oEPA
United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
4MB Report No. 80-INC-1
March 1982
Air
Evaluation Of An Oil-
Fired Incinerator
Emission Test Report
NVF, INC.
Kennett Square, Pennsylvania
-------
Final Report
SET 1935 01 0681
EVALUATION OF AN OIL-FIRED
THERMAL OXIDIZER
Contract No. 68-02-3544
Work Assignment 4
EPA Technical Manager: Winton Kelly \
Field Testing Section
Emission Measurement Branch
OAQPS
U. S. Environmental Protection Agency
Research Triangle Park, NC 27711
March 1982
SCOTT ENVIRONMENTAL SERVICES
A, Division Of
SCOTT ENVIRONMENTAL TECHNOLOGY, INC.
Plumsteadville, Pennsylvania 18949
Scott Environmental Technology Inc.
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TABLE OF CONTENTS
f
Page
1.0 INTRODUCTION 1-1
2.0 SUMMARY OF RESULTS AND CONCLUSIONS 2-1
2.1 PHASE I TESTING 2-1
2.2 PHASE II TESTING \.2-3
2.3 PHASE III TESTING 2-4
2.4 CONCLUSIONS 2-4
3.0 RESULTS AND DISCUSSION 3-1
3.1 PHASE I TESTS 3-9
3.2 PHASE II 3-9
3.3 PHASE III 3-9
4.0 DESCRIPTION OF PROCESS AND CONTROL EQUIPMENT
4.1 SOURCES OF SOLVENT VAPORS . 4-1
4.2 DESCRIPTION OF INCINERATOR 4-1
5.0 DESCRIPTION OF TEST PROGRAM 5-1
5.1 PHASE I TEST PROGRAM 5-1
5.2 PHASE II 5-1
5.3 PHASE III 5-5
6.0 SAMPLING AND ANALYSIS METHODOLOGY 6-1
6.1 PARTICULATE SAMPLING 6-1
6.2 HYDROCARBON MEASUREMENTS 6-3
6.3 NITROGEN OXIDES 6-7
6.4 CALIBRATION STANDARDS 6-8
6.5 CARBON DIOXIDE, CARBON MONOXIDE AND OXYGEN 6-9
6.6 MOISTURE , 6-9
6.7 FLOW MEASUREMENTS 6-9
7.1 QUALITY CONTROL AND QUALITY ASSURANCE 7-1
7.1 SAMPLING PROCEDURES 7-1
7.2 ANALYTICAL QUALITY CONTROL ; . . 7-2
Scott Environmental Technolosy Inc
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1-1
SET 1935 01 0681
1.0 INTRODUCTION
, Hydrocarbon emission control applications in which recovery of
the exhausted vapors is not cost effective, typically employ destructive
techniquesj such as direct fired afterburners. The applications, opera-
tional characteristics and performance of gaseous fueled incinerators have
been thoroughly documented. Due to an uncertainty in the availability of
gaseous fuels during portions of the year, particularly on the east coast
of the United States, some industries are employing incinerators with
multifuel capability and others are operating direct oil fired afterburners.
In order to supplement the data base compiled on gaseous fired
incinerators, the Emission Measurement Branch of the U.S. EPA, OAQPS con-
tracted Scott Environmental Technology, Inc. to study the performance of
an oil fired incinerator installed at NVF Company, Kennett Square, Pennsyl-
vania. The specific operational considerations under investigation included
the hydrocarbon destruction efficiency and emissions at various incinerator
operating temperatures and the contribution of the fuel to the organic carbon
emissions.
The performance of this investigation was directed toward achieving
the following program objectives.
Determination of the contribution of residual oil combustion
products to the VOC in the emissions from an oil fired thermal
incinerator.
Determination of the VOC destruction efficiency of this unit
as a function of temperature.
Determination of the typical incinerator emission range and
the effect of operating temperature on each emission parameter.
Determination of the capability of predicting incinerator
performance from one operating parameter e.g. incinerator
temperature.
Evaluation of measurement methodology for the determination
of VOC from oil fired afterburners.
The testing program was conducted in three, phases. The objectives'
of the first phase were to provide a complete emission characterization of
the unit under evaluation at three selected temperatures with and without
the plant process providing hydrocarbons for destruction. The second phase
Scott Environmental Technology Inc.
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1-2
SET 1935 01 0681
of the program consisted of continuous hydrocarbon monitoring of the incin-
erator outlet during a two month period under normal plant operating con-
ditions. The third phase of the testing program studied incinerator hydro-
carbon destruction efficiency in the 1200° to 1400° range.
Phase I was performed February 4 through 8, 1981.. Phase II was
conducted during April and May 1981 and Phase III was carried out on May 13
and 14, 1981. The Scott personnel responsible for this work assignment
were Gilbert Maines, Project Manager; Thomas Bernstiel, Chemist; and Timothy
Travers, Mark Daly and John Carney as the field crew.
Scott Environmental Technology Inc.
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2-1
SET 1935 01 0681
2.0 SUMMARY OF RESULTS AND CONCLUSIONS
2.1 PHASE I TESTING
, The pollutant concentrations in the emissions from the oil-fired
incinerator during Phase I of the test program are presented in Table 2-1
along with process flow and temperature data. During normal process
operation, the hydrocarbon destruction efficiency based on mass averaged
91.3% at an incinerator temperature of 1200°F and 99.8% at temperatures of
1400 and 1500 F. With the coating processes not in operation and room
air passing through the incinerator, the outlet non-methane hydrocarbon
concentration was 16 ppm-C at 1200°F and 1 ppm-C at 1400°F and 1500°F.
The nitrogen oxides concentration in the incinerator outlet ranged
from 23 to 81 ppm. The concentration increased with increasing incinerator
temperature. Carbon monoxide was present at an average concentration of
1830 ppm at the "1200 F, process on" test point. Carbon monoxide was not
detected at the other test conditions. Carbon dioxide increased with in-
cinerator temperature as additional fuel combustion was required to
achieve the set operating temperature.
An estimate of particulate loading at the inlet and outlet gas
sampling points was made from the weight of material collected on glass
fiber filters during each run. These heated filters were used to remove
particulate from the streams flowing to the gas analyzers. The process
streams were sampling at only one point, the center of the stack, at non-
isokinetic conditions. The results are presented for comparison only,
and they do not represent particulate loadings determined by any recognized
method.
' The outlet particulate concentration ranged from 0.009 to 0.032
grains per standard cubic foot (gr/SCF) with an average of 0.015 gr/SCF.
The corresponding inlet particulate was 0.001 gr/SCF. There was no con-
sistent difference between outlet particulate with and without the process
on. It thus appears that the particulate is a result of fuel combustion.
The mass of particulate emitted never exceeded 0.5% of the mass of fuel
burned, and extraction with solvents showed that less than 10% of the
particulate was organic.
2.2 PHASE II TESTING
The maximum daily one-hour average hydrocarbon concentrations
recorded during the continuous monitoring program are shown in Table 2-2.
Scott Environmental Technology Inc.
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©
Scott Environmental Technol
o
M Incinerator
v^
__ Run Temperature
2 No. °F
1 1200
2 1200
3 1200
10 1200
11 1200
4 1400
5 1400
6 1400
13 ~1400
14 1400
7 1500
8 1500
9 1500
16 1500
17 1500
TABLE 2-1 SUMMARY OF
Process
On/Off
On
On
On
Off
Off
On
On
On
-Off "
Off '
On
On
On
Off
Off
Flow Rate
(SCFM)
35000
36400
36500
35500
35800
36100
36700
35500
~ 38900
26600
35600
36200
35600
29800
32500
Inlet
NMHC*
ppm-C
5700
6410
5080
55
22
6100
5440
5220
"29 ~
18
5860
3950
3250
28
23
PHASE I DATA
Outlet
VOC Mass
Ib/hr
371
434
345
3.6
1.5
410
371
345
- "2.1
0.9
388
266
215
1.6
1.4
Flow Rate
(SCFM)
45800
38400
43300
41800
42100
42600
42200
''43000
41500
37200
39000
43600
47500
NMHC*
ppm-C
405
456
405
17
16
16
4.4
1.9
"""1.3 \-~
0.7
3.1
6.3
5.4
0.2
0
CO
(ppm)
1700
1910
1870
ND
ND
ND
ND
ND
ND '~
ND
ND
ND
ND
ND
ND
C02
(%)
1.56
1.72
2.18
2.02
2.16
2.98
2.89
2.65
"2.64
2.92
3.13
2.91
3.11
3.21
3.20
°?
18
18
18
17.8
16.8
18
19
1R
16 " *"'
16.6
17.2
16.8
16.5
16
16
NOX
(PPm)
23
32
49
46
42
52
44
53
64
64
61
63
65
70
81
VOC Mass
Ib/hr
^-
39
29
1.4
1.2
1.3
0.3
0.1
b.r
0.1
0.2
0.5
0.4
0.02
0
Particulate
gr/SCF
0.009
0.011
0.013
0.013
0.014
0.016
~ ' 0.012
0.010
0.032
0.015
0.020
HC Destruction
Efficiency
(% - Mass Basis)
91.0
91.6
99.7
99.9
100.0
99.9
99.8
99.8
en
pi
H
S
o
o
a*
00
K)
1
ND = Not Detected
* Based on gas chromatographic analyses.
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2-3
TABLE 2-2
MAXIMUM ONE HOUR NMHC CONCENTRATIONS - INCINERATOR OUTLET
Max 1 Hour NMHC
Date ppm-C
4/29/81 41
4/30/81 39
5/1/81 42
5/2/81 44
5/4/81 41
. 5/5/81 60
5/6/81 26
5/7/81 21
5/8/81 20
5/9/81 29
Scott Environmental Technology Inc.
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2-4
SET 1935 01 0681
During this period the incinerator was operated at a nominal temperature
of 1400 F. Based on typical inlet concentrations measured in other program
phases, the hydrocarbon destruction efficiency of the incinerator was 99%
or greater at all times.
2.3 PHASE III TESTING
The inlet and outlet hydrocarbon concentrations at the various
incinerator temperatures used in the Phase III testing are summarized in
Table 2-3 along with hydrocarbon destruction efficiency. Inlet data in
brackets were determined by interpolation. The temperature vs. efficiency
data are plotted in Figure 2-1. The efficiency ranges from 93% (91% on
mass basis) at 1200°F to greater than 99% at 1400°F which is in close
agreement with the Phase I results.
2.4 CONCLUSIONS
The three-phase test program of an oil fired incinerator
demonstrated that 99% reduction in inlet hydrocarbons can be accomplished
at operating temperatures of 1300 F and higher. When the operating
temperature is lowered to 1200 F, the reduction in hydrocarbons falls to
approximately 91% expressed on a mass basis. The slope of the temperature
vs. efficiency relationship changes rapidly between about 1250 and 1300 F,
indicating that for the test unit, this is the minimum temperature for good
combustion. Monitoring incinerator operating temperature should provide a
means for accurately estimating hydrocarbon destruction efficiency.
There was no evidence of unburned fuel (No. 6 oil) components
o
in the incinerator emissions in any of the test runs. At 1200 F the
contribution of fuel derived components to the hydrocarbon emissions is
at least an order of magnitude lower than that of the solvent and solvent-
derived components. This occurs despite the fact that approximately five
pounds of fuel are needed to heat each pound of solvent hydrocarbons to the
required operating temperature.
By operating the incinerator at 1400 F, NVF was able to maintain
a hydrocarbon reduction efficiency of 99% or higher at all times in an
extended continuous monitoring period. The use of the waste heat in the
incinerator exhaust to produce steam for process operation permits recovery
of the cost of much of the fuel used to combust the solvent emissions.
Scott Environmental Technology Inc.
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2-5
TABLE 2-3
INCINERATOR HC DESTRUCTION EFFICIENCY - PHASE III
Test 1 - 5/13/81 - Increasing Incinerator Temperature
Incin. Temp.
°F
1190
1220
1240
1270
1290
1320
1340
1375
1400
Test
Incin. Temp.
op
1390
1360
1330
1305
1260
1235
1220
1200
Inlet NMHC
ppm-C
2650
2920
(3050)
3170
2760
2920
2450
2380
2510
2 - 5/14/81 - Decreasing
Inlet NMHC
ppm-C
1170
3620
3560
3220
(2930)
2650
3750
3540
Outlet NMHC
ppm-C
187
135
92
32
20
13
19
3
12
Incinerator
Outlet NMHC
ppm-C
2
29
36
42
84
89
250
147
HC Destruction
Effic., %
92.9
95.4
97.0
99.0
99.3
99.6
99.2
99.9
99.5
Temperature
HC Destruction
Effic., %
99.8
99.2
99.0
98.7
97.1
96.6
93.3
95.8
*Based on concentration.
Scott Environmental Technology Inc.
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2-6
ioo-\
9*-
Hydrocarbon
Destruction
Efficiency
:o 0
Incinerator Operating Temperature °F
*Based on concentration.
Scott
Environmental
Technology
Inc.
FIGURE 2-1: NVF COMPANY, KENNETT SQUARE, PENNSYLVANIA
INCINERATOR CONTROL EFFICIENCY AT VARIOUS OPERATING
TEMPERATURES
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3-1
SET 1935 01 0681
3.0 RESULTS AND DISCUSSION
, This section presents the detailed results of the three-phase
test program of the oil-fired incinerator. Testing was conducted at: the
incinerator inlet, the heat exchanger outlet, and the waste heat boiler
outlet, which are shown in Figure 4-1. The significance of the results
are discussed in terms of the overall program objectives.
3.1 PHASE I TESTS
3.1.1 Gas Flow Data
The measured incinerator inlet and outlet flow rates are presented
in Table 3-1 along with indicated inlet flow rate by the plant's annubar
system. The flow rate is of interest in determining if the design residence
time of 0.7 seconds at 40,000 SCFM was being held during the program. The
data show that the measured outlet flows were consistently 10 to 20% higher
than the inlet flow. In fact, the total outlet flow remained near 40,000
SCFM even when the inlet flow dropped below 30,000 SCFM in the "process-off"
tests. This indicates that the forced draft fan was drawing in ambient air
through a damper or hole. However, this was not discovered during the testing
during an examination of the system. The addition of ambient air would
result in a proportional dilution of the measured inlet hydrocarbon concen-
trations which were sampled near the inlet flow measurement point. Thus,
the incinerator's efficiency must be calculated on a mass basis rather than
directly from the measured concentrations.
The plant annubar indicated inlet flows of approximately 70%
of the measured values. The annubar appears to be installed too .close to
a bend in the line to read accurately, but it does reflect flow rate changes.
3.1.2 Incinerator Operating Parameters
The various operating parameters of the incinerator system and
resulting stack temperatures are summarized in Table 3-2. All of these
data were recorded by NVF process instrumentation. The fuel flow rate was
recorded by the inlet fuel meter as the return flow fuel meter did not change
reading during the tests. Subsequent physical examination of the fuel
system indicated that some fuel was in fact returned to the storage tank
but it was not possible to determine the return flow rate. Thus, a carbon
balance cannot be derived for the system because of the uncertainty in the
fuel consumption rate.
Scott Environmental Technofosy Inc
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©
I
3 Run
X No.
j£ 2
1 3
V^ A
? 5
6
7
8
9
10
11
13
14
16
17
Inlet
Temp.
207
217
,212
214
216
223
206
208'
205
236
243
251
252
222
215
Indicated
Flow (scf
27000
27000
27000
26000
26000
27000
27000
26000
26000
20000
19000
20000
TABLE 3-1
PHASE I GAS FLOW MEASUREMENTS
Measured Flow
ml (acfm)
45,340
47,310
46,920
46,470
47,340
46,320
45,450
46,540
45,560
48,290
49,260
40,290
39,510
39,430
42,780
(scfm)
34,970
36,370
36,480
36,130
36,690
35,530
35,590
36,160
35,600
35,460
35,790
28,900
28,240
29,800
32,450
Heat Exchanger
T(QF)
396
377
362
373
391
383
350
377
358
361
314
319
356
-
acfm
29,260
22,900
21,170
25,500
26,030
16,680
18,800
25,930
22,900
23,000
18,880
18,550
22,200
-
scfm
-
17,430
14,100
13,260
15,760
15,750
10,140
11,840
15,810
14,040
14,050
12,190
11,890
13,720
-
Outlet
Waste Heat Boiler
T(UF)
346
365
351
331
368
367
377
371
375
363
359
357
351
353
-
acfm
37,430
45,840
38,270
44,380
43,210
42,530
44,260
44,226
45,500
47,970
46,900
51,400
48,010
54,480
-
scfm .
23,630
28,330
24,330
28,870
26,870
26,470
27,080
27,140
27,810
29,230
27,710
31,400
29,560
33,780
-
CO
w
H
vo
Ul
Total °
scfm o
OO
I--
45,760
38,430
42,130
42,630
42,220
37,220
38,980
43,620
43,270
41,760
43,590
41,450
47,500
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3-3
SET 1935 01 0681
TABLE 3-2 INCINERATOR OPERATING DATA - PHASE I
Run
No.
1
2
3
10
11
4
5
6
13
14
7
8
9
16
17
Fuel
Oil
Flow
QaL/hr.
234
233
235
228
295
257
255
263
260
259
270
290
298
336
458
Fuel
Oil
Temp.
°F
207
208
205
202
208
202
204
202
201
201
206
204
206
205
206
Fuel
Oil
Press.
PSIG
122
121
121
121
121
122
122
122
122
122
121
122
121
123
122
Incin.
Unit
Temp.
oF
1202
1202
1205
1200
1200
1400
1400
1400
1400
1400
1500
1498
1498
1500
1500
Heat
Exch.
Stack
Temp.
°F
480
486
480
460
460
460
480
480
410
400
490
460
480
460
480
WHB
Stack
Temp.
op
400
400
404
400
400
415
415
415
395
390
420
424
425
390
400
Steam
Flow
Rate
#/Hr
27500
30500
25500
26000
26000
35000
35500
35000
30000
27000
36500
36500
34000
31500
__
Unit
Flow
Rate
SCFM
27K
27K
27K
26K
26K
26K
26K
27K
2 OK
19K
27K
20K
___
Exhaust
Gas
Damper
Setting
WHB/^
60/40
60/40
60/40
55/45
55/45
60/40
60/40
60/40
60/40
Various
60/40
60/40
60/40
*A11 data were recorded by plant instruments.
Scott Environmental Technolosy Inc
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3-4
SET 1935 01 0681
The stack temperatures reflect variations in damper settings and
steam flow rate demand. They have no impact on pollutant emission rates.
3.1.3 Total Hydrocarbons (VOC)
The hydrocarbon concentrations in the inlet and outlet streams
of the incinerator were measured by three separate methods: continuous
flame ionization detector, gas chromatography, and EPA Method 25. It can
be seen from Table 3-3 that there are significant differences between
data obtained by the three methods. The gas chromatographic results are the
most rigorous measurements and are used as the reference for comparisons.
At the inlet, the GC and Method 25 data are in general agreement, with
the FID results substantially lower during the "process on" tests. The
FID data are analyses of the same integrated bag samples analyzed by GC,
so any differences are due solely to the methods employed. It is possible
that the FID data are in error because the sample flow from the bags was
too low or became mixed with ambient air via a leak. The span gas and
outlet samples were transferred to the FID from pressurized lines which
would have prevented dilution by leakage and probably yielded a higher
sample flow. The possibility of loss of linearity at high concentrations
was probed later in the laboratory, but did not appear to be capable of
producing the observed differences. The "process off" FID and GC data agree
well.
The total hydrocarbon data for the outlet stream by FID and GC
are in reasonably good agreement. The FID data are averages of continuous
readings recorded throughout each run. The GC data are analyses of in-
tegrated bags collected during the same period. The Method 25 outlet data
all appear to be erroneously high with most being from 500 to 700 ppm
higher than GC/FID data. A few samples, collected in new traps which must
have contained residual carbonaceous material, gave absurd results as high
as 21,000 ppm. The source and nature of the material which, upon combustion
produced the high C0« concentrations which in turn led to the high VOC
results is not known.
3.1.4 Individual Hydrocarbons in Inlet and Outlet Streams
The concentrations of hydrocarbons in the incinerator inlet and
outlet streams at the three incinerator operating temperatures are shown
in Tables 3-4 and 3-5 respectively. The inlet stream varied in concentration
Scott Environmental Technology Inc.
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X1
8
3
i
i
*
3T
w
v;
8
TABLE 3-3
CO
HYDROCARBON CONCENTRATIONS IN INCINERATOR INLET AND OUTLET AT VARIOUS OPERATING TEMPERATURES H
VD
Hydrocarbon Concentration (ppm-C)
Run
No.
1
2
3
10
11
4
5
6
13
14
7
8
9
16
17
Process
On/Off
On
On
On
Off
Off
On
On
On
Off
Off
On
On
On
Off
Off
Incinerator
Temp., °F
1200
1200
1200
1200
1200
1400
1400
1400
1400
1400
1500
1500
1500
1500
1500
Inlet
FID
1775
2000
1900
__
31
2425
2300
1725
38
32
1975
850
925
38
31
GC
5700
6413
5081
60
26
6101
5440
5219
32
21
5857
3945
3254
31
26
Method 25
6072
6243
3128
__
._
Cyl. Leaked
5374
Trap Leaked
4482
5056
Trap Leaked
FID
328
376
321
11
16
17
5
4
2
2
3
2
2
3
2
Outlet M
GC
405
456
405
17
16
16
4
2
1
1
3
6
5
0
0
Method 25 o
ON
1097
1102
1232
697
12020
770
652 V
V
20700
483
16600
10430
21300
592
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TABLE 3-4
intal Technology Inc
i
Incinerator Temperature:
Process' On/Off:
Run Number:
Constituent
Methane
Methanol
Ethanol
Acetone
Methyl Ethyl Ketone
Methyl CellosoJ.ve
Unknown A
Unknown B
Unknown C
Unknown D
Unknown E
Unknown F
Toluene
Xylene
Others
Total ppm C-,
1
2.7
2323
1473
1380
482
4.3
4.9
0.9
2.3
27.0
5700
CHROMATOGRAPHIC ANALYSIS, INCINERATOR INLET HYDROCARBONS - PHASE I
(ppm-C)
1200°F 1400°F
On
2 3
2.7 1.7
1750 544
1226 788
1348 1288
1183 1151
866 1277
1.1
17.8 13.8
19.2 2.5
14.3
6413 5081
Off
10 11 4
4.9 3.8 3.1
1177
1081
4.8 5.0 1352
22.9 13.9 1103
1355
16.8
2.5 2.8 2.1
7.7
16.8 10.8
59.6 25.5 6101
On
5
3.8
637
1009
1308
1142
1301
16.8
2.3
19.9
5440
Off
6 13
6.6 3.4
142
876
1526 10.7
1128 15.3
1435
34.2
17.4
20.6
1.5 2.5
23.8
8.0 ';
5219 31.9
14 7
3.5 2.6
66.2
70.2
3.4 898
12.4 3275
617
6.6
4.4
3.2
3.6
8.9
3.5
2.0 881
16.9
21.3 5857
en
M
H
h-1
VO
LJ
1500"F o
On Off o
8 9 16 17 P
2.8 2.8 3.7 3.4
136 120
70.9 49.3
761 894 13.1 8.2
1628 1009 12.5 12.7
948 1153 ^
0.9
1.8
1.6 0.7
1.4
4.7
373 25.2 1.9 1.9
14.4
3945 3254 31.2 26.2
-------
TABLE 3-5
X1
Incinerator Temperature:
~~ Process On/Off:
?F
3- Run Number:
2 Constituent
cT Methane
5
Ethylene & Acetylene
Propylene & Propane
Methanol
Ethanol
Acetaldehyde
Acetone & Isopropanol
Methyl Ethyl Ketone
Benzene
Toluene
Total NMHC ppm
IRAPHIC ANALYSIS,
1200°
1
14
111
17
44
13
13
138
65
2
2
405
On
2
16
123
28
72
30
14
123
64
2
456
INCINERATOR OUTLET HYDROCARBONS -
(ppm-C)
F 1400°F
Off
3
15
139
28
26
24
135
51
2
405
1
8
0
2
2
2
0
16
10
.2
.8
.6
.7
.0
.0
.5
.6
1
11
0
0
0
0
0
15
11
.1
.1
.9
.7
.8
.4
.6
.5
0
2
0
6
3
1
0
0
15
On
456
.8 0.8 0.5
.6 2.0 0.9
.3
.7 1.6
.1
.8 0.5 0.5
.7 0.3 0.5
.4
.6 4.4 1.9
Off ..
13 14
0.4 0.3
0.2 0.1
0.5 0.4
0.3
0.3
0.2
1.3 0.7
PHASE I * w
H
M
VO
to
l_n
O
M
1500°F I
On Off "~
7 8 9 16 17
0.4 0.4 0.3 0.6 0.3
1.2 0.8 0.6
0.9 2.4 1.0
0.5 1.0 1.3 0.1
0.5 2.1 2.5 0.1
3.1 6.3 5.4 0.2 0.0
-------
3-8
SET 1935 01 0681
and composition with time as various coating processes were placed in
operation. However, the inlet mixture was always composed of a few major
components including methanol, ethanol, acetone, methyl ethyl ketone and
methyl cellosolve. Toluene was also a major component in Runs 7 and 8
with the alcohols diminished.
At the 1200 F operating temperature, the unburned hydrocarbons
measured at the outlet averaged 420 ppm-C, with a corresponding inlet con-
centration of 5400 ppm-C. The unburned hydrocarbons consisted of both
cool flame partial combustion hydrocarbons (such as ethylene, acetylene,
methane, propylerie, propane and acetaldehyde) and unburned solvents. The
apparent absence of methyl cellosolve in the outlet is probably due to its
very polar nature which makes it difficult to quantify in low concentrations.
The small amount of benzene present is believed to result from incomplete
combustion of the fuel oil aromatics. At the 1400 and 1500 F operating
temperatures, the hydrocarbon concentrations are so low that their composition
is of little practical interest.
When tested without solvent vapor processes in operation and
using room air as the inlet gas mixture, the hydrocarbon emissions averaged
16 ppm-C at 1200 F. Ethylene and acetylene accounted for more than half
of the "process-off" emissions. If it is assumed that all of the "process-
off" emissions are due to the fuel oil, its contribution is only 4% of the
normal "process-on" emissions at 1200 F. AT 1400 and 1500 F the "process-
off" hydrocarbon emissions are 1 ppm-C or less, demonstrating complete fuel
oil combustion.
3.1.5 Other Emissions
The concentrations of C09, 00, CO, NO and particulates in the
£ £- X
incinerator outlet stream were summarized in Table 2-1 and discussed in
Section 2.1. The particulate concentrations are estimates based on a
modified procedure described in Section 6.1.
The NO data were obtained from a chemiluminescence analyzer,
X
and validations were done using triplicate EPA Reference Method 7 de-
terminations during Runs 4, 5, and 6. The results are summarized in
Table 3-6.
Scott Environmental Techndosylnc
-------
3-9
SET 1935 01 0681
TABLE 3-6
, OUTLET NO CONCENTRATIONS
x
(ppm)
Run
No.-
4
5
6
1
35.4
30.6
41.2
Method
2
44.2
52.5
38.3
7 '
3
59.3
42.0
44.3
Avg. Chemiluminescence
46.2
41.7
41.3
52
44
53
3.2 PHASE II
The incinerator outlet stack was monitored continuously for a
period in excess of 30 days using the heated flame ionization detector
(FID). Due to operational problems the data base summarized in Table 3-7
is for 11 days. All data indicated a hydrocarbon destruction efficiency of
99% or greater, based on outlet concentration measurements by FID and inlet
data from Phases I and III. Fifteen minute average outlet hydrocarbon data
and calculated frequency distributions are presented in Appendix B.
Plant operating charts show that the incinerator was always
operated at 1400 F. When the plant shut down on weekends, the incinerator
o
was started up at 1400 F approximately eight hours before the solvent coating
processes began operation. Thus, the only intervals during which solvent
vapors were being processed that the temperature was below 1400 F were
during the low temperature tests.
3.3 PHASE III
In the Phase I tests, the incinerator exhibited a hydrocarbon
destruction efficiency of 99.7% or better when operated at 1400° and 1500 F.
The efficiency decreased to 91.3% at 1200°F. It was desired to explore
efficiencies between operating temperatures of 1200 F and 1400 F to establish
the temperature at which destruction efficiency began to decrease at a
significant rate. This was accomplished in two test runs in which the
operating temperatures were varied in nominal 25 F increments. In the
o o
first test, the temperature was decreased step-wise from 1400 to 1200 F
while in the second test, the temperature was increased over the same range.
One hour was allowed at each temperature to assure system equilibrium.
Scott Environmental Technology Inc.
-------
3-10
SET 1935 01 0681
TABLE 3.7
Summary of Continuous
Outlet Monitoring
Outlet HC (ppm-C)
Date
4/28
4/29
4/30
5/1
5/2
5/4
5/5
5/6
5/7
5/8
5/9
Mean
9.4
15.9
13.0
. 13.3
14.2
16.1
21.8
14.3
9.7
8.4
11.8
Max
16.0
42.7
40.1
45.6
46.5
43.5
61.7
27.1
21.7
20.1
29.8
Min
4.2
1.9
1.9
2.2
1.1
2.5
2.4
4.5
1.7
0.9
4.8
Std.
Dev.
3.6
13.9
12.2
12.7
13.4
14.1
16.8
6.6
6.6
5.7
7.3
Scott Environmental Technology Inc.
-------
3-11
SET 1935 01 0681
It was planned to provide for continuous monitoring of the outlet
hydrocarbon concentration, .however, operational problems, later determined
to be badly contaminated instrument carrier gas, prevented this. Outlet
samples were collected in glass flasks near the end of each one hour test
segment and analyzed by gas chromatography. Inlet samples were collected
in Tedlar bags integrated over each one hour segment and also analys:ed by
gas chromatography.
The incinerator operating parameters as recorded by NVF instru-
mentation for each test segment are summarized in Table 3-8. The instru-
ment charts are included in Appendix A.
The concentrations of total non-methane hydrocarbons and individual
hydrocarbons present in the inlet and outlet streams at each test temperature
are shown in Table 3-9. These data, which were summarized in Table 2-3,
demonstrate that 99% destruction efficiency could be maintained at operating
o o o
temperatures as low as 1270 to 1300 F, arid below 1270 F the efficiency drops
rapidly, falling to approximately 93% on a concentration basis.at 1200 F.
This is equivalent to 91% on a mass basis using flow data from Phase I.
The individual hydrocarbons follow the pattern found in similar
Phase I analyses. The inlet stream contains four solvent hydrocarbons:
methanol, ethanol, acetone and methyl ethyl ketone which account for 99%
of the total. The outlet contains unburned solvent hydrocarbons as well as
cool flame combustion products such as ethylene, acetylene, propylerie and
methane. Of academic interest but little practical importance because of
the low absolute concentration is the fact that acetone is more difficult
to destroy than the other solvent hydrocarbons. Also, acetone and C_ un-
saturates (ethylene and acetylene) accounted for more than half of the
hydrocarbons emitted at all test temperatures. The small but increasing
concentration of benzene present as the temperature was decreased is be-
lieved to result from incomplete combustion of the fuel aromatics because
aromatics were not found in most inlet samples. However, there is no
evidence of any significant hydrocarbon contribution from fuel components.
Scott Environmental Technology Inc.
-------
3-12
SET 1935 01 0681
TABLE 3-8
INCINERATOR OPERATING CONDITIONS - PHASE III
Unit
Temp.
_^F
Run 1
1190
1220
1240
1270
1290
1320
1340
1375
1400
Run 2
1380
1360
1330
1305
1260
1235
1220
1200
(E) Scott
Fuel
Oil
Temp.
°;E .
- 5/13/81
205
201
205
204
204
201
206
201
202
- 5/14/81
204
205
206
205
202
205
205
204
Environmental
Fuel
Oil
Press.
PSIG
124
124
124
124
124
124
124
124
124
124
124
124
124
124
125
125
Incin.
Stack
Temp.
°F
280
450
250
430
250
580
580
440
540
680
500
470
370
520
300
310
125 310
Technolosy Inc
WHB
Stack
Temp.
°F
450
420
450
420
450
410
410
430
420
400
430
440
460
410
460
460
440
Steam
Flow
Rate
K#/Hr
27.5
20.0
28.0
22.0
30.0
19.0
20.0
28.0
26.0
24
27
30
33
26
30
32
31
Unit
Flow
Rate
KSCFM
29
29
28
27.5
28
31.5
31.0
29.0
27.0
/
31
31
31
31
31
33
30
29
Exhaust
Gas
Damper
Setting
WHB/SZ?
65/35
75/25
100/0
95/5
100/0
60/40
60/40
75/25
80/20
45/55
70/30
60/40
65/35
60/40
35/65
70/30
70/30
-------
TABLE 3-9
CONCENTRATION OF INDIVIDUAL HYDROCARBONS IN INCINERATOR INLET AND EXHAUST AS A FUNCTION OF OPERATING TEMPERATURE
(ppm-C)
Run 1 - 5/13/81
Operating Temperature "F
Constituent
Methane
C- Compounds
C, Compounds
Methanol
Ethanol
Acetone
Methyl Ethyl Ketone
Benzene
Miscellaneous
Total NMHC
1400
1375
1340
1320
1290
Inlet
1.6
372
38
755
1333
10
2508
Outlet
1.4
4.1
0.5
1.0
3.3
2.9
11.8
Inlet
1.7
345
35
763
1233
2376
Outlet
0.9
0.7
0.2
0.7
1.2
2.8
Inlet
1.6
423
38
731
1260
2
5
2459
Outlet
2.0
10.0
1.0
0.7
5.4
1.8
0.4
19.3
Inlet
1.6
445
50
849
1480
95
2919
Outlet
1.4
6.8
0.7
0.7
3.6
1.1
0.3
13.2
Inlet
1.6
84
34
875
1590
1
174
2758 .
Outlet
1.5
10.3
0.9
0.5
4.9
2.6
0.5
19.7
CO
1
w
-------
Table 3-9 Continued
CONCENTRATION OF INDIVIDUAL HYDROCARBONS IN INCINERATOR INLET AND EXHAUST AS A FUNCTION OF OPERATING TEMPERATURE
(ppm-C)
Run 1 - 5/13/81
Operating Temperature °F
Constituent
Methane
G£ Compounds
C-j Compounds
Methanol
Ethanol
Acetone
Methyl Ethyl Ketone
Benzene
Miscellaneous
Total NMHC
1270
1240
1220
1190
Inlet
1.6
581
82
803
1436
48
221
3171
Outlet
2.1
16.0
1.7
1.8
8.8
2.9
0.7
31.9
Inlet Outlet
4.9
34.4
4.2
5.0
41.0
4.9
1.0
1.2
2045.5* 91.7
Inlet
1.6
525
143
810
1397
45
2920
Outlet
5.3
61.3
20.8
5.7
0.4
31.1
10.2
2.2
3.6
135.3
Inlet
1.7
500
139
756
1068
189
2652
Outlet
5.0
47.0
15.5
14.4
1.8
72.4
28.4
1.6
5.6
186.7
U)
1
l1
interpolated Value
-------
Table 3-9 Continued
CONCENTRATION OF INDIVIDUAL HYDROCARBONS IN INCINERATOR INLET AND EXHAUST AS A FUNCTION OF OPERATING TEMPERATURE
(ppm-C)
Run 2 - 5/14/81
1390
Constituent
Methane
C, Compounds
C, Compounds
Methanol
Ethanol
Acetone
Methyl Ethyl Ketone
Benzene
Miscellaneous
Total NMHC
1360
Operating Temperature °F
1330
1305
1260
Inlet
1.8
301
15
379
471
1166
Outlet
0.8
0.7
0.1
0.1
0.7
1.6
Inlet
1.7
679
213
1054
1667
5
3618
Outlet
3.4 '
15.2
1.6
1.7
8.1
1.8
0.4
28.8
Inlet
1.7
1079
210
779
1491
5
3564
Outlet
2.3
17.7
2.2
1.8
9.7
1.3
0.6
2.8
36.1
Inlet
1.7
854
223
746
1385
10
3218
Outlet
2.7
20.5
3.3
2.3
10.3
2.3
0.7
3.0
42.4
Inlet Outlet
5.1
36.8
5.1
2.4
21.8
4.6
1.5
1.5
2838* 84.2
»._
OJ
1
^
interpolated Value
-------
Table 3-9 Continued
CONCENTRATION OF INDIVIDUAL HYDROCARBONS IN INCINERATOR INLET AND EXHAUST AS A FUNCTION OF OPERATING TEMPERATURE
(ppm-C)
Run 2 - 5/14/81
Constituent
Methane
C2 Compounds
C.j Compounds
Methanol
EtHanoi
Acetone
Methyl Ethyl Ketone
Benzene
Miscellaneous
Total NMHC
1235
Operating Temperature °F
1220
1200
Inlet
1.7
660
182
651
1124
16
15
2648
Outlet
4.3
37.6
6.4
7.9
0.4
28.2
6.7
1.1
0.8
89.1
Inlet
1.6
887
270
885
1690
14
3746
Outlet
7.2
69.2
20.8
37.3
4.2
84.9
30.3
1.7
1.2
249.6
Inlet
1.6
915
275
898
1440
10
3538
Outlet
5.7
58.8
14.2
9.2
1.2
47.5
13.6
1.5
1.1
147.1
CJ
I
-------
4-1
SET 1935 01 0681
4.0 DESCRIPTION OF PROCESS AND CONTROL EQUIPMENT
4.1 SOURCES OF SOLVENT VAPORS
NVF Company's Kennett Square facility manufacturers numerous
materials through various wrapping, weaving, pressing and compositing
techniques applied to fibers, cloth and paper impregnated with solvent
based resins. The primary solvents utilized in this manufacturing pro-
cess include methanol, methyl ethyl ketone, methyl cellosolve, ethariol,
toluene and acetone. After impregnation of the desired material with
the resin, the solvent is typically evaporated in an oven. A diagram
of the plant layout is given in Figure 4-1.
Fifteen ovens are capable of being in operation at this facility.
Each oven is equipped with a blower to introduce the emanating vapors into
ducting manifolded with the other oven exhausts, for vapor transport: to
the incinerator. The vapors in the transport ducting are at a concentration
well below their LEL, typically ranging from three to seven thousand parts
per million as C-, in air.
4.2 DESCRIPTION OF INCINERATOR
The incinerator was designed and supplied by Hirt Combustion
Engineers, Montebello, California. Its designed residence time is 0.7
seconds at a 40,000 SCFM gas flow at 1400°F. The incinerator firebox is heated
by a directly fired oil burner firing No. 6 oil. The burner incorporates steam
atomization of the fuel oil for combustion. No air is introduced through
the burner. The sole combustion air source is the vapor mixture from the
processes. A propane ignition system is provided with this burner.
The solvent vapors are driven through the incinerator by the
forced draft fan. Before entering the incinerator the vapors pass through
a heat exchanger which uses heat from the flue gas to preheat the vapor/
air mixture.
As the flue gas exits the incinerator, two potential flow paths
are offered. One path is through the heat exchanger described above and
out an exhaust stack. The second path is through a waste heat boiler
Scott Environmental Techndosy Inc
-------
4-2
FIGURE 4-1
NVF COMPANY PROCESS AND COMTROL SYSTEM
KENNETT SQUARE, PENNSYLVANIA
1.
2.
3.
A.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
Oven #14,'2000 cfm
Oven #15, 2000 cfm
Oven #10DE, 4000 cfm
Oven #11, 3500 cfm
Oven //11WE, 450Q cfm
Oven //10WE, 4000 cfm
Oven #9WE, 5000 cfm
Oven #9, 3500 cfm
Oven i-'SKE, 2400 cfm
Oven #8DE, 2600 cfm
Oven #12WE, 3200 cfm
Oven #13, 4000 cfm
Oven #12DE, 4000 cfm.
Oven #6, 3500 cfm
Oven #7, 3500 cfm
Incinerator FD Fan
Heat Exchanger Exhaust Stack
Heat Exchanger
Firebox
Waste Heat Boiler
Waste Heat Boiler Exhaust Stack
-------
4-3
SET 1935 01 0681
which supplies steam for process heat and out an exhaust stack. Each
«
exhaust stack is equipped with automatic proportional dampers to adjust
the flow through each path depending on operational considerations and
process steam demand.
Scott Environmental Technology Inc.
-------
SET 1935 01 0681 5~1
5.0 DESCRIPTION OF TEST PROGRAM
The field testing of the emissions from an oil-fired incinerator
\)as carried out in three phases. The first phase involved comprehensive
emission tests at three operating temperatures. Tests were conducted
under normal use conditions with organic solvent vapors being fed to the
incinerator as well as during periods when room air was substituted for the
solvent vapors. The tests in which room air was incinerated were performed
to define the contribution of the fuel oil to the pollutants emitted.
During the second phase, the incinerator outlet was continuously
monitored for total hydrocarbons during a 30 day period. Averages are
available for 11 days. The emissions data and corresponding operation data
recorded by plant instrumentation show incinerator performance in typical
plant operation.
The final phase was a two-day program to define, incinerator
hydrocarbon destruction efficiency as a function of incinerator temperature
at 25 intervals over the 1200 to 1400 F range. This range had been
indicated to cover a broad range of efficiencies in the first test phase.
5.1 PHASE I TEST PROGRAM
The parameters measured and the sampling locations are listed
in Table 5-1 and shown in Figure 5-1.
The test matrix for Phase I is shown in Table 5-2. Triplicate...:,.
tests were conducted at each test temperature with the plant processes in
normal operation. Following this, duplicate tests were run at each tempera-
ture with the processes shut down and ambient plant air flowing through the
incinerator.
5.2 PHASE II
The heated FID hydrocarbon analyzer provided a continuous measure-
ment of total hydrocarbons in the incinerator outlet over a 30 day period.
The analyzer span and zero were checked daily by a Scott field technician.
The corresponding plant operating data were acquired from chart records and
logs maintained by the plant operators.
Scott Environmental Technolosylnc
-------
5-2
SET 1935 01 0681
TABLE 5-1: OIL FIRED INCINERATOR TEST PARAMETERS, PHASE I
PARAMETER
At Incinerator Inlet and Outlet
Total organics
Individual hydrocarbons
C02, CO, 02
H20
Temperature
Gas flow rate
Pressure
Particulates
METHOD
Continuous heated FID, Method 25 GC/FID
GC/FID
Method 24, GC/FID, Method 3
Method 4
Thermocouple, operational data
Method 2, operational data
Manometer
Modified Method 5
At Incinerator Outlet Only
NO
Method 7, Chemi
Miscellaneous
Incinerator temperature
Fuel flow rate
Process data
Thermocouple
Fuel meter (operational data)
As available
Scott Environmental Technology Inc.
-------
5-3
Figure 5-1 /
NVF COMPANY PROCESS AND CONTROL SYSTEM
KENNETT SQUARE, PENNSYLVANIA
Outlet Test Point
J.
1
20
Outlet Test Point
Flow
THC
VOC
CO, C02, 0-
CH,
N0x
Particulates
H2°
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
GO, CO , 02
CH4
Particulates
Oven #14,'2000 cfm
Oven #15, 2000 cfm
Oven #10DE, 4000 cfm
Oven »11, 3500 cfm
Oven #11WE, 450Q cfns
Oven //10WE, 4000 cfm
Oven #9WE, 5000 cfm
Oven #9, 3500 cfra
Oven /-'SUE, 2400 cfm
Oven #8DE, 2600 cfm
Oven #12WE, 3200 cfm
Oven #13, 4000 cfm
Oven .'?12DE, 4000 c fir-
Oven #6, 3500 cfm
Oven in, 3500 cfm
Incinerator FD Fan
Heat Exchanger Exhaust Stack
Heat Exchanger
Firebox
Waste Heat Boiler-
Waste Heat Boiler Exhaust Stack
-------
SET 1935 01 0681
5-4
TABLE 5-2: PHASE I TEST MATRIX!
Manufacturing Process Active
Manufacturing Process Inactive
Incinerator Temperature
1200°F 1400°F 1500 °F
XXX XXX XXX
XX XX ' , X X
Incinerator Inlet Measurements:
Flow Rate By M2.
THC By FID
Specific HC By MllO/GC
VOC, CO, C02 & CH4 By M25
CO, C02 & 02 By M3
Particulates By MM5
Static Pressure By M2
Gas Temperature
X
X.
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X X
X X
X X
X X
X X
X X
X X
X X
X
X
X
X
X
X
X
X X
X X
X X
X X
X X
X X
X X
X X
XXX
XXX
XXX
XXX
XXX
X
XXX
XXX
Keat Exchanger Outlet Measurements:
Flow Rate By M2
X
X
X
X
X
X
X
X X
X
X X
XXX
Waste Heat Boiler Outlet Measurements:
Flow Rate By M2
THC By FID
Specific HC By MllO/GC
VOC, CO, C02 & CH4 By M25
CO, C02 & 02 By M3
NOY By M7
A
NOV By Chemi
A.
Particulates By MM5
H20 By M4
Flue Gas Temperature
Static Pressure By M2
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X X
X X
X X
X X
X X
X
X X
X X
X X
X X
X X
X
X
X
X
X
X
X
X
X
X
X X
X X
X X
X X
X X
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5-5
SET 1935 01 1081
5.3 PHASE III
A two day test program was conducted in which the incinera.tor
temperature was set at 25° intervals between 1200 and 1400°F. During each
one hour test period, samples of the inlet and outlet gas were collected and
analyzed by GC to determine the hydrocarbon destruction efficiency at each
temperature. On the first day the temperature was increased from 12:00° to
1400° while on the second day the temperature was decreased from 1400° to
1200°F. This was done to determine whether any extended lag time between
the temperature adjustment and system equilibrium occurred. System
operational parameters were recorded as in Phase II.
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6-1
SET 1935 01 0681
6.0 SAMPLING AND ANALYSIS METHODOLOGY
This section details the methods employed to collect and analyze
the incinerator inlet and exhaust gaseous and particulate samples. Standard
EPA Reference Method guidelines were adhered to, where possible. These
methods were applied to measurements of the gaseous velocities, moisture,
molecular weight, NOX concentration and VOC composition. Each sampling
location (incinerator inlet, heat exchanger exhaust and waste heat boiler
outlet) was provided with three-inch sampling ports, positioned at right
angles, to allow sample withdrawal and facilitate velocity traversing.
The overall sampling and analytical system configuration utilized during
Phase I effort is shown in Figure 6-1. The Phase II testing only required
the employment of one hot FID; therefore, the remainder of the equipment
was removed at the conclusion of Phase I.
6.1 PARTICULATE SAMPLING
In order to minimize the potential for carbonaceous particulate
interfering with the analysis of the condensate trap element of the Method
25 VOC determination, removal of the particulate from the sample stream was
incorporated. A standard Method 5 tared filter holder was positioned at the
incinerator inlet and waste heat boiler exhaust sampling locations, as
shown in Figure 6-1. Anisokinetic sampling of the gas streams was conducted
through 1/4" stainless steel tubing installed in the center of each stack
perpendicular to the flow of the gas streams.
The filter catch also provided a convenient means for assessing
whether the fuel produced significant amounts of carbonaceous or organic
particulate in the incinerator effluent.
At the end of each test run, the filter was removed from the
holder, transferred to a Petri dish and returned to Scott's Plumsteadville
laboratory. The filter was then desiccated and weighed as per the Method 5 '
procedure. The weight of the catch, the sampling time and flow rate were
used to calculate the stack particulate loading. Some of the filters were
extracted with chloroform and the extract was evaporated and weighed to
estimate the organic content of the particulate.
Scott Environmental Techndogy Inc
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6-1 FIELD SAMPLING-SYSTEM
ISJ
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6-3
SET 1935 01 0681
6.2 HYDROCARBON MEASUREMENTS
The Volatile Organic Carbon (VOC) content of the incinerator
inlet and outlet streams was determined by three separate methods:
Reference Method 25, continuous heated FID hydrocarbon analyzer and
Reference Method 110 sampling followed by gas chromatography (GC).
Copies of, the two Reference Methods are included in Appendix C.
. 6.2.1 EPA Reference Method 25
The Method 25 sample collection was performed in the laboratory
trailer. The filtered gas sample from the heated sampling line was passed
through a condensate trap maintained in a dry ice bath and then collected
in the sample tank. The sample flow rate through the trap was regulated
by an adjustable orifice. The Method 25 sampling procedures were followed
closely in each 1 hour sample run. The trap samples were packed in dry
ice and returned to Scott's Plumsteadville laboratory along with the sample
tanks.
The traps and condensate tanks were analyzed at Plumsteadville
using a Method 25 Analyzer fabricated by Scott. This analyzer consists of
two components. One component oxidizes the condensate sample and collects
the resultant C02 in an evacuated vessel. In this process, the condensible
organics are burned insitu, catalytically oxidized and collected. The
progress of the hydrocarbon oxidation is monitored by a nondispersive
infrared analyzer. The second component analyzes the COj collected from
the condensible organic sample and analyzes the gaseous carbon combustion
components from the non-condensible portion of the sample. The analysis is
performed in the following manner. The sample is partitioned into the CO,
C02, CH^ and TGNMO components through the use of a GC valve with backflush
capabilities and a series of separation columns. All components are then
catalytically oxidized to C02> to put all components on a C-^ basis, and
negate the varying FID response to different constituents. All of the
discrete C02 moieties are then catalytically reduced to CH^, to permit
analysis by the FID. Each CH, elutes in accordance with the retention
time of the original compound, therefore, separate peaks are produced for
each sample component.
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6-4
SET 1935 01 0681
6.2.2 Method 110 Sampling/Gas Chromatographic Analysis
i
In order to quantify the VOC emissions and provide a characteri-
zation of the constituents emitted, chromatographic analysis of the exhaust
gas was performed. Samples were collected by EPA Reference Method 110 for
the determination of benzene from stationary sources. In this procedure,
an integrated bag sample of the gas stream is obtained by filling an
evacuated Tedlar bag with sample gas by reducing the pressure on the bag
exterior at a constant rate.
Method 110 samples were collected during one hour test periods.
All samples thus obtained were subjected to on site gas chromatographic
analysis.
All gas samples collected were analyzed using a Shimadzu GC Mini-1
gas chromatograph equipped with dual flame ionization detectors, dual
electrometers, heated sample loop and a backflush system. Figure 6-2
shows a schematic of the backflush apparatus. The backflush system is
composed of a ten port sequence reversal valve and two columns, a scrubber
column for retaining high molecular weight compounds and an analytical
column. When the system is in the inject mode the scrubber column and the
analytical column are connected in series allowing sample components to
move from the pre-column to the analytical column. In the backflush mode
the columns are disconnected from each other and become two separate systems
each with its own carrier gas source. This arrangement allows the separation
and measurement of low molecular weight compounds while the scrubber column
is being backflushed of heavier sample components. These heavier components
are backflushed through the second detector where they are measured. Back-
flushing was initiated after the toluene peak eluted.
Scott Environmental Technology Inc.
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V
t
o
M
N3
CARRIER GAS A
A ><
\
PREP, COLUMN
SAMPLE INJECTION
B
/
s
CARRIER GAS B
^
INJECT
A, D, E OPEN
B, C CLOSED
BACKFUJSH
A, E CLOSED
B, C, D OPEN
GC COLUMN CONFIGURATION 'WITH BACKFLUSH
1
ANALYTICAL COLUMN
DETECTOR
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6-6
SET 1935 01 0681
A temperature programmed chromatographic analysis was used to
provide the necessary separation of the constituents of the sample mixture.
The conditions used for the analysis were:
Column Temperature (program) 50 - 200 C
o
Temperature Program Rate 20 C/min.
o
5 ml. Sample Loop, Temperature 50 C
Carrier Gas Flow Rate 50 cc/min.
Hydrogen Flow Rate 40 cc/min.
Air Flow Rate 240 cc/min.
Analysis Time 30 min.
Detector Flame lonization
The columns used for field analysis were:
A - Scrubber Column
1/8" x 1 m Stainless Steel
10% FFAP on 80/100 Supelcoport
B - Analytical Column
1/8" x 6' Stainless Steel
Carbopak C/0.1% SP-1000
Samples for chromatographic analysis were drawn into a 20 cc glass
syringe and introduced to the sample loop inlet. The samples once in the
sample loop were allowed to come to atmospheric pressure by waiting 15 seconds
prior to injection.
The gas chromatograph was calibrated with the propane, acetone,
toluene and xylene in nitrogen standards listed in Section 6.4. Samples of \
- - *
each calibration gas were analyzed at the beginning and end of each test
day. The average response factor in integration counts per ppm-C for each
standard was calculated and used to convert sample peak areas (by integrator)
to concentrations in ppm-C. The propane factor was used for aliphatics
and olefins, the acetone factor was used for all oxygenates and the toluene
factor was used for benzene and toluene. Unknown peaks were deemed to be
oxygenates from their broadened peak shape and calculated as such.
6.2.3 FID Sampling and Analysis
Inlet and outlet sampling and analysis was continuously performed
by Scott Model 215 Heated Flame lonization Detector during the performance
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SET 1935 01 0681
of the Phase I effort. In the early stages of the test effort, difficulties
w,ere experienced with the FID which was monitoring the inlet sample. Since
field repair of this unit could not be implemented, the inlet Reference
Method 110 integrated bag sample was introduced into the outlet FID to
determine the inlet total hydrocarbon concentration. This analyzer was
calibrated with standard gases of propane between each run and response
factors for oxygenated compounds generated in the laboratory were verified
daily, through the injection of standards after the initial propane
calibrations.
The FID fuel-air ratio had been adjusted in the laboratory to
give nearly equal response on a ppm-C basis to propane, acetone and toluene.
The daily field calibration showed that the response factors for acetone
and toluene remained within +10% of the propane factor. Therefore, the
concentrations were calculated from the propane factor expressed as per cent
of full scale response per ppm-C. The propane standard concentrations used
were. 331 ppm (993 ppm-C 'for the "process-on" inlet samples and 4.97 ppm
(14.91 ppm-C) for the remaining samples.
The sample introduced into these analyzers was conditioned for
particulate removal and the sample temperature was controlled. The FID was
o o
operated at 325 F while the sample temperature was maintained at 350 F in
the transport tubing, and the heated filter was maintained above this
temperature. This technique was employed to minimize hydrocarbon conden-
sation in the sampling system.
The same sampling system and instrumentation were used for the
continuous monitoring performed in Phase II. The analyzer was calibrated
daily using cylinders containing propane in air and nitrogen zero gas as
the calibration standards.
6.3 NITROGEN OXIDES
A Scott Model 125 Chemiluminescense Analyzer was employed to
measure the concentration of oxides of nitrogen at the incinerator outlet.
The NO analyzer was equipped with a high temperature converter so that the
X
NO concentration was read directly. The results of the chemiluminescence
NO analyses were checked by several EPA Method 7 Reference Method samples.
X
The samples were obtained directly from the source in evacuated 2-liter
flasks containing absorbing solution. After obtaining the three sets of
samples, the nine flasks were directly returned to the laboratory for analysis.
Scott Environmental Technology Inc
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6-8
SET 1935 01 0681
6.4 CALIBRATION STANDARDS
5
The calibration gases used for the instrumental analyses were
Scott Specialty Gas working standards. The specification for these
standards are ±5% in the 1-99.ppm range and ±2% in the 100 ppm to 16%
range.
The concentrations of the calibration gases used in this program
are as follows:
Gas Chromatographic Analyses
4.97 ppm propane for aliphatics and olefins
7.37 ppm acetone for oxygenates
4.04 ppm toluene for aromatics
4.75 ppm xylene for backflush components
Flame lonization Detector
4.97 ppm propane
331.0 ppm propane
EPA Method 25
0.504% methane
1.02% methane
1.04% C02
0.504% CO2
352 ppm C02
NOX
407.0 ppm NO
256.2 ppm NO
Scott Environmental Technolosy Inc
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6-9
SET 1935 01 0681
6.5 CARBON DIOXIDE, CARBON MONOXIDE AND OXYGEN
Carbon dioxide, carbon monoxide and oxygen were measured by
Reference Method 3 (Orsat). A pressurized sample was obtained from a
point adjacent to the Reference Method 25 sampling point. Difficulty
with the KOH solution was experienced during the early sampling intervals.
Upon replacement of this solution, the Orsat values were improved.
6.6 MOISTURE
Moisture was determined by Reference Method 4. Difficulties
experienced during the initial runs included the freezing of the moisture
in the collection system resulting in a loss of sample flow and potential
contamination of subsequent samples. This difficulty was alleviated by
positioning the entire system in a temperature controlled environment.
6.7 FLOW MEASUREMENTS
Stack gas flow rates were measured by Reference Methods 1 and 2.
All ducts traversed were circular in configuration and were equipped with
ports installed at right angles for traversing. A type S pitot tube and
inclined manometer were employed to determine the velocity profiles at
each test point. Leak checks of the differential pressure sensing system
were performed prior to each run.
Scott Environmental Technology Inc.
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7-1
SET 1935 01 0681
7.0 QUALITY CONTROL AND QUALITY ASSURANCE
*
This section describes the procedures utilized to insure that
representative uncontaminated samples were obtained and that the accuracy
of the analysis of these samples be insured. In this section quality
control is those actions taken to insure sample integrity and analytical
accuracy while quality assurance is those activities taken to insure the
quality control program is being properly implemented.
7.1 SAMPLING PROCEDURES
The quality control procedures for field measurements and sample
extraction concentrated on insuring leak-free sample delivery systems.
Heated sample delivery lines were leak-checked prior to each sampling run
by closing the line at the test port, drawing a vacuum and observing;
initial vacuum and 1 minute vacuum using the same criteria for acceptance
as specified in EPA Method 5. These heated lines provided all sample for
total hydrocarbon (THC) by flame ionization detector (FID), oxides of
nitrogen analysis by NDIR, EPA Method 110 sampling system, and the EPA
Method 25 sampling system.
The absence of leaks in the velocity measuring apparatus com-
prising pitot tube manometer and interconnecting tubing was established
prior to each sampling run. Similarly, the adequacy of the orsat values
was checked by .making an additional five passes after obtaining the reading
to establish the completeness of the absorption. Additionally, leak checks
of the orsat were conducted daily, during overnight intervals. The Method 4
sampling equipment was checked for leaks at the beginning and end of each
day. The temperature measuring devices were calibrated in the laboratory
prior to test initiation.
Leak checking for EPA Method 25 was performed per the requirements
stated in the method. These procedures consisted of evacuation of the
sample tank and observing the maintained vacuum. A decrease of less than
one mm of Hg over a five minute period is the criteria for an acceptable
leak check.
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7-2
SET 1935 01 0681'
The sample train was leak checked prior to testing and immediately
*
after each test. This consisted of closing the sample train at the probe
tip and observing the vacuum for a ten minute time period. An acceptable
check is less than 1 mm Hg reduction in vacuum.
7.2 ANALYTICAL QUALITY CONTROL
7.2.1 Gas Chromatography (Modified EPA Method 110)
Calibration of the gas chromatograph was performed before and
after each set of test run (1-hour composites) samples were analyzed. The
calibration gases were volumetric blends certified to within ±2% of nominal
concentration (See page 6-8). The calibration gases were certified against
NBS traceable reference standards (quality assurance was provided by a
separate standard of known concentration) which were analyzed in replicate
each sampling day with the calibrated GC to insure the precision and accuracy
of the analysis were within acceptable limits. Contamination of the Method
110 sampling system was minimized by triple flushing of the Tedlar bags with
nitrogen, leaving the bags partially filled with nitrogen and analyzing the
contents by GC twelve hours later. The resulting background concentrations
were recorded and only low background bags were used for expected low con-
centration samples. . Quality assurance was provided by filling a randomly
selected bag each sampling day with the QA audit gas and replicating
analyses on both the GC and FID.
7.2.2 Flame lonization Detector
The continuous heated flame ionization detectors were calibrated
in the laboratory to establish the operational conditions in which the
response to all anticipated sample constituents (determined through con-
sultation with plant personnel and analysis of samples obtained during the
presurvey) indicated maximum linearity among oxygenates. Correlation of
these results with propane calibration was then performed. During field
analysis the operational conditions established for the instrument in the
lab were utilized. Quality assurance was performed by injecting a standardized
oxygenated hydrocarbon after completion of the standardized propane cali-
brations. All instrumentation were calibrated before and after each test run.
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SET 1935 01 0681
7.2.3 Method 25 Determination of Total Gaseous Non-Methane Organic
Emissions as Carbon
Quality Control procedures for the analysis of volatile organic
emissions are well documented in the reference method as published. These
procedures are established in Section 5 of the method (See Appendix C). The
procedures include analysis of sample blanks, catalyst efficiency evalu-
ation, analysis of known mass of hydrocarbons into the oxidation/reduction
system and analyzer linearity and calibration checks.
In addition to these quality control steps an assurance audit
gas was prepared containing methane and three additional organics of known
concentration. This known was introduced through the analytical system
to provide a separate accuracy check.
7.2.3 Wet Chemistry
The analysis for oxides of nitrogen was performed using the
methodology specified in EPA Method 7. The quality control procedures
documented in the method were followed. In addition audit samples were
obtained from EPA Environmental Monitoring Support Laboratory to analyze
concurrently with the field samples to assure analytical accuracy.
Scott Environmental Technology Inc.
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