ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
EPA-330/2-77-G2
5
Emission Tests
Powerine Oil Company
Santa Fe Springs, (
California
(September 12-13,
1 977)
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
DENVER, COLOR
AND
ADO
y*osr%
REGION IX, SAN FR/
\NC1 SCO j 1

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(L)
ENVIRONMENTAL PROTECTION AGENCY
Office of Enforcement
EPA-330/2-77-025
EMISSION test:
POWERINE OIL COMPANY
Santa Fe Springs, California
(September 9-11, 1977)
December 1977
National Enforcement Investigations Center - Denver
and
Region IX - San Francisco

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CONTENTS
I INTRODUCTION 	 1
II SUMMARY AND CONCLUSIONS 	 2
III PROCESS DESCRIPTION 	 4
IV TEST PROCEDURES		6
SAMPLING LOCATIONS 		6
SAMPLING PROCEDURES	6
Particulate Sampling 		6
Sulfur Dioxide Sampling 		9
PROCESS MONITORING PROCEDURES 		11
V TEST RESULTS		12
FIGURES
1	FCC Pollution Control Equipment 		5
2	FCC Stack		7
TABLES
1	Data Summary		14
2	FCC Unit Particulate Emissions		15
3	Sulfur Dioxide Emissions 		16
4	Process Weight Summary 		17
5	Visible Emission Observation Summary ....	18
APPENDICES
A	Presurvey Inspection Report
B	Stack Sampling Equipment Description
C	Calibration and Data Procedures
D	Analytical Procedures and Data
E	Chain-of-Custody Procedures and Records
F	Production Data and Process Weight Calculations
G	Test Data and Emission Calculations

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I. INTRODUCTION
o
The Powerine Oil Company operates a 7,900 m (50,000 bbl)/day
integrated crude oil refinery in Santa Fe'Springs, California. On
November 5, 1975, at the request of Region IX Environmental Protection
Agency (EPA), the National Enforcement Investigations Center (NEIC)
inspected this facility to determine compliance.with the regulations of
the Los Angeles Air Pollution Control District (LAAPCD).* The sub-
sequent State Implementation Plan (SIP) inspection report recommended
that the Powerine fluid catalytic cracking (FCC) unit stack be source
tested to determine compliance with the applicable particulate regulations.
On Fnbruary 28, 1977, the EPA Region IX requested that the NEIC
source test the Powerine FCC stack. A presurvey inspection of the
facility was performed by NEIC personnel on July 18, 1977, to evaluate
j'imDiing locations and obtain process information [Appendix A]. It was
determined that sampling would be feasible provided that minor modi-
fications be made to the sampling location.
From September 9 to 11, 1977, the Powerine FCC stack emissions were
tested by NEIC to determine compliance with LAAPCD Rules 52 (concentration)
and 54 (emission rate) for particulate emissions. Visible emission
observations were also made and compared to Rule 50 of the LAAPCD
' ~1 
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II. SUMMARY AND CONCLUSIONS
From September 9 to 11, 1977, NEIC tested the Powerine FCC stack
emissions to determine compliance with LAAPCD Rules 52 and 54 for
particulate emissions. Three particulate sampling r^:.: ~"z
sulfur dioxide sampling run were performed according to Methods 5
and the required LAAPCD procedures. In addition, opacity readings
were also made to determine compliance with LAAPCD Rule 50 which
requires that visible emissions not equal or exceed 20% opacity.
LAAPCD defines "particulate" as the particulate less the sulfate
(as H^SO^ 'h^O) collected by the filter, acetone wash and impingers 1
2 and 3. Using the LAAPCD definition of particulate, the average
3	0
FCC particulate concentration was 110 mg/m (0.048 gr/std. ftJ) and
the average particulate emission was 5.3 kg (12.0 lb)/hr. These
O
emissions are in comoliance with Rule 52 (128 mg/m or 0.056 gr/scf)
and Rule 54 (13.6 kg/hr or 30 Ib/hr) by 14% and 61%, respectively.
Test results for the FCC stack were also calculated using the
following definitions of particulate matter:
Method 5	- Particulate collected at a temperature of
120°C (248°F) by the filter and acetone
wash
~	,. _ . „	'r Method 5
plus the inorganic, nonsulfate (as H^SO^
"2 H^O) particulate collected by impingers 1
2 and 3)

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3
As indicated below, particulate concentrations determined by both
Method 5 and Method 5 (+) procedures exceeded the 128 mg/m
limitation (Rule 52) by 2% and 9%, respectively. The average
particulate emission rates were less than the allowable 13.6 kg/hr
(30 lb/hr).
Concentration ^ Emission Rate
mq/m gr/std. ft kg/hr lb/hr
Method 5	130	0.058	6.5 14
Method 5 (+)	140	0.061	6.8 15
4.	The sulfur dioxide test determined that the FCC emissions had an
SO2 concentration of 1,020 parts per million volume (ppmv), and an
SO2 emission rate of 134 kg (295 lb)/hr.
5.	The FCC visible emissions complied with Rule 50 which limits the
emission opacity to less than 20%. The average opacity readings
were less than 18% and in most cases (6 of 8) were less than 10%.

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III. PROCESS DESCRIPTION
The Powerine Oil Company produces liquified petroleum gas (LPG),
3
gasoline, jet fuel, diesel fuel, fuel oil, and asphalt at this 7,900 m
(50,000 bbl)/day integrated crude oil refinery. Major processes include
crude desalting, atmospheric distillation, vacuum distillation, catalytic
cracking, catalytic reforming, hydrotreating, alkylation, asphalt manu-
facturing, and sulfur recovery.
The major particulate emissions source in the refinery is the FCC
unit1 [Figure 1]. Spent catalyst in this process is continuously removed
from the reactor portion and introduced through piping into the catalyst
regeneration portion. Here the petroleum coke, tars, and other residual
deposits which form on the catalyst surface are burned off. The recovered
catalyst is then recycled to the reactor. Catalyst particles which are
entrained in the exhaust gases are captured by a series of cyclone
separators internal to the regenerator unit.
Particles captured by these cyclones are returned to the regenerator.
The regenerator unit exhaust gases contain considerable amounts of
carbon monoxide, particulate matter, aldehydes, sulfur oxides, ammonia,
and oxides of nitrogen. To minimize the emission of particulates and
carbon monoxide (CO) and to recover the fuel value of this materiai, trie
regenerator exhaust gases are routed through a CO boiler for combustion,
then through an electrostatic precipitator (ESP), and into the stack.
1 "State Implementation Plan Air Pollution Inspection of Powerine Oil
Company"3 Los Angeles County, California, EPA-NEIC, EPA 530/2-76-014,
February, 1976.

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Figure 1: Powerine Oil Company* Sante Fe Sorinas. California
FCC Pollution Control equipment.

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IV. TEST PROCEDURES
SAMPLING LOCATIONS
The FCC stack [Figure 2] is 58 m (190 ft) high, tapering in inside
diameter incrementally from 3.6 m (12 ft) to 2.4 m (8 ft) to 1.2 m
(4 ft). Because the included angle of the tapered sections is only 15°,
these sections are not considered flow disturbances.2 The sampling
ports are on the south and west sides of the middle section of the
stack. This site is 20 m (65 ft), or 5.4 diameters, downstream from the
gas inlet, and 27 m (90 ft), or 11.2 diameters, upstream of -he stack
exit. The sampling platform is located 1.5 m (5 ft) below the sampling
ports. Based on Method 1 criteria3, a total of 28 sampling points were
required. Each point was sampled for 3 minutes.
SAMPLING PROCEDURES
Particulate Sampling
A preliminary velocity and temperature traverse was made on the FCC
stack on September 9. A Lear-Siegler S09/N0 analyzer with a 1.1 m (3.5
L A
ft) lone, 9 cm (3.5 in) diameter probe is 1 ~- (] ft) upstream
of (below) the west sampling port and 5° to the right. The preliminary
velocity traverse indicated that no aberrations in measured velocities
occurred at any traverse points. It was concluded that the probe did
not cause a flow disturbance at the sampling location.
2	"Gv.idslines for Sampling in Tapered StLCjkc'' by o. uo^r. R. T.
Shigehara, Environmental Protection Agency, Research Triangle Park,
North. Carolina, October 1974.
3	Code of Federal Regulations, Title 40, Part 60 Standards of Performance
for New Stationary Sources, Appendix A - Reference Methods, August 18,
1977.

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not to scale

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8
Particulate tests were conducted from September 9 to 11 , 1977. These
tests were conducted in accordance with the Method 53 procedures.
The sampling train used was the Model AP 5000 manufactured by
Scientific Glass, Inc. [Appendix B] which was configured as follows:
1.	Stainless stee'i (316) nozzle
2.	Glass-lined probe
3.	Glass fiber filter (11.4 cm diameter)
4.	First impinger -- . modified Greenburg-Smith with 100 ml
distilled water
5.	Second impinger -- Greenburg-Smith with 100 ml distilled
water
6.	Third impinger -- modified Greenburg-Smith, empty
7.	Fourth impinger -- modified Greenburg-Smith with approx-
imately 200 g of silica gel
Moisture content of the gas stream was determined from the increase in
volume in the first three impingers and the weight gain of the silica
gel (Method 4).3
Gas samples were obtained by the grab sample technique of Method 3.3
Analyses were performed with Fyrite* type combustion gas analyzers.
Stack gas molecular weight was based on the average analyses of the
three gas samples collected during each run.
Three sampling runs within the isokinetic range of 90% to 110% were
performed on the FCC stack. Prior to each run, the sampling train was
leak-cV-:''-J ?3 Ci~ (15 *n) !!c, "of each run, a
second leak check was conducted at the highest vacuum recorded during
the run. These checks were acceptable if the leakage rate did not
3	3
exceed 0.00057 m (0.02 ft )/min. During each sampling run, the sampling
time was 84 minutes and the	gas volume collected was 849 dry
standard liters (30 dry std. ft ). During the tests, probe and oven
* Brand name

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9
temperatures were held to averages of 119°C (245°F) and 127°C (261°F),
respectively within the acceptable temperature range of 120°C (248°F)
+14°C (25°F).
The pitobe assembly (10-2) and the dry gas and orifice meters used
in this test had been calibrated prior to leaving Denver and were re-
calibrated upon return [Appendix C].
A NEIC mobile laboratory, located at the plant, was used for all
sampling train preparation and sample recovery. Sample recovery pro-
ceeded as follows after each test run:
1.	The filter was returned to its storage container (petri
dish) and sealed with aluminum foil.
2.	The nozzle, probe, cyclone, and front portion of the glass
filter holder were washed with acetone and the washings
collected in a glass jar with a Teflon*-lined cap.
3.	The volume of the contents of impingers 1, 2, and 3 was
measured as part of the moisture determination. The contents
were then rinsed with distilled water into a second glass
jar with a Teflon-lined cap.
4.	Impinger 4, which contained silica gel, was weighed to
determine the moisture gain, after which the silica gel
was discarded.
All samples were returned to the NEIC laboratories for particulate
and sulfate analyses [Appendix D], which specifies that sulfate particulate
noc be included in particulate emissions calculations.
Chain-of-Custody procedures were followed at all times [Appendix E].
Sulfur Dioxide Sampling
Testing for sulfur dioxide (S02) emissions was conducted at the FCC
stack on September 11, 1977, in accordance with procedures in the LAAPCD
* Brand name

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10
Source Testing Manual, which require that all sulfate material be included
into the sample.4 Therefore, no isopropanol solution (for removal of
SO^) or filter (for removal of particulate and acid mist) was used in
the sampling train, as required in EPA Method 6.3 To ensure complete
capture of all sulfur compounds, a 5% hydrogen peroxide solution was
used in the impinger train (impingers 1 and 2). The sampling train used
was the Model AP 5000 manufactured by Scientific Glass, Inc. [Appendix B]
which was configured as follows:
1.	Stainless steel (316) nozzle
2.	Glass-lined probe
3.	Glass oven bypass
4.	First impinger -¦
5.	Second impinger --
6.	Third impinger --
7.	Fourth impinger --
modified Greenburg-Smith with 100 ml of
5% hydrogen peroxide solution
Greenburg-Smith with 100 ml of 5%
hydrogen peroxide solution
modified Greenburg-Smith, empty
modified Greenburg-Smith with approx-
imately 200 g of silica gel
The moisture content was determined as previously described for the
particulate tests.
One sampling run was performed at a constant sampling rate on the
FCC stack. The stack center point was sampled for 60 minutes. Leak
checks, oven and probe temperatures, and equipment calibrations were as
those described above in Particulate Sampling.
The mobile laboratory was used for all sampling trair, preparation
and sample recovery. Samnl- recovery proceeded as follows:
1.	The nozzle, probe, and oven bypass were washed with acetone,
and the washings were collected in a glass jar with a Teflon-
lined cap.
2.	The volume of the contents of impingers 1, 2 and 3 was measured
as part of the moisture determination. The contents were then
rinsed with distilled, deionized water into a second glass jar
with a Teflon-lined cap.
4 Air Pollution Source Testing Manual, 1972s LAAPCD, Rev. Ed. 3 Chapter 4.

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11
3. Impinger 4, which contained silica gel, was weighed to determine
the moisture gain, after which the silica gel was discarded.
Samples were retained for sulfate analysis.
PROCESS MONITORING PROCEDURES
To ensure normal operating conditions and to determine the process
weight rate, the FCC unit was monitored during'source testing [Appendix F].
The three most important process parameters observed and recorded
were:
1.	The oil feed rate to the FCC reactor
2.	The catalyst circulation rate to the FCC reactor
3.	The air feed to the FCC regenerator
The first two parameters were added together to determine the FCC process
weight. However, only the first and third process parameters were read
in the FCC control room. The second parameter, catalyst circulation
rate, was calculated by the Company and provided to the process observer.
The FCC pollution control equipment instrumentation was also
monitored primarily to determine whether the equipment was operated
steady-state during the sampling periods. The process observer recorded
the ESP primary and secondary current, primary voltage, spark rate, CO
boiler fiue gas tilu value, and air fsed rate at periodic intervals
[Appendix F]. Any changes observed in the instrument values were
considered possible process upsets; the unit operators were asked to
explain and/or to correct the upset.

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V. TEST RESULTS
The Powerine FCC stack was sampled four times—three particulate
runs and one sulfur dioxide run. Isokinetic sampling rates for the
three particulate runs ranged from 100.4% to 103%, which is within the
specified range of 90% to 110%. Sulfur dioxide testing was performed at
a constant sampling rate at the stack center point. Test data [Appendix
G] are summarized in Tables 1, 2, and 3.
During testing, the FCC unit was operating at a rate of about
1,800 m^ (11,300 bbl)/day of oil [Table 4]. The catalyst circulation
rate and air feed rate did not vary [Appendix F]. The FCC process
weight averaged 0.80 (1.74) million kg(1b)/hr which, based on LAAPCD
Rule 54, allows 13.6 kg (30 lb)/hr of particulate to be emitted. A
3	3
particulate concentration of 128 mg/m (0.056 gr/std. ft ) is allowed by
Rule 52 when the volumetric	,o c^o ...	sea. tc ;/nrin
[Table 1].
The test results presented in Table 2 have been interpreted using
the following definitions of particulate:
1.	LAAPCD - Inorganic particulate less the sulfate collected
by the filter, acetone wash, and impingers.
2.	Method 5 - Particulate collected at a temperature of 120°C
(248°F) by the filter and acetone wash, i.e., the
front half.
3.	Method 5 (+) - Particulate matter as defined in item 2 plus
the inorganic, nonsulfate particulate collected
by impingers 1, 2, and 3.
Based on the LAAPCD definition of particulate, the average FCC
3	3
particulate concentration was 110 mg/m (0.048 gr/std. ft ) and the
average particulate emission rate was 5.3 kg (12.0 lb)/hr. According to

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13
3	3
Rule 52, the allowed concentration is 128 mg/m (0.056 gr/std. ft ), and
thus the source is in compliance. Since the average particulate emission
rate is 5.3 kg (122 lb)/hr, or 39% of the allowed 13.6 kg (30 lb)/"nr,
the source is also in compliance with Rule 54.
Method 5 results were 130 mg/m^ (0.058 gr/std. ft^) and 6.5 kg
3
(14 lb)/hr. This particulate concentration (130 mg/m ) is about 2% over
the allowable concentration. The average particulate emission rate was
only 48% of the allowed 13.6 kg (30 lb)/hr.
The Method 5 (+) calculations resulted in an average emission con-
3	3
centration of 140 mg/m (0.061 gr/std. ft ) and particulate emissions of
6.8 kg (15 lb)/hr. The emission concentration (140 mg/m") exceeded the
3
Rule 52 limitation of 128 mg/m by 9%. However, the average emission
rate was only 50% of the allowed 13.6 kg (30 lb)/hr.
The sulfur dioxide test determined that the FCC emissions had an
SO^ concentration of 1,020 ppmv and SO^ emission rate of 134 kg
(295 1b)/hr [Table 3].
According to Rule 50, the FCC visible emissions are limited to less
than 20%. The highest average opacity during the source testing was 18%
[Table 5], which is in compliance with Rule 50. In most cases (6 of 8),
the average readings never exceeded 10%, and only twice did individual
opacity readings exceed 20%.

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14
Table 1
DATA SUMMARY
POWERINE OIL COMPANY
SANTA FE SPRINGS3 CALZi:.
1	2	3	4+
Parameter	9/9-10	9/10	9/11 9/11
Volume Sampled (STP)++
liters	1032	1095	956 662
fr	36.44	38.66	33.76 23.39
Moisture %	12.0	12.0	12.0 13.1
Barometric Pressure
cm Hg	77.2	77.2	76.1 76'. 1
in Hg	30.40	30.40	29.95 29.95
Stack Gas Temperature
°C	253	248	251 252
°F	488	478	.;J2 495
Molecular Weight (dry)	30.53	30.31	30.54 30.54
1 Isokinetic	103.0	100.4	101.3
Stack Gas Velocity
m/sec	5.7	6.2	5.5
ft/sec	18.8	20.2	17.9
Volumetric Flow Rate (STP)^+
m /min	800	871	753
ft /min	28,330	30,830	26,670
t Run #4 was for SO~- Runs 1-3 were for particulate.
++ STP-Standard Temperature (68°F) and Pressure (29.92 in. Hg) - dry.

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15
Table 2
FCC UNIT PARTICULATE EMISSIONS
POWERINE OIL COMPANY
SANTA FE SPRINGSJ CALIFORNIA
Run Number

1
2
3
Particulate Collected (mg)



p "1 "1 + p y»
138
66
67
Acetone wash
45
58
40
Impinger catch (inorganic)
31
41
151
Total
2i 4
165
258
Sulfate Collected as HoS0„ '2 Ho0



Filter 2 4 2
17
20
11
Acetone wash
20
10
20
Impinger catch
31*
41*
130
Total
68
71
161
Avg,
ft"
LAAPCD Procedure Particulate Results
Particulate catch (mg)
Concentration
gr/std. "
mg/m
*3 r. i on
1 b/hr
kg/hr
146
94 97

0.062
0.037 0.044
0.048
140
85 100
110
15
9.9 10
12
6.8
4.5 4.5
5.3
Method 5 Procedure Particulate Results
Particulate catch (mg)
183
124
107

Concentrati on
gr/std, ft
mg/m




0.077
0.049
0.049
0.058
180
110
110
130
Emission Rate




lb/hr
19
13
11
14
kg/hr
8.6
5.9
5.0
6.5
5 ( + ) Procedure Particulate Results
Particulate catch (mg)
Concentration
gr/std. ft
mg/m
Emission Rate
Ib/h-
kb/hr
183 124 128
0.077 0.049 0.058 0.061
180 110 130 140
8.6 5.9 5.9 6.8
* Actual value was greater than particulate catch3 therefore} the value of
the particulate catch was substituted.

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16
Table 3
SULFUR DIOXIDE EMISSIONS
POWERINE OIL COMPANY
SANTA FE SPRINGS3 CALIFORNIA
Run No.
Parameter	4
Sulfate collected (mg)
Acetone wash	9.5
Impingers	2740
Total	2749.5
Volume sampled (STP)t
liters	662
Sulfur dioxide concentration
ppmv	1020
Volumetric flow rate (STP)^
m /min	808
Sulfur dioxide emissions
lb/hr	295
kg/hr	134
t STP-Standard Temperature (68°F) and Pressure (29.92 in. Hg)
- dry.
ft Average of Runs 1, 2, and 3.

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Table 4
PROCESS WEIGHT SUMMARY
POWERINE OIL COMPANY
SANTA FE SPRINGS3 CALIFORNIA
Date
(September)
Catalyst*
Circulation
Rate
m. tons/hr
(tons/hr)
Oil Feed
i Rate
Total Process Weight Rate
.VI lowable
Linissi ons
kg/hr
(lb/hr)
m^/day
(bbl/day)
m. tons/hr
(tons/hr)
m. tons/hr
(tons/hr)
kg/hr
(lb/hr)
9
760
1,800
27
797
797,000
13.6

(840)
(11,300)
(30)
(870)
(1 ,740,000)
(30)
10
760
1,810
27
797
797,000
13.5

(840)
(11 ,400)
(30)
(870)
(1 ,740,000)
(30)
11
760
1,840
27
797
797,000
13.6

(840)
(11,550)
(30)
(870)
(1 ,740 ,000)
(30)
* Calculated by Company [Appendix F].

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Table 5
VT5ir*7 EMISSICS .ZZ-?.V\TION SUMMARY
POWERINE OIL COMPANY
SANTA FE SPRINGS, CALIFORNIA
Date

Range of
Average'
(September)
Run No.
Emission Opacity (%)
Opacities (%)
9
1
5-20
7.1

1
5-15
9.2
10
1
5-20
7.1

2
10-30
17.5
11
3
0-15
7.9

3
0-10
6.5

4
5-10
3.1

4
10-25
14.0
f Avi.rc.ys of ^ dings (6 minutes)

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APPENDIX A
PRESURVEY INSPECTION REPORT

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APPENDIX A
Chief, Field Operations Branch	August 10, 1977
Paul R. dePercin
Presurvey Inspection of the Powerine Oil Company, Sante Fe Springs,
California
On July 18, 1977, Art Powell, Los Angeles Air Pollution Control
District (LA APCD) and the writer inspected the Powerine Oil Company,
Sante Fe Springs, California, to obtain information necessary to conduct
a source test of the fluid catalytic cracking (FCC) unit stack. This
information included the FCC"and sulfur recovery process description,
air pollution control equipment configuration, source test feasibility,
and process and control equipment operating data availability. Of
particular interest were the available sampling locations and whether
modifications to such locations were necessary in order to conduct the
source test safely and acquire representative data.
The plant representatives contacted were Messrs. Walter Ziemba,
Environmental Affairs Coordinator, and David 'Jrayt, Operations Manager.
EPA, Region IX, requested rlEIC to source test the FCC stack for
particulates and sulfur dioxide (SO2), the FCC unit and tne sulfur
recovery unit emissions are emitted from the same stack. The results of
a June 5, 1959, source test by the LA APCD were 15.8 kg (34.9 lb)/hr of
particulate, wnicn exceeded the allowable rate (LA APCD, Rule S4) of
13.6 kg (30 lb)/hr. A source test conducted January 7, 1970, by KVii
Engineering aeterminea that the sulfur dioxide concentration was b79
ppmv (wet) and the mass emission rate was 243 kg {C>3G lb)/i:r. The FCC
unit SO? emissions are limited to 2,GOO ppmv (urvj (LA APCD, Rule 53.1)
while tne sulfur recovery unit SG;> emissions are limited to 500 ppmv
(dry) and 91 kg (200 lb)/hr (LA A^Q, Rule 53.2). Since the two units
emit through the same stack, compliance of the stack emissions depends
on the applicable SO2 regulation.
PROCESS DESCRIPTION
Powerine 011 Company operates a petroleum refinery at Sante Fe
Springs with a rated capacity of S0.J00 bbl/tiay of crude oil. Major
processes at this refinery include crude desalting, atmospheric dis-
tillation, vacuum distillation, catalytic cracking, catalytic reforming,.

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A-2
hydro treating, alkylation, asphalt r/aiuifacturint, and su3fur rccovsry.
Of these processes* two—catalytic cracking arid sulfur recovery--are
more fully described below.
Fluid Catalytic Cracking Itnit^
, SpBfvt cat£i/=t frr: i ±~.i . urii ii co-.cinjr-ulv	froa tse-
ts actor portion and introduced through piping into the catalyst regen-
eration portion. Here the petroleum coke, tars, and other residual
deposits vhicn form cm the catalyst surface are burned off the catalyst
fines. The recovered catalyst is then recycled! to tfvs reactor. Catalyst
particles whir-" are entrained in the exhaust gases are partially captured
by a series of cyclone separators internal to the regenerator unit.
Particles captured by these cyclones are returned to the regenerator.
2
Sulfur P^acovery Lnit
The hydrogen sulfide H2S rich off-gases frein the amine stripping
plant are processed in a 24 m. tons (£4 long tons)/ February
7975, page 5.
2 Ibid* pages II and 12.

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A-3
Sampling Location
Tim FCC and sulfur recovery unit emissions are exhausted fron a
tapered 55 m (130 ft) stack [Figure 2]. Sampling ports are situated
15.3 m (53 ft) downstream of the gas inlet and 27.4 
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A-4
PROCESS AND CONTROL EQUIPMENT QBSEkVATIOhS
Instruments in the FCC unit control room monitor operating conditions
of the FCC unit, the sulfur recovery unit, and the CO boiler. Instruuents
at a ground-level panel monitor operating conditions of the ESP's. All
instruments will be observed during each source test run to determine
whethsr steady-state operations existed.
The FCC unit process weight is defined as the sum of the oil feed
rate and the catalyst circulation rate to the reactor portion of the FCC
unit.* The oil reed rate has a direct instrument readout in the FCC
control room, but the catalyst circulation rate nust be calculated. The
Company should be requested to supply the oil feed rate and catalyst
circulation rate for each source test run. This will insure agreement
between EPA and the Company on the applicable process weight for each
run.
SUMKARY AMD CONCLUSIONS
The Powerine Oil FCC stack emissions can be source tested for
particulate and sulfur dioxide. A good sampling location is available
which with minimal modifications will allow EPA Method 5 and 5 sampling.
Tiiese modifies		 .	are required:
a.	Install padeyes 1.3 m (6 ft) above the FCC stack south and
west ports» i.e., the two ports 90° apart.
b.	Re/iiGve the temporary gas sample nrooe fro.ii the south port.
c.	Remove the Lear-Siegler S02/u0x monitor weather cover and do
not install the monitor until the sampling is complete.
In addition, to perform source testing, the following must be
provided by the Company:
a.	A parking spot for the MEIC air sampling van (8 ft x 40 ft)
near the base of the FCC stack.
b.	Electric power to the van. Either a standard range plug or
two-110 volt, 20 a:np lines wi"	t
Process operations will be monitored in the FCC unit control rooa
to determine whether normal operations exist. Therefore, access to
* Telephone conversation with James .Nance, LA APCD, on July li, 1977.

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this room viill be required by ths process observer. To determine th
FCC unit process weight, after each sampling run the Company should
supply the following process data for the sampling period:
a.	Oil feed rate to the FCC unit [ibis/day).
b.	Catalyst circulation rate (tons/rain).
A determination of the applicable sulfur dioxide regulation is
needed. The SO2 emissions must meet either the sulfur plant or the
general process SO2 regulations.

-------
APPENDIX B
STACK. SAMPLING EQUIPMENT DESCRIPTION

-------
APPENDIX B
STACK SAMPLING EQUIPMENT
The Scientific	Glass Model AP-5000 modular STAC-O-LATUR 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.
The AP-5000 control unit contains the following:
1.	Dual-inclined manometer (range 0-5" H?0) for indicating the
pitot tube velocity pressure and the orifice pressure drop.
2.	Temperature control for the oven and probe.
3.	A flow valve and a bypass valve for adjusting sampling rates.
4.	Digital Temperature Indicator (DTI) which gives an instant
readout from six (6) points; stack, probea 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 unit.*
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 Sheitr - of 316 stainless steel. The nozzle end
is packed "with asbestos string. The ball joint (sampling
unit) end has a woven teflon 0 Ring as packing material.
2.	'I	o' o.D. nidoiu.n '.'.'511 glass (pyrex) or stainless
steel (316) tubing logarithmically wrapped with nicrome heating
element, having a resistance of 2 ohms/ft. The liner is
insulated with fiberglass and asbestos with a type K thermocouple
V"':	ths p:"rbs temperature.
3.	Filter Frit - Porous glass frit (coarse) banded to silicone
rubber.
* Separate communication system used during this test program.

-------
B-2
4. Oven - Fiberglass insulated capable of maintaining 120°C
(248°F) in cold weather (0°C).
The vacuum unit (pump) is capable of drawing a high 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.

-------
APPENDIX C
CALIBRATION AND DATA PROCEDURES

-------
APPENDIC C
Discussion of Calibration
As discussed in the text, the pitobe assembly and the dry gas meter
were calibrated before and after the source test survey. Each piece of
equipment met the accuracy criteria contained in the procedures in this
Appendix prior to the source test survey. Post-survey calibrations are
conducted and compared with pre-survey calibrations.
The dry gas meter accuracy coefficient changed from 0.98 to 0.96.
However, the coefficient did not change by more than 5% as allowed in
Section 5.3 of Method 5 (40 CFR Part 60, Appendix A).
The calibration coefficient of pitobe 10-2 changed from 0.76 to 0.80
(+5.3%). However, Method 2 (40 CFR Part 60, Appendix A) makes no mention
of using the post-survey pitobe calibration coefficients, inferring initial
coefficients should be used in all calculations, i.e., for isokinetic and
emission rate determinations.
Using the pre-survey pitobe coefficients the isokinetic rates ranged
from 100.4% to 103.0%. With the post-survey pitobe coefficients, the
isokinetic rates would range from 95.3% to 97.8%.
If the post-survey coefficients for the dry gas meter and pitobe
; y v/ers used to rtcj. iuJiate une iriu-w	the eiriicc
would be to reduce the report results (12 lb/hr) by 3%.

-------
C-l
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
Treasure men ts with a calibrated wet test meter and the dry gas mets.r.
Th« tast 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 Ufct Test Meter, this will cause internal damage to the
meter,)
A. Warm up control i			ig vacuur. pump for 30 minutes
with vet test meter connected in series.
5.	Close the course valve and open the fine adjust (by-pass) valve.
6.	Turn or vacuum pump, open course adjust valve and turn the fine
adjust -waive until manometer reads 0.5" iljCi (£H).

-------
C-2
7.	Simultaneously record the dry gas meter reading, wee 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 rv.n until the wet test meter indicates
exactly 5 cubic feet of air have passed through the system
(10 cubic feet when a AH of 2, 3 and 4 inches H^O are used)
and record time.
10. Calibration recora will be kept ir. a permanent file at
Copies will be made for field use.
Calculations
Calculate the accuracy of the dry gas meter (y) as follows:
If Y ^ 1.00 (+0.02) then gas meter will be taken to Public Service
Company of Colorado gas meter shop for adjustment and/or repair.
9. Repeat steps 5-9 for AH of 1", 2" 3" and 4" H^O.
Vw Pb (td + 460)
V = Vd (Pb + AH (tw + 460)
13.6)
Where:
3
V = Volume of gas metered, wet test meter, ft.
w
3
= Volume of gas metered, dry gas meter, ft.
P = Atmospheric pressure, inches Hg
b
= Dry gas meter temperature, °F (t^ in — t^ out)
2
t = yet test meter temperature, °F
Orfice meter coefficient (AH@ = 0.317 AH
Pb(td+460) j_ „ _J

-------
-3-
C-3
Where:	^
Vw = Volume of gas metered, wet test meter, ft
= Atmospheric pressure
o_
tj = Dry gas meter temperature, F
t. - test: meter temperature, °F
0 *= Time elapsed, minutes

-------
C-4
NEIC Procedure for Pi tot Tube Calibration
Introduction
The Type-S pi tot tube is used by NEIC to measure stack gas
velocity during source sampling. The pitot tube coefficient (Cp)
of this instrument is determined by calibration against a trace-
able National Bureau of Standards (NBS) standard pitot tube. The
Type-S pitot tube is calibrated on a probe sheath with a h inch dia
nozzle atta'ched. All pitot tubes are calibrated from 305 m/min
(1000 ft/min) to 1524 m/min (5000 ft/min). Pitot tubes used during
tests will subsequently be recalibrated at a minimum of 3 points
v/ithin the velocity range observed during testing. Tubes which have
been damaged or suspected of being damaged du.-mg 7:sld use will be
recalibrated over the entire range (i.e. 305 to 1524 m/min).
I. Equipment Required
A. Flow System - Calibration is performed in a-ftlow system
meeting the following minimum requirements:
(1)	The air stream is confined in a well-defined cross
sectional area, either circular or rect	
The minimum size is 30.5 cm (12 inches) diameter
for circular ducts and at least 25 cm (10 inches),
as the shortest dimension for rectangular ducts.
(2)	Entry ports provided in the test section, shall be a
minimum of 8 duct diameters downstream and 2 diameters
upstream of any flow disturbance, e.g. bend, expansion,
contraction, opening, etc.

-------
-2-
C-5
(3) The flow system must have the capacity to generate over
the range of 305 m to 1524 m (1000 ft. - 5000 ft.)/min.
Velocities in this range must be constant with time to
guarantee steady flow during calibration.
B.	Calibration Standard
A standard type pitot tube either calibrated directly
by N.B.S. or traceable to an ti.B.S. standard shall be
the calibration standard.
C.	Differential Pressure Gauge
An inc". Ined or expanded scale manometer shall be
used to measure velocity head (aP). Such gauges 3iall be
capable of measuring AP to within + 0.13 mm (0.005 inches)
0
H2O. A micro-manometer capable of measuring with 0.013 mm
(0.0005 in) H2O will be used to measure AP of less than
13 (0.5") H20.
D.	Pitot Tube Lines
Flexible lines made of tygon or similar tubing shall
be used.
E.	Thermometer
n .nercu'o in y'>ass or uuicr type thermometer checked
agains a mercury in glass thermometer is considered suitable.
7. Barometer
A mercury column barometer shall be available to determine
atmospheric pressure.
II. Physical Check
-! tv,-	are sjiarp ancj Jq n0£ have a celled ec~c,
2. The impact planes of sides A & B are perpendicular to
the Traverse Tube axis [Figure 2].

-------
C-6
3- The impact planes are parallel to the longitudinal tube axis
[Figure 3],
III. Calibration Procedure
The Type-S pitot tube shall be assigned an identification
number. The first digit of the number is the effective length of
the tube, followed by :	:r.d consecutive niir.bsrs for the number
of tubes of the same effective length, i.e. 5-1 signifies a five
foot pitot-'tube and is th? number one tube. Calibration proceeds
as follows.
A.	Fill manometer with clean oil of the proper specific gravity.
Attach and leak check all pitot tube lines.
B.	Level and zero monometer.
C.	Position the standard pitot tube in the test section at
the calibration point. If the flow system is large enough
and does no interfere with the Type-S , ;r.:-
tube may be left in the system.
- 		-r,^_c t'bc? into the flow system.
E. Checks for the effect of turbulance are made as follows:
1.	Read LP on both Type-S and standard pitot tubes with
the'standard pitot tube in place and compare vnth read-
ings when the standard tube is withdrawn from system.
2.	Read AP on the Type-S tube at centerline of flow system,
then take readings while moving the tube to the side
of the system. This will define the boundary turbulance
layer.
3.	Position the Type-S tube so that there impact openings
are perpendicular to the duct cross sectional area and

-------
-4-
C-7
F.
G.
H.
I.
J.
K.
L.
check for null (zero) reading. Absence of a null reading at
this position indicates non-laminar flow conditions.
Read AP ^ and record on data table.
With the Type-S "A" leg orientated into the fl0.7 read aPs
and record on data table.
Repeat steps F and G until three sees of velocity data
have been obtained.
Remove Type-S pi tot tube and rotate probe nozzle until it
aligns with side "B" impact openings.
Insert the Type-S pitot tube and proceed as in steps F through
H.
Adjust flow system to new volocity and repeat F-J.
Record air temperature in the test system and barometric
pressure during testing.
1. At each "A"-side arr	-"^odty setting, calculate
the three valves of Cp (s) as follows:
pitot tubing inches H£0
APS - Velocity head1, measured by the Type-S
pitot tube, inches H^O
2. Calculate Cp, the average (mean of the three Cp(s)
valves.
IV. Calculations
Where:
Cp - Standard pitot tube coefficient O'BS)
AP - Velocity head, measured by Standard

-------
C-8
3. For each CP calculated in step 2, calculate a,'the average
deviation from the mean as follows:
o(Side "A" or "B") = $Icd (s) - Cp (A or B) I
3'
3
4.	The pitot is acceptable if:
(a)	The "A" and "B" side average deviations calculated by
equation 2 are <_ 0.01.
(b)	The difference of the "A" and "B" sides Cp calculated
by equation 1 is <_0.01 for each individual velocity.
5.	Calculate the test section velocity as follows:
V = KCp /tap std
V pm -
V.'here:
V" = Average test-section velocity, ft/min
K = 5130 (constant)
Cp = Coefficient of standard pitot tube
T = Temperature of gas stream °R
P = Barometric pressure, inches Hg
M = Molecular weight of air = 29.0
AP std = Average of the three standard pitot
tube readings, inches F^O
V. Record Keeping
Flow system data and rmation on each pitot tube shall
be recorded in a bound book.
The flow system data shall include:
1. The tunnel cross-sectional area and length
up-stream and down-stream of the test site )ft.)
from disturbances.

-------
-o-	C-9
2.	Time tunnel used (hrs)
3.	Air temperature (°F) in flow system and barometric
pressure (inches Hg).
4.	All checks for turbulance and flow distribution.
5.	Velocity range (ft/min).
The pi tot tube information shall include:
1.	I:*D. number
2.	Checks for physical dsjpages a errors noted and
modifications.
3.	Dates and surveys pi tot tubes were used.
4.	Date of calibrations, coefficient and dates of
re-caV'kration.
The calibration records vnll be kept on file at NEIC. Copies of
the appropriate calibration dates vail be furnished for each source
test project.

-------
C-10
idTTfrPf
id
f©
V
>
IE
r~
sTyT
•A
Figure 1- Measurement of ; ype-S^oitot tubs length (dimension "a") and impact pi^ns
separation cijtanco (dimension "b").	"	1
TRANSVERSE
TUBE AXIS
1.

-IMPACT-
PLANES
'Figure' 2. Typs-S pitotitube, endi
j'visw; impact-opening plar.js per-
pendicular to transverse tubs axis..
;A^SIDE PLANE
From "A TYPE-S PITOT TUBE CALIBRATIOf-i
Robert F. Vollaro, October 15, 1975

-------
C-ll
Orifice ^ster Calibration
Date
hp±LL
Box No.
-<^r
o
2 V- £>
Barometric pressure, 	in. Hg Dry gas meter Ho.
At6L^'~
^ CnGL-K fC !b ' /!< - O. C-		 .
Orifi ce
Manometer
setting,
AH
in. H^O
Gas volume
wet test
meter
V
ft3
Gas volume
dry gas
meter
vd»
ft3
Terp.Derature
Tima
0,
mw
Y
&m
VJet Test
Drv qas meter
Meter
Inlet
OutletlAverage
°F
fcdi'
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°F
td>
°F
0.5
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5

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2.0
0.147 1 /o^7q.(/3 (71..TV^i-o')
ft. n Co+' .^V77 V6 
-------
C-12
Date
Orifice Meter Calibration
"f/y-7 /-) -7	Box rio._

'la, q
Barometric pressure,^Ph= in. Hg Dry gas meter No.
SM- Uv-'r-. L D (
Z.r;-\V^-CV^.,r	^ = O O C^;^\
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Where: V = Volume, v/et test meter
Vd = Volume Dry gas meter
T.. = To~nor?^ura. t.fot Test Meter
Tj = Temperature, Dry Gas Meter
Pb = Atmospheric Pressure, Inches Hg
0 = Time, minutes
^ )-/
Calibration by: v. /¦--
\j ~	1
Checked by:
Remarks:
4/24/77

-------
its r'nvVron!i!-i,;i caT r'ro tectum Agency
National Enforcement Investigation'. Center-It' /er
Calibration Pit.ot Tubs: ID Number /VV?,S - /	
Type-S Pi tot Tube ID Number:	/r- -X	
C-13
CP

r^\


A p
Standard
Pi tot
aP S-T.ype Pi tot
C:>
0
Comments0^
A leq
B lecj
A ! B
, i io ¦
. % o
;i* o
. '7c?C- ! ..79"7
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,763
Leg Average Cp
probe shsath attached fes
nozzle attached
sampling' isok-inetical ly
Performed By:
Calibration Date:

-------
U3 1'tivironciini.o.1 ProLcction Agency
national En forcetfT.iit Invcitigot.ioris Cent
C-14
Calibration Pi tot Tube: ID Numbsr_
Typs-S Pi tot Tubs ID Number:	
cntcr-IJcnvi-r
a/7?
• i
Cp
f »
•/ X
' /
/c-
6?-H r
AP
Standard
Pi tot
-A P S-Type Pi tot
Cp
by 3 M.-v-vcrr
Comments
A leq
B leq
A
B
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7
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Leg Average Cp
iy • I LU v wU I I Ul U L> I Ul I •
probs sheath attached
nozzle attached
sampling' isokinejLically_
Performed By:
Calibration Date:
9,

-------
APPENDIX D
ANALYTICAL PROCEDURES AND DATA

-------
APPENDIX D
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80225
TO Mr. Paul dePercin	DArE December 2, 1977
Field Operations Branch
FROM
SUBJECT.
Deputy Chief
Chemistry Branch
Detection Limits for L.A. Source Test Data
The data transmitted on October 14, 1977, included less than values for
the particulate acetone, organic and inorganic impinger samples. All
weighings were performed on an analytical balance to the nearest 0.1 mg.
Positive results for the blank samples are from random contamination
during sample collection, handling and analysis. It is important that
results not be reported as real when in fact the positive values are
from contamination. This possibility is minimized by determining the
detection limit based on the determined blank values.
The detection limit is calculated by adding two standard deviations
(95% confidence level) of the blank values to the mean of the blank
values. If the mean blank is subtracted from all results, then this
value is excluded from the detection limit. Typically, only a few
blank measurements are made and one hiqh blank value can bias the de-
tection limit. However, this will provide a conservative reporting of
positive values. If any error is made, it will be on the side of not
reportinq some real values, but will guard against reporting values as
th?.t rssulted frcm contamination.
Mark J/ Carter
cc: Meigqs
Younq

-------
liAML w. Slim C I I— ' I I • 	" w r^C t, 1 £¦ o I
SAMPLE
NUMBER
STATION DESCRIPTION
TIME
; l%G/-GI - &=)JO
1- III £ Ol 1_ 0i>;
/5 5-7
/%Ol -OT. -O^/0
" It ll
03//^
\
/ Sro i -03 -0*7/0
it
1/
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/?o/ -o^-olil
" '1 Jj
	
/?6/ -oz-fi/o
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DMM^
	
W- CO IJ'll m I (VI C~
P fcfrU" wi
DATES COVERED	^/to - ^/19]
ANALYSES PERFORMED	rr^7\
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Prt RT»e o(_ATr
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-------
1IAL . . *wAL i"\K\ Rl-i ui\i IN\»j i ui^M	rciyo
NAME OF SURVEY	L.fl.	~T-n<7
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[*201-02-0119
n
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-------
Xnr-i -'V
Attachment II
METHOD 5 DETERMINATION OF PARTICULATE EMISSIONS
FROM STATIONARY SOURCES
ANALYTICAL PROCEDURES
Filters
The filters to be tared are desiccated at 20 -5.6°C (68 -10°F) and
ambient pressure for at least 24 hours and weighed at 6 or more hour
intervals to a constant weight, i.e.°,-5<_ mg. change from previous weigh-
ing, and results recorded to the nearest 0.1 mg. During each weighing
the filter is not exposed to the laboratory atmosphere for a period
greater than 2 minutes and a relative humidity above 50 percent.
The filters are received from the field in aluminum foil wrapped
Petri	The aluminum foil is removed and the Petri dishes placed
into a dessicator using indicating drierite as the dessicant. This
dessicant removes the uncombi^ed water on the filters. The filters are
desiccated at 20 + 5.6°C (68 -10°F) and ambient pressure for at least 24
hours and weighed in the same manner as in taring.
Prior to weighing the filters, both tared and gross, the single pan
analytical balanced is calibrated a:,	 		j,
prior to each weighing, dessicator and weighing room temperature and
humidity readings are recorded.
The filters in the Petri dishes are individually removed from the
dessicator immediately prior to weighing. Removal and all other handling
of the filters are performed with tweezers.
Acetone Wash
The acetone probe washes are received in quart glass jars with
Teflon lined lids. The contents of each jar are transferred into tared
250 ml breakers along with the acetone used to rinse the jars after
transferral. The beakers are then placed into a hood at ambient tempera-
ture for acetor
V\e>i>4
In the hamtd, the beakers are placed in an aluminum foil tunnel
which is designed to prevent any possible contamination by particulates
and to allow an efficient air flow for escape of acetone vapors. The
hood door is kept closed and tared beakers used as blanks are included
to verify that the samples did not become contaminated.

-------
After at least 24 hours in the evaporating tunnel, beakers are
removed and placed into dessicators using drierite as the dessicant.
The beakers remain in the dessicator for at least 24 hours and weighed
to a constant weight. The final weights are reported using a single
pan analytical balance calibrated against Class "S" weights. Room
temperature and humidity are measured during the dessication and
weighing process.
No filters or acetone residues are discarded after analysis. The
residue from the beakers are rinsed with a minimal amount of acetone
back into the mason jars in which they were.collected.
The filters and residues along with their respective sample tags
are stored in a predetermined place for at least a year.
•Raw Data Bench Cards
om/o
xO	,
u i>Y
C Ji /C r*"* ^	OA/
/x. ~r a
/l/rTAto r>
r/
f/iTfJS
WS/}JL
r/jutL.
TfiCC
/SS 7~~
!¦fHAU/Mfi
i>/r.
WT.

ssnrit
jTATt'*/
f/uflia'ti

F/J. Ttc
j;-: £
0,-Ccst
JL'rvr.

£J/J/t>S. 1 ¦+ /ACS.
0/tJd J^buJEK rttriAST*
CfA*	vf/^r/OA/	/Peerofe
/>!£ 7V/0 J)






»'7T
¦
—————

c
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•tf/jrjai/
J£/>T£
Field and Laboratory Blanks
Field filter blanks are collected and weighed one in every ten
samples with " minimum of two if less than ten Alters are collected.
Acetone blanks are collected and analyzed at approximately the same
rate as the filters. In addition, laboratory blanks are analyzed during
each batch analysis.

-------
U-0' '
Attachment III
PARTICULATES AND SULFATES ON WATER IMPINGERS
General
The impinger solutions are received in quart jars with Teflon lined caps.
After logging sample in, the volume in each jar is measured and a 250 ml
aliquot is removed for analysis.
Analysi s
Particulates
a)	Total - transfer the 250 ml aliquot into a desiccated and tared 250 ml
beaker, place in 90°C oven until dry.
b)	Organic - transfer the 250 ml aliquot into a 500 ml separatory funnel
and extract 3 consecutive times with 20 ml aliquots c; crcfcr.r.,
collecting the chloroform extract in a desiccated and tared 100 ml
beaker. Evaporate the chloroform extract to dryness by blowing a small
stream of nitrogen over it in a hood.
c)	Inorganic - transfer aqueous portion of (b) into a desiccated and tared
250 ml beaker. Place in 90°C oven until dry.
Place and leave dry beakers in a desiccator using (indicating desiccant)
for at least 24 hours and until the gross weight of each beaker is
stab i1ized.
Sulfates
100 ml of deionized distilled water was added to weaker. The beakers
were swirled gently, covered with parafilm and allowed to equilibrate for
24 hours bef-— "1	v;era re moved for sulfate analysis. ^Described on
following page.)

-------
- 2 -
D-7'
Methodology for Sulfate Analysis
Sulfate analyses v/ere performed according to Method 8 (Federal Register,
Vol. 36, No. 246--Thursday, December 23, 1971, pp. 24893-24895). Briefly,
the method is as follows:
Into a 250 ml Erlenmeyer flask was placed:
1.	A known aliquot of sample
2.	Deionized distilled water bringing the volume to 25 ml
3.	100 ml of isopropanol
4.	4 drops of thorin indicator
This orange solution was titrated to a pink endpoint using a 0.01 N barium
perchlorate solution.
Each day the Ba(C10^)o section v/as standardized against a O.01 M
standard solution which had been standardized against a 0.01 N NaOH
standard solution.

-------
AIR — SOUKCE TESTING FOR I WCUL/UES MO SULFATES
SAMPLE INFORMATION
PARTICULATES
00
I
o
KjjMjjijmwwWWjg
DESCRIPTION
TOTAL
VOLUML
Al. IQUO&J
USED H| BEAKER ft
~:i?i iL-*.
GROSS WT.
'¦'T-r-T.rrr
TARE WT.
~ i'r! T"1 i'¦ "
MET WT. |
i "ju'f .fi ¦ j»m %
SAMPLE
ALIOUO
ML
riTRArn
INITIAL
(so4)
"-3T
D1L
ACTOR
TOTAL J: SAM.VOL.
50,," M.LIQ.USED
TOTAL
S04a
ib&sx.
TOTAL
PART 1C.












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SULFATES
FINAL RESULTS

-------
D-9
SULFUR DIOXIDE EMISSIONS FROii 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% hLO^ diluted to 100 ml with deionized-distilled
water, the third impinger Ts empty and the fourth impinger contains
approximately 200 g of indicating type 6-16 mesh silica gel.
Particulates, sulfites, and sulfates and s0? are caught in the
first and second impingers. The sulfur dioxide is oxidized by the
hydrogen oeroxide to sulfate (S0.= ^:
S02 + H20 -v H2S03
H2S03 + H2°2 H2° + H2S04
The third impinger collects and carry over from the second arid 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
s-'ilfate. The sulfate 1-	by	titration with a standardized
_¦	o.ci i.: 80® isopropanol,
which enhances the formation of barium	sulfate and sharpens 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 Barium Solution
A standard solution prepared fr :i acidimetric grade potassium
hydrogen phthalate (KHP) is used to standardize a sodium hydroxide

-------
D-10
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 stoiciometry are described
below:
KHP + NaOH — NaKP + HgO
2NaOH + H2S04 — Na?S04 + 2^0
H2S04 + Ba(C104)2 -- BaS04 + 2HC1Q4
= (voK Na0H) (N Ne0H)
(H NaOH) = (weight KHP , <.)
XZM.2 q/eq}(q) (1 NaOH)
(vol. NaOH) (N NaOH) = (vol. H^) (N H^SO^)
(N H_S0,} = (vol, HaOH) (N NaOH)
1 4	(vol. H2S0^T"
2N h'2S04 1 M H2S04 = 1 H SQ^ =
(vol. H£S04) (M H?S04) = (vol. Ba(C?04)2) (M Ba(C104)2)
(M Ba(ClOj = (vol. HoS0„) (M H„S0J
4 (^^rr^ip4-
Analysis of Hydrogen Peroxide Sanples
Since hydrogen peroxide samples are mostly water, 100% isopropanol
must be added to the artiquots to obtain an optimum concentration of 80%
isopropanol. Table I indicates what volumes of 100% isopropanol are re-
quired for various aliquot volumes tD meet the optimum 80% final volumes.
I £1 l_ . ^ -
Sample
A1iquot
ml
20
15
10
5
2
1
0.5
Required
1 COS







Isopropanol
ml
80
60
40
20
8
• 4
2

-------
D-n
Before the mixture is titrated with the standardized barium per-
chlorate, the total volume in the flask is adjusted to 100 ml v/ith 80%
isopropanol. Four drops of thorin indicator are added and the solution
is titrated to a pink end-point. Replicate titrations should agree
within 1%.

-------
APPENDIX E
CHAIN-OF-CUSTODY PROCEDURES AND RECORDS

-------
nHntrtiH a*:' c
ENVIRONMENTAL PROTECTION AGENCY
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
CHAIN OF CUSTODY PROCEDURES
June 1, 1975
GENERAL
The evidence gathering portion of a survey should be characterized by the minimum
number 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
v/ill be determined prior to the survey.
Chain of 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 v/as in your physical possession and then you locked it up in a manner so
that no one could tamper with it.
V."	i ve .= eery : f the survey study plan and will be
knowledgeable of its contents prior to the survey. A pre-survey briefing will be held
to re-appraise all participants of the survey objectives, sample locations and Chain
of Custody procedures. After all Chain of Custody samples are collected, a de-briefing
v/ill be held in the field to determine adherence to Chain of Custody procedures and
v;!iether additional evidence type samples are required.
SAMPLE COLLECTION
1.	To the maximum exeunt achievable, as few people as possible should handle
the sample.
2.	Water, air, or solid v/aste samples shall be obtained, using standard field
sampling techniques.
3.	Sample tags (Exhibit I) shall be securely attached to the sample container
at the time the complete 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 JI ~. 1, second sample - sequence '	' "jlyses required and
samplers. The .hjsc. ae ' .	oaiipoint (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
contamination.
5.	A pre-printcd, bound Field Dct* ^.eccrd	shall be maintained to re-
cord field measurements and other pertinent information necessary to refresh
the sampler's 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 II and III) have been established to minimize
field entries and include the date, time, survey, type of. samples taken,
volume 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 bo signed by the field samplei . The preparation and conser-
vation of the field logbooks during t^e survey oe the responsibility
of the survey coordinator. Once the survey is complete, field logs will be
retained by the survey coordinator, cr 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 12 the receiving laboratory or turned
over to an assigned custodian. He r.jst assure that each container is in his
physical possession or in his view e: all times, or locked in such a place
and manner that no one can tamper witr. it.
7.	Colored slides or photographs should be taken which would visually show the
outfall sample location and any water pollution to substantiate any con-
clusions of the investigation. Urit.en documentation on the back, of the
photo should include the signature c:" the photographer, tine, elate and site
location. Photographs of this nature, which may be used as evidence, shall
be handled recognizing Chain of Custccy procedures to prevent alteration.
TRANSFER OF CUSTODY AND SHIPMENT
1.	Samples will be accompanied by a Chain of Custody Record which includes the
name of the survey, samplers' signat-res, static ^-ber, station location,
date, time, type of sample, sequence -umber, numoer ur I'.rjrz- analy-
ses required (Fig. IV). When turning over the possession of samples, the
transferor and transferee will sign, cate and time the shoat. This record
sheet allows transfer of custody of : group of samples in the field, to"the
mobile laboratory or when samples ar= dispatched to the fJEIC - Denver labora-
tory. When transferring a portion of 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	--'!-'->'-:jishing the samples. The field
laboratory person receiving the sacp; = 5 w. ii 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 properly packaging and dispatching samples
to the proper laboratory for analysis. The "Dispatch" portion of the "Chain
of Custody Record shall be properly filled out, dated, and signed.
3.	Samples will be properly packed in shipment containers such as ice chests, to
avoid breakage. The shipping conteiners 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 oricinal will accompany the shipment, and a
copy will be retained by the survey coordinator.
5.	If sent by mail, register the package with return receipt requested. If sent
by convr.on carrier, a Government Bill cf Lading should be obtained. Receipts
from post offices, and bills of ladin; will be retained as part of the perma-
nent Chain of Custody documentation.
6.	If samples are delivered to the laboratory when appropriate personnel are not
there to receive them, the samples r-;t be locked in a designated area within
the laboratory in a manner so that r.o one can tamper with them. The same per-
son i::ust then return to the laboratory and unlock the samples and deliver
custody to the appropriate custodian.

-------
3
E-3
LABORATORY CUSTODY PROCEDURES
1.	The laboratory shall designate a "sample custodian." An alternate will be
designated in his absence. In addition, the laboratory shall 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 custodian, 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.	Immediately upon recent the cus.o-Msn will place the sample in the sample
room, which will be locked at all tires except when samples -j-oved 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-sensitive 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 of 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 abnormal ties which occurred during the
testing procedure. In the event that the person who 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. 23758, October 16, 1973. If laboratory personnel deviate from
standar-' - they should be prepared to justify their decision dur-
ing CrO;j-.-,',_	ailCil.
9.	Laboratory personnel are responsible for the care and custody of the sample
once it is handed over to them and should be prepared to testify that the
sample was in their possession and 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-
gether 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.
11.	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.

-------
E-4
EXHIBIT I
EPA, NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Slation No.
Dalo
Time
Scqucnco No.
Station Location

Temp
2
u
«
_BOD
.Solids
.COD
_Nulricn}j
Samplers:
_MolaIs
_Oil end Grease
jy.o.
.Bad.
_Olfior
RomarS^ypfosorvative:
Front
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
53, sex	Denver federal center
DENVER, COLORADO 80225
*	xj

Back

-------
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
f
'"o ajf '¦"' ^ -1 — is ' L-
SAMPLERS: (Signature)
¦/ .Tty
STATION
NUMBER
STATION LOCATION
DATE
TIME
Sample type
SEQ
NO.
NO OF
CONTAINERS
analysis
REQUIRED
Wo
Comp
ter
G rao
Air
.Cot
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r?(
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it a vG
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Relinquished by: /Signature)
.fss-.r,< .^.1
Received by: (Signature)
Dcrc
'T-
/ J 1 111 w
Relinquished by: (Signature)
Received by: (Signature)
Date/Time
Relinquished by: (signatu.e)
Received by: (Signature)
Date
/Time
Relinquished by: (Signature)
Received by Mobile Laboratory for field
analysis: (Signature)
Date
/Time
Dispatched by: (Signature)
Date/Time
Received for Laboratory'by: 7
Date/Time
y i V,
Distribution: Orig. — Accompany Shipment
1 Copy—Survey Coordinator Field Files
«GPO 679-040

-------
E-6
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY,
1". I.:.'
SAMPLERS: fSignofureJ
s	i
i A ;
y
/.--V
STATION
station LOCATION
DATE
TIME
SAMPLE type
5EQ
NIC
NO OF
CONTAINERS
ANALYSIS
RfcOUIREO
Water
Aif
Comp
G rab
/;?o t
ro -i v-'-'¦'''
/ / —
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Relinquished by: (Signature)
¦y - /-

Received by: (Signature)
Date/T ime
Relinquished by: (Signature)
Re!i- -vished by: (Signoiu.-ej
Relinquished by: (Sig/ia/ureJ
Received by ! (Signature)
Received by: (Signature}
Received by Mobile Laboratory for field
analysis: (Signature)
Date/T ime
Date/T ime
Date/Time
Dispatched by: is ignature)
Date/T
ime
Received for Laboratory by^

Date/Time
¦?/
%A
*)<>£
Method of Shipment:
"V'
A
Distribution:" Orig — Accompany Shipment
1 Copy —Survey Coordinator Field Files
•SPO 679-040

-------
APPENDIX F
PRODUCTION DATA AND PROCESS WEIGHT CALCULATIONS

-------
¦ rtciy i'rowa Daud
Name:


FCC Feed 1 CO Bo
J a. fl . . , |
£b±xs*?|| Air(cfm) 1 Air Feed
i 1 er
Gas BTU Val
Primary
Voltaqe
ESP
. Primary . Secondary
I Amperaqe S Amperaqe
. Spark
I Rate
L- ¦' /oTFn
3S». Z_ //S~. /f 7 i
o~<>
(o cf

3 5 .S~
—"T s ' -r —¦>
.'J />.-
] ^ ^ ^ M m,
_/£2	
	/a	...
	c?.........
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-------
Refinery Process Data
Name: /ffrZtec.
,X»* a •*
te:	— c//tz/y7
	X >y.	^	
C1 ock
T i me
^ , r , FCC Feed
pre.^v\ pir^cii' 
Oil (bb 1 s) &i2^rstW?y1
/-U b/cuJsv
sue1' Ft—>•-'
( fV'O
Da
C/////~7 ~~7
QoL\i> A/% ' x /
To^ CO Boiler ^
p?£c i#/ rz/Tt'^
4(/C~ C^i?jZO\T

-------
"F-3J
T~''' •- /-•'"L •- : ~ ' 7 < .'v vs
¦ts>y (\
/•• ca__ r* «•»% i>r) y../^z&.ciCLf^- e. JsL'Jzl.
	/Cy/_		_ /•?
	/T-r.  	/-I'l"-: .
-/o.	t-fy		//y f/io		
//	/%			/£.. 	/.%..? So

-------
APPENDIX G
TEST DATA AND EMISSIONS CALCULATIONS

-------
APPENDIX G

-------
5-2

-------
Plant
vr
P/.T tL^ 	DL	
IMPORTANT - FILL IN ALL BLAITCS
Location
/*&jL
Date
—XX •—**—
Ope rator	
Re and record at the start of
e;i test point.
Time: Start Time_
End Time
Ambient Temp "F &
Bar. Pres:.. "Hg	
Assumed Huisture Z
Probe Tip Dia. In.	3^^
Pitot Tube No. //' - ^2
Sample Box No.
Meter Box No.	
Me t e r A .	/.7r
C/a
C-Factor
26.
[/(fCoc < Ty y^A UC.CS c
Probe Length/type_
Filter No. 4St£~ ,
Point
Clock
Dry Gas
Meter, CF
Pitot
in. H,0
AP
Orifice All
in H20
Dry Gas Temp.
°F
Pump
Vacuum
In. II-
Impinger
Temp.
°F
Oven
Temp.
*F
Probe
Temp.
° F
Stack
Temp.
°F
Stack
Temp.
°F
(#F+460)
Desired
Actual
Outlet
Inlet



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Comments :

-------
G-4
P'snt -Proper,' h-c	 Location Pf.(\ -S^r.k	
Unit 	 Run No.	/	Date *? / tf/V 7
Vm - volume of gas metered	fe. 9 Q Ft3
- barometric pressure	3Q. *r ^	in Hg
AH - average orifice pressure	O. b O in
Tm - average meter temperature	
-------
G-5
Plant
Unit
Location £ CC
Run No.
Date
1. Meter Volume
Vm$td =17.65 Vm
AH
Pk + 13.6
Tm
= 17.65 U-&.3 9)
'6. Ft3
2. Volume of water collected
Vw = .0472 Vu
= .0472 (/<%.$)
= f Ft3
3. Moisture
Bws - V
-------
Wet Molecular Weight
Ms =Md d- Bws) + 18 (Bws)
= ^1(1 -0.it) + 18 (0./2. )
= ?/ (i^-V-Z.) (2?, 02.)
= I 8.73 Ft/sec
O.Oi

/
— f
O.OG *" • O-z.'iS
C. O 7^~ ~ <9. 2 £.5"
0.c-£
O.
¦).oci L - (O. i:0O -
Stack Gas Volumetric Flow Rate
530
Ts
Qs - 3600 (1- Bws)/Vs As
= 3600 (1- L) (/= 7c) (r5Z3
= /. 7 X lO'* SFt3/hr 2c: r

¦ Ps



29.92

"530"

J'<3-
v?_


29
.92
Mass Emission Rate (Front Half)
A. Area Basis
MER =
a
(As)
(ms) (An)
453.59 (Theta)
i ) h	
453.59 (
",il~T- / ^
rflio^Ci-sle	COIC.
O.O&Z-z'	-
Q	OC5 f
£ .^/ 1
0.OSS9	f AcP
lbs/hr

-------
G-7
3
B.	Concentration Basis
MER =	("is) (Qs)
c	(Vmstdj (453.59)
( ) ( . ?
1) (453.59)
=	Ibs/hr
C.	Average Emission Rate
MER = MERa + MERr
AVC 	
= ( ) + ( )
2
-	lbs/hr
9. Mass Emission Rate (Total)
A. Area Basis
MERfl =
(AsJ
(ms) (An)
_453.59 (Theta)
/
= (.2^) (r—jf)
453.59 ( /. lbs/hr
C o fi < r <-« -r / o t'l F)
JJ'ZCr.r, r eve, 3
C-	^
JS6-V/
0
.09 lO

-------
G-8
C. Average Emission Rate
MERa + MERC
MER
AVC
. UV.7>Ui.6 )
2
= 23. J lbs/hr
10. Emission Rate
A. Front Half
ER_ =
MER
AVG
r
lbs/106 BTU's
6. Total Catch
ERi
MER
AVC
lbs/10 BTU's
11. Isokinetic
I =
100 Tf
(.00267) VLC
Vm
Tm~

60 Uhetaj^ F An
100(^8) (.00267) (/flkfi) +	&)'YO+ O.C?o )
(s Y< <1	13.6 .
60 (3^ } [iS. 78)	[O.oootf
) [0.2.SC + 2.0& )
{T7TJ~1
/o3
%

-------
G-9
12. Point Isokinetic Equations
a. I = *
0944 Ts Vmstd
Ps^s An ^Thst?"' H- Bws)
= -0944
{Zo.hi) ($4 )	(1 -o.il)
Ts ^mstd
s\r s
= (O.C60) Ts fastd , 103%
aT S
Vm = 17.65 Vm
std
p AH
Pb + T36
Tm
= 17.65 Vm
AH
+ 136
Tm
riJ.c = 85.48 Cn V£F ,/Ts.
/XAs	P	V Ps Ms
= 85.48 ( ) Vff" A j5{ ^
¦ ( » ^ /r^

-------
Plant

PARTICUL.'1 /IELD DATA
VERY IMPORTANT - FILL IN ALL BLANKS
Run No.
y—/&>/
Location
Date
"7
Operator

Rc&/pA^Or.	j~l_
1 ^
Sample Box No.	
Read and record at the start of
each test poLnt.
Time: Start Time ~7-
End Time
Ambient Temp °F	^7 $
Bar. Press. "Hr ZL ?,
Meter Box No.
Assumed ?!¦ '.-:ture Z
Probe Tip i.a. In. / 3s7/
Pitot Tube No. /C> -- c{
Probe Lenf,; h/type /V^T
Filter No. '/& .	,	
Meter A -jLZZ
.¦7C
(^Factor
Point
Clock
Dry Gas
Meter, CF
Pitot
in. HjO
AP
Orifice AH
in 1120 Y
Dry Gas Temp.
°F
Pump
Vacuum
In.' Hg
Impinger
Temp.
°F
Oven
Temp.
°F
1'robe
Temp.
"F
Stack
Temp.
° F
Stack
Te^.
("F+460)
Desired
Actual
Outlet
Inlet
Z. &/.
*r
c.J<$c AT

,/jt'


^JcAi

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4*4

Comments:

-------
Sheet of
Point
Clock
Dry ( ;
Metei CF
Pltot
in. H20
AP
Orifice AH
in H20
Dry Gas Temp.
°F
Pump
Vacuum
In. Hg
Impinger
Temp:
'F
Oven
Temp.
°F
.
Probe
Temp.
°F
Stack
Temp.
° F
Stack
Temp.
°F
'(°F+460)
Desired
Actual
Outlet
Inlet
.4 /
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j - .c
O/ dF
PO





V/c/77

/l$h
/'A=
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79
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(p. c r

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r
-------
Sheet "3 of 5*
Point
03

z
e/-
<>
Clock

fa :/X/9
Ac tA
' /°>Tr 'C-
Dry G j
Meter, CF
/r? o J
/£v £2:
ikL^r^
.-AjL
Ar C ?
£c^/' /g ^ Cj
Comments:
3/16/77
Pitot
ir. H20
P
Orifice AH
in H20
Dry Gas Temp.
°F
Pump
Vacuum
In. Hg
Impinger
Temp.
°F
Oven
Temp.
° F
Probe
Temp.
°F
Stack
Temp.
° F
Stack ¦
Temp.
°F
(°F+460
Desired
Actual
Outlet
Inlet
c or
6.6 2
d". 6 2
rc
r/
/- .1
rt

r? 9?


c c 9
c> 6 f
c.£ 7
ro
r/
//
r?
.1-7/
-23£
4/^6"

. or

d-63-
TC
r/
AY
rr
:2,2&
::>9o
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I
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-------
G-13
SAMPLE CLEANUP SHEET
Plant:		n Date: 9/ f~7	
Address:	Operators:_
Station No.: /	'	:	
Run No.:	/	Ambient Temperature: Q(^
Barometric Pressure:	Sample Box Number: 72	
Impinger 1
Final Volume_ Pi-
Initial Volume [ftp
Volume collected •?/
Impinger 2
Impinger 3
_ml of H^O
_ml
ml
Final Volume lift	ml of ('*)
Initial Volume lOO	ml
Volume collected /T	ml
Final Volume		ml of_
Initial Volume	O	ml
Volume collected C? ml
ml af
. ml
^sTml
-«wp




Final weight ^ . £ gm of	A&jP
Initial weight GTP.. yr gm
Weight collected /~2., ? Qm
Total Volume Collected JC 
-------
G-14
Plant K-
\ \ \
Unit /- C C C~tn c k
Location Scy.'H-.ri r ^ p r; r, c,:.-. . C-^t
Run No.
_2	Date 9 11Q 111
Vm - volume of gas metered
- barometric pressure
AH - average orifice pressure
Tm - average meter temperature
V^c - volume of water collected
C0£ - concentration of CO2
O2 - concentration of O2
CO - concentration of CO
Cp - Pi tot tube coefficient
AP - average velocity pressure
Ts - average stack temperature
Ps - average stack pressure
As - area of the stack
Theta - sample time
An - area of the nozzle
0 ** nc t ^ji i v w j : — ^ ^ ^
H - energy input
=1.0 & Ft3
in Hg
30. 10
0. £> 7	in ^0
'T-y -
:/3
14.8
14. Z
0.<-, - •<-
- - . - -1 <~
¦ 1 1
L1 , ! - f\

-------
Plant

Run No. ^ 	/ / J? /
Location A
Date /^/,r 7^
'/{X) :4l7
Operate Vh^,U>\'-/-b& 		

Sample Box Nj.
Meter Box No.
Meter A H
^>Factor_
r?
/¦yr
>7 (r
PA.	0 D
V Y IMPORTANT - FILL IN ALL BLANKS
1> .;d and record at the start of
e ch test point.
T ¦ tue: Start Time /-f? Yj3
End Time
Ambient Temp *F *-•' / J1
Bar. Press. "Hg_
Assumed Moisture Z / V
Probe Tip Dla. In¦ . '7/
Pltot Tube No. /~
Probe Length/cype_ ''c-s- /
Filter No.	.	
Point
CJ
Dry :as
Mete •, CF
Pltot
in. H20
fiP
Orl 1 .e AH
ii t20
Dry Gas Temp.
"F
Pump
Vacuum
In. Hg
Inpinger
Temp.
°F
Oven
Temp.
°F
Probe
Temp.
"F
St .ck
Tt. p.
" !'
Stack
Temp.
#F
("F+A60)
Des! d
Actual
Outlet
Inlet
/&A
r/
r'tT / ' <¦
/
r' //
> -
O.







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	j-
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1


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-------
Sheet ,% of ^3
Point
Clock
Dry t' as
Mete', , CF
PItot
in. H-0
AP
Orifice i 'I
in H20
Dry Gas Temp.
°F
Pump
Vacuum
In. Hg
Impinger
Temp.
°F
Oven
Temp.
° F
Probe
Temp.
°F
Stack
Temp.
°F
Stack
Temp.
°F
' (°F+^6G
Desired
Actual
Outlet
Inlet
b%
ibtx
l^o, $"-?
b of
. L?Cz>


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Consents:
3/16/77

-------
Sheet j3 of 3
Point
Clock
Dry G: ;
Meter., CF
r ot
j . h2o
\P
Orifice AH
in H20
Dry Gas Temp.
°F
I
Pump
Vacuum
In. Hg
Impinger
Temp •.
°F
Oven
Temp.
°F
Probe
Temp.
6 F
Stack.
Temp.
°F
Stack
Temp.
°F
(°F+460
Desired
Actual
Outlet
Inlet
A3
m'o
Z O 0 38
0?
c^-- &
Or-^f
O.CC
&/
go
'¦1
<»7
ZO
-2,36"
H^c(

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17.33
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CD
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Comments:
3/16/77

-------
SAMPLE CLEANUP SHEET
G-18
Plant:	sGsS 	Date:
Address: ~C.^r	Operators	
Station No.: yyz:/		
Run No.: ^,12	A"'.:¦' t Temperature: ^9
Barometric Pressure:	Sample Box Number: r?
Impinqer 1
/ fy mi of yv
Final Volume	
Initial Volume /#&	ml
Volume collected <$£/ ml
Impinqer 2
Final Volume	//^	ml of U- e^-
Initial Volume /&C	ml
Volume collected / 3.	ml
Impinqer 3
Final V o 1 um e	Q_	m ^ 0 ^	-.^r - -
Initial Volume	p_	ml
Volume collected	C ml
Impinqer
ml of
Volume collected	mT
, •
Impinger
Final vjeight ^7Z./	gm of		
Initial weight £?(?/.J2	gm
Weight collected /Dt 8 gm
Total Vo"1'^ Coi1 pcted //1/„ 
-------
G-19
Molecular Weight Determination
Station Mumber j O j f	
Method of Analysis: Fryrite
Orsat 	
Sample Type: ^Irab 1/	
Integrated 	
Run
No.
Tims
co2
¦ o2
CO
Collected
Analyzed
1
U2>0
U30
«7 'S/tss
2-1/z.S-/.

1
&30


&$/ O.g/
1,0











































Leak Check:	
Og Vyii jC.-x	/a Sya 		
CO2 Check	% against
Signature:	 Date:
Remarks:

-------
U-20
Plant V-
Unit
FCC C-l-f.ck
Location ;>¦. . rrr. P., ^ 0i ' c
Run No.
3
Vm - volume of gas metered
P^ - barometric pressure
AH - average orifice pressure
Tm - average meter temperature
Vi „ - volume of v/ater collected
C02 - concentration of CC^
O2 - concentration of 0£
CO - concentration of CO
Cp - Pitot tube coefficient
AP - average velocity pressure
Ts -• average stack temperature
Ps - average stack pressure
As - area of the stack
Tfteta - sample time*
An - area of the nozzle
ms - weight collected
H - energy input
/ '
JdU
Date ? /at 7 7
.5 7.3/
2-9.9:
j" - ¦
OP.
!%. f
tS. :j
6. 76
6.01Q
ciir.
zq.n
iSO.2. 
-------

py
L.'
.d r
AJ>
VERY IKPOKTAN'T - FILL IN ALL BLANKS
Run No.-?
/r^y
Operat or/,-1-^ A.
Locatloiu^^j^
Date	7
Sample Box No.
Meter Box No.
Meter A H
C^Factor_
Read and record at the start of
each test point.
Ambient Temp *F
Bar. Press. "He	
Assumed Moisture Z
Time: Start Tirr.e_
End Time
/ooL!
Probe Tip Dla. In. 0.3^/
Pitot Tube No. yfi~- 	
Probe LenRth/type /£u f
Filter N	.	
/•
c.?c:
CfffzrCh£dK<® '^'Ak =~ • OfaCrr^
Point
Clock
Dry Gas
Meter, CF
Pitot
in. H-0
AP
Orifice AH
In H20
Dry Gas Temp.
°F
Pump
Vacuum
In. HS
Inplnger
Temp.
*F
Oven
Temp.
#F
I'robe
T e nip.
"F
Stack
Tetnp.
*F
Stack
Temp.
"F
CF+460)
Desired
Actual
Outlet
Inlet
^/2f
"/DC/
207. Zl











0> ft/
/ooj
zoS-H 1
O o'7
• ^2_

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7Y
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7<

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ao?.-n
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7<
75"
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7<
26^

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-------
Sheet of 9-—
Point
Clock
Dry Gas
Meter, C ¦'
Pitot
In. H~0
AP
Orifice AH
in H20
Dry Gas Temp.
°F
Pump
Vacuum
In. Hg
Impinger
Temp-.
°F
Oven
Temp.
• °F
]' robe
Temp.
°F
Stack
Temp.
°F
Stack ?
Tenrp.
°F
'(°F+A60
Desired
Act !.
Outlet
Inlet

7/o?
,99^-O'r


r?/0 /"L
?c.Kf®
17'/A
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7^/-^ :





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Wl
q$y

Comments:	jJ0(J	R	!° f[f\~ .OlfrC-fl*1
3/16/77	^ ^	' ¦+. $-? ^&°

-------
'6-23
SAMPLE CLEANUP SHEET
Plant:		Date:		
Address':		Operators:	
Station No.: /rr/
Run No.: ^ ^	Ambient Temperature:	
Barometric Pressure:	Sample Box Number: ,^>
Impinger 1
Final Volume	!&&	ml of J J c—si~7~cr,i
Initial Voluine		ml
Volume collected Tf ml
Impinger 2
Final Volume	} OO ml of dd
Initial Volume /go	_ml
Volume collected o ml
Impinger 3
Final Volume	^	ml of
Initial Volume	£	ml
Volume collected n	 ml
Impinger
V
Final Volume_
Initial Volume	
Volume collected
Impinger

_ml of_
_ml
ml
Final weight	
Initial weight	
Weight collected_
£ fe.3 gm 0f_
6 7l-. £ gm
T. > qm
rc..i
C
Total Volume Collected	ml
Fi1ters
No.
yf
gm
_gm
Trsv P V|? '
	gm
	gm
Weight
Col 1ected
_gm
gm
Cleanup performed by
on

-------
6-24
Molecular Weight Determination
Station Number Sf&f —	J5*
Method of Analysis: Fryrite	y	
Orsat
Sample Type: Tirab	V
¦¦¦¦	| ¦¦ 1	¦
Integrated 	
Run
No.
Time
co2
°2
CO
Col lecteci
Analyzed
)


/Tc
7 c
r;
2
9. ft

/
2-C
0

/D'. <-c
/O'-co
/5:
Signature: /y ,¦		 Lsce:	/' 7"
Remarks:

-------
G-25
Plant	¦<¦-(¦^1. t	
Unit /:~r c7-	A~	
Vm - volume of gas metered
Pb - barometric pressure
AH - average orifice pressure
Tm - average meter temperature
Vic - volume of water collected
CO2 - concentration of CO2
O2 - concentration of O2
CO - concentration of CO
Cp - Pi tot tube coefficient
AP - average velocity pressure
Ts - average stack temperature
Ps - overage stack pressure
As - area of the stack
+"jme
An - area of the nozzle
ms - weight collected
H - energy inpu'.
Location C> ' /"•- "¦ v. -. y.
Run No. l/ Date V//-/? 7
t
' '///:•> Ft3
? 9.:-rr in Hg
	-r -r	in H2O
-r °R
	'7 .v / 	ml
		%
		%
%
in H^O
°R
in HgO
Ft2
min.
Ft?-
mg
10G BTU's

-------
Plant

Run No.
Y
¦To/
Location	s S/>f<:;~cr
y ^
Date_ 5S>/-*7	
Pr	5 D.
VERY li	tUTANT - FILL IN ALL BLANK'".
Read	record at the start of
each i	t point.
Amble,.t Temp °V
Bar. l'rress. "llg	
Assured Moisture 2
Time:
Operator	>t-/
Sample Box No.	
Meter Box No.	"2~
Meter A H /,ry'f
C^factor	
tart Titne_
nd Time
Probe Tip Dla. In. - ^
Pltot Tube No. /O


s
£>
pr>
r
Probi Length/type /cS-~
Flltt.- No./>£yx£.,	
d rj

I

Point
C lock
Jry Gas
Meter, CF
Pltot
in. H-0
AP
Orifice AS!
in H20
Dry Cos Temp.
°F
Pump
Vacui: 1
In. li-.;
Inpinger
Temp.
°F
Oven
Temp.
•F
Probe
Temp.
°F
Stack
Temp.
°F
Stack.
Teirp.
°F
CF+A60)
i/eaired
/¦ctual
Outlet
Inlet

cA
&&Ar c
A
h " //
? —
,

90
/' f>
ri
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72.
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Plant: y^
AZ.
Address: SU.^rc- /=<-
Station No.
Run No.:


Js#"-
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J2L
Barometric Pressure:
G-27
SAr^'.: CLEAr'!'"1 ^"EiT
	Date:
_0perators:_

_Ambient Temperature:,
_Sample Box Number:	
Impinqer 1
Final Volume	/s~V ml of
Initial Volume /cg	ml
Volume collected	•r ml
Impinqer 2
Final Volume	/n 9 ml of	K>/m.-y,oP S&L-.
Initial ,Vo 1 ume /e a ml
Volume collected	v	ml
Impinaer 3
Final Voiume	o	of		
Initial Volume	q.	
Volume collected o	ml
Impinqer
Final Volume^y	ml of	
Initial Volume X	ml
Volume collected	ml
Impinqer
Final weight	£C qm of j,L/c^ QtpL-
Initial weight <<•.£-/< 9 qm
Weight collected	y. ~7 qm
Total Volume Collected 1^ '? ml
Fi1ters
Wei ght
Tare Wei oh*. Collected
		gm		gm 	gm
	gm		gm 	gm
Cleanup performed by
on

-------
RECOftO OF VISUAL DETERMINATION C
COMPANY	OIL Cov
LOCATION	
TEST NU.'iEES / /fo/ .	
DATE 9/9 il^ ~~	
TYPE FACIL1TY (>L kk£-'¦ o£-0-0
CONTROL DEVICE	'
"*1—^ 		
M	!.. J
i\
O^o
®f&0
]ZZL
.J
-M
CLOCK TIME
OBSERVER LOCATi !
Distance to t; charge
Dfrection fn. Discharge
Hefght of Ob: .vatlon Point
BACKGROUND DESC PTIOf!
MATHER CONOITI .S
Kind Dlrectjc
Wind Speed
Ambient Ten;-., atur£
SKY CONDITION'S (clear®
overcast, % clouds3 etCo)
PLl'KE DESCRIPTION
Color
Dhtjr.ee Visible
OTIIW IliFORI'uMlOU
Initial
I&OO


Final
^bo


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lJ


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(%-% g-Pfr' 	
POIJiT OF EMISSIO:;S ^.-VK	
		 HEIGHT OF DISCHARGE FOI.'IT £c>o ' 	
SUKftRY OF AVERAGE OPACITY
Set
Number
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the tirr.c evaluation was rcade.
CD
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-------
cr>
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	 type rAc inrr c--.¦ / /.-v-a-,
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(Fit Dos.74-201J0 Tiled 11-11-H;U:4S tai)
fEDCRAt. MG.'ITEX, VOL 37, NO. 219—.TUESDAY, NO'.TMGtK 12, )9r<

-------
RECORD F yiSUAU DETEWUttTIOK of OPACITY
PAGc
cf
C( AKY Pc
QUO 6-C I A C.
Ll. AT IC N	(—c- S p .~~a vy
7i st number 	I	
DATE		
TYPE FACILITY a,' I a&^o ,-^
CONTROL DEVICE £ ;_P	
(Q)
oTMCn.

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INCURS OF OBSERVATION -j.'
OBSERVER TKo^a:p 6.. "R
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03SEIV/ER AFFILIATIC,N__Us£_£ : A/6
POINT OF EMISSIONS P£C -S ¦ 
-------
CO
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COX?AST
LOCATION
TEST	-7
91 -i / T

OBSERVATION RECORD	PAGE .
OBSERVER 1~Uo>^.ca^ C-
OF
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type rAcimr o;i
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OBSERVATION RECCR3
(Continued) *
PACS	OF	
COMPANY
iocAno:r^
TEST ll'JMSEK
DATE	
oascRvn _____
ty?e rACiim
POINT or CMJSSTwT
1
Mr. I t-Mn.
Sc
conds
STEAM PLUME
(chccV i f .iDfil feeble?)
COMMENTS
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C!c tacned
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apaky (ou>gfZf'^''
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03se;;ver affiliation 6-^" i^?-9-
POIIJT OF EMISSIONS
/z.7
height of discharge foint
OO
CLOCK TIMS'
OBSERVER LOCATION
Distance to Disch.
direction from Df:
Height of Observe
BACKGROUND DESCRIPT
MATHER CONDITIONS
Kind Direction
Wind Speed
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SKY CONDITIONS 2


















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, t--End
6 "77777
S'jn | Average
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Readings ringed from ,T to r- O % cpocit.y'
The source vms/'. -.s not In ccnplfance with 		.at
the time evdlua; on was rrade.

-------
CO
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OBSERVATION RECORD
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OBSERVATION REC0R3
(Continued)
PACE	OF
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ir :ArioM~^
1L' r II'JMSiR
DAI E	
OBSERVE* 	
TYPE FAClCTTr
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(chpcV 1 f jianl 1 c.'ble)
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[Fit Doc.74-2C1SO Filed U-1I-H;8;4S Oia!
•TDCXAt RISIITr?, VOL 37, NO. 21?-»TUc5DAr, NOVLMBK 12, W4

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TYPE FAC itTTT
PAGE	0F._
yc/77
POINT CF EMISSlOliS < ^t/r~
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OBSERVATION RECORD
(Continued) "
COMPAQ
lOCAriOtf\~
02SERVE3
TYPE FAC1CTT7
TEST UIT.SEKX
DATE	~*
FOIHT or EJUSSlfciS

Mr.
IMn.
Seconds
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[Fit Dos/M-SOliO Filed 11-11-7J;U:<5 tm]
fIDtRAt RICI5TE2, VOL 3?, NO. 219—.TUESDAY, NOVEMBIS 13, 1974

-------
comtm'PdW&R /a/<°
location J-DS A, tel. eS
TEST llUMZZ/tO / "ff= 3 .
DATE 9//J "¦¦ 	
TYPE FACILITY/?^ /
COIITROL DEVICE		
RECORD OK VISUAL DETCWIIKATIOK Or OPACITY
PA A?
AUu
HOURS OF OBSERVATION
OBSERVER /AM A/&->*SM A
OBSERVER CERTIFICATION DATl/Pf. A 7'7
OBSERVER Arr ILI AT ICII f* A	
POINT OF EMISSIONS 57~A^K 	
HEIGHT OF DISCHARGE FOIMT
CLOCK TIME
OBSERVER L0CAT1
Distance to r harge
Direction fri- Jlscharge
Hetght of Obse.vatlon Po"tnt
BACKGROUND DESCRIPTION
MATHER CONDITIO?!.,
Wind Direction
Hind Speed
Anblcnt Temperature
SKY CONDITION'S {clear,
overcast, % clouds# etc.)
PLUKt DESCRIPTION
Color
Distance Visible
0TIIL1 IHFORIJATIOII ^Ul/11 P
Initial
D9SS


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. jD 6 '7
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Readings ranged from -? to % cpacti.y
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the time evaluation was made.

-------
/<"
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OBSERVATION RECORD
PAGE
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CESEnVATIOM RECOW	PACE OF
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LOCATION
TEST ll'JI-'.SEK
DATE	
0DSERVE3 	
type FACiriT?
PQIIIT CF t^ISSlwT
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[Fit Do;.14-3(HS0 FUctf U-ll-7-i;ll:4J am]
FIDCitAl RIGHTED VOL 3?, NO. 2J9—.TUJSDAY, NOVEMBLK 12, 1974

-------
RECORD OF Y
'Po //(/£ £> }
COM?			
Iocat ;cn /-as* A	e
TEST K'JKCER J ft' -/.
DATE 77////7-7 	
TYPE FACILITY Zfc'/V/xg , ' V__
CO.'Hr.jL DEVICE

///-
CLOCK TIMc
OBSERVER LOCATION
Distance to Discharge
Direction from Dfschars
Height of Observation P .t
BACKGROUND DESCRIPTION
ViEATHER CONDITIONS
Wind Direct1on
Wind Speed
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SKY CONDITIONS (cioar„
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PLUMS DESCRI?TI0"{
Color
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CJ-eAfi-
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76
c+eAP-
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to '
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"crmOTION OF OPACITY
PAGc
cf
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*
£ d>3^'

HOURS OF OBSERVATION
OBSERVER 7^>/^ J/&. W --I-1 A
OBSERVER CERTIFICATION CATE.--//VP- '7 ~7
OBSERVER AFFILIATION J:/*, '	
POIliT OF EMISSIONS	.¦ ¦-
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O O '
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SUMMARY OF AVERAGE OPACITY
Set
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the time evaluation v;as made.
.at
CD
l
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-------
CT)
CO
OBSERVATION RECORD	PAGE	Or „
CCX?ANY	a	OBSERVER 7?/	4t 4 /¦*
LC^TICV	TYPE FACIUTTi- j=/a.V
TEST	7^ V"	POINT CF EMISr-i'ws'
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COWAVY
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TEST N'JMSElf
DATE
OBSERVATION RECORD
(Continued)
PASS	OF , ,
TYPE r/.ciLl"V ~
PoniT cr exissIwT
Mr.
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(c^ecV 1 f iido 1 Ic.'ble)
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[FU ;.1oc.1V201J0 Filed	rua]
KOtRAl MCISTE*, VOL 39, NO. 219—.TUEJDAY, OVEiMBtR 12, l?r4

-------
RECORD OF VISUAU DETEWlIfiATION, OF OPACITY
PAG" ' cf l
COMPANY fob
.o «£iw" i va-e-
o; I
LOCATION s>arv^ f e -S ,, - -
TEST NUMBER	
DATE gjT / M / 7"7	
TYPE FACILITY#.*! g g-^f 	
CONTROL DEVICE	"	

s t
	¦&¦
HOURS OF 03SERVATl0fl \HAO	
OBSERVER ' ^Q'WlkA Cj-.
OBSERVER CERTIFICATION L'ATE 0/30/7 7
03 SERVER ArF ILI AT ION l' t P fir ~ U&IC1.
'OIIiT OF EMISSIONS PCC S-fcoK 	
HEIGHT OF DISCHARGE FCINT ISO'
CLOCK TIME
OBSERVER LOCATION
Distance to Discharge
Direction from Discharges
Hefc^t of Observation Point
BACKGROUND DESCRIPTION
VitATHER CONDITIONS
Wind Direction
Hind Speed
Ambient Temperature
SKY CONDITIONS (clear,
overcast, % clouds* etc.)
PLl'KS DESCRIPTION
Color
0tstar.ee Visible
OTHER I.'IFOOTIOII
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/ cf^''cy


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the time evaluation was made.

-------
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(Continued) "
03SCaVE3 flower, £
TT?£ f/.CfLj'r1 cvTT
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JFH Do;.74-I01iO FiiNl 11-11	bjuJ
rromi wcister, vol a?, no. si?—Tuesday, KovtMsrc n, iw

-------
RECORD OF VISUAU DE7EWUMTI0K OF OPACITY
PAGE of
COMPA KY/Wfczff//^
LOCATICN	A/S&
test nukees. /tf O J
DATE /^/// /"7
TYPE FACILITY /?c?F/ A
COHTROL DEVICE ^	
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0 -ERVER 	
0 '.SERVER CERTIFICATION LV,TE_
C'.SEIiVER AFFILI AT IC.'I	
IViIIiT OF EMISSIONS
l.:iGI!T OF DISCHARGE POINT
CLOCK TIME
OBSERVER LOCATION
Distance to Discharg
Direction from Dfsch. s
Height of Observation flint
BACKGROUND DESCRIPTION
MATHER CONDITIONS
liMnd Direction
Wind Speed
Anbient Temperature
SKY CONDITIONS (clear,
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PLUK5 DESCRIPTION
Color
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Readings ranged fro.n /O to ? % epacli.y
The source was/was not in ccnpliancc with At
the tiir.c evaluation v:as made.

-------
CO
I
o
OBSERVATION RECORD
COXWWY fd >U<2% tvd
WJcnvCTpf
test vj.xsnr ;
eate 97///-7^
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[FR Doc.74-20110 FUMl lJ-ll-7i;U:
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