ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
EPA-330/2-77-027
EMISSION TESTS
DOUGLAS OIL COMPANY
PARAMOUNT, CALIFORNIA
(September 12-13, 1977)
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
DENVER, COLORADO
AND
REGION IX
^
SAN FRANCISCO.CALIFORNIA
DECEMBER 1977
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ENVIRONMENTAL PROTECTION AGENCY
Office of Enforcement
EPA-330/2-77-027
EMISSION TESTS
DOUGLAS OIL COMPANY
Paramount, California
(September 12-13, 1977)
December 1977
National Enforcement Investigations Center - Denver
and
Reqior) IX - San Francisco
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CONTENTS
I INTRODUCTION . 1
II SUMMARY AND CONCLUSIONS 2
III PROCESS DESCRIPTION 3
IV TEST PROCEDURES 7
SAMPLING LOCATION 7
SAMPLING METFIODS 7
PROCESS OBSERVATION PROCEDURES . 11
V TEST RESULTS . 12
FIGURES
I Simplified Process Diagram 4
2 Scott Tail Gas Incinerator 8
TABLE
1 Data Summary . . . . . . .13
APPENDICES
A Presurvey Inspection Report
B Stack Sampling Equipment
C Volumetric Flow Rate Estimates
D Calibration Procedures and Data
E Chain-ofCustody Procedures and Records
F Analytical Procedures and Data
G Process Data
H Field Data Sheets and Example Calculations
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I. INTRODUCTION
Douglas Oil Company operates an oil refinery at Paramount,
California, with a rated capacity of from 6,400 to 7,200 m 3 (40,000 to
45,000 bbl)/day. A State Implementation Plan (SIP) inspection conducted
on September 22, 1975, by personnel from the National Enforcement
Investigation Center (NEIC) concluded that Douglas Oil had operating
problems with the incinerator treating the tail gas from the Shell
Clause off-gas treatment (SCOT) unit. 1 It was therefore recommended that
sulfur dioxide (SO 2 ) tests be conducted to determine the compliance of
the incinerator with regard to the applicable regulations. Region IX of
the Environmental Protection Agency (EPA) subsequently requested NEIC to
conduct a source test of the Scot tail gas incinerator.
On July 13, 1977, NEIC personnel conducted a presurvey inspection
to evaluate sampling locations and obtain process information [ Appendix A].
It was initially concluded that testing the SCOT tail gas incinerator
required construction of a sampling platform. After further consideration,
however, it was decided that an alternative sampling location, which did
not require the construction of a platform, could be used.
On September 12 and 13, 1977, NEIC conducted SO 2 source tests at
Douglas Oil Company. Tests were conducted to determine compliance with
Los Angeles Air Pollution Control D strict (LAAPCD)*. Rule 53.2 (Sulfur
Recovery Units) which limits SO 2 emissions to 500 parts per million
volume (ppmv) and 91 kg (200 lb)/hr.
State Implementation Plan Air Pollution Inspections of Douglas Oil
Colm7any, Los Angeles County, California, EPA, NEIC, Report No.
EP.4 $3/2-76-O 13. 1ebruary 1976.
* The Agency title has since been changed to Metropolitan Zone, South
Coast Air Quality Management District (MZ, SCAQMD); however, not all
the SIP revisions have been approved by EPA. The LAAPCD regulations
are considered applicable by EPA.
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II. SUMMARY AND CONCLUSIONS
1. On September 12 and 13, 1977, the SCOT unit inci nerator was source
tested for sulfur dioxide emission. Three runs were performed by
the required LAAPCD procedures. During testing, process operating
data were recorded, and it was determined that the SCOT unit was
operating normally. The associated Claus plant was operating at
a sulfur production rate of 16.3 m ton (17.9 ton)/day which was
within the normal range of operation.
2. The source test showed that the average SO 2 concentration and mass
emission rate were 120 ppmv and 2.6 kg (5.8 lb)/hr, respectively.
This SO 2 concentration was 23% of that allowed (500 ppmv) by LAAPCD
Rule 53.2. Further, the average SO 2 emission rate was only 3% of
the allowed emission rate (91 kg/hr or 200 lb/hr).
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III. PROCESS DESCRIPTION
The Douglas refinery processes crude oil from California (25%
Wilmington and 25% Ventura), Arabia (20%) and Bolivia or Indonesia
(30%). Naphthas and other cndensates from the Douglas refinery at Santa
Maria are also processed. Finished products include asphalt, low sulfur
fuel, diesel oil, JP-4 and JP-5 jet fuels and gasoline. The refinery
employs 120 people and operates three 8-hour shifts/day, 7 days week,
year round.
The major processes at the refinery are crude desalting, atmospheric
d stillation, vacuum distillation, catalytic reforming, distillate
hydrotreating, gas oil desulfurizatiori, naphtha desulfurization, asphalt
blowing and sulfur recovery [ Hgure 1]. Because NEIC was specifically
requested by Region IX to sample the sulfur recovery plant emissions,
this installation and its air pollution control equipment are more fully
discussed below.
Sour gases from the naphtha, distillate and gas oil hydrosulfurizing
units are processed in di-isopropanolamine (DIPA), absorption units. The
hydrogen sulfide (H 2 S) is selectively absorbed by the DIPA units and
removed from the gas stream. The cleansed gases are then introduced
into the refinery fuel gas stream. -
The H 2 S is stripped from the rich amine solution and recovered as
a concentrated gas stream. The resulting lean DIPA solution is
recycled to the absorption units. The concentrated H 2 S stream is used
as a feed stock to the sulfur recovery piont.
Sour water which results from several refinery processes is another
source of H 2 S. The sour water is steam stripped in stripping towers and
the resulting H 2 S is also used as feed stock to the sulfur recovery plant.
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To Fuel
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0
4 )
0
C) E.
4
I .4
00
(J C )
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5
Douglas Oil recovers elemental sulfur with two 3stage Claus sulfur
plants, the larger unit rated at 25 m. tons (28 tons)/day of elemental
sulfur and the smaller at 7 m. tons (8 tons)/day. Normal refinery
operations necessitate that only the larger Claus unfL be on stream,
with the smaller unit held in reserve. Actual sulfur production is
dependent on the crude oil sulfur content fed into the refinery.
In the Claus process, a third of the entering H 2 S is burned to form
SO 2 . The SO 2 and remaining H 2 S then react in the presence of a bauxite
catalyst to form elemental sulfur and water vapor. Typical sulfur
recovery efficiencies for 3-stage Claus plants is 97% 2 To meet the SO 2
concentration limitations (500 ppmv) of LAAPCD Rule 53.2, Douglas
installed a SCOT unit to treat the emissic s from the Claus plants.
In the SCOT process, tail gases from the Claus plants are routed to
a cobalt/molybdenum catalyst reactor where all sulfur compounds and free
sulfur are completely converted to H 2 S in the presence of a reducing
gas. From the reactor- section, the tail gases contain less than 100
ppmv of carbonyl sulfide (COS) and carbon disulfide (CS 2 ) and less than
10 ppmv of SO 2 . These tail gases are cooled, and excess water is
condensed and sent to sour water stripping.
The cooled tail gases of the SCOT unit contain 20,000 to 40,000
ppmv of H 2 S. This I-! 2 S is removed by scrubbing in a DIPA absorption
column. The concentrated H 2 S stream is recycled as feed to the first
stage of the Claus units.
Off-gases from the DIPA absorption column are guaranteed by the
vendor to contain less than 300 ppmv H 2 S. These off-gases are burned in
2 Standen, Anthony, ed. 1969, RirkOthmer, Encyclopedia of Chemical -
Technology, Second Edition, Vol. 19. New York: John Wiley & Sons,
pp 354.
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6
the incinerator portion of the SCOT unit which has a single John Zink
fuel gas burner rated at 1.3 x io6 K cal (5 x BTU)/hr heat release.
The incinerator, using natural gas as an auxiliary fuel, has a rated
capacity of 808 kg (1,780 lb)/hr at a flow rate of 3,6-80 std.
(130,000 scf)/hr.
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IV. TEST PROCEDURES
SAIIPLING LOCATION
Combustion gases from the SCOT tail gas incinerator pass through a
flue duct into a 46 in (150 ft) stack. Two test ports are located 21 in
(70 ft) up the stack, at an ideal sampling location, but are inaccessible
because no sampling platform exists. The only alternate sampling location
was a single port used by the oxygen monitor in the flue duct [ Figure 2].
The Thermox oxygen monitor port is located 4.6 in (15 ft) down the
6.9 m (22.5 ft) long duct, and 0.5 m (1.5 ft) from the duct bottom. The
flue duct is 2.1 in (7 ft) tall by 0.9 m (3 ft) wide, thus the sample
location is 3.6 and 1.8 equivalent diameters downstream and upstream of
any disturbance.
SAMPLING METHODS
Sulfur dioxide sampling was conducted at Douglas Oil, Paramount,
California, on September 13, 1977 using LAAPCD procedures which require
that all sulfate material be included into the sample. Therefore, no
isopropanol solution (for removal of SO 3 ) or filter (for removal of
particulate and acid mist) was used in the sampling train, as required
in EPA thod 53 To ensure complete capture of all sulfur compounds, a
5% hydrogen peroxide solution was used in the impinger tra rnpingers
1 and 2).
co oj ieaera . Regulations) Part 40) - 60. Stana uf Peij o ance
for iJew Stationary Sources, Appendix A, Reference Methods, August18,
29??.
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0.9 m (3 ft.)-_
Note: Ladders have cages or
Fall Saftey Devices.
2-10 cm ports at 900
(No platform)
H MM:
8
8.5 m
(28 ft.)
10.7 m
(35 ft.)
/4 Platform
11.3 m
3.7 ft.
Incinerator Ground
Figure 2: Douglas Oil Company, Paramount, California
Scott Tail Gas Incinerator
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9
The sampling train used was the AP 5000 manufactured by Scientific
Glass, Inc. [ Appendix B]. Sampling arrangement was as follows:
1. Oxygen monitor ceramic probe
2. Stainless steel (316) probe
3. Filter bypass (Pyrex . lass*)
4. First irnpinger-niodified Greenburg-Smith with 100 ml of 5%
hydrogen perioxide solution.
5. Second impinqerGreenburg-Smith with 100 ml of 5% hydrogen
peroxide solution.
6. Third irnpinger-niodified Greenburg-Smith was empty.
7. Fourth impingerrnodified Greenburg-Smith with 200 to
300 grams of silica gel.
LAAPCD procedures specify that the material collected in the probe
be included in the sample. However, the oxygen monitor ceramic probe
could not be removed from the sampling port without breaking it.
Theoretically, the incinerator emissions contain no particulate which
.,ou]d collect in the probe and the temperature ( 65O°C) was high enough
to prevent condensation of H 2 S0 4 , therefore, it was decided to use the
ceramic probe.. This assumption was checked and verified by comparing
the sulfate collected in the front half (stainless steel probe and glass
filter bypass) acetone wash tothe impinger sulfate catch.
The sampling train probe was connected to the ceramic probe and the
gas samples removed frcrr the duct using the oxygen probe. The oxygen
probe extended to the mid point of the duct. Sampling was conducted at
a single point at a constant rate.
Test points were not available to perform velocity traverses at the
sampling location. Volumetric flow rates were estimated by the Company
* Brand Name
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10
using a heat balance around the incinerator [ Appendix C]. This proce-
dure was considered sufficiently accurate to establish compliance with
the SO emission rate limit (91 kg/hr) because of the anticipated low
concentration (<500 ppm) and flow rate (116 m /min or. 410O scfm).
Analysis of the gas composition was performed according to the grab
techniques of Method 33 Fyrite* analyses were performed three times
during the testing run and averaged.
Moisture content of the gas stream was determined from the volume
increase of the first three impingers and the weight gain of the silica
gel 3 . .
Leak checks were performed before and after every run. Oven temp-
eratures were held within 14°C (25°F) of 120°C (248°F) during the runs
[ Appendix H]. The stainless steel probe was not heated.
Calibration procedures for the sampling train dry gas meter and
orifice meter are included in Appendix D. Calibration of these units
was performed before and.after the survey.
An NEIC mobile laboratory, located at the plant, was used for all
sampling train preparation and sample recovery. Sample recovery pro-.
ceeded as follows:
1. The stainless steel probe was washed with acetone and the acetone
wash collected in a glass jar with a Teflon*_lined cap. The
ceramic probe was not washed sinceit could not be removed from the
port.
Brand Name
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Il
2. The impinger solutions 1, 2 and 3 were measured volumetrically and
saved in a glass jar with a Teflon-lined cap. Impingers 1, 2 and 3
were then washed with distilled water and this wash was saved with
the impinger catch.
3. The fourth impinger (silica gel) was weighed to determine moisture
gain.
All samples were returned to the NEIC laboratories for SO 2 analysis.
Chain-of-custody was maintained at all times [ Appendix E].
Analytical procedures and data are presented in Appendix F.
PROCESS OBSERVATION PROCEDURES
During testing, the following data were recorded by NEIC personnel
for the S ii unit Mppendix G]:
natural gas burner pressure
H 2 S and SO 2 inlet concentrations
stack temperature
stack draft
In addition, Company personnel monitored and recorded other process
parameters required to estimate the volumetric flow rate from the
incinerator [ Appendix C].
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12
V.. TEST RESULTS
Three 90 minute sampling runs were performed on September 13
[ Appendix H]. The average stack gas temperature and moisture was 658°C
(1215°F) and 9.8%, respectively [ Table 1].
The test results show that the average SO 2 concentration- in the
SCOT tail gas incinerator emissions was 120 ppmv, 23% of the 500 ppmv
allowed by LAAPCD Rule 53.2. Company personnel estimated the average
volumetric flow rate from the incinerator to be 131 m 3 (.4,630 scf)/min
during the tests. This flow rate is within 15% of the 116 m 3 (4,100
scf)/min flow measured during a June 3, 1Y76 source test. Using the 131
m 3 / mm flow rate, the average SO 2 emission rate is 2.6 kg (5.8 lb/hr).
This is only 3% of the allowable SO 2 emission rate of 91 kg (200 lb/hr).
From Table I , ba seen that no sul fur co;npounds were cci -
lected in the unheated stainless steel probe. Sulfur compound col-
lection in the ceramic probe was probably the same as the steel probe
since the stack temperature was 658°C (1215°F).
During the testing, the SCOT unit was monitored to ensure smooth
and representative operating conditions. The process data in Appendix G
and the charts in Appendix C show that the process was operating smoothly.
These data are c 4 iilar to data taken during the presurvey inspection
when the plant was reportedly operating normally. The Claus plant was
operating at a sulfur production rate of 16.3 m ton (17.9 ton) /day
[ Appendix C]. Company personnel indicated this was within the normal
range of operation.
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13
Table 1
DATA SUMMARY
DOUGLAS OIL
P .4RAMOUNTJ CALIFORNIA
Run Number
1 2 3
Volume Sampled (STP)*
li ers 1,020 1,070 1,060
Ft 36.04 37.94 37.50
Moisture % 8.6 10.9 9.9
Barometric Pressure
cm of Hg 76.3 76.3 76.3
in of Hg 30.05 30.05 30.05
Stack Gas Temperature
°c 654 660 657
°F 1,210 1,220 1,215
1o1ecu1ar Weight (Dry) 28.97 28.97 28.97
Vo1umet ic Flow Rate** (STP)*
1mm 4,630 4,630 4,630
m /min 131 131 131
Sulfate Collected (nig)
acetone iash 0 0 0
impingers 422 554 601
TOTAL 422 554 601
SO Emissions
2 PPMV 100 120 130
kg/hr 2.2 2.7 3.0
- Sta;Ldard L mp rature ( 68 Qp) and Pressure (2 of Hg) - Dry
Estimated by Company
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APPE WIXA
PRESIJRVEY INSPECTION REPORT
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ENV1RONME TA1 ROTECT$ON AGENCY
OFFICE OF ENFORCEMENT APPENDIX .A
t AT ONA ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53. BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80225
TO Chief, Field Operations Branch DATE: August 11, 1977
OM Paul R. dePercin
SUBJECT: Presurvey Inspection of the Douglas Oil Company, Paramount,
California
On July 13, 1977, Mr. Royce Haley, Los Angeles Air Pollution Control
District (LA APCD) and the writer inspected the Douglas Oil Company,
Paramount, California, to obtain information necessary to conduct a
source test of the SCOT* tai.l gas incinerator stack,. This information
included the Claus sulfur plant and SCOT process descriptions, air pollution
control equipment configuration, source sampling feasibility, and process
and control equipment operating data availability. Of particular interest
were the available sampling locations and the modification to these sampling
locations necessary to acquire representative data by EPA testing methods.
The plant representatives contacted were Messrs. H. E. McFarlin, Process
Superintendent and William Ge ubel1e, Environmental Coordinator.
EPA Region IX requested NEIC to source test the SCOT tail gas incinerator
emissions for sulfur dioxide (SO 2 ) because a past source test conducted on
June 3, 1976, by the LA APCD determined the sulfur dioxide (SO 2 ) emissions
to be 2429 ppmv (dry), nearly five times greater than the allowable concen-
tration (LA APCD Rule 53.2) of the 500 ppmv. However, the SO 2 mass emission
rate was found to be 45 kg (100 lb)/hr, only half of the allowable 91 kg
(200 lb)/hr.
PROCESS DESCRIPTION
Douglas Oil Company operates a petroleum refinery at Paramount,
California, with a rated capacity from 40,000 to 45,000 bbls per day of
crude oil. The major processes are crude desalting, atmospheric distillation,
vacuum distillation, catalytic reforming, distillate hydrotreating, gas/oil
desulfurization, naptha desulfurization, asphalt blowing, and sulfur recovery.
Because the sulfur recovery plant emissions were specifically requested to be
source sampled by NEIC, the sulfur recovery plant is more fully discussed
below.
*Shel] Claus Off-gas Ireatment (SCOT) System
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A- 2
Sulfur Plant 1
Sour gases from the naptha, distillate, and gas/oil hydrodesulfurizing
units are processed in diisopropanolanhine (DIPA) absorption units where they
are scrubbed with lean amine solution. The hydrogen sulfide (H 2 S) is
selectively absorbed in the solution and removed from the gas stream. The
cleansed gases are then introduced into the refinery fuel gas system.
The H 2 S is stripped from the rich amine solution and recovered as a
concentrated gas stream. The resulting lean solution is recycled to the
sour gas absorbers mentioned above. The concentrated H 2 S, stream is used as
a feed stock to the sulfur recovery plant.
Sour water which results from several refinery processes- is another
spurce of H 2 S. The sour water is steam stripped in stripping towers and the
resulting H 2 S is also used as feed stock to the sulfur recovery plant.
D6ug1as Oil recovers elemental sulfur with two 3-stage Claus sulfur plants,
the larger unit rated at 25 m tons (25 long toris)/day of elemental sulfur
and the smaller at 7 m tons (7 long tons)/day. Normal refinery operations
necessitate that only the larger Claus unit be on stream, with the smaller unit
held in reserve. -
In the Claus process, H 2 S is burned to form sulfur dioxide(S0 2 ). The
SO 9 and H S react in the presence of a bauxite catalyst to form elemental
suTfur arid water vapor. Typical sulfur recovery efficiencies for Claus plants
-are 85% for- one catalytic stage, 94% for two stages, and 97% for three stages.
The tail gases (i.e., exhaust emissions) from the Claus plants contain
H 2 S in excess of the concentrations allowableunder LA APCD Rule 53.2. In
the past, it was commonplace in the industry to burn the tail gases in an
incinerator unit, thus converting the H 2 S to SO 2 . However, the resulting
SO 2 emissions were well in excess of the 500 ppmv allowable under the current
requirements of Rule 53.2. To meet the new requirements, Douglas has installed
a Shell Claus off-gas treating (SCOT) tail gas treatment system.
AIR POLLUTION CONTROL EQUIPMENT 2
The SCOT process, tail gases from the Claus plants are routed to a
cobalt/molybdenum catalyst reactor where all sulfur compounds and free sulfur
are completely converted to H 2 S -in the presence of a reducing gas. From
the reactor section,- the tail gases contain less than 100 ppmv of carbonyl
sulfide (COS) and carbon disulfide (CS 2 ) and less than 10 ppmv of SO 2 . These
State Implementation Plan Air Pollution Inspections of Douglas Oil
Company, Los Angeles County, California, EPA, NEIC, Report No.
EPA 330/2-76013, February 1976, page 11 and 12.
2 Ibid. pages 12 and 13.
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1-3
tall gases are then cooled, and excess water is condensed and sent to sour
water stripping.
The cooled tail gases contain 20,000 to 40,000 ppmv of H 2 S. The H ,S
is. removed from the gas stream by scrubbing with di-isopropanolamine (DIPA)
solution in an absorption column. The FL,S-rich DIPA solution is regenerated
by stripping the H 2 S in a conventional steam stripping column. The concen-
trated H 2 S stream is recycled as feed to the first stage of the Claus units.
The lean DIPA solution is recycled back to the H 2 S absorption column.
Off-gases from the DIPA absorption column contain less than 300 ppmv
H,S (vendor guarantee). These off-gases are burned in a SCOT jncinerator
which h s a single John Zink fuel gas burner rated at 1.3 x 100 kg cal
(5 x 10° Btu)Jhr heat release. The. incinerator, using natural gas as an
auxiliary fuel, burns material at a rate of 810 kg (1,777 lb)/hr and a tail
gas flow rate of 3,680 std. m 3 (130,000 scf)/hr.
SOURCE SAMPLING FEASIBILITY
Sampling Locations
Exhaust gases from the SCOT tail gas incinerator pass through a flue
duct to a 1.4 m (4.6 ft).diameter, 46 m (150 ft) high stack [ Figure 1]. On
this stack are two 10 cm (4 in) sampling ports 10.7 in (35 ftor 7.6 diameters)
downstream of the stack breeching and 8.5 in (28 ft or 6.1 diameters) upstream
of a tapered section of stack. This would be an excellent location to
source sample the emissions, except there is no sampling platform. There
is also rio crane or cherrypicker at the refinery that can reach 21 m (70 ft)
to the sampling ports.
As an alternative to these ports, it is possible to remove the oxygen
monitor from the flue duct and sample through the remaining 9 cm (3.5 in) port.
This port is 1ocated 4.6 in (15 ft) down the 6.9 m (23 ft) long duct, and
0.5 in (1.5 ft) from the duct bottom. The flue duct is 2.1 m (7 ft) tall
by 0.9 in (3 ft) wide; thus the sample location is 3.7 and 1.8 equivalent
diameters do .rnstream and upstream of any gas flow disturbances, respectively.
Since the SCOT waste gases natural gas and air must be well mixed for
efficient incin r tor oper ti n, th incinerator combustion gases will reach
the sample location well mixed (of uni orm concenbr tion).
Besides determining the SO 2 concentration, the incinerator combustion
gas volumetric flow rate must be determined so that the SO 9 mass emission
rate can be calculated. However, a volumetric flow rate d termination
cannot be made at the oxygen monitor port because EPA Methods 1 and 2
(traverse points and velocity determination) requirements cannot be met.
The two sampling ports on the stack are ideal, but it would be too dangerous
to perform a velocity traverse from the stack ladder and it would cost $100
per hour to rent a cherrypickeru (minimum charge of one day).
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09 m (3 ft)__.._. .
Note: Ladders have cages or
Fall Saftey Devices
210 cm ports
(ito platform)
at 900
1
)H. ii
cm
P1 atforin
.3 m
37 ft
Incinerator Ground
Douglas Oil Company, Paramount, California
Scott Tail Gas Incinerator
8.5 m
(28 ft)
103 rn
(35 ft)
Figure
I
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A-4
However, the incinerator combustion gas flow rate can be calculated
because the incinerator is a combustion source. It is possible to perform
an oxygen or carbon mass balance around the incinerator, and determine the
Incinerator combustion gas flow rate, with the following parameters:
1. natural gas burned (CR1)
2. tail gas flow (CFM)
3. combustion gas oxygen concentration (%)
4. cc 5 stion gas carbon dioxide concentration. (%)
5. tail gas oxygen concentration (%)
At present, only approximate values of these parameters are available, but
most can be measured, during the sampling.
When the calculated emission rate is near (within 20%) of the allowable
emission rate, the calculated combustion gas flow rate is difficult to
support as a means of determining, compliance. In this case, however, based on
past source test flow data and the incinerator design gas flow rate (see
Control Equipment configuration), if the emissions meet the 500 ppmv so2
concentration limitation the 502 mass emissions would be only 20 to 30%
of the allowable emissions (91 kg/hr). Thus, even with errors in flow
calculations amounting to 200%, no 502 emission violation would occur without
a concentration violation.
Modifications
Only two minor modifications to the sampling facilities are needed to
source sample the SCOT tail gas incinerator emissions for sulfur dioxide.
The first modification is the rernoval.of the oxygen analyzer from the flue
duct, and the second is the installation of a padeye 1.8 m (6 ft) above
the anal,
Miscellaneous
The air sampling van can be parked near the stack, where adequate
electrical power is available. The sampling train will use the electric
power from the van.
PROCESS AND CONTROL EQUIPMENT OBSERVATION .
SCOT unit and tail gas incinerator operations will be regularly monitored.
The H 2 S and 502 concentrations of the SCOT unit feed gases are recorded in
the refinery controi room. Incinerator and stack conditions will be checked
from the following instrument readings at the incinerator location:
1. natural gas pressure to burner
2. temperature of corlibustion gases
Ά) .-t- ,j, 4... C4 -
4. burner operation
5. oxygen concentration
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A-5
Other than ensuring steadystate. operations, the process observations are
of minor importance becaUse there is no process weight regulation for SO 2
emissions.
SUMMARY AND CONCLUSIONS
The SCOT tail gas incinerator can be sampled for sulfur dioxide according
to EPA Method 6. Only two modifications to the sampling location are
necessary: -
A. Remove the oxygen analyzer from the incinerator flue duct.
8. Install a padeye 1.8 m (6 ft) above the analyzer port, capable
of supporting 45 kg (100 lbs).
In addition, a parking space, for the NEIC air samoling van, near the incinerator
stack is needed.
There is no convenient means of determining the gas volumetric flow rate
by EPA Methods 1 and 2, but as mentioned previously, the gas flow rate
calculation is adequate to determine the incinerator compliance, status. The
Company must provide these flow a culations with the data used in the calcu
lations to the project coordinator at the completion of the sampling.
Except for ensuring normal process operations, no process data are
needed. The sulfur dioxide regulation (Rule 53) is not based on process
weight. . .
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APPENDIX B
STACK SAMPLING EQUIPMENT
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APPENDIX B
STACK SAMPLING EQUIPMENT
The Scientific Glass Model AP-5000 modular STAC O LATURtm sampling
train consists of a control unit, a sampling unit and a vacuum unit.
The units are connected together with quick disconnect electrical and
air lines and umbilical cords. A ground fault interrupter provided
personnel safety from electrical shorts.
The AP-5000 control unit contains the following;
1. Dual-inclined monometer (range 0-5w H 9 0) for indicating the
pitot tube velocity pressure and the brifice pressure drop.
2. Temperature control for the oven and proble.
3. A flow valve and a bypass valve for adjusting sampling rates.
4. Digital Temperature Indicator (DTI) which. give an instant
readout from six (6) points; stack, probe, oven, impinger
outlet, meter inlet, meter outlet by the use of a selector
switch.
5. Umbilical cords of (50 and 100 ft lengths) which interconnect
the control and sampling units.
6. Communications sets are wired through control unit, umbilical
cord to the sampling urlit*.
The sampling unit is made up of three distinct sections; impinger
case, oven and probe. All three sections can be converted to form one
sampling unit or can be separated for unusual sampling conditions.
Below are the individual component descriptions:
1. Probe Sheath - Made of 316 stainless steel. The nozzle end
is packed ith s- stos string. The ball joint (sampling
UflitJ end nas a woven teflon 0 Ring as packing material.
2. Probe liner 5/8 0.D. medium wall glass (pyrex) or stainless
steel (315) tubing logarithmically wrapped with nicrome heating
element, having a resistance of 2 ohms/ft.
sulated with fiberglass and asbestos with a type K thermocouple
imbedded for sensing the probe temperature.
S :oarate courmunication system used during this test program.
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B-i
3. Oven Fiberglass insulated capable of maintaining 120°C
(248°F) in cold weather (0°C).
The vacuum unit (pump) is capable of drawing a Fuigh vacuum (50 cm
Hg) and a moderate volume (14 1pm) of air. The pump is rotary fiber
vane type which does not require lubrication, but oil bath filters are
used for pump protection.
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APPENDIX C
VOLUMETRIC FLOW RATE ESTIMATIONS
-------
APPENDIX C 4
DDU L S
OIL COMPANY OF CALIFORNIA
September 26, 1977
Mr. Paul R. DePercin
U. S. Environmental Protection Agency
P. 0. Box 25227 -
Denver, Colorado 80225
Dear Paul:
The calculations and associated data for determining the SCOT
incinerator effluent flow rate during the EPA source testing
on September 13, 1977, are attached. As indicated in D. P. Meyer S
memo, the average flow rate f r the three 90 minute test runs
was calculated to be 4632 SCFM. As shown by the process recorder
charts, the Sulfur Plant feed and SCOT tail gas rates varied very
little throughout the test perioη3... I bring this to your attention
since you expressed some interest in that aspect of the operation
during the t ti g.
We were pleased that the testing progressed smoothly and appreciate
the cooperation you and your personnel displayed during your visit.
If you have any questions or need more information, please do not
hesitate to call me.
Very truly yours,
1_/ // // ,
I
William G. Geubelle
Environmental Coordinator
WGG/lp
-------
C-2
00 U 6 LA S / / iz (y
September 14, 1977
To: Bill Geubelle
From: D. P. Meyer
Subject: EPA Source Testing on H 402 Incinerator
The calculations on our incinerator stack effluent during the
source testing on September 13, 1977 have been completed. Based
on the measured rates and compositions of streams feeding the
incinerator my calculations show the rate up the stack to be
20676 lb/hr or 4632 SCFM. The back-up data, recorder charts and
computer printouts . for these calculations have been included
with this letter. A tabulation of back-up data is shown below.
Page
Number Computer Print-Out
1 Sulfur Plant Feed Summary.
2 SCOT Unit Yield Summary
3 V Sulfur PlantYield Summary , V
4 Fuel Gas Physical Properties Summary
5 Fuel Gas Meter Factor Caics
6 Fuel Gas Meter Factor Chart
7 V Incinerator Material Balance
8 Incinerator Heat Balance
Chart
Letter Chart
A Acid Gas. Feed to Sulfur Plant
B SCOT Tail Gas Flow Trace
C Incinerator Stack Temperature
0 , Incinerator Fuel Gas Rate
qfl
D P. Meyer
Senior Process Engineer
DPM/bf
-------
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IN F I - X TE; i F: ThI . F : . .1 .______
AC TJ L I : TF:.l) TI! 1) .
4L X ST\CK , r-, .F _____________
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-------
APPENDIX D
CALIBRATION PROCEDURES AND DATA
-------
APPENDIX D
DISCUSSION OF CALIBRATIONS
As discussed in the test report, the dry gas meter was calibrated
before and after the source test survey. The meter met the accuracy
criteria contained in the procedures in this appendix prior to the
source test survey. A post-survey calibration was conducted and com-
pared with the pre-survey calibration.
The dry gas meter accuracy coefficient changed from 0.98 to 0.96.
However, the coefficient did not change more than 5% as allowed in
Section 5.3 of Method 5 (40 CFR Part 60, Appendix A).
If the post-survey coefficient for the dry gas meter was used to
recalculate the mass emission rate from the stack, the effect would be
to increase the report result (5.8 lb/hr) by 2%.
-------
D- 2
NEIC PROCEDURE FOR
CALIBRATION OF DRY GAS METER
AND ORFICE METER
Dry gas meters are used in source testing units to accurately
measure sample volumes drawn during testing. A critical .orfice is
also installed to provide a known sampling rate so that isokinetic
sampling can be maintained. These units will be calibrated before
and after each sampling trip.
Calibration is accomplished by making simultaneous total volume
measurements with a calibrated wet test meter and the dry gas meter.
The wet test meter must be previously calibrated from a primary standard.
Calibration is performed follows:
1. Level wet test meter and adjust the water level to the
proper point.
2. Level and zero the manometer on sampling control unit.
3. Leak check unit and air hoses at 15 inch Hg (leakage rate must
be zero). Assemble vacuum line to the wet test meter.
(Caution: NO NOT Leak Check System by Plugging the Inlet to
the Wet Test Meter, this will cause internal damage to the
meter.)
4. Warm up control unit, by operating vacuum pump for 30 minutes
with wet test meter connected. in series.
5. Close the course valve and open the fine adjust (bypass) valve.
6. Turn or vacuum pump, open course adjust valve and turn the
adjust valve until manometer reads 0.5 H 2 0 ( M l).
-------
D- 3
7. Simultaneously record the dry gas meter reading, wet test
meter reading and time. Record temperature of wet test
meter, inlet and outlet temperature of dry gas meter and
atmospheric pressure during the test run.
8. Allow pump to run until the wet test meter lndicates
exactly 5 cubic feet of air have passed through the system
(10 cubic feet when a L H of 2, 3 and 4 inches H 2 0 are used)
and record time.
9. Repeat steps 59 for H of 1, 2 3 and 4 H 2 0.
10. Calibration record will be kept in a permanent file at NEIC.
Copies will be made for field use.
Calculations
Calculate the accuracy of the dry gas meter (y) as follows:
Vw Pb (td + 460 )
I Vd (Pb + H (tw + 460)
13.6)
Where: 3
V = Vΰlume of gas metered, wet test meter, ft.
Vd = Volume of gas metered, dry gas meter, ft. 3
= Atmospheric pressure, inches Hg
td Dry gas meter temperature, °F ( tci 1n td out )
2
t = Wet test meter temperature,
If y L 1.00 (40.02) then gas meter will be taken to Public Service
Company of Colorado gas meter shop for adjustment and/or repair.
: cient 0. ;+4 0 )
Pb(td+460) L
-------
Wbere: 3
= Volume of gas metered, wet test ti eter, ft
= Atmospheric pressure
= Dry gas meter temperature,
t , = Wet test meter temperature, °F
0 = Timeelapsed, minutes
D-4
-------
D-5
Orifice Meter Calibration
Where: V , = Volume, wet test meter
= Volume Dry gas meter
T , 1 = Temperature, Wet Test Meter
Td = Temperature, Dry Gas Meter
Atmospheric Pressure, Inches Hg
0 = Time, minutes
Remarks:
Date 7j7/ 77
Barometric pressure., in. Hg
AtCU L
BoxUo.__
Dry gas meter Mo .
LC ac( / 1 .c d.Frc
.
Orifice
Manometer
setting,
in. H O
Gas volume
wet test
meter
Vw,.
.
Gas volume
dry gas
meter
V ,
. TemDerature
.
Time
0,
r
Wet Test Dryqas_meter
Meter
t ,
Inlet
t ,
Outlet
t 0 ,
Average
t
ft 3
ft 3
°F
°F
°F
°F
mm
y
H@
0.5
5
1.0
5
7 -
7L/
,_, 0 7
73
7 ? )
.73
2.0 10 , 73 7 L7
- 3.0 io . ,ic - 7 . / 7 ?_J ( (,
4.0 10 ?? c . i-
A Ver
1 J
Calculations - : .
u
u
1r6
P (t + 460) .
Vd t AH ) (ti, + 460)
L
0.0317M-1 1., + 460)o
h (td 460) L v ,
0.6
0.0368
136
r-L/LO)
η )(7. - c) ,
- :1-
o.o n - , c.c
( 3(-73. c- & )I -
LU
0.0137
o,o3 7 ).o tc7 -
/.(3( - J. ci-4&c)L J
72 #4& c )
2.0
3.0
0.147
U.2g ,
/o ?G.S-t--k-o)
!At)(. LJ, .? .
/ .(1 f- --- - -_.)
/C.
oη- ?o rc. -k c ,i2 7
. 76 J
0.D 7 .L .c r(7 -c v37
f- Jt c )L /0 1
4.0
0.294
c)
O.o3 7,&LL ft (?7
; . u c L /0
Calibration by:______________
Checked by
4/2 -J77
-------
D-6
Orifice Meter Calibration
Date f/ i Box r o.
Barometric ressure,Pb in. Hg On gas meter No .
L L ____
L - 7 =
:
H@
P Ltd + 460 )
___)_(ti,,_+_460)
2i/ )
(c1(,Lu-±
-
1.0
0.0737
L
I
2.0
0.147
tCi . LV3 - .
1 e/ 7
LJ 10 /
3.0
4 0
0.219 JC - Z.i4..( )(17 L - L η 5)
( .c- cft-c) I l() . 1-tIi. I
0 294 , - ?cJ /V4 Z 4 c q 9&LI c c
u i_ ?C ? . j
Where: V Volume, wet test meter Calibration by:_______________
= Volume Dry gas meter
T T moerature. Wet T r-
= Temperature, Dry uas Meter
Atmospheric Pressure, Inches Hg
0 Time, minutes
Remarks:
i2
Gas volume
Gas volume
TemPerature
.
Orifice
Manometer
setting,
wet test
meter
V , ,.
dry gas
meter
V ,
Wet Test
ry qas_meter
Time
0,
Meter
inlet
Outlet
Average
t , ,
t ,
t 0 ,
t ,
in. H 9 0
ft 3
ft
.
°F
°F
0 F
°F
mm
-r
M1@
0.5
S
1.0
T 17
5
(Sb
2.0
10
73
7i
io p:
iI.27
7 : 3
77
.73
0 -
I - ,
3.0
4.0
10
10
/O
.
7
7t
7 3
&
Calculations
75
f. 3
Mi
13.6
0.5
0.0368
I
L
O.031ThH
h (td+ 460)
E i 46o)sf
/_ o iq i
2.
Checked by:
4/24/77
-------
APPENDIX E
CHAIN-OF-CUSTODY PROCEDURES AND RECORDS
-------
4PPENDIX E
ENVIRONMENTAL PROTECTION AGENCY
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
CRAIN OF CUSTODY PROCEDURES
June 1, 1975
GENE RAL
The evidence gathering portion of a survey should be characterized by the minimum
rwmber of samples required to give a fair representation of the water, air or solid
waste sampled. To the extent possible, the quantity of samples and sample locations
wifl be determined prior to the survey.
Chain f custody procedures must be followed to maintain the documentation necessary
to trace sample possession from the time taken until the evidence is introduced into
court. A sample is in your custody if:
1. It is in your actual physical possession, or
2, It is in your view, after being in your physical possession, or
3. It was in your physical possession and then you locked it up in a manner so
that no one could tamper with it.
All survey participants will receive a copy of the survey study plan and will be
knowledgeable of its contents prior to the survey. A pre-survey briefing will be held
to reappraise all participants of the survey objectives, sample locations and Chain
of Custody procedures. After all Chain of Custody samples are collected, a de-briefing
will be held in the field to determine adherence to Chain of Custody procedures and
whether additional evidence type samples are required.
SAMPLE COLLECTION
1. To the maximum extent achievable,.as few people as possible should handle
the sample.
2. Water, air, or solid sNail be obtained, using standard field
sampling techniques.
3. Sample tags (Exhibit I) shall be securely attached to the sample container
at the time the complgte sample is collected and shall contain, at a minimum,
the following information: station number, station location, data taken,
time taken, type of sample, sequence number (first sample of the day
sequence No. 1, second sample sequence No. 2, etc.), analyses required and
samplers. The tags must be legibly filled out in ballpoint (waterproof ink).
4. Blank samples shall also be taken with preservatives which will be analyzed
by the laboratory to exclude the possibility of container or preservative
contami nation.
5. A pre-printed, bound Field Data Record logbook shall be maintained to re-
cord field measurements and other pertinent information necessary to refresh
th samplers memory in the event he later takes the stand to testify re-
garding his actions during the evidence gathering activity. A separate
set of field notebooks shall be maintained for each survey and stored in a
safe place where they could be protected and accounted for at all times.
Standard formats (Exhibits [ I and III) have been established to minimize
ficid entries and include the date, time, survey, type of samples taken,
vol uwe of each sample, type of analysis. sample numbers, preservatives,
sample location and field measurements such as temperature, conductivity,
-------
E-2
2
DO, pH, flow and any other pertinent information or observations. The
entries shall be signed by the field sampler. The preparation and conser-
vation of the field logbooks during the survey will be the responsibility
of the survey coordinator. Once the survey is complete, field logs will be
retained by the survey coordinator, or his designated representative, as a
part of the permanent record.
6. The field sampler is responsible for the care and custody of the-samples
collected until properly dispatched o the receiving laboratory or turned
over to an assigned custodian. He n st assure that each container is in his
physical possession or in his view a: all times, or locked in such a place
and manner that no one can tamper wjth it.
7. Colored slides or photographs should 5e taken which would visually show the
outfall sample location and any water pollution to substantiate any con-
clusions of the investigation. Written documentation on the back of the
photo should include the signature o the photographer, time, date and site
location. Photographs of this nature, which nay be used as evidence, shall
be handled recognizing Chain of Custcdy procedures to prevent alteration.
TRANSFER OF CUSTODY AVID SHIPHENT
1. Samples will be accompanied by a Chain of Custody Record which includes the
name of the survey, samplers signatures, station number, station location,
date, time, type of sample, sequence number, number of containers and analy-
ses required (Fig. IV). When turnin; over the possession of samples, the
transferor and transferee will sign, date and time the sheet. This record
si eet allows transfer of custody of group of samples in the field, to the
mobile laboratory or when samples are dispatched to the NEIC Denver labora-
tory. When transferring a portion o the samples identified on the sheet to
the field mobile laboratory, the individual samples must be noted in the
column with the signature of the person relinquishing the samples. The field
laboratory person receiving the samples will acknowledge receipt by signing
in the appropriate column.
2. The field custodian or field sampler, if a custodian has not been assigned,
will have the responsibility of prope ly packaging and dispatching samples
to the proper laboratory for analysis. The t ?Dispatchu portion of the Chain
of Custody Record shall be properly filled out, dated, and signed.
3. Samples will be pr perly packed in shipment containers such as ice chests, to
avoid breakage. The shipping containers will be padlocked for shipment to
the receiving laboratory.
4. All packages will be accompanied by the Chain of Custody Record showing iden-
tification of the contents. The oriη nal will accompany the shipment, and a
copy will be retained by the surveycoordinator.
5. If sent by mail, register thepackace with return receipt requested. If sent
by corrsnon carrier, aGovernrrent Bill cf Lading should be obtained. Receipts
from post offices, and bills of ladin; will be retained as part of the perni
nent Chain of Custody documentation.
6. If samples are delivered to the laboratory when appropriate personnel are not
there to receive them, the samples must be locked in a designated area within
the laboratory in a manner so that no one can tamper with then. The same per-
son must then return to the laboratorj and unlock the samples and deliver
custody to the appropriate custodian.
-------
E-3
3
LABORATORY CUSTODY PROCEDURES
1. The laboratory shall designate a sample custodian. An alternate will be
designated in his absence. in addition, the laboratory thafl set aside a
sample storage security area. This should be-a clean, dry, isolated room
which can be securely locked from the outside.
2. All samples should be handled by the minimum possible number of persons.
3. All incoming samples shall be received only by the cu todfan, who will in-
dicate receipt by signing the Chain of Custody Sheet accompanying the samples
and retaining the sheet as permanent records. Couriers picking up samples at
the airport, post office, etc. shall sign jointly with the laboratory custodian.
4. !mniediately upon receipt, the custodian will place the sample in the sample
room, which ill be locked at all times except when samples are removed or
replaced by the custodian. To the maximum extent possible, only the custo-
dian should be permitted in the sample room.
5. The custodian shall ensure that heat- - nsitive or light-sensitive samples,
or other sample materials having unusual physical characteristics, or re-
quiring special handling, are properly stored and maintained.
6. Only the custodian will distribute samples to personnel who are to perform
tests.
7. The analyst will record in his laboratory notebook or analytical worksheet,
identifying information describing the sample, the procedures performed
and the results pf the testing. The notes shall be dated and indicate who
performed the tests. The notes shall be retained as a permanent record in
the laboratory and should note any abnormalties which occurred during the
sti : r Tn the event that the merson ho performed the tests is
not available as a witness at time of trial, the government may be able to
introduce the notes in evidence under the Federal Business Records Act.,
8. Standard methods of laboratory analyses shall be used as described in the
Guidelines Establishing Test Procedures for Analysis of Pollutants,
38 F.R. 28758, October 16, 1973. If laboratory personnel deviate from
standard procedures, they should be prepared. to justify their decision dur-
ing cross-examination.
9. Laboratory personn 1 are responsible for the care and custody c i-h mo1e
once it is handed over to them and should be prepared to testify that ne
sample was in their possession ar d view or secured in the laboratory at all
times from the moment it was received from the custodian until the tests
were run.
10. Once the sample testing is completed, the unused portion of the sample to
gnther with all identifying . tags and laboratory records, should be returned
to the custodian. The returned tagged sample will be retained in the sample
room until it is required for trial. Strip charts and other documentation
of work will also be turned over to the custodian.
i . Samples, tags and laboratory records of tests may be destroyed only upon the
order of the laboratory director, who will first confer with the Chief,
Enforcement Specialist Office, to make certain that the information is no
longer required or the samples have deteriorated.
-------
E4
EXHIBiT 1
EPA, NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
5 ic.n No. Dale Time - - Sequence No.
2 Stahon Localion ________Gr E
_______________________________ Camp.
________BOD _________
________SoIid ________Oil an l Grease
_____COD _____D.O.
Nu tcien s _________Bad.
________Other
Samplers:
Front
ENViRONMENTAL PROTECTION AGENCY
OTF 1CE O ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
UUJLD 1NG 5 , OX 25227, DENVER FEDERAL CENTER.
DENVER, COLORADO 80225
Back
-------
EXRIBIT II
SURVEY, PHASE DATE
OF SAMPLE _______
NA!YS ES
STATION ESCRIPTIcm
REQ U RED
t)
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-------
Xlf III
FIELD DMA RECORD
S mp!ors:
.
Gag H.
TEMPERATURE
CONDUCT1V TY
pH
D,O.
or Flow
NUMBER
DATE
1ME
C
zmhos/cm
S.U.,
mg/I
FL or CFS
.
...
m i
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-------
ENVIRONMENTAL PROTECTION AGENCY
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227. Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
E7
H
t? I- y-
c.
r
SURVEY
.
SAMPLERS: (Signwu e)
STATION
NUMBER
STATION LOCATION
DATE
NME
SAMPLE TYPE
SEQ.
NO.
NO. OF
CONTAINERS
.
ANALYSIS
REQ1J IRE
Wc!er
Comp. Grab.
A r
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Received by: (Signature)
.
Date/Time
RelinRuished by: (Signature) .
Received by: (!sgl a tsrej
Dote/Time
Rehnquished by: (Sign Iu:e)
Received by: (Signot eJ
Date/Time
Relinquished by: (SignoJure) Receiyed by Mobile Laboratory for field
analysis: (Signature)
Dsp tc ed by: Dote/Time Received fo Loborat&ry.by: .-
..7
Dote/Time
f
Date/Time
c
Method of Shipment: S. .
/2)
Distribution:
Orig. Accompany Shipment
T Copy Survey Coordinator Field Files
*GPQ 679 O40
-------
APPENDIX F
ANALYTICAL PROCEDURES AND DATA
-------
APPENDIX F
SULFUR DIOXIDE EMISSIONS FRai STATIONARY SOURCES
Sampling Procedure
Stack gas samples are collected in an impinger train of Greenburg-
smith design which consists of four impingers. The train is cooled in
an ice bath to minimize evaporative loss of the absorbing solutions and
to enhance the tetention of stack gas components in these fluids.
The first and second impingers contains 100 ml each of 5% hydrogen
peroxide (10 ml of 30% H )0 diluted to 100 ml v ith deionized-distilled
water, the third impinge s empty and the fourth impinger contains
approximately 200 g of indicating type 6-16 mesh silica gel.
Particulates, sulfites, and sulfates and sO are caught in the
first and second impingers. The sulfur dioxide ts oxidized by the
hydrogen peroxide to sulfate (S0 4 ):
SO 2 + H 2 0 χ H, SO 3
H 2 S0 3 + H 2 0 2 - H 2 0 + H 2 S0 4
The third impinger collects and carry over from the second and the
fourth impinger removes water vapor from the stack gas.
The impinged solutions are transported from the stack site to the
laboratory in mason jars sealed with Teflon lid inserts. Chain-of-
custody procedures are followed. The liquid level in the jars is marked
in the field and checked in the laboratory for losses.
Analytical Procedures
All sulfur-containing species are collected as or converted to
sulfate. The sulfate is determined by titration with a standardized
barium solution. The titrations are carried out in 80% isopropanol,
,hich enhances the formation of barium sulfate andsharpens the end-
point of the reaction. Thorin is used as an indicator and changes from
yellow to pink at the end-point of the titration when there is an excess
of barium present.
Standardization of ;u;n Solution
A standard solution prepared from acidimetric grade potassium
hydrogen phthalate (KHP) is used to standardize a sodium hydroxide
-------
F-2
solution. The sodium hydroxide solution is used to standardize a sul-
furic acid solution, which is used in.turn to standardize a barium
perchlorate solution. The reactions and. stoicionietry are described
below:
KHP + NaOH -- NaKP + H 2 0
2NaOH χ H 2 S0 4 -- Na 2 SO 4 + 2H 2 0
H 2 S0 4 + Ba(C10 4 ) 2 -- BaSC 4
we19 t HP(g ) = (vol NaOH) (N NaOH)
(N NaOH) = ( weight KHP )
( 204.2 g/eq) (1 NaOH)
(vol. NaOH) (N NaOH) = (vol. H 2 S0 4 ) (N H 2 S0 4 )
(N H 2 S0 4 ) = ( vol. NaOH) (N NaOH )
(vol. V 2 S0 4 )
2N H 2 S0 4 1 M H 2 S0 4 1 M SO 4 =
(vol. H 2 S0 4 ) (N H 2 S0 4 ) = (vol. Ba Cl0 4 ) 2 ) (M Ba(Cl0 4 ) 2 )
(M Ba(C10 4 ) = ( vol. H 2 SO ) (M H S0 4 )
(vol. Bl(ClO 4 ) )
Analysis of Hydrogen Peroxide Samples
Since hydrogen peroxide samples are mostly water, 100% isopropanol
must be added to the aliquots to obtain an optimum concentration of 80%
isopropanol. Table I indicates what volumes of 100% isro ool are re-
quired for various aliquot volumes to meet the optimum 80% final volumes.
Table I
.
Sample
Aliquot
20
15
10
5
2
1
0.5
ml
Required
100%
Isopropanol
80
60
40
20
8
4
2
ml
-------
F 3
Before the mixture is titrated with the standardized barium per-
chlorate, the total volume in the flask is adjusted to 100 ml with 80%
isopropanol. Four drops of thorin indicator are adde i and the solution
is titrated to a pink end-point. Replicate titrations should agree
within 1%.
-------
APPENDIX G
PROCESG DATA
-------
APPENDIX G
Douglas Oil Co
Paramount ,Cal f.
Date:
Stack
Temerature
Stack
Draft
I
Nat. Gas Hydrogen
Burner Pres Sulfide
I
o oa
, 6
Su] fur
Dioxide
1: L::
i:
i
i
..
--
-
--
:
- -
7 /
--
---
-- --. -----
i lock
T i me
Concentration
. - c5
-/L/D j:z )
.
4!
C.7 r
, /-/ ,
- -
C /( fi , ce
ThIL 9/15
t -/c
A( .
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- -
& k
- ----
-
.-
/ ?
Th,
6
/,OQ
92
_# - --- - - -
______
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- -
-
c,Cc / 2 ,
4 -
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-
-
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- - - --
.
(ι
1
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- .
-
; -
.- -
a - -
-
-------
APPENDIX H
FIELD DATA SHEETS
AND EXAMPLE CALCULATIONS
-------
APPENDIX H
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-------
nbhnt TempF 7 -
Bar. Press. hg________________
Assumed Moisture Z_____________
Probe Tip Die. In. c -
Pitot Tube No.________________
P robe Length/type /( S. c
Filter No., -Z ,_______ ______
Jo. / ccI
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P1
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Read and record at the start of
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Titne Start Time_
End Time
t
La
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Temp.
F
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Probe
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F
.
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Temp.
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Temp.
F
(°F+460)
Desired
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Pump
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Comments:
3/16/77
-------
SAMPLE CLEANUP SHEET
H-4
Piant: 4 4 - (
Address : / _ - 27
Station No.: :2c 1
Run 1Io.:/
Barometric Pressure: ye . - c-
Impinger 1
Date: 9//t67
1 4-
uperau OrS.
_Ambient Temperature:
Sample Box Number:
jj pinger 2
of 7
pinger 3
of c-: ,
Final Volume____
Initial Volume_
Volume collected
Impi nger
ml
ml
/ ml
of
ml of
ml
n g e r
. .Q
Total Volume Collected
7T2 ml
Filters
No.
Final Weig
qm
Iare Weight
Wei g h t
Collected
gin
gin
qm
gin
Cleanup performed by________
on
/ F-
Final Volume
Initial Volume
Volume collected
/
ml
/ C
ml
5 ?
ml
Final Volume
Initial Volume
Volume collected
I/ O
.
ml
/ -
ml
ml,
Final
Initial Volume
Volume collected
in 1 i ht
Initial weight
Weight collected
& ?. .
gm of
-------
r jr No. .2 _ ZLc (
Loca t ion /
D ite
Q erator_____________________
Sample Dox No. 2
-i
Hoter Box No.
: ter ti H__________________
C Factor
VERY INFUJ T? T FILL IN ALL. BLANXS
Read and record at the Btart of
each test point.
Time: Start Time
End Time
Ambient TcnpF rC
Bar. Press. Hg _____
Assumed 1ioisture z_____________
Probe Tip Die. In.
Pitot Tube No.________________
Probe Lcngth/type/e rx :
Filter No., -(______ ______
L I Aeck
Pitot
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Dry Gas Temp.
Pump
Impin er
Oven
Probe
Stack
Stack
Point
Clock
Dry Ga3
Meter,
CF
in.
P
1{ O
in 1120
.
F
Vacuum
In. hg
Temp.
F
Temp.
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Temp.
F
Temp.
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Temp.
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( F+4 6O)
Desired
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3/16/77
Point Clo k
Dry Gas
Meter, CF
Sheet of______
Pitot
in. H 2 0
P
Orifice H
in H 2 0
Dry Gas Temp.
°F
Pump
Vacuum
In. Hg
Impinger
Temp.
°F
Oven
Temp.
°F
Probe
Temp.
°F
Stack
Temp.
°F
Stack
Tetrp.
°F
(°F+46O
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P1 ant: - ( .
Address:
Station No. : (
Run No.: 2.
8aromecr c Pressure: 9o 0 5
Irnpinger 1
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H- 7
Final Volume____
Initial Volume
Volume. collected
Impinger 3
Final Volume____
Initial Volume_
Volume collected
j. ml
ml
/ ml
of
Impinger
Final Volume . ..
Initial Volume
Volume collected
ml
inl
of
Impi nqer
2a cgm of
,7 7gm
; T gm
Total Volume Collected
ml
Filters
No .
Final t!eight
Wei qht
t oi t cte
ft/ci-
rn ________g in
SAMPLE CLEANUP SHEET
Date:__________________
Operators ,
Ambient Temperature:
E.o; Number:
Final Volume
Initial Volume
Volume collected
166
ml of 5
ml
ml
55
Irnpinger 2
-
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ml
nil
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Final weight
Initial weight
Ueight collected
,LIc-i g L
Cleanup performed by
on
-------
Plant P )uccL A5 /I _
Run.No. 3. r2t /
Location A4 O ( .A L
Date g//3 ___
!-P
Operator 4 4c45(-
Sample Box No. 2..
} cter Box No. 2..-
Neter A H 1 7 _______
C Factor
VERY Ila RTANT PILL IN ALL BLAN (S
Read and record at the start of
each test point.
Times Start Time_____________
End Tiin __________________
Ambient Temp P
Bar. Press. Hg 3
Assumed )foisture Z_____________
Probe Tip Din. In.
Pitot Tube No.________________
Probe Length/type/ S .5
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Temp.
°F
Oven
Temp.
F
.
Probe
Temp.
°F
Stack
Temp.
F
Stack
Temp.
F
(°F+46 0)
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3/16/77
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Clod.
Sheet . of
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eter, CF
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in. H 2 0
P
Orifice AH
in H 2 0
-
Dry Gas Temp.
°F
Pump
Vacuum
In. Hg
Irnpinger
Temp.
°F
.
Oven
Temp.
°F
Probe
Temp.
0 p
Stack
Tamp.
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Temp.
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.
?
/90
:
A t
/0
4f -
.
.I-
-
- I
,
-------
Impinger 1
SAMPLE CLEANUP SHEET
_______Date: ,:;Y / 7 .;:
____Operators:________________
____Ambient Temperature: - q
Sample Box Number:________
H-lO
Final Volume____
Initial Volume...._.
Volume collected
Impinger 2
Impinger 3
-, nil
ml
ml.
Final Volume_____
Initial Volume
Volume collect
Impi nger
I miof
6 ml
ml
-
ml of
ml
ml
o/ S
,) . - ) ml
Filters
No.
Final Weight
Tare Weight
Wei ght
Collected
gm
qm
gm
c m i
gm
gm
Plan
Address :_________________
Station No.: 2 c /
Ru.n No.:__________
Baronjetr c Pressure:
nil
ml
ml
Final Volume____
Initial Volume_
Volume collected
of .
of C ,e- - e . - .
I/Z
Fiρa o N
Initial Volum
Volume collected
Impinger
Final weight______
Initia lweight___
Weight collected.
Total Vo1ume Co1l:ected
726. q
7:
gm of
gm
5 ;; , c 1
Cleanup per formed by
on
-------
Molecular Weight Determination
Station Number cc /
Method of Analysis: Fryrite X
Orsat
Sample Type: Grab
Integrated
Run
1o
Tine
CO 2
02
.
CO
Collected
Analyzed
J
S
y /
// r
2
. S
/ . 2
.
7
L
w
:
-
S
/ 7
-
.
Leak Check:________________
02 Check. o. % against
_________________% aga ..
. 5 nfl
Remarks:
------- |