MIDWEST RESEARCH INSTITUTE
                      SOURCE TESTING—EPA TASK NO. 9
                          STANDARD OIL COMPANY
                         El Segundo, California
                                 by

                              E.  P. Shea
                       MIDWEST RESEARCH INSTITUTE
                       Kansas City, Missouri  64110
                       EPA Contract No.  68-02-0228
                        (MRI Project No. 3585-C)
                                                    REPORT
MIDWEST RESEARCH INSTITUTE  425 VOLKER BOULEVARD, KANSAS CITY, MISSOURI 64110 • AREA 816 561-0202

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MRI WASHINGTON, D.C. 20005-1522 K STREET, N.W. • 202 293-3800

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                           SOURCE TESTING—EPA TASK NO. 9
                                     PC  -If)
                                STANDARD  OIL COMPANY
                               El  Segundo,  California
                                         by

                                     E.  P. Shea
                             MIDWEST RESEARCH INSTITUTE
                            Kansas City,  Missouri   64110
                             EPA Contract No.  68-02-0228
                              (MRI Project No.  3585-C)
MIDWEST RESEARCH INSTITUTE  425 VOLKER BOULEVARD, KANSAS CITY, MISSOURI 64110  •  816561-0202

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                           I.  TABLE OF CONTENTS
II.   Introduction		     2




III.  Summary of Results	     4




IV.   Sampling and Analytical Equipment and Procedures  	    20




V.    Location of Sampling Points.  ................    30




VI.   Process Operating Conditions  . . .	    32




Appendix A	  .    33




Appendix B	    41




Appendix C	    57

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                             II.  INTRODUCTION








          Under the Clean Air Act of 1970, as amended, the Environmental





Protection Agency is charged with the establishment of performance stan-





dards for stationary source categories which may contribute significantly





to air pollution.  A performance standard is a standard for emissions of





air pollutants which reflects emission limitations attainable through the





best emission reduction systems that have been adequately demonstrated





(taking into account economic considerations).





          The development of realistic performance standards requires





accurate data on pollution emissions within the various source categories.





Sampling and analytical techniques had to be developed to acquire the data.





A method for analysis of carbon monoxide  (CO) from CO boilers is needed





for the petroleum refining industry.  The nondispersive infrared analyzer





(NDIR) for very low concentrations of carbon monoxide is an instrument





that can be used.  However, carbon dioxide (C02) interferes in this analy-





sis.  This report presents the results of the tests run at Standard Oil of





California's El Segundo plant for EPA for its determination of:  (1) the





applicability of the NDIR to CO analysis, and (2) interference from C02 in





the range of concentrations normally encountered in a CO boiler stack.





          Appendix A presents a proposed method developed by EPA to sample





and analyse for CO.   This method, with modifications, was applied for these





tests.  MRI did not attempt to concentrate on comprehensive method refine-





ment.  Rather, using mutually accepted modifications, we collected samples

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persuant to the method and analyzed them.  Our comments are limited to observa-





tions in using the method and on potential variations detected between runs.





          On Monday, 27 March 1972, the equipment was shipped to California





and E. P. Shea (MRI) and W. E. Kelly  (EPA) arrived to transport the equip-





ment to  the El Segundo refinery and do the test work.  Tuesday, the 28th





of March, the equipment was delivered to the test site and preparations





made for sampling and analysis.  A preliminary velocity and temperature





profile was obtained for reference with earlier traverse results, and the





NDIR was calibrated  for use.





          Four independent integrated gas samples were collected in Tedlar*





bags on 29 March, and again on 30 March 1972.  The samples are identified as





Runs 1 through 8.  The samples were analyzed in the field on the same dates.





An S shaped pitot tube with a thermocouple installed on it was used for





velocity and temperature measurements.





          Samples were collected from a port 55 ft above the inlet breech-





ing in a stack with an inside diameter of 13 ft 10 in.  A 5-ft,  glass-lined





probe was used to withdraw gas samples from the CO boiler stack into an





integrated gas bag.  The sampling point was 42 in. from the inside wall of





the stack,  and was located at 90 degrees from the inlet breeching.





          The following sections of the report treat:  (1) the summary of





results; (2) the description of sampling and analytical procedures; (3) the





location of sampling point; and (4) process operating conditions.
*  Mention of a specific company or product does not constitute endorsement




     by EPA.

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                          III.  SUMMARY OF RESULTS








          Table I presents a summary of results from the CO and C02 analy-





sis.  There were a total of eight sampling and analytical runs.  Table II





shows the results of the velocity and temperature profiles.  The following





discussion presents characteristics of each sample run.  Results between





runs cannot be accurately compared since process variations are undefined;





however, we present variations.





          Table I contains the calculated values for gas volume sampled by





the NDIR, the volume of CC>2 trapped by the ascarite, total sample volume





analyzed, the concentration of carbon monoxide, the percent CC>2 obtained





from the absorption of ascarite and by Orsat analysis, and the concentration





of CO unscrubbed.  The data are presented by run number and by date.  The





volume analyzed on the first day varied from 0.168 to 0.520 dry standard*





cubic feet.  The volume varied according to the length of time for analysis.





Run No. 1 only lasted 7 rain and 0.168 dscf was analyzed.  The other runs





lasted from 22 to 31 min and volume varied from 0.405 dscf to 0.520 dscf.





The volume of C02 varied from 0.0036 dscf on Run No. 1 to 0.0935 dscf on





Run No. 3.  Run No. 1 was too short and the results for C02, (2.1%) illus-





trate it.  On Run No. 3, water was not put into the ice bath and the ascarite





heated up.  The results for C02 (18.8%) and CO (23.6 ppm) for this run show





the need for the ice water bath in removing the heat generated in the absorp-





tion of C02 by the caustic in the ascarite.
*  70°F, 29.92 in. Hg

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                                          TABLE I

                         SUMMARY OF RESULTS WITH SAMPLE CALCULATIONS

           Run No.   1        2         3         4         5          6_       7.        i

Date             3/29/72  3/29/72  3/29/72  3/29/72  3/30/72  3/30/72  3/30/72  3/30/72

VMC std dcf       0.168    0.515    0.405    0.520    0.278    0.282    0.260    0.198

Vco  std dcf      0.0036   0.0423   0.0935   0.0648   0.039    0.0649   0.0648   0.0202

Vs std dcf        0.1716   0.5573   0.4985   0.5848   0.3165   0.3469   0.3243   0.2182

Cco ppm          12.25    11.6

% C02             2.1      7.6

% C02 Orsat

C£Q (unscrubbed

  sample) ppm     --      17.6      —      17.4     16.2     12.2     16.0     14.5

A wta grams       0.2001   2.4092   5.2301   3.6102   2.1789   3.6140   2.1023   1.124


Sample Calculations, Run No. 2:

                  Standard conditions 70°F and 29.92 in. Hg (dry).

1.  Gas volume

                                „  17 ,,    °R       ( VM cu ft PM in. He}
23.6
18.8
_ _
11.6
11.1
_ _
4.4
12.3
12.4
5.7
18.7
9.4
7.2
12,7
13.6
5.4
9.3
13.6
       VMC - v>
                                          in. Hg     V.    TM °R
       VMC - 17.71     °R      (0.5235 cu ft   29.97 in. Hg\  = Q.515 dscf
                     in. Hg    V        540°R            J

2.  Volume of carbon dioxide collected

       VC02 = 0.01797 Awta

       VCQ  - 0.01797  cu ft  x 2.4092 g = 0.0423 dscf

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                                     TABLE I (Continued)

3.  Sample volume

       VS = VMC + VH20 + VC0     Assume VH2Q = 0
       Vs = 0.515 dscf + 0.0423 dscf = 0.5573 dscf

4.  Concentration of carbon monoxide
       c    _ c
       ccos   CCOM
       C _  =12.5 ppm x  0.515 dscf  =11.6 ppm
        C°s               0.5573 dscf
5.  Percent carbon dioxide
                     f
       % C0  =        - ?—   x 100
       % C02 =            0.0423 dscf x 100      = 7.67,
                      0.5150 dscf + 0.0423 dscf

6.  Concentration of CO in the unscrubbed sample

       cco = cc,  (u.s.)  x   C!MC)
                n             \.VS '

       Cco = 19.0 ppm x  0.515 dscf    = 17.6 ppm
                         0.5573 dscf

       VMC   = Dry gas volume through meter at standard conditions cu ft (DSCF)
       VM    = Dry gas volume measured by meter cu ft (DCF)
       PM    = Barometric pressure at dry gas meter in. Hg.
       PSTD  = Pressure at standard conditions 29.92 in. Hg.
       TSTD  = Absolute temperature at standard conditions, 530°R.
       TM    = Absolute temperature at meter °R.
       Vs    = Volume of sample at standard conditions  (DSCF).
             = Concentration of CO in sample ppm by volume.
          s
       Ccom  = Concentration of CO measured by NDIR Analyzer ppm by volume.
       VC02  = Volume of C02 collected at standard conditions cu ft dry.
       A wta « Weight change in ascarite impinger in grams.
            (U.S.) = Concentration of CO measured by NDIR analyzer ppm by volume,
                       unscrubbed.

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                                   TABLE II
                        STACK VELOCITY AND TEMPERATURE*
Run
No.
Special
5 and 6
7 and 8
Equation
Date
3/28/72
3/30/72 (a.m.)
3/30/72 (p.m.)
V~ Avc- ffnm^ =
AP Avg.
in. H20
0.445
0.313
0.306
= K C (

JAP Avg.
in. H20
0.676
0.555
0.554

n
. 1 AP AvelO
TS Av§-
°R
1237
1233
1225

Cs Avg
                                              PSMS
           K  = 85.48 ft/sec
                                   Ib
                                Ib mol °RJ
           Cp = 0.85  (pitot coefficient)


           MS = 27.1  Ib/lb-mole


           PS = 29.93 in. Hg
                                                             vs
                                                           (ft/min)   Port


                                                            3,630      W


                                                            3,000      N


                                                            2,970      N
                                                        sec/min
*  Federal Register. 23 December 1971, p. 24884, Method  2,

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The values for CO in Runs Nos. 1, 2 and 4 are very close:  12.25, 11.6 and





11.6 ppm.  The unscrubbed values for CO in Runs Nos. 2 and 4 show the CO





contributed about 6 ppm to the CO reading on the NDIR.





          The results for the second day of sampling for CO show a variation





of 4.4 ppm to 7.2 ppm CO.  The C02 results from the absorption of ascarite





are close except for Run No. 6 (18.7%); they vary from 9.3% to 12.7%.  The





unscrubbed CO values are reasonably close for the four runs on the second





day with the exception of Run No. 6.  They show an average C02 contribution





to the NDIR reading for CO of about 10 ppm.  The values range from approxi-





mately 7 to 12 ppm.  The Orsat results for G02, with the exception of Run





No. 6, are reasonably close.  The average C02 concentration for Runs Nos.





5  (12.4%), 7 and 8 (13.6%) is 13.2%.  While performing the Orsat analysis





in Run No. 6, the bag was ruptured by excessive pressure.  This bag was





discarded and a new one installed in the holder before collecting Samples





Nos. 7 and 8.





          The velocity of the stack gas in Table II varies from 2,970 fpm





to 3,630 fpm with an average of  3,200 fpm and the temperature varies from





1225°R to 1237°R with an average of 1232°R.





          In Runs Nos. 2 through 8, the ascarite impinger was removed after





analyzing the gas stream for CO  and the gas passed  through the rest of the





equipment to assess the effect of C02 on the NDIR results.  Figures 1 through





8  are the charts from the recorder for each run.  The field data sheets

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corresponding to the recorder charts are presented in Appendix B.  The





numbers on the chart (Figure 1), 17.0 and 17.5 are the NDIR readings from





the data sheet.  The NDIR reading in the field data sheet is taken directly





from the indicator on the NDIR.  In Run No. 1 the data sheet shows that a





steady reading was reached after 3 min and the reading used for calculation





of ppm CO was an average taken after steady state was reached.





          In Runs Nos. 1, 2, 5, 6 and 7, examination of the recorder charts





and field data sheets show that a constant reading was obtained after 3 to





5 min.  Run No. 8 took about 9 min to reach a constant reading, but the





rotameter reading for this run was 8 instead of 14 and less total sample





was employed to obtain a steady reading.  Run No. 3 was started without





purging all lines with nitrogen and with no water in the ice water cooling





bath for the ascarite and silica gel.  This run, after 7 min, was stopped,





everything purged with nitrogen and then restarted.  This run gave results





that do not correlate with the data from the other runs.





          The NDIR value for Run No. 4 steadily increased for 20 min indi-





cating that the ascarite was not doing an efficient job of scrubbing out





the C02-  The calculated values for CO and C02 for Runs Nos. 2 and 4 are





comparable.  Examination of Figures 2 to 8 and the corresponding field





data sheets in Appendix B shows that with the exception of Run No. 3 all





readings without ascarite scrubbing reached a steady state after 2 min.





The reading was an average after steady state was obtained.  The readings





for Run No. 3 are unexplainable.

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Figure 1 - Run No. 1
         10

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-r~r

     Figure  2  -  Run No. 2
              11

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Figure 3 - Run No. 3
        12

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Figure 4 - Run No. 4
        13

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Figure 5 - Run No. 5
        14

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! :  ;TJ J .     .  •  '
~~     ~  ~  ™—-•
                                                 
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±U_LU_'_L.z=:
                                                           h
                                                           I-
                                                           U
                                                           J

                                                           §
                                                           U
                                                           I
                 Figure 7 - Run No.  7
                          16

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Figure 8 - Run No. 8
         17

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          Figure 9 is the calibration curve for the NDIR, that relates




the NDIR reading ;to ppm CO.  It was calibrated using nitrogen, 22 ppm CO,




41 ppm CO and 83 ppm CO for full scale deflection.
                                     18

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                             Beckman NDIR Calibration  (By MRI)
                 Date:  3-15-72
                 Calibrated by:  N. Stich
                 Cells:  15 1/2 in.
                 Zero Gas:  Nitrogen
Tune: 61
Gain: 618 Range 3
Full Scale Deflection: 83 ppm
Application:  CO
100
                                             PPM
                                           Figure 9

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            IV.  SAMPLING AND ANALYTICAL EQUIPMENT AND PROCEDURES


          The CO boiler stack at Standard Oil of California's El Segundo

plant was the site chosen for sampling the stack gas to determine the

applicability of the analytical method for CO using the nondispersive

infrared analyzer (NDIR).


A.  Sampling Equipment and Procedure

          Figure 10 is a schematic of the equipment used to obtain an

integrated gas sample.  A glass-lined heated probe was inserted through

a cover plate fastened to the port.  The probe was connected with. Tygon*

tubing to an air cooled condenser, a rate meter and the Tedlar* gas bag.

Flow was controlled by use of a micrometer adjusted needle valve.  A

vacuum pump was connected to the bag holder and the resulting vacuum

used to withdraw the sample from the stack.  The bag was leak checked

prior to obtaining a sample.

          Figures 11 through 14 are colored photographs showing the equip-

ment and arrangement of this equipment in sampling.  Figure 11 shows the

probe inserted through the port cover into the stack.  The probe and the

method of connecting with the Tygon* tubing is shown in Figure 12.  The

condenser and gas bag holder appear in Figure 13.  The flowmeter, microm-

eter needle valve, the gas bag holder, and the vacuum pump are displayed

in Figure 14.
*  Mention of a specific company or product does not constitute endorsement
     by EPA.

                                    20

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-Glass Wool

 Filter
                   J-
     Glass Lined Probe
4
                            O
                            o
                            o
Condenser
                       Flow Valve
                                       Rate Meter
                                    Gas Bag
                                                                                Pump
                    Figure 10 - Sampling Apparatus For Carbon Monoxide

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      Figure 11 -
  Port Cover - Probe
      Heater Cord
           Figure  12  -
       Probe and Connector
     Figure  13 -
Condenser - Bag Holder
          Figure 14 -
Rate Meter - Micrometer Valve
   Bag Holder - Vacuum Pump
                                22

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B.  Analytical Procedure and Equipment

          The schematic of the equipment used in analyzing the stack gas

for CO and CC>2 is shown in Figure 15.  Everything but the gas bag was purged

with nitrogen before and after sampling.  Purging with nitrogen sweeps out

entrained air or other gases.  A Bechman* Infrared Analyzer  (NDIR) Model

215°Awitha 15.25 in. CO sample cell and a 15.25 in. reference cell with

optical filters (for removal of interference from NH^) was used.  The

range of the instrument is from 0-150 ppm CO.  A Hewlett Packard* Model

No. 680 strip chart recorder was used with the NDIR.  The NDIR was zeroed

by using 100% nitrogen and the span was set by using an 83 ppm CO in

nitrogen.

          Figures 16 through 20 are colored photographs of the setup used

in the analytical procedure.  Figure 16 shows the nitrogen cylinder being

used to purge the tubing and the equipment and to zero the NDIR.  Figure

17 shows the 83 ppm CO (span gas) used to establish the upper limit of the

analytical instrument.  Figure 18 is an overall view of the equipment used

in analyzing the stack gas.  Figure 19 is a close-up of the  impingers con-

taining silica gel and ascarite in the ice water bath with the NDIR and dry

gas meter in the background.  Figure 20 is a close-up showing more details

of the hookup with  the Tygon* tubing from the gas bag to the impinger,

through the flowmeter, the drying tube, the filter, the NDIR with recorder

and the dry gas meter.  Figure 21 shows the Orsat being used to analyze

for C02 and 02-
*  Mention of a specific company or product does not  constitute endorsement

     by EPA.
                                    23

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Air 5-10 psig
      Gas Bag
          100% N.
  MV-
                                  t
                                        Ice Bath
Silica Gel |	Ascarite
Impinger    Impinger
CO 83 ppm
  In  N2
                        Rate
                        Meter
                                                                   •Glass Wool

                                                                    .Silica Gel
                                                                               Recorder
                                     Filter
                                     Furnished
                                     by NDIR
                                     Manufacturer
                                                                                      Thermometer
                                                                                 Dry Gas
                                                                                 Meter
                       Figure 15 - Analytical Apparatus For Carbon Monoxide

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     Figure 16 -
Setup With N2 Cylinder
      Figure 17 -
Analytical Setup With
       Span Gas
                          Figure 18 -
                   Overall View of Equipment
                       Analytical Setup
                              25

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        Figure  19  -
Impingers  in Ice Water Bath
        Figure 20 -
Close-Up of Analytical Setup
                             Figure 21 -
                           Orsat Analysis
                                  26

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          After purging all lines with nitrogen, the line to the gas bag

was connected to the impinger containing silica gel.  Air pressure was bled

into the gas bag holder forcing the sample gas out of the bag through the

impingers containing silica gel and ascarite; through the flowmeter (the

rotameter reading for the test was set at 14 on a Matheson* Model No.

620PBW603 flowmeter with an R-2-15B tube) a drying tube containing glass

wool and silica gel; a filter, furnished with the NDIR; the NDIR, equipped

with an external recorder, and finally through the dry gas meter (an

American Meter Company* Charcoal test meter Model No. AL-110, where tempera-

ture and total flow were measured).  The sample gas was run through the

system until a steady reading was obtained on the NDIR.  After the reading

stabilized on the NDIR, the flow was stopped and the ascarite removed fbr

weighing.  The weight gain provides CO  collected volume.  The flow of sample

gas was restarted and continued until a steady reading was again obtained on

the NDIR.  This reading is the effect of interference  (primarily C02)  and CO.


C.  Observations

          The geometry of the stack must be carefully considered in select-

ing a single sample point.  The carrier gas must be  thoroughly mixed at

the sample point, otherwise a sample traverse would be necessary.  On

negative pressure stacks, sealing of the port around the probe is essen-

tial.  If the opening is not properly sealed, there  is a possibility of
*  Mention of a specific company or product does not constitute endorsement

     by EPA.
                                    27

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diluting the sample with air.  A single-point sample should be located





well into the stack.





          Since the method does not allude to sample point criteria, the





above observations were incorporated to project a sample point 42 in. from





the inside wall and at 90 degrees from the inlet breeching at approximately





4 diameters downstream from the breeching.





          In the analytical procedure there are two very important pre-





cautions that must be taken.





          All of the equipment and tubing used in the analysis must be





purged with nitrogen before the sample is introduced to ensure that none





of the tubing or equipment is contaminated with the previous sample.  The





silica gel and ascarite impingers must be in an ice water bath, or the





caustic in the ascarite might react with other components of the gas stream,





particularly S02 and 803, if present.  Also, excess heat causes water to





be formed from the reaction between C02 and NaOH.





          The procedure "Gas Analysis for Carbon Monoxide" (dated 10





February 1972), as furnished by EPA is included in this report as Appendix





A.  We made some changes and additions to this procedure for this test.





These changes are:





5.3.5 - Used 25-30 grams of preweighed ascarite instead of 200 grams to





improve the accuracy in determining the weight change of the ascarite.





7.3 - The silica gel tube was not  weighed because this would only give





the percent moisture in the bag.  The sample was passed through a condenser







                                    28

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before filling the Tedlar* bag.  The volume of the water condensed from

the sample and the volume of gas sampled would have to be measured before

the stack moisture could be determined.  The percent moisture was not a

test objective.

9.4 - Assume V^20 = 0-

The additions are:

5.3.6 - Ice water bath for ascarite and silica gel.

5.3.7 - Needle valve to adjust and maintain constant flowrate.

5.3.8 - Span gas for NDIR.

5.3.9 - Flowmeter to measure flow rate.

5.4.0 - Dry gas meter with thermometer.

5.4.1 - Recorder for NDIR.

7.3   - The lines and equipment must be purged with nitrogen before the
          gas is analyzed.
   Mention of a specific company or product does not constitute endorsement

     by EPA.
                                    29

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                      V.  LOCATION OF SAMPLING POINTS







          Figure 22 shows the location of the two ports used in sampling





for CO analysis and for temperature and velocity profiles at the boiler





stack.  The samples were collected at an elevation of 55 ft (about four





stack diameters) above the inlet breeching.   The inside diameter of this





stack is 13 ft 10 in.   The CO samples and the first velocity profile were





taken from the port at 90 degrees from the inlet breeching.  The other





two velocity profiles  were taken from the port above the inlet breeching.
                                    30

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                        SAMPLING LEVEL
                          13 FT 10 IN,
            SIDE VIEW OF
            BOI LER  STACK
Figure  22 - Location of  Sampling Station
                 31

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           VI.  PROCESS OPERATING CONDITIONS
This section is to be furnished by EPA.
                         32

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                                APPENDIX A







          The following represents the suggested method of sampling and





analyzing for carbon monoxide.  This method was furnished by EPA.  Observa-





tions on the method are tabulated in Section IV-C.
                                    33

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                                    ^                   2-10-72
                       Gas  Analysis  for Carbon Monoxide


_ .1.   Principle and Applicability

        !•'  Principle.   An integrated or grab gas  sample is extracted from
            a  sampling point  and  analyzed for carbon monoxide content using
            a  nondispersive infrared  analyzer or equivalent.

        1.2  Applicability.   This  method should be  applied  only when speci-
            fied" by  the test  procedures for determining compliance with the
            new  source performance  standards.  The test procedure will
            indicate whether  a  grab or an integrated sample will  be.used.

    2.   .Range and Sensitivity.

        2.1  ' Ranse.   0-100  p.p.m.

        2.2  Sen_sj_ui .'Uy/.   Mini nun detectable sensitivity is 4 p.p.m.

    3-   Interferences           .'                               I      '

        3.1  Any  substance  having  a  strong absorption of infrared  energy
            will  interfere  to soi.ie  extent.   For example, discrimination
            ratios for water  and  carbon dioxide are 2.5:1 H^O/? p.p.rr. CO.
            and  10;;  CC^/ICp.p.in. CO, respectively, for devices :;;eesuring
            in tfie 1500 to  -3COG p.p.m.  range.  For devices measuring  in
            the  0-100 p.p.m.  ranae, interference ratios can be as high as
            3.5% H?0/25 p.p.;n.  CO and 102 C0?/50 p.p.m. CO.  The  use  of
            silica gel  and  ascar'ite .traps witl  aleviate the major^inter-
            ference  problems.   The  measured gas volume must be Corrected
            if these traps  are  used.

    4.   Precision  and /-.ecuracy

        4-1  £r.e_ci5_ip_n.   The precision of most NDIR analyzers is approximately
            ± ~2% vi  span.'  The  precision of the overall method is unknown.

        ^•2  Accuracy.   The  accuracy of most NDIR analyzers is approximately
            ± 5%  of  span after  califcration.   The accuracy  of the  overall
            method is  unknown.                                      .

    5.   Apparatus
                                                     *

        5.1  Grab  sample (Figure 3-1)  Federal  Register, 36, 24886, Dec. 23, 1971

            5.1.1  Probe.   Stainless  steel  or Pyrex glass, equipped with a
                   filter  to  remove particulate matter.

            5.1.2  Pump.   One-vay. squeeze b-jlb, or equivalent, or leakless
                   disphro-rr p-j.-p  cr equivalent, to transport gas  sample to
                   analyzer.
                                                                1      •       V
                                        34

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                             - 2 -

5.2  Integrated sample (Figure 3-2) Federal Register, 36, 24886,
 -   Dec. 23, T97i.

     5.2.1  Probe.  Stainless steel or Pyrex glass, equipped with
            a filter to remove particulate matter.

     5.2.2  Air cooled condenser or equivalent - to remove any
            excess moisture.                            _.

     5.2.3  Needle valve - to adjust flow rate.

     5.i?.4  Pump.  Leak-free diaphram type, or equivalent to pull gas.

     5.2.5  Rate meter.  To measure a flow range from 0 to 0.035 C.F.M.

     5.2.6  Flexible bag.   Tedlar, or equivalent, with a capacity of
            2 to 3 cubic feet.  Leak test the bag in the laboratory
            before using.

     5.2.7  Pitot tube.  Type S, cr equivalent, attached to the
            probe so that  the samoling rate can be regulated pro-
            portional  to the stack gas velocity when-velocity is
            varying with tine or a sample traverse is conducted.

5.3  AraJ^sJA-

     5.3.1  Nondispersive  infrared analyzer, or equivalent.

            fa) range-0-100 p.p.m.
            (b) output (iT'inimunJ-O-lO mv.      "         *
            (c) minimum detectable sensitivity-4 p.p.m.
            ("d) rise time  (maximum)-30 seconds to 90% response.
            (e) fall time  (maximum-30 seconds.
            (f) zero drift (maximum)-lO'i  in 8 hours.
            (g) span drift (maximum)-10%  in 8 hours.
            (h) precision-: 2%.
            (i) noise  (maximum)-: 1%.
            (j) linearity-2. of  scale.
            (k) Interference rejection ratio-C02 - 1000/1,  H20 - 500/1.

     5.3.2  Drying tube.   Approximately 200 g. of dry preweighed
            silica gel.
                                            «
     5.3.3  Calibration gas.              .

     5.3.4  Particulate filter.   As recommended by NDIR  manufacturer.

     5.3.5  C02 removal tube. Approximately 200 g. of•preweighed
            ascarite.(P
                               35

-------
                                  -  3 -

6.  Reagents

    6,1  Calibration  gas.   Known  concentration of CO in N? for instru-
         ment span, prepuri fie-ci grade of 'i\£ for zero.  Three concentra-
         tions corresponding  to span, 60%  span, 30'= span.  The span
         concentration shall  not  exceed 1.5 times the applicable source
        - performance  standard.

    6.2  Silica gel.  Indicating  type,  6-16 mesh, dried at 175°C
         (350°F)  for  2 hours.
    6.3

7,  Procedure

    7.1  Grab sampling.

         7.1.1  Set up  the equipnent  as  shewn in Figure 3-1  (Federal
                Register, 36,  24{x"'6,  Dec.  23, 1971)  making sure all
               .connections  are  leak  free.   Place the probe in the
                stack at a sampling -:oint  ar.d pur'..":-  tho sampling line.
                Connect the  analyzer  :,T.d cr^.-i sample into the analy/er.
                Allow five minutes  for  the  syst-?-:: tc stabilize and
                record  the analyser readir.j.   (See Sections  7.3 and 8.)

    7.2.  Integrated samp'ljng.                    :

         7.2.1  Evacuate the  flexible bag.   Set up the equipment as
              - shown in Figure  3-2 (Federal  Register, ?6 , 2^8.~,6, Dec. 23,
                1971) with the bag discc-rrect.-s-d.  Ploce the  probe in the
                stack and purge  the s a- :: ", i n ^  Lire.  Collect  the'bjg,
                making  sure  that  all  connections are tight and that
                there are no  leaks.   Sample at a rate propcriional to
                the stack velocity.

    7.3  Anajys_[s_.  Assemble  the  apparatus, calibrate the instru.vnt , and
         perform other  required  operations  as doscriced in Section 8.
         Direct the sarr.yle stream through  the instrument for the test
         period, recording the readings.   Check the  zero and span again
         after the test to insure that  any  drift or  malfunction is
         detected.  Record the sample volume  passed  through  the system.
         Remove and carefully weigh the^sTiTca gTpar.d ascarite tubes.
8.  Calibration.  Assemble the apparatus  according to Figure 1.  Care-
    fully weigh the silica gel and  ascarite  tubes  before assembly.
    Generally an instrument which is  started up  cold requires a warm-up
    period before stability is obtained.   Follow the manufacturer's
    instructions for specific procedure.   Allow  a  minimum time of one
    hour for warm-up.  Turing this  tiro chec-, the;  ifirir'il1 conditioning
    apparatt.-, , i.e., fi '!•.-:>-.. .:<••;•.•:•.<• •.?-•, c-'J''- '.-jbo
                                                                    -7 .  . _
                                                                    L'-\ (J
    and calibrate the instru:;:ont according  to  the  manufacturer 's procedures
    using nitrogen and the calibration  gases respectively.
                                     36

-------
                              - 4 -
Calculations
9.1  Volume of water_vaoor collected.
              A wt  /PH00
                  a
          •«  0.0474 cu. ft.  (A wtj
  "•                 ~~*r~
     where:
     VupO  =  Volume of water vapor collected at standard condi-
              tions, cu. ft.                                       .
     A wt  =  Weight increase in silica gel tube + weight of liquid
              water collected in air-cooled condenser, g.
     PH 0  =  0ens">ty °f water, 1 g./ml.                          .
     M^^O  =  Molecular weight of water,  18 Ib./lb.-mole.
       R   =  Ideal gas constant, 21.83 inches. Hg-cu.ft./lb. mole-°R.
     TSTD  =  Absolute temperature at standard conditions,  530°R.
     P _   =  Absolute pressure at standard conditions, 29.92 inches  Hg,
9.2  Vou:'e of carbon dioxide collected.         '         ".   '
     V     =  If. wt \    r-f•" .v.*.a •	
     VC02     v^ wV       44 g./moie        28.32 1./cu.ft.
           =  0.01797 A wt   '
                          a
     where:       *        .
     V£Q   =  Volume of CCL collected at standard conditions,  cu.  ft.
     A wt, =  Weight increase in ascarite tube,  g.
9.3  Gas volume.
           •  17'71
                               37

-------
                                  - 5 -

        /  where:

          VMC   = Dry gas volurre through meter at standard conditions,
                  cu. ft.
                                              i
          VM    e Dry gas volume measured by meter, cu. ft.

          p..    = Barometric pressure at dry gas meter, inches Hg.

       ""  ''sin  = Pressure at standard conditions, 29.92 inches Hg.

          TrjD  = Absolute temperature at standard conditions, 530°R.

          TM    = Absolute temperature at meter, °R.

     9.4  Sarpple_vplume.

          V       = v .  + v     + v
          VSAMPLE   VMC   VH20    VCO?

          where:

          ^SAMPLE = Vo^urr'e 0
-------
Continuous CO Monitoring System, Model  A 5611, Intertech Corp.,
Princeton, N. J.

Bendix--UNOR fnfrared Gas Analyzers.  Ronceverte,  W.  Va.
                               39

-------
  Sample
   Inlet
cXXl
                Silica Gel
                 Zero Gas
                 Span Gas
Ascarite
                       J    ^L
NDIR CO
Analyzer
Dry Gas
Meter
                                    Figure A-l

-------
                      APPENDIX B
The Field Data Sheets are contained in this appendix.
                         41

-------
                      VELOCITY' TRAVERSE FIELD DATA
Plant S-
Test
               /•
                    £•
         S pe. cy/9 L-
 Location C o ~B* ',/*>
 Date
 Operator
 Mcter All
Clock
T i rr.2
3PM



	 .
	




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A
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9
II
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oluck i t;n!j L . r i
                                                                 77?i
                                                                JZ.2X.
                                                                       r'

in.  II20  Average
 n.
                                42

-------
III. SAMPLE DATA
TEST
Project C 0 /-I &/)/, Sample Date W<2?772-

Test
&/9//y
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t-J r trff
Port
No.
UJ























Point
No.
tf
/A/.






















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Filter
No.









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Sample
Time
Min.
0
I
a
3
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7


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/o

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,




Start
Time
'£*





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'00

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43

-------
III. SAMPLE DATA
TEST
Project C(9 frf#L$smplie Data 3 / >7~
Port
No.
\JO














1 \
1
1






Point
No.
£
//>'"'
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Filter
No.















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Sample
Time
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o
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r
3
if
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7
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A?^a























44

-------
III. SAMPLE DATA
EMISSION TEST
Project CO, /hffl/. Sample Data 3/^9/7 2-
Test

Port
No.
'ti>
iP-
It*












1



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Point
No.
8
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,*>
















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Filter
No.







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Sample
Time
Min.
£
/
2-
3
//
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7
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$
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13
if-
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/
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45

-------
III. SAMPLE DATA
EMISSION TEST
Project £~0 fy/Ufll' Sample Data 3/^.^/77-
Test
Team.//L, Test NO. £/.
B^H*


/
Asc/9/nr^ utf-
Port
No.
li)
^P
ti&












fivfi
\







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No.















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k^/i/yi








RAC
Filter
No.















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Sample
Time
Min.
V
/
^
3
^
h
7
y
<).
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12.
ll
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!0
0
/
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^













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/t> u.
-------
III.  SAMPLE DATA
     EMISSION TEST
                            Test Team
                                                           L, Sample Data 3/3O/7
                                                                est NO.   £~
Port
 No.
Point
 No.
  RAC
Filter
  No.
Sample
 Time
 Min.
Start
Time
 T>i -f. 04,
 • in uo u
in.  Ik(
                                        Vacuum
                                        in. Hg
                                 Meter
                                  ft3
 Temp.  °F
Left Right
Temp.
  F
                                                                            S. Gel
                                                                            ft-otrrr
Temp.
•Temp~
 IV
8
(9
                                        3,6)
                    d
                    $
                                7,0
                    1
                     ?
                    9
                   /o
                    1C
                                                          goo
                                                                                           ,0
                                                 47

-------
                                ORSAT  FIELD DATA
         Location
         Date      3/30/7 2-
         Time
         Operator
iL.
                              Comments:
Test
M < ^X
-fr o -***
(^)
©





(co2)
Reading 1
// -z

/<2.)
/2,7





(02)
Reading 2
—&~£—r/-rt—±
^7T7-f 4^ 5^^
/6. / •
^'^ 4/,^





(CO)
Reading 3
G

0
O





                                 48
NCAP-31  (12/67)

-------
III.  SAMPLE DATA
     EMISSION TEST
Project
Test Teamyre//v-S/?a^v Test NO.
Sample Datfc 3J3O/7
Port
No.
«J
X
,/








/to*












Point
No.
$
It









£ /o/e ft












RAC
Filter
No.










f — *













Sample
Time
Min.
o
/
3-
J
^
3"
£
7
f
^
/P
/o
/2-'
/•
S,*-
%$'
X.V
P. 3
?,$
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'
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20, f
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fr,?









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ft3
,73%{










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Left
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cy^t
^ t/
-------
                                  ORSAT FIELD DATA
Location

Date
          Time	/
          Operator
                                                     Comments
            Test
                  (co2)
                  Reading 1
(Q2)
Reading 2
(CO)

Reading 3
                                                                 O
                                     50
NCAP-31 (12/67)

-------
                      VELOCITY TRAVERSE  HELD  DATA
  Plant  £r/y
 Test
 Location Co
33 oJ •
                  •>
 Operator   Sftx/7 ttfc'A L-/'
                           -f

 Meter AH
in. 1!20  Average	
                                  51
(12/CV)

-------
III. SAMPLE DATA
EMISSION TEST
Project £,O A ft/A/, Sample Date- J/ 30/7 2-
Test

Port
No.
u)
3.7*
*/;*>








* >c/>.



\








Point
No.
g
dl'1









Cfift ll












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Filter
No.











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Sample
Time
Min.
0
i
cZ
3
^
b
(o
7
t
c/
(0
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/^
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Team5/y>kl,/iW/\/
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Test NO. "7



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-------
                                  ORSAT FIELD  DATA
Location
6, /   67,
                   I     ,
          Date  3 1 3 0/7
          Operator
                  -
                                                     Comments:  £&  /%?<'/
Test
7
?c
^X^





(co2)
Reading 1
/2,6
/ 3, 6
H.b





(Q2)
Reading 2
/6,^ 70
/!-« (!T ^'^






NCAP-31 (12/67)
           53

-------
III. SAMPLE DATA
EMISSION TEST
Project 5A£2L^c/4£Sa


Port
No.
sv



\









/l/e/









Point
No.
&'
^
8











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Filter
No.
$&













IT*









Sample
Time
Min.
o
1
A
J
^
JT
^
7
ar
7
/^
/^.
/y
/^
/
a
3
/
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3
/D
/ 1
/ z-
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Start
Time
^ 4/
fa












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JTJj^^^^B X* >^^
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lata 1$ 3/3G/72-,
FO. %

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.









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Meter
Temp. °F
Left
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.














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Temp.
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^#5M

-













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i

i
!
j
' i

-------
                                  ORSAT  FIELD  DATA
          Date

          Ti me   *7/ 3 D     ?
          Operator
                                                     Comments:£&~fie f/
            Test
(co2)
Reading 1
(o2)
Reading 2
(CO)

Reading 3
            g*
NCAP-31 (12/67)
                                       55

-------
                           VELOCITY TRAVERSE HELD DATA
        Plant  %&cJ?- ,

        Test
                      Cr
        Location

        Date
        Operator

        Meter AH
 Clock
 Time
jirit
6 ''
?'<
/I"
,7"
?¥ ''
i<*'r
y
-------
                      APPENDIX C
The sampling and analytical logs make up this appendix.
                         57

-------
Analytical Log
Run
1
2
3

4
5
5
6
6
7
7
8
8
Pollutant
CO,
CO,
CO,

CO,
CO,
CO 2
CO,
C02
CO,
C02
CO,
CO 2
CO
CO
CO

CO
CO
, o
CO
, o
CO
> o
CO
, o
2
2
2

2
2
2
2
2
2
2
2
2
Date
3/29/72
3/29/72
3/29/72

3/29/72
3/30/72
3/30/72
3/30/72
3/30/72
3/30/72
3/30/72
3/30/72
3/30/72
Be
1:
2:
5:
6:
6:
5:
5:
12:
12:
1:
11:
1:
6:
6:
6:
7:
gan
52 p.m.
13
45
15
27
10
31
08
20
40
22
50
14
50
54
30
p.m.
p . m.
p .m.
p.m.
p.m.
p.m.
p .m.
p.m.
p.m.
p .m.
p .m.
p .m.
p .m.
p .m.
p .m.
Ended
1:
2:
5:
6:
6:
5:
5:
12:
12:
1:
11:
2:
6:
7:
7:
7:
59
40
52
25
32
30
42
18
27
50
37
00
41
00
24
40
p .m.
p .m.
p .m.
p .m.
p .m.
p.m.
p.m.
p .m.
p .m.
p .m.
p .m.
p .m.
p .m.
p .m.
p.m.
p .m.
Elapsed
Time
(min)
7
27

22
31
17
10
15
10
27
10
30
10
58

-------
Ul
VD

Run
1A
1
2
3
4
5
5 and 6
6
7
7 and 8
8

Location
Stack (W)
Stack (W)
Stack (W)
Stack (W)
Stack (W)
Stack (W)
Stack (N)
Stack (W)
Stack (W)
Stack (N)
Stack (W)
Sampling
Pollutant
Velocity and Temp.
CO, C02
CO, C02
CO, C02
CO, C02
co, co2, o2
Velocity and Temp.
CO, C02, 02
co, co2, o2
Velocity and Temp.
CO, C09, 00
Log
Date
3/28/72
3/29/72
3/29/72
3/29/72
3/29/72
3/30/72
3/30/72
3/30/72
3/30/72
3/30/72
3/30/72

Began
3:00 p.m.
9:30 am.
10:15 a.m.
3:00 p.m.
4:00 p.m.
9:00 a.m.
9:45 a.m.
9:45 a.m.
3:00 p.m.
3:45 p.m.
4:15 p.m.

Ended
3:30 p.m.
10:15 a.m.
11:00 a.m.
4:00 p.m.
5:00 p.m.
9:45 a.m.
10:00 a.m.
10:45 a.m.
4:15 p.m.
4:00 p.m.
5:30 p.m.
Elapsed
Time
(min)
30
45
45
60
60
45
15
60
75
15
75

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