EPA REPORT NUMBER 74-KPM-5
CD
O
POLLUTIO
EMISSION TEST
to*
CHAMPION INTERNATIONAL
COURTLAND, ALABAMA
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
-------
TABLE OF CONTENTS
Page
I. INTRODUCTION 1
II. SUMMARY OF RESULTS 3
III. PROCESS DESCRIPTION AND OPERATION , 41
IV. LOCATION OF SAMPLING POINTS 79
V. SAMPLING AND ANALYTICAL PROCEDURES 86
APPENDIX
A. PARTICULATE RESULTS AND EXAMPLE CALCULATION
B. GASEOUS RESULTS AND EXAMPLE CALCULATIONS
C. OPERATING RESULTS -
D. FIELD DATA
E. SAMPLING METHODS
F. LABORATORY REPORT
G. TEST LOG
H. RELATED REPORTS
I. PROJECT PARTICIPANTS AND TITLES
-------
I. INTRODUCTION
Under the Clean Air Act of 1970, as amended, the Environmental
Protection Agency is charged with the establishment of performance
standards for 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 must be gathered from the stationary source category
under consideration.
Champion International in Courtland, Alabama was selected for emission
testing to obtain data for the development of performance standards for
new kraft pulp mills. The tests were conducted during the period of October 29
to November 5, 1973.
The processes under investigation in this test series were the smelt-
dissolving tank, the lime kiln, and recovery furnace. Emissions from the
smelt-dissolving tank are controlled by a wet fan scrubber. Emissions from
the lime kiln are controlled by a variable disk venturi scrubber followed
by a cyclone separator demister. Emissions from the recovery furnace are
controlled by an electrostatic precipitator. A schematic diagram of the
simplified kraft process and the processes sampled is shown in Figure 1.
-------
tVJ
GREEN
LIQUOR
RECOVERY
FURNACE
GAS. FLOW
LIQUOR FLOW
DIRECT
CONTACT
EVAPORATOR
.....
BLACK
LIQUOR
SMELT-
DISSOLVING
TANK
WET FAN
SCRUBBER
FUEL
RECOVERY FURNACE
TEST SITE
PRECIPITATOR
STACK
VENTURI
SMELT-DISSOLVING
:TANK TEST SITE
LIME KILN
TEST SITE
1
CYCLONIC
SEPARATOR
DEMISTER
STACK
STACK
'Figurel. Schematic diagram of simplified Kraft Process
and processes sampled. '
-------
Three runs were conducted in the exit stack of the recovery
furnace to determine filterable and total particulate emissions.
Simultaneous determination of moisture content and dry molecular
weight were made of the flue gases.
Three runs were also conducted in the exit stack of the
smelt-dissolving tank to determine filterable and total particu-
late emissions in conjunction with the determination of total
reduced sulfur. Simultaneous determinations were again made of
moisture content and dry molecular weight of the flue gas.
The last three runs were conducted on the exit stack of the
.lime kiln to determine filterable and total particulate emissions
simultaneously with the determination of total reduced sulfur.
In addition to the normal moisture content and dry molecular
weight determinations, grab samples were taken for NO measurements.
.4 X
II. - SUMMARY OF RESULTS
Recovery Furnace
A summary of particulate emission data from the recovery
furnace is presented in Table 1. Table 4 presents a summary of
flue gas conditions for all tests. The filterable particulate as
measured by the probe.and filter catch averaged 19.9 pounds per
hour at a concentration of 0.027 grains per DSCF. Tests 11-1 and
11-2 agree fairly well. However, test 11-3 yielded a lower value
for the filterable particulate, indicating the possibility of a
leak around the filter.
The total particulate results agree fairly well and averaged
31.7 pounds per hour. The slightly high percent isokinetic sampling
rate on Test 11-1 did not apparently effect the final result
significantly.
-------
Table 1. SUMMARY OF PARTICULATE RESULTS
Run Number
.RECOVERY.FURNACE .
1,1-1
Date , 1973
Volume of Gas Sampled - DSCFa
Percent Moisture by Volume
Average Stack Temperature - ฐF
Stack Volumetric Flow Rate - DSCFM1
Stack Volumetric Flow Rate - ACFMC
Percent Isokinetic
Percent Excess Air
Percent Opacity
Feed Rate - ton/hr
Pairticulates - probe,
and filter catch
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
Particulates - total catch
rog
gr/DSCF -
gr/ACF
Ib/hr
Ib/ton feed
Percent impinger catch
11-2
11-3
11-1
113.236
30.3
321
85115
122080
117.2
226.3
0.0308
0.0143
22.50
303.5
0.0414
0.0191
30.18
11-1
106.025
31.5
310
90978
132839
102.7
198.8
0.0289
0.0134
22.56
310.8
9.0452
0.0209
35.28
11-2
93.b73
33.6
304
80268
120977
102.7
129.1
0.0213
0.0096
14.65
261.3
0.0431
0.0195
29.65
25.4
36.0
50.6
Dry standard cubic feet at 70ฐF, 29.92 in. Ilg.
Dry standard cubic feet per minute at 70ฐF, 29.92 in. Hg.
Actual cubic feet per minute.
-------
Smelt-Dissolving Tank
A summary of particulate emission data from the smelt-
dissolving tank is presented in Table 2. The particulate results
for the front half averaged 3.65 pounds per hour at a concentration
of 0.0454 grains per DSCF.
Test 22-3 had a low moisture percentage and a low particulate
n '
catch. This indicates that the sampling train was leaking during
the test run, or that some process operating condition changed.
The sampling train was leak checked before the run, and the
field data do not show evidence of a leak.
Lime KiIn
A summary of particulate emission data from the lime kiln
is presented in Table 3. The particulate results for the front
half averaged 12.38 pounds per hour at a concentration of 0.10
grains per DSCF. However, this average was largely influenced
by Test 33-3 which had about twice the front half catch as
compared to the other two runs. The high catch could have been
caused by a foreign particle from the particulate caked on the
inside of the stack. In any case, Test 33-3 does not appear
typical when compared to the other two runs. The average emission
rates for runs 1 and 2 were 8.84 pounds per hour for the filterable
particulate, and 9.73 pounds per hour for total particulate.
Nitrogen oxide concentrations, are shown in Table 4, and
averaged 240 ppm by value, 211 ppm, and 102 ppm on three separate
days. .
All tests for reduced sulfuir compounds were conducted by
QAP. personnel. .
-------
Reduced Sulfur Results
A summary of the reduced sulfur emission data is presented in
Table 5. This summary includes daily total reduced sulfur average
concentrations for both the smelt tank vent and the lime kiln. Tabel 6
summarizes the daily average TRS concentrations for each compound
separately. The Tables are followed by the field gas chromatograph
data used to obtain the daily averages. A detailed sampling and'
analytical method is included in Chapter V of thisrreport.
-------
Table 2. SUMMARY OF PARTICIPATE RESULTS
SMELT-TANK
Run Number
Date 1973
Volume of Gas Sampled - DSCFa
Percent Moisture by Volume
Average Stack Temperature - ฐF
Stack Volumetric Flow Rate - DSCFM
Stack Volumetric Flow Rate - ACFMฐ
Percent Isokinetic
Percent Excess Air
Percent Opacity
Feed Rate - ton/hr
Particulatos - probe,
and filter catch
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
Particulates - total catch
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
Percent impinger catch
22-1
11-1
59.785
41.2
172
8880
15109
107.4
223.3
0.0576
0.0278
4.39
.349.3
0.0902
0.0435
6.86
22-2
11-2
59.710
41.0
172
9339
15822
102.0
198.2
0.0512
0.0250
4.10
255.6
0.0661
0.0321
5.29
22-3
11-2
59.971
33.2 .
170
10787
10546
90.7
105.9
0.0273
0.0151
2.46
142.2
0.0366
0.0202
3.31
36.1
22.5
25.5
Dry standard cubic feet at 70ฐF, 29.92 in. Hg.
Dry standard cubic feet per minute at 70ฐF/ 29.92 in. Hg,
Actual cubic feet per minute.
-------
Table 3. SUMMARY OF PARTICULATE RESULTS
LIME KILN
Run Number
Date , 1973
Volume of Gas Sampled - DSCFa
Percent Moisture by Volume
Average Stack Temperature - ฐF
Stack Volumetric Flow Rate - DSCFM1
Stack Volumetric Flow Rate - ACFMC
Percent Isokinetic
Percent Excess Air
Percent Opacity
Feed Rate - ton/hr
Particulates - probe,
and filter catch
mg.
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
Particulates - total catch
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
Percent impinger catch
33-1'
11-3
55.674
40.0
168
13555
22599
96.2
224.9
0.0623
0.0311
7.24
251.8
0.698
0.348
8.11
33-2
11-5
57.894
38.1
164
14011
22638
36.8
326.1
0.0869
0.0451
10.44
354.5
0.0945
0-.0490
11.35
33-3
11-5
58.725
36.5
163
15114
23803
91.1
572.0
0.150
0.0798
19.47
602.3
0.158
0.0841
20.51
10.7
8.0
5.0
Dry standard cubic feet at 70ฐF, 29.92 in. Hg.
Dry standard cubic feet per minute at 70ฐF, 29.92 in. Hg.
ฃ
Actual cubic feet per minute.
d As determined from psychrometric chart at saturated conditions
8
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Table 4. SUMMARY OF GAS TEST DATA
- Source RF RF RF ST- ST ST ST . LK LK LK LK LK
LK
Run
Number
Date
Time
24 hour
% H-0
by Vol.
% co2
%o2
% CO
N0x ppma
dry
11-1
11/1/73
1210
1548
30.3
8.7
9.8
0
11-2 "
11/1/73
1803
2145
31.5
9.9
10.6
0
11-3
11/2/73
1055
1542
33.6
10.2
10.6
0
22
10/31/73
1430
1830
37.0
1
0.1
20.4 .
0
".
22-1
11/1/73
1400
1727
41.2
o.i1
19.4
0
"
22-2
11/2/73
0930
1202
41.0
0.1
20.4
0
"""
1 22-3
11/2/73
1320
1545
33.2
0.1
20.7
0
33-1
11/3/73
1450
1712
40.0
10.7 '
8.0
0
"
33-2
11/5/73
' 0950
1313
38.1
10.3
9.6
0
33-3
11/5/73
1347
1605
36.5
10.3
. 9-6
0
11/7/73
0830
1230
37.2
10.4
9.8
0
237
242
11/7/73
1530
1820
32.4
10. D
10.1
0
11/8/73
0940 .
1340
33.0
10.1
12.5
0
215
207
11/8/7
1340
1640
36.1
10.4
13.:'
0
60
144
a)Expressed as NO-
-------
TABLE 5
SUMMARY. OF RESULTS
Court!and, Alabama
Daily Average TRS
Daily Average SO,
Date
10-31-73
11-1-73
11-2-73
11-5-73
11-7-73
11-7-73
11-7-73
11-8-73
11-8-73
Location
Smelt Tank
Smelt Tank
Smelt Tank
Lime Kiln
Lime Kiln
Lime Kiln
Lime Kiln
Lime Kiln
Lime kiln
ppm/dry
7.64
7^42
5.96
3.85
24.09
2.80
5.68
4.64
17.76
Ib/hr
0.58
0.49
0.44
0.33
1.85
0.23
0.45
0.37
1.36
Ib/ADTPD
2.26 x 10"2
1.90 x 10"2
1.73 x 10"2
1.29 x 10"2
7.25 x 10"2
9.02 x 10"3
1.76 x 10"2
1.46 x 10"2
5.34 x 10"2
ppm/dry
<0.44
<0.30
0.76
<0.31
0.54
0.89
<0.25
0.96
<0.24
Ib/hr
<0.04
<0.03
0.08
<0.04 i
0.08
0.13
<0.04
0.14
<0.03
Ib/ADTPD
<1.57 x 10"3
<1.06 x 10"3
3.14 x 10"3
<1.57 x 10"3
3.14 x 10"3
5.10 x 10"3
<1.57 x 10"3
5.49 x 10"3
<1.18 x 10"3
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TABLE 6
SUMMARY OF DAILY AVERAGES OF COMPOSITE ODORANTS
Courtland, Alabama
Lime Kiln
Date Compound
Daily Average
(ppm, wet)
Daily Average
(ppm, dry)
Daily Average
(Ibs/hr)
Daily Average
(Ibs/ADTPD)
11-5-73
11-7-73'
(1st)
11-7-73
(2nd)
11-7-73
(3rd)
11-8-73
(1st)
11-8-73
(2nd)
H9S
2
CH-SH
3
SO,
2
DMDS
H9S
2
CH0SH
3
SO,
2
DMDS
H7S
2
CH-SH
3
S00
2
DMDS
H2S
CH.SH
3
S00
2
DMDS
HซS
2
CHgSH
SO,
2
DMDS
H,S
2
CH.SH
3
S00
2
DMDS
2.01
<.39
<.20
0.05
15.08
0.60
0.35
<.025
1.49
<.30
0.58
0.03
3.37
<.30
<.16
<.03
2.70
<.30
0.63
0.04
11.27
0.32
<.16
<.03
3.16
<.61
<.31
0.08
23.13
0.92
0.54
<.038
2.29
<.46
0.89
0.05
5.17
<.46
<.25
0.05
4.12
<.46
0.96
0.06
17.23
0.49
<.24
<.04
.24
<.07
<.04
0.02
1.74
0.10
0.08
<.01
0.17
<.05
0.13
0.01
0.39
<.05
<.04
0.01
0.31
<.05
0.14
0.01
1.30
0.05
<.03
<.01
9.41 x 10"3
<2.75 x 10"3.
<1.57 x 10"3
7.84 x 10"4
6.82 x 10~2
3.92 x 10"3
3.14 x 10"3
<3.92 x 10"4
6.67 x 10"3
<1.96 x 10"3
5.10 x 10"3
3.92 x 10"4
f\
1.53 x 10"^
<1.96 x 10"3
<1.57 x 10"3
3.92 x 10"4
1.22 x 10"2
<1.96 x 10"3
5.49 x 10"3
3.92 x 10"4
5.10 x 10"2
1.96 x 10"3 '
<1.18 x 10"3
<3.92 x 10"4
11
-------
TABLE 6 .
(continued)
Smelt Dissolving Tank Vent
Daily Average Daily Average Daily Average Daily Average
Date
10-31-73
11-1-73
11-2-73
Compound^
HS
CH3SH
so2
DMDS
H S
CH.SH
3
SO,
2
DMDS
H,S
2
CH,SH
3
SO,
2
DMDS
(ppm, wet)
0.66
3.80
<.28
0.35
1.11
3.81
0.27
0.99
2.80
0.51
0.23
(ppm, dry)
1.05
6.03
<.44
0.56
1.59
5.44
<.30
0.39
1.47
4.15
0.76
0.34
(Ibs/hr)
0.055
0.44
<.04
0.08
0.075
0.36
<0.027
0.051
0.08
0.31
0.08
0.05
(Ibs/ADTPD)
2.16 x 10"3
1.73 x 10"2
<1.57 x 10"3
3.14 x 10"3
2.94 x 10"3 -
1.41 x 10"2
<1.06 x 10"3
2.00 x 10"3
3.14 x 10"3
1.22 x 10"2
3.14 x 10"3
1.96 x 10"3
12
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CHAMPION PAPER COMPANY
Court!and, Alabama
Smelt Tank
Inject
Date Time Compound
10-31-73 1325 H2S
so2
CH3SH
(CH3)2S2
1340 H2S
so2
CH,SH
0
x /ru \ c
\v*no / o^o
1355 H2S
so2
,- CH^SH
CO J
(CH3)2S2 .
1410 H2S
so2 .
CH,SH
0
t ru \ c
\vrio/o^9
1425 H2S
so2
CH3SH
(CH3)2S2
Attenuation
(Amps)
4 x 10"7
4 x 10'8
4 ^ 10"7
4 x 10"8
4 x. 10"8
"
.n
4 K 10"7
4 x 10"8
"
"
4 x. 10"7
4 x 10"8
n
n
4 x 10"7
4 x 10"8
"
"
n
Peak
Height (%)
30.2
1.0
20.9
14.8
3.0
63.0
. 50.0
i.o . :
34.8
30.1
3.5
42.5
39.9
2.1
30.0
81.4 '
Concentration
(ppm, wet)
.37
.025
.54
.0082
.04
'.
.31
.062 '
.02
.24
.047
.04
;27
.056
.03
.22
.022
Dilution Corrected Concentration TRS
Factor (ppm, wet)
11.4 3.46
.29
" .6-16
" , .093
11.4 0.37
ซ
3.53
.730
11.4 0.19
II _
" 2.74
.536
11.4 0.37
.
3.08
.638
11.4 0.28
n ____
" 2.51
.251
{ppm, wet)
"9:/i
4.63
3.47
4.09
3.04
-------
Date
Time
10-31-73
(continued) 1440
1455
1510
1525
1540
1555
Compound
(Amps)
Heiqht (%)
(ppm, wet)
Factor
Co ed
(ppm, wet)
H2S
so2
CH3SH
(CH3)2S2
H2S
so2
CH3SH
(CH3)2S2
H2S
SO,
CH3SH
(CH3)2S2
K2S
so2
', CH3SH
(CH3)2S2
H2S '
so2
CH3SH
(CH3)2S2
H2S
S0?
. ฃ
! CH3SH
(CH3)2S2
_o
4 x 10 a 6.1
"
" 53.9
72.0 .
. 4 x 10"8 5.8
"
42.2
4 x.10"7 26.9
-ft
4 x 10 B 9.1
n ____
" . 39.2
4 x 10"7 .30.1
4 x 10"8 14.2.
II
58.0
76.9
4 x 10"8 23.5
" .
91.9
90.1
4 x 10"8 15.9
II
" 82-7
90.0
.06
.30
.021
.06
.28
.042
.07
.
.25
.048
.09
.31
.021
H
,
.37
.024
.09
.35
.023
,
11.4 0.56 .
n ....
3.42
.239
11.4 0.56
n ____
3.19
.479
'
. 11.4 0.65
, ....
2.85
.547
11.4 0.84
" .
3.53
.239 '
11.4 1.03
"' ' . ;
" 4.22
" .274
11.4 0.84
; ป
11 4.00
.262
(ppm, wet)
4.22
V.23
4.05
4.61
5.52
5.10
r
-------
Date
Time
10-31-73
(continued) 1610'
1625
1640
1655
1710
1725
pom, wet)
actor
, w
\ซ WHI^S V W 1 1\4 V ป">** 1
H2S - 4 x 10~8'
*ฐ2
M3$H "
(M3)2S2
H2S . 4 x 10"8
2
W3$H
/rij \ C II .
\Lปr1o /o^o ;
j t. C \ 1 1
H2S 4 x 10~8
so2
CH3SH "
(CH3)2S2 . "
_Q
H2S 4 x 10 B
so2
CH3SH 32 x 10"8
DMDS . 4 x 10"8
(CH3)2S2 4 x 10"8
H2S 4 x 10"8
so2
CH3SH "
DMDS "
H2S 4 x 10"8
so2
CH3SH "
DMDS "
36.2,
84.0
73.3,
34.0
70.2
59. 0(
9.0
43.6
45.8
12.6
....
64.2
3.1
66.7
5.9
66.9
94.3
6.0
. /
90.1
81.7
V nปf*tปi f * ป i
.13
.35.
.021i
.13
.33
.018,
1 ' 1
.07
.26
.016
.08
....
.81
tm ป
0.20
,06
.32
.024
.06
.
.37
.022
11.4 1,22,.
5.46
4.00'
.239,
11.4, 1.22,
"5V18
.."'.'. 3.76,
" . .205
' 11.4 0.65
. . i > ,
- . 3.79
" 2.96 '
.182
11.4 0.75
-' 10.21
" 9.23
" _, . s
. " .228 - '
11.4 6.56
* 4.48
3.65
.274
11.4 0.56
5.03
" 4.22
.251
-------
InJVBV '
Date . . Time Compound
11-1-73 1220 H2S
so2
CH3SH
(CH3)2S2
1235 H2S
so2
CH3SH
(CH3)2S2
1250 H2S
so2
CH3SH
(CH3)2S2.
1305 H2S
so2
CH,SH
' 3
<ป . (CH3)2S2
1320 H2S
so2
CH3SH
DMS
DMDS
AOTiatiMi
(Amps)
4 x 10"8
"
"
"
4 x 10"8
n
"
"
4 x 10"8
"
II
"
4 x 10"8
"
"
4 x 10"7
4 x'10"8
n
4 x 10"7
4 x 10"8
4 x 10"8
1
Height (%)
16.2
1.5
68.9
18.0 ;
6.0
20.5
35.5
11.4
21.2
41.3
39.6
34.2
40.5
29.2
33.4
3.0
37.1
kenMBon
(ppm, wet)
0.06
0.014
0.27
0.009
0.035
0.15
0.014
0.05
0.15
0.015
0.10
0.19 '
0.056
0.084
-___ ' .
0.56
ซ. <
0.014
DM on WortW CcMtra^
Factor (ppm, wet)
16.1 ' 0.79
" 0.23
" 4.35
0.15
16.1 0.46
"
" 2.42
0.23
16.1 . 0.66
H
2.42
0.24
16.1 1.29
"
" 3.06
" 0.90
16.1 1.11
ปซ _ ซ
" ' ' 9.02
n . ____
0.23
(ppm. wet)
5.29
3.32
5.25
10.35
\\
-------
Date
11-1-74
(continued)
^i
InjeTT
Time
1335
1350 .
1405
1420
1450
1505
1520
Compound
H2S
so2
CH3SH
DMDS
H S
CH3SH
DMDS
H2S
CH3SH
DMDS
H2S
CH3SH '
DMDS
H2S
CH3SH
DMDS '
H S
. CH3SH
DMDS
H S
CH3SH
DMDS
O w^^^^^xl Ul Q^r r^^^^^
(Amps) Height (55)
. 4 x 10"8 58.0
1.5
54.8
" 34.0
. 4 x 10"8 48.9
51.4
25.3
4 x 10"8 15.8
48.0
35.0 ' ' ,
4 x 10~&" "36.5
54.0
45.0
4 x 10"8 61.0
47.9 '
64.5
4 x 10"8 45.8
42.9.
11 45.5
4 x 10"8 30.5
" 30.9
47.9
lentflBm
(ppm, wet)
0.12
0.017
0.25
.13
0.11
0.23
0.011
0.060
0.22
0.014
0.094
0.24
0.016
0.12
0.22
0.012
0.0104
0.21
0.016
0.085
0.18
0.016
DiMง)n 0ฐrr
Factor
16.1
"
ii
"
16.1
II
II
16.1
II
II
16.1
II
II
16.1
tl
tl
16.1
II
II .
16.1
".'
H
'SB! HeW*1* *
1.58 .
0.27
4.02
0.21
1.45
3.70
0.18 ,
0.79
' 3.54
0.23
1.24
3.86
0.26
1.58
3:54
0.31
0.13
3,38
0,26
1.12
2.90
0.26
(ppi^lt)
5.81
'5.33
4.55
5'.36
5.43
3.77
4.28
-------
Date
11-1-73
(continued) 1535
CO
njt>B|'
Time
1535
1550
1605
. " i
1620
!,, ,1
i -, ' (
|1. 't.
Compound
H2S
CH3SH
DMDS
CH3SH
DMDS
H?S
CH3SH.
DMDS
CH3SH
DMDS ',
Ml.
,
'.Ii ' ii
- i.l.i...
. . ., ,1 '.,!
' l
' I
'
AtMtioM PiH
(Amps) Height (%)
4 x 10"8 66.2
43.8
38,8,
4 x 10"8 49.5
. , " , ' 45.7,
52r9,
4 x 10"8 67'.9>
" '' fi7 ?
4 x 10"8 14.1 '
., '" p. :| 47,0,.
'i!. 11
1 |H ' . I,|M
' ' .-I .. )
: ,,) V ' " " '..
1 ' ' v I. '1 . '
' I1- '' '
.' ill1 '.( ' '
(pptn, wet)
0.13
0.22
0.014
0.11
0.221
0.017
. .o.'is"
0.26 ,
0-011
.056' '
0.22 , ,
0..014
. 1! Hi*
1 , i t'
1 i /
Ii III/
> I . , | , 1 1
' ' .1.1"'
II ii!.!
1) H|l,
. '
Factor (ppm
16.1 ' l.
3.
0.
16.1 ' 1.
.".. 1 3'.
" . o.
16.1 1.
''. i . ' 4.
0.
16J , . 0.
'iV i 3:
0.
Ii, i 1
i' 1 I
;
1 ' ' l , . 1 . ' 1
' ' '
, wet^^ ippm, wet)
72 .
54
23 |
45' . ' ;
54 5.26 ' !|
27" . '""/1 .'j!
721' ' if
19- 6.09 ;r
18i . ' ' ;i
' t.
74 ,j
54- 4.50
23,. '. ..-' ,,j
::" " :j
.,1 ,' j
/ . , ป
1 . ' \\
*
,, , ; ; t
'.
' - 'Ii
"' ....-!..,. ;'f
. i
'"" -.' ' , ;{
\,
\
i
-------
Date
11-2-73
(continued)
Time
1115
1130
1145
1200
1215
1230
Compound
SO,
CH3SH
DMDS
so2
CH3SH
DMDS
H2S
so2
CH3SH
DMDS '
H2S
so2
CH3SH
DMDS
so2
CH3SH
DMDS
so2
CH3SH
DMDS
(Amps) i,
4 x 10"8 ,
.1
I)
II
. 8 x 10"8
. 4 x 10~8
8 x 10"8
4 x 10"8
II
4 x 10"8
"
" ....
"
4 x 10'8
"
II
"
4 x 10"8
n
H
"
4 x 10"8
"
"
,i
Pe^B C
HeignTTs)
23.9
92.1
54.2
52.1
45.2
55.9
66.3 . ,
33.9
29.4
44.9 ' -
-32.8
38.9
21.9
9.0
34.0
32.6
19.7
3.6
38.3
, 39.2
8.5
1.8
27.9
43.7
ft*UwSP
0.076
0.15
0.22
0.025
0.11
0.17
0.24
0.013
0.085
0.11 '
0.17
0.014
0.073
0.046
0.17
0.013
0.070
0.029
0.18
0.014
0.045
0.020 :
0.16
0.015
D1 li^b^ufl Cttrr&c^ftfi^^'OncAfi^Ctkt1 O^L
FaCTor ^^ (p|^^^/et)^^^
13.0 0.81
1.95
2.86
: " 0.33
13.0 1.17
2.21
:.... " . 3.12
0.17
13.0 . ' 0.91
1 " 1.69
2.21
11 0.18
13.0 0.78
" 0.60
2.21
11 o-1?
13.0 0.75
11 0.38
11 ' 2.34
0.18
13.0 0.48
"' 0.26
2.08
0.20
3.29
'4.46
4.99
.3.16
3.27
2.76
\'
-------
Date
11-2-73
(continued)
,ป
;
^L
'% -*
t
ro
o
Time
1245
\
1300 !.
1
!
i
1315
1330
1345
1400
V
Compound
H2S
S07
CH3SH
DMDS
H S
so2
'CH3SH
DMDS
H2S
so
'CH3SH
DMDS '
H2S
so2
'CK-SH
DMDS
H2S
so2
'CH3SH
DMDS
H2S "
so2-
'CH3SH
DMDS *
(Amps)
'
4 x 10"8
n
n
n
4 x 10'8.
"
"
n
4 x 10"8
n
"
"
8 x 10"8
4 x 10"8
n
8 x 10"8
4 x 10"8
"
"
"
4 x 10"8
"
it
"
Height (%)
i
21.3
35.9
46.7
11.3
1.0
37.2
100.0
t
8.0
^
42.9
%44.2
49.2
3.5
74.0
56.9
49.5
1.9
63.0
, 23.7
64.8
2.1
76.2 '
62.0
(ppm, wet)
0.072
0.18
0.016
0.052
0.015
0.18
0.25
0.044
0.20
0.015
0.16
0.028
0.25
0.027
. 0.11
0.021
0.23
0.011
.13
0.022
0.25 '
' 0.019
racror uJpmT we^^^ ^^* (pp^^?et) '
i !
I
13.0 0.77 . | '
II ' 0 00 '
---" O,OL
2.34
" - 0.21
13.0 '
;
"... ' ' --/ ' \
. , ' J
i
;
13.0 ' 0.47 . . [
" _- 1 97
---- _ i,CI
2.60
13.0 1.71 5.31 -
0.36
' 3.25 ' ;
0.35 , :
, -;
13.0 1.17 ' '
0.27 4.30
2.99 r:
I
0.14 {!
13.0 ; 1.39 ' |
. 0.29 -4.89' !
i
3.25. ;'|
0.25
"JL^.
-------
In.jgf'
Date Time
11-2-73
(continued) 1415
1430 .
1445
<.
1500
tv>
''
1515
Compound
H2S
so2
c.
CHgSH
DMDS
H2S
en
2
CH3SH
DMDS
H2S '
so2
CH3SH
DMDS' :
H2S
so2
CH3SH
DMDS .
H2S
SO
+i\J f\
CH3SH
DMDS
AJfff;^ซi HeWLttl
Q
4 x 10"ฐ 25.7
1.0
8 x 10"8 64.9
4 x 10"8 40.0 ..
. 4 x 10"8 32.9
n
53.3
57.5
4 x 10"8 90.3
" '
" 88.9
" 41.7
4 x 10"8 35.8
42.1
" .1 ' 36.0
>4 x 10~8 33.4
"
39.0
, 33.6
tffl^lHJ0"
0.080
0.015
0.33
'. 0.015
0.091
0.22
o.ois ; .
0.15
.
0.27
0.015
0.096
'0.19
' 0.014
0.091
0.19
0.013
DM?n CorrW! S
13.0 ฐ 0.85
" 0.20
" 4.29
11 - . 0.20
;13.0 0.97
n ____
' O
'" 2.86
" . 0.23
13.0 ' ' 1.60
n ____
3.51
0.20
.13.0 1.02
2.47
. 0.18
.13.0 0.97
H
2.47
0.17
qj^^tra^a^ JtR^
'^^* ^^ (p^^v
et)
e;n
"4-^6
5.30
3.67
3.61
-------
GASEOUS SULFUR EMISSION DATA AND RESULTS
Champion Paper Company
Court!and, Alabama
Lime Kiln
Inject
Date Time
11-5-73 1035
1050
1105
K 112ฐ
'
1135
1235
Attenuation
Compound
H2S
so2
CH3SH
. H2S
so2
CH3SH
DMDS
H2S
CH3SH
DMDS
H2S
CH3SH
DMDS
H S
CH3SH
DMDS
H S
CH3SH
DMDS
Peak
(Amps) Height (%)
4
4
4
4
4
8
8
. 4
x 10"7
x 10'8
"
x 10"8
11
n
M
x 10'8
"
"
x 10"8
"
"
x 10"8
n
"
x 10"8
x 10"8
II
26
5
4
54
1
4
70
1
5
87
1
5
71
1
' 4
93
1
1
.2
.5
.2
.6
.8
.0
.2
.9
.0
.0
.2
.0
.7
.7
.5
.7
.0
.3
.5
Concentration
(ppm
0.
0.
0-
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
, wet)
27
04
06
12
--
03 '
004
13
03
004
15
03
005
19 .
04
004
23
03
002
Dilution
Factor
13.3
II
II
13.3
II
II
II
13.3
n
n
13.3
"
, n
13.3
"
"
13.3
"
n
Corrected Concentration
(ppm,
2.
0.
0.
1.
0.
0.
1.
0.
0.
1.
0.
0.
2.
0.
0.
2.
0.
0.
wet)
94
53
80
31
--
40
06
42
40
06
64
40
06
05
53
06
51
40
03
TRS
(ppm, wet)
-/
3.74
1.76
1.87
2.10
2.63
2.94
-------
InjHI
Date Time
11-5-73
(continued) 1250
1305 i
1
j:
1
1320 /
,.ป
4k. 1335
1350
t\>
co
1405
1420
1435
Compound
H2S
CH3SH
DMDS
H2S
CH3SH
DMDS
H si
CH3SH
DMDS
H2S .
CH3SH.
DMDS :
H2S
CH3SH
DMDS
H2S
' DMDS
. H2S
DMDS
H S
CH3SH
DMDS
AMfcatifll
(Amps)
8 x 10"8
4 x 10"8 ''
" :
8 x 10"8
. 4 x 10"8,
"
8 x 10"8
4 x 10"8
"
4 x 10"8
"
H
8 x 10"8
4 x 10"8
n
8 x 10"8
4 x 10"8
4 x 10" -
"
8 x 10"8
4 x 10"8
n
' .' " l;/^''^r-*'
' HeigH\\^':v,V'J"
^L, J . .ซd,}flj.,J >. . ;:;;.._,
: '> ^^''jl'yl^'1^
"^VE^/'V ^l;,v';
J J ' 1 "* T" ."' 'l'V" ,S ' '?.';r -'''' I1 --'
> 3* , ' ' i ,v ,i- \- ' .,
1 'l 1 i'l' 'ป t' "'' ''" ,'":1 ''' ' - - i1
' !-',64^';' ;^ง:.4;,;r':;
"'ฅl..o':'il|f ';7
'.' 4;ฐ, fe^i3%i
' '5i.o;^i!t8!
'-."rl.o- 'r^;^|^
4.5 '.' ; /' '
88.2 '
1.0
4.0
50.8
0.8
3.8
54.0
3.9
97.6
2.2
60.0
0.5 '
1.6
MK'--nBB
"i -.~?p|':v' wet
'.'..I -V: ' ','!'"'. ^.!'
|dJ; 0.18 .}"
;;4|^0.04 ^
^^.p'.obs/v
^lj'ib.18'1!?-1-'
il^:o.o3 ?;:
^V'o.oo4v';-
vJ!v 0.16 " -
' '.:"! o.:03 '
1:' ' 0.004
0.15
0.03
. 0.004
0.16
0.004
0.16
0.004
0.16
. 0.003
0.18
0.002
on '''''''.''' DMMpon po
. ' ';':'^^'>, Factor
. '..'.' !$'.';',,"' !. . '
', ";'.'-'- :/'i "*,'. TOO
' '' !'"i ''','' U.O
.''.v;-!'j'' :,v:^ ''./.. .;'u
; !'i;lv'-'?:',1'.:':f-;'|:'i /""
'. i1 ' ]'''; 'ii'1'- 13.3
^ .--.;i ;:;'.::
''': ''; \; ''';' " n
/|;|i":!:-;-'':' " ' .. .- '
^;f ,,,,....: .-,..^- 13>3. .._, . .
; '" ''.,''. ' : :.
n
13.3
. ' "
M
13.3
n
11
13.3
u
13.3
n
13.3
n
u
rJM|ซi CqMMtra^^n M^
\pprn, wo^) ^^^ ippm^v/et)
1.96 .
0.53 2.53
0.05
1.96
0.40 2.41
0.05 """/
1.74 ;
0.40 2.19
0.06 '
1.64
0.40 2.09
0.05
1.74
1.79
0.05
1.74 ,
f
0,05 1.79
1.74
0^04 1.78
1.96
1.98
0.03
-------
Jate. ,
11-5-73
(continued) 1450
1505
1520
Compound
DMDS
'CH3SH
DMDS
H2S
DMDS
ps
4 x 10
8 x 10
4 x 10
-8
,-8
8 x 10
4 x 10
-8
-8
M
Heigh
Height (%}
OO *3 ' ' ' ; 'V-i"')'
oo.o ,'..'.,-;,:,"
<.><'::>ป :'"-:-i'
1 C :.'> '..-'"".' ""
1.0 ;, .;.. ,:t .:,.-..
ซซ. "$Sf
0.5 v-?;$;#;
'.'ป .. i
4,0 K' tv-^r
75.4 ' *>T1
4.8 : f v<
, wet)
0.15
0.002 '
0.18
0.004
0.20
0.048
13.3
13.3
13.3
it
rn. ve
1.64
0.03
1.96
0.05
2.18
0.64
7 wet)
1.67
2.01
2.24
ro
-------
CHAMPION PAPER COMPANY
Court!and, Alabama
Lime Kiln
Inject
Date ' Time
11 -7-7.3 940
955
1010
ro
01
1025
1040
1055
Compound
H2S
SO,
2
CH3SH
DMDS
H2S
so2
CH3SH
DMDS
H9S
Z
so2
CH3SH
DMDS
H2S
so2
CH3SH
H2S
so2
CH3SH
H2S
so2
CH3SH .
Attenuation
(Amps)
32 x 10"8
8 x 10"8
4 x 10"8
4 x 10"8
4 x 10"7
4 x 10"8
ii
ii
4 x 10"7
4 x 10"8
II
It
4 x 10"7
4 x 10"8
"
8 x 10"7
4 x 10"8
"
16 x 10"7
4 x 10'8
ii
Peak
Height (%) .
51.0
77.8
4.0
1.0
41.4
3.1
1.0
1.0
44^5
1.5
1.2
1.0
38.3
1.4
67.6
2.5 .
67.0
4.0
3.0
Concentration
(ppm, wet)
0.28
0.16
0.04
0.07
0.28
0.02
0.02
0.07
0.30
0.01
0.02
0.07
0.28
.
0.03
0.16
0.03
0.79
0.02
0.04
Dilution
Factor
14.5
n
H
n
14.5
II
II
II
14.5
n
n
n
14.5
n
n
14.5
"
"
14.5
n
II
Corrected Concentration
(ppm, wet)
3.33
2.32
0.58
0.10
3.33
0.29
0.29
0.10
3.57
0.14
0.29
0.96
3.33
0.44
1.90
0.44
9.39
0.29
0.58
TRS
(ppm, wet)
4.01
. /
-/
3.72
3.96
3.77
2.34
9.97
-------
Date
Time
11-7-73
(continued) 1110
. 1125
1140
1155
1210
en
1225
1240
Compound
H S
so2
CH3SH
H S
S02
CH3SH
H S
so2
CH3SH
H S
so2
CH3SH
H S
so2
, CH3SH
H S
so2
CH3SH
H2S
so2
CH3SH
*fl
. 4
4
4
. 4
4
4
'
4
4
4
4
4
4
16
4
(uat'Mi
imps)
x 10"6
x 10'8
n
x 10"6
x 10'8
n
x 10"6
x 10"8
"
x 10'6
x 10"8
"
x 10'6
x 10'8
II
x 10"6
x 10'8
II
~f\
x 10 6
xlO-8
"
Height (%)
33.0
4.4
3.8
63.0
6.0
4.9
78.2
7.0
5.0
67.9
. ""7.0
.5.0
73.0
7.0
5.0
73.4
7.5
5.0
47.0
8.0 .
^iDDm, wet) Tactor..
t
0.90 14.5
0.02
0.04 "
1.30 14.5
0.03 "
0.05 "
1.4 14.5
0.03 "
0.05
1.3 14.5
0.03
0.05 "
1.4 ' 14.5
; 0.03 " . "
0.05
1.4 14.5
0.03 "
1 0.05
'I
2.3 14.5
0.06
CorgMted Cfltt
^^, wW
(
10.70
0.29
0.58
15.46
. 0.44
0.72
16.65
0.44
0.72
15.46
0.44
0.72
16.65
0,44
0.72
16.65
0.44
6.72
't
27.35
0.87
1 ^^^ (l^jm^wet)
11.28
'16.18
'
17.37
. ' 16.18
17.37
t
17.37
.
28.22
-------
Date Time' Compound
11-7-73
(continued) 1.255 HgS
so2
CH3SH
1305 ' H,S
4
I CH3SH
1320 I H2S !
' so2
,ป CH3SH
4.^ 1525 H2S
so2 .
CH3SH
DMDS
1540 H2S
^j <;n
.. ' 5U2
CH^SH
. ซ3
DMDS
1555 H2S
. "2
CH3SH
(Amps)
8 x 10"6
4 x 10"8
"
16 -x 10"6
. 4 x 10"8
II
32 x 10"6
4 x TO"8
ii
4 x 10"7
4 x 10"8
" '
11
4 x 10"8
ii
M
"
4 x 10"8
11
"
1 : hceJPRlon
Height (%) (ppm, wet)
79.1
3.0
56.0
3.5
50.2
4.1
32.8
23.0
. 1-2
T.O
35.0
5.5
1.6
25.9
1.3
2.2
0.04
2.5
---
0.04
3.5
, .
0.05
0.25
0.59
.023
.0017
.074
.027
.0023 :
.062
.012
Factor
14.5
II
II
14.5
II
II
14.5
"
H
.14.5
M
M
"
14.5
ii
ii
. ti
' 14.5
11
"
CorMMbd CW^Ritra^^PP
(ppm, wet)
26.16
0.58
29.72
. 0.58
.41.62
0.72 .
2.98
8.56
0.33
.025
0.88
, 0.39
! '
. .033
0.74
0.17
*
Ippm, wet)
26.74
30.3
42.34
3.34
0.91
0.77
DMDS
1.2
.0019
.028
A'.. Va-
. f* '''. i?
-------
Date
Time
11-7-73
(continued) 1610
cป
162S
1640
1655
1710
1725
Compound
H2S
so2
CH3SH
.DMDS
H2$
so2
CH3SH
DMDS
H2S
so2
CH3SH
DMDS-
H2S
so2
CH,SH
/ j
DMDS
H2S
so2
C
CH3SH
DMDS
H2S '
SO,
2
, CH3SH
i DMDS
fltWfiuatTOT Peak
(Amos) Height (%) :
4 x 10"8 25.6
1.4
n ____
1.8
_n
4 x 10 B 31.5
" .8
" __
1.5
4 x 10~8 29.8
" i
n ____
" ' 1.4
4 x 10"8 '42.8
0.7 '
n ____
1.9
o
4 x 10'B 47.9
0.7
II '
1.8
4 x 10"8 43.4
n _.__
" ----
l.fi
Concentration
. (ppm, wet)
.062
.013
.0024
.069
.0022
.068
ซ ซ -.
.0021
.082
....
.0025
.088
..ซ.
.0024
.082
nw>
Dilution Corrected Concentration TRS '
Factor (ppm, wet) (ppm, wet) \:
i
. 14.5 " 0.74 f.
0.19 0.78 i
II
11 " .035
' t-
14.5 . 0.82
n .^
'0.85
ป , . j
' !
.032 . ('
14.5 - 0.81 ; :
H "if
0.84 ;j
" . .030 . .'.j
I , '
14.5 0.97
II %-.ป**
1.00
n __
.036 ' ;
t f k
'
14.5 1.05 ' . / '"
II 4 KM *
---- 1 08
1 UU <
" -
.035 1
14.5 0.97
" - 1.00
n '. i
___. .^
1 1
n
.033
-------
InjeM
Date Time Cqmgound
11-7-73
(continued) 1740 H2S
so2
. CH3SH
DMDS
1755 .H2S
so2
CH3SH
. DMDS
1810 H2S
so2
CH3SH
DMDS '
1825 H2S
so2
[Q CH3SH
DMDS
1840 H9S
c
so2
CH3SH
DMDS
1855 H2S
so2
jCH,SH
ซ3
:,DMDS
AttHitioflB PflH
(Amps) Height(%)
4 x 10"8 47.
II ___
II ^^^
1.
-ft
. 4 x 10 8 60.
"
11
2.
4 x 10"8 70.
"
n ___
" . 2-
4 x 10"8 99.
n ___
n ___
2.
4 x TO"7 66.
-ft
4 x 10 8
1 .
1 .
4 x 10"7 34.
4 x 10"8
0.
1.
1
-
-
9 .
2
-
-
8
2 '
-
-.
0
5
-
-
0
7
-
0
9
0
-
9
o
(ppm, wet)
.086
.0025
0.10
.0031
0.11
,
.0026
.0.13
.0026
0.37
.021.
.0025
0.26
' ' .'
. . .
' I .0025 '
DFM" ir'Ti*S';pi''atiiซ(ocTiwt>
!
- [
14.5- 1.02 . ;'
1.06
II
'
- .036 . ซ,'
- f
14.5 1.19 ;
V;- . ,
- i:23 i
1
.045
14.5 ' 1.31 ? \
" . 1 .#5
n ___ซ
.038 '
14.5 ' 1.55
-1.59 i
' ' :
"""""
" .038 '
/
14.5 4.40 ' '
i-
" . - 4-74 :
; 0.30 i
.036 ' i
. ' i
14.5 3.09 !
- ;''. !
" - ' 3.13
" ' ..r..036
If'
^
V-
-------
UU WC < ">** vwnifywviiivi
11-7-73
(continued) 1910 H,S
f.
so2
CH3$H
DMDS
1925 . H9S
s62
CH3SH
. DMDS
1940 H2S
so2
CH3SH
DMDS ' .
1955 hLS
L.
so2
co CH.SH
o J
DMDS
2010 H,S
C.
so2
CH3SH
' DMDS
\'
. 4
4
8
4
4
4
16
4
4
4
1 MI.K" /
x 10"7
_o
x 10 8
II
"
x 10"7
x 10"8
n
n
x 10"7
x 10"8
n . ...
"
x 10"7
o
x 10 8
n
ii
x 10"7
g
x 10 8
n .
n
1 1%. i *ii i * \ ซ* /
32.7
1.9
71.9
1.7
1.2
89.4
-1.5
1.4
67.8
1.0
51.8
1.0
' 1.4
0.25
.0025
0.57
. .028
.0019
0.44
.026
.0021
0.81
.0021
*
____
0.33
.021
.0021
* ' t
14.5 2.97 3.01
n ___
n ___,
.36
14.5 6.78
7. '22
. 0.41
. " .028
14.5 5.23 . .
. , - - . 5.64
" 0.38 .
" '.030 '
14.5 .9.63
n
ป .030 .9.66.
n ____ '
i
14.5 3.92 ,
4.25
0.30
.030
.,. . ป. . *. ซ-ซ-rป .
-------
Date ^me Compound
1-7-73
continued) 2025 H2S
so2
CH3SH
DMDS
,2040 . H2S
so2
CH3SH
DMDS
, 205, 5 H2S
SO,
CH3SH
DMDS '
2110 H2S
S02
/ CH3SH
DMDS
2125 H2S .
so2
CH3SH
, DMDS
*^|iH UHJ m
4 x 10"7 15.8
4 x 10'8 -
II
" . ,2.0 .
. 4x,10"7 J0,8
,4 x, 10"8
" ""
" . ,2.2
,4 x 10"8 46.2
4 x,10'7 ' -
r - - -.
,1,9 .
,4 x ,10"8 91.4
ป i. *
,0.8
2.0
4'x 10"8 73.7
"i "
. " r.,. '
,2.8
(ppm, wet)
0.17
.0026
,0.14
,.0027
,.086
. '
.0025
,0.13
. .0026
: 0,11
.0031
r\ j i .. A. j rt^ p/\^ปftAA.T on .t^ja^AnT Vfi^J^^rt ^_^A?S
J U 1 UH l^uMM^^BCCU ^^B|^BV 1 1 V f^^^^H 1 1 ^B^^l*
-. .;;
14.5 C 2.02 .
" . - 2.06
ป
-" , . .038
,14.5 1.66
'"{.70
n ___
" .039
,14.5 ' 1.02
- . 1.06
n ป__
" . .036 '
,14.5 1.55
" - -T.59'
n . .._..
- .038
/
,14.5 1.31 ' '
,1.35
'" ' --,--
II ' f\ A C
-------
Date
11-7-73
ro
Time Compound
2140 H2S
so2
CH3SH
DMDS
2155 . . H2S
so2
CH3SH
DMDS
2210 H2S
so2
CH3SH
DMDS '
2225 H2S
so2
CHjSH
DMDS
2240 H2S
so2
CH3SH
DMDS
lซmps) He^w: (W
4 x 10"8 52.8
n ____
n ....
2.0 .
. 4 x 10"8 86.5
"
0.9 .
2.0
4 x 10"7 48.9
4 x 10"8
1.4-
" 2>1
4 x 10"7 ' 14.9
4 x 10"8
i.o :.:',
1.5
16 x 10"8 51.9
4 x TO'8 -
1.4
2.0
O*i$)on '
.093
.0026
0.12
.
....
.0026
0.32
.025
.0027
0.16
.021 -
.0022
0.20
.025
.0026
Dilution Corrected Concentration TRS ; i
...-.- i ;
. !
14.5 ฐ 1.11 . !
" 1:15 '
. .038 i,
' '.' ' ' ' ;. I
14.5 1.43 -
" . '1.47
..." ' _ : t
.038 ' I
1 ' * *
14.5 ' 3.80 ' i
- . , 4.20
0.36 . :
" .039 '
';. '. 14.5 1.90 .
'' " . '2.23
" 0.30
.''.." .032
14.5 2.38
M
0.36
" .038 2.78
*
" " / '-V
-^sf **^fป -^,iyซw ^ r*-
-------
Date
ijecl
Time
11-7-73
(continued) 2255
2310
Compound
so2
CH3SH
DMDS
so2
CH3SH
DMDS
AttePBSion
(Amps)
4 x 10'7
4 x 10"8
4 x 10
4 x 10
7
'ht (%}
Height (%)
53.0
2.0
1.9
84.0
2.1
1.0
tra|i
ppm. wet)
0.33
.030
.0025
0.42
.031
.0017
D11
Fa
14.5
14.5
Correc
oncentrafion
m
3.92 .
0.44
.036
4.99
0.45
.025
4.40
i '
5.46
CO
co
-------
Ir-HM'
Date Time Compound .
11-8-73 935 H2S
so2
CH3SH
. ' DMDS
950 H2S
: ' S02
CH3SH
DMDS
1005 ' H2S
so2
CHjSH
DMDS^
1020 H2S
so2
CH3SH
ฃ DMDS
1035 H2S
so2
. CH3SH
DMDS
1050 H2S
so2
CH3SH
| DMDS
/Buatl
(Amps )
4 x 10"8
64 x 10"8
4 x 10"8
"
4 x 10"8
11
"
"
4 x '10*8
"
"
"
4 x 1(T8
"
"
n
8 x 10"8
4 x 10"8
II
II
32 x 10"8
4 x 10"8
n
M
Height (%}
32.0
.98
2.5 .
27.8
35.9
2.3
42.0
5.1
1.0
2.0
.-60.7
1.9
2.8
50.4
1.4
2.7
24.9
1.0
0.8
2.4
fncerflKlon QjjWpon
^ppm, wet) Flctor
-.081 12.9
0.61
_-__ "
.,0030 - .: '
.076 12.9
.086 "
....
.0028 j .- .* .
.094 12.9 '
.032 "
.027
1.0026/. "
0.11 12.9
.019
____ n
.0031 , . < .
0.15 T2.9
0.16
_--_ . .1
.0031 '
0.21 12.9
.013 "
-.=- . '.: " .
.0028 j
^ny*(^^^^^^cH ^i^ri^&^UA^ IP* A ^^^^^^
ujpnii w^^^ ^^^
0.86
7.87
.039
0.80
1.11
'
.,036 '
. 0.99
0.41
0.35 '
.034) -
1.16
0.24
.040 '
*
1.59
0.21
.040/.
2.22
0.17
'
1.036 ; ..
vet).
0,90
--0.84- -.
-1.37-
1.20
1.63
2.26
' * - -
^m-niprs-^i^'..^!^--ป.-. "-^*T*ปIป.*-
-------
Date Time . Compound
11-8-73
(continued) 1105 HgS
so2
CH3SK
DMDS
1120 . H2S
so2
CH3SH
DMDS
1135 H9S
c
so2
CH,SH
3 '
DMDS .
1150 H2S
so2
ฃ CH3SH
DMDS
1205 H2S
. S02
CH3SH
DMDS
1220 H2S
so2
CH3SH
DMDS
^^^^Ruatw^^^
(Amps)
16 x 10"8
4 x 10"8
II
II
16 x 10"8
4 x 10'8
n
n
16 x 10"8
-ft
4 x 10 a
"M
n
16 x 10"8
4 x 10"8
"
n
32 x 10"8
4 x 10"8
n
n
4 x 10"7
4 x 10'8
n
n
IHB: :v'l ' i
Height (%}' . ";W.<
i ' "'? ''n
r '. ': ' * ' t'j- ,
'.''',' *
51.4 .-.,,'>.'.;,
i," >' :, . ,:
0.8 '. ;F,;.
2.0 - :- ' _'", '
' 69.8 .' 't>::"' "'
/ '
0.9
1.8
95.6
--*
1:6
76.9
2.0
63.0
.
2.0
79.8 .
1.0
2.8
~\ '
licedBBlon
Jppm, wet)
0.21 .;,
:QQ26 :
0.25
.0024 ->-;
0.30
'^ - - - "
.0023
0.26
.0026
0.34
.
.0026 Vv '
0.44
..027
.0031;. '
' tMB.ionMปCorwfed CMf|ptra|^|
. Factor ^^ Tppm," we?n ^^
s.
1
*
12.9 2.22
n __.._
H , ____
.034 : ; i
12.9 2.64
n ___.
ii . ____ /
" '.O3i:- . '
12.9 3.17
H . .__..
1 ,
n ซ...
.030' '
12.9 2.75
n __
n ____
" . ; .034 '..-.;'
12.9 3.60
n ____
M ____
" .034.. !
12.9 4.65
.n _ _ _ _
0.35
v040> :
(p*Pfrwet/
2.25 '
2.67
3.20 :
-2.78- '
^.63
5.04 -/.-<
-------
( " .. '" " -' """ ' A " ' "*
' ' '
'
i ' . .
.: : ''fOEO*
.: 9E'0
I : ' EE'Cl
i :
- i wD D
f i ' * . "
i
--__
; f . grป
; ' ;OK)'- j
Efr'O
Ifi-fr- . -
tt'fr
; . :' '"9EO' '
f. . '
9ฃ'0
ฃi> ' -
i *E'*-
i . . ; . SEC* :
j
! i . ----
1 i
i X 09'ฃ
i
i , -.
,'\ i -ObO'
9ฃ'0
; ^,fr.
: El'*
i
!
1
i-i ฐ ^au
;.
,, ฃ200'
i, 820''
' ' . .
6*21 1?6'0
ii . ' ' - -
n -
n
6*21 9fr'0
ซ / tฃ00; ,
EEO-
n ----
6*21 2t?'0
: '8200'"
LW
n " ----
6*21 Lfr'O
' OEOO*
_
II
6'2l K'O
LEOO''
Z2U'
M ----
6*21 6ฃ'0
^n|jjpj~ ^- ^9M 'Ujdd^
^'t
L'L
6'88
2'frS
Z'2
9'L
t-'H
fr'2
*
O'L
""
L'OL
9*2
6* f I
u
6'8fr
Z'2
on
6'99
^^ (%MMJt9
II
II
8_0t x fr
z.0l x 91
..
n
g.Ol X fr
Z.OL x fr
n
8_0t x fr
z_0l x fr
H
g.OLXfr
n
n
8_0l x fr
Z.OL x fr
n
B
8_0l x fr
Z_OL x fr
H^Hi (|S
sawa ;.
HSCHO
zos
S2H
sawu
HSฃHO
zos
S2H
sawa
HSEHD
2OS
SZH
' sawa
* ^
US HO
ZOS
SZH
sawa
UO
. rii MJ
zos
SZH
sawa-
HSฃHD
ZOS
S H
punodiuoo
1MB tlHH
09ฃt
9ฃEl
02EI
90ฃt
: 0921
9E2L
ปfc
EZ-8-IL
-------
Data
Time
11-8-73
(continued) 1405
CO
1420
1435
1450
1505
1520
impound
HpS
so2
CH-SH
DMDS
H_S
so2
CH3SH
DMDS
H9S
ฃ
so2
CH3SH
DMDS' .
H9S
c
so2
CH3SH
DMDS
H9S
ป
so2
CH3SH
DMDS
HซS
ฃ
so2
CH3SH
Sualflj
DS)
. 8
, ' 4
. 8
4
8
4
8
4
32
4
16
4
_7
x 10 '
x 10'8
"
n
_7
X 10 '
x 10"8
n
n
_7
x 10 '
-ft
x 10 S
" -'
"
x 10"7
-R
x 10 B
n
n
_7
x 10 '
-R
x 10 B
n
n
_7
x 10 '
_Q
x 10 8
II
Height (%)
72.9
1.9
2.0
73.0
2.0
2.0
68.9
!- 2.0
2.4
96.7
1.8 .
50.9
2.2
1.9
77.9
, _. .
ippm, wet)
0.59
.037
.0026 .
0.59
' . .038 :.'''
.0026
0.58
,
.. ' ... <038 _ ,
. .0029
. 0.68
.0024
1.00
:o4o
.0025
0.86
'
I^^t1pr| Coi^^^ed ^^^ntr^i&n ^U|S -
\^RStor ^fflimi' ^^T (i^W we"
; >
12.9 6.24 .
.. ." 6.75
0.48
"- .034
12.9 6.24
II : '* '>/TC
- o./o
0.49
" . . .034
,
12.9 . 6.14 .
- 6-67
. " 0.49
.037 '
12.9 7.19
" . . .
7.22
" .031
/
i
12.9 10.58 '
11.13
11 ' 0.52
" .032
12.9 9.10
'
M .._.
: 9.13
DMDS
1.7
.0023
.030
-------
Date
11-8-73
00
Timer Compound
1535 H2S
so2
I CH3SH
DMDS
1550 . H?S
ฃ
so2
CHgSII
DMDS
1605 H9S
ฃ.
so2
CH3SH
DMDS ' .
t620 H,S
* c.
so2
CH3SH
DMDS
1635 H2S .
so2
CH3SH
DMDS
1650. H9S
C.
so2
CH3SH
DMDS
(
8
4
32
4
4
4
16
4
32
4
32
4
Amps)
x IO"7
x io'8
11
It
x 10"7
-ft
x 10 B
"
n
x 10"6
_o
x 10 8
"
"
X IO"6
-ft
X 10 B
II
II
x IO"6
x 10"8
II
II
x 10"6
_Q
x 10 8
"
n
Height (X).
95.8
1.8 .
50.4
2.2
1.3
60.9
-
2.4
67.9 .
3.4
--__
62.9
5.4
32.9
5.0
^KTSf"
0.68
.0024
1.00
.040
.0020
1.23
.042
. .
0.81
.050
.... _
3.71
.064
2.67
,061
'
S!ttn *ฐrr?lln we!P* * (ppiFtet)
12.9 7.19 .
I " .
' 7.22
" - .031
12.9 10.58
' J
" .
0.52. " / 11.13
.026
12.9 13.01
" '
0.54 13.55
" . ; '
12.9 8.57
"
0.64 9.21
ป ^
/
12.9 39.24
" 1-: 40.07
11 0.83
n ____
12.9 28.24
"
0.79 29.03
ii _.ซ
-------
Date Time
11-8-73
(continued) 1705
1720 .
Compound
H2S
so2
CH3SH
DMDS
H2S
so2
CH3SH
(Amps)
. 8 x
4 x
i
1
4 x
4 x
i
10'6
io-8
1
lO'7
io-8
1
"^ '' '. >
Height (%}
. r. .
ป ._. - -.
51.5
.,"''
5.0 '.f
, . : .
'.. 18.8 ; ;;
'
;
ConftHfatlgH^ ttlutii
(ppm, wet) . TactoT
. >
.
1.64 12.9
____ .' H
.; -061 "
... ' , "
0.20 i 12.9
. .... ป
. ' i,|,*- _ ' "
^H||cte|dtejncen||^1on ^JRS
4
.
17.35.
'
0.79 18.14
2.12
'--'
.. - ... ii ,2.12
DMDS
.1 -r
MIlA'T --
co
to
I I
-------
Date
.Smelt Tank 9/18
9/19.
9/20
Lime Kiln 9/24
9/25
9/26
9/27
Smelt Tank 10/31
11/1
11/2
Lime Kiln 11/3
11/5
11/7
11/8
MOISTURE AND FLOW RATE DETERMINATIONS
74-KPM-4
Escanaba, Michigan
Percent Moisture
23.8
26.2
23.3
76.1
61.3
65.9
64.2
74-KPM-5 '
Courtland, Alabama
37.0
30.3
32.6
40.0
37.3
34.8
34.6
Flow Rate DSCFM @ 70ฐF
and 29.92 in. Hg
19,540
18,740
19,610
13,928
13,928
13,928
13,928
9,822
8,880
10,063
14,226
14,226
14,226
14,226
40
-------
Ill- PROCESS DESCRIPTION AND OPERATION
The Champion Internationa.! operation at Courtla'nd, Alabama, is
a complete mill, producing about 500 tons of bleached kraft pulp per
day. The pulp is made into fine paper,(about 257 tons per day) and
other paper and board products.
The EPA test program conducted at this mill included emission
measurements on the recovery furnace (3 particulates), the smelt dissolving
tank (3 particulates and TRS), and the lime kiln (3 TRS).
Process Description .
A. General
Kraft pulp is produced from wood as shown in Figure 2 . In the process,
wood is chipped into small pieces, then cooked "in a continuous digester at
elevated temperature and pressure. 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 washed. The pulp is then
bleached, and made into paper.
The balance of the process is designed to recover the cooking chemicals.
Spent cooking liquor and the pulp wash water are combined for treatment. The
combined stream, called weak black liquor, is concentrated in multiple-
effect evaporators and stored. As needed, the black liquor is drawn
from storage and oxidized in an air sparging tank. The oxidized liquor
receives its final concentration in direct contact evaporators and is then
fired to a recovery furnace.
41
-------
tJood
is
*ฃ.
'j V.'ii"; to i"ii-iif;r
~i (f-.ru
c-
(NaOH
>-
c;
-l-J
o
t_>
DIG-ESTER
SYSTilM
SMOlt
(HagCOs + Ha2S)
_i
Watei
SMELT
DISSOLVING
Tn . t j t
/\iซiป
Green Liquor
(recycle to
digester)
carbonate
mud
Figure 2
42
-------
Combustion of the organics in the black liquor provides most of the
heat needed to generate process steam. Inorganic chemicals from the
black liquor are recovered as a molten smelt at the bottom of the furnace.
The smelt, consisting of sodium carbonate and sodium sulfide, is dissolved
in water and transferred to a causticizing tank: "Lime added to this tank
converts sodium carbonate to sodium hydroxide, completing the regeneration
of white liquor, which is then'recycled to the digester. The calcium
carbonate mud that precipitates from the causticizing tank, is recycled
to a kiln to regenerate lime. . . .
B.- Recovery Furnace and Smelt Dissolving Tank
The recovery furnace was designed by Babcock and Wilcox to burn
95,300 pounds of black liquor solids per hour, which corresponds to a
pulp production rate of 602 tons per day. The furnace has a conventional
design, with two parallel cyclonic direct contact evaporators. The
black liquor is oxidized in a single stage air sparged tank, just before
firing. The furnace system was installed in 1971.
Exhaust gases from the furnace are cleaned in an electrostatic preci-
pitator., erected on the roof of the recovery furnace building. The
precipitator was manufactured by Research Cottrell, and installed with the
furnace in 1971, as shown in Figure 3,
The molten smelt formed at the bottom of the recovery furnace is
drawn into a water filled tank, called a smelt dissolving tank. The'
reaction between the hot smelt ana the receiving water generates steam,
which is blown through a scrubber to remove entrained particulates.
43
-------
RECOVERY
FURNACE
Combustion
Gases
CYCLONIC
DIRECT
CONTACT
EVAPORATOR
(2)
1
ELECTROSTATIC
PRECIPITATOR
Black Liquor
FIGURE 3 - RECOVERY FURNACE AND ELECTROSTATIC PRECIPITATOR AT THE CHAMPION INTERNATIONAL MILL
IN COURTLAND ALABAMA. . ' .
-------
The scrubber has a wet fan design, and was manufactured by Ducon.
As shown in Figure 4, the scrubber was installed downstream of a set
of wire mesh demister pads.. Originally, the demister pads were the
only control device; they have been left in place to aid the scrubber
and to serve as a backup.
Gases pass-through the bottom of the scrubber receiving a light
wash from water draining from the top (refer to Figure4). The gases
leaving the scrubber are sprayed with water as they pass through a fan.
Reentering the upper half of the scrubber, the gases swirl out the top,
as the water drains downward and out the bottom. The scrubbing water
is the'discharge from the lime mud washers (weak wash); it is applied in
two 45 gpm streams, just before the fan and directly into the fan.
The product of the smelt dissolving tank is a water solution of smelt,
called green liquor. The green liquor is pumped from the dissolving
tank for further processing to recover pulping chemicals.
C. Lime Kiln .\ ....
The plant operates a single rotary kiln to regenerate lime from the
calcium carbonate slurry that precipitates from the causticizing tanks.
The slurry is washed and then dried on a rotary vacuum drum, as shown
in Figure 5. The dried cake is removed from the drum by a knife edge
and conveyed to the kiln. The kiln is heated by burning either natural
gas or oil. In the kiln, the calcium carbonate lime mud is roasted;
carbon dioxide is driven off leaving calcium oxide (lime) as product.
45
-------
o
Samblina Ports
Pressure
Relief
Valve
(from recovery furnace)
Smelt
Green <
Liguor
(to
causticizing)
J/ent J
SMELT DISSOLVING TANK
Fi-jijr.2 ^ Srolt Dissolving lank and Scrubber. Champion International
Mill at Court!and Alabama.
46
-------
-PS
'
Limestone
(makeup)
Limestone Mud
(main feed)
Mud
Washer
Lime
(product)
o
Stack
^Sampling
Ports
\
^ Bleed
(to Mud Washer)
Figure 5 Flow Diagram of Lime Kiln. Champion International Mill at Courtland Alabama,
-------
To make up for lime lost in the pulping and recovery process,
limestone is sometimes added. The stone is crushed, and charged to the
kiln as secondary fuel. During' the EPA tests, however, no limestone
make-up was charged.
Noncondensable gases from the multiple--e.ffect evaporators are burned
in the kiln to control odors. Dregs from the green liquor clarifier are
not burned in the kiln, but are washed and sewered.
The combustion gases from the kiln are cleaned in an adjustable
throat venturi scrubber, and then pass through a demister and out a
stack. The scrubbing water is recycle from the demister plus fresh
water make-up. A portion of the recycle water is bled off to prevent
excessive accumulation of solids. The bleed stream is returned to the
process as wash water for the lime mud. .
Process Operation
A. General
The purpose of the tests was to measure emission levels during normal
plant operation. Process conditions were carefully observed, and testing
was done only when the test facility appeared to be operating normally.
During the tests, important process conditions were monitored and recorded
on data sheets. Readings were taken about once every half-hour. These
data, and keys to the entries, are in the appendix. The data are summarized
below. .
48
-------
B. Recovery Furnace
As far as known from the process data (appendix) and conversations
with the operators,'the.equipment operated normally during the tests.
Black liquor charge rate varied-between 200-205 gallons per minute,
a little higher than its normal rate ;of?about 185 gallons per minute.
The black liquor solids content ranged from 61.0 to 64.0 percent; 64.0
percent is normal. Soot blowers operated continually during the tests,
as normal.
The operation of the precipitator was also monitored during the
tests. As far as known the precipitator operated normally during the
tests. The primary current drawn by each of the four control sections
was monitored from the furnace control room. The current, in amperes,
ranged from 54-56 (Section A): 58-59 (Section B); 150-151 (Section C);
125-127 (Section D).
-49
-------
C. Smelt Dissolving Tank
The flow of smelt to the dissolving tank cannot be directly monitored.
The best indication of a normal smelt flow rate, is the operation of the .
recovery furnace. When the furnace receives its usual charge of black
liquor and operates in its customary way, the production of smelt will
be normal. Accordingly, furnace operation was monitored along with
available process indicators for the dissolving tank. The latter included
the dissolving tank level, the flow rate of water to the dissolving tank,
and the total alkali in the green liquor. . .
As far as known from the process data and discussions with the
operators, the equipment operated normally during the tests. As shown
on the process data sheets, the black liquor charging rate ranged
narrowly between 199-205 gallons per minute (gpm); solids content, as
fired, ranged from 61.0-64.0 percent.
D. Lime Kiln
The operation of the lime kiln was in some ways unstable during the
tests. TRS emissions ranged up and down from a few ppm to about 70 ppm.
The swings were in contrast to the normally steady TRS emission levels
of about 3 ppm, reported by Champion on-the basis of a two month test
earlier in the year. A complete explanation for the variability in
TRS emissions is not known, but some contributing factors are discussed
below. ...........
The oxygen content of the combustion gases -is known to influence
TRS emissions. On some occasions, TRS levels were observed to change
significantly with 02 levels. On November 7, for example, TRS emissions
50 '
-------
were about 5 ppm with an Op concentration of 6 percent; TRS rose to about
18 and then 40 ppm, as Op concentration dropped to about 4 and 2 percent
respectively. On the basis of observation's during the tests, an Op level
of 5-6 percent seerrs des-irable. . Mill personnel indicate thafpreviously,
a level of 4 percent was adequate.
Another factor influencing TRS emissions is the residual sulfide .
content of the lime mud after washi-ng. The mud is normally washed
thoroughly at this mill, but equipment malfunctions during the EPA tests
may have lowered washing efficiency. The agitators in the mud washing
tanks broke down on November 6 at about 1300 hours, and the kiln was
shut down. Although the agitators were repaired, mill personnel were
not convinced that normal washing efficiency had been restored. Tests
on the lime mud showed, unusually high soda content of 1.0 percent instead
ป *
of the normal 0.3 percent. This may indicate poorer washing.
Two TRS runs were made on November 8. The first 4-hour run indicated
TRS emissions were less than 5 ppm. During the second run, TRS emissions
climbed to 20 ppm, although the Op concentration "remained above 5 percent.
Toward the end of the run, the kiln operator reported that the vacuum
filter was malfunctioning, and shut off the mud feed to clean the filter.
When operation was resumed, the TRS level dropped to 2 ppm within 30
minutes. It is possible that a plugged filter caused the higher TRS
emissions. If the filter plugs, the residual water and dissolved sulfides
will not be adequately removed from the mud before firing. Poor filtering
would also explain the abnormally high soda content of the mud mentioned
above. .
51
-------
The mill reports that the present filter was installed September 19,
1973, just prior to the EPA tests. The mill had not monitored TRS
emissions subsequent to the filter's installation. It seems likely that
the high TRS emissions can be partly explained by the vacuum filter gradually
plugging. Mill personnel do not believe, however, that this is a full
explanation.
The process data in the appendix indicate normal kiln operation
during particulate sampling. The main process parameters are summarized
in Table 7 below.
Table 7. Summary of Lime Kiln Process Data
Test
33-1
33-2
33-3
Date,
1973
Nov 3
Nov 5
Nov 5
Sampling .
Hours
1450-1712
0950-1313
1347-1605
During Particulate Sampling
Mud
Charging
Rate
gpm
190-193
165
165
.Kiln
Temp.
ฐF
1825-2050
1850-2000
1925-1950
Venturi
Pressure
Drop
In H?0
22-24
22-24
23.5-24
Fuel
Gas
Rate
103 scfh
64.5-65
51-55
55
Fuel
Oil
Rate
gpm
0
0
0
As shown, the feed rate was somewhat high during Run 33-1, at about 190
gpm. Particulate emissions, however, were lowest for that run. No
limestone makeup was charged during the tests. The venturi pressure
drop was steady between 22 and 24 inches of water. Natural gas was the
only fuel fired.
Emission measurements were substantially higher for the third run.
Examination of the process records does not reveal any explanation for
the high result.
52
-------
D. Equivalent Pulp Production Rates
In a kraft mill, recovery operations are quantitatively related to
pulp production. A given feed rate of lime mud to the kiln, for example,
is equivalent to a certain' p'ulp production rate in the digesters. As a
result, pollutant emission rates can be expressed oh the basis of
equivalent pulp production, as shown below:
0,
To use Equation 1 for calculating lime kiln emission rates, the
equivalent pulp production rate was assumed to be the average pulp
production rate at the mill, as determined the month preceding the tests.
In that period (October 1973), plant records indicate an average production
of 24.2 tons of unbleached air dried pulp per hour.
For calculating emission rates from the dissolving tank and .furnace, a more
accurate method was used, based directly on the amount of black liquor
charged during the tests. Equivalent pulp production is proportional to
the amount of black liquor fired during each test run, as shown below:
** Pulp to Liquor Ratio
ds
The last term in Equation 2 corrects for the actual percent solids (in
the black liquor charged) compared to the average percent solids on
which the" pulp to liquor ratio is based.
53
-------
The Pulp to Liquor Ratio in the above equation was determined from
plant records for the same month of October 1973. The total pulp
production during this time was 17,978 unbleached air dried tons.
Flow meter readings show-that 8,300,845. gal-lons of black liquor-were
charged during the same period. By division, the Pulp to Liquor Ratio
was found to be 0.00217 tons per gallon.
The average solids content of the balck liquor charged during the same
time period (base average), was determined from the furnace operator's
two-hourly records of solids content. The average of all the readings
was found to be 63.2 percent.
Substitution of the above determined values into Equation 2 gives:
/EquivalentX /Black \ A Solids \
[Pulp ./Liquor (0.00217 U (test avg.) Eauation
I Production I I ChargedMton/gallonrt 63.2 j . tquation
\tons / \gall ons/ \ /
Equation 3 was used to calculate the equivalent pulp production rate
during each test on the smelt dissolving tank. The calculations are
summarized in Table 8 below.
In summary, emission rates in units of pounds per ton of pulp are
calculated from Equation 1. Equivalent pulp production rates to use
in this equation are given in Table ?
54
-------
Table 8. Summary of Calculations for Equivalent Pulp Product!on-Rate
Date
1973
Oct. 31
Nov. 1
Nov. 2 .
Black Liquor Readings
Hours ^
Start
1105
0907
0907
Finish
1728
2146
1635
(?)
Integrator^ '
Start
0,047,435
0,023,946
0,026,913
Finish
0,122,183
0,173,747
0,117,100
(3)
Avg. % Solids
62.3
63.7
61.8
Black
1 Liquor
Charged
gal
74,748
149,801
90,187
Equivalent
Pulp
Production
tons
159.9
327.6
191.4
Elapsed
Time
hr
6.38
12.65
7.47
Equivalent
Pulp
Production
Rate .
ton/hr
25.1
25.9
25.6
en
en
(1) Item 12 on the process data sheets.
(2) Item 11 on the process data sheets.
(3) Item 14.on the process data sheets (average).
(4) Calculated from Equation 3.
-------
Table 9. SUMMARY OF EQUIVALENT PULP PRODUCTION RATES
TO BE USED WITH EQUATION 1. .. '
Day of Test
1973
Oct. 31
Nov. 1
Nov. 2
Nov. 3-8
Test Facility
Dissolving Tank
Dissolving Tank
and Recovery Furnace
Dissolving Tank
and Recovery Furnace
Lime Kiln
Equivalent Pulp Production Rate
ton/hr
25.1
25.9 - . ;
25.6
24.2
56
-------
KEY TO INSTRUMENT READINGS ON RECOVERY FURNACE PROCESS DATA SHEETS
1. Net rate of.steam production (not including steam used for soot blowing)
2. Running total of net steam production. '
3. Time corresponding to item 2.
4. Temperature of steam leaving the furnace (economizer exit).
5. Pressure of steam leaving the furnace (economizer exit).
6. Boiler feedwater flow rate.
7. Running total of boiler water fed.
8. Time corresponding to item 7.
9. Feedwater temperature. '
10. Feed rate of black liquor to the furnace.
1.1. Running total of black liquor fed to the furnace.
*
12. Time corresponding to item 11.
14- Percent solids in black liquor charged to the furnace.
15. Temperature of black liquor charged to the furnace.
16. Pressure of black liquor charged to the furnace.
17. Number of spray guns charging black liquor to -the furnace.
18. Diameter of spray gun nozzle.,
19. Setting of damper to bypass black liquor around the furnace.
20. Feed rate of salt cake makeup/feed rate of acid or brine makeup.
24. Auxiliary fuel flow rate: gas/oil.
25. .Number of auxiliary fuel burners.
26. Temperature of gas leaving the furnace (economizer exit).
27. Temperature of gas entering the precipitator.
2S. Temperature of gas in the stack.
22. Temperature of combustion air entering the furnace,
57
-------
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59
-------
31. Total flow rate of combustion air to the 'furnace,
32. Flow rate of primary combustion air to the furnace (uncalibrated).
33. Flow rate of secondary combustion air to the furnace (uncalibrated).
34. Flow rate of tertiary combustion air to the furnace (uncalibrated).
35. Concentration of oxygen in combustion ^ases leaving the furnace.
36. Concentration of combustible gases (CO, hydrocarbons) in combustion
gases leaving the furnace.
37. Combustion air blower pressure.
38. Induced draft fan vacuum.
39. Concentration of TRS in the furnace/stack (Company monitor).
40. Flow rate of weak wash to the-smelt dissolving tank.
.41. Liquid level in the smelt dissolving tank.
:42. Total alkali in the green liquor.
Note. At the bottom of the data sheets the primary current (amps) drawn
by sections A,B,C, and D of theprecipitator are given; readings
are taken from the furnace control room. Further below, the
primary volts, primary amps, and secondary amps are shown;
readings are taken from the precipitator control room on the furnace
roof. . ' .
58
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Ccrr,,, C,_f.,._ -.-U^. J hill C^U,,A k'nlfin. i
Onsratsrs E>r=*/ -<..- 7-i/ Instrurents
yes(ฃ)
Date / \A-V -? 3
Data 2?: ..o. --
P^o l-/o
Units
Calibrated Corrections Included
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O^-s-IO?^"1 I'?7'"' IK'O |'.?c-r
1 I-.;;?.- -I"1. - ^\-.!'~. !ie>- (h/d/- : ' J^i, :.3V~ฃ ;-i-!S i 2 * *
2 - tnt-r.
3 - Tire
4 Stear" To";". Out
5 Staa~ r-ress. Out
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6 Water Flcv: - Chart
7 . - Intir.
8 - Tir.e
9 'i.'ater Ter.~. - to Scilsr
\;
35 rv,-pi (Gns)
35 .Combustibles (Gas)
7o 0,
it
Pt C./7
-
-
30!
-?
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J.a'i 3.03.
31.5
-
o/o
31. iT
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Operators 7~3 c P^W*.-" Instruments
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Oat? i N,, 7.-5
Data Set ..o. ^
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2 - int-r.
3 - Tire
4 St-v." 7"-!?. Out
5 Stea.r. r-ress. '""ut
Units ! n=-n>n
A ' 'V.- ' . :
Calibrated Corrections Included
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lOtrf.'
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15-45
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BLACK L nun?
10 3L Feed Hate - Cnart
11 - Inter.
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GH
2 - Tire ! .74- !,,-..<-
4 Psrc-3.it Solids
15 5' Tnr:ri . tc F'jrn2C3
1
C- [JL "ress. tc Furnac3
* 17 ;.'c. of Snravs in Use
* 13 Size cf Siravs
* 13 3L i''-,.3ss Darrer
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!J Salt Cake Feed *e.ฐ/Br,,.g. i
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Se.lkv,ir 1.to/^i." || 35~*AL!''.I!
24 Flcv; ?.atc- (Gas/Oil)
* 25 No. of Lurrsers in I'se
IO-CFM/C-.W-
2G Gas Ten-: - fror: Boiler
"~
27 - tc frecim'taton 'V'A-r
25 - tc Stack
3D ;.ir Te~-. - to iioiler
31 Air Flcv; - Total
32 - Prirarv
33 - Secondary
CF
r /T
-
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'X-
34 - Tertiary i /,
35 (Vv-ai (Sfi*)
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35 .Corr.bustibl-'S fGas) 'ฑ
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O/o
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O/o
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37 FD Fan Out (Mr)
38 ID Fan Out (Gas)
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39 Tctal deduced Sulfur
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J7O | J7C
S U.ฃ' I
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57
ISC
ISO
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I ' I
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-------
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Instrurents Calibrated
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Cornjcticr.s Included
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Pat*
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K'm'ts ' Dei;1'?n'i
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4 Stv.- To-.". :>jt
5 $taar. rT03i. Out
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i
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6 Water Flew - Chart
7 - Int-r.
8 - Ti.-.e
9 i.'atsr Te:rj. - to -ssil^r
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CiO
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360
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310
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1 i
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10 3L Feed Rate - Cnart
11 - Inter.
' 2 - Tine
Gfn
Or./
0'0-'--i^
' f, Farcont Solids [ :,
15 BI TO-'), tc Furr^c3 i "r
1C 2L Press, tc Fumae*
* 17 lie. of Snravs in Use
* 13 Siz-"1 cf S"rav*
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24 Flcv; P.atc- (C-23/CiT)
* 25 No. of Lurnsrs i" L'se
i<..Jcr^vfc'''')
i
"25 Gas T2n- - frcr toiler
27 - tc frecinitatcr
25 - tc Stack
30 ;.ir To". - to Boilor
31 Air Flew - Total
32 - Prirarv
33 - Secondary
4 ~'
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Al^
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33 Tctal deduced S
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C.-i
6. 5"
I-C',
S-il
ft
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ltivic- 3 -i
I :x.c /,-?(/.
C * /
o;irinr
63
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f
Date ซo
ata i*t ..o. "5
Instruments Calibrated Corrections Included
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fTE'.V
"l i ':?." ]".: - i '<".
2 - Int-r.
3 - Tir?
4 ฃt-isr To-vi. Out
5 Stea- r-rcsj. "ut
6 Water Flcv: - Chart
7 - Inf;r.
8 - Tine
9 ;.'ater Te:r,. - to irioilซ?r
10 3L Feed Hate - Chart
11 - Inter.
' 2 - Tiro
U Percent Sri ids
15 5L TO-I. tc FLTP.-ICS
1C 2L Press, tr F'jrn?.c=
* 17 !!c. of S"ravs in Use
* 13 Sire cf S'iravs
* 13 3L H-'-:,5ss 3=r-=r
2J Salt Cake Feed *a*&-/ฃt..&,.
l-.lt<...k.C
24 Flew ?.atc- (C-as/Cil)
* 25 :;o. of Lurnsrs in I'sa
25 Gas Tanr: - frcr- toiler
27 <;c.i.'vV,.v- - tc frccinitstcr
2S - tc Stack
30 Mr T-;~-,. - to Boiler ''/'*-
31 Air Flcv. - Total
32 - Frirarv
33 - Secondary
34 . - Tertiarv
35 OYV-OI fr-^s)
35 Combustibles (G?.s)
37 FD Fan Out (Air)
33 ID Fan (Sit (Gas) &P
Units
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r-
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- L
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39 Tctal deduced Sulfurf---y/,^!"-^r> I
310
-*<<:
L,.,i
51
si !
5"?
I5I
1 SI
0-7.1
i.e any cnangas aurinr test ^2
I'
e-riiซ
64
-------
~:.^.,:...,,.. b.^^i hm
O^ratgrj 7-3 Ci-ปsFป
Date &-? **" ~>
Instrurents Calibrated Corrections Included
>-..;*
! Units ! ne<-icni!4l
.1 i:?-r '}?.: - ป'->.rt ifo-it/^1 .'J<=r' ;'J5ซ
2 - inf;r.
3 - Tire
4 Etour 7ซT<. Out
5 St23- l-ross. Out
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F
r*T*.~
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U j'i'o
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5^5
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3-45
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si1.;
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cc-rt?/;
IC-^S
5.-^'
S'i'S
4-*i
,
: i
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FEED'. .'ATE!? ' !
6 Water Flew - Chart
7 - Int^r.
8 - 71. ~e
9 i.'ater 7s:". - to Boiler
\/(ซ.
-
il^ .. j,^,..^
T
;
.
10 3L Feed .Hate - Chart
11 - Inter.
GP*'!
12 - Tiro !C"7-/..i-
14 Farcont Solids
15 BL Tฐ~i. tc Ffjrn-ic3
1C 2L ฐress. tc Furnacป
* 17 ."c. cf Snr5'/s in Use
* 13 Sir? cf ?ซr2vs
* 13 3L r-'iass Danrar
2J Salt Cake Feed
e'ซ'
'rf
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r**"j
fa" 0
':1 6?en
CPH/CPM
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-
-
07^
Oc?
-
Oc?
3cS"
-
-
Jo?
360
~
"'
^60
-
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300
-
-
2C?
BLACK LI?'Jj=
a.r-
!b?Tij;7J
'1 !f ex>
-
|! jjl.
!! 3i. c
1! 0-
II >,,.ป<
;
li o/o
24 Flo; .'.ate- (C-as/Cil)
* 25 r;n. of Lurnars in Us 3
it.:crt, /.,,
M -i
1
2G Gas Ten-: - frcr toiler
27 - tc rrecirntator
2S - tc Stack
3D Air Tc---;. - to Boiler
31 Air Flew - Total
32 - Prir.arv
33 - Sscondarv
fr
*\- /--r
CF/ซT
-
-4.
''I-
34 - Tertiarv i ':
:jr, nv_.f.art (f:riq)
35 .Corcbustibl2S (Gas)
",: at
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J
C-/-7
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-
~
33 1
J1 1
-
-
&'&
IT-/
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20 i
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J-l"i
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3C/S
-
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-
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20^
rtniw
lC->, 5
-
33"i
51-0
1 I
; i
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fC - ,iy'/ILT-'"v r.'1"';17"0 ift
Oi'o o/b
c, 1 O
0/0
0
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o
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KEY TO INSTRUMENT READINGS ON LIME KILN PROCESS DATA SHEETS
1. Feed rate of lime mud-to filter,
2. Density 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 primary air to the kiln.
6. Total amount of 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 at the hot end "of the kiln.
11. Temperature of gases leaving the kiln.
12. Pressure drop across the venturi scrubber.
13. Flow rate of caustic to'the scrubber (zero).
14. Flow rate of makeup water to the scrubber.
15. TRS concentration in the stack (Company Monitor).
16. Feed rate of limestone makeup to the kiln (zero).
17. Concentration of combustibles in kiln exit gases.
18. Charging pressure of primary air/secondary air.
66
-------
Company cU~.*-,
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
/%
FlowrLime Hud to Filter
So'lids to Filter
Fuel Oil Flow Rate
Fuel Gas Flo1.-/ Rate
Primary Air Flow Rate
Intearators: Gas
011
Time
Excess Oxygen
Temperature: Hot End
Cold End
Scrubber AP
Caustic to Scrubber
Make-up Water Flow
TRS
Limestone Make-up
1_.~ป- k.l. O>->-i,;-ii4,i/o:S
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Operators
Date
Data Set No.
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Unit No. 4'
Operators 7.. , vVf.r.i.-ฃป- ' Date 4ฐ ^ซ~ ~? 3
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1
2
3
4
5
6
7 .
8
9
10
11
12
13
14
15
16
17
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Flow: Li me Mud to Filter
Solids to Filter
Fuel Oil Flow Rate
Fuel Gas Flow Rate
Primary Air Flow Rate
Integrators: Gas
Oil
Time
Excess Oxygen
Temoerature: Hot End
Cold End
Scrubber AP
Caustic to Scrubber
Make-up Water Flow
TRS
Limestone Make-up
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Location
Facility ' Line Kiln
[Urn'tiNo.
Operators
Date
Data Set No.
| Page
1
2
3
4
5
6
7
8
g
10
n
12
13
14
15
16
n
it
FlowrLime Mud to Filter
Solids to Filter
Fuel Oil Flow Rate
Fuel Gas Flow Rate
Primary Air Flow Rate
Integrators: Gas
Oil
Time
Excess Oxygen
Temoerature: Hot End
Cold End
Scrubber AP
Caustic to Scrubber
Make-up Water Flow
TRS
Limestone Make-up
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Operators
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Or.
1
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Date
Data
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1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
n
1?
Flow: Li me Mud to Filter
Solids to Filter
Fuel Oil Flow Rate
Fuel Gas Flov; Rate
Primary Air Flow Rate
Integrators: Gas
Oil
Time
Excess Oxygen
Temperature: Hot End
Cold End
Scrubber L?
Caustic to Scrubber
Make-up Water Flow
TRS
Limestone Make-up
L,^.^ (<,/ C^^/a.-st^/r x
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Company c.!.........,..,,.-,.. ~; fif .-,-,= ,ฃ.*-**! {Location
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Company
Location Co-.^c if-. --. J '
Facility Lil,e K1ln
jUnit No. ฑ
Operators
Date 7
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Data Set No. 3
| Page :;. /;-
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
Flow:Lime 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
Cold End
Scrubber AP
Caustic to Scrubber
Make-up Water Flow
TRS
Limestone Make-up
Units
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! Location c.-='<:-.
Facility Linie Kiln
Operators "3-/i vj*,}-^..^
"- ~>a.~. A-'tfs-sc
C
jUnit No. i !
Date ^7 ^' "7-1 !
Data Set No. 3'.1'. I Page 3/2
I
2
3
4
5
6
7
8
9
10
n
12
13
14
15
16
I"?
12
Flow: Li me 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
Cold End
Scrubber AP
Caustic to Scrubber
Make-up Water Flow
TRS
Limestone Make-up
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{Unit No. /
Operators //--;,._. LV..:. ,;:,
Date
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Units
Page
Flow: Lime Mud to Filter
C7--M
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Fuel Oil Flow Rate
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Oil
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11
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75
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Company cL-ป -ป/>..
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Facility L1me Kl-ln
Unit No.
Operators 7-3
Date
Data Set No., g' . | Page
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
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Unit No.
Operators
Date <:ป?
Data Set No.
(Page
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
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Solids to Filter
Fuel Oil Flow Rate
Fuel Gas Flow Rate
Primary Air Flow Rate
Intearators: Gas
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Time
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Temperature: Hot End
Cold End
Scrubber AP
Caustic to Scrubber
Make-up Water Flow
TRS
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Operators
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Date ? Me,., 7j
Data Set No", c (Page ฃ=%.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
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Solids to Filter
Fuel Oil Flow Rate
Fuel Gas Flow Rate
Primary Air Flow Rate
Integrators: Gas
Oil
Time
Excess Oxygen
Temperature: Hot End
Cold End
Scrubber AP
Caustic to Scrubber
Make-up Water Flow
TRS
Limestone Make-up.
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'^
""'"/-^
/73o
n
-------
IV. LOCATION OF SAMPLING POINTS
Figure 2 shows the sampling ports and the number of sampl-
ing points at the recovery furnace exit stack. The test site
was located in an 84 inch inside diameter vertical stack, 25
feet (3.5 diameters) from the stack exit, and 35 feet (5
diameters) from the nearest downstream disturbance. Thirty-
two velocity traverse points (16 along each of two perpendicular
diameters) were determined as described in the Federal Register ,
Method 1.
Figure 3 shows the sampling ports and the number of sampl-
ing points at the smelt dissolving tank exit stack. The
vertical stack was 42 inches inside diameter, 20 feet (5.7
diameters) from the stack exit, and 10 feet (2.8 diameters)
from any downstream disturbance. Forty-eight velocity traverse
points- (24 along each of two perpendicular diameters) were
determined from the Federal Register , Method 1. Since only
one port existed on the stack, the points on the perpendicular
diameter were layed out graphically and were traversed from the
single port as shown in Figures 4 and 5."
Figure 6 shows the sampling ports and the number of
sampling points in the exit stack of the lime kiln. The vertical
-stack was 48 inches inside diameter, 15 feet (3.75 diameters)
from the stack exit, and 25 feet (6.25 diameters) from any down-
stream disturbance. Thirty-two velocity traverse points were
determined from the Federal Register , Method 1.
1) Federal Register, Vol. 36, No. 247, December 23, 1971.
79
-------
84" ID
3" NIPPLES
V W.T.
00
o
EAST
PORT
SOUT:-;
PORT
RECOVERY
FURNACE
*
DIRECT
CONTACT
EVAPORATOR
ELECTROSTATIC
PRECIPITATOR
Figure 2. Recovery furnace sampling site
-------
42" ID
3"NIPPLE
V'W.T.
o
13S
ooeooooooooo oooooooooooo
212
00
EAST
PORT
FROM
RECOVERY
FURNACE
GREEN
LIQUOR
SMELT-
DISSOLVING
TANK
WET FAN
SCRUBBER
Figure 3. Smelt-dissolving tank sampling site
-------
~ \ \ V N ! Original seale 1/4"=1" / ; / '.' / ^ -
' \ \ \ \ I \ T =TTI-\H+- V> a c Koon r-orl jir>Of^ I ' / /" ; r"
1 \;\ \ \ !\ Layout has been reduced.' ;/ , / f \ ;
J \ V X '\ 1 V - - \ ' ': -'\' '~^~~~i~ ~" I -r- . i--r A -,_- V ^ -1 V f ,__;_-
' \\\\\ \ - \ ' - / /! / -' /.7^T
_ _-^- ^ _ ^ .-. p- ^ p . ^ ^_ , , __ .^j, . .
!-\\\\\\\\i
rested on port wall
insure correct angle
Field copy of graphical grid layout
'"/ Sampling point
\
I---
-------
Figure 5. Picture of actual stack grid layout
83
-------
NORTH
PORT
00
EAST
PORT
o
15'
25'
LIME
KILN
VENTURI
SCRUBBER
CYCLONIC
SEPARATOR
Figure 6. Lime kiln sampling site.
-------
FILTER
00
in
HEATED
GLASS
PROBE
n
FLEXIBLE .TEFLON CONNECTOR
(OUTLET TRAIN ONLY)
THFRMnMFTFD
THERMOMETER
THERMOMETERS
/
UMBILICAL
CORD
CALIBRATED ORIFICE
MANOMETERi
Figure?. Particulate sampling train
-------
V. . SAMPLING AND ANALYTICAL PROCEDURES
All sampling procedures were selected by EPA prior to field
sampling. All analyses of collected samples were performed by
PEDCo. Appendix E contains detailed sampling and analytical
procedures. Sampling and analysis of total reduced sulfur
compounds was performed by GAP personnel at the site.
Velocity and Gas Temperature
All gas velocities were measured with a calibrated type S
pitot tube and inclined draft gage. In all cases velocities
were measured at each sampling point across the stack diameter
to determine an average value according to procedures described
in the Federal Register - Method 2. Temperatures were measured
with long stem dial thermometers or thermocouple.
Molecular Weight
A four hour integrated sample of the stack gases was
R
collected daily by pumping the gas into a Tedlar plastic bag
at the rate of approximately 0.015 CFM. ' This bag sample was
then analyzed with an Orsat analyzer for C02, G>2, and CO as
described in the Federal Register/ Method 3.
Particulates
2
Method 5 as described in Federal Register, was used to
measure particulate matter. A rigid train consisting of a heated
glass lined probe, a 3" glass fiber filter, and a series of
1) Federal Register, Vol. 36, No. 247, December 23, 1971
2) Federal Register, Vol. 36, No. 247, August 17, 1971
86
-------
Greenburg-Smith impingers was employed in all particulate tests
as shown in Figure 7.
Sampling was conducted under isokinetic conditions by
monitoring the velocity with a pitot tube and adjusting the
sampling rate accordingly.
Sample recovery consisted of triple rinsing the nozzle,
probe, cyclone by-pass, and front half of the filter holder with
acetone into a glass container. The back half of the filter
holder, impingers, and connecting tubes were first rinsed with
distilled water, and placed into a glass container along with the
impinger contents. These components were then triple rinsed with
acetone and these washings placed into another glass container.
The filter was placed in a separate container. Blank samples of
water and acetone were also taken.
NOX
Nitrogen oxides were collected in evacuated 2-liter flasks
containing 25 ml of a dilute sulfuric acid-hydrogen peroxide
absorbing solution. The sampling and analytical procedure, as
described in Method 7 of the Federal Register, was used except
that the final flask vacuum was read immediately after sampling.
The samples were analyzed using PDSA method.
1) Federal Register, Vol. 36, No. 247, December 23, 197!
87
-------
Moisture
Method 4 of the Federal Register was used to determine stack gas
moisture content. A flue gas sample was drawn from the gas stream
through a. heated probe, a series of midget impingers contained in an
ice bath, and a pump and dry gas meter assembly. The moisture was then
measured volumetrically and the proportion of water vapor -in the gas
stream was determined by calculating the equivalent volume of the
condensate.
The moisture for the lime kiln exit stack had to be determined by
the psychrometric chart because small water droplets were generated by
the venturi scrubber. These small droplets, when collected with the
condensate, will give higher than true moisture percentage when Method 4
is used, for moisture calculations.
Total Reduced Sulfur
The following Method 16, "Semi-continuous Sulfur Emissions from
Stationary Sources", contains the procedures used for obtaining the reduced
sulfur concentrations.
1)Federal Register, Vol. 36, No. 247, December 23, 1971
-------
METHOD 16 - SEMICONTINUOUS DETERMINATION OF
SULFUR EMISSIONS FROM STATIONARY SOURCES
1. Principle and Applicability
1.1 Principle. A gas sample is extracted from the emission source
and diluted with clean dry air. An aliquot of the diluted sample is
then analyzed for gaseous sulfur compounds by gas chromatographic separa-
tion and flame photometric detection. Two GC/FPD analytical systems
equipped with suitable columns are used for resolution of both low and
high molecular weight sulfur compounds.
1.2 Applicability. This method is applicable for determination of
to.tal reduced sulfur (TRS) in support of the New Source Performance Stan-^
dards for Kraft mills.
2. Range and Sensitivity
2.1 Range. The maximum range of the flame photometric detector for
each sulfur compound is about 1 ppm. This range is expanded by the a-
mount of sample gas dilution employed before analysis. Kraft mill gas
samples are normally diluted 10:1,and therefore the upper range is 10 ppm.
2.2 Sensitivity. The minimum detectable concentration is less than
0.5 ppb.
3. Interferences
3.1 Moisture. Condensation in the analytical column and FPD burner
block may cause interferences. This potential is eliminated by condition-
ing the sample with dilution air to lower its dew point below the operating
Sulfids gases, hydrogen, and c;;ygen. form toxic or flamable mixtures.
Work with these materials in a well-ventilated area.
-------
~- 2
temperature of the GC/FPD analytical system prior to analysis.
3.2 Carbon Dioxide and Carbon Monoxide. The concentrations of CCL
and CO in Kraft mills have a substantial desensitizing effect on the
detector even after 10:1 dilution. .The operating cohditions described in
this procedure eliminate this interference because C02 and CO are eluted
with the "air peak" prior to elution of any sulfur compound.
3.3 Particulate Matter. Particulate matter in gas samples causes
interference by eventual clogging of the analytical system. This inter-
ference is eliminated by use of a filtered probe described in Section 5.
4. Precision and Accuracy
*
4.1 Precision. Repeated analyses of the same standard sample, at any
dilution, should not exceed 5% relative standard deviation.
4.2 Accuracy. The accuracy is dependent on the accuracy of calibra-
tion standards used and the sample dilution employed. Permeation tube
standards are considered primary standards. When the analytical systems
are calibrated as described in Section 8, the error in analysis of other
permeation tubes or compressed gas standards, at any required dilution,
^
should not exceed 10%.
5. Apparatus
5.1 Sampling (Figure 16-1)
5.1.1 Probe. Stainless steel or sheathed borosilicate glass
equipped with a glass wool filter to remove particulate matter. The ex-
posed portion of the probe between the sample line and sampling port should
be heated with heating tape.
-------
5.1.2 Sample Line. 3/16 inch inside diameter FEP Teflon^ '
tubing, heated above 100ฐC.
5.1.3 Sample Pump. Leakless Teflon coated diaphragm type or
equivalent. The pump head should be heated above 100ฐC.
5.2 Dilution System. A schematic diagram of the dynamic dilution
system is given in Figure 16-1.-. Alternate-dilution systems may be used
if they meet specifications shown in the addenda 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.
A 10/1 dilution of sample is accomplished by combining 150 cc of sample
with 1350 cc of clean dry air as shown in Figure 16-1.
5.2.2 Valves. Three-way Teflon solenoid or manual type.
5.2.3 Tubing. Sufficient Teflon fittings and tubing to assure
that all sample and calibration gas contacts are Teflon.
5.2.4 Box. Insulated box, heated and maintained above 100ฐC, of
sufficient dimensions to house dilution apparatus.
5.2.5 Flowmeters. Rotameters or equivalent to measure flow from
0 to 1500 ml/min +_ 1.0% per dilution stage.
5.3 Kraft Mill Analysis. Two types of columns are used for separation
of low and high molecular weight sulfur compounds.
5.3.1 Analytical system for measurement of low molecular weight
sulfur compounds (GC/FPD-1), (See Figure 16-2 and Addendum A). Separation
Column - 36 feet by 0.085 inch inside diameter Teflon tubing packed with
(1)Mention of trade names or specific products does not constitute an en-
dorsement by the Environmental Protection Agency.
-------
4
30/60 mesh Teflon coated with 5% polyphenyl ether .and 0.05% orthophos-
phoric acid, or equivalent.
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,actuated by compressed air.
5.3.4 Oven. For containing sample valve, stripper column and
separation column. The oven should be capable of maintaining an elevated
temperature 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
-9-4
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.
5.3.11 Analytical System for Measurement of High-molecular Weight
Sulfur Compounds (GC/FPD-II). (See Figure 16-2 and Addendum A). 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 equivalent.
5.3.12 Sample Valve. Teflon six-port gas sampling valve equipped
-------
5
with a 10 ml sample loop, actuated by compressed air.
5.3.13 Other Components. All other components same as in
5.3.4 to 5.3.10.
5.4 Calibration. Permeation tube system (Figure 16-3).
5.4.1 Tube Chamber. Glass chamber of sufficient dimensions to
house permeation tubes.
' 5.4.2 Flowmeter. Rotameter or equivalent or measure flow range
from 0 to 10 1/min + 1.0%.
5.4.3 Constant Temperature Bath. Capable of maintaining permea-
tion tubes at certification temperature within +_0.1ฐC.
5.4.4 Temperature Monitor. Thermometer or equivalent or monitor
*
bath temperature within j^0.1ฐC.
6. Reagents
6.1 Fuel. Hydrogen (H2) prepurified grade or. better.
6.2. Combustion Gas. Oxygen (02) research purity or better.
6.3 Carrier Gas. Nitrogen (N,,) prepurified grade or better.
6.4 Diluent. Air containing less than 0.5 ppb total sulfur compounds
> (1}
and less than 10 ppm each of moisture and total hydrocarbons. MSAV ' fil-
ters are used to purify compressed air.
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
(T)Mention of trade names or specific products does not constitute an en-
dorsement by the Environmental Protection Agency.
-------
-- 6
may be purchased commercially. If commercial instruments are used, follow
the specific instructions given in the manufacturer's manual.
7.2 Sampling. Calibrate the dilution and analysis systems as de-
scribed in Section 8. Heat and maintain the sample Tine, pump and dilution
apparatus above 100ฐC. Check the sampling system for sample losses and leaks
by introducing a known concentration of hydrogen sulfide (H2S) into the
probes 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
5%, 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 re-
quired to maintain the sample below its ambient dew point. Usually, ten to
one will suffice. Condition the entire system with sample for approximately
15 minutes prior to commencing analyses.
7.3 Analysis of Kraft Mill Sulfur Compounds. Aliquots of diluted sam-
ple are injected simultaneously into both GC/FPD analyzers for analysis.
GC/FPD-I is used to measure the low-molecular weight reduced sulfur compounds.
The low molecular weight compounds are hydrogen sulfide, sulfur dioxide,
>
methyl mercaptan, ethyl mercaptan, and dimethyl sulfide. GC/FPD-II is used
to resolve the high-molecular weight compounds. The high molecular weight
compounds are propyl mercaptan, butyl mercaptan, dimethyl disulfide, dipropyl
sulfide, and dibutyl sulfide.
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.
-------
7
The valve is then de-actuated for approximately fifteen minutes in which
time, the analytical column continues to be foreflushed, the stripper
column is backflushed, and the sample loop is refilled.. Monitor the
responses. The elution time for each compound will be determined during
calibration. The chromatographic 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/min,oxygen flow of 20 ml/min and sample flow rate between 20 and
80 ml/min.
7.3.2 Analysis of High-molecular Weight Sulfur Compounds. The proce-
dure is essentially the same as above except that no stripper column is
needed. The operating conditions are also the same with the exception of
*a
an oven temperature of 70ฐC and nitrogen carrier gas flow of 100 ml/min.
f
8. Calibration
8.1 General Considerations. Accurately known concentrations (+_ 1%)
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 sul-
fur compound as a permeant./ These tubes consist of hermetically sealed FEP
Teflon tubing in which a liquefied gaseous substance is enclosed. The en-
closed gas permeates through the tubing wall at a constant rate. When the
temperature is constant, 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
-------
8
apparatus as depicted in Figure 16-3. Insert the permeation tubes into
the glass tube chamber. Check the bath temperature to assure agreement
with the calibration temperature of the tubes within j^0.1ฐC. 30ฐC is
recommended for the sulfur gas tubes. 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 cali-
brating the analytical and dilution systems. The airflow across the tubes
must at all times exceed the flow 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 = K -^ Equation 16-1
Where: C = concentration of permeant produced.in ppm.
P = permeation rate of the tube in ug/min.
M = molecular weight of the permeant (9 )
> *
L = flow rate of air over permeant @ 20ฐC, 760 mm Hg.
K = gas constant at 20ฐC.and 760 mm Hg = 24.04 1/g mole
^
8.3 Calibration of GC/FPD Analysis Systems. Generate a series of
known concentrations (usually three) spanning the linear range of the FPD
(approximately 0.01 to 1.0 ppm) for each sulfur compound anticipated to be
present in the gas stream analyzed. Inject these standards into the GC/FPD
analyzers and monitor their responses. -Peak heights, rather than integrated
areas, have proven satisfactory.
-------
9. Calculations
9.1 Determine the concentrations of each reduced sulfur compound de-
tected directly from the calibration curves.
9.2 Calculation of TRS. Total reduced sulfur wjll be determined for
each analysis made by summing the concentrations of each reduced sulfur
compound resolved during a given analys'is.
TRS = Z (H2S, MeSH, DMS, 2DMDS, x ) d Equation 16-2.
Where :
TRS = total reduced sulfur in ppm, wet basis.
H2S = hydrogen sulfide, ppm.
MeSH = methyl meraptan, ppm.
ซ
DMS = dimethyl sulfide, ppm. ;
DMDS = dimethyl disulfide, ppm.
x = other reduced sulfur compounds
d = dilution factor, dimensionless.
9.3 Average TRS. The average TRS will be determined as follows:
N
TRS -
' TRS "
N (1 - Bwo)>
Where :
Equation 16-3.
Avg. TRS = average .total reduced sulfur in ppm, dry basis.
TRS. = total reduced sulfur in ppm as determined by Equation 16-2.
N = number of analysis performed.
Bwo = fraction by volume of water vapor in the gas stream as de-
termined by Method 4 - Determination of Moisture in Stack
Gases (36 FR 24887).
-------
10
10. Bibliography
a. O'Keeffe, A. E. and Ortman, G. C., "Primary Standards for
Trace Gas Analysis", Anal. Chem. 38,760 (1966)..
b. Stevens, R. K., O'Keeffee, 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).
c. Mulick, J. D., Stevens, R. K., and Baumgardner, R., "An Analytical
System Designed to Measure Multiple Malodorous Compounds Related to Kraft
Mill Activities", Presented at the 12th Conference on Methods in Air Pol-
lution and Industrial Hygiene Studies, University of Southern California, '
Los Angeles, Ca., April 6-8, 1971.
d. Devonald, R. H. Serenius, R. S., and Mclntyre, A. D., "Evaluation
of the Flame Photometric Detector for Analysis of Sulfur Compounds", Pulp
and Paper Magazine of Canada, 73, 3 (March, 1972).
e. Grimley, K. W., Smith, W. S., and Martin, R. M., "The Use 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.
-------
ADDENDA-
A. Performance Specifications .for-Gas Chromatographic - Flame Photome-
tric Analyzers.
Range (linear) 0 to 1 ppm
Output (minimum) 0 to 1 MV full scale
at 1 K-ohm
Minimum Detectable Sensitivity 5 ppb
Precision (minimum) 5ซ relative standard devia-
tion
Noise (maximum) + 1% of full scale
*
Oven Stability + 0.5ฐC
B. Specifications for Dynamic Dilution Systems.
Design The dilution system shall
be constructed such that
all sample contacts are
made of inert materials.
Also, the dilution system
shall heat and maintain the
sample above 100ฐC both
prior and during dilution.
Range The dilution system shall be
capable of a minimum ten to
one dilution.
-------
Capacity
Drift
Precision
C. Definitions of Performance Specifications
Range
Output
Full Scale
.Minimuir, Detectable Sensitivity
.The capacity should be in
excess of that required for
analysis. The excess will be
vented to the atmosphere.
Output shall not change more
than +_ 2% over a 24-hour unad-
justed continuous operation.
+_ 2% of dilution factor.
The minimum and maximum mea-
surement limits.
Electrical signal which is
proportional to the measure-
6
ment; intended for connection
to readout or data processing
devices. Usually expressed as
millivolts or mi Hi amps full
scale at a given impedance.
The maximum measuring limit
for a given range.
The smallest amount of input
concentration that can be de-
tected as the concentration
approaches zero.
-------
Accuracy
Precision
Noise
Interference
The degree of agreement be-
tween a measured value and
the true value; usually ex-
pressed as +_ percent of full
scale.
The degree of agreement be-
tween repeated measurements cfr
the same concentration, ex-
pressed as the average devia-
tion of the single results
from the mean.
ซ
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.
-------
To Instruments
and
Dilution System
/,
\
.
Thermometer
-f
t'.'
I-
f
r
i
x~
H /i
M P
" "; ri!
Permeation
Tube
.
c^i Flownetcr
1
p:^j ' Drier
V ^ J 1
ป r
1
Stirrer
r& J>
T..^ .:. >
fri?
^ ' '
Constant
Temp era turd
Bath
Clans
Chamber ^ * ' .
Air
Nitroccn
FIGURE 16-3. APPARATUS FOR FIELD CALIBRATION
-------
tripper
Sc-pling Valve for
U
N,
Vccuun Ccrrier
Scr.ple
Loop
Sc-ole
Vent
ier
1 iTTT-1'-'1
Calibration
Gas
Flcir.c Photctnetric Detector
cxruiust
750V
Pover Supply
rr>- To GC/FPD-II
FICUriK 16-2. GAS ei:rxO;-;ATOCnA?IIIC-PLAKE PHOTOMETRIC
-------
Stack
''Wall
Probe ; Filter
Filter p
(jlasc wool) i
T~
" v . !
. \
^^
Heated X
Scir.ple
Line
ป i
'
Permc
7,
i. \
Tilir
VOซL x L.
c
\.
rx_
;.; M
;> Dicphrap:
. p-jnp
(Heated)
To GC/FPD Analysers
Gns
10:1
A
102:1
103:1
Dilution Box Heated
To 100ฐC
r ~ "
<
'' i
f
i
I .
i '.
. i .
Ion . .
tion |
ป ' ,' .
!
1
1
C=J ,
!
I
It
IA
e
\s
!
5
^
r:/-
1
I
ซ
4
;
K
IX
_x
J
^*
0
1
-v
7
u
(150 cc/min).
> 3 - Wjy
-^ Valvq
1 '
r r V '
^^ "'i_-^-
. *"
J
Dil
^
f
>
.UG
i
.r
.
ht
Ai
<
(
P-
::
* ^-
i
5 V C
1
\
:ie
cy
f
Jf
> c
X
an
Aii
3.
X
i
>5
ป
1350 cc/n:Ln
' Flovset-jr
Vent
FIGURE 16-1. SAMPLING AND DILUTION APPARATUS,
r
------- |