Report No.  74-SRY-4
  CD
o.
AIR  POLLUTION
EMISSION  TEST
                       STAUFFER CHEMICAL COMPANY

                       DELAWARE CITY, DELAWARE
         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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             P.O. Box 13454"UNIVERSITY STATION • GAINESVILLE, FLORIDA 32604• 904/372-3318
                            environmental science and engineering.,  inc.

                                     AN EQUAL OPPORTUNITY EMPLOYER

                                                73-153-001
•#V1RCWV£KTAL SCIENCES                             REffftENCE	L *J  \ •J >J \J\J I	                           ENVIRONMENTAL ENGlNEERIN


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                     SOURCE TEST REPORT
REPORT NO:         74-SRY-4
PLANT TESTED:       Stauffer Chemical  Company
                   Delaware City,  Delaware
EMISSIONS FROM:    Sulfur Recovery Plant
TESTOR:            Environmental  Science and Engineering,  Inc.
                   Post Office Box 13454
                   University Station
                   Gainesville, Florida  32604
CONTRACT NO:       68-02-1402, Task Order No.  1

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                        TABLE OF CONTENTS



                                                              Page No.



1.0  INTRODUCTION  	      1



2.0  SUMMARY AND DISCUSSION OF RESULTS  	      3



3.0  PROCESS DESCRIPTION  	      8



4.0  LOCATION OF SAMPLING  POINTS   	



5.0  ANALYTICAL PROCEDURES 	



     APPENDICES 	



     A.   EMISSION  TEST  RESULTS WITH SAMPLE CALCULATIONS .  .  .



         A-l.   CALCULATIONS	      A-l



         A-2.   SULFUR COMPOUNDS BY GAS CHROMATOGRAPHY ....      A-4



         A-3.   TOTAL SULFUR BY MELOY ANALYZER 	      A-7



         A-4.   SULFUR COMPOUNDS BY DUPONT .ANALYZER	      A-9



         A-5.   CO,  C02  and 02 (NDIR AND PARAMAGNETIC) ....      A-12



         A-6.   SULFUR DIOXIDE BY EPA METHOD 6	      A-l5



         A-7.   NOY  BY EPA  METHOD 7	      A-16
                A


         A-8.   ORSAT	      A-l 7



         A-9.   H2S  BY EPA  METHOD 11	      A-18



         A-10.  VELOCITY BY EPA METHOD 1 AND 2	      A-19



         A-T1.  MOISTURE BY EPA METHOD 4	      A-20



         A-12.  VISIBLE  EMISSIONS BY EPA METHOD 9	      A-Zl



         A-l3.  PLANT PROCESS DATA OBTAINED DURING TESTING .  .      A-22



     B.   FIELD DATA



         B-l.   SULFUR COMPOUNDS BY GAS CHROMATOGRAPHY . .  ., .      B-l



         B-2.   TOTAL SULFUR BY MELOY ANALYZER	      B-l 2



         B-3.   SULFUR COMPOUNDS BY DUPONT ANALYZER  	      B-16



         B-4.   CO,  C02  AND 02 (NDIR AND PARAMAGNETIC) ....      B-21







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              TABLE OF CONTENTS continued



                                                        Page No.



    B-5.   VISIBLE EMISSIONS 	      B-36



    B-6.   S02 BY EPA METHOD 6	      B-54



    B-7.   MOISTURE DATA	      B-58


    B-8.   NO  DATA	      B-62
           x


    B-9.   VELOCITY DATA	      B-74



    B-10.  H2S BY EPA METHOD 11	      B-78



C.   LABORATORY REPORT


    C-l.   S02 BY EPA METHOD 6	      C-l



    C-2.   NOY BY EPA METHOD 7	      C-4
           /\


    C-3.   H2S BY EPA METHOD 11	      C-6


D.   CALIBRATION STANDARDS 	      D-l



E.   PROJECT PARTICIPANTS  	      E-l
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                             1.0   INTRODUCTION

Under Section III  of the Clear  Air Act of 1970, as amended, the Environ-
mental Protection  Agency is  charged with the establishment of standards of
performance for new stationary  sources which may contribute significantly
to air pollution.   A performance  standard is based on the best emission
reduction systems  which  have been shown to be technically and economically
feasible.

In order to set realistic performance standards, accurate data on pollutant
emissions is normally gathered  from the stationary source category under
consideration.

The sulfur recovery system at Stauffer Chemical Company's Carbon Disulfide
Plant at Delaware  City,  Delaware, was designated as a well controlled
stationary source  and was thereby selected by the Office of Air Quality
Planning and Standards (OAQPS)  for an emission testing program.  Tests
were conducted on  the IFP sulfur  recovery unit during June 10-12, 1974.  The
tests were performed by  personnel  from Environmental Science and Engineering,
Inc., Gainesville, Florida,  and the Environmental Protection Agency, Emission
Measurement Branch, OAQPS, Research Triangle Park, North Carolina.

The sulfur recovery system consists of a 395  long  tons  per day  (LT/D)  Claus
Sulfur Recovery Unit followed by  a IFP-1500 tail gas plant for sulfur removal.
The IFP-1500 unit  treats the tail  gas from the Claus Unit to remove additional
sulfur before the  .gas is released to the atmosphere.
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Tests were conducted at a point downstream from  the  IFF unit in the duct
just before the  incinerator.  The tests were designed to determine the
average emission  rates during four-hour sampling periods on each of
three days.   The  emissions measured were:   sulfur compounds (hydrogen
sulfide, carbonyl  sulfide, carbon disulfide, sulfur  dioxide), carbon
dioxide, oxygen,  carbon monoxide, nitrogen oxides, and visible emissions.
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                  2.0   SUMMARY AND DISCUSSION OF RESULTS

  2.1   A complete  summary of all data collected for the three four-hour
       tests  completed  at Stauffer Chemical Company is included as  Table 1.
       To facilitate a  comparison of the results all concentrations are
       presented as ppmv dry (except % dry for C02 and 0^),  and all emission
       rates  are standardized as grams per hour (gm/hr).  Sample calcula-
       tions  and conversion factors are presented in Appendix A.

  2.2  Sulfur compound  concentrations were determined by gas chromato-
       graphy (COS, S02, H2S and CS2), DuPont Analyzer  (total  sulfur and
       S02),  Meloy Analyzer (Total Sulfur), EPA Method 6 (S02), and EPA
       Method 11 (H2S).

2.2.1   Average sulfur dioxide  concentrations, as obtained by the various
       methods, ranged  from 48 ppmv to 400 ppmv.  General agreement was
       obtained between the gas chromatography values and those determined
       by EPA Method 6  (78 ppmv versus 48 ppmv).  The S0? concentration
       obtained by the  DuPont Analyzer is much higher (400 ppmv) and can
       be attributed to the fact that (1) the system tested contains
       elemental sulfur; and (2) the analysis method (UV) does not discrim-
       inate  between sulfur dioxide and elemental sulfur.

2.2.2  The average results obtained for total sulfur (as S02) ranged from
       2230 ppmv to 2330 ppm.  When the results are compared for each
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                Table  1
DATA SMttW - OUTLET FROM IFP-1500.SULFUX RKOVERT UNIT
             STAUFFER CHEMICAL COKPAMT
              Delaware City, feliware
                                                  Emission Concentrations. PCCT. ary

Gate
10 June 1974
11 June 1974
12 June 1974
.12 June 1974


Location
IF? Outlet
IF? Outlet
IFP Outlet
Incinerator
Outle(
Flow
RIU ain1
421
431
414
•»

AVEKACE (IFF CUTLET) 422
urstt Data
'/Ma 1 toUture
30.9
37.7
39.0
31.6

35.9
X COj
1.3
1.1
1.1
...

1.2
t 02 1 CO
0.28 ~
0.35 —
0.31 —
... ...

0.31
MASS EMISSION RATES.
Date
10 Junt 1974
11 June 1974
12 June 1974
AVERAGE
1. KDIK
2. Paramagnetic
3. EPA KotJiaS 6
C0(l) SO.
9.37 x 104 3.90
7.25 x 104 2.84
8.93 X I04 2.73
8.52 x 104 3.16
-
~

4. Owcr.t Analyzer (Induces*
((3)
.x"!03' 2.
x 103 2.
x 103 2.
x 103 2.
' 6. Uas
6. Gas

S02(4) S02(5)
78 x. 104 5.42 x I03
91 x I04 4.87 x I0a
34 x 104 i.W x 103
68 x 104 5.16 x 103
'CnromtograpMc
cos(S)
B.17 x
4.83 x
a. 09 x
7.04 x
H2S<5)
I03 4.15xlU4
103 5.04 X 104
103 6.70 x 104
103 5.30 « 104
X C02(D
1.$
1.6
1.8
...

1.6
gn/hr
CS2<5)
3.60 x 104
1 .44 x I04
2.31 x 104
NS1R/PARWAGSETIC
X 02(2) CO
0.1
.—
0.1
...

0.1

TS16)
'1.49 X 105 1
1.30 x 105 1
1.11 x 105 1
2.45 x 10* 1.30x 105 1
ppav (1J
3240
2450
7140
...

2940

TS(7)
.58 x 105
.75 x 10s
.35 x 105
.56 x 10s
S02(3J
59
42
42
..

43

TS(4)
•1.57 x 105
1.72 x 105
1.35 x 105.
1.S5 x 10S
, Gas CnrOM-.OCrjjn Ktiav £hPont
S02M) S02(5) COS15) H2S(5) CS2(5J TS(5) TS(7J TS{4j
420 82 132 • 1190 460 2310 2390 2333 .
430 72 . " 141° 1M 1920 2590 25«
3M jfl 133 »50 300 2760 2070
... .. "" "" ™ ~ — — — -

400 78 m liM 3" 2333 H» 2330
.
NOx(8J H2S(9)
3.71 x 102 «.W x 104
0.49 x 102 "'6 « lfl4
1 R7 , ,02 «•» « '°4
2.02 X 102 8-Z3 « 1°'
VislS't
' . W,(B) HjS(?) EaUi(c.is(l3)
7.8 1715 0
1.0 3500 0
4.0 2403 —
— 16i2 -

4.3 2MO 0






9. EPA Kathod 11
tnrcrjtograp.Mc 'Sulfur Dat*
Siararlzod ac JO?

10. Visible

tatutifiS

By EPA Kitted 9





. .



7. raloy Total Sulfur Analyzer

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       individual  test,  the  total sulfur values obtained by the Meloy
       Analyzer and  the  DuPont Analyzer are in good agreement.  Individual
       values  obtained by  the gas chromatograph are less by several hundred
       ppmv for two  of the three tests.  The difference between gas chroma-
       tography and  the  other two methods was expected due to the fact that
       the other methods also respond to elemental sulfur.  No explanation
       is offered for the  increase  in total sulfur as determined by gas
       chromatography on the third  test.

2.2.3  Hydrogen Sulfide, as  determined by the gas chromatograph, varied from
       1190 to 1950  ppmv,  with the  average value for the test computed at
       1520 ppmv.  Hydrogen  sulfide determined by EPA Method 11 varied from
       1715 to 3800  ppmv.  The 3800 ppmv value  appears  to be in  error since
       it is much greater  than either the total sulfur or  the hydrogen sulfide
       as obtained by other  methods.  Other hydrogen sulfide values
       obtained by EPA Method 11 are higher than the corresponding values
       obtained by gas chromatography but are in the same  general range.
       General interferences with Method 11 are positive in nature and
       would tend to explain the differences.

2.2.4  Carbonyl Sulfide  and  Carbon  Disulfide, as analyzed  by gas chromato-
       graphy, varied from 77 to 133 ppmv and 180 to 460 ppmv, respectively.
       No comparative methods were  available for these components.

2.2.5  Carbon  dioxide was  determined by NDIR and gas chromatography
       (thermal conductivity).  The results obtained varied  from 1.1  to

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        1.3 (G.C.)  and 1.5  to  1.8%  (NDIR).   Agreement between the two
        methods is  within experimental  error.

 2.2.6  Oxygen v/as  determined  by  paramagnetic  analyzer and gas chromatography.
        A comparison of the results  indicated  that the values obtained by
        G.C.  were slightly  higher than  those obtained by the paramagnetic
        analyzer (0.31% vs.  0:1%, Avg.).

 2.2.7  Nitrogen oxides were determined by EPA Method 7.  The results obtained
        varied from a low of 1.0 ppmv to a high of 7.8 ppm.  Comparative
        tests by alternate  methods were not made for nitrogen oxides.

 2.2.8  Carbon monoxide was determined  by NDIR and varied from 2450 to
        3240  ppmv.   Comparative results were not obtained for carbon
        monoxide by alternate  methods.

 2.2.9  Visible Emissions were determined by qualified observers in
        accordance  with EPA Method 9.   This  phase of the test program
        was discontinued by the EPA  project officer after the first
        two tests resulted  in  an  average visible emissions of zero.

2.2.10  Hydrocarbons were not  determined during the testing period
        due to a malfunction of the  analyzer.

 2.3    The overall results obtained from the  various tests (S02,
        H2S,  COS, SO,,, CO,  C02, 02»  etc.) seem to be in agreement with
        the results expected from the IFP Sulfur Removal Process.

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Agreement between comparative methods, where available, tends
to substantiate the fact that the results are in the  correct
range and typify an operation of this  type.
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                      3.0   PROCESS DESCRIPTION



3.1   Process  Description -  Sulfur Recovery at Stauffer Chemical
     Company's  Carbon  Disulfide  Plant

     Figure 1  is  a  process  schematic of carbon disulfide production and

     sulfur recovery similar  to  that found at the Stauffer Chemical Com-

     pany carbon  disulfide  production facility at Delaware City, Delaware.

     The Stauffer plant produces CS  from the reaction between natural

     gas and  sulfur known as  the catalytic hydrocarbon-sulfur process.

     The reaction is:

           cnH2n+2  +   (3n+l)S—*n CS2 +  (n+1) H2S

     where n  =  1,2,3	



     After the  product carbon  disulfide is absorbed from the process gas

     stream,  the  absorber vent gas, containing nearly 93 percent hydrogen

     sulfide,  is  directed to  a sulfur recovery facility—a three stage,

     395 LT/D Claus plant.  The  Claus plant operates at approximately

     95 percent sulfur removal efficiency.  Tail gas from the Claus

     plant goes to  an  IFP-1500 tail gas plant (Figure 2 ) which went

     onstream in  December 1973.  Carbonyl sulfide (COS) and CS  are not

     recovered  by the  IFP process but their presence is minimized back

     in the Claus by a reducing  catalyst of cobaltimolybdenum and alumina

     in the first catalytic stage.



     The IFP  process reaction  is a continuation of the gas phase Claus

     reaction  in  the liquid phase:



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HRT\.'TAU

                                                                                   IFF
                                                                                      OLir
                                                    HCWV
   Figure 1.   Process Schematic of Sulfur Recovery in C$2 Production.

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                            Steom condensote
                            '.or temn control
H S 
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                       Cat.
           2H2S + S02  	•>   3S +  2 H20

     Tail  gas which  exits  the Glaus unit  is  induced directly into the
     IFP reactor without cooling the  gas.  The reactor is essentially
     a packed column with  a  specially designed boot for collecting
     sulfur.   Mixed  alkali metal salts of an organic acid serve to
     catalyze the reaction which takes place in a high boiling polyglycol
     solvent  above the  melting point  of sulfur—generally in the range
     250-260°F.  I he metal salts form a complex with H2S and S02 in the
     feed  gas, which in turn  reacts with  more of the two sulfur com-
     pounds to form  elemental  sulfur  and  regenerate the catalyst com-
     plex.  The sulfur  coalesces and  settles into the boot of the
     reactor, from which it  is drawn  as a molten product.  In the reactor,
     the water of reaction is vaporized and carried out with the cleaned
     tail  gas.  To maintain  the heat  balance in the reactor, condensate
     is injected and vaporized together with the water of reaction.  The
     solvent  is generally  a  polyalkylene  glycol, although alcohols, glycols,
     glycol ethers,  or  glycol  polyethers  may also be used.

3.2  Plant Operation During  Emission  Measurements
     During the test period,  process  variables were monitored to assure
     that  emissions  measured  would be representative of normal process
     operation.  For the Stauffer  Chemical test the monitored variables
     included:
          (1) tail  gas  H S and SCL
          (2) S02 from  incinerator stack

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    (3) IFP inlet gas temperature
    (4) IFP inlet solvent temperature
    (5) IFP solvent flow rate
    (6) acid gas feed rate to Glaus

As shown in the process data sheets (Tables  2,  3  and 4), the pro-
cess was very steady during testing.  The entire  sulfur recovery
system (Claus + IFP) ran at normal rates.   For  the  three tests,
sulfur recovery was calculated at 336 long tons per day (LT/D),
versus normal  operation of 341 LT/D.  Plant  design  is 395 LT/D.

The emission results of the tests performed  should  be representative
of IFP tail gas technology.
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                    4.0  LOCATION OF SAMPLING POINTS

The sampling points selected  for emission tests at Stauffer Chemical
Company are shown in Figure  3.

Port B, downstream from the  IFP Sulfur Removal Unit, was used to obtain
samples for hydrogen sulfide  (EPA Method 11), sulfur dioxide (EPA
Method 6), nitrogen oxides  (EPA Method 7), oxygen (paramagnetic), carbon
monoxide (NDIR-EPA Method 10), and carbon dioxide (NDIR).  Velocity
traverses and moisture determinations were also made at this sampling
point.  The sampling port at  this point consisted of a gate valve with
a 1 1/4" opening.

The EPA sampling port consisted of a 2" gate valve located downstream
from the IFP Unit and the Port B sampling location.  Heated probes were
installed at this point to extract sample gases for analysis by the Dupont
Analyzer, the Meloy Analyzer  and the gas chromatographic system.

Port A, as shown in Figure 3, was a 3" opening in the post-incinerator
breeching.  Moisture and hydrogen sulfide were determined at this sampling
location.

The major problems presented  by the location of the sampling points were
the small size of Port B and  the accumulation of moisture and elemental
sulfur at the EPA sampling port.  The problem at the EPA location was
diminished by backflushing the sampling lines between samples to minimize
the accumulation of elemental sulfur and moisture.
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Gas From
I.P.P.
Absorber
              Port B
                O
                                                                                           Stack
                                       I    Incinerator By-pass
EPA
Port
                               O
                                               Incinerator
                                                                         Port A
Figure 3.  Location of Sampling Points

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                        5.0  ANALYTICAL PROCEDURES

A brief summary of each  procedure  is presented in this section.
5.1  Sampling Procedures
     Sample gases were  extracted  from the emission source for the deter-
     mination of sulfur-containing compounds using a 3/16" FEP Teflon
     tubing sample line,  heated and maintained at 121°C (250°F).  This sample
     line terminated in the  dilution manifold in the EPA mobile laboratory.
     Either direct or diluted  sample could be withdrawn from the system as
     dictated by the analytical range of the instruments.  The samples
     were simultaneously  analyzed for total sulfur, carbon disulfide,
     sulfur dioxide, hydrogen  sulfide and carbonyl sulfide.  FEP Teflon
     parts or Teflon coated  parts (including the sample pump heads) were
     used throughout the  system to take advantage of the minimum reactivity
     of the Teflon to low level concentrations of sulfur compounds.  Figure
     4 is a diagram 'of  the sample dilution system in the EPA mobile
     laboratory.

     Sample gases were  extracted  from the emission source for the deter-
     mination of carbon monoxide, carbon dioxide and oxygen using a
     three foot,  1/4" stainless steel sample probe with Swagelok connectors
     to polethylene tubing.  The  sample passed through a dry impinger,
     immersed in an ice bath,  before passing through the pump.  A diagram
     of the sampling system  and the sample dilution system is shown in
     Figure 5.
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     Probe
     JBT3C
   Filter
(glass wool)
   Heating Sample Line-
                           Stack Wall
                           Filter
Permeation
   Tube
Calibration
    Gas
                               Diaphragm
                                 Pump
                               (Heated)
                      TO INSTRUMENTS

                   10:1     102:1     103:1
                                                                Vent
                                                        7
                                                      1-G
                                   •Vent
	^Vent
                                                                                  Posi
   I	Disp
   |_f   Pump

Pi   "50
                                            3 -
                                             Val
                                                             —C-
          ive
          acement

          cc/min.)
          lay
          •e
                                                                                                   Diluent  Air
                                                                                             Vent
                                                    Vent
                       rilution Box Heated
                            To 100°C
                                                                                                                <—1350 cc/min
                                                                                                           o o  o
                                                                                                                   —Flowmeter
                                                                          25 PSI
                                                                                                            Clean
                                                                                                           Dry Air
                                      Figure  4.0.    Sample Dilution System in
                                                        EPA Mobile Laboratory

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                                   To Atnosphcre (—.O— —-•»	
 •1	Dilution System
  j


4,-^	
                                                                                                         GJS  P.CW
                                                                                     Jl
                                                                          Atnosphcrc ( —••—J
            Figure  5.0.  .   Schematic of  sampling system for  C0_,  CO, and  02..

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    5.2  Analytical  Procedures  for  Sulfur Compounds
         Sulfur compounds  were  measured by three instrumental methods and
         two wet chemical  methods in order to obtain a comparison of methods.
         The analytical  methods for the various sulfur compounds are described
         in the following  paragraphs.

  5.2.1  Sulfur compounds  by  Gas Chromatography
         Sulfur compounds, when introduced into a hydrogen-rich flame, produce
         strong luminescent emissions between 300 and 423 nm.  Through the
         use of a narrow band optical filter that permits transmission at
         394 nit:,  a flame photometric detector (FPD) can measure the chemilum-
         inescent emissions produced by the $2 species and can differentiate
         between sulfur  containing  and non-sulfur containing compounds.
         Through the use of a gas chromatograph (GC) equipped with the
         appropriate analytical  columns, it is possible to separate and
         quantify the various sulfur compounds.

5.2.1.1  Applicability of  Method
         The compounds of  interest  in emissions from sulfur recovery systems
         are hydrogen sulfide (HoS), carbon disulfide (CS2)» sulfur dioxide
         (S02)  and carbonyl sulfide (COS).

         The two GC/FPD  systems available in the EPA mobile laboratory are
         capable of the  separation  and quantification of all of the compounds
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         of interest with  the  exception that COS and F^S could not be determined
       .  simultaneously on any one system due to the relatively small dif-
         ference in  the retention times and the relatively large differences
         in concentration  which results in the overlap of peaks.  The
         difficulty  presented  by the I^S - COS separation and determination
         was overcome through  the use of a scrubbing system which effectively
         removes one component (I^S) from the sample.  Silver wool, which
         reacts  readily with H?S, was installed in one of the GC systems
      .   between the sample loop and the analytical column.  Removal of the
         H£S makes  possible the determination of COS while the other system
         determines  HLS +  COS.   The difference in response observed between the
         two systems is used to calculate the I^S concentration.

5.2.1.2  Instrumentation and Standards
              GC/FPD System -  The system provided in EPA mobile laboratory
         was assembled from components available from various commercial-
         sources.
              Sulfur Compound  Permeation Tubes - Provided by EPA and gravi-
         metrically  calibrated by EPA personnel.

5.2.1.3  Analysis of Samples
         The sample   gas was extracted from the test source and diluted with
         clean,  dry, sulfur-free air in the dilution system.  Diluted sample
         was continuously  flowed through the sample loop and injected at
         fifteen minute intervals throughout the test.  The fifteen minute
         interval was selected due to the retention time of CS£-

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         Responses obtained from each  compound were  compared to the standard
         curve for that component and  the  concentrations were determined.
         In the series of tests  conducted,  two GC/FPD systems were utilized.
         GC#1  was equipped with  a scrubbing system and was used for a direct
         determination of COS concentration.  GC#2 was used to determine
         S02>  C$2, and h^S.   f^S was determined  on GS#2 by subtracting the
         COS concentration found with  GC#1  from  the  HoS + COS concentration.
         The analytical methods  used for the analysis of sulfur compounds in this
         series of tests were the same as. described  in an EPA preliminary
         draft method entitled "Semicontinuous Determination of Malodorus
         Reduced Sulfur Emissions From Stationary Sources".

  5.2.2   Total Sulfur by the Meloy Analyzer
         The detection system of this  instrument is  the same as for the gas
         chromatograph.  The major difference between the two systems is
         that  no analytical  column is  present to effect a separation of the
         various sulfur compounds.  Another difference between the systems
         is that sulfur compounds in the sample  gas  are oxidized to sulfur
         dioxide by passage through a  tube  furnace maintained at 1500°C in
         the presence of excess  oxygen before entering the Meloy Analyzer.
         The principal of the method and the  applicability, however, are the
         same  for the two systems.


5.2.2.1   Instrumentation and Standards
              Detector System -  Meloy  Sulfur  Analyzer, Model  160SA
              Oxidation System - Lindberg  Hevi - Duty Tube Furnace, Model 55035.

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              Calibration Standards  -  Permeation tubes provided by and
              gravimetrically calibrated by  EPA personnel.

5.2.2.2  Analysis of Samples
         The sample was  obtained  from  the  test source and diluted with clean,
         dry, sulfur-free air in  the dilution system.  Diluted sample was
         flowed through  the tube  furnace and into the Meloy Analyzer.  A
         continuous readout of total sulfur  concentration was displayed
         on a strip chart recorder.  Comparison of the recorder response with
         the analytical  curve obtained by  plotting response versus concen-
         tration gave the total sulfur (as $02) concentration presence in
         the sample stream at any given point in time.

  5.2.3  Total  Sulfur and Sulfur  Dioxide by  the DuPont Analyzer
         The detection system for this method is based on the absorption of
         ultraviolet radiation by sulfur species, in particular by sulfur
         dioxide.  A sample is pumped  into a cell where the sulfur dioxide
         is determined by a change in  the  intensity of ultraviolet radiation
         reaching the photocell.   The  cell is subsequently filled with oxygen
         and all the reduced  and  elemental sulfur species are converted to
         sulfur dioxide.   After the  oxidation step, the concentration is
         again  determined by  the  change in the intensity of the ultraviolet
         radiation reaching the photocell.

5.2.3.1  Instrumentation  and  Standards
              Detector System - DuPont Sulfur Analyzer
              Calibration Standards  -  Provided by DuPont Personnel
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5.2.3.2  Analysis  of Samples
         The sample was  obtained  from the test source as described above.
         DuPont personnel  calibrated and monitored the instrument throughout
         the test  period.   The  data were presented on a strip chart recorder
         and the responses of the individual samples'(this method is semi-
         continuous) were  compared to the standard calibration curve in order
         to obtain concentrations.

  5.2.4  Titrimetric Method for the Determination of Sulfur Dioxide
         Sulfur dioxide  was oxidized to sulfate in the presence of hydrogen
         peroxide  according to  EPA Method 6 as outlined in the Federal  Register,
         36, No. 59, Part  II, August 17, 1971.  The sulfate which was formed
         and collected was subsequently titrated with a standardized solution
         of barium perchlorate  in  the presence of thorin indicator, and the
         sulfur dioxide  concentration was calculated.

  5.2.5  Titrimetric Method for the Determination of Hydrogen Sulfide
         Hydrogen  Sulfide  was  determined by EPA Method 11 as outlined in the
         Federal Register, 39,  No. 47, Part II, March 8, 1974.  The sample
         gas was extracted from the source and reacted with a basic solution
         containing cadmium ions.  The cadmium sulfide formed was reacted  with
         an excess of standard  iodine solution and titrated with a standard
         solution  of sodium thiosulfate.  From the amount of iodine
         which reacted with the cadmium sulfide, the concentration of sulfide
         in the original sample was calculated.

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  5.3  Analytical  Procedures  for  Carbon Monoxide, Carbon Dioxide and Oxygen
       Carbon monoxide,  carbon  dioxide and oxygen were monitored continuously
       from the source during the three four-hour tests.  The sample was
       obtained as described  in section 5.1.

5.3.1  Instrumentation and  Standards
       Carbon Dioxide  -  Beckman Model 315A NDIR configured for 0-5% carbon
       dioxide.
       Carbon Monoxide - Beckman  Model 315B NDIR configured for 0-1000 ppm
       carbon monoxide.
       Oxygen - Beckman  Model  F-3,  paramagnetic oxygen analyzer capable of
       measuring 0-25% oxygen.
       Standard Gases  -  Obtained  from Matheson Gas Products, Inc., Cucamonga,
       California.  All  standards were either primary or certified and were
       analyzed by Matheson Gas Products, Inc.  All standards consisted of
       the component of interest  with the balance of the mixture as nitrogen.

5.3.2  Analysis of Samples
       The sample gas  was extracted from the test source and flowed through
       the instruments.   In the case of the carbon monoxide the sample was
       diluted with clean,  dry, carbon-monoxide free nitrogen in order to
       maintain the concentration within the operating range of the instrument.
       A schematic of  the instrument flow system is presented as Figure 5.

       Responses obtained from  the instrument were displayed on a strip chart
       recorder and these responses were compared to the appropriate standard
       curve to obtain the  concentrations of the different constitutents.
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     EPA Method 10 as  outlined  in  the  Federal Register 39, No. 47 on
     Friday,  March 8,  1974  was  used  as a guideline in the determination
     of carbon monoxide concentrations.

5.4  Analytical Procedure for Nitrogen Oxides
     Nitrogen oxides were measured according to EPA Method 7 which appeared
     in Federal Register, 39, No.  47,  8 March 1974.  A portion of the con-
     tents of the integrated  bag sample was collected in an evacuated
     flask which contained  sulfuric  acid and hydrogen peroxide.  After the
     oxides of nitrogen had been oxidized  to nitrate, the nitrate was reacted
     with phenoldisulfonic  acid and  a  spectrophotometric method was used to
     determine concentration.

5.5  Procedure for the Determination of Moisture
     The moisture content was measured at  a location downstream from the
     IFP Unit in accordance with EPA Method 4 which appeared in Federal
     Register, _36., No.  59,  Part II,  August 17, 1974.

5.6  Procedure for the Determination of Stack Gas Velocity
     The stack gas velocity was determined at a location downstream from the
     IFP Unit after sample  and  velocity traverse points were located.  EPA
     Method 1 and 2 as they appeared in Federal Register, 36, No. 59, Part II,
     August 17, 1974 were used  as  guidelines for these determinations.

5.7  Procedure for the Determination of Visible Emissions
     EPA Method 9, as  outlined  in  the  Federal Register, _36, No. 247, Part II,

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     December  23, 1971 was used as  the guideline in the determination of
     visible emissions.  A certified observer was used to observe  emissions
     from the  sample source.

5.8  Carbon Dioxide and Oxygen by Orsat
     A Carle gas chromatograph with a thermal conductivity detector was
     substituted for the Orsat Method in  the determination of carbon dioxide
     and oxygen.  This substitution was approved by the EPA Project Officer.
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