4-KPM-18
(REPORT NUMBER]
AIR POLLUTION EMISSION TEST
ST. REGIS PAPER COMPANY
(PLANT NAME;
Tacoma, Washington
(PLANT ADDRESS)
U. S. ENVIRONMENTAL PROTECTION AGENCY
Office of Air and Water Programs
Office of Air Quality Planning and Standards
Emission Standards and Engineering Division
Emission Measurement Branch
Research Triangle Park, N. C. 27711
-------
Emission Test Report
Emission Measurement Branch
Number 74 - KPM - 1A
Malodorous Reduced Sulfur
Emissions From
Various Kraft Mill
Unit Processes
ST. Regis Paper Co.
Tacoma, Washington
.James Eddjnqer '
Gary McAlister
Environmental Protection Agency
Office of Air Programs
Research Triangle Park, North Carolina
27711
-------
I. iINTRODUCTION
An emission source test was conducted at the St. Regis Pager Com-
pany k raft mill in Tacoma, Washington, during the period 4/3/74 to
4/10/74. This report represents the results of that test.
Under the Clean Air Act, as amended, the Environmental Protection
Agency is charged with the establishment of performance standards for
new or modified existing installations in source categories which may
contribute significantly to air pollution. Certain kraft mill operations,
including lime kilns, have been categorized with respect to odorous re-
duced sulfur emissions. The purpose of this test was to gather emission
data which would demonstrate the emission limitations obtainable.
The operation tested was a natural "gas-fired lime kiln used to con-
vert calcium carbonate to calcium oxide. Only the lime kiln outlet was
tested for total reduced sulfur content (TRS). The TRS emissions were
measured by EPA personnel using gas chromatographic separation with flame
photometric detection. In conjunction with the TRS tests, measurements of
velocity temperature, moisture, and 02, C02, and CO content were conducted
by Environmental Science and Engineering, Inc.
Subsequent sections o>f this report treat the following:
1. Summary and discussion of results.
2. Process description and operation.
.3. Sample point location.
4.. Sampling and analytical procedures.
-------
2
II. SUMMARY AND DISCUSSION OF RESULTS
The following tables summarize the gaseous sulfur determina-
tions made on each of the si* days" of testing. .
A detailed discussion of
operating parameters is included in section III.
Table 1 presents a summary of the average TRS and SCL emission
levels during each day of testing. Table II summarizes the
average concentrations of the component gaseous sulfur compounds
measured. A summary of supplementary flow rate, moisture, tempera-
ture, and orsat determinations is presented in Table III. Complete
results are tabulated in Appendix A.
Table I
Daily Average TRS Daily Average S0?
Date Location Run # PPM,Dry Lbs/hr PPM/Dry Lbs/hr
4/3/74
4/4/74
4/5/74
4/5/74
4/8/74
4/9/74
4/9/74
4/10/74
4/10/74
Lime
Lime
Lime
Lime
Lime
Lime
Lime
Lime
Lime
kiln
kiln
kiln
kiln
kiln
kiln
kiln
kiln
kiln
#2
#2
#2
#2
#1
#2
#2
#2
#2
1
2
3
4
5
6
7
8
9
. 78
48
4.
12
6
140
4.
4.
4.
5.
5
8
0
2
. 6.
:.3.
0.
0.
12
0.
0.
0.
0.
3
9
34
88
33
34
29
39
32
33
52
42
3.4
25
18
'16
37
4.
5.
7.
5.
0.
3.
2.
2.
5.
9
1
2
8
54
5
4
2
2
-------
Date Location
4/3/74 Lime kiln #2
4/4/74 Lime kiln #2
4/5/74 Lime kiln #2
4/5/74 Lime kiln #2
4/8/74 Lime kiln #1
4/9/74 Lime kiln #2
4/9/74 Lime kiln #2
4/10/74 Lime kiln #2
4/10/74 Lime kiln #2
Date Location Run
4/3/74 Lime kiln #2
4/4/74 Lime kiln #2
4/5/74 Lime kiln #2
4/8/74 Lime kiln #1
4/9/74 Lime kiln #2
4/9/74 Lime kiln #2
4/10/74 Lime kiln #2
4/10/74 Lime kiln #2
Run
1
2
3
4
5
6
7
8
9
#
1
2
3,4
5
6
7
8
9
# CMPD
H2S
H2S
H2S
H2S
H2S
HฃS
H2S
H2S
H2S
Flow Rate
(SCFM.Dry)
15,410
15,480
13,840
15,827
14,000
13,400
13,625
14,180
3
Table II
Ave. Ave. Average
(PPM", Wet) (PPM", Dry) (Ibs/hr)
54
32
3.6
9.7
85
3.5
3.7
3.0
3.8
Table III
Moisture
% by Volume
31.1%
32.9
21.8
37.9
22.9
26.0
25.8
26.8
78
48
4.6
12
140
4.5
4.8
4.0
5.2
Stack
Temperature (ฐi
159ฐ
164
142
170ฐ
146
152
155
154
6.3
3.9
0.34
0.88
12
0.33
0.34
0.29
0.39
co2 o2 .
%c/
fO
13.1 7.46
12.1 8.8
13.0 7.6
12.0 8.5
14.2 7.1
14.2 7.1
14.6 6.4
14.2 7.2
CO
0
0
0
0
0
0
0
0
-------
III. 'PROCESS DESCRIPTION AMD OPERATION
The St. Regis Paper Company mill at Tacoma, Washington produces
1000 tons of kraft pulp per day. About 15 percent of the pulp is
bleached and made into paper while the remaining pulp is made into
a variety of brown paper and paperboard products. The mill has been
operating since 1928.
Process Description
A. General
The process for making kraft pulp from wood is shown in Figure 1.
In the process, wood is chipped into small pieces and then cooked in
digesters (five batch and two continuous) at elevated pressure and
temperature. The cooking chemicals, called white liquor, are sodium
hydroxide and sodium sulfide in water solution. The white liquor
chemically dissolves lignin, leaving wood cellulose (pulp) which is
filtered from the spent liquor and washe'd. The pulp is made into
paper.
The balance of the pulping processes designed to recover the
cooking chemicals. Spent cooking liquor and the pulp water are com-
bined for treatment to recover chemicals. The combined stream, called
weak black liquor, is concentrated in steam heated multiple-effect
evaporators, including a special device called a concentrator. The
strong black liquor leaving the evaporators is burned in a recovery
furnace.
-------
TT
x VI 0 0 D ซ-ป*' ซ-ซซ*>-
x .WHITE LIQUOR '
(NaOH + Na2S)r
*
<$. m m m *
STACK
>-
*
I (N
_>
ij . .
* .
WATER *
G
1
DIGESTER
SYSTEM
ป
RECOVERY
FURNACE
SYSTEM
1
SMELT
a2C03 + Na2
1
SMELT
DISSOLVING
TANK
- PULP ~~~> PULP *~ PULP
. ^ WASHERS ,_WATฃR
*-HEAK BLACK LIQUOR*
4
HEAvV MULTIPLE
u ",?;,., EFFECT u
LIOUOR EVAPORATOR
LIQUOR SYSTEM
AIR
s)
ป*
1 *
REEN LIQUOR .XV<
I ^t>
1 WHITE LIQUOR r , IICT T r . 7 . .,
L/ocrvr-r -n .- CrtUSTICIZIrl
^(RECNCuE .0 TAfI/
DIGESTER) 1H"1X
^^
* - -r , IMr- A V ^^
CALCIUM
MUD
Figure 1 Tiie Kraft pulping procor.s at the St. Rcqi:
in TacoT.a , '>;:. ."h inn ton .
-------
6
Combustion of the organic matter in the black liquor pro-
vides heat needed to generate process steam. Inorganic chemicals
from the black liquor are recovered as a molten smelt at the bot-
tom of the furnace. The smelt, consisting of sodium carbonate and
sodium sulfide, is dissolved in water and transferred to a causti-
cizing tank. Lime added to this tank converts sodium carbonate to
sodium hydroxide, completing the regeneration of white liquor,
which is then recycled to the digesters. The calcium carbonate mud
that precipitates from the causticizing tank is recycled to the kilns
to regenerate lime.
B. Lime Kiln No. 2
The Number 2 lime kiln was installed in 1972 and was designed by
Traylor Company to produce 80 tons of lime per day. This is equiva-
lent to a pulp production rate of about 320 tons per day. This ro-
tary kiln is 170 feet long, with an inside diameter of 8.5 feet. It
is fired with either natural gas or No. 6 oil.
The feed to the kiln is the calcium carbonate slurry that pre-
cipitates from the causticizing tanks. The slurry is washed and then
dried on a rotary vacuum drum, as shown in Figure 2. The dried cake
is removed from the drum on a knife edge and conveyed to the kiln. In
the kiln, the calcium carbonate mud is roasted and carbon dioxide is
driven off, leaving calcium oxide (lime) as product.
Noncondensable gases from the digesters and multiple-effect eva-
porators are burned to destroy odors. These gases were burned in this
-------
LIMESTONE
MUD >
MUD
WASHER
AIR
GAS OR.-
NO. 6 OIL
. LIME
(PRODUCT)'
VACUUM
FILTER
SAMPLING PORTS
EXHAUST
* 1
GAS
FRESH
WATER'
VENTURI
STACK
\
Y
DEMISTER
RECYCLE-
^ BLEED
Figure 2 . Flow diagram of the No. 2 lime kiln at the St. Regis mill
in Tacoma, Washington.
-------
8
kiln during the testing. Dregs from the green liquor clarifier
are not burned in this kiln. ^
An adjustable throat venturi scrubber is used to control the
particulate emissions from the kiln. The scrubber was manufactured
by Air Pollution Industries, Inc., and installed in 1972. Fresh
water is used as makeup to the scrubber system.
C. Lime Kiln No. 1
The Number 1 lime kiln was installed in 1961. It was designed
by Allis-Chalmers Company to produce 196 tons of lime per day. This
is equivalent to a pulp production rate of about 784 tons per day.
This rotary kiln is 265 feet long, with an inside diameter of 10.5
feet. It is fired with either natural gas or No. 6 oil.
The feed to the kiln is the calcium carbonate slurry that pre-
cipitates from the causticizing tanks. The slurry is washed and then
dried in centrifuges, as shown in Figure3 . In the kiln, the calcium
carbonate mud is roasted and carbon dioxide is driven off leaving cal-
cium oxide (lime) as the product.
Noncondensable gases can be burned in this kiln. However, these
gases were not burned in this kiln during the testing. Dregs from
the green liquor clarifier are not burned in this kiln.
A venturi scrubber is used to control particulate emissions from
this kiln. The scrubber was manufactured by Peabody and was installed
in 1965. Fresh water is used as makeup to the scrubber system.
-------
LIMESTONE
NUD *
MUD
HASHER
AIR
GAS OR, -
NO. 6 OIL
LIME
(PRODUCT)'
CENTRIFUGAL
FILTER
SAMPLING PORTS
EXHAUST
l
GAS
FRESH
WATER'
VENTURI
STACK
\
DEMISTER
RECYCLE-
Figure 3 . Flow diagram of the No. 1 lime kiln at the St. Regis mill
in Tacoma, Washington.
-------
'
Process Operation j
i
A. General i
}
The purpose of the test program was to measure emission levels
' ' i
during normal mill operation. Process conditions were carefully j
observed, and testing was done only when the test facility appeared j
i
to be operating normally. During the tests, important operating
conditions were monitored and recorded on process data sheets. These
records and a key to the entries are in Appendix B. The process data
are summarized below.
B. Lime Kilns
A total of eight TRS tests were conducted on the No. 2 lime kiln.
4,
Only one complete TRS test was conducted on lime kiln No. 1. The TRS
emissions from both lime kilns are controlled by regulating the kilns'
operating parameters (oxygen and cold-end temperature). Mud samples
from both kilns were analyzed by Michael Franklin of the National
Council of the Paper Industry for Air and Stream Improvement (NCASI).
Data on the sulfide content of the lime mud are presented in Appendix
B.
Four TRS tests were first conducted on lime kiln No. 2 between
April 3 and 5, 1974. According to the operators, the first two tests
were performed while the kiln was in an overload condition. This con-
dition existed because the No. 1 lime kiln v/as taken off-line in order
to make some necessary repairs. The average mud flow rate to the
-------
11
filter during tests #1 and #2 were 75 and 63.5 gallons per minute,
respectively. The normal flow rate is about 50 to 55 gallons per
minute. The average oxygen level in the exhaust during these two
tests (as indicated by the control room oxygenmeter) was 4.1 and 5.0
percent, respectively. These oxygen levels are lower than normal (6
to 7 percent). The sulfide content of the lime mud was also higher
than normal(0.6% Na?S vs. 0.4%). Therefore, the first two tests
(31 and #2) are not considered valid tests since they were performed
during abnormal conditions. According to the operators, the No. 2
lime kiln was operating normally during tests#3 and #4.
After these four tests on lime kiln No. 2, testing was started
on lime kiln No. 1. Only one complete TRS test was conducted. This
test was performed on April 8, 1974. As far as is known from the
process information and conversations with the operators, lime kiln
No. 1 was operating normally during the testing. The TRS emissions
were about 140 ppm by volume (dry basis) during the test.
On April 9, 1974, another TRS test was started on lime kiln No. 1.
According to the operators all operating parameters were again normal.
The gas chromatography instrument indicated that the TRS emissions were
about 40 to 50 ppm by volume (dry basis). Since the TRS levels from
the No. 1 lime kiln were higher than expected (based on the mill's
data), the data would be of lesser value than the data obtained from
lime kiln No. 2 in the development of new source performance standards.
It was, therefore, decided to halt testing on lime kiln Mo. 1 and
resume testing on lime kiln No. 2 to verify the low TRS emissions re-
corded during tests #3 and #4 and to obtain sufficient data to indicate
-------
12
that these low levels are actually obtainable during normal lime
kiln operation.
Four more tests (#5 to #8) were performed on lime kiln No. 2.
As far as is known from the process information and conversations with
the operators, lime kiln No. 2 was operating normally during these
tests.
The differences in TRS emissions from the two lime kilns are
probably due to the differences in their operating parameters which
affect TRS emissions. The cold-end temperature, oxygen content in
the exhaust, and the sulfide content of the lime mud for lime kiln
No. 2 were about 700ฐF, 6 to 7 percent, and 0.4 percent, respectively,
compared to 450ฐF, 3 to 5 percent, and 0.9 percent for lime kiln No. 1.
This would indicate that the TRS emissions would be lower from lime
kiln No. 2.
IV. LOCATION OF SAMPLING POINTS
Figures 1 and 2 depict the location of the sampling points for
lime kiln No. 2 and No. 1, respectively. The two ports used for the
gaseous sampling and velocity profiles were approximately 20 feet
above the inlet breeching at lime kiln No. 2 and 40 feet above at
lime kiln No. 1. The gaseous sampling probe was inserted into one
of the sample ports and extended approximately two feet into the
stack.
V. SAMPLING AND ANALYTICAL PROCEDURES
The sampling and analytical procedure used for the determination
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13
of TRS emissions was ostensibly the same as described in Appendix
n
D, proposed Method 14 - "Semicontinuous Determination of Malodorous
Reduced Sulfur Emissions from Stationary Sources." Deviations from
and modifications of this draft reference method are listed below.
1. After the first test on 4/3 the electrometer in the GC/FPD-II
system malfunctioned. Since there were no measureable amounts of
high molecular weight sulfur compounds on the first day of testing,
it was decided to continue testing using only the GC/FDD-I system.
2. On the final day of testing, it was discovered that the HpS
permeation tubes used to standardize the instrumentation were expiring.
Since no other standards were available the GC/FPD systems had to be
standardized with S02 permeation tubes. After the equipment was re-
turned to Durham, a new FLS permeation tube was received and the
GC/FPD system was standardized to allow the calculation of an
HpS - SOp response ratio. All H^S data were calculated from SC^
standard curves on the basis of this ratio. The standard curve used
to calculate the ratio is shown in Figure 3.
Velocity moisture, and molecular weight were performed as
specified in reference Methods 1, 2, 3, and 4 described in the Federal
Register, Vol. 36, Nb. 247, December 23, 1971. with one slight modifi-
cation. The silica gel drying was removed because of repeated plugging
problems. Calculations were based on the assumption that the gases
entering the dry test meter v/ere saturated.
-------
//V/,% "I u- 1
VX'O ^.-1=lx o ^ -. n ซ
o.oto
F t ซ
-------
APPENDIX A
Results and Sample Calculations
-------
APPENDIX A-I
Run #
Date
Location
P , Barometric pressure at dry
gas meter, inches, Hg.
V , Volume of dry gas as
sampled at meter conditions,
T , Average gas meter temperature
m op
V Volume of water vapor
' collected, ml
% C02, Volume % dry
% 0~, Volume % dry
% CO, Volume % dry
% N2, Volume % dry
C , Pi tot tube coefficient
P dimensionless
T , Average stack temperature, ฐF
P , Stack gas pressure, inches
Hg absolute
2
A , Stack area, FT
' /~P~ Average square root of
1
4/3/74
Lime
Kiln
#2
30 in.
DCF
7.375
63ฐ
67 ml
13.1
7.46
0
79.4
0.83
158ฐ
30
12.3
. -
L.I 1 A */ซ/ J. WM
2
4/4/74
Lime
Kiln
#2
30
4.933
53
50.6
12.1
8.8
0
79.1
0.83
164
30
12.3
LSI \ t 11 f 1I1LS I\L-*,
3 and 4
4/5/74
Lime
Kiln
#2
t
30
4.825
57
27
13.0
7.6
0
79.4
0.83
142
30
12.3
J\JL i *j
5
4/8/74
Lime
Kiln
#1
30
5.370
63
55.8
12.0
8.5
0
79.5
0.83
170
30
15.6
6
4/9/74
Lime
Kiln
#2
30
5.201
62
30.5
14.2
7.1
0
78.7
0.83
146
30
12.3
7
4/9/74
Lime
Kiln
#2
30
5.143
69
30.2
14.2
7.1
0
78.7
0.83
152
30
12.3
8
4/10/74
. Lime
Kiln
#2
30
5.334
67
31
14.6
6.4
0
79.0
0.83
155
30
12.3
9
4/10/74
Lime
Kiln
#2
30
5.159
73
31
14.2
7.2
0
78.6
0.83
154
^
30
12.3
velocity head of stack
gas, inches HO
.558
.581
.431
.502
.449
.451
.459
.484
en
-------
GASEOUS SULFUR RESULTS
Date
4/3/74
Location
Lime
Kiln II
Inject
Time
1113
1128
1143
1158
1213
1228
1243
1328
1343
Corrected
Compound
so
so
so
so
H2S
so
so
so
so
S0
Attenuation
4 X 10"6
32 X 10"6
16 X 10"6
4 X 10"6
f>4 X 10"6
16 X 10"6
64 X 10"6
32 X 10"6
64 X 10"6
.16 X 10"6
64 X 10"6
16 X 10"6
16 X 10"6
4 X 10"7
<,4'X:ldr6
4 X 10"8
4 X 10"7
4 X 10"8
Peak
Height
93.0
55.0
71.9
63.1
52.1
48.5
57.0
88.0
52. '9
38.8
53.2
45.3
34.3
23.8
28.9
4.9
94.2
2.7
Concentration Dilution .
(PPM. Wet) Ratio
1.2 11:3:1
4.9 11.3:1
2.5
1.5
4.8
2.9
4.8
6.5
4.9
2.6
4.9
2.8
1.6 104:1
.20
.15
.018
.31
.013
Concent
(PPM.1
14
55
28
17
54
33
54
73
55
29
55
32
170
21
15
1.9
32
1.4
-------
GASEOUS SULFUR RESULTS
(Continued)
Location
Lime Inject
.Date .Kiln II Time
4/3/74 1358
1413
1428
1443
1458
1513
Compound
H2S
so2
H2S
so2
.H2S
so2
H2S
so2
H2S
so2
H2S
S00
Attenuation
4 X 10"7
4 X 10"8
4 X 10"7
4 X 10"8
4 X 10"7
4 X 10~8
4 X 10"6
4 X 10"7
4 X 10"6
4 X 10"8
4 X 10"6
4 X 10"8
Peak
Height
92.0
2.8
97.7
12.1
67.1
27.6
51.5
95.1
60.6
15.5
25.7
16.2
Concentration
(PPM. Wet)
.30
.013
.32
.032
.23
.053
.86
.46
.96
.035
0.57
.036
Corrects
Dilution Concentra'
Ratio (PPM.Wci
31
1.4
33
3.3
26
5.5
90
48
104:1 100
3.6
59
3.7
-------
Location
Lime Inject
Peak Concentration
Date Kiln II Time Compound
4/4/74 1115 H2
SO
1130 H2
SO
1145 ^ H2
SO
1200 H2
SO
1215 H2
SO
1230 H2
SO
1245 H2
SO
.
1300 H2
SO
1315 H2
SO
S
2
S
2
S
2
S
2
S
2
S
2
S
o
f.
S
2
S
o
Attenuation
4
4
4
4
4
4
4
4
16
'4
16
4
32
4
32
16
4
4
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
10~6(amps)
io-7
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
-7
-7
-6
-8
-8
-7
-6
-6
-6
-6
-6
-6
-6
-6
-7
-6
Height
31
8
33
. 16
21
52
off
67
73
67
73
49
52
60
48
54
9
.2
.4
.5
.8
.6
.0
scale
.7
.0
.7
.0
.0
.5
.4
.8
.9
.8
-(PPM. Wet)
.74
.51
.20
.20
.58
0.10
-
.52
2.6
1.8
2.6
1.8
3.2
2.0 .
3.7
3.2
.26
.22
Correct
Dilution Concentre
Ratio (PPM.V
12.8:1 9.
6.
2.
2.
7.
1.
6.
33
23
33
23
41
25
^ 48
41
118:1 31
25
<1
5
S
5
4
3
7
00
-------
Date
4/4/74
Location
Lime
-Kiln II
Inject
Time
1330
1345
1400
1415
1430
Compound
so2
V
S00
so2
H2S
so2
H2S
S00
Attenuation
4 X 1G~7
4 X 10"8
16 X 10"6
16 X 10"6
64 X 10"6
4 X 10"6
4'X 10"7
4 X 10"6
4 X 10"7
Peak Concentration
Height (PPM.Wet)
22.9
85.9
97.2
43.3
Saturated
45.2
79.8
10.8
22.2
.16
.13
3.2
3.0
.91
.49
.39
.23
Corrected
Dilution Concentration
Ratio (PPM.Wet)
19
16
12.8:1 41
' 38
118:1 110
58 ซ
46
27
]
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1
Location
Lime Inject
Date Kiln II Time
4/5/74 . 1050
1105
1120
1135
1150
1205
'
1220
1235
1250
Peak Concentration Dilution
Compound
H2S
so2 .
II2S
so2
H2S
so2
H2S
so2
H2S
SO,
H2S
so2
H2S
so2
H?S
so2
H2S
S00
Attenuation
4 X 10"6
8 X 10"6
4 X 10"6
32 X 10"6
4 X 10"7
64 X 10"6
4 X 10"6
64 X 10"6
4 X 10"8
4 X 10"6
4 X 10"8
4 X 10"6
4 X 10"8
4 X 10"8
4 X 10"8
4 X 10"7
4 X 10"8
4-X 10"6
Height
16.2
76.6
10.0
70.9
77.5
Saturated
14.4
Saturated
22.8
48.3
17.0
28.0
19.2
46.3
9.2
19.7
13.8
9.8
(PPM. Wet) Ratio
.47 11.1:1
2.6
.35
5.8
.30
.42
.037 102:1
1.2
.031
97
.033
.084
.021
.20
.027
.52
Corrected
Concentration
(PPM. Wet)
5.2
29
' 3.9
65
3.3
4.7
v
c
3.8
120
3.2
99
3.4
8.6
2.1
20.4
2.8
5.3
r
-------
I
J
i
\ . -.-_... ...-..
1 .
3
j Location
; Lime Inject
j Date Kiln II Time Compound
I 4/5/74 1305 H?S
I ' ^
so2
I 1320 H2S
;
; : sฐ2
i ' 1^5 H S
\ 1 tJ'J'J tlntj
; . sฐ2
! 1350 H2S
so2
1405 H2S
so2
: , 1420 H2S
,
so2
1435 H2S
SOo
V2 ...
Run i? 2
1450 H2S
SO,
Attenuation
4 X 10"8
4 X 10"7
4 X 10"7
-fi
32 X 10 ฐ
4 X 10"6
16 X 10"6
missed
16 X 10"6
4 X 10"6
8 X 10"6
4 X 10"7
-fi
8 X 10 ฐ
4 X 10"7
10 X 10"6
4 X 10"7
16 X 10"6
"_ .' '
Peak
Height
10.2
13.6
72.0
56.4
40.3
62.0
52.5
7.9
56.6
84.3
80.0
89.5
77.9
99.0
62.6
.
Concentration Dilution
(PPM. Wet) iv'atio
.023
.16
.29 11.1:1
5.1
.80
3.6
3.2
.31
2.2
.32
2.7
.33
4.1
.35
3.6
Con-fir. te-J
C'jpC'int.r..!:. ion
2-3
16.2
3.2
56
8.9
40
ro
36
3.4
24
3.6
30
3.7
4.6
3.9
40
...J
-------
1
-^~.a
Location
Lime Inject
Date Kiln II Time Compound
4/5/74 1505 H2S
Sฐ2 .
1520 H2S
SO,
1535 H2S
SO,
1550 H2S
SO,
1605 H2S
SO,
1620 H2S
so2
1635 H2S
so2
1650 H2S
so2
1705 H2S
SO,
Peak Concent rot ion Dilution
Attenuation
Missed
32 X 10"6
1 4 X 10"6
32 X 10"6
32 X 10"6
64 X 10"6
64 X 10"6
64 X 10"6
4 X 10"8
4 X 10"7
4 X 10"6
8 X 10"6
4 X 10"7
4 X 10"6
4 X 10"7
4 X 10"6
,4 X 10"6
64 X 10"6
Height
68.9
11.2
73.0
76.4
Saturated
50.8
Saturated
28.8
32.8
13.0
67.2
84.8
99.5
93.1
82.1
11.4
13.9
(PPM. Wet) Ratio
5.7
.31
5.9
4.1
-
5.1
-
.042 102:1
.27
.61 11.1:1
2.4
.32
2.1
.34
2.8
.30
3.3
Corrected
Concentration
(PPK.'Jet)
. 63
3.4
65
46
_
57
_
4.3
28
4.6
27
3.6 **ป
23
3.8
31
4.2
37
PO
ro
-------
4/5/74
Location
Li ir-" Inject
Kiln 11 Time
1720
1735
1750
1805
1820
1835
1850
Compound
H2S
so2
H2$
so2
H2S
SO,
H2S
SO,
H2S
so2
H2S
so2
M2$
SO,
Attenuation
4 X 10"7
_c
8X10ฐ
_7
4 X 10 '
-fi
8 X 10 ฐ
_7
4 X 10 '
Missed
_7
4 X 10 '
-ft
4 X 10 ฐ
_7
4 X 10 '
_c
4 X 10 ฐ
_7
4 X 10 '
4 X 10"6
_c
4 X 10 b
_c
8 X 10 ฐ
'*<)'.
Height
88.9
75.0
98.6
71.4
95.3
.
88.2
82.1
78.1
69.6
30.7
31.0
13.2
78.8
"oซv * -.:' ion :>. :.j.' - -,:-.
(IVM ,v..'t ) Rat1 >
.33
2.6
.28
2.5
.34
.33
2.8
.30
1.7
.17
1.0
.42
2.7
.< <<
C-i''' ' "i- ?'. '.if
vn./jct;
3.7
2.9
3.1
28
3.8
3.7
W
31
3.3
19
1.9
11
4.7
30
1905
-------
-1
Location
Lime Inject
Date Kiln I Time
4/8/74 1203
1218
. 1233
1248
1303
1318
1333
1348
1403
Compound
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
HฃS
so2
H2S
so2
H2S
so2
(AMPS)
Attenuation
4 x 10"6
4 x 10"8
4 x 10~6
4 x 10'8
4 x 10"6
4 x 10"8
4 x 10"6
4 x 10"8
4 x 10"6
4 x 10~8
4 x 10"6
4 x 10"8
4 x 10~6
4 x 10"8
4 x 10"6
4 x 10"8
4 x 10"6
4 x 10"8
(% scale)
Peak
Height
90.4
3.9
85.5
3.2
58.9
3.1
57.2
2.2
54.9
2.0
50.5
1.8
51.4
1.7
55.0
2.0
59.5
. 2.0
Concentration Dilution
.(PPM. Wet) Ratio
1.1
.024 115:1
1.0
.021
.87
.021
.80
.017
.80
.016
74
.015
.74
.015
.80
.016
.87
.014
Corrected
Concentration
130
2.7
120
2.4
100
2.4
92
_y^
2.0
92
1.8
85
1.7
85
1.7
92
1.8
100
1.8
-------
Location
Lime Inject
Date Kiln I Time
4/8/74 1418
1433
1448
1503
1518
1533
1548
1603
1618
Compound
H,S
c
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
(AMPS)
Attenuation
4 x 10'6
4 x 10"8
4 x 10"6
4 x 10"8
4 x 10"6
4 x 10"8
4 x 10'6
4 x 10'8
4 x 10"6
4 x 10"8
4 x 10"6
4 x 10"8
4 x 10"6
4 x 10"8
4 x 10"7
4 x 10"8
4 x 10"7
4 x 10"8
(ซ scale)
Peak
Height
59.8
1.5
86.9
1.0
81.5
$1.0
48.0
1.8
30.0
2.3
20.3
4.0
10.4
3.4
35.0
3.7
26.8
1.5
Concentration Dilution
(PPM. Wet) Ratio
.87
.014
1.1
.011
1.0
.011
.74
.015
.58
.018
.47
.024
.32
.022
.18
.023
.15
.014
Corrected
Concentration
100
1.6
130
1.3
120
1.3
85 I
1.7
67
2.1
54
. .2.8
37 ^
2.5
21
2.7
17
1.6
-------
Location
Lime Inject
Date Kiln II Time
4/9/74 1210
.'
1225
1240
1255
1310
1325
1340
1355
1410
Compound
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
SO,
. H2S
so2
H2S
so2
H2S
so2
H2S
so2
(AMPS)
Attenuation
4 x 10"7
16 x 10"6
4 x 10"8
4 x 10"6
4 x 10"8
4 x 10"7
. 4 x 10"7
8 x 10"6
8 x 10"8
4 x 10"7
4 x 10"8
4 x 10"7
4 x 10"8
4 x 10"7
4 x 10"8
4 x 10"7
4 x 10"8
4 x 10"8
(% scale)
Peak
Height
89.9
52.8
66.2
72.8
29.0
93.8
47.4
89.3
9.9
26.0
13.8
17.8
26.0
6.0
59.4
59.0
12.4
27.5
(PPM.Wet)
Concentration
.28
2.6
.074
1.4
.048
.48
.22
2.3
.038
.29
.032
.19
.045
.11
.067
.37
.031
.70
Dilution Corrected
Ratio Concentration
11.0:1 3.1
29
.81
15
.53
5.3
2.4
25
.42
3.2
.35
.2-1
.50 ^
1.2
74
4.1
.34
7.7
r
-------
Location
Lime Inject
Date Kiln II Time Compound
4/9/74 1425 H2$
' S02
1440 H2S
so2
1455 H2S
so2
1510 H,S
i
so2
1525 H2S
so2
1540 H2S
so2
1555 H2S
so2
(AMPS)
Attenuation
4 x 10"8
4 x 10"8
4 x 10"7
8 x 10"6
4 x 10"6
16 x 10"6
4 x 10"6
16 x 10"6
4 x 10"6
32 x 10"6
4 x 10"6
32 x 10"5
4 x 10"7
8 x 10"6
(* scale)
Peak
Height
9.0
25.0
99.0
77.5
10.0
63.5
52.3
79.5
66.2
87.9
9.5
57.4
26.7
53.0
(PPM.Wet)
Concentration
.025
.066
.33
2.2
.33
2.8
.74
3.2
.94
5.0
1.1
3.9
.16
1.8
Dilution Corrected
Ratio i Concentration
.28
.73
3.6
24
3.6
31
8.1 3
35
10
55
19
43
1.8
20
1
J
-------
Location
Lime
Date Kiln II
4/9/74
Inject
Time
1610
1625
1640
1655
1710
1725
1740
1755
1810
Compound
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
(AMPS)
Attenuation
_7
4 x 10 '
_c
4 x 10 D
4 x 10~7
4 x 10"6
4 x 10"7
4 x 10"6
4 x 10"7
4 x 10'6
4 x 10'6
4 x 10"7
4 x 10"6
4 x 10"7
4 x 10"7
_0
4 x 10 B
4 x 10"7
4 x 10~8
4 x 10"7
4 x 10"8
(% scale)
Peak
Height
73.9
85.0
66.0
88.0
63.0
49.2
71.7
9.7
42.0
27.5
14.5
13.1
69.2
66.0
40.5
59.6
26.6
69.0
(PPM.Wet)
Concentration
.28
1.6
.26
1.6
.25
1.2
.27
1.7
.74
.25
.40
.16
.27
.11
.20
.11
.16
.12
Dilution Corrected
Ratio Concentration
11.0:1 3.1
18
2.9
18
2.8
13
3.0
19
8.1
2.8
4.4
1.8
3.0
1.2
2.2
1.2
1.8
1.3
ro
CD
-------
Location
Lime Inject
Date Kiln II Time
4/9/74 1825
1840
1855
1910
1925
1940
1955
Compound
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
SO,
(AMPS)
Attenuation
4 x 10"7
4 x 10"6
4 x 10'6
4 x 10'6
4 x 10"6
16 x 10"6
4 x 10"6
16 x 10"6
4 x 10"7
16 x 10"6
4 x 10"7
8 x 10"6
4 x 10"7
4 x 10"6
(% scale)
Peak
Height
54.0
11.6
23.9
61.1
52.2
81.7
13.7
79.1
92.3
89.0
66.3
70.7
61.6
26.3
(PPM.Wet) Dilution
Concentration Ratio C
.23
.53
.52
.38
.80
3.2
.39
3.2
.31
3.4
.26
2.1
.25
.83
Correct
:oncentra
2.5
5.8
5.7
4.2
8.8
35
4.3
35
3.4
37
2.9
23
2.8
9.1
ro
10
2010
SO.
-ป :-
-------
Date
4/10/74
Location
Lime Inject
Kiln II Time
955
1010
1025
1040
1055
1110
1125
1140
1155
(% scale)
Compound
H2S
so2
H2S
so2
H9S
L.
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
S00
(AMPS)
Attenuation
4 x 10"6
4 x 10"6
4 x 10"7
8 x 10"6
4 x 10"7
8 x 10"6
Missed
4 x 10"6
4 x 10"7
4 x 10"6
4 x 10"7
4 x 10"6
4 x 10"7
4 x 10"6
4 x 10'6
8 x 10"6
Peak
Height
17.9
68.0
75.8
61.0
78.0
51.0.
99.4
85.0
78.4
75.0
11.5
41.0
18.0
19.9
84.4
(PPM.Wet)
Concentration
.44
1.3
.28
1.8
.29
1.2
1.6
.30
1.4
.28
.52
.21
.66
.47
2.2
Dilution Corrected
Ratio Concentration
9.0:1 4.0
12 .
2.5
16
2.6
11
14
2.7
. 13
2.5
4.7
1.9
5.9
4.2
20
CO
o
I
-------
Date
4/10/74
Location
Lime Inject
Kiln II . Time
1210
1225
1240
1255
1310
1325
1340
1355
1410
Compound
H2S
so2
H2S
so2
H2S
so2
H2S
SO,
H2S
so2
H2S
SO,
H2S
so2
H2S
so2
H2S
SO,
(AMPS)
Attenuation
4 x 10"6
4 x 10"6
4 x 10"6
4 x 10"6
4 x 10"6
4 x 10"6
4 x 10"6
4 x 10"6
4 x 10"6
8 x 10"6
4 x 10'6
8 x 10"6
4 x 10"7
Missed
4 x 10"7
4 x 10"6
4 x 10"7
4 x 10"6
(% scale)
Peak
Height
11.5
43.5
11.0
39.7
11.0
50.2
11.0
52.4
13.8
70.6
13.0
62.0
94.4
65.4
52.8
49.5
34.5
(PPM.Wet)
Concentration
.35
1.1
.35
1.0
.35
1.2
.35
1.2
.39
2.0
.38
1.8
.32
.26
1.2
.23
.94
Dilution Corrected
Ratio Concentration
3.2
9.9
3.2
9.0
3.2
11
3.2 "2
11
3.5
18
3.4
16
2.9
2.3
11
2.1
8.5 r
-------
Location
Lime
Date Kiln II
4/10/74
(% scale)
Inject
Time
1425
1440
1455
1510
1525
1540
1555
1610
1625
1640
1655
Compound
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H0S
(AMPS)
Attenuation
4 x 10~7
4 x 10"7
4 x 10"6
Saturated
c
4 x 10 b
Saturated
4 x 10"6
4 x 10"6
4 x 10"6
Missed
Missed
Peak
Height
45.5
73.8
51.9
17.1
11.8
98.0
16.4
(PPM.Wet) Dilution
Concentration Ratio C
.21 9.0:1
.42
.87 8.7
.43
.36
1.6
.42
Correct
)oncentra
1.9
3.8
7.5
3.7
3.1
14
3.6
so.
32 x 10
-6
73.8
4.2
36
,.
-------
Location
Lime Inject
Date Kiln II lime
4/10/74 1710
1725
1740
1755
1810
1825
1840
1855
1910
Compound
H2S
so2
H2S
so2
L
H2S
so2
H2S
so2
H2S
so2
H2S
so2
H2S
SO,
H2S
so2
H2S
so2
(AMPS)
Attenuation
4 x 10"7
32 x 10"6
4 x 10"7
32 x 10"6
4 x 10"7
32 x 10"6
4 x 10"7
32 x 10"6
4 x 10"7
16 x 10"6
4 x 10"7
8 x 10"6
4 x 10"7
8 x 10"6
4 x 10"7
8 x 10"6
(5! scale)
Peak
Height
95.0
82.0
85.5
88.0
93.7
54.6
99.2
86.8
58.0
85.0
70.0
92.5
68.0
87.0
27.8
75.0
(PPM, Wet)
Concentration
.48
4.4
.30
4.6
.32
3.5
.33
4.6
.25
3.1
.27
1.9
.27
1.8
.17
2.0
Dilution Corrected
Ratio Concentration
2.8
38
2,6
40
2.8
30
2.9
40
2.2
27
2.3
16
2.3
16
8.7:1 1.5
17
-------
Lime Inject
Date Kiln II Time
4/10/74 1925
1940
1955
2010
Compound
H2S
so2
HฃS
so2
H2S
so2
H2S
SO,
(AMPS)
Attenuation
4 x 10"6
64 x 10"6
Missed
Saturated
4 x 10"7
32 x 10"6
4 x 10"7
16 x 10"5
(% scale)
Peak
Height
15.5
51.0
70.0
98.6
80.5
55.5
(PPM, Wet)
Concentration
1.4
5.0
.27
4.9
.29
2.5
Dilution Corrected
Ratio Concentration
12
43
2.3
42
2.5
22
I I
-------
t .
r ...ป ;
. ^-T* --J>*yป4~ A
35
APPENDIX A - II
Sample Calculations
1. Volume of dry gas sampled at STP, DSCF
mstd
. 1? Y7.375 (1.0 - .0193) (30)V 7'
u'\ 460ฐ + 63ฐ / '"'
V = Fraction of water vapor in a saturated qas stream
m '. '
at the temperature of the dry gas meter.
2. Volume of water vapor at standard conditions, SCF
Vw = 0.0474 (Vf - Vt) + (Vm) (V^ )
= 0.0474 (67) + (7.375) (.0193) = 3.321
3. Moisture content in stack gas
V..
B.
wo
Vu + Vm
wc mstd
3.321
x 100%
3.321 + 7.347
x 1002
= 31.IX
4. Molecular weight of dry stack gas
Md = 0.44 (X C02) + 0.32 (% 0ฃ) + 0.28 (X N? + X CO)
= 0.44 (13.1) + (0.32) (7.46) + (0.28) (79.44 + 0)
= 30.39 Ib/lb-mole
-------
36
5. Molecular weight of stack gas
Ms = Md " - Bwo> + 18 Bwo
= (30.39) (1 - .311) + 18 (.311)
= 20.94 + 5.60
= 26.54 Ib/lb-mole
6. Stack gas velocity at stack conditions, FPM
(Tj avg.
Vs = Kp Cp (,/AP) avg.
= (85.48) (0.83) (0.558) 46go + 159ฐ
(36) (26.54)
= 34.91
7. Stack gas volumetric flow rate at stack conditions, CFM
- 60 (1 - .311) (34.91) -^25 _||_
= 15220
8. Reduction of chromatographic data, (PPM.Wet)
Compound - H?S ,
Attenuation - 4 x 10"
Peak Height - 93.0%
Dilution Factor - 11.3:1
Concentration from Cal . Curve - 1.2 ppm, wet
Corrected for dilution - 14.8 ppm, wet
9. Daily average of composite sulfur compounds (PPM, Wet)
^ = n H <:i
D.A.H2S = I VI
* w i = 1 N
14 + 28 + 54 + 54-+ 55 + 55 + 170 +15+32+31
T5
+ 33 + 26 + 90 + 100 + 59
= 54
-------
37 9
10. Daily average of composite sulfur compounds, (PPM, dry)
D.A.H.S
" 2 w
n A
U.A.
WO
54
_ = 78 ppm
11. Daily average of composite sulfur compounds, Ibs/hr.
D.A.HzSp - D.A.H;Sd ( - ซ ) (0.) (60)
= (78) (8178 x 10') (15,410) (60)
= 6.3 Ibs/hr.
12. Daily average total reduced sulfur, (PPM, dry)
TRSd = Z D.A.H2Sd + D.A.CH3SHd + D.A.OMSd + D.A.DMDSd
= 78 + 0 + 0 + 0
*,
= 78 ppm
13. Daily average total reduced sulfur, Ibs/hr.
TRS = D.A.H2S + D.A.CH3SH + D.A.DMSp + D.A.DMDSp
= 6.3 + 0 + 0 +V0
. = 6.3 Ibs/hr.
ygy.*--*v3*i
i
-------
APPENDIX B
KEY TO INSTRUMENT READINGS ON LIME KILN PROCESS DATA SHEETS
1. Feed Rate of lime mud to filter.
2. Density and percent solids of lime mud to the filter.
3. Flow rate of oil to the kiln.
4. Flow rate of natural gas to the kiln.
5. Flow rate of air to the kiln, primary/secondary.
6. Total amount of natural gas burned in the kiln.
7. Total amount of oil burned in the kiln.
8. Time corresponding to item 6 and 7.
9. Concentration of oxygen in kiln exit gases.
10. Temperature of gases in the kiln; hot end/center section.
11. Temperature of gases leaving the kiln.
12. -Pressure drop .across the venturi s.cr.ubber.
13. Flow rate of caustic to the scrubber (zero).
14. Flow rate of makeup water to the scrubber.
15. TRS in the stack (Company Monitor); chart reading/scale.
16. Feed rate of limestone makeup to the kiln (zero).
17. Concentration of combustibles in kiln exit gases.
18.- Lime Kiln No. 2. Flow rate of noncondensable gases to the kiln.
18.- Lime Kiln No. 1. Amperages of induced draft fan motor.
19. Vacuum in the hood at the cold end.
20.- Lime Kiln No. 2. Outlet pressure of the induced draft fan.
20.- Lime Kiln No. 1. Damper setting of the induced draft fan.
21. TRS concentration in the stack corresponding to item 15.
-------
-!;
Facility Umc K11n |Unit ?lo. -5
| Operators \) _ P. rฑM-fi,-3
i ,..
i
t
i
j
j
i
1
j.
i
(
j
1.
i
1
i
4
1
?
3
4
5
6
7
8
9
10'
11
12
13
K
15
1C
17
Ig
It
JO
Flow:Lirr,e Mud to Filter
Solids to Filter
Fuel Oil Flov/ Rate
Fuel Gas Flov/ Rate
Primary Air Flov/ Rate/^,
Intearators: Gas.
Oil
Time
Excess Oxygen
Temperature: Hot End/ซ..
Cold End
Scrubber iP
Caustic to Scrubber
Make-up Hater Flew
TRS
Limestone Make-up
Co-.t^LUc.*
At-Cv.J^.A/..
/-looci Cbr-taPt
X O O^llol Priiinra^v.7
//33
^.^r-
5D%o'
7/0
^9.0
3.^0 1 3.^0
//CO
0
^9.^-
"/><=c
O
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'./ 1-0^
A". 5"
/^o
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ฃ6~
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pro
"34
^
3.f
"C7Z-,,
ffio
&. 6"
.^00
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O
39. .5"
-.06
Date V- ^ - 7^
Data Set No. / | Page /
*
/.?.?c
,90
/. ^t/
X??
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"/yo
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/^.v
=?.<:-
"ฐ%,
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3*5-
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3.3
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-------
St.
>',
\\.
jUnit .;o.
Dato Sac :io.
!o. ,9 I ',-.-.*
^^ ,^>^-- --.._).Jป.' " '
Units ;' tf eOjT3CL_ J JB5ฃ_^?ฃJJ^3.^. -
ฃi;^i_i ~
" n
'
'5~/0 \
53 !FvOl 011 F-cv/ Rv.
r.T"7 ~ . ""
J l_l
Ji
T
-iป
6 I ir.t?r;r2i:ors: ซ5^
0.07*07
i
M Cold End ! T |[
;r ^7D 7/0 1 736 73.6 ^o j 7o5
|CdListic to Scrubber
3/5 3l.
} 14|y.f;ke-yp Vl-iUer F'iov;
pVJ C..^L.. ,{:.(..'c.
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~ "
-------
St
:"-.''ii"y i.-KC ;-:-;in
ilf;:T"!!!:L
|U:iit rlo.
Date
Data Set No.
Solid:; to
Fuel Oil Flcv; R?.te
jf^'el G55 Flow Flute
5 jfvi.i!3ry Air Flew P.ate/-
-\:-Ci ' -
ป 7
Oil
s r~
Tin:e*
! 7.0
; IGjVi.nncr^turs,: H^t HnfJ/.^i.
In! cold End
1 12|Sc..-jbber ^?
to Scrubber
4J"c':e-jjp viater FTcv; G..-.'-
"I
H //j/o! ///?oi x/4/o_! /!ซP
I 730 ! 7^6" I 730 j 730
_^/p._
"
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0'0'Vfi
5 TP.S
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I. '
23.0
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0
0
! O-
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'
\:.'.'.- : -.- .:.! -i. 2
' Bfliaffl
-------
.i I
3 i
.11
'-r,v:.nis..\
.0.
Date
Da to Set :-io. ^ \
t
(JLl
A) I
- .^- ,. . - -^ _ ^. ( ^..^ - _ -
Scl:dซi t- F11t:-.-_ ;Ok^A!| ^.rj ' /tf\ Z$Z.\--j^\-/&l\ ^ '^ /&
~" ~ ~"' ~' ' " " L_[_
L.!r-iol Oil Fio--y..''.it;
i
'Jf.l G^3 FTCW EC 1C
>lcO
5
rinary Air rlcv; Rota^j "
T
U-
on
.-.-- II-
nm"
Time,
9 I Excess O^vaers
it St
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r-r-perafjrg: Mot Er^d. <..:!
1
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i
r
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o ! o ! o
^03 o/ j
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-1
T
/
o
o-
'ซ-
-------
St
jl'nU rio.
Operators
Data Sot .*!o.
' ' Jri0-!?/*-1'1'- ':'-'-'-! to ^'*-f-
ป ?. ! Solids to F1U?r
t j
;3 !Fvel Oil Ficv; R^te
- . -..,., . -
_ir : ""aI::l Fc::::il'2' "_jJ '
/7
;7
Oil
I Ai y
37 \
yo
.?/
//a
i j ^iTo^pa^jc^rgj Hot Erd/--;...
h't
735" J
K^ I
I 3o..5 i 3/. O
to
376
15 H3
JAwJ,-^/" ij ฑ,j \ <-\ / " (*/
IX* s! _/L_J _//_ , x<
^~ vT i i" ' !
if\ C,.^;,...,t.fe;c,
3/0
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^ *. *V< o" j
./^C'- - Ar^^^c
H',0 *.ซ
\
-------
Unit .Jo.
.
Data Set No.
! 1
I I'n-its \\J6C6_ !AJt> LlloQlL&ฐllฃ2^JZu^ltfJtoฃ_.'
i i i ' * i I ป
tO 1 t f: ?
14 |r:,CM C-2S Row Re^s
M
/( "'*-.."- 5^-
Flew Rits.;,.. -'._.
i "ป ir-n'mary Air Flew Rits.
i I ; '_
>$ ' I-to or n tors: Gar.
!7P
011
Tlr-.i
. _.
Cold End
i;
/7/
I
;"r~7~~r.7,"~ !T~"11"
F1ow
GrK,
///go. i
3-5.0 J 33.oUp.
O I Vo?/O I
17,71
T'
IS
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7
-7
JO
IRS
.. . ... o.y - ..;-._ -^^
L C,..,,u..,U,',,
..,,.C,.,,>.;7,,.
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^
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31.0
.
/
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i
Coj!ipo"y s^. ^'-fix. "<,fMv- Co %~-> /jซ xi ซ, 'Locution 'c^c-.^-^.f K.xoป*'\iT7i/.>.v^
/ | __j. '
Facility Umc Klln ' jUnit No. 3
Operators ฃ. /r,... /, r.
I-.. . - - ^ .
!'
\
1
I
i.
I
i
i
!
i :
I.
'!
]
'(
i
i
[
i
I
i
I
i
!
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
It
It
JO
Flow:Lin:e Mud to Filter
Solids to Filter
Fuel Oil Flow Rate
Fuel Gas Flow Rate
Primary Air Flow Rate^
Integrators: Gas
Oil
Time
Excess Oxygen
Temperature: Hot End/ฃ.4
Cold End
Scrubber i?
Caustic to Scrubber
Make-up Water Flow
TF.S
Limestone Make-up
C* L t- Lt
^ป C* ^^ Ov^ i tป tQt G. ^
^G^^.A/,,
l-lc^ &^Pt
15 O-,UcL Prf^.,r*
Units
G,-n
$*%*&
lUAr-
^3Ar
'"^z:
So* ft*
/t*
0^ ^.
%
Xr
r
X.H^
N.A.
Gpn
^*d2^f
V
^
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x^c!^
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?.o
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7/c?
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*
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o
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-.04
/y.G
/0.7O
-co
''*%7
330
'70
^ <>ซ./
7/0
3a.^-
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//
o
3AT
1100
60
''%
J?3o
'K-r
ป
7.6
/..r
,^7C
3^/
0
.^.fl
-.06
WO
Date y-/o-~7
^T^
X'^,-
^36
'/^
^CT"?7
//V3
7V
*ฐ%f.
730-
310
*
37 <"
fl~Tc
O
^/,<-
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A?.0
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to
J^/L
^c
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ฐ'^
//.T7
^.9
?%c
735-
,fco
v?70
0,'set/i/
O
^/r
-6,-T
73.-^
/-^3C
^6
'^5-
o?-3c
/ 7/
c/ซ,W^
/ซ? 32
7V'
"%-'
7?o
33.6
37. /
7.6
"'%
7/5"
33.6'
?2J-
*i^; U^P.-JBJซปT;*^
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Sfc
.lil^l
jUnii ;:c. <2-
AS-itn
05 te
Data Sot :,'c.
_ j _rggo /
i n
Jr!ili*i4;Ji^J.ฃiฃJl;^^
. ' i I i I I _ *
n^-Jj Ll^j j^L,-vL.f.J-U.S
Soljji!s -:o Fil':;vi- i
f'O I
,. ^ r., r.,0/1 -'.T*' j'V 'V I '% ! '
<3t I /
~T~T~
0/OS73/7
Oil
u
.
7.0 | 6.7 I 6.
T
ijL^.
7.3 .
i^i^irT"^^";
Caustic to Scr.ibbsr
r " rov^fc-,.q~'" j'j
l^JMrike-vp^VJj^r Flov; jGr^j jj
JfeTd "
15hr.5
f
^j.^..c....j.-J...^,. T^jp
: I" * I! O !'0 j O j D I O _0_
I "-Zzllz/.O \3/-0 \3/.o !2o.5x I :?o.S\3/.0
VJฃ.
v.
IJI
d.\
|-Z^1
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^/. o yo.w
-------
I 4i
! S
5 i
i '<
t
k ]
)
!
j
ir
i
i
1
.
j
j
i .
;':
0-.
""
1
?.
3
4
5
6
7
o
*
11
~\7:
-, n
14
1 *
1C
.'V
, V
.*.
1
1-0
- ; > ' , i , . ... ,
1 ' '-' Lir'.o !" in
^ators P Sf^ ,s
V
Fk.v,-:Lin-.= Mi:.-J to Filtr--
Sollrls to Filter
Fusl Oil rlcv.1 Rate
,. - "
F:.'f.-1 Gas Flow ?.d!:e
rriniary Air Fie--/ Rate-.',.,
.,.xpnr,,t:)v.s. p.s
on
Tirco
L'XMSS Oxys?p. '
,._r....._ Uot rrH /
Cold End
Scrubber -P
Cjustic to Scrubber
v:ซike-up V'ster Flev/
TP.S
Ll^stone Mefee-JD
C^^^.^.tlr.*
:i-...C-^-,.i/M
i : _ . T^ . . .;/
XI3 0-.li-.'. I-V ซ,:,ซ-.
^-;P)
Units |
-,,ซ
v. j
ifc-./V
lioO 1
PtV:,r |
v:^- j
- - 1
1
C'-J ^.- 1
V
'o
' ,"/ '
T
i
t-,A- !
G f- i-i
^x^
w.r5"
' /,
rฐ^\.
,.,,,, I
..', I. -,.!-, |
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! ^)00
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30 p
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J37r
sy,
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kc6
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|:.':i-;t
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Detc
' Data
'
Set Ho
;
y
(
\ Poci--
^3 .
'
.
l
.::/.'..:.:-VA-ri'.:^;. :;;-;
:-: !' y..W:it:-:,.'>; /..;ป!ป'
Off
-------
r;-.,;"ii-;' /,,^P kil-n !!Ji::t .lo. I
= tf
Date
Deta
i i
"i
^
: ,1
:,|
: .si
^
6
1 7
i 8
: 9
:
; 12
i
: "
* . _
1 36
! n
i?
id
;*o
\
FT <.;: Li;-.* I'A.ri to Fi He-
Sol ids tu Filter
:uol Oil Flov/ F:c.ie
Fi",?'l Pas Flov; Rate
f ensure
Pt'ii"^v*v Air i "lo1.^ ^-"' "L^
Integrators: Gas
Oil
Time
c/:c:-'ss Cxvosn
Tir:-.;perature:Hct End .
Cole! Enc!
3cr,,fcl>er iP
loko-up Water Flcv;
-i sues tone Mnke-up
^. O '^ 0^'^ fp*"~,>
JT-^-rJ F., M0-Tc.
] Oru-fr- /Xซ,~r &-/
I'll 1 I.S |
. 9fซ
!
i
d*'x"oor i
i
|dCo Cf- T" I
JW /.r !
%
ฐF
9P-n
^^C
ฐfo
iป:0*&
am/J
i //30
1
_
1
1
7oo
/. /
eo-xwo
| //J7
J ^
1
vf^O
270
/6/50
O
-.06"
<^.^"
/QOO
760
/O
t-U
007037
//^J5
3-3
*5ฃO
<^?7O
^a
O
-. 6.6""
> X" C"
1300
HO
7DO
/n
/ O
.
Mฃ
3-V
^-7^"
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ฐ /fe&
O
-05"
^.^
/330
/^C
760
//^>
U
oo7 / as~
-
/530
J.^T
JTC
'
c=?70
5%
(3
. 05'
ฃ.<ฃ'
/^3G
^ /38
700
6?ป TO
007/7?
/4/JS'
3.3
4~73
270
/lo0
O
-.06
3<2C
^--T"
/^30
//5"
675-
/ /->
/. o
e>o 7 a3 3
/oTJ9
3.4
^70
o?70
/tOO
o
-. 06"
'
c5?O
L ฃ.0
IUG
/CO
C,CC
1 /S
/- O
oe^W
K02
^.1
s-^r
o?76
^
o
-or
=?? 6
6. 6
3 i'
ซ* tl . . , ^.
^:: '/.."/I.t ;f:
;;/ ; CJU^u, v~ A M**r *ฃ& "
:'/;;. ' /i6-=>/oo 5^ฐ^ ซS 3:
I// "/C
-------
Table IV
Data On The Sulfide Content Of The Lime Mud During The Testing
(Analysis Performed By Michael Franklin of NCASI)
Date
Time
Kiln
Sol id(2)
Sulfide Content
(% as Na2S)
4/4/74
4/4/74
4/5/74
4/9/74
4/9/74
4/9/74
4/10/74
4/10/74
1320
1320
1230
1230
1545
1140
1445
1
2
2
1
2
2
2.
2
65.9
65.1
70.1
64.0
69.1
69.5
68.5
75.0
0.87
0.61
0.4
0.86
0.43
0.46
0.40
0.43
-------
APPENDIX C
SAMPLING DATA SiiLET
Plant
Stock if
/C,/f.>
Remarks I/',.-,:!
Ccx/o.
Run Ho.
Date
Time of Sample
Earoniatric Prossuro, "Hg
Stack Pressure, "Hg
Final Dry Test Me.tc-r Reading, Ft3
Initial Dry Test Meter Reading, Ft3
Meter Volume Sampled P Meter Cond,, Ft3
Average Meter Temperature, ฐF
Average Stack Temperature, ฐF
Average Meter Vacuum, "Hg
Average Meter Orifice &H, "H20
Observed Sampling Rate, LPM
Gas Volume Sampled, Ft3, Dry, 70ฐF, 29.92 "Hg
, ! ' ,
ihh'/
~^&>M>o
5o
99. ฃ7.2
9& 2,oo
b. 0 2-2..
5:r
/ฅ?-
$,/#
Calculations:
-------
SAMPLING DATA SHEET FOR
Stack
Remarks Mo MRic.Tvr?/? T?L-.^' otu &- "?- K'Ji'J^
Run No.
Date
Time of Sample
Barometric Pressure, "Hg
Stack Pressure, "Hg
Final Dry Test Me-ter Reading, Ft3
Initial Dry Test Meter Reading, Ft3
Meter Volume Sampled P Meter Cond,, Ft3
Average Meter Temperature, ฐF
Average Stack Temperature, "F
Average Meter Vacuum, "Hg
Average Meter Orifice AH, "H20
Observed Sampling Rate, LPM
Gas Volume Sampled, Ft3, Dry, 70ฐF, 29.92 "Hg
^
^^
>>o
3&
JOt. Z2S~
-------
SAMPLING DATA SIIECT FOR
Plant S~ 7?;.-Co;g>
Remarks _ 7?,A.,)
Stack ft 2_ Li Mr.
- /
Run No.
Date
Time of Sample
Barometric Pressure, "Hg
Stack Pressure, "Hg
Final Dry Test Meter- Reading, Ft3
Initial Dry Te&t Meter Reading, Ft3
Meter Volume Sampled @ Meter Cond., Ft^
Average Meter Temperature, ฐF
Average Stack Temperature, ฐF
Average Meter Vacuum, "Hg
Average Meter Orifice AH, "H20
Observed Sampling Rate, LPM '
Gas Volume Sampled, Ft3, Dry, 70ฐF, 29.92 "Hg
7, 1 VX 1 P:
//."//'/
ci'^Z-ic:/1,'
~*>ChMj
3o
?>^
11^171
/7.0,-TOo
^77Z
ฃ7
/T2U
n.fo
Mซ/r/\ ~
^O /;'//:'
3o
"7^0
1*0. 8W
/zr..rzo
^.33t/
67
I&~
O./o
' ' vS"- J: '/>""
^Oi^J
3o
3o
' /3<$..2#
t^f./oO
^/&>
75
l^1/-
OrfD
Calculations:
-------
PRELIMINARY VELOCITY TRAVERSE
[]
11
D
PLANT_^
DATE ป- - /'---
LOCATION..'
STACK I.D..
BAROMETRIC PRESSURE, in. H*_
STACK GAUGE PRESSURE, in. H20.
OPERATORS, .'-.- ' -
/ |O"'
P-r
ซJ.,' * s
I'V v-
! ;-
/I P
,/D
pi tTo-..\.:r
TRAVERSE
POINT
NUMBER
/- /"
2. -2"
?-3-f
4-S^r
$-*ฃ
ฃ-*?
7 - "ฃ
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PRELIMINARY VELOCITY TRAVERSE
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LOCATION L
STACK 1.0
BAROMETRIC PRESSURE, in. Hg.
STACK GAUGE PRESSURE, in. H2
OPERATCRS___
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PRELIMINARY VELOCITY TRAVERSE
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LOCATION '
STACK I.D. ' "
BAROMETRIC PRESSURE, in. M?
STACK GAUGE PRE
OPERATORS
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PI-AHT '
DATE ' ' "
LOCATION ' ' ' ' '
STACK I.D. ' " '
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BAROMETRIC PRESSURE, in. H; 3o
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NUMBER
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TEMPERATURE
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-------
PRELIMINARY VELOCITY TRAVERSE
PLANT _ ^.7.
DATF
C.; 5
LOCATION f'-~7- ( .v-'r
STACK I.D. MV'7 "
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LI
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BAKOi/.ETRIC PRESSURE, in. H;
STACK GAUGE PRESSURE, in. H20
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CH:;AT DATA AND CALCI'LATIO;-? EHSST
il -y , i /I'flV
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Date
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Source
Location
Run .'.'o.
Date
Gas
Cr^at Analysis, Dry Easi
(^ Vol'J.-.o)
Dry Basis
ilerr.nrlcs
CO?
02
CO
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\->
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C02
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Air
Hun ป.'o.
1
2
3
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o 5.T.?. (SCF;-:)
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Eur'ners i
V.'aste
r'raction Of
IT> * T T
. r-.s /ill
Surr.ers
Operating
CC'o Fror:
BuiT.ers
(;* Vol)
CC2 Frcn
" .: - ~ a
"(.Hoi) '
nrinintni-nfal
-------
CttSAT DATA Af.'O CALCULATION 5H5ST
Source
C-. ;
<ฃl /L/ ITS /
Location
Run Koซ
/
1
5"
ฃ
Date
UJtSZ;
i Ls t
dj ,s'
ihL
W
i
Gas
CQ?
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CO
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up
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7.^
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Dry Basis
./
Renarks
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Run I.'o.
1
2
3
Ayr;. Kolec.
V.'gt. Of Dry
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.
/'.V^ซ
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(;")
Stack C-as 'iio'.-r Hate
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Burners
^'jj'^^-^5 ^
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Fraction Of
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rnfjinftrintj. nt:
-------
CR5AT DATA AI.'D CALCULATION SHKI-
Source
Location
Run I.'o.
/-
f
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S
Gas
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Dry Basis
./
Remarks
Run ;."o.
1
2
3
Av^ซ i-iolcc
V.'gt. Of Dry
Stack Gas
(v;Gt./;-;oic)
;;v'i'
Excess
Air
(;;)
Stack Gas Flo:.-: Hate
3 S.T.?. (SCF:-:)
Burners
Burners i
Waste
Fraction Of
?i:-3 .Ml
iB^^Ti^rs
Cpcratir..^
CO? -;'ror:
Eurnors
(;ป Vol)
CC? Frcn
:/asto
(.* Vol) '
ซ'n
-------
/
PRELIMINARY VELOCITY TRAVERSE
PLANT.
DATE,
LOCATION X^: '/ (>** /'ft'/."S_
STACK I.D. "M '<."'' _
BAROMETRIC PRESSURE, in. Hg Hi
STACK GAUGE PRCSSUfiE, in. H20.
OPERATORS //A^ 6///'/ฃ ^ ฃ
TRAVERSE
POINT
NUMBER
/- /"
7- 3"
3~ ^''
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TEMPERATURE
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SCHEMATIC OF TRAVERSE POINT LAYOUT
.TRAVERSE
POINT
NUMBER
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AVERAGE
VELOCITY
HEAD
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STACK
TEMPERATURE
(Ts). ฐF
-------
SAMPLING DATA SIICET FOR $*: '"""
Plant T
P.-- :-
Remarks
Stack :'' ' /..;/vr- .-V''
Run No.
Date
Time of Sample
Barometric Pressure, "Hg
Stack Pressure, "Hg
Final Dry Test Meter Reading, Ft3
Initial Dry Test Meter Reading, Ft 3
Meter Volume SampVfed 0 Meter Cond., Ft3
Average Meter Temperature, ฐF
Average Stack Temperature, ฐF
Average Meter Vacuum, "Hg
Average Meter Orifice AH, "H20
Observed Sampling Rate, LPM
Gas Volume Sampled, Ft3, Dry, 70ฐF, 29.92 "Hg
/
4 >//*
~?--^> s.r.'.r
3o
3o
/ 09.97*
/CA:'.*VO
S^io
V,3
\~70
7^"
5. -' )
i
I
1
Calculations:
-------
APPENDIX D
SAMPLING PROCEDURE
The following is a draft copy of Environmental Protection Agency Method 14.
This is the suggested method for the sampling and analysis of reduced sulfur
emissions.
-------
This documrnt is a preliminary drif*.
has not been formally rclcuscil by Ki'A
fM n,,, =nn...- no n,-:s.:i(
MTV 01 lOTE. UK V\ ป L. rep-oMHt Agency policy. It i* J.ci-.iB circu-
\\ 0 XUU latcd for conrrwit on its technical accuracy
and policv implications. 9
METHOD 14. SEMICOHTIfll'OUS DETERKINATIOfl OF
' MALODOROUS REDUCED- SULFUR
EMISSIONS FROM STATIONARY SOURCES
*
* *. ' .
1. Principle and Applicabni'ty ' .. . '
1.1 Principle. A continuous gas sample is extracted from the emission
source and is diluted with clean dry air. An aliquot, of the diluted sample
1s then analyzed for malodorous reduced sulfur compounds (i.e., hydrogen
. sulfide and organosulfur homologues) by gas chromatographic separation and
flame photometric detection. The flame photometric detector (FPD) measures
the sulfur compounds eluting from the separation column by detecting the
chemlluminescent emission of the excited Sp species formed when a sulfur
compound is burned in an hydrogen-rich air flame. A narrow band-pass opti-
cal fil'ter placed between the flame arid a photomultiplier tube permits the
transmission of a particular band of the emission at 394 nm. Thus, a 30,000:1
specificity ratio of sulfur to non-sulfur bearing constituents in the effluent
gas stream is achieved. Two GC/FPD analytical systems equipped with suitable
separation columns are utilized for the resolution of both. low and hioh mole-
cular weight reduced sulfur compounds. The first resolves hydrogen sulfide,
sulfur dioxide, methyl msrcaptan, ethyl mercaptan and dimethyl sulfide. The
second resolves propyl marcaptan, butyl mercaptan, dimethyl disulfide, dipropyl
sulfide and dibutyl sulfide.
1.2 Applicability. This method is applicable for the determination of
total reduced sulfur (TRS) emissions from stationary sources when specified by
the test procedures for determining compliance with the flow Source Performance
Standards. j
88 I
-------
2. Ranne and Sensitivity
2.1 Range. The range of the method is dependent on the amount of dilu-
tion used. The range of the flame photometric detector 1s approximately 0
'to 1 ppm for each compound resolved.
2.2 Sensitivity. The minimum detectable concentration 1s less than
0.5 ppb. "' - _
3. Interferences ,-' '.' -1
3.1 Moisture. Condensation in the analytical column and FPD burner block
may cause interferences. This potential is eliminated by conditioning the sam-
ple with dilution air to lower its dew point below the operating temperature
of the GC/FPD analytical system prior to analysis.
3.2 Carbon Dioxide and Carbon Monoxide. The presence of C02 and/or CO
1n the gas stream analyzed can be a major source of interference. Stack
amounts of CC^ and CO produce a substantial desensitizing effect on the FPD.
This effect is eliminated by adjusting the operating parameters of the chroma-
tograph so that all C02 and CO present in the sample aliouot elute to the FPD
with the "air peak" prior to the elution of any sulfur compound.
4. Precision and Accuracy ' . . -- .:
4.1 Precision. Estimated to be within +_ 5% of full scale. :
4.2 Accuracy. The accuracy is dependent on the accuracy of the calibra-
tion standards used. It will approximate +_ 5% of full scale.
5. Apparatus -
5.1 Sampling (Figure 14 - 1).
-------
5.1.1 Probe - Stainless steel or sheathed borosilicate glass
equipped with a glass wool filter to rerove participate matter.
5.1.2 Sample Line - 3/16 inch Inside diameter FEP Teflon tubing,
heated and maintained above 100ฐC.
5.1.3 Sample Pump - Leakless Teflon coated diaphragm type or equi-
valent. The pump head will be heated and maintained above 100ฐC.
5.2 Dilution Interface. The dynamic serial dilution inferface system
depicted in Figure 14 - 1 and described below is reconmended. Alternate dilu-
tion approaches must meet the criteria defined in Addendum B. -
5.2.1 Pump - Model A-150 Komhyr Teflon positive displacement type,
non-adjustable 150 ml min +_ 1.5%, or equivalent, per dilution stage.
5.2.2 Valves - Three-way Teflon solenoid or manual type.
5.2.3 Sufficient Teflon fittings and tubing to assure that all sample
and calibration gas contacts are Teflon.
i
5.2.4 Box - Insulated box, heated and maintained above VOOฐC, of
sufficient dimensions to house dilution epraratus.
5.2.5 Flowmeters - Rotameters or equivalent to measure flow from 0 to
1500 ml/min +_ 1.0% per dilution stage. . l '
5.3 Analysis. Analytical system for measurement of low-molecular weight
sulfur compounds (GC/FPD - I). (See Figure 14-2 and Addendum A).
5.3.1 Separation Column - 36 feet by 0.085 inch inside diameter Teflon
tubing packed with 30/60 mesh Teflon coated with 5% polyphenyl ether and 0.05%
orthophosphoric acid, or equivalent. ... . j
sement
Mention of a specific company or product nar.a doss not constitute endoi
by the Environmental Protection Agency.
90
-------
5.3.2 Stripper or Precolumn - 2 feet by 0.085 Inch Inside diameter
Teflon tubing packed as in 5.3.1.
5.3.3 Sample Valve - Teflon ten-port gas sampling valve, equipped
*
with a 10 ml sample loop.
5.3.4 Oven - For containing sample valve* stripper column and
separation column. The oven should be capable of maintaining an elevated tem-
perature ranging from ambient to 100ฐC, constant within +_ 5ฐC.
5.3.5 Temperature Monitor - Thermocouple pyrometer To'measure column
oven, detector, and exhaust temperature +_ 2%.
5.3.6 Flow System - Gas metering system to measure sample flow,
hydrogen flow, oxygen flow and nitrogen carrier gas flow.
5.3.7 Detector - Flame photometric detector as specified in Addendum A.
5.3.8 Electrometer - Capable of full scale amplification of linear
.0 -A
ranges of 10 to 10 __amperes full scale.
5.3.9 Power Supply - Capable of delivering up to 750 volts.
5.3.10 Recorder - Capable of full scale display of voltages from elec-
trometer amplifier in the 1 millivolt range.
5.4 Analytical system for measurement of high-molecular weight sulfur com-
pounds (GC/FPD - II). (See Figure 14-2 and Addendum A).
5.4.1 Separation Column - 10 feet by 0.085 inch inside diameter Teflon
tubing packed with 30/60 mesh Teflon coated with 10 percent Triton X-305, or
l
equivalent.
5.4.2 Sample Valve - Teflon six-port gas sampling valve equipped with
a"lO mi"sampleTdbp" "~ ~
5.4.3 Other Components - All other components same as in 5.3.4 to 5.3.10.
91
-------
' 5.5 Calibration. Permeation tube system (Figure 14 - 3).
5.5.1 Tube Chamber - Glass chamber of sufficient dimensions to
house permeation tubes. *
5.5.2 Flov.weter - Rotameter or equivalent to measure flow range from
0 to 15 lit/min +_ 1.02.. . '
5.5.3 Constant Temperature Bath - Capable of maintaining permea-
tion tubes at certification temperature within j^0.1ฐC
/
5.5.4 Temperature Monitor - Thermometer or equivalent to monitor bath
temperature within j^0.10C.
.r
6. Reagents
6.1 Fuel - Hydrogen (H^) prepurified grade or better.
6.2 Combustion Gas - Oxygen (02) research purity or better.
6.3 Carrier Gas - Nitrogen (N2) p.repurified grade or better.
6.4 Diluent - Air containing less than 0.5 ppb total sulfur compounds and
less than 10 ppm each of iroisture and total hydrocarbons.
6.5 Compressed Air - 60 psig for GC valve actuation.
6.6 Calibration Gases - Permeation tubes gravimetrically calibrated
and certified at 30.0ฐC+ 0.1ฐC.
7. Procedure '
7.1 Instruments may be assembled from the components described herein or
may be purchased corrniercially. If commercial instruments are used, follov/ the
specific instructions given in the manufacturer's manual.
7.2 Sampling. Calibrate the dilution and analysis systems as described in
Section I. Heat and maintain the sample line, pump and dilution apparatus
92
-------
above 100ฐC. Check the sampling system for sample losses and leaks by in-
trodudng a knov/n concentration of hydrogen sulfide (H-S) into the probe,
approximating the TRS level anticipated to be present in the gas.stream analyzed.
Monitor its response on GC/FPD-I. If sample losses are less than 555, insert
the probe into the test port making certain that no dilution air is entering
the stack through the port. Begin sampling and dilute as required to maintain
the sample below its ambient dew point. Usually, ten to one will suffice. Con-
dition the entire system vn'th sample for approximately '15 minutes prior to com-
mencing analyses.
7.3 Analysis. Aliquots of diluted sample are injected simultaneously in-
to both GC/FPD analyzers for analysis. GC/FPD-I equipped with a ten-port gas
sampling valve, stripper column and polyphenyl ether analytical column is used
to measure the low-molecular weight reduced sulfur compounds. GC/FPD-II equip-
ped with a six-port gas.sampling valve and a Triton X-305 analytical column is
" *
used to resolve the high-molecular weight compounds.
' '. 7.3.1 Analysis of Low-molecular Weight Sulfur Compounds - The sample
valve is actuated for one to three minutes in which time an aliquot of diluted
sample is injected into the stripper column and analytical column. The valve
1s then de-actuated for approximately fifteen minutes in which time the stripper
column is backflushod of heavy sulfur compounds, the analytical column continues
to be foreflushed, and the sample loop is refilled. Monitor the responses. The
elution time for each compound will be determined during calibration. The chro-
matographic and flame conditions will be as follows: nitrogen carrier gas flow
rate of 50 ml/min, exhaust'temperature of 110ฐC, detector temperature of 105ฐC,
oven temperature of 40ฐC, hydrogen flow rate of 80 ml/m1n oxygen flow of 20 ml/min
i
and sample flov/ rate betv/een 20 and CO ml/min.
93 '
-------
7.3.2 Analysis of High-molecular Height Sulfur Compounds?- The
procedure is essentially the same as above except that no strippsr column is
needed. The operating conditions are also the same with the exception of an
oven temperature of 70ฐC and nitrogen carrier gas flow of 100 ml/min.
8. Calibration
8.1 General Considerations. Accurately known concentrations (;M2) of
a variety of sulfur compounds can be generated by passing clean dry air or
other diluent gas over permeation tubes, each containing a specific sulfur com-
pound as a permeant. These tubes consist of hermetically sealed FEP Teflon tub-
ing in which a liquefied gaseous substance is enclosed. The enclosed gas per-
meates through the tubing wall at a constant reproducible temperature depend-
ent rate. A wide range of known concentrations can be generated by varying and
accurately measuring the flow rate of diluent gas passing over the tubes.
8.2 Calibration Procedure. Assemble the permeation tube calibration appara-
tus as depicted in Figure 14 - 3. Insert the permeation tubes into the glass
tube chamber. Check the bath temperature to assure agreement with the calibra-
tion temperature of the tubes within ^0.1ฐC. Allow several, hours for the tubes
to equilibrate. When equilibrated, vary the flow rate of diluent air flowing
over the tubes to produce the desired concentrations for calibrating the analy-
tical and dilution systems. The airflow across the tubes must at all times ex-
ceed the flov/ requirements of the analytical systems. The concentration in parts
per million generated by a tube containing a specific permeant can be calculated
as follows: | p
C = tr *r x 5 Equation 14 - 1
94
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Vlhere: . .
C = Concentration of Perrceant Produced in ppm.
Pr = Permeation Rate of Tube,' ug/min.
H = Molecular Height of Perr.eant, .
G = Gas Constant = .082 ^ltc
L e Flov/ Rate of Diluent, Liter/min.
T e Permeation Tube Temperature, ฐK. _>
/ ' ~
P = Barometric Pressure, atm.._
8.3 Calibration of GC/FPD Analysis Systems. Generate a series of known
concentrations (usually six) spanning the linear range of the FPD (approxi-
mately 0.01 to 1.0 ppm) for each sulfur compound anticipated to be present
1n the gas stream analyzed. Inject these standards into the GC/FPD analyzers
and monitor their responses. . . .
8.3.1 Calibration Curves - Plot the GC/FPD responses in current
(amperes) versus their causative concentrations in ppm on log-log coordinate
graph paper for each sulfur compound calibrated.
8.4 Calibration of Dilution System. Generate a known concentration of
hydrogen sulfide using the permeation tube system. Adjust the flow rate of
diluent air for the first dilution stage so that the desired level of dilution
1s approximated. Inject the diluted calibration gas into GC/FPD-I and monitor
Its reponse. Using the appropriate calibration curve, reduce the response and
determine the dilution factor by taking the ratio of the known concentration to
the resultant diluted concentration. -.Repeat- the procedure for each stage of
dilution required. - -------- --
95
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v. >
9. . Calculations
9.1 Determine the concentrations of each reduced sulfur compound de-
tected directly from the calibration curvps.
9.2 Calculation of TRS. Total reduced sulfur will be determined for
' each analysis made by suraiing the concentrations of each reduced sulfur com-
pound resolved during a given analysis.
TRS <= I (H2S, MeSH, DMS, DMDS) X d ' ' Equation 14 - 2.
Where:
TRS ซ Total Reduced Sulfur in ppm, wet basis. "
tLS = Hydrogen Sulfide, ppm.
MeSH = Methyl Keraptan, ppm.
DKS - Dimethyl Sulfide, ppm.
DKDS =_Dimethyl Disulfide, ppm.
d e Dilution Factor, Dimensionless
9.3"-. Average TRS. The __. . average TRS will he determined as
follows: -N
'-ZlllAvg. TRS = i-^pgr^r Equation 14-3.
ป U ^ I " DปVU)
Where:
--. Avg. TRS = . . average total reduced sulfur in ppm, dry basis.
- TRSj = Total reduced sulf'ir in ppm as determined by Equation
14-2. J
N = Number of analysis performed.
Bwo = Proporation by volume of water vapor 1n the qas stream
as determined by J'.ethod 4 - Determination of I'oisture in Stack Gases (36 PR 24RP7).
96 .
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10. Bibliography. - '
(1) O'Kceffe, A. E. and Ortman,' G. C., "Primary Standards for
Trace Gas Analysis", Anal. Chem. 38,760 (1966)
Stevens, R. K., O'Keeffo, A. E., and Ortman, G. C., "Absolute
Calibration of a Flame Photometric Detector to Volatile Sulfur Compounds
at Sub-Part-Per-Million Levels", Environmental. Science and Technology,
3:7 (July, 1969).
(3) Mulick, J. 0., Stevens, R. K., and Baumnardner, R., "An
Analytical System Designed to Measure Multiple Malodorous Compounds Re-
lated to Kraft Mill Activities", Presented at the 12th Conference on
Methods in Air Pollution and Industrial Hygiene Studies, University of
Southern California, los Angeles,. Ca. , April 6 -'8,; 1971.
(4) Devonald, 'R. H. Serenius, R. S., and Mclntyre, A. D., "Evalua-
tion of the Flame Photometric Detector for Analysis of Sulfur Compounds",
Pulp and Paper Magazine of Canada, 73/3 (March, 1972).
(5) Grimley, K. W.t Smith, H. S., and Martin, R. H., "The L'se of
a Dynamic Dilution System in the Conditioning of Stack Gases for Automated
Analysis by a Mobile Sampling Van", Presented at the 63rd Annual APCA
Meeting in St. Louis, Mo., June 14 - 19, 1970.
97
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ADDENDA
A. Performance Specifications for Gas Chromatographic - Flame Photo-
t
. metric Analyzers.
Range (linear): 0 to 1 ppm
Output (minimum): ' 0 to 1 HV full scale
-, at 1 K-ohm
Minimum Detectable Sensitivity: 5 ppb '
Zero Drift: ,..- ' 1% per hour at most sensi-
tive range
Span Drift: 1% per hour at most sensi-
tive range
Precision (minimum): ฃ 2% of full scale
Noise (maximum): . +_1% of full scale
Linearity: - 1% of full scale
Oven Stability: ฃ 0:5ฐC
Operating Humidity Range: . 10 - TOO percent
Operating Temperature Range: 5 to 50ฐC
B. Specifications for Dynamic Dilution Systems. ,
Design ' The dilution system shall be
-. constructed such that el":
sample contacts are mace :f
inert materials. Also, " =
dilution system shall he=t
and maintain the sample i::ve
250ฐF both prior and durir:
dilution.
Range } r The dilution system shall ': =
. ' capable of a minimum tar. ~o
. . one dilution.
98
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Output
Drift
Precision
The output shall be in excess
of that required for analysis.
The excess will be vented to
the atmosphere.
Output shall not chance rore than
+. 2% over a 24-hcur'uradjusted
continuous operation.
+ 2% of dilution factor.
C. Definitions of Performance Specifications
Range:
Output:
Full Scale:
Minimum Detectable Sensitivity:
Accuracy:
Zero Drift:
Span Drift:
The minimum and maximum r.easure- -
merit limits.
Electrical signal which is pro-
portional to the meeS'jrerr.ent;
intended for connection to
readout or data processing
devices. Usually expressed
as millivolts or miliiernps full
scale at a given impedance.
The maximum measuring limit for a
. given range.
The smallest amount of input con-
centration that can be detected
as the concentration approaches
zero.
The degree of agreement between a
measured value and the true
value; usually expressed as
i percent of full scale.
The change in instrument output
over a stated time period,
.usually 24 hours, of ..--adjusted
continuous operatic", .-.hen the
input concentration := zero;
usually expressed as zercent
full scale.
The change in instrument output
over a stated time period,
usually 24 hours, or" -nadjusted
continuous operation. -.%hen the
input concentration ; a btated
upscale value; usual"..- expres-
sed as percent full srale.
.. 99
-------
Precision:
Noise:
Interference:
Operating Temperature Range:
Operating Humidity Range:
The degree c^f agreement betv.een
repeated measurements of the
same concentration, .expressed
as the average deviation of
the single results from the
mean.
Spontaneous deviations from a
.mean output not caused by in-
... put concentration changes.
An undesired positive or nega-
tive output caused by a sub-
' ' stance other than the one _
being measured.
The range of ambient temperatures
over whfch the instrument v/ill
meet all performance specifica-
tions.
The range of ambient relative
humidity over v/hich the in-
strument will meet all perfor-
mance specifications.
. 100
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t^jc!j/;^^: Jlg^:j-laiLu3^;^^A^^jI'^
J
*
.
K
V.
i
ซ V
i
)
\
)
K
- f
' V
. 4SS*- V
T
Diluent
.'V
.-.>' : . J
'.. i .
Positive
DispL-J
cement
V (150 dc/min)
>. 3 - Wdy
^ Valvcj
v -.
Air
i
c
'*
1
<
v
f-
t
1 n i
1
0 ป 0 0
i
25
V
Clean
Dry Air
j
Dilution Box Heated
jmp . 1 ::
lted) ป To 100'C
Vent
FIGURE 14-1. SAMPLING AND DILUTION APPARATUS.
: " . >
.i
1350 cc/niti.
Flowrceteis
-------
-*uiJ*ij,l. v>xi~;!.t; '!;!'. ^*'l;!.^:^^ฃปVAw:X'^^'\^J^l^y.X>*^^Vl^-l^JX^l-ซ'*'C^!^l^*v^.^o^^/3fc'li*ป.lBV^.jfa^il^x>J^^
.: * .;
Stripper
ฃฃULfi_
Vent
Sample
-I or'
'; Calibration
Sampling Valve for
viC/T?D-iI
Separation
Column .
H,
Oven
Flame Photometric Detector
750V
Power Supply
To GC/FPD-II
FIGURE 14-2. GAS CHROMATOGRAPHIC-FLAKE PHOTOMETRIC ANALYZERS
-------
V I
O
CO
To Instruments
and
Dilution System
Thermometer
XI
Flowneter
Drier
' Diluent
jU
Stirrer
Constant
Temperature
Bath
Permeation
Tube
Glass
Chamber
or
Nitrogen
FIGURE 14-3. APPARATUS FOR FIELD CALIBRATION
.~J
t ,
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