Air Pollution Emission Test: Project Report No. 74-SRY-4, Stauffer Chemical Company (Delaware City, Delaware)


                       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
..

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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