EMB PROJECT REPORT  NO. 75-VCL-2
   CD
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                                         AMERICAN CHEMICAL COMPANY

                                            Carson, California
                 UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
                             Office of Air and Waste Management
                         Office of Air Quality Planning and Standards
                               Emission Measurement Branch
                          Research Triangle Park. North Carolina

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              SET  2526  02  0175
   Vinyl Chloride Testing Conducted at ttv
          American Chemical Company
             Carson,  California,
     WithfSupplemental Method Evaluation?

       EMB Project Report No. 75-VCL-2
                Prepared for:

       Environmental Protection Agency
Office of Air Quality Planning and Standards
Research Triangle Park, North Carolina 27711
     EPA Contract 68-02-1400, Task No. 8
               January 6, 1975
                     by

               Warren  C. Kelly

    SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
            2600 Cajon Boulevard
      San Bernardino, California 92411

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SET 2526 02 0175
                            TABLE OF CONTENTS
1.0  Introduction 	
2.0  Summary and Discussion of Results
3.0  Process Description and Operation
4.0  Location of Sampling Points   .  . .
5.0  Sampling and Analytical Procedures
Page Number
   1-1
   2-1
   3-1
   4-1
   5-1
     SCOTT RESEARCH LABORATORIES, INC.

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                                 1-1
SET 2526 02 0175

                            1.0  INTRODUCTION
        The Environmental Protection Agency (EPA) has recently under-
taken the task of establishing a test procedure and performance standards
for vinyl chloride emissions from stationary sources.  A performance
standard is a standard for emissions of air pollutants which reflect the
best emission reduction systems that have been adequately demonstrated
taking into account economic considerations.
        In pursuing this task, Scott Environmental Technology, Inc., was
contracted by the EPA to perform source sampling tests at the American
Chemical Company, Carson, California, during the week of October 9, 1974.
The purpose of the tests was  to obtain background data for development
of national new source performance standards in the vinyl chloride industry.
Data was collected in three areas:
        0 Evaluation of proposed vinyl chloride test procedure
        o Vinyl chloride emissions' to the atmosphere
        o Efficiency of emission reduction systems employed
        Data was collected at American Chemical Company's Vinyl Chloride
Monomer Plant.  Process exhaust gasses are passed through a caustic scrubber,
burned in an incinerator and pass through a water scrubber prior to venting
to the atmosphere.  The vinyl chloride test procedure used was "Tentative
Method for the Determination of Vinyl Chloride from  Stationary Sources."
dated September 4, 1974.  Gas samples were collected before and after
the incinerator and at the exit of the water scrubber.  Water samples were
collected at the inlet and outlet of the water scrubber.
        Moisture determinations were made using EPA Method 4 at each gas
sampling location.  Determinations of total chloride and chlorine
content were made at the gas outlet of the incinerator and water scrubber
and at the water inlet and outlet of the water scrubber.  Oxides1of nitrogen
content of gas exiting the scrubber to the atmosphere were made using EPA
Method 7.
      SCOTT RESEARCH LABORATORIES, INC.

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                                    1-2
SET 2526 02 0175
        The test team was  comprised  of  two EPA representatives and six
Scott employees.  Six complete  tests were performed.   The test equipment
was set up on October 7, 1974,  and tests were performed on October 7, 8
and 9, 1974.
    SCOTT RESEARCH LABORATORIES, INC.

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                                     2-1
SET 2526 02 0175

               2.0  SUMMARY AND DISCUSSION OF RESULTS
        This section is divided into four sub-sections,  Section 2,1
presents vinyl chloride emission results as well as results from
addition tests conducted at each sample point.  Section 2.2 presents
the results of a vinyl chloride degration study conducted.  Section
2.3 presents calibration data along with the results of a subsequent
reanalysis of the vinyl chloride samples, and Section 2.4 presents a
discussion of the mass spectrometer analysis conducted on several samples,

2,1  SUMMARY OF TEST RESULTS
        A summary of the test results from sample points A, B and
C (C1) are presented in Tables 2,1, 2.2 and 2.3 respectively.   A
second summary in terms of Kg/hr. with emission levels at points B and
C corrected to 10 percent oxygen equivalent is presented in Table 2.4.
Results are presented in both British and Metric Units.  Test results
of water samples collected at sample points D, D1 and E are presented
in Table 2.5.
        As indicated in Tables 2,1 through 2.3, supplemental tests
(moisture, chlorine and total chloride, and NO ) were conducted, once
                                              A
per day, during vinyl chloride tests 1, 3 and 5.  It was not decided
until the second day of testing to test for chlorine and total
chlorides at sample point B.
     SCOTT RESEARCH LABORATORIES, INC.

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1
^^-^— w^
10/7
2
10/8
3
10/8
4
10/8
5
10/9
6
10/9
                                 2-2

SET 2526 02 0175


                              TABLE 2.1

                         Summary of Results
                           Sample Point A
                       Entrance  to Incinerator

                            BRITISH UNITS


Run Number

Date (1974)

Volumetric Flow Rate -
 DSCFMU'                 22.02    26,03    23.29    14.78    45.74    59.56

Percent Mositure by
 Volume                   14.1              25.0              11.4

Vinyl Chloride
 Concentration - %         4.26    26.40    17.50     8.71     1.33     2.43

Vinyl Chloride
 Concentration -          71.3    441.6    292.2    145.6     22.2     40.6
 x 10~6  lbs/ft3               .        .                .  ,;:..

Vinyl Chloride Emissions   9.42    68.93    40.77    12.92     6.11    14.49
 Ibs/hr



                            METRIC UNITS


Run Number                  1        2,       3        4        5        6

Date (1974)                10/7     10/8     10/8     10/8     10/9     10/9

VolumetricvFlow Rate
 NmJ/hr.U;               37.4     44.2     39.5     25.1     77.7    101.1

Percent Moisture by
 Volume                   14.1              25.0              11.4

Vinyl Chloride
 Concentration - %         4.26    26.40    17.50     8.71     1.33     2.43

Vinyl Chloride
 Concentration -
 gms/m                   114.2    707.3    468.0    233.3     35.6     65.0

Vinyl Chloride
 Emissions, Kg/hr.         4.27    31.26  .  18.49     5.86     2.77     6.57


 '  'Dry  standard  cubic  feet per minute  at  70° F. and 29.92 in. Hg.

 (2)
   Dry  normal cubic meters per minute  at  21.1° F.  and 760 mm Hg.
     SCOTT RESEARCH LABORATORIES. INC.

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                                  2-3
SET  2526  02  0175


                               TABLE 2.2
                          Summary of Results
                            Sample Point B
                           Incinerator Exit

                             BRITISH UNITS

Run  Number                   1         2        3         4        5        6

Date (1974)                 10/7      10/8     10/8     10/8     10/9     10/9
Percent Moisture  by
 Volume                     5.0               3.0               7.8
Chlorine  Concentration -
 ppm U;                                     18.34              1.04
Chlorine  Concentration ->
 Ibs/Hr.  U;                               0.2626            0.0214
Total Chloride       ...
 Concentration -  ppm                         6.42              0.35
Total Chloride          ,_.
 Concentrations - Ibs/ r                   0.0945            0.0074
Vinyl Chloride
 Concentration -  ppm      <0.5      2.0      1.4     15.0      1.6      2.7
Vinyl Chloride
 Concentration -
  x 10-9  Ibs/ft3           <0.84     3.26     2.36    25.12     2.64     4.51
 Vinyl Chloride                  __
"Emissions,  Ibs/hr;-       <0.013~~  -0.049...   0.037    0.390  ~ 0.060    0.101
    It is assumed the chlorine concentrations are in error due to the
 fact they are greater than total chloride concentration  (see page 12 of
 Appendix G-II).
 (2)
    Flow data from point C was used for calculations at point B.
      SCOTT RESEARCH LABORATORIES. INC.

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SET 2526 02 0175
                                2-4
                         TABLE 2.2 (cont'd.)


                         Summary of Results

                           Sample Point B
                            METRIC UNITS
Run Number 1
Date (1974) 10/7
Percent Moisture by
Volume 5.0
Chlorine Concentration -
ppm
Chlorine Concentration *•
gms/hr (2)
Total Chloride f .
Concentration - ppm
Total Chloride
Concentration - gms/hr ' '
Vinyl Chloride
Concentration - ppm <0.5
Vinyl Chloride
Concentration - mg/m3 <1.34
""Vinyl Chloride ' - "~
Emissions y Kg/hr... <&.006
2 3
10/8 10/8
3.0
18.34
119.12
6.42
45.87
2.0 1.4
5.2 3.8
0.022 0.017.
4 5
10/8 10/9
7.8
1.04
9.71
0.35
3.36
15.0 1.6
40.2 4.2
0.177 .._ 0.027
6
10/9





2.7
7.2
0.046
   It is assumed  the  chlorine concentrations are in error due to the

fact they are  greater than total chloride concentration (see page 12 of

Appendix G~II).

(2)
   Flow data from point  C  was used for calculations at point B,
     SCOTT RESEARCH LABORATORIES. INC.

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                                             TABLE 2.3
                                          Summary of Results
                                           Sample Point C
                                 Water Scrubber Exit  to Atmosphere
                                                       BRITISH UNITS
Run Number
                            ,(1)
                            .(2)
                                              (2)
1
10/7
2598
9.06
7.6
23.09
0.3318
17.35
0.256
15.90
0.296
34.7
58.0
0.906
N/R
N/R
N/R
2 3
10/8 10/8
2588 2588
9.06
7.7
39.85
0.5704
38.06
0.560
68.50
1.271
24.3 34.7
40.6 58.0
0.632 0.902
30.0 27.0
50.3 45.1
0.781 0.699
4 5
10/8 10/9
2588 3719
13.47
7.7
9.28
0.1909
6.90
0.146
81.50
2.172
35.2 0.6
58.8 1.0
0.915 0.022
4.5 <0.5
7.5 <0.8
0.117 <0.017
6
10/9
6315








6.4
10.7
0.217
<0.5
<0.8
<0.017
Date (1974)
Volumetric Flow Rate - DSCFM
Velocity - ft/sec
Percent Moisture by Volume
Chlorine Concentration - ppm
Chlorine Emissions - Ibs/hr
Total Chloride Concentration - ppm
Total Chloride Emissions - Ibs/hr
NO  Concentration - ppm
NO  Emissions - Ibs/hr
Vinyl Chloride Concentration -
 ppm (PT.C)
Vinyl Chloride Concentration -
 x 10-9 ibs/ft3 (PT.C)
Vinyl Chloride Emissions -
 Ibs/hr (PT.C)
Vinyl Chloride Concentration -
 ppm (PT.C1)
Vinyl Chloride Concentration -
 x 10-9 lbs/ft3 (PT.C1)
Vinyl Chloride Emissions -
 Ibs/hr (PT.C1)
(1) Dry standard cubic feet per minute  at  70°  F.  and 29.92  in.  Hg.
(2) It is assumed the chlorine concentrations  are in error  due  to the fact they are greater
    than total chloride concentration  (see page 12 of Appendix  G—II.)
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                                         TABLE 2.3 (cont'd.)
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Summary or Results
Sample Point C
METRIC UNITS
Run Number
Date (1974)
3 (1)
Volumetric Flow Rate - Nm /hr
Velocity - M/sec
Percent Moisture by Volume
(2)
Chlorine Concentration - ppm
Chlorine Emissions - gms/hr
(2)
Total Chloride Concentration - ppm
Total Chloride - Emissions - gms/hr
NO Concentration - ppm
x KF
NO Emissions - gms/hr
1
10/7
4411
2.76
7.6
23.09
150.50
17.35
116.12
15.90
134.27
234
10/8 10/8 10/8
4394 4394 4394
2.76
7.7
39.85
258.73
38.06
254.02
68.50
576.53
5 6
10/9 10/9
6315 6315
4.11
7.7
9.28
86.59
6.90
66.23
81.50
985.22
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Vinyl Chloride Concentration -
 ppm (PT.C)
Vinyl Chloride Concentration  -
 mg/m3 (PT.C)
Vinyl Chloride Emissions - Kg/hr
Vinyl Chloride Concentration -
 ppm (PT.C1)
Vinyl Chloride Concentration -
 mg/m3 (PT.C1)
Vinyl Chloride Emissions - Kg/hr
(1)
34.7

92.9
 0.410

N/R

N/R
N/R
24.3

65.0
 0.286

30.0

80.5
 0.354
34.7

92.9
 0.408

27.0

72.2
 0.317
35.2

94.2
 0.414

 4.5

12.0
 0.053
 0.6

 1.6
 0.010

<0.5

<1.34
<0.008
 6.4

17.2
 0.098

<0.5

<1.34
<0.008
   Dry normal cubic meters per minute at 21.1° C. and 760 mm Hg.
(2)
   It is assumed the chlorine concentrations are in error due to the fact they are greater
   than total chloride concentrations (see page 12 of Appendix G—II).

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SAMPLE POINT
Vinyl

A
TABLE 2
Chloride Concentrations Before
Points B and C Corrected to 10


Incinerator Inlet


" Date
o Run Sampled
No. (1974)






1 10/7
2 10/8
3 10/8
4 10/8
5 10/9
6 10/9


NM3/
hr(D
37.4
41.2
39.5
25.1
77.4
101


VC.
4.26
26.40
17.50
8.71
1.33
2.43


vc,
kg/
hr
4.27
31.26
18.49
5.86
2.77
6.57


SAMPLE POINT
.4
and After Incinerator-Scrubber
Percent Oxygen Equivalent

•B


Incinerator Outlet/Scrubber Inlet


NM3/
hr(D
4411
4394
4394
4394
6315
6315
• -

VC,
PPM %02
0.5 10.7
2.0 10.2
1.4 9.79
15.0 9.96
1.6 10.2
2.7 10.2


vc,
PPM @
10% 00
0.5.
1.99
1.4
14.9
1.6
2.8


vc,
kg/
hr
0.005
0.022
0.016
0.171
0.026
0.044



NM3/
hrCD
4411
4394
4394
4394
6315
6315

SAMPLE POINT C
Scrubber Outlet


VC,
VC, PPM @
PPM %00 10% 00
34.7 10.5 ... 36.4
24.3 10.2 24.8
34.7 9.79 34.0
35.2 10.3 36.2
0.6 10.2 0.6
6.4 10.2 6.5




VC
kg/hr
0.398
0.278
0.396
0.402
0.010
0.105
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(1) Dry normal  cubic meters per  hour at 21.1° C.  and 760 mm Hg.

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                                   2-8

  SET 2526 02 0175
                                TABLE  2.5
                           Summary of  Results
                        Sample Points  D, D' and .E  ^  '
                                 Vinyl Chloride Runsv  '       ^  HCL Run

           Sample Point          1     2,  3,4     5,6

  Date  (1974)                  10/7     10/8      10/9          10/8      10/9
  Total Chlorides - ppm   D    6205       475       548           365      1095
                          D'   1825     1643      1825          2008      3103
                          E    9673   10,403   14,235          8213      5475


  No chlorine was detected in  the water samples,

  No vinyl chloride was  detected in  the water  samples.
   Sample Points D and D' - water to scrubber
   Sample Point E - scrubber discharge water
(2)
   Integrated Samples
       SCOTT RESEARCH LABORATORIES. INC.

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                                  2-9

SET 2526 02 0175


 2.2 VINYL CHLORIDE DEGRATION STUDY
         Several samples  collected underwent a degration study.   This
 involved analyzing each  sample in its original sampling container at
 periodic intervals.   Results of each analysis are presented  in  Table
 2.6.

 2.3 CALIBRATION DATA AND SUBSEQUENT SAMPLE REANALYSIS
      2.3.1 Calibration Data
         Each day vinyl chloride samples were to be analyzed, five
 vinyl chloride standards were made up (Section 7 of Appendix G-I).
 Concentrations of the five standards were 1, 10, 100, 1000
 and 5000 ppm.  Available also as calibration standards were  three
 high pressure cylinders  of vinyl chloride in nitrogen which  had
 previously been analyzed for vinyl chloride by the National  Bureau
 of Standards (NBS).  The results of this analysis by NBS were.Cylinder 1-
 0.883 t 0.044 ppm; Cylinder 2 - 40.6 ± 1.2.ppm; and, Cylinder 3 -
 874 i 15 ppra.  These cylinders were periodically analyzed during the
 vinyl chloride analyses; however, all vinyl chloride results reported
 in Section 2,1 are based on the calibration bag standards.
         Three discrepanices were noted during the first set  of  vinyl
 chloride and calibration analyses:  (1) hang up could occur  if  samples
 of markedly different concentrations were analyzed back to back.  This
 was attributed to the lack of a heated sample loop which was corrected
 jfor the subsequent reanalyses reported in Section 2.3.2,  (2)  An
 incorrect amount of nitrogen was being metered into the calibration
 bags.  It was determined that 8.19 liters of nitrogen were being used
 as opposed to 5.0 liters as specified in the test procedure.  All data
 presented in the report have been corrected.  This discrepancy was
 corrected for. the reanalyses reported in Section 2.3.2.
     SCOTT RESEARCH LABORATORIES, INC.

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                                 2-10

 SET  2526  02  0175

(3)  A "Chromosorb 102" GC column was not available during the first
day of analysis (10/8/74).  As a substitute, a "Porapak" column was
used which gave adequate separation,
        An analysis was conducted to determine the advantage, if any,
in using a least mean square fit of the calibration data instead of
the 5000 ppm or 1000 ppm  (NBS) calibration standard to reduce sample
results.  The term M (slope) in  the least mean square fit equation
Yi * mXi was evaluated where Y = nominal standard concentration and
Xi= area of standard peak  (counts) .
        Three sets of data were analyzed:
        10/14/74 Bag Standards
Xi
Yi
1
1553
10
1458
"100
7800
1000
64786
5000
384,303
                           M - 46.64
                 Y5000/X5000 = 46.92
                 'Difference = +0,6%

         10/21/74  Bag  Standards
Xi      1      1       10  I •'..    10       10   .   100      100      1000      5000
Yi   29,648   27,735  115,736.58,542   116,414 122 ,.314  123,774  100,504    5,278,314

                           :M = 643.4
                 Y5000/X5000 =644.5
                  Difference = +0.2%
     SCOTT RESEARCH LABORATORIES, INC.

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                                2-11

 SET 2526 02 0175

        10/21/74 Bag Standards
       Xi       1         50         50         1000         1000
        Yi    1187     50,338      49,769     1,001,680    1,007,272
                    M P  1004
                    ) =  1007
          Difference  =  +  0.3%
Y1000/X1000  = 1007
        As a result of these small differences, only the 5000 ppm
bag calibration standard was used to reduce vinyl chloride results,

      2.3,2  Subsequent  Sample Reanalysis
        As  a result of the  large variation  in  the  initial  calibration
data  and  the discovery that the sample loop should be  heated,  it was
decided that a  reanalysis of each  sample  should be conducted with
additional  calibration data being  collected.   Each sample  was  assessed
with  respect to both  a second  set  of  calibration bag  standards as  well
as the NBS  calibration standards.   Nitrogen blanks were  run during samples
and calibrations of distinctively  different concentrations to  eliminate
any hang  up of  vinyl  chloride.  Samples were either retained in their
original  sample container,  or  a vacuum flask was filled  with sample.
The results .of  the second analysis were considered to  be more  consistent
and subsequently used in the data  presented in Section 2.1.  Results  of
all analyses conducted are  presented  in Appendix A.
     SCOTT RESEARCH LABORATORIES, INC.

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Sample No.



   1C


   5A


   5C


   6A


   6C
Date of First

Analysis (1974)
                                                         TABLE 2.6

                                               Summary of Degration Results
                                               Day 0
10/9
10/10
10/10
10/10
10/10
» — — .BiB™^—
22.4
12,800
3.1
17,700
3.4
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                                                                   Sample Analysis (ppm)
                                                        Day 2     Day 4    Day 5



                                                        696.0(1)            16.8


                                                                  8,500


                                                                17:7/23.


                                                                15,300


                                                                   0.0
Day 11    Day 18    Day  19
                                                                                                          16.6
                                                                                    11,000


                                                                                     10.4


                                                                                    15,300


                                                                                      3.1
           18.0
            3.7
                                    M
                                    NJ
          (1)
             May be-results of no sample loop heating.
          (2)
             Results of two analyses.

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                 TABLE  2.7


Calibration Bag  Standards (Integrator Counts)

              Second Analysis
5000 ppm
Date . Counts
xlO"3
11/15 1,920
1,950
11/20 2,020
2,020
11/21 2,200
2,230
11/24 1,940
1,940



1000 ppm
Date Counts
xlO~3
11/15 453
448
450
462
420
422
11/20 466
470
11/21 434
425
11/24 384
390
100 ppm
Date Counts
xlO"3
11/15 56.7
55.8
49.8
49.8
11/20 52.9
57.9
53.9
11/21 54.2
54.2
11/24 48.6
47.0
10 ppm
Date Counts
xlO"3
11/15 45.8
47.1
11/20 .423
1.464
.523
1.640
.994
.994
11/21 6.200
6.000
11/24 5.380
S.fi7n
	 1
1 ppm
Date Counts.
xlO"3
11/15 11.5
10.8
11/20 0.312
0.312
11/21 0.340
0.755
0.330
11/24 0.483
0.567
0.600

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                                2-14
SET 2526 02 0175

2.3.3 Subsequent Standards Investigation
       As a result of inconsistencies noted in calibration standards
during testing, an investigation was conducted to attempt to resolve
these inconsistencies.  In preparation of this investigation, the
following action was taken:
       °A new cylinder of pure vinyl chloride was obtained.
       °The calibration bag evacuation technique was checked to
        verify complete evacuation was occuring.
       °New calibration bags were obtained.
       "The flow meter used to meter five liters of nitrogen
        was calibrated.
                         \
       °A bag, after being filled with five liters of nitrogen,
        was evacuated through a wet test meter and found to
        vary an average of less than 0.4 percent from five liters.
       A total of 19 tests were conducted.  Each test consisted of
repeated injections of one of three standards:
       °NBS high pressure cylinder of either 40.6 ppm or 874
        ppm vinyl chloride in nitrogen standard injected directly
        into chromatograph.
       °NBS standards transferred into tedlar bag prior to being
        injected into chromatograph.
       °50 and 1000 ppm vinyl chloride standard in nitrogen
        prepared in accordance with procedure.
       Summary results of the 19 tests conducted are presented in
Table 2.8 with complete results presented in Appendix D.  One calibration
bag previously filled with 874 ppm vinyl chloride in nitrogen was evacuated
and refilled with nitrogen.  Analysis of the bag contents after 14 hours
at room temperature indicated a vinyl chloride content of approximately
1 ppm.
    SCOTT RESEARCH LABORATORIES, INC.

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 18
 19
                                              TABLE  2.8

                                Summary of Standards Investigation
   Standard Type and
  Concentration (ppm)
  NBS   NBS Bag   Bag
 40.6
874

 40.6
 A0.6
874
N2(Bottle)
40.6
           N,
          40.6
874
 40.6
 40.6
874
          40.6
          40.6
         874
                Average GC  ..
               Area (Counts)









50
50
1000







111,989
2,637,763
117,533
118,616
110,782
2,686,327
2905=1 ppm
0
121,208
163,167
160,511
3,335,252
2,858,007
113,156
119,963
117,582
120,736
2,776,128
2,749,745
Number of
Injections'

    6
    5
    3
    2
    4
    3
    2

    3
    3
    3
    3
    4
    2
    5
    A
    2
    2
    2
Max. Deviation
From Average  (%)

      1.3
      6.4
      8.5
      4.0
      5.6
      6.4
     48.6
                                                       ,8
                                                       ,8
                                                     6.3
                                                     1.8
                                                     3.9
                                                     0.8
                                                    10.3
                                                     2.0
                                                     1.7
                                                     0.7
                                                     1.1
Counts per
   ppm

   2758.3
   3018.0
   2894.9
   2921.6
   2728.6
   3073.6
                       2985.4
                       3263.3
                       3210.2
                       3335.3
                       3270.0
                       2787.1
                       2954.8
                       2896.1
                       2973.8
                       3176.3
                       3146.2
                                                                                                      N>
                                                                                                      (Ji
                                                                                                      NJ
O
10
                                                                                 Ui
                                                                                                 S3
  Corrected to 760 mm Hg. pressure and 25° C.

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                                  2-16
SET 2526 02 0175
2.4 MASS SPECTROMETER ANALYSIS
        Following gas chromatograph analysis of each A sample,
the suspected vinyl chloride peak was analyzed using a mass
spectrometer for positive identification of vinyl chloride.  In
each case, the suspected vinyl chloride peak was positively identified
as vinyl chloride and composed of only vinyl chloride.  Vinyl  chloride
levels in the B, C and Cf samples were too low for mass spectrometer
analysis.
    SCOTT RESEARCH LABORATORIES, INC.

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                                 3-1
SET 2526 02 0175

               3.0  PROCESS DESCRIPTION AND OPERATION
        A total of 21 vents are combined to make the waste gas stream.
Two of the largest of these vents are from the EDC direct chlorination
reactor and the ethylene chloride reactor Csee Figure 3.1),   Upsets in
the operation of these reactors can be detecetd by the air loading on
the pressure control valves.  Data point A is the air pressure on the
EDC reactor vent."  The valve is air to close, 3-15 pounds per square
inch gauge (PSIG).   Data point B is the air pressure on the ethylene
chloride reactor vent.  The valve is air to open, 3-15 PSIG.
        The combined streams were measured at J with a type 710, two
inch Ellison Annubar.  Pressure differential was measured in inches of
water with a Vol-0-Flo magnetic pressure cell.  A sample of the inlet
gas stream was made at point 1 and the sampling rate at point 1 was
proportional to the flow measured at J.
        The incinerator-boiler was a modified Dixon Firetube (20' x
6') rated at 10,000 pounds of steam an hour  (Ibs/hr) at 250 pounds per
square inch gauge.  During this test the steaming rate was set at
7,500 Ibs/hr.  As the heat content of the waste gas went up and down,
natural gas was added automatically to maintain  this steaming rate.  It
was, therefore, possible to detect major changes in the composition of
the vent gas by observing the natural gas valve position and the draft
air valve position.  The natural gas valve position was recorded as
data point E (as percent open) and the draft air valve position was
recorded as data point F (as percent open).  The boiler steaming
rate was recorded as data point C, and the boiler pressure was recorded
as data point D.
        A sample of the flue gas was taken at point 2.  It was not
possible to measure flow at this location.
        The flue gas scrubber was a packed column, 54 inches in diameter
and 40 feet high,  The hot gas was cooled in a quench section of the
scrubber by city water.  Two Vee Jet 3/8 UNC 50 60 nozzles sprayed the
water into the gas stream.  A sample of this steam was taken at point 5,
     SCOTT RESEARCH LABORATORIES, INC.

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                                 3-2
SET 2526 02 0175

and the pressure on  the nozzles was taken as data point G.  From  information
provided with the nozzles  the  total flow from  the two nozzles was estimated
to be  15 gallons a minute,
        The  scrubbing water  for the column was taken from a waste water
sump^  A level control device  maintained a level in the sump by regulating
the water  to the top of the  scrubber  (valve a  on diagram).  During periods
of high waste water  flow valve b also opened and allowed water to bypass
the column directly  to the sump to waste treatment.  Valve a was  air  to
open 3-15  PSIG, valve b was  air to open 6-30 PSIG.  The air loading to
these  two  valves was recorded  as data point I, the pressure on the
discharge  of the pump as data  point H.  The pH of the waste water stream
was recorded as data point K,  and a sample of  the water stream was taken
.at point 4.   Flow at point 4 was estimated by  the plant engineer  to be
75 gallons per minute.  The  water effluent from the scrubber was  sampled
at point 6.
        The  exit gas from  the  scrubber was measured by traverse and
sampled at point 3.
     SCOTT RESEARCH LABORATORIES, INC.

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            AMERICAN CHEMICAL
            INCINERATOR TEST

            OCTOBER 7, 8, 9, 1974

            Data Points A etc.
            Sample Points 1. etc.
                                                              ro

                                                              O

                                                              o
 19  other
 vents
EDC
vent
                       a
              air
            natural
              8as TS-
                                        steam to
                                        plant
                                                                   A  to atmosphere
                               Boiler
                               Fire
                               Box
chloride
vent
                two
            Vee jet
            nozzles
city
water
                                                                                                                    CO

                                                                                                                    U)
                                                          to waste treatment

                                                  Figure 3.1
                                      waste water from plant

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                                  4-1
SET 2526 02 0175

                    4.0  LOCATION OF SAMPLING POINTS

          The exhaust gas from the vinyl chloride monomer operation passed
through a caustic scrubber, incinerator and water scrubber before exiting
to the atmosphere.  To facilitate testing, an exhaust stack was fabricated
and installed on the exit of the water scrubber.   Exhaust gas  was sampled
at four points:
          o Sample Point A - Inlet to Incinerator
          » Sample Point B - Inlet to Water Scrubber
          » Sample Point C - Exit to Water Scrubber
          « Sample Point C'- Exit to Water Scrubber
          Sample Points C and C1 were located at the same sample location
and were intended to determine variability in sample collection and testing.
          In addition to the exhaust gas samples collected, three water
samples were collected:
          o Sample Point D - Inlet to Scrubber - by product process
                                                 water from monomer plant
          o Sample Point D'- Inlet to Scrubber - city water
          o Sample Point E - Water Exit to Water Scrubber
          Figure 4.1 details each point sampled during testing.  Figure
4,2 shows the location within the stack of sample points, C and C1 ,
     SCOTT RESEARCH LABORATORIES. INC.

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r>
o
50
W
t/i
M

SO
n
D5

t"

03
O
SB


O

2
M
y
N4
z
rt
                          9
                                Sampling  Point
                                                                            Stack
                      Caust
                            Lc
scrubbers
                                                    Air
                                              Natural Gas
                                                                 Process Water
                                                                                         To Atmosphere


                                                                                                  i
                                                                                      a
                                                                                                                    Ul
                                                                                                                    N>
                                                                                      o

                                                                                      o
                                                                                    31.5
                                                                                                se-
                                                                                                  T
                                                                                                       72"
                                                                                              city water
                                                                                                                       N>
                                                                                             water out
          From Process
                                                       Incinerator
                                                       Figure 4,1

                                                Sampling Point Location
                                              Vinyl Chloride Monomer Plant
                                               American Chemical Company
                                                  Carson, California
                                                                                 Water Scrubber

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                                                                                a-
                                                                                H

                                                                                to
                                                                                Ui
                                                                                ro
                                                                                o
                                                                                to
                                                                                o
                                                                                H1
                                                                                    U)
                   Figure 4.2

Cross Section of  Stack (Sample Point C and C')

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                                 5-1
SET 2526 02 0175

               5.0  SAMPLING AND ANALYTICAL PROCEDURES
        Samples for the determination of vinyl chloride content
were collected in accordance with "Tentative Method for the Deter^
ruination of Vinyl Chloride From Stationary Sources" dated September 4,
1974, a copy of which is presented in Appendix G-I.   Two-hour  integrated
samples were collected proportional to the gas stream in Tedlar bags
sealed in 55 gallon fiber barrels.  The barrels were evacuated which,
in turn, would cause the bag to expand and fill.
        Four samples were collected as described in Section 4.0.  Dupli-
cate samples (C and C') were collected at the exit of the water scrubber
using one glass and one stainless steel probe each equipped with a glass
wool filter to remove particulate matter.  Sampling after the incinerator
(Point B) was accomplished using a stainless steel probe inserted into
the gas stream at an elbow of an 18-inch diameter pipe.  Sampling before
the incinerator (Point A) was accomplished at a liquid knockout trap
installed in a four-inch diameter pipe Immediately prior to entering
the incinerator.  No sample probe was used at this sampling location,
and a small glass bulb water trap was installed between the liquid
knockout trap and the sample line.
        Moisture determination was made at all three sampling points
using EPA Method 4 as described in "Determination of Moisture in Stack
Gases", Federal Register, Volume 36, No. 247, Tuesday, December 23,
1971.
        With the concurrence of the project officer, no heated sample
line was used at sample point A.  No moisture sample was collected
at point C', and only one moisture sample was collected at" each
sampling point per day.  Moisture samples were collected for1
approximately one hour at each sample point.
        Velocity measurements were made at point C at  the beginning of
each  test day in accordance with EPA Method 1, "Sample and Velocity
Traverses for Stationary Sources" and EPA Method 2, "Determination of
Stack GasiVelocity and Volumetric Flow Rate" as described  in  the above
referenced Federal Register.
     SCOTT RESEARCH LABORATORIES, INC.

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                                 5-2

SET 2526 02 0175

        Flow rate data was also determined at sample point A via an
Annubar installed in the process line,  A description of the
Annubar and its use is contained in Appendix G-III.  The Annubar
serial number was 53442, Model 715-316-SS and had a 2.067 inch
inside diameter,
        An NO  determination was made once per day at point C in
             X
accordance with EPA Method 7, "Determination of Nitrogen Oxide
Emissions From Stationary Sources" as described in the aforementioned
Federal Register. The total chloride and chlorine content of the
exhaust gas before and after the water scrubber (points B and C) was
determined once per day in accordance with "Determination of Hydrogen
Chloride and Chlorine in Stack Gas", U. S. Department of Health,
Education and Welfare, April 1968, a copy of which is contained in
Appendix G-.H.
        Water samples were also collected of the two scrubber water
inlets and one outlet.  Two samples were taken per day.  One sample
coincided with the EPA Method 4, Moisture Sampling, a sample of water
being collected every fifteen minutes during the one-hour mositure
test.  The other water sample was integrated over all the vinyl
chloride testing conducted each day.  A water sample was collected
every one half hour during each of the two-hour vinyl chloride  tests.
Each water sample was analyzed for vinyl chloride using a chromatic-
graph and for total chloride and chlorine in accordance with Appendix
G-II.
        Molecular weights of sample gas at points B and C were
determined using mass spectrometer analysis for 0~ and C0_ content and
subsequent molecular weight calculations.  Weights at point A were
determined by tare weighing an  evacuated flask, filling the flask with
sample gas to a known pressure and reweighing the' flask.
     SCOTT RESEARCH LABORATORIES, INC.

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