Report  No.  77-CKO-ll
                                                       With Appendices
O
                                             FINAL REPORT

                                            WISCONSIN STEEL

                                           CHICAGO, ILLINOIS
                 UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
                             Office of Air and Waste Management
                         Office of Air Quality Planning and Standards
                               Emission Measurement Branch
                          Research Triangle Park. North Carolina

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                  FINAL REPORT
                       on
STACK EMISSION SAMPLING AT WISCONSIN STEEL COMPANY
        COKE OVEN PLANT, CHICAGO, ILLINOIS
                       to
          ENVIRONMENTAL PROTECTION AGENCY
        (Contract No. 68-02-1409, Task 50)
                       by
                   Paul R. Webb
                       and
                Richard E. Barrett
                 November 4, 1977
                     BATTELLE
               Columbus Laboratories
                  505 King Avenue
               Columbus, Ohio  43201

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                               CONTENTS

1.  Introduction 	  1
2.  Summary and Discussion of Results	3
         Polycyclic Organic Matter' (POM) in Gas Stream	3
         Total Fluorescence Results	3
         Analysis of Samples	4
         Wet Electrostatic Precipitator Water Samples	4
3.  Process Description (by EPA)	24
4.  Location of Sampling Points	25
         Inlet Sampling	25
         Outlet Sampling	25
5.  Sampling and Analytical Procedures	28  .
         POM Sampling and Analysis	28
                                                               •t
         Total Fluorescence	33
         Molecular Weight of Stack Gas	33
         Gaseous Hydrocarbons Sampling and Analysis	34
      f i
6.  References	" .35
Appendices                                                              .
         A.  Field and Laboratory Data Related to Polycyclic
             Organic Matter  (POM) Sampling	A-l
         B.  Complete Sampling Results with Sample Calculations.  .  . .B-l
         C.  Wet ESP Water Sample Log	C-l
         D.  Integrated Gas  Collection Log	D-l
         E.  Daily Activity  Log	E-l
         F.  Gaseous Emission Laboratory Results	F-l
         G.  POM Sampling and Analysis using the Special POM
             Sampling Train	G-l
                                  iii

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                               FIGURES     	


Number                                                           Page

  1       Inlet Stack Geometry Configuration 	   26

  2       Outlet Stack Geometry Configuration	27

  3       POM Sampling Trains	29

  4       Schematic of Wisconsin Steel Byproduct Coke Plant
            with Wet Electrostatic Precipitator	30

  5       POM Cleanup Schematic	32



                                TABLES


  1       Inlet Gas Sampling Results 	    6

  2       Outlet Gas Sampling Results	    7

  3       POM Concentrations in Inlet and Outlet Gas Streams .  .    8

  4       POM Emission Rates	12

  5       Coke Oven Effluent Analysis Results by Gas Chromatic-
            Mass Spectrophotometry 	   16

  6       WESP Effectiveness for Controlling POM Emissions
            at Wisconsin Steel Coke Oven	18

  7      - Total Fluorescence Results, POM Samples, Wisconsin
            Steel - Coke Oven	19

  8       Analysis of Gaseous Emissions from Wisconsin Steel
            Coke Oven Plant	21

  9       Quantity of POM Compounds found in Wisconsin Steel
            Coke Oven WESP Water Samples	22

 10       POM Concentrations in Wisconsin Steel Coke Oven
            WESP Water Samples	23
                                   iv

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                                  SECTION 1
                                 INTRODUCTION

     Emissions from the coke manufacturing industry are reported to contri-
bute significant amounts of particulate and carcinogenic compounds into the
atmosphere*- »'.  Wet electrostatic precipitators (WESP) are being used as a
control device for such emissions.  In an effort to determine the efficiency
of WESP units relative to the process emissions from the coke oven doors,  the
United States Environmental Protection Agency contracted with Battelle-Columbus
Laboratories and Clayton Environmental Consultants to measure the emissions
from coke oven door leaks at the inlet and outlet of the WESP units of
Wisconsin Steel coke oven plant, Chicago,  Illinois.
     Battelle-Columbus Laboratory personnel were responsible for sampling
and analyzing the WESP inlet and outlet gas streams to determine the con-
centrations of about 20 polycyclic organic matter (POM) compounds in these
streams.  POM samples were collected using a Method 5 sampling train modified
to include a Tenax-adsorbent column between the filter and the first impinger.
Gas chromatography-mass spectrometry (GC-MS) analyses were conducted at the
Battelle-Columbus Laboratories.  Also, stack emission gases from the inlet
and outlet were collected in Tedlar bags at a relatively slow rate over the
8-hour sampling period.  Evacuated-flask samples were collected from the gas
samples in the Tedlar bags, and the gases were analyzed for concentrations
of benzene and ethyne  (acetylene) by gas chromatography.
     Clayton Environmental Consultants personnel were responsible for the
measurement of particulate concentrations in the WESP inlet and outlet gas
streams, for determination of the C0_, 0?, and CO concentrations in the gases
collected in the Tedlar bags, for visible emissions observations, and for
the collection of WESP water samples from the inlet and outlet water supply.
In addition, Clayton included an XAD-2 adsorbent column in their sampling
train to collect organic vapors.  Battelle determined the benzene-soluble
organic catch in the XAD-2 columns and analyzed the water samples for POM
compounds.

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     The following sections of this  report  cover  the  summary  of  results,
process description and operation,  location of sampling  points,  and  sampling
and analytical procedures.   Field and laboratory  data and  calculations  are
presented in various appendices as  noted-
     Results of the work performed by Clayton and Battelle analyses  of
Clayton samples are reported in a separate report prepared by Clayton.

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                               SECTION 2
                    SUMMARY AND DISCUSSION OF RESULTS

     The inlet and outlet gas sampling data and results are summarized and -
presented in Tables 1 and 2 respectively.   Raw field and laboratory data are
presented in Appendix A.  Complete sampling results, including additional
support data and sample calculations, are  presented in Appendix B.

POLYCYCLIC ORGANIC MATTER (POM) IN GAS STREAM
     Tables 3 and 4 present results for emissions of selected POM species at
the wet ESP inlet and outlet in terms of concentrations and emission rates,
respectively.  Table 5 is a tabulation of  the actual POM content of the
individual samples.  For each run, the probe wash residue and filter catch
were combined for one analysis; the Tenax adsorbent catch was analysed sepa-
rately.  Hence, in Tables 3, 4, and 5, two values are presented for each sample;
one represents the probe wash and filter,  the other represents the adsorbent
column.  Pre-clean up and blank values are also presented. (The outlet pre-
clean up results for the probe-wash-plus-filter are abnormally high with no
explanation at this time.) For the most part, the data show relativity high
values at the precipitator inlet when compared to the outlet, as would be
    /
expected.
     Table 4 presents results on the effectiveness of the wet ESP for
controlling emissions of individual POM species.  The wet ESP was reasonably
effective (over 90 percent) in reducing POM emissions of all species except
naphthalene.
     Table 6 summarizes the effectiveness of the wet ESP for controlling total
POM emissions from the coke oven.  In Table 6, the sum of the POM emissions
in the inlet and outlet streams are computed, and the control device efficiency
is calcualted.  For three runs, the control device efficiency was moderately
high, 80.7 to 92.4 percent.  The low efficiency for Run 4 of 17.2 percent
(attributed to a high naphthalene value for the outlet adsorbent column sample),
reduced  the average efficiency to 69.0 percent.  Neglecting naphthalene,
WESP efficiencies for the four runs are 93.5, 95.5, 98.9 and 94.5; an average
of 95.6

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TOTAL FLUORESCENCE RESULTS
     Table 7 presents results of total fluorescence for the air emission
samples.  Also shown in Table 7 are the total POM values obtained by
summing values for all POM species reported in Table 5, and the ratio of
total fluorescence to the sum of POM values by GC-MS.   Reviewing these
results shows that the total fluorescence values were much higher than the
summation of the POM values; ranging from a value 8 times as high as the
GC-MS value to a value over 8000 times the GC-MS value.  It appears that
there were large quantities of fluorescent compounds present in these
samples beyond the specific POM compounds examined by GC-MS technique.
It is known that most complex organics (non-POM compounds as well as POMs)
fluoresce when excited over a broad range of wavelengths.  Apparently the
bands of excitation and emission wavelengths used for these measurements
were not sufficiently selective for the POM compounds of interest.  A
possible improvement in the total fluorescence precedure might be to excite
the sample over a broad range of wavelenths, as was done here, but to
develop a mask, or screen, for the emission measurement  that will selectively
pass fluorescence in the wavelengths of harmful POM's, but not pass  fluorescence
in other wavelengths.

ANALYSIS OF SAMPLES  '
     Grab (flask) samples were taken from the integrated gas (bag) samples,
which were collected during the particulate runs.  The flask samples were
analyzed for C0H0 and C,KL.  Table 8 is a tabulation of these data.  The
              2. i      bo
accuracy of the reported values is estimated to be - 20 percent.
     Inlet and outlet data indicate little difference with CJH9 concentra-
tions ranging from 5 to 15 ppm, by volume, and C,EL. concentrations ranging
from 1 to 5 ppm by volume.

WET ELECTROSTATIC PRECIPITATOR WATER SAMPLES
     Water samples were collected from the inlet and outlet of the ESP unit
and analyzed for POM constituents.  Table 9 is a tabulation of the results of
the analysis.  Unfortunately, the volume of the water samples was not

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measured before extraction, either by Clayton at the sampling site,  or by
Battelle preceding extraction.  Interviewing the Battelle staff that provided
the sample containers and transported the filled containers back to the
laboratory for analyses revealed that the samples were transported in 1-liter
bottles, and the bottles were 60 to 90 percent full.  Assuming that the
bottles were 75 percent full, POM concentrations were calculated; these values
are reported in Table 10.
     If the inlet and outlet water flow rates were known, it would be
desirable to compare values  for the POM removed from the gas stream with the
POM increase for the water stream.

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                            TABLE 1.  INLET GAS  SAMPLING RESULTS
                                      (Metric Units)
INLET  RFSULTS, HISCONSIM  STEEL  CO.
RUN NO.
TEST DATE
VOLUME OF SAS SAMPLED, NCM
PERCENT MOISTURE 3Y VOLUME
AVERAGE STACK TEMPERATURE, C
STACK VOLUMETRIC FLOW RATE, NCMM
STACK VOLUMETRIC FLOU RATE, CUM .
PERCENT ISO
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                       TABLE 2.  OUTLET GAS SAMPLING RESULTS
                                 (Metric Units)
OUTLET  RESULTS,  WISCONSIN ^
                                  C0.
RUN NO.
TEST DATE
VOLUME 0^ GAS SA^?L£D» NCM
PERCENT KOISTURc 3Y VOLU1£
N
AVERAGE STACK T£MP£^fiTUFE, r
STACK VOLUMETRIC FLOW *ATc, NCMM
STACK /OLUHET'.IC FLOW RATE, C"v.
PERCENT ISOKINETIC
1
5/1G
8.35
1.7
16
53 6b
51*55
33.9
2
5/11
«J.6i>
1.6
22
5359
5552
99.8
3
5/12
6.77
a.c
26
5318
5582
101.9
L
5/17
8.89
2.<*
25
5277
5564
104.1
AVERAGE

8.67
1.9
22
5330
5543
98.7
                                   (English Units
OUTLET  PESUi-TS,  WISCONSIN ST;uiL  COjL
RUK NO.
TEST DATE
VOLUME OF GAS SAMPLED, OSCP
PERCENT MOISTUP^ BY VOLUME
AVERAGE STACK TEMFF = ATURf , F
STACK VOLUfcTKIC FLOH RATE, OSCFM
STACK VOLUHL'T^IC FLOH KflTE, ACFM
PERCEMT ISOKINETIC
1
5/10
295.9
1.7
62
.9U226
.9o379
88.9
2
5/11
3J6.7
1.6
73
189998
196620
99.8
,
5/12
31G.7
2.C
79
158526
197d6i
1C1.9
i.
. 5/13
315.?
2.L
77
187C92
197963
1C4.1
..AVERAGE,
307.1
' 1.9'
73
188961
196511
98.7

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                                TABLE 3.  POM CONCENTRATIONS IN INLET AND OUTLET GAS STREAMS
                                                     RUN 1
RUN 2
      Naphthalene
      Fluoranthrene
      Pyrene

      Benz(c)phenanthrene
      Chrysene
      Benz(a)anthracene

oo     DImethylbenz(a)anthracene
      Benz fluoranthrenes
      Benz(a)pyrene

      Benz(e)pyrene
      Cholanthrene
      Indeno(1,2,3-cd)pyrene

      Dibenz anthracenes
      Dibenz acridine
      Dibenz carbazole

      Dibenz pyrene
      3-Methyl cholanthrene
INLET
Probe
Wash
plus
Filter
2.24
560.
377.
51.8
535.
535.
<0.05
497.
150.
246.
<0.05
135.
108.
<0.05
<0.05
137.
<0.05
Adsorbent
Column
49.2
17.1
10.6
-
1.64
2.97
0.345
0.585
0.221
• —
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
OUTLET
Probe
Wash
plus
Filter
2.68
7.54
4.31
0.108
0.503
1.68
<0.06
1.86
1.34
0.383
<0.06
2.04
1.92
<0.06
<0.06
1.80
<0.06
Adsorbent
Column
35.8
116.
50.3
0.539
5.16
6.47
0.06
3.25
—
1.77
<0.06
<0.06
<0.06
<0.06
<0.06
<0.06
<0.06
INLET
Probe
Wash
plus
Filter
600.
613.
393.
30.3
297.
286.
9.53
469.
129.
227.
<0.05
143.
158.
<0.05
<0.05
131.
<0.05
Adsorbent
Column
2450.
419.
291.
17.0
93.3
81.5
<0.05
1.19
0.343
0.064
<0.05
0.107
<0.05
<0.05
<0.05
<0.05
<0.05
OUTLET
Probe
Wash
plus
Filter
0.416
8.67
5.20
0.590
6.96
3.58
<0.06
2.60
-
2.29
<0.06
1.85
1.85
<0.06
<0.06
1.85
<0.06
Adsorbent
Column
1090.
81.2
35.0
0.925
3.25 -
3.01
.<0.06
1.63
0.486
—
<0.06
<0.06
<0.06
<0.06
<0.06
<0.06
<0.06

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                         TABLE  3.   POM CONCENTRATIONS  IN  INLET AND OUTLET GAS STREAMS  (continued)
                                               RUN 3
RUN 4
Naphthalene
Fluoranthrene
Pyrene

Benz(c)phenanthrene
Chrysene
Benz(a)anthracene

Dimethylbenz(a)anthracene
Benz fluoranthrenes
Benz(a)pyrene

Benz(e)pyrene
Cholanthrene
Indeno(1,2,3-cd)pyrene

Dibenz anthracenes
Dibenz acridine
Dibenz carbazole

Dibenz pyrene
3-Methyl cholanthrene
INLET
Probe
Wash
plus
Filter
525.
3120.
798.
38.1
322.
284.
3.81
755.
195.
625.
<0.05
242.
272.
-
—
217.
-
Adsorbent
Column
883.
310.
180.
25.2
40.5
27.9
<0.05
3.93
0.286
0.011
<0.05
<0.05
<0..05
<0.05 ,
<0.05
<0.05
<0.05
OUTLET
Probe
Wash
plus
Filter
-
6.84
3.76
0.034
0.593
0.570
<0.06
0.969
0.741
0.148
<0.06
1.48
<0.06
<0.06
<0.06
1.25
<0.06
Adsorbent
Column
1120.
38.7
21.2
0.205
4.46
4.33
<0.06
1.49
0.422
0.011
<0.06
<0.06
<0.06
<0.06
<0.06
<0.06
<0.06
INLET
Probe
Wash
plus
Filter
576.
587.
357.
29.6
263.
223.
<0.05
291.
89.0
146.
<0.05
84.1
84.6
<0.05
<0.05
82.1
<0.05
Adsorbent
Column
9.45
1.73
0.974
18.8
73.0
52.5
<0.05
0.877
0.758
_
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
<0.05
OUTLET
Probe
Wash
plus
Filter
_
9.79
2.81
2.09
0.584
0.787
<0.06
1.97
3.37
0.315
<0'.06
1.91
2.02
<0.06
<0.06
1.69
<0,06
Adsorbent
Column
2210.
49.3
32.4
0.675
5.52
5.29
<0.06
2.04
0.922
0.067
<0.06
0.911
<0.06
<0.06
<0.06
<0.06
<0 = 06

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                        TABLE 3.   POM CONCENTRATIONS IN INLET AND OUTLET GAS STREAMS (continued)
                                                               AVERAGES
Naphthalene
Fluoranthrene
Pyrene

Benz(c)phenanthrene
Chrysene
Benz(a)anthracene

Dimethylbenz(a)anthracene
Benz fluoranthrenes
Benz(a)pyrene

Benz(e)pyrene
Cholanthrene
Indeno(1,2,3-cd)pyrene

Dibenz anthracenes
Dibenz acridine
Dibenz carbazole

Dibenz pyrene
3-Methyl cholanthrene

Probe
Wash
plus
Filter
426.
1220.
481.
37.5
354.
332.
'•3K36
503.
:4i.
311.
<0.05
151.
156.
<0.05
<0.05
142.
<0.05
INLET
Adsorbent
Column
848.
187.
121.
15.3
52.1
41.2
••M«.i»
1.65
0.402
0.019
<0.05
°<02^0.06:
<0.05
<0.05
<0.05
<0.05
<0.05

Total
1270.
1410.
602.
52.8
406.
373.
3.43X
505.
141.
311.
<0.10
3 . 151.
156.
<0.10
<0.10
142.
<0.10

Probe
Wash
plus
Filter
0.77
8.21
4.02
0.710
2.16
1.65
<0.06
1.85
1.36
0.784
<0.06
1.82
l-^.«
<0.06
<0.06
1.65
<0.06
OUTLET
Adsorbent
Column
1110.
71.3
34.8
0.586
4.60
4.78
<0.06
2.10
0.458
0.462
<0.06
°-22%.273
<0.06
<0.06
<0.06
<0.06
<0.06

Total
1110.
79.5
38.8
1.30
6.76
6.43
<0.12
3.95
1.82
1.25
<0 . 12
2.0^
1.^
<0.12
<0.12
r.6^
<0.12

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                         Footnotes to TABLE 3.
1.  Units are nanograms/normal cubic meter.

2.  Solvent and adsorbent column blanks were subtracted from POM mass values
    before concentrations were calculated.   Blank values reported as "less
    than" values were treated as zero values for these calculations.

3.  All calculated values were rounded off  to 3 significant figures to avoid
    implying excessive accuracy.
                                   11

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                                         TABLE 4.  POM EMISSION  RATES
                                                RUN  1
RUN 2
Naphthalene
Fluoranthrene
Pyrene

Benz(c)phenanthrene
Chrysene
Benz(a)anthracene

Dimethylbenz(a)anthracene
Benz fluoranthrenes
Benz(a)pyrene

Benz(e)pyrene
Cholanthrene
Indeno(1,2,3-cd)pyrene

Dibenz anthracenes
Dibenz acridine
Dibenz carbazole

Dibenz pyrene
3-Methyl cholanthrene
TOTAL
INLET
Probe
Wash
plus
Filter
0.687
171
116
15.9
164
164
<0.02
152
45.9
75.4
<0.02
41.4
33.1
<0.02
<0.02
42.0
<0.02
1021.39
Adsorbent
Column
15.1
5.24
3.25
_ _
0.503
0.910
0.106
0.179
0.067
—
<0.02
<0.02
<0.02
<0.02
O.02
<0.02
<0.02
25.36
OUTLET
Probe
Wash
plus
Filter
0.863
2.43
1.39
0.034
0.164
0.541
<0.02
0.599
0.432
0.123
<0.02
0.657
0.618
<0.02
<0.02
0.579
<0.02
8.43
Adsorbent
Column
11.5
37.4
16.2
0.173
1.66
2.06
<0.02
1.04
—
0.570
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02'
<0.02
70.60
INLET
Probe
Wash
plus
Filter
183
186
120
9.22
90.3
87.0
2.89
142
39.2
69.0
<0.02
43.5
48.0
<0.02
<0.02
39.8
<0.02
1059.91
Adsorbent
Column
744
127
88.5
5.17
28.4
24.8
<0.02
0.362
0.104
0.020
<0.02
0.033
<0.02
<0.02
<0.02
<0.02
<0.02
1018.39
OUTLET
Probe
Wash
plus
F-f 1 fPr
0.134
2.79
1.67
0.190
.2.24
1.15
<0.02
0.836
—
• 0.736
<0.02
0.595
0.595
<0.02
<0.02
0.595
<0.02
11.53
Adsorbent
Column
350
26.1
11.3
0.297
1.04
0.965
<0.02
0.524
0.156
__
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
390.38

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                                  TABLE 4.  POM EMISSION RATES (Continued)
                                               RUN 3
                                                    RUN 4
Naphthalene
Fluoranthrene
Pyrene

Benz(c)phenanthrene
Chrysene
Benz(a)anthracene

Dimethylbenz(a)anthracene
Benz fluoranthrenes
Benz(a)pyrene

Benz(e)pyrene
Cholanthrene
Indeno(1,2,3-cd)pyrene

Dibenz anthracenes
Dibenz acridine
Dibenz carbazole

Dibenz pyrene
3-Methyl cholanthrene
INLET
Probe
Wash
plus
Filter
161
952
244
11.7
98.9
86.9
1.17
231
59.7
191
<0.02
74.1
83.3
__
—
66.4
—
Adsorbent
Column
270
95.2
55.1
7.71
12.4
8,54
<0.02
1.20
0.088
0.004
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
OUTLET
Probe
Wash
plus
Filter
—
2.18
1.20 ''
0.010
0.190
0.182
<0.02
0.310
0.236
0.048
<0.02
0.473
<0.02
<0.02
<0.02
0.399
<0.02
Adsorbent
Column
357
12.4
6.76
0.066
1.42
1.38
<0.02
0.475
0.134
0.004
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
INLET
Probe
Wash
plus
Filter
173
176
107
8.89
79.1
67.0
<0.02
87.5
26.8
43.9
<0.02
25.3
25.4
<0.02
<0.02
24.7
<0.02
Adsorbent
Column
2.84
0.520
0.293
5.65
22.0
15.8
<0.02
0.263
0.228
• —
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
<0.02
OUTLET
Probe
Wash
plus
Filter
—
3.10
0.889
0.662
0.185
0.249
<0.02
0.624
1.07
0.100
<0.02
0.605
0.640
<0.02
<0.02
0.535
<0.02
Adsorbent
Column
699
15.6
10.3
0.216
1.75
1.67
<0.02
0.645
0.292
0.021
<0.02
0.288
<0.02
<0.02
<0.02
<0.02
<0.02
                            2261.17
450.24
5.23
379.64
844.59
47.59
                                                                                                  8.66
                                                                     729.78

-------
TABLE 4.  POM EMISSION RATES (Continued)
           AVERAGES
Naphthalene
Fluoranthrene
Pyrene
Benz(c)phenanthrene
Chrysene
Benz (a) anthracene
Dime thy Ibenz (a) anthracene
Benz fluoranthrenes
Benz,(a) pyrene
Benz(e)pyrene
Cholanthrene
Indeno (1 , 2 , 3-cd) pyrene
Dibenz anthracenes
Dibenz acridine
Dibenz carbazole
Dibenz pyrene
3-Methyl cholanthrene

Probe
Wash
Plus
Filter
129
371
147
11.4
108
101
1.02/1.03
153
42.9
" 94.8
<0.02
46.1
47.5
<0.02
<0.02
43.2
<0.02
INLET
Adsorbent
Column
258
57
36.8
4.63
15.8
12.5
.028/. 043
0.501
0.122
0.006
<0.02
0.008/0.023
<0.02
<0.02
<0.02
<0.02
<0.02

Total
387
428
184
17.1
124
114
1.05/1.07
154
43.0
94.8
<0.04
46.1
47.5
<0.04
<0.04
43.2
<0.04

Probe
Wash
Plus
Filter
0.997
2.63
1.29
0.224
0.695
0.531
<0.02
0.592
0.435
0.252
<0.02
0.583
0.463/0.468
<0.02
<0.02
0.527
<0.02
OUTLET
Adsorbent
Column
354
22.9
11.1
0.188
1.47
1.52
<0.02
0.671
0.146
0.149
<0.02
0.072/0.087
<0.02
<0.02
<0.02
<0.02
<0.02

Total
355
25.5
12.4
0.412
2.17
2.05
<0.04
1.26
0.581
0.399
<0.04
0.655/0.670
LO. 48/0. 49
<0.04
<0.04
0.53/0.55
<0.04
Control Device
Efficiency, percent
.Inlet-Outlet 1QQ.
. ( Inlet X 100)
8.3
94.0
93.3
97.6
98.3
98.2
96.2/100
99.2
98.6
99.6
—
98.6
99.0
—
—
98.8
—

-------
                         Footnotes to TABLE 4.
1.   Units are milligrams/hour (corrected for blanks).

2.   All above values for specific POM's were rounded off to 3 significant
    figures or 3 decimal places to avoid implying excessive accuracy.
                                  15

-------
                                           TABLE  5.   COKE OVEN EFFLUENT ANALYSIS RESULTS BY GAS CHROMATIC-MASS SPECTROPHOTOMETRY
o>
Pro-Clean- Up
INLET
OUTLET
Run 1
INLET
OUTLET
Run 2
INLET
OUTLET
Naphthalene
Fluoranthene
Pyrene
Benz(c)phenanthreno-
Chrysene
Bcnz( a) anthracene
Dime thy Ibenz (ft) Anthracene
Benz fluoranthenea
Benz (a) pyrene
Benx(e) pyrene
Cholsnthrene
Indeno ( 1 , 2 , 3- cd ) py ten*
Dibenz anthracene
Dibenz scrldlne
Dibenz carbazole
Dibeaz pyrene
3-Methyl cholanthrena
TOTAL POM

5.0
3.3
1.5
<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
9.2
No tat
24
4,5
<0.5
•tO. 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
16.8
1, All
6474
9492
5487
183
7237
5240
<0.5
42
14
3
<0.5
<0.5
<0.5
<0.5
<0.5
<0,5
<0.5
34,149.5
6.1
1.4
0.4
<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
1.8
24
5844'
3927
543
5583
5583
<0.5
5193
1574
2569
«0.5
1404
1122
<0.5
<0.5
1430
<0.5
34,773.5
525
178
111
2.4
20
31
3.6
13
9,1
0
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
861.9
23
63
36
3.3.
9
14
<0.5
23
18.2
3.4
<0.5
17
16
<0.5
<0.5
15
<0.5
218.4
311
972
420
7.5
46
54
<0.5
34
1.3
15.2
<0.5
' <0,5
<0.5
<0.5
<0.5
<0.5
<0.5
1,834.8
5607
5727
3666
285
2775
2667
89
4389
1216
2117

-------
                     TABLE 5.  COKE OVEH EFFLUENT ANALYSIS RESULTS BY GAS CHROMATIC-HASS 8PECTROPHOTOMETRY  (Continued)
Run 3
INLET
OUTLET
Run 4
INLET
OUTLET
•
Naphthalene
Fluoranthena
Pyrene
Benz(c)phenanthren«
Chrysene
Benz (a) anthracene
Diiae thy Ibenz (a) Anthracene
Benz fluoranthenes
Benz(a)pyrene
•Benz(e)pyrene
Cholanthrene
Indeno(l,2,3-cd)pyreiia
Dibenz anthracena
Dibanz ccrldlne
Dibenz carbazole
Dibenz pyrene
3-Hethyl cholanthr«n«
4955
29454
7536
362
3049
2685
36
7134
1844
5902
<0.5
2286
2565


2046

8346
2928
1698
241
385
263
<0.5
44
9.5
<0.5
<0.5
<0.5
<0.5
<0.5
^0.5
<0.5
<0.5
0.5
60
33
2.7
10
5
<0.5
16
13.5
1.5
<0.5
13
<0.5
<0.5
<0.5
11
<0.5
9631
339
186
4,8
42
38
<0.5
20
10.5
<0.5
0.5
<0.5
<0.5
<0.5
"<0.5
<0.5
<0.5
5319
5427
3301
276
2435
2062
<0.5
2700
829
1346
<0.5
777
782
<0.5
<0.5
759
<0.5
• 99
16
9
177
679
485
<0.5
15
14
0
<0.5
<0.5
0.5
<0.5
0.5
<0.5
<0.5
0.5
87
25
21
10
7
<0.5
25
22
3
<0.5
17
18
0.5
<0.5
15
<0.5
19677
438
288
9.0
52
47
<0.5
25
15
1
<0.5
8.1
< 0.5
<0.5
<0.5
<0.5
<0.5
0.6
<0.5
0.5
2.4
4.8
0
<0.5
7.5
7.0
0.2
<0.5
<0.5
0.5
<0.5
<0.5
<0.5
<0.5
11.;
0.!
0.!
3.(
2.!
0
<0.!
6.5
6.J
0.4
<0.5
<0.5
0.5
<0.5
<0.5
<0.5
<0.5
TOTAL POM
                      69,851.5  13,883.5    143.8   10,440.1    25,990.5  1,462.3     228.1    20,528.4

-------
                                TABLE  6.  WESP EFFECTIVENESS FOR CONTROLLING POM
                                          EMISSIONS AT WISCONSIN STEEL  COKE OVEN
00

Run
Run 1
Run 2
Run 3
Run 4
Average

Sample
307-308
309
318-319
320
329-330
331
340-341
342

Inlet (a)
Total POM
Emissions ,tng/hr
1,021.39
25.36
1,046.75
1,059.91
1,018.30
2,078.30
2,261.17
450.24
2,711.41
844.59
47.59
892.18

Sample
310-311
312
321-322
323
332-333
334
343-344
345

(a)
Outlet Inlet-Outlet.
Total POM Inlet U
Emissions ,mg/hr
8.43
70.60
79.03 92.4
11.53
390.38
401.91 80.7
5.23
379.64
384.87 85.8
8.66
729.78
738.44 17.2
69.0

       (a)   Inlet  and  outlet values equal mean value obtained by summation of GC-MS  values  minus blanks for
            individual runs.

-------
TABLE 7.  TOTAL FLUORESCENCE RESULTS,  POM SAMPLES,
           WISCONSIN STEEL - COKE OVEN
                                          Summation
                                                             Ratio of
Run
Pre-
Clean-up
Pre
Clean-up
Pre-
Clean-up
Pre-
Clean-up
Run 1
Run 1
Run 1
Run 1
Run 2
Run 2
Run 2
Run 2
Run 3
Run 3
Run 3
Run 3
Sampling
Position
Inlet
Inlet
Outlet
Outlet
Inlet
Inlet
Outlet
Outlet
Inlet
Inlet
Outlet
Outlet
Inlet
Inlet
Outlet
Outlet
_ , c -„ .,„ iui-aj. r iuuicai-ciii-t:
Total of GC-MS _ . „,.,,
, / x „, „„„ , to Summation POM
Sample(a) Fluorescence, pg POM values, ng
Filterable
Adsorbent
Filterable
Adsorbent
Filterable
Adsorbent
Filterable
Adsorbent
Filterable
Adsorbent
Filterable
Adsorbent
Filterable
Adsorbent
Filterable
Adsorbent
301-2
303
304-5
306
307-8
309
310-11
312
318-9
320
321-2
323
329-3
331
332-3
334
85
27
11,205
90
35,100
69
92
765
31,500
4,356
171
89
16,650
14,400
117
652
9
28
34,181
7
68,977
893
1,134
1,861
34,435
31,326
327
10,540
69,874
13,915
165
10,471
.8-15.8
.5-35.0
.8-34,185.8
.9-13.9
.8-68,980.3
.1-896.6
.0-1,136.5
.- 1,865.
.- 34,437.
.- 31,329.5
.7-330.2
.-10,544.
.-69,874.5
.-13,919.
.7-169.2
.8-10,475.8
6,641.
850.
328.
8,257.
509.
77.
81.
411.
915.
139.
520.
8.
238.
1,035.
699.
62.
                     19

-------
                  TABLE 7.  TOTAL FLUORESCENCE RESULTS, POM SAMPLES,
                            WISCONSIN STEEL - COKE OVEN (Continued)
Run
Run 4
Run 4
Run 4
Run 4
Blank
Blank
Run 3
Run 3
Run 4
Run 4
Blank
Summation _ ,. .R*t.1° of
_ , . „ .. , c /-./- «c Total Fluorescence
Sampling Total of GC-MS .
Position Sample (a) Fluorescence, yg POM values, ng to 5>ummatlon P°M
Inlet Filterable 340-1
Inlet Adsorbent 342
Outlet Filterable 343-4
Outlet Adsorbent 345
Solvents 351-3
Adsorbent 355
Inlet XAD-2 Column .
Outlet XAD-2 Column
Inlet XAD-2 Column
Outlet XAD-2 Column
XAD-2 Column
20,250 26, 013. -26, 015. 5 778.
3,150 1,494. -1,498. 2,106.
256 250. -253. 1,018.
900 20,560.1-20,563.6 44.
45 20.1-27.5 1,891.
52 31.7-36.7 1,520.
6,750 Not applicable
440 »
675 »
755 »
52 •• •
(a)   Filterable = Probe and glassware washes plus filter
     Adsorbent =  Adsorbent column (Tenax)  extract
     XAD-2 Column = Extract from adsorbent column incorporated into particulate sampling
                    train to collect vapors for BSO determination.
                                         20

-------
                                      TABLE  8.   ANALYSIS OF GASEOUS EMISSIONS FROM

                                                WISCONSIN STEEL COKE OVEN PLANT
to
I-1
EPA Volume concentration, ppm
Run
1
1
2
2
3
3
Location
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Sampling
Period
5/10/77,
5/10/77,
5/11/77,
5/11/77,
5/12/77,
5/12/77,
1200-1930
1200-1930
1030-1900
1030-1900
0930-1830
0930-1830
Sample
Number
S77-002-316
S77-002-317
S77-112-327
S77-002-328
S77-002-338
S77-002-339
C2H2
10
10
5
9
10
15
C6H6
3
3
2
2
4
1
Emission Rates
C2
3.
3.
1.
3.
3.
5.
H2
30
47
64
12
30
16
, kg/hr
C6H6
2
3
1
2
3
1
.97
.12
.96
.08
.96
.03
      Blank, filtered air
<0.05
<0.05

-------
           TABLE 9.   QUANTITY OF'POM COMPOUNDS  FOUND IN WISCONSIN STEEL
                     COKE OVEN WESP WATER SAMPLES^
CONSTITUENT
Naphthalene
Flyoranthene
Pyrene
Benz (c) phenanthrene
Chrysene
Benz (a) anthracene
Dimethylbenz (a) anthracene
Benz fluoranthene
Benz(a)pyrene
Benz(e)pyrene
Cholanthrene
Indeno (1,2, 3-cd) pyrene
Dibenz • anthracenes
Dibenz acridine
Dibenz carbazole
Dibenz pyrene
3-Methyl cholanthrene
RUN
Inlet
Sample
No. 313
2.4
2.1
<0.5
<0.5
~ 5.1
0
<0.5
8.4
7.5
0
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
1
Outlet
Sample
No. 314
4.5
3.3
0.9
6.1
7.3
<0.5
<0.5
14
11
2
<0.5
<0.5
13
<0.5
<0.5
<0.5
<0.5
RUN
Inlet
Sample
No. 324
<0.5
<0.5
<0.5
1.8
2.7
0
<0.5
7.5
6.4
0.8
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
2
Outlet
Sample
No. 325
<0.5
5.1
2.7
2.4
3.4
4.7
<0.5
9.9
10
1
<0.5
<0.5
12
<0.5
<0.5 •
<0.5
0.5
RUN
Inlet
Sample
No. 335
<0.5
<0.5
<0.5
1.8
3.9
0
<0.5
7.8
7.5
0
<0.5
<0.5
9.6
<0.5
<0.5
<0.5
<0.5
3
Outlet
Sample
No. 336
1.5
<0.5
<0.5
3.7
2.3
0.7
<0.5
7.5
6.5
0.7
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
RUN
Inlet
Sample
No. 346
<0.5
<0.5
<0.5
3.3
3.6
2.7
<0.5
9.9
8.0
1.0
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
<0.5
4
Outlet
Sample
No. 347
0.6
<0.5
<0.5
3.3
3.2
0.1
<0.5
7.2
7.5
0
<0.5
<0.5
<0.5
<0.5 .
<0.5
<0.5
<0.5
NOTES:  (a)  All data are nanograms; <0.5 ng indicates presence of the compound was detected,
             but at level below 0.5 ng.

-------
                 TABLE 10.   POM CONCENTRATIONS  IN WISCONSIN  STEEL  COKE
                            OVEN WESP WATER SAMPLES^
RUN 1


CONSTITUENT
Naphthalene
Flyoranthene
Pyrene
Benz (c) phenanthrene
Chrysene
Benz(a)'anthracene
Dime thylbenz (a) anthracene
Benz fluoranthene
Benz(a)pyrene
Benz (e) pyrene
Cholanthrene
Indeno (1 , 2 , 3-cd) pyrene
Dibenz anthracenes
Dibenz acridine
Dibenz carbazole
Dibenz pyrene
3-Methyl cholanthrene
Inlet
Sample
No. 313
3.2
2.8
<0.7
<0.7
6.8
0
<0.7
11.2
10.0
0
<0.7
<0.7
<0.7
<0.7
<0.7
<0.7
<0.7
Outlet
Sample
No. 314
6.0
4.4
1.2
8.1
9.7
0.7
<0.7
18.7
14.7
2.7
<0.7
<0.7
17.3
<0.7
<0.7
<0.7
<0.7
RUN 2
Inlet
Sample
No. 324
<0.7
<0.7
<0.7
2.4
3.6
0
<0.7
10.0
8.5
1.1
<0.7
<0.7
<0.7
<0.7
<0.7
<0.7
<0.7
Outlet
Sample
No. 325
<0.7
6.8
3.6
3.2
4.5
6.3
<0.7
13.2
13.3
1.3
<0.7
<0.7
16.
<0.7
<0.7
<0.7
<0.7
RUN 3
Inlet
Sample
No. 335
<0.7
<0.7
<0.7
2.4
5.2
0
<0.7
10.4
10.0
0
<0.7
<0.7
12.8
<0.7
<0.7
<0.7
<0.7
Outlet
Sample
No. 336
2.0
<0.7
<0.7
4.9
3.1
0.9
<0.7
10.0
8.7
0.9
<0.7
<0.7
<0.7
<0.7
<0.7
<0.7
<0.7
RUN 4
Inlet
Sample
No. 346
<0.7
<0.7
<0.7
4.4
4.8
3.6
<0.7
13.2
10.7
1.3
<0.7
<0.7
<0.7
<0.7
<0.7
<0.7
<0.7
Outlet
Sample
No. 347
" 0.8"
<0.7
<0.7
4.4 .
4.3
0.1
<0.7
9.6
10.0
0
<0.7
<0.7
<0.7
<0.7
<0.7
<0.7
<0.7


Average w

Inlet
0.8-1.3
0.7-1.2
0 -0.7
2.3-2.5
5.1
0.9
<0.7
11.2
9.8
0.6
<0.7
<0.7
3.2-3.7
<0.7
<0.7
<0.7
<0.7

Outlet
2.2-2. 4
2.8-3.2
1.2-1.6
5.2
5.4
2.0
<0.7
12.9
11.7
1.2
<0.7
<0.7
8.3-8.7
<0.7
<0.7
<0.7
<0.7
POM
Pickup
in
(Outlet
-Inlet)
1.3
2.1
1.1
2.8
0.3
1.1
-
1.7
1.9
0.6
-
-
5.1
-
-
-
™"
                                          o           o
NOTES:  (a)  All data are micrograms/meter ;  <0.7 mg/m  indicates presence of the compound was
             detected, but at level below 0.7mg/m3.  Sample volumes were not measured but consisted
             of 60 to 90 percent full 1-liter.containers; a sample value of 0.750 i, was assumed for
             all samples.
        (b)  Where reported values are given  as "less than"; averages were calculated using values
             of 0.0 and 0.7.

        (c)  Where averages are reported as a range,  the midpoint of the range was used to calculate
             pickup of POM by water.

-------
                SECTION 3




PROCESS DESCRIPTION AND PROCESS OPERATION




         (To be inserted by EPA)
                     24

-------
                                 SECTION 4
                         LOCATION OF SAMPLING POINTS

     Sample port and point locations were determined as outlined in the EPA
Federal Register, December 23, 1971, Method 1.
INLET SAMPLING
     Precipitator inlet stack gases were sampled from an 80 inch by 80 inch
horizontal duct as shown in Figure 1; the probe was inserted into the duct
vertically from above.  The stack geometry, as indicated in Figure 1, was
such that 48 sample points were required for representative sampling.
Sample ports were located 2.8 duct diameters downstream and 2.0 duct dia-
meters upstream from flow disturbances.
OUTLET SAMPLING
     Outlet stack sampling was from an 80-foot high, 8-foot diameter, verti-
cal stack.  The stack geometry, as presented in Figure 2, shows the sample
port location relative to the nearest upstream and downstream flow distur-
bance.  Straight, unobstructed distances upstream and downstream of the
sampling position were 5.5 and 2.0 stack diameters, respectively.  Accor-
dingly, 24 sample points, as presented in Table 1, were required.
                                    25

-------
                                                  Inlet  ports,
From coke oven
  exhaust hood
                                                       Top View



i

8(


1



e"
5
\
^
>A
j\'
each ^
3"
;

5 ^
f
f
1
— 1»


; —







I ,, .x-io-3/o . eacn i
U— 6-7/8 
-------
                     8'
N5
                                                       16'
                                    Sample  level
                                                      64
Effluent ducting
from precipitator
outlets
                                                            Sample ports
                                                                            Distance  of  Sampling Point  From  Wall
                                                                    Point
                                                                              13
            14
    15
    16
     17
      18
      19
                                                                                                            8
     20
                                               10
                                        II
                                         12
      21
      22
     23
     24
                                                                   Distance,
                                                                     inches
           6.4
    11.3
    17.
    24
     34.1
     61.9
    72.0
     79.0
     84.7
     89.6
     94.0
                                                                  % of  Diam
        2.1
6.7
11.8
17.7
25.0
35.5
64.5
75.0
82.3
88.2
93.3
97.9
                                     Figure 2.  Outlet Stack Geometry Configuration

-------
                                  SECTION 5
                     SAMPLING AND ANALYTICAL PROCEDURES

POM SAMPLING AND ANALYSIS
POM Sampling Procedures
     An established methodology to sample organic and POM compounds is not
yet available as an EPA method.  The state of the art, to date,  is to
incorporate a special organic adsorbent material (which is enclosed in a
temperature-controlled column) with the conventional particulate sampling,
train.  To accomplish this, EPA Method 5 sampling train was modified
to include the adsorbent column for the sampling of organic compounds from
the inlet and outlet of a wet electrostatic precipitator at Wisconsin Steel
Company coke oven plant (see Figure 3).  Details of the operation of the
column are described in Appendix G.
     Figure 4 shows the Wisconsin Steel Company coke oven control device,
including hood, wet electrostatic precipitator, and exhaust stack.  The
inlet sampling location is part of an 80-inch by 80-inch horizontal duct
connecting the coke oven hood to the WESP unit.  The traverse of this duct
was conducted by sampling vertically from above.  The filter and adsorbent
column were attached directly to the end of the sample probe to avoid any
line loss of organic material.  Collection efficiency of the column is
temperature dependent; therefore, the gas temperature entering the column
was monitored and the oven temperature was adjusted to maintain an optimum
collection efficiency gas temperature of 125 _F ± 5 F.  An umbilical line
comprised of a flexible polyethylene hose with the associated thermocouple
and electric lines was attached from the sample probe outlet to the stan-
dard Method 5 impinger box which in turn was connected to the meter box
(Figure 3).  Since the inlet probe had to be repositioned in the vertical
plane for traversing, this sampling configuration kept the probe weight at
a minimum.
                                    28

-------
ro
vo
           Nozzle, Probe
"S" Pitot Tube and
 Manometer
                                     —Thermometer (125 F ±5F Gas  Temperature)
                            r
                             ]	OVEN	J
                             Standard    Tenax
                             Filter       Packed
                                         Column
                                                                  Drierite in
                                                                  Ice  Bath
                                       Inlet Sampling Train  Configuration \
                                                                        -Pump,  Meter, etc.
                                       Thermometer (125F ±5FGas Temperature)
Nozzle, Probe ( .^
i >f-.5'^S- -

> ... ! ^$s

/////////j
/////////
/////////
1
1


i
\ \ 	 OVEN 	 j
S" Pitot Tube and Standard
Manometer Filter

Tenax
Packed
Column





















































/
/
/
i •— rump, ivieiei, eic.
H—-X^
^
%
'///,
W/<

Drierite


                                                         Impingers in Ice Bath
                                      [Outlet Sampling Train Configuration [

                                       FIGURE 3.  POM SAMPLING TRAINS

-------
UJ
o
                          Outlet Sampling
                            Location JL
                           Water Into W.  E. S.  P.

                         Location C
                                                           Inlet Sampling
                                                              Location
     Coke Oven Hood
                                                         Water removal.
                                                         Location D
                                                                           '• Slowdown
                                                                             Water
Location E
                                            Figure 4.  Schematic of  Wisconsin Steel

                                                        Byproduct Coke Plant  with Wet

                                                        Electrostatic Precipitator
                                                j

-------
     Since coke oven door leakage was of primary concern,  coke pushing was
minimized during the sampling period.  To avoid any particulate collection
by impaction when pushing occurred,  the inlet sample probe assembly was
turned 180 degrees so that the sample nozzle was pointing  away from the gas
flow.
     The precipitator outlet gases were sampled simultaneously with the
inlet in order to determine precipitator efficiency.  The  standard train
used at the outlet was identical to  the train used at the  inlet and con-
sisted of a Method 5 train modified  by incorporating a POM adsorbent column
just after the filter (Figure 3). The gas temperature going into the POM
column was monitored, as in the inlet sampling train, and  the oven tempera-
ture adjusted to maintain 125 ± 5 F  gas temperature.  The  outlet stack
geometry at the sampling location was a vertical stack so  the sample
probe was connected directly to the  impinger box, eliminating the necessity
for an umbilical cord between the probe outlet and impinger box.
     Sampling time for both inlet and outlet was selected  to be 8 hours due
to the expected low concentrations of organic material in  the gas streams. .
POM Sample Cleanup Procedures
     Because of the light sensitive  nature of polycyclic organic matter, it
is necessary to keep all samples in  the dark during sampling and after
cleanup.  Figure 5 is the sample handling procedure which  was followed
during cleanup.  To establish background data from solvents and sample train
constituents, a pre-cleanup of all glass components was made.
     After the sample was collected, the sample trains were removed from
the stack and taken to an on-site mobile laboratory.  Each Pyrex probe and
all glassware up to the front half of the filter holder was rinsed with
methylene chloride and acetone and the rinses stored in amber bottles.  The
filter was placed in a petri dish and placed in a dark container.
The back half of the filter holder and all glassware up to the POM column
was rinsed with methylene chloride and acetone and placed  in the amber
bottles containing the front half rinse.  The POM column ends were capped
and the body wrapped in a light-tight container.  This procedure was fol-
lowed for each run — the contents of the amber bottles and the filter catch
were then taken to Battelle labs to  be analyzed for organic matter.
                                    31

-------
Blank Methylene Chloride
Blank Acetone
Blank Filter

Blank Adsorbent Column
POM Analysis
POM Analysis
Pre-cleanup Methylene Chloride Wash
Pre-cleanup Acetone Wash
Pre-cleanup Filter

Pre-cleanup Adsorbent Column
POM Analysis
POM Analysis
Methylene Chloride Wash, probe & front-half glassware ~)
Methylene Chloride Wash, back-half glassware          J
Acetone Wash, probe & front-half glassware
Acetone Wash, back-half glassware
Filter

Adsorbent Column
     Amber bottle,
     store in dark
     Amber bottle,
     store in dark
     Store in dark

     Cap ends, store
     in dark
Weigh to
determine
volume

Weigh to
determine
volume
POM Analysis
                                                                                                  POM Analysis
                                   FIGURE 5.   POM CLEANUP SCHEMATIC

-------
POM Analysis
     The POM analysis was conducted using standard Battelle POM analysis
procedures.  These procedures are described in Appendix G,  pages G-6 to G-9.
Basically, the analysis procedure includes extracting the filter and adsor-
bent column with methylene chloride and pentane,  respectively.   Then the
three solvent solutions (probe wash, filter extract,  and adsorbent column
extract) are analyzed separately or in various combinations by gas chroma-
tography-mass spectroscopy (GC-MS) techniques.  For this task,  the methylene
chloride and acetone rinses of the probe and glassware were combined with
the filter to determine a single "filterable" POM value; the adsorbent
column was analyzed separately.
     Water samples were extracted with methylene chloride and the extracts
were processed in the same manner as air emission extracts, as described
above and in Appendix G, pages G-8 to G-9.
TOTAL FLUORESCENCE
     Pretest discussions between  EPA staff and Battelle staff had suggested"
that total fluorescence might provide a useful measure of total POM content
of emission samples.  Total fluorescence would be a more descriminating
measure of carcinogenic organics  than the frequently used benzene-soluble
organic (BSO), and is a less costly analytical procedure than GC-MS.  Thus,
Battelle was requested to determine total fluorescence for the POM emission
samples and the samples from the  XAD-2 Columns used for BSO vapors.
     Total fluorescence was determined for each sample on a Turner spectro-
                          o                     o
fluorimeter, using a 3500 A excitation and 4100 A emission wavelengths.
The emission slit was 25 A and the excitation slit was 100 X.  Results are
reported in Table 6.
MOLECULAR WEIGHT OF STACK GAS
     During the 8 hours of sampling for organic material, an integrated gas
sample was collected in a Tedlar  bag.  The sampling rate was adjusted so
that the bag would be essentially full at the end of the 8-hour test period.
Orsat analysis for concentrations of C0?, 0_ and CO was completed at the
end of each run.  These data were then used  to calculate the stack gas
molecular weight.  The collection schedule for the integrated gas samples
is presented in Appendix D.
                                    33

-------
GASEOUS HYDROCARBONS SAMPLING AND ANALYSIS
     To provide a gas sample for gaseous hydrocarbons analyses (benzene and
acetylene),  at the end of each run a gas sample was collected in an evacuated
flask by removing an aliquot from the integrated bag sample which had been
collected for Orsat analysis.  Both the inlet and outlet gases were sampled
in the same manner.
     The evacuated-flask samples were analyzed for benzene and acetylene
using a gas chromatograph with a flame ionization detector.   The instrument
used was a Aerograph, Model 20 C; the column was a 10mm (0.25 inch) x 0.48m
(10 feet) stainless steel column containing Poropak Q; the carrier gas was
helium, flowing at 48 ml/min; and the detector was a thermal conductivity
detector operating at a 275 milliamp current.  Instrument temperatures were
column, 30 C for acetylene and 200 C for benzene; detector, 93 C; and injector,
145 C.
     The compounds were calibrated against standard mixtures of acetylene in
nitrogen and benzene in nitrogen.
                                    34

-------
                               SECTION 6

                              REFERENCES
1.  "Exposure to Coke Oven Emissions,  Occupation Safety and Health Standard",
     Federal Register, Vol. 41,  No.  206,  October 22,  1976,  p46742 - 46790.

2.  "Particulate Polycyclic Organic Matter",  National Acadamy of Sciences,
    1972, p28.
                                   35

-------
                   APPENDIX A

FIELD AND LABOMTORY DATA RELATED TO POLYCYCLIC
          ORGANIC MATTER (POM) SAMPLING

            Nomograph Data Sheets
            Field Data Sheets
            Field Cleanup Data Sheets
            Sample Identification

-------
NOMOGRAPH DATA SHEETS
         A-l

-------
Nomograph data sheets for inlet
     runs are not available.
                A-2

-------
                       NOMOGRAPH DATA
 DATE
 SAMPLING LOCATION
CALIBRATED PRESSURE DIFFERENTIAL ACROSS
ORIFICE, in. H£0
j
AVERAGE METER TEMPERATURE (AMB1ENT+20°F),°F
PERCENT MOISTURE IN GAS STREAM BY VOLUME
BAROMETRIC PRESSURE AT METER, in. Hg
STATIC PRESSURE IN STACK, in. Hg
(Pra±0.073 x STACK GAUGE PRESSURE in in. H20)
RATIO OF STATIC PRESSURE TO METER PRESSURE
'AVERAGE STACK TEMPERATURE, °F
AVERAGE VELOCITY HEAD, in. H20
*
MAXIMUM VELOCITY HEAD, in. H20
C FACTOR
CALCULATED NOZZLE DIAMETER, in.
ACTUAL NOZZLE DIAMETER, in.
REFERENCE Ap, in. H20
AH@
T"avj.
•
Bwo
' Pm
PS
. PS/P
/rn
Ts
*avg.
APavg.
APmax.
//^
7^
. f>
j- •
•

I
.&*
/.w

1,0$
!,$z •
o. u-r '
/. 6r^^
EPA (Our) 234
   4/72
                              A-3

-------
                       NOMOGRAPH DATA
 PLANT.

 DATE_
 SAMPLIHG LOCATION
CALIBRATED PRESSURE DIFFERENTIAL ACROSS
ORIFICE, in. H20
AVERAGE METER TEMPERATURE (AMB1ENT + 20°F),°F
PERCENT MOISTURE IN GAS STREAM BY VOLUME
BAROMETRIC PRESSURE AT METER, in. Hg
STATIC PRESSURE IN STACK, in. Hg
(Pm±0.073 i STACK GAUGE PRESSURE in in. H20)
RATIO OF STATIC PRESSURE TO METER PRESSURE
'AVERAGE STACK TEMPERATURE, °F
AVERAGE VELOCITY HEAD, in. H20
/•
MAXIMUM VELOCITY HEAD, in. H£0
C FACTOR
CALCULATED NOZZLE DIAMETER, in.
ACTUAL NOZZLE DIAMETER, in.
REFERENCE Ap, in. H20
AH@
Tn}avg.
•
Bwo
Pm
PS
" S/Pm
savg.
APavg.
APmax.
I.9Z
/*f"
'£ •
•

/
73
l>te

• i, io
^ Jtl
>m •
/.6?
EPA (Our) 234
   4/72
A-4

-------
                        NOMOGRAPH DATA
 Pi ANT
      ~
 SAMPLING LOCATION
CALIBRATED PRESSURE DIFFERENTIAL ACROSS
ORIFICE, in. H20
AVERAGE METER TEMPERATURE {AMBIENT+200F},0F
PERCENT MOISTURE IN GAS STREAM BY VOLUME
BAROMETRIC PRESSURE AT METER, in. Hg
STATIC PRESSURE IN STACK, in. Hg
(Pm±0.073 x STACK GAUGE PRESSURE in in. H20)
RATIO OF STATIC PRESSURE TO METER PRESSURE
'AVERAGE STACK TEMPERATURE, °F
AVERAGE VELOCITY HEAD, in. H20
MAXIMUM VELOCITY HEAD, in. H£0
C FACTOR
CALCULATED NOZZLE DIAMETER, in.
ACTUAL NOZZLE DIAMETER, in.
REFERENCE Ap. in. H20
AH@
Tfl]avg.
•
Bwo
• pn
PS
S yp
/*n
savg.
APavg.
APmax.
/,f*
Pf
'£ •

-------
FIELD DATA SHEETS
       A-6

-------
                                                                 FIELD DATA
PLANT W,.^
DATE
SAMPLING LOCATION
SAMPLE TYPE
RUN NUMBER
OPERATOR	
AMBIENT TEMPERATURE/
BAROMETRIC PRESSURE
STATIC PRESSURE. (P$)
FILTER NUMBER (s)
                                                                                         PROBE LENGTH AND TYPE.
                                                                                         NOZZLE 1.0	£J.
                                                                                         ASSUMED MOISTURE. *
                                                                                         SAMPLE BOX NUMBER.
                                                                                         METER BOX NUMBER _
                                                                                         METER AHe	
                                                                                         CFACTOR	
                                     PROBE HEATER SETTING    J i ->
                                     HEATER BOX SETTING      I 3. <*
                                     REFERENCE *r
                                                                                                             / V
                                                         SCHEMATIC OF TRAVERSE POINT LAYOUT
                                                   READ AND RECORD ALL DATA EVERY
                             !ii MINUTES
! TRAVERSE  j
   POINT
  NUMBER
COMMENTS;
           73
           10
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GAS WETER READING      VELOCITY
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                                                               ORIFICE PRESSURE
                                                                DIFFERENTIAL
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                                 34/.P
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314,
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                          TEMPERATURE
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                                                                         TEMPERATURE
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                                                                      (Tnjn).°F
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                                               ^ J
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FPA f

-------
    TRAVERSE
     POINT
     NUMBER
                    CLOCK TIME
SAMPLING
 TIME, mm
                    CAS METER READING
                                              VELOCITY
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                                                    ORIFICE PRESSURE
                                                      DIFFERENTIAL
                                                      lAHl. in HjOl
                                                           DESIRED
                                                      ACTUAL
                                                                       STACK
                                                                    TEMPERATURE
                                                                      iTsi.°F
                                                                                 DRYGASMETCR
                                                                                 TEMPERATURE
                                                                                     INLET
                                                                                    (Tm)."F
                                                                                OUTLET
 PUMP
VACUUM.
 in Hg
TEHPER^TtlRE.
     °F
TEMPERATURE.
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-------
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ISTIIRF 5 __
( NUMBER _

5. METER BOX NUMBER _.

— 1

METER AHS
C FACTOR.


PROBE HEATER SETTING
HEATER BOX SETTING
REFERENCE
1ATIC OF TRAVERSE POINT LAYOUT
ORO ALL DATA EVERY j^-T' MINUTES
ORIFICE PRESSURE
DIFFERENTIAL
(AH), in. H20)
DESIRED
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                                                                           FIELD DATA
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-------
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                                                                     FIELD DATA
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-------
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-------
                                                              FIELD DATA
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-------
    TRAVERSE
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                                                              FIELD DATA
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-------
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-------
                                                                               FIELD DATA
                   PLANT
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                   SAMPLING LOCATION
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                   RUN NUMBER —r-T-
                   OPERATOR ^/^/-A ..
                   AMBIENT TEMPERATJffiE
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                                                                                                        SAMPLE BOX NUMBER
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                                                                       SCHEMATIC OF TRAVERSE POINT LAYOUT
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                                                                                                        REFERENCE Ap	
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-------
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                                                                     FIELD DATA
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                                              SCHEMATIC OF TRAVERSE POINT LAYOUT
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 NUMBER
                        CLOCK TIME
                      GAS METER READING
                          (Vm). tf
                                                           VELOCITY
                                                             HEAD
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                                                                   ORIFICE PRESSURE
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                                                           STACK
                                                         TEMPERATURE
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                                                                     FIELD DATA
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-------
                                                                 FIELD DATA
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-------
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-------

                                                                      FIELD DATA
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-------
                                                                        FIELD DATA
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                      DATE  J-//P./77
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                                                                                                           '9-
     C FACTOR
     PROBE HEATER SETTING
     HEATER BOX SETTING
     REFERENCE AP     JTl
                                                                SCHEMATIC OF TRAVERSE POINT LAYOUT
                                                         READ AND RECORD ALL DATA EVERY.
MINUTES
1
OJ


1

TRAVERSE
POINT
NUMBER
3-1






















TIME.fnin ^\. *•
~~ • — ——____
HI 5~ IS ,'31
ISP /f/y#

-~
ifro

















	 1
GAS METER READING
og. ft3

717/ "7
I'll/
775,£>2) erfrZ
"
—- — -"—
JJ/. ?6



.














VELOCITY
HEAD
(APS), in. H20
/; $ T


\ 	 	 "
A3'


















ORIFICE PRESSURE
DIFFERENTIAL
(AH), in. H20)
DESIRED
/,/f


«;



















ACTUAL
/,/6~


[_— - — "*
j
i '/^












•••





STACK
TEMPERATURE
(TS),°F
Zl

	 	 	 J"~
7t











,






DRY GAS METER
TEMPERATURE
INLET
7

...
/


















PUMP
VACUUM,
in. He
MtO




















^

SAMPLE BOX
TEMPERATURE,
°F
IU //V#






















IMPINGER
TEMPERATURE,
"F
U> e*.


-



















                                                                                                                                                                ll
COdWENTS;

EPA fOurl 235

-------
                                                                   FIELD DATA
                   /v
            PLANT.
            DATE \r//J/77
                         SAMPLING LOCATION
                         SAMPLE TYPE
                         RUN NUMBER.
                         OPERATOR
                                                                                           PROBE LENGTH AND TYPE.
                                                                                           NOZZLE I.D.    » /' 7.5"
            AMBIENT TEMPERATURE'_
            BAROMETRIC PRESSURE _
            STATIC PRESSURE. (Ps)	
            FILTER NUMBER (s)	
                                                                           ASSUMED MOISTURE. ".    •2-
                                                                           SAWPLE BOX NUMBER    vf
                                                                           METER BOX NUMBER    &•
                                                                           METER AH-     ' f~
                                                                           CFACTOR_
                                                                                                      1,10
                                                                                          PROBE HEATER SETTING.
                                                                                          HEATER BOX SETTING	
                                                                                          REFERENCEAP   //,£
                                                            SCHEMATIC OF TRAVERSE POINT LAYOUT
                                                       READ AND RECORD ALL DATA EVERY.
                                                                         MINUTES
TRAVERSE
 POINT   i
 NUMBER
                        CLOCK TIME
                            (24 -hr
                        GAS METER READING
                                        VELOCITY
                                         HEAD
                                       (AP5), in. H20
                                                    ORIFICE PRESSURE
                                                      DIFFERENTIAL
                                                      (AH), in. HZ0)
                                                                 DESIRED  ACTUAL
   STACK
TEMPERATURE
 DRY GAS METER
 TEMPERATURE
                                                                                            INLET    OUTLET
  PUMP
 VACUUM.
  in. Kg
 SA.YPLE BOX
TEMPERATURE.
  IWPINGER
TEMPERATURE.
     "F
  113
   o
           l'/7
            i If 1
                                           I'lO
                                   77^
                                           \.05-
                                                                                                   ti'ej 1M
OJ
                                        I
11 ,/'
                             3.2.
                     . H
                                                                                                   HA
            XL
                        £A
                                        1>330
                       £i:zb
                                           /.a>r
                                                                 *&.
                                                                                                       m/iHl
   /AT
l*o     ^/.'J
                                           L2o
 12.
j^
1ZL5
                                                                                                                   1 3.0
                                                                                                                     (,0
                                 H^
                        LL
                                                                                                                    l Ml I IS
xwo
          JJ1L
                                                                                              H^C.
                                                                                                                                  LO
      .COMMENTS:

      EPfl

-------
    TRAVERSE
     POINT
     NUMBER
   SAMPLING
    •T...I-
    TIME. mm
           CLOCK TIME
              i24-hi
                     CAS METER READING
                         iVm..«3
                                     VELOCITY
                                       HEAD
                                     (ipjl. in. H^O
ORIFICE PRESSURE
 DIFFERENTIAL
  lAHi. in HOi
                                                        DESIRED  ACTUAL
  STACK
TEMPERATURE
  (Tsi.°F
DRY GAS METER
TEMPERATURE
                                                                                INLET    OUTLET
 PUMP
VACUUM.
 in Hg
 SAMPLE BOX
TEMPERATURE.
    °F
  IMPINGER
TEMPERATURE.
         sf
                                       I.H0
                                                             23-
                                                                      10 3
                                                                      J*5
         V
   $0
                                                                             7?
                             133, 3
                                                                        33

                                                                      77
                       ' 1
                                       I V.f
                                                                                    W.O
         9-
   i no
                                               1,1,0
                                                                             ?'$>
            (O.T    ?•&',£
                                                              7.T
                                                                                           nt,//*/,?
                                                                                                       (,0
                                                         \,IO
                             VM, 7
                                                1,10
                                                     I, [0
                                                                      l&SL
                              ?7
                         13,0
            \ZD
                    m, 7
                                                     h/fl
                                                                            9 7
                                      J3,
                                                               Uff
                                                             7V
                                                                      lot
                                                                                              /."/I
             ?>o
            IS*
                                       1, 30
              ', ,TI
                                                                      '100
                                                                             
                                                                                           1 &>//*&
            ~t-(
4
                    23106?
                  JjLz.
                                                                      ML
                                                                      lot
                                                                                             $0,0
            Ibt
                                                                                id
                                                        1,1*5-
                                                              73
                                                                       10)
                                                                                    90 •
                                             )&//
-------
                                                                  FIELD DATA
                       PLANT
                       DATE
              SAMPLING LOCATION
              SAMPLE TYPE
              RUN NUMBER.
              OPERATOR
                                                                                 PROBE LENGTH AND TYPE
                                                                                 NOZZLE 1.0.  0> I

                                   L
AMBIENT TEMPERATURE ,
BAROMETRIC PRESSURE .
STATIC PRESSURE, (Ps)_
FILTER NUMBER ($)	
                                          $0
                                                          ASSUMED MOISTURE. 5 __£
                                                          SAMPLE BOX NUMBER   J~~
                                                          METER BOX NUMBER    ^
                                                          METER AH« _ /.#?
                                                          C FACTOR
                                                                                            A/,7
                                          3-1' 3 5~
                                                                                 PROBE HEATER SETTING
                                                                                 HEATER BOX SETTING
                                                                                 REFERENCE AP_   ///£,
                                                           SCHEMATIC OF TRAVERSE POINT LAYOUT
                                            READ AND RECORD ALL DATA EVERY
                                                                                     MINUTES
     TRAVERSE
      POINT
      NUMBER
             CLOCK TIME
              TIME.min
    GAS METER READING
                               VELOCITY
                                 HEAD
                              (AP5), in. H20
ORIFICE PRESSURE
 DIFFERENTIAL
  (4H), in. H20)
                                                                DESIRED  ACTUAL
   STACK
TEMPERATURE
  (TS),°F
DRY GAS METER
TEMPERATURE
                                                                                   INLET
                                                                                 (TB  ).°
                                                                                                   OUTLET
 PUMP
VACUUM,
 in. Kg
 SAMPLE BOX
TEMPERATURE,
     °F
  IMPINGER
TEMPERATURE,
     "F
 U)
 00
                       00 ',36
                                     ,
                                                       1,1)0
                                                       1,-3o
                                                                       23-
                                                                   ±L
              3-3-5
               oo '
I
                                                                                                                   //.C//.T.?
                                                              L2o_
                                                                                 7.P
                                                                                          f/
/ay
                                             77^?
                                                                                        //S3
                       Vi3.*
                                                                                            f/
                                              JaQ
                                                                                                           17-r
                                                                                                                         63
                        o \\38-
                                                                        77
                                 .572 , ?
                        OH HZ
                                                                         77
                                                                                    HO /I S3
                                                                UtiL
                                                              1>M.
                                                  -£2-
                                                  n*T
                                                                                             UZ//f3
                                                                        /i  0
                                                                                                                          f
                                                                                                                          la
£L
                                                                                            93
                                                                                    //£A\?
                                                        , 30
                                                                                                                          6
                                                                                                                                     .
                         7/7>3
                                                       7.30
                                                                            HuL
                                                                                                                                  IP °~
                                77.7.
                                                        l.fr
                                                                                                                    TT/^3
                                                                                                   £
    COMTHENTS:

-------
     TRAVERSE
      POINT
      NUMBER
                     CLOCK TIME
SAMPLING
 TIME, mm
                    GAS METER READING
                                         VELOCITY
                                           HEAD
                                        I4PS). in. H^O
                                               ORIFICE PRESSURE
                                                 DIFFERENTIAL
                                                 liHi. in H^Oi
                                               DESIRED  ACTUAL
                STACK
             TEMPERATURE
               |T$I.°F
                                                                DRY GAS METER
                                                                TEMPERATURE
                                                                                       INLET
                                                                                     •Tmln».°F
                                                                                OUTLET
 PUMP
VACUUM.
 in Hg
 SAMPLE BOX
TEMPERATURE.
     °F
                                                                                                            IMPINGER
                                                                                                          TEMPERATURE.
              337
         -12-
2ti2_
                                          i.'j.r
                                                                                       $•2,0
          /7
 3/S
                                                                                           3.3-, 0
                                                                                                ±o
                       03. l
                                                i, 7,r
                                                           A7T
         -LL
                                                               2J_
                                                                                                  /Jf/'/f/f
                                                                                                            AL
         JLL.
33Q     or,K
                                                                  -23.
          i.r
                                                               7.3
                                                                                              , 0
                                                                                                            £7
                               1010,2.
                                       1*5-0
                                                    1.7°
                                                                                to
                                        2-3,0
\zo
m
              363     03
                                                                   •7.53"
                                                                7.T
                       03 I
                                      1,5*0
              373
          AT
            11 A
                               \ CHS ,0k I
                                                1,75-
                                                                    77
                                                                                        33,0
          u
3?.5~
                                                                   79
-4
                                 FAS II
                                                                                re
                                                                             77
                                                                                         3.0
          /7
o<{ M\
                 }o
                                          A 517
                                                       A 7<5
                                         33,0
                                                                                                                            -
1Z£_
!'.££
                                                                             77
                                                                                57
                                                                                            3.0,0
                               Iff
                                                                                                    L3P.1&-.

-------
FIELD CLEANUP DATA SHEETS
           A-41

-------
                                   ANALYTICAL DATA
PLANT.
DATE-
 Wisconsin Steel Works
 Chicago,  Illinois
 G 2872.-5014	
MAV  9 197?
SAMPLING LOCATION
SAMPLE TYPE .
RUN NUMBER_
SAMPLE BOX NUMBER
CLEAN-UP MAN _
                                              COMMENTS:
FRONT HALF
  ACETONE WASH OF NOZZLE, PROBE, CYCLONE (BYPASS),
    FLASK, FRONT HALF OF FILTER HOLDER
  FILTER NUMBER
  9 *?J    tare
          net
  POM    // 305
                                             CONTAINER
                                              CONTAINER
                                              FRONT HALF SUBTOTAL
                                                                       LABORATORY RESULTS
BACK HALF
                                              CONTAINER.
IMPINGERS, CONNECTORS, AND BACK
HALF OF FILTER HOLDER
ACETONE \VASH OF IMPINGERS CONNECTORS
AND BACK HALF OF FILTER HOLDER

-S.J&J ~U MoJf-fJ/.rk
/p-i n^p '
voltes ml ml
MOISTURE
IMPINGERS 1 2 3
FINAI vnillfJF ml / ml
INITIAt VOIUMF /° ° ml '/
NFTVOIIIMF ml ml
SILICA GEL
FINAI \VFir.HT ^7 5 ' g |
IHITIAI Vi'EIC-IIT L{75 g g
NpjV.'Fir.llT I I
A-42
EPA (Dm) 231
4/72
ETHER-CHLOROFORM
CPNTAIHFR r.g
BACK HALF SUBTOTAL r?

TOTAL WEIGHT ns

ml ml ml

4 5 6
ml ml ral

ml - ml- mj ff, ]
E
E
E TOTAL KOISTURE f


-------
        Wisccr.sin Ste<=l  Works
        Cr.ic-rgo.  I] i
PLANT..  G *i-7-;-fTl
DATE.
         MAY   91977
SAMPLING LOCATION
SAMPLE TYPE	£j
RUN NUMBER_
                                   ANALYTICAL DATA
                          -e- Ci>
SAMPLE BOX NUMBER
CLEAN-UP MAN_
                                              o *—
FRONT HALF
  ACETONE WASH OF NOZZLE, PROBE, CYCLONE (BYPASS),
    FLASK, FRONT HALF OF FILTER HOLDER
  FILTER NUMBER
         _tare
          net
                                              CONTAINER
                                              CONTAINER
                                                                        LABORATORY RESULTr
  POM
                                              FRONT HALF SUBTOTAL
BACK HALF
                                              CONTAINER
IMPINGERS, CONNECTORS, AND BACK
HALF OF FILTER HOLDER
ACETONE WASH OF IMPINGERS, CONNECTORS,
AND BACK HALF OF FILTER HOLDER
Rinse *"7- *'** /vor f
* fs yyx* f~~ *^3X/ C P 'T ^
volumes ^\ mi
MOISTURE r?*£
IMPINGERS 1
FINAI vnnir:.F
INITIAI Vni I1MF .. /O °
NFTvnnii.',F
SILICA GEL
FINAL wFir.HT
INIT'AL v.'ElGHT ^7-^
NFT v.'riniiT
EPA(Dui)231
4/72
A X-/7OV Jt2? />
2
ml ml
_ral
ml ml
£ I
I E -
P E

ETHER-CHLOROFORM
FXTRAnrtnu
CONTAIUPR
BACK HALF SUBTOTAL

TOTAI WFIRHT

.r- 
-------
                                    ANALYTICAL DATA
 PLANT.

 DATE-
          Wisconsin Steel Works
          C.'-.icsgo. Illinois
          G 2f ~
              1  0 19/7
SAMPLING LOCATION _JL
SAMPLE TYPE    P* *t -

RUN NUMBER_
                           
                        rai
 ml
.ml
 ml
                                   ml
                                                CONTAINER	
                                                ETHER-CHLOROFORM
                                               BACK HALF SUBTOTAL
                                                TOTAL WEIGHT
                                                ml
                                                             .ml
                                                 JBl
                                                ml
jnl
 5     .     6
	ml	
                                                                         jnl
                                                           TOTAL MOISTURE
                                          A- A 4
                                                                                         rt
                                                                                         rE

-------
                                    ANALYTICAL DATA
        Wisconsin Steel Works
        Chicago,  Illinois
P|flHT   C 28-72' 5ci4	
         MAY 1 0 1977
SAMPLING LOCATION

"SAMPLE TYPE
RUN M11HRFR    I&IV-8-
SAMPLE BOX NUMBER

CLEAN-UP MAN
FRONT HALF
    FLASK, FRONT\HALF OF FILTER HOLDER
  ACETONE WASH
    FLASK, FR01

  FILTER NUMBER

  g  ??   tan

          net

 POM #  3l *- • -
                      . PROBE, CYCLONE (BYPASS),
      -.312-2.


BACK HALF

  IMPIHGER CONTENTS AND WATER WASH OF
    IHP1HGERS, CONNECTORS, AND BACK
    HALF OF FILTER HOLDER

ACETONE WASH OF IMPINGERS, CONNECTORS,
    AND BACK HALF OF FILTER HOLDER
            Rinse
           volumes
MOISTURE

  IMPINGERS
   FINAL VOLUME
   INITIAL VOLUME
   NET VOLUME   =-
                                 jnl
                                               COMMENTS:
                 1 ot>
.ml
 ml
 ml
  SILICA GEL   .
  . FINAL WEIGHT
   INITIAL'WEIGHT
   NET WEIGHT

  EPA (Our) ?31
     4/72
                  JJLJLl
.ml

 ml


-I

-E
                                                    -   l«*


                                               CONTAINER _
                                                                         LABORATORY RESULTS
                                                                                          I
                                               CONTAINER
                                               FRONT HALF SUBTOTAL
                                               CONTAINER	
                                               ETHER-CHLOROFORM
                                                 EXTRACTION

                                               CONTAINER	
                                               BACK HALF SUBTOTAL
                                                TOTAL WEIGHT
                                              jnl
                                                            .ml
                                                ml
_jnl
                                                             -ml  	
                                                                        .ml
                                           	 6
                                           	I
                                           A-45
                                                           TOTAL KOISTURE

-------
                                   ANALYTICAL DATA
        Wisconsi
        Chicago.
                n :~t-': :
      MAY
SAMPLING LOCATION
SAMPLE TYPE .
RUN NUMBER_
                       tt>
                  - fr -
SAMPLE BOX NUMBER _1
CLEAN-UP HAN.
                                              COMMENTS:
                                                    2 -
FRONT HALF
  ACETONE V/ASH OF NOZZLE, PROBE, CYCLONE (BYPASS),
    FLASK, FRONT HALF OF FILTER HOLDER
  FILTER NUMBER
  f 9f   tare
          net
  POM //
                                             CONTAINER
                                              CONTAINER
                                                                       LABORATORY RESULTS
                                              FRONT HALF SUBTOTAL
BACK HALF
IMPINGER CONTENTS AND WATER WASH OF
IMPINGERS, CONNECTORS, AND BACK
HALF OF FILTER HOLDER
ACETONE WASH OF IMPINGERS, CONNECTORS,
AND BACK HALF OF FILTER HOLDER
I /rut aw£)
Rinse
volumes _., ',
roi /ni
MOISTURE
IMPINGERS 1 2 3
FINAI vni nr;.F ml ml
INITIAI VDI IIMF 	 ml
NFTVnillMF ml r^l
SILICA GEL
FINAI v;Fir,HT g i ,
1NITIM v/rir.iiT — - f E
NFTV.Tir.HT I I
A-46
EPA (Dui) 231
4/72
rnHTftlMFR rp
ETHER-CHLOROFORM
CONTAINFP r-E
BACK HALF SUBTOTAL rs

TOTAI WFIfiHT ng

, ynl ml , pil
456
ml , p\\ p]

ml - nil ml fr-i
_ E "*
_ E
e TOTAL MOISTURE f


-------
                                    ANALYTICAL DATA
        Wisconsin Ste.?l Works
        Chicago.  Illinois
p| Wi   C 2B72.-5CI4	
             i 2S77  -
SAMPLING I.DCATIOH

SAMPLE TYPE   9
RUN MMHRFR    W5^ - 0 ' f» M -f-
                     T
SAMPLE BOX NUMBER

CLEAN-UP MAN
FRONT HALF

  ACETONE WASH OF NOZZLE, PROBE,-CYCLONE (BYPASS),
    FLASK, FRONT HALF OF FILTER HOLDER
  FILTER NUMBER
  //  ?6>   tare

          net
                                               COMMENTS:
                                             577-00?-
                                             323-
                                               CONTAINER
                                                                         LABORATORY RESULTS
                                               CONTAINER _-O
  POM
                                               FRONT HALF SUBTOTAL
BACK HALF

  IMPING ER CONTENTS AND V/ATER WASH OF
    IMPINGERS, CONNECTORS. AND BACK
    HALF OF FILTER HOLDER

ACETONE WASH OF IMPINGERS, CONNECTORS,
    AND BACK HALF OF FILTER HOLDER
                                               CONTAINER	
                                               ETHER-CHLOROFORM
                                                EXTRACTION

                                               CONTAINER	
                                               BACK HALF SUBTOTAL
-rg
                                                                                        r?
Rinse
volumes ral
MOISTURE
IMPINGERS 1 .
FINAI vm nr:.F \l* ml
INIJIAI vnniMF tfff ml
NETVni.UMF /L/ ml
SILICA GEL ^^ 0 /y
FINAL Vt'Eir-HT 52* g
INITIAL WEIGHT #7/" g
METv.'nniiT ^7 E
EPA (Dm) 731
4/72

TOTAI WFIRHT nr

ml ml ml ml
23 4 5 6
ml ml ml ral

ml "0 - p] - m] n-,)
v&/
5 a/ F 8 ^^
y/ $" e f V 7
f/5. f t ' * TOTAL!,:OISTURE/0~7 E
A-47 /0?

-------
                                    ANALYTICAL DATA
 PLANT.
        Wisconsin Steel Works
        Chicago.  I3iitcis
        G 2S?2i-5C'i4
         MAI  1 2137?
SAMPLING LOCATION

SAMPLE TYPE _

RUN NUMBER _
SAMPLE BOX NUMBER _:

CLEAN-UP MAN__£W
FRONT HALF
                                              COMMENTS:
                                           3.3 1 ~
  ACETONE WASH OF NOZZLE. PROBE, CYCLONE (BYPASS),    CONTAINER.
    FLASK, FRONT HALF OF FILTER HOLDER
  FILTER NUMBER
  #  
-------
                                    ANALYTICAL DATA
 PLANT.
 DATE_
Wisconsin Stec-1  Works
Chicago.  Illinois
E 2E72>-5G14	
COMMENTS:
SAMPLING LOCATION
RUN NUMBER
                                            33 i-
SAMPLE BOX NUMBER
CLEAN-UP MAN
FRONT HALF
  ACETONE WASH OF NOZZLE, PROBE, CYCLONE (BYPASS),
    FLASK, FRONT HALF OF FILTER HOLDER
  FILTER NUMBER
  0   IS  tare
          net
                                                            tj_ ffafa. 
-------
                                   ANALYTICAL DATA
         Wisconsin Steel Works
         Chicago, Illinois
PLANT.    G gS7fr-R
                                             -COMMENTS:
             1 31977 ~
SAMPLING LOCATION
SAMPLE TYPE  ?o
RUN
                             
-------
                                    ANALYTICAL DATA
       Wisconsin Steel Work.1?
       Chicago,
PLANT., G 2L?jf-af?]d
                                               COMMENTS:
SAMPLING LOCATION.
                                  esp
                                            $77-002-
RUN NUMBER.
SAMPLE BOX NUMBER

CLEAN-UP MAN J
                                                                    ft*** !••
                                            3¥f.   Port
FRONT HALF
  ACETONE WASH OF NOZZLE. PROBE, CYCLONE (BYPASS),    CONTAINER.
    FLASK, FRONT HALF OF FILTER HOLDER

                                               CONTAINER
                                                                          ff


                                                                          LABORATORY RESULTS


                                                                         	*S
// /*° tare a-.tW q
net
POM # Wb
BACK HALF .
IMPING ER CONTENTS AND WATER WASH OF
IMPINGERS, CONNECTORS. AND BACK
HALF OF FILTER HOLDER
ACETONE WASH OF IMPINGERS, CONNECTORS,
AND BACK HALF OF FILTER HOLDER
Rinse
volumes mj ml
MOISTURt
IMPINGERS 1 2
FINAI V01lir:.F Itl ml ml
1NITIAI VnillMF 10 O m,
NFTVHI llf.'.F W ml mi
qjft.SA'J*'
SILICA GEL ^ '
FINAI WFir.HT 6 64- g £07-° g
INITIAI v.'Fir.HT 55~C>," p ?5"° « .
NFTwnniiT $ i n-°i
FRONT HA1.FSIIRTOTAL rf
rntn-AiuFR r?
ETHER-CHLOROFORM
CONTAIHFR rf
BACK HALF SUBTOTAL rE

TOJAI WFIRHT nsl

ml ml ml
3 456
ml ml ml

jn}. tnl- nij jjij

, P
(• TOTAL 1,-OlSTURE /60.& I
  EPA (Dui) ?31
                                       A-51

-------
               IDENTIFICATION ICC OF SAMPLES COLLECTED
PI a n t     MMeir>nn-=Mn gfaal
               ngn  TUinMa
Location
Industry   G g872>-50j.4
Project No.
Battelle Record  Book No 333.gH
Collected & Recorded By
Page	of	.
EPA No'. Date
S77-002



'?t>l
-301
•~2t>l




3°i
3oS
30 4



















MAY g



























Run
Number

V5V- $
1977 -





WSUJ-i





















Sample Description

-P£>*i'CU
HO^ fc'^ay —
tterv.yt.eue crfu>x-f>Jc of- ,
•Qnfi*n nj-stf FttrfK *' 3f
Po /V- Co ^V/^/J ~ TTSWA X


J - part- CO

/Sf.f~":/LCVi. (t/t,o*.>v'S t?'f:'( f>f
£((JflL~l 7/SSt>! Mi"???? * 9^
Po /v - c a. W u • TL w y

















Remarks



*<*&, +&*#fJ &*'+±.'-3/~^'


•



(>fijfc ' v- fts-i c-e^^f^^'-^



















                                     A-52

-------
Plant
              IDENTIFICATION LOG OF SAMPLES COLLECTED

         Wisconsin Steel Works
         Ohic-ggo,  Illinois
•    ,    v*a*v-*^vf  .» » *
Location Q gQ7iJ) 6Q14
Industry	
Project No,
                                    Battelle Record Book No 332
                                    Collected & Recorded By
                                    Page	of	.
EPA No'.  Date
S-/7-002-
    Run
    Number
Sample Description
Remarks
               WSIV-A-  Pov-r- /  ( ,*,_*•   T*
ro
               IS77
 307
                      PflM-
                      3 -  POH-T- 1  (ourt-ET  TV  f£f)
 31 o
                           Pfloae
                                   4 LASS
 J'l
                            p/cma. *   qtf
 312.
           met-
    ESP
 313
                       e>uTL£f  - f*a**t
                                                t~sp.
                                                        ff/>6
-31 (,
                                                73'
 •311
 3*74
 310ft
                        A-53

                         - A
                                                   -.I

-------
Plant
  IDENTIFICATION LOG OF SAMPLES  COLLECTED
        Steel Works
.«n.   lUaois                      Battelle Record Book No  33 -2.8 S
Location n 9R73-5014 Collected & Recorded By @<^vfrx
Indust
Projec
ry cone e*tA£ Paqe
t No.

EPA No'. Date
S77-OG1





31 1
3/9
310



32 1
j;!
323



3M
025
32 £



317
31$

\2 lp fi
J ^ / /i
3i?W





MAY

























Run
Number


Ws*J- £

11 1977




VW St^J • {





Sample Description


• p -TfcioAX

\ — PoM *f~ - O f dt/T LfT r*2»(v*1 i«^«f ESry

M€7%«uj»i C^«.« R/wcr oP />^7f j
QM^<2T~t JIK-S'Jt ClLTOZ. •&- *JG>
Po 1 - CCUV/VIA) •«. Te.««»u':<>

(»>«<• E.5p - 10 ATEK SA^I PLE5 C^'M**S((^





3L.









iu L^T - ( f£*ces& ui/vren.)
OUTLET C Pietm tAsr ^ Hfsr fsp.)
BLO-DCW* U/ATOL rstw«.;

£v^c.u(«>Ttp FL^JK 5^Ai^tt5

( A< CCT Tt) l»K(f ESP
oort-er P*^H lotf ESP-

flCe~rt>'e Co**
/* ,'^J fff —

d^fu~^ C*&A . S**v*p -pr*

Of " N
Remarks





* At>S> fof/t!sCT)lU( C L.'lXS'V'^ft*'
•




C.< <"Ai&.n/u^ £iA5S'u>'jic£







'






#77-* 6t*Ss fi>tts(J*. fyc)









                          A-54

-------
IDENTIFICATION LOG OF SAMPLES COLLECTED
Plant Wisconsin st»ei worn* Battelle Record. Book No VJ 1 * f
Location ^icago. liiib- j





^/.








Sample Description


^ ^ POM-T-3

- THyRSMy
fterHYLe^cl e«u)/uoe Riw?e ^ p^^
$U4*.n TfSS^f Ficir^ /V'^ *?7
P0n rcc«/w« , ft.****. ^ %i#

3 - Pa M T - •

Mfe7»y(,€»l £?fJUn. 5

£*•" WATEI< SAMPLES

/»JLeT TD ESP
ooruer P(Z"£ j?tuff.tAfT/ti ttC. (?t»Sl
- ^£t^ — . ,
cUn^wij^T- i^t<^. -^ o^J^cU &&^

.of 	 .
Remarks





t AW0 O)N(tfvn*>t Ct^ii^r;^
•




A»*>> cifVtfnVt Gwdfju-'ATic



(CU&^K^^-S'Tt^





. ('ccrrvj^osr 7t^> ^




\6ftt>terfl*C{ .4-C '**•* '•'* -fi^~,'J-
ff 0(frL(T _ oU#r~ ~~~ 	

•




JIT:
                     A-55

-------
               IDENTIFICATION LOG OF SAMPLES COLLECTED
Plant       < ••.mala Steel WorkB
Location
Industry   r.
Project No.
                                 Battelle Record Book  No
                                 Collected 8, Recorded  By
                                 Page	of	.
EPA No'.  Date
577-001
Run
Number
Sample Description
Remarks
       MAY 1 5 1977
 340
                           R'WS£
                                                tAlf
 341
       Q
               vv
 313
 31 5
                       .  TEA/WAX
                           WATS'     SAMPLE-S
                        1 10 Le r - (
                           '• w^ rcfe. )
                                                    «n-#-^'
                      •dU^-tJET	PfcSrt(	£^
                      /\Cf.i(?r.C
                            . $**>**,  ff tt/lcT
               Otfltf
                                                 //
                                     A-56

-------
               IDENTIFICATION LOG OF SAMPLES COLLECTED
Plant     Wisoonain Steel Works
Location rcHoaio. Illinois
Industry  s ^2
Project No.
                        Battelle Record Book No  33
                        Collected & Recorded By
                        Page	of	.
EPA No.  Date
577-002
                Run
                Number
    Sample Description
            Remarks
                                TiSSw"    f'LTtft,  3
                                                2 00 v>.£ .B'^HOKk A*>1i  J AC U.J G. •'*'
 353
                                                                    P /s T/ i L n  /
                      f)eM>ve.i\*  - y ft a -2
      .
—   erf*
                            J   - y ft 0 2. c^rtv^v, •  -  g^A.
       tlK/77
                                   A-57

-------
SAMPLE IDENTIFICATION
         A-58

-------
              IDENTIFICATION  LOG OF SAMPLES COLLECTED
      International  Harvester
Plant Wisconsin Stell  Works                  Battelle Record Book No
tocat'ion_ChicaSOi -i-Hinois 6061?              Collected & Recorded Bv
Industry'coke ovens  ~                     Page 1  of 7	.
Project NO.-                         '
EPA No'. Date
.877-002-






•=501
302
303






304
305
306

















MAY 9
























Run
Number



Sample Description

PRE- SAMPLING CLEAN-UP

WSW-A-POM.t-CU (inlet to wet ESP)

tf//








MC«D *y
Remarks






Methvlene chloride rinse of probe and connecting glassw
Quartz tissue filter # 91
POM absorbing column # 221




WSW-E-POH.t-CU (stack)

















Methylene chloride rinse of pi
Quartz tissue filter # 9-2
POM absorbing column # 226










•









'obe and connecting glassv















are
are

                                    A-59

-------
              IDENTIFICATION LOG Of SAMPLES COLLECTED
       International Harvester
Plant  Wisconsin Stool Works                  Battelle Record  Book No  3328**
Location Chicago, Illinois 6o6l?              Collected & Recorded By  r-aytos
Industry  coke oven                           Page2   of 7  .
Project No.  G 2cJV2-
EPA No'. Date
S77-002-





30?
307A
308
309



310
310A
311
312
312W



Tl^
31^f
315



316
317




vlAY 1 0



























Run
Number


J3/>
Sample Description
»

Remarks

POM SPECIES COLLECTED BY MODIFIED METHOD FIVE
I»Eso*f (collected by Battelle')
WSW-A-POM.t- 1 (inlet side to wet ESP)











Methylene chloride rinse of probe and connecting glassware
Acetone rinse .of probe, etc. after MC rinse
Quartz tissue filter # 93
POM absorbing column, # 20°

WSW-B-POM.t- 1 (stack)




•















Methylene chloride rinse of t>r

filled with Tenax



obe'and connecting- classiv
Acetone rinse of probe, etc., after MC rinse
Quartz tissue filter # 9^
199
POM absorbing column, # p^
V/ater from first impinger only

-
filled with Tenax (-ueect ^


WATER SAMPLES COLLECTED FROM '.YET ESP, COMPOSITED


Inlet
Outlet, from both east and v.-es
Slowdown (at sewer discharge)
.
THREE LITER EVACUATED FLASK S£

Inlet
Outlet

	 A_fin 	



t ESP's

(gases composited i
...__...._ Tedlctr bag during
MPLES sampling period: i
sampling rate: IOC
start 12 no°Stop. 7:30pm


'
are
co]
n
cc/


-------
              IDENTIFICATION  LOG CF SAMPLES COLLECTED
       International  Harvester
Plant  Winconr.in Steel  Works                 Battelle Record Book No 3328**-
Location ciiicnro, Illinois 60617             Collected & Recorded By i-viy
Industry  coke oven                  •         page 5  of  7 «
Project No. ^ 2tt72
EPA No'. Date
S77-002-





318
318A
319
320



331
321A
322
323
323W



3?h
325
326



327
328




MAY i 1

















.
i








Run
Number


1977
Sample Description

Remarks

POM SPECIES COLLECTED BY MODIFIED METHOD FIVE
VVr

filled with Tenax



obe and connecting glassv;
Acetone rinse of probe, etc., after MC rinse
Quartz tissue filter # 96
POM absorbing column, # 203
V/ater from first impinger only


filled with Tenax
" — • •--• "" 	 — — 	

WATER SAMPLES COLLECTED FROM WET ESP, COMPOSITED


Inlet
Outlet, from both east and wee
Slowdown (at sewer discharge)

THREE LITER EVACUATED FLASK SJ

Inlet
Outlet

A 61



t ESP's

(gases composited i
	 .. Tedlar bag during
MPLES sampling period:
sampling rate: IOC
start 1030 stop. 1900



are
n
cc/nin


-------
              IDENTIFICATION LOG OF SAMPLES COLLECTED
       International Harvester
Plant  Wisconsin Steel Works                  Battelle Record Book No 3328*f
Location Chicago, Illinois 60617              Collected & Recorded By Baytos
Industry  coke oven                           Page  4-  Of  7 „
Project No.  ^ 2o72
EPA No'
S77-00;





329
329A
330
331



332
332A
333
33^
33*fW



^5
336
337



338
339


„ Date
3_


V1AY12



























Run
Number


1977
Sample Description

Remarks

POM SPECIES COLLECTED BY MODIFIED METHOD FIVE
T-tr

filled with Tenax



obe and connecting glassw
Acetone rinse of probe, etc., after MC rinse
Quartz tissue filter # 98
POM absorbing column, #205
Water from first impinger only


filled with Tenax


WATER SAMPLES COLLECTED FROM '.VET ESP, COMPOSITED

Inlet
Outlet, from both east and vies
Slowdown (at sewer discharge)

THREE LITER EVACUATED FLASK 5>£

Inlet
Outlet




t ESP's

(gases composited i
......... Tedlyr bag during
KPLES sampling period: i
sampling rate: IOC
start 0930 sto-D. 1830
'sampling stopped during


are
n
GC/IJIJ.J

                                   A-62

-------
              IDENTIFICATION LOG OF SAMPLES COLLECTED
       International Harvester
Plant  Wisconsin Steel Works                 Battelle Record Book No 33284
Location_Chicago,  Illinois 60617             Collected & Recorded ByBaytos
Industry  coke oven                          Page 5  of 7  .
Project No.  G 2072-5014              .
EPA No'. Date
S77-002-


t
t


340
340A
341
342



343
343A
344
345
345W



346
.,347
348



^ i

•2 r r>
>-?U




MY 1 3 1





























Run
Number


9-r •>
//
Sample Description

Remarks

POM SPECIES COLLECTED BY MODIFIED T-HCTHOD FIVE
FSipA^I (collected by Battelle^
WSW-A-POM.t- 4 (inlet side to wet ESP)






-




Methylene chloride rinse of probe and connecting glassware
Acetone rinse of probe, etc. af
Quartz-tissue filter #99
POM absorbing column, #204

WSW-B-POM.t- 4 (stack)














Methvlene chloride rinse of r>r
ter MC rinse
"

filled v/ith Tenax



obe and connecting: plassw
i
Acetone rinse of probe, etc., after KG rinse
Quartz tissue filter # 100
POM absorbing column, # 206
Water from first impinger only


filled with Tenax
i-- ---


WATER SAMPLES COLLECTED FROM WET ESP, COMPOSITED


Inlet
Outlet, from both east and wes
Slowdown (at sewer discharge)




t ESP's

(gases composited i
j-euj-ai1 uag, uurj.ng
THREE LITER EVACUATED FLASK SAMPLES sampling: period:








•fc o t r.
-,-.,-, , ^eQu-7i.
Inlel -"iied fo 	
Outlet i ^••^"'s r^j)
sampling rate: IOC

— o t a r fe 	 Etot>. '

uji




are
n
cc/

-------

              IDENTIFICATION LOG Of SAMPLES COLLECTED
      International  Harvester
      Wisconsin Steel  Works
Industry,
Project No,
              ovens
   Battelle Record Book No 33284
.   Collected & Recorded By
   Page 6  of 7 .__•
EPA No





351


352


353


354


355












. Date





















'








Run
Number



s*


























Sample Description


BLANKS


Quartz tissue filters, 3 ea.
#'s 88, 89, & 90

Methylene chloride, 200 ml
distilled in glass

Acetone 200 ml
distilled in glass

Demineralized dbl. distilled
water 200 ml

POM absorbing column, filled
Tenax, BCL # 220











Remarks





2500 QAST,
Pallflex Products Corpr
Putnam, .Conn. 06260

Burdick $e Jackson
Lot # 9452

Burdick & Jackscn
Lot # 9771

Prepared by Ohio State
Univ. Labs, Cat. # 97805

filled at Battelle













-------
              IDENTIFICATION LOG OF SAMPLES COLLECTED
Plant    Wisconsin Steel Worka
Location CM.C.TT>. Illinois
Industry G 2S72-5CU4
Project No.	
Battelle Record  Book No 33.28*f
Collected & Recorded By   u-iayfon
Page  7 of 7   .
EPA No'. Date
S77-002-






356



357
358
359

•




360



361


362







MAY ] 2











MAY I!













Run
Number

Sample Description

Remarks

POM SPECIES ABSORBED ON XAD-2

WSW-3
1977










WSW-if
51977













(collected by Clayton)

Inlet





.Single column, after filter and before 1st impinger

Outlet




Dual columns, after filter and before first im-pin^er
H?0 flush of base of XAD-2 tube
H20 blank




Inlet

Single column, betv/een 3d and

Outlet

Dual columns, between 3d and I


XAD-2 column, blank





.
. \



*)4fi impingers



 impingers







-------
                             TABLE 3.   ANALYSIS SCHEDULE OF WISCONSIN STEEL COKE OVEN  SAMPLES
CTi

;-:'.-.'!-:- ca— l'-
,c. v (O .---.- a' ^•-.••)'a' ••••- i-ji r

p77-OC2-301
1 -- V:77--,fi?-11.?
f. '•• 7- d!.-Z- "•.(;'.
i i . -. S77-M;2-'iW<
(V77-"02-3C7
^ :77-r,Ci2-"H)7.\
1 " ^:77-';r,i-y,o
1 - ' " '•!" ~-C3 •'- ^0'?
P7-M2-11U
ys77-r.Oi-3lCA
1 ' 1 -- \-,77-&:,2-';il
l 1 :;77-cc2-:j!i
: L " V/v-t.Ci-iL-,
f: 77- •."';:- -:2!
1 "" - \07-OU2-322
; ; - - ^77-002-323
/" -.7 ;-".••>- -OS
^77-OC2-y.O
/.r/7-(jo2-y.OA
1 " \r'7-co2-i-'a
f;77-002-3A1
(All.
for
	 ' e p-t°rnia.ion
(Inlet Prt-clrar.-uDl
;-'.i-thylcn'> filtr-r J 	 1
^^.' tt-nnx column 	 1
gjH«,,,,u,-i
-K— , J— ;
i-.un 2 O-.irltt
:-:..-t-iy)tni- c!:loride 1
f™ror J 	 X
r'2'j3 Lvnax column r?——.— .1
/!( Li:yl(-nc c'.iiorldc [
'•'•• i ij y i f-TT- chloride I
A-'.r'r'iuc- ! — j
Xf.hylane ci-.loridt 1
''"/'I '7.",: 	 1
",o l- liter J
••'2Ci tc-nax coiu-.n 	 1
r;-.'.-n A Out I fit)
v.c:!iylr-nt ci-.loridi-j
Acetonfi 	 1
'MOO iiltcr 1
l-'?.0fi r'-n.v. coltinm."— _1
""!'
I'uf
Future
(T?F)
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
l • ; ; . . -
<•"«• 	 1) .-,...,.. '""'•"
Analyses ts^^pin f^. :... . .t
(P0>0(a) (TPF)(b) (liN-f!)(c) Number Sample Information "?A "rr;^
Water San-.->los
1 -- -- S77-002-313 Run I WESP Inlet 1 I
1 — -- S77-ou:-3U Uun i i;i::;r Ouiii-t ; :
1 -- -- S77-002-32i Rim 2 UT.SP Ir.let 1 '.
i -- -- S77-002-3:1! i:mi : u;-sr >>uti<-'. '.
1 -- -- S77-002-335 Run 3 VE5P Inlet i
1 -- -- a/7-002-.lj!> Him 3 WIIUI' IV( K-t 1 : !
1 — -- S77-002-346 Run A UE3P Inlet ' I • 1
1 — -- S77-002-347 Kun '• \>':;S:' Outlet 1 ;
Bl.inki
^S77-002-351 'HOI filter (qu:rti>-
S77-002-352 Kethylcne chloride i 	 1 1
S77-002-353 Acetone J
11-- S77-002-335 '1210 tenax coUran '. '.
(Aliquot) ;.-,-.. '. ..''
An.il>-ses <:.,.,,,!„ .- .. ;-.... -..
(BSO)(d) (Tl'F)(b) Nun/aer Sa^le Inforat ton -r:. ..':.-'
1 1 S77-002-3?b i'2l5 .X-\D-2 column, win 3 Ir.'.c; ; 1
f S77-002-357 t^!t »ual :^M)-: colun.is,' Kur. 3 Outlet]
1 	 "2l7 1 ,
1 S77-002-353 K,0 Hush of collar., Run 3 .\i:i;-: j
1 1 S77-002-359 11,0 blank of H20 flush
I 1 S77-002-3uO *;07 :-u\u-2 tolu'.v.-.i. Ku:-. i !r.ii.t i
1 1 S77-002-361 li^in ®<-''3'L SAD- 2 c o 1 ur.-.r. } , Kun i Outlet :
1 1 S77-002-362 #212 XAD-2. column blank I 1
'a; ;'." C.-.T.?:-.--..-^ -- Ar.alyse for all listed in (Attachment A).
(O •'•"-'• • Jen?, r.achthylaalr.e and naphthalene.
'
-------
                    APPENDIX B




COMPLETE SAMPLING RESULTS WITH SAMPLE CALCULATIONS

-------
INLET RESULTS, WISCONSIN STEEL CO.
: RUN NO.
'•> TEST DATE
' SAMPLIN3 TIME, 2
5/11
1002
»»5DC
0.175
<»SO
29.55

1.69
3i»t». 3
86

331.2
73.0
3.5

1.03
0.99
.0
20.8
.0
79.2
-
28. P

28.7
0.85
90
48
-0.18
29.37
l»317
6«>DO

179696
191839
101.9
3
5/12
0921
1823
0.175
l»80
29.52

1.71
350.1
89

33i».6
73.0
3.5

1.02
0.99
.0
20.8
.0
79.2
• -
23. «

28.7
0.85
95
48
-C.18
29.3i»
«.l»D3
SUCO

18C992
195637
102.2
!»
5/13
2016
06Jt.
0.175
t»SD
29.35

1.57
3M.7
8«»

327.7
71.D
3,U

1.02
0.99
. 0
20.8
.0
79.2
-
28.9

28.7
0.85
9(»
48
-0.18
29.17
«»3?*
6<*3G

177622
192331
102.0
                                     B-l

-------
OUTLET RESULTS, HISCQKSIN STEEL CO.
RUN NO.
TEST TATE
SAMPLING TI*E, 2U HOUR CLOCK FcOh-
- ' - 	 TO
ON
TT
PH

V«
j*T.
I/H
VHGAS
Xtt
"BD
"X C02
X 02
"X CO
X N2
X EA
NMD
MW
'CP
TS
NP
PST
"PS
WS
OS
SAM"LIK'G NOZ2LE. DIAKFTER, IN.
NET TIKE OF TEST , HIN,
BAUOMETRTC PRESSUnL, IN. HG
ABSOLUTE
AVG. OxIFICE P*FSSU=E DROP,
IN. H20
VOLUME OF DRY GAS SAILED AT
METER CONDITIONS, DCF
AVG. GAS .ME.T-C TEMPERATURE, F
*OLU*L OF DRv GAS SAMPLED AT
"STANDARD CONDITIONS, "DSCF
TOTAL H20 COLLECTED IN IfPTNGE'RS
AND SILICA GEL, ML 	 	 	
VOLUME OF H20 VAFO^ COLLECTED , SCr
PERCENT MOISTURE IN STACK GAS
BY VOLUME
MOLECULAh FRACTION "F DRY GAS
VOLUMt PERCENT DRY 	 	
VOLUME PERCENT D"Y
VOLUME PF°CENT DRY "~
VOLUME PiRCENT D=Y
PERCENT EXCESS ATR
MOLECULAR WEIGHT OF STACK GAS,
DRY BASIS
MOLrCULA= HEIGHT OF STACK GAS,
HET 3ASIS
PITOT Tusi COEFFICIENT"
AVG. STACK 'TEM°£RA7U = E
NET SAMPLING POINTS
STATIC PRESSURE OF STACK GAS,
IN, HG.
STACK "GAS 'PRESSURE", 'IN. HG ASS.'
STACK GAS VELOCITY AT STACK
STACK AREA, SQ. .IN. _
DRY STACK GAS VOLUM'T^ic fLOW
RATE AT SIANOA'D CONDITI ONS, DSCrf
1
5/1-
ICtl
'1925
0.162
29. 5C
1.29
3C2.9
76
295.9
	 110. C
5.2

1.72
'0.96
.C
2u • 6
.C
79.2
28.6
26.6
u.85
62
48
.DC
29. FC
389C
. 7159. CL
190226
2
5/11
ICCl
1901
0.175
29.55
329.6
ICt
30 6.. 7
5.1
1.63
0.96
.C
2C.6
.C
79.2
28."
28.7
3. 35
73
48
.06
29.55
3960
'159.00
199999
3
5/12
0917
18*2
0.175
i»60
29.56
1.U5
332.0
1C1
31C.7
&.<•
2.C1
0. 99
oC
20.6
79.2
28.8
28.6
C.85
79
48
.CC
29.56
3961
7159.00
188526
t*
5/13
2017
06C9
C.17?
29. n
73?. 5
9C
315.2
160.6
7.6
2.3f
0.9c
,C
20.?
79.2
28."
23. t
0.8?
77
48
.CC
29. 3*
3967
7159. a
187091
 QA      STACK GAS VOLUMETRIC FLOW RATE
        AT  STACK CONDITIONS, AC.FM

 X I     PEPCENT  ISOK1NETIC
197779   19632C   197831    19796?

 _£6.9     99.6    1C1.9     10^.1
                                      B-2

-------
                    Sample Participate Calculations
                           Outlet  Run  No.  1


1.  Volume of dry gas sampled at standard conditions^3) , dscf
                            P
            17.7 x V (P  +-rr\)   17.7 x 303.9 ( 29.50 +
            _ m  P   JJ.D  _ _  .   _ oQr  Q j ^c
                 (T  + 460)      -        ( 78  + 460)         ' 295'9 dscf
2.  Volume of water vapor at standard conditions, scf
    V     = 0.0474 x V  = 0.0474 x 110.0  =   5.2  scf
     wgas             w
3.  Moisture in stack gas, percent

         100 x V
    7M = 	Vs  = 100 *  5.2
         V    + V       295.9  +5.2
          mstd   wgas
4.  Mole fraction of dry gas

    M  0 100 - °/
-------
 7.  Stack gas velocity at stack conditions(b), fpm



                                             1/2
     V  = 4,360 V AP  x (T  +460)  -—^-rrr
      s             s     s        P   x MW
          4,360 x 25.941
                         29.50  x  28.6)
                                      1/2
                        = 3890 fpm
 8.  Stack gas volumetric flow  rate  at  standard conditions,  dscfm
Q8 =
          °-123 X Vs X As  X Md  X Ps  _  0.123 x 3890 x 7159  x  0.98 x  29.50
T  + 460
 s
                                                 62 + 460
                                    =190226 dscfm
 9.  Stack gas volumetric flow rate  at  stack  conditions, acfm


                    v<


                   S    Q
10.  Percent isokinetic



          1,032 (Ts + 460)  x V_
                  S           m

          V  x T  x P  x M, x (D )
           s    t    s    d   v  n
                               std   =      1,032  ( 62 + 460) x  295.9


                                    "  389° X A8° X 29'5° X °'98 *  <°'182>2
                                    =  88.9
                              B-4

-------
       APPENDIX C




WET ESP WATER SAMPLE LOG

-------
Wisconsin Steel Works
Chicago,  Illinois
G 28721-5014
                Wet r.l ectrostncic Prccipjtntor Snmples


              Run Hun,b.r »*>' /  '               Date
              Composite of inlet water to V.'ESP - 1 qt Amber bottle
                             c*
                       S-n-ooi- 3/3             pOM Analyses
                                                 (Peter Jones)
              Composite of outlet water to V'BSP - 1 qt Amber bottle
                             D
                        $17-001- ~ 3IH           POM Analyses
                                                  (Peter Jones)
              Slowdown water - 1 qt Amber bottle (store)

                        j 77 - 00 2 - 3i f
                                    C-l

-------
Wisconsin Steel Works
Chicago.  Illinois
G 287 ;>»- 5Q14
                     Wot'  Electrostatic ProclpItntor Samples
                           wSiP - ^                         IUJAV i 1
                   Run Number    ^                   Date RftHT **
                   Composite of inlet water to VJESP - 1 qt Amber bottle

                                                      POM Analyses
                                                      (Peter Jones)
                   Composite of outlet water to WESP-- 1 qt Amber bottle

                                                       POM Analyses
                                                       (Peter Jones)
                   Blowdown water - 1 qt Araber bottle (store)
                                         C-2

-------
Wisconsin Steel Works
Chicago,  Illinois
G 2S72>-5C14
                 Wet  Electrostatic PrcclpiLnt:or  Samples

               p    M   .         -                       MAY
               Run Number
               Composite  of  inlet water  to WESP -  1  qt Amber  bottle

                    S 77 ^002- 33 f             POM Analyses
                                                  (Peter  Jones)
               Composite  of  outlet water  to WESP - 1 qt Amber  bottle

                                                  POM Analyses
               Slowdown  water -  1  qt Araber bottle  (store)
                                    C-3

-------
Wisconsin Steel Works
Chicago.  Illinois
G 2872^-5014
                Wet Electrostatic ProcipJ Entor  Samples

              Run Number  K5^ - V                Dat^A^ 1  3 1977


              Composite of  inlet water  to VJESP  -  1  qt Amber bottle
                        - -7 -7-00-     p          POM  Anaiyses
                                                  (Peter  Jones)
              Composite of outlet water  to VJESP  -  1  qt  Amber bottle

                                                   POM Analyses
                      S 77 -001 '  3*7           (Peter  Jones)
              Blowdown water -  1  qt Amber  bottle  (store)


                      577  -0°1~  3^   '
                      .'f' •'    ?S,l
                                   C-4

-------
         APPENDIX D




INTEGRATED GAS COLLECTION LOG

-------
Wisconsin Steel Works
Chicago. Ill
G 2872^-5014
                    Integrated  Bag  Gas  Sample




            Sampling Location   //t>M67   TO    £SP


            Bag Number   /"tcr	


            Evacuated Flask Number   S 77-002." 32-6


            Date
            Sample  Start Time     /O'3o * **

            Sample  Stop Time 	~^_
              Total Time  Samples
            Evacuated  Flask -  Keep in Dark
                               Benzene

                          Ethyne Acetylene
                               M ,
                         io corior; by oinnlo UL
                                 D-3

-------
Wisconsin Steel Works
Chicago,  Illinois
G 2S72-5C14
               Integrated  Bag Cos Sample




       Sampling Location  s   ^'	

       Bag Number
       Evacuated Flask Number   $7*7- &V2 " 327

                    1 1
       Sample Start Time

       Sample Stop Time
         Total Time Samples
       Evacuated Flask - Keep in Dark
                         Benzene

                    Ethyne Acetylene
                            x"
                            D-4

-------
Wisconsin Steel Works
Chicago,  Illinois
G 2372-5014
    - 3
                  Integrated  Bag  Gas  Sample
          Snmpling Location

          Bag Number
                                         ^ ^
         Evacuated  Flask  Number   S77-«?OT-~

         Date  MAY I 2 1977

         Sample  Start Time
          Sample Stop Time      /
-------
Wisconsin Steel Works

Chicago,  Illinois
G 2872>-5014
                 Integrated  Bag Gas Sample
         Sampling  Location  Q


         Bag  Number    &
         Evacuated  Flask Number  g 77 -QOl

         Date  MAY  1 2 1977


         Sample  Start Time 	^


         Sample  Stop Time 	'
           Total  Time Samples
         Evacuated  Flask - Keep in Dark
                           Benzene

                      Ethyne Acetylene
                               0)
                               fry
             Homologous aeries by single rR t>L
-------
    APPENDIX E




DAILY ACTIVITY LOG

-------
    ...v  Q
DATF.MW  9
                                                   Wisconsin Steel Worto

                                                   Chicago.  Illinois

                                                   G 28724-5014
                ,.-,,.
-  Pto.
                            E-l

-------
DATE
       MAY 1 0 W77 -
       WIAI i V A3//
                    fW
                                                              Wisconsin Steel  Works

                                                              Chicago. Illinois

                                                              G 2872^-5014
I o : a
                                                  I !/j<* r  "- R •

                                                  / y/§tO- /ft-
                                                                       - i

                                                                      ~ |
                c-v.
                                                               n "j."  P.
                                 ?••- •  •' •
                                     A/
                                      E-2

-------
                                          Wisconsin Steel Works
                                          Chicago,  in
                                          G 2872^-5014

    Ft-   to £ W -  2-
I)ATK  MAY 11 1977  - fl £*«* w -^                   Chicago, nlinoig
                 •^••\-, if-  •    .f
 / r ;•'
                                          /*W_V>   .
^ :'.'.! f!/i,
                                              .'•* t    - /•
                 E-3

-------
                                                            G 2872^-5014
r >•>•••
         f.*- /." JV ff  Hi
                               E-4

-------
  DATE
       MAY 1 3  1977
                                                                            G 2872*-50l4
              o*
V-'  •£'-'<•.  //)-. 'i-  /^r'.-c .1    OA^-,
                                   f>~  V-'  •'-'<•.  //)-. '-  /^r'.-c .1    OA^-,  ^..^  •&»••-.• •'•• '•

                                        '
                                        /r

/ .// j ."
     ./,.
                                        E-5

-------
            APPENDIX F




GASEOUS EMISSION LABORATORY RESULTS

-------
TABLE F-l.  FLASK SAMPLE IDENTIFICATION OF WISCONCIN STEEL
            COKE OVEN SAMPLES "
Flasks
1
2
3
4
5
6
7
Number
S77-002-31G
S77-002-317
S77-002-326
S77-002-327
S77-002-338
S77-002-339
Sample Informal ion
Inlet Run I, May 10, 1977
Outlet Run 1, May 10, 1977
Inlet Run 2, May 11, 1977
Outlet Run 2, May 11, 1977
Inlet Run 3, May 12, 1977
Outlet Run 3, May 12, 1977
(The seventh flask, an unused flask, should be
exposed to clean filtered air and analyzed as
a blank.)
                            F-l

-------
  PROJECT
                                    BATTELLE  MEMORIAL INSTITUTE
                                           COLUMBUS LABORATORIES
  DATE SUBMITTED

  SUBMITTED BY/_

  SECTION NO.
                                                                                  CARD NO../—' / -'->
                                  ANALYTICAL REPORT CARD CHEMD:  v ^ D  •-  "J

                                              , , _ 7," °F ANALYS1S: • *» D\ ^SSMS D^GMS.B" P. CHLM  D
                                  -' 'J'S ROOM
                                                                                                      / X-

                                                                                                     XRD D
                                                                         OM
                                                                                                     SIMS
                                                   APPROX. COMPOSITION
                                                          CO '.5 cr> ^
                                                   REMARKS
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SAMPLE NO.
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S.46413
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DESCRIPTION OF SAMPLE
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   OUAL'.TATIVE U
                     EEMl-O'JANT Q
                                        OUANT 13
   PROJECT
  DATE SUBMITTED I:	L_
SUBMITTED BY i.

SECTION NO.
   BATTELLE  MEMORIAL INSTITUTE
          COLUMBUS LABORATORIES

   ANALYTICAL  REPORT CARD
     ^  (,                TYPE OF ANALYSIS:
FXT "'•' '  " ROOM NO. •'' • -'-•:.-'' f_S
                                                                                                P  .I7'r>7
                                                                                                * '   .* ^"^ *
                                                                                     CARD NO. •-   *"	

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                                                                                            CMS Q''P. CKE//:
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                                                   APPROX. COMPOSITION

                                                   REMARKS * ' ^'r- "f^
SAMPLE NO.
!DO NOT FILL IN)
S^G-109

S-1G-110
/

S^P/411-.

S=3iR5:lS


DESCRIPTION OF SAMPLE
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                                          WHITE - RUPORT COPY     SYMBC>L'S-ON.-«EA/€-«S£rS1DE
                                         YELLOW ._ SUBDIVISION COPY                   ..
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                                                               REMARKS	 .' _.'	
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                                        OUANT
                                                 F-2

-------
              APPENDIX G

POM SAMPLING AND ANALYSIS USING THE
     SPECIAL POM SAMPLING TRAIN

-------
                     POM SAMPLING AND ANALYSIS USING THE
                           SPECIAL POM SAMPLING TRAIN
                                       Background

    Several years ago, the need for sampling and analysis of polycyclic organic material (POM)
arose on several programs at  Battelle. At that time the best available technology for sampling for
POM appeared to be some version of the  EPA Method  5 particulate  sampling train. Use of the
Method 5 sampling train produced inconsistent  POM  emission data  and led Battelle staff to ques-
tion the suitability of using this train for POM sampling. As a result, Battelle developed a POM
sampling train that retains many of the features and components of the Method 5 train, but which
incorporates an  additional  element  that serves to collect the majority of the POM in the gas
sample.

    Sampling for POM with the POM Sampling Train should be a straightforward procedure for
those already familiar and skilled with the operation of a Method 5 train for particulate collection.
The  POM  sampling procedure  utilizes   the  existing  Method 5  train,  but  also  includes  a
chromatographic adsorbent device (referred to as the adsorbent sampler). This additional compo-
nent,  and its auxiliary equipment, increases the time required  for setup, and requires  some ad-
ditional precautionary measures over those associated  with particulate  sampling alone, but the ad-
ditional effort and skill required to obtain  a meaningful  POM  sample is not appreciable and the
reliability of the  POM data obtained  is significantly increased.
                                     Sampling System
    The POM Sampling Train, as shown in Figure G-l, consists of a Method 5 train with an ad-
sorbent sampler  located between the filter and the impingers. Immediately after leaving the hot
filter, the gas sample passes into the cooling coil (120 x 0.8 cm) of the adsorbent sampler, and then
passes through a Pyrex frit and into a cylindrical column of Tenax adsorbent (7 x 3-cm diameter).
The  cooling coil and Tenax adsorbent  are maintained above the water dewpoint by means of a
thermostated circulating water bath. Thus, the incoming gases are cooled to maintain adsorbent ef-
ficiency, yet the adsorbent is maintained at a temperature which precludes condensation of water
vapor  present in all combustion effluents. The gases leaving the sampler are drawn through im-
pingers and a Drierite trap, dry gas meter, and leakless vacuum pump (as in Method 5 sampling).

     With the system, POM emissions can be determined from the analysis of the probe wash, filter
catch,  and adsorbent sampler catch. The impingers are only used to cool and dry the stack gases
before they enter the dry-gas meter. Laboratory tests, reported  later, have shown that  the probe.
filter, and adsorbent sampler  retain  all the POM, and that the POM can be recovered  during
analysis.

-------
Flue gas
flow '
               Probe
Filter
                                                                       Impingers
                                              Adsorbent
                                              Sampler
                                            Pump  Thermostated
                                                  Reservoir
                                                       00
                            FIGURE G-1. BATTELLE POM SAMPLING TRAIN

-------
                                          G-3
 Details of POM Absorber

     A schematic representation of the adsorbent sampler is shown in Figure G-2.The heat ex-
Changer section consists of 120 cm (4 feet) of 8-mm Pyrex tubing wound in approximately eight
 coils. The adsorbent is retained by an extra coarse Pyrex frit and a spring loaded glass wool plug,
 as shown; Tenax (35/60 mesh) is routinely used in the adsorbent trap of the  adsorbent sampler.
 The dimensions of the adsorbent section are 15-mm radius and 70-mm length. The 28/12 Pyrex
 joint on the inlet  to the sampler is compatible with the fittings commonly used in commercial EPA
 Method 5 sampling trains; the 15-mm Solv-Seal joint at the sampler outlet provides an efficient
 vacuum seal during sampling. (A 28/12 Pyrex joint could be used at the sampler outlet.) A vacuum
 hose coupling between the front sampler outlet and the impinger inlet is sufficient.
Adsorbent Sampler Temperature

     The collection efficiency of the adsorbent sampler is dependent on the temperature of the ad-
sorbent material. The optimum temperature of the adsorbent should be as low as possible without
condensing large quantities of water  vapor (present  in most stack gases) and plugging the adsor-
bent device. Generally, this temperature is 20 to 25 F (10 to 15 C) above the dewpoint of the stack
gases. For sampling gases that would consist primarily of vented air or products of combustion of
fossil fuels it has been  found that  125  F to  130  F (52 to 55  C)  is a satisfactory adsorbent
temperature.  Of course, the  adsorbent  temperature is  to  be  maintained at the  predetermined
temperature throughout the run to insure a continuous high POM collection efficiency.
 Auxiliary Equipment  .

     To  maintain the adsorber at  a  temperature above the dewpoint, a thermostated  controlled
 water bath  is used. A 10-C/min pump circulates water to the absorbent sampler from a 4-fi reser-
 voir.  An  acquastat  is  used to  control a  450-watt  heating  element to maintain  the  water
 temperature.  For stack gas temperatures up to at least 550  F (300 C)  and sampling rates  of 0.6
 scfm (0.017 Nm-Vmin) to 0.75 scfm (0.021 Nm-Vmin), the  heat loss from the water circulating loop
 to  the ambient  surroundings generally is greater than the heat gain from the stack gases to the
 water, so it usually is necessary to  supply auxiliary heat to  the water loop.  Although unlikely.
 depending upon the  conditions under which a  sample  is collected (at high  stack temperatures
 and/or high ambient temperature), it may be necessary to cool the circulating water to maintain
 the desired  temperature. A simple  calculation of the heat  transfer between the  gas sample and the
 circulating  water will determine whether or  not cooling  is needed.  If cooling is needed, an ad-
 ditional  cooling coil could  be inserted between the adsorbent sampler and the  reservoir.

-------
               FLOW DIRECTION
                    8-MM GLASS
                    COOLING COIL
GLASS WATER
JACKET
FRITTED STAINLESS STEEL DISC-

    15-MM SOLV-SEAL JOINT	
     FIGURE G-2.  ADSORBENT SAMPLING SYSTEM

-------
                                           G-5
                                          Sampling
     Sampling with the POM Sampling Train is conducted in essentially the same  manner  as
 sampling with the EPA Method 5 sampling train. The one difference between operation of these
"two sampling trains is that, in using the Battelle POM Sampling Train, it is desired to maintain the
 probe and  filter temperature at 350 F  (versus the  250 F when using the EPA sampling train).
'Maintaining the probe and filter at 350 F prevents  condensation and/or adsorption of SOj and
 POM on these components (followed by destructive reaction of SO3 with POM). Instead of being
 caught by the  probe and filter, the POM passes through these components and is retained in the
 absorbent sampler.

     When sampling for POM, the stack gases are sampled isokinetically as described in Method 5.
 (Isokinetic sampling is desired because some of the  POM may be physically associated with par-
 ticulate in the  gas stream.) The pressure drop  associated with the flow of stack gases through the
 adsorbent device may interfere  with maintaining an isokinetic sampling rate throughout the run,
 therefore it is usually a good idea to reduce the calculated nozzle size in order to reduce the flow
 rate and, thus, the pressure differential across the sampler.
                                Sample Recovery in the Field
                                  and Sample Preservation
     Polycyclic organic materials are readily photooxidized in the presence of ultraviolet light (and
possible visible light). Thus, the sampling train should be protected from sunlight and all other ul-
traviolet sources, both during and after sample collection. Also, some organic compounds which
are collected by the adsorbent sample may have an appreciable vapor pressure, and care must be
exercised  to minimize losses  of such  materials. To prevent loss of POM by phot.ooxidation, a
heavy dark  cloth is placed over the exposed sampling train glassware during sampling.  Immediate-
ly after sample collection is completed, the adsorbent sampler is sealed with ball-joint and Solv-
Seal stoppers and the filter and adsorbent sampler are stored in a cool  light-free container  for
transport  to the analytical lab.


     The probe and glassware up to the filter (including the filter holder) are washed with acetone
 followed by melhylene chloride*;  these solvents arc 'Distillcd-in-Ghiss' quality or hotter. The solu-
 tion and  paniculate matter from the probe rinse arc stored in a dark  (amber) glass bottle prior to
 analysis and kept cool.
  *To minimize evaporative sample loss during solvent extraction, solvents with very low boiling points arc used.

-------
                                          G-6
                              Sample Extraction and Recovery
     Sample  recovery from  the  POM  Sampling Train for POM analysis involves extraction  of
three separate portions of the total sampling train:

     (I) Probe and glassware up to the filter
     (2) Filter
     (3) The adsorbent sampler.

Initial recovery of Item (1) is done in the field (i.e., the probe is washed as described abovc)^ while
Items (2) and (3) are most conveniently extracted in the laboratory.
Sample Recovery from the Probe Wash

    The probe wash (a solvent and particulate mixture) is agitated for I  hour in an ultrasonic bath
before filtering off the solvent with a Whatman No. 40 filter.
Sample Recovery from the Filter

    Organic  material is extracted from the filter by means of Ebxhlet  extraction with methvlene
chloride ('Distilled-in-Glass'), or by ultrasonic agitation with methylene chloride followed by filtra-
tion using a Whatman No. 40 filter. While both methods have been found to be equally satisfac-
tory, ultrasonic extraction is somewhat faster.


Sample Recovery from the Adsorbent Sampler

    Great care must be taken not to expose the adsorbent sampler to polar solvents such as
methylene chloride or acetone, since the Tenax adsorbent is readily soluble in these solvents. Our
experience has shown that is it preferable to extract the adsorbent sampler with a low boiling point
hydrocarbon  such as pentane ('Distilled-in-GIass').

    To extract the adsorbent sampler, the two stoppers are first removed, and the extraction ap-
paratus assembled, as shown in Figure G-3,under yellow safe-lights. A double surface water cooled
condenser is preferred, the distilling flask is of 250-ml capacity. The adsorbent sampler is extracted
with 'Distilled-in-Glass' pentane. An initial volume of 180 ml is usually necessary since there is an
appreciable solvent holdup during extraction. The samplers are extracted with the continuous ex-
traction apparatus for 24 hours, and it is normal to experience a  small loss of pentane during this
period.  The  extraction  apparatus is then disassembled and  the pentane extract stoppered and
stored in darkness.

-------
                               G-7
           SOLVENT
           RETURN
           TUBE
                           TO CONDENSER
                                 f
                           TO  SOLVENT  FLASK
FIGURE G-3.  CONTINUOUS EXTRACTION ASSEMBLY FOR ADSORBENT SAMPLER

-------
                                            G-8
     Thus, three extracts are obtained from the adsorbent sampler-Method 5 sampling train:

     (1)  Acetone and methylene chloride probe extract
     (2)  Methylene chloride filter extract
     (3)  Pentane adsorbent sampler extract.

JThese extracts are sealed and kept in darkness while awaiting analysis.


                             Reactivation of Adsorbent Sampler
     Following extraction, air is drawn through the sampler with an aspirator to remove most of
the remaining pentane solvent. The sampler is then dismounted by withdrawing the stainless steel
spring with a hooked spatula, removing the stainless  steel perforated disk, discarding the glass
woo! plug, and emptying the almost dry Tenax into a clean glass container. The adsorbent sampler
body is cleaned by blowing with compressed air to remove any trace materials and then rinsed with
the following solvents in the order given:

     (1) Methylene chloride
     (2) Chromic acid
     (3) Water
     (4) Acetone
     (5) Methylene chloride
     (6) Pentane.

The sampler is then sealed with clean stoppers prior to  refilling with activated Tenax.

     Used pentane extracted Tenax may be  reactivated and thoroughly cleaned by placing it in an
oven at 200 C under nitrogen flow in a glass tube  for 24 hours. New Tenax  may be similarly
prepared by first  Soxhlet extracting with pentane for 24 hours and then heating under nitrogen. It
is generally desirable to maintain a small supply of activated Tenax, and to reactivate the  adsor-
bent from six  or more samplers at one time.

     An adsorbent sampler is  prepared by  filling the adsorbent  section with activated  Tenax to
within 3/4 inch of the top of the sampler while agitating the sampler with an electrical vibrator. A
clean glass wool plug is then inserted into  the neck,  followed  by a perforated stainless  steel disk
and the stainless steel retaining spring. The  sampler is then sealed with the appropriate 28/ 12 ball-
joint and  15-mm Solv-Seal stoppers and is ready to use.
                                    Analysis of Extracts
    The three extracts from the probe, filter, and absorbent samples, may be analyzed separately
for POM compounds, or they may be combined and a single POM analysis performed on the total
sample.

    Internal  standards  are added to the combined  extracts from each  sampling train prior to
volume reduction  by rotary evaporation and Kuderna-Danish evaporation.  The extract is sub-
jected  to a Rosen-type  liquid chromatography separation1 in  order to isolate the  POM fraction

-------
                                           G-9


before  carrying  out  gas  chromatographic-mass  spectrometric   (GC-MS)  analysis.  Gas
chromatographic separation is achieved using a 14-foot x 2-mm. 2'/2  percent, Dexil 300 column
programmed from 170 C to 350 C at 4 C min '. Separation of the benzpyrene isomers is routinely
accomplished  using  a one foot  1% N,N'-Bix (p-methoxy-benzylidene)-a,a -bi-p-toluidine column
isothermal at  130 C. Mass spectrometric analysis is carried out with a Finnigan 1015 quadrupole
mass spectrometer with a chemical ionization source; methane is routinely used as the carrier and
reagent gas.  Data acquisition is accomplished  with  a  System  Industries  150 data acquisition
system, and quantification of the  POM compounds present is accomplished  using a Digital  PDP8
computer.

     This mass spectrometric-computer quantification procedure makes use of specific absolute ion
currents.  The  bases  for  the  quantification  procedure  is  to   initially obtain the computer
reconstructed gas chromatogram and mass spectrum in the normal fashion; this reconstructed gas
chromatogram is then displayed on the CRT terminal and an  overlay for the  protonated molecular
ion of the POM of interest is superimposed. This overlay represents the ion current corresponding
to that specific POM molecular weight plus 1 mass unit. If there is an area in the reconstructed gas
chromatogram where the overlay indicates that this  mass number is prevalent, the mass spectrum
of this peak is displayed on the CRT unit, and the presence of the POM may be confirmed. If the
POM is found to be  present at a correct relative retention time to the internal standards, the com-
puter then sums the ion current  due to all important ions in the POM's mass  spectrum  which
represents the  area of the peak of interest. Quantification of each POM is achieved by ratioing its
ion current to  that of an internal standard of known concentration. The relative ionization efficien-
cies  of the internal standards and many POM species were previously determined, and the ap-
propriate factor is  used in quantification.

     This quantification technique overcomes the problems associated with interfering or overlap-
ping peaks and  poor base-line  separations  since these interfering species usually have different
molecular weights. Isomeric compounds such as pyrene and fluoranthrene  which have the same
molecular  weight  can be  quantified easily  since they are  very adequately separated by gas
chromatography and their order of elution is known.

     In order to obtain optimum sensitivity during  the gas chromatographic-mass spectrometric
analyses, the ionization voltage must ge adjusted at various stages during the analysis. This adjust-
ment necessitated the incorproation of three internal standards so that  an internal standard would
elute between each ionization adjustment. The internal standards chosen were 9-methylanthracene,
9-phenylanthracene, and 9,10-diphenylanthracene. It was fortuitous that 9,10-diphenylanthracene
elutes almost  coincident with the benz(a)pyrene/benz(e)pyrene isomers,  giving a very accurate
marker when searching for these important compounds. The relative retention times of other POM
species to one or more of the internal standards are generally sufficiently well known to permit
specific compound identification when the mass spectra are displayed.

     This ion integration technique has proven to be far superior to GC for the analysis and  quan-
tification of POM due to its very high selectivity; it also offers a very significant advantage in speed
of data handling.

-------
                                           G-10
                               Laboratory Validation Studies


     Preliminary experiments were carried out in order to determine the most suitable solvent for
extraction of the adsorbent sampler. Extraction was attempted with methylene chloride, acetone,
methyl alcohol, p-dioxane, pentane, cyclohexane, benzene, and toluene; only saturated hydrocar-
bons proved entirely suitable, on account of partial Tfenax solubility in more polar solvents. Pen-
tane was found to be the most suitable solvent, its high volatility minimized sample loss during ex-
traction. The relatively low extraction efficiency of pentane is overcome by  means of continuous
solvent extraction for a period of over 24 hours, as described above.

     Laboratory validation studies were performed  on the adsorbent sampler component  of  the
POM Sampling Train.  These validation  studies involved setting up an adsorbent  sampler, to
collect air drawn through a 500 F (260  C) tube  furnace. A precisely  measured  quantity of
polynuclear compounds in a few microliters of methylene chloride solution was then injected into
the inlet of the adsorbent sampler, and heated air was passed through the system for at least an
hour. Following solvent  extraction of the sampler, a suitable internal standard  was added, and
analysis for the spiked polynuclear compound was made by GC-MS analysis.

     Initial validation experiments  involved sampling and recovery  of measured quantities of
anthracene; during this work the temperature of  the sampler was allowed to rise to approximately
200 F (93 C), but quantitative anthracene recovery was always obtained.

     Subsequent validation experiments were carried out with the sampler at 130 F (55 C) using
pyrene, chrysene, perylene, benz(ghi)perylene, and coronene; these compounds are  representative
of commonly  encountered POM  species. Ten  thousand  ng of each of these  compounds was
separately sampled over a 2-hpur time period; following pentane extraction and addition of inter-
nal standard, each POM compound was quantified by GC-MS using specific absolute ion current
integration. The results  of several  representative laboratory validation experiments are .given in
Table G-l.
           TABLE G-l. RECOVERY OF POM FROM ADSORBENT SAMPLER
                                  Integration by GC-MS
POM
Pyrene
Chrysene
Perylene
Benz(ghi)perylene
Coronene
Spiked
(ng)
10,000
10,000
10,000
10,000
10,000
Sample #1
Average
% Recovery
91 ±3
90 ±5
91 ±4
101 ± 10
80 ± 7
Sample #2
Average
% Recovery
98 ±4
92 ±5
105 ± 5
106 ± 10
92 ±8
Sample #3
Average
% Recovery
104 ±4
106 ±5
102 ±6
103 ±7
100 ± 14

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                                       G-ll


                                    References

(1)  Moore, G. G., Thomas, R. S., and Monkman, J. L., /. Chromatog., 26, 456 (1967).

(2)  Neher, M. B., Jones,  P. W., and  Perry,  P. J., "Validation of the Battelle Adsorbent
    Sampler", Draft Final Report from Battelle-Columbus to Electric-Power Research In-
    stitute, 1977.

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