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
-------
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
-------
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
-------
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
-------
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.
-------
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.
-------
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
-------
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
-------
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.
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
S£L
/CO
lie
J/j
GAS WETER READING VELOCITY
HEAD
(Ap$), in. H20
ORIFICE PRESSURE
DIFFERENTIAL
(AH), in. H20)
34/.P
7. 0
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7 y, y
314,
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7
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-------
TRAVERSE
POINT
NUMBER
CLOCK TIME
SAMPLING
TIME, mm
CAS METER READING
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HEAD
lApj). in. H20
ORIFICE PRESSURE
DIFFERENTIAL
lAHl. in HjOl
DESIRED
ACTUAL
STACK
TEMPERATURE
iTsi.°F
DRYGASMETCR
TEMPERATURE
INLET
(Tm)."F
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in Hg
TEHPER^TtlRE.
°F
TEMPERATURE.
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j£
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( NUMBER _
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— 1
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C FACTOR.
PROBE HEATER SETTING
HEATER BOX SETTING
REFERENCE
1ATIC OF TRAVERSE POINT LAYOUT
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ORIFICE PRESSURE
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-------
TRAVERSE
POINT
NUMBER
CLOCK TIME
TlME.min
GAS METER READING
(Vmi. It3
VELOCITY
HEAD
tipi. in. H0
ORIFICE PRESSURE
DIFFERENTIAL
(AHl. in HOi
DESIRED
ACTUAL
STACK
TEMPERATURE
lTsi.°F
DRY GAS METER
TEMPERATURE
INLET
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OUTLET
PUMP
VACUUM.
in Hg
TEMPERATURE.
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TEMPERATURE..
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FIELD DATA
PLANT
DATE
~*r~/i/ /T
SAMPLING LOCATION.
SAMPLE TYPE
RUN NUMBER _____
OPERATOR,
PROBE LENGTH AND TYPE.
NOZZLE I.D £?/
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AMBIENT TEMPERATURE.
BAROMETRIC PRESSURE .
STATIC PRESSURE. (P)_
FILTER NUMBER ($) 35
ASSUMED MOISTURE, *
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PROBE HEATER SETTING.
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REFERENCE Ap
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TRAVERSE j
POINT
NUMBER
CLOCK TIME
GAS HETER READING
VELOCITY
HEAD
(4P,), in. H?0
ORIFICE PRESSURE
DIFFERENTIAL
(AH), in. H20)
DESIRED ACTUAL
STACK
TEMPERATURE
(T$),°F
DRYGASMETER
TEMPERATURE
INLET
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OUTLET
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COMMENTS:
EPA (Our) 235
-------
TRAVERSE
POINT
NUMBER
CLOCK TIME
SAMPLING
TIME. mm
CAS METER READING
VELOCITY
HEAD
iflpjl. in. H20
ORIFICE PRESSURE
DIFFERENTIAL
(AH), m H20:
DESIRED ACTUAL
STACK
TEMPERATURE
(T$i.°F
DRY GAS METER
TEMPERATURE
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PUMP
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in Hg
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77
77
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FIELD DATA
PLANT
DATE
SAMPLING LOCATION'
SAMPLE TYPE
RUN NUMBER
OPERATOR Jbfa^if
AMBIENT TEMPERATURE^
BAROMETRIC PRESSURE _
STATIC PRESSURE. (Ps)_
FILTER NUMBER (s)
PROBE LENGTH AND TYPE
NOZZLE i.o. a
ASSUMED MOISTURE, %
SAMPLE BOX NUMBER
METER BOX NUMBER
METER AHg
C FACTOR
PROBE HEATER SETTING.
HEATER BOX SETTING
REFERENCE Ap
SCHEMATIC OF TRAVERSE POINT LAYOUT
READ AND RECORD ALL DATA EVERY
MINUTES
TRAVERSE j
POINT i
NUMBER
CLOCK TIME
A
A
/?
T
M
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TIME,™
.?g.r
3/0
3 IS-
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x 7
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72.
72.
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-------
TRAVERSE
POINT
NUMBER
CLOCK TIME
TIME, min
CAS METER READING
.Vmi. It3
VELOCITY
HEAD
lAp). in. H
ORIFICE PRESSURE
DIFFERENTIAL
(AHl. in HjOl
DESIRED ACTUAL
STACK
TEMPERATURE
iTsi.°F
DRY GAS METER
TEMPERATURE
INLET I OUTLET
1
91
22-
33L
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17
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73
-------
FIELD DATA
PLANT
DATE
SAMPLING LOCATION
SAMPLE TYPE
RUN NUMBER
OPERATOR
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE
STATIC PRESSURE. (Ps)_
FILTER HUSBER (s)
PROBE LENGTH AND TYPE Y /°<4
NOZZLE I.D
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£L
COMMENTS;
EPA (Dur) 235
-------
TRAVERSE
POINT
NUMBER
TIME
SAMPLING
TIME, mm
CAS METER
.vm.. it3
VELOCITY
HEAD
DIFFERENTIAL
(4Hi. m H0i
DESIRED
ACTUAL
TEMPERATURE
(Tsi.°F
DRY GAS I
TEMPERATURE
INLET
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OUTLET
VACUUM.
in Ht
^fltfHl.^ BOA
TEMPERATURE.
°F
POM GAS
TEMPERATURE.
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fa,*
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12.0
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96
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-------
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PLANT Wi
GATE
SAMPLING LOCATION __
SAMPLE TYPE
RUN NUMBER
OPERATOR
PROBE LENGTH AND TYPE.
NOZZLE I.D
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE .
STATIC PRESSURE. (P$>_
FILTER NUMBER (J)
ASSUMED MOISTURE, %
SAMPLE BOX NUMBER
METER BOX NUMBER
METER AH0
CFACTOR
PROBE HEATER SETTING.
HEATER BOX SETTING
REFERENCE Ap
SCHEMATIC OF TRAVERSE POINT LAYOUT
READ AND RECORD ALL DATA EVERY.
MINUTES
TRAVERSE j
POINT j
NUMBER
CLOCK TIME
GAS METER READING
-------
TRAVERSE
POINT
NUMBER
CLOCK TIME
TIME, mm
GAS METER READING
VELOCITY
HEAD
(Apjl. in. HjO
ORIFICE PRESSURE
DIFFERENTIAL
(AH), in HjOl
DESIRED
ACTUAL
STACK
TEMPERATURE
(Tsi.°F
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TEMPERATURE
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PLANT.
DATE.
13
- 77
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SAMPLE TYPE
RUN NUMBER
OPERATOR
PROBE LENGTH AND TYPE
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ASSUMED MOISTURE, %
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METER BOX NUMBER
METER AHe
C FACTOR
/ 2.
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PROBE HEATER SETTING
HEATER BOX SETTING
REFERENCE AP
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CLOCK TIME
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-------
TRAVERSE
POINT
NUMBER
SAMPLING
TIME, mm
CLOCK TIME
l24-hi
CLOCK.
CAS METER READING
.Vi. It
VELOCITY
HEAD
(Apjl. in. HjO
ORIFICE PRESSURE
DIFFERENTIAL
I4HI. in HjO)
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STACK
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PUWP
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in Hg
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PLANT
DATE
SAMPLING LOCATION
SAMPLE TYPE
RUN NUMBER —r-T-
OPERATOR ^/^/-A ..
AMBIENT TEMPERATJffiE
BAROMETRIC PRESSURE
STATIC PRESSURE, (P).
FILTER NU'ilBER (J)
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ASSUMED MOISTURE. \
SAMPLE BOX NUMBER
METER BOX NUMBER
METER AHg
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SCHEMATIC OF TRAVERSE POINT LAYOUT
PROBE HEATER SETTING.
HEATER BOX SETTING
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MINUTES
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9-7
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77
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76
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°F
13 o
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-------
TRAVERSE
POINT
NUMBER
SAMPLING
TIME, mm
CLOCK TIME
hi
CLOCK>
^
CAS METER READING
.Vm.. II3
VELOCITY
HEAD
(Apl. in. H
ORIFICE PRESSURE
DIFFERENTIAL
liHi. in H20l
DESIRED
ACTUAL
STACK
TEMPERATURE
(T$i.°F
DRY GAS METER
TEMPERATURE
INLET
.°F
OUTLET
PUMP
VACUUM.
in Hg
TEMPERATURE.
°F
_imrlrHjUl '
TEMPERATURE.
C J
3
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FIELD DATA
PLANT
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PROBE LENGTH AND TYPE $
NOZZLE I-D. O.i?J
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SAMPLE TYPE
RUN NUMBER
OPERATOR
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AMBIENT TEMPERATURE
BAROMETRIC PRESSURE ,
STATIC PRESSURE. (PJ_
FILTER NUH8ER ($) _
ASSUMED MOISTURE. % .
SAMPLE BOX NUMBER,
METER BOX NUMBER.
METER AHg
C FACTOR __L
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PROBE HEATER SETTING.
HEATER BOX SETTING.
REFERENCE Ap_/Ja!
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31
SCHEMATIC OF TRAVERSE POINT LAYOUT
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TRAVERSE }
POINT
NUMBER
CLOCK TIME
GAS METER READING
(Vm). tf
VELOCITY
HEAD
(Ap,), in. H20
ORIFICE PRESSURE
DIFFERENTIAL
(AH), in. HZ0)
DESIRED ACTUAL
STACK
TEMPERATURE
(T$).°F
DRY GAS METER
TEMPERATURE
INLET
(Tmin).0F
OUTLET
PUMP
VACUUM,
in. HI
SAMPLE BOX
TEMPERATURE,
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210.
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-------
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POINT
NUMBER
SAMPLING
TIME,
CLOCK TIME
i24-hi
CLOCK,
CAS METER READING
iVi. II3
VELOCITY
HEAD
I4p). in. t<0
ORIFICE PRESSURE
DIFFERENTIAL
IAH). in HjOi
DESIRED ACTUAL
STACK
TEMPERATURE
iTsi.°F
DRY GAS METER
TEMPERATURE
INLET
.°F
OUTLET
lTi»ou«'-°F
PUMP
VACUUM.
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TEMPERATURE.
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-------
FIELD DATA
PLANT
DATE ir/10/77
PROBE LENGTH AND TYPE.
SAMPLING LOCATION
SAfoPLE TYPE
RUN NUMBER
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AMBIENT TEMPERATURE
BAROMETRIC PRESSURE .
STATIC PRESSURE, (Ps)_
FILTER NUMBER (s)
ASSUMED MOISTURE. %_£i_
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TRAVERSE
POINT
NUMBER
CLOCK TIME
l^-'1'
CLOCK)
GAS METER READING | VELOCITY
(Vm). It3 | HEAD
i (APS), in. H20
ORIFICE PRESSURE
DIFFERENTIAL
(AH), in. H20)
DESIRED | ACTUAL
STACK
TEMPERATURE
(TS),°F
DRYGASHETER
TEMPERATURE
INLET
(Tm ).°
OUTLET
PUMP
VACUUM,
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133
131
130
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119
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TRAVERSE
POINT
NUMBER
J3L
13-
r-J-X-
CLOCK TIME
JIME.min
ft'.Cl
^ffifr /7/.
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PS
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HEAD
lAps>. in. H20
I.FO
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1,30
1,30
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DIFFERENTIAL
IAHI. in H^Oi
DESIRED ACTUAL
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A?£
1, 10
110
l-lo
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1,20
1 20
1,5.0
:2.0
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1,3
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TEMPERATURE
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77
79
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133
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10.
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FIELD DATA
PLANT
DATE
SAMPLING LOCATION
SAMPLE TYPE
RUN NUMBER
OPERATOR
PROBE LENGTH AND TYPE § fa** //
NOZZLE I.D. -Ot /7iT ...._,
AMBIENT TEMPERATURE
BAROHETRIC PRESSURE
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DIFFERENTIAL
(4H). in. H20)
DESIRED
1,10
ACTUAL
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-------
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POINT
NUMBER
SAMPLING
T.,.r
TIME, mm
CLOCK TIME
GAS METER READING
iVm>. II3
VELOCITY
HEAD
Apjl. m. HjO
ORIFICE PRESSURE
DIFFERENTIAL
IAH). in HOi
DESIRED
ACTUAL
STACK
TEMPERATURE
iTsi.°F
DRY GAS METER
TEMPERATURE
INLET OUTLET
PUMP
VACUUM.
in H(
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TEMPERATURE.
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IMPINGER
TEMPERATURE.
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PLANT
DATE -£
SAMPLING -foCA/IOH C? O ~
SAMPLE TYPE f^ ^<
RUN NUMBER ,6??
OPERATOR Lr
PROBE LENGTH AND TYPE.
NOZZLE I.D. &, 77J~
ASSUMED MOISTURE, *
SAMPLE BOX NUMBER.
METER BOX NUMBER _
METER AH
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE
STATIC PRESSURE. (Pj)
FILTER DUMBER ($>
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C FACTOR
PROBE HEATER SETTING.
HEATER BOX SETTING
REFERENCE AP /> 6.
SCHEMATIC OF TRAVERSE POINT LAYOUT
READ AND RECORD ALL DATA EVERY.
MINUTES
TRAVERSE.
POINT
NUMBER
CLOCK TIME
GAS METER READING
og.it3
VELOCITY
HEAD
(Aps), in. H20
ORIFICE PRESSURE
DIFFERENTIAL
(AH), in. H20)
DESIRED
ACTUAL
STACK
TEMPERATURE
DRY GAS METER
TEMPERATURE
INLET
(Tmin!.0F
OUTLET
PUMP
VACUUW.
in. H{
SAMPLE BOX
TEMPERATURE,
IfilPINGER
TEMPERATURE,
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COMMENTS:
EPA (Our) 235
-------
TRAVERSE
POINT.
NUMBER
CLOCK TIME
TIME, mm
GW METER READING
3
VELOCITY
HEAD
(Apsl. in. H2
ORIFICE PRESSURE
DIFFERENTIAL
lAHi. m HOi
DESIRED ACTUAL
STACK
TEMPERATURE
(Tsi.°F
DRY GAS METER
TEMPERATURE
INLET
,n.
OUTLET
PUMP
VACUUM.
in Hg
SAMPLE BOX
TEMPERATURE.
IMPINGER
TEMPERATURE.
y-3,/
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tt',37
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ML
36 {,M?
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373.3
1,70
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1,70
1.70
77
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1*1,0
39.S.2.
.. v.
Joe
17 '.
17
!. 9
100
J&//S3
/AT
134
-------
FIELD DATA
PLANT 7£'-
DATE v5~7 / fl. '7
PROBE LENGTH AND TYPE
NOZZLE 1.0- O, /7,r
SAMPLING
SAMPLE TYPE
RUN NUIKBER
OPERATOR
3 -a
AMBIENT TEMPERATURE _£j
BAROMETRIC PRESSURE - &:
STATIC PRESSURE. (Pj)
FILTER NUMBER (s) ±
ASSUMED MOISTURE. % -3-
SAMPLE BOX NUMBER «£.
METER BOX NUMBER G
METER AH,
CFACTOR.
l.ffl.
I,
PROBE HEATER SETTING
HEATER BOX SETTING
REFERENCE *P
!• I,
SCHEMATIC OF TRAVERSE POINT LAYOUT
READ AND RECORD ALL DATA EVERY.
MINUTES
TRAVERSE
POINT i
NUMBER
CLOCK TIME
TIME.mln'
GAS METER READING
VELOCITY
HEAD
(AP,), in. H20
ORIFICE PRESSURE
DIFFERENTIAL
(AH), in. H20)
DESIRED ACTUAL
STACK
TEMPERATURE
(TS),0F
DRY GAS METER
TEMPERATURE
INLET
7.3
IS
jstfTW^.
-, c r o
/o
//&&
It?
30
,. 3.r
7
m//yf
70
7jr
m/.
ff.r
I/', at
loo
$.0.?
/.If
LJ1AL
MS-
Jf.O
flirt
SL
lib ,.r//.Y
JO-
25L
COMMENTS:
EPA (Our) 235
-------
TRAVERSE
POINT
NUMBER* ,
CLOCK TIME
TIME.min
GAS METER READING
'V- ll3
VELOCITY
HEAD
ORIFICE PRESSURE
DIFFERENTIAL
(AH), in HOi
DESIRED ACTUAL
STACK
TEMPERATURE
(T$i.°F
DRY GAS METER
TEMPERATURE
INLET
«Tminl.»F
OUTLET
PUMP
VACUUM.
SAMPLE BOX
TEMPERATURE.
IMPINGER
TEMPERATURE.
19-1
77
iir n\zi
Sff-f,
77
(07
1*1
\3L,o
/J<~
I' '.\ <• .
LtiL.
23-
l£JL
//*/.
Mi
IPS
JJLL
$3f> i
b^r
l^IL
l.sr
M£-
ML
,*.?
77
(e'P
(HO
I,
TL
3
I, re
77
lid
Ifi'l
u>
'
v
1,10
JJJL
-fcff
Ifi'b
7,0
•.i£
//A
7?
AV
17,0
6
1,5-0
7?
Id.o
US/fi?
-------
3
FIELD DATA
PLANT
DATE
P-/ i7 '/
PROBE LENGTH AND TYPE 8 ^
>,17!>-
SAMPLING LOCATION
SW.'.PLE TYPE __J^
RUN NUW8ER 3 -<
OPERATOR
AMBIENT TEMPERATURE
BAROKETRIC PRESSURE.
STATIC PRESSURE. (P,)_
FILTER NUMBER (»)
NOZZLE 1.0..
ASSUMED MOISTURE. %
SAMPLE BOX NUMBER.
METER BOX NUMBER _
METER Ah
C FACTOR
PROBE HEATER SETTING
HEATER BOX SETTING
REFERENCED //
SCHEMATIC OF TRAVERSE POINT LAYOUT
READ AND RECORD ALL DATA FVFRY
MINUTES
TRAVERSE
POINT
NUMBER
CLOCK TIME
-9
tf—*
£L
SAWPLING
TIME.min
MrO
fl'./t,
£70
Jtf',3.1
/f
.!&
/f-
ML
/7
$-$0
Wtf't,
ass
O
il!
-------
TRAVERSE
POINT
NUMBER
SAMPLIKC
TIME, mm
CLOCK TIME
CLOCK.
CAS METER READING
'V-1'
VELOCITY
HEAD
(Apj). in. H^O
ORIFICE PRESSURE
DIFFERENTIAL
(AH), in HOl
DESIRED ACTUAL
STACK
TEMPERATURE
(TS».°F
DRY GAS METER
TEMPERATURE
INLET OUTLET
PUMP
VACUUM.
m Hg
' SAMPLE BOX
TEMPERATURE.
IMPINGER
TEMPERATURE.
MOU
L/TT<=
Z.
10
38//P3
/3
,
l< IP
It!
m.
i&L
ILL
',HW
/v
91
1 <,'&(•>
102
lit-H
1*3
W, 7
110
IM(/v*
7/v) -5
//,-./ v ;>
?.-£>
It,
170
7/3
Hfffi
!(•,
ifil
zi^5:
uo
V?
IS
till!
in
108
no
Jli
17 i
hi*
mo
llO
J
-------
FIELD DATA
PLANT
DATE J-//P./77
SAMPLING LOCATION
SAMPLE TYPE A*7/1/
RUN NUMBER' 3
OPERATOR c*jZf>iJi1
ASSUMED MOISTURE. *
SAMPLE BOX NUMBER.
METER BOX NUMBER.,
METER
AMBIENT TEMPERATURE'.
BAROMETRIC PRESSURE .
STATIC PRESSURE. (P )_
FILTER NUMBER (»)
'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/_
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PROJECT
DATE SUBMITTED I: L_
SUBMITTED BY i.
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BATTELLE MEMORIAL INSTITUTE
COLUMBUS LABORATORIES
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-------
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
-------
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.
------- |