v>EPA
United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
EMB Report 83-WWS-2
March 1984
Air
Petroleum Refineries
Waste Water
Treatment System
Emission Test
Report
Chevron USA, Inc.
El Segundo Refinery
El Segundo,
California
-------
Contract No. 68-02-3545
Work Assignment 14
EMB Report No. 83 WWS 2
EPA Task Manager
W. E. Kelly
EMISSION TEST REPORT
PETROLEUM REFINERY WASTEWATER TREATMENT SYSTEM
CHEVRON U.S.A., INCORPORATED
EL SEGUNDO, CALIFORNIA
Contractor
TRW Environmental Operations
Post Office Box 13000
Research Triangle Park, North Carolina 27709
TRW Project Manager
J. B. Homolya
Prepared By
C. Stackhouse and M. Hartman
Prepared For
Emission Measurement Branch
Emission Standards and Engineering Division
U.S. Environmental Protection Agency
Research Triangle Park, North Carolina 27711
March 1984
-------
TABLE OF CONTENTS
Section Page
1 INTRODUCTION 1-1
2 SUMMARY AND DISCUSSION OF RESULTS 2-1
2.1 Effluent Treatment Plant Test Results 2-1
2.2 Unsegregated Water System, IAF Unit 2-31
2.3 Process Water Analyses 2-39
3 PROCESS DESCRIPTION 3-1
3.1 Refinery Wastewater System 3-1
3.2 Segregated System 3-1
3.3 Unsegregated System 3-7
3.4 Wastewater Monitoring System 3-9
3.5 Odor Control System 3-10
4 LOCATION OF SAMPLE POINTS 4-1
5 SAMPLING AND ANALYTICAL PROCEDURES 5-1
5.1 Gaseous VOC Methods 5-1
5.2 Permanent Gas Analysis 5-16
5.3 Gaseous Volumetric Flow Measurement 5-18
5.4 Liquid Sample Methods 5-22
5.5 Liquid Sample Analysis Methods 5-22
n
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LIST OF FIGURES
Figure Page
3-1 General scheme of wastewater flow: Chevron
Refinery - El Segundo, California 3-3
3-2 IAF system similar to that used at the Chevron
Refinery - El Segundo, California 3-8
3-3 Odor control system for DAF system 3-12
4-1 Dissolved air flotation treatment system at Chevron
Refinery - El Segundo, California 4-2
4-2 DAF outlet sample location with traverse points 4-3
4-3 Equalization tank system at Chevron Refinery -
El Segundo, California 4-4
4-4 Equalization tank outlet sample location
with traverse points 4-5
4-5 IAF treatment system at Chevron Refinery -
El Segundo, California 4-6
5-1 Gas bag sampling system 5-2
5-2 Example of GC/FID calibration for C1-C5 speciation . . . 5-4
5-3 Example of GC/FID analysis on DAF ventilation air -
gas bag sample for Cj-Cs speciation 5-5
5-4 Example of GC/FID analysis on IAF ventilation air -
gas bag sample for Cj-Cs speciation 5-6
5-5 Example of GC/FID analysis on equalization tank -
gas bag #2 sample for C1-C5 speciation 5-7
5-6 Example of GC/FID calibration for C6-C9 speciation . . . 5-9
(continued)
m
-------
LIST OF FIGURES (Concluded)
Figure Page
5-7 Example of GC/FID analysis on DAF ventilation air -
gas bag sample for C6-C9 speciation 5-10
5-8 Example of GC/FID analysis on IAF ventilation air -
gas bag sample for C6-C9 speciation 5-11
5-9 Example of GC/FID analysis on equalization tank #2
gas bag sample for C6-C9 speciation 5-12
5-10 Example of a calibration check with a
recalibration required 5-17
5-11 Example of GC/TCD calibration for stationary
gas analysis 5-19
5-12 Example of GC/TCD analysis on equalization tank #2
gas bag sample for stationary gases 5-20
5-13 Velocity measurement system adapted into IAF
ventilation air, Chevron - El Segundo, California .... 5-21
5-14 Mass spectrometer qualitative analysis by purge
and trap, sample no. DAF-IN-#1-VOA 5-28
5-15 Mass spectrometer qualitative analysis by purge
and trap, sample no. DAF-OUT-#1-VOA 5-29
5-16 GC/FID quantitative analysis by purge and trap,
sample no. DAF-IN-#1-VOA 5-30
5-17 GC/FID quantitative analysis by purge and trap,
sample no. DAF-OUT-#1-VOA 5-31
-------
LIST OF TABLES
Table Page
2-1 Sampling Log of Continuous Hydrocarbon Monitoring:
Sampling Locations at the Chevron Refinery -
El Segundo, California 2-2
2-2 Daily Time Table of Sampling Activities at the
Chevron Refinery - El Segundo, California 2-3
2-3 Summary of Daily Emission Rate Averages: Continuous
Monitoring Results - Effluent Treatment Plant,
Chevron - El Segundo, California 2-7
2-4 Continuous Emission Results: Hydrocarbon Monitoring
at the DAF Ventilation Air Sample Location, Chevron -
El Segundo, California - Test Day 8/3/83 2-8
2-5 Continuous Emission Results: Hydrocarbon Monitoring
at the DAF Ventilation Air Sample Location, Chevron -
El Segundo, California - Test Day 8/4/83 2-9
2-6 Continuous Emission Results: Hydrocarbon Monitoring
at the DAF Ventilation Air Sample Location, Chevron -
El Segundo, California - Test Day 8/5/83 2-10
2-7 Continuous Emission Results: Hydrocarbon Monitoring
at the DAF Ventilation Air Sample Location, Chevron -
El Segundo, California - Test Day 8/8/83 2-11
2-8 Continuous Emission Results: Hydrocarbon Monitoring
at the DAF Outlet Sample Location, Chevron -
El Segundo, California - Test Day 8/9/83 2-12
2-9 Continuous Emission Results: Hydrocarbon Monitoring
at the DAF Ventilation Air and DAF Carbon House
Outlet Sample Locations, Chevron - El Segundo,
California - Test Day 8/10/83 2-13
2-10 Continuous Emission Results: Hydrocarbon Monitoring
at the DAF Ventilation Air Sample Location, Chevron -
El Segundo, California - Test Day 8/11/83 2-14
(continued)
-------
LIST OF TABLES (Continued)
Table Page
2-11 Summary of Pitot Measurements to Determine the
DAF Ventilation Air Flow Rate, Chevron -
El Segundo, California 2-16
2-12 Gas Chromatography Results from the DAF -
Test Days 8/3/83 to 8/5/83, Chevron Refinery -
El Segundo, California 2-17
2-13 Gas Chromatography-Results from the DAF -
Test Days 8/8/83 to 8/11/83, Chevron Refinery -
El Segundo, California 2-18
2-14 Gas Chromatograph Results from the DAF Carbon House Vent
(V-204), Chevron Refinery - El Segundo, California . . . 2-20
2-15 Monitored Emission Results: Hydrocarbon Monitoring at
the Flocculation Tank (T-201) and the Flash/Mix Tank
(T-200), Chevron - El Segundo, California 2-21
2-16 Gas Chromatograph Results from the Flocculation Tank
(T-201) and the Flash/Mix Tank (T-200), Chevron
Refinery - El Segundo, California 2-22
2-17 Continuous Emission Results: Hydrocarbon Monitoring
at the Equalization Tank Ventilation Air Location,
Chevron - El Segundo, California - Test Day 8/3/83 . . . 2-24
2-18 Continuous Emission Results: Hydrocarbon Monitoring
at the Equalization Tank Ventilation Air Location,
Chevron - El Segundo, California - Test Day 8/4/83 . . . 2-25
2-19 Continuous Emission Results: Hydrocarbon Monitoring
at the Equalization Tank and Equalization Tank Carbon
House Outlet Locations, Chevron - El Segundo,
California - Test Day 8/5/83 2-26
2-20 Summary of Pitot Measurements: Flow Monitoring
at the Equalization Tank Outlet, Chevron -
El Segundo, California 2-27
2-21 Gas Chromatograph Results from the Equalization
Tank - Test Days 8/3/83 to 8/5/83, Chevron Refinery -
El Segundo, California 2-28
2-22 Monitored Emission Results: Hydrocarbon Monitoring at
the Equalization Tanks Ventilation Air and Carbon
House Exhaust, Chevron - El Segundo, California 2-29
(continued)
vi
-------
LIST OF TABLES (Continued)
Table Page
2-23 Gas Chromatograph Results at the Equalization
Tank - Test Day 8/12/83, Chevron Refinery -
El Segundo, California 2-30
2-24 Continuous Emission Results: Hydrocarbon Monitoring
at the IAF Ventilation Air Sample Location,
Chevron - El Segundo, California - Test Day 8/8/83 . . . 2-32
2-25 Continuous Emission Results: Hydrocarbon Monitoring
at the IAF Ventilation Air Sample Location,
Chevron - El Segundo, California - Test Day 8/9/83 . . . 2-33
2-26 Continuous Emission Results: Hydrocarbon Monitoring
at the IAF Outlet Sample Location, Chevron -
El Segundo, California - Test Day 8/10/83 2-34
2-27 Continuous Emission Results: Hydrocarbon Monitoring
at the IAF Outlet Sample Location, Chevron -
El Segundo, California - Test Day 8/11/83 2-35
2-28 Continuous Emission Results: Hydrocarbon Monitoring at
the IAF Outlet and IAF Carbon Drum Sample Location,
Chevron - El Segundo, California - Test Day 8/12/83 . . . 2-36
2-29 IAF Flow Measurements: Chevron -
El Segundo, California 2-37
2-30 Gas Chromatography Results from the IAF -
Test Days 8/11/83 to 8/12/83, Chevron Refinery -
El Segundo, California 2-38
2-31 Chevron, El Segundo, California Samples Taken on 8/3/83 . 2-40
2-32 Chevron, El Segundo, California Samples Taken on 8/4/83 . 2-42
2-33 Chevron, El Segundo, California Samples Taken on 8/5/83 . 2-43
2-34 Chevron, El Segundo, California Samples Taken on 8/8/83 . 2-44
2-35 Chevron, El Segundo, California Samples Taken on 8/9/83 . 2-47
2-36 Chevron, El Segundo, California Samples Taken
on 8/10/83 2-48
2-37 Chevron, El Segundo, California Samples Taken
on 8/11/83 2-49
(continued)
vii
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LIST OF TABLES (Concluded)
Table Page
2-38 Chevron, El Segundo, California Samples Taken
on 8/12/83 2-53
2-39 Ct to C7 Speciation by GC/FID Purge and Trap,
Chevron, El Segundo, California 2-54
3-1 Crude Throughput During Test Period 3-2
5-1 Continuous Monitor Calibration Gases 5-15
5-2 Replicated COD and 0 & G Measurements 5-25
5-3 GC/FID Readings for Accuracy/Precision Estimates .... 5-33
5-4 Precision/Accuracy Estimates for IAF/DAF Samples .... 5-34
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1. INTRODUCTION
Under Section 111 of the Clean Air Act, the Environmental Protection
Agency is required to develop standards of performance for stationary
sources that have been determined to contribute significantly to air
pollution. EPA is conducting a study to develop standards that would
limit volatile organic compound emissions from new waste water treatment
systems in petroleum refineries. Under contract to the Emission
Measurement Branch, EPA, TRW Environmental Operations personnel conducted
a testing program at the segregated and unsegregated water treatment
systems at the Chevron USA, El Segundo Refinery in El Segundo, CA during
August 1 to August 12, 1983.
The purpose of this test program was to provide estimates of the
organic compound release rates from dissolved air flotation units (DAF)
and induced air flotation unit (IAF). These release rates are necessary
to estimate uncontrolled emission rates from uncovered flotation devices
for potential emission reduction and cost effectiveness calculations.
The air flotation devices at Chevron's waste water treatment
facilities are equipped with covers. Ventilation air is mechanically
drawn or pumped through the covered spaces and is treated for odor
control prior to release to the atmosphere. The ventilation air prior
to the control devices was measured to estimate the organic release rate
that would have occurred if the flotation devices were uncovered. This
approach was used to estimate uncovered unit emission because of the
difficulty in measuring a dispersed-source fugitive emission. It is
assumed that the dominant factors affecting organic emission rates are
the water characteristics and the physical turbulence caused by bubbling
air through the water, and that meterological factors such as air
temperature and wind speed are secondary parameters.
-------
Tests were conducted to determine the mass flow rate and the organic
species composition of the ventilation air from the DAF and the
equalization basin in the segregated system effluent treatment plant,
and the IAF servicing the unsegregated water treatment system. Limited
screening tests were conducted after the activated carbon control devices
servicing these units to estimate the hydrocarbon removal. During the
air measurements, samples of the waste water were collected from various
points in the treatment system to characterize the liquid streams.
These samples were analyzed for chemical oxygen demand (COD), total
organic carbon (TOC), total chromatographical organics (TCO), and oil
and grease content using standard methods for water analysis.
The results of these tests are presented in Section 2. A description
of the process and the operation during the test period is given in
Section 3. The sampling locations and the sampling and analytical
procedures are discussed in Sections 4 and 5 respectively. The appendices
to this report contain example calculations, field data, test logs and a
list of project participants.
1-2
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2. SUMMARY AND DISCUSSION OF RESULTS
This section details the results of the testing and analysis at the
El Segundo Refinery waste water treatment units. The overall refinery
waste water treatment system is illustrated in Figure 3-1 and the sampling
locations are indicated in Figures 4-1, 4-3, and 4-5. Table 2-1 presents
a summary of the periods during which continuous hydrocarbon monitoring
was performed at the indicated sample locations. Table 2-2 presents a
summary of the periods during which integrated gas samples were collected,
velocity or flow rate measurements were conducted and when liquid samples
were collected from each location. The results are discussed separately
for the Effluent Treatment Plant (DAF and equalization tank), the
unsegregated water system (IAF) and the combined results of water analyses.
2.1 EFFLUENT TREATMENT PLANT TEST RESULTS
The results of testing at the dissolved air flotation (DAF) system
and the equalization tank are discussed separately in this section.
2.1.1 DAF System
A summary of the daily average total hydrocarbon mass flow rates in
the DAF ventilation air and the equalization ventilation air prior to
the emission control devices is presented in Table 2-3. The total
hydrocarbon measurement does not exclude methane. The hydrocarbon mass
flow in the DAF ventilation air ranged from 6.17 Ibs/hr to 9.01 Ibs/hr
(24-hour average basis) over the seven days of testing. The average
mass flow was 7.21 Ibs/hr (24-hour basis). The test results on a one-hour
average basis for each day of testing are presented in Tables 2-4 to 2-10.
The average total hydrocarbon concentration based on equivalents of
propane is presented for each one-hour period. Propane was chosen as
the calibration species because it is a stable compound and calibration
mixtures are easily acquired and stored. For the organic species expected
at refineries, the response of the analysis is directly proportional to
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Table 2-1. SAMPLING LOG OF CONTINUOUS HYDROCARBON MONITORING:
SAMPLING LOCATIONS AT THE CHEVRON REFINERY - EL SEGUNDO, CALIFORNIA
Date
8/3/83
8/4/83
8/5/83
8/5/83
£ 8/6/83
8/7/83
8/8/83
8/9/83
8/10/83
8/11/83
8/12/83
Sample
location
Ventilation
air
Ventilation
air
Ventilation
air
NO -
NO -
Ventilation
air
Ventilation
air
Ventilation
air
Exhaust
Ventilation
air
Ventilation
air
DAF tank
Sample location area
Equalization tank
No. No.
Time hours sample Time hours sample
sampled sampled location sampled sampled location
0800-2400
0000-2400
0000-1100
«._•»•-
1100-2400
0000-2400
0000-1100
1300-1600
1700-2400
0000-1400
16 Ventilation 1100-2400 13
air
24 Ventilation 0000-2400 24
air
16 Ventilation 0000-1300 13
air
Exhaust 1400-1700 3
TESTS ON
TESTS ON
13 Ventilation
air
24 Ventilation
air
11 Ventilation
air
3
7
14 Ventilation
air
Exhaust
Exhaust
IAF tank
No.
Time hours
sampled sampled
—
—
—
—
WEEKEND
WEEKEND
1700-2400 7
0000-2400 24
0000-2400 24
0000-1400 14
0900-1200 3
1200-1500 3
Exhaust = tank carbon house outlet vent.
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Table 2-2. DAILY TIME TABLE OF SAMPLING ACTIVITIES AT THE CHEVRON REFINERY - EL SEGUNDO, CALIFORNIA
loc«t
-------
Table 2-2. Continued
0»/D»t«
NT VwttUtfM A1r I/I
O
O
1000 1100 IMP 1300 1400 1SOO ICOO 1100
(0001-1600)
ro
•4 ftwtlUtlM Air I/I
O
O
tyi
(0001.1300)
O
a
Air l/t
(1100-2400)
O
Ui VMtlUtlM Mr I/I
(1700-MOO)
A
O
O
O
e
(MM* IMM •*)
-Wt)
-------
Table 2-2. Continued
OAF VmtlUtlM Atr a/9
1000
O
O
1100
1200
1300
1400
1500
•* (0001-2400)
1600
1700
o
0
FloccuUtlM TM*
VMlt
a/9
ro
tn
FlMk W« TMk taut a/9
O
DAT VMttUttm Air a/10
O
-A
(1700-2400)
O
O
OAFCiriMM HBUM
Exhaust
8/10
(1900-1600)
ft A
A
O
O
O
0
(MUM IMM fell
(ibttotf MkUtara)
(IMAM tU-TW)
-------
Table 2-2. Concluded
lec«t1on/D«U
IM VmtlUtlon Air 8/10
0900 1000
1100 1200 1300 1400
(0001.2400)
1500 1600
1700
IMF VmtiUtlM Air 8/11
O
O
— (0001-1400) • •
O o
MF VmtlUtlo* Air 8/11
(0001-1400)
ro
en
IAF Mutilation Air 8/12
0
O
O
-A
a a
a
(1200-1500)
EQ VmtlUttM Air 8/12
(MUM IMM IN)
EQ Carbon House 8/12
Exhaust
A
O
O
O
0
Wk)
«4hl
(MtMIM-TIC)
-------
Table 2-3. SUMMARY OF DAILY EMISSION RATE AVERAGES: CONTINUOUS MONITORING RESULTS
EFFLUENT TREATMENT PLANT, CHEVRON - EL SEGUNDO, CALIFORNIA
Sample location
Test day
8/3/83 8/4/83 8/5/83 8/8/83 8/9/83 8/10/83 8/11/83 8/12/83 Average
ro
DAF carbon house
outlet (Ibs/hr)
Equalization tank
ventilation air
(Ibs/hr)
Equalization tank carbon
house outlet (Ibs/hr)
4.18
4.65
Total hydrocarbon mass flow rate. Ibs/hr
4.24
— 4.62L
7.54c>d'e 4.36
0.77c'd -
a2 hour average basis.
2 hour average basis.
0.5 hour average basis.
Integrated samples collected for total hydrcarbon and species analysis.
p
Not included in average.
-------
Table 2-4. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT THE
DAF VENTILATION AIR SAMPLE LOCATION, CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/3/83
Time
0900C
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
Average
Concentration3
(ppm as C3H8)
533
470 .
508
513
523
546
506
507
491
482
479
476
475
518
958
786
Flowb
(SCFM)
2044
2044
2044
2044
2044
2044
2044
2044
2044
2044
2044
2044
2044
2044
2044
2044
Emission Rate
(Ibs/hr as C3H8)
6.98
6.15
6.65
6.72
6.85
7.15
6.62
6.64
6.43
6.31
6.27
6.23
6.22
6.78
12.54
10.29
7.18
Concentration is average value for continuous readings across the hour
(0-55 minutes) based on 5-minute readings.
No pitot measurement on initial test day (8/3/83), therefore used average
flow measurement during first week of test (8/3/83-8/5/83). See
Table 2-11.
Continuous Hydrocarbon Analyser (Beckman 400) on-line at DAF Outlet Sample
Location starting the test period.
2-8
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Table 2-5. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT THE
DAF VENTILATION AIR SAMPLE LOCATION, CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/4/83
Time
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
Average
Concentration3
(ppm as C3H8)
655
600
596
590
587
576
585
599
606
731
609
508
379
341
336
354
354
344
350
363
377
374
382
667
Flowb
(SCFM)
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
2007
Emission Rate
(Ibs/hr as C3H8)
8.42
7.72
7.67
7.95
7.55
7.41
7.52
7.70
7.79
9.39
7.83
6.53
4.87
4.38
4.32
4.55
4.55
4.42
4.50
4.66
4.84
4.81
4.91
8.57
6.37
Concentration is average value for continuous readings across the hour
(0-55 minutes) based on 5-minute readings.
Pitot measurements at initial and final periods of test day, therefore
used average of flows measurements. See Table 2-11.
2-9
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Table 2-6. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT THE
DAF VENTILATION AIR SAMPLE LOCATION, CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/5/83
Time
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300
1400
1500
1600C
Average
Concentration3
(ppm as C3H8)
552
504
477
459
450
437
613
597
583
573
551
512
495
482
482
456
Flowb
(SCFM)
2081
2081
2081
2081
2081
2081
2081
2081
2081
2081
2081
2081
2081
2081
2081
2081
Emission Rate
(Ibs/hr as C3H8)
7.36
6.72
6.36
6.11
6.00
5.82
8.17
7.96
7.77
7.64
7.34
6.82
6.60
6.42
6.42
6.08
6.85
Concentration is average value for continuous readings across the hour
(0-55 minutes) based on 5-minute readings.
Pitot measurements at initial and final periods of test day, therefore
used average of flows measurements. See Table 2-11.
cTest period discontinued for weekend period with instruments off-line
and flamed out.
2-10
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Table 2-7. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT THE
DAF VENTILATION AIR SAMPLE LOCATION, CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/8/83
Time
1100C
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
Average
Concentration3
(ppm as C3H8)
521
475
489
466
580
551
492
521
413
470
496
509
494
480
Flowb
(SCFM)
2119
2119
2119
2119
2119
2119
2119
2119
2119
2119
2119
2119
2119
2119
Emission Rate
(Ibs/hr as C3H8)
7.07
6.45
6.64
6.33
7.87
7.48
6.68
7.07
5.61
6.38
6.73
6.91
6.71
6.52
6.75
Concentration is average value for continuous readings across the hour
(0-55 minutes) based on 5-minute readings.
One pitot measurement during test day period, therefore used across test
day. See Table 2-11.
Continuous Hydrocarbon Analyzer (Beckman 400) on-line at DAF Outlet Sample
Location resuming the test period from 8/5/83.
2-11
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Table 2-8. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT
THE DAF OUTLET SAMPLE LOCATION - CHEVRON, EL SEGUNDO, CALIFORNIA
TEST DAY 8/9/83
Time
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
Average
Concentration3
(ppm as C3H8)
466
507
669
709
595
657
676
724
712
705
690
644
610
592
701
c
645
627
575
568
541
540
551
515
Flowb
(SCFM)
2133
2133
2133
2133
2133
2133
2133
2133
2133
2133
2133
2133
2133
2133
2133
—
2133
2133
2133
2133
2133
2133
2133
2133
Emission Rate
(Ibs/hr as C3H8)
6.37
6.93
9.14
9.69
8.13
8.98
9.24
9.89
9.73
9.63
9.43
8.80
8.33
8.09
9.58
—
8.81
8.57
7.86
7.76
7.39
7.38
7.53
7.04
8.11
Concentration is average value for continuous readings across the hour
(0-55 minutes) based on 5-minute readings.
One flow measurement taken during test period, therefore used flow
measurement across test day. See Table 2-11.
cHydrocarbon Monitor (Beckman 400) off-line for repairs.
2-12
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Table 2-9. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT
THE DAF VENTILATION AIR AND DAF CARBON HOUSE OUTLET SAMPLE LOCATIONS
CHEVRON, EL SEGUNDO, CALIFORNIA - TEST DAY 8/10/83
Time
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300d
1400d
! 1500d
I
1600
1700
1800
1900
2000
2100
2200
2300
2400
Average
Concentration3
(ppm as C3H8)
495
488
470
464
449
481
478
464
460
449
502
c
95
168
131
c
396
401
453
485
541
556
572
564
Flowb
(SCFM)
1998
1998
1998
1998
1998
1998
1998
1998
1998
1998
1998
—
1998
1998
1998
—
1998
1998
1998
1998
1998
1998
1998
1998
DAF Outlet
DAF Carbon
Emission Rate
(Ibs/hr as C3H8)
6.34
6.25
6.01
5.95
5.74
6.16
6.11
5.94
5.89
5.74
6.43
—
)
1.21 1
2.15 !
1.68 !
._ __j
5.06
5.13
5.80
6.21
6.92
7.11
7.32
7.22
6.17
House 1.68
Concentration is average value for continuous readings across the hour
(0-55 minutes) based on 5-minute readings.
One flow measurement taken during test period; therefore, used flow
measurement across test day. See Table 2-11.
cHydrocarbon Monitor (Beckman 400) off-line for switching sample locations.
Monitoring DAF carbon house outlet sample location.
2-13
-------
Table 2-10. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT THE
DAF VENTILATION AIR SAMPLE LOCATION, CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/11/83
Time
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300
1400C
Average
Concentration3
(ppm as C3H8)
575
581
604
623
608
556
658
623
508
395
564
764
687
558
Flowb
(SCFM)
2371
2371
2371
2371
2371
2371
2371
2371
2371
2371
2371
2371
2371
2371
Emission Rate
(Ibs/hr as C3H8)
8.73
8.82
9.18
9.46
9.23
8.44
9.99
9.46
7.72
6.00
8.57
11.60
10.43
8.47
9.01
Concentration is average value for continuous readings across the hour
(0-55 minutes) based on 5-minute readings.
One flow measurement taken during test period, therefore used flow
measurement across test day. See Table 2-11.
End of test period at DAF outlet.
2-14
-------
the carbon content. While the concentration results are on a propane
basis and are not equal to the true hydrocarbon concentration, the
calculated mass flow rates are equivalent to true hydrocarbon mass flow
rates. The average gaseous flow rate result that was used for calculation
of the mass flow is also given for each day of monitoring. A single
value is used for each day because the ventilation blowers operated at
constant speed and no changes were made to the ventilation configuration.
On three days of testing (8/4, 8/5, 8/10), two flow determinations were
performed each day to estimate the variation in the flow. These results
are presented in Table 2-11. The difference between the two measure-
ments ranged from 0 to 23.1 percent, with an average of 8.1 percent,
which is typical of variations in pitot tube measurements.
The daily one-hour summaries show that short-term increases in mass
flow rates occurred. Such increases occurred during 1400 hr 8/3, 2300 8/3
to 0100 8/4, 1000 8/4, 2400 8/4 to 0100 8/5, 0700 8/5, etc. These
increases are directly correlated to those periods when the DAF tank was
skimmed during each shift. After skimming was completed the measured
concentration returned to a relatively constant level.
The results of the analysis of integrated gas samples of the DAF
ventilation air are presented in Tables 2-12 and 2-13. The species
analyses were obtained using two field gas chromatographic systems and
were intended to generally identify the major components and their
approximate concentrations. Calibrations standards were available for
Cl to C5, benzene and m-xylene, so the results for these compounds can
be calculated directly. Hexane, heptane, and p-xylene are calculated as
equivalents of the nearest carbon number calibration species. Other
peaks were also grouped with the closest eluting calibration species for
computation. Since a benzene standard was used to establish a specific
retention time for that compound, it can be concluded that the peak
occurring at that time was benzene. However, these are some compounds
found at refineries that tend to elute near benzene (such as methyl-
cyclopentane and cyclohexane) and would be indistinguishable with this
analytical systems. However, since clear identification of toluene and
xylene were present, it is probable that at least part of the
concentrations attributed to benzene was actually benzene.
2-15
-------
Table 2-11. SUMMARY OF PITOT MEASUREMENTS TO DETERMINE THE DAF VENTILATION AIR FLOW RATE
CHEVRON - EL SEGUNDO, CALIFORNIA
IV3
I
CT»
Test day 8/3/83
8/4/83 8/5/83 8/8/83 8/9/83 8/10/83
8/11/83
Volumetric flow rate, SCFM
Morning NM
measurement
Afternoon NM
measurement
Average on/i/ia
(SCFM) 2044
% difference
between a.m.
and p.m.
2008 2095 2119 2133 1791
2006 2068 NM NM 2205
2007 2081 2119 2133 1998
0 1.3 23.1
2371
NM
2371
NM - Not measured.
a
Average of measured flow rates during test days 8/3/83 to 8/5/83.
-------
Table 2-12. GAS CHROMATOGRAPHY RESULTS FROM THE DAF
TEST DAYS 8/3/83 to 8/5/83
CHEVRON REFINERY, EL SEGUNDO, CALIFORNIA
DATE
TIME
RUN NO.
ANALYTICAL RESULTS
(ppmv as compound)
C-l
C-2
C-3
C-4
C-5
Hexane
Benzene
Heptane
Toluene
m-Xylene
o-Xylene
TOTAL HYDROCARBON3
(ppmv as compound)
CONTINUOUS MONITOR
DATA
Hydrocarbon Level
(ppmv as C3H8)
Emission Rate
(Ib/hr)
PROCESS CONDITIONS
% N2
% 02
8/3
1135-
1235
2
46.8
5.7
6.8
3.8
1.9
10.1
11.0
10.0
39.2
6.8
3.4
145
510
6.69
74.80
21.20
8/3
1445-
1545
3
46.5
7.0
8.1
5.0
3.4
16.9
15.1
11.8
45.3
6.1
3.0
168
526
6.88
74.80
20.7
8/4
930-
1010
1
53.6
6.4
8.3
4.9
4.9
23.0
19.8
21.3
55.5
15.9
7.9
217
668
8.59
75.00
21.30
8/4
1430-
1515
2
45.5
5.3
6.2
4.4
3.8
15.1
13.2
6.6
32.4
7.7
3.0
143
339
4.35
73.13
19.93
8/5
900-
945
1
53.8
6.7
7.1
4.2
4.6
10.7
24.4
2.6
46.7
13.6
5.0
179
583
7.82
78.00
20.15
8/5
1500-
1530
2
58.3
6.5
8.3
0.6
18.0
35.0
44.4
10.4
3.8
185
482
6.38
75.95
19.65
aTotal includes unidentified hydrocarbon responsive to GC/FID.
2-17
-------
Table 2-13. GAS CHROMATOGRAPHY RESULTS FROM THE DAF
TEST DAYS 8/8/83 to 8/11/83
CHEVRON REFINERY - EL SEGUNDO, CALIFORNIA
DATE
TIME
RUN NO.
ANALYTICAL RESULTS
(ppmv as compound)
C-l
C-2
C-3
C-4
C-5
Hexane
Benzene
Heptane
Toluene
m-Xylene
o-Xylene
TOTAL HYDROCARBON3
(ppmv as compound)
CONTINUOUS MONITOR
DATA
Hydrocarbon Level
(ppmv as C3H8)
Emission Rate
(Ib/hr)
PROCESS CONDITIONS
% N2
% 02
8/8
1100-
1300
1
55.3
4.5
5.6
4.0
3.4
16.1
39.8
46.4
11.3
3.9
190
495
6.72
77.15
19.75
8/8
1500-
1530
2
52.9
3.9
5.0
4.8
4.0
26.2
63.6
75.1
20.7
8.2
264
580
7.87
76.15
19.55
8/9
915-
1040
1
37.5
2.4
2.2
3.6
4.8
12.8
49.2
28.3
17.1
6.0
22.4
186
709
9.68
76.62
19.81
8/9
1400-
1455
2
34.8
1.8
2.6
3.2
4.8
0
8.0
44.4
17.4
7.0
24.2
148
592
8.09
75.49
19.55
8/10
904-
1004
1
26.4
2.1
2.0
1.7
0
6.7
23.7
7.0
0
12.7
5.2
87
460
5.28
77.45
19.92
8/11
1315-
1415
1
29.2
0
2.1
6.5
9.2
19.1
55.2
0
61.5
10.0
10.2
203
622
8.22
77.36
19.64
aTotal includes unidentified hydrocarbon responsive to GC/FID.
2-18
-------
Additional descriptions of the chromatographic techniques are given in
Section 5.
The general results of the species analysis are relatively consistent
and the major components are methane and C6 to C8 components. The
results of these analyses can be used to calculate a non-methane
hydrocarbon emission rate, but these calculations were not performed for
this report.
On 8/10/83, a short term test was conducted to estimate the hydro-
carbon concentration at the DAF carbon house exhaust. For a two hour
period, the average emission rate was 1.68 Ibs/hr, while the daily
average mass rate to the carbon house was 6.17 Ibs/hr. The hydrocarbon
removal efficiency for this short term test is 72.8 percent. This
result should not be necessarily used to represent typical hydrocarbon
control efficiencies of carbon absorption units because the system at
Chevron was installed for odor control and not for maximum hydrocarbons
emission reduction. A species analysis was also performed at this
location on 8/10 and the results are presented in Table 2-14.
Since the ventilation air system at the DAF served three process
tanks, measurements were performed at the individual vent tank lines to
estimate the relative contribution to the total hydrocarbon mass flow.
The sample locations are described in Section 4. The tests consisted of
a measurement with a pitot tube to estimate volumetric flow rate and the
collection of an integrated gas sample for total hydrocarbon concentration
measurement. The results of this flow distribution measurements are
presented in Table 2-15. The relative hydrocarbon mass flow from the
Flocculation Tank and the Flash Mix Tank were 3.1 and 0.3 percent,
respectively; therefore, 96.6 percent of the hydrocarbons measured in
the ventilation air were from the DAF Tank. The samples collected for
total hydrocarbon analyses were also analyzed for component identification.
The only detectable peak was at the benzene elution time, and this
compound concentration was much less than the corresponding peak in the
samples from total DAF ventilation air stream. The results of this
analysis are presented in Table 2-16.
2-19
-------
Table 2-14. GAS CHROMATOGRAPH RESULTS FROM THE
DAF CARBON HOUSE VENT (V-204)
CHEVRON REFINERY - EL SEGUNDO, CALIFORNIA
DATE 8/10
TIME 1205
RUN NO./LOCATION V-204
ANALYTICAL RESULTS (ppmv as compound)
C-l 0
C-2 0
C-3 0
C-4 0
C-5 0
Hexane 14.5
Benzene 24.0
Heptane 14.9
Toluene 35.8
m-Xylene 0
o-Xylene 0
TOTAL HYDROCARBON3 (ppmv as compound) 108
CONTINUOUS MONITOR DATA
Hydrocarbon Level (ppmv as C3H8) 131
Emission Rate (Ibs/hr) 1.85
PROCESS CONDITIONS
% N2 76.17
% 02 19.61
aTotal includes unidentified hydrocarbon responsive
to GC/FID.
2-20
-------
Table 2-15. MONITORED EMISSION RESULTS: HYDROCARBON MONITORING AT THE
FLOCCULATION TANK (T-201) AND THE FLASH/MIX TANK (T-200)
CHEVRON - EL SEGUNDO, CALIFORNIA
ro
ro
>-*
Flocculation Tank
Flash/Mix Tank
Average DAF
system
ventilation
Date
8/9/83
8/9/83
8/9/83
Concentration3
Time (ppm as C3H8)
1140 74
1510 14
1100-1500 541
Gaseous
flow
(SCFM)
570b
340b
2153
Mass flow rate
(Ibs/hr as C3H8)
0.27
0.0305
8.85
Percent
total
mass flow
3.1
0.3
—
Integrated gas bag analyzed with Beckman 400 FIA.
^Measured the velocity with plant installed pitot tubes.
-------
Table 2-16. GAS CHROMATOGRAPH RESULTS FROM THE
FLOCCULATION TANK (T-201) AND FLASH/MIX TANK (T-200)
CHEVRON REFINERY - EL SEGUNDO, CALIFORNIA
DATE
TIME
RUN NO. /LOCATION
ANALYTICAL RESULTS (pprav as compound)
C-l
C-2
C-3
C-4
C-5
Hexane
Benzene
Heptane
Toluene
m-Xylene
o-Xylene
TOTAL HYDROCARBON3 (ppmv as compound)
CONTINUOUS MONITOR DATA
Hydrocarbon Level (ppmv as C3H8)
Emission Rate (Ibs/hr)
PROCESS CONDITIONS
% N2
% 02
8/9
1140
T-201
0
0
0
0
0
0
4.6
0
0
0
0
20
74
0.27
76.66
19.76
8/9
1510
T-200
0
0
0
0
0
0
3.5
0
0
0
0
20
14
0.0305
75.26
19.42
aTotal includes unidentified hydrocarbon responsive to
GC/FID.
2-22
-------
2.1.2 Equalization Tank
A summary of the dally average total hydrocarbon mass flow rates in
the equalization tank prior to the emission control device is presented
in Table 2-3. The total hydrocarbon measurement does not exclude methane.
The hydrocarbon mass flow in the equalization tank ventilation air
ranged from 4.18 Ibs/hr to 4.65 Ibs/hr (24-hour average basis) over the
three days of testing. The average mass flow was 4.26 Ibs/hr (24-hour
basis).
The test results on a one-hour average basis for each day of testing
are presented in Tables 2-17 to 2-19. The average total hydrocarbon
concentration based on equivalents of propane is presented for each
one-hour period. The average gas flow rate result that was used for
calculation of the mass flow is presented in Table 2-20. The comparison
of the daily flow rate differences of 0.8 to 1.3 percent justified the
use of a single flow value for each day.
The composition analysis of the ventilation stream from the equali-
zation tank is presented in Table 2-20. The hydrocarbon species analysis
shows a relatively significant amount of methane and toluene and a
number of peaks associated with the benzene and m-xylene calibration
standards.
On 8/5/83 measurements were performed at the equalization tank
carbon house outlet to estimate the hydrocarbon removal efficiency. The
test results are shown in Table 2-19 at 1400-1600 pm. At the time, the
carbon was apparently saturated and was not removing any hydrocarbons.
The species analysis (Table 2-21) confirms that the hydrocarbons exiting
the carbon house were essentially the same as those entering. On 8/12/83,
tests were repeated at the equalization tank carbon house after the
carbon was changed. The total hydrocarbon mass flow data are presented
in Table 2-22 and the chromatographic speciation results are presented
in Table 2-23. For the test with fresh carbon, when the inlet total
hydrocarbon mass flow was 7.54 Ibs/hr, the outlet rate was 0.77 Ib/hr,
for a hydrocarbon removal efficiency of 89.8 percent. The species
analysis presented in Table 2-23 indicates that the hydrocarbons not
collected in the carbon house was solely methane, and the carbon was
achieving complete removal on heavier components, within the accuracy of
the measurement technique.
2-23
-------
Table 2-17. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT
THE EQUALIZATION TANK VENTILATION AIR LOCATION,
CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/3/83
Time
1200C
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
Average
Concentration3
(ppm as C3H8)
140
140
145
147
150
145
140
150
152
160
175
180
180
Flowb
(SCFM)
4240
4240
4240
4240
4240
4240
4240
4240
4240
4240
4240
4240
4240
Emission Rate
(Ibs/hr as C3H8)
3.80
3.80
3.94
3.99
4.07
3.94
3.80
3.99
4.13
4.35
4.75
4.89
4.89
4.18
Concentration is average value for continuous readings across the hour
(0-55 minutes) based on 5-minute readings.
One flow measurement taken during test periods; therefore, used flow
measurement across test day. See Table 2-20.
cHydrocarbon Monitor (Beckman 400) on-line.
2-24
-------
Table 2-18. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT
THE EQUALIZATION TANK VENTILATION AIR LOCATION,
CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/4/83
Time
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
Average
Concentration3
(ppm as C3H8)
185
185
190
190
190
190
192
190
185
180
190
175
175
170
165
160
155
155
150
155
160
165
160
170
F1owb
(SCFM)
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
4169
Emission Rate
(Ibs/hr as C3H8)
4.94
4.94
5.07
5.07
5.07
5.07
5.13
5.07
4.94
4.80
5.07
4.67
4.67
4.54
4.41
4.28
4.14
4.14
4.01
4.14
4.28
4.41
4.28
4.54
4.65
Concentration is average value for continuous readings across the hour
(0-55 minutes) based on 5-minute readings.
An initial and final flow measurement taken during test period; therefc
used average flow measurement across test day. See Table 2-20.
2-25
-------
Table 2-19. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT
THE EQUALIZATION TANK AND EQUALIZATION TANK CARBON HOUSE OUTLET LOCATIONS,
CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/5/83
Time
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300
1400C
1500C
r f
1600C'T
L
Average
Concentration3
(ppm as C3H8)
170
170
170
170
170
180
180
160
155
152
150
155
152
156d
190e
A
190e
Flow Emission Rate
(SCFM) (Ibs/hr as C3H8)
4035
4035
4035
4035
4035
4035
4035
4035
4035
4035
4035
4035
4035
4035
4035
4035
Ventilation air
Equalization
tank carbon
house outlet
4.39
4.39
4.39
4.39
4.39
4.65
4.65
4.14
4.01
3.93
3.88
4.01
3.93
4.03
4.91
4.91
4.24
4.62
Concentration is average value for continuous readings across the hour
(0-55 minutes) based on 5-minute readings.
Pitot measurements at initial and final periods of test day; therefore,
used average of flow measurements. See Table 2-10.
Continuous hydrocarbon analyzer moved to sample Equalization Tank Carbon
House Vent.
Upwind side of Carbon House Vent.
eDownwind side of Carbon House Vent.
End of test at the Equalization Tank area.
2-26
-------
Table 2-20. SUMMARY OF PITOT MEASUREMENTS:
FLOW MONITORING AT THE EQUALIZATION TANK OUTLET
CHEVRON - EL SEGUNDO, CALIFORNIA
Test Day 8/3/83
AM Measurement
(SCFM) NM
PM Measurement
(SCFM) 4240
Average
(SCFM) 4240
% Difference —
8/4/83 8/5/83
4185 4009
4153 4062
4169 4035
0.8 1.3
NM = Not measured.
2-27
-------
Table 2-21. GAS CHROMATOGRAPH RESULTS FROM THE EQUALIZATION TANK
TEST DAYS 8/3/83 to 8/5/83
CHEVRON REFINERY, EL SEGUNDO, CALIFORNIA
DATE
TIME
LOCATION
RUN NO.
ANALYTICAL RESULTS
(ppmv as compound)
C-l
C-2
C-3
C-4
C-5
Hexane
Benzene
Heptane
Toluene
m-Xylene
o-Xylene
8/3
1600-
1700
8/4
1053-
1235
8/4
1431-
1510
Ventilation
1
27.0
2.0
0
0
0
0
7.7
29.2
4.6
1.7
1
29.4
1.2
0
0
0
2.3
9.7
25.5
4.0
1.5
2
24.6
0
0
0
0
2.1
4.9
13.6
1.7
0
8/5
930-
1000
air
I
17.7
0
0
0
0
1.4
7.8
18.7
3.6
1.1
8/5
1228-
1252
2
20.4
1.8
0
0
0
2.1
12.5
29.8
7.0
2.4
8/5
1400-
1510
Carbon
house
outlet
OUT
22.3
1.6
0
0
0
0
20.4
26.8
0
0
TOTAL HYDROCARBON11
(ppmv as compound) 72 74
CONTINUOUS MONITOR
DATA
Hydrocarbon Level
(ppmv as C3H8) 150 182
Emission Rate
(Ib/hr) 4.07 4.87
PROCESS CONDITIONS
% N2 73.60 73.80
% 02 20.35 20.40
47
50
76
167
155
155
72
179
4.45 3.98 3.98 4.65
78.20 77.50 77.77 76.55
21.50 20.40 20.46 19.75
Total includes unidentified hydrocarbon responsive to GC/FID.
2-28
-------
Table 2-22. MONITORED EMISSION RESULTS: HYDROCARBON MONITORING AT THE
EQUALIZATION TANKS VENTILATION AIR AND CARBON HOUSE EXHAUST
CHEVRON - EL SEGUNDO, CALIFORNIA
Equalization
Tank Carbon
House Inlet
Equalization
Tank Carbon
House Outlet
8/12/83 1129
8/12/83° 1230
284
29
4146C
4146°
7.54
0.77
Used the average flowrate measured at the Equalization Tank Outlet Sample
Location during the test period 8/3/83 to 8/5/83.
^Tested hydrocarbon levels at the Equalization Tank Outlet (inlet to Carbon
House) and Carbon House Vent after Chevron changed the activated charcoal.
2-29
-------
Table 2-23. GAS CHROMATOGRAPH RESULTS AT THE EQUALIZATION TANK
TEST DAY 8/12/83
CHEVRON REFINERY, EL SEGUNDO, CALIFORNIA
DATE
TIME
LOCATION
RUN NO.
ANALYTICAL RESULTS
(ppmv as compound)
c-i
C-2
C-3
C-4
C-5
Hexane
Benzene
Heptane
Toluene
m-Xylene
o-Xylene
8/12/83
Ventilation
air
1
15.4
0
0
0
0
5.8
38.6
0
0
14.8
5.6
8/12/83
Carbon
1
24.4
0
0
0
0
0
0
0
0
0
0
8/12/83
house exhaust
2
23.5
0
0
0
0
0
0
0
0
0
0
TOTAL HYDROCARBON"
(ppmv as compound)
CONTINUOUS MONITOR
DATA
Hydrocarbon Level
(ppmv as C3H8)
Emission Rate
(Ib/hr)
PROCESS CONDITIONS
% N2
% 02
89
284
7.54
75.60
19.58
24
80.35
23.86
23
29
0.77
78.34
19.92
Total includes unidentified hydrocarbon responsive to GC/FID.
2-30
-------
2.2 UNSEGREGATED WATER SYSTEM, IAF UNIT
The one-hour average concentration results are presented in
Tables 2-24 to 2-28. The average total hydrocarbon concentration ranged
from 6558 to 7600 ppm as C3H8. The hydrocarbon concentration was
relatively constant and showed no trends. The flow from the IAF can be
characterized as a breathing-type flow. For intermittent periods these
would be small positive flows, followed by periods of zero flow or
in-breathing to the unit. The flow was monitored constantly during the
following periods: 1700-1900 8/10/83, 2100-2200 8/10/83, 0000-0100 8/11/83,
0900-1400 8/11/83, and 0900-1400 8/12/83. The results of these measure-
ments are presented in Table 2-29. The measured equivalent positive
flow rates were relatively consistant except for one period on
8/10/83-8/11/83. This lower measurement could have been caused by
fugitive losses from inspection doors that are normally opened each
shift. Prior to all other test runs, the doors were inspected and
sealed tightly prior to flow monitoring.
Because of the intermittent nature of the gaseous flow from the IAF
unit, no daily average mass flow rate in the ventilation air was
calculated. The total hydrocarbon mass flow rate for those periods when
ventilation air rates were available are listed in Tables 2-24 and 2-28.
The mass rate ranged from 0.27 to 0.31 Ib/hr, with an average of 0.27 Ib/hr,
when the low flow measurements are excluded. Attempts were made to
provide a constant, positive flow of plant nitrogen to the IAF to provide
a steady stream for measurement. These attempts were unsuccessful
because of a pressure relief valve that opened at a pressure less than
the ventilation stream backpressure.
The composition analysis of the ventilation stream from the IAF is
presented in Table 2-30. The hydrocarbon species analysis shows a
relatively significant amount of methane and a number of peaks in the
C4 to C7 range. The inert gas at this location was essentially nitrogen,
which corresponds to the expected results.
On 8/12/83, a test was performed to estimate the hydrocarbon removal
efficiency of the carbon drum. The results are presented in Table 2-28.
The inlet and outlet mass rates were essentially the same. Since this
system was installed for odor control and the low flow rates from the
IAF were not causing a detectable odor, Chevron was not routinely replacing
2-31
-------
Table 2-24. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT THE
IAF VENTILATION AIR SAMPLE LOCATION, CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/8/83
Concentration3 Flow Emission Rate
Time (ppm as C3H8) (SCFM) (Ibs/hr as C3H8)
1800C 6725 NM —
1900 6967 NM —
2000 7000 NM —
2100 7000 NM —
2200 7000 NM —
2300 6917 NM —
2400 6900 NM —
Average 6930 ppm as C3H8
Concentration is average value for continuous readings across the hour
(0-55 minutes) on 5-minute readings.
Due to varying flowrates between day and night periods, emission rate
calculations are based on actual flow measurements only at the times
monitored. See Table 2-29.
Continuous Hydrocarbon Analyzer (Beckman 402) on-line at IAF Outlet
Sample Location starting the test period.
NM = Not measured.
2-32
-------
Table 2-25. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT THE
IAF VENTILATION AIR SAMPLE LOCATION, CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/9/83
Concentration3 Flow Emission Rate
Time (ppm as C3H8) (SCFM) (Ibs/hr as C3H8)
0100 6850 NM —
0200 6800 NM —
0300 6800 NM —
0400 6800 NM —
0500 6800 NM —
0600 6800 NM —
0700 6817 NM —
0800 6853 NM —
0900 6796 NM —
1000 6810 NM —
1100 6558 NM —
1200 6571 NM —
1300 6693 NM —
1400 6769 NM —
1500 6815 NM —
1600 6800 NM —
1700 6995 NM —
1800 7090 NM —
1900 7138 NM —
2000 7144 NM —
2100 7117 NM —
2200 7075 NM —
2300 6990 NM —
2400 6950 NM —
Average 6868 ppm as C3H8
Concentration is average value for continuous readings across the hour
(0-55 minutes) on 5-minute readings.
Due to varying flowrates between day and night periods, emission rate
calculations are based on actual flow measurements only at the times
monitored. See Table 2-29.
NM = Not measured.
2-33
-------
Table 2-26. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT
THE IAF OUTLET SAMPLE LOCATION, CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/10/83
Concentration3 Flow Emission Rate
Time (ppm as C3H8) (SCFM) (Ibs/hr as C3H8)
0100 6900 NM —
0200 6900 NM —
0300 6825 NM —
0400 6800 NM —
0500 6780 NM —
0600 6750 NM —
0700 6690 NM —
0800 6660 NM —
0900 6640 NM —
1000 6650 NM —
1100 6700 NM —
1200 6750 NM —
1300 6810 NM —
1400 6890 NM —
1500 6750 NM —
1600 6775 NM —
1700 6900 5.7 0.25
1800 7050 5.7 0.25
1900 6850 5.7 0.25
2000 6800 NM —
2100 6850 0.38 0.017
2200 6800 0.38 0.017
2300 6790 NM —
2400 6700 NM —
Average 6792 ppm as C3H8
Concentration is average value for continuous readings across the hour
(0-55 minutes) on 5-minute readings.
Due to varying flowrates between day and night periods, emission rate
calculations are based on actual flow measurements only at the times
monitored. See Table 2-29.
NM = Not measured.
2-34
-------
Table 2-27. CONTINUOUS EMISSION RESULTS: HYDROCARBON MONITORING AT
THE IAF OUTLET SAMPLE LOCATION, CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/11/83
Time
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300
1400C
Average
Concentration3
(ppm as C3H8)
6650
6700
6750
6730
6720
6750
6800
6890
6950
7170
7250
7300
7490
7600
Flow
(SCFM)
0.41
NM
NM
NM
NM
NM
NM
NM
6.3
6.3
6.3
6.3
6.3
6.3
Emission Rate
(Ibs/hr as C3H8)
0.018
—
—
—
—
—
—
—
0.28
0.29
0.29
0.29
0.31
0.31
0.29
Concentration is average value for continuous readings across the hour
(0-55 minutes) on 5-minute readings.
Flow measured 4 times between 0951-1559 with 4 flow values averaging to
6.3 SCFM. See Table 2-29.
GTest period discontinued at IAF outlet until following day period.
NM = Not measured.
2-35
-------
Table 2-28. CONTINUOUS EMISSIONS RESULTS: HYDROCARBON MONITORING AT
THE IAF OUTLET AND IAF CARBON DRUM SAMPLE LOCATION
CHEVRON - EL SEGUNDO, CALIFORNIA
TEST DAY 8/12/83
Time
Concentration3
(ppm as C3H8)
Flow
(SCFM)
Emission Rate
(Ibs/hr as C3H8)
i 0900°
i
j 1000
1
1 1100
L
6271d
6589d
6614d
5.8
5.8
5.8
0.22
0.24
0.24
1
i
i
i
i
1
J
1200C
1300
1400f
Average
7222
7222
7292
5.8
5.8
5.8
IAF Ventilation
air
IAF Carbon Drum
0.27
0.27
0.27
0.27
0.23
Concentration is average value for continuous readings across the hour
(0-55 minutes) on 5-minute readings.
Flow measured 4 times between 1033-1446 with 4 flow values averaging to
3.8 SCFM. See Table 2-29.
Continuous Hydrocarbon Analyzer (Beckman 402) on-line at IAF Carbon Drum
Vent Sample Location restarting the test period.
On-line at the IAF Carbon Drum Vent.
Continuous Hydrocarbon Analyzer (Beckman 402) switched to IAF ventilation
air sample location.
End of test period.
2-36
-------
Table 2-29. IAF FLOW MEASUREMENTS:
CHEVRON - EL SEGUNDO, CALIFORNIA
Date
8/10/83
8/10/83
*> 8/11/83
" 8/11/83
8/11/83
8/11/83
8/11/83
8/12/83
8/12/83
8/12/83
8/12/83
Temperature
Time (°F)
1745-1903
2145-22303
0045-0120*
0951-1016
1032-1103
1310-1357
1517-1559
1033-1119
1130-1215
1230-1315
1400-1446
84
72
72
88
88
88
88
84
84
84
84
Feet
744
194
190
1275
1725
2042
2294
2197
1725
2080
2194
Time
period
in min
15
45
40
25
30
47
42
46
45
45
46
Anemometer
average rate
(ft/min)
Indicated
49.6
4.3
4.7
51.0
69.0
43.4
54.6
48.1
38.3
46.2
48.1
True
68.8
b
b
70.8
91.1
66.3
75.8
66.8
58.5
64.2
66.8
Actual
volumetric
flowrate
(ACFM)
6.0
0.38
0.41
6.1
7.9
5.8
6.7
5.8
5.0
5.6
5.8
Standard
volumetric
flowrate
(SCFM)
5.7
0.38
0.41
5.8
7.5
5.5
6.4
5.4
4.9
5.4
5.7
Flow measurements monitored during night period with lower process gas temperatures.
JNot within manufacturer's range suggested for the anemometer.
-------
Table 2-30. GAS CHROMATOGRAPHY RESULTS FROM THE IAF
TEST DAYS 8/11/83 to 8/12/83
CHEVRON REFINERY, EL SEGUNDO, CALIFORNIA
DATE
TIME
LOCATION
RUN NO.
ANALYTICAL RESULTS
(ppmv as compound)
C-l
C-2
C-3
C-4
C-5
Hexane
Benzene
Heptane
Toluene
m-Xylene
o-Xylene
TOTAL HYDROCARBON3
(ppmv as compound)
CONTINUOUS MONITOR
DATA
Hydrocarbon Level
(ppmv as C3H8)
Emission Rate
(Ib/hr)
PROCESS CONDITIONS
% N2
% 02
8/11
0924-
0942
8/11
1213-
1245
Ventilation air
1
1602
7.6
18.2
42.0
283
1288
835
826
421
252
145
5720
6950
0.20
91.98
6.00
2
2818
3217
2913
80.5
220
6127
2642
938
0
105
31.7
19,092
7300
0.21
93.90
6.60
8/12
1213-
1254
Carbon drum
1
2156
8.2
21.8
72.1
510
2005
2101
793
0
385
106
8158
7222
0.18
90.71
7.19
8/12
1040-
1120
outlet
2
1762
4.5
12.8
36.4
110
2033
1074
449
0
168
67.8
5717
6601
0.16
83.09
12.98
3Total includes unidentified hydrocarbon responsive to GC/FID.
2-38
-------
the drums. It would be expected that the carbon would become saturated
under these conditions. A sample of the drum outlet stream was collected
and analyzed, and the results are shown in Table 2-30. This result
confirms the similarity of the inlet and outlet gases.
2.3 PROCESS WATER ANALYSES
Tables 2-31 through 2-39 provide the process water analysis for the
composite and grab samples taken during the hydrocarbon (air) monitoring.
Designated samples (item, location) were analyzed for the following
parameters:
• TOC (total organic carbon);
• COD (chemical oxygen demand);
• oil and grease; and
• TCO (total chromatographable organics/hydrocarbon speciation
(C7-C30) and VOA by purge and trap GC/FID.
All analytical parameters are reported in milligrams per liter (ppmw),
except purge and trap values which are given in parts per billion (ppbw).
The most critical factors in the measurement of the process water
parameters were the collection of representative samples at the site
location and obtaining a representative aliquot for analysis in the
laboratory. In most cases the samples involved two-phase oil/water
mixtures which contributed to the non-homogeneity of the samples and to
the variation in the sample values.
The sampling points at the Chevron Effluent Treatment Plant were
dictated by the physical layout and available sample locations. The
samples were collected from streams at elevated temperatures, stored on
ice, and shipped to the TRW laboratory. Sample preservatives were not
utilized in preference to immediate analysis (24-48 hours) and to the
elevated levels of hydrocarbons in the streams. Upon arrival at the
laboratory all samples were homogenized prior to analysis; however, the
two-phased system and the cooling of the sampling affected the homogeneity
of the samples. All samples were brought to room temperature and shaken
vigorously before samples were removed. In addition, due to the high
levels of the parameters being measured, the size of the sample aliquots
were small which also contributed to the variability from sample to
sample.
2-39
-------
Table 2-31. CHEVRON, EL SEGUNDO, CALIFORNIA SAMPLES TAKEN ON 8/3/83
COD Oil /grease
TRW No. mg/L mg/L
Liquid Composite Samples
DAF-in 4,957 2,969 491
3,008 535
DAF-out 4,961 1,748 133
144
EQ-out 4,972 1,911 123
1,870 120
Volatile Organic Samples
DAF-in #1 VOA (1650)a 4,973 — —
DAF-out #1 VOA (1650) 4,975 — —
EQ-out VOA (1650) 4,987 — —
TOC TCO
mg/L mg/L
— 71.56
—
— 30.90
—
— 21.00
611 —
365 —
661 —
aTime sample taken.
(continued)
2-40
-------
Table 2-31. Concluded
Liquid Composite Samples
DAF-in
DAF-out
EQ-out
Note: Benzene could not
solvent.
TRW No.
4,957 Toluene
C8
C9
C9
Cn
Cj2
Ci2
Ci2
"12
"12
"12
Ci2
Cjs
GIS
Cl4
Cis
Cl5
4,961 Toluene
C9
CIQ
Cn
Cn
Cn
C13
4,972 Toluene
C9
C9
CIG
Cl2
be determined due to a co-el uting
Note: These values were calculated using average response
C7-Cn, Cu-C16, and C17 to C25 hydrocarbons. Due
response of C17 to C2s hydrocarbons as compared to
values of some C17-C2s compounds were found.
mg/L
13.302
2.278
1.328
1.040
17.709
2.679
4.207
4.940
5.339
12.214
2.932
1.436
1.930
1.487
10.496
3.128
4.838
3.570
3.066
3.643
2.595
15.412
4.972
5.549
0.828
1.383
2.679
2.232
2.257
3.301
2.460
11. 538
3.927
3.617
1.180
peak in the
factors of
to the reduced
C7-Cu, high
2-41
-------
Table 2-32. CHEVRON, EL SEGUNDO, CALIFORNIA SAMPLES TAKEN ON 8/4/83
TRW No.
Liquid Composite Samples
DAF-in 4,958
DAF-out 4,962
EQ-out 4,970
Volatile Organic Samples
DAF-in-VOA pm (1500) 4,974
DAF-in-VOA (1000) 4,977
DAF-out VOA pm (1500) 4,976
DAF-out VOA (1000) 4,982
EQ-out VPA (1000) 4,988
EQ-out VOA (1500) 4,989
COD
mg/L
4,024
4,228
1,545
1,585
1,565
2,033
2,155
—
—
—
—
—
—
—
Oil/grease
mg/L
440
441
125
94
126
148
142
—
—
—
—
—
—
—
TOC
mg/L
—
—
—
—
—
—
484
a
478
475
550
542
464
455
511
Sample lost; replaced with aliquot from DAF-in, TRW #4958, liquid
composite sample result was 1,096 mg/L.
2-42
-------
Table 2-33. CHEVRON, EL SEGUNDO, CALIFORNIA SAMPLES TAKEN ON 8/5/83
Liquid Composite Samples
DAF-in
DAF-out
EQ-out
Volatile Organic Samples
DAF-in VOA (0915)
DAF-in VOA (1530)
DAF-out VOA (0915)
DAF-out VOA (1530)
EQ-out VOA (1530)
EQ-out VOA (0915)
TRW No.
4,959
4,963
4,971
4,978
4,979
4,983
4,984
4,990
4,991
COD Oil /grease TOC
mg/L mg/L mg/L
8,056 6.14 —
2,179 2.37 —
1,240 110 —
1,301 109 —
a
— — 722
— — 578
— — 713
— — 600
_ _ b
TCO
mg/L
—
aSample lost; replaced with aliquot from DAF-in, TRW #4,959, liquid
composite samples. Results are 849, 940, 860 mg/L.
Sample lost; replaced with aliquot from EQ-out, TRW #4,971, liquid
composite samples. Results are 416, 398, 476 mg/L.
2-43
-------
Table 2-34. CHEVRON, EL SEGUNDO, CALIFORNIA SAMPLES TAKEN ON 8/8/83
COD Oil/grease TOC TCO
TRW No. mg/L mg/L mg/L mg/L
Liquid Composite Samples
DAF-in
DAF-out
API-2 Inlet A (201)
API-2 Inlet B (202)
API-2 Inlet C (203)
API-2 Inlet D (204)
API-4
Volatile Organic Samples
DAF-in VOA (1100)
DAF-in VOA (1500)
DAF-out VOA (1100)
DAF-out VOA (1500)
4,960
4,964
4,965
4,966
4,967
4,968
4,969
4,980
4,981
4,985
4,986
2,155
2,114
1,470
20.3
2,560
463
480
2,440
—
—
—
—
383
376
0.21
6.4
65.49
20.9
26.97
18.26
—
—
—
—
— 41. 94
— —
— 22.38
— 1.74
— 84.00
— 9.30
— 8.26
— 45.66
538 —
a
622 —
b _
aSample lost; replaced with aliquot from DAF-in, TRW #4,960, liquid
composite samples. TOC result is 616 mg/L.
Sample lost; replaced with aliquot from DAF-out, TRW #4,964, liquid
composite samples. TOC result if 774 mg/L.
(continued)
2-44
-------
Table 2-34. Continued
TRW No.
mg/L
Liquid Composite Samples
DAF-in
DAF-out
API-2 Inlet A (201)
API-2 Inlet B (202)
4,960 Toluene 9.920
C8 2.312
C9 13.518
C10 3.935
C10 3.901
C10 1.871
C12 4.727
C12 1.407
C12 0.783
C12 0.801
C13 4.496
C14 2.837
C15 0.838
C15 3.285
C16 3.136
4,964 Toluene 5.085
C9 10.601
C9 3.697
C10 3.284
C10 1.210
4,965
4,966 Toluene 2.571
C8 1.005
C9 2.065
C9 23.039
C9 1.858
C10 7.464
C10 12.990
Cn 5.835
Cn 0.932
Cu 0.051
C1± 1.153
Cn 4.145
C12 14.226
(continued)
2-45
-------
Table 2-34. Concluded
TRW No.
mg/L
API-2 Inlet C (203)
API-2 Inlet D (204)
API-4
4,967
4,968
4,969
^14
c"
C19
Toluene
C8
Toluene
C8
C12
C12
Cl4
CIB
ell
Civ
13.544
4.316
8.411
2.306
9.465
7.679
59.638
45.744
65.488
2.165
1.034
6.595
1.848
12.555
3.390
3.291
3.341
8.448
2.
1.
1.
7.
1.
436
395
447
986
654
5.173
1.
5.
,388
.558
4.977
46.394
2-46
-------
Table 2-35. CHEVRON, EL SEGUNDO, CALIFORNIA SAMPLES TAKEN ON 8/9/83
COD Oil /grease TOC TCO
TRW No. mg/L mg/L mg/L mg/L
Liquid Composite Samples
DAF-out
API-2 Inlet A (201)
API-2 Inlet B (202)
API-2 Inlet C (203)
API-2 Inlet D (204)
API-4
Volatile Organic Samples
DAF-in VOA (0900)
DAF-in VOA (1342)
DAF-out VOA (0900)
DAF-out VOA (1340)
5,022 1,579 154 — —
5,028 693 61.56 — —
5,029 3,155 19.50 — —
5,040 5,179 32.27 — —
5,041 2,230 18.28 — —
5,030 620 23.90 — —
5,007 — — 482 —
5,010 — — 440 —
5,006 — — 341 —
5,008 — — 509 —
2-4,7
-------
Table 2-36. CHEVRON, EL SEGUNDO, CALIFORNIA SAMPLES TAKEN ON 8/10/83
COD Oil /grease TOC TCO
TRW No. mg/L mg/L mg/L mg/L
Liquid Composite Samples
DAF-in
DAF-in
DAF-out
API-2 SP 201
API-2 SP 202
API-2 SP 203
API-2 SP 204
Volatile Organic Samples
DAF-in VOA (0920)
DAF-in VOA (1600)
DAF-out VOA (0920)
DAF-out VOA (1600)
5,024 2,170 23.80 — —
5,025 2,121 53.98 — —
5,023 2,078 47.75 — —
5,031 594 33.80 — —
5,012 2,764 42.48 — —
5,013 950 70.03 — —
5,014 2,635 32.62 — —
5,002 — — 619 —
5,005 — — 471 —
5,004 — — 546 —
5,011 — — 511 —
2-48
-------
Table 2-37. CHEVRON, EL SEGUNDO, CALIFORNIA SAMPLES TAKEN ON 8/11/83
Liquid Composite Samples
DAF-in
DAF-out
lAF-in
lAF-out
API-4
API-2 SP 201
API-2 SP 202
API-2 SP 203
API-2 SP 204
Volatile Organic Samples
DAF-in VOA (0900)
DAF-in VOA (1530)
DAF-out VOA (0900)
DAF-out VOA (1530)
lAF-in VOA (1000)
lAF-in VOA (1600)
lAF-out VOA (1000)
lAF-out VOA (1600)
COD
TRW No. mg/L
5,027 2,316
5,026 1,410
5,034 811
5,035 201
5,033 1,616
5,015 100
5,016 1,700
5,021 99
5,017 450
5,001 —
5,003 —
5,000 —
5,009 —
4,993 —
4,994 —
4,992
4,995 —
Oil /grease TOC TCO
mg/L mg/L mg/L
43.74 — 95.26
54.92 — 22.42
61.58 — 12.58
46.73 — 11.06
43.59 — 96.20
17.97 — 9.20
37.24 — 30.68
24.45 — 8.60
33.06 — 51.98
— 530 —
— 355 —
— 454 —
— 343 —
— 64.5 —
— 402 —
134
— 52.0 —
(continued)
2-49
-------
Table 2-37. Continued
TRW No.
mg/L
Liquid Composite Samples
DAF-in
DAF-out
lAF-in
lAF-out
5,027 Toluene
C8
cg
C8
C8
C9
C9
C9
CIQ
CIQ
CIQ
Ci2
C13
Cj3
C14
Cl5
Cl6
Civ
Cis
Cj9
^20
5,026 Toluene
C8
C9
C9
CIQ
GIO
Cn
Cj2
Cl3
5,034 Toluene
C8
5,035 Toluene
C8
14. 141
1.211
1.471
5.429
1.901
2.553
6.035
3.027
5.068
7.398
6.526
15.370
14.351
4.388
9.436
10.194
6.915
58.459
47.247
44. 281
28.031
4.430
0.838
0.805
7.528
4.021
3.658
1.375
0.852
0.920
1.549
0.668
1.334
0.581
(continued)
2-50
-------
Table 2-37. Continued
API-4
API-2 SP 201
API-2 SP 202
API-2 SP 203
TRW No.
5,033 Toluene
C8
Ca
C9
C9
C9
C9
CIQ
CIQ
CIQ
CIQ
CIQ
CIQ
Cn
Cn
Cn
C12
Cj3
Cis
Cl6
5,015
5,016 Toluene
C8
C9
Cg
CIQ
CIQ
Cn
Cis
Cis
C13
Cl4
Cl5
5,021 Toluene
mg/L
39.430
28.123
11. 348
4.708
2.586
0.954
13.200
3.242
1.512
1.126
4.686
3.127
2.379
1.349
1.502
1.561
1.976
1.679
1.832
2.025
2.221
1.434
1.188
3.697
3.205
3.147
1.684
4.622
1.450
2.900
4.285
3.544
0.902
(continued)
2-51
-------
Table 2-37. Concluded
TRW No. mg/L
API-2 SP 204 5,017 Toluene <0.5
Cn 4.055
Cu 1.755
Cu 1.505
Cu 1.002
Ctl 1.395
Cu 2.130
C12 12.261
C12 3.872
C12 4.312
C13 10.914
C14 7.363
C15 3.839
C16 70.078
2-52
-------
Table 2-38. CHEVRON, EL SEGUNDO, CALIFORNIA SAMPLES TAKEN ON 8/12/83
COD Oil /grease TOC TCO
TRW No. mg/L mg/L mg/L mg/L
Liquid Composite Samples
lAF-in
lAF-out
API-4
API-2 SP 201
API-2 SP 202
API-2 SP 203
API-2 SP 204
Volatile Organic Samples
lAF-in VOA (0900)
lAF-in VOA (1250)
lAF-out VOA (0900)
lAF-out VOA (1330)
5,036 320 14.14 — —
5,038 302 64.95 — —
5,039 202 26.5 — —
5,020 405 12.0 — —
5,019 1,584 70.71 — —
5,018 1,000 36.74 _ _
5,037a — — — —
4,998 — — 86.0 —
4,999 — — 57.0 —
4,997 — — 162 —
4,996 — — 46.0 —
aSample broken in laboratory.
2-53
-------
Table 2-39. Cx to C7 SPECIATION BY GC/FID PURGE AND TRAP
CHEVRON, EL SEGUNDO, CALIFORNIA
TRW No. Sample Number
4973 DAF-IN-01-VOA
4975 DAF-OUT-tfl-VOA
4987 EQ-OUT-VOA
4987 EQ-OUT-VOA
4980 DAF-302-IN-VOA-1100
4985 DAF-302-OUT-VOA-1100
5003 DAF-202-IN-1530-VOA
Compound
C2H6S2
Benzene
Toluene
C2H6S2
Benzene
C4H10S2
Toluene
C2H6S2
Benzene
C4H10S2
Toluene
C2H6S2
Benzene
C4H10S2
Toluene
Benzene
Toluene
Benzene
Toluene
C2H6S2
Benzene
C4HiS2
Toluene
Concentration
Date Taken (in ppb)
8/03/83 187
118
341
8/03/83 1420
2660
432
7200
8/03/83 939
1970
411
5710
8/03/83 943
1770
410
5020
8/08/83 11400
13000
8/08/83 9790
11600
8/11/83 204
9230
274
9860
(continued)
2-54
-------
Table 2-39. Concluded
TRW No. Sample Number
Concentration
Compound Date Taken (In ppb)
5009
DAF-202-OUT-1530-VOA
4994
4994
4995
IAF-IN-VOA-1600
IAF-IN-VOA-1600
IAF-OUT-VOA-1600
Benzene
C4H10S2
Toluene
Benzene
Toluene
Benzene
Toluene
Benzene
Toluene
8/11/83
8/11/83
8/11/83
8/11/83
7750
59
8940
2120
2110
1980
2000
1970
2080
2-5.5
-------
The differences in the results obtained from the utilization of the
two water sampling procedures is attributed to the collection of 40 ml
samples (VGA bottles) versus a composite sample 4 liters) integrated
over time. In addition, analysis of samples from a composite bottle at
a later date for purgable VOCs is affected by the homogeneity of the
sample and the loss of volatiles during storage.
-------
3. PROCESS DESCRIPTION
The Chevron refinery in El Segundo is a large refinery with a crude
throughput capacity of 405,000 barrels per calendar day (b/cd).1 The
Effluent Guidelines Division of the Environmental Protection Agency (EPA)
places Chevron in refinery subcategory C which includes refineries
producing petroleum products by the use of topping, cracking, and petro-
2
chemical operations. At the time of the test, the refinery was operating
at less than full capacity. Table 3-1 lists the crude throughputs
reported during the test period.
3.1 REFINERY WASTEWATER SYSTEM
The refinery wastewater system at Chevron, (Figure 3-1) is divided
into two separate systems. The segregated system handles the majority
of the oily wastewater while the unsegregated systems handles mostly
non-oily wastewaters. Each system will be described in detail below.
3.2 SEGREGATED SYSTEM
The main components of the segregated system are the #4 API separator
and the Effluent Treating Plant (ETP). Wastewater is collected at
individual process units and directed by a main trunkline to the
#4 separator. An additional API separator (#3 separator) collects tank
draw off water from one section of the plant and also empties into the
trunkline leading to the #4 separator. In the newer units, process
drains in the segregated system have raised hubs which prevent stormwater
and other surface waters from entering the drain. In the older units,
raised concrete barriers surround each unit and limit water flowing to
the segregated drains.
The segregated system handles approximately 2.3 million gallons of
wastewater each day (MGD). The principal contributors of wastewater are
crude storage tank water draws, desalters, sour water concentrators,
caustic oxidizers, and the Isomax unit. Not all of these processes
-------
Table 3-1. CRUDE THROUGHPUT DURING TEST PERIOD
Date
8-1-83
8-2-83
8-3-83
8-4-83
8-5-83
8-6-83
8-7-83
8-8-83
8-9-83
8-10-83
8-11-83
8-12-83
Crude throughput (b/cd)
181,600
183,500
183,300
178,800
177,600
183,900
184,700
170,400
116,800
182,300
172,100
Not available
3-2
-------
00
CO
Cooling Tower Rlowdown
Bolltr lloMdmin
Stora Runoff
12 API
Separator
Regeneration tutor from f 1 Nator trcater
Unsegregsted Sjrsteai
Desal ten
Stripper iottoM
Foul Hater Oxldlien
Tank Drawl
Oily hup Cooling Water
Barrel Hash
Other Segregated Hater
Tank
i Segregated Systea
Discharge
Effuent Treataent Plant (ETP)
Flash Mix Floe Dissolved Clarlflars Activated Eqoalliatlon
Tanks Tanks Air Flotation Sludge Tanks
I ianus ianus Air
Figure 3-1. General scheme of wastewater flow: Chevron Refinery - El Segundo, California.
-------
produce oily wastewaters. Wastewater from the oxidizers and concentrators
is directed to the segregated system because of high biological oxygen
demand (BOD) and not due to oil concentrations.
The main components of the segregated system are shown in Figure 3-1.t
The #4 API separator has a volume of 240,000 gallons of water and handles
an average flow of 1600 gallons per minute (gpm). Retention time for
wastewater in the separator is approximately 4 hours. The separator is
equipped with a concrete cover having caulked joints. Breather valves
protect the cover against excessive pressure or vacuum. Manholes provide
for visual inspection of the separator and oil skimming troughs are
adjusted manually to maximize oil removal. Actual skimming of the
separator is performed manually as needed by plant operators in charge
of maintaining all of the API separators. The #3 API separator has a
volume of 50,000 gallons and serves one section of the refinery as
described above.
Effluent from the #4 separator is pumped to a storage tank designated
T-190. This tank serves as an equalization tank for the ETP. The
effects of any sudden change in water quality or quantity can be minimized
by controlling the flow from T-190 to the ETP. T-190 is 35 feet high
with a diameter of 115 feet. Maximum capacity is approximately 2.5 million
gallons although normal capacity is roughly 60 percent of this. With an
average flow of 1600 gpm, retention times of 25 hours can be achieved.
The constant flow and water quality supplied to the ETP enhances the
effectiveness of the biological treatment processes.
From T-190, wastewater flow splits into dual treatment trains.
Each train contains a flash mix tank (T-200 and T-300), a flocculation
tank (T-201 and T-301), and a dissolved air flotation system (T-202
and T-302). Following the dissolved air flotation systems, the wastewater
« ....
converges into an equalization basin (T-500) and then again splits into
dual trains. Two activated sludge tanks (T-600 and T-700) and
two clarifiers (T-601 and T-701) complete the wastewater treatment steps
before the effluent is sent to the refinery forebay. Effluent from the
unsegregated system combines with effluent from the segregated system at
the forebay and the combined stream is discharged to Santa Monica Bay.
3-4
-------
The flash mix tanks are used for pH adjustment and polymer addition.
An acid tank, a caustic tank and a polymer tank feed both flash mixers.
At the time of the test, no chemicals were being mixed with the wastewater.
Chemical addition is usually used to improve the effectiveness of dissolved
air flotation. However, since Chevron was having no difficulty meeting
their effluent guidelines (as established by the National Pollution
Discharge Elimination System [NPDES] permit), the refinery did not feel
the additional cost of chemical addition was warranted. Chevron was
currently reevaluating the use of chemical addition.
The flocculation tanks following the mix tanks are designed to
provide adequate retention time so that the flocculation process can
function effectively. Retention times of up to 30 minutes are possible.
As with the mix tanks, wastewater was flowing through the tanks at the
time of the test but no function was being served.
The dissolved air flotation systems were manufactured by EIMCO
Envirotech and installed in 1974. Each tank is 52 feet in diameter and
11 feet high, not including the height of the cover. Nominal capacity
for the tank is 155,000 gallons. Only one DAF was in operation. Each
tank was provided with a fiberglass cover which rose vertically 5 feet
from the sides of the tank and covered the entire flotation chamber.
The cover had twenty-one 4 inch holes spaced around its side to allow
ventilation air to enter the DAF. There were also three access doors on
each cover, and a center hole in the cover for ventilation.
The air flotation process consisted of recycling a portion of the
treatment wastewater and saturating it with air. A 75 Hp pump was used
to recycle approximately 520 gpm of treated wastewater. A 10 Hp compressor
pressurized the saturated wastewater to approximately 60 to 80 psi.
Release of this pressurized stream into the flotation chamber at
atmospheric pressure produced the bubbles needed for flotation.
The skimmer mechanism in the DAF was operated intermittently. The
skimmer removed floating oil and suspended solids to a slop tank located
next to the DAF's. Usually the skimmer was operated less than one hour
per shift (3 shifts per day). The capacity of the slop tank was a
factor considered by the operators in determining use of the skimmer.
Oil and solids collected in the slop tank were removed periodically by a
vacuum truck and disposed at a landfarm operated by Chevron.
3-5
-------
As mentioned above, only one DAF was operating at the time of the
test. The operators manual for the ETP at Chevron stated that when one
treatment train was down, higher oil content may be expected in effluent
leaving the DAF. To compensate for this, it was recommended that the
polyelectrolyte dose be increased, feed to the DAF be minimized, and
excess oil entering the equalization tank be skimmed off by a vacuum
tank. Operators did not find it necessary to implement any of these
strategies while the second DAF was down.
Effluent from the DAF's converges into a single trunkline which
directs the wastewater to the equalization basin. The equalization
basin is a large, rectangular tank (116 feet x 160 feet) with a capacity
of 1.51 million gallons. Fifty-four static aerators are used to maintain
aerobic conditions in the wastewater. Normal air flow from the aerators
is 800 scfm. Under usual conditions, Chevron would expect little free
oil at this stage of treatment. If floating oil is present, it is
removed by vacuum trucks.
The principal purpose of the equalization basin is to maintain a
wastewater flow which is consistent in quantity and quality entering the
biological treatment system. Dual activated sludge tanks follow
equilization, each with a capacity of 900,000 gallons. Normal flow of
wastewater to each of the activated sludge tanks is 880 gpm (not including
recycle). Bio-oxidation takes place with the help of 230 static aerators
in each tank. Normal air flow is 5520 scfm. Maintenance of consistent
quantity and quality wastewater enhances bio-oxidation by providing a
stable environment where micro-organisms can thrive.
Following each activated sludge tank is a clarifier 80 feet in
diameter and 13 feet deep. Wastewater is introduced into the clarifier
through a center well 28 feet in diameter. Entrance through the center
well reduces the velocity of the influent and creates a quiescent stage
which allows for optimal settling of the solids. Polyelectrolyte can be
added to enhance settling but Chevron was not adding these chemicals
during the test period. Settled sludge in the clarifier contains micro-
organisms which are valuable to the activated sludge process. Therefore
some of the sludge is returned to the activated sludge tanks to maintain
effective bio-oxidation. Excess sludge is directed to sludge thickening
tank, the sludge digestor, and is then removed to the refinery landfarm.
3-6
-------
Finished water from the clarifier is sent to the refinery forebay
for discharge to Santa Monica Bay. The forebay is a large, buried tank
with a volume of 634,000 gallons. The average flow of effluent from the
forebay is 4500 gpm. Wastewater from both the segregated and unsegregated
systems is discharged at this point.
3.3 UNSEGREGATED SYSTEM
The unsegregated system is comprised of the #2 API separator and
the induced air flotation system (IAF). Four trunklines collect wastewater
from different sections of the refinery and empty into the separator.
The main contributors of wastewater to this system are cooling tower
blowdowns, boiler blowdowns, pump gland flushwater, and stormwater.
Overflow from the segregated system can also be directed to this separator.
The unsegregated system is also shown in Figure 3-1.
The #2 separator is the largest separator at Chevron with a capacity
of 2.05 million gallons. The normal flow of wastewater to this separator
is 3000 gpm. Nominal residence time is 11 hours but this varies
substantially due to short-circuiting of wastewater through the separator.
Actual residence time of 3-4 hours are more realistic. The separator is
divided into 5 sections; A, B, C, D, and E. Sections A, B, and C comprise
only one-third of the total separator volume but remove the majority of
the oil. From these sections, wastewater flows to section D and E
through port holes and under curtain walls. Outfall from sections D
and E enters a collection box where it is pumped to the IAF.
The #2 separator is completely covered with concrete panels. The
joints are caulked and breather valves protect the roof against excessive
vacuum or pressure. Any section of the separator can be taken out of
service for repairs. Diversion boxes on each trunk allow wastewater to
be diverted to the #4 separator should a major upset occur in the section
of the refinery served by the trunkline. During the test, wastewater
from one trunkline was being diverted to the segregated system.
The IAF was installed in 1981 as part of the refinery effluent
compliance plan. The unit is a WEMCO Model 144X capable of treating a
maximum of 5000 gpm of wastewater. At Chevron, average flow is
approximately 3000 gpm but fluctuations can result, particularly following
storms. An example of an IAF system is shown in Figure 3-2.
3-7
-------
CO
OD
Olly-Mttr
Influent
vtltt
FlMt (N'erfKt by fravlty tt «•*»
Figure 3-2. IAF system similar to that used at the Chevron Refinery - El Segundo, California.
-------
The IAF was installed to remove insoluble wastewater contaminants
such as oil, coke, catalyst fines, and precipitant metal. All forms of
unsegregated water flow to the IAF with the exception of effluent from
the #1 water treater which is low in insoluble contaminants. This
wastestream is mixed with the effluent from the IAF and sent to the
forebay for discharge.
Polyelectrolyte can be added to the IAF to enhance oil removal. By
design, this addition would be made only if effluent oil concentrations
were observed to be high. During the test period no chemical addition
was necessary.
Final disposal of all refinery wastewater is through the forebay.
As mentioned above, both segregated and unsegregated wastewaters converge
at this point. The forebay was constructed in 1958 and is a buried
concrete structure with a volume of 634,000 gallons. Average wastewater
flow is 4,500 gpm with the nominal residence time being approximately
2 hours. If required, final oil skimming is performed at the forebay
before discharge to the Santa Monica Bay.
3.4 WASTEWATER MONITORING SYSTEM
Chevron employs a wastewater monitoring system which is designed to
detect process upsets as quickly as possible. Numerous sample points
are located throughout the drain system and water from five primary
sample points is collected each shift. Samples are analyzed for
temperature, pH, sulfides, ammonia, phenols and oil concentration.
There is one primary sample point located in each trunkline of the drain
system. These sample points are designated SP-401 (segregated system),
SP-201, SP-202, SP-203, and SP-204 (unsegregated system). If samples
from any of the primary points exceed specification for a given parameter,
further samples are taken in the trunkline to isolate the source of the
upset. Remedial action to correct upsets may include diversion of an
unsegregated trunkline to the segregated system or an increase in residence
time for wastewater in tank T-190 preceding the ETP. Information acquired
through the sampling program is reported each shift in the effluent
turnover report.
3-9
-------
Operating parameters and wastewater characteristics are also recorded
for the various processes in the ETP and IAF systems. These are reported
in the turnover report along with the information mentioned above. This
allows Chevron to monitor NPDES compliance parameters on a regular
basis.
3.5 ODOR CONTROL SYSTEM
Since the Chevron refinery is located in a densely populated area,
efforts are made to control odorous air emissions. All facilities in
the wastewater system that handle oily wastewater are provided with
covers and in some cases, odor control devices are also used. Specific
odor control techniques for the wastewater system will be discussed
below.
3.5.1 IAF System
The WEMCO IAF is designed to be gas tight. There are eight access
doors located on the unit and each door is gasketed and can be tightly
sealed. Plant utility air can be introduced to the vapor space at the
effluent end of the IAF. By design, the pressure of the utility air
would be slightly greater than that found in the vapor space of the IAF.
This would allow clean air makeup to be continually fed to the unit
while accumulated hydrocarbons are forced out. The gaseous emissions
are directed to two 55-gallon drums of activated carbon. During the
test, only one drum was connected to the outlet pipe. The activated
carbon drums are supplied by Calgon and hold 150 Ibs of carbon. The
estimated life span of a drum is four to six months.
After installing the IAF, Chevron evaluated the effectiveness of
the odor control system. Because the hydrocarbon concentration in the
IAF remained well below the lower explosive limit the use of utility air
for purging was discontinued. This removed a potential source of odor
problems and decreased maintenance of the carbon drums.
Additional odor control devices were used on equipment associated
with the IAF. Activated carbon stacks were located on the roof of the
clarifier and oily sludge sump. The clarifiers received oil skimmings
and sludge from the IAF. Settled sludge was directed to sludge treatment
facilities and any floating oil was recycled to the #2 API. The carbon
stacks prevented any odors from being emitted from these tanks.
3-10
-------
3.5.2 Effluent Treating Plant
Extensive odor control measures have been taken by Chevron in the
ETP. The fuel tanks, flash mix tanks, and dissolved air flotation tanks
are all covered with vapors vented to an activated carbon bed. A diagram
of this system is shown in Figure 3-3.
The covers on the tanks in the ETP are not air tight but are provided
with ventilation holes. The cover of each flash mix tank has three 3-inch
diameter ventilation holes and 1 inspection door. The cover of each
flocculation tank has ten 3-inch ventilation holes and three inspection
doors. Further, the cover on each dissolved air flotation tank has 22
3-inch ventilation holes and three inspection doors. As shown in
Figure 3-3, each tank is connected to the vapor recovery system by
fiberglass reinforced piping. Two blowers (one operating, one 100 percent
spare) rated at 4000 cfm create a vacuum within the system which draws
VOC emissions and ventilation air from each tank. The approximate
amounts of air drawn from each tank are shown in the figure. Ventilation
air accounts for nearly 98 percent of the air flow to the carbon beds.
Before entering the carbon beds, air passes through demister pads
to remove excess moisture and a preheater which can raise the air
temperature 5-10°F. The preheater is a finned tube exchanger with plant
steam used as the heat source.
There are two activated carbon beds which receive vapors from the
flash mix, floe, and DAF tanks. Only one bed is on line at any time.
The dimension of each carbon bed is 12'xl2'x4' high. Activated carbon
particles range from 1/16 to 3/16 inches in size. By design, the expected
life of the activated carbon is four to five weeks. Carbon replacement
times vary, however, since breakthrough at the beds is determined by
odor detection. The primary purpose of the carbon beds is odor control,
and therefore, the beds are only changed if significant odors are detected
by the operators.
A similar odor control system is used on the equalization tank.
The equalization tank has 13 8-inch ventilation holes located on one
side of the basin. Eight outlet ports are located on the opposite side.
Fiberglass reinforced piping connects the outlet ports to dual activated
carbon beds identical to those described above. Two blowers (one operating,
one 100 percent spare) rated at 4000 cfm create a vacuum which draws
3-11
-------
4000 eta
Blower
DMlitor
Air Prthtator
CO
I
ro
Mil Carton
AdMrBtfOlll
Air Prthoator
Dnlitor
Flocctilatlon Tank
(400 eta)
Flaih HI* Tank Flocculatlon Tank
(200 eta) (400 eta)
4000 cfm
Blower
Total air flow to ifmtt ^
carbon a4*orttlon bH • 4000 eta
Figure 3-3.
Odor control system for DAF system. FRP = fiberglass reinforced pipe.
parenthesis indicate approximate air flow from each unit.)
(Numbers in
-------
vapors to the carbon beds. Operation of the carbon beds is the same as
that described above. Only one bed is on line at a given time and
carbon replacement is based on odor detection. The odor control system
for the equalization tank is shown in Figure 3-3.
3.5.3 Process Upsets During Test
Gaseous VOC emissions from the DAF and equalization tanks were
monitored during the test period. Monitoring ports were installed in
the fiberglass reinforced piping which carried the gaseous vents of
these tanks to the activated carbon beds. Gaseous emissions from the
floe tanks and flash mix tanks added a small quantity of flow to that
being drawn from the DAF. Only one DAF train was in operation during
the test. However, the blowers were still drawing flow from the DAF
train not in service. Flow measurements established that the out of
service train was having no effect on the flow of gases from the operating
DAF.
Process upsets could be monitored with the assistance of the
wastewater treatment plant operators at Chevron. Normal operating
practice called for process unit operators to inform the treatment plant
when an upset had occurred in the plant. An upset would include any
event which could potentially disrupt the biological treatment processes
or result in a failure to meet NPDES requirements. Examples of upsets
include excessive acidic or caustic wastewater entering the drain system,
or sudden surges of oily wastewater.
Due to the design of the effluent treating plant, most process
upsets are easily controlled. Tank T-190 serves to equalize the quantity
and quality of wastewater flowing to the ETP. Therefore, the influent
wastewater to the DAF remains relatively constant. A few minor process
irregularities were reported during the testing period but little, if
any, change was observed in the VOC concentration of the DAF vent.
Operational practices of the DAF did result in abrupt changes in
gaseous VOC emissions as recorded by the continuous monitoring equipment.
As discussed earlier, the skimmer mechanism was operated only
intermittently. Because of this, an oil film was allowed to build up on
the surface of the flotation chamber. This oil film acted to suppress
VOC emissions from the unit. When the skimmer was turned on, the oil
film was removed and VOC were released into the vapor space of the
3-13
-------
flotation chamber. The continuous monitoring equipment recorded a
sudden increase in VOC concentration which gradually reached a maximum
level. When the skimmer was shut down, VOC concentrations returned to
the level observed before skimming.
Tables 3-2 and 3-3 summarize the major parameters characterizing
wastewater flow to and from the DAF and IAF systems. The data given
were acquired from the refinery effluent turnover reports compiled
during each shift by Chevron operators. For the DAF (Table 3-2),
fluctuations in influent waste quantity, temperature, pH, and oil
concentration was observed. The quantity of wastewater flowing to the
DAF varied from 1400 gpm to 2000 gpm. Temperature of the influent
wastewater ranged from 72°F to 96°F while pH valued ranged from 8.1
to 10.8. In most cases, the changes in these parameters were gradual
over time. These fluctuations had little effect on the VOC concentrations
recorded by the continuous monitoring equipment.
Influent oil concentrations exhibited a wide range. The lowest
concentration recorded was 47 mg/1 and the highest concentration was
420 mg/1. The fact that measurements for oil concentration are
instantaneous measurements could account for the wide range observed.
Table 3-3 summarizes the parameters characterizing wastewater flow
to and from the IAF. Influent flow rates ranged from 800 gpm to 3780 gpm.
The recording device that measures flow to the IAF was malfunctioning
during the test and the flow rates given are based on the estimated
effluent from the #2 API separator. Wastewater temperatures ranged
from 90°F to 106°F. This temperature range is higher than that for DAF.
The DAF inlet temperatures would be expected to be lower because of the
effect of Tank T-190 which acts as a holding tank.
Influent oil concentrations to the IAF ranged from 12 mg/1 to
60 mg/1. These low concentrations would be expected since the IAF
handles relatively non-oily wastewater. As with the concentration
observed in the DAF influent, the range of concentrations observed may
be due in part to sampling techniques.
3-14
-------
Table 3-2. SUMMARY OF REFINERY EFFLUENT SYSTEM TURNOVER - DISSOLVED AIR FLOTATION SYSTEM
u>
tt
Oitl
7-25
7-26
7-27
7-28
7-29
7-30
7-31
8-1
8-2
8-3
8-4
Shift
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
, 3
1
2
3
1
2
3
1
2
3
1
2
3
f4 API
•f fluent oil
(•g/i)
220
240
98
120
290
79
210
...
48
110
240
200
300
270
260
...
71
220
210
93
210
320
125
260
160
210
120
120
175
90
130
260
100
DAF
Influent GPM
1600
2800
1800
1800
1900
1800
1900
1800
2000
1900
1600
1600
1500
1600
1600
...
2000
2000
2000
2000
1800
1800
1900
2000
1600
1800
1800
1900
1900
2000
1900
2000
2000
°F
92
93
88
87
92
86
87
92
88
88
93
75
89
95
75
...
90
91
91
95
75
89
94
90
88
93
88
88
93
87
90
75
88
pH
8.6
8.9
9.3
9.2
9.3
9.6
9.2
9.2
9.3
9.3
9.6
9.5
9.4
9.8
9.9
...
8.9
8.7
8.6
8.6
8.5
8.9
8.9
8.8
8.8
9.4
9.9
9.4
9.4
9.5
9.1
10.1
10.8
DAF
Influent oil
(ma/7)
410
205
190
213
175
180
100
160
260
200
240
250
300
250
310
...
110
240
260
180
260
180
190
180
47
280
320
120
210
260
140
330
76
DAF
if fluent oil
(•8/D
115
110
90
135
110
110
15
110
30
20
95
50
60
20
200
—
40
150
140
80
150
85
88
94
43
95
78
29
0
38
54
210
50
Recycle
rate (GPH)
530
525
530
540
530
540
540
540
520
530
530
550
530
530
550
540
540
540
...
550
520
540
530
520
530
530
520
530
530
520
525
520
Dissolved «1r
(C01)
1.5
1.5
1.6
1.3
1.5
1.6
1.3
1.5
1.8
1.5
1.5
1.5
1.4
1.5
1.5
1.6
1.7
1.7
...
1.5
1.5
1.6
1.5
1.5
1.6
1.5
1.5
1.6
1.5
1.5 •
1.5
1.5
(continued)
-------
Table 3-2. Concluded
Date
8-5
8-6
8-7
8-8
8-9
8-10
8-11
Shift
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
14 API
effluent oil
(»g/l)
130
200
90
180
280
110
100
260
83
89
180
180
120
120
—
68
240
200
160
270
DAF
Influent GPM
1900
1900
2000
2000
2000
2000
2000
2000
1600
1600
1600
1400
1400
1600
1800
1800
1800
1800
1800
2000
°F
90
78
85
94
78
85
96
75
92
95
72
91
95
88
89
94
87
91
75
89
pH
9.0
9.0
9.3
9.0
8.6
8.6
8.3
8.1
8.3
8.3
8.2
9.0
8.5
8.2
8.4
8.5
8.5
8.6
9.1
8.8
OAF
Influent oil
(mg/1)
86
190
106
150
220
94
180
210
260
140
190
100
120
400
290
130
55
57
70
420
OAF
•f fluent oil
(mg/1)
19
100
31
71
110
42
88
160
110
110
100
34
44
68
50
64
24
23
65
31
Recycle
rate (GPH)
520
525
520
530
525
530
530
525
530
530
525
520
520
530
510
S20
510
520
525
520
dissolved air
(CFM)
1.5
1.5
1.5
1.6
1.5
1.5
1.6
1.5
1.6
1.6
1.5
1.5
1.6
1.6
1.5
1.6
1.5
1.5
1.5
1.4
-------
Table 3-3. SUMMARY OF REFINERY EFFLUENT SYSTEM TURNOVER—INDUCED AIR FLOTATION SYSTEM
CO
I
Date
7-25
7-26
7-27
7-28
7-29
7-30
7-31
Shift
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
#2 API effluent
(IAF feed - GPM)
800
2520
2200
3060
2900
2600
2180
2200
2400
1700
2480
3140
3380
3600
2320
___
3040
2400
4080
2800
2600
°F
90
106
94
104
102
95
100
102
96
100
98
96
101
102
104
___
107
102
100
100
99
IAF influent oil
(mg/1)
21
25
19
26
22
30
50
20
30
60
30
___
30
—
28
—
22
25
21
—
22
IAF effluent oil
(mg/1)
«..*•
8
10
___
16
10
20
5
10
5
0
10
5
—
18
—
10
16
16
—
15
(continued)
-------
Table 3-3. Continued
#2 API effluent
Date Shift (IAF feed - GPM)
CO
I—"
00
IAF influent oil
(mg/1)
IAF effluent oil
(mg/1)
8-1
8-2
8-3
8-4
8-5
8-6
8-7
8-8
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
2840
—
2400
2960
2600
2680
2500
2780
2320
2260
2480
___
2900
2740
2000
2880
3600
3200
2160
2800
2560
2400
2400
2600
100
96
100
99
97
97
98
98
97
98
99
95
98
99
98
98
98
94
95
95
95
96
94
92
22
18
___
25
24
18
20
21
18
22
25
20
24
24
18
31
25
12
23
24
19
13
—
30
8
9
18
19
10
12
0
9
14
12
19
14
12
17
10
9
16
7
9
_-_
7
8
11
18
(continued)
-------
Table 3-3. Concluded
#2 API effluent
Date Shift (IAF feed - GPM)
co
i—"
UD
IAF influent oil
(mg/1)
IAF effluent oil
(mg/1)
8-9
8-10
8-11
1
2
3
1
2
3
1
2
3
1800
2400
2360
2200
2600
2200
2200
1280
M — •»
93
90
94
96
96
100
100
96
_ _ ••
21
18
24
20
29
28
25
25
...
7
12
15
10
17
14
17
8
""
-------
4. LOCATION OF SAMPLE POINTS
The gaseous and water sampling locations during testing at the
Effluent Treatment Plant serving the segregated waste waters are shown
in Figures 4-1 and 4-3.
The sample location for the combined ventilation air from the
dissolved air flotaton unit was located in a horizontal run of nominal
18-inch fiberglass pipe. The pipe was fitted with two 1-inch ports
at 90° orientation for velocity traverses. The ports were located more
than eight pipe diameters downstream and more than two diameters upstream
of a disturbance. The location of velocity measurement points in the
flow crossection at this site are shown in Figure 4-2. The duct was
also equipped with a separate one-inch port within one foot of the flow
measurement plane for access for collection of gaseous samples.
The test locations for estimating the flow contribution to the
total ventilation air from the DAF tank, the flocculation tank, and the
mix tank were located in horizontal runs of fiberglass pipe. Access to
the flow stream was through ^rinch fittings installed as pressure taps
for process flow meters. These locations were usually near bends in the
duct work and were not ideal flow measurement sites. The gas velocity
was measured at a "typical" or average point in the crossection. Gas
samples were extracted through the same fittings.
The test site for the ventilation air from the equilization tank
was in a horizontal run of 24-inch fiberglass pipe. Two ports at 90°
orientation were installed for velocity measurement at a location more
than two diameters upstream of a disturbances. The points on the area
crossection used for velocity measurements are shown in Figure 4-4.
The water sampling sites during these tests were the influent and
effluent of the DAF system, the effluent from the equilization tank and
the #4 API separator forebay. The DAF influent was obtained from a
sampling tap installed in the feed line from T-190 to the T-200 mix
-------
-p.
ro
UASTEHATER INFLUENT SAMPLE
\
\
X
.— EFFLUEI
/ V-200 \.J
1 WEE?
j AIR SATURATION IT
V VESSEL 7
1
HATER
i.
LEO
DISSOLVED AIR FLOTATION TANK
DAF SAMPLING LOCATION
I. 0. FAN
CARBON HOUSE
V-204
V-304
x- Flow and composit screening test sites
OUTLET TEST LOCATION
Figure 4-1. Dissolved air flotation treatment system at Chevron Refinery -
El Segundo, California.
-------
DAF OUTLET
Port A
Port B
17.5" diameter
Traverse Point Number
1
2
3
4
5
6
Distance from Sample Port, Inches
0.7
2.5
5.2
12.3 -
14.9
16.7
Figure 4-2. DAF outlet sample location with traverse points.
4-3
-------
s
•if
i.irm
^.•.w.
<*X tttttt
OOMTIMQUS,
MWlItt
UttTIM
OPUTOMV1CKT
TMK
EFFLUENT HATER SAMPLE
MMMICN. nunar vm
ubbbfefefefefe
Figure 4-3. Equalization tank system *t Chevron Refinery - El Segundo, California.
-------
EQUALIZATION TANK OUTLET
Port A
Port B
23.25" diameter
Traverse Point Number
1
2
3
4
5
6
Distance from Sample Port. Inches
1.0
3.4
6.9
16.4
19.8
22.2
Figure 4-4. Equalization tank outlet sample location
with traverse points.
4-5
-------
rVW
rROM PROCESS DRAINS
^^^^^^^W
*
nraueto AIR FLOTATION UNIT
r© <—
ANEMOMETER
FLW MEASUR0CNT ADAPTATION
.11 j
jt r T r
flUTUT^ 1
1
1
1
4
J
\
\
«B^B^
^~
IAF Si
1
>t
J
J
NMPL
J
CARSON DRUM
MOBILE LABOMTWT
Figure 4-5. IAF treatment system at Chevron Refinery - El Segundo, California.
-------
tank. The DAF effluent sample was obtained from a sampling tap in the
recycle pump discharge. The equalization basin effluent and API influent
samples were obtained by dipping a grab sample from the overflow sump
and forebay, respectively.
The sampling location after the carbon absorption control devices
was at the exit crossection to the atmosphere. The carbon house exhausts
through a rectangular opening on the roof of the building. The sample
collection probe was positioned near the center of the opening, or at
the downwind portion if prevailing wind conditions caused turbulence at
the leading edge.
The sample location for measurement of ventilation air from the IAF
was at the vent line to the carbon drums. This line was a two-inch
plastic pipe. The total flow in this line was routed through a volume
measurement meter. Samples for determination of gaseous components were
extracted through a ^-inch hole in the meter housing duct.
Influent and effluent water samples were collected from the sampling
stations used by Chevron at the IAF inlet and outlet. Water samples at
the #2 API separator were collected at three separate forebays by dipping
a grab sample.
4-7
-------
5. SAMPLING AND ANALYTICAL PROCEDURES
The sampling and analytical procedures used to evaluate the gaseous
and liquid streams are presented in this section. The methodologies are
discussed separately as gaseous VOC methods (5.1), fixed gas analysis (5.2),
gas flow measurement (5.3), liquid sampling (5.4), and liguid sample
analysis (5.5).
5.1 GASEOUS VOC METHODS
Two procedures were used to measure the VOC content of the gaseous
streams. EPA Method 18 was used to determine the general VOC species in
the samples, and a procedure similiar to EPA Method 25A was used to
measure the equivalent total hydrocarbon content of the streams.
5.1.1 EPA Method 18
"EPA Method 18. Measurement of Gaseous Organic Compound Emissions
by Gas Chromotography", (promulgated October 18, 1983, Federal Register
48 FR 48328) was used to characterize the organic components in the
streams tested. Samples were collected using the integrated bag technique
of Method 18. Figure 5-1 illustrates the apparatus.
A clean 2.5 cubic foot TEDLAR® flexible bag was used for each run.
The bags were cleaned by filling with dry nitrogen and venting the bag
contents to the atmosphere until no background organics were detected by
the analysis system. Prior to sampling the sampling apparatus and
flexible bag were leak checked by evacuating each to 29" Hg vacuum and
monitoring the pressure for 10 minutes. If a change of less than 1" Hg
is observed, the components are judged leak-free. The sample probe,
sample connecting tubing, and the sample bag were operated at ambient
temperature. To prepare for sampling the vacuum source can was evacuated
to -29" Hg. The system was then assembled and the sample probe was
placed near the centroid of the duct to be sampled. Sampling was
-------
Probe
5' Teflon Tubing
Pinch Clamp
en
Grommet
A1r Tight Steel Drum
Sample Bag
PVC Tubing
Directional
Needle Valve
Quick Disconnectors
Evacuated Steel
Drum
Figure 5-1. Gas bag sampling system.
-------
started by opening the flow control valve and was maintained at a constant
rate using the rotameter for about one hour. At the end of the sampling
period, the flow valve was closed, the probe was disconnected, and the
bag inlet was sealed. The sample bag was transported to the on-site
mobile laboratory for analysis.
Two gas chromatograph systems with flame ionization detectors were
used to analyze each sample. One system was used to separate and quantify
low molecular weight parafins and olefins while the other system was
used to measure aromatics and higher molecular weight components.
The system used to measure low molecular weight compounds (termed
Cj-Cs components) was a Shimadzu GC Mini 1 with a Shimadzu Chromatopac
digital integrator/recorder. The operating parameters were:
• Column: 6 ft x 1/8 in. I.D. stainless steel.
• Column support: Poracil C.
• Column temperature/program: 35°C/constant.
• Sample loop size/temperature: 1 ml/ambient.
• Carrier gas/flow: He/50 ml/min.
A calibration gas mixture containing known concentrations of methane,
(15.1 ppm) ethane (14.6 ppm), propane (15.6 ppm), butane (15.2 ppm), and
pentane (15.6 ppm) in nitrogen was used to obtain a area factor and
retention time for each of these compounds. Figure 5-2 presents an
example of a GC/FID calibration run for C:-C5 speciation. During sample
analysis, the peaks near these retention times were grouped as the
nearest carbon number, and the concentration was calculated using the
corresponding calibration factor for that carbon number. Figures 5-3
to 5-5 present examples of GC/FID analysis runs for Cj-Cs speciation at
each sample location.
The GC/FID analysis example run for Ct-C5 speciation (Figure 5-4)
provides an illustration of problems with inconsistencies in the analytical
procedures. Standards were not available to provide elution time standards
for the 18 peaks identified by the GC/FID with areas. Therefore, the
total organic concentration from the analysis was a sum of all the peaks
and not just the identified peaks. Another problem was the slight
variance of the elution time during the test day. The operator justified
5-3
-------
START 88.94.19.49.
1.99
4.93
C-Rlfl
SMPL »
FILE •
REPT t
METHOD
ee
7
31
44
N
1
2
3
6
NRHE
METH
ETHft
PROP
HEXA
TIME
e.4i
8.57
8.94
1.99
4.93
11.1
11.36
11.51
11. B6
12.91
19.83
CONC
e
e
e
HK
V
V
V
TOTAL
e
e
AREA
867
632
957
1292
1461
71
164
138
147
1738
281
7647
Figure 5-2. Example of GC/FID calibration for
speciation.
5-4
-------
DRF-392-2
STftRT 98.94.15.18.
r
r
8.58 '
9.95
1.7
2.91
4.26
5.
11.18
12.86
STOP
C-Rlfl
SMPL #
FILE *
REPT *
METHOD
99
7
39
44
*
1
2
3
HflME
METH
ETHft
PROP
TIME
8.42
9.58
8.95
1.7
2.01
4.26
5.
11.18
12.06
TOTftL
CONC
0
9
0
MK
V
V
V
V
fiRER
2668
244
389
139
339
823
379
158
225
5358
Figure 5-3. Example of GC/FID analysis on DAF ventilation air
gas bag sample for Ci-Cs speciation.
-------
IftF-IH
STftRT 88.12.13.62.
0.38
12.59
STOP
C-R1R
SHPL t
FILE t
REPT »
HETHOD
tt
1
2
ee
7
189
44
NBME
HETH
ETHfl
PENT
PENT
HEXR
TIME
8.38
8.52
8.85
1.2
1.55
1.85
2.93
3.3
3.95
4.65
5.27
6.69
6.99
7.95
18.32
11.32
12.59
14.79
CONC
8
8
TOTBL
HK
T
T
T
T
TV
RRER
119387 -c/
584- €>•
1864- «•>
78
2214
8467-M
278
68
69883 ,
69964 - *•
26865
394
31
9734
142835
194984 ,_
183987- t,
1475
832124
Figure 5-4. Example of GC/FID analysis on IAF ventilation air
gas bag sample for Ci-Cg speciation.
5-6
-------
E8-2
STftRT 88.84.16.17.
0.41
0.58
8.93
E&-2
STOP
C-R1R
SMPL *
FILE *
REPT t
HETHOD
1
2
3
88
7
32
44
NRME TIME
METH 8.41
ETHft 8.58
PROP 8.93
TOTflL
COHC
8
8
8
8
MK
T
fiRER
1491
12
27
1531
Figure 5-5. Example of GC/FID analysis on equalization tank
gas bag #2 sample for Ci-Cs speciation.
5-7
-------
the difference from the Chromatopac peak labels and the operator notes
(see Figure 5-4) as the temperature differential in the field laboratory
across a test day.
The system used to measure aromatic and higher molecular weight
compounds (termed semi-volatile) was a Shimadzu GC Mini II equipped with
a Shimadzu Chromatopac integrator. The operating parameters were:
• Column: 6 ft x 1/8 in. I.D. stainless steel.
t Column support: OV-1 on 80/100 Supelco.
• Column temperature/program: 25°C/constant.
• Sample loop size/temperature: 1 ml/225°C.
• Carrier gas/flow: He/20 ml/min.
A calibration mixture of 49.8 ppm benzene and 49.9 ppm m-xylene in
nitrogen was used to determine calibration factors and retention times
for these two compounds. Qualitative gaseous standards were prepared
from liquid hexane, heptane and toluene were used to determine the
retention time for these compounds. Figure 5-6 presents an example of a
GC/FID calibration run for C6-C9 speciation. During sample analysis,
hexane, heptane, benzene and toluene were expressed as equivalent benzene
concentrations and C8 and higher components were expressed as m-xylene
equivalent concentrations. Figures 5-7 to 5-9 present examples of
GC/FID analysis runs for C6-C9 speciation at each sample location.
5.1.2 EPA Method 25A
Procedures similiar to those described in EPA Method 25A (Federal
Register 48 FR 37595) were used to continuously measure the total
hydrocarbon concentration in the gaseous streams tested. Two Beckman
Model 400 and one Beckman Model 402 flame ionization analyzers were used
at the respective sample locations. The sample probes were placed near
the centroid of the duct to be sampled. A continuous sample flow was
maintained through heated Teflon® sampling lines. The instrument operating
parameters were:
Site: DAF ventilation and carbon house
• Analyzer: Beckman Model 400.
• Serial #: 100216 and 1001826.
5-8
-------
CRL
5TRR7 08.94.15.56.
STOP
C-Rlfl
SWPL f
FILE •
REPT t
METHOD
1
3
88
2
138
44
NRHE TIME
C1-C5 8.75
BENZ 1.31
6 -II XVL 3.57
TOTRL
COHC
8
8
8
8
RKEfl
6515
7935
18798
25249
Figure 5-6. Example of GC/FID calibration for C6-C9 speciation.
5-9
-------
DBF-382-2
START 08.84.13.16.
6.31
8.11
9.33
STOP
SMPL t
FILE t
REPT t
METHOD
*
1
2
3
4
3
88
2
128
44
NRHE
C1-C3
HEXfl
BENZ
HEPT
TOLU
6 -M XVL
7
ODXVL
TIME
8.76
1.86
1.32
1.47
1.76
2.82
2.51
2.83
3.13
3.58
4.13
4.71
5.13
6.51
8.11
9.33
TOTflL
CONC
0
8
0
0
0
0
0
V
V
V
V
V
V
V
V
V
V
V
V
flREfl
10824
2335
2876
1061
1498
5242
466
731
321
1642
635
281
31
115
192
71
27342
Figure 5-7. Example of GC/FID analysis on DAF ventilation air
gas bag sample for C6-C9 speciation.
5-10
-------
1RF-IN-2RRNGE1E2 ..
STRRT 88.11.16.54.^
8.41
11.18
'STOP
r-PiR
SMPL t
FILE t
REPT •
METHOD
t
1
88
2
208
44
3
4
NRME
C1-C3
HEXR
BENZ
HEPT
6 -tl XVL
7 ODXVL
TIME
8.76
B.9
1.84
1.19
1.36
1.65
1.92
2.34
2.85
3.28
3.81
4.26
4.66
5.88
5.38
5.83
-6.55
CONC
8
8
8
8
8
" .'•' 11.18
-,--- r TOTflL -
MX
V
V
V
V
V
V
V
V
V
V
V
V
V
V
V
V
V
V
V
1.92
RRER
12853
17628
61568
11532
41149
14933
16229
6116
5684
8173
2827
2411
738
1342
1754
869
1875
1682
1854
654
218114
Figure 5-8. Example of GC/FID analysis on IAF ventilation air
gas bag sample for C6-C9 speciation.
5-11
-------
EQ-2
STflRT
98.84.16.32.
STOP
C-Rlfl
SMPL
FILE
REPT
. *
: t
r t
IOD
»
1
2
3
3
88
2
132
44
NRME
C1-C3
HEXft
BENZ
TOLU
TIME
8.73
1.86
1.29
1.73
1.98
2.75
3.48
4.81
TOTflL
CONC
8
8
8
8
8
MK
V
V
BRER
6197
331
781
763
2171
233
333
146
11881
Figure 5-9. Example of GC/FID analysis on equalization tank #2
gas bag sample for C6-C9 speciation.
5-12
-------
• Fuel Pressure: 22 PSI.
• Sample Pressure: 3.0 PSI.
• Air Pressure: 15 PSI.
• Sample line length/approximate temperature: 25 feet/ambient.
Site: Equalization tank and carbon house
• Analyzer: Beckman Model 402.
t Serial #: 1001303.
• Fuel Pressure: 25 PSI.
• Sample Pressure: 3.0 PSI.
• Air Pressure: 16 PSI.
• Sample line length/approximate temperature: 25 feet/ambient.
Site: IAF ventilation air and carbon drum
• Analyzer: Beckman Model 402.
• Serial #: 1001303.
• Fuel Pressure: 25 PSI.
• Sample Pressure: 3.0 PSI.
• Air Pressure: 16 PSI.
t Sample line length/approximate temperature: 25 feet/ambient.
The sampling period varied among the separate sites tested. However,
during the duration of sampling at a site, the analyzer were operated
continuously 24-hours per day. The analyzers were equipped with strip
chart recorders for data reduction. The instruments were calibrated
with compressed gas standards of propane in a balance of air.
The calibration gas standards were supplied by Scott Speciality
Gases and certified to within ±2 percent of the labeled calibration gas
values. The calibration gas standards used at Chevron are, listed in
ppm as propane: 49.9, 100.1, 500.5, 1002.5, and 4010.1.
The initial calibration prior to commencing a test series at a test
location, or follow-up calibration prior to re-commencing a test series
5-13
-------
after an instrument shut-down, included the following calibration sequence.
First a trial sampling of the source stream would indicate the appropriate
concentration range for which the instrument would be operated. Second,
the initial calibration of the instrument on this pre-determined scale
included introducing zero gas and the high-level calibration gas separately
to the sample manifold. The output was then adjusted to the appropriate
levels. No instrument adjustments were made after this time. Third, a
periodic response check was performed by introducing the zero and high
level calibration gas with no adjustments. A response within ±1 percent
of span value was required or recalibration would have been performed.
Fourth, a linearity check was performed on the instrument span range by
introducing mid-level and low-level calibration gases. The difference
between the measurement system responses and the predicted response were
recorded. The differences were assured to be less than five percent of
the respective calibration gas values before the measurement system was
placed on-line for monitoring. Table 5-1 lists the operational parameters
and calibration gas standards used at each sample location.
A monitor system response time check was performed at each sample
location. The check was performed by introducing the high-level
calibration gas at the inlet to the sample line feeding the measurement
system. The time interval was measured for the analyzer to respond by
95 percent of the calibration gas value. The short sample lines gave
response times of 15-17 seconds within the allowed limit of 30 seconds.
Zero and span drift determinations were made during and after each
test period. The frequency of drift checks were determined by the
operational status of the analyzer and total length of the test. During
the initial operation of the analyzer, after the measurement system had
been powered down, the FIA required frequent drift checks (one to
two hours) for maintaining the drift values below the specified
three percent limit. A complete calibration sequence was completed if a
drift check demonstrated the necessity. After the frequent drift checks
verified the calibration stability of the measurement system, the drift
checks were performed three times during the 12-hour test day period
(0600, 1200, 1800). Test periods of less than 12-hour periods required
the two-hour drift check frequency.
5-14
-------
Table 5-1. CONTINUOUS MONITOR CALIBRATION GASES
CJl
I
en
Sample location
DAF Ventilation Air
DAF Carbon House Exhaust
IAF Ventilation Air
IAF Carbon Drum
Equalization Tank
Ventilation Air
Equalization Tank Carbon
House
Instrument
Beckman 400
Beckman 400
Beckman 402
Beckman 402
Beckman 402
Beckman 402
Scale
(ppm)
0-1000
0-100
0-10,000
0-10,000
0-1000
0-1000
Calibration gas
(low)
100.1
NA
500.5
500.5
100.1
100.1
(mid)
ppmv as (
. 500.5
49.9
1002.1
1002.1
500.5
500.5
levels
(high)
* u
'3^8
1002.5
100.1
4010.0
4010.0
1002.5
1002.5
NA = Not available.
-------
Figure 5-10 presents an example of a calibration check at the DAF
sampling location with a recalibration required. The sequence was
initiated at 0800 on 8/4/83 by introducing zero, high, and mid-calibration
gases separately. The upward drift at the three levels was approximately
one percent. Therefore, the zero and high standards were re-introduced
and analyzer adjustments made. Next, a linearity check is performed
with the mid standard (no adjustment) and the sample reconnected for
monitoring.
The calibration gas level reintroduced for the drift check was
determined by the sample measurement levels. The DAF sample locations
ranged from 600-1000 ppm and the 1002.5 ppmv as C3H8 was used for the
span drift check; the IAF sample locations ranged from 6000-7500 ppm and
the 4010.0 ppmv as C3H8 was used. The equalization tank sample locations
ranged from 100-200 ppm and the 100.1 ppmv as C3H8 was used.
The continuous monitor data were reduced by determining the average
organic concentration measured into ppmv as propane. Direct computation
of the recorded stripchart outputs was applicable because the high-level
calibration was equivalent to 100 percent of the recorder span value.
The exception was the IAF measurement system calibrated on the 0-10,000 ppm
scale. The IAF calibration was performed with 40 percent of scale being
equivalent to the 4010 ppmv as propane.
The measured concentrations are presented on a ppmv as propane
equivalent. The one-hour concentration averages were calculated from
direct output readings at five-minute intervals. The results were
calculated on the hour; therefore, periods with drift checks and
calibration were averaged to the hour from the partial measurements.
5.2 PERMANENT GAS ANALYSIS
A gas chromatograph equipped with a thermal conductivity detector
was used to analyze each bag sample collected for VOC analysis to determine
the nitrogen, oxygen, and carbon dioxide content. This procedure was
intended to characterize the balance gas constituents and is allowed in
Section 1.2 of EPA Method 3 (42 FR 41768) for this purpose.
The chromatograph used was a Shimadzu GC-3BT with a Shimadzu
Chromotopac integrator. The operating parameters were:
5-16
-------
Figure 5-10. Example of a calibration check with
a recalibration required.
5-17
-------
• Column: 6 ft x 1/8 in. I.D. stainless steel.
• Column support: 60/80 molecular sieve.
• Column temperature/program: 105°C/constant.
• Sample loop size/temperature: 2 ml/35°C.
• Carrier gas/pressure: He/3 PSI.
The chromatograph was calibrated with a cylinder standard of Scotty II-Mix
containing (by volume) 14.8 percent C02, 7.07 percent 02, 78.13 percent
N2 with a ±2 percent certification. Figure 5-11 provides an example of
GC/TCD calibration and Figure 5-12 provides an example of a GC/TCD
analysis run for the balance gas constituents.
5.3 GASEOUS VOLUMETRIC FLOW MEASUREMENT
Two procedures were used to measure the gaseous flow rate at the
sample sites, depending on the flow rate and system configuration. At
the DAF tank vents and the equalization tank vent, EPA Methods 1, 2,
and 3 were used to determine the volumetric flow rates using a pitot
tube. The measurement location were ideal as defined by Method 1 and no
problems were encountered during testing. Measurement was performed in
the morning and afternoon of each day of testing and the two measurements
were averaged for a daily value.
At the induced air flotation unit vent a modification of EPA Method 2A
(Federal Register Vol. 48, No. 247, December 22, 1983) was used. The
flow rate at this site was small and variable and the allowable back-
pressure allowed on the IAF unit was essentially zero. Unsuccessful
attempts were made to used a turbine-type meter with a 9000 cubic foot
per hour rating. The system that proved useable was a fabricated meter
based on a 4" diameter aneometer housed in a section of duct with the
same nominal diameter as the aneometer:
A Jewelled Anemometer was used at the IAF sample location for
measuring the velocity through a four-inch adaption between the IAF
ventilation air and the carbon drum inlet. Figure 5-13 provides a
schematic representation of the velocity measurement system.
The anemometer was calibrated by the manufacturer (Davis Instrument
Mfg.) and the calibration/correction data is provided in Appendix A. No
in-house calibration was performed since this was the first use of the
anemometer.
5-18
-------
CflL
STflRF
68.64.16.18.
0.55
STOP
C-R1R
SMPL *
FILE *
REPT *
METHOD
*
1
2
3
4
09
4
1486
44
NflME TIME
RIR 0.55
CO-2 1 . 3
0-2 1 . 95
N-2 2.6
TOTRL
COMC
92.3258
14.9985
6.6363
73.2655
186.2362
MIC
RREft
52856
10832
3915
42487
189293
CflLIB -
C-R1R
5MPL *
FILE *
REPT *
METHOD
CLB Cl
W
1
2
3
4
ID TBL
MRX
MODE
00
4
1487
44
1
NflME TIME
RIR 0.55
CO-2 1.3
0-2 1 . 95
N-2 2.6
TOTflL
4
5
1
1
2
3
4
CONC
0
flRER
52856
19832
3915
42487
189293
NflME TIME WINDOW
RIR
CO-2
0-2
N-2
0.55
1.26
1.95
2.56
10
F1/F2
0.901892
0.901475
0.901895
0.991839
C1/C2
180
14.8
7.97
78.13
Figure 5-11. Example of GC/TCD calibration for stationary gas analysis.
5-19
-------
EQ-2
5TflRT
68.84.16.36,
C-R1R
SMPL *
FILE *
REPT *
METHOD
1
3
4
STOP
ee
4
1498
44
NflME TIME
flIR 8.55
0-2 1.92
N-2 2.59
TOTflL
8.55
2.59
CONC
116.9525
78.2411
216.7821
ftREfl
61818
11913
42549
116288
Figure 5-12.
Example of GC/TCD analysis on equalization tank #2
gas bag sample for stationary gases.
5-20
-------
in
CQ
c
re
01
H
u>
w <
• o
n.
o -••
O (D
3 0>
)
I C
m r*
to
c tf>
O r*
• (D
3
O
0> 0>
— ' Q.
_i. 0)
O c*
-i m
•3 Q.
_J<
Q) *J*
• 3
INDUCED AIR FLOTATION SYSTEM
n>
•=>
OJ
c+
O*
-------
The operation of the IAF unit was that it flucculated in flow rate
and direction. For limited intervals during the test period, the meter
was monitored and dial readings were taken at each flow reversal point,
along with the time. The positive flows were accumulated for the test
period, and an average equivalent flow rate was calculated. This
equivalent flow was used to calculate a VOC mass flow rate only for
those periods of actual flow determination because of the variability of
the flow.
5.4 LIQUID SAMPLE METHODS
Liquid process samples were collected from sample taps used by the
refinery for process quality control. Two types of samples were collected
and were termed "void of air" (VOA) and "composite".
The void of air samples were collected by completely filling a
40 mL bottle with a grab sample. These bottles are fitted with a special
cap to eliminate air bubbles from the sample. The composite samples
were collected by cummulatively combining three to four equal volume
grab samples into a one gallon amber bottle.
Both sample types were taken from a process stream flowing in a
pipe, through a sample line which was purged prior to sample collection.
The samples were stored on ice in insulated containers after collecting,
and during shipment to the TRW facility at the Research Triangle Park,
North Carolina for analysis. The bottles were prepared by the following
cleaning procedures.
5.5 LIQUID SAMPLE ANALYSIS METHODS
5.5.1 Total Organic Carbon (TOG)
This method is applicable to the measurement of organic carbon in
drinking and surface waters as well as domestic and industrial wastes.
5.5.1.1 Summary of Method. Organic carbon in a sample is converted
to carbon dioxide (C02) by photochemical oxidation. The C02 is measured
to determine the total organic carbon. The sample is initially purged
by vacuum to remove inorganic carbon. Sample inorganic carbon is
eliminated or must be compensated for because it is usually a large part
of the total carbon. The instrument is calibrated versus a standard
solution of potassium hydrogen phthalate (KHP).
5-22
-------
5.5.1.2 Interferences/Qua!ity Control. Removal of carbonate and
bicarbonate by acidification and purging with nitrogen or-other inert
gas can result in the loss of volatile organic substances. Volatiles
also can be lost if the samples are allowed to heat up.
Repeatability of replicate injections can be effected by non-
homogeneity of samples. This can occur if large carbon containing
particulate matter is not representatively collected in the sample
injection syringe. It is also necessary to collect and maintain the
samples in bottles with no head space so as to minimize the volatilization
of organic components. This phenomenon is apparent after the TOC analysis
of theoretically identical samples in which one was collected in a VOA
bottle (no head space) and another collected in a larger sample bottle
only half to three-quarters full. Repeatability and representativeness
can be improved by homogenizing (by mixing) the samples prior to analysis.
The precision measurement based upon repeated injection of three
randomly selected samples appears to be a function of the concentration
when measured on the basis of the standard deviation. The standard
deviations in one case for two of the samples cannot be considered to be
equal (at the 95% level of significance), but there appears to be no
difference between the standard deviations when comparing one of the
first two with the third. When compared on the basis of the relative
standard deviation, RSD, (or % RSD), the precision for all three measure-
ments appears to be the same.
The accuracy of the technique is best represented here by injecting
a known volume of the calibration standard and comparing the results to
the theoretical value. In this case, the highest standard used to
calibrate was a 100 mg/L (100 ppm) solution of KHP.
The accuracy measurement is based on an in-house standard and
indicates about a 9% positive bias (or accuracy), based on the mean of
the measurements. However, a statistical hypothesis test that the bias
is zero would be accepted at the 95% level of confidence. Stated
differently there is a 95% probability of being correct if we say that
our data does not show a significant difference from zero.
All samples were diluted as necessary to fall within the limits of
the calibration.
5-23
-------
5.5.2 Chemical Oxygen Demand (COD)
This test method is considered an independent measurement of the
organic matter in a sample. The Chemical Oxygen Demand (COD) method
determines the quantity of oxygen required to oxidize the organic matter
in a waste sample, under specific conditions of oxidizing agent,
temperature, and time.
5.5.2.1 Summary of Method. Organic and oxidizable inorganic
substances in the sample are oxidized by potassium dichromate in 50%
sulfuric acid solution at reflux temperature. Silver sulfate is used as
a catalyst and mercuric sulfate is added to remove chloride interference.
The excess dichromate is titrated with standard ferrous ammonium sulfate,
using orthophenanthroline ferrous complex as an indicator.
5.5.2.2 Interferences/Quality Control. Volatile straight-chain
aliphatic compounds are not oxidized to any appreciable extent. This
limitation occurs partly because volatile organics are present in the
vapor space and do not come in contact with the oxidizing liquid.
Straight-chain aliphatic compounds are oxidized more effectively when
silver sulfate is added as a catalyst. However, silver sulfate reacts
with the halides to produce precipitates that are only oxidized partially.
This can be partially overcome by adding mercuric sulfate to complex the
halides prior to the reflux step.
The replicated chemical oxygen demand readings are given in Table 5-2.
Seven samples were replicated and the means, standard deviations, and
coefficients of variation for the COD readings are given in Columns 4,
6, and 8, respectively in the table. Assuming that the coefficient of
variation of the chemical oxygen demand (COD) readings should remain
constant, the pooled estimate of the coefficient of variation is 0.0435,
or 4.4% and is a good measure of the precision.
5.5.3 Oil and Grease
This method includes the measurement of fluorocarbon-113 extractable
matter from industrial and domestic wastes. It is applicable to the
determination of relatively nonvolatile hydrocarbons, vegetable oils,
animal fats, waxes, soaps, greases and related matter.
5.5.3.1 Summary of Method. The sample is acidified to a low pH
(<2) and serially extracted with fluorocarbon-113 in a separatory funnel.
The solvent is evaporated from the extract and the residue weighed on an
analytical balance.
5-24
-------
Table 5-2. REPLICATED COD AND 0 & G MEASUREMENTS
no
tn
COD
TRW Sample # mg/L
4957 2968
3508
4958 4106
4024
4228
4960 2155
2114
4961 1748
1748
4962 1545
1585
1565
4971 1240
1301
4973 1911
1870
0 & G
mg/L
491
535
453
440
441
382
376
133
144
125
94
126
110
109
123
120
Standard
Means Deviation
COD 0 & G COD 0 & G
mg/L mg/L mg/L mg/L
3238 513.0 381.8 31.1
4119 444.7 102.6 7.23
2135 379.0 29.0 4.24
1748 133.5 0.0 0.71
1565 115.0 20.0 18.2
1271 109.5 43.1 0.71
1891 121.5 29.0 2.12
Coefficient
of
Variation
COD 0
0.1179* 0.
0.0249 0.
0.0136 0.
0.0000 0.
0.0218 0.
0.0340 0.
0.0153 0.
& G
0606
0163
0112
0053
1582
0065
0175
-------
5.5.3.2 Interferences/Quality Control. Fluorocarbon-113 has the
ability to dissolve not only oil and grease but also other organic
substances. No known solvent will selectively dissolve only oil and
grease. Solvent removal results in the loss of short-chain hydrocarbons
and simple aromatics by volatization. Significant portions of petroleum
distillates from gasoline through No. 2 fuel oil are lost in the process.
In addition, heavier residuals of crude oils and heavy fuel oils contain
a significant percentage of residue-type materials that are not soluble
in fluorocarbon-113.
Replicated oil and grease (0 & G) readings for seven samples are
shown in Table 5-2. Sample means, standard deviations, and coefficients
of variation are shown in Columns 5, 7, and 9, respectively. Pooling
the coefficients of variation for 0 & G gives a precision of 7.9, or
almost double the precision of the COD readings.
5.5.4 Total Chromatographable Organics (TCO)/Hydrocarbon Speciation
This method is applicable for the measurement of hydrocarbons in
surfaces waters, domestic and industrial wastes.
5.5.4.1 Summary of Method. The analysis for TCO was performed by
gas chromatography with flame ionization detection. Component speciation
was done by separation with a fused silica capillary (0.25 mm), GC
column (SPB-1 boiling point column). The reported values are in milli-
grams per liter of sample, and is a total integrated value representing
hydrocarbons ranging between C5 and C30.
For additional breakdown, i.e., hydrocarbon speciation, the resulting
chromotography was broken down into C (toluene) through C30 hydrocarbons.
The values in milligrams per liter were calculated using average response
factors of C7-Cllt Cn-C16 and C17 to C25 hydrocarbons. Due to the
reduced response on a FID of C17 to C2s hydrocarbons as compared to
Cy-Cn high values of some C17-C2s compounds were found.
Each sample was prepared by extracting a 500 ml aliquot with methylene
chloride both at an acidic and basic pH, combining the methylene chloride
extracts, and then reducing the solvent to a final volume of 25 ml.
Each sample was spiked with an internal spike to check recovery.
5.5.4.2 Interferences/Quality Control. The sample is serially
extracted with methylene chloride and concentrated to provide sufficient
hydrocarbons for analysis. The concentration step results in the loss
5-26
-------
of short-chain hydrocarbons and simple aromatics (BP < 100°C) by
volatilization. In addition, the extraction partition coefficient for
certain compounds does vary. For a measure of extraction efficiency,
each sample and control samples (distilled organic free water) were
spiked with Napthalene-d8 which resulted in recoveries between 75 and
85 percent.
5.5.5 Purge and Trap (Volatile Organic Analysis)
The volatile organics in water were qualitatively identified by
utilizing EPA Method 624 with mass spectral identification. After
examination of several representative samples, each water sample was
quantitated by purge and trap with GC/FID.
5.5.5.1 Summary of Method. The GC/MS analysis was performed on a
Finnigan 4000 with an INCOS data system. A Tekmar purge and trap apparatus
was used according to EPA Method 624. The GC column used was a 6 ft x 1/8
in stainless steel packed with 0.2% CW 1500 on 60/80 Carbopack C. Oven
conditions were 15°C programmed to 190°C at 10°C/min and held for
25 minutes. A 5 ml aliquot of each sample was taken for analysis and
spiked with 750 ng Bromofluorobenzene (BFB) for an internal standard.
Comparison by identification by GC/MS was done by spectral library
searches and comparison with known standards (Figures 5-14 and 5-15).
Quantitative analysis was obtained by GC/FID (Figures 5-16 and 5-17)
using the same identical chromatography conditions as employed with
GC/MS qualitative analysis runs.
5.5.5.2 Interferences/Quality Control. Contamination can occur
whenever high-level and low-level samples are analyzed sequentially.
When utilizing GC/FID detection only, co-eluting peaks can give a positive
bias to values obtained for the components of interest.
Data quality techniques utilized for these analyses included the
following:
1. A complete page of the system following a high level VOA
sample.
2. Bromoflurobenzene (BFB) was used as an internal standard in
all samples and control standards. In addition, benzene and
toluene were quantitatively based on their respective response
values to BFB.
3. When evidence of co-eluting was detected, values were not
reported for selected compounds.
5-27
-------
tn
ro
CO
RIC
RIC DATA: 83093 «589
09/23/83 11:22:00 CALI: 0923 #4
SAMPLE: TRMf 4973 + 750NG BFB (UOA)
RANGE: G 1/1000 LABEL: N 0. 4.0 QUAN: A 0, 1.0 BASE: U 20, 3
613
uetvft.
SCANS
i TO
200
6:40
400
13:20
600
20:80
26:40
1300470
1000 SCAN
33:20 TIME
Figure 5-14. Mass spectrometer qualitative analysis by purge and trap, sample no. DAF-JN-#1-VOA.
-------
108.
01
RIC
200
6:40
RIC
89/26/83 15:41:00
SAMPLE: TRM #4975 (DAF-OUTH750NG BFB
RANGE: G 1,1898 LABEL: N 0, 4.0 QUAN: A
421
DATA: 83094 #1
CALIi 0923 #4
0. 1.0 BASE: U 28, 3
SCANS 200 TO 1000
380
10:00
I
400
13:20
I
500
16:40
I
600
20:00
700
23:20
26:40
i
900
30:00
1000 SCAN
33:20 TIME
Figure 5-15. Mass spectrometer qualitative analysis by purge and trap, sample no. DAF-OUT-fl-VOA.
-------
en
t
00
o
fs
E
Figure 5-16. GC/FID quantitative analysis by purge and trap, sample no. DAF-IN-#1-VOA.
-------
en
oo
r
cm
_.U_l. .!.__IJ-.I.-L
v«h«n /Sunnyvale, calil p/n 039063*700
Figure 5-17. GC/FID quantitative analysis by purge and trap, sample no. DAF-OUT-#1-VOA.
-------
Table 5-3 gives concentration and quality parameters for an in-house
standard and replicated results for TRW Sample No. 4973. BFB is bromo-
fluorobenzene and was spiked into the in-house standard sample and the
three replicated samples at the same concentration. The accuracy is
estimated as the percent bias the mean of the three BFB readings is from
the in-house standard, and is calculated to be about 52 percent. Precision
is estimated as the pooled coefficient of variation for all the compounds
(including BFB) and is calculated to be 9.6 percent. The sample here
was not filtered before the replicated samples were drawn.
Table 5-4 gives GC/FID data for an induced air flotation (IAF)
sample and a dissolved air flotation sample. These samples were filtered
before analysis. Accuracy estimates for IAF and DAF, respectively are
9.8 and 19.3 percent. The precision is 29.3 and 3.7 percent, respectively.
In view of the fact that only duplicate analyses were performed, the
precision figures for the filtered samples appears not to be significantly
different (29.3 and 3.7 percent) from those for the unfiltered sample
(9.6 percent). The accuracy for the filtered samples (9.8 and
19.3 percent) appear to be significantly better than the accuracy of the
unfiltered sample (52 percent). It appears that the solid material in
the unfiltered matrix decreased the accuracy possible in the analysis.
5^32
-------
Table 5-3. GC/FID READINGS FOR ACCURACY/PRECISION ESTIMATES
TRW Sample No. 4973
Compound
C2HgS2
C6H6
CgHsCHs
BFB
In-house
Standard
ppb
—
352
348
596
Replication
1
ppb
240
187
502
863
2
ppb
227
174
519
927
No.
3
ppb
198
142
441
927
Means
ppb
221.7
167.7
487.3
905.7
Std. dev.
ppb
21.5
23.1
41.0
37.0
CV
0.0970
0.1381
0.0842
0.0408
* Arrnr-nrw - 905' 7"596 v inn - R1 0*
% Precision = pooled CV for compounds in Sample No. 4973 = 9.6%.
5-33
-------
Table 5-4. PRECISION/ACCURACY ESTIMATES FOR IAF/DAF SAMPLES
IAF, TRW #4987
Compound
£6^2 > PPb
CeH6. PPb
£4^1052 » PPb
C6H6CH3, ppb
BFB, counts
For IAF:
Standard 1
— 939
— 1970
— 411
— 5710
170417 143078
170417 - ((143078 +
2
943 0.
1770 0.
410 0.
5020 0.
164324 0.
164324)72)
DAF, TRW #4994
CV 1 2
0030 — —
3860 2120 1980
0017 — —
0909 2110 2000
5370 135529 139579
inn - q ft*
CV
—
0.0483
—
0.0379
0.0208
170417
For DAF:
Accuracy = 170417 - (("5529^ 139579)72) „ ,„„ . „_
Precision:
Pooled CV for IAF = + 29.8%.
Pooled CV for DAF = + 3.7%.
5-34
-------
REFERENCES
1. Cantrell, Aileen. Annual Refining Survey. Oil and Gas Journal.
March 21, 1983.
2. Environmental Protection Agency. Petroleum Refining Point Source
Category Effluent Limitations Guidelines, Pretreatment Standards,
and New Source Performance Standards. 47 FR 46434. October 16, 1982.
-------
APPENDIX A
SAMPLE CALCULATIONS AND RESULTS
• Flow and Emission Rate Calculation
Examples
• Summary Gas Analysis Sheets
• DAF and Equalization Tank Flow
Computations
• IAF Flow Results
t Continuous Monitor Results
-------
" APPENDIX A - EXAMPLE CALCULATIONS
Example #1) IAF - Flow Measurement with Vane Anemometers
V ' X
V X 17.64 X Ph
(B) Vs (SCFH) = ( *" T + 460 - ->
(Example of flow measurement calculation at 1745 during IAF run on 8/10/83)
van @ 1745 Run 8"10 (CFM) = I X '°873
- 4'3 CFMan
fcrPM\ - /4.3 X 17.64 X 29.
(SCFM) - ( - 84 + 460
84 + 460
4.18 SCFM
SCFM = standard cubic feet per minute
V = volume measured through vane anemometer
an
V = volume standardized to standard temperature and pressure
Pb = barometric pressure
T = temperature of stack gas
-------
Example #2) DAF and Equalization Tank Flow Measurements with a Standard Pi tot
(A) Average molecular weight of dry stack gas = MWd
MW = (XC02 X $ ) + (»2 X jg ) + ( XN2 X
(B) Stack velocity @ stack conditions, fpm • V£
Vc * 4310 X /APe X (Te + 460) Pe X MW = fpm
5 55 5
(C) Stack gas volume @ dry standard conditions, DSCFM = Qs
17.64 X Vs X As X Ps
Qs " (T$ + 460)
(Example of flow measurement calculation at DAF during 8/8/83 run)
(A) MHd • (0 X $ ) + ( 19.7 X ) + ( 76.1 X
= 27.61
(B) Vs = 4310 /-.44 X 545 ( 29.8Q 27
= 1316.18 fpm
/C) n = 17.64 X 1316.18 fpm X 1.67 ft2 X 29.80 in. Hg
5 ' 545 °F
= 2119.07 SCFM
-------
Example #3) Mass Emission Rate for VOC as C-Hg
(A) Sample calculation to provide the conversion factor
of CoHg fronTppm to mg/m
TP - I 445 \ f 1 mole x / .28.32 L x / 35.31 ft x / 1000 mg x
CPC3H8 " ( mole J ( 25.71 L ' ( ~^3 > ( ~^3 ' ( ~g }
/ 3
/ mg/m x
10 ppm
- 1.71 mg/m
(B) Emission rate = Ib/hr
r - / VOCppm x , 1.71 mg x , m3 x , Q f t3 x / 60 min
tVOC ~ ^ ' ^ 3 ' * - ~3 ' ^ -1 _ ' * ~h^ -
VUL m"3 35.31 ftj min hr
f
1
1000 453. 6g
Example - of Emission Rate calculation on IAF 8/10/83 run at 0900
3
P _ / 6640ppm x / 1.71 mg x / m x / 4.1 ft x / 60 min
VOC ~ * ' * 3 ' » 5" ' v ~mTri ' * ~Tr
VUL mj 35.31 ftJ min hr
/ 9 ) f Tb x
1 1000 mg ; l 453.6 g '
= 0.17 Ibs/hr
-------
IAF FLOW RESULTS
-------
IAF FLOW MEASUREMENTS:
CHEVRON - EL SEGUNDO, CALIFORNIA
Measured Rate
Date
8/10/83
8/10/83
8/11/83
8/11/83
8/11/83
8/11/83
8/11/83
8/12/83
8/12/83
8/12/83
8/12/83
Time
1745-1903
2145-2230*
0045-0120*
0951-1016
1032-1103
1310-1357
1517-1559
1033-1119
1130-1215
1230-1315
1400-1446
Temperature
(BF)
84
72
72
88
88
88
88
84
84
84
84
(Time Period
(Feet) In M1n)
744
194
190
1275
1725
2042
2294
2197
1725
2080
2194
15
45
40
25
30
47
42
45.7
45
45
45.6
Anemometer
Average Rate
( Ft/Ml n)
49.6
4.3
4.7
51
69
43.4
54.6
48.1
38.3
46.2
48.1
Actual
Volumetric
Flowrate
(ACFM)
4.3
0.38
0.41
4.4
6.0
3.8
4.8
4.2
3.3
4.0
4.2
Standard
Volumetric
Flowrate
(SCFM)
4.1
0.38
0.41
4.2
5.7
3.6
4.6
3.9
3.2
3.9
4.1
Flow measurements monitored during night period with lower process gas temperatures.
-------
Davis Anemometer Correction Chart
BAVB umnwtf *T MH. eo, we.
eoimtcnoH aturr
XMUU. NO
June
TYK BAU. BCAKDK)
TMUf
MJI.
30
SO
78
to
100
200
300
400
500
MO
TOO
MO
«oo
1000
1300
1400
1*00
INDICATED
tut.
11
M
S3
- 7S
•S
1*0
aw
400
SO*
410
TIS
120
«3J
IOSO
123$
I44S
!*?»
mui
FfJI.
• IMO
20OO
2200
2400
2400
2SOO
3000
S200
3400
1400
MOO
4000
4200
4400
4400
4(00
5000
MOfCATEO
ffM.
1340
2045 ••
227S
24«0
37(MI
2*10
3120
33U
S550
ST«
s*n
41W
43*0
45W
4*00
M2S
1240
-------
SUMMARY GAS ANALYSIS SHEETS
-------
WORK SHEET
JS7 9
Mfft
,
Sia-
*•?<-
*/>
^77
79
*"
JF7I
1716
6
*/
*/<
*/*
7V5"
*/*
s///
•7
-781
*/
„
/931
ft*
-------
WORK SHEET
8
S/3
£3
/077/
S/3
,1
lull
,7 S7
' */*
lot 11
folfr
V/
-------
TRW
fNVlHONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
C-2
7.0
JLfL
C-3
ItaJlsnnr
U*k>*-rr+jS^n
11*
//./ *
v./
3.7
±L
TOUEWE C-(a
f7./
ic, -6
J±J_
n.L
**
**
(£p<4>Vt^<.el ^"
TOTAL
HC
C02
MO
CO
wo
% N?
73
0?
% cm
TOTAL %
-------
ENVIRONMENTAL ENGINEERING DMSION
*3
SUMMARY GAS ANALYSIS
. COMPONENT RUN
C-l
Jo^i
*
C-2
5-7
C-3
JLO.
Z.o
c-sV
v./
:-5"
•/.f
3
**
TOTAL
IX
% C02 MO
% CO ysJ.O
J2_
% cm
TOTAL %
-------
ENVIRONMENTAL ENGINEERING DIVISION
Sttf-WARY GAS ANALYSIS
- /
COMPONENT RUN
C-l
^
C-2
/ 5"
C-3
< J
C-4
C-5
C-5
**
BENZENE
79
7.7
*•/*
V
-------
TRW
'NVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS ft/JF ~3o3i ~ /
. COMPONENT RUN
C-1
C-2
C-3
s-o
Jjjb
15.
77
^
19.6
TOTAL
HC
CO?
% CO
% N?
% 0?
% CH4
TOTAL %
(La
w-
rr
-------
TRW
fWIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
'ft' '3°5 ~
COMPONENT RUN
C-l
C-2
C-3
*-"
•*
/5-3 *
S£.
16,1**
s-/*5*
C
r,
TOTAL
HC
% CO?
CO
2 N?
73' t
3.. -
•73 '-
% o?
&L.
% CH4
TOTAL %
-------
CNVIRONMENTAL fNGINEEfUNG DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
C-2
jL£
C-3
<
C-4
C-5
C-6
2-3
BENZENE
7Y,
#>•/
*'
3.0^*
TOTAL
Hc
%M
% C02
CO
% N2
73.
% 02
% cm
TOTAL %
-------
CNVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
£Z.
C-2
9
C-3
-------
Co t-
ENVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
.. COMPONENT RUN
C-l
Uji.
ton
C-2
C-3
UI4
1 b
C-4
'i-/
•f-f
II. "2.
/Or/
ft*
5.?
-BBtTENE c«
3. .
-XYtEttF
TOTAL
HC
SM
% CO? A;Q
% CO
% N2
*£.
% 02
% CHa
TOTAL %
-------
rosy
ENVIRONMENTAL £NGINEERJNG DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
M.IZ.
C-2
C-3
s
*JL
•L.I
jxf
Ht- XYt
/C.2.
EEH2ENE
TOLUENE
ATtefrE
TOTAL
HC
C02
% CO
% N?
% 02
% CHa
TOTAL %
-------
fNVIRONMENTAL ENGINEERING DMSION
SUMMARY GAS ANALYSIS
T
. COMPONENT RUN
C-l
d-X?/
C-2
C-3
C-4
C-5
C-6
/.V
BENZENE
TOttOE U IL
XYLCHE
TOTAL
%M
% C02
% CO
N?
77 -
% o?
% CH4
TOTAL %
-------
TVSff
ENVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
'**#
C-2
2,2-
C-3
AL
C-5
C-6
BENZENE
. C
XY4EWE U
4 /
TOTAL
HC
%M
5S C02
CO
% N?
0?
% CHA
TOTAL %
-------
fNVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
-g^>Y
c-e
C-3
C-4 MM-
C-5
C-6
jjn_
BENZENE
T6LIOC
to
lo.g'
XYLENE
TOTAL
HC
% C02
% CO
N2
% 0?
TOTAL %
-------
INVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
r
COMPONENT RUN
C-l
C-2
C-3
5-3
*/.«
•I.**-
u/i.
n.t?
£. I
1.1
BENZENE
1.8
TOLUENE £6
LENE
TOTAL
HC
221. J?
%M
% C02
% CO
N?
-I£
% 0?
% CH4
TOTAL %
-------
TRW
ENVIRONMENTAL ENGINEERING DIVISION
r
SUMMARY GAS ANALYSIS
COMPONENT RUN
fc-1
r^-firm-
C-2
3,5'
UJL
J*±.
C-3
C4
Jd£.
6,7
/3,3
A), 3
Z6'/
B
JZENE
f./
LUENE
UK-
UK.
LENE
aK
H.I
I'l
3.1-
5
7,3
TOTAL
-y.
XM
CO?
CO
% N?
% 0?
% CHA
TOTAL %
-------
TRW
eWIRONMSNTAL £NG1NE£R/NG DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
C-2
a. r
(AIL
io-3
S- 2.«/
c-a:
A.a
'•
UK.
/4,-j 17,5"
BEH2S1E
~ «f
U.3
St
.1- f
TOTAL
HC
CO? ' .
% CO
N?
% 02
% CHd
TOTAL %
-------
TRW
CNVIRONMENTAl ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
t'3"
-28'* -15*0
JLL
3JL
Cf/Z
/*>«/
8,3
7.8
%M
% C02
% CO
% N?
% 02
% CH4
TOTAL %
-------
TRW
ENVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
.COMPONENT RUN
C-l
C-2
C-3
C-4
C-5
r K ++&'£'
BENZENE
JtOtH£WE *K
XYLENE
TOTAL HC
JM
% C02
56 CO
% N?
% 0?
% CH/i
TOTAL %
W»i
rr/t
^.l
^.i
^.s
1.-?
50 *(
•
7^«^
/?/57
pp»*
• . -^
/op
1,1
1.-)
-70
«»'»
j£*r
It, .51
H.b^
• »
•
-------
TRW
ENVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
. COMPONENT RUN
C-l
C-2
C-3
C-4
C-5
c-6 -±«J££
BENZENE
I0U£KEI*^a*£
U.IL
J&fcEttE
TOTAL HC
%M
% C02
% CO
% N?
% 02
% cm
TOTAL %
!|0**
/<*.-»-
/.4
3.3
5T.<^
. 2_
as-'7
•
•^5"- 3^
1$>V&>
l<<"
1<4
3.L
C,,i
—
ZT'
-?^,/f
/9-3^
•
i
-------
TRW
ENVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
C-2
C-3
t-V
C-4-
6=5-
- 1.1
I'S
BE8ZENE C4
4,7
•XYLEME
-------
ENVIRONMENTAL 1-NGINEEHtNG DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
1 %,
C-2
C-3
C-4
H )L,
TSLUEItE
St¥t±NE
TOTAL
HC
%M
% C02
% CO
% N?
JQ2_
% CHA
TOTAL %
-------
TRW
ENVIRONMENTAL ENGINEERING DIVISION
I
SUMMARY GAS ANALYSIS
. COMPONENT RUN
13
C-1
C-2
C-3
it
»£>,«/
<.<(
BENZENE
TOlUENE
XYUNE
//o
TOTAL
HC
%M
CO?
% CO
% N?
% 0?
% CH/i
TOTAL %
-------
BWIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
166-7
nv
C-2
C-3
UK
/sw
HAXU
c-
BEBZENE
TOLUENE
34.7
UK
XVLENE
265
\-i i
tTAL
**'*
%M
% C02
% CO
N?
% 0?
% CH/t
TOTAL %
-------
BWiaONMENTAl ENGINEERING DIVISION
SUMMARY a-J ANALYSIS
, COMPONENT RUN
Q/-J Uii-
7 2
I3
T4
cU
C-f
BEBZENE
TOI UENE
XYl ENE
7
TOTAL HC
m
% C02
% CO
% N2
% 02
% CH4
TOTAL %
1
05
;&*
/psr
•74,1-
i/^
*/*-
'S,-23^
•
.
IV
?r,7
V3/2
^o-/
—
7.'
• •*/£ <--?
^
•
i
•
-------
TRW
ENVIRON'MENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
. COMPONENT RUN
C-l
C-2
J. /
C-3
2/o
Uld
B
ZENE
LUENE
7.5?
LENE
CO?
CO
N?
% 0?
% CH/t
TOTAL %
-------
ENVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
. COMPONENT RUN
C-
c-
c-
c-
c-
c-
BE
TO]
X^
.
i
X uR
2
3
i*
>
$
IZENE
.UENE
LENE
TOTAL HC
XM
% C02
% CO
% N?
% 02
% CH4
TOTAL 55
!.
S-,5-
r,7
i./
r.s^
•?'/
r/T
333,«r
•
.
3,3'
5"/^
I*/
in
-7.}
?.<*
^3o,>
•
-------
eNVIRONMENTAL CNGINEERING DIVISION
3
SUWARY GAS AMALYSIS
». COMPONENT RUN
C-1
U7<
IS"!
C-2
C-3
C-4
£<•/
B
NZENE
.UENE UK
£5"
ue
3*7?
LENE
UK
TOTAL
HC
%M
CO?
CO
N?
% 0?
% CM*
TOTAL %
6. -
-------
ENVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
. COMPONENT RUN
C-l
c*
c
c
c-
c-
BE
TO
XY
TO
»
2 u*-
3 Uli
4 L,'£
5 t//^
6 Li^
NZENE u/^
LUENE a'^-
^^
.ENE
rAL HC
% C02
% CO
% N2
% 02
% CH/j
TOTAL %
!
JL-b^
i-$
1 .0
l.H
I,1*"
i'l
L'h
l,*~
37>f
—
3^'V
7S.2/
/ $ S4)'
•
•
-------
TRW
BWtRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-1
.£££.
1.3
TOUENE
X1LENE
TOTAL
HC
%M
% C02
% CO
Ng
7^-2-17
% 0?
% CHd
TOTAL %
-------
TRW
ENVIRONMENTAL ENGINEERING DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-1
3,5*
OK
D/3
C— 5
UiL
<- 1
7/3
/?£-/
%M
% C02
% CO
% N2
% 02
% CH4
TOTAL %
-------
TBSff
CNVIRONMENTAl £NGINEEftlNG DIVISION
SUMMARY GAS ANALYSIS
COMPONENT RUN
C-l
C-2
C-3
c-i
g<3
BNZENE
a
TOLUENE
L/K
041,
5T3
XYENE
TOTAL
_%M
% C02
% CO
% N?
% 0?
% CHa
TOTAL %
HC
-------
DAF AND EQUALIZATION TANK FLOW COMPUTATIONS
-------
TEST DAY 8/1/83
-------
Press 'key code* to enter variable. Press
for result*.
CURRENT VALUE
68
.65
O
29.8
1.6
1
O
21
74.8
240.529
1
.3
7.21571
Tt
Pb'.in.Hg. )
I C02
•/ 02
'/ N2
SDR(DELPS)
As<3q. in. )
Ts
Barometric Pressure (in.Hg)
Meter Prt-ssure TO COM7INUE.
V,-a(s=f) .999521
Vi,i(£Ci:i/ .0283064
Vw gas(scf) 0
•.••_.-..•_ J . . ^ _- f\
/• iT.u-j _ L Lt, & V
Md 1
MVJd 27.664
ril-J 27.664
Vstrjj-' 1275.17
r]o**<^-r,-A> 2129.96
r:ov4(i_i.;;i;,») 60.3206
~1 a- 1 (•-,-.:? A,) 2O43.56
riouC^i ....ii) 57.8737
:; I 1497.9
:: EA -1676.25
-------
TEST DAY 8/3/83
-------
Press 'key code' to anter variable. F-.-gsa *Z' For results.
CURRENT VALUE
68
•-.5
• o
27.3
1.6
. 1 - .- •
' 0 .
20.3
73,6 " ....
424.553
« i
.1
3. J3541
. '•-•' ' : •'-".'••
TtC/nin.)'
. Dn (in. >".•• '-.-.,-.
Pi (in.H2O)
V*«(cu.ft.) -».
Vn(g
T^ ;FJ
KEY CODE •
A .
D
c .
D
^
r-
Q- "
H
T
T * *
U
Is-
t '
'1
PRESS
1 .
.- . .1- ,'
-.5 ' '.
1
0 -
1.6
60
29.3
0
20.3'
73.6
8,43541
424.553
93.9999,
PA~;.-.MET2rvS IN METHODS 2-5
MstiV T^inperature (F)
3ta;:k CtaLic Pressure (in.H2Q)
Stjulc .Maisture Collected (gm>,.
Bar u«,a trie Pressure (in.Hg), y
flats:- .Prajsare TO CONTINUE.
V.TjCscf) .999521
Vtt(=Cir.) .02B3064
' V/i ijaa v3cF) 0
'- % ;nci^ture O
, ' ru • i
n;:j • 27.104
rr.'i - 27. 104
Va:rpra> 1517.11 '
7'.3,j<^cffn> ' 4472.93
Fl _>;j (ac'cur*) 126.673
rio.j(3iiFa> 4240.71
n JM ( -c.-a.-i) ' 120.097
:•; i '.. 1274. i
?'. 2A ' -2334.41
-------
TEST DAY 8/4/83
-------
Press ' key
CURRENT VALUE
68
.65
O
29.8
1.6
1
O
20.6
74.2
24O.529
1
.1
7.O7O12
code' to enter
KEY CODE
A
B
C
D
E
F
G
H
I
J
K
L
M
Ttdiun.J
DnCin.)
Ps
Pm
Stack Static Pressure (in.H2O)
Stack Moisture Collected (gro)x .
Barometric Pressure (in.Hg)
Meter Pressure TO COITTINUE.
Vm
-------
TEST DAY 8/5/83
-------
Press 'key code' to enter variable. Prass *Z' for results.
PARAMETERS IN METHODS 2-5
Metar Temperature
Vmtcu.ft.)
Vwtgm.)
Pm(in.H20>
Tm(F) '
Fbtin.Hg.)
7.' CQ2
X 02
7. N2
SQR(DELPS)
Asfsq.in.)
Ts(F)
PRESS
,;.;65 .-
O
1.6
68
29.8
O
19.9
76.9
7.39987
24O.529
93.9999
TO CONTINUE.
VirUscf J
Vm(scm>r ^•-'-.'•
Vw gasCscf)
'/. moisture
Md
MWd
MUJ .
Vs (f pin)
Flow(acnun)
Flovi(scFm)^''
X I
"/. EA
.4"
.999521
.O283064
0
O
1
27.9-
27. 9 !
1302.17
2175.O7
61.5979
2068
58•5658
1480.2
4955.18
-------
Press 'key code* to enter variiblj. rv.235 *Z* far results.
IT VALUE
i3 '*
.35 .
O
27.8 "'
1.6
1
o
20.4
73.3
424.553
1
KEY CODE
A
B
C
D
- E
F
G
H
I
a . ,
K
3.31435
Tt (fflin.:>
DnUn. >
Ps(in.H20)
V,Ti(CU.ft.)
P.n«in.H2O)
PbUn.Hg.)
V. C02 ' ' .
•/. O2
7. N2
SCR(DELPS)
As(sq.in.)
PAn.",ri2T2n3: IN METHODS 2-5
Mata;- T^.iiperature
Sta^.!; 2t^Lic Pressure (in.H2O)
Sta^U t1ai=»ture Collected .J
Barw.iietrie Pressure (in.Hg) :
Matisr Pressure TO COMTINUE.
.35
1
O
1.6
63
29.S
O
20.4
73.3
8.31435
424.558
93.9999
?
Vstfpni) .,
Flaw(acFffl)
.O283064
- O
O
1
27.192
27.192
1482.57
4371.O7
123.789
4152.84
117.609
13O1.O5
-2225. 13
-------
Prers 'key code' to enter variabls. P.-=253 *2' for results.
:NT VALUE .
£8
.33
O
29.3
1.6
1
A
21.5
73.2
424.558
4
i
«
* *.
0.21207
TtCmin.)
Dn
Vm(cu.ft.>
V«-i(gm. )
Puivin.H2O>
TmCF)
PbUn.llg.)
;:- cos ;
•/. 02
% N2
SCR(DELPS)
Ar» Csq. in. )
Ts IF)
KEY CODE
A
D
C
D
E
F
B
H
I
J
K
L
M
PRESS
' !'•
... .f - '
.35
1
O
j.6
63
. 29.8
O
»
21.5
73.2
8.21207
424.558
9O.9999
PAriAMETEHS IN hETHDDS 2-5
Mai_-r Te.sparature zzzle diameter (in.)
Dal^i Cut;routine result"
*-.-..' -j*- • •;.'"•-
^c»* i taj ww>4tXi *L]&» * -"'" • •
V;a(scF) ; .995521
V.a < 3C.r.) ' . . 0283064
'/;>> aa.*v3Cf > O
•» _» -A .._-._. " ' ' " A *-*
J» itlW*J. «^^Ul 6 " ' . V • — '
^U . r .'-.-. .'-::1-.-.' '" •
rJVJd '.^ Jv '23.776
rW • -v ^ 28.776
•v-sCfpai. 1423.45 .
-lovitacfsi) , 4196.8
Fla.; C^coiin)' 118.853
rii3.j(.3i:Fin) 4008.98-
• PI 3iv < =c,%in»> ' 113. 534
r: I ' 1347.74
T; CA " -2514.03
-------
TEST DAY 8/8/83
-------
Press 'key code' to enter variable. Press '2' -for results.
iURRENT VALUE
68
-.44
O
29.8
1.6
1
0
19.7
76.1
24O. 529
1
.1
7.4308
Tt(min.)
Dn(in.)
Ps(in.H20)
Vm
Pbdn.Hg.)
% C02
% O2
% N2
SQR(DELPS)
As(sq.in. )
Ts TO CONTINUE.
Vin(scf) .999521
Vm(scm) .0283064
Vw gas(sc-f) O
X moisture O
Md 1
MWd 27.612
MM 27.612
Vs(fpm) 1316.18
FlOM(acfm) 2198.47
FloH(acmm) 62.26O7
Flow(sc-Fm) 2119.07
Flow(scmm) 60.O12
% I 1444.53
% EA 5046.13
£^> •^O'X. ^/v^ilS
^ \
\,
-------
TEST DAY 8/9/83
-------
Press 'key code* to enter variable. Press "Z* for results.
^PARAMETERS IN METHODS 2-5
Meter Temperature
StVck Static Pressure (in.H2O)
ck Moisture Collected
oinetric Pressure (in.Hg)
CURRENT VALUE
63 ' •
-.45
O
29 .'85
1.6
1
' 0
19.8
76.62
247. 45
1
. 1
7.22097
KEY CODE
A
B
C
D
E
F
G
H
I
J
K
L
M
Stc
Bar
He]
.sr Pressure
TmCF)
PbCin.Hg.)
'/. C02
7. D2
7. N2
SQR(DELPS)
As(sq.in.)
Ts(F)
PRESS
1
.1
-.45
1
O
1.6
68
29.85
O
19.8
76.62
7.22097
247.45
80
TO CONTINUE.
Vm(scF)
Vm
7m moisture
• Md
MWd
MW
Vs(fpm>
Flow(acfm)
Flow(acmm)
Flow
/I I
7. EA
1.Q0119
.02S3539
O
O
1
27.7896
27.7896
1273.87
2189.O2
61.9931
2133.02
6O.4071
1473.84
4629.62
-------
TEST DAY 8/10/83
-------
Press 'key code* to enter variable. Press '2' far results.
PARAMETERS IN METHODS 2-?
Meter Temperature (F)
Stack Static Pre^s«**ie-.
Barometric Pressure (in.Hg)
Meter Pressure (in.H2Q)
Meter Volume (cu.-ft.)
Percent C02
Percent 02
Percsnt M2
Stack dimension (sq.in.)
Sampling time (min.)
Sampling nozzle diameter (in.)
Delps Subroutine result
NT VALUE
63
-.42
0
29.85
1.6
1
O
2O. 1
77.83
247.45
1
.1
6. 1984
KEY CODE
A
B
C
D
E
F
6
H
I
J
K
L
M
Tt(min.)
Dn(in.>
P3(in.H2O>
Vm(cu.-ft.)
Vw(gjn. )
Pin(in.H2O>
PbUn.Hg.)
V. C02
7. O2
7. N2
SQR(DELPS)
A5(sq.in.)
Ts(F)
PRESS
1
.1
-.42
1
O
1.6
63
29.85
0
20.1
77.83
6.1984
247.45
87.8333
TO
Vnj(scf)
Vm<3cm)
Vw gasfsc-F)
"i moisture
' Md
MWd
MW
Vs(fpai)
Flow(acfm)
Flow(acmm)
Flow(scfm)
Flow(scmm)
'& I
'/. EA
1.00119
.0283538
0
O
1
28.2244
28.2244
1084.98
1364.43
52.8008
1790.39
SO.718
1761.36
4495.43
202.
-------
TEST DAY 8/11/83
-------
Press 'key code* to enter variable. Press 'Z* -for results.
CURRENT VALUE
60
•~. «j
0
27.35
1
O
17.62
76.38
2-', 7. 45
1
KEY CODE PARAMETERS IN METHODS 2-5
A Meter Temperature (F)
D Stack Ctctic Pressure <.in.H20)
C Stack Moisture Collected
F Mettr Volume TO CCr,TINUE.
i v..-i ( ie r /
1 1 1. . / — r~ — *
• 5 ' '~ ' n~ ~ ' ~c.f )
1 « mci-ture
0 • "d
1 . 6 Ml.'d
63 rr.:
29.85 VsCpa)
O ria;j(-effn)
19.62 rio;.'^*3^ $r / /, V <> *
I Y
-------
CONTINUOUS MONITOR RESULTS
-------
DAF CONTINUOUS MONITOR INSTRUMENT CHARTS
-------
TRW
LOCATION
#3
JD ^
POLLUTANT
\/ O d-
DATE
INSTRUMENT RANGE (PPM) Q-
CALIBRATED BY
Record Data Every 3-5 Minutes
Time
Q/.5
)
/3V-5
Scale
Readi ng
*..«.
/ S ,J?.
-_> C>1
S
ppm
SSK3
sll.3
-
VS). /
W.I
SW.3
.sal.
S3i,3
13
[53-c?
Scale
Reading
•^ C*'
-S o^
5° 5°
ppm-
5V/.J
557.?
SfcJ
/If
-------
TRW
LOCATION
Thp.£p POLLUTANT
INSTRUMENT RANGE
Record Data Every 3-5 Minutes /
Time
tfcfo
VMf
fab
1*16
112D
.3000
JO 36
Scale
Reading
1 1
» 0
/O
1 1
.iZ
NOTES: UOO
ppm-
•HI. 2
vft./
V7I.)
47I-)
CALIBRATED BY
Time
31 to
34.%
^00
Scale
Reading
^ 7
70
96
9?
ppm-
111,1
701.7-^
5
-------
TRW
LOCATION
INSTRUMENT RANGE (PPM)_
Record Data Every 3-5 Minutes
POLLUTANT V&rf DATE
~ CALIBRATED BY
Time
MS
Scale
Reading
ft?-
8,
76
73
7
7.
V if
to
5f,sy
/
(o f 60
ppm-
§72.1
7/A7
(£\. L •
Time
MS*
Scale
Reading
Sf
5f
Xf
51
ppm-
•ho h /
400
NOTES:
-------
TRW
LOCATION
POLLUTANT
DATE
INSTRUMENT RANGE (PPM) Q-
Record Data Every 3-5 Minutes /oo9.S^ffn
CALIBRATED BY
Time
•to
66
10
It
Qo
3o
NOTES:
Scale
Reading
(.0
$9
S7
ppm-
^ IF if
Time
Of 'oo
/o
If
So
45
Scale
Reading
r?
sr
ppm-
-------
TRW
T^F
LOCATION^ u* If* »Lu^ ~TIL>L Pt
INSTRUMENT
Record Date
Time
o->*4
3o
3*
Vo
<£
S*
S3
OS DO
O9 1 0
t?
90
s?
Zo
3
STf
S&
Sf
•ss
&3
>o
99
53
' \
*>?
ppm-
sn
4t?t
^», — AS^T
NOTES:
-------
TRW
LOCATION
POLLUTANT
INSTRUMENT RANGE (PPM) Q_
Record Data Every 3-5 Minutes
DATE
CALIBRATED BY
Time
/oao
30
5-0
JldO
30
3*
Scale
Reading
6*
63
ppm-
Time
90
30
SsT
I3oo
Scale
Readi ng
s?
SB
SI
S3
vs
Vo
ppm-
NOTES:
-------
TRW
LOCATION *SLu*\i'u*
3S
3V
3^
J3
3flt
/ /
nutes /ood.:
ppm-
3U
.
DLLUTAN
PV%
5/V"^
T to>CL DATE ^-/V/»^
CALIBRATED BY /»7*;/J
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Time
if3^
Vo
vr
^0
rr
AToo
0^
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/^
90
VS
sa
ar
Va
^^
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^'r
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Reading
33
3V
3*
3V
3V
33
33
33
33
33
5V
33
S<,
33
JS
3y
JT
ppm-
Wl
5* %b
A lu ^
NOTES:
-------
TRW
LOCATION
*
POLLUTANT Vo g.
DATE
Sltlti
INSTRUMENT RANGE (PPM). O-JOee fp^
Record Data Every 3-5 Minutes too*.
Time
1700
10
I*
9$
So
3*
•to
30
Scale
Reading
3V
3*
34
34
39
34
34
.S.S-
ppm-
CALIBRATED BY
Time
nss
IJfOO
0*
10
ts
3o
3r
3o
3T
Vo
vr
^0
rr
;?bo
o^
/o
iS
Scale
Reading
3
-------
TRW
LOCATION
POLLUTANT Vo
-------
TRW
LOCATION
INSTRUMENT RANGE (PPM) Q- joeo
POLLUTANT Vo
DATE
Record Data Every 3-5 Minutes
CALIBRATED
Time
99/0
Po
30
/o
00VO
Scale
Reading
37
37
3?
34
39
3?
ppm-
Time
5-0
o; CO
/o
do
09 o a
Scale
Readi ng
I*
63
t;
S)
ft
Si
ppm-
NOTES
-------
TRW
LOCATION
POLLUTANT
DATE
* I *
INSTRUMENT RANGE (PPMfr~/g>o» »^
Record Data Every 3-5 Minutes
CALIBRATED BY /*7K/KJ
Time
90
30
O3OD
/o
30
Scale
Reading
55
V?
ppm-
Time
01
yo
oO
«*/
Scale
Readi ng
V?
v?
ppm-
4-97
NOTES:
-------
WORK SHEET
0700
ofoo
oS
r?
JO
43
ja.
if
Oo
9*
**<
9*
or
if
VO
Vo
61
Vf
so
66
do
04 Oft
VI
/o
60
Lf
a,r
30
40
3LT
-0
So
5-0
12.
-------
WORK SHEET
Hoc
)3oo
331
or
JtC.
10
/o
90
90
do
a/
30
Vf
Vo
V
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351
S)
>V
of
oi"
/o
/a
3o
30
S'o
__^L
O
-------
TRW
LOCATION
-CHgyj <.€)*/
POLLUTANT T H C
DATE
INSTRUMENT RANGE (PPM) Q
Record Data Every 3-5 Minutes
Time
1100
1200
1300
Woo
1S0O
1600
(700
($00
Woo
2,000
1(00
Zloo
-LJOO
Scale
Reading
S2.o
47.^
W
•/t.?
sg.i
55.4
H9.5
52.4
HI- 5
M7.3
H^.9
£1.2.
H^.T-
ppm
521.3
4?5.3
48?.S
WU.3
580.^
550.?
HT2.2
521.3
Hl-Z.?-
H70.2
M9^.2
509.3
H9H.2
CALIBRATED BY C
Time
Scale
Reading
ppn
NOTES:
-------
LOCATION
INSTRUMENT RANGE (PPM) O~(OQD
POLLUTANT
DATE
CALIBRATED BY CBS
Record Data Every 3-5 Minutes * C »*v«*Vtr
-------
TRW
POLLUTANT
DATE 8-
LOCATI ON P/4f-C4gVK.CM/
INSTRUMENT RANGE (PPM) O~-
Record Data Every 3-5 Minutes «*• Cox/i>e*f««/ To bounty4e/\j*e*4f*f-
CALIBRATED BY
Time
0000
0(00
OZ6O
03oc
0500
0^00
f 0 oo
HOO
IZOO
!3c?o
ISo0
IGoo
Scale
Reading
SI. 5
49.5
47.0
H5.I
5o.5
pni-
So 2. 5
131.3
Time
r^-oo
/^oo
1^00
•LOCO
2l<5«>
2,XOo
^^oo
AM-
Scale
Reading
3<*s
Vaa
qs.3
w?.«/
sq.o
S5.5
6?J
ppm-
3^5.7
qoo.6
t/53J
^^.7
s<*0.s
555.S
s?/.s
NOTES:
A/0
-------
TRW
LOCATION OAF'CkevtLw POLLUTANT.
INSTRUMENT RANGE (PPM) O-/000
Record Data Every 3-5
T # C
DATE
Time
(7060
0(00
0200
O300
0400
oboo
0200
0^00
11 Oo
lloo
1300
iqoo
Scale
Reading
. 1
63,0
as
SO
39,5
54.3
ppm-
564.1
$91.
S5G.S
396-0
_ CALIBRATED BY_
Aft u H ry
Time
05
Reading
ppm-
NOTES:
-------
EQUALIZATION TANK CONTINUOUS MONITOR INSTRUMENT CHARTS
-------
TRW
LOCATION
INSTRUMENT RANGE (PPM) . £-
Record Dats Every 3-5 Minutes
POLLUTANT
#=
DATE
Time
/boo
/t/
180
/7/6
NOTES:
Scale
Reading
J£
15
to'
H
pm-
fal
/vb-3
Kt)
Mo
ISO
CALIBRATED BY
Time
ffos
Zioo
3I3D
Scale
Readi nq
ft
ffd
/r
IL
IL
ppm-
.MO
Mo
Ho
A5D
I5b
ILO
/r
o
-------
LOCATION
POLLUTANT \fp C
INSTRUMENT RANGE (PPM)_£
Record Data Every 3-5 Minutes
DATE
CALIBRATED BY M
Time
2230
0100
NOTES:
Scale
Reading
17
18
it
\b
\s
1L
$-
if
PP"1'
160
170
IS)
/ffl
Ift)
ISO
)%P
Time
J/T
730
Scale
Reading
Jt
It
t
/T
ppm-
9A
/to
tfn
(90
-------
TRW
LOCATION
POLLUTANT
DATE
INSTRUMENT RANGE (PPM): £_-
Record Data Every 3-5 Minutes
NOTES:
CALIBRATED BY
Time
OTtS
<9
ppm-
ttl
/9/0
fio
Ifo
ISO
i£o
Bo
tfo
1?^
/&&
no
/7/>
/a
r;n
/70
170
IGO
S//wJ
Time
M/5
30/5
Scale
Reading
ft
D
1C,
!7
14
1*7
1
-------
TRW
LOCATION
I—
POLLUTANT
DATE
INSTRUMENT RANGE (PPM) O^
Record Data Every 3-5 Minutes
CALIBRATED BY
Time
Scale
Reading
Jl
ppm-
Time
Scale
Reading
ppm-
Jl
i7
t7
i7
1-7
J3i
(7
n
n
n
SD.
nn.
170
M
170
no
J?a
/ a?
NOTES:
-------
TRW
i.OCATION
POLLUTANT
DATE
INSTRUMENT RANGE (PPM) /9
record Data Every 3-5 Minutes
Time
Illo
Scale
Reading
It, .
/5
'IST.S
ppm-
ILL
/s
CALIBRATED BY
Time
Scale
Reading
ppm-
NOTES:
-------
TRW
LOCATION
POLLUTANT
DATE
INSTRUMENT RANGE (F-PM)_
Record Data Every 3-5 Minutes
CALIBRATED BY
Time
Scale
Reading
ppm-
SfiA*
Time
Scale
Reading
ppm-
NOTES:
-------
IAF CONTINUOUS MONITOR INSTRUMENT CHARTS
-------
TRW
LOCATION
INSTRUMENT RANGE (PPM)- Q-\
Record Data Every 3-5 Minutes
POLLUTANT \JQ C DATE
CALIBRATED BY
Time
3/00
0 Aor
/ooo
Scale
Reading
^9,67-
ppm-
Wo
6-j v4-
Time
1 7
Scale
Reading
10,^0
s'O
OQ
ppm
Jr P-T
NOTES:
-------
TRW
LOCATION
r
A
/ \.K<^/O.
POLLUTANT VO C
DATE
- *
INSTRUMENT RANGE (PPM) O~/o,oos
Record Data Every 3-5 Minutes
Time
£6 GO
/loo
NOTES:
Scale
Reading
£7. 58
. /o
. 70
10.
SO
ppm-
&SXO
CALIBRATED BY
Time
•9/OO
Of 00
09 C
O3OO
Cfioo
JooO
IQoO
Scale
Reading
6 t> -50
. 5 o
67, oo
67. 30
.00
7o
.50
ppm
67^0
730 0
-------
TRW
LOCATION _^/?F .^
^ *r, 60
os-.oo
••
nutes ^O/o
ppm-
-)3
-------
TRW
LOCATION X/AF -
POLLUTANT T H
DATE 8-
Oft. WAV
INSTRUMENT RANGE (PPM) Q- I Q OOP CALIBRATED BY C GS
Record Data Every 3-5 Minutes -tCe«/*.•«.*«•< T0 h*u*.ly
Time
Time
0300
10 00
1100
1Z0 O
I3CPO
moo
Scale
Reading
W.b
fi. /"7 n
(0 •• i
68.1
?2.6
72.6
73.3
•
ppm
6588.7
GGM.O
7221.9
7221.9
7291.?
X
Scale
Reading
NOTES:
-------
APPENDIX B
FIELD DATA SHEETS
• DAF and Equalization Tank
Velocity Traverse Sheets
• IAF Anemometer Measurements
• Liquid Sampling Log
-------
DAF Velocity Traverse Sheets
-------
VELOCITY TRAVERSE
PLANT.
DATE
LOCATION
STACK 1.0.
BAROMETRIC PRESSURE, in. Hg_
STACK GAUGE PRESSURE, in. H20
OPERATORS
A*
* •
&orttju^ UM
\?«>V -
fc&ji JMLMtf wd&Jtted dtJfr'c ;
flJd tuba ^HEMATIC OF TRAVERSE POINT LAYOUT
JAJii
TRAVERSE
POINT
NUMBER
7~-2o/
f^ K^CCl4U^/»vt
Ik
r
AVERAGE
VELOCITY
HEAD
Ups), in.H20
•fiu^^
n n-/ V/ji
r o.W
T
^, '
TRAVERSE
POINT
NUMBER
T-200
lJAA£
J/U*J?
?
T-2o?
4b»3-
AVERAGE
VELOCITY
HEAD
Ups), in.H20
0. 20 -O.It
= o.o^" M.I
a.iarf**Eu. •*•
3%) e!^
T^
A*r
O. 30-0.0*5
- o.2S
/)A- ^"AS
3«KO c£w.
/'
T- W
//
EPA (Dun 233
472
-------
PRELIMINARY VELOCITY TRAVERSE
J-*JZ£
PLANT.
DATE
LOCATION
STACK I.D.
BAROMETRIC PRESSURE, in. Hg_
STACK GAUGE PRESSURE, in. H20.
OPERATORS
76
6-
TRAVLRit
POINT
NUMBER
* ^V *— /
*J /
a
^
T~ /
3L
3
AVERAGE
VELOCITY
HEAD
(Aps ), in. H20
./o
/o
JO
•°¥
.01
1 fb
STACK
TEMPERATURE
(Ts). -F
^7
^
<§•*}
S-S
§9
?S
%_ — ,„ fls 1 \
-^ __ n -V 1
A
SCHEMATIC OF TRAVERSE POINT LAYOUT
TRAVERSE
POINT -<•
NUMBER
AVERAGE
VELOCITY
HEAD
(Aps), in.H20
STACK
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COMPOUND
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COMPOUND
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DATE;
COMPOUND
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-------
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COLUMN:
RUN NUMBER:
DATE;
COMPOUND
RETENTION TIME
IN CM.
COUNTS
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AHENUATION
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RUN NUMBER;
DATE;
COMPOUND
RETENTION TIME
IN CM,
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(JTHC)
ENVIRONMENTAL £NGINEEMNG DIVISION
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RUN NUMBER:
DATE;
COMPOUND
ci
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TOlUENE
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T(/TAL
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RETENTION TIME
IN CM.
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ENVIRONMENTAL ENGINEERING DIVISION
-------
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RUN NUMBER:
DATE;
COMPOUND
Is} W
i 2 b*«»v
\
3 Mjy*
r4 '
b
c)
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TOTAL
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RETENTION TIME
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-------
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ci
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I
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£* U)C
B £NZ£N€
M-'/lC
TOLUENC
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RETENTION TIME
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•
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COMPOUND
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-------
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RUN7 NUMBER:
DATE;
COMPOUND
RETENTION TIME
IN CM.
COUNTS
SPAN
ATTENUATION
DILUTION FACTOR
(Diluted w/N2)
CONCENTRATION AS
COMPOUND
CONCENTRAWON AS
BENZENE
(L
l.cH
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1-n*-
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-------
'/.
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RUN NUMBER:
DATE;
COMPOUND
C1
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<£
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XYL^NE
1
TOTAL
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CARBONS
(iTHC)
RETENTION TIME
IN CM.
*,^. .!5S
•
•
/
COUNTS
'icO
•
SPAN
^
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(Diluted w/N2)
•
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-------
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'J
RUN NUMBER:
DATE:
COMPOUND
flu.t
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4 *
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% 1
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TOJ.UENEy
XYLENE *
k
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(iTHC)
RETENTION TIME
IN CM.
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-------
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DATE:
COMPOUND
Cl
q
°z
c? '
9
c*]
BENitNE
TOLUENE
XYLEk
TOTAL
HYDRO-
CARBONS
(iTHC)
RETENTION TIME
IN CM.
o.-bS •
*
•
/
COUNTS
\^i.f>
•
•
SPAN
•
ATTENUATION
•
*
DILUTION FACTOR
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•
•
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COMPOUND
/3"Y
CONCENTRATION AS
BENZENE
0-oMj
•
•-
TRW
CNVIRONMENTAL
-------
GC WORKSHEET
COLUMN:
RUN NUMBER:
DATE:
COMPOUND
n ^A
\2 ^
f 3 (
* \
fs \
L
l^ENZEN
j/OLUEW
t
•
XJLENE
1
TOTAL
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(ifc)
RETENTION TIME
IN CM.
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ENVIRONMENTAL CNGINEERINO DIVISION
-------
GC WORKSHEET
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RUN NUMBER:
DATE:
COMPOUND
Cl
<£X
C^ u*
c?
CB)
C*S
BENZENE
TOLUENE
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/
TOTAL
HYDRO-
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(|THC)
RETENTION TIME
IN CM.
o&b •
\,%(>
\^
•
/
COUNTS
H-loL
i*Y
32-
SPAN
U9^
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iSj6/
ATTENUATION
•
DILUTION FACTOR
(Diluted w/N2)
•
•
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CONCENTRATION AS
COMPOUND
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CONCENTRATION AS
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CNVIRONMEHTAL CNOINCERING DIVISION
-------
2,
GC WORKSHEET
COLUMN:
RUN NUMBER:
DATE:
COMPOUND
RETENTION TIME
IN CM.
COUNTS
SPAN
ATTENUATION
DILUTION FACTOR
(Diluted w/N2)
CONCENTRATION AS
COMPOUND
CONCENTR£HtJN AS
f 33
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TOTAL
HYDRO-
CARBONS
(iTHC)
ENVIRONMENTAL ENGINEERING DIVISION
-------
GC WORKSHEET
COLUMN:
RUN NUMBER:
tri-P -
DATE:
cs
COMPOUND
cv
C2
C3
C^ ui2-
c57^
r / ^
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TOTAL
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RETENTION TIME
IN CM.
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-------
GC WORKSHEET
COLUMN:
'J-
RUN NUMBER; J/f f-
DATE:
COMPOUND
RETENTION TIME
IN CM.
COUNTS
SPAN
ATTENUATION
DILUTION FACTOR
(Diluted w/N2)
CONCENTRATION AS
COMPOUND
CONCENTRATION AS
BENZENE
\,ol
k
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TO
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CNVIRONMENTAL £NGINEEKING DIVISION
-------
APPENDIX D
SAMPLING METHODS AND ANALYTICAL TECHNIQUE
-------
503 OIL AND GREASE
In the determination of oil and grease.
an absolute quantity of a specific sub-
stance is not measured. Rather, groups of
substances with similar physical charac-
teristics are determined quantitatively on
the basis of their common solubility in tri-
chlorotrifluoroethane. "Oil and grease" is
an> material recovered as a substance sol-
uble in trichlorotrifluoroethane. It in-
cludes other material extracted by the
solvent from an acidified sample (such as
sulfur compounds, certain organic dyes.
and chlorophyll) and not volatilized during
the test. It is important that this limitation
be understood clearly. Unlike some con-
stituents that represent distinct chemical
elements, ions, compounds, or groups of
compounds, oils and greases are defined
by the method used for their determina-
tion.
The methods presented here are suit-
able for biological lipids and mineral hy-
drocarbons. They also may be suitable for
most industrial wastewaters or treated ef-
fluents containing these materials, al-
though sample complexity may result in
cither low. or high results because of lack
of analytical specificity. The method is not
applicable to measurement of low-boiling
fractions that volatilize at temperatures
below 70 C.
1. Significance
Certain constituents measured by the oil
and grease analysis may influence waste-
water treatment systems. If present in ex-
cessive amounts, they may interfere with
aerobic and anaerobic biological process-
es and lead to decreased wastewater treat-
ment efficiency. When discharged in
wastewater or treated effluents, they max
cause surface films and shoreline deposit*
leading to environmental degradation.
A knowledge of the quantity of oil and
grease present is helpful in proper desigr
and operation of wastewater treatment
systems and also may call attention to cer-
tain treatment difficulties.
2. Selection of Method
For liquid samples, three methods arc
presented: the partition-gravimetric meth-
od (A), the partition-infrared method
(B). and the Soxhiet method (C). Meth
od B is designed for samples that migh:
contain volatile hydrocarbons that other
wise would be lost-in the solvent removx
operations of the gravimetric procedure
Method C is the method of choice uher
relatively polar, heavy petroleum fra*
tions are present, or when the level> *''
nonvolatile greases may challenge the >oi-
ubility limit of the solvent. For low lewi-
of oil and grease (<10 mg'L). Method B :•
the method of choice because gravimetn.
methods do not provide the needed pre^i
sion.
Method D is a modification of the So\
hlet Method and is suitable for sludges arc
similar materials. Method E can be used;'
-------
OL « GREASE/Pmrtition-Gravim^ric Method
461
conjunction with Methods A. B. C, or D to
obtain a hydrocarbon measurement in ad-
dition to. or instead of. the oil and grease
measurement. This method separates hy-
drocarbons from the total oil and grease
on the basis of polarity.
3. Sampling and Storage
Collect a representative sample in a
wide-mouth glass bottle that has been
rinsed with the solvent to remove any de-
tergent film, and acidify in the sample
bottle. Collect a separate sample for an oil ,
and grease determination and do not suit.
divide in the laboratory. When informa-
tlon is requirefTabout average grease con-
centration over an extended period, exam-
ine individual portions collected at
prescribed time intervals to eliminate loss-
es of grease on sampling equipment during
collection of a composite sample.
In sampling sludges, take every possible
precaution to obtain a representative
sample. When analysis cannot be made
immediately, preserve samples withlmL
cone HCI/80 g sample. Never pfeserve
samples witn CHtl3 or sodium benzoate.
503 A. Partition-Gravimetric Method
1. General Discussion
a. Principle: Dissolved or emulsified oil
and grease is extracted from water by in-
timate contact with trichlorotriffuoro-
tthane. Some extractables, especially
unsaturated fats and fatty acids, oxidize
readily; hence, special precautions regard-
ing temperature and solvent vapor dis-
placement are included to minimize this
effect.
b. Interference: Trichlorotrifluoroelhane
has the ability to dissolve not only oil
and grease but also other organic sub-
stances. No known solvent will selectively
dissolve only oil and grease. Solvent re-
moval results in the loss of short-chain hy-
drocarbons and simple aromatics by vol-
atilization. Significant portions of petro-
leum distillates from gasoline through No.
2 fuel oil are lost in this process. In addi-
tion, heavier residuals of petroleum may
contain a significant portion of materials
that are not extractabie with the solvent.
2. Apparatus
a. Separator? funnel. 1 L, with TFE*
aopcock.
Tiffin or equivalent.
b. Distilling flask, 125 mL.
r. Water bath.
d. Filter paper, llcmdiam.t
3. Reagents
a. Hydrochloric acid, HC1. 1 + 1.
b. Trichlorotrifluoroethanet (1.1.2-tri-
chloro-1.2,2-trifluoroethane). boiling' point
47 C. The solvent should leave no mea-,ur-v
able residue on evaporation; distill if nee-/
essary. Do not use any plastic tubing to
transfer solvent between containers.
r. Sodium sulfate. NajSO4. anhydrous
crystal.
4. Procedure
Collect about 1 L of sample and mark
sample level in bottle for later determina-
tion of sample volume. Acidify to pH 2 or
lower; generally. 5 mL HCI is sufficient.
Transfer to a separatory funnel. Carefully
rinse sample bottle with 30 mL tri-
chlorotrifluoroethane and add solvent
washings to separatory funnel. Preferably
shake vigorously for 2 min. However, if it
tWhatman No. 40 or equivalent.
tFreon or equivalent.
-------
462
ORGANIC CONSTITUENTS (500)
is suspected that a stable emulsion will
farm, shake gently for 5 to 10 min. Let lay-
ers separate. Drain solvent layer through a
funnel containing solvent-moistened filter
paper into a clean, tared distilling flask. If
a clear solvent layer cannot be obtained.
add I g Na.SC), to the filter paper cone and
slowly drain emulsified solvent onto the'
crystals. Add more Na.SO4 if necessary.
Extract twice more with 30 mL solvent
each but first rinse sample container with
each solvent portion. Combine extracts in
tared distilling flask and wash filter paper
with an additional 10 to 20 mL solvent.
Distill solvent from distilling flask in a wa-
ter bath at 70 C. Place flask on a water
bath at 70 C for 15 min and draw air
through it with an applied vacuum for the
final I min. Cool in a desiccator for 30 min
and weigh.
5. Calculation
If the organic solvent is free of residue.
the gain in weight of the tared distilling
flask is mainly due to oil and grease. Total
gain in weight. A. of tared flask less calcu-
lated residue. B. from solvent blank is the
amount of oil and grease in the sample:
(A - B) * 1.000
mL sample
mg oil and grease/L
6. Precision and Accuracy
Methods A. B. and C were tested by a
single laboratory on a sewage sample. B>
this method the oil and grease concentra-
tion was 12.6 mg/L. When 1-L portions of
the sewage were dosed with 14.0 mg of a
mixture of No. 2 fuel oil and Wesson oil.
recovery of added oils was 93*3 with a
standard deviation of 0.9 mg.
503 B. Partition-Infrared Method (TENTATIVE)
1. General Discussion
a. Principle: Although the extraction
procedure for this method is identical to
that of Method A. infrared detection per-
mits the measurement of many relatively
volatile hydrocarbons. Thus, the lighter
petroleum distillates, with the exception
of gasoline, may be measured accurately.
Adequate instrumentation allows for the
measurement of as little as 0.2 mg oil and
grease L.
h. Interference: Some degree of selec-
tivity is offered by this method to over-
come some/ of the coextracted inter-
ferences discussed in Method A. Heavier
residuals of petroleum may contain a sig-
nificant portion of materials insoluble in
trichlorotrifluoroethane.
r. Definitiiina: A "known oil" is de-
fined as a sample of oil and/or grease that
represents the only material of that type
used or manufactured in the processes
represented by a wastewater. An "un-
known oil" is defined as one for which a
representative sample of the oil or grease
is not available for preparation of a stan-
dard.
2. Apparatus
u. Separator? fiinne 1. I L. with TFE
stopcock.
h. Infrared spertrtiphntumeter. double
beam, recording.
c'. Cells, near-infrared silica.
d. Filter paper. II cm diam.*
3. Reagents
a. Hydnichlnric utid. HCI. I + I.
h. TricMtmttrifliuwtlmnc. See503A..Vv
c-. Sodium sulfute. Na;SO4. anhydrous.
crystal.
•Teflon or equivalent.
tWhatman No. 40 or equivalent.
-------
ON. & GREASE/Soxhlet Extraction Mtfhod
463
d. Reference ink Prepare a mixture, by
volume, of 37.5^r iso-octane. 37.5*3- hex-
adecane. and 25** benzene. Store in
sealed container to prevent evaporation.
4. Procedure
Refer to Method A for sample collec-
tion, acidification, and extraction. Collect
combined extracts in a 100-mL volumetric
rtask and adjust final volume to 100 mL
with solvent.
Prepare a stock solution of known oil by
rapidly transferring about 1 mL (0.5 to 1.0
gi of the oil or grease to a tared 100-mL
volumetric flask. Stopper flask and weigh
to nearest milligram. Add solvent to dis-
solve and dilute to mark. If the oil identity
i% unknown (f It) use the reference oil
ir 3t/> as the standard. Using volumetric
technics, prepare a series of standards
over the range of interest. Select a pair of
matched near-infrared silica cells. A I-cm-
path-length cell is appropriate for a work-
ing range of about 4 to 40 mg. Scan stan-
dards and samples from 3.200 cm"1 to
2.700 cm"' with solvent in the reference
beam and record results on absorbance
paper. Measure absorbances of samples
and standards by constructing a straight
baseline over the scan range and measur-
ing absorbance of the peak maximum at
2.930 cm"1 and subtracting baseline ab-
sorbance at that point. If the absorbance
exceeds 0.8 for a sample, select a shorter
pathlength or dilute as required. Use scans
of standards to prepare a calibration
curve.
5. Calculation
mg oil and grease.'L
A x l.OQO
mL sample
where:
A » mg of oil or grease in extract as deter-
mined from calibration curve.
6. Precision and Accuracy
See 503A.6. By this method the oil and
grease concentration was 17.5 mg L.
When 1-L portions of the sewage were
dosed with 14.0 mg of a mixture of No. 2
fuel oil and Wesson oil. the recovery of
added oils was 999c with a standard devia-
tion of 1.4 mg.
503 C. Soxhlet Extraction Method
i General Discussion
a. Principle: Soluble metallic soaps are
Indrolyzed by acidification. Any oils and
x>lid or viscous grease present are sepa-
rated from the liquid samples by filtration.
After extraction in a Soxhlet apparatus
»i(h trichlorotrifluoroethane. the residue
remaining after solvent evaporation is
*tighed to determine the oil and grease
>offlent. Compounds volatilized at or be-
lo» 103 C will be lost when the filter is
Jned.
*. Interference: The method is entirely
empirical and duplicate results can be ob-
tained only by strict adherence to all de-
tails. By definition, any material recov-
ered is oil and grease and any tiitrable tri-
chlorotrifluoroethane-soluble substances.
such as elemental sulfur and certain organ-
ic dyes, will be extracted as oil and grease.
The rate and time of extraction in the
Soxhlet apparatus must be exactly as di-
rected because of varying solubilities of
different greases. In addition, the length of
time required for drying and cooling ex-
tracted material cannot be varied. There
may be a gradual increase in weight, pre-
sumably due to the absorption of oxygen.
and/or a gradual loss of weight due to vol-
atilization.
-------
464
ORGANIC CONSTITUENTS (500)
2. Apparatus
a. Kxlmcliiw apparatus. Soxhlet.
h. Vacuum pump or other source of
vacuum.
c'. Ruchm-r funnel. 12 cm.
J. Electric lieatinn mantle.
f. £\7rif(7/iw tlu'nihle. paper.
./". Filter paper. 1 1 cm diam.*
V- MiHtlin ft»tli /.\Av. II cm diam.
3. Reagents
sludge. After drying- the oil and grea>e
can be extracted with trichlorotrifluoro-
ethane.
sulfate monohydrate is capable of com- h. Interference: See 503C. l/».
-------
ft GREASE/Hydrocvbons
465
2. Apparatus
a. Extraction apparatus. Soxhlet.
b. Vacuum pump or other source of
vacuum.
c. Extraction thimble, paper.
d. Crease-free cotton: Extract non-
absorbent cotton with solvent.
3. Reagents
a. Hydrochloric acid. HCI. cone.
b. Magnesium xitljate inonohytlrate:
Prepare MgSO.-HjO by overnight drying
of a thin layer in an oven at 150 C.
r. Trichlorntrifinorm'thane: See 503A.3A.
4. Procedure
In a 150-mL beaker weigh a sample of
wet sludge. 20 ± 0.5 g. of which the dry-
\olids content is known. Acidify to pH 2.0
(generally. 0.3 ml_ cone HCI is sufficient).
Add 25 g MgSO4 H2O. Stir to a smooth
paste and spread on sides of beaker to fa-
cilitate subsequent removal. Let stand un-
til solidified. 15 to 30 min. Remove solids
and grind in a porcelain mortar. Add the
powder to a paper extraction thimble.
Wipe beaker and mortar with small pieces
of filter paper moistened with solvent and
add to thimble. Fill thimble with glass
wool or small glass beads. Extract in a
Soxhlet apparatus, using trichlorotri-
fluoroethanc. at a rate of 20 cycles/hr for 4
hr. If any turbidity or suspended matter is
present in the extraction flask, remove by
filtering through grease-free cotton into
another weighed flask. Rinse flask and cot-
ton with solvent. Distill solvent from ex-
traction flask in water at 70 C. Place flask
on a water bath at 70 C for 15 min and
draw air through it using an applied vacu-
um for the final ] min. Cool in a desiccator
for 30 min and weigh.
5. Calculation
Oil and grease as 9c of dry solids
gain in weight of flask, g x |QQ
weight of wet solids, g x dry solids fraction
6. Precision
The examination of six replicate sam-
ples of sludge yielded a standard deviation
of4.6C?.
503 E. Hydrocarbons
1. Significance
In the absence of specially modified in-
dustrial products, oil and grease is com-
posed primarily of fatty matter from ani-
mal and vegetable sources and hydro-
carbons of petroleum origin. A knowledge
of the percentage of each of these constit-
uents in the total oil and grease minimizes
the difficulty in determining the major
source of the material and simplifies the
correction of oil and grease problems in
•astewater treatment plant operation and
>tream pollution abatement.
2. General Discussion
n. Principle: Silica gel has the ability to
absorb polar materials. If a solution of hy-
drocarbons and fatty materials in tri-
chlorotrifluoroethane is mixed with silica
gel. the fatty acids are selectively removed
from solution. The materials not eliminat-
ed by silica gel adsorption are designated
hydrocarbons by this test.
b. Interference: The more polar hydro-
carbons, such as complex aromatic com-
pounds and hydrocarbon derivatives of
chlorine, sulfur, and nitrogen, may be ad-
-------
OXYGEN DEMAND (CHEMICAL)
489
rection is unnecessary if dilution water
meets the blank criteria stipulated above.
If the dilution water does not meet these
criteria, proper corrections are difficult
ind results become questionable.
7. Precision and Accuracy
In a series of interlaborutory studies.
each involving K6 to 102 laboratories (and
as man) river water and wastewater
seedsi. 5-da> BOD measurements were
nude on svnthetn: water samples contain-
mg a 1:1 mixture of glucose and glutamic
acid in the total concentration range of 5 to
.UO mg L. The regression equations for
mean value. T. and standard deviation. 5.
from these studies were:
T » O.f*5 udded level. mgL) - 0.149
5*0.120 (added level, mg L) - 1.04
For the 300-mg L mixed primary standard.
the average 5-dav BOD was 199.4 mg L
with a standard deviation of 37.0 mg L.
6 References
I Yin\c. J.I I9"9. Chemical methods for
nitrification control. J. Hn/ir Pullm.
f,J. 45:637.
I l.S. t->VIR(IV\l|N| AL PROJtlTHIN
rv. OFFICE ot RESEARCH A DEVFLOP-
MEST. ENVIRONMENTAL MONITORING &
SrmiRi LABORATORY. CINCINNATI. OHIO.
1978. Personal communication. D.W. Bal-
linjer to C.N. McDermott.
9. Bibliography
THFMIAII r. H.J.. P.D MtNAMM & C.T.
Bi TTIRHHIV 1931. Selection of dilution
water for use in oxygen demand tests, fiih.
Hi-tilth Kt-p. 48:1084.
Li \. W.L & M.S. Nit HOLS. 1937. Influence of
phosphorus and nitrogen on biochemical
oxygen demand. 5e»ETT & H.R. RAMH». 1950 Experience
with modified methods for BOD. 5r»
-------
490
ORGANIC CONSTITUENTS (500)
di/ed it' they have sufficient contact with
the oxidants.- While the carbonaceous
portion ol' nitrogen-containing organic
matter is oxidized, no oxidation of am-
monia, either present in a waste or liber-
ated from the nitrogen-containing organic
matter, takes place in the absence of sig-
nificant chloride concentrations.
2. Sampling and Storage
lest unstable samples without delay.
Homogenize samples containing settleable
solids in a blender lo permit representative
sampling, inhere Js.jpJ»LA delay before
analysis, preserve life sample .by acid-
ification to pH 2 or lower with cone sulfu-
ric -acid THjSO.,). Make preliminary dilu-
tions lor wastes containing a high COD to
reduce the error inherent in measuring
small volumes of sample.
508 A. Dichromate Reflux Method
i General Discussion
u. I'ri'h //i/i-.- Most types of organic mat-
ter are oxidiied by a boiling mixture of
chromic and sulfuric acids. A sample is re-
Ihixcd in strongly acid solution with a
known excess of potassium dichromaie.
iK.Cr.O:i. After digestion the remaining
unreduced K^Cr^O? is titrated withjerrous
ammp.oium *uliate i£ASJ. the amount of
K.-Cr.-Or consumed is determined, and the
amount of oxidizable organic matter is cal-
culated in terms of oxygen equivalent.
h. //i/ir/t'mifw iiiiii HniitiitH>n.\: Vola-
tile straight-chain aliphatic compounds are
not oxidi/ed to any appreciable extent.
1 his failure occurs partly because volatile
orpinics are present in the vapor space
and do not come in contact with the oxi-
di/ing liquid. Straight-chain aliphatic com-
pounds are oxidized more effective!)
when silver sulfate (Ag:SO() is added as a
catalyst. Howeve'r. Ag^SO, reacts with
chloride, Mromidc. and iodide to produce
precipitates that are oxidized only partial-
ly. The difficulties caused by the presence
of halides can be largely, though not com-
pletely, overcome by complexing with
mercuric sulfate \ add 10 mg sulfamic
acid mg NO; -N present in the refluxing
flask. Also add the same amount of sul-
famic acid to the reflux flask containing
the distilled water blank.
Reduced inorganic species such as fer-
rous iron, sulfide. manganous manganese.
etc.. are oxidized quantitatively under the
test conditions. For samples containing
significant levels of these species, stoi-
chiometric oxidation can be assumed
from known initial concentration of the in-
terfering species and corrections can be
made to the COD value obtained.
t\ Minimum JrU-iliihlc i-tnnTHtruiii>ii:
Determine COD values of >50 mg L using
0.250.V K,Cr..O:. With 0.025.N K..Cr.O-.
COD values from 5 to 50 mg. L can be de-
termined but with lesser accuracy.'
2. Apparatus
Retfux apparatus, consisting of 500-mL
-------
OXYGEN DEMAND (CHEMICAL)/Dic*romat» Reflux Method
or 250-mL erlenmeyer flasks with ground-
glass 24 40 neck" and 300-mm jacket Lie-
big. West, or equivalent condensers. +
with 24-40 ground-glass joint, and a hot
plate having sufficient power to produce at
least 1.4 Wcnv of heating surface, or
equivalent.
3. Reagents
491
titii\siiim dii-hromate s
ti,m. 0.250V: Dissolve 12.259 g K.-Cr/):.
primary standard grade, previously dried
at 103 C for 2 hr. in distilled water and
dilute to 1.000m L.
h. Sili-rr MI!l,iit-. Ag.SO,. reagent or
technical grade, crystals or powder.
t. Stiltiirii- mill reiigent: Add Ag;SOt to
cone H;SO, at the rate of 22 g Ag;SO»4 kg
bottle. Let stand I to 2 days to dissolve
AfcSO,.
d. Siiltiirii in-ill. H..SOi. cone.
e. ri-rritin imlii-utiir .\n: Dissolve
1.48? g I.IO-phenanthroline monohydrate
and 69? mg FeSO,-7H..O in distilled waier
and dilute to 100 mL. This indicator solu-
tion max be purchased already prepared. +
f. Stuiiiliinl fern>u!t iintiitiininnt siilfiiie
titraat. approximately 0.25V: Dissolve 98
I Fe(NH,MSO,),-6H..O (FAS) in distilled
water. Add 20 mL cone H.-SO,. cool, and
dilute to 1.000 mL. Standardize this solu-
tion daily against standard K.-Cr-O: solu-
tion, as follows:
Dilute 10.0 mL standard K;Cr..O: solu-
tion to about 100 mL. Add 30 mL cone
H;SO, and cool. Titrate with FAS titrant.
osing 0.10 to 0.15 mL (2 to 3 drops) ferroin
indicator.
Normality of FAS solution
Volume 0.23.V K.CrzO.
: solution titrated. mL
Volume FAS used in titration. mL
x 0.2?
*Conmf 5000 or equivalent.
•Cormoj 23«. »I54«. or equivalent.
=G F. S«Mh Chemical Co.. Cohimfetn. Onw.
g. Mnrurir sulfaie: Hf SO,, crystals or
powder.
h. Siilfumic iidil: Required only if the
interference of nitrites is to be eliminated
(see f Ih above).
/'. PiHusxium hyilntjten phthalate stun-
Jnnl: Lightly crush and then dry PO'^S-
sium acid phthalate (HOOCCH.COOKi
to constant weight at 120 C. dissolve 425
mg in distilled water, and dilute to 1.000
mL. Potassium hydrogen phthalate has a
theoretical COD of 1.176 g Oyg and this
solution has a theoretical COD of 500 mg
O»L. Prepare fresh for each use.
4. Procedure
i*. Treat mem «>/' samples with s.VJ mg
C()f>L: Place 50.0 mL sample (for sam-
ples with COD >VOO mg COD'L. use a
smaller sample portion diluted to 50.0 mL)
in the 500-mL refluxing flask. Add I g
HgSO,. several glass beads, and very
slowly add 5.0 mL sulfuric acid reagent.
with mixing to dissolve HgSO4- Cool while
mixing to avoid possible loss of volatile
materials. Add 25.0 mL 0.250V K..Cr,0:
solution and mix. Attach flask to condens-
er and turn on cooling water. Add remain-
ing sulfuric acid reagent (70 mL) through
open end of condenser. Continue swirling
and mixing while adding sulfuric acid re-
agent. CAL I ION: .U/.v reflux mixture tliar-
iniKhly hefure applying heat to prevent h>-
ciil heating iifffiuk huttitm ami a pn\xihle
Mtnvout afjHu\i ciuiteMx. If sample vol-
umes other than 50 mL are used, keep ra-
tios of reagent weights, volumes, and
strengths constant. See Table 508:1 for ex-
amples of applicable ratios. Maintain
these ratios and follow the procedure as
outlined above.
Use I g HgSOi with a 50.0-mL sample
to complex up to a maximum of 100 mg
chloride (2.000 mg'L) For smaller samples
use less HgSO4. according to the chloride
concentration: maintain a 10:1 ratio of
HgSO,:CI. A slight precipitate does not
affect the determination adversely. Gener-
-------
492
ORGANIC CONSTITUENTS (500)
Sample
Si/e
.MIX: I. R| M,l M Ql
0.25V
Standard
Dichromate
ml
AND No«MM ITIIS MIR V 4HIOI S SfMPI L Sl7tS
Sulfurk
Acid
Reagent
mf.
15
30
- -_45
60
75
HgSO.
02
0.4
-0.6
0.8
1.0
Normality
of
FAS
005
010
015
0.20
0.25
Final
Volume
before
Titration
mL
70
140
210
2«0
350
ally. COD cannot be measured accurate!)
in samples containing more than 2.000 mg
chloride L.
Reflux mixture for 2 hr. L'se a shorter
peruvJ tor particular wastes if it has been
shown that the shorter period yields the
same COD as that found b> 2-hr refluxing.
Cover open end of condenser with a small
beaker to prevent foreign material from
entering refluxing mixture. Cool and wash
down condenser with distilled water.
Disconnect reflux condenser and dilute
mixture to about twice its volume with dis-
tilled water. Cool to room temperature
and titrate excess KjCr^Or with FAS. us-
ing 0.10 to 0.15 mL (2 to 3 drops) ferroin
indicator. Although the quantity of ferroin
indicator is not critical, use the same vol-
ume lor all titrations. Take as the end
point of the titration the first sharp color
change from blue-preen to reddish brown.
The blue-green ma> reappear.
Rcllux and titrate in the same manner a
blank containing the reagents and a vol-
ume of distilled water equal to that of
sample.
h. Alternate pruti-Jurc -fur Itn\--Ct)l)
Minifl, \: Follow the above procedure.
* 4 of a weight ratio of 10:1.
HgSO4:CI. using the amount of chloride
present in the original volume of sample.
Carry a blank reagent through the same
procedure.
This technic has the advantage of con-
centrating the sample without significant
losses of easily digested volatile materials.
Hard-to-digest volatile materials such a*
volatile acids are lost, but an improvement
is gained over ordinary evaporative con-
centration methods.
f. Dctrrininiiliiin nf Miiiiiliinl \nlntitin:
Evaluate the technic and quality of re-
agents by testing a standard potassium h\-
drogen phthalate solution.
5. Calculation
mg COD L
1.4 - flt > .V x K.QOQ
mL vitnpfc
where:
A • volume FAS used Tor Hank. mL.
B • volume FAS used for sample. mL.
.V • normality of FAS.
-------
PESTICIDES XORGANlQ/Organocttorirw PM*CK*S
493
6 Precision and Accuracy
A set of synthetic samples containing
potassium hydrogen phthulute and NaCI
•is tested by 74 laboratories.* At 200 mg
COD-L in the absence or chloride, the
standard deviation was z 13 mg/L (coeffi-
cient of variation. 6.5%). At 160 mgCOOL
and 100 mg chloride/L the standard de-
viation was = 14 mg/L (coefficient of vari-
ation.
508 B. References
MDORL. \V A . R. C. KnoNtR & C.C.
RUHHOI i. 1949. Dtchromale reflux meih-
ftl for Jeterminaiion of o\ygen consumed.
Anal. Chem. 2I:9J3.
MOOKE. VV.A.. F. J. LitJ/*cK &
C.C. RICHHOFT. 1951. Deiermifution of
oxvfen-con^umed values of organic wastes.
Anal. Chrm. 23:1297.
MEDALIA. A.I. 1951. Test for traces of or-
ganic mailer in water. Aunt. C/irm. 23:13IK.
DOHHS. R.A. & R.T. Wu i i\xis. l%3. Klimi
nation of chloride interference in the chem-
ical ox>gen demand te*t. .Ami/ ( Inm
35:1064.
ANALVTITAI. REFERENCE SERVICF. USHHW-
PHS. 1965. Oxygen Demand No. 2. Study
No. 21. Environmental Health Ser.. W^ter.
PHS Publ. No. 999-WP-26.
-------
ORGANIC CARBON, TOTAL
Method 415.1 (Combustion or Oxidation)
STORET NO. Total 00680
Dissolved 00681
1. Scope and Application
1.1 This method includes the measurement of organic carbon in drinking, surface and saline
waters, domestic'and industrial wastes. Exclusions are noted under Definitions and
Interferences.
1.2 The method is most applicable to measurement of organic carbon above 1 mg/1.
2. Summary of Method
2.1 Organic carbon in a sample is converted to carbon dioxide (CO2) by catalytic combustion
or wet chemical oxidation. The CO2 formed can be measured directly by an infrared
detector or converted to methane (CH4) and measured by a flame ionization detector.
The amount of CO2 or CH4 is directly proportional to the concentration of carbonaceous
material in the sample.
3. Definitions
3.1 The carbonaceous analyzer measures all of the carbon in a sample. Because of various
properties of carbon-containing compounds in liquid samples, preliminary treatment of
the sample prior to analysis dictates the definition of the carbon as it is measured. Forms
of carbon that are measured by the method are:
A) soluble, nonvolatile organic carbon; for instance, natural sugars.
B) soluble, volatile organic carbon; for instance, mercaptans.
C) insoluble, partially volatile carbon; for instance, oils.
D) insoluble, paniculate carbonaceous materials, for instance; cellulose fibers.
E) soluble or insoluble carbonaceous materials adsorbed or entrapped on insoluble
inorganic suspended matter; for instance, oily matter adsorbed on silt particles.
3.2 The final usefulness of the carbon measurement is in assessing the potential oxygen-
demanding load of organic material on a receiving stream. This statement applies
whether the carbon measurement is made on a sewage plant effluent, industrial waste, or
on water taken directly from the stream. In this light, carbonate and bicarbonate carbon
are not a part of the oxygen demand in the stream and therefore should be discounted in
the final calculation or removed prior to analysis. The manner of preliminary treatment
of the sample and instrument settings defines the types of carbon which are measured.
Instrument manufacturer's instructions should be followed.
Approved for NPDES
Issued 1971
Editorial revision 1974
415.1-1
-------
4. Sample Handling and Preservation
4.1 Sampling and storage of samples in glass bottles is preferable. Sampling and storage in
plastic bottles such as conventional polyethylene and cubitainers is permissible if it is
established that the containers do not contribute contaminating organics to the samples.
NOTE 1: A brief study performed in the EPA Laboratory indicated that distilled water
stored in new, one quart cubitainers did not show any increase in organic carbon after
two weeks exposure.
4.2 Because of the possibility of oxidation or bacterial decomposition of some components of
aqueous samples, the lapse of time between collection of samples and start of analysis
should be kept to a minimum. Also, samples should be kept cool (4*Q and protected
from sunlight and atmospheric oxygen.
4.3 In instances where analysis cannot be performed within two hours (2 hours) from time of
sampling, the sample is acidified (pH < 2) with HC1 or H2SO4.
5. Interferences
5. 1 Carbonate and bicarbonate carbon represent an interference under the terms of this test
and must be removed or accounted for in the final calculation.
5.2 This procedure is applicable only to homogeneous samples which can be injected into the
apparatus reproducibly by means of a microliter type syringe or pipette. The openings of
the syringe or pipette limit the maximum size of particles which may be included in the
sample.
6. Apparatus
6.1 Apparatus for blending or homogenizing samples: Generally, a Waring-type blender is
satisfactory.
6.2 Apparatus for total and dissolved organic carbon:
6.2.1 A number of companies manufacture systems for measuring carbonaceous
material in liquid samples. Considerations should be made as to the types of
samples to be analyzed, the expected concentration range, and forms of carbon to
be measured.
6.2.2 No specific analyzer is recommended as superior.
7. Reagents
7.1 Distilled water used in preparation of standards and for dilution of samples should be
ultra pure to reduce the carbon concentration of the blank. Carbon dioxide-free, double
distilled water is recommended. Ion exchanged waters are not recommended because of
the possibilities of contamination with organic materials from the resins.
7.2 Potassium hydrogen phthalate, stock solution, 1000 mg carbon/liter: Dissolve 0.2128 g
of potassium hydrogen phthalate (Primary Standard Grade) in distilled water and dilute
to 100.0 ml.
NOTE 2: Sodium oxalate and acetic acid are not recommended as stock solutions.
7.3 Potassium hydrogen phthalate, standard solutions: Prepare standard solutions from the
stock solution by dilution with distilled water.
7.4 Carbonate-bicarbonate, stock solution, 1000 mg carbon/liter: Weigh 0.3500 g of sodium
bicarbonate and 0.4418 g of sodium carbonate and transfer both to the same 100 ml
volumetric flask. Dissolve with distilled water.
415.1-2
-------
7.5 Carbonate-bicarbonate, standard solution: Prepare a series of standards similar to step
7.3.
NOTE 3: This standard is not required by some instruments.
7.6 Blank solution: Use the same distilled water (or similar quality water) used for the
preparation of the standard solutions.
8. Procedure
8.1 Follow instrument manufacturer's instructions for calibration, procedure, and
calculations.
8.2 For calibration of the instrument, it is recommended that a series of standards
encompassing the expected concentration range of the samples be used.
9. Precision and Accuracy
9.1 Twenty-eight analysts in twenty-one laboratories analyzed distilled water solutions
containing exact increments of oxidizable organic compounds, with the following results:
Increment as
TOC
ing/liter
4.9
107
Precision as
Standard Deviation
TOC. ing/liter
3.93
8.32
Bias,
Accuracy as
Bias,
ing/liter
+ 15.27
+ 1.01
-1-0.75
+ 1.08
(FWPCA Method Study 3, Demand Analyses)
Bibliography
t
1. Annual Book of ASTM Standards, Part 31, "Water", Standard D 2574-79, p 469 (1976).
2. Standard Methods for the Examination of Water and Wastewater, 14th Edition, p 532,
Method 505, (1975).
415.1-3
-------
APPENDIX E
TEST LOG
-------
APPENDIX E - TEST LOG
Date
Time
Task Performed (with comments)
8/1/83
8/2/83
8/3/83
0800 TRW Test Crew and EPA representative arrive at the Chevron
facility in El Segundo, California.
0830 Chevron provides introductory/safety meeting.
0900 Crew begins set-up at test sites. Problems with electricity
supply, safety restrictions, and hot work permits cause
delay in commencing the test period.
1630 Crew departs test facility.
0800 TRW Test Crew and EPA representative arrive at the Chevron
facility.
0900 Chevron contact having problems with obtaining hot work
permit and safety guidelines.
1300 One of the two DAF tanks is down for repair. The off-line
DAF unit will be tested for a background level.
1500 Chevron requires a TRW operator on-site with the test
instruments. Therefore, shift work is required.
1700 Crew departs test facility.
0600 TRW Test Crew and EPA representative arrive at the Chevron
facility.
0830 Chevron personnel supply Hot Work Permit.
0945 Continuous hydrocarbon monitors placed on-line for testing
at DAF 202 and DAF 302 sample locations. (DAF 202 - Beckman
400 Analyzer, DAF 302 - Beckman 400 Analyzer),
1030 DAF 202 #1 gas bag sample.
1045 Beckman 400 with DAF 202, flames out. Lite and recalibrated.
1135 DAF 202 #2 gas bag sample.
1140 Beckman 400 with DAF 202, flames out. Lite and recalibrated,
1200 Beckman 400 with DAF 202 flames out. Therefore, switch
instruments with Beckman 400/DAF 302. The DAF 302 tank was
down for repair and hydrocarbon level was slightly above
ambient (= 15 ppm).
-------
Date Time Task Performed (with comments)
1200 Liquid composite samples started at DAF-IN, DAF-OUT, and
(cont.) equalization tank sample location. Because DAF 302 was
down for repair and not being sample, the DAF 202 being
tested was referenced only as DAF.
1235 Continuous hydrocarbon monitors placed on-line for testing
at equalization tank sample location.
1445 DAF #202 gas bag sample #3.
1600 Equalization tank gas bag sample #1.
1650 Liquid VOA samples at DAF-IN, DAF-OUT, and Equalization
tank.
1900 Crew departs test facility with the exception of the
continuous analyzers operator. Night operator worked
1800-0600.
8/4/83 0600 Morning operator replace night operator.
0900 TRW Test Crew and EPA representative arrive at the Chevron
facility. Liquid composite samples started at DAF-IN,
DAF-OUT, and Equalization OUT.
0930 DAF gas bag sample #1 (DAF 202 referenced as DAF after
DAF 302 was taken off-line).
1000 Liquid VOA samples at DAF-IN, DAF-OUT, and Equalization
OUT.
1053 Equalization OUT gas bag sample #1.
1430 DAF gas bag sample' #2.
1431 Equalization OUT gas bag sample #2.
1500 Liquid VOA sample at DAF-IN, DAF-OUT, and Equalization
OUT.
1800 Crew departs test facility with night operator arriving
for night shift.
-------
Date
Time
Task Performed (with comments)
8/5/83
8/8/83
8/9/83
0600 Morning operator replaces night operator.
0900 TRW Test Crew and EPA representative arrive at Chevron
facility. Liquid composite sampled and VOA samples taken
at DAF-IN, DAF-OUT, and Equalization OUT. DAF gas bag
sample #1.
0930 Equalization OUT gas bag sample #1.
1228 Equalization OUT gas bag sample #2.
1400 Moved Beckman 402 Analyzer from the Equalization OUT
sample location to the Equalization tank carbon house
outlet vent. Carbon house gas sample bag.
1500 DAF gas bag sample #2. Liquid VOA samples at DAF-IN,
DAF-OUT, and Equalization OUT.
1600 End of test at Equalization tank carbon house.
1700 End of test at DAF. Flame-out all instruments and packed
for weekend.
1800 Crew departs test facility.
0830 TRW Test Crew and EPA representative arrive at Chevron
facility.
1100 Beckman 400 on-line at DAF 202. DAF gas bag sample #1.
Liquid composite and VOA at DAF.
1200 Chevron personnel will take API liquid samples at API 201,
202, 203, 204, and API #4.
1500 DAF gas bag sample #2. Liquid VOA samples at DAF-IN and
DAF-OUT.
1800 Beckman 402 on-line at IAF outlet (before carbon drum).
1900 Crew departs test facility with night operator arriving
for night shift.
0600 Morning operator replaces night operator.
0900 TRW Test Crew and EPA representative arrive at Chevron
facility.
0915 DAF gas bag sample #1.
-------
Date
Time
Task Performed (with comments)
8/9/83
(cont.)
8/10/83
8/11/83
1000 Liquid composite and VOA samples at DAF-IN and DAF-OUT
Chevron personnel will take API liquid samples at API 201,
202, 203, 204 and API #4.
1140 T-201 (flocculation tank) gas bag sample; analyzed on
Beckman 400.
1400 DAF gas bag sample #2.
1510 T-200 (Flask/Mix tank) gas bag sample; analyzed on
Beckman 400.
1700 Liquid VOA samples at DAF-IN and DAF-OUT.
1800 Crew departs test facility with night operator arriving for
night shift.
0600 Morning operator replaces night operator.
0900 TRW Test Crew and EPA representative arrive at Chevron
facility.
0904 DAF gas bag sample #1.
1000 Liquid composite and VOA samples at DAF-IN and DAF-OUT.
Chevron personnel will take API liquid samples at API 201,
202, 203, 204 and API #4.
1205 Beckman 400 switched to DAF carbon house outlet (V-204).
V-204 gas bag sample.
1600 Liquid VOA samples at DAF-IN and DAF-OUT.
1800 Crew departs test facility with night operator arriving
for night shift.
0600 Morning operator replaces night operator.
0900 TRW Test Crew and EPA representative arrive at Chevron
facility. Liquid composite and VOA samples at DAF-IN and
DAF-OUT. Chevron personnel will take API liquid samples
at API 201, 202, 203, 204 and API #4.
0924 IAF gas bag sample #1.
1000 Liquid composite and VOA samples at IAF-IN and IAF-OUT.
1315 DAF gas bag sample #1.
-------
Date
Time
Task Performed (with comments)
8/11/83
(cont.)
8/12/83
1500 - All instruments off-line and flamed out.
1530 Liquid VOA sampels at DAF-IN and DAF-OUT.
1600 Liquid VOA samples at IAF-IN and IAF-OUT.
1700 Crew departs test facility.
0800 TRW Test Crew and EPA representative arrive at Chevron
facility.
0900 Beckman 402 on-line at IAF carbon drum outlet. Liquid
composite and VOA samples at IAF-IN and IAF-OUT. Chevron
personnel will take API liquid samples at API 201, 202,
203, 204, and API #4.
1129 Gas bag sample at Equalization tank outlet (Charcoal house
inlet); ran on Beckman 400.
1200 Beckman 402 switched to IAF outlet (Carbon drum inlet).
1213 IAF gas bag sample #2.
1230 Gas bag sample #1 at Equalization tank charcoal house outlet;
ran on Beckman 400.
1250 Liquid VOA samples at IAF-IN and IAF-OUT.
1259 Gas bag sample #2 at Equalization tank charcoal house
-outlet; ran on Beckman 400.
1500 All instruments off-line and flamed out.
1700 Crew departs test facility.
-------
APPENDIX F
PROJECT PARTICIPANTS
-------
PROJECT PARTICIPANTS
U.S. Environmental Protection Agency (Representatives)
Winton Kelly
Randy McDonald
Radian Corporation (NSPS Representatives)
Barry Mitsch
Chevron USA, Inc. (Plant Contacts)
Joe Monti
Joe Bacon
TRW, Inc. (Field Test Team)
Michael Hartman
Cecil Stackhouse
Carol Haney
Don Ackerman
Gary Henry
Dave Savia
------- |