United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
EMB Report 80-BYC-5
March 1981
Air
Benzene
Coke Oven By-Product
Plants
Emission Test Report
Bethlehem Steel
Corporation
Burns Harbor, Indiana
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SET 1957 07 0181
BENZENE SAMPLING PROGRAM
AT COKE BY-PRODUCT RECOVERY PLANTS:
BETHLEHEM STEEL CORPORATION,
BURNS HARBOR, INDIANA
EPA Contract 68-02-2813
Work Assignment 48
ESED Project No. 74/4J
Prepared For:
Mr. Daniel Bivins
U.S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Emission Measurement Branch, ESED, MD-13
Research Triangle Park, North Carolina 27711
March 1981
SCOTT ENVIRONMENTAL SERVICES
A Division Of
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
Plumsteadville, Pennsylvania 18949
Scott Environmental Techndosy I"0
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TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1-1
2.0 SUMMARY OF RESULTS 2-1
3.0 RESULTS AND DISCUSSION 3-1
3.1 TAR DEHYDRATOR 3-1
3.2 TAR DECANTER 3-3
4.0 PROCESS DESCRIPTIONS 4-1
5.0 FIELD SAMPLING AND ANALYSIS METHODOLOGY .... 5-1
5.1 DETERMINATION OF BENZENE FROM STATIONARY SOURCES:
EPA METHOD 110 AND MODIFICATIONS . 5-1
5.2 SAMPLE HANDLING 5-4
5.3 FIELD ANALYSIS 5-4
6.0 FIELD SAMPLING PROCEDURES 6-1
6.1 TAR DEHYDRATOR 6-1
6.2 TAR DECANTER 6-3
7.0 LABORATORY SAMPLE ANALYSIS 7-1
7.1 SAMPLE PREPARATION 7-1
7.2 PURGE AND TRAP PROCEDURE FOR EXTRACTION OF BENZENE FROM
LIQUID PHASE TO GASEOUS PHASE 7-2
7.3 GAS CHROMATOGRAPH 7-4
8.0 QUALITY CONTROL AND QUALITY ASSURANCE 8-1
8.1 FIELD ANALYSIS PROCEDURES 8-1
8.2 PROCEDURES FOR ANALYSIS OF PROCESS LIQUIDS 8-2
APPENDIX A - SAMPLE CALCULATIONS ' A-l
APPENDIX B - FIELD DATA SHEETS B-l
APPENDIX C - LABORATORY DATA SHEETS C-l
APPENDIX D - EPA METHOD 110 D-l
APPENDIX E - PROJECT PARTICIPANTS E-l
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SET 1957 07 0181 Page 1-1
1.0 INTRODUCTION
Scott Environmental Services, a division of Scott Environmental
Technology, Inc., conducted a testing program at Bethlehem Steel Corporation
in Burns Harbor, Indiana to determine benzene emissions from two sources in
the coke by-product recovery plant. The work was performed for the United
States Environmental Protection Agency under Contract No. 68-02-2813,
Work Assignment 48. This plant was one of seven plants visited to collect
"data for a possible National Emission Standard for Hazardous Air Pollutants
for benzene.
Sampling was conducted at Burns Harbor on September 23rd and
24th, 1980. Integrated air samples and liquid samples for benzene analysis
were collected from the tar decanter and the tar dehydrator.
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SET 1957 07 0181 Pa§e 2~1
2.0 SUMMARY OF RESULTS
Benzene Emission Rate
Process Ib/hr kg/hr
Tar Decanter 9.73 4.42
Tar Dehydrator 3.99 1.81
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SET 1957 07 0181 Page 3-1
3.0 RESULTS AND DISCUSSION
3.1 TAR DEHYDRATOR
The dehydrator holds tar from the decanter at an elevated
temperature for dewatering prior to pumping it to tar storage. Benzene
\
contained in the tar will potentially be removed with the water.
Three Method.110 tests were run on the tar dehydrator with an
average result of 3.99 Ib/hr benzene. The test results are summarized
in Table 3-1. The tests were conducted at one of the three vent stacks
on the dehydrator. (See Figure 6-1). The other two vents were blocked
while the sampling runs were being conducted.
Liquid samples were collected at the dehydrator outlet from a
pump. The liquid samples had a temperature of 162°F and an average benzene
concentration of 1990 ppm.
All stack flowrates were corrected to the average conditions at which
the benzene concentrations were measured in the Tedlar bags; assumed to be
saturated at 68°F and 29.92 in. Hg. (2%% moisture). Example calculations are
shown in Appendix A.
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TABLE 3-1
I
Process Tar Dehydrator
1AK.
Plant Bethlehem Steel, Burns Harbor, IN
Stack
Run Sample Temp.
No. Date Period (°F)
1 9/24/80 1005-1035 149
2 9/24/80 1100-1130 152
3 9/24/80 1202-1232 158
Standard Conditions: Saturated
Liquid Sample Data
Sample Location
Tar Dehydrator Outlet
L)liniUR.AIUK. LIA1H dUMTLRKI
Stack Diameter 4"
CO
w
H
M
VO
Stack Area 0.087 ft2 3
Flow Rate Flow Rate
Barometric Stack Stack Standard
Pressure
(in. Hg)
29.5
29.5
29.5
at 68°F,
Date
9/23/80
9/23/80
9/23/80
Velocity Conditions Conditions
(ft/min) (ACFM) (SCFM)
710 61 38
680 59 36
710 62 35
29.92 inches Hg
f
Sample
Time Temp (°F)
1420 162
1420 162
1420 162
Avg.
O
00
Benzene ^
Benzene Emission
Concentration Rate
(ppm) (Ib/hr)
8615.2 3.97
9968.0 4.30
8816.4 3.69
Avg. 3.99
Benzene Concentration
(ppm by weight)
1956
1834
2171
1987 ppm
fa
00
ro
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SET 1957 07 0181 Page 3-3
3.2 TAR DECANTER
The tar decanter tested at Burns Harbor (Decanter B) was receiving
tar from the primary cooler. There are three vent stacks on the decanter,
which were sampled simultaneously. (See Figure 6-2).
The results of the testing are shown in Table 3-2. The average
benzene emission rate from the decanter (total of all three stacks) was
measured to be 9.73 Ib/hr. Vent A was nearest the inlet and had the
highest measured benzene concentrations, and Vent C, nearest the outlet,
had the lowest.
Liquid sample data is given in Table 3-3. Samples were dipped
from the hatchway in the center of the decanter and from the weir outlet
at the end of the decanter. Average benzene concentrations were 92 ppm
and 4506 ppm respectively.
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©
I
C1 Proct
§ Plani
1
prl Run
9- No.
tvent
1
8 2
3
Vent
1
2
3
Vent
1
2
3
;ss Tar Decanter B
TABLE 3-2
TAR DECANTER DATA SUMMARY
Vent
Stack Diameter 51/2
: Bethlehem Steel, Burns Harbor, IN
Date
A
9/23/80
9/23/80
9/23/80
B
9/23/80
9/23/80
9/23/80
C
9/23/80
9/23/80
9/23/80
Sample
Period
1020-1050
1150-1220
1407-1437
1020-1050
1150-1220
1407-1437
1020-1050
1150-1220
1407-1437
Stack
Temp.
(°F)
109
101
101
108
106
107
107
104
106
Barometric
Pressure
(in. Hg)
29.47
29.47
29.47
29.47
29.47
29.47
29.47
29.47
29.47
Stack Area 0.165
Stack
Velocity
(ft/min)
406
380
475
420
440
620
415
390
460
A Vent B
9 3/4"
C/3
Vent C H
5 1/2" £
^j
ft2 0.518 ft2 0.165 ft2 o
Flow Rate Flow Rate Benzene M
oo
Stack Standard Benzene Emission M
Conditions Conditions Concentration Rate
(ACFM) (SCFM) (ppm) (Ib/hr) -
67
63
78
218
228
321
68
64
76
58
55
69
188
197
278
59
56
66
4760.0
3198.7
4701.6
1819.0
2252.2
2350.8
850.0
1126.1
1207.7
3.34
2.14
3.94
4.14
5.38
7.91
0.61
•0.76
0.96
Total Emission Rate (A + B + C)
Run 1 8.09 Ib/hr
Run 2 8.28 Ib/hr
Run 3 12-81 ib/hr
Avg- 9.73 Ib/hr
Standard Conditions: Saturated at 68°F, 29.92 inches Hg.
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SET 1957 07 0181 Page 3-5
TABLE 3-3
TAR DECANTER LIQUID SAMPLE DATA
Sample Benzene Cone.
Sample Location Date Time Temp (°F) (ppm by weight)
Dipped from center hatch 9/23/80 1525 120 181.6
(between Vents B and C) co .
jo. 1
35.5
Avg. 91.7
Weir Outlet (near Vent C) 9/23/80 1415 178 4387
4637
4495
Avg. 4506
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SET 1957 07 0181 Page 4-1
4.0 PROCESS DESCRIPTION
The processes used at Burns Harbor for recovery of coke oven gas
are primary cooling, tar decanting and dehydrating, turbine exhausters,
tar electrostatic precipitation, Wilputte semi-direct ammonia absorption,
naphthalene scrubbing,;and a hydrogen sulfide absorption. The desulfurization
process is currently not in use at the plant. A process flow diagram of
the gas and liquid streams is depicted in Figure 4-1.
The gas leaving the ovens is collected in the collecting main
where it is sprayed with flushing liquor for initial cooling. The gas and
flushing liquor leave the battery area and are transported from the col-
lecting main through cross-over mains into the suction main and into the
by-product recovery area. The gas and liquid initially separate in the by-
product recovery area at a downcomer where the flushing liquor falls out
and is discharged to the tar decanter and the gas continues to the primary
cooler.
The three tar decanters separate the liquor into tar and water
layers and sludge. Inputs to the three tar decanters are mainly the flushing
liquor from the downcomer, but the middle decanter receives effluents from
the primary cooler sump and common tar sump for the exhausters and electro-
static precipitators. The tar layer at 75°C is sent to the tar dehydrator
where the tar is held at 65°C for reduction of the moisture content from
'10-12 percent to 2-3 percent. There are steam coils on the tar dehydrator
but at the present time they are disconnected. From the tar dehydrator,
the tar is pumped to final storage before sale. From the tar decanters,
the water layer is discharged at 68°C to a flushing liquor tank where it
is stored before being pumped either through a pressure filter to the col-
lecting main for flushing or to cooling and settling basins before deep
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SET 1957 07 0181 Page 4-3
well injection. The sludge is scraped off the bottom of the decanter and
transferred to a ball mill where it is crushed and heated to 86°C to reduce
the viscosity of the sludge before it is pumped to storage. From storage,
the tar sludge is mixed with coal for charging in the coke ovens.
The gas stream at the downcomer goes to the primary coolers at
approximately 80°C. Gas from the wash oil strippers is combined with the
main gas stream before entering the primary coolers. The three primary
coolers are direct contactors, without packing, of the water and the gas.
_2 3
The water is pumped to the primary coolers at 3.5 x 10 m /s (500 gpm).
The water is circulated within the primary coolers twice before indirect
cooling in the circulating liquor spiral coolers. Tars are pumped from
_ o «
the primary cooler sump at 1.3 x 10 nr/s (20 gpm) to the tar decanters.
The gas stream leaves the primary coolers at approximately 32°C.
From the primary copiers, the gas enters the turbine exhausters
where the pressure changes from vacuum to positive. The three turbine
exhausters provide the motive power for the by-product recovery operations.
Some tars are separated in the exhauster and drained to the common tar
sump before pumping to the tar decanter. The gas leaving the exhausters is
approximately 38°C due to heat of compression.
The gas from the exhausters enters the tar electrostatic pre-
cipitators where additional tar is separated from the gas and discharged
to the common tar sump from the seal pots on each electrostatic preceipitator.
There are four electrostatic precipitators, but only three are in operation
at a time.
The gas stream leaving the electrostatic precipitators is injected
with steam to elevate the temperature to 50°C. In the ammonia absorber, the
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SET 1957 07 0181 Page 4-4
gas is sprayed with sulfuric acid in a Wilputte system producing ammonium
sulfate. In this system, the spray is not saturated with salt and a separate
crystalizer is operated by evaporative cooling under' subatmospheric pressure.
Water vapor with entrained impurities passes through steam ejectors in a
cascade. Barometric condensers exhaust the hot condensate to a sump. The
blowdown from the system is discharged to the No. 1 battery quench station
as make up water.
The gas then enters the naphthalene scrubbers at approximately
55-60°C due to the exothermic heat of reaction in the ammonia absorber.
Two of three naphthalene scrubbers are operated in parallel. The remaining
naphthalene scrubber serves as a spare. The gas stream leaving the naphthalene
scrubbers is approximately 35°C before entering the hydrogen sulfide absorber.
Part of the wash oil, rich in naphthalene, is cooled in an indirect spiral
cooler, and part 2.5 x 10" ^ rar/s (40 gpm) is sent to a stripping operation.
A light oil scrubber would operate at 7.6 x 10~^ x nrVs (1200 gpm) as in-
dicated by the plant personnel. The reason for the lower rate is that the
plant only desires to remove the naphthalene from the gas; the light oil
is not recovered but burned with the clean coke oven gas at various plant
combustion facilities. A higher rate of stripping would facilitate removal
of the light oil by the wash oil in the naphthalene scrubber.
The rich wash oil bleed stream sent to the wash oil stripper
passes through a vapor/oil heat exchanger and spiral heater before entering
the wash oil stripper. Condensate from the vapor/oil heat exchanger is
drained to an oil/water separator. The oil from the oil/water separator
is drained to a pump tank and then.pumped to the wash oil stripper. The
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SET 1957 07 0181 Page 4-5
water from the oil/water separator is discharged to a sump (No. 5). In
the wash oil stripper, steam is injected and naphthalene rich vapors leave
the top of the stripper at approximately 155 C and are piped to the gas
stream before the primary coolers. The stripped lean wash oil returns
through the vapor/oil heat exchanger to the suction line of the top re-
spray pump of the naphthalene scrubber.
An oil/water sludge layer accumulates in the naphthalene scrubber
and is drained to sump No. 5. The oil and water in sump No. 5 are pumped
to an oil/water separator. The separated oil is returned to the wash oil
layer in the nap'thalene scrubber and the water layer is pumped to another
sump (No. 8). The water in this sump is then used as makeup water for
quenching of the coke.
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Page 5-1
SET 1957 07 0181
5.0 FIELD SAMPLING AND ANALYSIS METHODOLOGY
5.1 DETERMINATION OF BENZENE FROM STATIONARY SOURCES:
EPA METHOD 110 AND MODIFICATIONS
EPA Method 110 consists of drawing a time-integrated stack gas
sample through a probe into a Tedlar* sample bag, which is enclosed in a
leak-free drum, by use of a pump hooked to the drum outlet which slowly
evacuates the drum, causing the bag to fill. A copy of the method is
included in Appendix D.
The method was modified by Scott because as it stands the
method doesn't account for moisture in the sample stream, and is only
designed to measure benzene concentration, not mass emission rate. The
following modifications were made to all tests done using Method 110:
1. To obtain mass emission rates, velocity and temperature
readings were taken at the top of the stack at 5 minute intervals during
the 30-minute sampling runs. This information was used to calculate flow-
rate, which was used in conjunction with the benzene concentration to
yield the mass emission rate. Velocity readings were made using a vane
anemometer with direct electronic readout.
2. A personnel sampling pump was substituted for the pump,
needle valve, and flowmeter of the method. The personnel pumps have
built-in flowmeters and rate adjustment screws and have the further
advantage of being intrinsically safe, as required in many areas of
the coke plant.
* Mention of trade names or specific products does not constitute endorsement
by the U.S.. Environmental Protection Agency.
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Page 5-2
SET 1957 07 0181
3. Swagelok fittings were used in place of quick-connects.
4. Rather than discarding Teflon sample lines after each set
of samples, they were washed with propylene carbonate and/or acetone and
flushed with nitrogen before reuse.
5. An orifice and raagnehelic gauge were inserted in the sampling
line before the Tedlar bag to indicate that air flow was reaching the
bag.
6. A water knockout trap was inserted between the probe and
magnehelic gauge to collect any condensate in the sample line.
7. The following cleanup procedures were followed:
If any condensate was collected in the trap or sample line, it
was measured and saved for analysis. The probe, line and trap were then
washed with propylene carbonate, which was also saved for analysis. Any
benzene found in these washes and water catches was added to the total found
in the sample bag to determine mass emission rates.
Bag volumes were measured whenever water was collected in the
trap by -emptying the bag through a dry gas meter after the sample was
analyzed. The volume of water collected in the trap was then converted
to an equivalent air volume and was added to the volume in the bag to
determine the percent moisture in the sample stream.
After the probe, line and trap washes were completed, the lines
were washed with acetone to remove the propylene carbonate film and flushed
with nitrogen to dry.
Figure 5-1 shows the modified Method 110 setup.
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SET 1957 07 0181
Page 5-3
FIGURE 5-1
Stainless Steel Probe
•Swagelok Fittings
Stack
Teflon Sampling Line
Water Knockout Trap
/Magnehelic Gauge
-Tygon Tubing
•Personnel Sampling
Pump
Leak-proof Barrel
Tank
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MODIFIED METHOD 110 SAMPLING TRAIN
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SET L957 07 0181 Page 5-4
5.2 SAMPLE HANDLING
. After being collected the gas samples were immediately
transported to the gas chromatograph and analyzed. The elapsed time
between sample collection and analysis never exceeded one hour.
To verify that there was no sample degradation in samples of this type
some of the samples were retained for 24 hours and reanalyzed. The
loss of benzene and isobutane observed was typically less than 5%.
5.3 FIELD ANALYSIS
All gas samples collected were analyzed using a Shimadzu
GC Mini 1 gas chromatograph equipped with dual flame ionization
detectors, dual electrometers, heated sample loop and a backflush
system. Figure 5-2 shows a schematic of the backflush apparatus.
The backflush system is composed of a ten port sequence reversal valve
and two columns, a scrubber column for retaining high molecular weight
compounds and an analytical column. When the system is in the inject
mode the scrubber column and the analytical column are connected in
series allowing sample components to move from the precolumn to the
analytical column. In the backflush mode the columns are disconnected
from each other and become two separate systems each with its own
carrier gas source. This arrangement allows the separation and measure-
ment of low molecular weight compounds while the scrubber column is
being backflushed of heavier sample components. Backflush times for
different mixtures of sample components must be predetermined to insure
that the compound(s) of interest are transferred to the analytical
column before backflushing is started.
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.
\ ^
•n
n
(D
Ln
I
NJ
A >
CARRIER GAS A
A
*'
CARRIER GAS B
PREP, COLUMN
.•u
(j
m
I v
I «'f
L/l
ANALYTICAL COLUMN
SAMPLE INJECTION
INJECT
A, D, E OPEN
B, C CLOSED
BACKFLUSH
A, E CLOSED
B, C, D OPEN
GC COLUMN CONFIGURATION WITH BACKFLUSH
DETECTOR
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SET 1957 07 0181
Page 5-6
Samples for chromatographic analysis were drawn into a 20
cc glass syringe then introduced to the sample loop inlet. The
samples once in the sample loop were allowed to come to atmospheric
pressure by waiting 15 seconds prior to injection. The following
chromatographic conditions were maintained:
Column Temperature (isothermal) - 100 C
o
Injector and Detector Temperature - 200 C
5 ml Sample Loop, Temperature
Carrier Gas Flow Rate
Hydrogen Flow Rate
Air Flow Rate
Analysis Time
Detector
- 50° C
- 32 cc/min.
- 40 cc/min.
- 240 cc/min.
- 5 min.
- Flame lonization
The columns used for field analysis were:
A - Scrubber Column
10% FFAP on Supelcoport 80/100
1/8" x 1 m Stainless Steel
B - Analytical Column
20% SP-2100, 0,1% Carbowax 1500
100/120 Supelcoport
1/8" x 10' Stainless Steel.
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SET 1957 07 0181 Page 6-1
6.0 FIELD SAMPLING PROCEDURES
6.1 TAR DEHYDRATOR
Three Method 110 test were conducted on the tar dehydrator.
As shown in Figure 6-1, the dehydrator has three vents, which are normally
all open. Sampling was conducted at the end vent nearest the stairs as
marked on the diagram, and the other two vents were blocked off during
testing. Ideally all three vents should have been sampled simultaneously,
but the end vent furthest from the walkway was not safely accessible for
sampling. Since only one vent was sampled, the calculated mass emission
rate of 4 Ib/hr is possibly low. The maximum emission rate could be as
high as 12 Ib/hr (3 vents x 4 Ib/hr) although this is not considered likely
because field observations revealed that no steam plume emanated from the
test vent until the center vent was blocked, since the center vent, was
lower and'of larger diameter, and located within 5 feet of the test vent.
The vent on the far end had an observable plume before it was blocked.
Also, the prime driving force of the emissions is the volatilization
of organics in the heated tar, which would not be affected by closing the
vents. The only change would be the elimination of breathing losses
through those two vents. For these reasons, it is estimated that the actual
emission rate is on the order of 6 to 8 Ib/hr maximum.
The moisture content of the stream was about 30%, i.e. saturated,
as determined by the volume of condensate collected in the water trap and
the sample volume in the bag.
Liquid samples were collected from a pump at ground level at the
dehydrator outlet.
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SET 1957 07 0181
Page 6-2
S/DE VIEW
BLOCKED
BLOCKED Do«\K>G-
o
VI
L
K
A
Y
TEST
POINT
PLAN VIL
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FIGURE 6-1 TAR DEHYPRATOR
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SET 1957 07 0181 Page 6-3
6,2 TAR DECANTER
Three sets of simultaneous Method 110 tests were conducted on
the three vent stacks on the tar decanter. Figure 6-2 depicts the decanter
and shows the.locations of the vents and the hatchway and weir outlet
where liquid samples were collected. All hatchways were closed during sampling.
The tests were run according to the revised Method 110 procedure
outlined in Section 5.1, except that one of the sampling trains did not
include the magnehelic gauge because only two were available. No problems
were encountered with the sample line plugging.
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SET 1957 07 0181
Page 6-4
COLLECTING MAIN
HA TC H WA y $M AI~L VEN TS
H-E. CANTER
in
-'c
INLET
5"
12'
HATCH MV
'
DECANTER VT
Wei f? OUTLET
VE"NT A : 5 '2 " ID-
VENT 8 : ^ ^"'l.^
C :
DECANTER
LIQUID LEVEL - Z +>
v£r>rrs ABC — ID-IT.
•*
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FIGURE 6-2 TAR DECANTER "B1
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SLT 1957 07 0181 . Pa8e 7~L
7.0 LABORATORY SAMPLE ANALYSIS
Two types of liquid samples were collected: process liquids, and
sample line and water trap catches and washes. All liquid samples were
stored in amber glass bottles and returned to Scott's Plumsteadville laboratory
for analysis.
7.1 SAMPLE PREPARATION
Depending upon the complexity of the sample, one of the following
sample preparation procedures was followed prior to the "purge and trap"
procedure and analysis.
Samples Containing Immiscible Liquid Phases
Using a clinical centrifuge (International Equipment Company,
Massachusetts) immiscible liquid phases were separated and each phase was
analyzed separately for benzene.
Samples Containing Solid and Immiscible Liquid Phases .
Samples containing solids of higher density than the liquid phase
were separated by centrifuge or by simple decantation of the liquid. The
different phases in the liquid fraction were then further separated by
centrifuging. Solid and liquid phases were analyzed separately.
Samples Containing Finely Crystalline Solid Suspension
In analyzing these samples the stoppered sample jars were shaken
for at least half an hour for homogenizing the solution. The uniform
distribution of suspended fine crystalline solid particles was tested by
determining the percentage of dry solid in several aliquots of the homoge-
nized mixture. A weighed amount of the mixture was analyzed for benzene.
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SET 1037 07 Old Page 7-2
Sampl. inr. System Washings
All washings were clear solutions having only one liquid phase.
The total weight of the liquid phase was determined using a balance correct
to ±0.1 g. The total weight of each washing WcS more than 25 grams, so an
error of 0.1 g in weighing the mass will contribute an error of only 0.4%
to the final analytical data. A weighed aliquot of the washing was analyzed
for benzene by following the "purge and trap" and analysis procedures out-
lined in the following sections, and using this analysis data the weight
of benzene present in the total mass of washing was calculated.
7.2 PURGE AND TRAP PROCEDURE FOR EXTRACTION OF BENZENE FROM LIQUID PHASE
TO GASEOUS PHASE
An accurately weighed quantity of the sample to be analyzed was
diluted with 20-25 ml of propylene carbonate in a .specially designed glass
purging apparatus which was kept immersed in a thermostatted water bath
maintained at 78°C. Benzene free nitrogen gas was bubbled through the
propylene carbonate solution in the purging apparatus at the rate of
0.2 - 0.3 liters/minute, and collected in leak free Tedlar bags. Under
these experimental conditions, 1 1/2 - 2 hours were sufficient to purge
off all the benzene from the liquid phase to the gaseous phase. The total
volume of nitrogen gas used to purge the sample was accurately measured
by a calibrated dry gas meter. A diagram of the purge and trap set-up is
shown in Figure 7-1.
Propylene carbonate was found to be an ideal diluting solvent
for the extraction of benzene from all types of liquid samples containing
viscous tar, pitch, light and heavy oil and insoluble particulates. It
was chosen for its high boiling point, low density, and good, solvatrng
capacity.
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DM OA.S HtTEP.
. FLOW
CONTAINING SAMPLE
FIGURE 7-1 PURGE AND TRAP METHOD EQUIPMENT SET-UP
I
U)
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SET 1957 07 0181 Page 7-4
7.3 GAS CHROMATOGRAPH
A Perkin-Elmer 900 gas chromatograph was used for the analysis
of the purge bags. A 10 ft. by 1/8 inch stainless steel column packed with
20% SP-2100/0.1% Carbowax 1500 on 80/120 mesh Supelcoport was used for the
analysis. This column gave complete resolution of the benzene peak from
other components present in the purge bags. The 'peak height' method was
utilized to calculate the concentration of benzene in the purge bags
analyzed. The Perkin-Elmer 900 used for analysis was not equipped with
a backflushing unit. Gas chromatograph conditions were as follows:
GC column temperature: 70°C isothermal
Detector temperature: 190°C
5 ml loop at a temperature of 120°C
Carrier gas flow rate: 30 cc/min He
Hydrogen flow rate: 45 cc/min
Oxygen flow rate: 400 cc/min
Detector: Flame lonization Detector (FID)
In addition to benzene, the purge bags contained other volatile
hydrocarbons present in the liquid samples such as toluene and naphthalene.
Because this chromatograph was not equipped with a backflush, it was
necessary to elute all heavy organics from the column by heating the column
to 150°C after every two injections for one hour with the carrier gas on.
After cooling the column to 70°C the absence of any organic in the column
which might overlap the benzene peak in the next analysis was checked. When
the column was found to be satisfactorily clean, the next analysis was
continued under the conditions previously described.
Scott Environmental Technology Inc.
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SET 1957 07 0181 Page 8-1
8.0 QUALITY CONTROL AND QUALITY ASSURANCE
The following sections will address quality control and quality
assurance procedures for the: field analysis of benzene in air samples and
the laboratory analysis of process liquids.
8.1 FIELD ANALYSIS PROCEDURES
All samples were analyzed in duplicate and as a rule peak heights
were reproduced to within 5%. For some very high concentration samples
(percent range) it was necessary to make dilutions for analysis. When this
was done a fresh dilution was prepared for each injection and peak heights
were reproduced to within 10%. To verify that the system was retaining no
benzene, frequent injections of the standard and nitrogen were made. In all
cases the result was satisfactory.
The Tedlar bags that were reused for sampling were flushed three
times with nitrogen and allowed to sit overnight after being filled to
approximately three quarters of their capacity. They were analyzed for
b.enzene content the following day. The background concentrations of the
bags were recorded and varied from 0 to 10 ppm benzene. Care was taken to
use sample bags whose background concentration was very low compared to the
expected concentration of the source.
The accuracy and linearity of the gas chromatographic techniques
used in this program were tested through the use of EPA Audit Samples. Two
standards, a 122.5 ppm and 6.11 ppm benzene were used to analyze the audit
cylinders.
Scott Environmental Technoicsy Inc
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SET 1917 07 013L Page 3-2
8.2 PROCEDURES FOR ANALYSIS OF PROCESS LIQUIDS
Scott's benzene standards, checked against EPA Audit Standards,
were used as reference standards throughout this program. The accuracy and
linearity of the gas chromatographic technique for benzene analysis was
tested through the use of EPA Audit Standards which were available to Scott.
Gas chromatographic analysis of the samples and standard were performed
under identical conditions to assure the accuracy of the analytical data
generated.
Each batch of propylene carbonate which was used as the diluting
solvent in the purge and trap technique was analyzed for benzene content by
subjecting 25 ml of propylene carbonate to the purge and trap procedure
followed by gas chromatographic analysis of the trapped gas under identical
conditions as described in Section 5.2. All batches of analytical grade
propylene carbonate were found to be free from benzene.
Every day before the analysis of samples the purging apparatus and
trapping bags were tested for absence of benzene. Whenever the whole system
was found to be free from benzene to the lowest detectable limit of the.
instrument, the samples were analyzed using the purging apparatus and the
trapping gas sampling bags.
Generally an accurately weighed mass of each sample was subjected
to purge and trap procedure only once and the trapped gas sample was repeat-
edly analyzed by GC until the analytical data of consecutive GC analyses varied
by ±0.5% or less.
Scott Envfronn^ntarTcJChnoto Inc
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SET 1<}57 07 0181 afie ~3
For randomly selected samples, the whole analytical procedure was
repeated with a different weighed mass of the source sample to check the
validity and accuracy of the analytical methodology. The analytical data
for different runs were found not to vary by more than 5%.
By purging the sample with nitrogen under the experimental con-
ditions as utilized by Scott, the recovery of benzene from the sample was
quantitative and this has been verified by analyzing a standard benzene
solution in propylene carbonate containing tar and pitch.
Scott Environmental Technology Inc.
-------
Page A-l
APPENDIX A
SAMPLE CALCULATIONS
Scott Environmental Technolosy Inc
-------
SET 1957 07 0181 Page A-2
APPENDIX A
SAMPLE CALCULATIONS
1. Calculation of percent moisture from water catch and bag volume
Example: tar dehydrator, Run 1
Water trap catch volume: 13 ml
Tedlar bag volume (gas sample): 45.43 liters
Gaseous volume of collected water, standard conditions:
• 10 1 1 gm 1 mole 24.15 1 ... .. , .„
13 ml x —521- x -7-5 x ; = 17.44 liters
ml 18 gm mole
Percent moisture:
17.44
17.44 + 45.43
x 100 = 27.74%
2. Flow rate at standard conditions (saturated at 68°F, 29.92 inches Hg)
A. Correction for temperature and pressure:
528°R
Flow Rate (STP) = Flow Rate (source) x
T(°F) + 460 29.92
Example: Tar dehydrator, Run 1
r00 OQ C
Flow Rate (STP) = 62 cfm x ~ x = 53 cfm
B. Correction for moisture:
Percent moisture (stack conditions) = 27.74%
Percent moisture (saturated at 68°F) =2.5%
Flow Rate (dry) = Flow Rate(STP) x (100 - % Moisture)/100
= 53 cfm x (100 - 27.74)7100
= 38 cfm
Flow Rate (saturated at 68°F) = Flow Rate (dry) x 1.025
= 38 cfm x 1.025
= 39 cfm
Scott Environmental Technology Inc.
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SET 1957 07 0181 Page A-3
3. Calculation of mass emission rate
Example: Tar dehydrator, Run 1
Flow Rate (standard conditions) = 39 cfm
Benzene concentration: 8615.2 ppm
39 ft3 28.32 1 60 min 8615.2 78 g 1 mole 1 Ib , .. ....
: x ~— x — x 2— x —r-3- x —.—. c ,• x -r-=-.— = 4.06 Ib/hr
mm ft3 hr ±QO mole 24.15 1 454 g
Scott Environmental Technology Inc.
-------
Page B-l
APPENDIX B
FIELD DATA SHEETS
Scott Environmental Technology Inc.
-------
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
Page B-2
PROJECT 1957 07 0181
PLANT:
f
PROCESS: Tn
PROCESS NOTES:
METHOD 110 DATA SHEET
DATE:
AMBIENT TEMPERATURE:_
BAROMETRIC PRESSURED
TEDLAR BAG NUMBER:
BAG f\
4-
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
lo:o5 0
^'00
5
/I
nJL . /v
tb
ISO
"7oo
S.
$0
3.5
GOO
65-0
O
5
in
IfT/
6
1
&3D
76-0
o
Gt 0 PPM
o
. 2I.9O x?
7-
G/
57
-------
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
Page E-3
PROJECT 1957 °7 0181
METHOD 110 DATA SHEET
PLANT: KvOlo M\/,f?6r~ DATE: ' I / K\JW
TIME
5
1
2x0
36?
31 j
0ffVf"<5
4-
^3-
V ^
;^
^7
34
4-
Cf
1 S
an
^(C,
3o
STACK TEMP
If/ °^
j fl ^ * £-
10 6 ° p
/! / °P
il 0
5
Kl;rw
loa °-P
(o^l
' /DO
'/ #0 *^^
/O)
/ /"i "~>
I 0 ,A
ftt/rvJ
(0^ °^-
10^
100
/oo
ID i
. ^
GAS VELOCITY
^^C ?p^
4 00 Can
3°|0 -fp^,
^00
3^o
A $ft(5 G-
'
330 U,
3^0
?Zo
3oo
3 10
^O A
y cvu
-2, f? A ^ ^
"?:> 5 0 -T p ;r1
<35"0
-7^0
5" 00
^ 'c\ C
^foo
R BAG NUMBER:
I , cw / v S4 6- B
PUMP FLOWRATE
*
t
.
(
.
-------
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
Page B-4
PROJECT -1957 07 0181
PLANT:
METHOD 110 DATA SHEET
PROCES s ; ~Y& v.A ft c a
PROCESS NOTES:
6
DATE:
AMBIENT TEMPERATURE:
BAROMETRIC PRESSURE; A^-^ "7
TEDLAR BAG NUMBER:
TIME
STACK TE-IP
GAS VELOCITY
PUMP FLOWRATE
3
~> \ 0 4-
9
I 03
10 '-1
10
//
"
W
3^0
3
3 ^ o' A?
o d
[0^7
-------
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
Page B-5
PROJECT 1957 07 0181
PLANT:
METHOD 110 DATA SHEET
DATE:
PROCESS;
PROCESS NOTES:
/s C
AMBIENT TEMPERATURE; "^ \
BAROMETRIC PRES SURE; ^
TEDLAR BAG NUMBER:
\ ,.C/M 4, &AG-
TIME
STACK TEMP
GAS VELOCITY
PUMP FLOWRATE
in:ZO 0
7
• YOG
Vf-
JOS
' 3*8-0
3
; -'
^' L
-------
PROJECT 1957 07 0181
SAMPLE DATA
Plant Dt/jg/V'£ n&rbo& Process T/|£ c( Qf ft ft/ri? i^" Date
Sample No. Trt^ PiC0\ W\~£Y~ ' (—, ."~7> Time Sampled J i o 5
v-^ -_^_
Sample Type:( Liquid Air
• . i ~) o 'J r
Sample Temperature /
-------
. Page .01
APPENDIX C
LABORATORY DATA SHEETS
Scott Environmental Technology Inc.
-------
Project No. 1957 07 0181
CHROMATOGRAPHIC ANALYSIS LOG
7
Date
Analyst
w
H
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
cc
Vo
x/o
I
-------
tf
o
Project No. 1957 07 0181
CHROMATOGRAPHIC ANALYSIS LOG
Date *?/
Analyst 1
Crt
w
H
Time
Sample Identification
Peak
Height /Area
Concentration
Factor
Concentration
Comments
\0
tx
-------
X1
O
Project No. 1957 07 0181
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst
en
M
H
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
.* /o
Bo
-------
X*
o
Project No, 1957 07 0181
CHROMATOGRAPHIC ANALYSIS LOG
Date
Analyst
(T~O
CO
w
H
Time
Sample Identification
Peak
Height /Area
Concentration
Factor
Concentration
Comments
57
1 "SCe X to'
rv--,
-------
tf
o
Project No, 1957 07 0181
CHROMATOGRAPHIC ANALYSIS LOG
Date
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
X'O
.
*
A
os
(oo-o
VO
//O
?o
-------
X*
o
CHROMATOGRAPHIC ANALYSIS LOG
Project No,
Date
3-
Analyst
M
en
W
H
Time
Sample Identification
Peak
Height/Area
Concentration
Factor
Concentration
Comments
& Jl /O
-------
Page D-l
APPENDIX D
EPA METHOD 110
Scott Environmental Technokxjy Inc
-------
i. -t:i. Xo. 7" / I-';:-! -V. A:v;! lii, i'
2G677
• •I'-.'M'n1!! (- 'i:1.!''!'.:!1!. arnKxinrt. and \:.<.:.i
;.-::o;''i, :•;;;] i';.1: •-.•;! ch successive' 15-nunute
!' ' ••••'•
;..; '.'•.•.•::!-"•••: or o^rrttcr;; of ;;!!
i.'! a;:ci.i\i.iace iviir, ;iii.s .vii.'.'.vrt sn.'-ii
c'v.-c'-v t!i!-: ;:.::? :.:-.d span dr.i:r..'.--.i'ir;;r. The
iTni:'.'.:I'i;c!Mnjr niust have rncuntmeniicu a-
•.•.axiiv.i;.".; shcl! l!:'j i'-jr c":^h cy'ir.dijr so
;4 's .-•iniuidi Js will i:Oi be used i; iiu:ir
.... .
~5 ;M::'"I:;I; i:o::i thf: Ci'i'iiii'jiJ Vulau. li:s:
d.i!.:: of ,qas cviir.d'ir priiparfilion.
r.c-lifiod hcr.ZL'ra: concentration, and
r;-. oi'ina'tit'nd mavim!:r\ shrif ti-'r> r;u;:;t
h. ••.;•'.: bri.'n ;:i;'i.\f;i.l to the ryii;ider b fibre
i:::;i;n(>r!t fron \\;a s^np'.if.ir.tiirc;1 to 'ii'3
bu\ ur !i a ,ua3 c:;:T-;r;:Uo^ra;:h ;.: usciJ as
I:-..: civ.tiy.v.o'.is :r.o-.',itjri::^ svst^n-. ihesc
•.;.:S irii.xi'ji'i-s iHi'.y be used (iircctiv to
prepare a ctirurp.ntcrrsph calibration
-•>::•>••.; as dyscrihod i.i Sfjlicn 7.C of T^st
Mjthoil 110 fcr ci;:t: "cation of cylinder
.:: bv !'•..' Ai';:;:;':^t:':iior for a
r!i:i::r.ii:n ot 2 \T".i"i.
l.i..S.C. ni i1!
App-:r.:Ji\ '! — Ti-«u.'.i:nc From
St.'ili'jn;!ry Soun.i;*
Pn [(>:•:;•.. i net: of t!:is netho.i .-:hi;-:!d not be
titii'iv1'--;! I'v p"rs-ir.a rr^i::!:!' sr v.-ith '!:!•
'•.;--'-.i:i.i;i nf .1 -.;;, •.:-.— r- :;•••;-.:;-!:. r:i;r by
ihLiu;; v. ho j.-f; i:-i!'j;::ii.-r -.. ,'h :,.iar>:t!
s.-ur.piirr.:. !)•..":. ins;: k no •-•.•:•. i'';f b"ynnd the
scop-: n ! this proscnt.ition ;.; rrn'.i'rcd. Care
must be <:xi:riased to prf.". iir.t exposure of
s.implir.5 pi-rsonny! to benxfr.a, a
1.1 Applicaliiiiry. This r.viho-J applies to
tho mea.surt.>:ru;nl ot biinzune in stack gases
from pnxL'-vs ,ij ;:poc:;'ii;d ia Ins
rcj;i:l;itii.n.-5. 'ih-: nicthocl don.s not ron.iove
bi;rizer.o r.uatair.cd in p.irtlcuiatB niatti.T.
1.2 Prir.ciple. An i-tenr:'t'"J !)••:? s.-'mple of
slar.k ^;as r.oatrtiair.,'-1 i.>enx^r'.^ and O!'.:I.T
ov;!;ii!i(;s is h'jijjuctcd 10 gas chroma io^raphic
(CCj aa.,i;. .-a... U;>;n;4 J i'iaiau ionizjtioa
detector |K:D).
2. fiar.yv and Sensitivity
'tin; ran :c ui i.::s "iciriod io D.I to TO ppm.
Tho iippc:- ;.::•:; may bs extended by
extrtf.di:;.- the calibration ra~3u or by diluting
Thn chr'.-.v.itn-iv.ph columns nr.d ;hs
corrfipen;::;^ opjra:;"^ pararnot^rs iurcia
.•.'Kricri.'iiid ':,'r:;:.i!;v n-xv;.<:o an aiii'euale
n.v-i.'iiiiirn i>f !;""..-.iT.i\ hnv/.-i'iT. rcMjintioti
intorferi;iii;i!S tr.ay iin encountered on some
source's. Ti; ':vfuri:. lha chrori'.'j Aiyraph
ci::jrat::r sh:'.;l select the column and
>"!p.'r:!!ir"4 :.::r~a;-;;;r3 b"s! svii:r;d to his
p-irtici:iar arialy?^ probii'"-.. subjnct to the
annrov,:! of thi; . \-Jivni..:.". -tni'. Apivriva! is
analysis \vi;h a uiifcie.'t column or CC/mass
spectroscopy, and has the data available for
review by thi! Ad.Tur.isi'r.i'uir.
•J. /li'piv;';;.';:.?
•!.l San-p'.inj (s,:e Figure UO-1). The
sa.n:p;iu^ train consists of the following
•l.l.t Prol1.;. S:,iin!:'S3 steel. P\ro>; ' glass.
permits!. ('"'t'.iiypi.'J v, !;h a j:i,.^s woo! plug to
ri'i'.'.uvi; pa.'ii; ::;ato ~J!'CT.
•4.1. 2 Siir::;:''j I.i.-.i'-s. T;:fle;\ G.-i r\::i outsido
Ji;i;ni'';i-r. oi -'.'i^ci'.'p.t '.r?.-.'';i U' rop.'.ii.'Ct
ea,:h s::;'i:'5 nf b:v: s.impij's that r:::'..::i;.::es an
emission test ui'.d discard upon cumplttion of
the H:st.
•!.).r> Q'l-i.'s Connor;?. S'.'ii-.l^s.s s'.'f?!.
mcili; ;_i ;sr.d li-.r.a'iL' (-). v, nil ii.iii i :n.-cl\s (one
u1- shown in ii^iiro 11(>-
•1.1.4 T-.-.ll.ir or aiimv-i-.cd M;. Lir bags. 100
i. capacity, !:> Ciintaiii 'i.^iioli.'.
•J.1.5 '[J-i.; Cuii!ji.:i:rs. i?a;jiJ Iccikptonf
protect con.li'ats fr:;:a Si:.~.li':ht.
•t.l.G \«'ed!e Vu!v iho
average nois.; lavel. (R.'.-'.ionse is measured
from thii iivcra'.ifl vaii!" ••••( 're b::^;i ''"e to the
maximum of the ivu\tifi.T~:. v. h;!-: ?'. itidard
oporuting conditions are in usa.|
BILLING COOS 6560-01-M '
-------
FILTER
(GLASS WOOL)
•I iV-i^r / Vol. 43, No. 77 / Frir.Lv. /vor;'. i ' ir::;0 / PIT-'JO.-:;.--! ilnioj
^.:^\:,vr^
rt?^^^
STACK WALL
l/x
PROBE
TEFLON
'SAMPLE LINE
OUiCK
COr-JNECTS
FEMALE
TEDLAR OR
ALUMINIZED
MYLAR BAG
FLOW METER
CHARCOAL TUBE
\
PUMP
RIGID LEAK-PROOF
CONTAINER
Figure 110-1. Integratocl-bag sampling train. (Mention of trade names or specific products
does not constitute endorsement by the Environments! Protection Agency.)
BILLING CODE 6560-01-C
-------
'-.»(•<• / V,'!. -Fv \'n. 77
,!. ! -•• .! '-i 1..-.V. i .••,>:: .!;.-.; tr ,y i.se other
st • .:.irus are i:.-i ::::," ii:-.'d ar.d i:c has
t.1'.."':'• ii':> .idi''.'iiii'o ri'.v.'iiition of tho
lii.:v;r.-.- pr.ik. (.\::.-.T.,-,!'e reioiutioii •::
di •:.:..-.; ,K ',:n .in'.i f>v.:,-J.ip of p.'if mnrr- than
10 \. :,....".t of ti'.i; hen-ec.e peak by an
ir.ti : :• r 'i'.l p!;:'k. C.i!c;:!.it',Piri of nrea ovnrl.ip
;•; ••••-,•! .ncd in Arpi'r:;:i\ E. Suppiomenl A:
.... -.. ..
4 .T.J.I Column A: IIsT.r.erie in tr.t: Presence
of A!irtha!ics. Staii-.l'.'ss s'erl, 2.44 m by 3.2
mm. cont.iinina 10 percent 1.2.3-tris (2-
cyiip.cKihox'v) propi'.no (TCMP) on );0/100
Chromosorb P AW.
4.3.2.2 Co:::~:i B: !.'en-enfi \\'-.i\\
S?p-ir-:ion nf the ! -.-imers of X\ iene.
Stainless sleel, l.fl.3 m by 3.2 run. containing 5
pcrccr.l SI' 1.200/1.73 percent De:itonc 34 on
100/120 Suplecoport.
•1.3.3 Flow Meters (2). Rotameter type, 100
mL/rr.in opacity.
4.3.4 Ga; Regulators. For required gas
cylinders.
4.3.5 Thermometer. Accurate to 1° C, to
measure temperature of heated sample loop
at time of sample injection.
4.3.G Barometer. Accurate to 5 mmM.q. to
measure atmospheric pressure around gas
r.hro::'..i!'.\o,r'!ph d'.'rlr..1! ';a™p!u aaa'.Yiis.
4.3.7 Pump. Leak-free, with minimum of
100 mL/niin capacity.
4.3.3 Recorder. Strip chart type, optionally
equipped with t.-i'.her disc or electronic
i.-!i.'j)ru!cir.
4.3.3 Plunimeter. Optioruii. in place of disc
or electronic integrator, on rucordsr, to
measure chiomalc-firaph peak aross.
4.4 Calibration. Sections -1.4.2 through
4.4.5 are for the optional procedure in Section
7.1.
4.4.1 Tubing. Teflon. 0.4 mm outside
diameter, separate pieces marked for each
calibration consent ration.
4.4.2 Tcular or Ahiminized Mylar Bags. 30
I. capacity, with, valve: separate bag marked
for each calibrali;:.; cor.--jr;l.-.itio:i.
4.4.3 Syrin.;-js. 1.0 ;iL ar.u 10 p.L. "as ti-ht.
individually calibrated to dispense liquid
benzene.
4.4.4 Dry Gas Meter. With Temperature
and Fjvsiiire Gaujiis. Accurate to ~2
pcrcrnt. to meter nitre.::-.1"! in preparation of
siancarJ yas niixtures. calibrated at the How
late used to prepare standards.
4.4.5 Midjet Impir.gt.'r;hio! Plato
AfSi!.'"!.1!;. . To vaporise; brnznno.
UfC ijr.ly riTinnnts that are of
chrunatrj'raphic sratlu.
5.1 .'-.r.alvsis. Tiie fjllo'.vinq are needed
fo:-s.-:-..iiy.'!:i:"
S.1.1 i .':?liurn or .\'i'.ro;_oa. Zero gradfi, for
chro.T.ato^rapii carrier CMS.
5.1.2 il\virogcM. Zrro ;;rads.
5.!.?. CK;..^or. cr .\ir. Zero grade, as
r.-.nil.n: 'f.1 thn i:i'ii:::tor.
3 J l!..!.i]r.!t:r:n. Usy cno f>f the following
ppti'i:-.-" t-.'hiT 1.2.1 :!i;;l "i.: ?..".. cr 5.2.3.
.">- ! i. ':. .:•:•.•'.<•• I :.'.„{ i'erc^nt Pus;:.
(.-." :i • ..'.••:•'.' n::i::i:f.:^;arer '.; cnntain a
minimum <>('.•'• Mi'l purrent uiT.i'.'nc: tor ess
in :!':.? pr. p.!r..:..;a ••}'. .sianu'.iril ;: .-. i::i\U:ri.s
;i.i d."i!-rii;-'.| i;; S.-:-ti(!r. 7.1.
." 2.-' .Nitre-.'- n. /"'TO i.::.n!i'. :".•: .•:':ipar.i!inn
of standard jjas nnxturw as lii::'.-:: :in:d in
bn:\;<-.\ 7.1.
5.2.3 C;:':;.;:T(;!a:idard:; (;;: r\.:-: mixture
stap.ii.u-.::: i"ii. •!;:. ..nil 5 OPT. '••• •' in
nitrc'^n cy!:nd:T' |. T'::: tci-'.tr :;• .-y i:...i
cylinder siavd in!s to usrectly prr';:are a
chrf.ir.'it'.'vraph cjiibratiun curvr :s
Ui:sc.nb':d in S.:;:iion 7.2.2, if thi; iV-lawina
i:'jr-d:!:.'".s are rr.1!: (.1) The n;;;:: : ..::uri:r
r.:::'i;f;ps I'r.e i;,is coniposkion w.;:: ,in
octy.ir.iry of i j pcruc-nt or bet:.-.- Ueo Section
5.2.3.1). (I)) Ti:i! a; ir.aLicturer :•;••::i.-.i.-r.i.T.ds a
maximum shelf !:f-.; over which th-j ;:as
concentration docs not change by greater
than ±5 or:ci.-r;t from the rcri'i'ii1.! •..'.!;:!!. (';)
Tiie mti;iiif>iCt>>:'t!r ::i:";xcs Liie C[,,;^ 01 ^as
cylinder pn-parai'iin, certified ;!rf;.-:i\-.ii
concentration. a::d ruccirimcn'Ji"J maximum
shelf lifo lii the cylinder before sinpaiont to
the buyer.
5.2.3.1 Cylinder Standards Certification.
The manuf.ict'jrr.r shall certify thu
concentration of benzene in nitrogen in each
cylinder by (a) directly anu!v^ir:;; i-acii
cylinder and (ij) calibrating his ar.aiytical
procedurs on tho day of cySin-.J:1: analysis. To
calibrate his analytical procedure, the
manufacturer shall use. as a miniiiium. a
three-point calibration curve. It is
recommended iha: tho nian;:!\:c;;.;i:r n.nnt.iia
(1) a high-concentration calibratior; standard
(between 50 and 100 ppm) to pn-pare his
calibnition curvr by a:; appropriate dilution
tcchnicjr;': 'i;;J '..'?! a !o\v-cc.r.ccr.:-'".'i.:n
calibration standard (between 5 and it) ppm)
to verify the dilution technique u>.:d. If ;he
differsiico boi'.vcen the npf/art.:';'.
concentration read from the cn'i'/-. :ion curve
and the true rorvjer.tration n.-.-=i-;:>:;: to tho
low-concentration standard e\ccnds 5
percent of the Ir.io concnntratiop.. ihe
manufacturer shall determine tho source of
error and correct it. then repeat t!:e ihrce-
point calibration.
5.2.3.2 Verificatinn of Mani:.r,-!C.'-.:;or's
Calibration Standards. Before u'jir.j, ih.s
mari'.:fjc'..:rnr ?;u!l verify eich ca. '-ration
standard by (a) comparins ii to j; ••:, mixtures
prepared (u-i;h 99 Mol percent b«:nii:r.B) in
accordance with tl-..? procedure drsr.ribid in
Section 7.1 or by (U) havir.'.! it a:-al\ r-r-d by tha
National Bureau oi'Standards. THs: ayreetnent
between the initially determined'
concentration value and the verification
concentration value must be wiihi.i :±5
percent. The manufacturer ~-.i^t rnviirity u!l
calibration standards on a timi1 i:'.;:TV.':i
consistent with ihe shuif life of ;l-.o cylinder
standards sold.
• 5.2.4 Audit Cylinder Standards (:]. Gas
mixture standards with concer.iratit.'ns
':now:i o.'.iv to ih;: :'cr:;on suoer\ i.-ir.; ihe
I'n-.tertinn Arvrrv. Ivn-jnirivi'al ?.f,->ni'»rini:
.-'::•.! St!|'pi-rt l,.i!n)r:i!orv. '.^nabtv As.Miraiii'O
.". .-!f:h'(MI) -77! -.-«••.•-:..". Tri i:-:!-: I'.srk.
N::r!ii C.iriiiina ::. "II. li .i'id.1 cyiiriiiers are
r.i.1! available at the KivrcTTiental P-nt'Tlicn
A^:.-::cy. thu testier must scuiri: an alleniativt;
standard;; s::a!i ho idjnliwiily prpparod as
those in Section 5.2/.I (.benzene in nitrogen
cylinders). Tr.e concentrations 01 M:S audit
cyliniier rhoiild !:-- one l;)\v-co"c.:'",'";:iion
cylinder in the r:::-..:r- of 5 !o 20 p;: " ivnKca
and or.n h:;-:h-r:oncvp.iratii;n cyl.r.d:-.- in the
r.iiv:r; of '.'') '.:', 'i1'-! ;>":" '••"i"-".-. '.'•"• •';
iivaiiabli:. !iu t:'::t- r may obi.i'-i .••••lit
c\ ii:if.!oi'o b\' c^nUi :tinc: U.S. i^r. i. ^:'.:::0ata
0.1 Snrr.plir'j. Asse-:;!i!e the sample train
as shown in l-'i,;ur;; 1 li!-l. P"rform a S/ay leak
cl.cck accordiiis la Section 7.3.2. loin the
i;::ii.!\ cc.nnocts as iliii.-^ralcd. and uon :;.".inn
th.it all cr,i!r:ecti'.ir;s bf-'twcun the ha;; and the
probe arc tijjht. Place the end of the probe at
the cuiitroid uf thu stack, and start the pump
with the noudlo valve .idjusted to yield a flow
that will more than half fill the bag in the
:;: crified simple period. After allowln;;
M!i';'icic:nt time to purye tiie line several times.
cor'.r.L'c! the vacuum line ty the bag ar.d
evacuate the bag uiuil the rot.imutcr ii;clicates
r.o flow. At all times, direct the gas exiting
the rotnrneter away from sampling personnel.
At the end of the sample period, shut off the
pump, disconnect the sample line from the
bii», and disconnect the vacuum line from the
bag container. Protect the bag container from
sur.lijjhl.
0.2 Sample Storage. Keup the sample bays
out of direct sunlight. Perform the analysis
within 4 days of sample collection.
0.3 Sample Recovery. With a new piece of
Teflon tubing identified tor that bag. connect
a bag inlet valve to the gas chromatOHraph
sample valve. Switch the valve to receive gas
f.'-'j;i! Ihe bay; tliroii^h th» sample loop.
AiT'inSf! the en.uiprr.cn; so 'hrf sample g.r'i
passes from the sample valve to a 100-mI./
min roljmeter with tiu'.v control v^iive
followed by a charcoal tube and a 1-in.
pressure ja;:;.;.'!. 'Ihe tCiilcr may niaii;l,.iir. the
sample flov; either by a vacuun pump or
container preosurization if the collection ba»
ruir.ains in the rigid contniner. After sample
loop piirjiri^ is ceased, always allow thn
pressure ijaugo to return to aurn before
cctivaling the uas saT.rlins vulve.
G.4 Ar.alysis. Sft tl-i; coiurnn temperature
to Kb1 C (i;o: F) for coliiir.n A or 75' C (1(j7J
Fl ft-r ccl;:;:;:: 13, a:id tho ilelector teniprraairi!
to 225' C {•IJ7'1 I"). When op'imum hydrr^en
and oxygen flow rates hava been determined.
verify and maintain th'.-so flow rates during
all ' ::rom :!o?;r;:ph opera;.ons. Using zero
l-.ivlluin or r.i;roj;e:i as the i:;'.r:iRr gas.
establish a flow rate in the rnm:a consistent
with the manufacturer's requirements for
sntijf.ictory dn-iector oporaiion. A flow rate of
apprjximalcly 20 mL/min should produce
u;:t:vi".ite separations. Observe the base line
periodically arid determine that the noise
level has stabilized and that base-line drift
has ceased. Purge the sample loop for-110 sec
at ihu rctc of 100 mL/rv.ir:. lh.cn activate the
sa::ip:e vaive. Record l!:.1! ininction time (the
position of the pen on ihe chart at the timrof
sample ii;jt:ctiu:i). the san:r!e number, the
san-.ple loop temperature, iho column
t(.'n:pi;ratvire. carrier ";is tlnw rate, chart
rp:-.-r!. and i!:i: at!i-:v.i;>!or .,:jtti;^. From the
chart, note the piv.k having the retention 'ime
cornispondi::,'.' to benzene, as Cetermined in
S :>,::^n ;'.2.1. Mi ;:s:iri: ;:.. :"T:;:c'ne peak ,1:00.
A,,,. !:y use of a disc ink--'~.'!ti)i, electronic
iiiti-^ratur, or a planimt'tor. Record An and
-------
i.T-'W-'W* TXfTim*
the reteniii".! time. Repeat tin: injection at
least two : .••".•; or '.:;•':! U\ n cn:r o:..:!ivc!
vMue? fo" •'••.(• total nrc.i of Ih1.: IVTV.'-. ••:•:: peak
do not v;::! concentration.
G.5 Dctf.i ruination of Dag \Vu!<;r Vapor
Content. NiuaMiro th-j amUunt temperature
and barometric pressure near the bag. From a
water saturation vapor pressure table,
determine and record the water vapor
content oi the ba« as a decimal figure.
(Assume I ho relative humidity to be 100
percent ur.ioss a lesser value is known.)
7. Prcpcrd'on of Standard Gas Mixtures,
Calibration, and QaalityAssurar.es
7.1 Preparation of Benzene Standard Gas
Mixtures. (Optional procedure—delete if
cylinder standards are used.) Assemble the
apparatus shown in Ki-:are 110-2. Evacuate a
f)0-L Tt:i)i;::- or aliimi"i".i:d Mylar beg that has
parsed a !e;;k check (described in Section
7.3.2) cind mcl'.T in aheut iO L of nitrogen.
Measure ihe bnromeUic pressure, the relative
press\ire at the dry R-IS meter, and the
temperature' at the dry 'MS meter. While the
bap is filli:1'.:. use the H'uL syringe to inject
lOfiLof 99-r percent benzene through the
septum on Ion cf the impi'i^rr. This pives a
conccntralir.n of anp-oxi^aioly 50 pprn of
benzene. !n a i'.ke m^nnor, use tho other
syringe to prepare rii!iitio::s having
approximately 10 ppm tp.d 3 ppm benzene
concentrations. To calculate tlie specific
concer.'r.r,!e:ir.. refer in T.er.lion R.I. These gas
mixture st.:r.-':trds r.v.'y be used for 7 days
from the dale, of preparation, after which time
preparation of ne.w >'as mixtures is required.
[Caution: If ihe new mis'mixture standard is a
lower nnncenira'.ion than the previous gas
mix!,ire ii.'v.ikrd. comamination may be a
problem v.hcn a bay is reused.)
7.2 Calibration.
7.2.1 Determination of Benzene Retention
Time. (1'nis section can be performed
simultaneously with Section 7.2.2.) Establish
chromatovjraph conditions identical with
those in Suction G.'', a!;ov^. netermine proper
attenuator position. Flush the sampling loop
with zero helium or nitrogen and activate the
sample valve. Kecoid the injection time, the
sample loop temperature, the column
temperature, the carrier gas P.ow rate, the
chart speed, end the attenuator setting.
Record peaks and detector responses that
occur in Ihc absence of benzene. Maintain
conditions, with the cnviipmenl plumbinn
arranged identically to Section 6.3. and (lush
the sample, leap for '.Ci sec at the rate of 100
mL/min wish one of the benzene calibration
mixtures. Thrrn activate ihe sample valve.
Record the infection linifi. Selocl the peak
that ror.-osronds to benzene. Measure Ihe
distance OM ihe char; train ihe inieclion time
to the tirrif a! which !i:;: peak maximum
occurs. This distance divided by the chart
speed is defined as the ber.zeru: pe.-,!»
retention time. Since it is (51:1(1: hKcly that
there will bs other orjtanics prrsnnt in the
&::r.:pli:. it is very i:n;:cr'.j:;l that positive
identification ol the benzene peak be made.
BILLING COCC 6SCO-01-U
-------
F-'!'-r:l R;;<:is!<>r / V<.'. Jri, N'o. 77 / "ri:!.iv. Ar-"it Vi. IHfiO / P.-n-uiscr.! Ri!!:':3
2GH31
DRY GAS METER
TEDLAR BAG
CAPACITY
50 LITERS
Figure 110-2. Preparation of benzene standards (optional).
BILLING CODE 6550-01-C
-------
5.2.3 cr 7.1.1! is:-:;: : rc:-...!i:ic:is IJi-nlica! with
those listed in f: v.,;. TIS 6.3 m-.d ti.-l. i'lufh the
snmp'iirj looj .•••;• ,.M :.!•'; ;j.i the rale of rr.L/
mill with OUR o: :hf: standard ••."-= mixtures
and iiclivatc tin: s;::r.;?e valve. Record Cc, the
conrer.tratior '.•: bi'T.ifne injt-i'.trd. the
aller.untor :;ett:nr. chart spend. |)e;.'k area,
sample lo'.ip t'jrr.;:.j:;!iure. cnliima
temperature, car;-cr pcs flow rale, and
retention time. [iT,-ird the laboratory
pressure. CalcuL'lo Ac. tr.e peak area
multiplied by thi! ••.itenuator celling. Repeat
until two co'is!.-r::!iv2 injection are,is nre
within r> ;;i!icer.t. l:p.yn plot the average of
those t'.vn v.ihnis versus Cr. When the other
slandjrd JMS lY.ix'ni.-s have been similarly
amilyzed and plowed, draw a straight line
through Ihe points deiiveu by liio least
squiiraf. rn.ithcKJ. i';j:;o:m calibration daily, or
before and i'ficr c.:ch set of bag samples,
whichever is mure frequent.
7.3 Qunlily A::r>!irani:e.
7.0.1 Ara!y~:.s Aflit. Immediately after
the preparation o; me calibration curve and
before the sauipie analyses, pcnnrai the
f
['.•jrior:;1".'-.' lu'i-'-ie U:!-:; •:: :. A:'.I.T e.tnh use,
m:>k'j iiirj ..i Dci^vli ; :;• : •.• :v.-:o;; IU.INS by
conni.ctii'1.''! a '.v.iici- m.'.::irr;-!er a:i:l
pre^--yri;:i:v: ;ne i/.i': ; ' " \.t ili crt! 1 i^O [2 \t.
i:;. i I.'.'!. A;!o-.v !o :,!.:i-..i ior 10 m:n. Any
in(;:r.ai'.'s vi ic-.iK. /-.i;.o. i r;..( k tp.e ir-.".d
cuii'aip.cr lor I.I'.JN? ii: :!••;•. manner. ^i\ote: a
nltrrnaiive leak c.-,.;-'..- TV
the h.i;- to 3 to :Q cr.i i i.i.
and ,'ijiow in star,;! ovi";
ri'-ltfi conl.-.iner. i/i.n r ;! r
hnd is to pressurize
!;•.(• rulaniLitcr k)
bag appears to be
empty indicates a leak.
8. Ccluuiaticns
8.1 Optional Renxn;ie Standards
Concentrations. C.'ilr.vl.i'i! each benzene
siani'ard concent;-;,:.>;:i !Cr in pprn'l prepared
in accordance with Section 7.1 as follows:
3(0.27Q6H10J)
233
"
760
C.
'_
where:
3
701.9
BT
(110-1)
0.27C5
103
= Volume of bonzene injected, (nicrol iters.
= Gss volume measured ty dry gas ir.eter, liter?.
= Dry gas meter calibration factor, dinensionless.
= r.osolute pressure of the dry gas meter, n:.T.:ig.
= ADsolute tc.T.perature of the dry oas meter, °K.
= Ideal gas volume of benzene at 292° K and 750 -~.^g L/T.L.
= Conversion factor [(pc,ii)(mL)/(jL].
8.2 Benzene Sample Concentrations. From the calibration curve de-
scribed in Section 7.2.2 above, select the value of C tnat corresponds to
Afi. Calculate the concentration of oenzene in the sa-.ple (C in pprr.) as
follows:
where:
C,
CCPrTi
(110-2)
Ti
Tr =
Concentration of benzene in the sasple, cr.™.
Ccr.cer.tration of ber.iere indicated by the ySi cr.ro-atograpri,
ppm.
Reference pressure, the barc-etric press^'S nicorsec! curi.-g
calibration, rrcnHg.
Sj~ple loop tenparature at tre tine of analysis, °K.
Barometric pressure at ti.r.e of analysis, ir-:-;j.
Reference tcrr-cerature, the sa.-ple Icop tfroerature recorced
during ca.l ioration, °K.
Water vapsr content of the bsc saT.ole. -.o'^-.r fraction.
. ',;.. f\.\\. K,-ni:i!,.:. !!. J.
.). _Q. Uvi:::!:^.
•! ;-!'G.i5."!"is Organic:
r'.ni>jf;:.i-.ii A"TC.V. i:i''A Con'.;1:!::!
Nurr.bt:."'."..!-''2-1.;(X. !.;n;:;;ry 1973.
Revi.«=f.j i-v EPA Ai:-::::,! 107M.
2. Kno!i. l-r..-;ih f!.. \'.ad!- !1 Penny, and
Ro-i.iLy '.:. M::;,:ctl. ;i'i; L';:f cffedlar
Sunplei a; So'.-.rr.o Uv-i. U.S.
2r.vircnir.cr.iai Prc'.rtction A-c~cy.
Research Tiiar..;!vj Park. N.C. Monitoring
Series. nPA-VC.';)/4-78-037. October 197G.
3. Siipeirn. IPC. Separation of Hycircc.irbons.
B;:':Lf^n!c. P.-;. t:.u:!i:;i:;R 7'!3A, 7-10C. and
4. Current Peaks. 10:1. Carle Instruments. Inc.
F'jilarlcr.. Caiif. 1P77.
5. Knoll. Joseph K. Communications
C.7ri'-erni:v: Chrorr,i:tc;;r:!phif: Columns
fur iier.-.'.er.o Analysis. October 18, 1977.
6. Knoll. Joseph E. Communications
Cor.cnrnip;.: Car, Chromalo.eraphic
Co',jn:ns for Secara;iny Dknr.er.e From
Other Or^anics in Cumer.e and Maieic
Ar.hyrihila iiroce^s 1-!.'fluents. November
10. 1977.
AppenHix C
Supplement A—Determination of Adequate
Chromaloyrr.phic Peak Resolution
In this tr.rtr.r-:! ofdcaiinj with resoultion.
the extent t.j which one chromaluf-ruphic
peak o''ori."!?s pn'^her if, rii'lerminnd.
For rnnver.'rnce, consider the range of the •
elution curve of each compound as running
from — 2u- to -r-2or. This rr.nur; is used in other
resolution criieiin. and it contains 35.-15
percent of the area of a nor:na! curve. If two
peaks are separated by a known distance, b,
cnn cer. ci'.'i",r::;ne :hs frnrtlon uf the area of
one curve that lies within the range of the
other. 1 lie extent to which the eiution curve
of a contaminant compound overlaps the
cuuo u! u t.u.'.'.pound ihai is under uildlvsls is
found bv ;n:Ci.ratir.2 the contaminant curve
over limits b-2cr,, to b + 2tr.. \vhern cr,, is
the standard deviation o! the sample curve.
There are several ways ibis caU/.ihdion can
be simplii'Cd. Overiaa can ue determined for
curves ;.! unit a'.ea; inen actual areas can be
ii:lrod'ii:i"J. Tha ci-ii.'
rff.'.cived i:;'o two ir.:
distribution fuiv,:;i>::!
CO.T. criiT.t c::!'":H!t!~
'cd !nl";4Mtio:i can ba
r;rals of the normal
lor v.'hii:;! th'.TO ,iro
-r! p:(vr,::r.F and tallies.
An exarr.pii.' v.-^u.j ';••.• i-n;}.-. •„:;-. 15 i:1. Texas
Instrumerli I';opr.im Muiiual S'I'l. 1973,
Texas Instruments. Inc.. Ddiias, Texas 7:322.
-------
_L
.'i
c dt =
-]- J e " * „. - -L
e "• dx.
f j! !.;~ir..l calculation stcos -ire required:*
tc/2s2 In
Q(«,) = _L ! e " 2 dx
' J "0 C 5
Percentage overlap = A x ICO
2
A - The area of tne sample peak of interest determined by elec-
tronic integration, or by the formula A. = h.t .
4_ = TV area of the co:iio~inar.t. pe-tk. riete:vii.i^ r.cir;".)! 'Jiitrio'-ition r'u.ic\.ion .'ron x, to
' i
i > f i n i ty.
!!-n int^rjral of thr; nor.~a) distribution i.i'-;Ci.ion f.-c™ ; »•;;> o! li.tiissinn fiiv-cli'iiis to (!psr.ribe-
c!1.; u-'iMtt;-:: .:;\".!C clution cnrvi's is
\vi(ii;spr';.'ui. Hovvaver. soiv.i; tiutinn curves
si: tiiacs where
ihtj s.impii1 pi1. ik is foilov. c'tl by a
cunt;iiniin;int th.it hns a !-j;ifl:n'! r<\-': th.it
n:u;s sh;ir;>lv tai! thf? curve :'::(•••, tails oft", it
m;iy hu1 pr"'.'.i!-!!- to clufire .'in cff(;i::ivc xvidth
for I0 as "tu'irri; !ho distuncfi frOTi thn leading
edyc to a prtrpnndictilar lino ihroii'.;ri the
maxim of ti:L% contuniiniint curve, measured
alon^ a p(;rpt'nilicul*ir bisor.tinn of that lino."
SiippluiTifjiit H — Procedure for Field Auditing
GC Anjijsis
Rt'sponsibililir-s of audit supervisor and
analyst at tiin source sampling site include
tlic folioivin^:
A. Check Ijuit ciudit cylirv.'ors arc stored in
a safe location both before nnd after the audit
to proven! v;inr!:i!ism of s;irr.i!.
B. At the b'.'.-;i:ip.in.a and c:in,-;!asinri of the
audit, record each cylinder n'imbf;r anrl
cylinder piv.sium. Never unaiyzo an audit
cylinder when !ha pressure drops below 200
pai.
C. D'irip^ t!v .i'id:t. thi: analyst is to
pi.Tl'orm a minimum of two consecutive.
analyses of s.vich ntidit cylinder ,cas. The audit
must be conducted to coincidi? with the
nnaiysis ui •.••<•.•.;••.•.•.•'. ipsl siiiivji-.-s. Norn>i'iy. it
wiii bi; C'ir.ii'.i'y.cd iri:;i!ccii.ii"iy alijr ii'i; CC
Citlibralion and prinr to ih:; s.implf; fiiialvscs.
D. At Ihr: fin. -I i'f ;n:riit ap.:-r.7r:s. the -'tudit
si:p(!n.-is!!r r"i.;'.|f: = !s the calcuiiilod
(;;>;!!. .::;;rd!ic;.i:> irurn ihe juimv-!! anri th°n
compaics !:u; rr.i.:its wii'i I!:L.' jctuul ,i;;dil
concontra'ions. !f each mtiiisurnd
coiiucntration aareos ivith !hu respective
aclu.il concrrilra!!.",-. within ~10 n.Trrta.it, he
ih'jn diri'Lts t!-.;: .;;-,r:!ys! to of. ;:n thi: P.n.v.iysis
uf ;>i.i;irc;? r:in:r'.-i:-. Ai:ilit S'a: -"vi.sor juci-.'rncnt
n'ij/ur su|.';:'v;s.i;-v policv >::.:. .•rniinc course
of action w::h i'v^'TTicnt i1; rr? within ~10
(•..•rci-p.i. \Vi''!-;i! ;; cunEistcrt !)i:!S in exr::js of
li) pores;:'.; i.; :.r.;nd. it may :>o jiossibis to
proceed witii thi; sample ^ruiyscs. witli a
co.Ti'irJivi: factor in cin applied to t'c.c rc'uits
;•!::! ;:;.-r 'i1!^:. ! ' ..•.-.• vcr. <::\:r: ..itc;; ;•••
siiijulj bo ni.ii.ii! ;>'! iocnte ii:e cai'sn uf '.l:a
dl-iT.^p.-i!-.".1.-. ;. • :; tr.:>y be n\is;r-ii::i:;.:. j hn
:iu;::t si:p;:.'vi';.ir is tij record ".!r;h ry'indnr
it'j;iib(:r. cyiiru.'iT pressure (a: ;!:.) end of :h
-------
Page E-l
APPENDIX E
PROJECT PARTICIPANTS
Scott Environmental Technology Inc.
-------
SET 1957 07 0181 Page_E-2
APPENDIX E
PROJECT PARTICIPANTS
The following people participated in some phase of the sampling
program at Bethlehem Steel, Burns Harbor, Indiana:
From Scott Environmental Technology, Inc.:
Tom Bernstiel, Chemist
Jack Carney, Chemist
P. K. Chattopadhyay, Chemist
Dan FitzGerald, Manager, Eastern Operations
Kevin Gordon, Technician
Carolyn Graham, Chemical Engineer
Dan Miesse, Instrument Technician
Lou Reckner, Vice President & General Manager
From Research Triangle Institute:
Peter Mehta
From U. S. Environmental Protection Agency
Lee Beck
Scott Environmental Technology Inc.
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|