap bottles at 4°C and
             protect from light. Stock standard solutions must be checked frequently for
             signs of degradation or evaporation, especially just before using them to
             prepare calibration standard solutions or spiking solutions.
                                                        V
             Replace stock standard solutions every 12 months or more frequently if
             comparison with quality control check samples according to Section 7.4.1
             indicates  a problem.

7.2.3        Calibration Standards

             Prepare calibration standards at a minimum of five concentration levels. One
             of the calibration standards should be at a concentration near, but above, the
             method detection limit.  The others should include the range of
             concentrations found in real samples but should not exceed the linear range
             of the GC/MS system.

             Prepare calibration working standard solutions by combining appropriate
             volumes of individual or mixed calibration standards with internal standard,
             recovery standards, and alternate standard spiking solution and making up to
             volume with hexane to obtain the solution concentrations given in Tables 5,
             6, and 6A.  The suggested ranges are 0.25 ng/x/L to 5.0 ng/x/L for LRMS and
             10 pg///L  to 500 pg/fjl for HRMS.

             All standards must be stored at 4°C or lower and must be freshly prepared if
             the check according to Section 7.4.1 indicates a  problem.

7.2.4        Internal Standard (IS) Spiking Solution

             The concentration of internal standard in the IS spiking solution must be such
             that the amount of solution added to the calibration standard solution and the
             sample is  at least 2 ml.

             Prepare the internal standard spiking solution by using appropriate volumes of
             stock solutions of Section 7.2.2B to give the concentrations shown in
             Table 4 or 4A. A volume of 2 mL of either the LRMS or HRMS spiking
             solution will provide the amount of  the internal standards that must be
             added to the sample (Table 7 or 7A) before extraction to achieve, in a final
             volume of 500 pi, the sample extract concentrations shown in Table 8 for
             LRMS and Table 8 or 8A for HRMS analysis. The target concentrations in
             Tables 8 and 8A are based on a final volume of 500//L and 100 percent
             recovery of the internal standards added to the sample.

7.2.5        Recovery  Standard Spiking Solution

             The concentration of recovery standard in this spiking solution must be such
             that the amount of solution added to the concentrated sample extract is
             50  //L to give a final extract volume  of  500 pL,

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             Use an appropriate volume of stock solution of Section 7.2.2C to prepare a
             recovery standard spiking solution with the concentrations shown in
             Table 4or 4A. Store at 4 °C or lower,

             A volume of 50 fjL of the recovery standard spiking solution shown in
             Table 4 or 4A will provide the amount of each recovery standard required by
             Table 7 or 7A to achieve the target sample concentration of Table 8 or 8A.
             Final volumes, may be adjusted depending on the target detection limit.

 7.2.6        Surrogate Standard Spiking Solution

             The concentration of surrogate standard in this spiking solution must be such
             that the amount of solution added to the calibration standard solution and the
             sorbent module is at least 2 mL.

             Prepare the surrogate standard spiking solution by using the appropriate
             volume of stock solution  of Section 7.2.2E to give the concentration shown
             in Table 4 or 4A. A volume of 2 ml of either the LRMS or HRMS spiking
             solution will provide the amount of the surrogate standards that must be
             added to the sample (Table 7 or 7A) before sampling to achieve the sample
             extract concentrations shown in Table 8 or 8A in a final sample volume of
             500 fjL.

 7.2.7        Alternate Standard Spiking Solution

             The concentration of alternate standard in this spiking solution must be such
             that the amount of solution added to the calibration standard solution and the
             sample extracts is at least 2 ml.

             Prepare the alternate standard spiking solution by using the appropriate
             volume of stock  solution  of Section 7.2.2D to give the concentration shown
             in Table 4 or 4A. A volume of 2 mL of either the LRMS or HRMS spiking
             solution will provide the amount  of the alternate standard that must be
             added to the sample (Table 7 or 7A) before extraction to achieve the sample
             extract concentrations shown in Table 8 or 8A in a final sample volume of
             500 //L.

 7.2.8        Calibration Check Standard

             The calibration check standard shall be used for column performance checks,
             and  for continuing calibration checks. Solution #3 from Table 5 shall be the
             calibration check standard for LRMS, while Solution #3 from Table 6 or 6A
             shall be the calibration check standard for HRMS.

 7.3      INITIAL CALIBRATION

         An acceptable initial calibration (7.3.8) is required before any samples are
         analyzed, and then intermittently throughout sample analyses as dictated by
         results of the continuing calibration  procedures described in Section 7.4. The
         GC/MS system must be properly calibrated  and the performance documented
         during the initial calibration.
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7.3.1       Retention Time Windows
             Before sample analysis, determine the retention time windows during which
             the selected ions will be monitored. Determine Relative Retention Time
             (RRTs) for each analyte by using the corresponding 2H - labelled standard.

7.3.2        GC Operating Conditions

             The GC column performance (Section 7.3.5) must be documented during the
             initial calibration.  Table 10 summarizes GC operating conditions known to
             produce acceptable results with the column listed.  The GC conditions must
             be established by each analyst for the particular instrumentation by injecting
             aliquots of the calibration check standard (7.2.8). It may be necessary to
             adjust the operating conditions slightly based on observations from analysis
             of these solutions. Other columns and/or conditions may be used as long as
             column performance criteria of Section 7.3.5 are satisfied.

             Thereafter the calibration check standard must be analyzed daily to verify the
             performance of the system (Section 7.4).

7.3.3        GC/MS Tuning Criteria

             A.  Low Resolution Mass Spectrometry

                Use a compound such perfluorotributylamine (PFTBA) to verify that the
                intensity of the peaks is acceptable. If PFTBA is used, mass spectral
                peak profiles for m/z 69, 219 and 264 must be recorded, plotted, and
                reported.  The scan should include a minimum  of +/- two peaks (i.e, m/z
                67-71 for the m/z 69 profile).

             8.  High Resolution Mass Spectrometry

                Tune the instrument to meet the minimum required resolving power of
                8,000 at 192.9888 or any other PFK reference signal close to 128.0626
                (naphthalene). Use peak matching and the chosen PFK reference peak
                to verify that the exact mass of m/z 242.9856 is within 5 ppm of the
                required value. The selection of the low and high mass ions must be
                such that they provide the largest voltage jump performed in any of the
                three mass descriptors.

7.3.4        MS Operating Conditions

             A,  Low Resolution Mass Spectrometry

                Analyze standards and samples with the mass spectrometer operating in
                the Selected Ion  Monitoring (SIM) mode with a total cycle time of 1
                second or less.
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             B.   High Resolution Mass Spectrometry

                 Analyze standards and samples with the mass spectrometer operating in
                 the SIM mode with a total cycle time (including the voltage reset time)
                 of one second or  less.

                 A reference compound such as Perftuorokerosene (PFK) must be used to
                 calibrate the SIM  mass range.  One PFK ion per mass descriptor is used
                 as a lock-mass ion to correct for mass drifts that occur during the
                 analysis.  In addition to the lock-mass ion, several ions characteristic of
                 PFK are monitored as QC check ions (Table 13).

 7.3.5        GC Column  Performance Criteria

             A.   The height of the  valley between anthracene and phenanthrene at m/z
                 178 or  the 2H-analogs at m/z 188 shall not exceed 50 percent of the
                 taller of the two peaks.

             B.   The height of the  valley between benzo{b)fluoranthene and
                 benzo(k)fluoranthene shall not  exceed 60 percent of the taller of the two
                 peaks.

             If these criteria are not met and normal column maintenance procedures are
             not successful, the column must be replaced and the initial calibration
             repeated.

 7.3.6        Mass Spectrometer Performance

             A.   Low Resolution Mass Spectrometry

                 Verify acceptable sensitivity during initial calibration.  Demonstrate that
                 the instrument will achieve a minimum signal-to-noise ratio of 10:1 for
                 the quantitation and confirmation ions when the calibration standard
                 with the lowest concentration is injected into the GC/MS system.

             B.   High Resolution Mass Spectrometry

                 Record  the peak profile of the high mass reference signal (m/z
                 242.9856) obtained during peak matching by using the low-mass PFK
                 ion at m/z 192.9888 (or lower  in mass) as a reference.  The minimum
                 resolving power of 8.000 must be demonstrated on the high-mass ion
                 while it is transmitted at a lower accelerating voltage than the low-mass
                 reference ion, which is transmitted at full sensitivity.

                 The format of the peak profile representation must allow manual
                 determination of the resolution, that is, the  horizontal axis must be a
                 calibrated mass scale (amu or ppm per division).

                 The peak width of the high mass ion at  5 percent of the peak height
                 must not exceed 125 ppm in mass.
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7.3.7        Calibration Procedure

             Using stock standards, prepare at least five calibration standard solutions,
             using the same solvent that was used in the final sample extract.  Keep the
             recovery standards and the internal standards at fixed concentrations. Adjust
             the concentrations recommended in Tables 5 and 6, if necessary, to ensure
             that the sample analyte concentration fails within the calibration range. The
             calibration curve must be described within the linear range of the method.
             Calibrate the mass spectrometer response using a 2 pL aliquot of each
             calibration solution. Analyze each solution once.

             Calculate:

             A.  the relative response factors (RRFs) for each analyte as described in
                 Sections 7.7.1.1, 7.7.1.2, and 7.7.1.3.

             B.  the mean RRFs as required by Section 7.7.1.4,

             C.  the standard deviation (SO) and relative standard deviation (RSO) as
                 required by Section 7.7.2.

             Report all results as required by Section 10.2,

7.3.8        Criteria for Acceptable Initial Calibration

             An acceptable initial calibration must satisfy the following performance
             criteria:

             A.  The requirements of Sections 7.3.5 and 7.4.6  must be met.

             B.  The signal to noise ratio (S/N) for the GC signals present in every
                 selected ion current profile (SICP) must be > 10:1  for the labelled
                 standards and unlabelled analytes.

             C.  The percent relative standard deviation for the mean relative response
                 factors must be no greater than 30 percent for both the unlabelled
                 analytes and internal standards (Section 7.7.2). Otherwise, take
                 corrective action as required by Section 7.7.2.

7.4      CONTINUING CALIBRATION

         The continuing calibration consists of an analysis of the calibration check
         standard (Section 7.2.8) once during each 12-hour shift as described in Section
         7.4.1.

         The criteria for acceptable continuing calibration are given in Section 7.4.2.
         These must be satisfied or else corrective action must be taken as required by
         Section 7.4.2.
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 7.4.1        Calibration Check

             The calibration check standard (Section 7,2.8) must be analyzed at the
             beginning and end of each analysis period, or at the beginning of every 12-
             hour shift if the laboratory operates during consecutive 12 hour  shifts.

             Inject a 2-fjL aliquot of the calibration check standard (Section 7.2-8} into the
             GC/MS. Use the same data acquisition parameters as those used during the
             initial calibration.

             Check the retention time windows for each of the compounds.  They must
             satisfy the criterion of Section 7.4.2C

             Check for GC resolution and peak shape. Document acceptable column
             performance as described in Section 7.3.5.  If these criteria are  not met, and
             normal column maintenance procedures are unsuccessful, the column must
             be replaced and the calibration repeated.

             Calculate the continuing RRF and ARRF, the relative percent difference (RPD)
             between the daily RRF and the initial calibration mean  RRF as described in
             Section 7.7.1.5.

             Report the results as required by Section 10.2.

 7.4.2        Continuing Calibration Performance Criteria

             An acceptable continuing  calibration  must satisfy the following performance
             criteria:

             A.  The signal to noise ratio (S/N) for the GC signals present in  the selected
                 ion current profile (SICP) for all labelled and unlabelled standards must
                 be> 10:1.

             B.  The measured RRFs of all analytes (labelled and unlabelled)  must be
                 within 30 percent of the mean values established  during the initial
                 calibration. If this criterion is not satisfied, a new initial calibration curve
                 must be established before sample extracts can be analyzed.

             C.  The retention time for any internal standard must not change by more
                 than 30 seconds from the most recent calibration check.  Otherwise,
                 inspect the chromatographic system for malfunctions and make the
                 necessary corrections.  Document acceptable performance with a new
                 initial calibration curve,

7.5      GC/MS ANALYSIS

         The laboratory may  proceed with the analysis of samples and blanks only after
         demonstrating acceptable performance as specified in Sections 7.3 and 7.4.

         Analyze standards, field samples and QA samples (Section 8.1) with the gas
         chrornatograph and  mass spectrometer operating under the conditions
         recommended in Sections 7.3.2 and 7.3.4.

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         Approximately I hr before HRGC/LRMS or HRGC/HRMS analysis, adjust the
         sample extract volume to approximately 500 /L/L. This is done by adding 50 ji/L of
         the recovery standard spike solution (Section 7.2.5, and Table 4 or 4A) to the
         450 ;/L final volume (Section 6.6.2) of the concentrated sample extract give the
         sample extract concentration required by Table 8 or 8A. If the sample volume
         must be changed to achieve a desired detection limit, the recovery spike solution
         concentration must be adjusted accordingly to achieve the target concentrations
         of Table 8 or 8A.

         Inject a 2 //L aliquot of the sample extract (Section 6.6.2) on to the DB-5
         column. Use the same volume as that used during catibration.  Recommended
         GC/MS operating conditions are described in Section 7.3.

         The presence of a given  PAH is qualitatively confirmed if the criteria of Section
         7.6.1  are satisfied.

         The response for any quantitation or confirmation ion in the sample extract must
         not exceed the response of the highest concentration calibration standard.

         Collect, record, and store the data for the calculations required by Sections
         9.1.7, 9.1.8, 9.1.9, and 9.1.10.  Report the results as required by Section 10.2.

7.6      QUALITATIVE ANALYSIS

7.6.1        Identification Criteria

7.6.1.1          Ion Criteria

                 For LRMS analysis, all quantitation and confirmation ions (Table  13)
                 must be present.

7.6.1.2          Relative Retention Time (RRT) Criteria,

                The relative retention time (RRT) of the analyte compared to the RRT for
                 the 2H-standards must be within ±0.008 RRT units of the relative
                 retention times obtained from the continuing calibration (or initial
                calibration if this applies).

7.6.1.3         Signal to Noise Ratio

                The signal to mean noise ratio must be 10:1 for the internal standards.
                This ratio for the unlabelled compounds must be greater than 2.5 to 1
                for the quantitation ions for HRMS and for both quantitation and
                confirmation ions for LRMS,

                If broad background interference restricts the sensitivity of the GC/MS
                analysis, the analyst must employ additional cleanup on the archive
                sample and reanalyze.
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 7.7      QUANTITATIVE ANALYSIS

 7.7.1        Relative Response Factors (RRFs)

 7.7.1,1          RRF for Unlabelled PAH and Surrogate Standards
                 from Initial Calibration Data

                 Use the results of the calibration and Equation 429-13 to calculate the
                 relative response factors (RRFs) for each calibration compound and
                 surrogate standard in each calibration solution (Tables 5  or 5A).  Table
                 11  shows the assignments  of the internal standards for calculation of
                 the RRFs for the calibration solution shown in Table 5. Table 11A
                 shows the assignments of the internal standards for calculation of the
                 RRFs for the calibration solution shown in Table 5A.  Report the  results
                 as required by Section  10.2.

 7,7.1.2          RRF for Determining  Internal Standard Recovery

                 Use the results of the calibration in Equation 429-18 to calculate the
                 relative response factor for  each internal standard relative to an
                 appropriate recovery standard. Table 11 shows the assignments of the
                 recovery standards for calculating internal standard recoveries for the
                 calibration solution shown in Table 5.  Table 11A shows the
                 assignments of the recovery standards for calculating internal standard
                 recoveries for the calibration solution shown in Table  5A. Report the
                 results as required by Section 10.2.

 7.7.1.3          RRF for Determining Alternate Standard Recovery

                 Use the calibration results and Equation 429-19  to calculate the
                 response factor for the alternate standard relative to the  appropriate
                 recovery standard. Table 11 shows the assignment of the recovery
                 standards for calculating alternate standard recovery for the calibration
                 solution shown in Table 5.  for the calibration solution shown in Table 5.
                 Report the results as required by Section 10.2,

 7.7.1.4          Mean Relative Response Factor

                 Use Equation 429-20 to calculate the mean RRF for each compound
                 (unlabelled calibration standards, surrogate standards, internal standards
                 and alternate standard). This is the average of the five RRFs calculated
                 for each compound (one RRF calculated for each calibration solution).
                 The mean RRF may be used if the linearity criterion  of Section  7.7.2 is
                 satisfied.
                 Report  the results as required by Section 10.2.

 7.7.1.5          RRF from Continuing  Calibration Data

                 Analyze one or more calibration standards (one must be the medium
                 level standard) on each work shift of 12 hours or less. Use Equations
                 429-17, 429-18, and 429-19 to calculate the RRFs for each analyte.
                 Use Equation 429-22 to calculate ARRF, the relative percent difference

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                 between the daily RRF and the mean RRF calculated during initial
                 calibration. Check whether the performance criterion of Section 7.4,2B
                 is satisfied.  Report the results as required by Section 10.2.

7.7.2       Relative Standard Deviation of Relative Response Factors

            For each analyte, calculate the sample standard deviation (SO) of the RRFs
            used to calculate the mean RRF.  Use Equation 429-21 to calculate the
            percent relative standard deviation (%RSD) for each analyte. The analyst
            may use the mean RRF if the percent relative standard deviation  of the RRFs
            is 30% or less. If the RSD requirement is not satisfied, analyze additional
            aliquots of appropriate calibration solutions to obtain an acceptable RSO of
            RRFs over the entire concentration range, or take action to improve GC/MS
            performance.  Otherwise, use the complete five point calibration  curve for
            that compound.

8        QUALITY ASSURANCE/QUALITY CONTROL

         Each laboratory that uses this method is required to operate a formal quality
         control program.  The minimum quality control requirements of this program
         consists of an initial demonstration of laboratory capability (according to
         Sections 7.3 and 8.1.3.1),  and periodic analysis of blanks and spiked samples as
         required in Sections 8.1.1 and 8.1.3.2 as a continuing check on performance.

         The laboratory must maintain performance records to document the quality of
         data that are generated.  The results of the data quality checks must be
         compared  with the method performance criteria to determine if the analytical
         results meet the performance requirements of the method. The laboratory must
         generate accuracy statements as described in Section 8.4.1.

8.1      QA SAMPLES

8.1.1       Laboratory Method Blank

            The analyst must run a  laboratory method blank with each set  of 15 or fewer
            samples. The method blank must be a resin sample from the same batch
            used to prepare the sampling cartridge and the laboratory control samples.
            The method blank must be prepared and stored as described in
            Sections 4.3.4 and 4.3.5.

            The analyst shall perform all of the same procedures on the method blank as
            are performed on the solid samples (Section 6.5.2.1) from the  beginning of
            sample extraction through to the end of the GC/MS analytical procedures.

8.1.2       Performance Evaluation Samples

            The laboratory should analyze performance evaluation samples quarterly
            when these samples become available. These samples must be prepared and
            analyzed by the same methods used for the field samples.  Performance for
            the most recent quarter should be reported with the results of the sample
            analysis.
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 8.1.3        Laboratory Control Sample ILCS)

 8.1.3.1          Initial Demonstration of Laboratory Capability

                 Before performing sample analyses for the first time, the analyst shall
                 demonstrate the ability to generate results of acceptable precision and
                 accuracy by using the following procedures.

                 Prepare spiking solutions from stock standards prepared independently
                 from those used for calibration. Spike at least four resin samples
                 cleaned as described in Section 4.2.2 with each of the target unlabelled
                 analytes as indicated in Table 9. Blank resin contamination levels must
                 be no greater than 10 percent of the levels of  the spiked analytes.  Add
                 the amounts of internal standards required by  Table 7 or 7A.  Add the
                 alternate standard to the extract to monitor the efficiency of the cleanup
                 procedure.

                 The LCS spikes shall undergo all of the same procedures as are
                 performed on the solid samples (Section 6.5.1.2) from the beginning  of
                 sample extraction through to the end of the  GC/MS analytical
                 procedures.

                 Calculate:

                 (A) percent recoveries for the internal  standards and alternate standard,
                 (B)  the mass of each target analyte in //g/sample or ng/sample,
                 (C) the average of the results for the four analyses inpg/sample or
                     ng/sample,
                 (D) the average recovery (R) as a percentage of the amount added, and
                 (E)  the relative standard deviation SR.
                 Report the results as required by Section 10.2.4.

                 If all the acceptance criteria of Section 8.2.6 are satisfied for all of the
                 target PAH, the analyst may begin analysis of  blanks and samples.
                 Otherwise, corrective action must be taken as required by Section 8.2.6,
8.1.3.2          Ongoing Analysis of LCS

                 The analyst must run two laboratory control samples with each set of
                 15 or fewer samples.  The resin for the LCS must be taken from the
                 same batch used to prepare the sampling cartridge and the laboratory
                 method blank.  The LCS resin must be prepared and stored as described
                 in Sections 4.3.4 and 4.3.5,

                 Prepare spiking solutions from stock standards prepared independently
                 from those used for calibration.  Spike each resin sample with each of
                 the target unlabelled analytes as indicated in Table 9.  Blank resin
                 contamination levels must be no greater than 10 percent of the levels of
                 the spiked analytes. Add the amounts of internal standards required by
                 Table 7 or 7A. Add the alternate standard to the extract to monitor the
                 efficiency of the  cleanup procedure.

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                 The LCS spikes shall undergo all of the same procedures as are
                 performed on the solid samples (Section 6.5.1.2) from the beginning of
                 sample extraction through to the end of the GC/MS analytical
                 procedures.

             Calculate:  •  •     •••  . •            ••         • ••        ;.•:•••-

             (A)  percent recoveries for the internal standards and alternate standard,
             (B)  the mass of each target analyte in pg/sample or ng/sample,
             (C)  the average of the results for the two analyses in pg/sample or
                 ng/sample,
             (D)  the average recovery as a percentage of the amount added, and
             (E)  the relative percent difference for the two analyses.

             Report the results as required by Section 10.2,

             Add the results which satisfy the performance requirements of Section 8,2,6
             to the results of the initial LCS analyses (8.1.3.1) and previous ongoing data
             for each compound in the LCS sample.

             Update the charts as described in Section 8.4.1.

8.2      ACCEPTANCE CRITERIA

8.2.1        Blank Trains

             The levels  of any unlabelled analyte quantified in  the blank train must not
             exceed 20 percent of the level of that analyte in the sampling train. If this
             criterion cannot be met, calculate a reporting limit that is  five times the
             blank value (Equations 429-32 and 429-33). Do  not subtract the blank value
             from the sample value.

8.2.2        Surrogate Standard Recovery

             Acceptable surrogate (field spike) recoveries should range from 50 to  150
             percent. If field spike recoveries are not within the acceptable range, this,
             must be clearly indicated in the laboratory report. The affected sampling run
             must be identified in the report of the calculated emissions data.

8.2.3        Internal Standard Recovery

             Recoveries for each of the internal standards must be greater than 50
             percent and less than 150 percent of the known value.

             If internal standard recoveries are outside of the acceptable limits,  the signal
             to noise ratio of the internal standard must  be greater than 10.  Otherwise
             the analytical procedure must be repeated on the stored portion of the
             extract.

             NOTE;  This criterion is used to  assess method performance.  As this is an
                    isotope dilution technique, it is, when properly applied, independent
                    of internal  standard recovery.  Lower recoveries do not necessarily

August 9, 1996                                             Proposed M-429  Page 54

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                     invalidate the analytical results for PAH, but they may result in
                     higher detection limits than are desired.

             If low internal standard recoveries result in detection limits that are
             unacceptable, the cleanup and GC/MS analysis must be repeated with the
             stored portion of the extract. If the analysis of the archive sample gives low
             recoveries and high detection limits, the results of both analyses must be
             reported.

 8.2.4       Laboratory Method Blank

             The laboratory method blank must not contain any of the  target analytes
             listed in Table 1  at levels exceeding the PQL or 5 percent  of the analyte
             concentration in the field sample.

             If the method blank is contaminated, check solvents, reagents, standard
             solutions apparatus and glassware to locate and eliminate the source of
             contamination before any more samples are analyzed. Table 3 shows those
             compounds that commonly occur as contaminants in the method  blank, and
             the ranges of concentrations that have been reported.

             If field samples were processed with a laboratory method  blank that showed
             PAH levels greater than 5 percent of the field sample, they must be re-
             analyzed using the archived  portion of the sample  extract.

             Recoveries of the internal standards must satisfy the requirements of 8.2.3.
             If the internal standard recoveries are less than 50%, the  S/N ratio must be
             greater than 10 for the internal  standard.

 8.2.5       Performance Evaluation Sample

             The following will be a requirement when performance evaluation samples
             become available, and performance criteria have been established:

             Performance for the most recent quarter must be reported with the results of
             the sample analysis. If the performance criteria (to be established) are not
             achieved, corrective action must be taken and acceptable  performance
             demonstrated before sample analysis can be resumed.

 8.2.6        Laboratory Control Samples

 8.2.6.1      Initial and Ongoing Analysis

             The signal of each anatyte in the initial and ongoing laboratory control
             samples must be  at least 10 times that of the background.

             Acceptable accuracy is a percent recovery between 50 and 150 percent.
             Acceptable precision for the  initial LCS samples is  a relative standard
             deviation (RSD) of 30 percent or less.
             Acceptable precision for the  ongoing analysis of  duplicate  samples is a
             relative percent difference of 50 percent or less.
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             If the RSD for the initial demonstration exceeds the precision limit, or any
             calculated recovery falls outside the range for accuracy, the laboratory
             performance for that analyte is unacceptable.
             If the RPD for any ongoing duplicate analyses exceeds the precision limit, or
             any calculated recovery falls outside the range for accuracy, the laboratory
             performance for that analyte is unacceptable.

             Beginning with Section 8.1.3.1, repeat the test for those analytes that failed
             to meet the performance criteria.  Repeated  failure, however, will  confirm a
             general problem with the measurement system.  If this occurs, locate and
             correct the source of the problem  and repeat the test for all compounds of
             interest beginning with Section 8.1.3.1  for the initial analysis and
             Section 8,3.1.2 for  the ongoing analysis.

8.3      ESTIMATION OF THE METHOD DETECTION LIMIT IMDL) AND PRACTICAL
         QUANTITATION LIMIT  (PQL)

8.3.1    Initial Estimate of MDL  and PQL

         The analyst shall prepare a batch of XAD-2 resin as described in Sections
         4.2.2.1 to 4.2.2.3, then check for contamination as required by Section 4.2.2.4.
         Identify those PAH analytes present at background levels that are too high for
         the MDL determination.  Use the procedure of Appendix A to calculate MDLs for
         the remaining target PAH compounds. A suggested initial spike level for the
         MDL determination is 5 times a theoretical method quantitation limit (TMQL)
         estimated according to  Equation 429*16.


                          TMQL  =CxXx100x2                  429-16
                                          P

         Where:

         C   =  the concentration of the PAH in the lowest concentration calibration
                standard used in the initial calibration, (ng/^uL)

         V   ss  the final extract volume, U/L)

         P   =  the assumed percent recovery (50%) of the internal standard

         2   =  a factor to account for the fact that the final extract volume  (V) contains
                one half of the  analyte in the  sample. The other half is archived.

8.3.2    Ongoing Estimation of MDL and PQL

         Once every quarter in which this method is used, the analytical laboratory must
         analyze one spiked resin sample as described in  Appendix A. Include all initial
         and quarterly results in the calculation of the standard deviation and MDL for
         each analyte that has not been identified as a common contaminant of the
         XAD-2  resin.
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         If the MDL for any analyte exceeds the MDL established during the initial
         determination, take corrective action as necessary, and repeat the monthly
         analysis. If any MDL still exceeds the  initial MDL, then the initial standard
         deviation estimation procedure (Appendix A) must be repeated.

 8.4      LABORATORY PERFORMANCE

         The analyst must have documented standard operating procedures (SOPs) that
         contain specific stepwise instructions for carrying out this method.  The SOPs
         must be readily available and followed  by all personnel conducting the work.  The
         SOP must be made available for review upon request by the Executive Officer,
         the tester or reviewer of the analytical results. The analyst may impose
         restrictions on the dissemination of the information in the SOP.

         The analyst must have documented precision and accuracy statements
         (Section 8.4.1} readily available.

         The analyst must have results of the initial and ongoing estimates of the  MDL
         (Sections 8.3.1 and 8,3.2} readily available.

 8.4.1    Precision and Accuracy Statement

         The precision and accuracy statements for the analytical procedure shall, be
         based on the results of the initial and ongoing LCS analyses.  The frequency of
         analysis is stated in Section 8.1,3.

         Prepare a table of the recoveries and the relative percent difference for each
         ongoing analysis  of the LCS and LCS duplicate. Figure  15A is an example of
         such a table.  This must be included in the analytical data package submitted for
         each set of sample analyses.

         Prepare a quality control chart for each target analyte that provides  a  graphic
         representation of continued laboratory  performance for that target analyte.
         Figure 15B is an example  QC chart for benzo(a)pyrene.

 9.       CALCULATIONS

         Carry out calculations retaining at least one extra decimal figure beyond that of
         the acquired data.  Round off figures after the final calculation.

 9.1      ANALYST'S CALCULATIONS

         The analyst shall  carry out the calculations described in Sections 9.1.1 to
         9.1.11.
August 9, 1996                                             Proposed M-429 Page 57

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9,1.1    Relative Response Factors (RRFJ for Unlabelled PAH and Surrogate Standards

         Calculate the RRF for each target unlabelled PAH analyte and surrogate standard
         in each calibration solution .  Use Equation 429-17 and the data obtained during
         initial calibration (7.3.7) or continuing calibration (7,4.1).


                                RRF    '-A                             29-17
                                         Ais  x  Qs
            Where:
            As  =  Area of the response for characteristic ions of the unlabelled analyte
                   or surrogate standard (Tables 11 or 11 A, 13, and 14).

            Ais  =  Area of the response for characteristic tons of the appropriate internal
                   standard (Tables 11 or 11 A, 13, and 14).

            Qs  =  Amount of the unlabeiled PAH calibration analyte or surrogate
                   standard injected on to GC column, ng.

            Qis  =  Amount of the appropriate internal standard injected on to GC column, ng.

9.1.2    RRF for Determination of Internal Standard Recovery

         Calculate RRFjs according to Equation 429-18, using data obtained from the
         analysis of the calibration standards.

                                D D c    —.    is    ^^rs
                                nnrjc  -  —	——
                                         Ars x Qis

            Where:

            Ars  =  Area of the response for characteristic ions of the appropriate
                   recovery standard (Tables 11 or 11 A, 13, and 14).

            Qrs  =  Amount of the appropriate  recovery standard  injected on to GC
                   column, ng.

9.1.3    RRF for Determination of Alternate Standard Recovery

         Calculate RRFas according to Equation 429-19, using data obtained from the
         analysis of the calibration standards.

                                BRp     .  Aas  x  Qrs              429-19
                                RRFaS  -  _	   Q
                                         *Vs x  uas

            Where;

            Aas  =  Area of the response for characteristic ions of the alternate standard
                   (Tables 13 and 14).

            Qas  =  Amount of alternate standard injected on to the GC column, ng.

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 9.1.4    Mean Relative Response Factors (RRF)

         Calculate the mean RRF for each target unlabelled PAH, surrogate standard,
         internal standard and alternate standard using Equation 429-20 and the RRFs
         calculated according to Sections 9.1.1, 9.1.2, and 9.1.3.


                               RRF  = 1  V (RRF)i
                                        n  jtf
            Where:
                    =  RRF calculated for calibration solution "i" using one of Equations
                       429-17, 429-18 or 429-1 9.

              n     =  The number of data points derived from the calibration. The
                       minimum requirement is a five-point calibration (Section 7.2.3,
                       Tables 5 and 6 or 6A)

9.1,5    Percent Relative Standard Deviation (%RSD) of Relative Response Factors

         Use Equation 429-21 to calculate the relative standard deviation of the Relative
         Response Factors for each analyte.

                             %RSD  - -SD  x  100%
                                        RRF

         Where:
         RRF  =   Mean relative response factor of a given analyte as defined in
                   Sections 7.7.1.4 and 9.1.4.

         SD   =   The sample standard deviation of the relative response factors used
                   to calculate the mean RRF.

9.1.6    Continuing Calibration ARRF

         Use Equation 429-22 to calculate ARRF, the  relative percent difference (RPD)
         between the daily RRF and the mean RRF calculated during initial calibration.


                                  RRF,.  - RRF                     429-22
                         ARRF  -     c	_  x  100%
                                       RRF
         Where:

         RRFC   =  The RRF of a given anaiyte obtained from the continuing calibration
                   (Section 7,4).
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9.1.7    Percent Recovery of Internal Standard, Rls

         Calculate the percent recovery, RIS for each internal standard in the sample
         extract, using Equation 429-23.

                             'A*  *  °-       x  100%            429'23
                              Ars x
         Where:
          RRF-IS =  Mean relative response factor for internal standard (Equations 429-18
                   and 429-20).
9.1.8    Percent Recovery of Surrogate Standard, R
                                               3S
         Calculate the percent recovery, Rss for each surrogate standard in the sample
         extract, using Equation 429-24.
                       Rss  =        "             x  100%
                              AIS  x RHF; x  Q^
         Where:
         Ass    =  Area of the response for characteristic ions of the surrogate standard
                   (Tables 13 and 14).

         Qss    =  Amount of the surrogate standard added to resin cartridge before
                   sampling, ng,

          RRFS  BS  Mean relative response factor for surrogate standard (Equations
                   429-1 7 and 429-20).

9.1 .9    Percent Recovery of Alternate Standard, R^

         Calculate the percent recovery, Ras for the alternate standard in the sample
         extract, using Equation 429-25.
                       as
                                                   x  100%
         Where:

          RRTas =  Mean relative response factor for alternate standard (Equations 429-
                   19 and 429-20).
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 9.1.10  Mass of the Target Analytes and Surrogate Standards in
         Emissions Sample or Blank Train

            Use Equation 429-26 to determine the total mass of each PAH compound or
            surrogate standard in the sample:

            Report the PQL (9.1.11) for those analytes that were not present at levels
            higher than the PQL provided to the tester prior to testing (2.3,3).

                                 M  -   °is  x  As                  429'26
                                       AJS x  RHF

         Where:

         M      =  Mass (ng) of surrogate standard (Ms) or target analyte (Mt) detected
                    in the sample.

         Qis     =  Amount of internal standard or surrogate standard added to each
                    sample.

         As      —  Area of the response for characteristic ions of the unlabelled analyte
                    or surrogate standard (Tables 13 and 14).

         Ais     =  Area of the response for characteristic ions of the appropriate
                    internal standard (Tables 13, and 14).
         RRF    =  Mean relative response factor of a given analyte calculated as
                    required by Sections 7.7.1.4 and 9.1.4.

9.1 .1 1   Analytical Reporting Limit

            The analyst shall report the PQL (Section 2.3.3) for those analytes that were
            not present in the emissions sample or blank train at levels higher than the
            pre-test estimate of the PQL.

9.2      TESTER'S CALCULATIONS

9.2.1    Sample/Blank Train PAH Mass Ratio

         Use Equation 429-27 to calculate the sample/blank train mass ratio for each PAH
         detected at levels above the MOL in both the field sample and the blank train.

                                  RATiO
                                            MBT

         Where:

         Mt      =  Mass of target PAH analyte detected in the sampling train
                    (Equation 429-26).

         MBT    =  Mass of the same PAH analyte detected in the blank train.


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         If the sample to blank train PAH mass ratio is less than five, calculate the
         reporting limit for the tested source as required by Section 9,2.4,2.  Do not
         calculate Mc (Section 9.2.2) or Me (Section 9.2.3) for the emissions report.

9.2.2    PAH Concentration in Emissions

         Use Equation 429-28 to calculate the concentration in the emissions of  1) the
         PAH analytes detected in the sampling train but not in the blank train, and 2J the
         PAH analytes that satisfy the minimum sample to blank train mass ratio required
         by Section 9.2.1.
9.2.3
                                    Mt
                                        1
                                                          429-28
                                  Vm(std)     0.028317
         Where:


         Mc



         Mt

         Vm(std)
          =   Concentration of PAH in the gas, ng/dscm, corrected to standard
              conditions of 20°C, 760 mm Hg (68°F, 29.92 in. Hg) on dry
              basis.

          =   Mass of PAH compound in gas sample, ng {Equation 429-26)

          =   Volume of gas sample measured by the dry gas meter, corrected
              to standard conditions, dscf (Equation 429*10)
0.028317 =   Factor for converting dscf to dscm.

PAH Mass Emission Rate

Use Equation 429-29 to calculate the mass emission rate for each PAH
compound that satisfies the minimum sample/blank train PAH mass ratio
(Section 9.2.1).
                                      M.
                                                       429-29
                                               "60-
         Where:
          Jstd
         60
        —  Mass emission rate for PAH analyte, ng/second

        =  Mass of PAH compound in the gas sample, ng (Equation 429-26)

        =  Average stack gas dry volumetric flow rate corrected to standard
            conditions, dscf/min.

        =  Factor for converting minutes to seconds
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                                                 Proposed M-429  Page 62

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 9.2,4    Source Reporting Limit

 9.2.4.1  PAH Not Detected in Either Sampling or Blank Train

         Use Equation 429-30 or 429-31 to calculate the reporting limit for those anaiytes
         that were not detected at levels above the PQL in sither the sampling or blank
         train.
                           RL
                                     PQL
                            1
                                               429-30
                             cs
                                   V
                                     mlstd)
                        0.028317
         Where:
                             RL
                                es
                 PQL       Qstd
                           "60"
                                                                     429-31
                                      vm{std)
                    =  Reporting limit for the tested source, {ng/dscm), corrected to
                       standard conditions of 20°C, 760 mm Hg (68°F, 29-92 in.  Hg) on
                       dry basis,

                    =  Reporting limit for the tested source, (ng/sec.).

         0.028317  -  Factor for converting  dscf to dscm.
         60         =  Factor for converting minutes to seconds.

9.2.4.2  PAH Detected in Blank Train and Sample/Blank Train Ratio < 5

         If the sample to blank train PAH mass ratio is less than five, then Equation
         429-32 or 429-33 shall be used to calculate the reporting limit for that PAH.
         Where:
         RL
           cb
         RL
           eb
         M
           BT
                                   5 X MDT
                          RLcb  «       OT  X
                                   vm«std)
                                  _  5 x MBT
                                  -
                             1
                        0.028317
                                              429-32
                                             429-33
                                      V
                                       mfstd)
                           "60"
Reporting limit for the tested source, (ng/dscm), corrected to
standard conditions of 20°C, 760 mm Hg (68°F, 29-92 in. Hg) on
dry basis.

Reporting limit for the tested source, {ng/sec.).

The total mass of that PAH analyte in the field blank train.
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                                    Proposed M-429  Page 63

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10.      REPORTING REQUIREMENTS

         The source test protocol must contain all the sampling and analytical data
         required by Sections 2.2 to 2.5, 4.2.1.1, and 4.2.2.4, as well as the information
         listed in Sections  10.T and  10.2 that pertain to identification and quantitation of
         the samples.

         The emissions test report must contain all of the sampling and analytical data
         necessary to calculate emissions values for the target analytes or to demonstrate
         satisfactory performance of the method.

         The end user or reviewer should be able to obtain from the source test report all
         information necessary to  recalculate all reported test method results or to verify
         that all required procedures were performed.

         Any deviations from the procedures described in this method must be
         documented in the analytical and sampling report.

10.1     SOURCE TEST PROTOCOL

         At a minimum, the source test protocol must include all of the data  required by
         Section 2.2 and the information listed in Sections 10.1.1 through 10.1.4.

10.1.1      Preparation of Filters

            A.  Manufacturer's lot number for  the batch  of filters to  be used in the test.

            B.  Contamination check of filter {Section 4.2.1.1)

                 (i)  Date of cleaning.
                 (ii) Date of PAH analysis.
                 (iii) Table of results of PAH analysis required by Section 4.2.1. The
                    analytical report must include all of the data listed in Section 10.2.

            C.       Storage conditions prior to the test  (4.3.3)

10.1.2      Preparation of XAD-2 resin

            A.   ID for the batch to  be used in the test.  The same batch must be used
                for the sampling train and the laboratory QC samples.

            B.   Contamination check of resin (Sections 4.2.2.1 to 4.2.2.4)

                (i)  Date of cleaning.
                (ii)  Date of PAH analysis.
                (iii) Table  of results of PAH analysis required by Secton 4.2.2.4. The
                    analytical report must include all of  the data listed in Section 10.2.

            C.   Addition of surrogate standards to the resin cartridge.

                (i)  Amount of each compound.
                (ii)  Date of spiking.

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            D.   Storage conditions prior to the test (Section 4.3,3)

 10.1.3      Method Detection Limits and Practical Quantitation Limits

            The MDL and PQL for each target analyte determined as required by Sections
            2,3.2 and 2.3.3.

 10,1.4      Target Sampling Parameters

            A.   Source target concentration of each emitted PAH of interest.

            B.   Results of calculations required by Sections 2.5.2 to 2.5.5.

            Figure 9 shows the minimum required calculations of target sampling
            parameters.

 10.2    LABORATORY REPORT

         The  analyst  must generate a  laboratory report for each pre-test analysis of the
         sampling media (Sections 2.3, 4.2.2.1, and 4.2.2.4) and each post-test analysis
         of the sampling trains and laboratory QC samples.

         A minimum  of 7 post-test analyses are required to determine the emissions from
         the source and to document the quality of the emissions data.  These are the
         analyses of three sampling runs, one blank train, one laboratory method blank
         and two laboratory control samples.

         At a minimum, any report (data package) from the analyst to the tester shall
         contain the information listed in Sections 10.2.1 to 10.2.6 pertaining to
         identification and PAH quantitation of all samples.

 10.2.1       Five-point Initial Calibration

             The report of the results of the initial five-point calibration must include the
             data listed in A, B, and C below:

             A,   Mass chromatograms for each initial calibration solution that show at a
                 minimum:

             (i)   Instrument ID,
             (ii)   laboratory sample ID on each chromatogram.
             (iii)  date and time of GC/MS analysis,
             (iv)  mass of monitored ions for each compound in the calibration solution -
                 unlabelled PAH, internal standard, surrogate standard, alternate
                 standard and recovery standard,
             (v)   retention time for each compound in the calibration solution, and
             (vi)  either  peak height or area of the signals observed for the monitored ion
                 masses.
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             B.   A summary table of the data obtained for each initial calibration
                  solution that shows at a minimum:

             (i)   Instrument ID,
             (it)   laboratory sample ID.
             (iii)  date and time of GC/MS analysis,
             (iv)  retention time for each compound - unlabelled PAH, internal standard,
                  surrogate standard, alternate standard and recovery standard,
             (v)   relative retention time for each unlabelled PAH,
             (vi)  either peak height or area of the signals observed for the monitored ion
                  masses,
             (vii)  the relative response factors for each unlabelled PAH, internal standard,
                  surrogate standard, and alternate standard, and
             (viii) analyst's signature

             Figure 14A is an example of a summary table that contains the minimum
             required information for  the analysis of a single calibration solution.

             C.   A summary table that shows at a minimum:

             (i)   Instrument ID,
             (ii)   the date  and time of the GC/MS analysis,
             (iii)  the relative response factor (RRF) calculated for each unlabelled PAH,
                  internal standard, surrogate standard, and alternate standard in each
                  calibration solution,                	
             (iv)  the average relative response factor (RRF] calculated for the five point
                  calibration,
             (v)   the relative standard deviation of the relative response factors, and
             (vi)  the recovery of each internal standard in percent.

             Figure 14B is an example of a report that contains the minimum required
             information for a five point calibration summary.
10.2.2       Continuing Calibration
             The report of the results of a continuing calibration must include the data
             listed in 10.2.2 A, B, and C below:

             A,   Mass chromatogram that shows at a minimum the information listed in
                  10.2.1 A.

             B.   A summary table of the raw data obtained for the continuing calibration
                  that shows at a minimum, the information listed in 10.2.1 B.

             C.    A summary table that shows at a minimum:

             (i)   the relative response  factor (RRF) for each unlabelled PAH, internal
                  standard, surrogate standard, and  alternate standard in the continuing
                  calibration solution,                 	
             (ii)   the average relative response factor (RRF) for each compound
                  calculated for the five point calibration.
August 9, 1996                                             Proposed M-429  Page 66

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             (iii)  ARRF for each unlabelled PAH, internal standard, surrogate standard,
                  and alternate standard in the continuing calibration solution,
             (iv)  the recovery of each internal standard in percent.

             Figure 14C is an example of a summary report that contains the minimum
             information required by Section 10.2.2C for the analysis of the continuing
             calibration solution.

 10,2.3      Laboratory Method Blank

             The laboratory report of the results of the analysis of the method blank must
             include at a minimum the data listed in  10.2.3 A, B, and C below:

             A.   Mass chromatograms that show at a minimum the information listed in
                  10.2.1 A.

             B.   A summary table of the data obtained for each method blank that
                  shows at a minimum, the information listed in 10,2.5 B.

             C.   A summary table that reports the same data as listed in 10.2.5 C
                  below.

 10.2.4      Laboratory Control Samples

             The report of the results of the analysis of the LCS samples must include at
             a minimum the data listed in  10.2.4 A,  B, and C below:

             A.   Mass chromatograms that show at a minimum the information listed in
                  10.2.1 A.

             B.   A summary table of the raw data for each sample that shows at a
                  minimum, the information listed in 10.2.1 B, and in addition:

             (i)   Client's sample ID
             (ii)   mass of each analyte,
             (iii)  the recovery of each internal standard, and alternate standard,

             Figure 16A is an example of a summary table that contains the minimum
             information required by 10.2.4 B.

             C.   A summary table that reports for the two LCS analyses:

             (i)   client's sample ID,
             {ii}   sample matrix description,
             (iii)   date of cleaning  of the XAD-2 resin,
             (iv)  lot number for the resin  (resin for all field samples and QA samples
                  must come from the same lot),
             (v)   date of extraction of LCS samples,

             Figure 15A is an example of a summary table that contains the minimum
             information required by 10.2.4 C.
August 9, 1996                                            Proposed M-429  Page 67

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10.2.5       Emissions Samples
             The report of the results of the analyses of the three sampling trains and the
             blabk train must include the data listed in 10,2.5 A, B, and C below:

             A.   Mass chromatograms that show at a minimum the information listed in
                  10.2.1  A, and in addition,

             (i) client's sample ID

             B.   A summary table of the data for the analysis of each sample that
                  shows at a minimum, the information listed in 10.2.1  B, and in
                  addition,

             (i)   client's sample ID
             (ii)   Date of five point initial calibration (ICAL)
             (iii)   ICAL ID,
             (iv)   mass of each analyte,
             (v)   the recovery of each internal standard, alternate standard and surrogate
                  standards in percent.

             Figure 16A is an example of a summary table that contains the minimum
             information required by 10.2.5 B.

             C.   A summary table that reports:

             (i)   client's sample ID (from a chain of custody record submitted by the
                  tester),
             (ii)   sample  matrix description,
             (iii)   date of cleaning of the XAD-2 resin,
             (iv)   lot number for the resin (resin for all field samples and QA samples
                  must come from the same lot),
             (ii)   date of submittal  of the tester's samples
             (v)   date of extraction of samples,
             (vi)   Initial calibration Run ID,
             (vii)   Continuing calibration ID

             Figure 16B is an example of a summary table  that contains the minimum
             information required by 10.2.5C.
10.2.6       Data Flags

             The laboratory report must include an explanation of any qualifiers that are
             used to indicate specific qualities of the data.

10.3     EMISSIONS TEST REPORT

         The emissions test report should include narrative that describes how the test
         was done. The tester's report must also include all the appropriate sections used
         in a report from a Method 5 test such as a description of the plant process,
         sampling port locations, control equipment, fuel being used, genera! plant load
August9, 1996                                             Proposed M-429  Page 68

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          conditions during the test {description of plant production equipment problems,
          etc.), and anything else necessary to characterize the condition being tested.

          The tester's report must also include all of the information listed in Sections
          10.3.1  to 10.3.4.

 10.3.1       Tester's Summary of Analytical Results

              The tester must summarize the results of the minimum seven analyses
              required for each source test. At a minimum, the summary must contain the
              information listed in Figure 17A including all data flags,

              The tester must obtain the detailed analytical results (Section 10.2) from the
              laboratory and include them in the appendices as required below.

 10.3.2       Reid Data Summary

              The report from the tester to the end user must contain a field data
              summary. This summary must include at a minimum a table of the results of
              the calculations required by Section 4.5. as well as the values which were
              used to calculate the reported results.  Figure 17B is an example of a field
              data summary that contains the minimum required information.

 10.3.3       PAH Emissions Results

              Figure 17C show the calculations of the concentrations and mass emission
              rates of the target PAH. The reviewer should be able to use the data in
              Figures 17A and 17B to check the calculations in Figure 17C. The reviewer
              should also be able to check the appendix to the report to determine the
              accuracy and the quality of the data summarized by the tester in Figures
              17A and 17B.

 10.3.4       Appendix to the Emissions Test Report

              At a minimum, the following raw data or signed copies must be included in
              an appendix to the emissions test report.

              A.   Record of data for sample site selection and minimum number of
                  traverse points.

              B.    Moisture determination for isokinetic settings.

              C.    Velocity traverse data.

              D.    Gas analysis for determination of molecular weight.

              E.    Calibration records.

              F.    Method 429 sampling run sheets,

             G,    PAH  laboratory reports listed in Section 10.2
August9, 1996                                            Proposed M-429  Page 69

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         The information listed above is to be considered as the minimum that should be
         included to characterize a given operating condition.  The end user or the
         executive officer may require  additional information for any given project,

11.      BIBLIOGRAPHY

11,1       U.S. Environmental Protection Agency/Office of Water Engineering and
           Analysis Division (4303), Washington D.C., Method 1613. Tetra-through
           Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS.
           EPA821-B-94-005. (1994).

11.2       U.S. Environmental Protection Agency/Office of Solid Waste, Washington
           D.C., Method 3611 A.  Alumina Column Cleanup and Separation of Petroleum
           Wastes.  In "Test Methods for Evaluating Solid Waste-Physical/Chemical
           Methods" SW-846 (1986).

11.3       U.S. Environmental Protection Agency/Office of Solid Waste, Washington
           D.C., Method 3630B.  Silica Gel Cleanup. In "Test Methods for Evaluating
           Solid Waste-Physical/Chemica! Methods" SW-846 (1986).

11.4       Thomason, J.R., ed.. Cleaning of Laboratory Glassware. Section 3, A, pp 1-7
           in "Analysis of Pesticide Residues in Human and Environmental Samples",
           Environmental Protection Agency, Research Triangle Park, N.C. (1974).

11.5       ARB Method 428. Determination of Polychlorinated Dibenzo-p-dioxin (PCDD)
           and Polychlorinated Dibenzofuran (PCDF) Emissions From Stationary Sources.
           September,  1990.

11.6       U. S. Environmental Protection Agency, Method 1625 Revision B -
           Semivolatile Organic Compounds by Isotope Dilution. 40 CFR Ch.1 (7-1-95
           Edition) Pt. 136, App. A.

11.7       Rom, Jerome J., Maintenance, Calibration, and Operation of Isokinetic Source
           Sampling Equipment. Environmental Protection Agency. Research Triangle
           Park, NC.  APTD-0576. March, 1972.

1-1.8       Shigehara, R.T., Adjustments in the EPA Nomograph for Different Pilot Tube
           Coefficients and Dry Molecular Weights. Stack Sampling News, 2: 4-11.
           October,  1974
                                                                 (•
11.9       "Prudent Practices in the Laboratory.  Handling and Disposal of Chemicals,"
           National Academy Press. Washington D.C. 1995.
August 9, 1996                                           Proposed M-429 Page 70

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                                     TABLE 1
                         METHOD 429 TARGET ANALYTES
                                 Naphthalene
                                 2-Methylnaphthalene
                                 Acenaphthene
                                 Acenaphthyiene
                                 Fluorene
                                 Phenanthrene
                                 Anthracene
                                 Fluoranthene
                                 Pyrene
                                 Benzo(a)anthracene
                                 Chrysene
                                 Benzo(b}fluoranthene
                                 Benzo(k)f!uoranthene
                                 Benzole) pyrene
                                 Benzo(a)pyrene
                                 Perylene
                                 Indenod ,2,3-cd)pyrene
                                 Dibenz(a,h}anthracene
                                 Benzo(ghi)perylene
August9.  1996                                           Proposed M-429 Page 71

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                                TABLE 2




              PRACTICAL QUANTITATION LIMITS FOR TARGET PAHs
Naphthalene
2-Methylnaphthalene
Acenaphthene
Acenaphthytene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(e)pyrene
Benzo(a)pyrene
Perylene
Indenod ,2,3-cd)pyrene
Dibenz(a,h)anthracene
Benzo(ghi)perylene
LRMS
(//g/sample)
1. HO
244
1.25
0.210
0.104
0.207
0.85
0.146
0.346
0.191
0.167
0.272
1.119
0.738
0.146
0.191
0.143
0.798
0.465
0.305
HRMS
(ng/sample)
480
66
5.0
5.0
16.5
22
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
370
19
5.0
5.0
5.5
14
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
August 9, 1996
Proposed M-429  Page 72

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                                                 TABLE 3




                       PAH ANALYSIS BY HRMS OF DIFFERENT LOTS OF CLEANED RESIN
PAH ANALYTES
Naphthalene
2-Methylnaphthalene
Acenaphlhylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluorantherie
Pyrene
Benzo (a| anthracene
Chrysene
Benzol bHIuoranthene
Benzo(k)fluoranthene
Ben7o(e)pyrene
Benzo(a)pyrene
Perylene
CONCENTRATION (ng/sample)

A1
480
65
< 5.0
< 5.0
16.5
22
< 5.0
< 5.0
< 5.0
< 5.0
< 5,0
< 5.0
< 5.0
< 5.0
< 5.0
A2
SAMPLE
A3 | A4
A5 I A3 i
220 1 198 S 120 I 350 [340 i
• - » I 1
32
38 | 15.6 f 32 | 15.6
< 5.0 j < 5.0 I < 5.0
j ^
< 5.0 j < 5.0
< 5.0 j < 5.0 f < 5.0 1 < 5.0 I < 5.0
: I i i
9.6
16
13 ! < 5.0
5.7 I 5.4
!
IDENTIFICATION
A7 IAS JA9 JAio IAII
A12 [A13
320 I 360 I 370 ( 38O f 340 j 520 I 220
................... .!.....,.. .j,._™ 	 ;........... i._... „„ «.
32 j 26 i 19 ! 45 j 15
< 5,0 i < 5.0 [ < 5.0 I < 5.0
Si!
< 5.0 | < 5.0 ! < 5.0 ! < 5.0
! ! :
7.4 i 5.8 i 5.5 j 10
i 1 i
32 j<12.5"j 14 i 14.0 1 16 j 12 | 14 I 24
__ 	 ! 	 ___r 	 ..1 . __: 	 I . I .L...
< 5.0 j < 5.0 I < 5.0 ? < 5.0 I < 5.0 j < 5.0 j < 5.0 I < 5.0 i < 5.0
.,.....».,*.,.....!..«*» ....,.,,..*..l.,,,m»».,*, .... 	 -*. — - - —i—,. L . . - . L .
< 5.0 i < 5.0 I < 5.0
........... „.„.* 	 * 	
< 5.0
< 5,0
< 5.0
< 5.0
< 5.0
< 5.0 j < 5.0
i < 5.0 1 < 5.0
< 5.0 < 5.0
i
< 5.0 j < 5.0
< 5.0 1 < 5,0
1 < 5.0 j < 5.0 f < 5.0 { < 5.0
!,„,.„„ ....:............ _„_,!- 	 s - -
! < 5.0 1 < 5.0
1 < 5.0 1 < 5.0
I J
< 5.0 i < 5.0
j
< 5.0 | < 5.0
< 5.0 < 5.0 ! < 5.0 i < 5.6 I < 5.0
«i I 1 i
< 5,0 ! < 5.0 1 < 5.0 I < 5.0
i : 1
< 5.0 j < 5.0 j < 5.0 | < 5.0
< 5.O i < 5.0 I < 5.0 ! < 5.0
i i i
< 5.0 j < 5.0 j < 5.0 j < 5.0
< 5.0 1 < 5.0 1 < 5.0 | < 5.0
< 5.0 ] < 5.0 ] < 5.0 i < 5.0
< 5.0 | < 5.0 1 < 5.0 | < 5.0
< 5.0 | < 5.0 j < 5.0 j < 5.0 | < 5.0 \ < 5.0 f < 5.0 j < 5.0 j < 5.0
< 5.0 | < 5.0
i
lndenon,2,3-cd)pyrene { < 5,0 I < 5,0
Dibenzo(a,h)anthracene 1 < 5,0 | < 5.0
Benzo(g,h,i|perylene < 5.0 > < 5.0
i < 5.0 j < 5.0
i._n........u....|..M.u.M.ra.u...
] < 5.0 | < 5.0
< 5.0 1 < 5.0 1 < 5.0 ! < 5.0 i < 5.0 ! < 5.0
....................I..................! 	 	 s 	 - 	 	 ! 	 	 i 	 	
< 5.0 I < 5.0
1 < 5"B 1 < 5.0 ! < 5.0 I < 5.0
1 < 5.0 ! < 5.0 < 5.0 ! < 5.0
< 5.0 i < 5.0 j < 5.0 f < 5.0
< 5.0

< 5.0
5.5
13
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0 1 < 5.0 I < 5.0 i < 5.0 ! < 5.0
< 5.0 | < 5.0 I < 5.0 | < 5.0 [ < 5.0
32 S 48
j
< 5.0 f < 5.0
:
< 5.0 | < 5.0
6.8 i 5,0
f
<13.0'| 14
< 5.0 f < 5.0
< 5.0 i < 5.0
< 5,0 1 < 5.0
< 5.O | < 5,0
:
< 5.0 i < 5.0
< 5.0 1 < 5.0
:
< 5.0 j < 5.0
< 5,0 i < 5.0
i
< 5.0 1 < 5.0
< 5.0 j < 5,0
< 5.0 ! < 5.0
< 5.0 j < 5.0
:
< 5.0 i < 5.0
5 x the concentration of the lowest calibration standard

-------
                                      TABLE 4

                  COMPOSITION OF THE SAMPLE SPIKING SOLUTIONS
     Spiking
     Solutions
   Analytes
                                                            Concentration
                                                LRMS
 HRMS
        1.        Surrogate Standards

                 d10-Fluorene
                 d14-TerphenyI

        2.        Internal Standards

                 ds-NaphthaIene
                 d-io-2-MethyInaphthalene
                 d8-Acenaphthylene
                 d10-Phenanthrene
                 d^j-Fluoranthene
                 di2-Benzo(a)anthracens
                 d12-Chrysene
                 d12-Benzo(b)fluoranthene
                 d T 2-Benzo(k)f luoranthene
                 d! 2-Benzo(a)py rene
                 d12-Perylene
                 _t  •  I .   * M
312-reryiene
d12-lndeno(1,2,3,c-d)pyrene
d14-Dibenz{a,h)anthracene
d 12*BBnzo(ghi)perylene
3.       Alternate Standard

         d10-Anthracene

4.       Recovery Standards

         dl0-Acenaphthene
         d^-Pyrene
         d 12~benzo(e)pyrene
                                        1.0
                                        1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                 1.0
                                                         1.0
                                                        20.0
                                                        20.0
                                                        20.0
                                                              250
                                                              250
100
100
100
100
100
100
100
200
200
200
200
200
200
200
                                                     100
                                                   2000
                                                   2000
                                                   2000
Augusts, 1996
                                         Proposed M-429 Page 74

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                                     TABLE 4A

             COMPOSITION OF ALTERNATIVE SAMPLE SPIKING SOLUTIONS
       Spiking
       Solutions
   Analytes
                                                           Concentration
HRMS
          1A.
          2A.
Surrogate Standards


-------

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                                TABLE 5

      CONCENTRATIONS OF PAHs IN WORKING GC/MS CALIBRATION STANDARD
             SOLUTIONS FOR LOW RESOLUTION MASS SPECTROMETRY
CONCENTRATIONS (ng/#L)
Solutions

Calibration Standard?
Naphthalene
2-Methylnaphthalene
Acenaphthene
Acenaphthylene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(e)pyrene
Benzola)pyrene
Perylene
Indenod ,2,3-cd)pyrene
Dibenz(a,h)anthracene
Benzo[ghi)perylene
Internal Standards
d8-NaphthaIene
d10-2-Methylnaphthalene
d8-Acenaphthylene
d10-Phenanthrene
d1C|-Fluoranthene
d-|2-Benzo(a)anthracene
d^-Chrysene
d12-Benzo(b)fluoranthene
d12-Benzo(k)fIuoranthene
d12-Benzo(a)pyrene
d12-Perylene
d12-lndeno(1 ,2,3,c-d)pyrene
d14-Dibenz(a,h}anthracene
d12-Benzo(ghi)peryIene
1

0,25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25

1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
2

0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5

1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
3

1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0

1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
4

2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5

1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
5

5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0

1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
August 9, 1996
Proposed M-429  Page 76

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                                TABLE 5 (CONT)

       CONCENTRATIONS OF PAHs IN WORKING GC/MS CALIBRATION STANDARD
             SOLUTIONS FOR LOW RESOLUTION MASS SPECTROMETRY
                                              CONCENTRATIONS (ng/i/L)

                                                      Solutions
       Surrogate gtandards

       d10-Fluorene
       d14-TerphenyI

       Altfroitf Standard

       d10-Anthracene

       Recovery Standards
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
d10-Acenaphthene
d-jQ-Pyrene
d , 2-benzo(e)pyrene
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
August 9, 1996
               Proposed M-429  Page 77

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                                 TABLE 6

      CONCENTRATIONS OF PAHs IN WORKING GC/MS CALIBRATION STANDARD
             SOLUTIONS FOR HIGH RESOLUTION MASS SPECTROMETRY
                                           CONCENTRATIONS (pg/frL)

                                                  Solutions
Calibration Standards
Naphthalene
2-MethylnaphthaIene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(e)pyrene
Benzo(a)pyrane
Perylene
Indenod ,2,3-cd)pyrene
Dibenz(a,h)anthracene
Benzo(ghi)perylene
Internal Standards
dg-Naphthalene
d8Methylnaphtha!ene
d8-Acenaphthylene
d-iQ-Phenanthrene
d10-Fluoranthene
d12-Benzo(a)anthracene
d12-Chrysene
d T 2-Benzo{b)fluoranthene
d12-Benzo(k)fIuoranthene
d12-Benzo{a)pyrene
d12-Perylene
d T 2-Indeno{ 1 (2,3,c-d)pyrene
d14-Dibenz(a,h)anthracene
d 1 2-Benzo(ghi)peryIene

10
10
10
10
10
10
10
10
10
10
10
10
1O
10
10
10
10
10
10

100
100
100
100
100
100
100
200
200
200
200
200
200
.200

50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50

100
100
100
100
100
100
100
200
200
200
200
200
200
200

100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100

100
100
100
100
100
100
100
200
200
200
200
200
200
200

200
200
200
200
200
200
200
200
200
200
200
200
200
200
200
200
200
200
200

100
100
100
100
100
100
100
200
200
200
200
200
200
200

500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500

100
100
100
100
100
100
100
200
200
200
200
200
200
200
August 9, 1996
Proposed M-429  Page 78

-------
                               TABLE 6  (CONT)

       CONCENTRATIONS OF PAHs IN WORKING GC/MS CALIBRATION STANDARD
             SOLUTIONS FOR HIGH RESOLUTION MASS SPECTROMETRY
                                             CONCENTRATIONS (pg///L)

                                                    Solutions
Surrogate Standards
d10-Fluorene
d14-Terpnenyl

100
100

100
100

100
10O

100
100

100
100
       Alternate Standard

       d10-Anthracene               100     100     100     100     100

       RecoveryStandards

       d10-Acenaphthene             200     200     200     200     200
       dto-Pyrene                   200     200     200     200     200
       d12-benzo(e)pyrene             200     200     200     200     200
Augusts, 1996                                       Proposed M-429  Page 79

-------
                                TABLE 6A

     CONCENTRATIONS OF PAHs IN ALTERNATIVE WORKING GC/MS CALIBRATION
        STANDARD SOLUTIONS FOR HIGH RESOLUTION MASS SPECTROMETRY
CONCENTRATIONS (pg/j/L)
Solutions

Calibration Standard?
Naphthalene
2-Methy!naphthaIene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzofalanthracene
Chrysene
Benzo{b)fluoranthene
Benzo(k)fluoranthene
Benzo(e)pyrene
Benzo(a)pyrene
Perylene
Indenod ,2,3-cd)pyrene
Dibenz(a,h)anthracene
Benzo(ghi)perylene
Internal Standards
dg-Naphthalene
ds-Acenaphthy!ene
d ! Q- Acenaphthene
d10-FIuorene
d10-Phenanthrene
d10-Fluoranthene
d ! 2-Benzo(a)anthracene
d12-Chrysene
d 1 2-Benzo(b)fIuoranthene
d12-Benzo(k)fluoranthene
d12-Benzo{a)pyrene
d12-Indeno(1 ,2,3,c-d)pyrene
d14-Dibenz(a,h)anthracene
d12-Benzo(ghi)perytene
1

10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10

100
100
100
100
100
100
100
100
200
200
200
200
200
200
2

50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50

100
100
100
100
100
100
100
100
200
200
200
200
200
200
3

100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100

100
100
100
100
100
100
100
100
200
200
200
200
200
200
4

200
200
200
200
200
200
200
200
200
200
200
200
200
200
200
200
200
200
200

100
100
100
100
100
100
100
100
200
200
200
200
200
200
5

500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500

100
100
100
100
100
100
100
100
200
200
200
200
200
200
August 9, 1996
Proposed M-429  Page 80

-------
                              TABLE 6A  (CONT)

     CONCENTRATIONS OF PAHs IN ALTERNATIVE WORKING GC/MS CALIBRATION
        STANDARD SOLUTIONS FOR HIGH RESOLUTION MASS SPECTROMETRY
                                            CONCENTRATIONS

                                                    Solutions
       Surrogate Standards

       d12-benzo(e)pyrene             100    100     100      100     100
       du-Terphenyl                 100    100     100      100     100

       Alternate Standard

       d10-Anthracene                100    100     100      100     100

       Recovery Standards

       d10-2-Methy!naphtha!ene        200    200     200      200     200
       d10-Pyrene                   200    200     200      200     200
       d12-Pery!ene                  200    200     200      200     200
August 9, 1996                                       Proposed M-429 Page 81

-------
                                 TABLE 7




                    SPIKE LEVELS FOR LABELLED STANDARDS
Time of
Addition
Before
sampling


Before
extraction














Before
extraction

Before
GC/MS



Analyte
Surrogate Standards

d-|0-Fluorene
d14-Terphenyl
Internal Standards

d8-Naphthalene
d 1 0-2-Methylnaphthalene
dg-Acenaphthylene
d10-Phenanthrene
d10-Fluoranthene -
d12-Benzo(aJanthracene
d12-Chrysene
d1 2-Benzo(b)fluoranthene
d1 2-Benzo{d)fluoranthene
d12-Benzo{a)pyrene
dl2-Perylene
dl2-lndeno{1 ,2,3,c-d)pyrene
du-Dibenz(a,h)anthracene
d1 2-Benzo(ghi)perylene
Alternate Standard

dl0-Anthracene
Recovery Standards

d10-Acenaphthene
d10-Pyrene
d12-benzo(e)pyrene
LRMS
(//g/sample)


2.0
2.0


2.0
2.0
2,0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0


2.0


1.0
1.0
1.0
HRMS
(ng/sampte)


500
500


200
200
200
200
200
200
200
400
400
400
400
400
400
400


200


100
100
100
August 9, 1996
Proposed M-429 Page 82

-------
                                   TABLE 7A

   SPIKE LEVELS FOR LABELLED STANDARDS FOR ALTERNATIVE HRMS SPIKING SCHEME
        Time of
        Addition
     Analyte
  HRMS
(ng/sample)
        Before
        sampling
        Before
        extraction
        Before
        extraction
        Before
        GC/MS
Surrogate Standards

d T 2~benzo(e}pyrene
du-Terphenyl

Internal Standard?

dg-Naphthalene
dg-Acenaphthylene
d10-Acenaphthene
dl0-FIuorene
dTQ-Phenanthrene
djg-Fluoranthene
dt 2-Benzo(a)anthracene
d12-Chrysene
d12-Benzo{b)f!uoranthene
d| 2~Benzo(d)fluoranthene
d12-Benzo(a)pyrene
d12-lndeno(1 ,2,3,c-d)pyrene
d)4-Dibenz(a,h)anthr3cene
d, 2-Benzo(ghi)perylene

Alternate Standard

d10-Anthracene
                         d 1 0-2-Methylnaphthalene
                         dl0-Pyrene
                         d12-Perylene
                                                            500
                                                            500
                                                            200
                                                            200
                                                            200
                                                            200
                                                            200
                                                            200
                                                            200
                                                            200
                                                            400
                                                            400
                                                            400
                                                            400
                                                            400
                                                            400
                                                            200
                                   100
                                   100
                                   100
August 9, 1996
                               Proposed M-429  Page 83

-------
                                    TABLE 8

    TARGET CONCENTRATIONS FOR LABELLED STANDARDS IN SAMPLE EXTRACT1
                                               ng//y[
                                               LRMS
         HRMS
SurrogateStandards

d10-Fluorene
di4-Terphenyl

Internal Standards

dg-Naphthalene
d 10-2-Methylnaphthalene
dg-Acenaphthylene
d10-Phenanthrene
d10-Fluoranthene
d ! 2-Benzo{a)anthracene
d12-Chrysene
d 12-Benzo(b)fluoranthene
d 1 2-Benzo(k|fluoranthene
d12-Benzo(a)pyrene
dl2-lndeno{1,2,3,c-d)pyrene
d14-Dibenz(a,h)anthracene
d12-Benzo(ghi)perylene

Alternate Standard

d10-Anthracene

Recovery Standards

d 1 g-Acena phthene
d10-Pyrene
d-|2-benzo(e)pyrene
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                2.0
                                                1.0
                                                1.0
                                                1.0
                                                1.0
         500
         500
         200
         200
         200
         200
         200
         200
         200
         400
         400
         400
         400
         400
         400
         400
         200
         200
         200
         200
   1 Assuming 100 percent recovery.
August 9, 1996
Proposed M-429  Page 84

-------
                                   TABLE 8A

    TARGET CONCENTRATIONS FOR LABELLED STANDARDS IN SAMPLE EXTRACT
              OBTAINED WITH ALTERNATIVE HRMS SPIKING SCHEME1
                                                         HRMS
           Surrogate Standards

           d12-benzo(e)pyrene                               500
           d14-Terphenyl                                    500

           Internal Standards

           ds-Naphthalene                                  200
           dg-Acenaphthylene                               200
           d10-Acenaphthene                                200
           d10-Fluorene                                     200
           d^-Phenanthrene                                200
           d10-Fluoranthene                                 200
           d12-Benzo(a)anthracene                           200
           d12-Chrysene                                    200
           d12-Benzo(b)fluoranthene                          400
           d12-Benzo(k)fluoranthene                          400
           d12-Benzo{a)pyrene                               400
           d12-lndeno(1,2,3,c-d}pyrene                       400
           d14-Drbenz(a,h)anthracene                         400
           d12-Benzo(ghi)perylene                            400

           Alternate Standard

           d10-Anthracene                                  200

           Recovery Standards

           d10-2-Methy (naphthalene                          200
           d10-Pyrene                                      200
           d12-Perylene                                     200


   1 Assuming 100 percent recovery.
August 9, 1996                                       Proposed M-429 Page 85

-------
                               TABLE 9




   CONCENTRATIONS OF COMPOUNDS IN LABORATORY CONTROL SPIKE SAMPLE
ng/sample

Unl abelled Qgmpo un ds
Naphthalene
2-Methylnaphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(8)pyrene
Benzo(a)pyrene
Perylene
Indenod ,2,3,c-d)pyrene
Dibenz(a,h)anthracene
Benzo(ghi)perylene
Alternate Standard
d10-Anthracene
LRMS

2.0
2.0
2.0
2.0
2.0
2.0
2.0
. 2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

2.0
HRMS

1000
200
200
200
200
500
200
200
200
200
200
200
200
200
200
200
200
200
200

200
August 9, 1996
Proposed M-429 Page 86

-------
                                  TABLE 10
              RECOMMENDED GAS CHROMATOGRAPHIC OPERATING
                        CONDITIONS FOR PAH ANALYSIS
          Column Type

          Length (m)

          ID (mm)

          Rim Thickness (//m)

          Helium Linear Velocity (cm/sec)

          Injection mode

          Splitless Time (sec)

          Initial Temperature (°C)

          Initial Time (min)

          Program Rate (°C/min)

          Final Temperature (°C)

          Final Hold Time


          Injector Temperature (°C)
    DB-5

    30

    0.25

    0.32

    30

    Splitless

    30

    45

    4

    8

    300

    until benzo(ghi)
    perylene has eluted

    320
August 9, 1996
Proposed M-429 Page 87

-------
                                    TABLE 11
        ASSIGNMENTS OF INTERNAL STANDARDS FOR CALCULATION OF RRFs
        AND QUANTITATION OF TARGET PAHs AND SURROGATE STANDARDS
            Analyte
Internal Standards
          Unlabeled PAH
          Naphthalene
          2-MethyInaphthalene
          Acenaphthyfene
          Acenaphthene
          Fluorene
          Phenanthrane
          Anthracene
          Fluoranthene
          Pyrene
          Benzo(a)anthracene
          Chrysene
          Benzo(b)fluoranthene
          Benzo (k)f I uora nthene
          Benzo(e)pyrene
          Benzo(a)pyrene
          Perylene
          Indenod ,2,3-cd)pyrene
          Dibenz(a,h)anthracene
          Benzo(ghi)perylene
dg-Naphthalene
d ^-2-Methylnaphthalene
dg-Acenaphthylene
dg-Acenaphthylene
d10-Phenanthrene
di0-Phenanthrene
d10-Phenanthrene
d-iQ-Fluoranthene
d10-Fluora nthene
d^ 2-Benzo(a)anthracene
d12-Chrysene
d^ 2-Benzo(b)f luoranthene
d^ 2-Benzo(k)fluoranthene
d12-Benzo(a)pyrene
d12-Benzo(a)pyrene
d12-PerylenB
d12-lndeno(1,2,3,c-d)pyrene
d14-Dibenz(a,h)anthracene
d12-Benzo(ghi)perylene
          Surrogate Standards
          d10-Fluorene
          d14-Terphenyl
d10-Phenanthrene
d10-Fluoranthene
August 9, 1996
     Proposed M-429  Page 88

-------
                                  TABLE 1 1A

       ASSIGNMENTS OF INTERNAL STANDARDS FOR CALCULATION OF RRFs
       AND QUANTiTATION OF TARGET PAHs AND SURROGATE STANDARDS
                   USING ALTERNATIVE HRMS SPIKING SCHEME
          Analyte
   Internal Standards
        Unlabeled PAH
        Naphthalene
        2-MethylnaphthaIene
        Acenaphthylene
        Acenaphthene
        Fluorene
        Phenanthrene
        Anthracene
        Fluoranthene
        Pyrene
        Benzo(a)anthracene
        Chrysene
        Benzo(b)fluoranthene
        Benzo(k)fluoranthene
        Benzo(e)pyrene
        Benzo(a)pyrene
        Perylene
        Indenod ,2,3-cd)pyrene
        Dibenz(a,h)anthracene
        Benzolghi)perylene

        Surrogate Standards
        d14-Terphenyl
        d12-Benzo{e}pyrene
dg-Naphthalene
d 1 Q-Acenaphthene
da-Acenaphthylene
d10- Acenaphthene
dl0-Phenanthrene
d10-Phenanthrene
d10-Fluoranthene
d10-Ftuoranthene
d12-Benzo(a)anthracene
d12-Chrysene
d12-Benzo(b)fluoranthene
d12-Benzo(k)fluoranthene
d12-Benzo(a)pyrene
d12-Benzo{a)pyrene
d12-Benzo(a)pyrene
d^-lndenon^S.c-dlpyrene
d14-Dibenz(a,h)anthracene
d T 2-Benzo(ghiJperylene
d10-Fluoranthene
d12-Benzo(aIpyrene
August 9, 1996
         Proposed M-429 Page 89

-------
                                    TABLE 12
          ASSIGNMENTS OF RECOVERY STANDARDS FOR DETERMINATION
              OF PERCENT RECOVERIES OF INTERNAL STANDARDS AND
                           THE ALTERNATE STANDARD
                Analyte
Recovery Standard
             InternalStandards

             ds-Naphthalene

             d10 -2-Methylnaphthalene

             dg-Acenaphtnylene

             d-jQ-Phenanthrene

             d10-FIuoranthene

             d12-Benzo(a)anthracene

             d12-Chrysene

             d 12-Benzo(b)f luoranthene

             d T 2-Benzo(k)f luoranthene

             d12-Benzo(a)pyrene

             d12-Perylene

             d! 2-'ndeno( 1,2,3,c-d)pyrens

             d14-Dibenz(a,hJanthracene

             d12-Benzo{ghi)perylene


             AlternatfStandard

             dig-Anthracene
d-jQ-Acenaphthene

d-iQ-Acenaphthene

d10-Acenaphthene

d10-Pyrene

d10-Pyrene
d12-Benzo(e)pyrene

d j 2-Benzo(e)pyrene

  d12-Benzo(e)pyrene

dj 2-Benzo(e)pyrene

d12-Benzo(e)pyrene

d12-Benzo(e)pyrene

d12-Benzo(e)pyrene
August 9, 1996
   Proposed M-429  Page 90

-------
                                   TABLE 12A

         ASSIGNMENTS OF RECOVERY STANDARDS FOR DETERMINATION OF
       PERCENT RECOVERIES OF INTERNAL STANDARDS AND THE ALTERNATE
              STANDARD USING ALTERNATIVE HRMS SPIKING SCHEME
             Anaiyte
         Internal Standard?

         d8-Naphthalene

         d10 -2-Methylnaphthalene

         dg-Acenaphthylene

         d! 0-Phena nthrene

         d10-Fluoranthene

         d12-Benzo(a)anthracene

         d12-Chrysene

         d12-Benzo(b)f!uoranthene

         d 12-Benzo( k)fluoranthene

         d12-Benzo(a)pyrene

         d12-Pery!ene

         d12-lndeno(1,2,3,c-d)pyrene

         d14-Dibenz(a,h)anthracene

         d] 2-Benzo(ghi)perylene


         AlternateStandard

         d10-Anthracene
Recovery Standard
d10-2-Methylnaphthalene

d10-2-MethylnaphthalBne

d j Q-2-Methylnaphthalene

d10-Pyrene
d10-Pyrene

d10-Pyrene

d12-Perylene

d12-Perylene

d-|2-PeryIene
d12-Perylene

d12-Pery!ene

d12-Perylene
d10-Pyrene
                                   H
August 9, 1996
   Proposed M-429  Page 91

-------
                                TABLE 13

             QUANTITATION AND CONFIRMATION IONS FOR SELECTED
                   ION MONITORING OF PAHs BY HRGC/LRMS
Analyte
Naphthalene
d8-Naphthalene
2-Methylnaphthalene
d10-2-Methylnaphthalene
Acenaphthyiene
dB-Acenaphthylene
Acenaphthene
diQ-Acenaphthene
Fiuorene
d10-FIuorene
Phenanthrene
dnj-Phenanthrene
Anthracene
d10-Anthracene
Fluoranthene
d10-Fluoranthene
Pyrene
d10-Pyrene
Benzo{a)anthracene
d^ 2-Benzo(a)anthracene
Chrysene
d14-Terphenyl
Quant.
Ion
128
136
142
152
152
160
154
164
166
176
178
188
178
188
202
212
202
212
228
240
228
240
244
Confirm.
Ion
127
68
141
153
153
165
176
94
176
94
101
106 '
101
106
114
120
114
120
122
% Relative
Abundance of
Confirm. Ion
10
80
80
15
86
80
15
15
15
15
15
15
15
August 9, 1996
Proposed M-429  Page 92

-------
                              TABLE 13 (CONT)

             QUANTITATION AND CONFIRMATION IONS FOR SELECTED
                   ION MONITORING OF PAHs BY HRGC/LRMS
Analyte
Benzo(b)fluoranthene
d12-Benzo|b)fluoranthene
Benzo(k)fluoranthene
d1 2-Benzo( k)f luora ntbene
Benzo(e)pyrane
d^-Benzofelpyrene
Benzo(a)pyrene
d12-Benzo(alpyrene
Perylene
lndeno(1 ,2,3-cd)pyrene
dl2-lndeno(1 ,2,3-cd)pyrene
Dibenz(ah)anthracene
d14-Dibenz(ah)anthracene
Benzo(ghi)perylene
d 1 2*Benzo
-------
                                 TABLE 14




     MASS DESCRIPTORS USED FOR SELECTED ION MONITORING FOR HRGC/HRMS
Descriptor Analyte
No.
1









2
















IS
SS
AS
RS
LOCK
QC

Naphthalene
PFK
dg-Naphthalene
2-Methylnaphthalene
d ! Q-2-Methylnaphthalene
Acenaphthylene
dg-Acenaphthylene
Acenaphthene
d10-Acenaphthene
PFK'
Fluorene
d10-Fluorene
Phenanthrene
d10-Phenanthrene
Anthracene
d10-Anthracene
Fluoranthene
d-|D-Fluoranthene
Pyrene
PFK
d10-Pyrene
Benzo(a)anthracene
d ^-Benzo-a-Anthracene
Chrysene
d^-Chrysene
PFK
du-Terphenyl
= Internal Standard
= Surrogate Standard
= Alternate Standard
= Recovery Standard
= Lock-Mass Ion
- Quality Control Check Ion
Ion
Type
M
LOCK
IS
M
IS
M
IS
M
RS
QC
M
SS
M
IS
M
AS
M
IS
M
QC
RS
M
IS
M
IS
LOCK
SS






Accurate
m/z
128.0626
130.9920
136.1128
142.0782
152.1410
152.0626
160.1128
154.0782
164.1410
169.9888
166.0782
176.1410
178.0782
188.1410
17S.0782
183.1410
202.0782
212.1410
202.0782
204.9888
212.1410
228.0939
240.1692
228.0939
240.1692
230.9856
244.1974






August 9, 1996
Proposed M-429 Page 94

-------
                             TABLE U(CONT)




     MASS DESCRIPTORS USED FOR SELECTED ION MONITORING FOR HRGC/HRMS
Descriptor Analyte
No.


















The
H =
IS
ss
AS
RS

3 Perylene
d12-Perylene
PFK
Benzo(b)fiuoranthene
d1 2-Benzo(b}fluoranthen8
Benzo(k)fluoranthena
d<| 2-Benzo-k-fluoranthene
Benzo(e)pyrene
d|2-Benzo(e)pyrene
Benzo(a)pyrene
d 1 2-Benzo(a)pyrene
Benzo(ghi)perylene
d12-Benzo{ghi)pery!ene
Indenod ,2,3-cd)pyrene
d|2-lndeno(1 ,2,3-cd)pyrene
Dibenzo(ah)anthracene
PFK
d14-Dibenzo(ah)anthracene
following nuclidic masses were used:
1.007825 2H = 2.014102
= Internal Standard
= Surrogate Standard
= Alternate Standard
= Recovery Standard
Ion
Type
M
IS
QC
M
is
M
IS
M
RS
M
IS
M
IS
M
IS
M
LOCK
IS

C = 12.000000




Accurate
m/z
252.0939
264.1692
268.9824
252.0939
264.1692
252.0939
264.1692
252.0939
264.1692
252.0939
264.1692
276.0939
288.1692
276.0939
288.1692
278.1096
280.9824
292.1974






LOCK = Lock-Mass Ion
QC
= Quality Control Check Ion


August 9. 1996
Proposed M-429 Page 95

-------
                                                         FIGURE 1
   1
METHOD 429 FLOWCHART
                     7
    11.3.9  The end user is identified
    §1.3.10 The tester is designated
           The end user chooses:
    §2.1.1  •  source target concentration
    52.1.2  The tester selects analyst with documented
    §8.4    experience in satisfactory performance of analytical
    §8.4.1   procedures
            Tester and laboratory coordinate:
    §4.3.2  •  pre-test cleaning of glassware
    §4.2    •  pre-test cleaning, contamination checks, and
    §4.3.3    storage of sampling materials and reagents
    §4.3.4  •  preparation of filter, sorbent cartridges, method
              blanks, and LCS
§10.1
§10.1
§10.1
Tester requests pre-test analytical results from
laboratory:
.1 • contamination check of filters
.2 • contamination check of XAD-2 resin
.3 • Method detection limits (MDLs) and
Practical quantitation limits (PQLs)
6
§2.5
Tester calculates and plans:
• S3 sampling runs and S1 blank sampling train
• sample volume
• sampling time
• source reporting limit
• chain of custody
§4.3.1
Tester performs:
• calibration of equipment

8
§2.2
Tester writes:
• pre-test protocol

9
§4.4.1
§4.4.2
§4.4,3
§4.4.4
§5
Tester performs;
• preliminary field sampling determinations
• sampling train preparation
• leak checks
• sampling procedure
• £3 sampling runs
• SI blank sampling train
• recovery of all runs and blank sampling train
10
§5.3
§5,4
Tester delivers:
• recovered sampling runs and blank train(s)
• chain of custody record
11
§6
§7
§8
19
§10.2
Laboratory performs:
• extraction of field samples
• analyses
• QA/QC procedures
• chain of custody
• reporting requirements

                                                                     12
                                                                              Tester performs:
                                                                      §4,3,1   •  post-test calibrations
                                                                      §9.2    •  calculations
                                                                      §10,3   •  data recording and chain of Custody
                                                                              •  reporting requirements
August 9, 1996
                                                   Proposed M-429  Page 96

-------
                                                      Oven
            Heated Probe,
             S-typa Pitoi
           & Tomp. Sensor
  Stack
  Wall
     Ttmp.         L_
    Readout
                Pilot
             Manometer
                       Orifice
                     -C
                  Orifice
                Manometer
Thermocouple
     o
                                        DryGis
                                         Miter
                     Cyclone (Optional)


                     Filter Assembly

                      — Transfer Line
                          Condenser
                          (water cooled)

                           —Thermocouple

                          Sorbent Module
                          (water cooled)
                                                      ImpingersinlceBath:
                                                    Buffer Solution in 11
                                                           W Empty
                                                         Silica Gel in #4
                                                           Bypass
                                                           Valve
                                                                      Main
                                                                      Valve
                                                                              Check
                                                                             /Vilve
                                                           Pump
                                  Figure 2

                          PAH Sampling Train
August 9, 1996
                         Proposed M-429 Page 97

-------
in
c
u
i-r

(O
(O
CO
05
                                        H To Suit h
                                                   Glass Wool
                                                     Plug
                                                               lifvSjsiJ i^HfivVj
                                                               nsaftp ai^l^l'
                             8 mm Glass
                             Cooling Coil
                  Water Jacket—1
XAD-2
                                                            >^
Glass Sintered
    Disk
o
T3
O
M
                              Condenser
                                       Sorbant Trap
fO
CD


~Q
D>

-------
           Liquid Take Off
       Liquid Nitrogen
          Cylinder
          (150L)
                               Loose Weave Nylon
                                  Fabric Cover
                                      10.2 cm (4')
                                      Pyrex Pipe
                               0.95 cm (3/81)
                                / Tubing
Heat Source
                                                      *•»•»•»"»•*•*>!*
                               »« •»•.>•»#*<»•»
                          !»«>»StS«-» •»*»**** *
                         8M»«N
                                                           Rne Screen
                                Figure 4

             XAD-2 Fluidized Bed  Drying Apparatus
August 9, 1996
                     Proposed M-429 Page 99

-------
                                                      FIGURE 5
                                          METHOD 429 FIELD DATA RECORD
Run No.	
Location 	
Date ,	
Operator	
Meter Box No,
Local Time
 Start/Stop _
Pilot Tube Factor
Probe Tip Dia, in.
Probe Length 	
Sampling Train Leak Test
Before	in. Hg  _
After
in. Hg
Stack Diameter 	
Meter Box Calibration
Factor (Y) 	
Leak Check Volume
Pitot Tube Leak Check
Before	 After
 Leak Rate
	cu.ft/min
	cu.ft/min
     cu. ft.
Project No.	
Plant Name	
Ambient Temp °F 	
Meter Temp °F 	
Bar. Press, "Hg 	
Stack Press, "H2O 	
Assumed Moisture, % _
Heater Box Setting, °F _
Probe Heater Setting, °F
Assumed M.W. (wet%)
Assumed M.W. (dry%)
Sampling
Point
Start












Clock
Time













Dry Gas
Meter, cu, ft.













Pitot AP
in. H20













Orifice AH
"H2O
Desired













Actual













Temperature (°F)
Impinger













Filter box













Stack













Pump
Vacuum
in. Hg













   August 9, 1996
                                                                Proposed M-429  Page 10

-------
 c,
 
 a
NJ
(0
a
id
a>
C                Container    \\
             ,    Nal     ))
 Mark liquid level,
Store at fC or lower
  away from light
                         Transfer
C                         Container  \\
                           No 2    JJ
 Store at 4"C
or lower away
  from light
                     Rinse with known volume:
                             1. acetone
                         2. methylene chloride
                             3.hexane
                                             /       3.hexane   \
                                                    Fitter support,
                                                     Back half
                                                     filter holder
                                                    Transfer   Condenser |
 Mark liquid level,
Store at 4 C or lower
  away from light
                                Cap
c
                                                       Resin
                                                     cartridge
                                                                                     Store at 4 Cor lower
                                                                                       away from light
                                                                                                            A. Tare weigh Container i4
                                                                                                            8. Decant contents ol
                                                                                                              Impingers into tared
                                                                                                              Container f4
                                                                                1
                                                                                                C. Weigh Container /4
                                                                                                D.Mark liquid level,
                                                                                                  Store at 4T or lower
                                                                                                  away from light
                                                 A. Tare weigt;
                                                   cartrtridgt
                                                   silica gel
                                                 B. Weigh afte
                                                   sampling
                                                                                                                                         Silica ge
                                                                                                                                         cartridgi
                                              Rinse with known volume:
                                                  1. acetone
                                                  2. methylene chloride
                                                  3. hexane
                                                                                                                                           if
                                                                                                                                         Recycle
                                                                                                   Mark liquid level.
                                                                                                   Store at 4°C or lower
                                                                                                   away from light

-------
                            Figure 7
     Flow Chart for Sampling, Extraction and Cleanup for
            Determination of PAH in a Split Sample
                             Surrogate Standards
                            Added to XAD-2 Resin
                                Sampling
                         t
                            ^Containers No. land No, 3
August 9, 1996
Proposed M-429 Page 102

-------
                            Figure 8
    Flow Chart for Sampling, Extraction and Cleanup for

        Determination of PAH in a Composite Sample
                              Surrogate Standards
                             Added to XAD-2 Resin
               MeCI2
           Soxhlet Extraction
                              Recovery Standards
        Containers No. land No. 3
                               G.C./ Mass Spec.
August 9, 1996
Proposed M-429 Page 103

-------
                                        FIGURE 9

               EXAMPLE OF PRE-TEST CALCULATIONS FOR PAH EMISSIONS TEST


Naphthalene
2-MethylnaphthaIene
Acenaphthylene
Acenaphthene
Fluorene1
Phenanthrene
Anthracene
Fluorantnene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fiuoranthene
Benzo(k)fluoranthene
Benzolejpyrene
Benzo(a)pyrene
Perylene
Indenoll ,2,3-c,d)pyrene
DiBenzo(a,hjanthracene
PQL
Ing/sample)
2400
330
5.0
5.0
83
110
5.0
„.„.„..,..___
5.0
____.
"" To""
5.0
__--_.
"••-•-"••g-0""
5.0
5.0
5.0
"""""""""576™""
STC
(ng/dscm)
MSV
(dscf)
MST
(hours)
PST m
PSV =
F
<1500 >56.5 ! > 1.89 NA
NA
180
D
<6
120
<6
'•"" iT"
46
..„,.,»«.«* . »«*«...»,
<6
:::«"'":::
50
___
NA
<6
NA
<6
""""""< 6
NA
0.98
29.4
>489
32.4
>29.4
3.8
"">29!4"""
4;"2~~
3.5
>29.4
NA
NA
0.03
0.98
>16.3
1.08
>0.98
0.13
_.„....
0.12
"™NA™""~"
>0.98
'""""NA™
6 hours
180 dscf
SRL
(ng/dscm)
471
NA I 64.7
183 I 0.98
6 I 6.98
*N"A i
6 !
NA
—*L—\
NA"---"'
NA
"""NA""
>29.4 ^ >0.98 j NA
§enzo{g,h,i)perylene ! 5.6 <6 j >29.4
>0.98 ! NA
16.3
21.6
0.98
0.98
0.98
™™_™_
0.93
0.98
67§8
0.98
Average Volumetric Sampling Rate (VSR) = 0.5 dscfm = 30 dscf/hr
 PQL  =   Practical quantitation limit for analyte (based on pre-test analysis of XAD-2 resin)
 STC  =   Source target concentration for analyte.  (From previous emissions test.  Samples
           were analyzed by HRGC/LRMS).
 MSV  =   Minimum sample volume required to collect detectable levels of target analyte,
           (MSV = PQL -H STC)                          Equation 429-1
 MST  =   Minimum sample time required to collect detectable levels of target analyte at VSR.
           (MST = MSV -»• VSR)                         Equation 429-2
 PST  =   Planned sampling  time (6  hours chosen as the longest practical sampling
           time for the planned emissions test)
 PSV  =   Planned sample volume (PSV = PST x  VSR)     Equation 429-4
 F     =   Safety factor (> 1) that allows for deviation from ideal sampling and analytical
           conditions.  (F =  PSV •*• MSV)                  Equation 429-5
 SRL  =   Source reporting limit if the target analyte cannot be detected with the planned test
           parameters. (SRL = PQL * PSV)                Equation 429-7
 NA       This calculation is not applicable either because there is no STC value available or the
           STC is a detection limit.

       1    PSV is lower than the  MSV.  Therefore, the analyte is not expected to be detected if it
           is present at the target concentrations.  It will only be detected if the actual
           concentration is lower than the indicated SRL.
August 9, 1996
Proposed M-429  Page 104

-------
RUN NO.
PLANT NAME
SET-UP DATE
RECEIVED BY
                                       FIGURE 10
                 CARB METHOD 429 IPAHs) SAMPLING TRAIN SET-UP RECORD
                                    PROJECT NO.
                                    PLANT LOCATION
                                    SET-UP BY
                                    DATE/TIME
        COMPONENTS
  1.           NOZZLE
  2,
  6,
      PROBE
        FILTER HOLDER
  5.    TRANSFER LINE
     AND CONDENSER
     Fittings
XAD-2 RESIN
 CARTRIDGE
  7. IMPINGERS;  No. 1
          U-Connector
                No. 2
          U-Connector
                No. 3
          U-Connector
              COMPONENT ID
               FILTER   Lot*
             OTHER INFORMATION
                 Material
                Diameter
            Liner material
                  Length
         Before set-up, all
      openings sealed with
        Filter support type
              Filter Type
                   Size
     Contamination check?

      Transfer line material
       Both ends sealed in
        lab prior to set-up
                 Fittings
     Contamination chack?
                Spiked?
      Charge with 100 mL
impinger solution and weigh
      Charge with 100rnL
impinger solution and weigh

            Weigh empty
  8.
  SILCA GEL
 CARTRIDGE
            Tare weight
                                          Appearance
August 9, 1996
                                                   Proposed M-429 Page 105

-------
                                           FIGURE 11

                   CARB METHOD 429 {PAHs) SAMPLING TRAIN RECOVERY RECORD

RUN NO.	  PROJECT NO.       	:	
PLANT NAME    	  PLANT LOCATION   	
RECOVERY DATE	  RECOVERED BY     	
 1.  CHECK whether openings were covered.          RINSE 3x each with Acetone, MeCI2, Hexane.
    MARK liquid level and STORE containers at temp. <4°C away from light.

                      Openings       	Rinse volume (mL)	     Storage
    Component         covered?       jAcetgne         MeCI^	     Hexane      Containers) IDs
    Nozzle             	     :	__	   	   	
    Probe liner          	       ..._:		   		
    Rlter holder front    	„     ,	,	   _	   	
2.  STORE filter(s) at temp. <4°C away from light,       RECORD ALL sample storage information.
                                                           Storage              Storage
    Component          Appearance after sampling         (Temperature & light)     Containerisl JD
    Filter              	      	  	
    Rlter	      	  	
    Filter              	,      	.  .	

3,  CHECK whether openings were covered.          RINSE 3x each with Acetone, MeCI2, Hexane.
    MARK liquid level and STORE containers at temp. <4°C away from light.

                     Openings  	Rinse volume (ml)	      Storage      Storage
    Component        covered?  Acetone-      MeCI2      Hexane     Temp.Alight  ContainerID
    Filter support and
    fitter holder back   	  	    ,    	   	„    ,   		
    Transfer line	„  _________    	   	  	  	
    Condenser         	,  r_.__,__ r,_.:_:    ^-r—:-;r..,,.._   	  	,	

4.  STORE Resin cartridges at temp. <4°C away from light.   RECORD ALL storage information.

    	ID	      Appearance after sampling          Storage temperature & light conditions
5. WEIGH impinger contents and silica gel cartridge.
   MARK liquid level and STORE impinger contents at temp. <4°C away from light.
                                                             Additional impingers     Silica gel
      Weight            No. 1        No. 2       No. 3        No. 4        No, 5       cartridge
   Final (g)            	   _____   .	    	    _______    	
   Before sampling Ig)
   Gain !g)        (A)	IB)          (C)	 (D)_	(EJ	  (F),

   Total condensate  (A) + IB) + 1C) + |D) + JE) + (F)	(g>

   STORAGE CONTAINER ID(s)      	.   	    	      .	
6. RINSE impingers 3x each with Acetone, MeCI2. Hexane.
   MARK liquid level and STORE impinger rinses at temp. <4°C away from light.
   Rinse volumes (mL)  Acetone
                     MeCI2
                     Hexane

   STORAGE CONTAINER ID(s)
   August 9, 1996                                                   Proposed M-429 Page 106

-------
                               FIGURE 12

                   CHAIN OF CUSTODY SAMPLE RECORD
Project ft
Date;
Source name; 	
Sampling location:	
Chain of Custody Log Record # (s)

SAMPLE STORAGE INFORMATION
   Start:	
   Stop:	
   Sample/Run #
   Sample type: _
   Operator:	
SAMPLE PRESERVATION
Ice/Dry ice?

Comments


CHAIN OF CUSTODY
             ACTION
       DATE
TIME
GIVEN BY   TAKEN BY
RELATED
IDs
FR
F
BR
C
1
IR
DESCRIPTION/COMMENTS
Front rinse (nozzle, probe, filter holder front)
Filter in sealed storage container
Back rinse (filter support, filter holder, sample line &
condenser
Resin cartridge
Impinger contents
Impinger rinses
Log #s






Augusts, 1996
                      Proposed M-429  Page 107

-------
                                     FIGURE 13

                          CHAIN OF CUSTODY LOG RECORD
 PROJECT NO.
                                                    Page
                                                     of
  Log*
Sample

  ID
Date
Time
Comments
Given

 by
Taken by
  Sample Identifier

        FR
        F
        BR
       IR
                        Sample Description

        Rinses of probe and front half of filter holder
        Filter in sealed storage container
        Rinses of filter support, back half of filter holder, sample transfer line and
        condenser
        Aluminum foil wrapped, capped resin cartridge
        Impinger contents
        Impinger rinses
Augusts, 1996
                                                 Proposed M-429 Page 108

-------
                                    FIGURE 14A
     EXAMPLE GC/MS SUMMARY REPORT (HRMSJ FOR INITIAL CALIBRATION SOLUTION #1
  CALIFORNIA AIR RESOURCES BOARD METHOD 429 POLYCYCLIC AROMATIC HYDROCARBONS
ICALID:  STT120A1
RUN *:   PAHCS1
ACQUIRED:  12/3/94  16:23:24
PROCESSED: 12/3/94
                         RT
        RRT
Area
                   INSTRUMENT: W
                   OPERATOR:   MPA
RRF
Naphthalene
2-MethylnaphthaJene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
BenzotaJanthracene
Chrysene
Benzo(b) f luoranthene
Benzofklfluoranthene
Benzolelpyrene
Benzo(a)pyrene
Perylene
IndenoM ,2,3-c,d)pyrene
Oibenzo(a,h)anthracene
Benzole, h,i)perylene
dg-Naphthalene
dg-Acenaphthylene
d10- Acenaphthene
d10-Fluorene
d10-Phenanthrene
d10-Fluoranthene
d 1 2-Benzo|a)anthracene
d12-Chrysene
d12-Benzo|b)fluoranthene
d 1 2-BenzoIk)f luoranthene
d12-Benzo|a)pyrene
d 1 2-ln
-------
                                       FIGURE 14B

                    EXAMPLE OF INITIAL CALIBRATION (ICAL) RRF SUMMARY
     CALIFORNIA AIR RESOURCES BOARD METHOD 429 POLYCYCLIC AROMATIC HYDROCARBONS
ICAL ID; ST1120
RUN #: NA


Naphthalene
2-Methylnaphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chn/sene
Benzo(b)f!uoranthene
Benzo(tc)fluoranthene
Benzolelpyrene
Benzo(a)pyrene
Perylene
Indenod ,2,3-c,d)pYrene
Dibenzo(a,h)anthracene
Benzo(g,h,i)perylene
da-Naphthalene
d8-Acenaphthylene
d10- Acenaphthene
d10-Fluorene
d10-Phenanthrene
d10-Fluoranthene
d12-Benzo(a)anthracene
d12-Chrvsene
d12-Benzo(b)1luoranthene
d12-Benzo(k)fluoranthene
d ., 2-Benzo (a) py rene
d12-Indeno(1,2,3'C,d!pyrene
d1 4-Dibenzo(a,h)anthracene
d12-Benzo(g,h,i)perylene
d14-Terphenyl
d T 2-Benzo(e)py rene
ACQUIRED: 3-DEC-94
PROCESSED: 3-DEC-94
RRF#1

0,75
1.30
1.44
0.94
1.05
1.15
.02
.26
.31
.13
.13
1.69
1.24
1.20
1.07
0.70
2.19
1.66
2.23
4.22
1.29
1.32
0.93
0.82
1.03
0.75
0.82
1.35
1.95
1.91
0.92
0.87
0.80
0.52
0,37
RRF #2

0.66
1.15
1.27
0.84
0.94
1.06
1.00
1.15
1.27
1.05
1.02
1.45
1.25
1.12
0.99
0.63
2.01
1.60
2.05
4.15
1.29
1.34
0.95
0.82
1.00
0.70
0.79
1.39
1.95
1.96
0.88
0.84
0.76
0-52
0.37
RRF #3

0.61
1.10
1.24
0.80
0.88
1.01
0.98
1.08
1.13
1.05
0.97
1.46
1.14
1.06
0.96
0.58
1.92
1.56
1.96
4.16
1.28
1.32
0.94
0.82
1.07
0.70
0.81
1.46
2.14
2.11
0.98
0.91
0.83
0.49
0.37
RRF #4

0.64
1.12
1.28
0.83
0.92
1.05
0.95
1.13
1.15
1.04
0.98
1.42
1.18
1.06
0.96
0.60
1.99
1.61
2.00
4.18
1.27
1.30
0.95
0.86
1.07
0.72
0.83
1.27
1.84
1.82
0.85
0.78
0.73
0.48
0.36
RRF 05

0.71
1.26
1.43
0.94
1.07
1.23
1.14
1.28
.41
.23
.11
.86
.26
.19
.14
0.70
2.26
1.87
2.32
.4.10
1;30
1.32
0.95
0.88
0.99
0.70
0.84
1.32
2.11
1.99
0.98
0.89
0.80
0.51
0.36
INSTRUMENT: W
OPERATOR: MPA
Mean
RRF
0,67
1.19
1.33
0.87
0.97
1.10
1.02
1.18
1.25
1.10
1.04
1.58
1.21
1.12
1.02
0.64
2.07
1.66
2.11
4.16
1.29
1.32
0.94
0.81
1.03
0.71
0.82
1.36 '
2.00
1.96
0.92
0.86
0.78
0.51
0.36
SD

0.056
0.089
0.096
0.067
0.082
0.088
0.074
0.085
0.115
0.082
0.073
0.194
0.052
0.066
0.080
0.059
0.143
0,122
0.154
0.044
0.012
0.013
0.011
0.026
0.038
0.022
0.021
0.072
0.124
0.107
0.059
0.049
0,042
0,018
0.005
%RSD

8,29%
7.47%
7.19%
7.72%
8.43%
8.00%
7.25%
7.21 %
9.22%
7.43%
7.00%
12.33%
4.32%
5.89%
7.81%
9.12%
6.90%
7.35%
7.28%
1.05%
0.91%
1.00%
1.21%
3,09%
3.71 %
3.09%
2.56%
5.32%
6.23%
5.46%
6.40%
5.71%
5.36%
3,59%
1,50%
d10-Anthracene

d, 0-2-Methylnaphthalene
d,0-Pyrene
d,2-Perylene
0.69
0.73
0.74
0.80
0.90
0.77    0.080    10.40%
 August 9, 1996
                                      Proposed M-429 Page 110

-------
                                         FIGURE 14C

                   EXAMPLE OF CONTINUING CALIBRATION (CONCAL) SUMMARY
     CALIFORNIA AIR RESOURCES BOARD METHOD 429 POLYCYCLIC AROMATIC HYDROCARBONS
CONCAL ID:
CONCAL DATE:
CC1202              ICALID:     ST1120
12/3/94              ICALDATE:  3-DEC-94

               RRF    ICAL RRF    ARRF
                                                           RPD
                                   INSTRUMENT:  W
                                   OPERATOR:    MPA
  Naphthalene
  2-Methylnaphthalene
  Acenaphthylane
  Acenaphthene
  Fluorene
  Phenanthrene
  Anthracene
  Fluoranthene
  Pyrene
  Benzo(a]anthracene
  Chrysene
  Ben zo |b)f luoranthene
  Benzo(k)fluoranthene
  Benzolelpyrene
  Benzolajpyrene
  Perylene
  lndeno(l,2,3-c,d)pyrene
  Dibenzola,h)anthracene
  flenzo|g,h,i|perylene

  dg-Naphthalene
  dg-Acenaphthylene
  d10- Acenaphthene
  d10-Fluorene
  d10-Phenanthrene
  d10-Fluoranthene
  d, 2-B enzolalanthracene
  d12-Chrysena
  du-Benzo(b)f!uoranthene
  d, 2-Benzo(k)fluoranthene
  d12-Benzo(a)pyrene
  d12-IndenoU,2(3-c,d)pyrene
  d]4-Dibenzo(a,h|anthracene
  d,2-Benzo(g,h,i)perylene

  d,4-Terphenyl
  d]2-Benzo(e)pyrene

  d10-Anthracene

  d10-2-Methylnaphthalene
  d10-Pyrene
  d12-Perylene
0.68
1.42
1,42
0.91
0.98
1.10
0.98
1.12
1.18
1.08
1.04
1.46
1.12
1.04
0.95
0.62
2.04
1.61
2.11
4.78
1.20
1.25
0.85
0.79
1.05
0.69
0,82
1.24
1.91
1.87
0.84
0.80
0.76
0.50
0.37
0.67
1.19
1.33
0,87
0.97
1.10
1.02
1.18
1.25
1.10
1.04
1.58
1.21
1.12
1.02
0.64
2.07
1.66
2.11
1.16
1.29
1.32
0.94
0.81
1.03
0.71
O.82
1.36
2.00
1.96
0.92
0.86
0.78
0.51
0.36
0.01
0.23
0.09
0.04
0.01
0.00
-0.04
-0.06
-0.07
-0.02
0.00
-0.12
-0.09
-0.08
-0.07
-0.02
-0.03
-0.05
0,00
0.68
-0.09
-0.07
-0.09
-0.02
0.02
-0.02
0,00
-0.12
-0.09
-0.09
-0.08
-0,06
-0.02
-0.01
0.01
1.5
17.6
6.6
4.5
1.0
0.0
4.0
5.2
5.8
1.8
0.0
7.9
7.7
7.4
7.1
3.2
1.5
3.1
0.0
15.3
7.2
5.5
10.1
2.5
1.9
2.9
0.0
9.2
4.6
4.7
9.1
7.2
2.6
2.0
2.7
0.71
                         0.77
          1.000
          1.000
-0.06
8.1
 Augusts, 1996
                                    Proposed M-429 Page 111

-------
                                           FIGURE 15 A.
                          EXAMPLE OF SUMMARY REPORT OF LCS RESULTS
       CALIFORNIA AIR RESOURCES BOARD METHOD 429 POLYCYCLIC AROMATIC HYDROCARBONS
Client ID  GARB
Lab ID: 14129/LCS1/LCS2
Instrument:  W	
Operator:   MPA	
Reviewer:    JCM	

           COMPOUND:
  Naphthalene
  2-Methylnaphthalene
  Acenaphthylene
  Acenaphthene
  Ruorene
  Phenanthrene
  Anthracene
  Fluoranthene
  Pyrene
  Benzo(a)anthracene
  Chrysene
  Benzo[b)flucranthene
  Benzo(k)1Iuoranthene
  Benzo(e)pyrene
  Benzo[a)pyrene
  Perylene
  lndeno[1,2,3-c,d)pyrene
  Dibenzo[a,h)anthracene
  Benzol8,h.i)perylene
  Internal Standards (%R)
  d8-Naphthalene
  d B-Acena phthy lene
  d10- Acenaphthene
  d10-Fluorene
  d10-Phenanthrene
  d10-Fluoranthene
  d 12-Benzo(a)anthracene
  d12-Chrysene
  dl2-Benzo(b)fIuoranthene
  d12-Benzo(k)fluoranthene
  d12-Benzo(a)pyrene
  d l2-lndeno(1,2,3-c,d)pyrene
  d 14-Dibenzo[a,h)anthracene
  d12-Benzo{g,h,ilperylene

  Alternate Standard (%R)
  d,0-Anthracene
Sample Matrix: XAD-2
Date Received:   NA
Date Extracted:  1 1/30/94
d: 12/3/94
nt: Sampjg
LCS1
%R
100
96
95
92
94
93
91
90
87
87
83
92
92
97
89
89
87
88
89
67
73
75
79
88
84
96
96
88
85
92
104
96
102
CONC
Units;
LCS2
%R
103
95
97
94
96
94
89
92
89
86
89
93
95
99
92
89
90
90
91
64
70
75
81
93
80
98
91
85
84
90
105
96
103
ICAL ID;  ST112Q
ICAL DATE:
CONCAL ID:
12/3/94
 NA
                                         NA
                                  NA
                                       RPD
                                         3.0
                                         1.0
                                         2.1
                                         2.2
                                         2.1
                                         1.1
                                         2.2
                                         2.2
                                         2.3
                                         1.2
                                         7.0
                                         1.1
                                         3.2
                                         2.0
                                         3.3
                                         0.0
                                         3.4
                                         2.2
                                         1.2
Resin Lot #: LC1130M
LCS IDs:  NA
LCS DATE:  NA
              83
 85
 Augusts, 1996
                                         Proposed M-429 Page 112

-------
•§
I
<0
CO

CO
        FIGURE 15B

LCS RECOVERIES FOR BENZO(a}PYRENE
o
T3
O
to
to


3"
CO
o
             150


             140
             120



            o5 110



            o 100
            03


           ^  90


               80


               70
               50
                                  _^1
                                        C5
\
                                                 I J
         8/18/92-5/21/93

-------
                                    FIGURE ISA
              EXAMPLE GC/MS SUMMARY REPORT (HRMSI FOR SAMPLE RUN #32
   CALIFORNIA AIR RESOURCES BOARD METHOD 429 POLYCYCLIC AROMATIC HYDROCARBONS
Lab ID:  14129-02
Acquired:  12/3/94  16:23:40
Client ID: M429-32
ICALID: 12/3/94  16:23:40
1CALDATE: 12/3/94
                          RT
   RRT
Area
Naphthalene
2-Methyl naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo{a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo[e)pyrene
Benzotalpyrene
Peryiene
Indenoll ^.S-c.dlpyrene
Dibenzo(a,h)anthracene
Benzo[g,h,iiperylene
tig-Naphthalene
d6-Acenaphthylene
d10-Acenaphthene
d10-Fluorene
d10-Phenanthrene
d10-Fluoranthene
d12-Benzo(a)anthracene
d^-Chrysene
d12-Benzo(b)fIuoranthene
d12-Benzo(kSfiuoranthene
di2-Benzo[a]pyrene
d12-lndeno|1,2,3-c,d)pyrene
d14-Dibenzola,h)anthracene
d12*Benzo(g,h,i)peryIene
d14-Terphenyl
d12-Benzo(elpyrene
d10-Anthracene
d10-2-Methylnaphthalene
d10-Pyrene
d15-Pervlena
8:21
9:41
11:03
11:19
12:05
13:17
13:21
14:36
14:52
16:32
16:32
18:49
Not found
19:36
19:46
20:01
23:54
23:56
25:09
8:13
11:01
11:16
12:02
13:16
14:34
16:28
16:31
18:45
18:50
19:41
23:46
23:45
24:60
14:55
19:32
13:20
9:38
14:51
19:56



















1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1,000

1.000
1.000
1.000
1.000
1.000
1.053 E+10
1.790E + 08
9.371 E + 08
7.649 E + 06
2.417 £ + 07
8. 402 E + 08
2.905 E + 07
5.932 E + 08
7.611 E + 08
3.120E + 06
9.620 E + 06
1.030 E + 06
0.0
1.646 E + 07
4.936 E + 06
1.823 E + 06
5. 728 E + 06
5.875 E + 05
1.584 E + 07
4.794 E + 08
1,972 E + 08
2.1 42 E + 08
1.658 E + 08
1.652 E + 07
3.955 E + 08
2.835 E + 08
2.987 E + 08
3.439 E + 08
4.304 E + 08
4.895 E + 08
2.529 E + 08
2.400 E + 08
2.006 E + 08
7.988 E + 08
3.011 E + 08
6.795 E + 07
1,844 E + 07
6. 576 E + 08
3.057 E + 08

RRF
0.67
1.19
1.33
0.87
0.97
1.10
1.02
1.18
1.25
1.10
1.04
1.58
1.21
1.12
1.02
0.64
2.07
1.66
2.11
1.16
1.29
1.32
0.94
0.81
1.03
0.71
0.82
1.36
2.00
1.96
0.92
0.86
0.78
0.51
0.36
0.77
...
...
...
Instrument:
Operator:
Reviewer;
Amt. (ngj
10,478.37
140.98
712.59
8.21
30.02
925.53
34.54
254.36
307.62
1.9
6.2
7.6

13.61
3.95
2.32
4.37
0.59
14.95
124.92
1 66.07
176.19
190.71
213.39
116.22
121.18
111.08
165.79
1 41 .02
163.67
179.71
182.65
167.24
523
676.33
95.29
100
100
100
W
MPA
JCM
%REC



















62.5
83.0
88.1
95.4
106.7
58.1
60.6
55.5
41.4
35.3
40.9
44.9
45.7
41.8
105
135.3
47.6



August 9, 1996
                          Proposed M-429 Page 114

-------
                                           FIGURE 168

               EXAMPLE LABORATORY REPORT OF PAH RESULTS FOR SAMPLE RUN #32
      CALIFORNIA AIR RESOURCES BOARD METHOD 429 POLYCYCLIC AROMATIC HYDROCARBONS
Client ID  M429-32
Lab ID:  14129^02,
Instrument:   W
Operator:   MPA
Reviewer:    JCM
         COMPOUND:
Sample Matrix: M429      ICAL ID:  ST1120
Date Received:  14/18^34  ICAL DATE:  12/3/94
Date Extracted:  11/30/94  CONCALID:   NA
Date Analyzed: 12/3/94
Sample amount: Sample

             Cone.                R.L.
         CONCALDATE:   N
         Units:   no/sampla
                                Resin Lot #:  LCI 13QM
                                LCS IDs: 14129-LCS1/LCS2
                                LCS DATE: _ 12/3/94
                                             Flags
Naphthalene
2-Melhylnaphtha!ene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b) fluoranthene
Benzo(k)fluoranthene
Benzo
-------
                                            FIGURE 17A
                    EXAMPLE OF TESTER'S SUMMARY OF LABORATORY REPORTS
Run #;

31
32
33
Field
Blank
Method
Blank
ng/sampla
Naphthalene j 4300
2-Methylnaphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fluaranthene
Benzo (k)f luaranthene
Benzofeipyrene
Benzo{a)pyrene
Perylene
IndenoU ,2,3-c,dSpyrene
Dibenzo(a,h)anthracene
8enzQ(g,h,ilpervlene
Internal Standards (%RI
d8-Naphthalene
d8-Aoenaphthylene
d^-Acenaphthene
d10-Fluorene
d10-Phenanthrene
d10-Fluoranthene
d12-BBnzo{a)anthracBne
d12-Chrysene
d12-Benzo(b)fluorantnene
d12"Benzo(k)fluoranthene
< 94
140
9.2
27
310
»,JL...
83
110
< 5,0
< 5.0
< 5.0
< 5.0
35
< 5.0
< 5.0
< 5.0
< 5.0
"" < 85

66
82
85
91
106*
79
100
91
69
62
d12-Benzo(a)pyrene f 70
d12-Indeno(1,2,3-c,d)pyrene f 82
d14-Dibenzoia,h)anthracene I 72
d1z-Benzo(g,h,i!perylene ] 84
Surrogate Standards (%RI
d14-Terphenyl
dtz-Benzo(e)pyrene
Alternate Standard |%R|
d|0-Anthracene

125
72

67
10000 !460000 *
140
710
8.2
30
930
„,....!!...„..
250
310
< 5.0
6.2
7.6"
< 5.0
< 35
< 5.0
< 5.0
< 5.0
< 5.0
< 85

62
83
88
95
107
58
61
56
41 H
35 H
41 H
45 H
6400 *
85000 *
500
180
43000 *
2400"
16000 •
20000 *
170
300
340
89
530
240
110
100
8.4
440

57 •
85 *
80 *
102
79 »
75 *
108
99
60
50
58
58
42 H 58
45 H I 58
•:-'--:.ti:-:j-,-T:, ; •.--.
105
135

48 H
TestDate |1 1/15/94 h 1/16/94 |

90
112

115
11/17/94 i
<1600
< 94
9.1
< 5.0
< 27
< 80
5.3
16
19
< 5.6
< 5.0
< 5.0
< 5.0
6.9
< 5.0
< 5.0
< 5.0
< 5.0
17.0

53
73
81
90
107
83
114
102
85
78
86
106
<1700
<78
< 5.0
< 5,0
< 27
< 74
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0
< 5,0
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0
< 5.0
"" < 5.0

55
?9
75
82
93
80
93
88
84
84
89
106
92 92
107 I
..+-.<• :
123
103

116
11/16/94
LCS »\
LCS #2
percent recovery
100
96
95
92"
94
93
91
90
87
87
83
92
92
97
89
89
*87
88
89

67
73
76
79
88
84
96
96
88
85
92
103
95
97
94
96
94
89
92
""""89 ""'"
86
89 ~* "
93
95
99
92
89
90
90
91
' V ' ,'*' 'U
64
70
75
IT
93
80
98
91
85
84
90
104 | 105
96 !
104 | 102 I

130
112

101
NA




83
NA j
96
._.„._.„.
, , •



85
NA
Date received by lab. |Tl/i 8/94 ill/1 8/94 ffl/ 18/94 jli/Ti/94 JNA JNA }NA~
Date extracted 1 11/30/94 ]1 1/30/94 H 1/30/94 1 11/30794 j 11730/94 11/30^4] 11/30/94
Date analyzed 1 12/3794 1 12/3/94 1 12/3794 712/3/94 {12/3/94 |l273/9"4 112/3794
*<" denotes that the compound was not detected at levels above the indicated reporting limit.
"H" indicates internal Standard Recovery Results below 50%, but signal-to-noise greater than 10:1.
" *" indicates compounds reanalyzed at 1:50 dilution due to saturation.
  August 9, 1996
Proposed M-429  Page 116

-------
                                  FIGURE 178
                   FIELD DATA SUMMARY FOR PAH EMISSIONS TEST
RUN ID
DATE
STAflT/STOP TIME
LOCATION
STACK DIAMETER
NOZZLE DIAMETER
METER BOX ID
STANDARD DRY GAS VOLUME Vm((,dl
vm

AH.VB
T
KT
Y
PERCENT MOISTURE Bwl
Impinger + tare
Final wt.
Net imp. catch
Silica gel tare
Post sampling wt.
Moisture gain
Total moisture IV]
Vwltid
v k^
K2
MOLECULAR WEIGHT Md
M.

CO
CO2
N2

GAS VELOCITY v.
Ap
T.
Pg
P.
M.
KP

VOLUMETRIC FLOW RATE Q,td
&vn
vp
A
sec/min
Kl
ISOKINETIC RATIO I
T.

P.""""
v.
e
B
*r

31
1t -15-95
1016/1436
STACK
36.5 in.
0.3105
6419
146.19
132,66
29,78
1.15
60.0
17.64
1.08
12.9
2183.3
2509.8
426.6
1561.8
1690.0
28.2
c) 464.7
21.43
146.19
0.0471
29.93
28.40
11.25
O.OO
9.26
79.5O
12.86
38.4
0.530
420
-0.27
29.76
28.40
86.49
0.83
8241
12.86
38.38
6.8736
60
17.64
96
420
146.19
29.76
38.38
240
12.86
0.00053
0.09460
32
11-16-35
1020/1646
STACK
36.6 in.
0.313 in.
6419
235.67
213.67
29.98
1.36
60.0
17.64
1.08
16.0
2092.3
2934.9
842.6
1788.8
1826.9
38.1
88O.7
41.50
236.57
0.0471
29.95
28.16
10.76
0.00
9.60
79.76
14.98
4O.88
0.66
428
-0.27
29.96
28.16
85.49
O.83
8631
14.98
40.88
6.8736
60
17,64
99
428
236.57
29.96
40.88
360
14.98
O.OO063
0.09460
33
11-17-95


0855/1525
STACK
36.5 in.


0.3125 in.
6419
260.76
228.10
29.88
1.66
60.0
17.64
1.08
18.4
2063
3210.2
1147.2
1585.7
1636.2
49.6
1196.7
66.39
260.76
0.0471
30.08
27.86
10.00
0.00
1O.60
79.50
18.36
43.2
0.59
427
-0.27
29.86
27.86
85.49
0.83
8641
18.36
43.23
6.8736
60
17.64
104
427
250.76
29.86
43.23
360
18.36
0.00063
O.09460

DSCF(68° F)
cubic ft
Inches Hg
inches H20
°F


p ere ant
grams
grams
grams
grams
grams
grams
grams
DSCF(68" F)
DSCF(68e F)

Ib/lbmole
Ib/lbmole
percent
percent
percent
percent
percent
feet/second
inches HZ0
"F
inches H20
inches Hg
Ib/lbmole


oscFtea0 n
percent
feet/second
sq. feet


percent
°F
DSCFM|68° Ft
inches Hg
feat/second
minutes
percent
sq. feet

August 9, 1996
Proposed M-429  Page 117

-------
                                      FIGURE 17C

                          EXAMPLE OF EMISSIONS TEST REPORT

(ng/dscm)
Naphthalene
2-Methyinaphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fiuoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthena
BenzolWfluoranthene
Benzotejpyrene
Benzolalpyrene
Perytene
Indenol 1 ,2,3-e,d)pyrene
Dibenzo(a,h)anthracene
Benzolg.h.ijperylene

'••• -"-f^:" •x^£:Cng/sec|-.v :;;.
Naphthalene
2-MethylnaphthaIene
Acenaph thy I ene
Acenaphthene ~~" "*"""'
Fluorene
Phenanthrene
Anthracene
Fiuoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo{b)fluoranthene
Benzofklfluoranthene
Benzo(e)pyrene
Benzolalpyrene
Perylene
Indenod ,2,3-c,dJpyrene
Dibenzo(a,h}anthracene
Benzotg.ruSperylene
Run #31

I 1046
I <23
34
2.2
6.6
75
<6.3
20
27
<1.2
<1.2
<1.2
<1.2
„„,.„._„,..._
<^""2""
<1.2
<1.2
<1.2
<21


4068
<89
132
"""""""""O
26
293
<25
79
104
<4.7
<4.7
<4.7
<4.7
<33
<4.7
<4,7
<4.7
<4.7
<80
Run #32

1499
21 .0
106
1.2
4.5
139
5.3
38
47
<0.75
0.92
i.i
<0.75
„.„„,„„..„_,„„„.„..
__..._„.,
<0.75
<6.75
<0.75
<13


6036
85
429
,__
18
561
21
151
187
<3.0
3.7
4.6
<3.6
<21
<3.6
<3.0
<3.6
<3.0
<51
Run #33

64782
901
11971
70
25
6056
338
2253
2817
24
42
48
13
....... ™. „..>..
"34
16
14
0.90
62

' i =
264180
3676
48816
"""""""287
103
24695
1378
9189
11488
99
172
195
51
304
138
63
57
3.7
253
Standard Conditions: 68 deg.F (20 deg.C) & 29.92 in. Hg. (760 mm Hg)
" <"  indicates that the compound was not detected above the reporting limit.
August 9, 1996
Proposed M-429 Page 118

-------
                             METHOD 429 - APPENDIX A

                 DETERMINATION OF THE METHOD DETECTION LIMIT

 This procedure is based on the approach adopted by the EPA and included as Appendix B
 to Title 40, Part 136 of the Code of Federal Regulations (40 CFR 136).  The samples shall
 be subjected to the same extraction, concentration, cleanup, and analytical procedures as
 those required for the field samples.

 A1       Procedure

          A1.1   Make an estimate of the detection limit (MDL) of each target compound
                 using one of the following;

                 (a)  The concentration value that corresponds to an instrument
                     signal/noise ratio in the range of 2.5 to 5.

                 (b)  The concentration equivalent of three times the standard deviation
                     of replicate instrumental measurements of the analyte in reagent
                     methylene chloride.

                 (c)  That region of the standard curve where there is a significant
                     change in sensitivity, i.e., a break in the slope of the standard curve,

                 (d)  Instrumental limitations.

                 (e)  The concentration equivalent to five times the theoretical
                     quantitation limit (Section 8.3.1 of the test method)

             The experience of the analyst is important to this process, but one of the
             above considerations must be included in the initial estimate of the detection
             limit.                      /

         A1.2  Prepare according to the procedures described in Sections 4.2.2.1 to
                4.2.2.4 enough XAD-2 resin to provide, at a minimum, eight aliquots
                each with mass equal to that required to pack a Method 429 sorbent
                cartridge. A contamination check must be conducted to identify those
                PAH for which a MDL cannot be determined by this method.

         A1.3  To each of seven (7) aliquots of the clean resin, add an amount of each
                target analyte equal to the estimated detection limit. The mass of each
                resin aliquot must be  known, and should be approximately 40 grams, the
                amount required to pack a Method 429 sorbent cartridge.  The eighth
                aliquot shall be a blank.

         A1.4   Process each of the eight samples through the entire PAH analytical
                method. All quality criteria requirements of the analytical method must
                be satisfied,
August 9, 1996                                            Proposed M-429 Page 119

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         A1.5   Report the analytical results. The laboratory report must satisfy all of the
                reporting requirements of Section 10 of the test method.

         A1.6   It may be economically and technically desirable to evaluate the
                estimated method detection limit before proceeding with step A1.3. This
                will: (1) prevent repeating this entire procedure and (2) insure that the
                procedure is being conducted at the correct concentration.  It is quite
                possible that an inflated MDL will be calculated from data obtained at
                many times the real MDL even though the level of analyte is less than
             '   five times the calculated method detection limit. To insure  a good
                estimate of the method detection, it is necessary to determine that a
                lower concentration of analyte will not result in a significantly lower
                method detection limit. Take two aliquots of the sample to be used to
                calculate the method detection limit and process each through the entire
                method, including blank measurements as described above in  step A1.3.
                Evaluate these data:

                (1)  If the sample levels are in a desirable range for determination of the
                    MDL, take five additional aliquots and proceed.  Use all seven
                    measurements for calculation of the MDL according to Section A2.

                (2)  If these measurements indicate the selected analyte level is not in
                    correct range, reestimate the MDL with a new sample  as in A1.2
                    and repeat steps A1.3 to A1.5.
A2      Calculation
         A2.1   Calculate the variance (S2) and standard deviation (S) of the replicate
                measurements, as follows:
                                                             429-(AM34)
            Where:
                i = 1 to n, are the analytical results in the final method reporting units
                obtained from the n sample aliqouts and £ refers to the sum of the X
                values from i = 1 to n.
August 9, 1996                                            Proposed M-429 Page 120

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         A2.2  (a)   Compute the MDL as follows:


                           MDL  » t(n_,. T^ .0.99) X  (S)          429(A)-(35)

                Where:

                     MDL = the method detection limit

                     t(n.T T^ _ 0 99j = Students" t-value appropriate for a 99%
                     confidence level and a standard deviation estimate with n-1 degrees
                     of freedom. See Table 429(A)-1.

                     S = standard deviation of the replicate analyses,

                (b)   The 95% confidence interval estimates for the MDL derived in
                     A2,2(a) are computed according to the following equations derived
                     from percentiles of the chi square over degrees of freedom
                     distribution (x2/df).

                                 LCL = 0.64 MDL
                                 UCL = 2,20 MDL

                     where:       LCL and UCL are the lower and upper 95%  confidence
                                 limits  respectively based on seven aliquots.

A3      Optional Iterative Procedure

         A3.1   This is to verify  the reasonableness of the estimate of the MDL and
                subsequent MDL determinations.

                (a)   If this is the initial attempt to compute MDL based on the  estimate
                     of MDL formulated in Step A1.1, take the MDL as calculated in Step
                     A2.2, spike the matrix at this calculated MDL and repeat the
                     procedure starting with Step A1.3.

                (b)   If this is the second or later iteration of the MDL calculation, use S2
                     from the current MDL calculation and S2 from the previous MDL
                     calculation  to compute the F-ratio.  The F-ratio is calculated by
                     substituting the larger S2 into the numerator S2A and the other into
                     the denominator S B. The computed F-ratio is then compared with
                     the F-ratio found in the table which is 3.05 as follows: if
                     S2A/S2B<3.05, then compute the pooled standard deviation by the
                     following equation:
                                           2 .  fic:2
                                           A +6SB
                                            12
                              429{A)-(36)
          DE> » + nt»r,
Spooled =
August 9, 1996                                           Proposed M-429 Page 121

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               if S2A/S2B>3.05, respike at the most recent calculated MDL and process
               the samples through the procedure starting with Step A1.3. If the most
               recent calculated MDL does not permit qualitative identification when
               samples are spiked at that level, report the MDL as a concentration
               between the current and previous MDL which permits qualitative
               identification.

               (c)   Use the Spo0|ed as calculated in Equation 429(A)-3 to compute the
                    final MDL according to the following equation;


                              MDL =2.681 (Spited)              429(A)-(37)


               Where:  2.681 is equal to t(12( i^ - .99).

               (d)   The 95% confidence limits for MDL calculated using Equation
                    429(A)-4 are computed according to the following equations derived
                    from percentiles of the chi squared over degrees of freedom
                    distribution.

                                LCL = 0.72 MDL
                                UCL =  1.65 MDL

               where LCL and UCL are the lower and upper 95% confidence limits
               respectively based on 14 aliquots.
                                 TABLE 429(A)-1

      SELECTED STUDENT'S t VALUES AT THE 99 PERCENT CONFIDENCE LEVEL
                                                       ' '   V
Number of
Replicates

7
8
9
10
11
16
21
26
31
61
Degrees
of Freedom
(n-1)
6
7
8
9
10
15
20
25
30
60


Vl, ,99)
3.143
2.998
2.896
2.821
2.764
2.602
2.528
2.485
2.457
2.390
August 9, 1996                                          Proposed M-429 Page 122

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FORMULA: Table 1

H.W.: Table 1
  POLYNUCLEAR AROMATIC HYDROCARBONS
  ,                       __    .    HETHOD.  5506
                                    ISSUED:  5/15/85
OSHA: proposed for B[a]P:  0.2 jig/m3
ACGIH: suspect carcinogen  (B[a]P)
 PROPERTIES: Table 1
COMPOUNDS:  acenaphthene
            acenaphthylene
            anthracene
            benz[a]anthracene
            benzo[b]f1uoranthene
  	    benzo[k]f1uoranthene
benzotghiIperylene
benzo[a]pyrene
benzo[e]pyrene  .- "
chrysene
dibenz[a,tr]anthracene
fluoranthene	
nuorene
indeno[l,2,3-cd]pyrene
naphthalene
phenanthrene
pyrene
SYNONYMS: PAH; PNAi also see Table 2.
                    SAMPLING
                        MEASUREMENT
SAMPLER: FILTER * SORBENT
         (2-ym, 37-nra PTFE +• washed XAO-2,
         100 mg/50 mg)

FLOW RATE: 2 L/min

VOL-HIN:  200 L
   -MAX: 1000 L

SHIPMENT: transfer filters to culture tubes;
          wrap sorbent and culture tubes in
          A1 foil; ship @ 0 °C

SAMPLE STABILITY: unknown; protect from
                  heat and UV radiation
    !METHOD: HPLCt FLUORESCENCE/UV DETECTION
    i
    i.ANALYTE: compounds above
    i
    SEXTRACTION: 5 mL organic solvent appropriate  to
    !            sample matrix (step 7)
    i
    !COLUMN: 15 on x 4.6 mm, reverse phase, 5-ytn C\Q
    i
    !INJECTION VOLUME: 10 to 50 yL
    i
    !MOBILE PHASE: H20/CH3CN gradient @  ambient
    !              temperature

    !FLCW RATE: 1.0 mL/min
FIELD BLANKS: 10% (>3) of sanples
MEDIA BLANKS: 6 to 10

AREA SAMPLES: 8 replicates on preweighed
              filters for solvent selection
	ACCURACY	

RANGE STUDIED, BIAS, AND OVERALL
PRECISION (sr): not measured
    'DETECTORS: UV 9 254 ran;  fluorescence @ 340 ran
    !           (excitation), 425 nm (emission)
    i
    iCALIBRATION: external  standards in CH3CN
    i
    •RANGE, LOD AND PRECISION (sr):  EVALUATION OF
    i                               METHOD
APPLICABILITY:  The working range for B[a]P is  1  to 50  vg/m3 for a 400-L  air sanple.
Specific sample sets may require modification in  filter extraction solvent, choice of
measurement method, and measurement conditions  {see EVALUATION OF HETHOD).	
INTERFERENCES:  Any compound which elutes at the  same HPLC retention time may interfere.  Heat,
ozone, N02, or UV light may cause sample degradation,

OTHER METHODS:This revises P4CAM 206 and 251  [1],The spectrophotometric methods.P&CAM 184
and 186 [1]. have not been revised.  Also see Method 5515 (GC).
5/15/85
 5506-1

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POIYMUCLEAR AROMATIC HYDROCARBONS
                                          METHOD:   5506
REAGENTS:
1. Filter extraction solvent:
   benzene,* cyclohexane, methylene
   chloride, or other appropriate
   solvents, pesticide grade
   grade (step 7).
2. Water, distilled, deionized.
   degassed.
3. Acetonitrile. HPLC grade, degassed.
4. PAH reference standards,*
   appropriate to the PAH-containing
   matrix sampled.
5. Calibration stock solution,
   0.25 mg/mL.*  Check purity of each
   PAH reference standard by GC/FID,
   HPLC/fluorescence and/or melting
   point.   Purify,  if necessary, by
   recrystallization.  Weigh 25 mg
   of each  PAH into a 100-fflL volumetric
   flask; dilute to volume with
   acetonitrile.  Stable six months
   if refrigerated  and protected
   from light.
    *See SPECIAL PRECAUTIONS.
EQUIPMENT:
 1. Sampler:
    a. Filter.  PTFE-1 aminated membrane filter, 2-in
       pore size, 37-mn diameter (ZEFLOUR, Hembrana,
       Pleasanton, CA or equivalent), backed by a
       gasket (37-mn 00, 32-flm ID) cut from a cellulose
       support pad, In cassette filter holder.
       NOTE 1: If sampling is to be done in bright
               sunlight, use opaque or foil-wrapped
               cassettes to prevent sample degradation.
       NOTE 2: Take filters to be preweighed from the
               filter package and allow to equilibrate
               24 hrs Kith laboratory atmosphere before
               taring.
    b. Sorbent tube, connected to filter with minimum
       length PVC tubing.  Plastic caps are required
       after sanpling.  Washed XAO-2 resin (front =
       100 mg; back = 50 mg)  (Supelco ORBO 43 or
       equivalent).  Pressure drop at 2 L/min airflow
       1.6  to 2  kPa  (15 to 20 cm H^).
 2. Personal sampling pump capable of operating for
    8 hrs at 2 L/min, with flexible connecting tubing.
 3. Aluminum  foil.
 4. Vial, scintillation, 20-mL, glass, PTFE-lined cap.
 5. Refrigerant, bagged.
 6. Culture tubes, PTFE-lined screw cap,  13-rnn x
     100-mn.
 7. Forceps.
 B. Filters, 0.45-um, PTFE or nylon  (for filtering
    sample  solutions).
 9. Pipet,  5-rtt.
 10. Syringe or micropipets.  I-  to  100-vL.
 11. Ultrasonic bath.
 12. HPLC, with gradient  capability,  fluorescence
     (excitation  @ 240 nm,  emission @ 425  nm)  and UV
     (254 nm)  detectors in  series, electronic
     integrator,  and  column [HC-ODS-SILX  (Perkin-Elmer
    Corp.), Vydac  201TP  (The Separations  Group) or
    equivalent;  see  page 5506-1],
 13.  Volumetric flasks,  10- and  100-mL.
 14.  Lighting  in  laboratory:   incandescent or
     UV-shielded  fluorescent.
 15.  Kuderna-Danish extractor.
 SPECIAL PRECAUTIONS:  Treat benzene and all polynuclear aromatic hydrocarbons as carcinogens.
 Neat compounds should be weighed in a glove box.   Spent samples and unused standards are toxic
 waste.  Regularly check counter tops and equipment with 'black light" for fluorescence as an
 indicator of contamination by PAH.
 5/15/85
    5506-2

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HETHOO:  5506	POLYNUCLEAR AROMATIC HYDROCARBONS

SAMPLING:
 1. Calibrate each personal sampling pump with a representative sampler in line.
 2. Take personal samples at 2 L/min for a total sample size of 200 to 1000 L.  Take a
    concurrent set of eight replicate area samples at 2 to 4 L/min on preweighed, 2-pm PTFE
    filters in an area of highest expected PAH concentration.
    NOTE: The area samples are needed for solvent selection (step 7).
 3. Immediately after sampling, transfer the filter carefully with forceps to a scintillation
    vial.  Hold filter at edge to avoid disturbing the deposit.  Cap the scintillation vial  and
    wrap it in aluminum foil.
    NOTE: This step is necessary to avoid loss of analytes due to sublimation and degradation
          by light.
 4. Cap the sorbent tube and wrap it in aluminum foil.
 5. Ship to laboratory in insulated container with bagged refrigerant.

SAMPLE PREPARATION:
NOTE: UV light may degrade PAH.  Use yellow, UV-absorbing shields for fluorescent lights or use
      incandescent lighting,
 6. Refrigerate samples upon receipt at laboratory.
 7. Determine optimum extraction solvent.
    a. Allow the preweighed area filter samples to equilibrate 24 hrs with the laboratory
       atmosphere.
    b. Weigh the area filters.  Determine total weight collected on each.
    c. Extract the first pair of area filters with acetonitrile, the second with benzene, the
       third with cyclohexane, and the fourth with methylene chloride, according to step 8.
       NOTE: Use alternate solvents, if appropriate.  PAH of interest may be entrained within,
             and adsorbed by, particulate matter collected on the filter.  It is necessary to
             determine the solvent which maximizes recovery of the PAH from each sample
             matrix.  For example, methylene chloride [2,3] and benzenerethanol  (4:1 v/v) [4]
             have been recommended for extraction of PAH from diesel exhaust particulate.
    d. Analyze the extracts for the PAH of interest (steps 10 through 18).  Normalize the total
       mass of PAH found to the mass of sample collected.
    e. Choose the solvent which gives the highest recovery of PAH of interest.  Use the solvent
       chosen to extract the personal filter samples.
 8. Extract filters.
    a. Add 5.0 ml of the solvent chosen in step 7 to each scintillation vial containing a
       filter.  Start media and reagent blanks at this step.
    b. Cap and let sit 15 to 20 min in an ultrasonic bath,
       NOTE 1: SoxhTet extraction may be required when large amounts of highly adsorptive
               particulate matter (e.g., fly ash or diesel soot) are present.
       NOTE 2: The sample must be dissolved in acetonitrile for chromatography.  If needed,
               perform solvent exchange as follows:
               CAUTION: To avoid loss of volatile components, do not allow the sample to go to
                        dryness at any time.
               (1) After filtration (step 10), take the sample to near dryness in a
                   Kuderna-Danish extractor.
               (2) Add ca. 1 mL acetonitrile, take to near dryness, and adjust final volume to
                   1.0 mL with acetonitrile and filter again.
 9, Desorb PAH from sorbent.
    a. Score each sorbent tube with a file in front of the front (larger) sorbent section.
       Break tube at score line.
5/15/85                                     5506-3

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POLYNUCLEAR AROMATIC HYDjg3CARBpNS	METHOD:  5506

    b.  Transfer glass wool  plug and  front sorbent section to a culture  tube.   Discard  the foam
       plug.  Transfer back sorbent  section to a second culture tube.
    c.  Add 5.0 ml acetonitrile to each culture tube.   Cap the culture  tubes.
    d.  Allow samples to sit for 30 min.  Swirl occasionally.
10. Filter all sample extracts through an 0.45-ym membrane filter.

CALIBRATION AND QUALITY CONTROL:
11. Calibrate daily with at least five working standards.
    a.  Dilute aliquots of calibration stock solution with acetonitrile in 10-mL volumetric
       flasks (e.g., to 2.5. 0.5, 0.1, 0.02, and 0,002 ug/mL).
    b.  Intersperse working standards and samples in the measurements.
    c.  Prepare calibration graphs (peak area vs. vg of each PAH per sample).
12. Recovery and desorption efficiency.
    a.  Determine recovery  (R) from filters and desorption efficiency (DE) from sorbent tubes at
       least once for each lot of filters and sorbent tubes used in the range of interest.
       (1) Filters.  Using a microliter syringe or micropipette, spike four filters at each of
           five concentration levels with a mixture of the analytes.  Allow the filters to dry
            in the dark overnight.  Analyze the filters (steps 8, 10, and 14 through 16.
           Prepare graphs of R vs. amounts found.
           NOTE: This step may not be used for some highly adsorptive parti oil ate matrices for
                 which calibration by the method of standard additions may be more accurate.
       (2) Sorbent tubes.  Transfer an unused front sorbent section to a culture tube.  Prepare
           a  total of 24 culture tubes in order to measure DE at five concentration levels plus
           blanks in quadruplicate.  Using a microliter syringe or micropipette, add
            calibration stock solution directly to sorbent.  Cap culture tubes and allow to
            stand overnight.  Analyze  (steps 9,  10, and 14 through 16).  Prepare graphs of DE
           vs. amounts found.
    b. Check  R and DE at two levels for each sample set, in duplicate.  Repeat determination of
       R and  DE graphs if  checks do not agree to within +51 of DE graph.
13. Analyze at least three field blanks for each sample medium.

MEASUREMENT:                                   {
14. Set HPLC  according to manufacturer's recommendations and to conditions on page 5506-1.
    Equilibrate column at  601 CHgCN/W H20 at  1.0 mL/min for  15 min before injecting first
    sample.
15. Inject  sample aliquot.  Start mobile phase gradient:
    a. Linear gradient 601 CHjCN to 1001 CJ^CN, 20 min.
    b. Hold at 1001 CHsCN  for 20 min.
       NOTE:  Hold longer if necessary to prevent carryover of background, e.g., from coal  dust.
    c. Linear gradient to  initial condition, 5 min.
16. Measure peak areas.
    NOTE 1: Approximate retention times appear  in Table 3.
    NOTE 2: If peak area is above the calibration range, dilute with appropriate solvent,
            reanalyze, and apply dilution factor in calculations.
    NOTE 3: If sample has many  interferences, additional sample cleanup may be necessary.   Many
            cleanup procedures  have been published.  Liquid-liquid partitioning between
            cyclohexane and nitromethane [5,6]  is widely used, but other techniques may be more
            appropriate for specific samples.
 5/15/85                                     5506-4

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METHOD:  5506 _ POLYHUCIEAR AROMATIC HYDROCARBONS

CALCULATIONS:
17. Read the mass, tig  (corrected for R or DE) of each analyte found on the filter (W) and
    front sorbent  [Wf) and back sorbent (WQ) sections, and on the average media blank
    filter (B) and front sorbent (Bf) and back sorbent (B^) sections from the calibration
    graphs.
18. Calculate concentration, C (ug/m3),  in  air  as  the sum of the particulate concentration
    and the vapor concentration using the actual air volume sampled, V (L) .
                          C .
    NOTE: Wf and V^,  include analyte originally collected on the filter as particulate, then
          volatilized during sampling.  This can be a significant fraction for many PAH (e.g.,
          fluoran thane, naphthalene, fluorene, anthracene, phenanthrene) .

EVALUATION OF METHOD:
The fluorescence detector used in this method is both sensitive and selective.  The detector
can "see" as little  as 50 pg of many PAH injected on the column.  LOOs for the 17 analytes
range from 50 to 350 ng per sample.  It does not respond to non-fluorescent molecules such as
aliphatics.  The method is, therefore, most amenable to determination of trace amounts of PAH
in mixtures of aliphatic compounds.  Successful applications include:  aluminum reduction
facilities, asphalt  fume, coal gasification plants, coal liquefaction plants, coal tar pitch,
coke oven emissions, creosote treatment facilities, diesel exhaust, graphite electrode
manufacturing, petroleum pitch, and roofing tearoff operations.

This method has been evaluated by analyzing spiked filters, spiked sorbent tubes, and complete
spiked sampling trains through which were drawn 500 L of air [7].  Each of the three groups was
spiked with each analyte at two concentration levels in sextuplicate.  Particular note should
be made that the effect of particulate matter has not been evaluated, and every sampling matrix
is unique.  The data on the following page were obtained on spiked samplers stored refrigerated
in the dark for three months followed by measurement with HPLC.
5/15/85                                     5506-5

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                                                                                  METHOD:  5506
CALIBRATION RANGE (u

1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
COMPOUND
ACENAPHTHENE
ACENAPHTHYLENE
ANTHRACENE
BENZ[a]ANTHRACENE
B£NZO[b]FLUORANTHENE
BENZO[k]FLLJORANTHENE
BENZO[ghi]PERYLENE
BENZO[a]PYRENE
BENZO[e]PYRENE
CHRYSENE
DIBENZ[a,h]ANTHRACENE
FLUORANTHENE
FLUORENE
INDENO[1 ,2,3~cd]PYRENE
NAPHTHALENE
PHENANTHRENE
PYRENE
(yg per sample)
2.
1.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0
0
4
4
4
4
5
4
5
4
5
4
7
5
6
0.4
0.5
- 13
- 100
- 13
- 13
- 12
- 13
- 25
- 14
- 13
- 12
- 25
- 13
- 13
- 12
- 13
- 13
- 13
LOO
g per
sample)
0.
0.
0.
0.
0.
0.
0.
8
35
05
15
1
15
2
0.2
0.
0.
0.
0.
0.
0.
0.
2
15
2
15
25
2
25
0.1
0.2
MEASUREMENT PRECISION
SPIKED +
SPIKED* AIR1*
.058 S .093
.032 S .075
.039 S .037
.032
.027
.025
.031
.027
(0
.039
.026
.084
.028
.027
.029
.029
(50)
(100)
(5)
(S)
(10)
(1)
(10)
(5)
(c)
.024
.029
.026 S .050
.031 S .090
.044 F .032
.041 S .125
.036 S .070
(5)
(10)
(10)
(10)
(10)
(50)
(2)
(c) (c)
aRSD for filter (F) where volatilization is nil  or for sorbent (S) where substantial
 volatilization may occur during sampling.
bR5D determined at the yg level shown in parenthesis for a spiked filter followed by a
 sorbent tube.  After spiking, laboratory air was drawn through the sampling train at 2 L/min
 for 4 hrs.
cNot determined.

REFERENCES:
 [1] NIOSH Manual of Analytical Methods, 2nd ed.. Vol.  1,  U.S. Department of Health,  Education,
     and Welfare, Publ. (NIOSH) 77-157-A (1977).
 [2] Breuer, 6. H.  Anal. Lett.. Jl(All), 1293-1306 (1984).
 [3] Zweidinger, R. 8., S. B. Tejada, D. Dropkins, 0.  Huisingh, and L. Claxton.   "Characteriza-
     tion of Extractable Organics in Diesel Exhaust Particulate," paper presented at  Symposium
     on Diesel Particulate Emissions Measurement Characterization, Ann Arbor, HI (1978).
 [4] Swarin, S. 0. and R. L. Williams.  "Liquid Chromatographic Determination of Benzo[a]pyrene
     in Diesel Exhaust Particulate:  Verification of the Collection and Analytical  Methods,"
     Polvnuclear Aromatic HydrocarbQns:   Physical and Biqioflical Effects. Bjorseth, A.  and
     Dennis, Eds., Battelle Press, 771-790 (1980).
 [5] Wise, S. A., et al_.  "Analytical Methods for the Determination of Polycyclic Aromatic
     Hydrocarbons on Air Particulate Matter," Polynuclear  Aromatic Hydrocarbons;  Physical and
     Biological Chemistry. Cooke, Dennis and Fisher, Eds., Battelle Press, 919-929 (1982).
 [6] Novotny, H., H. L. Lee and K. D. Bartle,  J. Chromatog.  Sci.. J2., 606-612 (1974).
 [7] Backup Data Report for Method 5506, Analytical Report for NIOSH Sequence 4170 (NIOSH,
     unpublished. March 16, 1984).
 [8] Studt., P., Liebias Ann. Chem.. 528 (1978).
 [9] Clar, E.  Polj^yclk Hydrocarbons.  Academic Press (1964).
[10] Handbook of Chemistry and Physics.  62nd ed,, CRC Press  (1982).

METHOD REVISED BY:  B. R. Bel inky and E. J. Slick, NIOSH/DPSE.
5/15/85
5506-6

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METHOD:  5506
                                POLYNUCLEAR AROMATIC HYDROCARBONS
Table 1. Formulae and physical properties.

COMPOUND (by M.H.)
1. NAPHTHALENE
2. ACEMAPHTHYLENE
3. ACENAPHTHENE
4. FLUORENE
5. ANTHRACENE
6. PHENANTHRENE
7. FLUORANTHENE
8. PYRENE
9. BENZ[a]ANTHRACENE
10. CHRYSENE
11. BENZO[b]FLUORANTHENE
12. BENZO[k]FLUORANTHENE
13. BENZO[a]PYRENE
14. BEMZO[e]PYRENE
15. BENZO[ghi]PERYLENE
16. INDENO[l,2,3-cd3PYRENE
17. DIBENZ[a,h]ANTHRACENE
EMPIRICAL
FORMULA
CIOHB
Cl2"8
^12^10
Cl3H10
Ci4H10
C14H10
Cl6H10
Cl6«10
C18H12
C18H12
C20H12
C20"12
C20H12
C20H12
C22"12
C22H12
C22H14
MOLECULAR
WEIGHT
128.17
152.20
154.21
166.22
178.23
178.23
202.26
202.26
228.29
228.29
252.32
252.32
252.32
252.32
276.34
276.34
278.35

DETECTOR
UV
UV
UV
UV
UV
UV
FL
FL
FL
UV
FL
FL
FL
FL
FL
FL
FL
MELTING
POINT
(°C)
80
92-93
96.2
116
218
100
110
156
158-159
255-256
168
217
177
178-179
273
161.5-163
262
BOILING
POINT
("O*
218
265-275
279
293-295
340
340
_
399
—
—
—
480
—
—
—
—
-—


REF.
[9]
CIO]
[10]
t9]
[9]
[9]
[93
[93
[9]
[93
[93
[103
[93
[93
[93
[83
[93
*Hany of these compounds will sublime.
Table 2.  Synonyms.

 COMPOUND (alphabet!cal1y)

 1. ACENAPHTHENE
 2. ACENAPHTHYLENE
 3. ANTHRACENE
 4. BEN2[a]ANTHRAC£NE

 5. BENZO[b]FLUORANTHENE

 6. BENZO[k3FLUORANTHENE
 7. BENZO[ghi3PERYLENE
 8. BENZO[a3PYRENE
 9. BENZO[e3PYRENE
10. CHRYSENE
11. DIBENZ[a,h]ANTHRACENE
12. FLUORANTHENE
13. FLUORENE
14. INDENO[1.2,3-cd]PYRENE
15. NAPHTHALENE
16. PHENANTHRENE
17. PYRENE
                            SYNONYMS
CAS# 83-32-9
CAS# 208-96-8
CAS# 120-12-7
1,2-benzanthracene; benzo[b]phenanthrene; 2.3-benzophenanthrene;
tetraphene; CAS# 56-55-3
3,4-benzofluoranthene; 2>3-ben20fluoranthene;
benz[e]acephenanthrylcne; B[b]F; CAS# 205-99-2
11,12-benzofluoranthene; CAS* 207-08-9
1,12-benzoperylene; CASf 191-24-2
3,4-benzopyrene; 6,7-benzopyrene;-B[a3P; BP; CAS# 50-32-8
1,2-benzopyrene; 4,5-benzopyrene; B[e]P; CAS# 192-97-2
1,2-benzophenanthrene; benzo[a]phenanthrene; CAS# 218-01-9
1,2,5,6-dibenzanthracene; CAS» 53-70-3
benzo[jk]f1uorene; CAS# 206-44-0
CASff 86-73-7
2,3-phenylenepyrene; CAS# 193-39-5
naphthene; CAS* 91-20-3
CAS# 85-01-8
benzo[def]phenanthrerw; CAS# 129-00-0
5715/85
             5506-7

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POLYNUCIEAR AROMATIC HYDROCARBONS
                                      METHOD:   5506
Table 3.  Approximate PAH retention times.

             	COMPOUND	

              1. NAPHTHALENE

              2. ACENAPHTHALENE

              3. ACENAPHTHENE

              4. FLUORENE

              S. PHENANTHRENE

              6. ANTHRACENE

              7. FLUQRANTHENE

              8. PYREHE

              9. BENZ[a]ANTHRACENE

              10. CHRYSENE

              11. BENZO[e)PYRENE

              12. BENZO[b]FLUORANTHENE

              13. BENZOtk]FlUQRANTHENE

              14. BENZO[a]PYREHE

              15. OIBENZ[a,h]ANTHRACENE

              16. BENZO[ghi]PERYlENE


              17. INDENOn,2,3-cd]PYRENE
               RETEMT10N TIHE (nrin)*

                        2.4

                        2.8

                        3.6

                        3.9

                        4.7

                        5.8

                        6.8

                        7.7

                        11.2

                        12.1

                        14.0

                        14.8

                        16.5

                        17.3

                        20.0

                        20.0

                        2K2
 *NOTE:  Determined with a Perkin-Elmer HC-OOS-SILX column.  Actual retention times will vary
        with  individual columns and  column age.
 5/15/85
5506-8

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METHOD;  5506
                   POLYNUCLEAR AROHATIC HYDROCARBONS
 ACENAPHTHENE
   ACENAPHTHYLENE
ANTHRACENE
 BENZODANTHRACENE   BENZOCb)FLUORANTHENE BENZODOFLUORANTHENE
 BENZOCgh HPERYLENE   BENZOCcOPYRENE
    CHRYSENE
DfBENZCo,»OANTHRACENE
    FLUORENE
INDENOCI.2.3-C
   PHENANTHRENE
        PYRENE
Figure 1.  Structures of PAH.
                           BENZOQOPYRENE
FLUORANTHENE
 NAPHTHALENE
5/15/85
       5506-9

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TECHNICAL REPORT DATA
Please read instructions on the reverse before completing
I. REPORT NO. 2,
EPA-454/R-99-OOIC
4. TITLE AND SUBTITLE
Final Report - Emissions Testing of Combustion Stack and Pushing Operations at Coke
Battery No, 2 at Bethlehem Stee! Corporation's Bums Harbor Division in Chesterton, Indiana
Volume III of 111
7. AUTHOR(S)
Franklin Meadows
Daniel F. Scheffel
9, PERFORMING ORGANIZATION NAME AND ADDRESS
Pacific Environmental Services, Inc.
Post Office Box 1 2077
Research Triangle Park, North Carolina 27709-2077
12, SPONSORING AGENCY NAME AND ADDRESS
U.S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Emissions, Monitoring and Analysis Division
Research Triangle Park, North Carolina 277 1 1
3. RECIPIENT'S ACCESSION NO.
5. REPORT DATE
February 1999
6. PERFORMING ORGANIZATION CODE
8. PERFORMING ORGANIZATION REPORT NO.
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-D-9S-004
13. TYPE OF REPORT AND PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
  16. ABSTRACT

     The United States Environmental Protection Agency (EPA) is investigating the coke making industry to characterize hazardous air pollutants (HAPs)
  emitted from coke pushing operations and combustion (underfire) stacks. This test report addresses pushing emissions from a coke oven, and emissions
  from the combustion (underfire) stack that serves Coke Battery No. 2 at Bethlehem Steel Corporation's Burns Harbor Division in Chesterton, Indiana.
  The purpose of this test program was to quantify emissions from the inlet and outlet of the baghouse controlling emissions from the coke pushing
  operation and to quantify emissions from the combustion outlet stack. The data may be used by the EPA in the future to support a residual risk
  assessment for coke oven facilities.

     The testing was performed to quantify uncontrolled and controlled air emissions of filterable particulate matter (PM), methyiene chloride extractable
  matter (MCEM) and 19 polycyclic aromatic hydrocarbons (PAHs) including acenaphthene, acenaphthylene, anthracene, benzo(a)anthracene,
  benzo(a)pyrene, benzo(b)fiuoranthene, benzo(e)pyrene, benzo(k)fluoranthene, benzo(ghi)perylene, chrysene, dibenzo(a,h)anthracene, fluoranthene,
  fluorene, indeno(l,2,3-cd)pyrene, 2-methylnaptha!ene, napthalene, perylen«, phenanthrene, and pyrene. In addition, following the PM and MCEM
  analyses, the samples were analyzed to screen for the presence of 17 trace metals, Baghouse dust samples were also collected and analyzed for 16 trace
  metals. Simultaneous testing was performed at the inlet and outlet of the baghouse controlling emissions from the coke pushing operation. Sampling
  was also performed on the combustion outlet stack. In addition to pollutant testing, oxygen (02) and carbon dioxide (COj) were measured at each
  location. During the sampling program, Research Triangle Institute (RTJ), another EPA contractor, monitored and recorded process and emission
  control system operating parameters.

     This volume (Volume III) is comprised of 363 pages and includes Appendices: D (Calculations), E (QA/QC Data), F (Participants),
  and G (Sampling and Analytical Procedures).
1 7. KEY WORDS AND DOCUMENT ANALYSIS
a. DESCRIPTIONS
Baghouse
Coke Ovens
Emission Measurements
Hazardous Air Pollutants
Metals
Methylene Chloride Extractable
Matter
Particulate Matter
Polycyclic Aromatic Hydrocarbons
1 8. DISTRIBUTION STATEMENT
Unlimited
b. IDENTIFIERS/OPEN ENDED TERMS

19. SECURITY CLASS (This Report)
Unclassified
20. SECURITY CLASS (This page)
Unclassified
c. COAST1 Field/Group

21. NO. OF PAGES
960
22. PRICE
EPA Form 2220-1 (Rev. 4-77)   PREVIOUS EDITION IS OBSOLETE
F:\U\FMeadows\TRD.Frm\WI

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