United States
Environmental Protection
Agency '
Office of Air Quality EMB R6POrt 80-BYC-T
Planning and Standards March 1981
Research Triangle Park NC 27711
Air
Benzene
Coke Oven By-Product
Plants
Emission Test Report
Bethlehem Steel
Bethlehem,
Pennsylvania
-------
vvEPA
United States
Environmental Protection
Agency
Office of Air Quality EMB Report 80-BYC-l
Planning and Standards MiTCh 1981
Research Triangle Park NC 27711
Air
Benzene
Coke Oven By-Product
Plants
Emission Test Report
Bethlehem Steel
Bethlehem,
Pennsylvania
-------
SET 1957 05 1280
BENZENE SAMPLING PROGRAM
AT COKE BY-PRODUCT RECOVERY PLANTS:
BETHLEHEM STEEL CORPORATION
BETHLEHEM, PENNSYLVANIA
EPA Contract 68-02-2813
Work Assignment 48
ESED Number 74/4J
Prepared For:
Mr. Daniel Bivins
U. S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Emission Measurement Branch, ESED, MD-13
Research Triangle Park, North Carolina 27711
March 1981
SCOTT ENVIRONMENTAL SERVICES
A Division Of
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
Plumsteadville, Pennsylvania 18949
Scott Environmental Technology Inc.
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TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1-1
2.0 SUMMARY OF RESULTS 2-1
3.0 RESULTS AND DISCUSSIONS 3-1
3.1 COOLING TOWER 3-1
3.2 TAR DECANTER 3-4
3.3 LIGHT OIL CONDENSER VENT 3-6
3.4 NAPHTHALENE DRYING TANK 3-8
3.5 DENVER FLOTATION UNITS 3-10
3.6 NAPHTHALENE MELT PIT 3-14
4.0 PROCESS DESCRIPTIONS 4-1
5.0 FIELD SAMPLING AND ANALYSIS METHODOLOGY 5-1
5.1 DETERMINATION OF BENZENE FROM STATIONARY SOURCES:
EPA METHOD 110 AND MODIFICATIONS 5-1
5.2 TRACER TESTING 5-4
5.3 SAMPLE HANDLING 5-4
5.4 FIELD ANALYSIS 5-5
6.0 FIELD SAMPLING PROCEDURES 6-1
6.1 COOLING TOWER-DIRECT WATER FINAL COOLER 6-1
6.2 TAR DECANTER 6-3
6.3 LIGHT OIL CONDENSER VENT 6-5
6.4 NAPHTHALENE DRYING TANK 6-7
6.5 DENVER FLOAT UNITS 6-11
6.6 NAPHTHALENE MELT PIT 6-16
7.0 LABORATORY SAMPLE ANALYSIS 7-1
7.1 SAMPLE PREPARATION 7-1
7.2 PURGE AND TRAP PROCEDURE FOR EXTRACTION OF BENZENE FROM
LIQUID PHASE TO GASEOUS PHASE 7-2
7.3 GAS CHROMATOGRAPH 7-4
8.0 QUALITY CONTROL AND QUALITY ASSURANCE 8-1
8.1 FIELD ANALYSIS PROCEDURES 8-1
8.2 PROCEDURES FOR ANALYSIS OF PROCESS LIQUIDS 8-2
Scott Environmental Techndosy Inc
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Table of Contents
(Continued)
Page
APPENDIX A - SAMPLE CALCULATIONS A-l
APPENDIX B - FIELD DATA SHEETS B-l
APPENDIX C - LABORATORY DATA SHEETS C-l
APPENDIX D - TRACER GAS METHOD DEVELOPMENT D-l
APPENDIX E - FIELD AUDIT REPORT E-l
APPENDIX F - PROJECT PARTICIPANTS . . . F-l
APPENDIX G - EPA METHOD 110 G-l
Scott Environmental Technology Inc.
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SET 1957 05 1280 Page 1-1
1.0 INTRODUCTION
Scott Environmental Services, a division of Scott Environmental
Technology, Inc. conducted a testing program at Bethlehem Steel Cor-
poration, Bethlehem, Pennsylvania to determine benzene emissions from
six sources in the coke byproduct recovery plant. The work was per-
formed for the United States Environmental Protection Agency, Emissions
Measurement Branch, under Contract No. 68-02-2813, Work Assignment 48.
Data collected from this plant and six others are being used for the
development of a possible National Emission Standard for Hazardous
Air Pollutants for benzene.
Sampling was conducted at Bethlehem Steel from July 7th to
24th, 1980. Integrated air samples and liquid samples for benzene
analysis were collected from the following processes: Denver
flotation unit, naphthalene melt pit, naphthalene drying tank,
cooling tower - direct water final cooler, light oil condenser vent, and
the tar decanter from #5 battery.
Scott Environmental Technology Inc.
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SET 1957 05 1280
Page 2-1
Process
Cooling Tower
Tar Decanter
Light Oil Condenser Vent
Naphthalene Drying Tank
Denver Float Units
Naphthalene Melt Pit
2.0 SUMMARY OF RESULTS
Benzene Emission Rate
Ib/hr. kg/hr.
73.4 33.3
2.6 1.2
28.8 13.1
0.04* 0.02*
28.2 12.8
19.8* 9.0*
*Not a continuous process.
Scott Environmental Technology Inc.
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SET 1957 05 1280 ' Page 3-1
3.0 RESULTS AND DISCUSSIONS
3.1 COOLING TOWER
The cooling tower circulates the hot water from the direct water
final coolers after the naphthalene is removed via the Denver float units.
The tower is about 30 feet high and has four 13-foot diameter fans on top
for pulling air countercurrent to the falling water. Benzene which is
contained in the final cooler water is in part released as a vapor as it
passes downward through the cooling tower. This benzene is picked up as
a contaminant in the final cooler spray towers.
The three tests run on the cooling tower were fairly consistent,
ranging from 66 to 79 lb/hr., with an average result of 73.4 Ib/hr. The
stack velocities for each run reported in Table 3-1 are an average of the
velocities measured across the 24-point traverse. The velocities measured
were generally lower near the stack wall and in the center over the hub of
the fan, as would be expected. Field data (showing the measured velocities)
can be found in Appendix B.
All stack flow rates were corrected to the average conditions at
which the benzene concentrations were measured in the Tedlar bags; assumed
to be saturated at 68°F and 29.92 inches Hg (2 1/2 % moisture). Example
calculations are shown in Appendix A.
Liquid samples were collected from the hot and cold wells. Average
benzene concentrations were 6.8 ppm and 3.5 ppm respectively. The hot and
cold well temperatures were 86°F and 82°F, indicating that the cooling tower
was not really cooling the water significantly, and as noted on page 6-1,
Scott Environmental "fechnotasy Inc
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TABLE 3-1
COOLING TOWER DATA SUMMARY
Process: Cooling Tower-direct water final cooler Stack Diameter: 13
Plant: Bethlehem Steel, Bethlehem, PA Stack Area: 133 ft.
Flowrate Flowrate
Stack Barometric Stack Stack Standard
feet (1 of 4 stacks)
2
Benzene Benzene
Concen- Emission
vo
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Run
No.
1
2
3
Sample Temp.
Date Period °F
7/10/80 1034-1140 84
7/10/80 1150-1255 84
7/10/80 1417-1520 83
Standard conditions: Saturated
LIQUID
Sample
SAMPLE DATA SUMMARY
Location
Hot Well
Cold Well
Pressure
(in. Hg)
29.58
29.58
29.56
at 68°F,
Date
7/10/80
7/10/80
Velocity
(ft/min.)
870
905
860
29.92 in Hg.
Time
15:40
15:45
Conditions Conditions
(ACFM) (SCFM)
115,000 109,000
120,000 114,000
114,000 108,000
Sample Temp.
86°F
82°F
tration
(ppm)
12.56
14.38
14.27
Benzene
(ppm by
I'.l] AV<
3-2) .
Rate g
(Ib/hr) °
1 Fan 4 Fans
16.6 66.2
19.9 79.5
18.6 74.5
Ave.
73.4
Concentration
weight)
jrage 6.8
TO
(C
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SET 1957 05 1280 Page 3-3
was due to the malfunction of a faulty level control. Past plant operating
experience shows that an average temperature reduction from 86°F to 76°F is
experienced during the summer months and from 62°F to 48°F during the
winter months.
Scott Environmental Technolosy Inc.
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SET 1957 05 1280 Page 3-4
3.2 TAR DECANTER
The. tar decanter collects tar and flushing liquor from the #5
battery and from the primary coolers. It is allowed to settle and the
flushing liquor is decanted off the top while the tar is drained from the
bottom. The decanter is vented to the atmosphere, and is a potential
benzene emission source.
The average result for the tar decanter emissions is 2.6 lb/hr.,
with a range of 1.4 to 3.7 lb/hr. Velocities measured were quite consistent
over all three runs but the concentration of benzene differed considerably,
as shown in Table 3-2. The large differences between sample runs is
probably due to fluctuations or changes in the process feed streams, as
the samples were not all collected on the same day.
Liquid samples were collected at three locations: The surface
liquid in the decanter, the inlet to the decanter from the coke gas cross-
over main from the #5 battery, and the inlet to the decanter from the
primary cooler. Average benzene concentrations in the liquid samples were:
In the surface samples - 1.6 ppm, in the crossover main samples - 4.9 ppm,
and in the primary cooler samples - 16.4 ppm in the light fraction (flushing
liquor) and 1810 ppm in the heavy fraction (tar).
Scott Environmental Technology Inc.
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%^ TAR DECANTER DATA SUMMARY
Jv Process: Tar Decanter - #5 battery
^ Plant: Bethlehem Steel, Bethlehem, PA
1
t Stack Barometric
Run Sample Temp. Pressure
No. Date Period (°F) (in.Hg)
? 1 7/8/80 1453-1523 158 29.53
2 7/9/80 1020-1121 161 29.71
3 7/9/80 1530-1600 163 29.67
Standard Conditions: 68°F, 29.92 inches Hg.
LIQUID SAMPLE DATA
Sample Location
Flushing liquor on surface
Flushing liquor inlet from coke
gas crossover main
Inlet to decanter from primary cooler
Heavy fraction (tar)
Light fraction (liquor)
Stack Diameter: 10-1/8"
2
Stack Area: 0.559 ft.
Stack
Velocity
(ft/min.)
500
490
490
Date
7/8/80
7/8/80
7/9/80
7/9/80
7/9/80
Flowrate
Stack
Conditions
(ACFM)
280
275
280
Time
1525
1600
1415
1545
1545
Flowrate Benzene
Standard Concen-
Conditions tration
(SCFM) (ppra)
170 1447.2
160 717.8
150 1975.0
Sample Temp. ( F)
176
180
N.A.
140
140
Benzene
Emission
Rate
(Ib/hr)
2.9
1.4
3.6
Ave.
2.6
Benzene Cone.
(ppm by Weight)
5.6
4.2 Ave. 4.9
1.6
1736
1888 Ave*
16.4 . ., ,
16.3 Ave' 16'4
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SET 1957 05 1280 Page 3-6
3.3 LIGHT OIL CONDENSER VENT
Benzene in the wash oil is removed by heating the wash
oil and condensing out the benzene. Noncondensibles in the wash
oil, possibly including some benzene, are vented to the atmosphere.
For this reason the light oil condenser vent was considered a
potential benzene emission source.
The average of the three good runs on the light oil
condenser vent (Run 3 was voided) was 28.8 lb/hr., as shown in
Table 3-3. Although the flow rate was very low, the benzene con-
centration was approximately 10% so the mass emission rates were
comparable to higher flow sources.
Scott Environmental Technology Inc.
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n
5T
TABLE 3-3
LIGHT OIL CONDENSER VENT DATA SUMMARY
Process: Light Oil Condenser Vent Stack Diameter: 6"
Plant: Bethlehem Steel, Bethlehem, PA Stack Area: 0.20 ft,
*Run 3 not included in calculations due to sampling system leak.
Standard Conditions: Saturated at 68°F, 29.92 in. Hg.
NOTE: No liquid samples were taken at this source.
w
H
Run
No.
1
2
3
4
Date
7/11/80
7/11/80
7/11/80
7/11/80
Sample
Period
1015-1045
1056-1126
1212-1242
1600-1630
Stack
Temp.
(°F)
95
96
109
104
Barometric
Pressure
(in. Hg)
29.51
29.51
29.51
29.49
Stack
Velocity
(ft/min.)
120
130
120
120
Flowrate
Stack
Conditions
(ACFM)
24
25
23
24
Flowrate
Standard
Conditions
(SCFM)
23
23
21
22
Benzene
Concen-
tration
(ppm)
91,900
109,800
53,300
110,500
Benzene
Emission
Rate
(Ib/hr.)
25.3
31.1
*
29.9
Ave.
28.8
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SET 1957 05 1280 Page 3-8
3.A NAPHTHALENE DRYING TANK
The drying tank collects the melted naphthalene after
the melt process, and steam is applied to the tank to drive off any
water present in the naphthalene. This is a batch process and runs
for approximately 12 to 14 hours, during which time benzene is
emitted along with the steam, through the open process vents on the
tank.
Testing the" naphthalene drying tank involved a special test
modification using impingers which is described in detail in Section
6.4. The test method was given a trial run on July 18, and the
resulting total emission rate (stack plus vent) was 1.57 Ib/hr. A
series of 8 tests were run on July 22 over a 15-hour period, and the
average for these runs was 0.04 Ib/hr. The results of the 8 tests
varied widely since the drying cycle is a batch process. As expected,
the emissions dropped off as the cycle progressed and the water was
driven off the naphthalene, and emissions increased when the tank
temperature increased, as seen in Table 3-4. Vent "A" refers to the
process vent stack, and "B" is the large opening in the tank for steam
lines, which was tested as a vent.
The benzene emissions from the drying tank vary widely from
day to day depending on how long the naphthalene was heated in the
melt pit prior to transferral to the drying tank. Ideally the melt
process and the drying tank should be sampled on the same day to de-
termine benzene emissions from the naphthalene handling processes as
a whole.
Scott Environmental Technology Inc.
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TABLE 3-4
NAPHTHALENE DRYING TANK DATA SUMMARY
Process : Naphthalene Drying Tank
Plant: Bethlehem Steel, Bethlehem, PA
Run
No.
T
1
2
3
4
5
6
7
8
Date
7/18/80
7/22/80
7/22/80
7/22/80
7/22/80
7/23/80
7/23/80
7/23/80
7/23/80
Test
Period
1353-1423
1337-1410
1610-1640
1813-1843
2130-2200
2415-2445
0220-0300
0255-0320
0404-0455
Stack
Temp.
206
209
210
202
195
192
190
210
199
Stack
Velocity
(fpm)
A B
630 350
850 610
730 110
690 *
590 *
540 *
590 *
780 100
660 *
Stack Diameter: A:
Stack Area: A:
Barometric Pressure
Stack
Flowrate
(ACFM)
A
120
170
140
140
110
110
120
150
130
B Total
560 680
980 1150
170 310
* 140
* 110
* 110
* 120
250 400
* 130
6" B: 22"
0.196 ft2 B: 1.6 ft.
: 29.5 in. Hg.
Standard Benzene
Flowrate Concen-
(SCFM) tration
Total (ppm)
71
106
3
18
27
27
34
14
22
1824
168.60
428.11
32.34
16.09
40.78
45.40
218.16
117.05
Benzene
Emission
Rate
(Ib/hr.)
1.57
0.217
0.016
0.007
0.005
0.013
0.019
0.037
0.032
Ave. 0.043
to
W
H
Ui
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OO
O
Standard Conditions: Saturated at 68 F, 29.92 in. Hg.
NOTE: No liquid samples were collected at this source.
* No flow detected with anemometer.
Pi
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SET 1957 05 1280 Page 3-10
3.5 DENVER FLOTATION UNITS
The Denver units skim naphthalene from the surface of the
hot water collected from the final coolers. The skimming is accom-
plished by blades rotating on a shaft that spans the length of the
flotation tank. The system is comprised of four adjacent units, three
of which are in operation at any given time. This is a constant
operation and constitutes a potential benzene emission source because
the impure naphthalene is contaminated with benzene and the Denver
units are agitated and at temperatures above ambient level.
The results of the tests of the Denver float units are
presented in Table 3-5. The tracer gas sampling strategy and sampler
locations for each test are detailed in Section 6.5. Each test
consisted of two runs, with the second run designed to estimate the
contribution of the unit adjacent to the test unit (#2) to the
total being measured from the test unit (#1). This became irrelevant
in tests 2 and 3 because unit 2 was not in operation.
In tests 2 and 3 the data from sampler 3 was rejected
because the sampler was inadvertently located adjacent to a "hot
spot" benzene emission point in the naphthalene melt pit.
In each test the benzene/isobutane ratio is lower for the
center sampler than the outer samplers. This would be expected
because the tracer discharge manifold was not long enough to cover
the entire tank axis. Thus, the center portion of the tank shows a
higher relative isobutane concentration.
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SET 1957 05 1280
Page 3-11
TABLE 3-5
DENVER FLOAT UNITS
Test 1, Run 1
Tracer on Tank //I
Isobutane release rate - 1.39 Ib/hr
Denver Units Operating: 1, 2, 3
Date: 7/8/80
Test Start: 11:24
Sample
Loc.
1
2
3
Cone, of
Benzene
(ppm)
3.51
8.61
14.51
Cone, of
Isobutane
(ppm)
0.50
1.72
2.02
Mass to Mass
Ratio d>/ic,
1 4_^
9.38
6.73
9.66
F*
Ib/hr
Benzene
0.739 9.60
0.789 7.35
0.665 8.91
kg/hr
Benzene
4.36
3.34
4.05
Test 1, Run 2
Tracer on Tank #2
Isobutane. release rate - 1.25 Ib/hr
Avg. 8.62 Avg. 3.92
Date: 7/8/80
Test Start: 12:09
1
2
3
3.03
7.69
16.61
0.15
0.40
1.13
Test 2, Run 1
Tracer on Tank #1
Isobutane release rate - 1.27 Ib/hr
Denver Units Operating: 1, 3, 4
Date: 7/15/80
Test Start: 10:30
1
2
3
5.16
5.42
18.96
1.02
1.09
1.16
6.80
6.68
21.94**
1.00 8.64
1.00 8.48
1.00 27.86**
3.93
3.85
12.66**
Test 2, Run 2
Tracer on Tank #2
Isobutane release rate - 1.25
Avg. 8.56 Avg. 3.89
Date: 7/15/80
Test Start: 11:19
1
2
3
4.42
5.68
18.45
0.20
0.48
2.40
* Fraction from Tank #1.
** Data rejected, interference from another source.
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SET 1957 05 1280
Page 3-12
Table 3-5
(Continued)
Test 3, Run 1
Tracer on Tank #2
Isobutane release rate - 1.28 Ib/hr
Denver Units Operating: 1, 3, 4
Date: 7/15/80
Test Start: 13:30
Sample
LOG.
1
2
3
Cone, of
Benzene
(ppm)
7.13
8.39
14.00
Cone, of
Isobutane
0.22
0.50
1.97
Mass to Mass
Ratio 4>/ic,
F*
Ib/hr
Benzene
kg/hr
Benzene
Test 3, Run 2
Tracer on Tank 1
Isobutane release rate 1.28 Ib/hr
Date: 7/15/80
Test Start: 14:00
1
2
3
6.64
7.16
13.67
0.95
1.26
1.24
9.45
7.66
14.83*
1.00
1.00
1.00
12.10
9.80
18.98**
5.5
4.45
8.63**
Avg. 10.95 Avg. 4.98
* Fraction from Tank #1.
** Data rejected, interference from another source.
Scott Environmental Technology Inc.
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SET 1957 05 1280 Page 3-13
The benzene emission rates for a typical Denver Float Unit
tank were determined to be 8.6, 8.6 and 11.0 pounds per hour. While
statistical determination of confidence limits is not possible, the
relative good agreement of data points and the small estimated error
due to the assumptions made in the calculations lead to the judgment
that the emission rates are within one pound per hour of the true rate
at each process/ambient condition tested. The total emissions from the
Denver unit with three tanks in operation would be 26, 26 and 33 pounds
per hour.
Test 3 was performed on the same day as Test 2 and under the
same experimental conditions except that the ambient temperature was
approximately 5 F higher in Test 3. A comparison of corresponding
Test 2 and Test 3 data (2-1 to 3-2 and 2-2 to 3-1) shows that the
isobutane tracer concentration changed very little from test to test.
Yet, the benzene is clearly higher at Sampling Locations 1 and 2 in
each case. This indicates that the higher emission rates in Test 3
can be attributable to the higher ambient temperature.
Scott Environmental Techndosylnc
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SET 1957 05 1280 Page 3-14
3.6 NAPHTHALENE MELT PIT
The melt pit collects the naphthalene slurry that was skimmed
off in the Denver units, and once a day steam is applied to melt the
naphthalene to facilitate pumping into a drainage tank. Benzene con-
tained in the naphthalene cake is released when the steam is applied
to the melt pit.
The results of the four tracer gas tests on the naphthalene
melt pit during melt operations are shown in Table 3-6. For each test
the first half-hour.run was conducted while the cake was still melting.
The second run was made after ammonium sulfate salt had been added to
*
the melt and prior to its being pumped to the drying tank. There are
considerable test to test differences in benzene emission rates.
It is believed that the differences are real, and that they are the
result of variations in the process step timing, the portion of the
process cycle sampled and ambient conditions.
A test was performed on 7/17/80 after the melt was com-
pleted and the pit was beginning to refill. The results of this test
are presented in Table 3-7. This test serves as the basis for estimates
of emissions from the pit at times other than when the melt was in
progress. This test was planned to assess the contribution of the
Denver float unit to the melt pit emissions measured during the melt
cycle. However, it became apparent that the melt pit made a substantial
contribution to the benzene found in this test. On 7/22/80, three sets
of grab air samples were collected over the melt pit at ground level.
The results areas follows.
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SET 1957 05 1280
Page 3-15
TABLE 3-6
NAPHTHALENE MELT PIT
Date: 7/15/80
Tracer Test #1, Run #1
Test Start - 8:00 a.m.
Isobutane Emission Rate: 1.16 Ib/hr
0.53 kg/hr
Weather Conditions: Wind SSW 0-5 mph
Temp 75°F
Cone, of Cone, of
Sample Benzene Isobutane Mass to Mass Ib/hr kg/hr
Loc. (ppm) (ppm) Ratio 4>/ic, Benzene . Benzene
1 11.48
2 17.54
3 16.58
Upwind 0.71
Date: 7/15/80
Tracer Test #1,' Run #2
Test Start - 8:35 a.m.
1 ' 9.45
2 13.48
3 14.90
Upwind 1.03
Date: 7/16/80
Tracer Test #2, Run #1
Test Start: 7:30 a.m.
1 14.99
2 15.18
3 10.22
Upwind 1.02
Date: 7/16/80
* Tracer Test #2, Run #2
Test Start - 8:09 a.m.
1 11.35
2 5.48
3 8.87
Upwind 0.77
* Run voided due to leak
0.713
1.02
0.93
ND
0.977
1.32
1.49
ND
21.66 25.13
23.06 26.75
23.97 , 27.81
Avg. 26.56 Avg.
Isobutane Emission Rate:
• •
Weather
13.01
13.75
13.45
Cond i t ions : Wind
Temp
15.10
15.95
15.60
Avg. 15.55 Avg.
Isobutane Emission Rate:
1.25
1.52
0.754
ND
Weather
16.16
13.41
18.24
Conditions: Wind
Temp
20.86
17.16
23.35
Avg. 20.46 Avg.
Isobutane Emission Rate:
1.54
2.12
1.39
ND
in flowmeter.
Weather
9.93
3.47
8.57
—
Conditions: Wind
Temp
11.22
4.55
11.23
Avg. 9.00* Avg.
11.42
12.16
12.64
12.07
1.16 Ig/hr
0.53 kg/hr
SSW 0-5 mph
75°F
6.86
7.25
7.09
7.07
1.28 Ib/hr
0.58 kg/hr
SSW
75°F
9 .40
7.80
10.61
9.30
1.31 Ib/hr
0.60 kg/hr
SSW
75°F
5.10
2.07
5.10
4.09*
• f-fty
^\j Scott Environmental TechnoJosy '"C-
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SET 1957 05 1280
Page 3-16
TABLE 3-6
(Continued)
Date: 7/17/80
Tracer Test #3, Run #1
Test Start - 7:15 a.m.
Isobutane Emission Rate: 1.26 Ib/hr,
0.57 kg/hr
Weather Conditions: Wind - Variable
Temp. 75°F
Sample
Loc.
1
2
3
Upwind
Cone, of
Benzene
(ppm)
6.56
6.86
6.80
0.49
Cone, of
Isobutane
(ppm)
0.80
1.41
1.78
ND
Mass to Mass
Ratio /icy
11.03
6.54
5.14
—
Ib/hr
Benzene
13 . 90
8.24
6.48
kg/hr
Benzene
6.32
3.75
2.95
Date: 7/17/80
Tracer Test #3, Run #2
Test Start - 8:18 a.m.
Avg. 9.54 Avg. 4.34
Isobutane Emission Rate: 1.24 Ib/hr
0.56 kg/hr
Weather Conditions: Wind - Variable
Temp. 75°F
1
2
3
Upwind
5.28
5.61
6.16
0.61
0.261
0.430
0.421
ND
27.18
17.64
19.71
33.70
21.87
24.44
Avg. 26.67
15.32
9.94
11.11
Avg. 12.12
Date: 7/18/80
Tracer Test #4, Run //I
Test Start - 7:36 a.m.
1 18.60
2 19.68
3 19.44
Upwind 1.83
Date: 7/18/80
Tracer Test #4,
3.31
6.84
4.79
0.087
Run #2
Test Start - 8:30 a.m.
1 4.41
2 5.70
3 6.18
Upwind 2.83
{\} Scott Environmental
2.57
3.99
4.50
ND
Technology Inc.
Isobutane Emission Rate: 1.29 Ib/hr
0.59 kg/hr
Weather Conditions: Wind N, Steady
7.56
3.87
5.46
9.75
4.99
7.04
4.43
2.67
3.20
Avg. 7.26 Avg. 3.43
Isobutane Emission Rate: 1.29 Ib/hr
0.59 kg/hr
Weather Conditions: Wind N, Steady
2.31
1.92
1.85
2.98
2.48
2.39
1.35
1.13
1.09
Avg. 2.62 Avg. 1.19
-------
SET 1957 05 1280
Page 3-17
TABLE 3-7
BACKGROUND FOR NAPHTHALENE MELT PIT
Date: 7/17/80
Tracer Test //I, Run //I
Test Start - 11:22 a.m.
Sample
Loc.
1
2
3
Upwind
Cone, of
Benzene
(ppm)
14.65
15.21
9.71
0.56
Cone, of
Isobuta'ne
(ppm)
3.01
3.89
2.04
ND
Date: 7/17/80
Tracer Test #1, Run #2
Test Start - 11:55 a.m.
1
2
3-
Upwind
13.49
15.82
13.43
0.25
1.52
3.5.4
3.75
ND
Denver Units Operating - 1, 2, 3
Isobutane Emission Rate: 1.28 Ib/hr
0.58 kg/hr
Weather Conditions: Wind SSW, 0-5 mph
Temp 80°F
Mass to Mass
Ratio 4>/ic,
6.55
5.25
6.42
Ib/hr
Benzene
8.38
6.72
6.94
kg/hr
Benzene
3.81
3.05
3.15
Avg. 7.35 Avg. 3.34
Denver Units Operating - 1, 2, 3
Isobutane Emission Rate:
Weather Conditions:
11.93
6.01
4.82
1.28 Ib/hr
0.58 kg/hr
Wind SSW, 0-5 mph
Temp 80°F
15.27 6.94
7.69 3.50
6.17 2.80
Avg. 9.71 Avg. 4.41
Scotr Environmental Technology Inc
-------
SET 1957 05 1280 . Page 3-18
BENZENE OVER MELT PIT AT GROUND LEVEL
Grab Samples Collected 7/22/80
Time Benzene Concentration (ppm)
Edge of Pit Middle of Pit
1330 46 27
1800 67 36
2300 116 ' 42
It can be seen that the benzene concentration was higher
at the edge of the pit, which was above the point where incoming
slurry splashed into the pit, than at the center of the pit. In
addition, the concentrations increased with time as the pit filled.
The contribution of the Denver unit to the samples
collected during the melt tests was estimated to be negligible be-
cause the plume rise from the heated pit caused the emissions from
the Denver unit to rise well above the samplers. Furthermore, the top
of the Denver unit from which point the Denver unit's emissions emanated
was approximately six feet above ground level (top of melt pit).
Thus, it is quite unlikely that the Denver unit emissions could reach
the samplers during the tests on the melt pit when the melt was in
progress.
The following engineering estimates of overall daily naphthalene
melt pit emissions are based on all of the data collected. The benzene
emission rate from the melt pit is highest during the time when the
naphthalene cake is being melted. The emission rate during this half
hour period is from 20 to 30 pounds per hour. During the following
half hour the emissions decrease to the 10 to 20 pounds per hour range.
Scott Environmental Technology Inc.
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SET 1957 05 1280 Page 3-19
The emissions continue to decrease over the period that the melted
naphthalene remains in the pit and the benzene content in the mix
becomes depleted. Once the melt has been transferred to the drying
tank and filling of the pit with slurry from the Denver units resumes,
benzene emissions begin at the rate of three to six pounds per hour.
As filling continues and the liquid level in the pit rises, the
emission rate increases to the order of 10 pounds per hour or more
until the next melt is started. These emission rates can easily
vary by a factor of 2 or 3 from day to day. The temperature of the
material in the pit is the primary variable which affects the benzene
rate at any given time.
Scott Environmental Techndosylnc
-------
SET 1957 05 1280 Page 4-1
4.0 PROCESS DESCRIPTION AND OPERATION
4.1 PROCESS DESCRIPTION
The by-product recovery operations for tar and flushing liquor at
Bethlehem Steel Corporation, Bethlehem, Pennsylvania are two separate systems;
Batteries 2, 3, and A as well as a separate system for Battery 5. These gas
streams combine before entering the ammonia saturator. Batteries 2 and 3
have 102 ovens each and were constructed in 1941-43 using a Koppers-Becker
design. Battery A has 80 McKee-Otto ovens that began operation in 1976.
Batteries 2 and 3 produce a heavy tar because the hot top of the oven cause's
cracking of the carbon compounds in the coke oven gas. The specific gravity
of the heavy tar is in the range of 1.25. Battery 5 has 80 Koppers ovens
with horizontal flues that were constructed in 1953. Battery 5 produces
light tar with a specific gravity of approximately 1.19.
The processes used at the Bethlehem plant for coke oven gas
recovery are primary cooling, tar decanting, exhausting, tar electrostatic
precipitation, ammonia still and saturator, final cooling, light oil scrubbing
and rectifying, and Sulfiban desulfurization with Glaus recovery. A process
flow diagram of the gas and liquid streams is depicted in Figure 4-1.
The gas leaving the ovens is collected in the collecting mains
where it is sprayed with flushing liquor. The gas and flushing liquor leave
the battery area and are transported from the collecting main through cross-
over mains into the suction main and into the by-product recovery area. The
gas and liquor initially separate at the downcomer where the flushing liquor
falls out and the gas continues to the primary coolers. The flushing liquor
from Batteries 2 and 3 enters an interceptor pit before being pumped to the
Scott Environmental Technology Inc.
-------
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LEHEM STEEL CORPORATION, BETHLEHEM, PA
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-------
SET 1957 05 1280 Page 4-3
tar decanter because ground elevations will not allow for gravity flow. The
interceptor pit removes some sludge which is stored in a dumpster before
disposal. The detention time in the interceptor pit is very short with a
flow rate of 189 1/s (3000 gpm). The flushing liquor from Battery A does
not enter this pit, but flows by gravity to the tar decanter.
As previously stated the tar and flushing liquor operations are
two separate, but similar systems. This discussion will address the operations
for Batteries 2, 3 and A because the plant tour surveyed this system. The
gas stream from Battery 5 joins the gas stream from Batteries 2, 3 and A
before the ammonia saturator. Excess flushing liquor from both systems are
steam stripped in the same 'ammonia still.
The dirty flushing liquor enters the two parallel tar decanters
where it is separated into liquor, tar, and sludge. Liquor from the over-
flow pit is also separated in the tar decanters. The flushing liquor flows
by gravity to a surge tank before returning to the spray system on the
collecting mains. Excess flushing liquor from the surge tank is treated
with lime before stripping in the ammonia still. The flushing liquor
ammonia concentration is approximately 3000 mg/1 before the still. The
ammonia rich vapors exit at the top of the ammonia still and combine with
the main gas stream before the ammonia saturator. The ammonia concentration
in the effluent from the ammonia still is 1.2 mg/1 before entering the
aeration basins. In the future the plant will increase the ammonia concen-
tration to approximately 40 mg/1 to enhance the biological wastewater
treatment process.
Scott Environmental Techndosy I"0
-------
SET 1957 05 1280 Page 4-4
The tar layer from the tar decanter is pumped to tar storage. The
water content of the tar is approximately 10-12% from the tar decanter and
3-4% after tar storage. The water content of the tar from the tar decanter
could increase to approximately 35% when charging problems occur. The tar
in storage is heated to 94°C for several days before shipping. Heavy tar
from Batteries 2, 3, and A is produced at a rate of 181.7 cubic meters
(48,000 gallons) per day. Light tar from Battery 5 is produced at a rate
of 45.4 cubic meters (12,000 gallons) per day. The sludge layer from the
tar decanter is pulverized in a ball mill before storage and disposal.
The gas stream enters four parallel primary coolers at 77°C where
it is sprayed with circulating liquor. During the visit two old primary
coolers were not operating due to reactivation. The circulating liquor is
cooled by indirect coolers before recirculating in the primary coolers.
Excess circulating liquor and tars are drained to the overflow sump from
the old primary coolers. The excess liquor from the new primary coolers
goes directly to the decanters. The gas leaves the primary coolers at
approximately 44°C.
The gas stream enters the exhausters where the prime motive
power for the system is supplied. The gas then enters four parallel tar
electrostatic precipitators where additional tar is removed from the gas
and drained to the overflow pit (drain pit).
The gas from the tar electrostatic precipitators is combined with
the gas stream from Battery 5 and the vapors from the ammonia still before
entering the ammonia saturator. The ammonia saturator is an Otto design
that sprays 2% sulfuric acid through the gas as it rises in the saturator
Scott Environmental Technology Inc.
-------
SET 1957 05 1280 Page 4-5
column. The system produces 65.3 metric tons (72 tons) of ammonium sulfate
per day. Before the ammonia still was installed the plant produced 54.4
metric tons (60 tons) of ammonium sulfate per day.
The gas leaving the ammonia saturator is approximately 55-60°C
before entering the final coolers. The final coolers are arranged in three
parallel rows with two rows having two coolers each in series and one row
having one cooler. There is normally one cooler in each row in service at
any given time. The final coolers circulate water which is indirectly
cooled before respray. The naphthalene/water slurry from the bottom of
the final coolers is conveyed to a Denver flotation unit via an open trough.
In the Denver unit the naphthalene slurry is floated and scraped from the
surface and then drained to a melting pit. The naphthalene slurry is
heated in the melting pit before pumping to the draining tank. From the
draining tank the naphthalene goes to a drying tank and then to a shipping
tank. The water from the Denver flotation is pumped to the atmospheric
cooling tower for the final coolers. All operations are vented to the
atmosphere.
The gas leaves the final coolers and enters the light oil scrubbers
at 18°C in the winter but rises as high as 32°C in the summer. The wash
oil scrubbers are arranged in three parallel rows with two rows having four
scrubbers each in series and one row having two scrubbers in series. In the
light oil scrubbers the wash oil flows are countercurrent to the gas stream
and remove the light oil from the gas stream. The benzolyzed wash oil is
then stripped of the light oil in the wash oil still. The debenzolyzed wash
oil from the wash oil still is indirectly cooled in the wash oil chillers
Scott Environmental Technology Inc.
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SET 1957 05 1280 Page 4-6
before the wash oil decanter. In the wash oil decanter entrained water is
periodically separated from the wash oil and flows by gravity to the Gale
oil sump (see Figure 4-2). The wash oil from the wash oil decanter is then
returned to the light oil scrubbers for reuse.
The light oil vapors from the wash oil still enter a rectifier
which fractionates the light oil into primary and secondary oil. The
separation between primary and secondary oil occurs at 140°C (284°F). The
crude secondary oil is the BTX fraction of the light oil and is shipped to
the Sparrows Point plant operated by Bethlehem Steel Corporation for further
refining. The primary oil is the heavy fraction of the light oil and is
burned with bunker oil throughout the plant. The plant in the past has
refined the secondary crude oil, but in the fall of 1977 the unit was moth-
balled. The refining operations produced a caustic and acid sludge at 3.8
cubic meters (10,000 gallons) per day each and cost for the ultimate
disposal of these sludges made the refining operation economically impractical.
The Gale oil sump receives waste stream inputs from the final
cooler, wash oil still, wash oil chiller, wash oil decanter, rectifier,
primary light oil storage, secondary light oil storage, desulfurization
blowdown or condensate, and miscellaneous runoffs. The Gale oil sump
separates the wastewaters into oil and water layers. In the future the
water layer will be pumped to the influent to the aeration basins. The
oil layer is pumped to a tank car. If the Gale oil sump receives excessive
inputs the overflow flows to quench.
The gas stream from the light oil scrubbers then enters the
Sulfiban desulfurization process. The gas stream initially enters two
Scott Environmental Technology Inc.
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SET 1957 05 1280
Page 4-7
GRAB _
SAMPLE*
SPRAYS
tm
5
Q
'(HIGHER
LEVEL)
WATER
(LOWER LEVEL)
OIL
TO TANK CAR
31T
ScXDtt
Environmental
Technology
Inc.
FIGURE 4-2 GALE OIL SUMP (TOP VIEW)
-------
SET 1957 05 1280 Page 4-8
packed contact columns for absorption of the sulfur and the "sweet" coke
oven gas exits the top of the contact columns for reuse. The absorbing
solution is 15% monoethanolamine (MEA) in water. The rich MEA is stripped
in the still column to lean MEA which is returned to the contactor columns.
In the still column the acid gases exit the top and are passed through a.
heat exchanger before entering the cyanide destructor. Some of the con-
densate or reflux from the still column condenser and heat exchanger are
pumped to the Gale oil sump. The acid gases enter the cyanide reactor at
approximately 149°C (300°F) and the cyanide is destroyed by heating to
approximately 233°C (450°F) with the aid of bauxite and activated alumina
catalyst bed. The acid gases leaving the cyanide reactor are then processed
in a Glaus sulfur recovery system which produces elemental sulfur and
incinerates the tail gas.
The sweet coke oven gas after the contactor columns is held at
25 inches of water by a system that supplies natural gas at 23 inches of
water and flares at 27 inches of water. The coke oven gas is used at the
coke ovens and at other places within the steel mill. The heat value of
the gas is approximately 530 Btu per cubic foot.
4.2 PROCESS OPERATING PARAMETERS
During the two-week test period, the plant average coke production
rate was 3,900 tons per day. This resulted in generation, on the average,
of 78 x 10 cubic feet of raw coke gas per day. Thus, we can state that
the plant was operating at about 75% capacity. This capacity factor was
discussed with Bethlehem personnel. While it was acknowledged that some
Scott Environmental Technology Inc.
-------
SET 1957 05 1280 Page 4-9
variations result from the longer coking cycles, there is no reason to
believe that the benzene emissions, per ton of coke produced, would be
significantly different from when the plant is at full capacity.
Other process operating data are presented in Table 4-1.
Scott Environmental Technology Inc.
-------
TABLE 4-1
PROCESS DATA, BETHLEHEM STEEL CORP., BETHLEHEM, PA
Weeks of July 7 and 14, 1980
Oven Flue Temperatures (Avg., °F)
Batt. A . 2 3
2,409
2,410
2,413
2,415
2,384
2,411
2,390
2,383
2 , 380
2,256
2,260
2,247
2,235
2,234
2,250
2,240
2,233
2,232
2,230
2,220
2,238
2,236
2,199
2,272
2,234
2,236
2,221
2,262
2,252
2,240
2,240
2,251
2,269
2,256
2,263
2,246
710
745
725'
720
740
704
657
688
707
Coke Production (TPD)
Batt. 5 Total Breeze
3,995
4,098
3,828
4,074
3,928
3,974
3,718
3,567
3,887
101
101
101
101
101
182
151
151
151
CO
w
H
Ui
•^J
O
N>
oo
o
July
Date
7
8
9
10
11
14
15
16
17
Coke-Oven
Gas (MSCF)
Tar
(GPD)
Light Oil
(GPD)
80,170
78,630
77,070
80,840
77,170
77,820
78,200
73,820
74,600
60,093
66,896
31,365
42,911
45,338
37,403
47,900
45,200
44,263
26,500
10,500
17,700
12,500
15,100
11,. 000
10,000
10,000
9,000
Primary Oil
(GPD)
1,032
1,000
766
1,400
2,500
1,100
1,000
1,000
3,500
Naphthalene
(GPD)
600
500
700
900
800
1,200
700
500
800
oo
ID
I
(-•
o
-------
SET 1957 05 1280 Pase -~
5.0 FIELD SAMPLING AND ANALYSIS METHODOLOGY
5.1 DETERMINATION' OF BENZENE FROM STATIONARY SOURCES:
EPA METHOD 110 AND MODIFICATIONS
EPA Method 110 consists of drawing a time-integrated stack gas
sample through a probe into a Tedlar* sample bag, which is enclosed in a
leak-free drum, by use of a pump hooked to the drum outlet which slowly
evacuates the drum, causing the bag to fill. A copy of the method is
included in Appendix D.
The method was modified by Scott because as it stands the
method doesn't account for moisture in the sample stream, and is only
designed to measure benzene concentration, not mass emission rate. The
following modifications were made to all tests done using Method 110:
1. To obtain mass emission rates, velocity and temperature
readings were taken at the top of the stack at 5 minute intervals during
the 30-minute sampling runs. This information was used to calculate flow-
rate', which was used in conjunction with the benzene concentration to
yield the mass emission rate. Velocity readings were made using a vane
anemometer with direct electronic readout.
2. A personnel sampling pump was substituted for the pump,
needle valve, and flowmeter of the method. The personnel pumps have
built-in flowmeters and rate adjustment screws and have the further
advantage of being intrinsically safe, as required in many areas of
the coke plant.
* Mention of trade names or specific products does not constitute endorsement
by the U.S. Environmental Protection Agency.
Scott Environmental Technofosylnc
-------
SET 1957 05 1280 Pa§e 5~2
3. Swagelok fittings were used in place of quick-connects.
4. Rather than discarding Teflon sample lines after each set
of samples, they were washed with propylene carbonate and/or acetone and
flushed with nitrogen before reuse.
5. An orifice and magnehelic gauge were inserted in the sampling
line before the Tedlar bag to indicate that air flow was reaching the
bag.
6. A water knockout trap was inserted between the probe and
magnehelic gauge to collect any condensate in the sample line.
7. The following cleanup procedures were followed:
If any condensate was collected in the trap or sample line, it
was measured and saved for analysis.. The probe, line and trap were then
washed with propylene carbonate, which was also saved for analysis. Any
benzene found in these washes and water catches was added to the total found
in the sample bag to determine mass emission rates.
Bag volumes were measured whenever water was collected in the
trap by emptying the bag through a dry gas meter after the sample was
analyzed. The volume of water collected in the trap was then converted
to an equivalent air volume and was added to the volume in the bag to
determine the percent moisture in the sample stream.
After the probe, line and trap washes were completed, the lines
were washed with acetone to remove the propylene carbonate film and flushed
with nitrogen to dry.
Figure 5-1 shows the modified Method 110 setup.
Scott Environmental Technckxjy Inc
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SET 1957 05 1280
Page 5-3
FIGURE 5-1
Stainless Steel Probe
Swagelok Fittings
Stack
Teflon Sampling Line
Water Knockout Trap
/Magnehelic Gauge
Tygon Tubing
Personnel Sampling
Pump
Leak-proof Barrel
Tank
Inc.
MODIFIED METHOD 110 SAMPLING TRAIN
-------
SET 1957 05 1280 Page 5"'*
5.2 TRACER TESTING . . .....-•
The tracer gas method is a practical procedure for quantifying
mass emissions of volatile organics from sources which are essentially
open to the atmosphere without disturbing flow, dispersion patterns or
the source operation. This method utilizes the release of a tracer gas
directly over the source of interest; the tracer gas will then follow the
same dispersion patterns as the emissions from the source. The mass of
tracer released over the sampling period is known and the mass to mass
ratio of benzene to the tracer gas in the sample is determined by gas
chromatography. The emission rate of benzene can be calculated with this
information.
This method is based on the principle that*- the chosen tracer gas
will model the dispersion of benzene from the source. The tracer gas
chosen for this project was isobutane because it was not present in the
sources to be tested and it could readily be separated from other source
trace components by the same column used for benzene. In addition, isc-
butane is. a non-toxic gas that can readily be dispensed from a pressurized
cylinder at a uniform measured rate.
When this method was used triplicate tests were performed. Each
test consisted of two 1/2 hour runs. For each run clean and backgrounded ten-
liter Tedlar bags were used. Integrated samples were collected using
Emission Measurements, Inc. Air Quality Sampler II systems. The AQS II
samplers are self-contained units capable of collecting one or more inte-
grated samples at a preset rate. For tracer tests the sampling rate used
was ten liters per hour.
5.3 SAMPLE HANDLING
After being collected the gas samples were immediately transported
to the gas chromatograph and analyzed. The elapsed time between sample
collection and analysis never exceeded one hour. To verify that there was
no sample degradation in samples of this type some of the samples were
retained for 24 hours and reanalyzed. The loss of benzene and isobutane
observed was typically less than 5%.
Scott Environmental Technology Inc.
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SET 1957 05 1280 . Page 5"
5.4 FIELD ANALYSIS
All gas samples collected were analyzed using a Shiraadzu GC Mini 1
gas chromatograph equipped with dual flame inoization detectors, dual
electrometers, heated sample loop, and a backflush system. Figure 5-2 shows
a schematic of the backflush apparatus. The backflush system is composed
of ten port sequence reversal valve and two columns, a scrubber column for
retaining, high molecular weight compounds and an analytical column. When
the system is.in the inject mode the scrubber column and the analytical
column are connected in series allowing sample components to move from the
precolumn to the analytical column. In the backflush mode the columns are
disconnected from each other and become two separate systems each with its
own carrier gas source. This arrangement allows the separation and
measurement of low molecular weight compounds while the scrubber column
is being backflushed of heavier sample components. Backflush times for
different mixtures of sample components must be predetermined to insure that
the compound(s) of interest are transferred to the analytical column before'
backflushing is started.
Samples for chromatographic analysis were drawn into a 20 cc glass
syringe then introduced to the sample loop inlet. The samples once in the
sample loop were allowed to come to atmospheric pressure by waiting 15
seconds prior to the injection. When only benzene was of interest the
following chromatographic conditions were maintained:
Column Temperature (isothermal) - 100°C
Injector and Detector Temperature - 200°C
5 ml Sample Loop, Temperature - 50°C
Carrier Gas Flow Rate - 32 cc/min
Hydrogen Flow Rate - 40 cc/min.
. Air Flow Rate - 240 cc/min.
Analysis Time - 5 min.
Detector - Flame lonization
Scott Environmental Technology Inc.
-------
Q
Ul
Is)
CARRIER GAS A
CARRIER GAS B
PREP, COLUMN
ANALYTICAL COLUMN
SAMPLE INJECTION
INJECT
A, D, E OPEN
B, C CLOSED
*
BACKFLUSH
A, E CLOSED
B, C, D OPEN
GC COLUMN CONFIGURATION WITH BACKFLUSH
DETECTOR
r?
r.
wi
i
-------
SET 1957 05 1280
Page 5-7
The columns used for field analysis were:
A - Scrubber Column
10% FFAP on Supelcoport 80/100
1/8" x 1 m Stainless Steel
B - Analytical column
20% SP-2100, 0.1% Carbowax 1500
100/120 Supelcoport
1/8" x 10' Stainless Steel
When samples from tracer tests were analyzed the chromatographic
conditions were changed to provide adequate separation of the isobutane
tracer from the other light components of the sample. The temperature
program used for this analysis was:
1) Start at room temperature with external cooling fan
on and oven door open.
2) Inject @ 0.0 min.
3) Turn external cooling fan off @ 1.0 min.
4) Eackflush @ 1.8 min.
5) Isobutane elutes @ 2.3 min.
6) Close oven door @ 3.0 min. with oven temperature
set at 100°C.
7) Benzene elutes @ 7.0 min.
8) After the elution of benzene, open the oven door and
turn on the cooling fan. The next injection can be
made after 2 minutes of cooling:
9) When the tracer gas is used analysis time will be
approximately 10 minutes.
The columns and flow rates were the same as for- isothermal.
Scott Environmental Technclosy Inc
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SET 1957 05 1280 Page 6-1
6.0 FIELD SAMPLING PROCEDURES
6.1 COOLING TOWER-DIRECT WATER FINAL COOLER
The cooling tower was sampled on July 10, 1980. The tower
has four 13-foot diameter fans on top as shown in Figure 6-1.
Sampling was conducted at only one fan and the results were multi-
plied by four to obtain mass emission rates from the whole cooling
tower. This approach is expected to yield accurate emissions data
without the necessity of testing at all four fans, because the fans
were operating under identical conditions.
Air sampling was conducted following EPA Method 110 using a
24-point sampling and velocity trayerse across two diameters of the
fan shroud to obtain an integrated sample. At two minutes per point,
each of the three sampling runs lasted 48 minutes.
Triplicate liquid samples were dipped from the hot and cold
wells with temperatures of 30 C and 27.8 C respectively (86 F and
82 F). At the time of sampling, the cold well was mixing back into the
hot well at one location due to a faulty level control. Liquid samples
were dipped from points well clear of the mixing area. The plant
indicated that average normal operating temperatures for summer are
86°F and 76°F.
Scott Environmental Technology Inc.
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SET 1957 05 1280
Page 6-2
FIGURE 6-1
PLAAJ VIFW
FAM SHROUD
FAM
MOTOR
FAKJ
SIDF VIEW
2'
Scott
Environmental
Technology
Inc.
COOLING TOWER - DIRECT WATER FINAL COOLER
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SET 1957 05 1280 Page 6-3
6.2 TAR DECANTER
Three half-hour Method 110 tests were conducted on the tar
decanter from the #5 battery on July 8th and 9th, 1980. The tar
decanter is shown in Figure 6-2. Problems were encountered with naph-
thalene plugging the sample line. The decanter was the first source
we tested using Method 110, and at the beginning several tests were
run in which the sample line clogged without our knowledge resulting
in no sample collection.
At this point we spent considerable time revising the method
for application to this project. The equipment was modified to include
an orifice and magnehelic gauge in the sample line to register flow
into the bag and a water knockout trap in the line before the orifice
to prevent moisture from entering the bag. Clean-up procedures were as
described in Section 5.1.
From here on, all tests referred to as Method 110 include
these revisions.
The tar decanter receives tar arid flushing liquor from the
coke gas crossover main from the #5 battery and also from the primary
cooler. A total of five liquid samples were collected as follows:
Two were dipped from a hatchway on top of the decanter at the outlet
end, one was collected from the gas crossover main, and two were
taken from the primary cooler outlet.
Scott Environmental Technology Inc.
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SET 1957 05 1280
Page 6-4
FIGURE 6-2
it
HOOD
0
' a't
II'?
HOOD
• u
©
•A
TEST V£NT S'
56'
inc.
BATTERY^ TAR DECANTER
EPA METHOD HO
-------
SET 1957 05 1280 Page 6-5
6.3 LIGHT OIL CONDENSER VENT
Four half-hour EPA Method 110 tests were conducted on the
light oil condenser vent on July 11, 1980. The results of the analysis
showed the benzene concentration in the third sample to be about half
that found in the first two, indicating a possible leak in the system.
Upon inspection of the sample line, the leak was found to be caused
by an improperly seated gasket in the water knockout trap, and the
third run was voided. A fourth test was run, and the analytical
results were consistent with those of the first two runs.
The top of the existing stack had a 1/2 inch steam injection
pipe running into the top, as shown in Figure 6-3. A stack extension
was constructed from a section of steel stovepipe that extended the
top of the stack past the steam pipe so we could accurately
measure flow rate with a vane anemometer.
The plant maintenance crew provided scaffolding for access
to the testing site.
No liquid samples were collected at this source.
Scott Environmental Technology Inc.
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SET 1957 05 1280
Pa.ge 6-6
FIGURE 6-3
1/2" Steam
Injection -
Pipe
6" Diameter
Vent Stack
Sampling Platform
•Stack Extension
•Slot for 1/2" Pipe
Scott
Environmental
Technology
Inc.
LIGHT OIL CONDENSER VENT
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SET 1957 05 1280 Page 6-7
6.4 NAPHTHALENE DRYING TANK
The naphthalene drying tank presented several new problems
in sampling strategy. The tank is shown in Figure 6-4 as Draining
Tank #2. There is a large opening in the center of the tank with
steam lines running in, in addition to a tall 6-inch diameter vent
stack located at the end of the tank. More emissions come from
the large opening than from the vent, and an attempt was made to
cover the opening with plywood and fiberglass packing, but due to the
pipes in the opening this was not very successful in stopping leaks.
It was decided to construct a sheet metal collar around the opening,
with slots to fit around the steam lines, and treat it as a vent
stack. Method 110 samples were collected from the tall vent stack .
and velocity readings were taken at both the stack and the big vent
opening. The assumption was made that the concentration of benzene
is the same at the big vent opening as it is in the stack. Mass
emission rates were therefore determined using the benzene concen-
tration in the stack sample with the flow rates from the stack and
the vent opening.
The second major problem encountered was naphthalene plugging
the sample line and probe. The line plugged so fast there was no use
in cleaning the line periodically. The solution was to bubble the
sample stream through propylene carbonate to knock out naphthalene,
using a large diameter glass elbow as a probe. A bucket containing
three impingers was hooked on top of the stack. The first two
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SET 1957 05 1280
Page 6-8
FIGURE 6-4
From Naphthalene Melt Pit
1
Jt
Draining
Tank
I
//I
Draining
Tank
#2
P
L22"
Diam.
Steam Line
Opening
r
Test
|
N6" Pipe
t>
Vent
i
i
i
I
l
I
Draining
Tank
#3
I
Draining
Tank
#4
t
*
*
Shipping Tank
^^^_ ^_^A
bCOt
Environmental
roiofly
NAPHTHALENE HANDLING TANKS
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SET 1957 05 1280 Page 6-9
impingers contained. 100 ml of propylene carbonate and the third was
empty. A Teflon sample line connected the impinger train to the
sampling drum and the glass elbow used for the probe was connected
directly to the first impinger (See Figure 6-5).
Cleanup consisted of saving the impinger catches and washes
in addition to the sample line and water trap washes. The sample
volume contained in the Tedlar bag was measured after the sample was
analyzed by emptying the bag through a dry gas meter.
A test run was done on the drying tank on July 18 to verify
the success of the new procedures. The bag sample collected was
analyzed but the propylene carbonate catch was not, as it was just a
trial run. Results of the bag analysis are included with the data
in Table 3-4 for purposes of comparison. Naphthalene from the melt
pit is pumped into a draining tank after the melt each morning, and
the tank is steam heated from about 1:00 p.m. until about 4:00 a.m.
when a night shift operator shuts it off. Benzene emissions are not
expected to be constant over the heating cycle, so in order to measure
accurately the emissions from the tank it must be tested over the
entire heating cycle. We collected eight half-hour Method 110 tests
modified as described at about two hour intervals during the cycle
on the night of July 22, 1980.
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SET 1957 05 1280
Page 6-10
FIGURE 6-5
Glass
Stack
Stack
Flow
Empty
100 ml
Propylene
Carbonate
— Teflon Sampling Line
Magnehelic Gauge
30 liter
Tedlar Bag
Tygon Tubing
Personnel
Sampling
Pump
•Leak-proof
Barrel
Tank
Scott
Environmental
Technology
Inc.
MODIFIED METHOD 110 SAMPLING TRAIN WITH PROPYLENE
CARBONATE KNOCKOUT TRAP
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SET 1957 05 1280 Page 6-11
6.5 DENVER FLOAT UNITS
The Denver float unit presented a complex problem to the use
of a tracer gas for quantifying the unit's benzene mass emissions.
First, there are 4 separate Denver float tanks, of which 3 were
normally in use during these tests. The particular tank which was out
of service varied from day to day. Second, the naphthalene melt pit
was immediately adjacent to the Denver float tanks on one of the
sides that was physically accessible for downwind sampling. While the
emission rate from the melt pit was low, compared to the Denver float
tanks, some "hot spot" points contributed to the downwind samples.
For example, the point at which the Denver float overflow trough
serving Units 1 and 2 empties its contents into the melt pit was
shown to be a "hot spot" for benzene in subsequent grab samples.
Figure 6-6 shows the processes and flow directions for the entire
naphthalene handling operation. Figure 6-7 shows specifically the
Denver float units and the positions of the samplers for the Denver
unit tests.
The sampling strategy used was believed to be the best
means of arriving at reasonably accurate emission rates without unduly
elaborate and costly sampling procedures. The simultaneous use of a
different tracer gas at each tank and tests utilizing different
tracer gas release configurations would probably have resulted in better
confidence in the emission rates during a particular test period.
However, the emission rate varies from day to day due to variations in
Scott Environmental Technology Inc.
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T -I ITl
P ft .;'
O ')
o J
c
C
/fi*
a i.
Mecr
HOT
*\ .
lMi
TAWK
M
O
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SET 1957 05 1280
Page 6-13
FIGURE 6-7
^ 2^1 Walkway
21'
©
Downwind
Samplers
Unit
//I
!
6'
!
Unit
#2
Unit
#3
Unit
/M
Melt Pit
Upwind
Sampler
Underflow to
Hot Well
To Drainage
— ^ tank
(During melt)
To Drainage Tank
Wind
Direction
Scott
Environmental
Technology
Inc.
DENVER FLOTATION UNITS
-------
SET 1957 05 1280 Page 6-14
both process and ambient conditions. Thus, it was not cost effective
to perform very elaborate test procedures.
The approach used in the Denver float unit tests was to measure
the emissions from a single tank. The tracer gas was dispersed onto
the surface of this tank with the gas discharge probe located along the
center longitudinal point; there will be contributions of benzene from
the other two Denver tanks then in use. The relative contribution from
the second tank was estimated by releasing the tracer onto the surface
of the second tank in a test immediately following the first tank test
without changing the position of the samplers. The relative contribu-
tion of the two tanks to each sampling location is proportional to the
relative amounts of tracer found at that location. There are two
assumptions inherent to this conclusion. First, the benzene emission
rates from the two tanks are equal. This should be true because the
temperature, feed material and size were the same for the two tanks.
Second, the diffusion patterns were the same in the two tests. This
was demonstrated by comparing the benzene concentrations in each
sampler for the two tests.
The sampler locations for Test 1 are shown in Figure 6-7.
The isobutane tracer concentrations from the two tests were normalized
for differences in isobutane release rate and differences in dispersion.
The normalized values were then used to calculate the fraction of the
benzene due to emissions from Tank 1. The contribution from Tank 3
was not determined. Because of the additional spacing between Tanks
2 and 3, the contribution ratio of Tank 3 to Tank 2 would be less than
Scott Environmental Technology Inc.
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SET 1957 05 1280 Page 6-15
that of Tank 2 to Tank 1. It is believed that Tank 3 contributed
less than 5% of the total found in the samples. The calculations
shown in Appendix A assume a negligible contribution from Tank 3.
The upwind background from distant sources was also assumed to be
negligible. The trace benzene concentrations found in the upwind
sampler were primarily due to the Denver unit tank emissions swirling
during wind shifts. No source was immediately upwind of the Denver
unit, and grab samples verified the absence of benzene in the back-
ground air mass.
In Tests 2 and 3, the test procedure was the same as in
Test 1. However, during Tests 2 and 3, Tank 2 was out of. service and
thus did not contribute to the benzene found. In Tests 2-2 and 3-1
the tracer gas should have been dispersed over Tank 3 rather than
Tank 2 which was out of service. Unfortunately, this was not recog-
nized .because this newly developed procedure had not been used before
under these circumstances. Tests 2-2 and 3-1 serve as replicates for
the benzene concentrations found in Tests 2-1 and 3-2, respectively.
All of the benzene found in Tests 2 and 3 is attributable to
Tank 1, since Tank 2 had no emissions, and it is assumed that the
Tank 3 contribution to the samplers was negligible as in Test 1.
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SET 1957 05 1280 Page 6-16
6.6 NAPHTHALENE MELT PIT
The naphthalene melt pit is diagrammed in Figure 6-8. The
melt pit is 24 feet long, 6 feet wide and approximately 8 feet below
grade. Generally there is one melt cycle per day at the beginning of
the first shift. During the melting operation, which lasts approxi-
mately one hour or until all the naphthalene is melted, massive
emissions of steam and naphthalene are released from the melt pit.
These emissions were sufficiently large that small variations in wind
speed and direction would not interfere with plume dispersion and the
collection of representative samples.
The sampling strategy was to position samplers downwind from
the melting process at a distance that would prevent samplers from
becoming clogged with naphthalene. Three samplers were placed approxi-
mately 10 feet from the edge of the melt pit and were 5 feet apart, an
upwind sampler was also positioned approximately 10 feet from the
source. At these sampling locations it was assumed that there was no
contribution from the Denver float units because the mass and velocity
of the plume rising from the melt pit would essentially block emissions
from that source from reaching the sampling locations. The gas dis-
persion bar was positioned on the 'grating which covered the melt pit
approximately 5 feet above the surface of the naphthalene slurry. It
is preferable to disperse the tracer at the liquid level of the source
but in this case proper safety procedures precluded that arrangement.
Scott Environmental Techndosyinc
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SET 1957 05 1280
Page 6-17
FIGURE 6-8
•
2'
•I,
Walkway
D e
^\'
//I
n v
e r Flo
t a t i
on U n :. t si
#3
Tracer Gas Dispersion Bar
Melt Pit
•24'
©
Downwind Samplers
Wind
Direction
\
Scott
Environmental
Technology
Inc.
NAPHTHALENE MELT PIT
-------
SET 1957 05 1280 Page 6-18
The sampling strategy used was believed to be the best means
of arriving at reasonably accurate emission rates without unduly
elaborate and costly sampling procedures. The simultaneous use of a
«
different tracer gas at the melt pit and on the Denver float units
and tests utilizing different tracer gas release configurations would
probably have resulted in better confidence in the emission rates
during a particular test period. However, the emission rate varies
from day to day due to variations in both process and ambient conditions.
This, it was not cost effective to perform very elaborate test procedures.
Between Runs 1 and 2 of Test 2, the dry gas meter was dropped
and a leak developed at the rotameter at the exit of the gas meter.
This was not detected until after Run 2. As a result, a portion of the
tracer gas was released to the air near Sampler 2 instead of through
the dispersion probe. Thus, the benzene emission results for Samplers
1 and 3 are somewhat high and that for Sampler 2 is too low. In
addition, the leak was after the dry gas meter, so the metered release
rate of isobutane was not the rate at which isobutane left the dis-
persion probe. For these reasons, Test 2, Run 2 was not valid. The
results were included in Table 3-6 for comparison of the benzene concen-
trations measured, which are valid.
Four tests were run on consecutive days. During the first
three tests, the wind was from the S to SW and the sampler location
was as shown in Figure 6-8. During Test 4, the wind direction was
from the north. For this reason sampler positioning for this test was
Scott Environmental Technology Inc.
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SET 1957 05 1280 Page 6-19
different than for the first three tests. The samplers were positioned
two feet from the melt pit between the melt pit and the Denver units
and approximately five feet from the dispersion bar.
After Test 3, a test was performed to measure the emissions
present at the sampling locations when a melt cycle was not in progress.
The tracer apparatus and samplers were set up as they were for Tests
1, 2 and 3 on the melt pit. During this test the wind was light but
steady over the Denver units. The benzene found in these samples
could come from the filling melt pit, the feed troughs and from the
Denver units. It was believed that the results of this test could be
helpful in interpreting the data obtained at the same locations during
the melt cycle.
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Page 7-1
SET 1957 05 1280
7.0 LABORATORY SAMPLE ANALYSIS
Two types of liquid samples were collected: process liquids, and
sar.ple line and water trap catches and washes. All liquid samples were
stored in amber glass bottles and returned to Scott's Plumsteadville laboratory
for analysis.
7.1 SAMPLE PREPARATION
Depending upon the complexity of the sample, one of the following
sample preparation procedures was followed prior to the "purge and trap"
procedure and analysis.
Samples Containing Immiscible Liquid Phases
Using a clinical centrifuge (International Equipment Company,
Massachusetts) immiscible liquid phases were separated and each phase was
analyzed separately for benzene.
Samples Containing Solid and Immiscible Liquid Phases
Samples containing solids of higher density than the liquid phase
were separated by centrifuge or by simple decantation of the liquid. The
different phases in the liquid fraction were then further separated by
centrifuging. Solid and liquid phases were analyzed separately.
Samples Containing Finely Crystalline Solid Suspension
In analyzing these samples the stoppered sample jars were shaken
for at least half an hour for homogenizing the solution. The uniform
distribution of suspended fine crystalline solid particles was tested by
determining the percentage of dry solid in several aliquots of the homoge-
nized mixture. A weighed amount of the mixture was analyzed for benzene.
Scotc Environmental Technology Inc
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7_2
SET 1957 05 1280
Sampling System Washings
All washings were clear solutions having only one liquid phase.
The total weight of the liquid phase was determined using a. balance correct
to ±0.1 g. The total weight of each washing w£S more than 25 grams, so an
error of 0.1 g in weighing the mass will contribute an. error of only 0.4%
to the final analytical data. A weighed aliquot of the washing was analyzed
for benzene by following the "purge and trap" and analysis procedures out-
lined in the following sections, and using this analysis data the weight
of benzene present in the total mass of washing was calculated.
7.2 PURGE AND TRAP PROCEDURE FOR EXTRACTION OF BENZENE FROM LIQUID PHASE
TO GASEOUS PHASE
An accurately weighed quantity of the sample to be analyzed was
diluted with 20-25 ol of propylena carbonate in a specially designed glass
purging apparatus which was kept immersed in a thermostatted water bath
maintained at 78°C. Benzene free nitrogen gas was bubbled through the
propylene carbonate solution in the purging apparatus at the rate of
0.2 - 0.3 liters/minute, and collected in leak free Tedlar bags. Under
these experimental conditions, 1 1/2 - 2 hours were sufficient to purge
off all the benzene from the liquid phase to the gaseous phase. The total
volume of nitrogen gas used to purge the sample was accurately measured
by a calibrated dry gas meter. A diagram of the purge and trap set-up is
shown in Figure 7-1.
Propylene carbonate was found to be an ideal diluting solvent
for the extraction of benzene from all types of liquid samples containing
viscous tar, pitch, light and heavy oil and insoluble particulates . It
was chosen for its high boiling point, low density, and good, solvating
capacity.
Scott Environmental Technolosy Inc
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T.
pa
03
rai
FIGURE 7-1 PURGE AND TRAP METHOD EQUIPMENT SET-UP
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SET 1957 05 1280 PaRe 7"4
7.3 GAS ClIROMATOGRAPH
A Ferkin-Elmer 900 gas chromatograph was used for the analysis
of the purge bags. A 10 ft. by 1/8 inch stainless steel column packed with
20% SP-2100/0.1% Carbowax 1500 on 80/120 mesh Supelcoport was used for the
analysis. This column gave complete resolution of the benzene peak from
other components present in the purge bags. The 'peak height' method was
utilized to calculate the concentration of benzene in the purge bags
analyzed. The Perkin-Elmer 900 used for analysis 'was not equipped with
a backflushing unit. Gas chromatograph conditions were as follows:
GC column temperature: 70°C isothermal
Detector temperature: 190°C
5 ml loop at a temperature of 120°C
Carrier gas flow rate: 30 cc/min He
Hydrogen flow rate: 45 cc/min
Oxygen flow rate: 400 cc/min
Detector: Flame lonization Detector (FID)
In addition to benzene, the purge bags contained other volatile
hydrocarbons present in the liquid samples such as toluene and naphthalene.
Because this chromatograph was not equipped with a backflush, it was
necessary to elute all heavy organics from the column by heating the column
to 150°C after every two injections for one hour with the carrier gas on.
After cooling the column to 70°C the absence of any organic in the column
which might overlap the benzene peak ir. the next analysis was checked. When
the column was found to be satisfactorily clean, the next analysis was
continued under the conditions previously described.
Scott Environmental Technciosy
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SET 1957 05 1280 '• Pa"e 8~1
8.0 QUALITY CONTROL AND QUALITY ASSURANCE
The following sections will address quality control and quality
assurance procedures for th«: field analysis of benzene in air samples and
the laboratory analysis of process liquids.
8.1 FIELD ANALYSIS PROCEDURES
All samples were analyzed in duplicate and as a rule peak heights
were reproduced to within 5%. For some very high concentration samples
(percent range) it was necessary to make dilutions for analysis. When this
was done a fresh dilution was prepared for each injection and peak heights
were reproduced to within 10%. To verify that the system was retaining no
benzene, frequent injections of the standard and nitrogen were made. In all
cases the result was satisfactory.
The Tedlar bags that were reused for sampling were flushed three
times with nitrogen and allowed to sit overnight after being filled to
approximately three quarters of their capacity. They were analyzed for
benzene content the following day. The background concentrations of the
bags were recorded and varied from 0 to 10 ppm benzene. Care was taken to
use sample bags whose background concentration was very low compared to the
expected concentration of the source.
The accuracy and linearity of the gas chromatographic techniques
used in this program were tested through the use of EPA Audit Samples. Two
standards, a 122.5 ppm and 6.11 ppm benzene were used to analyze the audit
cylinders.
Scott Environmental Technology Inc.
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SET 1957 05 1280
8.2 PROCEDURES FOR ANALYSIS OF PROCESS LIQUIDS
Scott's benzene standards, checked against EPA Audit Standards,
were used as reference standards throughout this prcgram. The accuracy and
linearity of the gas chroma tographic technique for benzene analysis was ;
tested through the use of EPA Audit Standards which were available to Scott.
Gas chroma tographic analysis of the samples and .standard were performed
under identical conditions to assure the accuracy of the analytical data
generated.
Each batch of propylene carbonate which was used as the diluting
solvent in the purge and trap technique was analyzed for benzene content by
subjecting 25 ml of propylene carbonate to the purge and trap procedure
followed by gas chroma tographic analysis of the trapped gas under identical
conditions as described in Section 5.2. All batches of analytical grade
propylene carbonate were found to be free from benzene.
Every day before the analysis of samples the. purging apparatus and
trapping bags were tested for absence of benzene. Whenever the whole system
was found to be free from benzene to the lowest detectable limit of the
instrument, the samples were analyzed using the purging apparatus and the
trapping gas sampling bags.
Generally an accurately weighed mass of each sample was subjected
to purge and trap procedure only once and the trapped gas sample was repeat-
edly analyzed by GC until the analytical data of consecutive GC analyses varied
by ±0.5% or less.
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Page 8-3
SET 1957 05 1280
For randon.lv- selected samples, the whole analytical procedure was
repeated with a different weighed, mass of the source sample to. check the
validity and accuracy of the analytical methodology. The analytical data
for different runs were found 'not to vary by more than 5%.
By purging the sample with nitrogen under the experimental con-
ditions as utilized by Scott, the recovery of benzene from the sample was
quantitative and this has been verified by analyzing a standard benzene
solution in propylene carbonate containing tar and pitch.
Scott Environmental Technology Inc
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Page A-l
APPENDIX A
SAMPLE CALCULATIONS
Scott Environmental TechrsclcKjy Inc
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Page A-2
APPENDIX A
SAMPLE CALCULATIONS
1. Tracer Gas Calculations
Example: Naphthalene melt pit, Test 1, Run 1
Concentration of Benzene: 11.48 ppm
Isobutane release rate: 1.16 Ib/hr
Calculation of mass to mass ratios:
Benzene 11.48 ppm x 78 g/mole = 895.44
Isobutane 0.713 ppm x 58 g/mole = 41.35
£ x 1.16 Ib/hr = 25.12 Ib/hr benzene
2. Flow Rate at Standard Conditions (saturated at 68°F, 29.92 inches Hg)
Example: Naphthalene drying tank, Run 1
A. Correction for temperature and pressure:
528°R
Flow Rate (STP) = Flow Rate (source) =
T(°F) + 460 29 92
COQ OQ C
Flow Rate (STP) = 1150 cfm x 2Q9 + 46Q x -g^- = 895
B. Correction for moisture
Imp ing er and water trap catch volume: 76cc
Tedlar bag volume(gas sample): 0.474 ft3 = 13.42 1
Gaseous volume of collected water, standard conditions:
_, 1 gm 1 mole 24.15 1 1 m ._ .
76 cc x — °— x -r-r - x - - - = 101.97 1
cc 18 gm mole
Scott Environmental Technology Inc.
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Page A-3
Percent moisture:
101.97
101.97 + 13.42
= 83.4 %
Flow Rate corrected for moisture:
Flow Rate (dry) = Flow Rate (STP) x (100 - % Moisture) /100
= 895 x (100 - 88.4)/100
= 104 cfm
Flow Rate (saturated at 68°F) = Flow Rate (dry) x 1.025
= 104 cfm x 1.025
= 106 cfm
3. Correcting Benzene Concentration for Benzene Found in Water Trap Catch
Example: Naphthalene dyring tank, Run 1
Mg benzene in catch: 1.42 mg
Tedlar bag volume (gas sample): 0.474 ft3 = 13.42 1
Measured benzene concentration: 135.96 ppm
A. Mg benzene in collected gas sample:
135.96 ,, /0 - 78 g 1 mole , QQ
x 13.42 1 x — -f- x 0/ . , , = 5.89 mg
mole 24.15 1
B. Total mass of benzene (air + liquid)
5.89 + 1.42 = 7.31 mg
C. Corrected benzene concentration:
. --__. 1 mole 24.15 1 106 n,Q ,.
0.00731 g x -=^ x x . = 168.60 ppm
° 78 e mole 13.42 1
Scott Environmental Technotosy Inc
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Page A-4
4. Calculation of Benzene Mass Emission Rate
Example: Naphthalene drying tank, Run 1
Flow Rate (standard conditions) = 106 cfm
Benzene concentration = 168.60 ppm
.^ft3 28.32 1 ,_min 168.60 78 g 1 mole 1 Ib . .„ , ,,
106—r- x r— x 60r-— x 2— x —r6- x .. . g . x -7-=-. = 0.22 Ig/hr
mm £t3 hr ±QO mole 24.15 1 454 g
Scott Environmental Technolosy Inc
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Page B-l
APPENDIX B
FIELD DATA SHEETS
Scott Environmental Technology Inc.
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Page B-2
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
PLANT;
METHOD 110 DATA SHEET
DATE:
PROCESS ; (Loo/f'>\
PROCESS NOTES:
£
AMBIENT TEMPERATURE:
BAROMETRIC PRESSURE:
TEDLAR BAG NUMBER:
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
0
Z
3
4
TOO
P
(-OOC
5-7-75-
1^00
(0
& 00
^ 6?
II
/o
1
7
(3
1C,
(7
%H
A
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Page B-3
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
. PROJECT 1922
PLANT:
METHOD 110 DATA SHEET
»t
?? gf/t fc/t
DATE:
PROCESS ; dCQ//'jt
PROCESS NOTES:
.g df^.ir
. I O 4- T~.
AMBIENT TEMPERATURE:^
BAROMETRIC PRESSURE:_
TEDLAR BAG NUMBER:
F
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
-A An1
f
(00(9
19,00
10
IQ
155"
^00
105-0
oo
Zo
fl
L.5~
'•
34-
5 DO
-*t
^/oo
1T5"
60
/ . 5"
IS
4(3
C
pS/Vvs-rI >
-------
Page B-4
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
3
PROJECT 1922
PLANT;
METHOD 110 DATA SHEET
DATE:
PROCESS-: Ceoft'MT f QtD e
PROCESS NOTES:
AMBIENT TEMPERATURE:^
BAROMETRIC PRESSURE:
pu^
\3
TEDLAR BAG NUMBER: /
TIME
STACK TEMP
. GAS VELOCITY
PUMP FLOWRATE
F
iS
4
1 0 0
/OO 0
/. fT
/O
f.-T
/QQ H/m/
m in
4
400
S'
3
[06~0
ID
00
1
^
n
CO
i-r
2.^0
c . 5-
/.5
3
300
. 5T"
1. 5
1,5
r
n
.5"
qu
1. S
-------
Page B-5
PROJECT 1906 BENZENE/BaP PRESURVEY
SAMPLE DATA
Plant 6 1
jft.Sf ^
tfkU Ufa
Process Coo (t\&ibwvr do/rC
Q
Date 7//O/56?
•
•
Sample No.
CT MlO^
ill 1
Time Sampled
IS;?
0
Sample Type: Liquid Air
Sample Temperature $) 6
,• ,
kef
L)
Ambient Temperature
/ / /
Description of Sampling Location:
/)
~~ftJL#J\.
en ue r.
Sample No. C "T" nfflU e II cA
Sample Type: Liquid Air
Time Sampled
/Q • T ^
Sample Temperature
Ambient Temperature
U & r^
r
Description of Sampling Location:
Description of Sampling Location:
1 d UJ-e // f I
C 0 UJ-e
Scott Environmental Techix^osy Irx.
n/(J^f
' <>tr?7(__
Sample No . C Cx3 I 6u
Sample Type: /'Liquid
Sample Temperature
Ambient Temperature
€((
Air
^7
' N C7\ Time Sampled \J-I^
)
2. 'F
6 *F
-------
PROJECT NUMBER
IEST NUMBER
PLANT
SfcW
DATE 7/lofVQ
Page B-6
DRY f.!CLECULAil WEIGHT DETERMINATION OY
SAMPLING Ti.VE (24-hr CLOCK)
SAMPLING LOCATION
fAHPLING LOCATION G?o/'/ui
SftiY.PLE TYPE (BAG, INTEGRATED. CONTINUOUS).
ANALYTICAL KETHOO
AMBIENT TEMPERATURE •
SAMPLE TYPE
llUN NUMBER
OPERATORS CG-
1 10
/
T\fiJ £~ G-
AMBIENT TEMPERATURE
ftROMETER
YRITE ANALYSIS
2 —
co2
FIEU) DATA
MOISTURE
Meter Heading
Meter Reading
aiaetric Pressure
ieter Temp. In
Out
otameter Setting
acer Volume Final
er Volume Initial
Volume
perator
:OMMENTS
J
">^v^ RUN
i CAS ^^^.^
COZ
0 J'.IET IS ACTUAL Oj
KE*o:::3 sinus ACTUAL
CO; RtJO.'.'IQ
CO,:iir:s*cruALCO
RttMc .visus ;.CTUAL
0; KCAOItlQ
'IjIMiTiSIM MIKUS
ACTUAL CO RUC;»O
ACTUAL
ar.\'."(t;
NET
ACTUAL
PfATOO
t
NET
ACTUAL
SE;,o:;n;
NET
>VtR,\CE
ntr
vctu:,:E
TRAVERSE POINT LOCATION & VELOCITY DATA
BY
POINT
1
2
3
4
5
6
7
8
9
10
11
12
13
14
IS
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
. 32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
A-FRACTION
OF I.D.
3- /
G,.~7
][.'S
I7.T
3.^,0
?>5:i-
t^/.V
"75". 6
T)^! 3
o ?..3
-------
Page B-7
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
PLANT:
PROCESS : Ik r p e £. a
PROCESS NOTES:
10*"
METHOD 110 DATA SHEET
DATE:
b d fof -
AMBIENT TEMPERATURE:_
BAROMETRIC PRESSURE:_
TEDLAR BAG NUMBER:
. S3
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
0
7o °
V.
/f
f o -rf«i/>
Apfrvy
f/M/'/i
30
70/.
-------
PROJECT 1922
PLANT:
Page B-8
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
METHOD 110 DATA SHEET
DATE:
6
PROCESS;
PROCESS NOTES:
AMBIENT TEMPERATURE:_ ~
BAROMETRIC'PRESSURE:_
TEDLAR BAG NUMBER:
"I . 5"3
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
0
5"
-f-^e-
f -e
/O
70,4
I/.. 3 °C
5- 7?
/, /:
3C?
VOIP
etc
co
-------
Page B-9
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
PLANT;
PROCESS ;"fcvtjeCan'fc
PROCESS NOTES:
METHOD 110 DATA SHEET
DATE:
- V
AMBIENT TEMPERATURE:
BAROMETRIC PRESSURE;
TEDLAR BAG NUMBER: 3
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
D
s
10
^00
10
p
o
50(9
veto
/Ait?
ivw\(> to//grf£f(
-------
Page B-10
PROJECT 1906 BENZENE/BaP PRESURVEY
Plant
SAMPLE DATA
Process ojr
Toj
Date
Sample No.
TD i
Time Sampled
Sample Type: Liquid Air
Sample Temperature
T) ^
o
r- c/
Ambient 'Temperature
Description of Sampling Location:
Q
f>
Sample No.
rp
Time Sampled
Sample Type: \Liquid ) Air
Sample Temperature
8" a
Ambient Temperature
Description of Sampling Location:
I
LC>TJ3
-t~ C t
(T
Q
Sample No.
Time Sampled
Sample Type: Liquid Air
Sample Temperature
Ambient Temperature
Description of Sampling Location:
Scott Environmental Technology Inc.
-------
Page B-ll
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
PLANT;
METHOD 110 DATA SHEET,.
DATE:
PROCESS: T5 y- j ggq/vt'e r-^S" (?cx //g rs/
0
PROCESS NOTES:
-3'
AMBIENT TEMPERATURE: ~
BAROMETRIC PRESSURE:
TEDLAR BAG NUMBER:
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
10 '
0
^00
if U>v \~ uA
letk.OL
¥-
!c-
fO
o
ff cd
SLO
as
1)0
-------
Page B-12
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
PLANT:
METHOD 110 DATA SHEET
DATE:
PROCESS;
'^5
PROCESS NOTES:
\t>" ID
AMBIENT TEMPERATURE: ~ 95" V-
BAROMETRIC PRESSURE; c
TEDLAR BAG NUMBER:
4-
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
0
S~l O C f
0
•73
/r
13 "C
ft-/*,;^.
39
^•70
to
/?
x
r
q -7
-------
Plant
Page B-13
PROJECT 1906 BENZENE/BaP PRESURVEY
SAMPLE DATA
Process
Date
. / Q <3
Sample No
Sample Type: (Liquid ) Air
Sample Temperature / 7 C/
Time
Sampled « '-> i T'>
Issuer
I
>y £$d k r
Ambient Temperature ^ I o
Description of Sampling Location:
Sample No.
t,
Time Sampled
/^
Sample Type: (Liquid Air
Sample Temperature
Ambient Temperature
Description of Sampling Location:
Sample No.
Sample Type: Liquid Air
Sample Temperature
Ambient Temperature
Description of Sampling Location:
Scott Environmental Technology !nc
Time Sampled
-------
PROJECT 1922
PLANT;
Page B-14
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
METHOD 110 DATA SHEET
DATE:
PROCESS: L^M-oi'l (WdecTSeT we n't" AMBIENT TEMPERATURE:
PROCESS NOTES: BAROMETRIC PRESSURE: 2.*? .S~l
£, " 3lO vevft" TEDLAR BAG NUMBER: ^
TIME
IC'.lC" ^
5"
10
f£
SO
3^
30
1
STACK TEMP
GAS VELOCITY t PUMP FLOWRATE
//O
130 -(+/Wv(>
(3n
130
lao
132)
|^O
-
•*.
j*\ i f fiit f*^
) // xi A **> V 1- ^i
2 £#Zz_
l'^ j^n^ ^ ^/^^
\& JlLy^ (c^&l
,3 ,0 JLpL^ 6^ &&
2s) 6 ^ 9K
.-%/ f / /^ ^ '^j
•
-------
Page B-14
SCOTT ENVIRONMENTAL TECHNOLOGY, INC..
PROJECT 1922
PLANT;
g-fee/
METHOD 110 DATA SHEET
-\trt\ DATE:
PROCESS :
PROCESS NOTES:
AMBIENT TEMPERATURE:
BAROMETRIC PRESSURE:
TEDLAR BAG NUMBER:
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
0
F
3
57 6*
5
SlO
CO
as
-------
PROJECT 1922
PLANT;
i'age rs-j.5
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
METHOD 110 DATA SHEET
3
DATE
: 7/11
PROCESS;
PROCESS NOTES:
AMBIENT TEMPERATURE:
BAROMETRIC PRESSURE: £
TEDLAR BAG NUMBER :__"7_
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
o
loH'F
//O
**?/!
/oo
10
3D
30
ib
US"
a
3(9
-------
Page B-16
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
PLANT;
PROCESS:
PROCESS NOTES:
METHOD 110 DATA SHEET
DATE:
12.
AMBIENT TEMPERATURE:_
BAROMETRIC PRESSURED
TEDLAR BAG NUMBER:
f-
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
. (o7
-------
PROJECT 1922
PLANT:
Page B-17
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
METHOD 110 DATA SHEET
.DATE:
?f~
PROCESS;
PROCESS NOTES:
AMBIENT TEMPERATURE
BAROMETRIC PRESSURE
TEDLAR BAG NUMBER:
TIME
C
STACK TEMP
GAS VELOCITY
5% fnKi
10
'5
iol
-*_y
-------
Page B-17
PLANT; iH ."•'•'
PROCESS; t\'ciu^t('£. ]r t'ig '(\^! T<\ ^U
PROCESS NOTES : ,-, ,
TIME
0
GA
-7 •' "' *~> .' '">• /
;V,TE:_._ LLL^LL':.^
/ii-iBiE:.";. :-;-;Fr:- .:".;i-:..:._
BARCMLVUIC ?EE^SUi;. '.:
)I>.R BAG NUMBER: /
/;c_ :£:...„
f-
fT
T7
ID
/o , 7?o
l-o
i-
79 'C.
i j 6 r-'
$
to
(n£> • Vp
ze
o
3, X9/ Pi-
-------
PROJECT i&2^..
Page B-18
'\
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
•METHOD liO D±iTA oluLEIT
DATE:
4 ,
PROCESS ;
tf
\
* i » <:i ^ /
VVQ •
PROCESS NOTES:
AMBIENT TEMPERATURE:
.- i
«BAJWMETRIC PRESSURED
HDLAR .BAG NUMBER:
TIME
STACK TEMP
GAS^VELOCITY
PUMP FLOWRATE
£•13 0
0.
10
6*60
ft
7/ e c
/o
-------
Page B-19
iiCOT-" ?f UO:;ME;--.T;J. 'rj .OOLOGY, INC.
PROJECT 192?
110
PLAMTJ
DATE:
PROCESS:
PROCESS NOTES:
AMBIENT TEMPERATURE:.
BAROMETRIC PRESSURE:,
BAG NUMBER:
TINE
STACK TEMP .
GAS VELOCITY
PUMP ..fLOWRATE
/o
c
30
no
ct
JTo
0
~^0&f
/yfU
-------
Page B-20
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
7
PROJECT 1922
PLANT ;
METHOD 110 DATA SHEET
DATE:
•Ui-
PROCESS:
PROCESS NOTES: <,-)•£ a ii^ cn &
^—. \/ o / /_/
AMBIENT TEMPERATURE:_
BAROMETRIC PRESSURED
TEDLAR BAG NUMBER:
TIME
STACK TEMP
GAS VELOCITY
PUMP FLO',>/RATE
n
/o
Sax
.
0 \A<\( ;
A . ^ Hn l*» llw
K.,v
x / ^'^
s—7T ~y i f / L » • •> -&
f 0 , 51 ^Iki^^S
n e J
f^g-f 9.
l
j in
-------
PROJECT 1922
PLANT: &
PROCESS; ftJnftV^
PROCESS NOTES:
Page B-21
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
METHOD 110 DATA SHEET
DATE:
Af
^, f&>
"
AMBIENT TEMPERATURE:
BAROMETRIC PRESSURE:
TEDLAR BAG NUMBER: \J?
TIME
STACK TEMP
GAS VELOCirf
PUMP FLOWRATE
-1GO./00 r
0
(T
20
j£/'/2 - Itol.Zoo
0
9 i M ?
-------
Page B-22
<3
3
6
l/'C -
-H
- /.-:•"
4
I r-. .A
<>i *
' J -".
-------
Page B-23
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
PLANT;
PROCESS t OgwtV
PROCESS NOTES:
TRACER GAS DATA SHEET
/-fofKWim Pfl
DATE:
WIND SPEED;
u-a.-u a.
I f na
Sampler Number
Distance from Source
Sampling Rate
Pump Numbers
Tedlar bag numbers
Start Time
Stop Time.
WIND DIRECTION:
incL . IVl" n€ & )-€$-/• AMBIENT TEMPERATURE: 7^ 5~.
<{
C IA,
BAROMETRIC PRESSURE;
fttfr
/O tp
!3
(0
ir.T.1
ir.s^f
3
c fc u'
UPWIND
1T
ISOBUTANE RELEASJ::: Gas Temperature
TIME
o
3
G
70
9.0
30
METERED VOLUME
-7
-74.
7S". 5^77
7o
76. /
"76, -7^0
77. 3
Gas
C\r^.
TIME
METERED VOLUME
-------
Page B-24
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
I £(,A)
PROJECT 1922
TRACER GAS DATA SHEET
PLANT: J5£ThU/\fi,m D'^J/ ) V €//
JdJ^ju^ DATE: ' / [Q 1 6^
PROCESS: JP(\\tfir HocJ- Unf-\-
PROCESS NOTES:
Sampler Number
Distance from Source
Sampling Rate
Pump Numbers
Tedlar bag numbers
Start Time
Stop Time
WIOT SPEED:
WIND DIRECTION:
AMBIENT TEMPERATUI
BAROMETRIC PRESSUI
DOWNWIND
(
ID fr.
Id
£>
14
a o?
£fk
13V31I
£
(^ fr
IV.tpl^
3
S3
I a: of
Q; 31
IE: S~ &C Cf
IE: '21\5"5~
e^'V
3
/-5v -Pf-
|0 ^/v
3
34
1 ~> A?
/#•
J°.-tpk
^
39s.
fc:/o
ll^o
ISOBUTANE RELEAS:.'.: Gas Temperature
TIME
0
/•o
G
an
3 c
METERED VOLUME
. 3 )
$1 . 447
ff L
3 . o i a
.. / 3
^•3.100
* o.
Gas
TIME
f>w
METERED VOLUME
-------
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
PLANT;
PROCESS ;
PROCESS NOTES:
F(
oa
Sampler Number
Distance from Source
Sampling Rate
Pump Numbers
Tedlar bag numbers
- Start Time
Stop Time
TRACER GAS DATA SHEET
DATE:
o
WIND SPEED:
WIND DIRECTION:
A i
/HIT 1
AMBIENT TEMPERATURE:,
BAROMETRIC PRESSURE:
DOI^WIND
3
UPWIND
4*
/o:. 30
ISOBUTANE RELEAS;:: Gas Temperature
TIME
10 '.-So 0
4-
lo
12.
f?
lo
METERED VOLL"1E
•fo-7.
Gas
I D°l*
.1/0
do.
hQ.r 14 .ft'
• lUfl^
TIME
METERED VOLUME '
-------
PROJECT 1922
PLANT;
PROCESS:
PROCESS NOTES:
Sampler Number
Distance from Source
Sampling Rate
Pump Numbers
Tedlar bag numbers
Start Time.
Stop Time
Page B-26
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
TRACER GAS DATA SHEET
DATE:
WIND SPEED theses
rf-
AMBIENT TEMPERATURE:,
BAROMETRIC PRESSURE:
DOWNWIND
o
G
10
I/:
=!?
3
/ WIND DIRECTION: frvp^ffy S<9
/I AMBIENT TEMPERATURE: ^KO
UPWIND
(3
ISOBUTANE RELEAS::: Gas Temperature
TIME
U'.ll
0
(o
IZ
1C?
METERED VOLUME
1)0
1 4.
IK.
//IT.330 .
Gas
:IME
METERED VOLUME
-------
PROJECT 1922
Page B-27
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
TRACER GAS DATA SHEET
PLANT: SeVMC-Vvevw ^>\
-2-
-^
->
3
IfT
3
3
/G
UPWIND
^
/7
•
ISOBUTANE RELEAS:-'.: Gas Temperature
TIMEfMETERED VOLUME
/o
^^
0,
So
Gas
TB1E
METERED VOLUME
-------
PROJECT 1922
PLANT ;
Page B-28
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
TRACER GAS DATA SHEET
DATE:
-TEsr 3
PROCESS : Denver F(oa4-
WIND SPEED:
PROCESS NOTES:
WIND DIRECTION; Most"//
AMBIENT TEMPERATURE :
BAROMETRIC PRESSURE:
ff $"
Sampler Number
Distance from Source
Sampling Rate
Pump Numbers
Tedlar bag numbers
.Start Time
Stop Time
DOWNWIND
lo
2-
11
UPWIND
ISOBUTANE RELEAS": Gas Temperature
TIME
o
10
Zo
Z.G
is
50
METERED VOLUME
Gas
TIME
METERED VOLUME
, ^ o. /3^74
/HOT/
-------
Page B-29
PROJECT 1906 BENZENE/BaP PRESURVEY
Plant
su,
'roc ess
Date
f,
Sketch of Process;
Include dimensions and flow directions.
Process Description;
Scott EnvironmentaJ Technolosylnc
-------
Page B-30
PROJECT 1906 BENZENE/BaP PRESURVEY
Plant
Date 7
/f/ffr
Sketch of Process:
Include dimensions and flow directions.
Process Description:
Scott Environmental Technolosy lr>c.
-------
Page B-31
PROJECT 1906 BENZENE/BaP PRESURVEY
Plant
Process
f 6//t/Y" Date 7 7/57
Sketch of Process;
Include dimensions and flow directions.
Process Description;
;<**)
4"
Scott Environmental Technology Inc
-------
Plant
Page B-32
PROJECT 1906 BENZENE/BaP PRESURVEY
— s AM PL E - D A-T-A •
Process
Sample No.
Time Sampled
Sample Type: / Liquid/ Air
Sample Temperature
Ambient Temperature
Description of Sampling Location:
Sample No. /fcywgf
^
Date
Sample Type: ( LiquidJ Air
Sample Temperature ^ (# C
Ambient Temperature
Description of Sampling Location:
Time Sampled
Sample No.
Sample Type: \Liquid) Air
Sample Temperature
Ambient Temperature
u-
Time Sampled
Description of Sampling Location:
Scott Environmented Technology Inc
-------
Page B-33
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
TRACER GAS DATA SHEET
PLANT ; f f k if . U IK
fe/A. /£ /t
DATE:
PROCESS :
WIND SPEED:
PROCESS NOTES:
SUv+eJ? T'S~0*«~
WIND DIRECTION:
AMBIENT TEMPERATURE•:
BAROMETRIC PRESSURE:
Sampler Number
Distance from Source
Sampling Rate
Pump Numbers
Tedlar bag numbers
Start Time
Stop Time
DOWNWIND
10
Id
f.o*
£.0k
10
//}
3
10
(0
3
ti'OO
UPWIND
ISOBUTANE RELEASE: Gas Temperature
TIME
13
(0
^^
METERED VOLUME
. o-rs"
. 3
Gas
TIME
C a h
k
loo/C.S
, t v
d
foo
fn
METERED VOLUME
fv/7l/
i/m
Lover "ft? i/h^n V
f
iT
r .(23
-------
Page B-34
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
TRACER GAS DATA SHEET
PLANT: \9 ^mV^Vxi/K 3*&\. .^ &MObJMUv^ •
PROCESS: $Vanl\\t*CLl<£h.C. KK^ r
PROCESS NOTES: <* . /•>£
5* If ?K *£: 5>£>
Sampler Number
Distance from Source
Sampling Rate
Pump Numbers
Tedlar bag numbers
Start Time
Stop Time
• DATE: / / \0 / iSU
- WIND SPEED:
WIND DIRECTION:
AMBIENT TEMPERATURE:
. BAROMETRIC PRESSURE:
DOWNWIND
(0 (4
to toL
Lf
13
1^
Uf4
• 10
3
34
Jpk
^
(o 4-4
/o JtoL
6U
•i
i
UPWIND
4
Cf-f-
jo J^pL
I
3
ISOBUTANE RELEASE: Gas Temperature
TIME
lo
i
zz
30
METERED VOLUME
. 000
"Tt,.
Q-7.
7. 3 K
Gas PrpggiiT-o
TIME
•ffto
_£'
-
METERED VOLUME
F
ft
^~
*f
- A
-------
Page B-35
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
TRACER GAS DATA SHEET
PLANT;
DATE:
7
PROCESS;
32.f/3
/ - 9
13:?,
1 3s: o to
Gas
TIME
-.0
7.
-
;f
.-.
METERED VOLUME
-------
Page B-36
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
5
PROJECT 1922
PLANT :
TRACER GAS DATA SHEET
S/T I f ;
DATE:
o
PROCESS ;
rfl£(-f
WIND SPEED; Van*R.bl
PROCESS NOTES:
WIND DIRECTION:
AMBIENT TEMPERATURE :
BAROMETRIC PRESSURE:
, S)
Sampler Number
Distance from Source
Sampling Rate
Pump Numbers
Tedlar bag numbers
• Start Time
Stop Time
\p\ AJ O
DOWNWIND
10
1-
ISOBUTANE RELEASE: Gas Temperature
TIME
10
It
IS*
zz
so
METERED VOLUME 4H- '
iS~~7. 4,3-0
5-7 .
10
72.7
3.10^/30,
-------
B-37
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
PROJECT 1922
TRACER GAS DATA SHEET
PLANT: &>;Uvtd\AM<\ SWj? . • DATE: ~? f {$ \ £0
PROCESS: Aj^h^ffAfinL VW&(jC
PROCESS NOTES:
PtlNVtrvvirte. (,2- 3 (
Sampler Number
Distance from Source
Sampling Rate
Pump Numbers
Tedlar bag numbers
Start Time
Stop Time
WIND SPEED: ^ ^ £ ,cA^M
WIND DIRECTION: A/
T-^
AMBIENT TEMPERATURE:
BAROMETRIC PRESSURE:
DOWNWIND
[
<] ft
- /o j0/?A
?
^^G
•
i
H
$:30
7^
i 2 ^f-
/n J^P/A
_L^ , 1^
"'7'. 3fc j^:so
^,
3 -fi-
. fo *pL
n ^y
73(o S\3o
UPWIND
it
Z5 ft-
.-lOApL
.
2^ 2~?-
'7--5fo ^N3C>
k
ISOEUTANE RELEASE: Gas Temperature
TIME
0
In
20
30
METERED VOLUME
I-77J
1T7.
17^.0,3
S
7*7
Gas
TIME
/ D
IZ
w
u
METERED VOLUME
/S2./00
-------
PROJECT 1922
Page B-38 .
•SCOTT ENVIRONMENTAL TECHNOLOGY., INC,
•;TRACER .GAS-DATA SHEET
DATE;
.PROCESS: DdJS&
PRCESS .NOTES-:-,
.
pi-J'. : .WIND SPEED;''., /ffr/L'f'
.
WIND. -DIRECTION: 5
AMBIENT TEMPERATURE:_
. ; BAROMETRIC PRESSURE: :.
Sampler Number
Distance .from Source
Samp.iing Rate • • . ;
Pump Numbers
Tedlar .bag numbers
.Start.Time : .;.. '•' '.' ...'•
Stop .Time . •• •
DOWNWIND .
/r
ISOBUTANE-. RELEASTi:: . Gas Temperature
TIME
6-
#.
-.I.Q
-11.
METERED VOLUME .'
:i3f. •.-.•
_ly • ££ 4'*>Q
Tip I•• y IT:
Gas
TIME .
to
a-
..
.UPWIND
METERED VOLUME
•[ "70/70.0 '..
>
-------
PROJECT 1922
Page B-39
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
TRACER GAS DATA SHEET
VOIP
PLANT: '3c*Kid>.vi Steel , FHUlfeken~ • DATE: • 7//W'?<9
PROCESS: '"VfU'gv" uvoi t" - n£JlU~ - will
PROCESS NOTES:
' i — •;—
Btf-CK'H'Cx-'n J -v-c i'' w\
UVu »KvS ^ h"Ylts?- ^H-iX
Sampler Number
Distance from Source
Sampling Rate
Pump Numbers
Tedlar bag numbers
Start Time
Stop Time
WIND SPEED:
WIND DIRECTION: ^> - S W '
>
AMBIENT TEMPERATURE: ^ ^ ° p '
BAROMETRIC PRESSURE: '1 ^ , 5^7"
DOWNWIND
-^'^ (-+-
10 'U'k-
(D
H-
[0\2S
1
."2-
^ff
—S
/«/ li
I *y * '— *-^ , -J
i
' 3 •
^Pf
1^
/O'.iS
\c\
\\.of
UPWIND
£j-
loC-f-
?
0
10
30
141,3-70
3.3/9
Gas
TIME
:0
•'If
0
/0/
3c
METERED -VOLUME
7, ^5"
is-/,
-------
Page B-40
PROJECT 1906 BENZENE/BaP PRESURVEY
Plant
gc-VKUk
Process 'we i
Date
Sketch of Process;
Include dimensions and flow directions.
Process Description;
Scott Environmental Techndogy Inc
-------
Page C-l
APPENDIX C
LABORATORY DATA SHEETS
Scott Environmental "technology Inc
-------
Project No,
CHROMA*
Date
ANALYSIS LOG
Analyst_
Time
Sample Identification
" '
(A
..«-
.
\\ ' - - -X
/-> ll: /
o- /
-------
I
s
g
ANALYSIS LOG
Project No,
Date
Analyst_
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
(1- C-
,,/ O -i t"\
(f >AvV
riA WVV
.
trc
U"
OQ
(B
x
n
CO
-------
Project No.
CHROMATOGRAPHIC ANALYSIS LOG
Date
\s.-
Analyst
v '6
Time
i
'
Sample Identification
\
' /> 7 J" O* \ / 1 ( 1 \ i: 'V- *. J i ,-- - , , { ; i
f -^ — i«^_ , •'«.. -'^-- \_
C ' •"• '•*-
\i> \e)-'^ ^ t O
•VI a', ^.-..^''t-"^
(^uwlU.J" '.'''. "f^
( ** • / ^X
•'^\ ( t — __i;. j. M J
'
-------
•X1
CHROMATOGRAPHIC ANALYSIS LOG V
Project No,
Date
? "(\ - '>.
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
V
.^_»- yf'
' < -J.-- '-<-••' ^
/cv'b
6-6 b
06 6'
. ^6 -X
/•TV
.&- -.
-------
1
CHROMATOGRAPHIC ANALYSIS LOG -'\rtl\X:. I
Project No,
Date
7 ' /(. \c
Analyst
-
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
v<
*
•} H.X
c~" v - *- ' -ff"
V '.^c-r— - — '— -v. - \T\ '- — -> 3
x^" ' <1
V /Ay (e-y /o.^VA/
/O
•c
/ -5"
/ ^
(kt,,..<.f^,Xi
AX-I- - -^
A
- —
tu
OQ
n>
o
o\
-------
CHROMATOGRAPHIC ANALYSIS LOG VS . v;. i'.s 0'. (;. ^ "~V~f V i \,
Project No, !'"'-'';-^
Date
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
..7.7. -vv>— • TE^'
(,"/
• o ,
0/6
/ 'j %'j" - •
i O>>
-------
CHKUMATUUKAi'tUU ANALI5IS LUU ,-./ ,". •! ,j • ( . • (' '* '
Project No, I'-W'A Date " / ' 1 1 ''->> Analyst "X V> ^-/ .
Time |
'<- '/.'Ov.-
->:X
Sample Identification
c^fr-^TM
/" ,v
-^-_ •*-' ( '•'•
^ " T" V~~ \ '^
\ ^ .,,'• •-'--- --• -.( \ (C'(/Jf '*-*
I ^
^ ..v .-.-.,^- \,j...
-. ^_ ^
V'- v%^ * •— ^-y-A
/.-.-^ C .)..-,;% '«
'' J
'M^
Peak
Height/Area
->/- -3 '
' 9- ^ T
' '-V C
_ '"'
r^5C-Y3
'-/. ^>
•~~)
..-,- . .-j^ A'v
Concentration
Factor
• ,.x-/.
•
•
. -j
-------
Project No.
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
/CCC X
^ V, O Jl
/3s-1 - ^'
/* -i ' ' I*'!
.1- •" 'j 11 •{
'ccc v - ^ Si-
(I Q >5l:/«
2r& t~'f
^j,.9.^
r 25 v;
-------
I
CHROMATOGRAPHIC ANALYSIS LOG
Project No,
Date
- >rc-
Analyst y \S
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
3
I
*<
?
T- r~f'. 0
/,*>-=••—•--> — > _;-"_>.'v
T-;v £:'
VK
/S
oft
-------
Project No,
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst j
Time '
i
Sample Identification
- . fv\,-3i '"'
^£y^:£^
:wZ Z
33 *t -
. C^/XIO
Peak
Height/Area
v
^9
Concentration
Factor
'
V/3
x^
,y(.( f
•
Concentration
V//.5,
Comments
/ / /57o ^ _^
• '^"
-------
I
f
Project No,
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst_
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
ft j&'
./-A isr v
^
/-J. 'rA
.
'/-• j
7<; >
70
/•(*(
.'^'5 c^^_
*
3
I "3
-------
CHROMATOGRAPHIC ANALYSIS LOG
S .-"CiUtO.: —. ^.--
» ]>
Project No,
Date
'?-/'•/ %<•"""
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
^oc
' (O X
-'•
-,;
5'. s a
"io.S'3
.i A 10
-------
I
Project No. iS.) .
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
s
-.f-'f— .
VV.
-------
Project No. / 'M-^
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst
Time
Sample Identification
Peak
Height /Area
Concentration
Factor
Concentration
Comments
\\
o,^
^
•- Tr-fv
- /OX
IT?. 51
x->^
PI
00
ID
I
(Ji
-------
Project No,
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst |rS
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
m \ AC .--.»;
ftwr™^
^ /' / C-
ClO.v:' O
OQ
m i
o j
M '
OS
• V
-------
CHROMATOGRAPHIC ANALYSIS LOG
Project No,
Date
Analyst
''-Time
Sample Identification
Peak
Height/Area
Concentration
Factor '
Concentration
Comments
'> OJ1
, cT XT«?
'{"'•• *
••^.r)^^
.. • •;-• S
v
6*.
n
15.76
77.5
-^-^ — ^
A
fu
OQ
(D
-------
I...
Project No.
CHROMATOGRAPHIC ANALYSIS LOG
Date /
Analyst
Sample Identification
.';JC%
Ss v
-
/OC
Peak
Height/Area
7
/7
Concentration
Factor
. o
0. (
Concentration
Comments
a
••a
p>
TO
(T>
o
M
00
-------
Project No,
CHROMAT(A-_ -xC ANALYSIS LOG
Date
Analy s t
O
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
•-?
JO
v
»
\
6
O ^
X7V *
4
^
>; x
D<^ V
- ^
\
<^L
C
-------
?•
CHROMATOGRAPHIC ANALYSIS LOG
Project No,
Date
"?
Analyst
•Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Cone en t r a t ion
Comments
>.
0
( '
d
0.1.9?
//o
/ . C-,^J
-------
ANALYSIS LOG
Project No,
Date /- /(»•> X>
v;
Analyst \ C>
f
Time ;
• Mitvo
U ^-f
• .
•
Sample Identification
/ \^y s^-- ^ - j , •+ • . ^ U* x. *f~- * L ^ C * t-*- • c" V " J J
^V ' I \ ^v.""
(" > :(i '"' :>'•'-<••-.
\7} C'" l'l ^^ - 'I « /(.i*^
$ "
ft^"" ^C)
t -^ ^*\ '
o
/-"^ -ffc.
Ou-c /Q)
iS.-s*1 ti
(\ ^^
X"V '-
Peak
Height/Area
!
A/0
-. O
- //^
V'j
/VO
x/0
,
Concentration
Factor
i
-s
O1'-' ^
Concentration
!
Comments
-------
Project No,
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Conunents
'b
A/O
r;H
>>
-------
Pro j ect No ," 3.
CHROMATOGRAPHIC ANALYSIS LOG
Date
CS
Analys t
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
^
*
o
o
.v-
V
"J"h
//O
I.O
O. i°-
•^•r -
. iO
-------
Project No. /
,-c.
CHROMATOGRAPHIC ANALYSIS LOG
Date - !. "7 ~
Analyst_
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
A
\\
,^
-P-r
- <"?..
- <**
Jo
i
51
-------
CHROMATOGRAPHIC ANALYSIS LOG
Project Not
Date
7-n -/o
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
3 \
.0 -
^5° ^"
/)
i
7
VS
50.5-
Wo
6'
-
-r -f >r-
a
-------
CHROMATOGRAPHIC ANALYSIS LOG
Project No,
Date
/ ~~ f / ~ c
Analyst
\>'V
Time
Sample Identification
Peak
Height /Area
Concentration
Factor
Concentration
Comments
10
Co . 1 1
7* '
,-2
-^ v'-i.
^
^
X
X
3
O.
5? 5
o
C-fc
5.0
, 05^
• r ' -
|f ^
<;rv
A" A -
-------
CHROMATOGRAPHIC ANALYSIS LOG
Project Not
Date
; - -J r~— 1 *' " -^
/- 1 ( 6^-
Analyst_
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
ftc^y
O
.-i.s
^
( ' V
"6 • « o
Oi
-------
Project No, j wi >
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
^ 5o^
cv
0
-------
X*
8
i1
Project No.
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst_
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
'4
^b ** ^(
£
*-.
""h
\
- -v v --
;*
5V
7 7. S"
3
/v
c-.JVo
cc
C.
-------
I
CHROMATOGRAPHIC ANALYSIS LOG
';- t7-. S> '
—«.-*• T-O. -v"v"\. ^^ ». •
Project No,
j , >J .)
Date
"/
Analyst ~\V:>
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
\
-if
'\
'ct
-Z #•
/
'5C-. 75"-
Mo
O.oS 7
e.c<7
OJO
:
. » v
7. j>
-------
CHROMATOGRAPHIC ANALYSIS LOG
Project No.
Date "? -
Analyst t"^v
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
.x-x A^— c c ---- -v
, ^ 6
R-^t
/-— "v \ - A^^.C^^-rV// O
hd
w
00
a>
o
-------
Project No.
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst_
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
<4-
V
Ac 3
/65
^
X
^
5)
frA Vt> ' ' O
/H ~
1 .((3 r.
V
5
-------
Project Not
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
,
- v.
,,t
, X,
•*
•<; ,-co
t-'^-T"
-------
Project No,
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analys t / Q
Time
Sample Identification
• «- ^ lot- v-\
:M^
-jf-'ivi'-
'
Peak
Height/Area
6(0
Concentration
Factor
C.
Concentration
/y->»
— ,
Comments
v>£t zUt
XT"-
OQ
o
i
U> i
'
-------
Project No.
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst ^ •«">
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
0
/
rf
i
6-A/J5
, <> c-/
ft ^%
/Vrr-Ju_f7tr,
65
Coo
. X
o,ci7
c '
/C
. .L^*-, .
Ov, __ _>
-------
Project No.
CHROMATOGRAPHIC ANALYSIS LOG
Date / ' d'--• *~ V
-------
Project No,
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
-------
Project No,_
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst
Time
Sample Identification
.~.«Q^
-,
&
«»^L
. OfiJ?
Peak
Height/Area
Concentration
Factor
2.
Concentration
Comments
13
00
n>
o
i
u>
oo
-------
Project No.
CHROMATOGRAPHIC ANALYSIS LOG
Pate
Analyst
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
°V 7
"
"
7 A
60
oO
^^ — " '
^^^
S '
1 '
<. lo
-------
APPENDIX D
TRACER GAS METHOD DEVELOPMENT
Scott Environmental Technology Inc.
-------
Page D-l
;•' . APPENDIX D .
TRACER GAS METHOD DEVELOPMENT
D.I Tracer Gas Selection
The initial consideration when using the tracer gas method
is the choice of a suitable gas. There are several criteria used in
the selection: First, the tracer gas must not be present in the atmos-
phere at the sampling location. Second, the tracer gas must be separable
from other components in the background at the sampling location and
quantifiable on the same GC column without interfering with the elution
of the compound(s) of primary interest. The tracer gas should also be
readily available, transportable, economically feasible, and safe for
the given usage situation.
For the determination of benzene emissions at secondary by-
products plants, isobutane is the recommended tracer gas. The second
choice for a tracer gas is a halogenated hydrocarbon. At secondary by-
products plants the hydrocarbons in the background atmosphere are almost
exclusively emissions from the coking operation and neither isobutane
nor halogenated hydrocarbons are present to any significant degree.
Isobutane was chosen over a halogenated hydrocarbon on the basis of
chromatographic elution characteristics. Isobutane elutes well before
the benzene peak thus eliminating any interference when using a tempera-
ture program for the chromatographic analysis.
The separation of isobutane from mixtures containing concen-
trations of hydrocarbons typical of secondary by-products plants was
verified by spiking samples collected at different sources in a secondary
by-products plant with various concentrations of isobutane and performing
Scott Environmental Technology Inc.
-------
Page D-2
a temperature program of chromatographic analysis to achieve the desired
degree of separation. In all cases the desired separation was achieved.
D-2 Dispersion Apparatus
The apparatus for the dispersion of tracer consists of a
cylinder of the tracer gas connected to a dry gas meter, a rotameter and a
dispersion tube. All necessary connecting lines are Teflon.
Two different dispersion tube configurations were tested, both
were constructed from 1/4" O.D. stainless steel tubing. The first tube
tested was 8* long with the tracer source connected to one end of the tube.
The tube contained holes every 19" which were progressively larger moving
away from the gas source. The hole size ranged from 0.062" to 0.031".
The second tube was 8' long in two 4' sections which are connected via a
T-joint to each other and to the tracer gas source. This dispersion tube
has 0.041" holes every 19" and the ends are capped.
L/W5"
<— D?N 6AS METER.
Of the two types of dispersion tubes tested the latter described
was more efficient for the dispersion of the tracer. This judgement was made
by visual inspection of the holes in each tube while isobutane was flowing at
Scott Environmental Techndosy Inc
-------
Page D-3
0.1 CFM. At this rate isobutane can be seen as it leaves the dispersion
tube and differences in the relative volume leaving each hole are visually
discernible. The first configuration had all gas coming out of the first
2 holes, whereas the second configuration had uniform emissions from each
orifice.
Benzene was also released in two ways; by evaporation and
a heated bubbler. Both methods proved adequate for experimental determina-
tions. When evaporation was used to release benzene, a stainless steel
pan 16" x 24" x 1/2" was employed to contain the benzene. During an
experimental determination benzene was added to the pan in 50 cc aliquots
at intervals frequent enough to maintain a constant surface area of benzene.
This was done in order to keep the emission of benzene at a constant rate.
However, this evaporation method proved unsatisfactory on days when the wind
speed exceeded 15-20 MPH due to the changing evaporation rate resulting
from gusting wind. A more steady emission of benzene was achieved by
using a heated bubbler. The bubbler system consisted of a 500 cc
impinger of the Greenburg-Smith design wrapped with a heat tape. The
impinger was kept at a constant temperature below the boiling point of
benzene. A rubber diaphragm pump was used to push atmospheric air through
a bubbler. Flow was regulated with a rotameter.
Scott Environmental Technology Inc.
-------
Page D-4
It was necessary to add more benzene during an experimental
run, because the emission rate drops substantially if the benzene level
drops too low in the impinger. The frequency of addition and the quantity
of benzene per addition are dependent on the emission rate being used.
For our determinations it was necessary to add 50 cc of benzene at intervals
of approximately 10 minutes.
D-3 Experimental Determinations
An experiment consists of the release of a known amount of
isobutane and benzene simultaneously. Samples are collected along a 30
arc, 25 feet downwind from the source of the emissions.
10'
Initially samples were grab samples collected in clean one
liter glass gas flasks. Later samples were integrated over a 1/2 hour
period and collected in clean 10-liter Tedlar bags via Emission Measure-
ments Air Quality Sampler with a flow rate of 10 LPH.
In initial determinations, portions of actual presurvey
samples containing 62% benzene were released in an effort to simulate
Scott Environmental Technology Inc.
-------
Page D-5
the type of sample which would be encountered in the field. Various amounts
of the sample mixture from 0.20 to 10 cc were released and samples were
collected downwind in 1-liter gas flasks. When these samples were analyzed
the amount of benzene detected was very small, approximately 20 ppb. From
this it was apparent that it would be necessary, to release significantly
more benzene in order to produce the necessary concentration at the
sampling location so that quantative mass to mass ratios could be calculated.
Because of the necessity of releasing more benzene and avoiding
the foul odor which the high concentration benzene field samples possessed,
it was decided that pure benzene be used for all subsequent determinations.
For the next series of experiments evaporation as previously
described was used to release benzene. This series of experiments produced
results accurate to within 10% of the theoretical mass to mass ratios
with a minimum benzene emission of 0.54 Ib/hr for the series. These
experiments were performed on days when the wind speed was light (5 - 10
MPH) and the wind direction was steady (See Table D-l).
The next experiment was designed to test the variations which
might be introduced when the wind speed and direction were less than favorable.
On the day selected the wind speed was 20-25 MPH and the direction was 180
variable due to a changing weather system. The rate of evaporation of the
benzene was noticeably affected by the conditions as were the dispersion
patterns of the emissions. Erratic results were produced by the meteorological
stress on key experimental variables. Calculated mass to mass ratios differed
from the theoretical value from 15% to as much as 56%, demonstrating the
effect of high and variable winds on the technique. In order to reduce
stress on the experiment the benzene bubbler as described was used to provide
Scott Environmental T^ndogy
-------
Page D-6
a steady source of benzene emission at a rate that would be independent
of meteorological conditions. On the day chosen to use the bubbler system.
the wind speed was 15-20 MPH and the direction was steady. Favorable re-
sults were obtained despite the relatively strong wind demonstrating that the
tracer technique is valid in winds up to 20 MPH depending on the sampling
location (see Table D-l).
D-4 Summary !
When using the tracer gas method it is necessary to verify
that the tracer gas is detectable at the sampling location of choice
as the method is somewhat dependent upon meteorological conditions.
The method works best when the wind speed is light to moderate, 5-15 MPH,
and the wind direction is steady. When the wind speed exceeds approximately
20 MPH or if there is no wind and/or the wind direction is too variable,
dispersion patterns condusive to accurate sampling are disturbed and
quantitative mass to mass relationships are difficult to establish.
The upper limit of stress with respect to meteorological conditions can
be examined by the spread of mass to mass ratios for each individual
sample for a given sampling run. If the calculated ratios are inconsistent
or the deviation between each calculated ratio and their mean is greater
than 20%, it would be necessary to seek an explanation based on process
variations or meteorological conditions or to void the sampling run and
possibly suspend sampling until conditons are more favorable.
D-5 Field Sampling Strategy
The program for a sampling run will generally involve the
collection of triplicate downwind samples and a single point upwind sample.
Actual sampler locations will be determined by the gas chromatograph on
Scott Environmental Technology Inc.
-------
Page D-7
site. Grab samples will be collected in glass flasks and analyzed to
determine the benzene concentration in the vicinity of the source to be
tested. This information will be correlated with wind speed and direction
to choose the exact sampler locations. In the ideal case downwind
samplers will be equidistant from the source and along approximately a
30° arc.
Two sets of samples will be integrated over separate one-
half hour periods and together constitute a single test. Samples
will be collected by Environmental Measurements AQS II sampling system
into clean 10-liter Tedlar bags. Tedlar bags to be reused for sampling
will be flushed three times with nitrogen and allowed to sit overnight
three quarters full. Prior to their next use each will be analyzed for
benzene content.
The tracer gas dispersion apparatus will be positioned over
the source to be tested as near as possible to the actual emissions.
Ideally the dispersion tube or support member will span the source of the
emissions at its center.
Scott Environmental Technology Inc.
-------
TABLE D-l
EXPERIMENTAL DATA
Release Benzene
Rate Release Wind Wind Theoretical /ic, 4>/icA
g/min Method Sample Type Speed Direction T/ic, #1 #2 //3 "* Average
41 - Benzene
ic, - Isobutane
* No benzene, only Isobutane detected.
i ° 5226 Evaporation Grab 0-5 MPH Steady 0.005 *NO NO NO ---
4
d> fl QQ1
* a ,, Evaporation Grab 0-5 MPH Steady 0.120 *NO NO NO ---
ic, o.e.1
t 4*75ifi Evaporation Grab 0-5 MPH Steady o'.59 0.64 0.64 0.65 0.645
1C4 ''-1"
* 9.40
ic, 6.38 Evaporation Integrated 5-10 MPH Steady 1.47 1.57 1.43 --- 1.50
t 10ii5^o Evaporation Integrated 20-25 MPH Variable 0.80 1.29 1.82 0.94 1.35
ic . x j • j y
ic9 8°25 Bubbler Integrated 15-20 MPH Steady 1.14 1.40 1.93 1.02 1.18
iC6'3<3 48 Bubbler Integrated 0-5 MPH Steady 0.91 0.97 0.96 0.96 0.96
J 6*J8/Q Bubbler Integrated 0-5 MPH Steady 1.00 0.91 0.86 0.89 0.89
1C f V • ^O
t)
oo
-------
APPENDIX E
FIELD AUDIT REPORT
Scott Environmental Technology Inc.
-------
Page E-I
FIELD.AUDIT REPORT
PART A - To be filled out by organization supply unit cylinders (RTI)
1. Organization supplying*audit sample(s) and shipping address
• —
Research Triangle 'institute, Post Office Box. 12194, Research Triangle Park,-NC
. . ._ __
2. Audit supervisor, organization, and phone number (EMB Technical
. Manager) „.«,.«. •
Dan Bivens, EPA
3." Shipping instructions '- Name, 'Address, Attention
*
Scott Environmental technology '
Post Office Box"D-11
PTurnsteadviHe, PA 18949 'ATTN: Bob Denyszyn'
t
4. Guaranteed arrival date for cylinders 6/10/80
5. Planned shipping date for cylinders 6/10/80
&. Details on audit cylinders for last analysis •
. . ' Low Cone. High Cone.
a. Date .of. last analysis 5/30/80- 5/30/80
b. Cylinder number B-1372 'B"921
c. Cylinder, pressure,. PSI 1750 1500
d. Audit gas(es)/balarice, gas vv Benzene/N? Benzene/N?
e. Audit gasCes) ppm ""7.93 154.4 .
f. Cylinder construction Steel Steel
-------
PART B - To be filled out by audit supervisor
1. Organic chemical manufacturing process Cofcc
2. Location of audit
Page E-2
3. Name of individual audit and organization
4. Audit results
a. Cylinder number
b. Cylinder pressure before
audit, psi
c. Cylinder pressure after
audit, psi
d. Audit date and measured
concentration, ppm
Date
'Analysis #1 ?'/ v/jC-
' . «™^^^^^^^^^^^^^^^^™—
•Analysis £2 77 *y'j C<
Analysis #3 _£
7 '
e. RTI concentration, ppm
(Part A, 6d)
Low Cone. High Cone.
CH3TZ,
7't-"/
I4CO
" /3'f.Z/
(l-
-------
f. Audit accuracy* . Pase E~3
Analysis £1 - '.'%.'*- -/
Analysis ?2 ~'$
• .Analysis S3 • • — Z// -/3,06
' \ *Percent accura^ ^Measured' Concern tone. 'x 1QQ =-' ' .
g. Problems detected (if an.>? S^/7 "''s Wr x.-v.> •.•>/>;/.'
-------
-JOT
FROM:'.
Page E-4
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
Plumsteadville, Pennsylvania 18949
INTERDEPARTMENTAL MEMORANDUM
DATE. TuLy \g
SUBJECT:.
HU;j
CM ( t/
t/~
^ j> c S~£LJJ -V-
..JLV £0^ *?•
U ' VbW' 2 ff^
Vy^- ± i'l
V\
("0 --r
—-—7 / / - • .. ^
^/': :.--•
-------
Page F-l
APPENDIX,F
PROJECT PARTICIPANTS
Scott Environmental Technology Inc.
-------
SET 1957 01 1080
APPENDIX F
PROJECT PARTICIPANTS
The following people participated in some phase of the sampling
program at Bethlehem Steel.
From Scott Environmental Technology, Inc.:
Tom Bernstiel, Chemist
Jack Carney, Chemist
P. K. Chattopadhyay, Chemist
Dan FitzGerald, Manager, Eastern Operations
Kevin Gordon, Technician
Carolyn Graham, Chemical Engineer
Scott Henderson, Environmental Scientist
Lou Reckner, Vice President & General Manager
Joe Wilson, Senior Technician
From Research .Triangle Institute:
Ralph Roberson
Dave Marsland
From U. S. Environmental Protection Agency
Lee Beck
Dan Bivins
Scott Environmental Technology Inc.
-------
Page G-l
APPENDIX G
EPA METHOD 110
Scott Environmental Technology Inc.
-------
Page G-2
Federal Roaster / Vol. 45. No. 77 / Friday, April 18. 1080 / Prcnosed Rules
2RS77
(f) All con'iri1.:*'.'! monitoring systr-ms
used in accordante-with this section are
to complete a minimum of one cyrii; of
operation (sampling.-analyzing, and data
recording] fur each successive 15-minute
period.
(y) Owners or operators of all
continuous monitoring systems installed
in accordance with this subpart shall
check the zero and span drift at least
once daily in accordance with ihe
method prescribed by the manufacturer
of such systems unless the manufacturer
of such systems recommends
adjustments at shorter intervals, in
which case such recommendations shall
be followed. The daily span check is to
be conducted with reference gas
containing a concentration of benzene
determined to be equivalent to the
emission limit for that source based on
the emission tests required by § 61.94.
(h) The calibration is to be done with
either—
(1) A calibration mixture prepared
from the liquids and gases specified in
Section 5.2.1 and 5.2.2 of Test Method
110 and in accordance with Section 7.1
of Test Method 110: or
(2) A calibration gas cylinder
standard containing the appropriate
concentration of benzene. The gas
composition of the calibration gas
cylinder standard is to have been
certified by the manufacturer. The
manufacturer must have mcorr.mended a
maximum shelf iifo ."or each cylinder so
g-is standards vail no: be used if their
concentration has chanced greater than
±5 percent from the certified value. The
data of gas cylinder preparation.
certified benzene concentration, and
r(.comn;oncled maximum shell life must
have been affixed to the cylinder before
shipment from the manufacturer la the
buyer. If a gas ch.-ornatogr^.ph is used as
the continuous monitoring system, these
gas mixtures may be used directly to
piepare a chrorr.atograph calibration
curve as described in Section 7.2 of Test
Method 110 for certification of cylinder
standards and for establishment and
verification of calibration standards.
(ij After receipt and consideration of
written application, the Administrator
may approve use of an alternative or
equivalent continuous monitoring
system, alternative monitoring
procedures, or alternative monitoring
requirements.
(Sec. 114. Clean Air Act as amended [42
U.S.C. 7414|)
§ 61.9S Recordkeeping requirements.
(a) The owner or operator of each
source to which this subpart applies
shall maintain daily records of the
monitoring information specified in
I 61.95[a).
(b) Records arc to b.2 retained at the
source and made available for
inspection by the Administrator for a
minimum of 2 years.
(Sec. 114. Clean Air Act as amended [42
U.S.C. 7414))
Appendix B—Test Methods
Method 110. Determination of Benzene From
Stationary Sources
Performance of this method should not be
attempted by persons unfamiliar with the
operation of a gas chronmtoqraph. nor by
those who are unfarr.ilar with source
sampling, because k.-.owledse beyond the
scop* of this presentation is required. Care
must be exercised to prevent exposure of
sampling personnel to benzene, a
carcinogen.
/. Applicability and Prinicple
1.1 Applicability. This method applies to
the measurement of benzene in stack gases
from processes as specified in the
regulations. The method does not remove
benzene contained in particulate matter.
1.2 Principle. An integrated bng sample of
stack gas containing benzene and other
organics is subjected to gas chromatographic
(CC) analysis, using a flame ionization
detector (FID).
2. Range and Sensitivity
The range of this method is 0.1 to 70 ppm.
The upper limit may be extended by
extending the calibration range or by diluting
the sample.
3. Interferences
Thi; chromatn.araph columns ar.J the
coiTL-spon:::.-^ cpuru:ir.5 pjraniat'.rs herein
•Jcs^ribad normal':;' pro\ids an adequate
resolution of benzene: however, resolution
interferences may be encountered on some
sources. Therefore, the chromatograph
operator sh:i!l select the column and
operating parameters best suited to his
particular analysis croblem. subject to the
approval of the Adrrir.istrutor. Approval is
automatic provided i.-.si! the tester produces
confirming data throuoh an adequate
supplemental analytical technique, such as
analysis with a different column or GC/mass
spectroicopy. and hus the data available fur
review by the Administrator.
•}. Apparatus
4.1 Sampling (see Figure 110-1). The.
sampling train consists of the following
components:
4.1.1 Probe. Stainless steel. Pyrex * glass.
or Teflon tubing (as stack temperature
permits), equipped with a glass wool plug to
remove paniculate matter.
4.1.2 Sample Lines. Teflon, 6.4 mm oursiJe
diameter, of sufficient lenvjih to connect
prol:e to bag. Use a new unused piece for
each series of bag samples that constitutes an
emission test and discard upon completion of
the test.
4.1.3 Quick Connects. Stainless stoel,
male (2) and female (2). with ball uhscks (one
p.->ir without) !iicn!o
-------
2GG73
Page G-3
Fcder.il Register / Vol. 45. No. 77 / Friday, April 10, 1980 / Proposed Rules
STACK WALL
FILTER
(GLASS WOOL)
X
f
*==)=.-----..•
I
s
PROBE
/
^----.-- = z
1
/
TEFLON
SAMPLE LINE
VACUUM LINE
QUICK
CONNECTS
FEMALE
TEDLAR OR
ALUMINIZED
MYLAR BAG
NEEDLE
VALVE
FLOW METER
CHARCOAL TUBE
\
PUMP
RIGID LEAK-PROOF
CONTAINER
Figure 110-1. Integrated-bag sampling train. (Mention of trade names or specific products
does not constitute endorsement by the Environmental Protection Agency.)
BILUNQ CODE 6560-01-C
-------
Page G-4
Federal Register / Vol. 45. Nn. 77 / Friday. April 18, .1980. / Proposed Rules
26679
4.3.2 Chrorr.atographic Columns. Columns
as listed below. Th>' analyst rrviy use other
columns provided that the precision and
accuracy of the analysts of benzene
standards are not impaired and he has
avdil.ible foe review information cnm'irming
that there is adequate resolution of the
benzene prak. (Adequate resolution is
defined as an area overlap of not more than
10 percent of the benzene peak by an
interferent peak. Calculation of area overlap
is explained in Appendix E. Supplement A:
"Determination of Adequate
Chromatographic Peak Resolution.")
4.3.2.1 Column A: Benzene in the Presence
of Aliphatics. Stainless steel, 2.44 m by 3.2
tr.m. containing 10 percent 1.2.3-tris (2-
cyanoetho.xy) propane (TCEP) on 80/100
Chromosorb P AW.
4.3.2.2 Column B: Benzene With
Separation of the Isomers of Xylene.
Stainless steel. 1.83 m by 3.2 mm. containing 5
percent SP 1.200/1.75 percent Bentone 34 on
100/120 Suplecoport.
4.3.3 Flow Meters (2). Rotameter type. 100
mi/min capacity.
4.3.4 Gas Regulators. For required gas
cylinders. •
4.3.5 Thermometer. Accurate to 1° C. to
measure temperature of heated sample loop
at time of sample injection.
4.3.6 Barometer. Accurate to 5 mmHg, to
measure atmospheric pressure around gas
chromatograph during sample analysis.
4.3.7 Pump. Leak-free, with minimum of
100 mL/min capacity.
4.3.8 Recorder. Strip chart type, optionally
equipped with either disc or electronic
integrator.
4.3.9 Planimeter. Optional, in place of disc
or electronic integrator, on recorder, to
measure chromatograph peak arsas.
4.4 Calibration. Sections 4.4.2 through
4.4.5 are for the optional procedure in Section
/ .1.
4.4.1 Tubing. Teflon, 6.4 mm outside
diaiTiuter, separate pieces marked for each
calibration consentration.
4.4.2 TeJlar or Aluminized Mylar Bags. 50
L capacity, with valve: separate bag marked
for each calibration concentration.
4.4.3 Syringes. 1.0 nL and 10 /iL. gas tight;
individually calibrated to dispense liquid
benzene.
4.4.4 Dry Gas Meter, With Temperature
and Pressure Gauges. Accurate to :r2
percent, to meter nitrogen in preparation of
standard gas mixtures, calibrated at the fiotv
rate used lo prepare standards.
4.4.5 Midget Itr.pinger/Hot Plate
Assembly. To vaporize benzene.
5. Reagents
Use only reagents that are of
chromatographic grade.
5.1 Analysis. The following are needed
for analysis:
5.1.1 Helium or Nitrogen. Zero grade, for
chromatograph carrier gas.
5.1.2 Hydrogen. Zero grade.
5.1.3 Oxygen or Air. Zero grade, as
required by the detector.
5.2 Calibration. Use one of the following
options: either 1.2.1 and 5.2.2. or 5.2.3.
5.2.1 LV:'.ze:ii;. 03 Mol Percent Pure.
Certified l;y the- manufacturer to contain a
minimum of 99 Mol percent benzene; for use
in the preparation of standard gas mixtures
as described in Section 7.1.
5.2.2 Nitrogen. Zero grade, for preparation
of standard gas mixtures as described in
Section 7.1.
5.2.3 Cylinder Standards (3). Gas mixture
standards (50.10. and 5 ppm benzene in
nitrogen cylinders). The tester may use
cylinder standards to directly prepare a
chromatograph calibration curve as
described in Section 7.2.2, if the following
conditions are met: (a) The manufacturer
certifies the gas composition with an
accuracy of ±3 percent or better (see Section
5.2.3.1). (b) The manufacturer recommends a
maximum shelf life over which the gas
concentration does not change by greater
than ±5 percent from the certified value, (c)
The manufacturer affixes the date of gas
cylinder preparation, certified benzene
concentration, and recommended maximum
shelf life to the cylinder before shipment to
the buyer.
5.2.3.1 Cylinder Standards Certification.
The manufacturer shall certify the
concentration of benzene in nitrogen in each
cylinder by (a) directly analyzing each
cylinder and (b) calibrating his analytical
procedure on the day of cylinder analysis. To
calibrate his analytical procedure, the
manufacturer shall use. as a minimum, a
three-point calibration curve. It is
recommended that the manufacturer maintain
(l).a high-concentratio.i calibration standard
(between 50 and 100 ppm) to prepare his
calibration curve by an appropriate dilution
technique: and (2) a low-concentration
calibration standard (between 5 and 10 ppm)
to verify the dilution technique used. U' the
difference between the apparent
concentration read from the calibration curve
and the true concentration assigned to the
low-concentration standard exceeds 5
pcrctr.l of the true eonccntratior., ;he
manufacturer shall determine the source of
error and correct it, then repeat the three-
point calibration.
5.2.3.2 Verification of Manufacturer's
Calibration Standards. Before using, the
manufacturer shall verify each calibration
standard by (a) compiling it to gas mixtures
prepared (with 99 Mol percent benzene) in
accordance with the procedure described in
Section 7.1 or by (b) having it analyzed by the
National Bureau of Standards. The agreement
between the initially determined
concentration value and the verification
concentration value must be within ±5
percent. The manufacturer must reverify all
calibration standards on a time interval
consistent with the shelf life of the cylinder
standards sold.
5.2.4 Audit Cylinder Standards (2). Gas
mixture standards with concentrations
known only to the person supervising the
analysis of samples. The audit cylinder
standards shall be identically prepared as
those in Section 5.2.3 (benzene i:i nitrogen
cylinders). The concentrations of the audit
cylinder should be: one lov.'-cr;ncentration
cylinder in the rar.ge of-5 to £0 ppm benzene
and one hi.",h-concen:ratioa cylinder in the
range of 100 to DUO ppm benzene. When
available, the tester may obtain audit
cylinders by contacting: U.S. Eruironme.ital
Protection Agency, Environmental Monitoring
und Support Laboratory. Quality Assurance
Branch (MD -77). research Trian.qle Park.
North Carolina 27711. If audit cylinders are
not available at the Environmental Protection
Agency, the tester must secure un alternative
source.
6. Procedure
6.1 Sampling. Assemble the sample train
as shown in Figure 110-1. Perform a bag leak
check according to Section 7.3.2. Join the
quick connects as illustrated, and determine
that all connections between the bag and the
probe are tight. Place the end of the probe at
the centroid of the stack, and start the pump
with the needle valve adjusted to yield a flow
that will more than half fill the bag in the
specified sample period. After allowing
sufficient time to purge the line several times,
connect the vacuum line to the bag and
evacuate the bag until the rotametcr indicates
no flow. At all times, direct the gas exiting
the rotameter away from sampling personnel.
At the end of the snmple period, shut off the
pump, disconnect the sample line from the
bag. and disconnect the vacuum line from the
bag container. Protect the bag container from
sunlight.
6.2 Sample Storage. Keep the sample bags
out of direct sunlight. Perform the analysis
within 4 days of sample collection.
C.3 Sample Recovery. With a new piece of
Teflon tubing identified for that bag, connect
a bag inlet valve to the gas chromatograph
sample valve. Switch the valve to receive gas
from the bag through the sample loop.
ArrAnge the equipment so the sample gas
pnsscs from the sample valve to a 100-rr.L/
min rotameter wita flow cor.troi valve
followed by a charcoal tube and a 1-in.
pressure gauge. The tester may maintain the
sample flow either by a vacuum pump or
container pressurization if the collection bag
ruir.uir.s '.n the ri^id container. Afler sar.iple
loop purging is ceased, always allow the
pressure gauge to return lo zero before
activating the gas sampling valve.
6.4 Analysis. Set the column temperature
to 80° C (1761 F) for column A or 75" C (107°
F) for column B, and the detector temperature
to 225' C (-337° F). When optimum hydrogen
and oxygen flow rates have been determined,
verify and maintain these flow rates during
all chromatograph operations. Using zero
helium or nitrogen as the carrier gas,
establish a flow rate in the range consistent
.with the manufacturer's requirements for
satisfactory detector operation. A flow rate of
approximately 20 mL/min should produce
adequate separations. Observe the base line
periodically and determine lhat the noise
level has stabilized and that base-line drift
has ceased. Purge the sample loop for 30 s.ec
at the rate of 100 mL/min, then activate the
sample valve. Record the injection time (the
position of the pen on the chart at the time of
sample injection), the sample number, the
sample loop temperature, the column
temperature, carrier gas flow rate, chart
speed, and the attenuator setting. From the
chart, note the peak having the retention time
corresponding to benzene, as determined in
Section 7.2.1. Measure the benzene peak area.
Am, by use of a disc integrator, electronic
integrator, or a planimetcr. Record Am and
-------
Page G-5
Federal Register / Vol. 45. N'o. 77 / Friday. April 18, 1980 / Proposed Rules
SYRINGE
DRY GAS METER
TEDLAR BAG
CAPACITY
50 LITERS
Figure 110-2. Preparation of bsnzene standards (optional).
26681
BIUING CODE 6560-01-C
-------
Page G-6
Federal Register / Vol. 45. No. 77 / Friday. April 18, 1900 /'Proposed Rules
the rrlnnticn lir.ie. Rcpniil the injpr.tion at
least two times or us\'i\ two consecutive
values for thi; totnl area of (lie benzene peak
do not vary more than 5 percent. Use the
average value of Iiie.sc two total areas to
compute the bag cun.-.entration.
6.5 Determination of Bag Water Vapor
Content. Measure (he ambient temperature
and barometric pressure near the bag. From a '
water saturation vapor pressure table,
determine and record ihe water vapor
content of the bag as a decimal figure.
(Assume the relative humidity to be 100
percent unless a lesser value is known.)
7, Preparation of Standard Cos Mixtures.
Calibration, and Quality Assurance
7.1 Preparation of Benzene Standard Gas
Mixtures. (Optional procedure—delete if
cylinder standards are vised.) Assemble the
apparatus-shown in Figure 110-2. Evacuate a
50-L Tedlar or aluminizud Mylar bag that has
passed a leak checi; (described in Section
7.3.2) and meter in about 50 L of nitrogen.
Measure the barometric pressure, the relative
pressure at the dry «as meter, and the •
temperature at the dry gas meter. While the
bag is filling, use the lO.uL syringe to inject
lOfiL of 99+ percent benzene through the
septum on top of the impingcr. This gives a
concentration of approximately SO ppm of
benzene. In a like manner, use the other
syringe to prepare dilutions having
approximately 10 ppm and 5 ppm benzene
concentrations. To calculate the specific
concentrations, refer to Section 8.1. These gas
mixture standards may be used for 7 days
from She dale o!' preparation, after which time
preparation of ne-.v g;is mixtures is required.
(Caution: If the new i;us mixture standard is a*
lower concentration than the previous gas . . .
mixture standard, contamination may be a
problem when a bag is reused.)
7.2 Calibration.
7.2.7. Dttermination of Benzene Retention
Timp. (This section can be performed
simultaneously with Section 7.2.2.) Establish
chromato^raph conditions identical with
those in Section 6.4, above. Determine proper
attenuator position. Flush the sampling loop
with zero helium or nitrogen and activate the
sample valve. Record the injection time, the
sample loop temperature, the column
temperature, the carrier gas flow rate, the
chart speed, and the attenuator setting.
Record peaks and detector responses that
occur in the absence of benzene. Maintain
conditions, with the equipment plumbing
arranged identically to Section G.3. and flush
the sample loop for 30 sec at the rate of 100
mL/min with one of the benzene calibration.
mixtures. Then activate the sample valve.
Record the injection time. Select the peak
that corresponds to benzene. Measure the
distance on the chart from the injection time
to the time at which the peak maximum
occurs. This distance divided by the chart
speed is defined as the benzene peak
retention time. Since it is quite likely that
there will be other organics present in the
sample, it is very important that positive
identification of the benzene peak be made.
BILLINO CODE (SW-01-M
-------
26632
Page G-7 .
Federal Register / Vol. 45, No. 77 / Friii;;y. April 18. 1930 / Proposed Rules
Question.
• 7.2.2 Prrjpar.'itinn of Chromatocraph
Calibration C;:rvo. Mnkr. a pas
chromatopraphic nmasiircnont of each
standard gas n;i.\!ure (described in Sf:ction
5.2.3 or 7.1.1) usi.-.j: conditions identical with
those listed in Sections G.3 and 6.4. Flush the
sampling loop for 30 sec at the rate of ml./
min with one of the standard gas mixtures
and activate the sampe valve. Record Cc. the
concentration of benzine injected, the
attenuator se'.tui;:. chart speed, peak area, •
Siimpie loop temperature, column
temperature, carrier gas flow rate, and
retention lime. Record [he laboratory
pressure. Calculate Af, the peak area
multiplied by the attenuator setting. Repeat
until two consecutive injection areas are
within 5 percent, then plot the average of
those two values versus Cc. When the other
standard gas mixtures have been similarly
analyzed and plotted, draw a straight line
through the points derived by the least
squares method. Perform calibration daily, or
before and
-------
i-\:dr;r;il Register / Vol. 45, No, 77 / Fridiv. A">ri! 18. In30 / Proposed Rule1?
26683
Th?
1
2
3.
4.
S.
7.
3.
9.
^.C:-K
<* « J b-2, '
dt =
dx
following calculation steps are required:*
2c.
tc/2;2 In 2
.j.f
V25 J
» x_
e " Z dx
6. Q(x2) .
- Q(x2)
Percentage overlap = AQ x 100
A = Ths area of the sample peak of interest determined by elec-
tronic integration, or by the formula A = "c^c-
- The area of the contaminant peak, determined in the same
«iar,~er as A .
a
b = The distance on the chromHographic chart that separates the
isaxima of the two peaks.
H = The oeak height of the sample compound of interest. neasurPd
fro;! thff average value of the oase!in* to the maximum of the
curve.
t_ - The width of the sample peak of interest at 1/2 of peak
height.
l - The wi'jth of the contaminant peak at 1/2 of peak height.
(i = The standard deviation of the sample compound of interest
elution curve.
u = The standard deviation of tne contaminant eluticn curve.
Q(< ) = fho inteyra! of the normal distribution function from x^ to
infinity.
Q!*.>) = Tne integral of the normal distribution function fron x. to
infini ty.
The overlap integral.
The area overlap fraction.
1r. judging thn sui!;ibi!i!y of a!ti:rr.a'h:c ci'mditions. one can
•'Riploy the area overlap as the resolution
pnr.-imotrr with a specific maximum
•permissible value.
The use of Gaussian functions to describe
khi'uiii.itoijriiphic elution curves is
widespread. However, some elution curves
are hiphly Hsymmelric. In those cases where
thf! sample p«ak is followed by a
contaiminant that has a lisi'dini; ed^n that
risus sharply but the curve then tails off. it
may be possible to define an effective width
for tj as "twice the distance from the leading
edge to a perpendicular lino through the
rnaxim of the contaminant curve, measured
along a perpendicular bisection of that line."
Supplement B—Procedure for Field Auditing
CC Analysis
Responsibilities of audit supervisor and
analyst at the source sampling site include
the follow-in":
A. Check that audit cylinders are stored in
a safe location both before and after the audit
to prevent vandalism of same.
B. At the beginning and conclusion of the
audit, record each cylinder number and
cylinder pressure. Never analyze an audit
cylinder when the pressure drops below 200
psi.
C. During the audit, ths amlyst is to
perform a minimum of two consecutive
analyses of each audit cylinder gas. The audit
must bo conducted to coincide with the
analysis of so;ir;:o tost sarnuies. Normally, it
will he conducted irririicdin:::!y ufter the CC
calibration and prior to tha i^mplii analyses.
D. At the end of.auriit analyses, tho audit
supervisor requests the calculated
concentrations from ihc analvst and then
compares the rosuits with the actual audit
concentrations. If nach :nons:ired
concentration agrees with the respective
act'.nl concentration within ±10 perront, he
thon dirccis the analyst to begin the analysis
*of source samples. Audit sut.-pm'sor ji:d2ment
and/or supervisory policy dutermine course
of action with agreement is not within ±10
percent. VVhnre a consis'^nt bias in excass of
10 percent is found, it rruy be possible to
proceed with Ihe sample analyses, with a
corrective factor to be applied to the results
at u later tinip. However, every attempt
should be made to locate the causi; of" this
discrepancy, as it may be misleading. The
audit supervisor is to record er?ch cylinder
number, cylindor pressure (at the end of the
nuilit). and all calculated concuntrations. The
individual buin;; audiiRd niiist not unu'erany
circumstance be tald the actual audit
concentrations until the calculated
concentrations have been submitted to the
audit supervisor.
BILLING CODE 6560-01-M
ri;;t instances, Q(<;) is very small and may be neglected.
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