EPA
United States
Environmental Protection
Agency
Research and
Development
EPA-600/7-84-074b
July 1984
ENVIRONMENTAL ASSESSMENT OF
A CRUDE-OIL HEATER USING STAGED AIR
LANCES FOR NOX REDUCTION
Volume II. Data Supplement
Prepared for
Office of Air Quality Planning and Standards
Prepared by
Industrial Environmental Research
Laboratory
Research Triangle Park NC 27711
-------
RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
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The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
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6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
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This report has been assigned to the INTERAGENCY ENERGY-ENVIRONMENT
RESEARCH AND DEVELOPMENT series. Reports in this series result from the
effort funded under the 17-agency Federal Energy/Environment Research and
Development Program. These studies relate to EPA's mission to protect the public
health and welfare from adverse effects of pollutants associated with energy sys-
tems. The goal of the Program is to assure the rapid development of domestic
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essary environmental data and control technology. Investigations include analy-
ses of the transport of energy-related pollutants and their health and ecological
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This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
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EPA-600/7-84-074b
July 1984
ENVIRONMENTAL ASSESSMENT OF A
CRUDE-OIL HEATER USING STAGED AIR
LANCES FOR NOX REDUCTION
Volume II
Data Supplement
By
R. DeRosier and B. DaRos
Acurex Corporation
Energy & Environmental Division
555 Clyde Avenue
P.O. Box 7555
Mountain View, California 94039
EPA Contract 68-02-3188
EPA Project Officer: Robert E. Hall
Industrial Environmental Research Laboratory
Research Triangle Park, North Carolina 27711
for
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Washington. DC 20460
-------
ABSTRACT
This volume of the report presents emission results obtained from field
testing of a crude-oil process heater burning a combination of oil and refi-
nery gas. The heater had been modified by the addition of a system for in-
jection of secondary air to reduce NOX emissions. One test was conducted
with the staged air system (low-NOx), and one was conducted without it
(baseline). Tests included continuous monitoring of flue gas emissions and
source assessment sampling system (SASS) sampling of the flue gas with
subsequent laboratory analysis of samples utilizing gas chromatography
(GC), and low resolution mass spectrometry (LRMS) for organics; and ato-
mic absorption spectrometry (AAS) and spark source mass spectrometry
(SSMS) for trace metals. Flue gas concentrations of NOX were reduced 30
percent (from 83 to 56 ng/J) with the staged air system. Total organic
emissions dropped from 17.1 to 3.4 mg/dscm from the baseline to the low-
NOX test. This was primarily due to a reduction in the Cl to C6 boiling
point range compounds which constituted most of the organic emissions.
GC/MS analysis identified 11 semivolatile priority pollutant compounds in
both tests, most of them present in higher concentrations during the base-
line test. LRMS analysis suggested the presence of eight compound cate-
gories in the organic emissions during the baseline test and four compound
categories in the low-NOx test. Biological tests indicated that the organic
sorbent module extracts from both tests were of moderate toxicity and
moderate-to-high mutagenicity.
11
-------
TABLE OF CONTENTS
Section Page
1 INTRODUCTION 1-1
2 PRELIMINARY EQUIPMENT CALIBRATION 2-1
3 HEATER OPERATING DATA 3-1
4 SAMPLING DATA SHEETS 4-1
4.1 KVB Continuous Emissions Monitoring Report 4-2
4.2 Operating Data for EPA Method 5 4-21
4.3 Operating Data for Controlled Condensation Train . . 4-34
4.4 Operating Data for SASS 4-41
5 ANALYTICAL RESULTS 5-1
5.1 Ultimate Analysis of Fuel Oil 5-2
5.2 Composition of Refinery Gas 5-4
5.3 SASS Particulate Emissions 5-7 .
5.4 EPA Method 5 Particulate Emissions 5-13
5.5 Sulfur Oxides Emissions by Turbidimetric Analysis . 5-23
5.6 Trace Element Analysis 5-28.
5.7 Total Chromatographable Organics (TCO), Gravimetric
Organics (Grav), Infrared (IR) Spectra, Gas
Chromatography/Mass Spectrometry (GC/MS) and Low
Resolution Mass Spectrometry (LRMS) of Total Sample
Extracts 5-42
5.8 G^-CS Chromatograms 5-60
5.9 Radiometric Analysis Results 5-129
5.10 Bioassay Reports 5-131
Mutagenicity Evaluation of XAD Resin Extracts in the
EPA Level 1 Ames Salmonella/Microsome Plate Test 5-132
Cytotoxic Evaluation of XAD Resin Extracts in the EPA
Level 1 Rodent Cell (CHO) Clonal Toxicity Assay 5-168
111
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SECTION 1
INTRODUCTION
The purpose of this data supplement is to document data in greater
detail than was possible in Volume I (Technical Results) of this report.
It is intended to provide sufficient detail for researchers to perform
their own analysis of the data obtained. Readers are referred to the
technical volume for objectives, description of source emission results,
interpretation, and conclusions.
The remaining sections of this data supplement contain the
following information:
Section 2 — Preliminary Equipment Calibration Data
Section 3 — Heater Operating Data: crude-oil temperatures and pressures,
process rate, burner pressures, fuel flowrates
Section 4 — Sampling Data Sheets: KVB continuous emissions monitoring
report, operating data tables for EPA Method 5 (for particulate
mass emissions), controlled condensation (for S02 and SQ-$
sampling), and SASS (for trace element and organic sampling)
Section 5 ~ Analytical Laboratory Results: ultimate analysis of the fuel
oil, composition of reabsorber gas, SASS particulate
emissions, sulfur oxides emissions by turbidometric analysis,
trace element emissions by spark source mass spectrometry (SSMS)
analysis and atomic absorption spectroscopy (AAS) analysis; total
1-1
-------
chromatographable organic (TCO) and gravimetry (GRAV) results;
infrared (IR) spectra; determination of organic compounds by gas
chromotography/mass spectrometry (6C/MS); low resolution mass
spectrometry (LRMS) of total sample extracts; Ci-Ce
chromatograms, radiometric analysis results, and biological assay
reports on the SASS train samples.
1-2
-------
SECTION 2
PRELIMINARY EQUIPMENT CALIBRATION
2-1
-------
»T»
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2-2
-------
SECTION 3
HEATER OPERATING DATA
Process rate
Crude oil temperature and pressure
Inlet
Outlet
Reabsorber gas flow
Burner pressures
Oil
Steam
Gas
Crude API gravity
Tube temperatures
Notes
3-1
-------
UNIT OPERATING DATA
Test No. /
Date /*? <
/9? /
Location
_Engr-
Unit No. ///y/3
Unit Type £/
Fuel
Capacity
JJurner Type C
Test Description:
Test number
Time
Process Rate x 1847.7 bbl/d
Crude Tin (°F)
Crude Tout (°F)East
Crude Tout (°F-) West
Crude Pin (psig) East
Crude Pin (psig) West
Crude Pout (psig)
ReabsSl5U§! iT-o3 Scf/d)
Burner #1
Burner #2
Burner #3 oil P/steam p
Burner #4 (psig)
Burner #5
Burner #6
P to Burner #1 GAS
P to Burner #2 ,,
P to Burner #3 //
P to Burner #4 "
P to Burner #5 n
P to Burner #6 //
Air Registers (%open) ,
Crude API Gravity
Flame Observations
Tube 13 Pass A
Tube 13 Pass B
Tube 15 Pass A
Tube 15 Pass B
/
// • .5"6
6-3
,?.? 5
Lu-o
£3*?
130
- —
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3-2
-------
'iest No.
Unit No.
UNIT OPERATING DATA - CONTINUED
Date i*3iM&..rt& Locati on
Engr./' 2)&
11 If 13
Fuel
Capaci ty
Unit Type
Burner Type
Test Description:
Tube 20 Pass A
Tube 20 Pass B
Tube 25 Pass A
Tube 25 Pass B (outlet)
Stack
Gas Pressure to Heater
74**"
77=r
77
-------
Tost Ho.
Date
UNIT OPERATING DATA
Location 7~o&co
Engr
Unit No. 11HI3
Unit Type
Fuel 0.
Capaci ty
_Burner Type
Test Description:
Test number
Time
Process Rate x 1847.7 bbl/d
Crude Tin (°F)
Crude Tout (°F)East
Crude Tout (°F) West
Crude Pin (psig) East
Crude. Pin (psig) West
Crude Pout (psig)
69 Sxrz85.Bl Ifo3 scf/d)
Burner 11 \
Burner #2
Burner #3 oil p/steam p
Burner #4 (psig)
Burner #5
Burner #6
P to Burner #1
P to Burner #2
P to Burner #3 Gas p
P to Burner #4 " (psig)
P to Burner #5
P to Burner #6
Air Registers (%open) ,
Crude API Gravity
Flame Observations
. Tube 13 Pass A
Tube 13 Pass B
Tube 15 Pass A
Tube 15 Pass B
/
&fo
£.3
383
t>35
&3$
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3-4
-------
Test No.
Unit No.
///V/3
UNIT OPERATING DATA - CONTINUED
Date /% -.AM/.* x^ Locati on_
Fuel o
-------
UNIT OPERATING DATA
Test No. 3.
Unit No. liHl.
Date j^i ^7aM& m^l \
3 Fuel Ou- J&&C, \
Unit Type C/ZUTO. /-ife/m-tf. \
Location
Engr.
Capacity
Burner Type
Test Description:
Test number
Time
Process Rate x 1847.7 bbl/d
Crude Tin (°F)
Crude Tout (°F)East
Crude Tout (°F) West
Crude Pin (psig) East
Crude Pin (psig) West
Crude Pout (psiq)
ReabTS8E.gS IV scf/d)
Burner #1
Burner #2
Burner #3 oil p/steam p
Burner #4 (psig)
Burner #5
Burner #6
P to Burner #1 "'
P to Burner #2
P to Burner #3 Gas p
P to Burner #4 (psig)
P to Burner #5
P to Burner #6
Air Registers (%open) ,
Crude API Gravity
Flame Observations
Tube 13 Pass A
Tube 13 Pass B
Tube 15 Pass A
Tube 15 Pass B
SL
/O '• oo
d>3
356"
£^3
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Test No. 3
Unit No. ////y3
Date /9 c
Fuel
SiiMiS rfS 1 \
1
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UNIT OPERATING DATA - CONTINUED
tion -fisco
Engr.
Capaci ty
*3 5-0
• i—liniiLiii -.._
Burner Type
Test Description:
Us;>v6- J
-------
UNIT OPERATING DATA
Test No. £
Unit No. ///v/
Date /-5 ^-*
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-------
Test No._
Unit No.
UNIT OPERATING DATA - CONTINUED
Date /c
// tit 3
Fuel
_Capaci ty
Unit Type
Burner Type
Test Description:
Tube 20 Pass A
Tube 20 Pass B
Tube 25 Pass A
Tube 25 Pass B (outlet)
Stack
Gas Pressure to Heater
7v-^-
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3-9
-------
Note ~
1. Gas flowmeter dropped from 3.3 to 2.1 (x205856 scfd) when cofiring
with oil commenced.
2. During previous testing, KVB found the gas flowmeter to be reading
high. A correction factor of 0.83 should thus be applied to all
readings.
3-10
-------
SECTION 4
SAMPLING DATA SHEETS
4.1 KVB Continuous Emissions Monitoring Report
4.2 Operating Data Tables for EPA Method 5
4.3 Operating Data Tables for Controlled Condensation Train
4.4 Operating Data Tables for SASS
4-1
-------
4.1 KVB CONTINUOUS EMISSIONS MONITORING REPORT
4-2
-------
NOx EMISSIONS ASSESSMENT:
GASEOUS EMISSIONS FROM A
REFINERY PROCESS HEATER IN
BASELINE AND LOW-NOx
CONFIGURATIONS
KVB11 47800-1284
CONTRACT NO.
RB59313A
PREPARED FOR:
ACUREX CORPORATION
MOUNTAIN VIEW, CALIFORNIA
PREPARED BY:
R.J. TIDONA
KVB, INC.
RESEARCH AND ANALYSES DIV
JULY 1981
18006 SKYPARK BLVD., IRVINE, CALIFORNIA 92714 • (714) 641-6200
HOUSTON TX (713) 780-8316 • MINNEAPOLIS, MN (612) 545-2142 • HARTSDALE, NY (914) 949-6200
4-3
-------
ABSTRACT
Gaseous emissions were measured on a natural draft refinery process
heater in support of NO emissions assessment testing by Acurex Corporation.
Species measured continuously by KVB were NO, CO, C02/ O2, and SO2- Two test
configurations, baseline and low-NOx, were tested at a process rate of 77.11
m3/h (11,640 bbl/d) of crude feed. A mixture of refinery gas and No. 6 oil
was fired for both tests. The low-NOx configuration was obtained by staging
approximately one-third of the total combustion air. The staged air was
introduced through twenty-four lances (four per burner) at a height of 1.2m
(4 ft) above the fuel injection plane. The average baseline NO emission was
172 ppm, dry at 3 percent O2. At the low-NOx conditions the average NO
emissions dropped to 118 ppm, dry at 3 percent O2 for a reduction of
31.4 percent. This result was in accordance with expectations based on
previous tests taking into account differences in the relative proportions of
No. 6 oil and refinery gas fired in the present tests. Emissions of the other
continuously measured gaseous species at low-NOx conditions were largely
unchanged from their baseline levels.
KVB 11-47800-1284
4-4
-------
CONTENTS
Section Page
ABSTRACT 4~4
1.0 DESCRIPTION OF TESTS 4-6
2.0 GASEOUS EMISSIONS TEST METHODS AND INSTRUMENTATION 4-8
3.0 PRESENT TEST RESULTS 4-11
4.0 CONCLUSIONS 4-14
APPENDICES:
A. GASEOUS EMISSIONS MEASUREMENTS TAKEN DURING
SASS TESTS AT REFINERY PROCESS HEATER 4-15
KVB11-47800-1284
4-5
-------
SECTION 1.0
DESCRIPTION OF TESTS
KVB participated as a subcontractor to Acurex Corporation in the NOX
Emissions Assessment program (Contract No. RB59313A) at a refinery process
heater from June 15, 1981 through June 19, 1981. During the test period KVB
was responsible for continuously measuring NOx, CO, CO2, 02, and S02 gaseous
emissions. The emissions were measured on a natural draft refinery process
heater firing a mixture of approximately one-third No. 6 oil (by heat input)
and two-thirds refinery gas. The heater was equipped with staged air
lances. One baseline test was conducted without staged combustion air and a
second low-NO__ test was run with maximum staging at about the same or a
X
slightly lower level of excess oxygen. Concurrent SASS, EPA Method 5, and wet
chemical SOX tests were run by Acurex Corporation.
Originally, plans had been made to operate the heater with a 50/50
mixture of gas and oil, however, the plant was unable to flare enough fuel gas
to allow that much fuel oil to be burned. This situation occurs frequently
during the summer when process offgases are more abundant. In addition, two
oil guns were plugged during the tests. Due to scheduling problems with the
plant maintenance department, the-guns could not be cleaned in time to allow
both SASS tests to be completed in the allotted time. It was nevertheless
felt that the tests should be conducted and that appropriate allowances for
the effect of oil/gas ratio on emissions could be made.
It is also important to note that the excess O- level (~4 percent)
maintained in the low-No,, test was considered to be the lowest continuous
A ^••••"•••••MMM^paii...*™^^™
operating level by the plant, although previous tests by KVB had shown the
system to be capable of operating over a short-term at 2 percent O2« Problems
in maintaining adequate combustion air flow had occurred during a 30-day test
conducted on the same heater previously firing 100 percent refinery gas when
2 percent 02 was the target operating condition. After an incident in which
the unit nearly went down because of air starvation, the plant decided to
KVB11-47800-1284
4-6
-------
maintain 4 percent 0, as the minimum operating level and this decision was
carried over to the present tests with the oil/gas fuel combination. Thus,
the NO^ reduction in the present low-^NOx test was due primarily to the staged
air system. Lowered excess air was essentially not a factor in the NO reduc-
X
tion as it had been in some past tests.
KVB11-47800-1284
4-7
-------
SECTION 2.0
GASEOUS EMISSIONS TEST METHODS AND INSTRUMENTATION
All emission measurement instrumentation was carried in an 8 x 42 ft
mobile laboratory trailer. The gaseous species measurements were made with
analyzers located in the trailer.
The emission measurement instrumentation used was the following:
TABLE 1. EMISSION MEASUREMENT INSTRUMENTATION
Species
Carbon Monoxide
Oxygen
Carbon Dioxide
Nitrogen Oxides
Sulfur Dioxide
Manufacturer
Sectarian Instruments
Teledyne
Beckman Instruments
Thermo Electron Co.
DuPont Instruments
Measurement Method
IR Spectrometer
Polar ographic
IR Spectrometer
Chemi luminescent
UV Spectrometer
Model
No
865
326A
864
10A
400
2.1
GAS SAMPLING AND CONDITIONING SYSTEM
A flow schematic of the flue gas sampling and analyzing system is
shown in Figure 1. The sampling system uses one of three double-headed
positive-displacement diaphragm pumps to continuously draw flue gas from the
stack into the laboratory. The sample pumps pull from up to six unheated
sample lines. Selector valves allow composites of up to six points to be
sampled at one time. The probes are connected to the sample pumps with 0.95
cm (3/8") or 0.64 cm (1/4") nylon line. The positive displacement diaphragm
sample pumps provide unheated sample gas to the refrigerated condenser (to
reduce the dew point to 35°F), a rotameter with flow control valve, and to the
02» NO, CO, and CO2 instrumentation. Flow to the individual analyzers is
measured and controlled with rotameters and flow control valves. Excess
sample is vented to the atmosphere.
KVB11-47800-1284
4-8
-------
o
Hot
Preaaure
MOnoi
o
Mot
Vacuum
Hot
Pump
lero
£ j filter
I? Micron*)
MC
00,
-e*. vent
HO_
Q
Heated Lin*
manifold
Vacuu*
Pump
Hot
Sample Dry Sample Llnee
Line (Typical Set-Up Bin Lines)i
M
Plltera («|
IT »lcron«)
Sample
Pumpa
Condense*
»«
Hot/Cold
•Switch
Refrigeration Condenaer
anple Preaaure
00
o
o
to
00
Figure 1. Flue gas sampling and analyzing system.
-------
To obtain a representative sample for the analysis of NO2/ SO2 and
hydrocarbons, the sample must be kept above its dew point, since heavy hydro-
carbons may be condensible, and S02 and NO2 are quite soluble in water. For
this reason, a separate electrically heated sample line is used to bring the
sample into the laboratory for analysis, -me sample line is 0.95 cm
(3/8-inch) Teflon line, electrically traced and thermally insulated to main-
tain a sample temperature of up to 400«F. A heated diaphragm pump provides
hot sample gas to the hydrocarbon, S02 and NOX analyzers and cold, dried gas
to the other continuous analyzers via the condenser described above.
The laboratory trailer is equipped with the analytical instruments
shown in Table 1 to continuously measure concentrations of NO, N02, CO, CO2/
°2' SO2' and hydrocarbons. All of the continuous monitoring instruments and
sample handling system are mounted in the self-contained mobile laboratory.
The instruments themselves are shock mounted on a metal console panel. The
sample flow control measurement, and selection, together with instrument
calibration are all performed from the console face. Three-pen recorders
provide a continuous permanent record of the data taken. The sample gas is
delivered to the analyzers at the proper condition and flow rate through the
sampling and conditioning system described previously. A Monitor Laboratories
Model 9300 Data Logger is normally used to record and average data from the
analyzers and can be coupled with a Techtran Model 815 Datacassette recorder
to provide digital storage of the data.
KVB11-47800-1284
4-10
-------
SECTION 3.0
PRESENT TEST RESULTS
The test unit was first run at a baseline operating condition at a
process rate of 77.11 n^/h (11,640 bbl/d) of crude throughput. A sketch of
the unit is shown in Figure 2. The secondary air registers were approximately
40 percent open and the excess oxygen at the stack was maintained at approx-
imately four percent. For this baseline test the ratio of oil/ gas by heat
input was 37/€3.
The gaseous emission measurements were taken by means of a single
probe and heated sample line from the stack approximately five feet above the
outlet of the transition section for both the baseline and the low-NOx test
which followed. Dry measurements of CO, C02/ NO, and 02 were made while a wet
measurement was taken for
The low-NO configuration on this process heater was achieved by means
of staged air lances inserted through the heater floor. Roughly one-third of
the total combustion air was introduced through the lances. This was the
maximum staging capability of the system. An excess oxygen level of approx-
imately 3-4 percent was maintained and the secondary air registers were
adjusted to ten percent open as in previous tests conducted by KVB. The
process rate was again 77.11 m /hr of crude oil, but the oil/gas ratio changed
slightly to 31/69.
(All numbers given for the operating parameters are approximate daily
averages . )
The table below summarizes the emissions measured and the standard
deviation in the emission measurements along with the range of values and
number of measurements taken for both the baseline and the low-NOx tests. S02
measurements are reported as wet values at measured excess C>2. The values for
NO emissions are reported as dry at measured excess 02 • The average NO
emissions were corrected to 3 percent O2 using that average O2 concentration
KVB11-47800-1284
4-11
-------
NATURAL DRAFT REFINERY PROCESS HEATER
,1
*,*
l
•
CD
D
U
STACK
4'-6" O.D. (1.4D
CONVECTION SECT IC.:
NOT TO SCALE
RADIANT SECTION
16'-9i" O.D. (S.lir.)
15'-9i" I.D. (4.8rO
•AIR PLENUM AND SOUND
SUPPRESSION BOX
Figure 2. Sketch of the process heater tested.
4-12
KVBll-47800-1284
-------
both tests. The gaseous emission measurements were 15 minute averages as
determined by manually interpreting the strip chart recordings for each ana-
lyzer. This procedure was made necessary by the failure of the electronic
data logger just prior to the start of the tests.
TABLE 2. SUMMARY OF GASEOUS EMISSIONS DATA FROM
REFINERY PROCESS HEATER SASS TESTS
Baseline Test Low NO Test
J* . .. ..
Species
02 (%, dry)
C02 (%, dry)
CO (ppm, dry)
S02 (ppm, wet)
NO (ppm, dry)
NO (ppii, dry
at 3% 02)
Cmin/
c s cmax n c
4.0 0.20 3.3/4.3 37 3.3
12.1 0.87 10.5/13.6 33 11.7
3.8 2.9 0/10 38 7.3
151 11.6 120/170 21 148
162 6.0 152/174 37 116
172 — 156/186 — 118
* &
0.27 3.1/4.2
0.32 11.3/12.4
3.4 0/10
11.4 125/170
3.8 108/125
109/134
n
20
17
20
20
20
H
1 72 •• 118
172
The complete set of gaseous emission measurements is given in the
Appendix. No significant NO2 was measured during either test.
4-13
KVB11-47800-1284
-------
SECTION 4.0
CONCLUSIONS
The data show that an average NO emission reduction of 31.4 percent
from the baseline emission of 172 ppm, dry at three percent 02/ was obtained
in the low-NOx configuration. The CO emissions remained very low in both
tests. The high standard deviations reflect the fact that the CO levels were
at the lower limits of detectability of the CO analyzer being used. SO2
emissions were approximately the same in both baseline and low-NOx configura-
tions.
The percent reduction in NO emissions due to the staged air system was
approximately the same as the reduction observed in previous tests when firing
a 50/50 mixture of oil and gas fuels under roughly the same operating condi-
tions. In those previous tests the heater process rate was 78.3 m /h (11,800
bbl/d) and the overall excess 02 was about 4 percent. In those tests, how-
ever, the baseline NO emission was 207 ppm, dry at three percent 02.
The difference in baseline NO emissions between the present tests and
the past tests is due to the difference in oil/gas ratio. From previous
tests, it is known that the thermal NOX alone at baseline conditions is about
125 ppm, dry at 3 percent oxygen. The baseline level of 172 ppm in the pre-
sent tests for a 37/63 oil/gas mixture represents a 47 ppm increment above
this emission level. One may predict an emission level for the 50/50 oil/gas
mixture as follows (assuming a constant fuel nitrogen conversion efficiency):
50
(rz- x 47) + 125 = 189 ppm
This value is within 10 percent of the observed value of 207 ppm.
KVB11-47800-1284
4-14
-------
APPENDIX A
GASEOUS EMISSIONS MEASUREMENTS TAKEN
DURING SASS TESTS AT REFINERY PROCESS HEATER
KVB11-47800-1284
4-15
-------
TEST z-
hi
Date
Tijr.e
0615
0630
0645
0700
0715
0730
0745
0800
0815
0830
0845
0900
0915
0930
0945
1000
101 S
1030
104S
n nn
in.
TMO
n«
,,nn
NO
ppm
- STA/^T
11*2.
°2
Percent
OP S*
H.-l
Percent
rs 7£-s r
CO
ppm
/2-;0£
/o
Load
x 1000
; —
y J1
Co^rent
Gtdes
"•
Page 2
4-16
A Research-Cottrell Company
KVB 6317
9/80
-------
T£sr r -
Date
Time
NO
PP">
Percent
Percent
CO
ppm
Load
X 1000
Coirenent
CpQes
1215
/w
1230
1245
/S*
1300
1315
133
H, 3
1345
14OO
H.I
1415
t/.Z
/S.3
5
141D
/S.3
1445
/7V
H. 2
/3,3
1500
/z.S
JT
1515
1530
l&z
] it-al
1 545
Ifil 5
5,7
/A?
i-mn
.3,9
1-MC
IS?
3
C+L
1730
3.9
1745
//. 3
/eo
1800
/70
H.2
(Q
4-17
A Researth-Cottrefl Company
Page 3
KVB 6017
9/80
-------
Date
Time
181!
NO
-EEL
°2
Percent
"2
Percent
CO
ppm
Load
'x 1000
Cotnment
Codes
/SO
1830
153
33
It
O
184!
-3,?
ti.O
o
1900
•191!
72.0
V930..
-//.?
• i Jfh_''
'1945
2000
2015
/A?
2030
3.8
2045
75^
//.o
2100
2115
/55
O
2130
"2145"
4-18
Page 4
A Research-Cottrefl Company
JCVB 6017
9/80
-------
l! HIS
Date
Tins
0615
0630
0645
0700
0715
0730
0745
0800
0815
0830
0845
0900
0915
0930
0945
1000
1015
1030
!0d«;
1 100
1 1 1 C
1 1 -.~
"«
i ^.^r1.
NO
trcm
5-4SS '
f25
no
/It
I/H
n?
us
°2
Percent
re^r *J
q,Z
3.1
s.s
3-L)
3,LI
3-H'
CO,
Percent
ZP S7^/^7
X-. / , /
x*- r.L
L^Cl (s f C
h.3
If .3
II.}
IM-
(l.>
ft. T-
CO
*5ptn
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fC*&"~'£-
O
0
5
5
;0
(0
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x 1000
TOO
\
~-J :i
v.c.-^rent
-/ies
/
|
-
l"5
145
HS
.If5
HO
ll«
sJote^f CAT
Page 2
o?-
*t™" iy
A Research-Cottrell Company
KVB 6317
9/80
-------
f (Z
A Rewarch-Cottrell Company
1C7B 6017
9/80
-------
4.2 OPERATING DATA FOR EPA METHOD 5
4-21
-------
TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
TOSC.O
l&l
PLANT _
DATE _
SAMPLING LOCATION
INSIDE OF FAR WALL TO
OUTSIDE OF NIPPLE, (DISTANCE A) _
INSIDE OF NEAR WALL TO
OUTSIDE OF NIPPLE, (DISTANCE B) _
STACK I.D., (DISTANCE A - DISTANCE B)
NEAREST UPSTREAM DISTURBANCE
NEAREST DOWNSTREAM DISTURBANCE.
CALCULATOR.
58.
tog
•siacfe
•fro**.
SCHEMATIC OF SAMPLING LOCATION
TRAVERSE
POINT
NUMBER
FRACTION
OF STACK I.D.
STACK I.D.
PRODUCT OF
COLUMNS 2 AND 3
(TO NEAREST 1/8 INCH)
DISTANCE B
TRAVERSE POINT LOCATION
FROM OUTSIDE OF NIPPLE
(SUM OF COLUMNS 4 & 5)
&t>9
/Z
O. 67 f
_&J
3.3V
3".
7.ys"
7?
/Z.
0./R&
9.2.X
/Z
2/.2.J
O.23&
/Z
0.
/Z.
O 3
0.6/&
30. 28
O.
3¥. So
33.7V
/Z
/J
37.
0, fi/2
37.7^
#9
S/.7/
6.&H
£2*
6,1*5
5"7.33
n
/a
*-96*
EPA (Our) 232
4/72
4-22
-------
PRELIMINARY VELOCITY TRAVERSE
PLANT
DATE
LOCATION
STACK I.D..
BAROMETRIC PRESSURE, in. tig 29.V2
STACK GAUGE PRESSURE, in. H;Q - Q.3/
OPERATORS..
SCHEMATIC OF TRAVERSE POINT LAYOUT
TRAVERSE
POINT
NUMBER
A-/
3.
3
*
f
(.
7
&
f
/O
//
/2.
/3
/¥
/£
/&.
/7
/R
a\£ I
— - r
AVERAGE
VELOCITY
HEAD
(Aps), in.H20
O./O
o./o
o./o
O'/O
6./Q
6.O3
O.O
V
/
(.
7
s
9
/o
//
/ft
/.«
/
O.O&
O.OQ
<0.08
O.o7
0 .<^4
O.Ob
•>
-/C" " fe'
• oil
STACK
TEMPERATURE
rrs), °F
t>9^
t.42
&9V
lo/
700
•70 /
•7fiA
7ofi
7ofl
7/3fl
•5o9
70 L
EPA (Dur) 233
4/72
4-23
-------
DRY MOLECULAR WEIGHT DETERMINATION
PLANT
DATE
TOSCO
COMMENTS:
SAMPLING TIME (24* CLOCK) fi:o7 ant
SAMPLING LOCATION_
SAMPLE TYPE (BAG, INTEGRATED, CONTINUOUS GRAB) Fpi+C,
ANALYTICAL METHOD. _
AMBIENT TEMPERATURE.
OPERATOR
7S V
^\^ RUN
GAS ^^^\
C02
02(NET IS ACTUAL 02
READING MINUS ACTUAL
C02 READING)
CO(NET IS ACTUAL CO
READING MINUS ACTUAL
0? READING)
N2(NET IS 100 MINUS
ACTUAL CO READING)
I
ACTUAL .
READING
NET
/A
t*
2
ACTUAL
READING
NET
/Si
V*
3
ACTUAL
READING
NET
X/.5-
s.o
AVERAGE
NET
VOLUME
//U3
***
0
83.V
MULTIPLIER
M/100
3Z/100
n/ioo
^/lOO
TOTAL
MOLECULAR WEIGHT OF
STACK GAS (DRY BASIS)
Md, Ib/lb mole
r.^i
/.^f
X
^3.3^
20.0V
^
to
EPA (Dur) 230
4,72
-------
Plant_
Date
TASCO
ISOKINECTIC SAMPLING WORKSHEET
Reformed by_
Sample Location Slack.
Test No./Type Mf
K - 782.687 (Cp)2 (1-BWO)2 Ps Md
Ms Pm
where: K = Contant of fixed and assumed parameters (dimensionless)
Pitot coefficient (dimensionless)
Water vapor in the gas stream
(proportion by volume)
Absolute stack gas pressure (in. Hg)
Molecular weight, stack gas dry
(Ib/lb-mole)
Orifice coefficient (dimensionless)
Molecular weight, stack gas wet
(Ib/lb-mole) Md(l-Bwo) + 18(BWQ)
Abo lute meter pressure (in. Hg),
782.687 (.a*)2 (l-_^2j2 (a* 39) (3o.e?)
(.6t9t)Z torn-) (gf.iO
CP
BWO
PS
Md
KO
" MS
Pm
K
O.M*
0./2,
J9-3?
30.07
O.M9?
3S.GZ.
J?.*Z
/000.&S"
4-25
-------
Plant_
Date
TOSCO
ISOKINECTIC NOZZLE CALCULATION
AND
SAMPLING RATE CALCULATION
Performed by
Sample Location_
Test No./Type
AH T
where: N^ = Nozzel diameter (inches)
Average pressure differential across the
orifice meter (in. 1^0)
Temperature stack gas, average (°F)
Temperature of gas meter, average (°F)
Stack gas velocity pressure (in 1^0)
/ (/-a) (760 + 460) \-25
\(/m*Jf ('** + 460) (.OS)/
AH
' ' Ts
Tm
AP
Nd
/.^
700
/05"
0.06
0 . #/6Q
AH
(AP)
where: AH = Pressure differential across the orifice meter (in
Nozzel diameter, actual (inches)
Temperature of gas meter (°F)
Temperature of stack gas (°F)
Stack gas velocity pressure (in H20)
( ( ) ( )4 ! + 460I ( }\
\ ( — * 46°5 ~ /
Maqic number /
-------
FIELD DATA
Page I of 2>
p ! ant
Date
Sample Location £g
Sample Type /V)-C"
Run Number /
n O | M*T~
-------
Page 2 of .
Clock Time
Traverse
Point
Number
Gas Meter
Reading
Velocity
Head
(APS).
In. H20
Orifice Pressure
Differential
(AH), In. H20
Desired
Actual
Temperature °F
Stack
Probe
Imp1 nger
Organic
Module
Oven
Gas Meter
In
Out
Pump
Vacuum
In. Hg
Avg.
J?£l
/'*.
. BtfO
7/7-P7S'
Q.9/
ft*
HJL
.300
Ji.
7/9. X
o
ni
in
300
o.Ol
0.1/
739
88
t'Q
/to
300
4L
o.o*
041
555.
HO
(to
.Joo
•??7.fliP
&L
300
to
00
A,
>^f
HI
•300
71*
37£
. 2AO
o./t
'41
8$
•JTf
3/0
VI
£.
73*
fj
ML
UL
.7,5-0« f/O
A./3
i^
0./1
1
75-7. SAO
0./3
750
"3
340
Run No.
Date
Sampling Location
Coiments:
-------
Page 3 of 3
Traverse
Point
Number
Clock Time
(24-hr)
Clock
Sampling
Time, min
Gas Meter
Reading
(VM), ft 3
Inlt.
Velocity
Head
(APS),
In. H20
Orifice Pressure
Differential
(AH), In. H20
Desired
Actual
Temperature °F
Stack
Probe
Implnger
Organic
Module
Oven
Gas Meter
In
Out
Pump
Vacuum
In. Hg
Avg.
Az&-
A3/
tff
360
Q^1l
&L
J&
4*0
Q.tO
£±.
3/
76S
Q./O
/.oo
?J*
^£.
//o
J&.
e
-------
ACUREX
Corporation
NOZZLE MEASUREMENT
B
DIAMETER
DIMENSION
A
R
C
NOZZLE SERIAL
DATE
RECORDED BY
4-30
-------
FJELD DATA
Page
/ of 3
Plant
Date
TO SCO
Sample Location
Sample Type /•? £
Run Number 2,
Operator
Impinger Volumes
Initial Final
'0O
Net Gain
Probe Length and Type_
Nozzel Size & I.D.
Ambient Temperature "7f /QO *F
Barometric Pressure £4
Static Pressure, (H20) —_
Filter Number(s)___7/_-1v'
Pitot Coefficient & I.D. J
Assumed Moisture O.I357
Molecular Weight, Dry, (Md)
Silica Gel
Meter Box Number^
Meter Coefficient
<* Factor
K =
I.OI
. 9/
K(Nd)
Leak Check: Initial at /*/ " Hg, .003 CFM
Final at " Hg, CFM
Pitot Leak Check:
K(Nd)
p)
SASS Condensate
Total Volume
I
CO
Traverse
Point
Number
Clock Time
(34-hr)
Clock
Gas Meter
Reading
Velocity
Head
(4P,),
in. H20
Orifice Pressure
Differential
UH). in. H20
Desired
Actual
Temperature °F
Stack
Probe
Impinger
Organic
Module
Oven
Gas Meter
In
Out
Pump
Vacuum
in. Hg
Avg.
A^L
/.37
&L
1&3L
.37*
. -700
0./3
730
jsa.
&L
j3L
.340
7^.735"
0./2
/.it,
?*/
Ra,
102.
Zfi£
.360
o./*
7*1
/.n
-------
Page 2 of 3
Traverse
Point
Number
Clock Time
(24-hr)
Clock
Sampling
Time, rain
Gas Meter
Reading
Init.
Velocity
Head
(APS).
in. H20
Orifice Pressure
Differential
(AH), in. HgO
Desired
Actual
Temperature °F
Stack
Probe
Implnger
Organic
Module
Oven
Gas Meter
In
Out
Pump
Vacuum
in. Hg
Avg.
A-to
o.flfe
££L
f2Q-
_&
0.Q9
_&fiL
362
ML
300
-1&.
j * f *P *
Ol
&7Q
o.oe
7.26
fiS
flae. Me?
HA
.lao
O.Q^
i
CO
to
tb
.ass
e,o<\
a±
m.
.J.o
n.
0.01
in
Q.ol
^241
U'.ao
0.1*8.
1,11
i.ao
13
Ml
g^s.ggo
1. 3D
77
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o./i
I- 01
111
r
D.ll
. 10
73^
lift
O.IO
l.flO
lie
lift
A.
o.io
IIS
No.
Date
Sampling Location
Comments:
A -18 for °\
T 5
-------
Page .3 of 3
Traverse
Point
Number
Clock Time
(24-hr)
Clock
Sampling
Time, mln
Gas Meter
Reading
<»•). "
Init.
Veloclty
Head
(&PS).
1n. H20
Orifice Pressure
Differential
(AH), in. H20
Desired
Actual
Temperature °F
Stack
Probe
Impinger
Organic
Module
Oven
Gas Heter
In
Out
Pump
Vacuum
in. Hg
Avg.
o.ofl
JL21
£2L
113-
iii
o.o ft
Q.ftO
J&.
292
M.
Q.oB
JL&Q.
111
If
8 n> */o
1*L
o.fio
_j2a_
J2&
P.gQ
J^£
« f
JL
J&&.
0-80
Jlk
IL
88a.
o.o 7
O.QO
b. 04
0.79
241
115"
iH
n
_$i_
nu
»•'• I
Run No.
Date •- -I'V--^/
I'^.i
Sampling Location
Conments:
-------
4.3 OPERATING DATA FOR CONTROLLED CONDENSATION TRAIN
4-34
-------
6> -
CONTROLLED CONDENSATION SYSTEM (CCS)
FIELD CHECKPOINT SHEET
Checkpoint
Initials
Supervisor
QA
Inspector
Remarks
LABORATORY PREPARATION
• Inspect and clean CCC. Both filter holder and CCC
are cleaned with hot chromic acid solution and
O.I. H20.
0 Rinse with acetone and air dry CCC.
• Place Tissuequartz filter in filter housing.
• Check seal between end of joint and filter.
• Do not use grease on joints.
• Inspect and clean all glass joints.
SITE SETUP
• Rinse the inside of probe prior to run.
• Rinse probe with acetone until rinse solution is
clear.
• Perform leak test.
• Leak rate must be less than 80 ml/min (0.003 cfm).
• Thermocouple leads attched to probe and filter.
• CCC water bath held at 60°C (140°F) +1°C.
• Leak test train.
0 Probe temperature maintained at 316°C (600°F)
t Gas temperature out of filter holder held at
228°C (550°F).
• Fresh solutions placed in impingers.
• Fresh absorbent replaced in final impinger.
• Adjust flowrate in system to 8 1pm.
oo
4-35
-------
CONTROLLED CONDENSATION SYSTEM (CCS)
FIELD CHECKPOINT SHEET — Continued
Checkpoint
SAMPLING RUN
t Turn vacuum pump on just before Inserting probe
In stack.
• Check seal between probe and port to prevent any
outside air from entering stack.
• Run test for 1 hour or until coils are frosted to
1/2 or 2/3 their length.
• After run, cap both ends of probe and lay in
horizontal position.
• Rinse the CCC coils into the modified Erlenmeyer
flask with a maximum of 40 ml D.I. H20.
• Was any of the solution lost ( v ml estimated)?
• After probe has cooled, it is rinsed with a maximum of
40 ml D.I. HgO into a 25-ml Erlenmeyer flask.
- Was any solution lost ( ^"ml estimated)?
- Clean support equipment priot to next run.
- Save filter for titration.
Initials
Supervisor
-
QA
Inspector
C-^
^
^
^
^"
\^
^
^
\^
Remarks
Comments:
4-36
-------
CONTROLLED CONDENSATION SYSTEM (CCS)
FIELD DATA SHEET
Plant
Date
^o
P'.g
Sample Location
Run No. / / c.c<
Operator
I-HC-ATT?P
Ambient Temperature
Barometric Pressure
Meter Box Number a
/Q*f
,c .
Meter Orifice Coefficient
Meter a Factor / °i °? Sr
Clock Time
(24-hr)
clock
Sam-
pling
Time, ?$
min
Gas
Meter
Reading
Init.
Temperature (°F)
Stack
Probe
Filter
Skin
Out
Recirc
Water
Exit
Coil
Dry Gas
Meter
In
Out
to
'SI
US'
ttf
C-o
Average
7/V-.7
6 o
i.r
,.3
4-37
-------
CONTROLLED CONDENSATION SYSTEM (CCS)
FIELD CHECKPOINT SHEET
Checkpoint
LABORATORY PREPARATION
• Inspect and clean CCC. Both filter holder and CCC
are cleaned with hot chromic acid solution and
O.I. HgO.
• Rinse with acetone and air dry CCC.
• Place Tissuequartz filter 1n filter housing.
• Check seal between end of joint and filter.
• Do not use grease on joints.
• Inspect and clean all glass joints.
SITE SETUP
t Rinse the inside of probe prior to run.
• Rinse probe with acetone until rinse solution is
clear.
• Perform leak test.
• Leak rate must be less than 80 ml/min (0.003 cfm).
• Thermocouple leads attched to probe and filter.
• CCC water bath held at 6Q°C (140°F) il°C.
• Leak test train.
• Probe temperature maintained at 316°C (600°F)
• Gas temperature out of filter holder held at
228°C (550°F).
t Fresh solutions placed in impingers.
• Fresh absorbent replaced in final impinger.
• Adjust flowrate in system to 8 1pm.
Initials
upervisor
QA
Inspector
Remarks
4-38
-------
CC-5
CONTROLLED CONDENSATION SYSTEM (CCS)
FIELD CHECKPOINT SHEET -- Continued
Checkpoint
SAMPLING RUN
t Turn vacuum pump on just before Inserting probe
In stack.
• Check seal between probe and port to prevent any
outside air from entering stack.
t Run test for 1 hour or until colls are frosted to
1/2 or 2/3 their length.
• After run, cap both ends of probe and lay in
horizontal position.
• Rinse the CCC coils into the modified Erlenmeyer
flask with a maximum of 40 ml O.I. HjO.
• Was any of the solution lost (/^ml estimated)?
t After probe has cooled, it is rinsed with a maximum of
40 ml D.I. HgO Into a 25-ml Erlenmeyer flask.
- Was any solution lost (tfs ml estimated)?
- Clean support equipment priot to next run.
- Save filter for titration.
Initials
Supervisor
QA
Inspector
u-
^
>^
^
^
^^
^
^
^
Remarks
— """
"""
Comments:
4-39
-------
CONTROLLED CONDENSATION SYSTEM (CCS)
FIELD DATA SHEET
P1 ant "^ >
Date k-i
Operator _
.c.
Ambient Temperature
Barometric Pressure
Meter Box Number
-J X
-------
4.4 OPERATING DATA FOR SASS
4-41
-------
Plant -r/»cr-r>
Date &-&-%.
ISOKINECTIC SAMPLING WORKSHEET
Reformed by ZL.
Sample Location o.£.oc>ff_
Test No. /Type
K - 782.687 (Cp)2 (1-BWO)2 Ps Md
Ko2 Ms Pm
where: K = Contant of fixed and assumed parameters (dimensionless)
Pitot coefficient (dimensionless)
Water vapor in the gas stream
(proportion by volume)
Absolute stack gas pressure (in. Hg)
S TA-TIC - -0.3 f
Molecular weight, stack gas dry
(Ib/lb-mole)
Orifice coefficient (dimensionless)
Molecular weight, stack gas wet
(Ib/lb-mole) Md(l-BwQ) + 18{BWQ)
Abolute meter pressure (in. Hg.) .
782.687 (0-^4)2 (1-^/^)2 (f?.3ff(lo.aT
( 3^2 (£Li4 (^D
CP
Bwo
PS
Md
KO
Ms
Pm
K
0,&
U%_
£jLfr*—~-— <
39. 3^7
^^-07
/^5sy(^c"X>
3,7^0)
^a-62
Xt^S u -^t
-------
FIELD DATA
Page J_ of _2
I
4*.
CO
Plant TeK.e.f>>
Date /..-/fl-
Sample Locat Ion Qfoj>£
Sample Type
Run Number /
Operator
Implnger Volumes
Initial Final Net Gain
JQto
Probe Length and Type_
Noziel Size ( 1.0.
Pitot Coefficient t t.O.
Assumed Moisture
/, ,
,7:
Ambient Temperature
Barometric Pressure
? f
Molecular Height. Dry. (Hd)
Meter Bo» Number SJ X
Static Pressure. (H;0)
Filter Humberts)
" Q, 3
Silica Gel
Meter Coefficient^
<* Factor
K
3.
/,
Leak Check: Initial afgj " Hg»OZ/_ CFM
Final at • Hg. CFM
Pitot leak Check: "
SASS Condensate
Total Volume
Traverse
Point
Number
Wr
C'ock Time
<2<-lw
clock
Gas Meter
Reading
>, ft
.050
•8/2,4
Velocity
Head
<«P«).
In. R20
Orifice Pressure
Differential
UH), In. H?0
Desired Actual
$7.3
9-, A
A
2.4
Temperature °F
2J
Stack
732
-73$
Probe
•731
7(9
2*5
733] 7e^
Implnger
12
92
13
Organic
Module
Oven
Gas Meter
In
96
7?
(OS.
ICP
/OS
tos
Out
9S
9?
/*>
/Oo
\o<. {ol
Pump
Vacuum
in. Hg
/£"
/S"
A»g.
760Z/5/,Bl/Bev
Cooments:
i4tt Profit.
*<> 1>C
-------
Page ft_ of
Traverse
Point
Number
Clock Time
(24-hr)
Clock
Sampling
Time, rain
Gas Meter
Reading
10-}
/ 7
ta
1,2.
/"I
1 -sot.-?
3.2
7-r-a
&£/o4
'00
PtVi
/s
/Obi-
102
Run Ho. / — CMC?
Date
Sampling Location C/c.ff>f
P t
Comnents:
-------
NOZZLE MEASUREMENT
B
DIAMETER
DIMENSION
A f.l/^
B
C
D
E
F /Z3>
NOZZLE SERIAL
4-45
DATE
RECORDED BY
Form AC-268 8/78
-------
Plant )OSC(?
Date
ISOKINECTIC SAMPLING WORKSHEET
Peformed by_
Sample Location
Test No./Type
K = 782.687 (Cp)2 (1-BWO)2 Ps Md
Ko2 Ms Pm
where: K = Contant of fixed and assumed parameters (dimensionless)
Pitot coefficient (dimensionless)
Water vapor in the gas stream
(proportion by volume)
Absolute stack gas pressure (in. Hg)
#3.40- o^y,-$.(*
Molecular weight, stack gas dry
(Ib/lb-mole)
Orifice coefficient (dimensionless)
Molecular weight, stack gas wet
(Ib/lb-mole) Md(l-Bwo) + 18(BWQ)
3/. ,91 '4 ^?.4-3
Abolute meter pressure (in. Hg)-
^q.4o* *°A*.(.
^,70S(a ,-74SZ
782.687 (,Q^4)2 (1-aisd2 (g
fe.-7fr>')2 (<;-j<> (£A&
/4-13^
CP
BWO
. PS
Md
KO
"MS
Pm
K
0>%4
01
/3-s A
/4^SOWte|>
5?. 377
30- 0"?
Q^*-~~*«JC'
*5.7to/
^S.44
Ou*~~+£i
W. S€
•3^-724
4-46
-------
FIELD DATA
Page /_ of
f 1 antTOSC.0,
Date £, -ft -{ft
,CA
Sample Loption Cg
Sample Type
Run Number
Operator 7*.
Imptnger Volumes
Initial Final
era
Het Gain
5V g
Probe Length and Type <
Nozzel Size i 1.0.
Pilot Coefficient I 1.0.
Assumed Moisture
Ambient Temperature_
Barometric Pressure g*i,SO
Static Pressure, (HgO) - Q.
Molecular Height, Dry, (Md)_
Meter Box Number_
Meter Coefficient
i Factor
K •
30. OT
. T fcp JL Ac 0\
"" '
0//2.
Filter Humberts) /v\vi-a II -fetrt
Leak Check: Initial at
Final at
Leak Check:
Hg,
Hg.
r377S"
Traverse
Point
Number
48
Gas Meter
Reading
704-7
#31.02
- si
. ST5"
Velocity
Head
<*'*>•
In. fl20
Orifice Pressure
Differential
UH). in. H;0
OesIred Actual
Temperature °F
Stack
Probe
Imptnger
Organ ic
Module
Oven
Gas Meter
In Out
12
111
&L
in
/OS
M4
JtZ
\IZ
t'i
/»*>
Pump
Vacuum
In. Hg
/a
1C,
n
Avg.
vSP"
3-7.?* ~ ,
'O/J
SfaMJS IN I^/WP,
7602/5/,81/Rev
S"'*••*>
-------
Page J_ of
00
Traverse
Point
Number
Clock Time
(24-hr)
Clock
Sampling
Time, mln
Gas Meter
Reading
Intt.
(46,6. .SO
IS30-*Q
Velocity
Head
(APS).
In. H20
Orifice Pressure
Differential
(AH). In. HjO
Desired
22.
2-2
^•^.
2.*-
Actual
26
Temperature °F
Stack
Probe
^73
67s
Implnger
Organic
Nodule
(,0
foo
2.14
Oven
Gas Meter
In
/4
fit
Iti
III
IOL f
ul
t'i
Out
at,
(a*
Pump
Vacuum
in. Hg
n
/7
n
Avg.
Hun Ho.
Date
Sampling Location *r*jg..n^
Comments:
z/
•z/*
-------
SECTION 5
ANALYTICAL RESULTS
5.1 Ultimate Analysis of Fuel Oil
5.2 Composition of Refinery Gas
5.3 SASS Particulate Emissions
5.4 EPA Method 5 Particulate Emissions
5.5 Sulfur Oxides Emissions by Turbidometric Analysis
5.6 Trace Element Analyses
5.7 Total Chromatographable Organics (TCO), Gravimetric Organics
(GRAV), Infrared (IR) Spectra, Gas Chromatography/Mass Spectrometry
(GC/MS) and Low Resolution Mass Spectrometry (LRMS) of Total Sample
Extracts
5.8 CI-CG Chromatograms
5.9 Radiometric Analytical Results
5.10 Bioassays
5-1
-------
5.1 ULTIMATE ANALYSIS OF FUEL OIL
5-2
-------
Prelim. No. 7520
Lab. No. 81ml35
--„/ 1- U-- re si*** & A
/V; ''- ? 7P 3 DRTGINAL
November 16,1981
Page 2 of 2
en
O3
#1, Code 813781
1st 2nd 3rd
Test Test Test
(C) ,% .- 87.37 —
Hydrogen (H),% 10.47 —
Oxygen (O),
by difference,% 0.31 —
Nitrogen (N),% .71 .88
Sulfur (S),% — .92. .94
Heating Value:
BUT per Pound 18,720 —
Gravity, API
70°F 12.3
60°F 11.8
»2, Code 813782
1st 2nd 3rd
Test Test Test
86.66 —
10.98 —
0.55 —
,90~ .74 .90
,96 .93 .90
18,760 —
12.3
11.8
.92
.88
-------
5.2 COMPOSITION OF REFINERY GAS
5-4
-------
TOSCO CORPORATION
BAKERSRELD REFINERY
GAS ANALYSIS REPORT
LABORATORY:
OPERATOR:
DATE
UNIT.
urud
•To J/ H
SAMPLE DATE
SAMPLE TIME
PERCENT
HYDROGEN
NITROGEN
OXYGEN
CARBON MONOXIDE
AtL
CARBON DIOXIDE
HYDROGEN SULFIDE
METHANE
ETHANE
ETHYLENE
PROPANE
PROPYLENE
.£3-
ISOBUTANE
I/,}
NORMAL BUTANE
1,7
TOTAL BUTENES
1 , 3-BUTADIENE
ISOPENTANE
NORMAL PENTANE
TOTAL PENTENES
TOTAL Ce PLUS
Speof/'e.
&.
jj-*'
REMARKS:
8108919-801
5-5
-------
TOSCO CORPORATION
BAKERSFIELD REFINERY
GAS ANALYSIS REPORT
LABORATORY
.
Lao
OPERATOR:
ATOR
DATE.
UNIT:
CruJ
"70 '
SAMPLE DATE
*//*/*/
SAMPLE TIME
PERCENT
HYDROGEN
_£3
NITROGEN
OXYGEN
CARBON MONOXIDE
CARBON DIOXIDE
HYDROGEN SULFIOE
METHANE
ETHANE
ETHYLENE
PROPANE
PROPYLENE
3.1ft
ISOBUTANE
NORMAL BUTANE
TOTAL BUTENES
1. 3-BUTADIENE
ISOPENTANE
65
0,2,
NORMAL PENTANE
0,}
TOTAL PENTENES
TOTAL Ce PLUS
0,5-
1,1 0+1
R-vr
8108919-801
REMARKS:
PREPARED BY
L^ jy. f ^
BMITTEDBY:
5-6
-------
5.3 SASS PARTICULATE EMISSIONS
5-7
-------
ISOKINETIC PERFORMANCE WORKSHEET & PARTICIPATE CALCULATIONS
Plant T*^n RA^g,^c*.g..fN r A, Performed by
Date
Sample Location
Test No./Type
Barometric Pressure (in. Hg)
Meter volume (std),
17.64 /U/V^\
\"/lTm + 4M/
/Ck> 1.50(0
/( )\/(m0 + (^\
r 61 I 13-6
• yy.c.//ay y/g?.-?) + 460 y
Volume of liquid collected (grams)
Volume of liquid at standard condition (scf)
Vlc x 0.04707
Stack gas proportion of water vapor
vw std , (J^W
\ std + Vm std I J + v ; + "T5 -Z—
pb
Vm std
vtc
vw std
wu
Md
Ms
Pc
s
^^7>Z
^•JS.^0
lo^.Y
i^srso
v^. ;^-~3
^ f
50. »iZ.
.*•/• -i'.'i
Jy
ST. Si
7602/5/8T/Rev 1
5-8
-------
Temperature stack gas, average (°F)
St^rk velocity (fos)
/cavg + 460
,5
Pc Mc
S 5
/(?/*.•?) + 460
85 49 ( I' 1 /...I'lTT1;,, „
— M^^; J^xsw)
Total sample time (minutes)
Nozzle diameter, actual (inches)
Percent isokinetic (%)
17.33 (Ts + 460)(VW std * Vm std)
0 Vs Ps Nd2
17.33 (7/jK^+ 460)((f«>gw) + (_23f rC3
(^5*^" )U7.rr~)(2^.^ )( /.22)*
Area of stack (ft2) ». 3.1416
nr2 -T- 1 44 , n- (_ !2-r-l 44
Stack gas volume at standard conditions (dscfm)
60 (1 - Bwo)Vsavq A' / 528 \ / Ps \
wo avg , i T^ ayg + 4goj (29.92) '
60 (1 - )( )( )/ 528 \ /( }\
\ + 460 / U29.92)/
\ • / \ /
Particulate matter concentration, dry (gr/dscf)
15 13o M (grams) 15 13, ( )
Vm d ( )
Emission rate of particulate matter (Ib/hr)
0.00857 (QJ C, , 0.00857 ( )( )
- -(std)
TS
Vs(avg)
e
Nd
%l
AS
QS .
r
i*e
S(std)
E_
P
U
1i^.~]
^••''•"'>
*5T
-------
ISOKINETIC PERFORMANCE WORKSHEET & PARTICULATE CALCULATIONS
Performed by
Date
Sample Location £.g.;>
Test No. /Type a /CAI<;
"
Barometric Pressure (in. Hg)
Meter volume (std),
™^/V^\
\U/\Tm+4M/
joSfi. 35"!
/( )\/ftvro) + (2*0 \
r Gil J! 13-6
VO.OM J/Uio.-?) + 460 /
\ / \ '
Volume of liquid collected (grams)
Volume of liquid at standard condition (scf)
Vlc x 0.04707
Stack gas proportion of water vapor
vw std , < )
vw std - vm std i_j + ( )
Molecular weight, stack gas dry
(Ib/lb-mole)
(% C02x 0.44) + (% 02x 0.32) + (% N2+ % CO x 0.28)
( x 0.44) -(- ( x 0.32) + ( + x 0.28)
Molecular weight, stack gas wet
(Ib/lb-mole)
MdO-B ) + 18(8 ), (30.00) (1-..^) + 18fri-52.)
Absolute stack pressure (in. Hg)
p + Pstack ««' H2°) f _ (_)
Kb 13.6 ' ( > 13.6
Pb
u
vm std
vic
vw std
Bwo
Md
Ms
P.
s
^.HO
nr.^^
•3 no.*
14^. 2^
•IS'2-
2o.iTO
2%,^
U
4<7.Sfc
7602/5/81/Rev 1
5-10
-------
Temperature stack gas, average (°F)
Stack velocity (fps)
85.49 (C ) (V2P5 avg) /
V
OC An 1 »£%W „„«, \ / — —
Tgavg + 460
Ps Ms
&>) + 460
_'\4_: — '
Total sample time (minutes)
Nozzle diameter, actual (inches)
Percent isokinetic (%)
17.33 (T_ + 460)(Vta) std + Vm std
5 • w m
}
0 Vs Ps Nd2
(5
-------
01
I
ACUREX
Corporation
ANALYSIS LABORATORIES
DATA REPORTING FORM
CUSTOMER COI
RESULTS REPOI
VJTRACT NO
3T rn
307605.92
L. Waterland
ACUREX C(
TELEPHON1
3NTRACT N
n A81 -07-011
TOSCO
SAMPLE ID (CUSTOMER)
SAMPLE ID (LAB)
PARAMETER
Weight
Initial weight
Ash weight
I -Probe
543
=====
P. 0077
II Probe
556
E^^^^^^=
^=
0.0453
.
I -Filter
545
^— -—_:., „'!.•>_'_,-
3.1424
2.9029
0.2395
II-FHtei
038
jLr^r^n'^-i^',"',''"^
3.2191
2.9939
0.2252
Filter B'
571
MM_,^, ,,,^,M,^MI..,M,.,.,,,,JM,illli,,,
2.9151
2.9151
< 0.0004
k
l5T77'-"'"u— -J -'-,-•---'-
=
^^^^^^^^^^^^
^^^^^^==
UNITS
aram
gram
gram
Form EEO-057 4/M
ANALYST _
REVIEWER .
-------
5.4 EPA METHOD 5 PARTICIPATE EMISSIONS
5-13
-------
ISOKINETIC PERFORMANCE WORKSHEET & PARTICULATE CALCULATIONS
, gAE^g.sc-N.e.*. Performed by_
Date
Sample Location
Test No. /Type
Barometric Pressure (in. Hg)
Meter volume (std),
^4/!m\/Pb+^A
\°V\Tm+460/
/os.nf- . ..
/( )\ /«*V*) + (^-}\
r 61 I 13-6
\(L*l°.)/\(aL& + 46° /
Volume of liquid collected (grams)
Volume of liquid at standard condition (scf)
Vlc x 0.04707
Stack gas proportion of water vapor
Vw std , (112^
Vw std + Vm std ('^2£iJ + (t&&>
Molecular weight, stack gas dry
(Ib/lb-mole)
(% C02x 0.44) + (% 02x 0.32) + (% NZ+ % CO x 0.28)
( 12.1 x 0.44) + (y-.o x 0.32) + "(_2£/+ •» x 0.28)
Molecular weight, stack gas wet
(Ib/lb-mole)
MdO-B ) + 18(B ), feo.«i)(l..;^) + 18(.'51)
1
Absolute stack pressure (in. Hg)
Pstack (in- H20) <-5<)
p StdCK ^ f~iM"1 +
Kb 13.6 ' (±±1±> ' 13.6
Pb
w
vm std
V1C
vw std
Md
Ms
P,
s
^l.f-2
T3.1*l
5"7fo.t
n."?o^
.i^^
3o,iiZ
3*.\°1
J?1 .S6!
y
5-14
-------
Temperature stack gas, average (°F)
Stark vplncitv (fos)
/eavg + 460
5
Pc Mc
S S
/(in-."?) + 460
85 /JO f glf W «,r, 1 / . .
— )( '^ JtelJteLG.)
Total sample time (minutes)
Nozzle diameter, actual (inches)
Percent isokinetic (%)
17.33 (Ts + 460)(VW std + Vm std)
e vs ps Nd2
17.33 (-T/JO + 460)((,Vjo|) + (^3>"?f)?
( /*0 )(^.31 )U°I.<31 )( .j*?.)74
Area of stack (ft2) »= 3.1416
fff2 -r- 1 44 , »r (_ ^2-H 44
Stack gas volume at standard conditions (dscfm)
60 (1 - B )Vs A, / 528 \ / Ps \ '
wo avg „ /T^ avg + 460 i U$.92j
60 (1 - )( )( )/ 528T \ ((—)\
( + 460 / \(29.92)/
\ ' \ !
Particulate matter concentration, dry (gr/dscf)
15 4oo M (grams) ]5 13, ( )
Vm-td ( }
Emission rate of particulate matter (Ib/hr)
0.00857 (QJ C. , 0.00857 ( )( )
- -(std)
TS
Vs(avg)
e
Nd
%I
AS
QS
r
Lc
s(std)
ED
P
-)>*• 1
?*,31
l%0
.1.55^.
103,5-7
il,*7?
•
tlf*
7602/5/81/Rev 1
5-15
-------
ISOKINETIC PERFORMANCE WORKSHEET & PARTICULATE CALCULATIONS
P1 ant -TV.- -- « r*A«)
/(?9>r)\ /Cmd + (— } \
r 61 )( 13-6
\(ii£JL2)/\(/i^.i) + 460 /
\ / \ '
Volume of liquid collected (grams)
Volume of liquid at standard condition (scf)
Vlc x 0.04707
Stack gas proportion of water vapor
Vw std . te£)
Vw std + Vm std (tl&> + &M&
Molecular weight, stack gas dry
(Ib/lb-mole)
(% C02x 0.44) + (% 02x 0.32) +,(% N2+ % CO x 0.28)
(/(.I x 0.44) + C2.£x 0.32) + ( ?^+ x 0.28)
Molecular weight, stack gas wet
(Ib/lb-mole)
Md(l-Bwo) + 18c
S-7-^53
Jfe7.1
n. >otf
. i !f~^4 if-,
f ,
^t:.oo
•^,03
2% tt
7602/5/81 /Rev 1
5-16
-------
Tc$.c.o
Temperature stack gas, average (°F)
Stack velnrity (fns)
/T.avg + 460
85/19 fp ^ f/dP \ / ,,s, , „ ,
os.iy iy (V^HS aygj /
*,/ s s
/(tffc.fc) + 460
85/ig (.
Total sample time (minutes)
Nozzle diameter, actual (inches) (>A^1o'|N
Percent isokinetic (%)
17.33 (Ts + 460)(VW std + Vm std) 2or^-. &
Q vs ps Nd2
S S tl.k1>
17.33 ^H.t+ 460)((/%$oi) + ( ))
( /Src.' )( i«.S )U^.SV " )( .5S2.)2"
Area of stack (ft2) »• 3.1416
nr2 -•- 1 44 , n (_ ^2-M 44
Stack gas volume at standard conditions (dscfm)
60 (1 - B JVs A / 528 \ / Ps \
wo avg J /T^ ayg + 46Qj /29.92J
60 (1 - )( )( )/ 528' \ /( }\
+ 460 / \(29.92)/
\ ' ' \ '
Particulate matter concentration, dry (gr/dscf)
15 43° MD(9ram*) 15 /I32 ( )
Vm d ( )
Emission rate of particulate matter (Ib/hr)
0.00857 (QJ C_ , 0.00857 ( )( )
- -(std)
TS
Vs(avg)
0
Nd
XI
AS
QS
r
^c
S(std)
ED
P
fe*7<*.(tf>
W-t
/¥J
,%VZ
lO^H-
j
< ;. ,
7602/5/81/Rev 1
5-17
-------
TOSCO
01
/
.30
e.c
-------
ACUREX
ANALYTICAL REPORT
Sample of:
Sample
Requested By:
I.D. Number:
Analytical Method:
Date Of Analysis
Lab I.D. Number
Component
Analytical Result
Unit
r
V
7.5V
Analysis By
5-19 Date
Form EED--082 5/81
-------
ACUREX
ANALYTICAL REPORT
Sample of:
Sample
/
Requested By:
I.D. Number:
Analytical Method:
Date Of Analysis S
'-
Lab I.O. Number
Component
Analytical Result
Unit
a/.
,00301^
5-20
Analysis
Date.
By (J. J^zZ>
.
Form EED--082 5/81
-------
ACUREX
ANALYTICAL REPORT
Sample of:
Sample
Requested By:
I.D. Number:
Analytical Method:
Date of
Lab I.D. Number
Component
Analytical Result
Unit
5-21
Analysis By££-£
Date.
' f ' s
Form EED--082 5/81
-------
ACUREX
ANALYTICAL REPORT
Sample of:
Sample
Requested By: >O/tt*Gf
: >O/
1.0. Number:
Analytical Method:
Date of Analysis:
Lab I.D. Number
Component
Analytical Result
Unit
5-22
Analysis By.
Date.
Form EED—082 5/81
-------
5.5 SULFUR OXIDES EMISSIONS BY TURBIDOMETRIC ANALYSIS
5-23
-------
CONTROLLED CONDENSATION SYSTEM (CCS)
LABORATORY DATA SHEET
Date u-fr-fri
Sample Location _
Run No. /-ccs.
Analyst K.
Date Lab Analysis Completed
R.,ciu Titration Data
Method Tfchrttiv Titrant 0rrA Normality -,r?/k6 Indicator r
Sample
Description
Sample No.
Vol. of Sample
Vol . of Aliquot
Vol. of Titrant
Used
Average Vol. of
Titrant Used
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Vol. of Gas Sampled (VM)
Meter Pressure (PM) AI
. Calculations
y ft3, Avg. Meter Temp (TM) //£.2 °F.
"Hg, Meter a. Factor ,^" dimensionless
'48'15
£.. TM+460)
__
S04 96
ppm S04
PPM
S00
48.15
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S°2
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5-Z4
-------
ISOKINETIC PERFORMANCE WORKSHEET & PARTICIPATE CALCULATIONS
Plant ro^co ; ^^t^gg.^^ ki^ (LA Performed by
Date /^-.ifr-fr/
Sample Location
Test No./Type > ) <^.<
Barometric Pressure (in. Hg)
Meter volume (std),
"•"(M/V^
Vu/VTm*wo/
/e^y^LiJN
yaasc.) / \U-s) + 4<>o /
Volume of liquid collected (grams)
Volume of liquid at standard condition (scf)
Vlc x 0.04707
Stack gas proportion of water vapor
Vw std , ( )
Vw std + Vm std <: > + t J
Molecular weight, stack gas dry
(Ib/lb-mole)
(X C02x 0.44) + (% 02x 0.32) + (X N£+ X CO x 0.28)
( x 0.44) + ( x 0.32) +.( + x 0.28)
Molecular weight, stack gas wet
(Ib/lb-mole)
Md(l-BWQ) + 18(BWQ), ( )(1- ) + 18( )
Absolute stack pressure (in. Hg)
P.t,ck (in. H,0) ( )
P + S13C .~ ,. . .. . ( \ + n „„"!,,
pb 13.6 • ( ' 13.6
Pb
Vm std
Vlc
vw std
Bwo
Md
Ms
p
rc
3
2*1 ,4-Z
vT.3^
7602/5/81/Rev 1
5-25
-------
P ^ ant
Date
CONTROLLED CONDENSATION SYSTEM (CCS)
LABORATORY DATA SHEET
Analyst /?.
Date Lab Analysis Completed
Sample Location
Run No. 2 - Q^
Method T
Rrrfg.,Titration Data
Titrant £nvr Normality ,p/t,/u Indicator
Sample
Description
Sample No.
Vol. of Sample
Vol. of Aliquot
Vol. of Titrant
Used
Average Vol. of
Titrant Used
Probe,
Nozzle
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Rinse
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. Calculations
Vol. of Gas Sampled (VM) 2/r?ar"ft3. Avg. Meter Temp (TM)
Meter Pressure (P^) o^l^-l "Hg, Meter a Factor ,-"7*»'/ dimensionless
PPM
(
'48'15 C-.
, TM+460)
n
96
-. V)( a^.y- . P)
M
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ppm S04 =
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S0
48.15 ( . MgS09 )(//££, TM+460)
- t 1*1
. PM)
ppm S02 "' ;/v--7
5-26
-------
Plant
Date
ISOKINETIC PERFORMANCE WORKSHEET & PARTICULATE CALCULATIONS
Ofr- Performed by
/
Sample Location r/?,
Test No./Type___o/£C
-------
5.6 TRACE ELEMENT ANALYSES
Fuel
Filter
Filter Blank
XAD
XAD Blank
Impinger 1
Impinger 1 Blank
Mercury, Antimony, Arsenic
5-28
-------
COMMERCIAL TESTING & ENGINEERING CO.
OFFICES: 19* MOUTH IA SAIXE »T»EET, CHCCAOO. ILLINOIS «0«01 • AKEA CODE 319 T9f->494
Reply to iNsnuwENTAi ANALYSIS DIVISION. 320
9
45
15
10
<0.1
=0.2
NR
NR
NR
0.1
0.9
NR
STD — Internal Standard
NR - Not Rcpornd
All clement) not d«Mct*d<
INT — InMrtanmot
0.
Approved:
5-29
-------
COMMERCIAL TESTING & ENGINEERING CO.
QENE*AL OFFICE!: »»« NOHTH LA SALLE STREET, CMICAOO. ILLINOIS «0»01 • A»EA CODE 3IJ ?3».8«3«
Reply fO INSTIUMtNTAl ANALYSIS DIVISION. \O3i WBt U1H AVINUi. OOIDEN, COIOSAOO «MO\. *«3Ht M3-J7«-9SJI
To: Mr. Roy Belletto V^fck
Acurex Corporation ^fcilBk.
485 Clyde Street ""'""
Mountain View, CA 94042
Release No. 7
P. O. No.:
, SshipleNo.: 10-24-5
CTE 782
ELEMENT CONC.
Uranium <0.8
Thorium <0.9
Bismuth
Lead 0.9
Thallium
Mercury NR
Gold
Platinum Ml
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafni urn
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
SPARK SOURCE MASS SPECTROGRAPHIC ANALYSIS
CONCENTRATION IN PPM WEIGHT
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samari urn
Neodymium
Praseodymium
Cerium
Lanthanum
Bari urn 1
Cesium
Iodine
Tellurium
Antimony
Tin
Indium STD
Cadmium
Silver
Palladium
Rhodium
* Heterogeneous
ELEMENT CONC.
Ruthenium
Molybdenum
Ni obi urn
Zirconium
Yttrium
Strontium 0.5
Rubidium
Bromi ne
Selenium
Arsenic
Germanium
Gallium 0.1
Zinc 3
Copper 6
Nickel 8
Cobalt l0.2
Iron 26
Manganese 0.5
Chromi urn 1
Date: December 29, 1981
Analyst: J .
Oldham
IAD No.: 97-H690-116-13
ELEMENT
Vanadium
Titanium
Scandi um
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
0.8
10
16
66
5
33
5
16
13
12
6
=0.4
NR
NR
NR
1
2
NR
NO - Not Reported
All •Iwnwttt not d*tKt«d<
MC - M«jer Component
INT — InWrftrtnn
Q.
Approved:
M L
5-30
-------
COMMERCIAL TESTING & ENGINEERING CO.
SENERAL OFFICES: 331 NORTH LA SALLE STREET, CHICAGO. ILLINOIS 60(01 • AREA COOE 313 73I-««34
Reply tO INSTIUMENTAl ANALYSIS DIVISION. !4MS WEST *»TH AVENUE. GOLDEN. COIOSADO 90J01. PHONE: 303-27J.9521
To: Mr. Roy Belletto
Acurex Corporation
485 Clyde Avenue
Mountain View, CA.
94042
Date: October 14, 1981
Release No. 6 Exhibit A
P. 0. NO.: Subcontract No. SW59159A
Sample No.: ^81 -07-011 -545 SPARK SOURCE MASS SPECTROGRAPHIC
<7""C'i5Ce? » PitTE^ CONCENTRATION IN vg/cm2
ELEMENT CONC.
Uranium
Thorium
Bismuth
Lead 0.003
Thallium
Mercury NR
Gold
Platinum
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thul i urn
Erbium
Hoi mi urn
Dysprosium
ELEMENT
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium
Cesium
Iodine
Tellurium
Antimony
Tin
Indium
Cadmi urn
Silver
Palladium
Rhodi urn
CONC.
<0.0001
0.0002
0.0003
0.009
0.0002
0.0001
NR
<0.0001
STD
0.0002
0.001
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromi urn
ANALYSIS
CONC.
0.004
< 0.0001
0.005
0.0001
0.001
0.0007
0.003
<0.0001
NR
<0.0001
0.001
0.05
0.004.
MC
0.01
0.2
0.002
0.004
Analyst: J.
Old ham
IAD No, 97-H437-116-13
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodi urn
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
0.2
0.004
<0.0001
MC
>0.4
0.008
>0.2
0.01
MC
>0.03
MC
>0.08
=0.1
NR
NR
NR
>0.6
<0.001
0.01
NR
STD — Internal Standard
NR - Not Reported „ „_„, , 2
All elements not detected< 0.0001 ug/Cm
MC - Major Component >1
INT — Interference
Approved:
5-31
-------
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: llf NORTH LA SALLE «T»EET, CHICAGO. ILLINOIS «0«01 • AREA CODE 3U 71I-H34
Reply tO INSTHUMENTAL ANAIYSIS DIVISION. '4335 WEST 44TH AVENUE. GOIOEN, COIOIAOO KUOI, PHONE: 303-278.9521
To: Mr. Roy Belletto ,^11?"
Acurex Corporation •**!?. E.Tffii'
485 Clyde Avenue
Mountian View, CA 94042
Release No. 6 Exhibit A
P. 0. No.Subcontract No. SW59159A
Sample No.:A81-07-011-038SPARK SOURCE MASS SPECTROGRAPHIC
TOSCO -2- f=ft.7&^ CONCENTRATION IN ug/cra2
ELEMENT CONC.
Uranium 0.0003
Thorium 0.0003
Bismuth
Lead 0.006
Thallium
Mercury NR
Gold
Platinum
Indium
Osmium
Rhenium
Tungsten
Tantalum
Hafni urn
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
STD - Internal Standard
NR - Not Reported
All elements not detected <
MC — Major Component >
ELEMENT
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymi urn
Cerium
Lanthanum
Barium
Cesium
Iodine
Tellurium
Antimony
Tin
Indium
Cadmi urn
Silver
Palladium
Rhodi urn
O.OOOl ug/cm
1 yg/cm2
CONC.
<0.0001
0.0005
0.0004
0.02
0.0001
<0.0001
NR
0.0001
STD
0.0002
0.01
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromi ne
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
Approved: ^7
ANALYSIS
CONC.
0.009
<0.0001
0.002
0.0003
0.002
0.0003
0.002
0.0004
NR
0.0002
0.001
0.05
0.01
0.9
0.02
0.3
0.01
0.04
Date: October 14, 1981
Analyst: j _
Old ham
IAD No.: 97.H437-116-13
ELEMENT
Vanadium
Titanium
Scandi urn
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryl 1 i urn
Lithium
Hydrogen
fA^
CONC.
0.2
0.02
<0.0001
MC
>0.4
0.02
>0.2
0.02
MC
>0.03
MC
>0.08
=0.1
NR
NR
NR
0.1
<0.0001
0.002
NR
^&
5-32
-------
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: lit NORTH LA SALLE STREET, CMICASO. ILLINOIS «0«01 • AREA CODE 319 731-9434
Reply to iNsuuMENtAi ANALYSIS DIVISION. < 1 yg/Ctir
ELEMENT .
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromi ne
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
Approved: /^
ANALYSIS
CONC.
0.0002
0.0001
0.009
<0.0001
0.005
0.0008
0.001
NR
<0.0001
0.0006
0.006
0.002.
0.01
0.0003
0.02
0.002
0.0004
Wfr.
IAD No.. 97-H437-116-13
ELEMENT
Vanadium
Titanium
Scandi urn
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodi urn
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryl 1 i urn
Lithium
Hydrogen
X-te.4^,0—
CONC.
0.0003
0.1
<0.0001
MC
>0.5
MC
0.06
0.007
MC
>0.04
MC
>0.09
=0.3
NR
NR
NR
0.2
0.0005
NR
-^A
INT — Interference
5-33
-------
COMMERCIAL TESTING & ENGINEERING CO.
OSHEHAt. OFFICES: 12> NOHTH LA SAUE STREET, CHICAGO. UUNOIS «0«OI • A«EA COOE 311 78«-«434
Reply to iNsnuwtNtAi ANAIYSIS DIVISION. >ini west *»TH AVINUI. GOLDIN. COIOBABO HMOI. PHONE. 303.278-9521
4*
To: Mr. Roy A. Belletto ><^Lf~
Acurex Corporation AastLc^,
485 Clyde Avenue '""*•
Mountain View, CA 94042
Release No.
P. O. No.:Subcontract
Sample No.A81 -07-011
TOSCO 1 >:rft
ELEMENT CONC.
Uranium
Thorium
Bismuth
Lead 0.2
Thallium
Mercury NR
Gold
Platinum 0.7
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
6 Exhibit A
No. SW59159A
~569 SPARK SOURCE MASS
SPECTROGRAPHIC ANALYSIS
Date. October 12, 1 981
Analyst: J. Oldham
IADN0.;97-H437-116-13
? CONCENTRATION IN PPM WEIGHT
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samari urn
Neodymium
Praseodymi urn
Cerium
Lanthanum
Barium 2
Cesium <0.1
Iodine 0.1
Tellurium
Antimony - NR
Tin
Indium STD
Cadmium
Silver
Palladium
Rhodium
ELEMENT CONC.
Ruthenium
Molybdenum 0.2
Niobium <0.1
Zirconium 0.2
Yttrium
Strontium 4
Rubidium <0.1
Bromine 2
Selenium
Arsenic NR
Germanium
Gallium <0..1
Zinc 7
Copper 3
Nickel 9
Cobalt <0.1
Iron 6
Manganese 0.3
Chromi urn 1
ELEMENT CONC.
Vanadium <0.1
Titanium 1
Scandium <0.1
Calcium 36
Potassium 39
Chlorine 4
Sulfur 8
Phosphorus 1
Silicon 9
Aluminum 0.6
Magnesium 1
Sodium 11
Fluorine *0.1
Oxygen NR
Nitrogen NR
Carbon NR
Boron <0.1
Beryllium
Lithium <0-1
Hydrogen NR
MR - Not Reported
All elements not detected <
MC — Major Component
INT — Interference
0.1 ppm
5-34
-------
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 99* NO»TH LA SALLE STREET. CHICASO, ILUNOIS «0«OI • AREA CODE 319 »9e-«434
Reply to iNsnuMiHtAi ANAITSIS DIVISION. i«is west «IH AVINUJ. GOLDEN. COIOIAOO *MOI. PHONE: 303.278.9521
To: Mr. Roy A. Belletto ^iP*'
Acurex Corporation ^"SP,"?"*1
485 Clyde Avenue
Mountain View, CA 94042
Release No.
P. O. No.: Subcontract
6 Exhibit A
No. SU59159A
Sample No, A81-07- 011-562 SPARK SOURCE MASS
TOJCc? 9- Xfa
ELEMENT CONC.
Uranium
Thorium
Bismuth
Lead 0.2
Thallium
Mercury NR
Gold
Platinum 3
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thul i urn
Erbium
Hoi mi urn
Dysprosium
Date. October 12, 1981
Analyst: J. Old ham
SPECTROGRAPHIC ANALYSIS
IAD No.: 97-H437-116-13
{? CONCENTRATION IN PPM WEIGHT
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samari urn
Neodymi urn
Praseodymi urn
Cerium
Lanthanum
Barium 3
Cesium <0.1
Iodine 0.3
Tellurium
Antimony NR
Tin
Indium STD
Cadmium 0.1
Silver
Palladium
Rhodi urn
ELEMENT CONC.
Ruthenium
Molybdenum 0.9
Niobium
Zirconium 1
Yttrium
Strontium 0.5
Rubidium <0.1
Bromine 5
Selenium
Arsenic NR
Germanium
Gallium <0.1
Zinc 4
Copper 8
Nickel 1
Cobalt <0.1
Iron 32
Manganese 0.3
Chromi urn 5
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryl 1 i urn
Lithium
Hydrogen
CONC.
0.2
2
<0.1
150
250
15
74
8
170
20
3
>150
=0,2
NR
NR
NR
<0.1
<0.1
NR
STD — Internal Standard
NR - Net Reported
All elements not detected <
MC — Major Component
INT — Interference
0.1
Approved:
5-35
-------
COMMERCIAL TESTING & ENGINEERING CO.
SENEGAL OFFICES: 338 NORTH LA SAU.C STREET, CHICAGO. ILLINOIS «0«01 • AREA CODE 311 72»-«434
Reply tO INSTRUMENTAL ANALYSIS DIVISION. '4335 WEST 44TM AVENUE. GOLDEN. COLOBADO 10401. PHONE; 303.J78.V52I
To: Mr. Roy Belleto >
Acurex Corporation ^*
485 Clyde Avenue
Mountain View, CA 94042
Release No. 6 Exhibit A
P. 0. No.:Subcontract No. SW59159A
Sample No, A81 -07-011- 580 SPARK SOURCE MASS
4L
sSBBbBB*.
SPECTROGRAPHIC ANALYSIS
Date: October 15, 1981
Analyst: J. Old ham
IAD No.: 97-H437-116-13
~T05«? ^/Itf gLAWP CONCENTRATION IN PPM WEIGHT
ELEMENT CONC. ElEMENT CONC
Uranium Terbium
Thorium Gadolinium
Bismuth Europium
Lead 0.3 Samarium
Thallium Neodymium
Mercury NR Praseodymium
Sold Cerium
Platinum *44 Lanthanum <0.1
Iridium Barium *1
Osmium Cesium
Rhenium Iodine <0.1
Tungsten Tellurium
Tantalum Antimony NR
Hafnium Tin
Lutetium Indium STO
Ytterbium Cadmium
Thulium Silver
Erbium Palladium
Holmium Rhodium
Dysprosium Heterogeneous
ELEMENT CONC.
Ruthenium
Molybdenum 0.3
Niobium <0.1
Zirconium
Yttrium
Strontium 1
Rubidium
Bromine u-6
Selenium
Arsenic NR
Germanium
Gallium <0.1
Zinc *5
Copper 2
Nickel 5
Cobalt <0.1
Iron 3
Manganese °-2
Chromium u-3
ELEMENT CONC.
Vanadium <0.1
Titanium 3
Scandium <0.1
Calcium 71
Potassium 15
Chlorine !
Sulfur 4
Phosphorus 1
Silicon 5
Aluminum 3
Magnesium 1
Sodium 3
Fluorine <0.1
Oxygen NR
Nitrogen NR
Carbon NR
Boron <0.1
Beryllium
Lithium 0-1
Hydrogen NR
NR - Not Reported
All elements not detected< 0.1 ppm
MC - Major Component
INT — Interference
Approved:
5-36
-------
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 331 NORTH IA SAU.E STREET, CHICAGO. ILLINOIS «0«01 • AREA CODE 319 7J«-8434
Reply tO INSTtUMENTM ANALYSIS DIVISION. '433S WEST 44TH AVENUE. GOLDEN, COLORADO «
INT — Interference
Approved:
5-37
-------
COMMERCIAL TESTING & ENGINEERING CO.
OENERAL OFFICES: 99* NORTH LA JALLE STREET, CHICAGO. ILLINOIS «0«01 • AREA CODE 319 ?9«-S«34
Reply to iNsnuMCNtAi ANAITSIS DIVISION. i«35 WIST «TH AVENUE. GOIDEN. COIORAOO 80
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium 0.009
Cesium
Iodine
Tellurium
Antimony NR
Tin 0.02
Indium STO
Cadmium
Silver 0.8
Palladium
Rhodi urn
•Heterogeneous
0.002 wg/mL
10 ug/mL
IN ug/mL
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
Approved: St
ANALYSIS
CONC.
*0.02
0.003
0.004
<0.001
0.04
NR
0.01
0.01
0.008
<.0.001
0.05
0.001
0.01
Wk
Date October 12, 1981
Analyst: j _
Oldham
IAD No, 97-H437-116-13
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
,/•/
'fr^.
CONC.
0.004
0.02
<0.001
1
1
*3
0.3
0.8
*0.7
0.09
<0.02
0.2
=0.002
NR
NR
NR
<0.001
<0.001
NR
0~^&\
5-38
-------
COMMERCIAL TESTING & ENGINEERING CO.
QENERAL OFFICES: 3» NOHTN LA SALLE STUEET, CHICAGO. ILLINOI* 80601 • A*EA CODE 3IJ 7J«-«43«
Reply to iNStiuMtNtAi ANAITSIS DIVISION. !«MS west *«IM AVENUE. ooiofN. COIOBADO 10401. mom. J03.i7».»sji
To: Mr. Roy Belletto
Acurex Corporation
485 Clyde Street
Mountain View, CA
Release No.
.*.... Subcontract
P. O. No.:
4
94042
6 Exhibit A
No. SW59159A
,.
Date: October 14, 1981
Sample No.: A81-07-011-561 SPARK SOURCE MASS SPECTROGRAPHIC
T&CO 3- <$#/> 4. CONCENTRATION
ELEMENT CONC.
Uranium
Thorium
Bismuth
Lead 0.009
Thallium
Mercury NR
Gold
Platinum
Iridium
Osmium
Rheni urn
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thul i um
Erbium
Holmium
Dysprosium
STO — Internal Standard
NR - Not Reported
All elements net detected <
MC — Major Component >
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymi um
Praseodymi um
Cerium 0.009
Lanthanum 0.02
Barium 0.08
Cesium
Iodine <0.002
Tellurium <0.004
Antimony . NR
Tin 0.003
Indium STD
Cadmium
Silver °-08
Palladium
Rhodi um
0.001 iig/mL
10 vg/raL
IN ug/mL
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromi ne
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobal t
Iron
Manganese
Chromi um
Approved: ^/
ANALYSIS
CONC.
0.009
0.02
0.03
0.002
0.02
<0.02
<0.03
<0.02
NR
0.003
0.8
0.2
0.2
<0.001
0.5
0.1
0.05
27/4
Analyst.- j >
Old ham
IAD No.: 97.H437-116-13
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
^L.
CONC.
0.004
0.06
<0.002
1
1
0.1
MC
0.008
3
0.04
0.008
MC
=0.01
NR
NR
NR
<0.001
<0.001
NR
Sf
^£A
INT — Interference
5-39
-------
COMMERCIAL TESTING & ENGINEERING CO.
OENEHAl OFFICES: lit NORTH LA SAU.C STREET, CHICAGO. IU.INOIS «0«OI • ARE* CODE 3IJ 758-8434
Reply to iNsnuMiNtAi ANAIYSIS DIVISION. >O3i west «TM AVSNUE. GOLDIN. COIOBAOO uuoi, mQNt JD3-17I-9SZ)
To: Mr. Roy A. Belletto >^lP®>
Acurex Corporation ^SF**3*
485 Clyde Avenue
Mountain View, CA 94042
Release No.
P. O. No.: Subcontract
6 Exhibit A
No. SW59159A
Sample No,A81-07-011-560SpARK SOURC£ ^
TCJCC c2 3Lft f £,
ELEMENT CONC.
Uranium <0.01
Thorium <0.01
Bismuth
Lead
Thallium
Mercury NR
Gold
Platinum
Iridium
Osmium
Rheni urn
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thul i urn
Erbium
Hoi mi urn
Dysprosium
STD — Internal Standard
NR - Not Reported
All elements not detected <
MC — Major Component >
SPECTROGRAPHIC
Date October 12, 1981
Analyst: J .
Old ham
ANALYSIS IAD No-97-H437-l 1 6-1 3
P<-J#K. CONCENTRATION IN pg/mL
aEMENT CONC.
Terbium
Gadolinium
Europi urn
Samari urn
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium 0.04
Cesium 0.006
Iodine 0.002
Tellurium
Antimony . NR
Tin 0.01
Indium STO
Cadmium
Silver 0.03
Palladium
Rhodi urn
*Heterogeneous
0.001 ug/mL
1 0- ug/mL
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
Approved: ^y
CONC. ELEMENT
Vanadium
0.003 Titanium
Scandi urn
0.002 Calcium
Potassium
0.003 Chlorine
0.005 Sulfur
0.01 Phosphorus
Silicon
NR Aluminum
Magnesium
0.003 sodium
0.1 Fluorine
0-02. Oxygen
°-01 Nitrogen
<.0.002 Carbon
0-09 Boron
0.02 Beryllium
°-01 Lithium
Hydrogen
1/V&^
CONC.
0.001
0.02
<0.001
0.9
*MC
2
0.5
1
5
0.5
0.07
>4
=0.05
NR
NP
NR
0.001
0.008
NR
-^
5-40
-------
01
I
ACUREX
Cofpofation
ANALYSIS LABORATORIES
DATA REPORTING FORM
GMEA
cus
RES
AC
TfKl
TOMER COI
ULTS REPOI
IPRFRS
MTHACT NO
^f TO
307605.92
1 . Uaterlanrf
ACUREX C(
TELEPHONi
3NTRACT N
n A81 -07-011
rn
[ SAMPLE ID (CUSTOMER)
SAMPLE ID (LAB)
PARAMETER
Hg Aliquot
Hg blank Aliquot
Hg
As Aliquot
As blank
As
Sb Aliquot
Sb blank
Sb
F11ter-l
545
iTiiirrnia|ir. ; ^ ^ ; ^ -
-
3
4
<0.07
-
-
-
-
-
-
XAD-1
569
as
"... •.;.":— ii,,,.,,!,,.,,.,...,,,,...... ..
-
<2
3
<0.5
-
-
-
-
-
-
Imp 1-1
539
.. .'•'%. • ~j- — ""~^jvr
;-,..„..„„ : '. ,, „ - M -— — ^==^
<}
<0.07
-
-
-
-
-
-
Imp 2&3-1
555
!jJB" '->!-"." ""-•'-'""' ~
=T==
-------
5.7 TOTAL CHROMATOGRAPHABLE ORGANICS (TCO), GRAVIMETRIC ORGANICS (GRAV ,
INFRARED (IR) SPECTRA, GAS CHROMATOGRAPHY/MASS SPECTROMETRY (GC/MS)
AND LOW RESOLUTION MASS SPECTROMETRY (LRMS) OF TOTAL SAMPLE EXTRACTS
5-42
-------
ACUREX
Corporation
Energy & Environmental Division
ACUREX September 21, 1981
M.S. 2-2260 Acurex ID #A81-07-011
#A81-07-033
Client P.O. 307605.92
Attention: L. Waterland
Sample: 2 SASS Train, received 7/8/81
The above referenced samples were analyzed per level 1 protocol. Arsenic and
antimony were determined by furnace AAS.
Polynuclears were determined by a modified EPA method 625. 1 ul of sample
was injected onto a SE-54, J and W 30 meter capillary column using Grob
injection. The column was held at 30°C, then ramped at 10°C per minute to
270°C.
Benzo (c) phenanthrene, dibenzo (c,g) carbozole, 7, 12-dimethylbenz (a) an-
thracene, 3-methyl chloranthene, and perylene were not detected (<40 ng/.ul
injection) in any sample analyzed by GC/MS.
The GCMS analysis of XAD-2 resin spiked with 100 mg of naphthalene, phenanthrene,
and pyrene gave a recovery of 33% for naphthalene, 38% for phenanthrene, and
<1% for pyrene.
Prepared by: Authorized by:
M. C. Ferguson H
Sample Control Custodian
GN/MCF/kfh
485 CLYDE AVENUE, MOUNTAIN VIEW, CA 94042 PHONE (415) 964-3200 TELEX: 34-6391 TWX: 910-3796593
b-43
-------
rs ACUREX
T"x Corporation
ANALYSIS LABORATORIES
DATA REPORTING FORM
CMEA
CUSTOMER
CUSTOMER CONTRACT NO. 3Q7605.92
RESULTS REPORT TO L. Haterland
ADDRESS
TOSCO
DATE
ACUREX CONTRACT NO. A81-07-011
TELEPHONE
SAMPLE ID (CUSTOMER)
SAMPLE ID (LAB)
PA P Aim PTPR
GRAV Uncorrected
GRAV Blank
GRAV
TCO Uncorrected
TCO Blank
TCO
GRAV and TCO
FHter-1
545
<6
<10
<6
.
«•
— m
<0.2
XAD-1a
569
21
. 10
11
39
30
9
0.7
OMC-1
541
<4
<4
<4
<0.04
<0.04
<0.04
<0.1
Filter-2
038
<8
<10
<8
—
.
.
<0.3
XAD-2a
562
18
10
8
25
30
<5
0.3
OMC-2
559
6
4
6
0.64
<0.04
0.64
0.2
XAD-QC
033-5
-
0.74
<0.02
0.74*
_
XAD-lb
569
11
0.5
10
0.76
XAD-2b
567
2.3
0.5
1.8
0.35
UNITS
mg
mg
mg
mg
mg
mg
mg/dscm
CJl
*Spiked at 1.00 mg TCO
acontaminated XAD, high blank
^Sample/blank contamination corrected by GC/MS
ANALYST
Form E^O-OST * BO
REVIEWER
-------
tft RETORT
SAMPLE:
Tosco 1 Filter 545
Immaity
No Peaks
5-45
-------
tft REPORT
SAMPLE:
Tosco 1 XAD 569
W«M Nareto
tiittraity
ACfigpflMflt
Commtnti
2920
CH Alkane
CH Alkane
5-46
-------
IK REPORT
SAMPLE:
Tosco 1 Omc 541
lm»raity
AnignnMOt
Commmti
No Peaks
5-47
-------
IR REPORT
SAMPLE:
Tosco 2 Filter 038
WmNsmto
< (-•')
*
Inttnity
f
••
AttiytiMfrt Commmti
No Peaks
•
-
5-48
-------
Ill REPORT
tAMPLE: Tosco 2 XAD 562
Wm1ltmb«
tmtraity
Alignment
Cemmmti
No Peaks
5-49
-------
Ill REPORT
SAMPLE:
Tosco 2 Omc 559
WmMmtar
Anignimnt
Commmti
No Peaks
5-50
-------
m RETORT
SAMPLE:
Tosco Filter Blank 571
Intimity
AuigntiMnt
CommmtB
No Peaks
5-51
-------
IK REPORT
Tosco XAD Blank
Wmftimfctr
Intimity
AnigpfMflt
Commtnts
No Peaks .
5-52
-------
ACUREX
Corporation
ANALYSIS LABORATORIES
DATA REPORTING FORM
CUSTOMER
CUSTOMER CONTRACT NO. 307605.92
RESULTS REPORT TO L. Waterland
DATE
ACUREX CONTRACT NO. AST-07-01II
TELEPHONE
ADDRESS
TOSCO
SAMPLE ID (CUSTOMER)
SAMPLE ID (LAB)
PAH AM El tH
Phenol
!.
Blank '
corrected
* • 4
1 ,3-Dichlorobenzene
1 ,4-Dichlorobenzene
1 ,2-Dichlorobenzene
Nitrobenzene
2-Nitrophenol
Diphenylamine
Azobenzene
Phenanthrene
2, 6-Dinitro toluene
Other Polynuclears
Units
XAD-1
569
26
^1
2
1
3
4
<5
3
36
30
<1
<1
ng/ul
XAC-2
562
6
9
<1
1
<1
1
11
2
<1
3
3
<1
ng/ul
XAD-2 Dup
562DS
14
20
<1
2
<1
2
'10
2
1
4
<1
<1
ng/ul
.
XAD-1
569
1.0
:0.04
0.08
0.04
0.1
0.2
:0.2
0.1
1.4
1.2
:0.04
,0.04
ug/dscm
XAD-2
562
0.2
0.4
cO.04
0.04
:0.04
0.04
0.43
0.08
:0.04
0.1
0.1
cO.04
ug/dscm
XAD-2 Dup
562DS
0.55
.78
cO.04
0.08
<0.04
0.08
0.39
0.08
0.04
0.2
'0.04
'0.04
ug/dscm
i iMnra
01
I
en
Co
FormEEO-057 4/80
ANALYST _
REVIEWER
-------
ACUREX
Corporation
LYSIS LABORATORIES
DATA REPORTING FORM
CJI
1
Ol
^
«_>«-> o
CUS
RESI
AC
TC
i v_/mtn ___
TOMER COI
LJLTS REPOI
MtRFfiS
>4TRACT NO
3T rn
307605.92
L. Waterland
ACUREX C(
TELEPHONE
DNTRACT N
n A81 -07-011
)SCO
SAMPLE iO (CUSTOMER)
SAMPLE ID (LAB)
PARAMETER
Naphthalene
Other Polynuclears
Naphthalene
Other Polynuclears
.
Filter-1
545
.... .- . i .-.:..-.
<1
<1
<0.05
<0.05
-.!
Fllter-2
038
• ~^~
' - --•- • — •
j.",;.!."..1.-? -' ' _-~~-~-
<1
<1
<0.08
<0.08
Filter 81
571
• •• • ••
-
r=r==s==^=:
======i==i
<1
<1
-
-
,
c OMC-1
541
.......•.•.• •-•• !U"_i.' '•'••
-^ Ml ..- ..-.
-"---•• ••••-•-!• l"1"-
<1
<1
<0.04
<0.04
OMC-2
559
• ^-- "^^_'''~'':'_'^ •
~ '•^..'r.-r-j-— -;-^--^=
-------
OUGANICS ANALYSIS DATA SHEET
LABORATORY NAME Acurex
21 A
27.A
20 A
31A
3*) A
57 A
5SA
59A
60A
60A
*§5A_
IB *
SB
SB
9B
12B
1SB
20B
25B
26B
27B
2SB
KB
HB
37B
}9B
IOB
GCMS Detection Limits
ACID COMPOUNDS
2,*, 6- trichlofophenol
p-chloro-in-cresol
2- chlorophenol
2,4-d2ch)orophcno]
*
2,*»- dirncthylphcnol
2- nitrophenol
*- nitrophcnol
2,4- dinitrophenol
*j6- dinitro-o-cresol
pentachiorophenol
phenol
BASE/NEUTRAL COMPOUNDS
•cenaphthene
benzidine
• 1,2, ft- trichiorobenzene
• hexachlorobenzene
he x ach 1 or oc thane
bis(2-chloroethyl)ether
2-chloronaphthalene
1,2-dichlorobenzene
1,3-dichIorobenzene
l,fc-dichlorobenzcne
3,3'-dichlorobcnzid»ne
2,*- dinitrotoluene
2,6- dinitrotoluene
1,7- diphenylhydrazine
(as azobenzene)
fiuoranthene
»- ehlorophenyl phenyl ether
-na
5
5
5
5
5
20
20
20
5
1
1
20
1
1
1
1
1-
1
1
1
5
1
1
1
1
1
BASE/NEUTRAL COMPOUNDS
4 IB %-bromophcnyl phenyj ether
*2B'-
«3B
32B
33B
5* B
*35B
36B
61B
€2B
€3B
*66B
*fc7B
*6SB
*69B
*70B
*71B
72B
73B
74B
75B
7CB
77B
7SB
79B
SOB
SIB
S2B
S3B
S*B
bis (2-chloroisopropy!) ether
, bis (2-chlorocthoxy) methane
hexachlorobutadiene
hexachlorocyclopentadiene
isophorone
naphthalene
nitrobenzene
N-nitrosodimethyIam5ne
. N-nitrosodiphenylamine
N-ni trosodi-n-propy iamine
bis (2-ethy!hexyl) phthalate
butyl benzyl phthalate
di-n-butyl phthalate
di-n-octyl phthalate
diethyl phthalate
dimethyl phthalate
benzo(a)anthracene
benzo(a)pyrene.
3,4-benzofluoranthene
benzo(k)fluoranthene
chrysene
acenaphthylene
anthracene
benzofehOperylene
fluorene
phenanthrene
d!benzo(a,h)anthracene
Indenof 1 ,2,3-cd)pyrene
pyrene
JQi
1
1
1
1
1
1
1
1
NA
1
5
1
1
1
1
1
1
1
1
1
1
1
1
1
5
1
1
5
5
1
* Normally found 1n laboratory blanks 5-55
-------
ACUREX
Corporation
CMEA/ACUREX
ATTENTION: L. Waterland
Energy & Environmental Division
December 4, 1981
Acurex ID#: A81-10-011, A81-10-022
Client P.O.I: 307605
Samples: 9 extracts from Tosco and Ethan Allen
The above referenced samples were analyzed by direct probe mass spectrometry.
Searches have been made for classes of compounds most likely to be found in
the various 1C fractions, according to procedures described in the "IERL-RTP
Procedures Manual: Level 1 Environmental Assessment". The following frag-
ment ions used for search are given below:
Compound Class
Polycyclic aromatic hydrocarbons
Aliphatic hydrocarbons
Halogenated aliphatics
Aromatic hydrocarbons
Ethers
Alcohols
Phenols
Nitriles
Phthalate esters
Ami nes
Ketones
N-heterocyclics
Mercaptans, sulfides
Benzothiophenes
Carboxylic acids
Amides
Fragment ions (m/e-)
178,202,216,228,252,276
57,71
79,81,93,95,107,109;49,63
50,51,77,78,79,91
45,59,73
45,59,61,73,75
51,77,94
54,68,82
61,59,71,87
44,58
51,71
117,167;129,179
47,61,75
57,58,59,69,70,85,97,111,125
60,73,149
58,72,86,100
To test the analysis procedure, a standard mixture containing ethers, amines,
polycyclic aromatic hydrocarbons, nitrosamines, phenols, etc., was analyzed
under identical conditions as the samples. Losses of the very volatile
compounds such as naphthalene, bis(2-chloroethyl)ether, low molecular weight
nitrosamines were observed, however the higher molecular weight compounds in
a particular class were recovered.
Prepared by:
Greg Mfcoll
Program Director
Approved by:
Viorica Lopez-Avvfa, Ph.D.
Technical Director
6N/VLA:es
5-56
485 CLYDE AVENUE. MOUNTAIN VIEW. CA 94042 PHONE (415) 964-3200 TELEX: 34-6391 TWX: 910-3796593
-------
LP.MS REPORT
SAMPLE:
Toxco I XAD 569
Major CittfoHtt
Intimity
TOO .
TOO
100
10
10
10
Crtxgory
Ethers
Heterocyclic sulfur compounds
Carboxylic acids
Halogenated aliphatlcs
Aromatic hydrocarbons
Nitriles
MWRinei
Sub»Cat*soriM. Specific Compounds
Intimity
Composition
Othtr
5-57
-------
LRMS REPORT
SAMPLE: Tosco I XAD 569 (cont)
Major
Intanjiry
10
10
Cmqory
Alcohols
Heterocyclic nitrogen compounds
m '
.
MW Rjngi
Sub-Cat»5ori«, Sp*eifie Compounds
Intinaty
Citt^ory
m/t
Composition
Oth tf
5-58
-------
LRV.S REPORT
SAMPLE; Tosco II XAD 562 and OMC 599
Major CmjoriM
Inttntity
100
100
10
10
Cmeory
Aliphatic hydrocarbons
Amines
Aromatic hydrocarbons
Carboxylic acids
t
MW Ranoi
Sub*Cat>sor>tf. Sp«eific Compounds
Intinary
Othtr
Composition
5-59
-------
5.8 C-G CHROMATOGRAMS
5-60
-------
TOSCO
Run
Time
Bulb
cl C2
C3
C4
C5
C6
6/18/81
a
Sample
Sample
Sample
Sample
Cal 11
Blank
Blank
Samp 1 e
Sample
Cal 16
Sample
Sample
Sample
Sample
Blank
Blank
7
8
9
10
12
13
14
15
17
18
19
20
24
25
1330
1335
1330
1335
1627
1649
1702
1740
1750
1920
1945
1950
1945
2055
2155
2205
A
B
A
B
--
B
A
B
A
--
A
.8
A
A
A
B
5.2
0.9
1.3
ND
17.0
2.0
2.1
1.2
ND
17.0
2.5
0.9
1.2
2.3
2.1
2.0
ND
ND
ND
ND
10
0
ND
0
ND
10
7
8
3
4
ND
ND
.3
.3
.3
.3
.8
.0
.7
.3
ND
0.8
3.0
1.2
10.6
ND
ND
1.5
1.4
10.6
5.6
5.6
1.6
1.4
ND
ND
ND
ND
4.9
0.2
10.8
ND
ND
ND
ND
10.8
7.0
7.3
2.0
0.9
0.2
ND
ND
ND
0.2
ND
10.4
ND
ND
ND
0.9
10.4
0.7
ND
2.4
ND
ND
ND
ND
ND
ND
ND
10
0
ND
ND
ND
10
ND
ND
0
ND
ND
ND
.1
.4
.1
.2
6/19/81
Cal 27
Sample
Sample
Sample
Sample
Sample
b
Cal 2
Sample
Sample
b
Cal 1
Blank
Blank
,28,29
30
31
32
33
34
3
4
2
3
1110
1115
1115
1400
1405
1624
1645
1650
1621
1819
1831
A
B
B
A
B
__
A
B
__
B
A
17.0
1.1
1.1
1.1
1.3
1.0
17.0
1.5
0.7
17.1
1.6
1.3
10
1
1
1
1
1
10
3
3
10
ND
•ND
.3
.1
.8
.6
.8
.1
.3
.0
.0
.3
10.6
0.1
ND
ND
ND
ND
10.6
ND
ND
10.6
1.4
ND
10.8
ND
ND
0.1
ND
ND
10.8
0.2
ND
10.8
ND
ND
10.4
ND
ND
ND
ND
ND
10.4
ND
ND
10.4
ND
ND
10
ND
ND
ND
ND
ND
10
ND
ND
10
ND
ND
.1
.1
.1
aAll values ± 10 percent, less than 0.5 ppm.
bLost power
Note: All values calculated by averaging the before and after (where
applicable) calibration amount/area. Values less than 0.1 ppm are NDa.
Tests run at 110°C, 26 psi through two Varian model 3700 GC packed with
6 ft of Super Q (see appendix A of Volume I for more detail).
5-61
-------
TOSCO 6-18-81
Run
Run
Run
Run
Run
Run
1 (Recal B) Ci-Ce
Cl
C3
C4
^
C6
2 Blank B 1819
Cl
C3
2 (Recalibrated B)
Cl
C2
C3
4
i
6
3 Blank A 1831
Cl
3 Sample A 1645
Cl
C2
C3
4 Sample B 1650
Cl
C2
C3
RT
0.26
0.42
0.72
1.46
3.28
7.88
0.22
0.75
Cl-Cfi
0.26
0.41
0.71
1.45
3.28
7.87
0.22
0.23
0.47
0.96
0.23
0.47
0.96
Amount/Area
9.1123 x 10-4
3.4823 x 10-4
2.2827 x 10-4
1.6147 x 10-4
1.3578 x 10-4
1.1422 x 10-4
1,728
6,076
8.9310 x 10-4
3.4392 x 10-4
2.1631 x 10-4
1.4770 x 10-4
1.2880 x 10-4
1.1383 x 10-4
1,441
1,649
8,656
1,610
•
764
8,548
613
PPM
17.0
10.3
10.6
10.8
10.4
10.1
1.6
1.4
17.0
10.3
10.6
10.8
10.4
10.1
1.3
1.5
3.0
0.2
0.7
3.0
0.09
5-62
-------
TOSCO 6-18-81 (Continued)
Run
Run
Run
Run
Run
Run
RT
Amount/Area
PPM
6 Calibrated Ci-Cfi
c
Cp
C3
C4
c&
7 Sample
Cl
8 Sample
Cl
C3
9 Sample
Cl
Cs
C4
C5
10 Sample
Cl
C3
C4
11 Ci-Cfi
Cl
C2
C3
C4
C5
C6
0.24
0.41
0.70
1.42
3.22
7.74
A 1330
0.22
B 1335
0.22
0.47
A 1330
0.22
0.46
0.96
1.33
2.89
B 1335
0.22
0.46
0.97
1.34
(Recalibrated)
0.23
0.41
0.70
1.42
3.23
7.76
9.2372 x 10-4
3.4661 x 10-4
2.2535 x 10-4
1.5594 x 10-4
1.3019 x 10-4
1.0560 x 10-4
5,888
1,069
4,126
1,572
15,299
26,831
10,875
1,579
0
6,388
371
867
8.3600 x 10-4
3.0853 x 10-4
1.6758 x 10-4
1.0577 x 10-4
1.2584 x 10-4
2.1048 x 10-4
17.0
10.3
10.6
10.8
10.4
10.1
5.2
0.9
0.8
1.3
3.0
4.9
0.2
0
1.2
0.2
17.0
10.3
10.6
10.8
10.4
10.1
5-63
-------
TOSCO 6-18-81 (Continued)
Run
Run
Run
Run
Run
Run
12 Blank Bulb B
Cl
C2
C6
13 Blank Bulb A
Cl
C4
14 Sample B 1740
Cl
C2
C3
15 Sample A 1750
Cl
C3
C5
16 (Recalibrated
cl
C2
C3
C4
C5
C6
17 Sample A 1945
Cl
C2
C3
RT
1649
0.22
0.37
3.82
4.99
5.62
1702
0.22
0.91
0.22
0.31
0.46
0.23
0.47
1.75
B) 1920
0.25
0.42
0.71
1.45
3.27
7.86
0.24
0.38
0.46
0.69
Amount/Area
2,286
991
1,231
1,188
274
2,366
57
1,371
951
7,432
0
6,885
6,903
LOST POWER
9.2447 x 10-4
3.5481 x 10-4
2.3173 x 10-4
1.5875 x 10-4
1.3516 x 10-4
1.2190 x 10-4
2,748
9,701
12,396
24,034
PPM
2.0
0.3
0.4
2.1
0.01
1.2
0.3
1.5
0
1.4
0.9
17.0
10.3
10.6
10.8
10.4
10.1
2.5
7.8
5.6
5-64
-------
TOSCO 6-18-81 (Continued)
Run 17 Sample A 1945
C4
C5
C6
Run 18 Sample B 1950
Cl
C2
C3
C4
Run 19 Sample A 1945
Cl
C2
C3
C4
C5
C6
>C6
Run 20 Sample A 2055
Cl
C2
C3
C4
C6
Run 21, 22, 23 Flame
RT
Cont.
0.96
1.41
2.30
2.55
2.72
2.95
2.99
6.03
0.22
0.38
0.45
0.68
0.95
1.37
0.21
0.38
0.45
0.69
0.95
1.43
2.14 .
3.31
5.00
8.63
0.20
0.37
0.46
0.69
0.95
1.37
4.0
Out
Amount /Area
17,404
26,507
196
1,499
865
1,194
1,530
592
1,000
9,514
13,108
24,088
18,656
27,033
1,312
3,032
7,373
7,114
2,921
9,483
8,550
9,376
1,717
748
2,526
3,346
8,645
6,058
2,888
2,537
0
PPM
7.0
0.7
0.07
0.9
8.0
.5.6
7.3
1.2
3.7
1.6
2.0
2.4
0.2
—
2.3
4.3
1.4
0.9
0
5-65
-------
TOSCO 6-19-81 (Continued)
Run
Run
Run:
Run
Run
Run
Run
24 Blank A
r1
C4
25 Blank B
>C6
27, 28,
1
C5
31 Sample
Cl
C2
32 Sample
C2
C4
33 Sample
C2
34 Sample
Cl
C2
RT
2155 Zero Air
0.22
1.18
2.38
2205 Zero Air
0.22
9.25
and 29 (Recalibrated
0.25
0.40
0.69
1.43
3.26
7.82
B 1115
0.22
0.38
0.47
B 1115
0.22
0.37
0.47
0.96
A 1400
0.22
0.46
B 1405
0.22
0.32
0.46
LOST
Amount/Area
2,283
1,277
658
2,189
174
B) Ci-Cfi)
9.6424 x 10-4
3.5852 x 10-4
2.3319 x 10-4
1.5990 x 10-4
1.3517 x 10-4
1.1796 x 10-4
1,220
666
4,480
1,220
680
3,754
665
1,409
5,096
1,101
331
2,729
POWER
PPM
2.1
0.2
0.09
2.0
17.0
10.3
10.6
10.8
10.4
10.1
1.1
1.8
1.1
1.6
0.1
1.3
1.8
1.0
1.1
5-66
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client
, Location To£c.o
, Job No. Jo-iu.og.Si
yl A J5 . C^JL\
Injection Date £-^-8| , Time ,2.:^.<~7 , Instrument ID 3-1*0
Recorder/Printout Reference No.
Purpose of Run c, - c.fr n-*i
1 , Recorder ID HP^s-ioA
>iPf-)tA-P l?aAJ ANJAL.VC.lC
Sample Description , i?,? •? • ;_.-?• A.
GC CONDITIONS
Amount Injected 3.OrAv_ , Inj. Port or Sample Loop Used a..Ut*^ Loot
Detector Used: FID •* , ECO
Detector Attenuation H
Column: Liquid Phase
Length &' , O.D. (/s- "
, FPD , TCD (Current )
, Amplifier or Range it>~^
, Solid Phase ^oft-fvPA^c. Q .
, I.D. , Material S.S.
Temperature: Injector /Zo °C, Oven /s~o °O, Detector AS~c> °C-
Temperature Program x s^y ^ £ ftYv\w L.
SAMPLE RUN
Sampling Method €*£A.C> • ^"oo cv>u i-S- Sous
RT Area Peak He
• +Z £f>W
ight Amount (j>pH| Component
•r*-? /-
Name of Operator f*\.b. o.ai
, Date _i-
5-67
-------
I lit
W
W S W
O "^ : —•= 5-
Pi/
s: • =
3 i C
T3 3
O O :
2K
fl> :»
RUN I
ESTD
RT
JUH/18/81 13=^5=57
AREA TYPE CM.*
5888 BP 1R
WOUNT
5.439
TOTftL ARF.A= 5888
MUL FACTOR= 1.
RUN I
JUN/18/81
= 55 =
ESTD
RT
8.22
TOTAL AREA*
HUL FACTOR= 1
AREA TYPE
5888 BP
5888
CALt
1R
AMOUNT
5.433
5-68
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client Cry\Gt\
, Location TO&C.O
, Job No.
Injection Date fc-vy-6< . Time , 5r;*~'. ci? • Instrument
Recorder/Printout Reference No. 5T _ , Recorder ID
Purpose of Run Q, - C.^
Sample Description
GC CONDITIONS
Amount Injected a.0fvvv_ . Inj. Port or Sample Loop Used a.Pr*.t. Loo/»
Detector Used: FID X t ECO _ , FPD _ , TCD _ (Current _ )
Detector Attenuation H _ » Amplifier or Range ip-
5-69
-------
8
S
(/> 3 CO CO
tFrlllls
no ••O m 2
gf
>-: «
Mi
V<:
STT.
=• : : 0
-
a JO :
:
'
a h
-
o
52 !
N •
CD :
jai x;
|i ^
rkl
TI *^ ^* •***
_ :r» : -v TI
." . \n — •••£
o r* i ^-2. g
xf * : : ?—
O ?v
z*
^ir
o o:
0 O :
RUN t 3
ESTD
RT
8.22
JUM/18/81 15=48=86
AREfl TYPE ML*
1869 PV 1R
flMOUNT
8.988
TOTflL AREfl= 1869
HUL FACTOR= i.8888E+88
OP * 6 8
RPRT UHC PKS
YES
RUN * 3
ESTD
RT
a.ae
8.47
JUH/lS-'Sl 15 = 48 =
AREA 'FYPE CAI.I
1869 PV 1R
4126 VB
AMOUNT
9.988
8.888
TOTflL AREfl= 5195
HUL FACTOR= 1.8888E+88
5-70
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Qv>g*\
, Location
» Job No.
Injection Date fc-iy-St . Time
Recorder/Printout Reference No.
Purpose of Run Q, — c./.
_, Instrument ]
, Recorder ID
Sample Description
GC CONDITIONS
Amount Injected 3.0fv\u . Inj. Port or Sample Loop Used aj
Detector Used: FID y. . ECD , FPD , TCD (Current )
Detector Attenuation H , Amplifier or Range ip""1*
, Solid Phase
Column: Liquid Phase _
Length &' . O.D.
Temperature: Injec
Temperature Program
, I.D.
Temperature: Injector /Zo C, Oven /so C., Detector
, Material S.S.-
o.
Sampling Method £A.
SAMPLE RUN
fv\\. £.£
RT
,% ^
.•+<<-
.i^
i-1-
>.-'\
Area
<>TL
i ~ ^n
x i»^3 (
icif-i?
' >"1^
Peak Height
\
Amount (pp^
;, s
J. c
\ ^^
;
c . L
Component
'— •(
'•— "'.
\
/
'-'^
Name of Operator FA.b. c.^i
, Date _i-f
19 9f|
5-71
-------
LIST' ZERO = 8, 9.9
-2.89
w o Q
> "i 2
gl£2m-5|i
IE?!if!B
"2| i
« 5 Jf
D:
g395o! g??*j
* £^* 5! "«*
O U. • . :e» •
fo
•a — •
i SifcfiSi
iprriili
t7
>
b it? • :.-a 5- s; 2
i %f • • * Dl ••* 1 Q)
• /• * * • • ^™ O • •
•f r •: '• r. :_a:N-
3^1; I;
t!*|! rojoidl
? : ? : ? O O : :
ST
RUN t
ESTD
RT
8.82
8.46
9.36
1.33
e.89
JUH/18/81 15 •• 53 '38
AREA TYPE
1572
15E99
£6831
18875
1579
PV
VV
VV
V8
BV
CM.I
1R
4R
flBOUNT
1.452
8.808
8.888
1.696
8.888
TOTAL flREfl=
NUL FACTOR=
56156
.8880E-t88
5-72
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client
, Location Tos,c.o
> Job No.
Injection Date b-\V-%\ , Time
Recorder/Printout Reference No.
Purpose of Run QJ -_c/_
'; ;S , Instrument ]
, Recorder ID
Sample Description
tf -
GC CONDITIONS
Amount Injected 3.pfv\v. . Inj. Port or Sample Loop Used a.t?NM Loofr
Detector Used: FID X . ECD , FPD , TCD (Current )
Detector Attenuation H . Amplifier or Range it)"***
Column: Liquid Phase
Length £/
, Solid Phase
, O.D.
, I.D.
Temperature: Injector /Zo C, Oven
Temperature Program _
, Material 5.S-
°O, Detector AS^a °C_
Sampling Method
SAMPLE RUN
S"oo CAU &-S- EocS
RT
.'2.2.
,HC-
•m
\ . 3V
Area
5
'
-------
4i>
fl.34
Ope
as
Tf |
iaf a B^
II
£ S 2
SCflWHXTIjOaj
!5 2 m /^ 3_ _ _.
33 : o 3 •? T
o : 5? 3-1!8 - ~
UM »* CP uJ • O- ; .
* 5" ?_
tr
W :
I'D:
H p.
i
3
iOi S
C
n
' H I1 2-
i or.'1 fa
• 3. -o
93
0)
« X * • O
•Z.S 'c>'oO
^w-* O
V - 2
^••3. 3 ^ :
1 : af :
: >- r- w :
=•00
? O O :
RUN * 10
JUN/18/81 1605=19
ESTD
RT
8.22
9.46
9.97
1.34
TOTAL AREft=
HUL FftCTOR= 1
flREft TYPE
9
6338
371
867
PP
PB
B8
88
CflLf
1R
4R
7576
^9
AMOUNT
9.135
5-74
-------
GAS CHROMATG. nPH OPERATING CONDITIONS AND FIELD LOG
Client
, Location TP&CC?
, Job No.
Injection Date t^-.v-?' . Time '.„•.:, —. !.^ . Instrument
Recorder/Printout Reference No. i, , Recorder ID H
Purpose of Run
Sample Description
/V>uf- - Curves.
Amount Injected 3.0
GC CONDITIONS
, Inj. Port or Sample Loop Used
Detector Used: FID y t ECO _ , FPD _ , TCD _ (Current
Detector Attenuation _ ^- _ , Amplifier or Range )
Column: Liquid Phase
Len9tn C>/
, Solid Phase
Q> *
C>/ O.D.
Temperature: Injector
Temperature Program
"
I.D.
Oven ;
, Material
» Detector
SAMPLE RUN
Sampling Method p.igc^• i J-
~ • 1 -;
*-\T/«
' /Area
, -."*
*.S^cc
>^ ^^"3
— : -~V'
i, «3 ( > 3
, /^ :*^X- . ',
(,*~ > '-''-
i.'i-^'.r-r
7. rVv'
">•( ~^ t i— '
Peak Height
.
Amount ^>p^
n.o
\O-S
fo.o,
lo. Sf
10>
lO. \
Component
cr
c,
c^
c*,
Ce-
Cfe
Name of Operator M . ft .
, Date
19
5-75
-------
c
RUH I 11
ESTD
RT
9.35
8.4£
8.72
1.45
3.£8
4.33
7.35
JUH/18'81 16=27=39
flREA TYPE
£8335
33384
S3253
183118
82646
9846
47986
PV
VV
VV
VB
BV
VV
BP
CAL*
1R
ZR
3R
4R
5R
5R
flMQUHT
18.784
11.571
14.254
15.923
18.759
8.800
5.967
TOTflU AREA= 358768
HUL FflCTOR= 1.8008E+80
5-76
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client
, Location Tog.co
, Job No.
Injection Date fa-ifr-St . Time )(=,-.MV. /i- . Instrument I
Recorder/Printout Reference No. • 9 , Recorder ID
Purpose of Run Q.-C.,,
Sample Description
GC CONDITIONS
Amount Injected 3.0fy\\_ . Inj. Port or Sample Loop Used a.pNvu Loot*
Detector Used: FID y . ECD _ , FPD _ , TCD _ (Current _ )
Detector Attenuation H _ > Amplifier or Range io~^
Column: Liquid Phase
Length &'
, Solid Phase
O.D.
"
. I.D.
Temperature: Injector /Zo C, Oven
Temperature Program T SOT H c fcrAR L
, Material
*C, Detector
SAMPLE RUN
Sampling Method *~*
* •& • a,f• •• -'-M
RT
• ."•' "^
• ."5 "1
• ', 1
" ^ . ** -*"
''i"'\'\
~^- • *•• -,-
Area
x^^
^" i
-, J. •'
' '~ 3 i
', v •< ''
^•1 T-
Peak Height
\
Amount (^>p^
^.c
c« 1
\
/ •-. -i-
/
Component
C •
^
•-*» ".-
\
'••— -^
Name of Operator
, Date _3-»
19 9r>
5-77
-------
l$0'c
!,*,„-"
RUN t 12
ESTD
RT
8.22
9.37
3.82
4.99
5.62
JUN/18/81 16=49:16
AREA TYPE
2286 BP
99 i P8
1231 D PB
1188 0 BE
274 BB
CALf
1R
2R
AMOUNT
1.911
9.386
9.968
9.986
TOTAL AREA=
MUL FACTOR=
5979
5-78
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client Cfy\<£(\
, Location fo^co
» Job No. Jo
Injection Date fe-iy-St . Time IT- -''2: >5" , Instrument ]
Recorder/Printout Reference No. j£ , Recorder ID
Purpose of Run Q, - c./.
Sample Description
"••
GC CONDITIONS
Amount Injected 3.pfww . Inj. Port or Sample Loop Used a.o*u. Coofr
Detector Used: FID y . ECO , FPD , TCD (Current )
Detector Attenuation H » Amplifier or Range it>~tv
Column: Liquid Phase
Length fe,'
, Solid Phase
,0.0.
, I.D.
, Material S.S-
Temperature: Injector /Zo _C, Oven
Temperature Program
O, Detector
SAMPLE RUN
Sampling Method
RT
• ^ -^
. T ,
Area
'•i Ifcfc
•>"1
Peak Height
Amount (,ppv!|
2>i
.c \
Component
"*^ /
C>
Name of Operator tA.b. c.^i
, Date _g-
199f|
5-79
-------
'91
3 2 ™
'sSsjSSiJJ
!lafi9v:ii
0
1
3 %
3
RUN I 13
ESTO
RT
8.2£
8.91
JUH/18/81 17'32;35
AREft TYPE CAL*
2366 PB 1R
57 BB
(MOUNT
1.978
8.800
TOTftL AREft=
«UL FACTOR=
2483
5-80
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client Crv\Gf\
, Location
» Job No.
Injection Date fc-\y-6t . Time //:;- ^ . Instrument 1
Recorder/Printout Reference No. \V , Recorder ID
Purpose of Run Q, - C./,
Sample Description
GC CONDITIONS
__, Inj. Port or Sample Loop Used fl.P*At. Loot*
Detector Used: FID X , ECD , FPD , TCD (Current )
Amount Injected
Detector Attenuation ^
Column: Liquid Phase
Length &'
, O.D. Vfr" . I.D.
_, Amplifier or Range it>~^
, Solid Phase ~
, Material S.S.
Temperature: Injector /Zo °Ct Oven /£~o °Ot Detector AS^>
Temperature Program
Sampling Method
SAMPLE RUN
.S~oo mv. S-S-
RT
• 2.2.
« — • /
• rG?
Area
f ' J "' /
53"-
7^;- L
Peak Height
Amount (j>f>A/$
/. :~
C.'l
I ->~~
Component
l— t
'^* -.
••** -.
Name of Operator
, Date
5-81
-------
\TiO
T.M1 1*3'
.44
RUN * 14
ESTO
RT
9.32
9.31
9.46
I <.M/W«,
JUH/18/81 18=19=99
flREA TYPE CflLI
1371 PV 1R
951 VP
7432 PB
AWOUHT
1.146
8.998
9.966
Co o
m
lr||of|||^||i |
^•hl I sl i gi 8^ ? ir
^i"^:r!o:isl I
r ia
p :• -a
CO :
io;
Hf
O 3
t7
? | i rg: *.
•n \-% • •&* '•
o-
r> o o ;
£_ 3 =
J-'3. a a
3 . **
lLj,
v!£i^
TOTAL AREA= 9754
NIJL FACTOR= 1.8888E+9e
5-82
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client
, Location
, Job No. .3o"iu>02.Sl
Injection Date fe-iy-Si . Time /••'."?/• g"u- , Instrument 1
Recorder/Printout Reference No. ;S" , Recorder ID
Purpose of Run Qj.-_C./_
Sample Description <~
.r- A
Amount Injected
GC CONDITIONS
__, Inj. Port or Sample Loop Used fl.P***,. loofc
Detector Used: FID y_, ECD , FPD , TCO (Current )
Detector Attenuation H » Amplifier or Range it>""u
, Solid Phase 5W*PAtc. Q
, I.D. , Material S.S-
Column: Liquid Phase __
Length t,' . O.D.
Temperature: Injector /Zo °C.t Oven /go °O, Detector
Temperature Program _
Sampling Method
SAMPLE RUN
^"oo '•* 7
/ , I C"
Area
f.
fev>r-
/^jc?
Peak Height
Amount (,ppM|
—
/. V
^.1
Component
c,
d--»
'••H* "
Name of Operator fA.b. r ai
, Date _i-f_
19 2f|
5-83
-------
l-fiff
I 75
ST
CO S «
til
ab!
B!
DET
i i
•O 33 33 S
3 33 D) -0
3
P: i.:i|
?"< 3" : ?
li
r> o
o ^
fS
1 ff
o
**r
*-»
«
^ s- =•
; IP'"-
o o:
O O i
;i
:i
XT-
2:
RUN * IS
JUN/18/81 18=21'54
ESTD
RT
8.33
8.47
1.75
AREA TYPE
8 PP
6885 PB
6983 0 88
CflLI
1R
flNOUHT
8.880
8.088
TOTAL ftREA= 13788
NUL FACTOR= 1.8888E+80
5-84
-------
GAS CHROMATG. *PH OPERATING CONDITIONS AND FIELD LOG
Client e/vi£A Location TP&CP
, Job No.
Injection Date £-^-yiu_, Time . y. ;c; r^ , Instrument ]
Recorder/Printout Reference No. /,_ , Recorder ID
Purpose of Run
Sample Description
f- n -
Amount Injected
GC CONDITIONS
, Inj. Port or Sample Loop Used g.OMil/^
Detector Used: FID x , ECD , FPD , TCD (Current )
Detector Attenuation ^_ , Amplifier or Range
, Solid Phase
Column: Liquid Phase
Length <*' O.D. !/j." . I.D. _
Temperature: Injector t?t> °C.t Oven __£
Temperature Program _
, Material
'c., Detector
SAMPLE RUN
Sampling Method Pn£c^g. (_of>P
RT
Peak Height
Amount
Component
G,
c,
. I
Cfe,
Name of Operator
. 6 .
, Date
19 fir/
"5-85
-------
\-T-f
o a
O fi>
1
ir-rriis! *•
? 3 : :- !*;•*': 5 I
"Utpy ^
|n||^°00j f ! ?
b^; f'l^l k= if
-,
2 **
p! I; II J.I 5
Hi! I! ll?l?ri! i
RIM t 16
ESTD
RT
8.23
8.42
9.71
1.45
3.27
4.26
7.86
AREA TYPE CftLI
18389
29838
45742
68833
76947
1719
32853
BV
VB
BB
PB
BV
W
PB
1R
2R
3R
4R
5R
6R
JUN/18/81 19=28=39
ffflOUHT
15.373
3.957
7.666
7.196
9 683
9.900
17.439
TOTAL AREft= 332718
HUL FACTOR- 1.88e8E+98
5-86
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client CfY\Gf\
, Location Tog.c.0
, Job No.
Injection Date fe-iy»Si , Time ^/; :ci\ -if . Instrument ID
Recorder/Printout Reference No. .") , Recorder ID
Purpose of Run Q.-d,_
Sample Description
GC CONDITIONS
Amount Injected 3 .0 rAU . Inj. Port or Sample Loop Used a.P»M..
Detector Used: FID X . ECO _ , FPD _ , TCD _ (Current _ )
Detector Attenuation H _ , Amplifier or Range IQ->* _
Column: Liquid Phase . Solid Phase
Length fc/ O.D.
7/
I.D.
, Material S.S.
Temperature: Injector /Zo °.C, Oven jfo °C.t Detector AST& °C-.
Temperature Program
Sampling Method
SAMPLE RUN
fv%\. S.-S*
RT
Peak Height
Amount
Component
1-lc
,
Name of Operator
, Date s-
19 9f{
5-87
-------
RT
V • -"'^
;;.r-;T
", "— • '-5
A ' / '—
X 0>""
A ,~i -;
;' f- "?
c; « — ^.
^rea
jC-T-
\ r«u
I'tn4!
»*>"
"7 r
& ^
i .— —. —
5*7 2.
Peak Height
-
Amount (p^)
\
c .1
C? ,C"?
Component
~ y
'"• <^
5-1
-------
S7
rn > m 2. IS
t/>3COC/»HXTj33:o3C/>QC ™
-wflO'f-ssfrP.SO 3 ft
CO O
S
RUN 8 17
ESTD
RT
8.34
8.38
8.46
8.69
8.36
1.41
3.38
2.55
2.72
2.95
3.39
6.83
JIJM/18/81
AREA TYPE
2748 8V
9781 VV
12396 VV
24834 VV
17484 VV
26587 VB
196 D B8
1499 SB
865 D PB
1194 BV
1538 D VB
592 D SB
CflLI
1R
2R
3R
4R
5R
AWOUHT
2.549
3.442
9.eee
5.579
9.089
4.288
8.388
.
8.888
8. £87
8.888
TOTAL AREAs 98666
HUL FACTOR= 1.8888E+68
5-89
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client
, Location Tog,co
» Job No.
Injection Date fe-ifr-St . Time aar/?;^ » Instrument IDj
Recorder/Printout Reference No. \¥ . Recorder ID
Purpose of Run g, — °~~
*^t-^ v
.T!r"
,-j;-?
Area
/ -JTV
i£*i%
4 "> 1 0 '/
^*C^
/ -r ^,r^
^1^3
Peak Height
\
\
/
Amount (j>pM(
fc,6!
"S
N
/ "" "
S*-U
\
; '• '
Component
— i
-d.
^—"?
"~ V
Name of Operator
, Date *?«
19 Sri
5-90
-------
1.37
RUN I 18
ESTD
RT
8.32
8.33
8.45
8.68
8.95
1.37
JUN/18/81 £8=12-58
AREA TYPE
1888
5514
13188
34888
18656
27833
PV
VV
W
VV
VV
VB
CALi
1R
3R
4R
AMOUHT
9.9S5
8.888
4.651
5.582
13.908
4.291
TOTAL AREA=
&UL FACTOR=
93399
5-91
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client C/y\€f\
, Location Tog.co
, Job No. .3o-n«,02
Injection Date (p-\y-%( , Time ic: t?:'2.i. Instrument ID^o**0
Recorder/Printout Reference No.
Purpose of Run G./-C.fr H-vt
;-) , Recorder ID HP-STSOA
^«o**.jhiAJ *.«-.. v/^'ie
Sample Description p>-r~ (? -. p -- A;
GC CONDITIONS
Amount Injected ^.Orv\\_ , Inj. Port or Sample Loop Used £.c*v». Loot*
Detector Used: FID y , ECO
Detector Attenuation ^
Column: Liquid Phase
Length &' , O.D. V*"
, FPD , TCD (Current )
, Amplifier or Range lt>"~iv
, Solid Phase ^0e.fvPAi<- ^ ,
,1.0. , Material S.S.
Temperature: Injector /?o °C, Oven /5"o °C-, Detector AS~b °C_
Temperature Program ^ ^p~ H c I£/^A L
Sampling Method ^^^C> _S"oo
RT Area Peak He
. •? , ^ "i * L
,2;' >C3Z. N-,
, '4 .r" ~) i 1 ' ''
•^ ?/ «r
••\r~ in i, \-
i .-ri i ^-r I ;
SAMPLE RUN
ight Amount (j>p«^| Component
/ . — ^- j
— <.
*^ i>
^ ' -
> « — ; ^»
Name of Operator fA.b. o.»;i
, Date s-
19 fri
5-92
-------
RT
?.,-y-
'? f !
.}..»,
r-cc
Area
i'rr^
1 1~;:-0
* 1 1 1
-> v cr
i t <*>
Peak Height
\
\
(
-
Amount (pp,v)
/"
• 02
Component
V
• — • ^f
C (^
> Cfc
5-93
-------
RUN * 19 JUN/18/81 2e=32-22
ESTD
RT AREA TYPE ML* flUOUHT
8.21 1312 PB 1R 1.213
8.38 3832 PV 8.088
8.45 7373 W 2R 2.616
8.69 7114 VV 3R 1.649
9.35 2321 VB 8.088
1.43 9483 8V 4R 1.535
2.14 8558 VV 8.888
3.31 9376 VB 5R 1.267
5.80 1717 BB 8 808
3.63 748 PB 8.888
TOTflL ftREfi=
WJU FACTOR=
51626
1.9888E488
5-94
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client
, Location Tog.c.o
, Job No.
Injection Date fc-ty-Si . Time 2i'.cc}'...;£. » Instrument 1
Recorder/Printout Reference No. ^ ^ , Recorder ID
Purpose of Run Q, - C.^
AiAJA.UVg.l.C.
Sample Description _ ?
±*- A
GC CONDITIONS
Amount Injected a.Prwv. , Inj. Port or Sample Loop Used a.
Detector Used: FID y f ECD _ , FPD _ , TCD _ (Current _ )
Detector Attenuation H _ > Amplifier or Range ID."*11 _
Column: Liquid Phase _
Length &'
, Solid Phase
O.D.
, 1.0.
, Material S.S-
Temperature: Injector /go ^C, Oven /£""D °C., Detector
Temperature Program x SOT Hgl
Sampling Method
SAMPLE RUN
£"oo <*\\* &.S..
RT
>10
•?*1
*x 1
•N-t
»U-~v
Or
, '"^ *^J
\ * > '
H-.c-
Area
'^r2i?
s>v^
3^'tr
tcc^
A * <* ;i'
^ST"?
' O
Peak Height
\
/
v
/
Amount (£>p*4
5.2
\
\ o
/
; . v-
V
N r- c,
-* % (
/
f-^
Component
^^
..-•
'—
*— r^
r
T
y— •
^ u
Name of Operator CA.b.
, Date _5-
5-95
-------
„«
1.37'
ST
RUN i 20
ESTD
RT
9.29
8.37
9.46
9.69
9.95
1.37
4.99
JUH/18/81
AREA TYPE
BV
VV
VV
3346
8645
6858
2888
2537
9
VV
VB
BB
PB
CALi
2R
3R
4R
99=12
flKOUNT
9.999
1.187
9.989
1 484
9.889
8.40?
9.889
TOTAL flREA= 26989
HUL FACTOR= 1.9088E+89
5-96
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client Crv\<£(\
, Location To£co
, Job No.
Injection Date fe-yy-61 . Time ;3r.gy r>x » Instrument ]
Recorder/Printout Reference No. '^: -f- , Recorder ID
Purpose of Run Q, - c./. *^pgr^*rt>ea/o A>^Ai,v<-«g
Sample Description
f? ;•_<•*"-
Amount Injected
GC CONDITIONS
__, Inj. Port or Sample Loop Used a.o<*u Coej*
Detector Used: FID %_t ECD , FPD , TCD (Current )
Detector Attenuation H » Amplifier or Range "*u
Column: Liquid Phase , Solid Phase/
Length &' , O.D.
Temperature: Injector
Temperature Program _
, I.D.
}C, Oven
, Material S.S.
'o, Detector ;
Sampling Method
SAMPLE RUN
.Too CAV. &-S
RT
• ) •?
i < i e/r
4 ' '" '•'-
Area
32 ^2
rz-n
' ^^•^
Peak Height
Amount (£>pvj|
A'. (
o.Z
c.cl
Component
c,
-y-
,•- —
Name of Operator
, Date _5-f
19 Sf|
5-97
-------
-1 • • r-*C^
LIST' ZERO = 8, 8.8
*""" ~ 18
1.18
2.38
RUN « 24
JUN'18'81
ESTD
RT
9.18
f.18
2.38
TOTflU flREA=
NUL FACTOR=
ftREft TYPE CflL»
3219 0 PV
2283 VB 1R
1277 D 88
S58 PB
7437
1 .8888E+86
ftMOUHT
3.869
2.111
9.889
8.898
w S c/»
ar a
II
Hi
Q:
IT
>••
ll
;
b! 3
m
•~ ' - •
i *\ |(?
S 0 j>:
•U ' O O
I
3
1 i
: S* »
2\S
!T
.
3 : i
=o°o°;
5-98
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client Crv\<£(\
, Location To£c.o
, Job No.
Injection Date fe-\y-8( , Time 3.2'.r,r-r7» Instrument ]
Recorder/Printout Reference No. ^' Recorder ID
Purpose of Run Q, - c.^
Sample Description
GC CONDITIONS
Amount Injected 3.0rAU , Inj. Port or Sample Loop Used 3.3**^ Loofc
Detector Used: FID V . ECD , FPD , TCD (Current )
Detector Attenuation H » Amplifier or Range \is~"
Column: Liquid Phase
Length &' O.D.
, Solid Phase
, 1.0.
, Material
Temperature: Injector /Zo °C, Oven /jro °C, Detector
Temperature Program
Sampling Method
SAMPLE RUN
fv\v. &-S- goes
RT
• '-'.
3 ••> .^-~
Area
+ . -7
/- v
Peak Height
Amount (£>p*/}
2.c
— •
Component
"—t i
^> 's_ -^,
Name of Operator
, Date 1-
5-99
-------
frig
o o
II
**S|M
o 3 2« :
O :
V\l
f!
r- 33
•• !•(! •
X '• s" w *? :
P ** : _. a :
: xj 3"-^»— o D ^ :
~ f5 » :
£>i f i
*j» o i- :
»*>;•,: • j?-ffl
* S» W : o * S-
' : g ;N»
: « ; L
^S.-hj° : ? j T
n : »^ _ 3 : : • :\
L. '• r-3. 5 9 : 9 >-
V ': : : » = : » *P
ig-i
- =• :
3-
: r:
Id ':
o" o: :
O O : :
RUN * 25
JUH/13/81 22-85=57
ESTD
RT
8.82
9. £5
AREfl TYPE
2189 PB
174 0 PB
CAL*
1R
AMOUNT
2.924
9.880
TOTAL ARE«=
NUL FACTOR=
2363
5-100
-------
GAS CHROMATG. nPH OPERATING CONDITIONS AND FIELD LOG
Client e/v?£A _ * Location Tz?£cc?
, Job No.
Injection Date :>->7~^; « Time £'j:£2:c-V, Instrument ]
Recorder/Printout Reference No. 21 , Recorder ID
Purpose of Run cLAuA&«+Tiff~J
Sample Description
Amount Injected
GC CONDITIONS
p^i , Inj. Port or Sample Loop Used g.OinLl«oA
Detector Used: FID _£_, ECD , FPD , TCD (Current )
Detector Attenuation y.. , Amplifier or Range
Column: Liquid Phase , Solid Phase_
Length £,' , O.D.
"
, 1.0.
Temperature: Injector flo ^-, Oven —£
Temperature Program _
, Material 5.5.
'c., Detector 2?$
SAMPLE RUN
Sampling Method
/
RT *
i~.i ^~~
•M-3
• c-7
i * • «i
J - 1'^
1.^1
'/Area
t •-"
•7, i'-« 'i'*-
>.rfra
^3 ^.i
/j-^r
-? ^~ —
, , — -, ^
Peak Height
Amount £>e>^
\1.0
\o.2
/O.c,
lo. ST
»O.H-
10. \
Component
c,
C,
c^
C^
Cc-
Cfe,
Name of Operator M . ft
.. Date
5-101
-------
LIST: ZERO = 8, 8.
1.46
co
I
a>
: § ga|
i!!if fsr*
1 : 5 a o 2 33 :
>; S§$loi 2
H fblrH "
'• • • P 3 '• o 3"
c/>
•a
? ?
a.?
|
i^ii
•^ r» st
»;
=0:
3»5
ri
»
b
: a i p > i : S- : '
h Si o? i": » >3 !"•
N/ xJ 52. 3 • fii [<% • '
if S ff " • 5- a »,'
§ if!
Q Vioa :
-------
GAS CHROMATG. aPH OPERATING CONDITIONS AND FIELD LOG
Client C/V)£A Location TP&C.P
, Job No.
Injection Date L-- ri-/! . Time j*:,S~:.t$~ . Instrument
Recorder/Printout Reference No. '2, -; , Recorder ID H-ftg3
Purpose of Run
Sample Description
iA/i-A>/veA ' , O.D.
Temperature: Injector f Q D ^C, Oven /
Temperature Program
, Material
c.t Detector
Detector Used: FID y , ECO _ , FPD _ , TCD _ (Current _ )
Detector Attenuation _ vj,_ _ , Amplifier or Range >p-H _
.... ..... » Solid Phase
C> t
SAMPLE RUN
Sampling Method
RT
Peak Height
Amount
Component
n. o
^- — i
i ' /
. \
Name of Operator M .b
, Date
19S-/
5-103
-------
.
.72
1.46
3.23
7.8?
w o
en
H 00
fi 2. ^
O'^rc^f'ti<2»OQ>
-------
GAS CHROMATG, *PH OPERATING CONDITIONS AND FIELD LOG
Client e/v)g.A Location TPS.CO
, Job No.
Injection Date fc-.T--'; Time ,r\w-.;;-;. , Instrument IDj
Recorder/Printout Reference No. -;-, , Recorder ID
Purpose of Run
Sample Description
Mi'
GC CONDITIONS
Amount Injected 2.o ^i_ . Inj- Port or Sample Loop Used £
Detector Used: FID y , ECD , FPD , TCD (Current
Detector Attenuation <±. , Amplifier or Range
, Solid Phase
Column: Liquid Phase __
&' O.D.
, I.D.
, Material
Length & /
Temperature: Injector fQo °C, Oven / 57? °c,. Detector
Temperature Program
O ,
SAMPLE RUN
Sampling Method
RT
, / •*."
.'T L
' / '—
i * ^ ^ '
1. L-
—
^/Area
;~ C'i-.~~
^nc~
r5" 'J ^ -r
4/*' ^ "^
. — _- _ ^^ • -~~
Peak Height
Amount tpc^
n. o
\o-S
(0,^,
l«. ST
^o.H-
lO. \
Component
cf
c,
C^
C^
c^-
Cfa
Name of Operator M .h.
, Date °i-l
19
5-105
-------
1.4S
3.£9
w
IB 2
•"•• tj : oa "°
RUN t 29
ESTD
RT
8.25
8.42
8.72
1.46
3.23
JUH/19/81 19=27=17
AREA TYPE
17567 PV
28757 V8
45384
S7312
77845
SB
BB
BV
CftLt
1
3R
3R
4R
5R
.
19.315
18.547
19.745
18.583
TOTAL flREfl= 236798
«UL FrtCTOR= 1.0888E+88
5-106
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client
, Location Tos,<-o
, Job No.
Injection Date $,-Mi-8\ , Time ,• / ; 2 1 ""L. » Instrument ID^A^f*0
Recorder/Printout Reference No.
Purpose of Run G, - C.^ t+^t
lT/> * Recorder ID HPSS^OA
>^r>e-j^P C9AJ AfkJAt_V<-lC
Sample Description t,.,-r. r>
•^ C - A-
GC CONDITIONS
Amount Injected ^.OPAV. , Inj. Port or Sample Loop Used 2.c**i. Cool*
Detector Used: FID y , ECD
Detector Attenuation ^
Column: Liquid Phase
Length &' , O.D. (/s- "
, FPD , TCD (Current )
, Amplifier or Range ID~1V
, Solid Phase ypft.f\pftjc_ O »
, I.D. , Material S.S.
Temperature: Injector /Zo C, Oven /jr"o C-, Detector AS^> C-
Temperature Program xsofHe ^A^^*^
SAMPLE RUN
Sampling Method £>£A.>V i" "7 /'
'"" ^ S-~*' ^
/ w fit
' 1 r F'7 t
ight Amount (,pp^ Component
c ,
N .
-
C.| C-:
c . tj_ .
Name of Operator m.b. c.^i
, Date 5-
19 9f|
5-107
-------
HID
"3": 3~: = =°
!• : a- oo:
? : ? O O :
RUN * 38
JUH/13/31 ll'-24<02
ESTD
RT
9.22
8 33
9.46
8.79
8.96
AREA TYPE CALt
1194
738
2459
479
596
PV
VV
VB
B8
BB
1
ZK
3R
ftMOUHT
t.151
9.265
0.809
6.112
TOTAL AREA= 5466
MUL FACTOR= 1.0000E+99
5-108
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client
, Location To£co
, Job No.
SA*£<8.S.*.'fXt>,C,K
Injection Date fe-i--6| , Time //•. •?;.. T; , Instrument lD^s££**
Recorder/Printout Reference No.
Purpose of Run C, - C.^ n~*t
'J.\ , Recorder ID Hf»22SoA
>Pr,P,.rf>*B/0 AWALVLfl-""*v
, Solid Phase YJP^P^PAIC. fo »
, I.D. , Material S.S-
Temperature: Injector /So °C, Oven /5^o °C., Detector AS~t> °C-
Temperature Program j;^YHIfif?1'w\^L
SAMPLE RUN
Sampling Method £»£A.£ . .Too -.L U-LZ
' s <&!&(*,
.r'i T^v
Name of Operator fv\.^>. o.^i^S
ight Amount (£>f>A/i Component
; . / c,
\
; , • ;' ^i.
, Date ^-» 19 2r|
5-109
-------
LIST- ATT 2t = 9
ATT 2t - £ 8
LIST' flTT 2t = -8
f
> m > S ,„ _ £• 5
S*»H53sBi2?i 3
?§ I 29-5 11-1 &i §
r" w 3 3 o B 23 : _ o = z :_
: 2 °1 * o= ?? 3-* o =<
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• ?"£.?: 5" :l
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RUN I 31
ESTO
RT
3.22
8.38
8.47
JUH/19/81 11=36:81
TYPE CftLt
1228 PV 1
666 VV ER
4480 VB
ffllOUNT
1.176
8.239
8.860
TOTflL flREft=
NUL FflCTOR=
6366
5-110
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client
, Location To£c.o
, Job No. Jo-K«03
SA*ewcub,c.*
Injection Date fe- ' Sj , Time /2.'i7:C:T" > Instrument lOs^f**0
Recorder/Printout Reference No.
Purpose of Run G, - Ct H-*I
'~? , Recorder ID Hf>2S^oA
^ ^^ «
Sample Description , ,r~ P:V f-./i
GC CONDITIONS
Amount Injected ^.Orv\v_ , Inj. Port or Sample Loop Used 2.01***. Loofr
Detector Used: FID X , ECD
Detector Attenuation ^f
Column: Liquid Phase
Length &' , O.D. y& "
, FPD , TCD (Current )
, Amplifier or Range 10""^
, Solid Phase YP^P^PAIC. O >
, I.D. , Material S.S.
Temperature: Injector /?o °C, Oven /^To °O, Detector AS"t> °CL,
Temperature Program x^oT^f te^Mvt-
SAMPLE RUN
Sampling Method ^^^^S . ^"oo >"~r
-i^ ^y^
ight Amount (^p*/) Component
/•/ C,
,
-,
0. i -s- M_
, Date ^-/ 19 Sr?
5-111
-------
.47
RUH t 32
JUN/19'81
o
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S^ngiH
B) -
3 •
=• o o:
? O O :
ESTD
RT
8. 22
8.37
8.47
9 96
AREA TYPE CftL»
I228 py 1
688 VP 2R
3754 Pl
665 BB
1.178
8-244
I'm
8. see
TOTAL flREA= 6319
«UL FftCTOR= 1.0888E+88
5-U2
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client CfY\<~(\
, Location
, Job No. Jo "1(^02.Si
Injection Date fe>- -fit t Time /K^VX , Instrument ]
Recorder/Printout Reference No. _y , Recorder ID
Purpose of Run g, - c.*.
A.WA.
Sample Description
Amount Injected
GC CONDITIONS
_, Inj. Port or Sample Loop Used £.
(Current
Loot*
Detector Used: FID y . ECD , FPD , TCD
Detector Attenuation H » Amplifier or Range ip—n
, Solid Phase"
Column: Liquid Phase __
Length &' , O.D.
Temperature: Inject
Temperature Program
, I.D.
, Material S.S.
Temperature: Injector /3o °C, Oven _/s~o_ °C.t Detector
(
Sampling Method
SAMPLE RUN
. .Too r*\v. S-S- (Iocs
RT
\ ^
•VW
Area
JVT.C,
rn,.
Peak Height
Amount (fp/^
f • J>
CVJ
Component
c,
C.^
Name of Operator
.Date -
19 2f|
5-113
-------
ST
£ rn
£!»S?3$
fS3|3t
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WOC™
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RUN I 33 JUH/19/81 14=£€=42
MO CflLIB PEflKS FOUND
RT
a.as
8.46
TYPE
1489 PV 0.854
5996 VV 6.112
Si. 669
73.348
TOTftL AREA= 6585
NUL FftCTOR= 1.8888E488
5-114
-------
GAS CHROMATOGRAPH OPERATING CONDITIONS AND FIELD LOG
Client CA-^
, Location 7^c.j
, Job No. jc i
Injection Date c? -\ - .<; , Time r-r\". *_*&*•*, A.V*_•*<_:<
Sample Description ./-f^r
Amount Injected ^.r
GC CONDITIONS
, Inj. Port or Sample Loop Used ^.q
, Solid Phase Yb'S
Detector Used: FID X , ECD _ , FPD _ , TCD _ (Current _ )
Detector Attenuation H _ , Amplifier or Range it). ""'.'' _
Column: Liquid Phase _
Length ^'
, O.D. V*- " I.D.
, Material
Temperature: Injector / lo °C, Oven / r o ° O, Detector AST's
Temperature Program TISrT -^gr^V
Sampling Method
SAMPLE RUN
T3 c r>\ u s •> • .-? c i
RT
Area
Peak Height
Amount
Component
Name of Operator
, Date -,-
19
5-115
-------
ST
w S w w
l?s g
S fi s» §
Si i 5
i?!
y>-
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2
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flip
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5"
M_
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RUN t 34
HO CALIB PEAKS FOUND
JUN/19/81 14'39'-89
RT
9.22
8.33
H. 46
AREA TYPE AR/HT AREA*
1181 PV 9.944 £6.469
331 VB 9.966 7.955
2789 PB 9.978 65.585
TOTAL AREA* 4161
NUL FACTOR= 1.9990E408
5-116
-------
GAS CHROMATGv .-vPH OPERATING CONDITIONS AND FIELD LOG
Client e/Mg.A . Location TP&C.P
, Job No.
Injection Date L.-'.V^ , Time
Recorder/Printout Reference No.
Purpose of Run eLAufi.&t+T«r»J
_, Instrument ID
, Recorder ID H
Sample Description
GC CONDITIONS
Amount Injected y.p Mi Inj. Port or Sample Loop Used ^
Detector Used: FID _£__, ECD , FPD , TCD (Current
Detector Attenuation J^. , Amplifier or Range
Column: Liquid Phase , Solid Phase
Length & ' . O.D.
"
_, I.D. _
Temperature: Injector rlo °C_, Oven _j_
Temperature Program
, Material
'c-, Detector
SAMPLE RUN
Sampling Method
RT
Area
Peak Height
Amount
Component
i '-r ~i
10. \
Cfe,
Name of Operator
, Date
19 fiV
5-117
-------
C, -
4.25
7.37
w
w 2 w
l?s
ir
: .; rijl
p: | »| S
* i ™ f P «
?z : o 1C
^ny-:
4f"f*5 JS5
^ 3"ir 03" -w:
iv||:^*^:
* • ir 3 •**:
RUN *
JUN'19/Sl 16=4£=1!
RT
9.26
8.41
9.71
1.45
3.38
4.25
7.37
AREA TYPE
19934 D PV
29949 0 VV
49994 D VV
73116 VB
39746 BV
6241 V8
38727 BB
AR/HT
9.835
9.975
9.896
9.184
9.499
9.722
9.939
5.488
3.535
14.139
21.982
23.282
1.399
25.583
TOTAL AREA= 346829
HDL FACTOR= 1.8999E+99
5-118
-------
GAS CHROMATOo..APH OPERATING CONDITIONS AND FIELD LOG
Client
, Location
No.
Injection Date L--."^-^\ » Time \~i\ r'. t •'•' * Instrument ID
Recorder/Printout Reference No. ,° , Recorder ID
Purpose of Run G.,-o H./
Sample Description
GC CONDITIONS
Amount Injected 2.Dn/\£L_ . Inj. Port or Sample Loop Used ^.
Detector Used: FID x . ECD _ , FPD _ , TCD _ (Current _ )
Detector Attenuation H. _ , Amplifier or Range lE>"n _
, Solid Phase
Column: Liquid Phase
Len9th <-' °-D- Y*" » J-0'
Temperature: Injector /^Q __€-, Oven _
Temperature Program ^TSi
D
, Material S.S..
t Detector
Sampling Method
SAMPLE RUN
. Srr?o iv\l s.S . 6ov.C
RT
• '^•3
• v» ~
• "/ ^
Area
i^-f-i
3-r^
Peak Height
Amount (pp
'—-'-•—
Name of Operator
, Date
5-U9
-------
R
33 :
nge
ncn
*t\\l\!
°\ r
=• a i '
'£. g 2
Z. '• S-: = "• a : : ™
f 11; I? iio-oi"
= : a I =00;
ScE!
•ft*
RIJH t 3
HO CALIB PEAKS FOUND
JUH/19/81 17=14=88
AREA*
RT
8.33
8 47
8.%
AREfl TYPE flR/HT
1649 PV 9.881
865S VV 8.163
1618 VB 8.184
13 S49
7S.S48
13.512
TOTAt AREA* 11915
MUL FACTOR= 1.8888E+88
5-120
-------
GAS CHROMATG*..APH OPERATING CONDITIONS AND FIELD LOG
Client
, Location TOSC.Q
No.
Injection Date l-.-.V^ . Time .~;-.^i;-.'. .1 . Instrument ID
Recorder/Printout Reference No. V, , Recorder ID
Purpose of Run
— C.
/
i v
Sample Description
Amount Injected 2.D
GC CONDITIONS
» Inj. Port or Sample Loop Used ^.
Detector Used: FID x , ECD _ , FPD _ , TCD _ (Current
Detector Attenuation ty. _ , Amplifier or Range \
Column: Liquid Phase __
Len9th £./
, Solid Phase
D
O.D.
"
t I.D.
, Material
Temperature: Injector /3o 0<^. Oven /S"D °^. Detector
Temperature Program l
Sampling Method
SAMPLE RUN
STDO i^L S>S .
RT
1 **^
• ' ^
'~~i •"
Area
x-^-
,'W- T-
'-'SV,'
/ - -7
Peak Height
Amount (pp
-------
ftTT 2t - 3 8
LIST: 2ERO = 9, 9.8
.47
ST
SA
o
m
c« 3 v> & =J
l?s a..
^rii
*": 2 m ?
gi P
RIJH t 4
NO CflLIB PEflKS FOUND
JUH/19/31 17=36=12
AREA*
PT
8.23
8.47
8.96
AREA TYPE flR/HT AREAX
764 PV 8.859 7.698
8548 VB 8.144 96.126
613 PB 8.106 6.176
TOTAL AREA= 9925
«UL FACTOR= i.eeeee+ea
5-122
-------
GAS CHROMATC. .^PH OPERATING CONDITIONS AND FIELD LOG
Client -:I."-,<'",£.- Ji , c:-,
Injection Date <.-•- -•'. . Time ••^~2':.i^ , Instrument ID
Recorder/Printout Reference No. i
Purpose of Run c.^L^^.-*-.^
, Recorder ID
Sample Description
GC CONDITIONS
Amount Injected ?.? f., , Inj. Port or Sample Loop Used Q.O^ _ _^A
Detector Used: FID x. . ECD , FPD , TCD (Current )
Detector Attenuation v- , Amplifier or Range ;c-'»'-
Column: Liquid Phase
Length _J^_
, Solid Phase £•-*• L
, O.D. '/,-. " I.D.
, Material
Temperature: Injector /
Temperature Program ^ .
-, Oven / 5.1? ° ~ , Detector o rr °c
SAMPLE RUN
Sampling Method
RT
• ,\ I*.
'~T •'-*
." '>^
, • -r »
*7 -,-,
'"/. '''i
^/Area
, "~- "^
\ t \ • *~* ^
3.*^
•J.'2'il
i. *?.T^
i • 7 r? -'
i. iV22.
Peak Height
Amount tpfOv
\1.D
\c.$
(C.(0
te.Z
IC.'-r-
. 1"^
\ — '• i
Component
C:
c?
C,-?
,-'-•
C r-
"""•^ 'cT
Name of Operator f\.}. ^ . c^
, Date
19 ::
5-123
-------
LIST; ZERO = 8, 8.8
- c o
g !3 O : o • '.
3 en > • rr :
• •• *j» : '~**.
STOP
RUN «
MEM
RT
9.25
8.41
0.71
1.45
3.28
4.29
JUN/19/81 16 81=18
flREfl TYPE
18155 BV
88629 V8
44871
66644
79336
5653
BB
PB
BV
VB
AR/HT
8.859
9.849
9.871
8.162
9.394
9.725
ARES*
7 463
11.768
18.444
27.393
32.619
2.324
TOTHL AREA=
MIL FACTOR=
243299
5-124
-------
GAS CHROMATQu..APH OPERATING CONDITIONS AND FIELD LOG
Client
, Location TOSC.O
No.
Injection Date 6-n-j-j . Time iy':;1v?Z. , Instrument ID
Recorder/Printout Reference No. ^ , Recorder ID
Purpose of Run £L.-C/ w./t>/z.pi
Sample Description
GC CONDITIONS
Amount Injected 2.D r»Sl . Inj. Port or Sample Loop Used
Detector Used: FID x . ECD _ , FPD _ , TCD _ (Current
Detector Attenuation t^. _ , Amplifier or Range )b"u
Column: Liquid Phase
Len9th 6. /
, Solid Phase
6. / O.D. V*" . . I.D.
Temperature: Injector /3O 0<^> Oven
Temperature Program I
, Material S.S.
, Detector
SAMPLE RUN
Sampling Method
RT
* -i '-
* / ^^
Area
, ~ 2. :-:
*& i *£>
Peak Height
Amount (pp
-------
RUN *
ESTD
RT
0.32
a.75
W O O H g g
SwcnHx-oajjoSwoe-j
-g(Dorni
-------
GAS CHROMATOo:,APH OPERATING CONDITIONS AND FIELD LOG
Client
, Location TOSC.Q
No.
Injection Date £»-,.-'1 -\\ , Time K :2 ;-.^") . Instrument ID ^^
Recorder/Printout Reference No. .7 > Recorder ID
Purpose of Run £.,-O H./t>/2.pg
~- ' /^••"'•"^•^^""••^^•^'•""•'•'•"•^
,0^0
i 5
Sample Description
GC CONDITIONS
, Inj. Port or Sample Loop Used ^.
Amount Injected g.;
Detector Used: FID x . ECD , FPD , TCD (Current
Detector Attenuation ty. , Amplifier or Range )b~*_V.
Column: Liquid Phase , Solid Phase_
Length 6. / O.D.
D
" , I.D.
, Material S.£.
Temperature: Injector I2.Q 0<^-t Oven /5T> °^, Detector
Temperature Program 2T.S^
Sampling Method
SAMPLE RUN
'--• ^C=x<£^_ ^2_
~~r~™~ X^^ : :
RT
• '2.2.
Area
Ivt-l
Peak Height
Amount (p&^\
/• "3>
Component
c.
Name of Operator
, Date
19%*!
5-127
-------
ha*
ST
OH
$9
u>
p? S
fc&; «
i^. • w
r'A!
s
W :
8 i
J>o;
N i
• b 3"
: < 5"
: :
: O : :_r a
i ft • ^>: %
Z*i.
O 3
J=--21 '
•t' • 2, 3 ^ .'
: • a s. •
r- IB :
: 3-
if*
it
RUN t 3 JUN/19/81 18^31=4?
HO CflLIB PEAKS FOUND
RT
a.22
TYPE ftR/HT
1441 PB 8.852
TOTflL flREfl= 1441
NUL FACTOR= 1.8888E+98
5-128
-------
5.9 RADIOMETRIC ANALYSIS RESULTS
5-129
-------
SAFETY SPECIALISTS, Inc.
3194 De La Cruz Blvd., Suite 15 • Santa Clara, California 95050 • Telephone (408) 988-1111
ASSAY REPORT
Acurex Corporation
485 Clyde Avenue
Attn: Ms. Linda Bohannon, M/S 0-1212
Mountain View, California 94042
Date: December 28, 1981
Date Samples Received: 11/11/81
Customer Order No. RB59185A, Rel. 20
Activity1*
SSI No. Client Description
81388A #1, A81-07-011-038, TOSCO 2 Filter
B #2, A81-07-011-545, TOSCO 1 Filter
C #3, A81-07-011-571, TOSCO Filter
Blank
Gross Beta
pCi/Filter
60.6 ± 7.8
75.0 ± 11.3
99.6 ± 13.6
Gross Gamma
pCi/Filter
< 143
< 143
< 142
SSI No. Client Description
81388A No. 1, A81-07-011-38, TOSCO 2 Filter
B No. 2, A81-07-011-545, TOSCO 1 Filter
C No. 3, A81-07-011-571, TOSCO Filter
Blank
Gross Alpha
pCi/liter
15 ± 12
1 18
< 19
-<* ?.'./* flfatrs/
Analyst: Fariba DariesT
Approved:«K C. Noble, Director
Safety & Health Services Division
*The ± values are the two sigma Poisson standard deviation of the counting
error. 3
The < values are equal to or less than three sigma of the counting error.
5-130
-------
5.10 BIOASSAY REPORTS
5-131
-------
GENETICS ASSAY NOS. 6153-6156
LBI SAFETY NOS. 7535-7538
MUTAGENICITY EVALUATION OF
XAD RESIN EXTRACTS
IN~THE
EPA~LEVEL 1
AMES SALMONETLA7MICROSOME
"PLATE TEST
FINAL REPORT
SUBMITTED TO:
ACUREX CORPORATION
485 CLYDE AVENUE
MOUNTAIN VIEW, CALIFORNIA 94042
SUBMITTED BY:
LITTON BIONETICS, INC.
5516 NICHOLSON LANE
KENSINGTON, MARYLAND 20895
LBI PROJECT NO. 22064
REPORT DATE: MARCH 1982
BIONETICS 5-132
Litton
-------
PREFACE
This assay conforms to the standard EPA Level 1 procedure for the
Ames Salmonella/microsome mutagenesis assay as described in "IERL-RTP Proce-
dures Manual: Level 1 Environmental Assessment Biological Tests"1. The
data were evaluated and formatted as recommended in "Level 1 Biological
Testing Assessment and Data Formatting"2.
The Ames Salmonel1 a/mi crosome mutagenesis assay has been shown to be
a sensitive method for detecting mutagenic activity for a variety of chemi-
cals representing various chemical classes3. This assay is one of several
recommended by EPA to identify, categorize and rank the pollutant potential
of influent and effluent streams from industrial and energy-producing pro-
cesses. This assay has been well validated with a wide range of positive
and negative control chemicals and complex environmental samples.
All procedures and documents pertaining to the receipt, storage,
preparation, testing and evaluation of the test material shall conform to.-r
Litton Bionetics, Inc. standard operating procedures, the U.S. Food and
Drug Administration's Good Laboratory Practices Regulations of 19794 and
the proposed U.S. Environmental Protection Agency's Good Laboratory
Practice Guidelines5'6. Deviations from standard procedure shall be
fully documented and noted in the report.
All test and control results in this report are supported by fully
documented raw data which are permanently maintained in the files of the
Department of Molecular Toxicology or in the archives of Litton Bionetics,
Inc., 5516 Nicholson Lane, Kensington, Maryland 20895. Copies of raw
data will be supplied to the sponsor upon request.
5-133
._ BIONETICS
utton
-------
TABLE OF CONTENTS
Page No.
PREFACE ""
I. SUMMARY l
II. OBJECTIVE -._•_.• • • 2
III. TEST MATERIAL • 3
A. Description ~
8. Handling and Preparation 3
IV. MATERIALS
5
Litton
A. Indicator Microorganisms ._ 5
B. Media 6
C. Activation System . 6
I. S9 Homogenate 6
2. S9 Mix 6
V. EXPERIMENTAL DESIGN 7
A. Dose Selection ." 7
B. Mutagenicity Test 7
1. Nonactivation Assay 7~
2. Activation Assay 8
C. Control Compounds 8
D. Recording and Presenting Data 10
VI. RESULTS 11
A. Interpretations 11
1. TOSCO 2 XAD + OMC 11
2. TOSCO 1 XAD 12
3. MOHAWK 1 XAD 12
4. MOHAWK 2 XAD 13
B. Tables 14
VII. ASSAY ACCEPTANCE AND EVALUATION CRITERIA 27
A. Surviving Populations 27
B. Dose-Response Phenomena 28
C. Control Tests 28
D. Evaluation Criteria for Ames Assay 28
1. Strains TA-1535 and TA-1537 29
2. Strains TA-98 and TA-100 29
3. Pattern 29
4. Reproducibility 29
E. Relation Between Mutagenicity and
Carcinogenicity 30
F. Criteria for Ranking Samples in the Ames Assay . . 30
VIII. REFERENCES 32
BIONETICS 5_134 i
-------
I. SUMMARY
Four resin extract samples supplied by Acurex Corporation were tested
and evaluated for their mutagenic activities in the EPA Level 1 Ames
Sal monell a/mi crosome mutagenesis assay. The samples, supplied in methylene
chloride, were solvent exchanged to 2.0 ml of dimethyl sulf oxide (DMSO)
prior to testing. The samples were identified as TOSCO 2 XAD + OMC (A81-
07-011-562,559), TOSCO 1 XAD (A81-07-011-569), MOHAWK 1 XAD (A81-09-007:488)
and MOHAWK 2 XAD (A81-09-007-495).
In order to preserve the maximum quantity of test material, it was
decided to test each sample in only two strains, TA-98 and TA-100 using
a single plate per dose. Tests were conducted in duplicate both with
and without S9 metabolic activation mix. Even with these modifications,
it was impossible to reach the Maximum Applicable Dose (MAD) for the Ames
assay which is 5000 ug/plate. In the Mohawk 2 XAD sample no activity
was observed in the highest dose, but based on the limited organic content,
a Non Detectable classification could not be assigned. The sample was
ranked as having undetermined mutagenicity, but moderate or less. The
TOSCO 2 XAD sample was the most mutagenic with a Minimum Effective Concen-
tration (MEC) of 30 ug/plate, placing the sample in the high mutagenicity
category. Mohawk 1 XAD and TOSCO 1 XAD, were the next most active samples
with MEC values of 75 ug/plate (moderate mutagenicity) and 85 ug/plate
(moderate mutagenicity), respectively.
Insufficient quantities of test material prevented standard Level 1
Ames testing of the four samples. While three of the samples were found
to be mutagenic and were ranked by EPA Level 1 evaluation criteria the
MEC of those samples should be viewed with some caution. Adequate retest
ing was not possible to confirm the accuracy of the reported MEC values.
Submitted by:
Reviewed by:
tbdy Director
nthia Rabenold, B.S.
Submammalian Genetics,
Department of Molecular
Toxicology
Date
_
David J. Brusicl .
Director,
Department of Molecular
Toxicology
, _
Utton
BIONETICS
5-135
-------
II. OBJECTIVE
The objective of this study was to determine and rank the genetic
activity of four XAD resin extract samples in the EPA Level 1 Ames Sal-
monella mutagenesis assay with and without the addition of mammalian
metabolic activation preparations. The samples were solvent exchanged
into dimethylsulfoxide (DMSO) before Ames testing was initiated. The
genetic activity of each sample was measured in these assays by its
ability to revert the Salmonella indicator strains from histidine
dependence to histidine independence. The degree of genetic activity of
a sample was reflected in the number of revertants that were observed on
the histidine-free medium. Standard EPA Level 1 mutagenicity evaluation
criteria for the Ames mutagenesis assay were used to rank the mutagenic
potential of each test material.
LLJ BIONETICS
Litton
-------
HI. TEST MATERIAL
A. Description
Four samples were supplied by Acurex Corporation, Mountain View,
California. The samples were assigned LBI safety numbers and LBI assay
numbers upon receipt. The Acurex code numbers, sample identification,
LBI safety numbers and LBI assay numbers are identified below. All labora:
tory documentation used the LBI assay number to identify samples.
The four test materials were received as clear, yellow solutions of
organic material in methylene chloride except for the TOSCO 1 XAO sample.
That sample was an amber-colored, clear solution with a few suspended
particles. The quantity of organic material in each sample, as determined
by Acurex Corporation, is identified below. No information on sampling
parameters (such as the equivalent volume of stack gas represented by
the sample) was provided.
Sample Quantity LBI LBI
Acurex Corp. Code Identification (mg organic) Safety No. Assay No.
A81-Q7-011-562, 559 TOSCO 2 XAD + OMC 12 7537 6153
A81-07-011-569 TOSCO 1 XAD 17 7538 6154
A81-09-007-488 MOHAWK 1 XAD 6 7535 6155
A81-09-007-495 MOHAWK 2 XAD 4 7536 6156
B. Handling and Preparation
The test materials were received at LBI on February 8, 1982. The
samples were shipped in small, clear-glass vials sealed with crimp-top
aluminum caps with rubber liners. The samples were received intact and
were stored at +4°C in the dark until processed.
5-137
_ BIONETICS
Litton
-------
Pretest sample preparation consisted of solvent exchanging the samples
into dimethysulfoxide (DMSO). The samples were transferred with methylene
chloride rinses into graduated conical tubes. The methyl chloride was
gradually evaporated (50°C under a stream of nitrogen) and DMSO was
sequentially added. The samples were brought to volume in 2.0 ml of
DMSO. The samples were transferred to glass vials and sealed with teflon-
coated rubber rounds. The solvent exchanged samples were stored at
+4°C in the dark.
LJu BIONETICS 5-138
Litton
-------
IV.
MATERIALS
A.
Indicator Microorganisms
The Salmonella typhimurium strains used in this assay were obtained
from Dr. Bruce Ames, University of California at Berkeley7-12. The following
four strains were used.
Strai n
Designation
TA-1535
TA-1537
TA-98
TA-100
Gene
Affected
Ms G
his C
his D
his G
Additional Mutations
Repai r
A uvr B
A uvr B
A uvr B
A uvr B
IPS R Factor
rfa -
rfa
rfa pKMlOl
rfa pKMlOl
Mutation Type
Detected
Base-pair
substitution
Frameshift
Frames hi ft
Base-pair
substitution
All the above strains have, in addition to the mutation in the histi-
dine operon, mutation (rfa-) that leads to defective lipopolysaccharide coat,
a deletion that covers genes involved in the synthesis of vitamin biotin
(bio-) and in the repair of ultraviolet (uv) - induced DNA damage (uvrB-).
The rfa- mutation makes the strains more permeable to many large molecules.
The uvrB- mutation decreases repair of some types of chemically or physi-
cally damaged DNA and thereby enhances the strain's sensitivity to some
mutagenic agents. The resistant transfer factor plasmid (R factor) pKMlOl
in TA-98 and TA-100 is believed to cause an increase in error-prone DNA
repair that leads to many more mutations for a given dose of most mutagens11
In addition, plasmid pKMlOl confers resistance to the antibiotic ampi-
cillin, which is a convenient marker to detect the presence of plasmid
in the cells.
All indicator strains were kept at 4°C on minimal medium plates sup-
plemented with a trace of biotin and an excess of histidine. In addition,
the plates with plasmid-carrying strains contained ampicillin (25 ug/ml) to
Utton
B10NETICS
5-139
-------
ensure stable maintenance of plasmid pKMlOl. New stock culture plates
were made as often as necessary from the frozen master cultures or from
single colony reisolates that were checked for their genotypic charac-
teristics (his, rfa, uvrB, and bio) and for the presence of plasmid.
For each experiment, an inoculum from the stock culture plates was grown
overnight at 37°C in nutrient broth (Oxoid CM67) and used.
B. Media
The bacterial strains were cultured in Oxoid Media #2 (Nutrient Broth).
The selective medium was Vogen _Bonner Medium E with 2 percent glucose13.
The overlay agar consisted of 0.6 percent purified agar with 0.05 mM
histidine, 0.05 mM biotin and 0.1M NaCl according to the methods of Ames
et al_12.
C. Activation System
1. S9 Homogenate
A 9,000 x 2 supernatant prepared from Sprague-Dawley adult male rat
liver induced by Aroclor 1254 (Ames et al_.12) was purchased commercially
and used in these assays.
2. 59 Mix
S9 mix used in these assays consisted of the following components:
Concentration per Milliliter
Components S9 Mix
NADP (sodium salt) 4 umoles
D-glucose-6-phosphate 5 umoles
MgCl2 8 umoles
KC1 33 umoles
Sodium phosphate buffer
pH 7.4 100 umoles
Organ homogenate from rat
liver (S9 fraction) 100 uliters
CB B.ONET.CS
Litton
-------
,_ BIONETICS
utton
V. EXPERIMENTAL DESIGN
A. Dosage Selection
Test strategy and dose selection depend upon sample type and sample
availability. The Level 1 manual1 recommends solids to be initially
tested at the maximum applicable dose (MAO) of 5 mg per plate and at lower
concentrations of 2.5, 1, 0.5, 0.1 and 0.05 mg per plate. Liquids are
tested initially at the MAD of 200 ul per plate, and at lower concentra-
tions of 100, 50 and 10 ul per plate. Samples are retested over a narrower
range of concentrations with strains showing positive results initially-
Alternate doses are employed if sample size is limiting or at the direction
of the sponsor.
Because sample size was limiting, a preliminary test was performed
with strain TA-98, both with and without S9 metabolic activation, at 10 ul
per plate for each sample. Doses selected for the second trial with each
sample were either 1, 5, 10 and 50 ul per plate for TOSCO 2 XAD + OMC or
1, 10, 25 and 50 ul per plate for the other three samples. The third
trial used 50 ul per plate and, in some cases, also included 25 and 75 ul
per plate.
B. Mutagenicity Testing
The procedure used was based on the paper published by Ames et. a]_.12
and was performed as follows:
1. Nonactivation Assay
To a sterile 13 x 100 mm test tube placed in a 43°C water bath the
following was added in order:
2.00 ml of 0.6 percent agar containing 0.05 mM histidine
and 0.05 mM biotin.
Aliquot of test sample to give the appropriate dose.
5-141
-------
0.1 ml to 0.2 ml of indicator organism(s).
0.50 ml of 0.2M phosphate buffer, pH 7.4.
This mixture was swirled gently and then poured onto minimal agar
plates (see IV B, Media). After the top agar had set, the plates were
incubated at 37°C for approximately 2 days. The number of h1s+ revertant
colonies growing on the plates were counted with an automatic colony
counter and recorded.
2. Activation Assay
The activation assay was run concurrently with the nonactivation assay.
The only difference was the addition of 0.5 ml of S9 mix (see IV C, Acti-
vation System) to the tubes in place of 0.5 ml of phosphate buffer which
was added in nonactivation assays. All other details were similar to
the procedure for nonactivation assays.
A detailed flow diagram for the plate incorporation assay is pro-
vided in Figure 1.
C. Control Compounds
A negative control consisting of the solvent used for the test material
was also assayed concurrently with the test material. For negative con-
trols, step 'b1 of Nonactivation Assays was replaced by 0.05 ml of the
solvent. The negative controls were employed for each indicator strain
and were performed in the absence and presence of S9 mix. The solvent
used to prepare the stock solution of the test material is given in the
Results section of this report. All dilutions of the test material were
made using this solvent. The amount of solvent used was equal to the
maximum volume used to give the appropriate test dose.
LU BIONETICS 5'142
Litton
-------
AMES ASSAY [PLATE INCORPORATION METHOD]
Molten [43°C to 45°C] overlay agar
appropriately supplemented
0.01 ml to 0.2 ml Test, positive or solvent
control chemical
0.1 ml
Aliquot of an overnight culture
of bacteria [1Q.9 cells/mi]
Aliquot of
buffer ~"S"
9 +S-
0.5 ml S-9 mix [hepatic
• homogenate from PCB
pretreated rat plus
necessary cofactorsj
Overlay poured on selective
bottom agar medium
Plates incubated at 37°C
for approximately 2 days
The numbers of revertants/plate counted
Data analyzed
Interpretation /Conclusion
Figure 1 AMES SALMONELLAIM 1CROSOME MUTAGENESIS ASSAY
5-143 9
-------
Specific positive control compounds known to revert each strain were
also used and assayed concurrently with the test material. The concentra-
tions and specificities of these compounds to specific strains are given in
the following table:
Assay
Nonactivation
Activation
Chemical
Sodium azide
2-Nitrofluorene
(NF)
9-aminoacridine-
(9AA)
2-anthramine
(ANTH)
Concentratio
per plate
Solvent (ug)
Water
D i methyl -
sulf oxide
Ethanol
D i methyl -
sulf oxide
10.0
10.0
50.0
2.5
rr"
Salmonel
Strains
TA-1535,
TA-98
TA-1537
For all
la
TA-100
strains
D.
Recording and Presenting Data
The number of colonies on each plate were counted and recorded on
printed forms. These raw data were analyzed in a computer program and
reported on a printout. The results are presented as revertants per
plate for each indicator strain employed in the assay. The positive and
solvent controls are provided as reference points.
m
Utton
BIONETICS
5-144
10
-------
VI. RESULTS
A. Interpretation
With the limited amount of each sample received, the size of each
Ames test was reduced to two strains, TA-98 and TA-100. A preliminary
range-finding trial was performed with each sample (Trial 1 for each
sample) using the single dose of 10 ul/plate in strain TA-98. The results
from this single data point were used to select an appropriate dose range
for testing. This modified test strategy helped somewhat to conserve
limited test material. Even with this step, the amount of sample was
not sufficient to produce reproducible MEC value. The MEC values calcu-
lated for this study used the best data available from each series of
tests.
The results of the assays showed that three of the four samples
were mutagenic in either one strain or both. The most mutagenic sample
on a per-weight basis was TOSCO 2 XAD (MEC of 30 ug/plate) followed by
Mohawk 1 XAD (MEC of 75 ug/plate) and TOSCO 1 XAD (MEC of 85 ug/plate)
Mohawk 2 XAD was not mutagenic under the test conditions employed up to
a level of 100 ug organics per plate.
1. TOSCO 2 XAD + OMC
The primary stock of the sample was prepared at 6 ug organics per
ul DMSO. The test material was evaluated in Salmonella strains TA-98
and TA-100 both with and without S9 metabolic activation mix. The dose
range used in Trial 2 was 1, 5, 10 and 50 ul per plate. The test sample
was positive in TA-98 and marginally positive in TA-100 and appeared to
be slightly more active without S9 mix. The sample was retested (Trial 3)
at 50 ul and 75 ul (TA-100 only) per plate to verify the positive effect
and because the TA-98 spontaneous background in Trial 2 was higher than
assay acceptance criteria permit (see Section VII.B.).
5-145
BIONET1CS 11
Utton
-------
The minimum effective concentration (MEC) based on this data was
5 ul (30 ug organics) per plate with strain TA-98 without S9 metabolic
activation. The sample showed a dose response over the range of concen-
trations tested in Trial 2. Based upon the EPA Level 1 evaluation
criteria, the sample was ranked as having high (H) mutagenic activity.
2. TOSCO 1 XAD
The primary stock of the sample was prepared at 8.5 ug organics per
ml of DMSO. The initial trial at 10 ul per plate with TA-98 was positive,
both with and without S9 metabolic activation. The test material was
then evaluated in Salmonella strains TA-98 and TA-100 both with and without
59 metabolic activation mix. The dose range used in Trial 2 was 5, 10,
25 and 50 ul per plate. The test sample was not mutagenic for TA-98 in
Trial 2, but showed a positive effect in Trial 3 at 50 ul per plate.
The reason for this was attributed to the high spontaneous mutant back-
ground with TA-98 in Trial 2.
The test sample was weakly mutagenic for TA-100 in Trial 2 showing
a dose-related increase in the number of revertants, but never quite
reaching the threshold for a positive response. The Trial 3 TA-100 results
were positive with activation 50 and 75 ul per plate. The minimum effec-
tive concentration was selected from Trial 1 for TA-98 (MEC of 10 ul per
plate; 85 ug organics) TOSCO 1 XAD was found to.have moderate mutagenic
activity, but at a level closely approaching the high mutagenicity cate-
gory. The sample was ranked as having moderate (M) mutagenicity based
upon the EPA Level 1 evaluation criteria. Had sufficient sample been
available for adequate testing, a clearer picture of the potency could
have been obtained.
3. MOHAWK 1 XAD
The test material was prepared at a stock concentration of 3 ug
organics per ml DMSO. The test material was evaluated in Salmonella
strains TA-98 and TA-100 both with and without S9 mix. The initial range-
BIONETICS 5"146
Litton 12
-------
finding trial with TA-98 at 10 ul per plate was negative. The dose range
used in Trial 2 was 5, 10, 25 and 50 pi per plate. The material was
positive for both TA-98 and TA-100 although the solvent control values
for TA-98 were higher than normal. Activity in the presence of S9 mix
was greater than without S9 mix. This suggests the presence of promutagens
in the mixture. Strain TA-98 exhibited a dose-related increase in the
number of revertants both with and without metabolic activation. Trial 3
was conducted to confirm Trial 2 and because the TA-98 spontaneous values
from Trial 2 were higher than assay acceptance criteria permit.
The minimum effective concentration (MEC) based on this data was
25 M! (75 [jg organics) per plate with both TA-98 and TA-100 in the presence
of S9 mix (Trial 2 and Trial 3). Therefore, the Mohawk 1 XAD sample was
ranked as having moderate (M) mutagenic activity based upon the EPA Level 1
evaluation criteria. The MEC of 75 |jg per plate closely approaches the
moderate/high borderline of 50 |jg per plate. Had sufficient test material
been supplied to adequately test the sample, the MEC could have been
determined with greater precision.
4. MOHAWK 2 XAD
Only 4 mg of test material was supplied for both Ames and CHO testing.
The sample was prepared i.n 2 ml DMSO giving a primary stock concentration
of 2 ug organics per ul. The initial range-finding trial was conducted
with TA-98 with and without S9 mix at 10 pi per plate. The nonactivation
trial was negative, while the activation trial just reached the threshold
for a positive response. The test material was then evaluated in Sal-
monella strains TA-98 and TA-100 both with and without S9 mix. The dose
range used in Trial 2 was 5, 10, 25 and 50 ul per plate. Both strains
appeared to be negative and no dose-related increase in mutant levels
was noted. The TA-98 solvent controls in Trial 2 were higher than assay
acceptance criteria permit. Trial 3 was conducted at 50 ul per plate to
confirm Trial 2 responses and because of the elevated TA-98 spontaneous
mutant background level.
R-147
, BIONETICS ° *' 13
Utton
-------
This test material was not mutagenic in either strains TA-98 or
TA-100 under test conditions with and without S9 mix. No MEC could be
detected under the test conditions employed. The very weakly positive
result with strain TA-98 with activation at 10 ul per plate (Trial 1)
was considered to be an anomaly because it was not reproducable and because
no dose response was observed. Additional testing at higher concentrations
was impossible because of the lack of sufficient test material. Since
the sample could not be tested up to the maximum applicable dose (MAD)
of 5000 ug per plate and none of the doses tested were mutagenic, the
test material could not be evaluated. The MEC, if the sample is mutagenic,
was found to be greater than 10_0 ug per plate. The mutagenicity of the
sample was interpreted as being undetermined, but moderate or less.
B. Tables
This report is based on the data provided in Tables 1 through 12.
E 5-148
BIONETICS 14
Litton
-------
Ol
I
CO
FESL-LTS lieu t
A. NAME OR COir CfSIGMTION CF THE TEST CCfPCUIkC: TOSCO 2 K*D«OMC CA81-07-011-562t559l
E. ICLUM: wcur
C. TEST IMTIITICN C»US: 03/C5/62
0. 1ES1 CCPPIETICN D«TE: 03/Cf/82
F. S-S 1C1«: PEKCB£
kCIEt CCKCEMf AT] (NJ »FF 6TVEN IN flOROUTEFS PER PL* If
PEIEF1IK1S F F 8 PLATE
1ES1 SPECIES TISSUE TA-Sf
123
NONACTIVA1ICM
NEGATIVE CONTROL 61
NEGATIVE CONTROL ... .„ 6g
PCSI1IVE CCMFOl** --- S^6 i
POSITIVE CCMROl" S71
TEiT CCfPCllkC
10.00 II --- --- 31
ACTIVATIO*
NEGATIVE CONTROL RM LIVFP 72
NEGATIVE CONTROL RAI IIVER f,
POSITIVE CCKTPOl'** PAT IIVEF 1S21
POSITIVE CCKTPOL'*' RAT LIVER 656
TEJT COFCtkC
1C.00 III RAT LIVED 0
--...-.-^.
2-NI1RCFLLCREKE
1C UC/PLATE
2-AMHRAMNE
L£/FLATt
-------
RESULTS
TAHLE 2
A. NAHE OR CODE DESIGNATION OF THE TEST COWPCUfiC : 10SCO 2 XAD*OMC < AB1-0/-011-562 «559 I
p. SOLVENT: cn^E
C. TFST INITIATION (1ATFS: 03M5/B2
n. VEST COMPLETION HATE: 03/1P/P2
F. S-9 COT*: PFK OB5
NOTF: CCNCFNTRITICNS ARF GTWFK IN HICISCIIIEPS PER FLATE
TEST
NONACTIVATICN
SFECIFf TISSUE
REfcEPTANTS PER
TA-^e TA-ioo
1 ? 3 123
PLATE
Ul
O
CTl
CONTROL
SOLVENT CTNTPOL
104
POSITIVE CCMROL**
POSITIVE CONTROL**
TEST COMPOUND
1.00 l)L
5.00 UL
10.00 Ul
•50.00 UL
ACTIVATION
SOLVENT CONTROL PAT
SOLVENT CONTROL RAT
POSITIVE CONTROL*** RAT
POSITIVE CONTROL ••• RAT
TEST COWPUNO
1.00 UL PAT
=.00 UL PAT
10.00 UL PAT
•iO.OO Ul RAT
* t
TA-9fl ?-NITnCFLUCPFrf'"
TA-100 SCDIU" A2IDE
SOLVENT "iO IIL/PLATF
SOP
5«15
15?
22f
300
5-. 3
LIVER '97
LTVEP 101
LIVER 'PIO
LIVER 22flP
1 TVER 152
LIV^R 1*1
LIUFR II"
LIVFP *01
11 -1
1217
2C3
218
235
3C7
W
l*f
?^2
1051
lr;2
1 C0
117
261
* * *
10 UC/FI AT- TA-96 2-AMTHRAHlMt 2 .5 LG/HLATL
10 UU/FI.ATI TA-10Q 2-AMHKAhlNC ^ .b UG/PLATt
1
-------
01
i—*
O1
RESULTS TAflLt 3
A. N«MF OR COCr DESIGNATION CF THE TEST COPPCUNOt TOSCO 2 XAD+OHC
-------
Ol
CJ1
ro
RESULTS T»BLF *
ft. N««E OB COnr (V STGNfVTJON OF THE TEST COMPOUND: TOSCO I KAD IA81-07-011
P. sriVENT: N^NF
C. TEST INITIATION nATrct 03/PS/B3
0. TFSt COMPLETION OATFt 0?/OI«/B?
^. s-q LOTH: RrKOflfi
NOTE: CONCFNTRATIOMS ARF GIWFN TN HTCROI.IT«^RS PER PHTC
REVEPT*NT5: PFR PtATE
TFST SPcflF.S TISSUE 1A-9B
1 ? T
NONACTIVATION
NEGATIVE CONTROL — "" 67
NEGATIVE CONTROL —7 —
POSITIWF CONTROL*'
POSITIVE CONTROL** 1*1
TEST COHPOUND
10.00 WL I*1
ACTIVATION
NEGATIVE CONTROL RAT UVtR 7?
NEGATIVE CONTROL «"»T LTVFR f-l
POSITIVE CONTROL*** RAT LIVFR 19?t
POSITIVE CONTROL*** RAT LIVER • H^fe
TFST roWPOUND
10.00 UL RAT IIVFP K-«i
TA-"}fl
2-NIT»OFLUORENE
10 U6/FLAT1.
2-ANTHRAHlNt 2.5 UG/PLATL
CX)
-------
RESULTS
TABLE 5
Ol
CO
A. NAME OR COOr DESIGNATION OF THC TEST COMPOUND: TOSCO 1 KAO IA81-07-01J-56*)
R. SOLVENT: NONE
C. TfST INITIATION DATE0.: 03/15/H2
0. TF?T COMPLETION DATE: OVIB/BZ
r. S-9 LOT»: RF.KOB5
NOTE: CONCENTRATIONS ARE GIVEN IN <»ICHOLITE«S PER PLATE
RtVERTANTS PfR PLATE
TEST SPECIE?
NONACTIVATION
SOLVENT CONTROL
SOLVENT CONTROL
POSITIVE CONTROL**
POSITIVE CONTROL**
TEST COMPOUND
5.00 UL
10.00 UL
25.00 UL
bO.OO UL
ACTIVATION
SOLVENT CONTROL
SOLVENT CONTROL
POSITIVE CONTROL***
POSITIVE CONTROL*'*
TEST COMPOUND
5.00 UL
10.00 UL
25.00 UL
50.00 UL
* *
TA-9fl 2-NIT°0
TA-1QO SODIUM
^__ a
— — —
RAT
RAT
RAT
RAT
RAT
RAT
RAT
R*T
FtlinRr
A7IOP
TISSUE
— - —
LIVtB
LFVER
LIV^R
LIVER
LIVER
LIVER
LIVER
LIVER
NE
TA-98
1 2
10%
105
508
5fi5
65
106.
112
9*
•57
101
224t>
?2H6
107
^1
114
102
TA-100
3 123
irs
174
1121
1217
19C
20^
232
?90
13fl
1 46
99?
1051
194
ise
211
192
* **
10 Ufi/PLATE TA-'IW 2-ANTHRAMINE 2.i> U6/PLATE
10 Uk/PLATE TA-100 2-ANTHRAH1NE ^.5 U6/PLATL
-------
RESULTS
TABLE b
Ol
r>o
O
A. NAHE OR COCF DESIGNATION OF THE TEST COMPOUND: TOSCO 1 XAD (A81-07-011-569)
R. SOLVENT: NONE
C. TEST INITIATION DATES: OS/I^/P?
O. TEST COMPLETICN DATFT 03/22/82
r. s-«J LOTB: nrKOR*i
NOTE: CONCENTRATION?- ARE GIVEN IN
TEST
NONACTIVATION
~RS PER PL Alt"
REVEPTANT? PfR
SPECIE* TISSUE T»-98 1A-100
» »»» — «..«. _ __«» — — —• •.•_•— — •—*—-•*.•- • »• ••»•«» — — —.—.«•.•• — — -•••—•••
123 12:
PLATE
SOLVENT CONTROL
SftLWFNT CONTROL
POSITIVE CONTROL"
POSITIVE CONTROL•«
TEST COMPOUND
50.00 UL
ACTIVATION
853
136
SOLVENT 75 IIL/PLATF
- INDICATES TEST MAS NOT DONE
t 0!
97
1 *f,l
1 52P
SOLVENT CONTROL
SOLVENT CONTROL
POSITIVE CONTROL***
POSITIVE CONTROL***
TEST COMPOUND
SO. 00 UL
75.00 UL
RAT
RAT
RAT
RAT
RAT
RAT
LIVER
LIVKR
LIVER
LIVER
LIVER
LIVER
37
2"
15*1
J-6M
199
-
A 4
TA-9fl 2-NITROFLUORFNF
TA-100 SOniUH AZTOE
*6
113
2337
23 = 3
222
323
10 Ufi/PLATf
1C UG/PLATF
1
* **
TA-98 2-ANTHRAMlNti 2.5 U6/PLATL
IA-100 2-ANIHRAMIME ; 2 .5 U6/PLATE
-------
en
ui
RFSOLTS TABLE 7
A. NA««E OP C00r 0' SIGN»TI(JN OF THE TEST COMPOUND: MOHAUK1XAD (A 81-09-007-4881
B. SOLVCNT: NONE
C. TEST INITIATION OATrS: 03/OS/H2
D. TEST COMPLETION DATE: 03/08/82
F. S-9 LOT»: RFK085
NOTf: CONCENTRATIONS «Rf 6IVFN IN M ICRW.I T^RS PER PLATf
RFVfRTANTS P'R PLATE
TEST SPFCIES TISSUE TA-98
1 "> ?
NONACTIVATION
NEGATIVE CONTROL -~ — *7
NEGATIVE CONTROL — •• — **>
POSITIVE CONTROL**
POSITIVE CONTROL**
TEST COKPQUN1
10.00 Ul 110
ACTIVATION
NEGATIVE CONIROL RaT LIVER r?
NEGATIVE CONTROL "»T LIVER fi
POSITIVE CONTROL•»* RAT LIVER 19?1
POSITIVE CONTROL*** RAT LIVER ' R56
TEST COMPOUND
10.00 UL RAT LlVrn 88
TA-9H
?-NITROFLUORENE
10 UG/PLATE
TA-98 2-ANTHRAMIN^ 2.5 UG/PLAIL
-------
RFSULTS
A. NAH' OP CODF DESIGNATION OF TH? TEST COMPOUND: MOHAWK1 HAD CAB 1-09-007-488)
B. SOLVEN': NONF
C. TFST INITIATION OAT^S: OS/l'./R.'1
D. TFST COMPLETION DA^F: 03M8/82
F. S-9 LOTH: RFKORfS
NOTE: CONCENTRATIONS ARE GIVEN IN HICROLITERS PER PLATI
TFST
NONACTIVATION
PEVF.RTAKTS P t R PLATE
SPrCICS TISSUE TA-98 IA-100
125 ! ? 3
01
01
ro
SOLVFNT CONTROL
SOLVENT CONTROL
POSITIVE CONTROL**
POSITIVE CONTROL**
TEST COMPOUND
104
50R
565
174
1217
5.00 UL
10.00 UL
25.00 UL
50.00 UL
ACTIVATION
SOLVFNT CONTROL
SOLVENT CONTROL
POSITIVE CONTROL**
POSITIVE CONTROL**
TFST COMPOUND
5.00 UL
10.00 UL
2«J-00 UL
•50.00 UL
- —
RAT
RAT
• RAT
• PAT
RAT
R«T
^AT
RAT
fO
ISO
204
255
LIVER ' "7
LIVER 101
LIVER ?24f-
ITV^R ?2*f,
1 TVER 11 <
LIVER 174
LIVER 265
LIVFR 43*
* •
TA-9P 2-NITROFLI'OPEMF
TA-100 SODIU''
A^Tr)F
230
244
?19
2-=0
HP
1 4<
992
1 0 f . I •
229
1 97
?84 '
34S
10 UC/Pl. ATr
10 UP/PL ATP
TA-98 2-ANTH«AMINt ^.b Uti/PLATt.
TA-100 2-ANTHrtAHINt 2.b UG/PLAIE
-------
RESULTS
A. NAKF OP CODE DESIGNATION OF THl TEST COMPOUND: MOHAWK 1 XAD CA 81-0 9-007-48H)
B. SOLVENI: NONE
C. TEST INITIATION DATES: D5/>9/«2
0. TEST COMPLETION OATr: 03/22/8?
f. S-9 LOT»: RFKOH5
NOTE: CONCENTRATIONS A^F eivrw IN MICROLTTERS PER PLAIT
TEST
NONACTTVATTON
RFVEPTANT:
SPFCIFS TISSUE TA-98 TA-
123 1
PER
PLATE
en
i—1
01
SOLVENT CONTROL
SOLVENT CONTROL
POSITIVE CONTROL**
POSITIVE CONTROL**
TEST COMPOUND
50.00 UL
7-j.OO UL
ACTIVATION
lin
ro
SOLVENT 75 UL/PLATf
INDICATES TEST MAS NOT DONE
1C1
17
132«
1367
IflO
SOLVENT CONTROL RAT LIVFR 27
SOLVENT CONTROL PAT LIVER 29
POSITTVr CONTROL*** P" T LIVER 15'-l
POSITIVE CONTROL*** RAT LIVFR lf>(l
T^ST COMPOUND
25.00 UL IAT IIVFH MS
r>0.00 Ul PAT LIVFR 235
* •
TA-98 2-NITROFLUORENf:
TA-1P" SODTU" A^rnE
<*f,
11?
tto
"
'
»*«
10 Ufi/PL ATE TA-98 2-ANTHRAMINE i.ti UG/PLATE
10 un/fLATl TA-10C 2-ANTHHAHINE ^.5 Ub/PLAU
-------
tn
01
CD
RfSULTS fAHLC 10
A. NAHE 0» COO^ DESIGNATION OF THE tEST COHPCUNI): MCHAUK2 KAO IA8l-09-007-«95l
n. SOLVENT: NONF
C. TFST INITIA'ION DATFS: 03/P«>/H?
n. TFST COHPtFTION HAT^:
-------
RfSULTS
TAHLE 11
A. NAHE OP COOP DESIGIAMON OF THE TCST CO*POUNO: HONAHK 2 HAD C«81-0 9-007-4951
fl. SOLVENT: NtlNF
r. TFST INITIATION DATES: 03/15/82
0. TEST COMPLETION OATC: 0318 '82
r. s-9 LOTH: REHO^^
NOTf: CONCENTRATIONS ARE 6IWFN TN MICROLITERS PER FLATF
Ol
I
co
ro
tn
TEST SPFriFS
NONACTIVA TTOM
SOLWFNT CONTROL
SOLVENT CONTROL
POSITIVE CONIPOL*«
POSITIVE CONTROL"
TEST COMPOUND
5.00 UL
10.00 UL
2^.00 UL
f>0. 00 UL
ACTIVATTON
SOLVENT CONTROL
SOLVENT CONTROL
POSITIVE CONTROL"*
POSITIVE CONTROL***
TEST COMPOUND
*>.00 UL
10.00 UL
??i.OO UL
•^0.00 UL
* *
_ _—
RAT
RAT
RAT
RAT
RAT
RAT
PAT
RAT
TISSUE
---
LIVER
LTUFR
IIVFR
LIVFR
LIVER
itvrp
LIVER
LTVFP
TA-98
1 ?
104
105
506
565
60
96
98
9B
1 <»?
101
•>2*,c
22B6
107
109
106
105
TA-9R 2-NITROFLHORENf
TA-1PO SOOTUM
A2TOE
TA-100
3 1 ? 3
1 75
1T«
1121
131T
81
121
ieu
161
lie
14fi
992
10M
17?
1P4
i«in :
139
A *•
10 UG/PI ATF TA-98 2-ANTHKAMIM£ 2.S UG/PLAlt.
10 UC./PLATC IA-100 2-ANTHRAMl^t i -b Uti/PLAlL
-------
CJI
I
RESULTS TAfSLE «
». NAME OR COD r*-siGNATION OF TH? TEST COMPOUND: MOHAWK? KAD < A«l-0b>
n. SOLVENT: NONE
C. TrST INITIATION DATE^t 03/t9/8?
D. TEST COMPLETION DATE: 03/22/H2
f . S-9 LOT»: R^KOWT
NOTE: CONCENTRATIONS ARE GIVEN IN MICROLITEPS PER PLATE
PEVERTAKTS PER PLAIE
TEST SPECIES TISSUE TR-98
1 ?. 3
NONACTIVATION
SOLVENT CONTROL 27
SOLVENT CONTROL 0"
POSITIVE CONTROL** " «53
POSITIVE CONTROL** »*•*
TEST COMPOUND
50.00 UL 2*
ACTIVATION
SOLVENT CONTROL RAT LIV^R ?*
SOLVENT CONTROL RAT LIVER ?'»
POSITIVE CONTROL*** "»T LIVER ISf-l
POSITIVE CONTROL*** RAT LIVER 16fI
TEST COMPOUND
50.00 UL RAT LIVER 47
TA-9B
SOLVENT
?-NITROFlUOHENr
75
10 UG/PIATE
TA-96
2-ANTHRAMINE
UG/PLATE
-------
VII. ASSAY ACCEPTANCE AND EVALUATION CRITERIA
Statistical methods are not currently used, and evaluation is based
on the criteria included in this protocol.
Plate test data consists of direct revertant colony counts obtained-
from a set of selective agar plates seeded with populations of mutant
cells suspended in a semi sol id overlay. Because the test material and the
cells are incubated in the overlay for approximately 2 days and a few
cell divisions occur during the incubation period, the test is semiquanti-
tative in nature. Although these features of the assay reduce the quantt-
tation of results, they provide certain advantages not contained in a
quantitative suspension test:
The small number of cell divisions permits potential
mutagens to act on replication DNA, which is often more
sensitive than nonreplieating DNA.
The combined incubation of the test article and the cells
in the overlay permits constant exposure of the indicator
cells for approximately 2 days,
A. Surviving Populations
Plate test procedures do not permit exact quantitation of the number
of cells surviving chemical treatment. At low concentrations of the test
material, the surviving population on the treatment plates is essentially
the same as that on the negative control plate. At high concentrations,
the surviving population is usually reduced by some fraction. Our protocol
will normally employ several doses ranging over two or three log concen-
trations, the highest of these doses being selected to show slight toxicity
as determined by subjective criteria.
5-161
,_ BIONETICS 27
Utton
-------
B. Dose-Response Phenomena
The demonstration of dose-related increased in mutant counts is an
important criterion in establishing metagenicity. A factor that might
modify dose-response results for a mutagen would be the selection of
doses that are too low (usually mutagenicity and toxicity -are related).
If the highest dose is far lower than a toxic concentration, no increases
may be observed over the dose range selected. Conversely, if the lowest-
dose employed is highly cytotoxic, the test material may kill any mutants
that are induced, and the test material will not appear to be mutagenic.
C. Control Tests
Positive and negative control assays were conducted with each experi-
ment and consisted of direct-acting mutagens for nonactivation assays and
mutagens that require metabolic biotransformation in activation assays.
Negative controls consisted of the test material solvent in the overlay
agar together with the other essential components. The negative control
plate for each strain gave a reference point to which the test data was
compared. The positive control assay was conducted to demonstrate that
the test systems were functional with known mutagens.
The following normal range of revertants for solvent controls are
generally considered acceptable.
TA-1535: 8-30
TA-1537: 4-30
TA-98: 20-75
TA-100: 80-250
D. Evaluation Criteria for Ames Assay
Because the procedures to be used to evaluate the mutagenicity of the
test material are semi quantitative, the criteria to be used to determine
ffl
Litton
5-162
BIONETICS 28
-------
positive effects are inherently subjective and are based primarily on a
historical data base. Most data sets will be evaluated using the following
criteria.
1. Strains TA-1535 and TA-1537
If the solvent control value is within the normal range, a test
material that produces a positive dose response over three concentrations
with the highest increase equal to three times the solvent control value
will be considered to be mutagenic.
2. Strains TA-98 and TA-100
If the solvent control value is within the normal range, a test
material that produces a positive dose response over three concentra-
tions with the highest increase equal to twice the solvent control value
for TA-98 and TA-100 will be considered to be mutagenic.
3. Pattern
Because TA-1535 and TA-100 are both derived from the same parental
strain (G-46), to some extent there is a built-in redundancy in the microbial
assay. In general, the two strains of a set respond to the same mutagen
and such a pattern is sought. Generally, if a strain responds to a mutagen
in nonactivation tests, it will do so in activation tests.
4. Reproducibility
If a test material produces a response in a single test that cannot be
reproduced in additional runs, the initial positive test data lose signi-
ficance.
5-163
BIONET1CS 29
-------
The preceding criteria are not absolute, and other extenuating factors
may enter into a final evaluation decision. However, these criteria
will be applied to the majority of situations and are presented to aid
those individuals not familar with this procedure. As the data base is
increased, the criteria for evaluation can be more firmly established.
E. Relation Between Mutagenicity and Carcinogenicity
It must be emphasized that the Ames Salmonel1 a/Microsome Plate Assay
is not a definitive test for chemical carcinogens. It is recognized,
however, that correlative and functional relations have been demonstrated
between these two endpoints. The results of comparative tests on
300 chemicals by McCann et aJL7 show an extremely good correlation between
results of microbial mutagenesis tests and i_n vivo rodent carcinogeiiesis
assays.
All evaluations and interpretation of the data to be .presented in
the final report will be based only on the demonstration, or lack, of
mutagenic activity.
F. Criteria for Ranking Samples in the Ames Assay
The goal of EPA Level 1 Ames testing is to rank source streams by
relative degree of genetic toxicity (mutagenicity). Samples are first
identified as mutagenic or nonmutagenic by the criteria in Section D
above and then ranked using the mutagenicity categories presented in the
table below. The lowest concentration giving a positive response in any
strain, with or without metabolic activation, is identified as the minimum
effective concentration (MEC) for that sample. The mutagenicity of the
sample is evaluated as high (H), moderate (M), low (L), or nondetectable
(ND) according to the evaluation criteria developed in the Level 1 manual1
and summarized below. Samples with no detectable activity at the maximum
applicable dose (MAD) are ranked nondetectable (ND).
E5-164
BIONETICS 30
Litton
-------
Another evaluation scheme is proposed for extracts obtained from
SASS train gas volumes. The proportion of the total gas volume corres-
ponding to the volume of extract used in the bioassay is calculated and
expressed as liters per plate. A criterion of 5000 L/plate is set as
the limit for nondetectable toxicity. The subsequent toxicity ranges
are defined by 10-fold dilution steps to conform to standard procedure.
Evaluation criteria based on equivalent gas volumes are tentative and
under evaluation.
Ames Assay Mutagenicity Ranking Criteria1
Mutagenic
Activity
High (H)
Moderate (M)
Low (L)
Not Detectable (ND)
Solids
(MEC in ug/plate)
<50
50-500
500-5000
>5000
Liquids3
(MEC in M! /pi ate)
<2
2-20
20-200
>200
Equivalent
Gas Volumes
(MEC in liters/plate)
<50
50-500
500-5000
>5000
Concentration of organic extracts is based upon organic content (ug
organics per plate) and not volume (ul extract per plate) of sample
tested.
Lrtton
BIONETICS
5-165
31
-------
VIII. REFERENCES
1. Brusick, D.J. and Young, R.R.: IERL-RTP Procedures Manual: Level 1
Environmental Assessment Biological Tests. EPA-600/8-81-024, Litton
Bionetics, Inc., Kensington, MD, October, 1981, 150 pp.
2. Brusick, D.J.: Level 1 Bioassay Assessment and Data Formatting.
EPA-600/7-80-079, Litton Bionetics Inc., Kensington, MO, April 1980-,
100 pp.
3. Brusick, D.J. and Young, R-.R.: Level 1 Bioassay Sensitivity.
EPA-600/7-81-135, Litton Bionetics, Inc., Kensington, MD, August
1981, 52 pp.
4. DHEW Food and Drug Administration "Nonclinlcal Laboratory Studies;
Good Laboratory Practice Regulations." Federal Register, volume 43,
No. 247, pp. 59986-60020, Part II, December 22,.1978.
5. Proposed Health Effects Test Standard for Toxic Substances Control
Act Test Rules; Good Laboratory Practice Standards for Health Effects.
Federal Register, Part II, volume 44, No. 91, May 1979 and Part IV,
volume 44, No. 145, July, 1979.
6. Guidelines for Registering Pesticides in the United States: Proposed
Good Laboratory Practice Guidelines for Toxicology Testing. Federal
Register, volume 45, No. 77, April, 1980.
7. McCann, J., Choi, E., Yamasaki, E. and Ames, B.N.: Detection of
carcinogens as mutagens in the Salmone11 a/microsome test: Assay of
300 chemicals. Proc. Nat. Acad. Sci., USA 72:5135-5139, 1975.
8. Ames, B.N., Gurney, E.G., Miller, J.A. and Bartsch, H.: Carcinogens
as frameshift mutagens: Metabolites and derivatives of 2-acetylamino-
fluorene and other aromatic amine carcinogens. Proc. Nat. Acad.
Sci., USA 69:3128-3132, 1972.
LtJ BIONETICS 5"166 32
Utton
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9. Ames, B.N., Lee, F.D., and Durston, W.E.: An improved bacterial
test system for the detection and classification of mutagens and
carcinogens. Proc. Nat. Acad. Sci., USA 70:782-786, 1973.
10. Ames, B.N., Durston, W.E., Yamasaki, E. and Lee, F.D.: Carcinogens
are mutagens: A simple test system combining liver homogenates for
activation and bacteria for detection. Proc. Nat. Acad. Sci., USA
70:2281-2285, 1973.
11. McCann, J., Springarn, N.E., Kobori, J. and Ames, B.N.: Detection
of carcinogens as mutagens.: Bacterial tester strains with R factor
plasmids. Proc. Nat. Acad. Sci. USA 72:979-983,. 1975.
12. Ames, B.N., McCann, J. and Yamasaki, E.: Methods for detecting
carcinogens and mutagens with the Salmonella/mammalian-microsome
mutagenicity test. Mutation Res., 31:347-364, 1975.
13. Vogel, H.J. and Bonner, D.M.: Acetylornithinase of E. coli partial
purification and some properties. J. Biol. Chenu , 218:97-106, 1966.
, BIONETICS 5-167 33
Lrtton
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GENETICS ASSAY NOS. 6153-6156
LBI SAFETY NOS. 7535-7538
CYTOTOXIC EVALUATION OF
XAD RESIN EXTRACTS
IN THE
EPA LEVEL 1
RODENT CELL
. (CHO)
TY ASS/
CLONAL TOXICITY ASSAY
FINAL REPORT
SUBMITTED TO:
ACUREX CORPORATION
485 CLYDE AVENUE
MOUNTAIN VIEW, CALIFORNIA 94042
SUBMITTED BY:
LITTON BIONETICS, INC.
5516 NICHOLSON LANE
KENSINGTON, MARYLAND 20895
LBI PROJECT NO. 22064
REPORT DATE: MARCH 1982
E 5-168
BIONETICS
Litton
-------
PREFACE
These assays conform to the standard EPA Level 1 procedure for the
Chinese hamster ovary cell (CHO) clonal toxicity assay as described in
"IERL-RTP Procedures Manual: Level 1 Environmental Assessment Biological
Tests"1. The data were evaluated and formatted as recommended in "Level 1
Biological Testing Assessment and Data Formatting"2.
The CHO clonal toxicity assay has been shown to be a sensitive method
for detecting cytotoxic activity for a variety of chemicals representing
various chemical classes 3. This assay is one of several recommended by
EPA to identify, categorize and rank the pollutant potential of influent
and effluent streams from industrial and energy-producing processes.
This assay has been well validated with a wide range of positive and
negative control chemicals and complex environmental samples.
All procedures and documents pertaining to the receipt, storage,
preparation, testing and evaluation of the test, material shall conform
to Litton Bionetics, Inc. standard operating procedures, the U.S.
Food and Drug Administration's Good Laboratory Practices Regulations of
19794 and the proposed U.S. Environmental Protection Agency's Good
Laboratory Practice Guidelines.5'6 Deviations from standard procedure
shall be fully documented- and noted in the report.
All test and control results in this report are supported by fully
documented raw data which are permanently maintained in the files of the
Department of Molecular Toxicqlogy or in the archives of Litton Bionetics,
Inc., 5516 Nicholson Lane, Kensington, Maryland 20895. Copies of raw
data will be supplied to the sponsor upon request.
5-169
BIONETICS
-------
TABLE OF CONTENTS
Page No.
PREFACE
I. ASSAY SUMMARY
II. OBJECTIVE
III. TEST MATERIAL
A. Description
B. Handling and Preparation
IV. MATERIALS ."....
A. Indicator Cells ....
B. Media
C. Controls
V. EXPERIMENTAL DESIGN
A. Dose Selection
B. Clonal Toxicity Assay .
VI. RESULTS
A. Interpretation
1. TOSCO 2 XAD + OMC .
2. TOSCO 1 XAD ....
3. MOHAWK 1 XAD ...
4. MOHAWK 2 XAD ...
B. Tables and Figures . . .
VII. ASSAY ACCEPTANCE CRITERIA . .
VIII. ASSAY EVALUATION CRITERIA . .
IX. REFERENCES . . . . '
1
2
3
3
3
5
5
6
7
7
9
9
9
10
11
12
21
22
24
m
Litton
BIONETICS
5-170
-------
I.
SUMMARY
Four resin extract sample supplied by Acurex Corporation were tested
and evaluated for their cytotoxicities in the EPA Level 1 Chinese hamster
ovary (CHO) cell clonal toxicity assay. The samples, supplied in methylene
chloride, were solvent exchanged to dimethylsulfoxide (DMSO) prior to
testing. The samples were identified as TOSCO 2 XAD + OMC (A81-07-011-562,
559), TOSCO 1 XAO (A81-07-011-569), MOHAWK 1 XAO (A81-09-007-488) and
MOHAWK 2 XAD (A81-09-007-495).
TOSCO 2 XAD + OMC and TOSCO 1 XAD were both ranked as having moderate
toxicity with EC50 values of 70.8 ug organics/ml and 37.4 ug organics/ml,
respectively. CHO toxicity testing was limited by the small amount of
test material supplied for MOHAWK 1 XAD (6 mg organics) and MOHAWK 2
XAD (4 mg organics). EC50 values could not be located for these two
samples. No toxicity was observed up to the maximum applicable dose
(MAD) of 20 ul/ml (60 UQ organics/ml) with MOHAWK 1 XAD and only slight
toxicity at the MAD of 20 Ml/ml (40 ug organics/ml) with MOHAWK 2 XAD.
Therefore, the toxicities of these two samples were evaluated as being
undetermined but moderate or less.
The results indicate that quantities less than 10 mg organics of this
type of sample were not sufficient for adequate Level 1 testing. While
minimum testable sample size is often a function, of the biological activity
of the sample, efforts should be made to supply at least 20 mg of SASS
train organics for combined Ames and CHO testing.
Submitted by:
Study Director
Robert Yc
Study Director,
Environmental Assessment
Section
Department of Molecular
Toxicology
Date
Reviewed by:
J. Brusick, Ph.D.
Director,
Department of Molecular
Toxicology
5-171
Litton
BIONETICS
-------
II. OBJECTIVE
The objective of this study was to determine and rank the cytotoxi-
cities of four resin extract samples to cultured Chinese hamster cells
(CHO-K1 cell line). The samples were solvent exchanged into dimethyl -
sulfoxide (DMSO) before CHO testing was initiated. The measure of cyto-
toxicity was the reduction in colony-forming ability of CHO-K1 cells
after a 24-hour exposure to the test material. After a period of recovery
and growth, the number of colonies that developed in the treated cultures
was compared to the colony number in unexposed vehicle control cultures.
The concentration of test mater-ial that reduced the colony number by 50
percent was estimated graphically and referred to as-the EC50 value.
Standard EPA Level 1 toxicity evaluation criteria for the CHO clonal
toxicity assay were used to rank the toxicity potential of each test
material.
CB B.ONET.CS 5'172
Lrtton
-------
III. TEST MATERIAL
A. Description
Four samples were supplied by Acurex Corporation, Mountain View,
California. The samples were assigned LBI safety numbers .and LSI assay
numbers upon receipt. The Acurex code numbers, sample identification,
LBI safety numbers and LBI assay numbers are identified below. All labora-
tory documentation used the LBI assay number to identify samples.
The four test materials were received as clear, yellow solutions of
organic material in methylene chloride except for the TOSCO 1 XAD sample.
That sample was an amber-colored, clear solution with a few suspended
particles. The quantity of organic material in each sample, as determined
by Acurex Corporation, is identified below. No information on sampling
parameters (such as the equivalent volume of stack gas represented by
the sample) was provided.
Acurex Corp. Code
A81-07-011-562, 559
A81-07-011-569
A81-09-007-488
A81-09-007-495
Sample
Identification
TOSCO 2 XAD + OMC
TOSCO 1 XAD
MOHAWK 1 XAD
MOHAWK 2 XAD
Quantity
(mg organic)
12
17.
6
4
LBI
Safety No.
7537
7538
, 7535
7536
LBI
Assay No.
6153
6154
6155
6156
B. Handling and Preparation
The test materials were received at LBI on February 8, 1982. The
samples were shipped in small, clear-glass vials sealed with crimp-top
aluminum caps with rubber liners. The samples were received intact and
were stored at +4°C in the dark until processed.
5-173
BIONETICS
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Pretest sample preparation consisted of solvent exchanging the samples
into dimethysulfoxide (DMSO). The samples were transferred with methylene
chloride rinses into graduated conical tubes. The methyl chloride was
gradually evaporated (50°C under a stream of nitrogen) and DMSO was
sequentially added. The samples were brought to volume in 2.0 ml of
DMSO. The samples were transferred to glass vials and sealed with teflon-
coated rubber rounds. The solvent exchanged samples were stored at
+4°C in the dark.
A total volume of 0.42 ml of each test sample was used in the CHO
assays. The maximum concentration of 20 ul/ml was obtained by adding
0.12 ml of sample to 5.88 ml of F12 medium; this resulted in 2 percent
(v/v) DMSO in the medium and effectively limited the concentration of
test material that could be assayed. Only two plates were dosed at the
top dose in order to conserve sample. Another 0.12 ml aliquot of sample
was added to 11.88 ml of F12 medium to prepare the 10 ul/ml test concen-
tration. An additional 0.18 ml of test sample was used to prepare a
series of dilutions in DMSO from which 1:100 dilutions into growth medium
were performed to obtain the lower assayed concentrations. Thus, except
for the 20 pi/ml test concentrations, the final DMSO concentration was
constant at 1 percent (v/v).
E 5-174
BIONETICS
Lrtton
-------
IV. MATERIALS
A. Indicator Cells
The indicator cells for these assays were Chinese hamster CHO-K1
cells (ATCC No. CCL 61) obtained from Flow Laboratories, Inc., Rockville,
MD. This cell type was derived from ovarian tissue and has spontaneously
transformed to a stable, hypodiploid line of rounded, fibroblastic cells
with unlimited growth potential. Monolayer cultures have a fast doubling
time of 11 to 14 hours, and untreated cells can normally be cloned with
an efficiency of 80 percent or -greater. Laboratory stocks were maintained
by routine serial subpassage. Cells were cultivated-in Ham's F-12 nutrient
medium at 37°C in an atmosphere of 5 percent C02 and saturated humidity.
Stocks were continually observed macroscopically and microscopically for
possible microbial contamination. Laboratory cultures were periodically
checked by culturing and staining methods for the absence of mycoplasma
contamination. Laboratory cultures were discarded every three months
and new cultures started from mycoplasma-free, Tong-term frozen cultures.,
B. Medi a
The CHO-K1 cell line has an absolute requirement for proline and
therefore must be maintained in culture medium containing sufficient
amounts of this amino acid. Ham's F12 medium, which contains 3 x 10-4 M
L-proline was used, supplemented with 10 percent fetal bovine serum, 2mM
L-glutamine, 100 units/ml of penicillin, 100 ug/ml of streptomycin, and
0.9 ul/ml of amphotericin B. •
C. Controls
The negative control for all four assays consisted of three untreated
cultures in F12 medium carried through the same experimental time period
as the treated cells. Since the test materials were tested as solutions
in an organic vehicle (DMSQ) and were diluted into the medium to provide
each test concentration, two sets of vehicle control cultures containing
5-175
BIONET1CS
-------
DMSO at one percent and two percent by volume were prepared in triplicate
for each assay. The average number of colonies in the negative control
established the cloning efficiency of the CHO cells used in the assays
and the appropriate vehicle controls provided the reference points for
determining the effects of different concentrations of the solid test
materials on cell survival.
E5-176
BIONETICS
Lrtton
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V. EXPERIMENTAL DESIGN
A. Dose Selection
Unless the approximate toxicity is already known, or the sample
size is limiting, the following minimum dose ranges are recommended by
the Level 1 manual1 for testing different sample" forms. Aqueous samples,
suspensions, or slurries are tested from 600 ul/ml to 6 ul/ml, usually
in five dose steps. Dry, particluate material is dissolved or suspended
in culture medium and tested at five dose levels from 1000 ug/ml to 10 ug/ml,
Samples that are solvent-exchanged into DMSO are tested from 20 ul/ml to
0.5 ul/ml, in five dose steps. Eight doses are often used when the amount
of test sample is limited to provide a more precise description of toxicity
in the event of sharp dose-response curves. A second dose study is per-
formed with an adjusted dose range if the EC50 was not located properly
in the initial test. However, EC50 values greater than 1000 ug/ml for
particulate material, 600 ul/ml for aqueous samples, or 20 yl/ml for
organic solutions will not be determined.
In this work the test materials were tested as resin extracts in an
organic vehicle. The concentrations used for the samples started with
the maximum applicable dose (MAD) of 20 ul/ml and included seven other
doses that were 10, 6, 3,.l, 0.6, 0.3 and 0.1 ul/ml.
B. Clonal Toxicity Assay
Cells from monolayer stock cultures in logarithmic growth phase
were trypsinized with 0.1 percent trypsin plus 0.01 percent versene for
4 minutes, and the density of the resulting cell suspension was determined
by hemocytometer. A number of 60-mm culture dishes were then seeded
with 200 cells and 4 ml of culture medium per dish. The cultures were
incubated for approximately 6 hours at 37°C in a humidified atmosphere
containing 5 percent C02 to allow attachment of the cells. The 6-hour
attachment period was used in order to avoid cell division and the subse-
quent formation of two-cell colonies prior to treatment.
5-177
BIONETICS
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The medium was aspirated from the cultures and 4 ml of control medium
or medium containing the test material was applied. Three cultures were
exposed to each test concentration. After an exposure time of 24 hours
at 37°C, the medium was removed by aspiration and each culture washed
two times with approximately 4 ml aliquots of Dulbecco's phosphate buffered
saline (pre-warmed to 37°G). Fresh culture medium (5 ml)..was placed in
each dish, and incubation at 37°C was continued for an additional 6 days
to allow colony development.
If the test material caused a color change in the culture medium,
the pH of the medium containing-the high dose would be determined at the
time of treatment. The pH at the lowest dose that results in a slight
color change would also be recorded. At the end of the treatment period,
the pH values of the discarded media from the two described treatments
would be recorded again. No sample-related pH changes were noted in any
of the treatments.
After the incubation period, the medium was drained from the culturesf
and the surviving colonies were fixed with 100 percent ethanol and stained
with Giemsa. Colonies were counted by eye; tiny colonies of approximately
50 cells or less were arbitrarily excluded from the counts.
DB BIONETICS 5"178 8
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VI. RESULTS
A. Interpretation
The results of the Chinese hamster ovary (CHO) clonal toxicity assays
are presented In Tables 1 through 4. The calculated relative survival
values were obtained by comparing the average number of colonies per
dish for each of the assayed concentrations to the appropriate control
value. The relative survival values were then plotted as functions of
the applied concentration of test material per ml of culture medium in
Figures 1 through 4. Curves were fitted to the data points by eye in
order to determine the EC50 value for each sample and to rank each sample
according to EPA Level 1 evaluation criteria presented in Section VIII.
1. TOSCO 2 XAD + OMC (A81-07-011-562, 559)
The application of the DMSO solution of the TOSCO 2 XAD + OMC sample
(A81-07-011-562, 559) to the CHO cell cultures caused a rapid lowering
of the number of cells able to form colonies as the concentration was
increased above 6.0 ul/ml. As shown in Figure 1, the relative survival
remained above 90 percent in the 0.1 to 6.0 ul/ml range but dropped to
zero at the 20.0 ul/ml dose level. The full range of survival was ex-
pressed between 6 ul/ml (>90 percent relative survival) and 20 ul/ml
(0 percent relative survival).
The concentration expected to kill 50 percent of the cells (EC50)
was found to be 11.8 ul of test material per ml of culture medium. The
concentration was equivalent to 70.8 ug of organic material per ml of
culture medium. This value placed the test material in the moderate (M)
toxicity range defined for the IERL-EPA CHO clonal toxicity bioassay1.
2. TOSCO 1 XAD (A81-07-011-569)
The TOSCO 1 XAD sample (A81-07-011-569) in DMSO was found to be
toxic to CHO cells in culture at concentrations above 1.0 ul/ml. The
5-179
_ BJONETICS
utton
-------
ffi
Utton
ability of CHO cells to form colonies was unaffected by a 24-hour exposure
to concentrations of test material between 0.1 and 1.0 Ml/ml. The relative
survival values covered the full range of toxicity between 1 ul/ml (104.3
percent relative survival) and 10 ul/ml (0 percent relative survival).
The EC50 was found to be 4.4 ul of test material per ml of culture
medium. This concentration was equivalent to 37.4 ug of organic material
per ml of culture medium. The test material was ranked as having moderate
(M) toxicity based upon the evaluation criteria developed for the IERL-EPA
CHO clonal toxicity bioassay1.
3. MOHAWK 1 XAD (A81-09-007-488)
The exposure of CHO cells in culture to the MOHAWK 1 XAD sample
(A81-09-007-488) in DMSO essentially caused no decrease in the number of
cells able to form colonies as the concentration was increased to the
maximum applicable dose (MAD) of 20 Ml/ml. As shown in Figure 3 the
relative survival to all of the treatments remained above 90 percent.
Since none of the tested doses caused killing that even approached
50 percent of the cells, an EC50 could not be estimated. However, the
lack of toxicity at the MAD of 20 ul/ml (60 ug organics/ml) excluded the
sample from the high toxicity category and from at least 60 percent of
the moderate toxicity range, based on the IERL-RTP evaluation criteria1.
Because very sharp and well-defined toxicity curves have been observed
with similar samples, it is possible that if sufficient test material
had been supplied, toxicity could have been observed in the moderate or
low toxicity ranges. The toxicity of the sample was therefore evaluated
as undetermined but moderate (M) or less.
Testing and evaluating materials such as this sample indicate the
need to supply sufficient quantities of test material to ensure adequate
testing. While minimum testable sample size is often a function of the
biological activity of the sample, efforts should be made to supply at
least 20 mg of SASS train organics for combined Ames and CHO testing.
B10NETICS 5"180 10
-------
4. MOHAWK 2 XAD (A81-09-007-495)
The application of DMSO solution of the MOHAWK 2 XAD sample
(A81-09-007-495) to the CHO cells in culture caused only a small de-
crease in the number of cells able to form colonies as the concentration
was increased to the maximum applicable dose (MAD) of 20 ul/ml. Rela-
tive survival remained above 90 percent between 0.1 and 3 |7l/ml. Between
3 and 10 ul/ml there was a noticable increase in sample toxicity. As
shown in Figure 4, the relative survival decreased to about 72 percent
for the 20 Ml/ml treatment.
Since none of the tested doses caused killing approaching 50 percent
of the cells, an EC50 could not be calculated. However, an EC™ value
greater than 20 ul/ml (40 ug organics/ml) excluded the sample from the
high toxicity category and nearly half of the moderate toxicity categories
based on the IERL-RTP evaluation criteria1. The plotted results suggested
the possibility of an EC50 in the 30 to 90 ul/ml range (60 to 180 ug
organics/ml), so the sample could have been evaluated as having moderate
or low toxicity had sufficient sample been available. The toxicity of
the sample was therefore evaluated as undetermined but moderate (M) or
less.
Testing and evaluating materials such as this sample and MOHAWK 1
XAD indicate the need to supply sufficient quantities of test material
to ensure adequate testing. Only 4 mg of organic material was supplied
for both Ames and CHO testing - an insufficient quantity for adequate
testing for all but the most mutagenic and toxic samples.
The cells used for the four assays were in logarithmic growth phase
and the cells in suspension prior to cell plating were 99.6 percent viable
as determined by trypan blue dye exclusion. Greater than 77 percent of
the seeded cells formed colonies in the negative controls for each of the
four assays (80.5 ±2.9 percent). Colony growth was normal and well
distributed on the culture dishes in all trials. The combined results
achieved the assay acceptance criteria discussed in Section VII, which
5-181
BIONET1CS
-------
provided confidence in the assumption that the recorded data represented
typical responses to the test materials.
B. Tables and Figures
This report is based on the data provided in Tables 1 through 4 and
Figures 1 through 4.
E 5-182
BIONETICS 12
Lrtton
-------
TAHLE I
CLONAl CYTOTOXICITY ASSAY
SAMPLE IDENTIT1* : TOSCO. 2 MAD » OHC
DESCRIPTION OF SAMPLE: CLEAR. YFLLOU LIOUIO
LBI ASSAY NO. 6153
DATE RFCEIVEO: FEBRUARY H, 19B2
TEST DATE: HARCH 4t 198*
VEHICLE: OIMETHYLSULFOXIOF toMso»
CEIL TYPE: CHO-KI
CELLS SEEDED PER DISH: 200
ECSO VALUE: 10.a UG/HL ui.t» UL/MD
TOXICITY
CLASSIFICATION: MOOERATL IH>
PH ALTERATIONS: NOME.
COMMENTS ON TREAIMtNl: 12 HG OF ORGANIC MATERIAL WERE
SUPPLIED FUR ILSTIN6. SAMPLE WAS SOLVENT EXCHANGED
INTO 2.0 ML DNSO (ilbING A PHIHARY STOCK CONCENIRAT ION
Of 6 UG ORGANIC PLR UL OF DHSO.
COLONY COUNTS
01
1— '
00
CO
1 — 1
SAMPLE
NC
VC, IX
VCt 2X
TEST
TEST
TEST
TEST
TEST
TFST
TEST
TEST
APPLIED
CONCENTRATION
UL/ML
10
20
O.I
0.3
0.6
1.0
1.0
«.o
10.0
20.0
DISH
HI
165
M*
156
IfO
169
165
146
ISi
M9
104
n
01 SH
«2
1RO
167
155
167
157
159
159
158
1*2
114
0
DISH
»3
162
157
149
161
149
156
152
143
152
105
S
AVERAGL
COUNT
169.0
156.0
153. J
162.7
158. J
160.0
1 152.3
151.3
147.7
107.1
0.0
RELATIVE
SURVIVAL*
i PERCENT)
10U.O
100.0
100.0
104.3
101.5
102.6
97.6
97.0
1 44. 7
69.0
0.0
CLONING
EFFICIENCY
tPERCENT)
84.5
78.0
/6.7
NC = NEGATIVE CONTROLt Fl?
VC = VfHICLE CONTROLt PERCENT GIUEN KIR OIMPTHYLSULEOXID? COMSOI
S = P14TF NOT SET UP TO CONSFRJF LIHITEO SAHPLF
•HFLATIVE 10
-------
TABLE 2
SAMPLE CnFMTItt: TOSCQ 1 XAD
I ABl-OT-011-<>6
-------
SAMPLE IDENTITf: MOHAWK 1 XAO
60 UG/ML <> 20 UL/MLI
TOXICIlY
CLASSIFICATION:
PH ALTERATIONS: NONL
COMMENTS ON IKtAIMLMI: b MG Of OftCANIC HATCRIAL
SUPPLIED FOR ItSIINb. SAMPLE UAS SOLVLNT EXCHANGED
INTO 2.0 ML OHSO GIVING A PRIMARY STOCK CONCENTRATION
OF 3 UG ORGANIC PtR UL OMSO.
COLONY COUNTS
01
1— '
oo
01
i — »
en
SAMPLE
NC
VC* IX
VC, 2X
TEST
TEST
TEST
TEST
TEST
TEST
TEST
TEST
APPLTF.D
CONCENTRATION
UL/HL
10
20
0.1
0.3
0.6
1.0
3.0
6.0
10.0
20.0
DISH
ftl
160
135
137
142
153
142
130
129
131
132
135
DISH
112
171
148
151
150
135
150
143
124
129
129
137
'
DTSH
»3
150
149
146
157
140
140
132
129
135
130
S
AVERAGL
COUNT
I
1.0.3
144.0
144.7
149.7
142.7
144.0
t 135.0
127.3
131.7
130.3
136.0
RELATIVE
SURVIVAL*
CPLHCLNT>
100.0
100.0
100.0
104.0
99.1
100.0
93.8
8B.4
i 91.5
90.5
44.0
CLONING
EFFICIENCY
(PERCENT)
80.2
72.0
72.4
NC =~NEr,ATTVE CONTROI , F12 MEDIUM
VC = VFHICIF CONTROL, PF«CFNT GIVEN (-OR Dt*fTHVlSUIFOX IOF
-------
SAMPLE IDENTITY: MOHAWK 2 HAD
IABl-09-007-495)
DESCRIPTION OF SAMPLE: CLEAR, VFLLOU LlOUlO
LBI ASSAY NO.
DATE BFCFIVCO: FEflRUARV H, 1982
TEST DATE: MARCH 4, 1982
VEHICLE: DIMETHYLSULFOXIDF (OHSO»
CELL TYPE: CHO-KI
CELLS SEF.OED PER DISH: 200
TAflLt 4
CLONAL CVTOTOXICITY ASSAY
FCSO VALUE: to TO luu UG/ML <30 TO SOUL/ML*
TOXICITY
CLASSIFICATION: UNDLIERMINLD
PH ALTERATIONS: NONL
COMMENTS ON TREATMENT: 4 MG OF ORGANIC MATERIAL UERE
SUPPLIED FOR TESTING. SAMPLil UAS SOLVENT EXCHANGED
INTO 2.0 ML OMSO GIVING A PRIMARY STOCK CONCENTRATION
OF 2 UG ORGANIC PEK UL UMSO.
COL"NY COUNTS
Ui SAMPLE
1
00
04 NC
VCt IX
VC* 2X
TEST
TEST
TFST
TEST
TEST
TEST
TEST
TEST
r->
:r»
APPLIED
CONCENTRATION
UL/ML
10
30
O.t
0.5
0.6
1.0
3.0
6.0
10.0
20. n
DISH
HI
164
143
150
14R
139
M3
131)
133
125
113
103
DISH
H2
153
148
147
153
153
139
142
143
134 '
12«
110
DISH
03
149
156
148
156
149
145
149
144
137
1?3
S
AVLRAGC
COUNT
i
15b.3
149.0
14R.3
152. 3
147.0
142.3
1 143.0
140. 0
132.0
121. J
106. ti
RELATIVE
SURVIVAL*
JPtRCtNM
100.0
100.0
100.0
102.2
*«.7
95.5
96.0
94.0
'i 88.6
bl.4
11.8
CLONING
EFFICIENCY
CPtRCENT)
77.7
74.5
74.2
NC = NFGATTVF CONTROLt F12 MEDIUM
VC = VfHTCLF CONTROL, PERCENT GIWFN FOR OIHCTHYl SULFOK IDF
s = PHTF. NOT JET UP TO CONSFRVF IIMMFO
•RlLATIVt TO 2X VL FOR 20 UL/ML
TKFATHENT AND TO i* VC FOK OTHER
TRFATMLNT'S
-------
FIGURE 1
RODENT CELL (CHO) CLONAL TOXICITY ASSAY
EC50 DETERMINATION
TOSCO 2 XAD + OMC
A81-07-011-562, 559
CONCENTRATION,
5-187
17
-------
0.1
FIGURE 2
RODENT CELL (CHO) CLONAL TOXICITY ASSAY
EC50 DETERMINATION
TOSCO 1 XAD
AST-07-011-569
140
130
120
«m
10tf
•M
on
« Of)
H
^
£ 7n
cc
Z3
I/)
H-
uj £n
Q£
An
*rU
on
in
•a
^ _
M
; •
-i —
•jti~
X
J
I
>.
•J
I
^
IMB
.
k.
1
k_
• '
! !
^s^
. .
.. ..
1 ' '.
\
JJ —
s
X
i
1
v
V
^
llll
\
\
\
1
\
1
i
\
1
.
\
\
1
\
\
\
-_)
4^
^
^
\
-
^
iy , '
i
1
i
!
1
i
1
•
i
l
— i—
„..
-4
—
....
—
T
i
i
—
100
CONCENTRATION, ill/ml
5-188
18
-------
FIGURE 3
RODENT CELL (CHO) CLONAL TOXICITY ASSAY
EC50 DETERMINATION
MOHAWK 1 XAD
A81-09-007-488
LU
ce
1 10
CONCENTRATION, yl/ml
100
5-189
19
-------
FIGURE 4
RODENT CELL (CHO) CLONAL TOXICITY ASSAY
EC5Q DETERMINATION
MOHAWK 2 XAD
AST-09-007-495
ee.
3
(/)
UJ
»
i
UJ
ee
0.1
1 10
CONCENTRATION, yl/ml
5-190
20
-------
VII. ASSAY ACCEPTANCE CRITERIA
The assay is considered acceptable for evaluation of the test results
if the following criteria are met:
The average cloning efficiency of the CHO-Kl.cells in the
negative controls is 70 percent or greater, but not exceeding
115 percent.
The distribution of colonies in the treated cultures is
generally uniform over the surface of the culture dish.
The data points for each test concentration critical to
the location of the EC50 are the averages of at least two
treated cultures.
A sufficient number of test concentrations are available
to clearly locate the EC50 within a toxicity region as
defined under Assay Evaluation Criteria.
If the EC50 value is greater than 1000 ug/ml, 600 uliters
of aqueous sample/ml, or 20 uliters of nonaqueous sample/ml,
the plotted curve does not exceed 110 percent of the negative
control.
,_ BIONETICS 5"191 21
Utton
-------
VIII. ASSAY, EVALUATION CRITERIA
The EC50 value represents the concentration of test material that
reduces the colony-forming ability of CHO cells to 50 percent of the
vehicle or negative control value. EC50 values are determined graphi-
cally by fitting a curve by eye through relative survival data plotted
as a function of the logarithm of the applied concentration. Each data
point normally represents the average of three culture dishes. In order
to indicate the variability of the data, the high and low colony counts
for each concentration are used to calculate the relative survivals, and
the range is shown by a bar at_the position of the plotted average. If
no bar is shown, the variability was within the size of the symbol.
Statistical analysis is unnecessary in most cases for evaluation.
The toxicity of the test material is evaluated as high, moderate,
low, or nondetectable according to the range of ECso values defined in
the following table:
CHO ASSAY EVALUATION CRITERIA
Solids
Toxicity (EC50 in ug/ml)
High <10
Moderate 10 to 100
Low 100 to 1000
Not Detectable >1000
Aqueous Liquids
(EC50 in ul/ml)
<6
6 to 60
60 to 600
>600
Nonaqueous Liquids
(EC50 in ul/ml)
<0.2
0.2-2
2-20
>20
Evaluation criteria formulated by Litton Bionetics, Inc. for IERL-RTP
Procedures Manual: Level 1 Environmental Assessment Biological Tests1.
Criteria for nonaqueous liquids are tentative and under evaluation.
If the organic or solids content is known, the sample is evaluated under
the solids criteria.
E 5-192
BIONETICS 22
Utton
-------
Another evaluation scheme is proposed for extracts obtained from
SASS train gas volumes. The proportion of the total gas volume corre-
sponding to the volume of extract used in the bioassay is calculated and
expressed as liters of gas per milliliter of culture medium (L/ml) or as
dry standard cubic feet of gas per milliliter of culture medium (DSCF/ml).
A criterion of 1000 L/ml is set as the limit for nondetectable toxicity.
This gas volume corresponds to the average volume breathed""by humans over
a 2-hour period. The subsequent toxicity ranges are defined by 10-fold
dilution steps to conform to standard procedure. The toxicity ranges
are defined in the following table for liter and dry standard cubic feet
units:
Toxicity
High
Moderate
Low
Nondetectable
rrSO In
Liters/ml (L/ml)
10-100
100-1000
>1000
ECg-o In
Dry Standard Cubic Feet/ml
<0.35
0.35-3.5
3.5-35
>35
(DSCF/ml)
|1S- BIONETICS 5"193 23
utton
-------
IX. REFERENCES
1. Brusick, D.J. and Young, R.R.: IERL-RTP Procedures Manual: Level 1
Environmental Assessment Biological Tests. EPA-600/8-81-024, Litton
Bionetics, Inc., Kensington, MD, October 1981, 150 pp.
2. Brusick, D.J.: Level 1 Bioassay Assessment and Data Formatting.
EPA-600/7-80-079, Litton Bionetics, Inc., Kensington, MD, April 1980,-
100 pp.
3. Brusick, D.J. and Young, ..g.R.: Level 1 Bioassay Sensitivity.
EPA-600/7-81-135, Litton Bionetics, Inc., Kensington, MD, August
1981, 52 pp.
4. DHEW Food and Drug Administration "Nonclinical Laboratory Studies;
Good Laboratory Practice Regulations" Federal Register, volume 43,
No. 247, pp. 59986-60020, Part II, December 22, 1978.
5. Proposed Health Effects Test Standard for Toxic Substances Control
Act Test Rules; Good Laboratory Practice Standards for Health Effects.
Federal Register, Part II, volume 44, No. 91, May 1979 and Part IV,
volume 44, No. 145, July, 1979.
6. Guidelines for Registering Pesticides in the United States: Proposed
Good Laboratory Practice Guidelines for Toxicology Testing. Federal
Register, volume 45, No. 77, April, 1980.
m5-194
BIONETICS 24
Lrtton
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing}
1. REPORT NO.
EPA-600/7-84-074b
2.
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
Environmental Assessment of a Crude-Oil Heater
Using Staged Air Lances for NOX Reduction; Volume
II. Data Supplement
5. REPORT DATE
1984
July
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
R. DeRosier and B. DaRos
8. PERFORMING ORGANIZATION REPORT NO.
TR-82-94/EE
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Acurex Corporation
P.O. Box 7555
Mountain View, California 94039
10. PROGRAM-ELEMENT NO.
11. CONTRACT/GRANT NO.
68-02-3188
12. SPONSORING AGENCY NAME AND ADDRESS
EPA, Office of Research and Development
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
Final; 6/81 - 11/83
14. SPONSORING AGENCY CODE
EPA/600/13
15. SUPPLEMENTARY NOTES IERL-RTp project officer is Robert E. Hall, Mail Drop 65; 919/
541-2477. Volume I consists of Technical Results.
. ABSTRACT
volume of the report is a compendium of detailed emission and test
data from field tests of a crude-oil process heater and laboratory analyses of collec-
ted samples. The process heater, burning a combination of oil and refinery gas, was
tested in two operating modes: baseline (normal operation) and with staged combus-
tion air for NOx reduction. The test data include preliminary equipment calibration,
detailed heater operation, and complete flue gas emission measurement results. Ex-
haust gas emission measurements included continuous monitoring for criteria gas
pollutants; onsite gas chromatography (GC) for volatile hydrocarbons (C sub 1 to C
sub 6); and source assessment sampling system (SASS) for total organics in two boi-
Ung point ranges (100-300 C and > 300 C). Organic compound category information
was obtained using infrared spectrometry (IR) with specific quantitation of the semi-
volatile organic priority pollutants using gas chromatography with mass spectrome-
try (GC/MC). Fractions were determined using liquid chromatography separation of
organic extracts with total organic and IR and low resolution mass spectrometry
(LRMS). Trace elements were determined by spark source mass spectrometry
(SSMS) and atomic absorption spectrometry (AAS). Biological assays of organic sam-
ple extracts were also performed.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c. COSATI Reid/Group
Pollution
Nitrogen Oxides
Crude Oil
Gases
Assessments
Flue Gases
Lances
Pollution Control
Stationary Sources
Refinery Gas
Environmental Assess-
ment
Staged Combustion
Air Lances
13 B
07B
11H, 08G
07D
14B
21B
131
13. DISTRIBUTION STATEMENT
Release to Public
19. SECURITY CLASS (This Report)
Unclassified
21. NO. OF PAGES
260
20. SECURITY CLASS (Thispage)
Unclassified
22. PRICE
EPA Form 2220-1 (9-73)
5-195
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|