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
Scott Environmental Techndogy Inc

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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.
 Scott Environmental Technology Inc.

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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
Scott Environmental Technology Inc.

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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.
 Scott Environmental Technology Inc.

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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.
Scott Environmental Technology Inc.

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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.
                                                                                                           hd
                                                                                                           w
                                                                                                          OQ
                                                                                                           m

                                                                                                           OJ

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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
 Scott Environmental Technology Inc.

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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





Scott Environmental Technology Inc.

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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
Scott Environmental Technology Inc.

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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
Scott Environmental Technology Inc.

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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.
Scott Environmental Technology Inc.

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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.
Scott Environmental Technology Inc.

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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
Scott
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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.







Scott Environmental Technology inc

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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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Technology
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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.
                             •*
Scott
Environmental
Technology
Inc.
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.
Scott Environmental Technology Inc.

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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.





Scott Environmental Technology Inc.

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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.

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                                                      Page A-l
                                 APPENDIX A



                            SAMPLE CALCULATIONS
Scott Environmental Technolosy Inc

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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.

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                                                      Page B-l
                               APPENDIX  B




                            FIELD DATA SHEETS
Scott Environmental Technology Inc.

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                     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

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                       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

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                                                                     Page D-l
                               APPENDIX D




                             EPA METHOD  110
Scott Environmental Technokxjy Inc

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                                                  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


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                                                  Page E-l
                                APPENDIX E




                              PROJECT PARTICIPANTS
Scott Environmental Technology Inc.

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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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