COAL PREPARATION PLANT EMISSION TESTS
TEST NO. 1281-25
CONSOLIDATION COAL COMPANY
Bishop, West Virginia
PREPARED FOR
ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park
North Carolina 27711
Contract No 68-02-0233
SCOTT RESEARCH LABORATORIES, INC.
PLUVSTEADVILLE. PENNSYLVANIA 18949
-------
SRL 1281 25 0472
Test No. 1281-25
Consolidation Coal Company
Bishop, West Virginia, Norman R. Troxel
SCOTT RESEARCH LABORATORIES, INC.
Plumsteadville, Pennsylvania 18949
68-02-0233
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SRL 1281 25 0472
TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1-1
2.0 SUMMARY OF RESULTS 2-1
3.0 PROCESS DESCRIPTION AND OPERATION 3-1
4.0 LOCATION OF SAMPLING POINTS 4-1
5.0 SAMPLING AND ANALYTICAL PROCEDURES 5-1
5.1 PARTICULATE SAMPLING AND ANALYTICAL PROCEDURES 5-1
5.2 GASEOUS SAMPLING PROCEDURES 5-1
5.3 SO SAMPLING AND ANALYTICAL PROCEDURES 5-2
5.4 NO SAMPLING AND ANALTYICAL PROCEDURES 5-3
x
5.5 ORSAT SAMPLING AND ANALYTICAL PROCEDURE 5-3
APPENDIX A COMPLETE PARTICULATE RESULTS WITH
EXAMPLE CALCULATIONS A-l
APPENDIX B COMPLETE GASEOUS RESULTS WITH
EXAMPLE CALCULATIONS B-l
APPENDIX C FIELD DATA C-l
APPENDIX D STANDARD SAMPLING PROCEDURES D-l
APPENDIX E LABORATORY REPORT E-l
E.I ON-SITE HANDLING AND TRANSFER, PARTICULATE E-l
E.2 LABORATORY HANDLING AND ANALYSIS, PARTICULATE E-2
E.3 ORSAT ANALYSIS E-4
E.4 SO ANALYSIS E-7
E.5 NO ANALYSIS ' E-14
x
APPENDIX F TEST LOG F-l
APPENDIX G PROJECT PARTICIPANTS AND TITLES G-l
SCOTT RESEARCH LABORATORIES, INC.
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1-1
SRL 1281 25 0472
1.0 INTRODUCTION
Scott Research Laboratories, Inc. performed source sampling
tests at the Bishop, West Virginia plant of Consolidation Coal Company
during the week of February 28, 1972. The plant uses a Research
Cottrell venturi scrubber to control the exhaust gas emissions from a
coal cleaning and preparation operation.
The outlet exhaust gases, as they were being emitted to the
atmosphere, were sampled and analyzed for the determination of total
particulate loading, oxides of nitrogen, sulfur dioxide, carbon dioxide,
carbon monoxide, carbon dioxide, and oxygen concentrations. Since
there was an easily accessible location for sampling the exhaust gases
before they entered the venturi scrubber, samples were also collected
in the inlet to the scrubber and the same analyses performed as on the
outlet samples. The particulate samples were collected simultaneously
at the inlet and outlet of the scrubber; and the gaseous samples were
taken at both locations during the particulate traverses.
Three complete runs were performed at the plant. One run was
conducted each day on February 29, March 1, and 2, 1972. Figure 1
shows the location of the sampling points at the plant.
SCOTT RESEARCH LABORATORIES, INC.
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1-2
SRL 1281 25 0472
FIGURE 1 - SAMPLE POINT LOCATIONS
CONSOLIDATION COAL Co.
BISHQP, Kl.
OUTLET
81-
M1ST
ELIM1NATOR
J
VENTUKI
U> — SCRU8BG ft
-v
E
LE VAT I ON
SCOTT RESEARCH LABORATORIES, INC
INLET
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2-1
SRL 1281 25 0472
2.0 SUMMARY OF RESULTS
.;
A summary of test results is presented in Table 1. The particulate
weights are summarized and shown in Table 2, with all of the particulate
results included as Appendix A. Appendix B presents all of the gaseous
results, and the raw data sheets are included as Appendix C.
From Table 2 it is observed that the particulate matter collected
from the outlet during Run 1 is somewhat higher than what was collected
during the other two runs. The higher weight was due to an increase both
in the front half and back half of the train. The amount of particulate
matter collected at the inlet varied considerably from run to run. The
first day a total of 55,612.5 mg. were collected, while the next day
83,626.0 mg. were collected, and then only 37,437.0 mg. were collected
during the third run. , :
The average value for the outlet concentration of the second
and third run was only 0.013 gr/scf, considering only the front half.
This amounts to an emission rate of only 12.5 Ibs/hr.
From Table 1 it is observed that the sulfur dioxide concentra-
tions vary all the way from 0.8 ppm up to 3155.6 ppm. The values do not
appear to be questionable since the outlet and inlet values both show
the same variation from one run to another.
The NO values were fairly consistent for both the inlet and
X
outlet. The outlet NO concentration averaged 57.1 ppm and the average
inlet concentration was 73.1 ppm.
On the basis of the front half of the particulate train values
(gr/scf) the collection efficiency of the scrubber varied from 99.79%
SCOTT RESEARCH LABORATORIES, INC.
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Run Number
Sample Point Location
Sample Date
Sample Gas Vol., scf.
Moisture, %
Stack Gas Temp., °F
Stack Gas Vel., fpm
Stack Gas Vol., SCFM
Particulate Collected
Probe, cyclone, filter, mg.
Total, mg.
Particulate Concentratiom
Probe, cyclone, filter, gr/scf
Total, gr/scf
Particulate Emissions
Probe, cyclone, filter, Ib/hr.
Total, Ib/hr.
Percent Isokinetic
Carbon Monoxide, %
Carbon Dioxide, %
Oxygen, %
Sulfur Dioxide, ppm
NO, ppm
CO
to
m
TABLE 1 - SUMMARY OF TEST RESULTS
1-0
Outlet
2/29/72
90.78
14.37
125
4054
106,330
98.1
121.3
0.017
0.021
15.16
18.77
96.95
0.0
1.0
19.2
0.8
57.7
2-0
Outlet
3/1/72
87.48
12.98
125
4060
107,530
76.3
89.7
0.013
0.016
12.39
14.55
92.39
0.0
0.7
19.7
3155.6
51.1
3-0
Outlet
3/2/72
88.78
12.74
125
4232
111,560
77.4
89.3
0.013
0.015
12.83
14.81
90.37
0.0
0.1
20.6
214.1
62.5
1-1
Inlet
2/29/72
95.44
13.26
149
3906
113,630
55,612.5
55,743.5
8.974
8.995
8739.00
8759.40
102.58
0.0
0.9
19.7
17.1
64.8
2-1
Inlet
3/1/72
89.84
15.32
145
3935
112,030
83,626.0
83,702.5
14.336
14.349
13764.00
13776.40
97.93
0.0
0.9
18.6
2904.2
69.4
to
o
3-1 S
Inlet
3/2/72
94.76
15.32
145
4055
114,860
37,437.0 N>
37,474.0 tl>
6.084
6.090
5988.80
5994.70
100.75
0.0
1.0
19.0
300.0
85.1
-------
8
30
PI
CO
m
>
x
n
§
SO
I
£
o
Run Number:
Sample Location
Container 1, mg.
Container 2, mg.
Container 3a, mg.
Container 3b, mg.
Container 5, mg.
Probe, cyclone filter, mg.
Total, mg.
TABLE 2 - PARTICULATE WEIGHTS SUMMARY
1-0
Outlet
39.8
58.3
3.0
8.1
12.1
98.1
121.3
2-0
Outlet
51.5
24.8
2.9
1.7
8.7
76.3
89.7
3-0
Outlet
30.0
47.4
0*
3.1
8.8
77.4
89.3
1-1
Inlet
273.5
55,339.0
3.0
21.0
107.0
55,612.5
55,743.5
2-1
Inlet
253.0
83,373.0
32.0
32.5
12.0
83,626.0
83,702.5
3-1
Inlet
202.0
37.235.0
6.0
22.0
9.0
37,437.0
37,474.0
OO
N3
U1
NJ
I
* Blank was higher than sample value.
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2-4
SRL 1281 25 0472
to 99.91%. For Run 1 the efficiency was 99.81%, Run 2 it was 99.91%,
and for Run 3 it was 99.79%.
SCOTT RESEARCH LABORATORIES. INC.
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3-1
SRL 1281 25 0472
3.0 PROCESS DESCRIPTION AND OPERATION
The Bishop preparation plant was built in the mid 1950's and
has been upgraded to process coal through froth flotation cells. An
old Link-Belt multilouvre thermal dryer was replaced by a Link-Belt
Fluid Bed dryer in March 1970. At that time, a Research Cottrell
Flooded Disc scrubber was installed to clean the exhaust gases before
being emitted to the atmosphere. The dryer exhaust fans are rated at
183,000 cfm at 170°F and the scrubber design calls for a 26" AP according
to Research Cottrell.
The Bishop preparation plant has the capability to process all
stored coal in 5 hours of continuous operation. Thus, only one test
could be made per day. During the tests, 50 percent of the filter cake
from flotation cells was being dried in the thermal dryer. This is the
maximum amount of cake allowed by design specifications.
Loadout of rail care during the tests indicated the plant
production rate was 400 TPH of cleaned coal. Of this it was calculated
300 tons were being fed to the dryer. Design capacity of the dryer
was 368 TPH cleaned, dried coal and 40 TPH exhaust moisture. Plant
blueprints gave an operating load of 293 TPH to the dryer.
The control panel in the plant was monitored and the following
data taken during the tests:
SCOTT RESEARCH LABORATORIES, INC.
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3-2
SRL 1281 25 0472
1st Run 2nd Run 3rd Run
Exhaust fan, amp. 300 300 300
Roll feeder temp., °F 780-800 800 800
Furnace air temp., °F 1020-1240 1000-1210 960-1190
Dryer-inlet temp., °F 910-1030 940-1060 880-1020
Pulverizer temp., °F 180-185 180-185 175-185
Dryer Exhaust, °F 130-140 130-140 130-140
Exhaust fan inlet, °F 170 170 165-170
Taps were installed across the venturi throat so that the
pressure drop could be measured during the tests. Readings showed that
the scrubber was not operating as designed. The pressure drop measured
was in the range of 16-17 in. water gauge.
SCOTT RESEARCH LABORATORIES, INC.
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Pi
i. RUT :
DATX-
si
242
to
oo
to
Ui
o
J>
^J
10
U3
TPM
PROCESS DIAGRAM
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4-1
SRL 1281 25 0472
4.0; LOCATION OF SAMPLING POINTS
The exhaust gases from the coal cleaning operation pass through
an 84 inch diameter duct into a Research Cottrell venturi scrubber. From
the venturi scrubber, the gases flow through a mist eliminator and are
then emitted to the atmosphere through an 81 inch diameter stack.
The location (inlet) for sampling the gases before they enter
the venturi scrubber was chosen in a straight vertical section of the
84 inch diameter duct. The two ports were installed at 90 apart and
were located approximately 40 feet downstream from a bend and approximately
15 feet upstream from a bend. Special sampling platforms were required
to support the sampling train at both ports. An angle iron support
extending ten feet out from the stack supported a plywood platform.
The location (outlet) for sampling the gases prior to the
discharge to the atmosphere was in a straight section of the 81 inch
diameter stack atop the mist eliminator. The sampling ports were located
approximately 7 feet upstream from the top of the stack and approximately
10 feet downstream from the outlet of the mist eliminator.
There were three sample ports spaced 45 apart at the outlet
location. The two ports at 90° apart, were used for the particulate
sampling. The center port was used for gaseous sampling. The outlet
ports were approximately 30 feet above the platform area where the
particulate sample control units were located. Again, special support
systems were required to hold the particulate sampling train. Figure 1
shows the physical layout of the system and the location of the sample
ports.
SCOTT RESEARCH LABORATORIES, INC
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4-2
SRL 1281 25 0472
Figure 2 shows the traverse points used at each sample point
location. At the inlet, 36 traverse points were sampled four minutes
each. At the outlet, 48 traverse points were sampled 3 minutes each.
At the outlet location, in order to stay at least two inches away from
the wall, the first two and last two points on the traverse were
combined. Thus, the first and last points (each containing two traverse
points) were sampled for six minutes each. The traverse points were
chosen in accordance with Method 1 published in the Federal Register,
Volume 36, No. 24.
The two ports at each location were designated as A and B.
A was the port on the left and B was the port 90 to the right of A.
SCOTT RESEARCH LABORATORIES, INC
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SRL 1281 25 OA72
4-3
CONSOLIDATION COAL CO.
BISHOP, W. VIRGINIA
B
FIGURE 2 TRAVERSE POINT LOCATIONS
SCOTT RESEARCH LABORATORIES, INC,
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4-4
SRL 1281 25 0472
CONSOLIDATION COAL CO.
BISHOP, W. VIRGINIA
FIGURE 2 TRAVERSE POINT LOCATIONS
(continued)
SCOTT RESEARCH LABORATORIES, INC
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5-1
SRL 1281 25 0472
5.0 SAMPLING AND ANALYTICAL PROCEDURES
5.1 PARTICULATE .SAMPLING AND ANALYTICAL PROCEDURES
Samples were collected for the determination of particulate
matter simultaneously from the inlet and outlet of the venturi scrubber.
The sampling and analytical procedures used were the same as those
specified by Method 5, "Determination of Particulate Emissions from
Stationary Sources", and published in the Federal Register, Volume 36,
No. 247, Thursday, December 23, 1971. This method is attached as
Appendix D. In addition, the impinger catch was analyzed.
Briefly, the method consists of withdrawing a sample isokinetically
from the stack through a heated glass probe into a cyclone, filter, and
impinger train. The cyclone and filter are contained in a heated box.
The sample volume is measured with a dry gas meter, and isokinetic conditions
are maintained by monitoring the stack gas velocity with an '"S" type pitot
tube. After testing is completed, the train is thoroughly washed including
the probe. The washings are evaporated, dried, and weighed along with the
filter in order to obtain a total weight of particulate matter collected.
The stack gas velocity and flow rate were measured using
Method 2, "Determination of Stack Gas Velocity and Volumetric Flow Rate
(Type S Pitot Tube)", and published in the Federal Register. Using both
the weight of sample collected and the flow rate determined, a total
particulate emission rate was calculated.
5.2 GASEOUS SAMPLING PROCEDURES
Stack gas samples were taken at regular intervals during
each particulate sampling traverse to determine the concentration of
SCOTT RESEARCH LABORATORIES, INC
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5-2
SRL 1281 25 0472
0,, CO, CO,, NO and SO, present in the stack effluent. The sampling
^ £* X £f
locations were the same with respect to the venturi scrubber as those
used for the particulate samples. The sampling and analytical procedures
used were in accordance with Federal Register, Volume 36, No. 247,
December 23, 1972, "Standards of Performance for New Stationary Sources".
5.3 S02 SAMPLING AND ANALYTICAL PROCEDURES
All S02 samples were taken through a %. inch O.D. glass probe
heated to approximately 250 F. This was connected to a glass sample
train consisting of one bubbler and three impingers connected in series.
The bubbler contained 15 ml. of 80% isopropanol and was used to remove
any S0_ present in the sample stream. The SO, was collected in the
next two impingers, each containing 15 ml. of 3% H20 . The third impinger
was used to trap any overflow from the two SO impingers.
Each sampling period was 30 minutes in duration, and the
sampling rate was maintained at approximately 1 liter per minute with
an in-line flowmeter. A temperature compensated dry gas meter was used
to measure the total volume of gas sampled.
Following each test, the SO, samples were transferred to
polyethylene bottles with distilled water washes. All samples were then
returned to the laboratory where they were diluted to volume in a 50 or
100 ml. volumetric flask. A suitable aliquot of each sample was
then titrated with a 0.01 N barium perchlorate solution in the presence
of thorin indicator. The results were reported as parts per million SO,.
SCOTT RESEARCH LABORATORIES, INC
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5-3
SRL 1281 25 0472
5.4 NO SAMPLING AND ANALTYICAL PROCEDURES
x • . . •
The NO samples were taken using the same heated glass probe
X
described in Section 6.3. Each sample was drawn through this probe
into a previously evacuated 2 liter flask containing 25 ml. of NO
X
absorbing solution. The flasks were shaken for 5 minutes following
each sampling period and then allowed to stand for at least 16 hours.
Following this, the samples were shaken again for 2 minutes just prior
to measuring the final flask pressure. The samples were then transferred
to glass shipping bottles with distilled water washes and neutralized
with 1.0 N sodium hydroxide. At the end of the test period, all samples
were returned to the laboratory for analysis.
The samples were analyzed via the phenoldisulfonic acid
procedure described in the aforementioned Federal Register. The absor-
bances were measured with a Bausch and Lomb Spectronic 20 Colorimeter.
The results were reported as parts per million NO-.
5.5 ORSAT SAMPLING AND ANALYTICAL PROCEDURE
Integrated gae samples were taken for Orsat analysis (CO, C0~
and 0_) during each particulate sampling period. The sampling apparatus
consisted of a \ inch O.D. stainless steel probe, a stainless steel
coiled tube condenser, a glass water trap, a carbon vane pump, a flow-
meter and needle valve assembly, a 3 inch #21 stainless steel hypodermic
needle, and a 5 liter Tedlar sample bag fitted with a syringe cap.
The sampling procedure was initiated by purging the probe
and condenser system with stack air, adjusting the sample flow rates to
approximately 80 cc per minute, and inserting the hypodermic needle
SCOTT RESEARCH LABORATORIES. INC
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5-4
SRL 1281 25 0472
into the syringe cap on the sample bag. The integrated sample was taken
over a 1 hour period yielding approximately 4.8 liters of sample for
analysis.
At the end of each test day, the sample bags were analyzed
by Orsat for CO, C02 and 0~. Repetitive analyses were performed on
each bag to insure satisfactory duplication. The results were reported
in percentages.
SCOTT RESEARCH LABORATORIES, INC
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A-l
SRL 1281 25 0472
APPENDIX A
COMPLETE PARTICULATE RESULTS WITH EXAMPLE CALCULATIONS
SCOTT RESEARCH LABORATORIES. INC
-------
A-2
OF
SOURCE TEST] KG CALCULATION FORMS
Test. No.
flame of Firm
Location of Plant
Type of Plant
L
Cs/rL
Co.
. V,
Control Equipment
Sampling foint Locatios J.^
o
Pollutants Sarpp1edjfl1ftuijftfo> ;
N
Time of Participate Test:
-ftun No. f I <± 4 O Date
Begin
Run No. £ J 4" £ Q Date_
Run No. 31 4 3 0 Date
Beg i n
No. Runs' 31+30
Begin /Q //
End
End
End
I
'PARTICIPATE EMISSION DATA
Run No.
p barometric pressure, "Hg Absolute
p orifice pressure drop, "ILO
—fl £....
V - veJTume of dry gas sampled P meter
ra cdnditions, ft. 3
Tm Average- Gas Meter Temperature, °F
V Volume of Dry Gas Sampled 0 Standard
std. Renditions, ft. 3
V Total I-LO collected, ml., Impinger*
w . & Silica.l Gel.
V( ~ Volii;r,e.'of Water Vapor Collected
'oas ft. 3 ^ Standrird Conditions*
IX
10
I.13L
$9
K.&56
20
a?
55
30 !
•r i
*m\
I.SSfk
T
—-t
\&8
' * 70°F, 29.92" Hg.
-------
A-3
l'.u«;,'o. . :.. . ,
£M - % M;»isl'ji'£ i;; «.'.:: lit;:';!; c^.r-i by voli-iir.e
— ,... • -
"!i f - Mole fraction of dry ^ias
% C0?
*" • '
*N2
M 1-! , - rial cellar weight, of dry sue!; gas
Ci
M W - Molecular weight of stack gas
<-APs - Velocity Ik-ad of stack gas, In. HO
" TS - Stack Temperature, °F
« "~ S S
P - Stack Pressure, "Hg. .Absolute
o
V - Stack Velocity Q stack conditions, fpm
A - Stack Area, in.
Q - Stack Gas Volume (3
s Standard Conditions, *SCI:K
T, - Net Time of Test, min.
D ^.- Sampling Noir^le Dimeter, in.
%I ' - Percent isokirurlic
nu - Particulsts - proba, cyclone
1 and filter, mg.
ni - Parti cul ate - total, inn.
C - Particulatc •- probe, cyclone.,
an and, f .liter, gr/SCF
C - PeirticulaU' - total, qr/SCF
ao
il
10
„..' . 1
* *• " * '
ttfo
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-------
A-4
SSlQ'!•,':•:,'A f •;:•:! t.
Run ib.
Uck cond.
ttfid filter, li'/nr1.
C - Particulate - total, Ib/iir.
3X
% EA - 5S Excess air 0
Sunu/l ing point
II*
' 1*731
70°F. 23.S£" Hg.
10
32 j
-------
A-5
PAP.TICULA'iE C/.LCULAVjOilS
1. Volwic of dry rji'S sarr:plc\i si standard conditions - 70°F» 29.92rt •- .
st.d
!177X" /P -' P ^
V ]_^y
PI
2-. .Volume of water vapor at 70°F 'fi 29.92!l Hg, Ft.'
- o. 0
-o 7.
3. % moisture .in stack gas
.100 X V.
w
Sli =
S;M = v + v
nistd wgas
4. Mole fraction of dry gas
Md s'
TOO - C/M
100
O.
5. Avorcigf: rcoleci.fUr v/eiglit or dry stack gas
A<5<3"5>
f
-------
A-6
.
W d X K v IS 0 - .1 ~
7. Stack velocity P sbcl: conditions, f|,r,
- 4350 XMP
r
\:._
?
L^f
X H W
=- fprn -
8. Stack gas vplunjs @ standard conditions, SCFH
• (Ts t. "-
Per cent isokinetic
1032 X (T -I- 460) X V
vs X Tt X Ps X ^d X
10. Par-ticulate ~ probe, cyclone, & filter, gr/SCF
'» • .
-------
A-7
ciilfl'.- total . sr/SCF
0.0154 X vA ••* .gr/scF
12. Pcrt/iculato - probe, cyclone & filter,
gr/CF at stack conditions
-'17.7XC XP X M ,
" dn s d
...
•c'-t =
(Ts + 460)
- gr/CF
13. Particulate - total, gr/CF P stack conditions
au
"J17.7 X Cao X Ps X Md
(TS + 160) .
11. Particulate - probe, cyclone, & filter,
C,., « 0.008U7 X C..n X Qc = Ib/hr.
'
„ .
1I>. Particulate .- total, Ib/hr.
CAV = 0.00857 X C X Q ,
a>v ao 's = l
-------
'A c:xc;t.'r.v i
-------
B-l
SRL 1281 25 0472
APPENDIX B
COMPLETE GASEOUS RESULTS WITH EXAMPLE CALCULATIONS
SCOTT RESEARCH LABORATORIES, INC
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B-2
en n'.vcc »•-.•.! r;.'iT.\
CV>. l.i
Run No.
pate
nig SO
T - Average Gas Kstor Temperature, F
P. - Bircwetric Pressure, "Hg abs.
V - VoH;n-e of dry g?s sampled & ins tor
m conditions, ft.-*
±L
«.n
^8,17
60
2M2,
2.7,78
1,3?
ppin SO 2
n.i
:0.8
060
S0.7332 X mg S02 X (Tm + 4GO)
ppm SO=
. \
-------
B-3
no, t:=;i:
Run iu.
mg N
Tr - Fles!; Tenipcrtiture, F
~v7-~7iasirVchiiiieT litorT~
P- - Initial Fliisk Vacuum, "frj
Pf- Final Flask Vacuum, "Hg.
ppm nc?
0.123
-6,7
- 2.
2.1
_.
'0.173
73
2 MO
J, 0
. 7
2,113
O.H2.
f
2-0 81
*
29.63 x mg NO 2 X (Tf + 460)
ppm
Vf X (P. - Pf)
v
-------
B-4
m. t;-;iss.jo:j
, A
Run io.
.Oats
tng NC
T. - Flask Tender?: tuiAe, F
Vf - Flask Volume, liters
Pf - Initial Flask Vacuu;n, "H-j.
P^- Final Flask Vacuum, "Hg.
ppm ilCo
Z-l
73
rvTT^
7o
1,110
2,
0.4,
0.108
o. » 86
O. (o
ppm N02=
29.63 x mg'K02 X. (Tf + 460)
Vf X (P. - Pf)
-------
B-5
e 0
i-'
KG. ti-;;.SSION'
Run i-o.
,Qate
mg K
Ti: - Flo?.!; Tcr.i.oGrr-ture, °F
u _ ri.->ci- v'rl'•••>-•> lit-T^
\ £ riv*o;\ Vulu-ii^. $ iiu^io
P-. - Initial FILLS/; V;;ciiu;:i, "Kj.
Pf- Final Flask Vacuum, "Hg.
ppm lie.
•3-
70
•8-2-
: I
--!--
70
83, \
1.7
70
0.2.17
1.6
88.1
3.H-
0.197
7o
2,oQ^
-3-6
63
2,113
2,4,
ppm -
29.63 x mg NO 2 X (Tf + 460)
Vf X (P1 - Pf)
-------
B-6
SRL 1281 25 0472 . *
ORSAT ANALYSIS DATA SHEET
Run Sample
No. Location Date
1 Inlet Feb. 29
1 Outlet Feb. 29
2 Inlet March 1
2 Outlet March 1
3 Inlet March 2
3 Outlet March 2
Analysis
Number
1
2
3
Avg.
1
2
3
Avg.
1
2
3
Avg.
1
2
3
Avg.
1
2
3
Avg.
1
2
3
Avg.
%
"CO
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
%
CO
0.9
0.9
0.9
0.9
0.9
1.0
1.0
1.0
0.9
1.0
0.9
0.9
0,5 .
0.9
0.8
0.7
1.0
1.0
1.0
1.0
0.2
0.1
0.1
0.1
%
°2
19.4
20.0
19.6
19.7
19.1
19.2
19.2
19.2
18.5
18.8
18.6
18.6
19.7
19.8
19.6
19.7
19.1
18.9
19.0
19.0
20.6
20.5
20.6
20.6
SCOTT RESEARCH LABORATORIES, INC
-------
C-l
SRL 1281 25 0472
APPENDIX C
FIELD DATA
SCOTT RESEARCH LABORATORIES. INC
-------
— CW-e-f
%
Run
meet
Date
g
Sampling Train (Downstairs)
Gel Number
Correcfeinn
-------
?:';s$?};v>
&#*\ • ••'••'>'
Run
Sheet
y*
V,
Date
Sampling Train (Jovnstedrs)
Total
(SP in. H20)
Stack j Cal. Orifice
Temp. (AH, in, HaO)
-------
•J
vj
Run
Sheet
Date
Sampling Train (Downstair^)
Silic/Cel
Corfectlon
Probe'tip Dia. inches
Form 001
6/26/70
,^:,..^;-^»^ji^i-"^-
-------
W A T E R V 0 L' U It E
Run No./
DATE
Bubbler f 1
2 /
. V
Silica Gel No. Wgt. g S'p^. 3>
Bubbler # 4
Gross
Water Added (-)
Gross Wgt. (-)
Net
(A)
cc Net
(B)
g
Net
(A)
Het(B)(+).
Total Water
3d
cc
Fom R & D 109
-------
;.... vii. -Sheet,
Date Z / ? 9
Sample
Point
Time
7
f
IT
/
Vol.
(H3)
Pitot Tube
Sampling Train (Downstairs)
Press
00
lY
Vac.
Total
1
Stack i Cal. Orifice
(AP in. H20) I Temp. KAH in. HaO)
/<
it
2/0
°F j °F
76,
'&(
tin
'*%
Draft
(Ps in. H20
Silica Gel I-'uMber
Correction
Filter W^t. .<»
Tip Dia. inches
Vac.
in. Hg.
o
Form 001
.6/26./70
-------
Run
Sheet
Date
Sampling Train (Downstairs)
{
Sample | Time
Point
Vol.
(H3)
Pitot Tube
Press
Vac.
Total
(AP in.
Stack j Cal. Orifice
Temp. KAH in. H20)
Draft
(Ps in. HaO
Vac.
in. Hg.
/C"
/7
, > J
y
r?
/- //
V
n
Silica Gel '-'umber
Correction
Filter W?t. <>
Tip Dia. inches
JFprm 001
-------
/
Run
{'£>
Sheet
Date
Sampling Train (Downstairs)
Sample | Time
Point I
Vol.
(H3)
Pitot Tube
Press
Vac.
Total
in. HaO)
Stack i Cal. Orifice
Temp. KAH in. HoO)
OF
T2
oF
Draft
(Ps in. H20
Vac.
in. Eg.
/
5"
•T
so
zt-
"7
tr
f
2--V
o
oo
,47
•to
/2--3
Silica Gel I-'unber .;' /,-
Correction T
Filter
Probe Tip Dia. inches
Form 001
6/26/70
r>it?
. •^r'>* '
-------
Run
Sheet
Date
Sampling Train (Downstairs)
Sample | Time
Point 1
Vol.
(H3)
Pitot Tube
Press
Total
Vac. I (AP in. H20)
Stack i Cal. Orifice
Temp. KAH in. HaO)
Draft
(Ps in. H20
Vac .
in.
>3
,$Q
y
H
. V
4-
-
f.l*
i
jr
/.-r
!$<*
I-'umber
Filter Wi»t. a
T'robe Tip Dia. inches
Form 001
6/26/70
-------
WATER VOLUME
Run No.
Bubbler # 1 3
Silica Gel No. 8 Wgt. g
#3 / O
Bubbler # A
Gross
Water Addad (-)
Gross Wgt. (-)
. 2.O
H.t
(B)
g
Ket
(A)
Total Water
/ f /
Forn R & D 109
-2>
/ QQ X / $ .
/ (f^. 0
-------
\\
,'/6>?.i ,„*;'•
Sampling Train (Downstairs)
Cal. Orifice
in. HaO)
Total
(AP in. H20)
Sample | Time
Point
'"" -ki^fc'W^ll^S**-
ftfe->i*v-:sjlif; 'r'*k A/V&SJSSB',
fe,; -':-:-:'4,a>-tjae^r;?'-*ic.J*-.*.«t--'^.,r^ .-.
-------
Sampling Train (Downstairs)
Sample Time
Point 1
-------
<.--(-t>
Run
Sheet
Date
///V>X
Sampling Train (Downstairs)
Pitot Tube
Stack i Cal. Orifice
Sample | Time
Point
(AP in. H20)
(Ps in. H20
Silica Gel timber .._. ..*
Correct-ion
. .Probe Tip Dia. inches ' f2. 4
Form 001
-------
W A T E R A' 0 L U H E
No. DATE ^ / /
-. ^^u
Bubbler #1 3 ^ d Silica Gel No. 1 Wgt. g _ j J7^ f S"
3 * a ° Bubbler t
*f' S
Gross "
Water Added (-) - _ Gross Wgt. (-)
Net(A) .cc Het(B) $, 7 5 B
Ket(A)
Total Water ^-> < cc
3/3
Fora R & D 109
-------
Run
Sheet
Date
Sampling Train (Downstairs)
Sample
Point _J
v.:..
-'-
-;
./
;-
Time
,y
9
•; -"
'' Y(
,'- !
. ,
'. ./
:> ..'
^
' ^ y
Vol.
(H3)
*?rtf
TrtJ^,
7V>
•7££
' <5r //
<^< x°
'•' i
^<>3
^o:
fasC
#t,*f
<$,7\
Pitot Tube m
Press j
i
i
»
#
f S
I
>
>
i
Vac.
Total
(fiP in. H20)
ito
***°
~> '^
li (
/ s —
^^
//2.
f<0
tr*
/,^-
' ti?-
Stack i
Temp.
/;. f
•••/
f
Cal. Orifice
{AH in. H20)
^V
/^ ^
"^•5 — '
z.?
z, ^
A 7
'/7
'••y
7
A 7
/;7
oj
?'J
^^
&B-
7/
T^
^3
^^
^v
11
1 ~"
ff>
T2
op
6?
^^
7^
7X
73
7>
7^
77
7f
*0
8X
Draft
(Ps in. H20
> '
- /, -7 *
-A r"
"/^
-,. g2>
',6Z.
-r>y
— "6
^":vf ^- •• -
s ^r
Vac.
in. HK.
7
7
^
^*
V
^
3
3 *'
^^ • ^ 1
1
3 )
5
(%
^t^v(>°
J- Silica Gel I-'umber
Correction ^
Filter W
Probe Tip Dia. inches
(^ll^
r^-^i. Form 001
6/26/70
-------
Run
Sheet
Date
Sampling Train (Downstairs)
Sample
Point
Time
Vol.
(H3)
Pitot Tube
Press
Vac.
Total
(AP in. H20)
Stack ! Cal. Orifice j TI
Temp. |(AH in. H20) I °F
T2
OF
Draft
(Ps in. H20
Vac.
in. HR.
W"
o
.57
X
lo
•z.
**
.« 5
s-i
XV*'
la**
I
z
\tfrt
Silica Gel I-'unber
Correction
.-*•/
Filter W^t. ?»
Probe Tip Dia. inches
.
Form 001
6/26/70
-------
f
Run
Sheet
Date
Sampling Train (Downstairs)
Sample | -Time
Point I
Vol.
(H3)
Pitot Tube
Press _
Vac.
Total
(AT in. H20)
Stack i Cal. Orifice
Temp.
in. Had)
T2
OF i OF
Draft
(Ps in. H20
Vac.
in. Hg.
2,
fir?
*
7
is*
t*
A?
AX.
2. -6
A?
,19
rf^*iM*p
o
'5*
//T
W/5''
•/:.,. 7-
fP
Silica Gel t'umber
Correction
Filter
<»
*Tobe Tip Dia. inches
Form 001
6/26/70
-------
Sheet
Date
Sampling Train (Downstairs)
Sample Time
Point
Pitot Tube
Total
(fiP in. H20)
Stack ! Cal. Orifice
Temp.
AH in. HaO)
Op
op
; Draft
(Ps in. H20
Vac
in.
'fe
'*
to
.XT'
/oo
oo
/o/
to
Silica Gel Jfriber
Correction
Filter
-------
C-19
A T E R V 0 L U It E
"(•
Run No.
DATE
Bubbler # 1 'Z
Silica Gsl No. Wgt. g
7
Bubbler #
Grose
Water Added (-)
Gross Wgt. (-)
Net
(A)
cc
Net
(B)
«8t
(A)
Net(B)(+)
Total Water
Form R & D 109
cc
-------
U-f
Run.
T/? -V
Sheet
?•• "<,...
Date
'•
...> y
.
Sampling Train (Downstairs)
-------
Run
Sampling Train (Downstairs)
Stack i Cal. Orifice
Sample | Time
Point
(IT) Press
(AP in. H20) \ Temp.
(Ps in. H20
/£_ >*
a- s' ** * -•--*-•. •• • •'"TV&-•/(*•-• _-. >' ,-.-.V: .'- -V^.-^'*•}-:,{- f f
i iJJ «£.<-.- jf' P ^"^ -" '•'- : •'''• '• $***$&- "" •" '-'-''•'' 'v' •'" i=-^i'^?^?-'>•---""•
'%5
-------
Run
Sheet
Date
Sampling Train (Downstairs)
•'.sfeyfr??:*'" '• ••'•••Ji'i'-.'i'1?'.-"/^*
"m*. *'*^iiifi
tM
**-;
Probe Tip Dia. inches :/.:•!g? »fe ^i^- - JM^
:..-- • —in .-. * <•- K AM—S~'." • • -lE^S1
Sample j Time
Point i
Vol.
(H3)
Pi tot Tube
Press
Vac.
Total
(AP in. H20)
Stack i Cal. Orifice
Temp. KAH in. H2Q)
8-.
-
*/
7/7,
/,/ r
tub
.12
7/7
f 3
.00
. 77
7*7
73^
.J€^
;*&
<>. :.•.
Correction factor 'x||V'>;'.'f'jfe
-------
L f T 7
E ''*'J / < I/
WATER VOLUME '' fa/
Run No.
Bubbler /!1 7 Lf- O
«9 i ^s'
Date
Silica Gel No,
i>^f
Gross
Water Added(-)
Net
(A)
S
cc
Bubbler
Gross Wgt.(-
Net
(B)
Net
(A)
Net (+)
(B)
37
Total Water
cc
Forn R&D 109
-------
Run
Sheet
i
Date
i"7
Sampling Train (Downstairs)
Sample
Point
•?
*
>r"
;•- ' /
P
i
Time
"'• '7
' «,; •
Vol.
(H3)
/frj;^
/*£y V
t f '
to
/
j
:
Vac.
... ~A /6 ,, .-. v^ Silica Gel
,- •• ^* .-> -^ -X »•—.
* i; ^(v •; Correction
'JO ''- '' ' " y f4
/r ,/>' ; ->u ' \.'-~? $ "••'
\\\J~ * ;.1-' r l'+ ' • -*/
Total
(flP in. H20)
1ST
1O
7*—
i ^i_,,.'
/ G
... -l'ffl
7'- 3)
(< Z.
' /.'• -i—
/ ".'.'„-
. /, ^ --"
(< to
. j
Stack
Temp.
/x-r-
Number . 5 ' 0 ;-. • rf- .
Cal. Orifice
~)
t,y
f
OF
7*
6 x
3-6
rq
f.;7
f2-
?^
'^y
•f-y
c?-/
?'>
OF
70
?o
If
72L
>y
/
V
>g!
.)^
'^;?-
&/
Draft
(Ps in. H20
- 'a
— 2., T'
• 2 ,- v- '
- z . :r"
- 2. (7
c
-^ 3
-f -r .PX. 2 9
-------
Run
Sheet
••¥•/' o
'/•/ /
Date
/ / •> -
Sampling Train (Downstairs)
Sample
Point
f *"~p
i •*"
Y
' C!
'-.-• "
Time
"^9
•f 2-
// -
;lry:'
'? f
-, i/
/'
"'
'- - •
Vol.
(H3)
/#r
5~
>
_-^
r
> .'
r.r
r?
j
'?
Vac.
Total
(AT in. H20)
tf
! ^
Av X
r^U
.40
,HJ
• ,ri
/ v ;?
(7^>
M /
'6^
i
Stack i
Temp.
/2~ "}"
i f A
•
Cal. Orifice
(AH in. H20)
f:y_
1 6 r"
,"~~'
'' ^ _-jiiii_
-~ • ,
/ff
4 6
,, >/
[
vyc?
/, ^o
4
?£•
?.^
^6.
'/^
fAt
"? *r
^.i
7^
^
It: •
< 6
T2
^3
^•3
^y
^3
^3
'6{
i
bb
". j
r>
V V™"^
Draft
(Ps in. H20
- /, :T •
^ v ^J
— , V >
~ y--
-.'-."^
~ ' ffl 0
"• 75""" -
- , & 6
-,-gr^
.-•"-» , "~""*
"^' * 4 ^\
* • \J '" .'
-,1 £
Vac.
in. HR.
$
3
2~.
2^
^,.
ZL.
' -2L- -
5 •';
, 3
5 •
j>
>
. -•
N>
Silica Gel I'umber
Correctinn
Filter W<»t. o
Probe Tip Dia. inches
Form 001
6/26/70
-------
Run
Sheet
Date
0. H-7'r: SamplinR Train (Downstairs)
j
s
•*,
1
j;
!•"
;'i
Sample
Point
Time
••
Vol.
(H3)
*' v.
2 '
-> ^ ":r
?^J
ha?.
I* .„ ''•'
&>>*>
- 3 ••>
i
i
i
Pitot Tube _,
Press ,
?
sr"
7
f"
''i
} ' i~^
2
i* .. .
-7
*•
7
Vac.
Total
(AP in. H20)
}',-/
2
. V •' ;"~~"
/v-'
'
Stack
Temp.
-/ :• .;•--
Cal. Orifice
[{AH in. H20)
:;,£"
1.0
-} , ~?
?~- 3
/.-^
(
A C
/ ' ?
) ^"'"~"
/ . ^
'' 7
••'- y
f
Ti
oF
^3
•-7 .- " -
;' -1 • .-
-' •-.
,*»
1W"
9 •-?
•'-rt/
/ M)
1?
.•'*/-'
••--I (
.^f.
• t '•-./
/n
T2
OF
Jra
r'7" ./
'n:; .>
*-v
v •.,
b'T"
.-.-> "«-.,
>' X
» ;> . -;
S£
f '
Draft
(Ps in. H20
- /. ,r~ •
... // , .>
- ;:; , ^
- ?- - O
— ', >
- / r
- /.y
-d
-~ f, )'•'"
-/. 7
y r~- — •"
— ... f , -j
Vac.
in. HK.
&
(3
5"^"'
J**"
Z/
^::\:"'--
•A ;-.-•
^
V
_,.>'••
f
f
O
Silica Gel I-'unber
Correction
Filter
Tip Dia. inches
Form 001
6/26/70
-------
'Ran
Sheet
Date '*-/V/."-V
2 5>,» 7
Sampling Train (Downstairs)
Cample | Time
Vol.
(H3)
Pi tot Tube ^
Press
Vac.
Total
(AP in. H20)
Stack ! Cal. Orifice
Temp.
Tt
°F
T2
°F
Draft
(Ps in. HaO
Vac.
in. Hg.
M
/
n-
,
NJ
Rilica Gel du
Correction
Filter
\<* >- C
Probe Tip Dia. inches • • ^ •"'.•
-------
C-28
A i E r. v o L u
Bubblar j? 1 c0 O^ Silica Gal Ho. _ ___ Wgt. £ _i5..L
0 2 A££
Uoter ^^dcd
Nct(A) ,JV;i' CC NeL(B)
Het(A)
Tol;al Water <^~~ ' ~> cc
Fom R & D 109
-------
C-29
LABORA
4ND-6EN'ill
LABORATORY
-------
C-30
LABOR
4ND-GEN-1 I
LABORATORY
- 2.
TEST ENGINEER
•"•''•STM^'1"
-------
C-31
LABORATORY
LABORATORY TEST SHEET
4ND-GEN-1 Mftw V ••••,; i-:-i*(Vt. „«•«,•;.-....,..,. ,
-------
LABORATORY TEST SHEET
'
C-32
LABORATORY
12,81-2.
TEST ENGINEER
•"'i
OBSERVERS
DATE ^
T»«T EQUIPMENT
A
/4ft?
21/6
o*
0700
67 00 • -
w
X. : ./'
. '(
v . •)
•a • .:'
A . /
. .*
n*
855?£i-i_
**' '
. ': , ..--<
-------
C-33
LABORATORY TEST SHEET
4NO-GEN.I 1 IB
LABORATORY
-------
C-34
- 3,i^
LABORATORY TEST SHEET
4ND-GEN-! Ill
LABORATORY
fl/0<
TEST ENGINEER
OBSERVERS
TEST EQUIPMENT
. /•?
$• &fr*/g
£.
1(00
A/I-
111/
/iOO
1(00
73
Jl oO
i**?1
4. ft?
7*
27.98
••*"'•
-------
LABORATORY TEST SHEET
4ND-GEN-I It! , /.''•'• , ' •
C-35
LABORATORY
TEST ENGINEER
OBSERVERS
TEST EQUIPMENT
-------
C-36
LABORATORY TEST SHEET
JNO.'GEN.HH
LABORATORY
TEST ENGINEER
OBSERVERS
/
TEST EQUIPMENT
:\-;£-:c£:£v*'*$:- •.
TO
• - •• .. >•- •
,-VVjV;4VV.*
•X";-1- :VX'f V.
-------
C-37
LABORATORY TEST SHEET
4No-6EN-l I IB
LABORATORY
TEST ENGINEER
OBSERVERS
TICT EQUIPMENT
riAKfc
-------
D-l
SRL 1281 25 0472
APPENDIX D
STANDARD SAMPLING PROCEDURES
The sampling procedures used during the test are the same
as those published in the Federal Register, Volume 36, Number 247,
Thursday, Dcember 23, 1971. These methods are as follows (Methods 1,
2, 3, 5, 6, and 7). In addition, the impinger catch was analyzed.
SCOTT RESEARCH LABORATORIES, INC
-------
method (s) prescribed by the manufac-
turer(s) of such instrument, the instru-
ment shall be subject to manufacturers
recommended zero adjustment calibra-
tion procedures at least once per 24-hour
operating period unless the manufac-
turer^) specified or recommends cali-
bration at shorter intervals, in which
case such specifications or recommenda-
tions shall be followed. The applicable
method specified in the appendix of this
part shall be the reference method.
(c) Production rate and hours of op-
eration shall be recorded daily.
(d) The owner or operator of any sul-
furic acid production unit subject to the
provisions of this subpart shall maintain
a file of all measurements required by
this subpart. Appropriate measurements
shall be reduced to the units of the ap-
plicable standard daily and summarized
monthly. The record of any such meas-
urement and summary shall be retained
for at least 2 years following the date
of such measurements and summaries.
§ 60.85 Test methods and procedures.
(a) The provisions of this section are
applicable to performance tests for deter-
mining emissions of acid mist and sulfur
dioxide from sulfuric acid production
units.
(b) All performance tests shall be con-
ducted while the affected facility is oper-
ating at or above the maximum acid
production rate at which such facility
will be operated and under such other
relevant conditions as the Administrator
shall specify based on representative per-
formance of the affected facility.
(c) Test methods set forth in the ap-
pendix to this part or equivalent methods
as approved by the.Administrator shall
be used as follows:
(1) For each repetition the acid mist
and Sd concentrations shall be deter-
mined by using Method 8 and traversing
according to Method 1. The minimum
sampling time shall be 2 hours, and mini-
mum sampling volume shall be 40 ft.*
corrected to standard conditions.
(2) The volumetric flow rate of the
total effluent shall be determined by using
Method 2 and traversing according to
Method 1. Gas analysis shall be per-
formed by using the integrated sample
technique of Method 3. Moisture content
can be considered to be zero.
(d) Acid produced, expressed In tons
per hour of 100 percent sulfuric acid
shall be determined during each 2 -hour
testing period by suitable flow meters and
shall be confirmed by a material balance
over the production system.
(e) For each repetition acid mist and
sulfur dioxide emissions, expressed in lb./
ton of 100 percent sulfuric acid shall be
determined by dividing the emission rate
in Ib./hr. by the acid produced. The
emission rate shall be determined by
the equation, lb./hr.=QsXc, where
Q3=volumetric flow rate of the effluent
in it.'/hr. at standard conditions, dry
basis as determined in accordance with
paragraph (c) (2) of this section, and
c=acid mist and SO, concentrations in
lb./ft.* as determined in accordance with
paragraph (c)(l) of this section, cor-
rected to standard conditions, dry basis.
APPENDIX — Test METHODS
METHOD 1— 8AMPU AND VELOCITY TRAVERSES
FOB STATIONARY 8OT7BCES
1. Principle and Applicability.
1.1 Principle. A sampling site and the
number of traverse points are selected to aid
In 'the extraction of a representative sample.
1.2 Applicability. This method should
be applied only when specified by the test
procedures for determining compliance with
the New Source Performance Standards. Un-
less otherwise specified, this method Is not
Intended to apply to gas streams other than
those emitted directly to the atmosphere
without further processing.
2. Procedure.
2.1 Selection of a sampling site and mini-
mum number of traverse points.
2.1.1 Select a sampling site that Is at least
eight stack or duct diameters downstream
and two diameters upstream from any flow
disturbance such as a bend, expansion, con-
traction, or visible flame. For rectangular
cross section, determine an equivalent diam-
eter from the following equation:
2.1.2 When the above sampling site
criteria can be met, the minimum number
of traverse points Is twelve (12).
2.1.3 Some sampling situations render the
above sampling site criteria Impractical.
When this Is the case, choose a convenient
sampling location and use Figure 1-1 to de-
termine the minimum number of traverse
points. Under no conditions should a sam-
pling point be selected within 1 Inch of the
stack wall. To obtain the number of traverse
points for stacks or ducts with a diameter
less than 2 feet, multiply the number of
points obtained from Figure 1-1 by 0.67.
2.1.4 To use Figure 1-1 first measure the
distance from the chosen sampling location
to the nearest upstream and downstream dis-
turbances. Determine the corresponding
number of traverse points for each distance
from Figure 1-1. Select the higher of the
two numbers of traverse points, or a greater
value, such that for circular stacks the num-
ber Is a multiple of 4, and for rectangular
stacks the number follows the criteria of
section 2.2.2.
2.2 Cross-sectional layout and location of
traverse points.
2.2.1 For circular stacks locate the tra-
verse points on at least two diameters ac-
cording to Figure 1-2 and Table 1-1. The
traverse axes shall divide the stack cross
section Into equal parts. .
NUMBER OF DUCT DIAMETERS UPSTREAM'
(DISTANCE A)
FROM POINT OF ANY TYPE OF
DISTURBANCE (BEND, EXPANSION, CONTRACTION. ETC.)
. ,
equivalent
„/ (length) (width)
equation 1-1
NUMBER OF DUCT DIAMETERS DOWNSTREAM*
(DISTANCE B)
Figure 1-1. Minimum number of traverse points.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
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Table 1-1. Location of traverse points in circular stacks
(Percent of stack diameter from inside wall to traverse point)
Figure 1-2. Cross section of circular slac'k divided Into 12 equal
areas, showing location of traverse points at centroid of each area.
0
0
— «*M • 1 M. ••
O
I
1
o .,' 9
i
!____,__.!.__ __..
1
O I " O
J
1
, 1 „.,
1
0 1 0
1
o
o
o
Figure 1-3. Cross section of rectangular stack divided into 12 equal
areas, with traverse points at centrpid of each area.
Traverse
point
number
on a
diameter
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
Number of traverse points on a diameter
2
14.6
85.4
4
6.7
25.0
75.0
93.3
6
4.4
14.7
29.5
70.5
85.3
95.6
8
3.3
10.5
19.4
32.3
67.7
80.6
89.5
96.7
10
2.5
8.2
14.6
22.6
34.2
65.8
77.4
85.4
91.8
97.5
12
2.1
6.7
11.8
17.7
25.0
35.5
64.5
65.0
82.3
88.2
93.3
97.9
14
1.8
5.7
9.9
14.6
20.1
26.9
36.6
63.4
73.1
79.9
85.4
90.1
94.3
98.2
16
T.6
4.9
8.5
12.5
16.9
22.0
28.3
37.5
62.5
71.7'
78.0
83.1
87.5
91.5
95.1
98.4
18
1.4
4.4
7.5
10.9
14.6
18.8
23.6
29.6
38.2
61.8
70.4
76.4
81.2
85.4
•89.1
92.5
95.6
98.6
20
1.3
3.9
6.7
9.7
12.9
16.5
20.4
25.0
30.6
38.8
61.2
69.4
75.0
79.6
83.5
87.1
90.3
93.3
96.1
93.7
22
1.1
3.5
6.0
8.7
11.6
14.6
18.0
21.8
26.1
31.5
39.3
60.7
68.5
73.9
78.2
82.0
85.4
88.4
91.3
94.0
96.5
9S-.9
24
1.1
3.2
5.5
7.9
10.5
13.2
16.1
19.4
23.0
27.2
32.3
3.9.8
60.2
67.7
72.8
77.0
80.6
83.9
86.8
89.5
92.1
94.5
96.8
98.9
v»
I
o
I
o
v>
No. 247—Pt. n-
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
K
oo
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24884
RULES AND REGULATIONS
2.2.2 For rectangular stacks divide the
cross section into as many equal rectangular
areas as traverse points, such that the ratio
of the length to the width of the elemental
areas Is between one and two. Locate the
traverse points at the centrold of each equal
area according to Figure 1-3.
3. References.
Determining Dust Concentration in a Gas
Stream, ASME Performance Test Code #27,
New York, N.T., 1957.
Devorkin, Howard, et al., Air Pollution
Source Testing Manual, Air Pollution Control
District, Los Angeles, Calif. November 1963.
Methods for Determination of Velocity,
Volume, Dust and Mist Content of Gases,
Western Precipitation Division of Joy Manu-
facturing Co., Los Angeles, Calif. Bulletin
WP-50, 1968.
Standard Method for Sampling Stacks for
Paniculate Matter, In: 1971 Book of ASTM
Standards, Part 23, Philadelphia, Pa. 1971,
ASTM Designation D-2928-71.
METHOD 2 DETERMINATION OP STACK GAS
VELOCITY AND VOLUMETRIC FLOW HATE (TTPE
S FTTOT TUBE)
1. Principle and applicability.
1.1 Principle. Stack gas velocity is deter-
mined from the gas density and from meas-
urement of the velocity head using a Type S
(Stauschelbe or reverse type) pltot tube.
1.2 Applicability. This method should be
applied only when specified by the test pro-
cedures for determining compliance with the
New Source Performance Standards.
2. Apparatus.
2.1 Pltot tube—Type 8 (Figure 2-1), or
equivalent, with a coefficient within ±6%
over the working range.
2.2 Differential pressure gauge—Inclined
manometer, or equivalent, to measure velo-
city head to within 10% of the minimum
value.
2.3 Temperature gauge—Thermocouple or
equivalent attached to the pltot tube to
measure stack temperature to within 1.5% of
the minimum absolute stack temperature.
2.4 Pressure gauge—Mercury-filled U-tube
manometer, or equivalent, to measure stack
pressure to within 0.1. in. Hg.
2.5 Barometer—To measure atmospheric
pressure to within 0.1 In. Hg.
2.6 Gas analyzer—To analyze gas composi-
tion for determining molecular weight.
2.7 Pltot tube—Standard type, to cali-
brate Type S pitot tube.
3. Procedure.
3.1 Set up the apparatus as shown In Fig-
ure 2-1. Make sure all connections are tight
and leak free. Measure the velocity head and
temperature at the traverse points specified
by Method 1.
3.2 Measure the static pressure In the
stack.
3.3 Determine the stack gas molecular
weight by gas analysis and appropriate cal-
culations as indicated In Method 3.
PIPE COUPLINC
TUBING ADAPTER
4. Calibration.
4.1 To calibrate the pltot tube, measure
the velocity head at some point in a flowing:
gas stream with both a Type S pltot tube and
a standard type pitot tube with known co-
efficient. Calibration should be done In the
laboratory and the velocity of the flowing gas
stream should be varied over the normal
working range. It is recommended that the
• calibration be repeated after use at each field
site.
4.2 Calculate the pitot tube coefficient
using equation 2-1.
=CD
equation 2-r
where :
CP
t = Pitot tube coefficient of Type S
pitot tube.
CPstd=Pitot tube coefficient of standard
type pitot tube (If unknown, use
0.99).
Ap«ta= Velocity head measured by stand-
ard type pitot tube.
Apt,Bt = Velocity head measured by Type S
pltot tube.
4.3 Compare the coefficients of the Type S
pltot tube determined first with one leg and
then the other pointed downstream. Use the
pitot tube only if the two coefficients differ by
no more than 0.01.
5. Calculations.
Use equation 2-2 to calculate the stack gas
velocity.
P.M.
Equation 2-2
where:
(VOov«.=Stack gas velocity, feet per second (f.p.s.).
are used.
Cp=pitot tube coefficient, dlmenslonless.
(T,)a,,.=Average absolute stack gas temperature,
°R.
.=Average velocity head of stack gas, inches
HiO (see Fig. 2-2).
P.=Absolutc stack gas pressure, inches Hg.
M,=Molecular weight of stack gas (wet basis),
ib./lb.-mole.
Md(l-B,0)+18B..
Md = Dry molecular weight of stack gas (from
Method 3).
Bwo = Proportion by volume of water vapor in
the gas stream (from Method 4).
Figure 2-2 shows a sample recording sheet
for velocity traverse data. Use the averages
In the last two columns of Figure 2-2 to de-
termine the average stack gas velocity from
Equation 2-2.
Use Equation 2-3 to calculate the stack
gas volumetric flow rate.
Q.=3600
I
Figure 2-1. Pitot tube-manometer assembly.
Equation 2-3
There:
Q,= Volumetric flow rate, dry basis, standard condi-
tions, ft.Vhr.
A = Cross-sectional area of stackj ft.1
Tiu=Absolute temperature at standard conditions,
830° K.
Piw=AbsoIute pressure at standard conditions, 29.02
Inches Hg.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
RULES AND REGULATIONS
24885
6. References.
Mark. L. a.. Mechanical Engineers' Hand-
book, McGraw-Hill Book Co., Inc., New York,
N.T.. 1951.
Perry, J. H., Chemical Engineers' Hand-
book, McGraw-Hill Book Co., Inc., New York,
N.Y., 1960.
Shlgehara, B. -T., W. F. Todd, and W. S.
Smith, Significance of Errors In Stack Sam-
PLANT_
DATE
RUN NO.
STACK DIAMETER, in.
BAROMETRIC. PRESSURE, in. Hg._
STATIC PRESSURE IN STACK (Pg), in. Hg.
OPERATORS
pllng Measurements. Paper presented at the
Annual Meeting of the Air Pollution Control
Association, St. Louis, Mo., June 14-19, 1970.
Standard Method for Sampling Stacks for
Partlculate Matter, In: 1971 Book of ASTM
Standards, Part 23, Philadelphia, Pa., 1971,
ASTM Designation D-2928-71.
Vennard, J. K., Elementary Fluid Mechan-
ics, John Wiley & Sons, Inc., New York, N.Y.,
1947.
SCHEMATIC OF STACK
CROSS SECTION
Traverse point
number
Velocity head,
in. H2O
Stack Temperature
-------
24886
RULES AND REGULATIONS
METHOD 3 GAS ANALYSIS FOE CARBON DIOXIDE,
EXCESS AIR, AND 'DRY MOLECULAB WEIGHT
1. Principle and applicability.
1.1 Principle. An Integrated or grab gas
sample Is extracted from a sampling point
and analyzed lor Its components using an
Orsat analyzer,
1.2 Applicability. This method should be
applied only when specified by the.test pro-
cedures for determining compliance with the
New Source Performance Standards. The test
procedure will Indicate whether a grab sam-
ple or an Integrated sample is to be used.
2. Apparatus.
2.1 Grab sample (Figure 3-1).
2.1.1 Probe—Stainless Bteel or Pyrex1
glass, equipped with a filter to remove partic-
ulate matter.
2.1.2 Pump—One-way squeeze bulb, or
equivalent, to transport gas sample to
analyzer.
1 Trade name.
2.2 Integrated sample (Figure 3-2).
2.2.1 Probe—Stainless steel or Pyrex1
glass, equipped with a filter to remove pnr-
ticulate matter.
2.2.2 Air-cooled condenser or equivalent—
To remove any excess moisture.
2.2.3 Needle valve-^To adjust flow rate.
2.2.4 Pump—Leak-free, diaphragm type,
or equivalent, to pull gas.
2.2.5 Rate meter—To measure a flow
range from 0 to 0.035 cfm.
2.2.6 Flexible bag—Tedlar,1 or equivalent,
with a capacity of 2 to 3 cu. ft. Leak test the
bag In the laboratory before using.
2.2.7 Pilot tube—Type S, or equivalent,
attached to the probe so that the sampling
flow rate can be regulated proportional to
the stack gas velocity when velocity Is vary-
ing with time or a sample traverse is
conducted.
2.3 Analysis.
2.3.1 Orsat analyzer, or equivalent.
PpOBE
FLEXIBLE TUBING
TO ANALYZER
TERIG
FILTER (GLASS WOOL)
SQUEEZE BULB
Figure 3-1. Grab-sampling train.
RATE METER
VALVE
AIR-COOLED CONDENSER
PROBE
FILTERloLASSWOOLJ
QUICK DISCONNECT
RIGID CONTAINER"
I Figure 3-2, Integrated gas • sampling train.
3. Procedure.
3.1 Grab sampling.
3.1.1 Set up the equipment as shown In
Figure 3-1, making sure all connections are
leak-fret. Place the probe in the aback at a
sampling point and purge the sampling line.
3.1.2 Draw sample Into the analyzer.
3.2 Integrated sampling.
3.2.1 Evacuate the" flexible bag. Set up the
equipment as shown in Figure 3-2 with the
bag disconnected. Place the probe In the
stack and purge the sampling line. Connect
the bag, making sure that all connections are
tight and that there are no leaks.
3.2.2 Sample at a rate proportional to the
stack velocity.
3.3 Analysis.
3.3.1 Determine the CXX, O,, and CO con-
centrations as soon as possible. Make as many
passes as are necessary to give constant read-
ings. If more than ten passes are necessary,
replace the absorbing solution.
3.3.2 For grab sampling, repeat the sam-
pling and analysis until three consecutive
samples vary no more than 0.5 percent by
volume for each component being analyzed.
3.3.3 POT Integrated sampling, repeat the
analysis of the sample until three consecu-
tive analyses vary no more than 0.2 percent
by volume for each component being
analyzed.
4. Calculations.
4.1 Carbon dioxide. Average the three con-
secutive runs and report the result to the
nearest 0.1% CO.J.
4.2 Excess air. Use Equation 3—1 to calcu-
late excess air, and average the runs. Report
the result to the nearest 0.1% excess air.
%EA =
v '0 ^2> "-"' 10 ^> v 100
0.264(% Nj) - (% Oj) +0.5C% CO) A
equation 3-1
where:
%EA=Percent excess air.
%O.=Percent oxygen by volume, dry basis.
%Nj=: Percent nitrogen by volume, dry
basis.
% CO=: Percent carbon monoxide by vol-
ume, dry basis.
0.264=Ratio of oxygen to nitrogen In air
by volume.
4.3 Dry molecular weight. TJse Equation
3-2 to calculate dry molecular vreight and
average the runs. Report the result to the
nearest tenth.
Md = 0.44(%COn) +0.32(%O.,)
+ 6.28(%N.,+ %CO)
equation 3-2
where:
M«=Dry molecular weight, Ib./lb-mole,
%COa=Percent carbon dioxide by volume,
•dry basis.
%Os=Percent oxygen by volume, dry
basis.
%Nj=Percent nitrogen by volume, dry
basis.
0.44=Molecular weight of carbon dloxld*
divided by 100.
0.32=Molecular weight of oxygen divided
by 100.
0.28=Molecular weight of nitrogen aod
CO divided by 100.
FEDERAL REGISTER, VOL 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
5. References.
Altshuller, A. P., et al., Storage of Gases
and Vapors in Plastic Bags, Int. J. Air &
Water Pollution, 6:75-81, 1963.
Conner, William D., and J. S. Nader, Air
Sampling with Plastic Bags, Journal of the
American Industrial Hygiene Association,
25:291-297, May-June 1964.
Devorkin, Howard, et al., Air Pollution
Source Testing Manual, Air Pollution Con-
trol District, Los Angeles, Calif., November
1963.
METHOD 4 DETERMINATION OP MOISTURE
IN STACK GASES
1. Principle and applicability.
1.1 Principle. Moisture is removed from
the gas stream, condensed, and determined
volumetrically.
1.2 Applicability. This method is appli-
cable for the determination of moisture in
stack gas only when specified by test pro-
cedures for determining compliance with New
Source Performance Standards. This method
does not apply when liquid droplets are pres-
ent in the gas stream' and the moisture is
subsequently used in the determination of
stack gas molecular weight.
Other methods such as drying tubes, wet
bulb-dry bulb techniques, and volumetric
condensation techniques may be used.
2. Apparatus.
2.1 Probe—Stainless steel or Pyrex - glass
sufficiently heated to prevent condensation
1 If liquid droplets are present in the gas
stream, assume the stream to be saturated,
determine the average stack gas temperature
by traversing according to Method 1, and
use a psychrometric chart to obtain an ap-
proximation of the moisture percentage.
"Trade name.
.P.tdM
H20
where:
Vwc=Volume of water vapor collected
(standard conditions), cu. ft.
Vi=Final volume of impinger contents,
ml.
Vi=Initlal volume of impingei con-
tents, ml.
R=Ideal gas constant, 21.83 Inches
and equipped with a filter to remove partlcu-
late matter.
2.2 Implngers—Two midget implngers,
each with 30 ml. capacity, or equivalent.
2.3 Ice bath container—To condense
moisture in Implngers.
• 2.4 Silica gel tube (optional)—To protect
pump and dry gas meter.
. 2.5 Needle valve—To regulate gas flow
rate.
2.6 Pump—Leak-free, diaphragm type, or
equivalent, to pull gas through train.
2.7 Dry gas meter—To measure to within
1% of the total sample volume.
2.8 Rotameter—To measure a flow range
from 0 to 0.1 c.f.m.
2.9 Graduated cylinder—25 ml.
2.10 Barometer—Sufficient to read to
within 0.1 inch Hg.
2.11 .Pitot tube—Type S, or equivalent,
attached to probe so that the sampling flow
rate can be regulated proportional to the
stack gas velocity when velocity is varying
with time or a sample traverse is conducted.
3. Procedure.
3.1 Place exactly 5 ml. distilled water in
each impinger. Assemble the apparatus with-
out the probe as shown in Figure 4-1. Leak
check by plugging the Inlet to the first 1m-
plnger and drawing a vacuum. Insure that
flow through the dry gas meter is less than
1 % of the sampling rate.
3.2 Connect the probe and sample at a
constant rate of 0.075 c.f.m. or at a rate pro-
portional to the stack gas velocity. Continue
sampling until the dry gas meter registers 1
cubic foot or until visible liquid droplets are
carried over from the first Impinger to the
second. Record temperature, pressure, and
dry gas meter readings as required by Figure
4-2.
3.3 After collecting the sample, measure
the volume increase to the nearest 0.5 ml.
4. Calculations.
4.1 Volume of water vapor collected.
SILICA GEL TUBE
ml.
equation 4-1
Hg—cu. ft./lb. mole-°R.
piino—Density of water, 1 g./ml.
Titd=Absolute temperature at standard
conditions, 530° R.
Pstd=Absolute pressure at standard con-
ditions, 29.92 Inches Hg.
MH2o=Molecular weight of water, 18 lb./
Ib.-mole.
HEATED PROB!
ROTAMETER
FILTER
ICE BATH
Figure 4-1. Moisture-sampling train.
LOCATION.
TEST
DATE
COMMENTS
OPERATOR
BAROMETRIC PRESSURE
CLOCK TIME
GAS VOLUME THROUGH
METER, (Vm),
ft3
ROTAMETER SETTING
ft3/mirl_
METER TEMPERATURE,
•P
v»
§
m
O
v»
Figure 4-2. Field moisture determination*
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
QO
25
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24888
RULES AND REGULATIONS
4.2 Gas volume.
V,P,\
- In. Hg\ Tm equation 4-2
where:
Vine =Dry gas volume through meter at
standard oondltlODS, cu. ft.
Vm =Dry gas volume measured by meter,
co. ft.
Pm = Barometric pressure at the dry gets
meter, Inches Hg.
P.ta=Pressure at standard conditions, 29.93
inches Hg.
T.td=Absolute temperature at standard
conditions, 530° R.
Tm = Absolute temperature at meter ( °F+
460), "R.
4.3 Moisture content.
Vw.
-+B.
V..
-+(0.025)
"°~V^ + V.
equation 4-3
*here:
Bwo=Proportion by volume of water vapor
In the gas stream, dlmenslonless.
V»« = Volume of water vapor collected
(standard conditions), cu. ft.
Vm. =Dry gas volume through meter
(standard conditions), cu. ft.
BWM = Approximate volumetric proportion
of water vapor in the gas stream
i leaving the Impingers, 0.025.
5. References.
Air Pollution Engineering Manual, Daniel-
eon, J. A. (ed.), UJ3. DHBW, PHS, National
Center for Air Pollution Control, Cincinnati,
Ohio, PHS Publication No. 999-AP-40, 1967.
Devorkin, Howard, et al., Air Pollution
Source Testing Manual, Air Pollution Con-
trol District, Los Angeles, Calif., November
1963.
Methods for Determination of Velocity,
Volume, Dust and Mist Content of Gases,
Western Precipitation Division of Joy Manu-
facturing Co., Los Angeles, Calif., Bulletin
WP-fiO, 1968.
METHOD 5—DETERMINATION or PAKTICUUITE
EMISSIONS FROM STATIONARY SOCHCES
1. Principle and applicability.
1.1 Principle. Particulate matter is with-
drawn Isoklnetlcally from the source and Its
weight Is determined gravimetrically after re-
moval of uncomlblned water.
1.2 Applicability. This method Is applica-
ble for the determination of partlculate emis-
sions from stationary sources only when
specified by the test procedures for determin-
ing compliance with New Source Perform-
ance Standards.
2. Apparatus.
2.1 Sampling train. The design specifica-
tions of the particulatc sampling train used
by EPA (Figure 5-1) are described in APTD-
0581. Commercial models of this train are
available.
2.1.1 Nozzle—Stainless steel (316) with
sharp, tapered leading edge.
2.1.2 Probe—Pyrex1 glass with a heating
system capable of maintaining a minimum
gas temperature of 250° F. at the exit end
during sampling to prevent condensation
from occurring. When length limitations
(greater than about 8 ft.) are encountered at
temperatures less than 600° P., Incoloy 825»,
or equivalent, may be used. Probes for sam-
pling gas streams at temperatures in excess
of 600° F. must have been approved by the
Administrator.
2.1.3 Pltot tube—Type S, or equivalent,
attached to probe to monitor stack gas
velocity.
3.1.4 Filter Holder—Pyrex» glass with
beating system capable of maintaining mini-
mum temperature of 225° F.
2.1.5 Implngers / Condense!1—Four Impin-
gers connected In series with glass ball joint
fittings. The first, third, and fourth Impln-
gers are of the Greenburg-Smith design,
modified by replacing the tip with a %-lnch
ID glass tube extending to one-half Inch
from the bottom of the flask. The second 1m-
plnger la of the Greenburg-Smlth design
with the standard tip. A condenser may be
used In place of the impingers provided,that
the moisture content of the stack gas can
still be determined.
2.1.6 Metering system—Vacuum gauge,
leak-free pump, thermometers capable of
measuring temperature to within 6° F., dry
gas meter with 2% accuracy, and related
equipment, or equivalent, as required to
maintain an isoklnetlc sampling rate and to
determine sample volume.
2.1.7 Barometer—To measure atmospheric
pressure to ±0.1 Inches Hg.
2.2 Sample recovery.
2.2.1 Probe brush—At least as long as
probe.
2.2.2 Glass wash bottles—Two.
2.2.3 Glass sample storage containers.
2.2.4 Graduated cylinder^-250 ml.
2.3 Analysis.
2.3.1 Glass weighing dishes.
2.3.2 Desiccator.
2.3.3 Analytical balance—To measure to
±0.1 mg.
2.3.4 Trip balance—300 g. capacity, to
measure to ±0.05 g.
3. Reagents.
3.1 Sampling.
3.1.1 Filters—Glass fiber, MSA 1106 BHi,
or equivalent, numbered for Identification
and preweighed.
3.1.2 Silica gel—Indicating type, 6-16
mesh, dried at 175° C. (350* F.) for 2 hours.
3.1.3 Waiter.
3.1.4 Crushed Ice.
3.2 Sample recovery.
3.2.1 Acetone—Reagent grade.
3.3 Analysis.
3.3.1 Water.
IMPINGER TRAIN OPTIONAL. MAY BE REPLACED
BY AN EQUIVALENT CONDENSER
HEATED AREA FILTER HOLDER / THERMOMETER CHECK
^VALVE
PROBE
REVERSE-TYPE
PITOT TUBE
IMPINGERS ICE BATH
BY-PASSVALVE
.VACUUM
LINE
THERMOMETERS'
VACUUM
GAUGE
MAIN VALVE
DRY TEST METER
AIR-TIGHT
PUMP
Figure 5-1, Particulate-sampling train.
3.3.2 Desiccant—Drierite,1 indicating.
4. Procedure.
4.1 Sampling
4.1.1 After selecting the sampling site and
the minimum number of sampling points,
determine the stack pressure, temperature,
moisture, and range of velocity head.
4.1.2 Preparation of collection train.
Weigh to the nearest gram approximately 200
g. of silica gel. Label a filter ot proper diam-
eter, desiccate * for at least 24 hours and
weigh to the nearest 0.5 mg. in a room where
the relative humidity is less than 50%. Place
100 ml. of water in each of the first two
Impingers, leave the third Impinger empty,
and place approximately 200 g. of preweighed
silica gel In the fourth impinger. Set up the
train without the probe as In Figure 5-1.
Leak check the sampling train at the sam-
pling site by plugging up the inlet to the fil-
ter holder and pulling a 15 In. Hg vacuum. A
leakage rate not In excess of 0.02 c.f.m. at a
vacuum of 15 in. Hg Is acceptable. Attach
the probe and adjust the heater to provide a
gas temperature of about 250° F. at the probe
outlet. Turn on the filter heating system.
Place crushed ice around the Impingers. Add
1 Trade name.
1 Trade name.
'Dry using Drierite *
at 70° F.±10° F.
more ice during the run to keep the temper-
ature of the gases leaving the last Impinger
as low as possible and preferably at 70° F.,
or less. Temperatures above 70° F. may result
in damage to the dry gas meter from either
moisture condensation or excessive heat.
4.1.3 Particulate train operation. For each
run, record the data required on the example
sheet shown In Figure 5-2. Take readings at
each sampling point, at least every 5 minutes,
and when significant changes In stack con-
ditions necessitate additional adjustments
In flow rate. To begin sampling, position the
nozzle at the first traverse point with the
tip pointing directly Into the gas stream.
Immediately start the pump and adjust the
flow to isokinetio conditions. Sample for at
least 5 minutes at each traverse point; sam-
pling time must be the same for each point.
Maintain Isokinetlc sampling throughout the
sampling period. Nomographs are available
which aid in the rapid adjustment of the
sampling rate without other computations.
APTD-0576 details the procedure for using
these nomographs. Turn off the pump at the
conclusion of each run and record the final
readings. Remove the probe and nozzle from
the stack and handle in accordance with the
sample recovery process described In section
4.2.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
RULES AND REGULATIONS
24S89
nun
tOCATION_
OPERATOR_
DATE
RUN NO.
SAUUBOINOj.
METER'BOX N0._
METER AH,
C FACTOR .
AU8IENT TEMPERATURE^
BAROMETRIC PRESSURE.
ASSUMED MOISTURE.»_
HEATEB BOX SETTING.,
MOSLENaiH.il
NOBLE DIAMETER. ta._
PROBE HEATER SETTING.
SCHEMATIC OF STACK CROSS SECTION
TRAVERSE POUR
NUMBER
TOTAL
SAMPLING
TIME
|0). irfiv
AVERAGE
STATIC
PRESSURE
(Ps). hi. Hg.
STACK
TEMPERATURE
Oy.'f
VEiocrrt
HEAD
I»PS!.
PRESSURE
DIFFERENTIAL
ACROSS
ORIFICE
METEB '
UHJ.
to. HjO
>
GAS SAMPLE
VOLUME
(Vml.fl3
SAS SAMPLE TEMPERATURE
AT DR» GAS METER
WLET
It-ta.l.*'
Avg.
OUTLET
ir»^.'f
A.J.
Avg.
SAMPLE BOX
TEMPERATURE.
"f
tE»ER»TtlRE
OF GAS
LEAVING
COTOEKEROR
LAST IMPINGE*.
°F
Tm=Average dry gas meter temperature,
Pb.r = Barometric pressure at the orifice
meter, Inches Hg.
AH = Average pressure drop across the
orifice meter, Inches H2O:
13.6= Specific gravity of mercury.
P.ld= Absolute pressure at standard con-
ditions, 29.92 inches Hg.
6.3 Volume of water vapor.
v..,d=v,j
where:
RT..
)-
Co.0474^^-"
V ml. J,
equation 5-2
Figure 52. Paniculate Held data.
4.2 Sample recovery. Exercise care In mov-
ing the collection train Irom the test site to
the sample recovery area to minimize the
loss of collected sample or the gain of
extraneous partlculate matter. Set aside a
portion of the acetone used in the sample
recovery as a blank for analysis. Measure the
volume of water from the first three 1m-
pingers, then discard. Place the samples in
containers as follows:
Container No. 1. Remove the filter from
its holder, place in this container, and seal.
Container No. 2. Place loose paniculate
matter and acetone washings from all
sample-exposed surfaces prior to the filter
in this container and seal. Use a razor blade,
brush, or rubber policeman to lose adhering
particles.
Container No. 3. Transfer the silica gel
from the fourth Implnger to the original con-
tainer and seal. Use a rubber policeman as
an aid In removing silica gel from the
impinger.
4.3 Analysis. Record the data required on
the example sheet shown In Figure 5-3.
Handle each sample container as follows:
Container No. 1. Transfer the filter and
any loose partlculate matter from the sample
container to a tared glass weighing dish,
desiccate, and dry to a constant weight. Re-
port results to the nearest 0.5 mg.
Container No. 2. Transfer the acetone
washings to a tared beaker and evaporate to
dryness at ambient temperature and pres-
sure. Desiccate and dry to a constant weight.
Report results to the nearest 0.5 mg.
Container No. 3. Weigh the spent silica gel
and report to the nearest gram.
5. Calibration.
Use methods and equipment which have
been approved by the Administrator to
calibrate the orifice meter, pltot tube, dry
gas meter, and probe heater. Recalibrate
after each test series.
6. Calculations.
6.1 Average dry gas meter temperature
and average orifice pressure drop. See data
sheet (Figure 5-2).
6.2 Dry gas volume. Correct the sample
volume measured by the dry gas meter to
standard conditions (70° F., 29.92 Inches Hg)
by using Equation 6-1.
(m
T»«
Tm
AH
= Volume of water vapor in the gas
sample (standard conditions),
cu. ft.
Vi0 = Total volume of liquid collected in
Implngers and silica gel (see Fig-
ure 5-3), ml.
PHSO=Density of water, 1 g./mL
MHSO=Molecular weight of water, 18 lb./
Ib.-mole.
R=Ideal gas constant, 21.83 Inches
Hg—cu. ft./lb.-mole-°R,
T.td=Absolute temperature at standard
conditions, 530' R,
PitlI = Absolute pressure at standard con-
ditions, 29.92 inches Hg.
6.4 Moisture content.
equation 5-3
where:
B w» = Proportion by volume of water vapor in the fiiS
stream, dlmensionlcss.
^*.ui=Volume of water in the gas sample (standard
conditions), cU. ft.
^"•td—Volume of gas sample through the dry gas motor
(standard conditions), cu. ft.
6.6 Total partlculate weight. Determine
the total partlculate catch from the sum of
the weights on the analysis data sheet
(Figure 6-3).
6.6 Concentration.
6.6.1 Concentration in gr./s.c.f.
equation 5-1
c'. = (o.0154j|^
where:
Vm...
Volume of gas sample through the
dry gas meter (standard condi-
tions), cu.'ft.
Vm = Volume of gas sample through the
dry gas meteor (meter condi-
tions) , cu. ft.
• ,tl — Absolute temperature at standard
conditions, 530° R.
equation 5-4
where:
o'i=Concentration of particulate matter In stack
gas, gr./s.c,f., dry basis.
M0=Total amount of partlculate matter collected,
mg.
^™.M=Volume of gas sample through dry gas meter
(standard conditions), cu. ft.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
24890
RULES AND REGULATIONS
PLANT.
DATE_
RUN NO.
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICIPATE COLLECTED,
mg
FINAL 'WEIGHT
x^
TARE WEIGHT
:xi
WEIGHT GAIN
FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME.
ml
SILICA GEL
WEIGHT,
g
9"| ml
CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
INCREASE BY DENSITY OF WATER. (1 g ml):
INCREASE- 9 = VOLUME WATER, ml
(1 g/ml)
6.6.2
Where:
c,
«3,600
Figure5-3. Analytical data.
Concentration in Ib./cu. ft.
/ 1 lb.\
.V453,600mgJM°
c. = -
Btd
Concentrat)on of pavticulate matter in stack
pas, lb./s.c.f., dry basis.
Mg/lb.
-=2.205X10-«vp!!-
Vm»td equation 5-5
Mn=Total amount of particulate matter collected,
mg.
Vn,Bl(J=Volume of gas sample through dry gas meter
(standard conditions), cu. ft.
6.7 Isokinetic variation.
v.0(PH,o)R
M
H.O
AH
flV.P.A.
X100
where:'
I=Percent of Isokinetic sampling.
V](.=Total volume of liquid collected In Implngers
and silica gel (See Fig. 5-3), ml.
PH,o=Denslty of water, 1 g./rnL
R=Ideal gas constant, 21.83 Inches Hg-cu. ft./lb.
mole-°R.
Mn^^Molecular weight of water, 18 Ib./Ib.-mole.
Vm =Volume of gas sample through the dry gas met er
(meter conditions), cu. ft.
T0=Absolute average dry gas meter temperature
(see Figure &-2),°R.
Pbar=Barometric pressure at sampling site, Inches
Hg.
AH=Average pressure drop across the orifice (see
Fig. 5-2), inches II2O.
T,=Absolute average stack gas temperature (see
Fig. 6-2), °R
9=Total sampling time, mln.
Vt=Stack gas velocity calculated by Method 2,
Equation 2-2, ft./sec.
P,=Absolute stack gas pressure, inches Hg.
A0=Cross-sectional area of nozzle, sq. ft.
6.8 Acceptable results. The following
range sets the limit on acceptable Isokinetic
sampling results:
If 90%
-------
necessary only If a sample traverse la re- 2.3.1 Glass wash bottles—Two.
quired, or If stack gas velocity varies with 2.2.3 Polyethylene storage bottles—To
time. store Implnger samples.
2.2 Sample recovery. 2.3 Analysis.
PROBE (END PACKED
WITH QUARTZ OR ./ 5^CK WALL
PYREX WOOL? • '-^
SILICA GEL DRYING TUBE
MIDGET BUBBLER MIDGET IMPINGERS
TYPESmOT
•PUMP
DRY GAS METER
Figure 6-1. SOg sampling train.
2.8.1 Pipettes—Transfer type, 8 ml. and
10 ml. sizes (0.1 ml. divisions) and 26 ml.
size (0.2 ml. divisions).
2.3.2 Volumetric flasks—50 ml., 100 ml.,
and 1,000 ml.
2.3.3 Burettes—5 ml. and 50 ml.
2.3.4 Erlenmeyer flask—125 ml.
3. Reagents.
3.1 Sampling.
3.1.1 Water—Deloulzed, distilled.
3.1.2 Isopropanol, 80%—Mix 80 ml. of iso-
propanol with 20 ml. of distilled water.
3.1.3 Hydrogen peroxide, 3%—dilute 100
ml. of 30% hydrogen peroxide to 1 liter with
distilled water. Prepare fresh daily.
3.2 Sample recovery.
3.2.1 Water—Delonized, distilled.
3.2.2 Isopropanol, 80 %.
3.3 Analysis.
3.3.1 Water—Deionized, distilled.
3.3.2 Isopropanol.
3.3.3 Thorln Indicator—l-(o-arsonophen-
ylazo)-2-naphthol-3,6-dlsulfonlc acid, diso-
dlum salt (or equivalent). Dissolve 0.20 g. in
100 ml. distilled water.
3.3.4 Barium perchlorate (0.01 N)—Dis-
solve 1.95 g. of barium perchlorate
[Ba(ClOJ,'3HaO] in 200 ml. distilled water
No. 247—Pt. H 3
and dilute to 1 liter with Isopropanol. Stand-
ardize with sulfuric acid. Barium chloride
may be used.
3.3.5 Sulfurlo acid standard (0.01 N) —
Purchase or standardize to ±0.0002 N
against 0.01N NaOH which has previously
been standardized' against potassium acid
phthalate (primary standard grade).
4. Procedure.
4.1 Sampling.
4.1.1 Preparation of collection train. Pour
15 ml. of 80% Isopropanol into the midget
bubbler and 15 ml. of 3% hydrogen peroxide
into each of the first two midget implngers.
Leave the final midget impinger dry. Assem-
ble the train as shown in Figure 6-1. Leak
check the sampling train at the sampling
site by plugging the probe inlet and pulling
a 10 Inches Hg vacuum. A leakage rate not
In excess of 1% of the sampling rate is ac-
ceptable. Carefully release the probe inlet
plug and turn off the pump. Place crushed
ice around the implngers. Add more ice dur-
ing the run to keep the temperature of the
gases leaving the last Impinger at 70° F. or
less.
4.1.2 Sample collection. Adjust the sam-
ple flow rate proportional to the stack gas
velocity. Take readings at least every five
minutes and when significant changes in
stack conditions necessitate additional ad-
justments in flow rate. To begin sampling,
position the tip of the probe at the first
sampling point and start the pump. Sam-
ple proportionally throughout the run. At
the conclusion of each run, turn off the
pump and record the final readings. Remove
the probe from the stack and disconnect It
from the train. Drain tlie Ice bath and purge
the remaining part of the train by drawing
clean ambient air through the system for 15
minutes.
4.2 Sample recovery. Disconnect the Im-
plngers after purging. Discard the contents
of the midget bubbler. Pour the contents of
the midget Implngers Into a polyethylene
shipment bottle. Rinse the three midget Im-
plngers and the connecting tubes with dis-
tilled water and add these washings to the
same storage container.
4.3 Sample analysis. Transfer the contents
of the storage container to a 50 ml. volu-
metric flask. Dilute to the mark with de-
ionized, distilled water. Pipette a 10 ml.
aliquot of this solution Into a 125 ml. Erlen-
meyer flask. Add 40 ml. of Isopropanol and
two to four drops of thoriu indicator. Titrate
to a pink endpolnt using 0.01 N barium
perchlorate. Run a blank with each series
of samples.
5. Calibration.
5.1 Use standard methods and equipment
which have been approved by the Adminis-
trator to calibrate the rotameter, pltot tube,
dry gas meter, and probe heater.
5.2 Standardize the barium perchlorate
against 25 ml. of standard sulfuric acid con-
taining 100 ml. of Isopropanol.
6. Calculations.
6.1 Dry gas volume. Correct the sample
volume measured by the dry gas meter to
standard conditions (70° F. and 29.92 inches
Hg) by using equation 6-1.
17.71 ;
°R /VmPb
in. HgV To,
equation 6-1
where:
Vm.,
Volume of gas sample through the
dry gas meter (standard condi-
tions) , cu. ft.
- Vm = Volume of gas sample through the
dry gas meter (meter condi-
tions) , cu. ft.
Tsld= Absolute temperature at standard
conditions, 530* R.
Tm =• Average dry gas meter temperature,
?,,„ = Barometric pressure at the orifice
meter, inches Hg.
P ia=Absolute pressure at standard con-
ditions, 29.92 Inches Hg.
6.2 Sulfur dioxide concentration.
= (7.05X10-^-)
\ g.-ml./
equation 6-2
where:
030.,= Concentration of sulfur dioxide
at standard conditions, dry
basis, Ib./cu. ft.
7.05 X 10-"= Conversion factor, Including the
number of grams per gram
equivalent of sulfur dioxide
(32 g./g.-eq.), 453.6 g./lb., and
1,000 ml./l., Ib.-l./g.-ml.
V,= Volume of barium perchlorate
tltrant used for the sample,
ml.
Vtl = Volume of barium perchlorate
tltrant used for the blank, ml.
W=Normallty of barium perchlorate
tltrant, g.-eq./l. <
v.oin=:Total solution volume of sulfur
dioxide, 50 ml.
V,= Volume of sample aliquot ti-
trated, ml.
V™, 14= Volume of gas sample through
the dry gas meter (standard
conditions), cu. ft., see Equa-
tion 6-1.
7. References.
Atmospheric Emissions from Sulfurlc Acid
Manufacturing Processes, U.S. DHEW, PHS,
Division of Air Pollution, Public Health Serv-
ice Publication No. 999-AP-13, Cincinnati,
Ohio, 1965.
Corbett, P. P., The Determination of SO2
and SOa in Flue Gases, Journal of the Insti-
tute of Fuel, 24:237-243, 1961.
Matty, R. E. and E. K. Diehl, Measuring
Flue-Gas SO., and SO3, Power 101:94-97, No-
vember, 1957. ;
Patton, W. F. and J. A. Brink, Jr., New
Equipment and Techniques for Sampling
Chemical Process Gases, J. Air Pollution Con-
trol Association, 13, 162 (1963).
METHOD 7—DETERMINATION Or NITROGEN OXIDE
EMISSIONS' FROM STATIONABT SOURCES
1. Principle and applicability.
1.1 Principle. A grab sample Is collected
In an evacuated flask containing a dilute
sulfuric acid-hydrogen peroxide absorbing
solution, and the nitrogen oxides, except
I
O
JO
m
O
0
FEDERAL REGISTER, VOL. 35, HO. 1',7- TSIUa^AY, D^CEMQSi! 23, 1971
-------
24892
nitrous oxide, are measure colortmetrically
using the phenoldisulfonlc acid (PDS)
procedure.
1.2 Applicability. This method Is applica-
ble for the measurement of nitrogen oxides
from stationary sources only when specified
by the test procedures for determining com-
pliance with New Source Performance
Standards.
2: -Apparatus.
2.1 Sampling. See Figure 7-1.
2.1.1 Probe—Pyrex1 glass, heated, with
filter to remove particulate matter. Heating
is unnecessary if the probe remains dry dur-
ing the purging period.
2.1.2 Collection flask—Two-liter, Pyrex,1
round bottom with short neck and 24/40
standard taper opening, protected against
implosion or breakage.
1 Trade name.
PROBE
r
riLTER
GROUND-GLASS SOCKET.
§ NO. 12/6
fvV. 2 in.
3-WAY STOPCOCK:
MORE.». PYREX
2-mrn BORE, fi-mm OD
GROUND-GLASS CONE,
STANDARD TAPER. GROUND-GLASS
I SLEEVE NO. 24/40 SOCKET, 5 NO. 1Z/5
S PYREX
RULES AND REGULATIONS
2.1.3 Flask valve—T-bore stopcock con-
nected to a 24/40 standard taper Joint.
2.1.4 Temperature gauge—DlAl-type ther,
mometer, or equivalent, capable of measur-
ing 2" P. Intervals from 25* to 125° F.
2.1.5 Vacuum line—Tubing capable of
withstanding a vacuum of 3 Inches Hg abso-
lute pressure, with "T" connection and T-bore
stopcock, or equivalent.
2.1.6 Pressure gauge—U-tube manometer,
36 Inches, with 0.1-inch divisions, or
equivalent.
2.1.7 Pump—Capable of producing a vac-
uum of 3 inches Hg absolute pressure.
2.1.8 Squeeze bulb—One way.
2.2 Sample recovery.
2.2.1 Pipette or dropper.
2.2.2 Glass storage containers—Cushioned
for shipping. «
SQUEEZE BULI
IMP VALVE
PUMP
8-'/. in.
FOAM ENCASEMENT
,-'^BOILING FLASK -
2-LITER. ROUND-BOTTOM. SHORT NECK,
WITH j SLEEVE NO. 24/40
Figure 7-1. Sampling train, flask valve, and flask.
2.2.3 Gloss wash bottle.
2.3 Analysis.
2.3.1 Steam bath.
2.3.2 Beakers or casseroles—250 ml., one
for each sample and standard (blank).
2.3.3 Volumetric pipettes—1, 2, and 10 ml.
2.3.4 Transfer pipette—10 ml. with 0.1 ml.
divisions.
2.3.5 Volumetric flask—100 ml., one for
each sample, and 1,000 mL for the standard
(blank).
2.3.6 Spectrophotometer—To measure ab-
Eorbance at 420 nm.
2.3.7 Graduated cylinder—100 inl. with
1.0ml. divisions.
2.3.8 Analytical balance—To measure to
0.1 mg.
3. Reagents..
3.1 Sampling.
3.1.1 Absorbing solution—Add 2.8 ml. of
concentrated H2SO4 to 1 liter of distilled
water. Mix well and add 6 ml. of 3 percent
hydrogen peroxide. Prepare a fresh solution
weekly and do not expose to extreme heat or
direct sunlight.
3.2 Sample recovery.
3.2.1 Sodium hydroxide (IN)—Dissolve
40 g. NaOH in distilled water and dilute to 1
liter.
3.2.2 Red litmus paper.
3.2.3 Water—Deionized, distilled.
3.3 Analysis.
3.3.1 Fuming sulfurlc acid—15 to 18% by
weight free sulfur trloxlde.
3.3.2 Phenol—White solid reagent grade.
3.3.3 Sulfuric acid—Concentrated reagent
grade.
3.3.4 Standard solution—Dissolve 0.5495 g.
potassium nitrate (KNO8) In distilled water
and dilute to 1 liter. For the working stand-
ard solution, dilute 10 ml. of the resulting
solution to 100 ml. with distilled water. One
ml. of the working' standard solution Is
equivalent to 25 Ag- nitrogen dioxide.
3.3.5 Water—Deionized, distilled.
3.3.6 Phenoldlsulfonic acid solution—
Dissolve 25 g. of pure white phenol In 150 ml.
concentrated sulfuric acid on a steam bath.
Cool, add 75 ml. fuming sulfuric acid, and
heat at 100° C. for 2 hours. Store in a dark,
stoppered bottle.
4. Procedure.
4.1 Sampling.
4.1.1 Pipette 25 ml. of absorbing solution
Into a sample flask. Insert the flask valve
stopper into the flask with the valve In the
"purge" position. Assemble the sampling
train as shown In Figure 7-1 and place the
probe at the sampling point. Turn the flask
valve and the pump valve to their "evacuate"
positions. Evacuate the flask to at least 3
Inches Hg absolute pressure. Turn the pump
valve to Its "vent" position and turn off the
pump. Check the manometer for any fluctu-
ation In the mercury level. If there is a visi-
ble change over the span of one minute,
check for leaks. Record the Initial volume,
temperature, and barometric pressure. Turn
the flask valve to its "purge" position, and
then do the same with the pump valve.
Purge the probe and the vacuum tube using
the squeeze bulb. If condensation occurs in
the probe and flask valve area, heat the probe
and purge until the condensation disappears.
Then turn the pump valve to Its "vent" posi-
tion. Turn the flask valve to its "sample"
position and allow sample to enter the flask
for about 15 seconds. After collecting the
sample, turn the flask valve to Its "purge"
position and disconnect the flask from the
sampling train. Shake the flask for 5
minutes.
4.2 Sample recovery.
4.2.1 Let the flask set for a minimum of
16 .hours and then shake the contents for 2
minutes. Connect the flask to a mercury
filled U-tube manometer, open the valve
from the flask to the manometer, and record
the flask pressure and temperature along
with the barometric pressure. Transfer the
flask contents to a container for shipment
or to a 250 ml. beaker for analysis. Rinse the
flask with two portions of, distilled water
(approximately 10 ml.) and add rinse water
to the sample. For a blank use 25 ml. of ab-
sorbing solution and the same volume of dis-
tilled water as used In rinsing the flask. Prior
to shipping or analysis, add sodium hydrox-
ide (IN) dropwlse into both the sample and
the blank until alkaline to litmus paper
(about 25 to 35 drops in each).
4.3 Analysis.
4.3.1 If the sample has been shipped In
a container, transfer the contents to a 250
ml. beaker using a small amount of distilled
water. Evaporate the solution to dryness on a
steam bath and then cool. Add 2 ml. phenol-
disulfonlc acid solution to the dried residue
and triturate thoroughly with a glass rod.
Make sure the solution contacts all the resi-
due. Add 1 ml. distilled water and four drops
of concentrated sulfuric acid. Heat the solu-
tion on a steam bath for 3 minutes with oc-
casional stirring. Cool, add 20 ml. distilled
water, mix well by stirring, and add concen-
trated ammonium hydroxide dropwlse with
constant stirring until alkaline to litmus
paper. Transfer the solution to a 100 ml.
volumetric flask and wash the beaker three
times with 4 to 5 ml. portions of distilled
water. Dilute to the mark and mix thor-
oughly. If the sample contains solids, trans-
fer a portion of the solution to a clean, dry
centrifuge tube, and centrifuge, or filter a
portion of the solution. Measure the absorb-
ance of each sample at 420 nm. using the
blank solution as a zero. Dilute the sample
and the blank with a suitable amount of
distilled water If absorbance falls outside the
range of calibration.
5. Calibration.
6.1 Flask volume. Assemble the flask and
flask valve and fill with water to the stop-
cock. Measure the volume of water to ±10
ml. Number and record the volume on the
flask.
5.2 Spectrophotometer. Add 0.0 to 16.0 ml.
of standard solution to a series of beakers. To
each beaker add 25 ml. of absorbing solution
and add sodium hydroxide (IN) dropwlse
until alkaline to litmus paper (about 25 to
35 drops). Follow the analysis procedure of
section 4.3 to collect enough data to draw a
calibration curve of concentration In ng. NOs
per sample versus absorbance.
6. Calculations.
6.1 Sample volume.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
RULES AND REGULATIONS
24893
V.0
P«d
(V'~25 "L> -
where:
V,c = Sample volume at standard condi-
tions (dry basis), tni.
Teld== Absolute temperature at standard
conditions, 530° B. •
PBtJ = Pressure at standard conditions,
29.92 inches Hg.
Vf = Volume of flask and valve, ml.
V, = Volume of absorbing solution, 25 ml.
P,=Final absolute pressure of flask.
Inches Hg.
P, = Initial absolute pressure of flask,
Inches Hg.
T,=Final absolute temperature of flask,
°R.
T, = Initial absolute temperature of flask,
°B.
6.2 Sample concentration. Bead fig. NO,
for each sample from the plot of /tg. NOa
versus absorbance.
where:
C = Concentration of NO^ as NOa (dry
basis), Ib./s.c.f.
m=Mass of NO, in gas sample, ng.
Vsc=Sample volume at. standard condi-
tions (dry basis), ml.
7. References.
Standard Methods of Chemical Analysis.
6th ed. New York, D. Van Nostrand Co., Inc.,
1962, vol. 1, p. 329-330.
Standard Method of Test for Oxides of
Nitrogen In Caseous Combustion Products
(Phenoldisulfonic Add Procedure), In: 1968
Book of ASTM Standards, Part 23, Philadel-
phia, Pa. 1968, ASTM Designation D-1608-60,
p. 725-729.
Jacob, M. B., The Chemical Analysis of Air
Pollutants, New York, N.Y., Interscience Pub-
lishers, Inc., 1960, vol. 10, p. 351-356!
METHOD 8—DETERMINATION OP STJLFDRIC ACID
MIST AND SULFTJB DIOXIDE EMISSIONS FROM
STATIONARY SOURCES
1. Principle and applicability.
1.1 Principle. A gas sample Is extracted
from a sampling point in the stack and the
acid mist Including sulfur trloxlde is sepa-
rated from sulfur dioxide. Both fractions are
measured separately by the barium-thorln
titratlon method.
1.2 Applicability. This method is applica-
ble to determination of sulfuric acid mist
(including sulfur trloxlde) and sulfur diox-
ide from stationary sources only when spe-
cified by the test procedures for determining
equation 7-2
compliance with the New Source Perform-
ance Standards.
2. Apparatus.
2.1 Sampling. See Figure 8—1. Many of
the design specifications of this sampling
train are described in APTD-0581.
2.1.1 Nozzle—Stainless steel (316) with
sharp, tapered leading edge.
2.1.2 Probe—Pyrex1 glass with a heating
system to prevent visible condensation dur-
ing sampling.
2.1.3 Pitot tube—Type S, or equivalent,
attached to probe to monitor stack gas
velocity.
2.1.4 Filter holder—Pyrex * glass.
2.1.5 Impingers—Four as shown In Figure
8-1. The first and third are of the Greenburg-
Smlth design with standard tip. The second
and fourth are of the Greenburg-Smith de-
sign, modified by replacing the standard tip
with a %-lnch ID glass tube extending to
one-half Inch from the bottom of the Im-
pinger flask. Similar collection systems,
which have been approved by the Adminis-
trator, may be used.
2.1.6 Metering system—Vacuum gauge,
leak-free pump, thermometers capable of
measuring temperature to within 5° F., dry
gas meter with 2% accuracy, and related
equipment, or equivalent, as required to
maintain an isoklnetlc sampling rate and
to determine sample volume.
2.1.7 Barometer—To measure atmospheric
pressure to ±0.1 inch Hg.
1 Trade name.
STACK
FILTER HOLDER
PROBE
REVERSE-TYPE
PITOT TUBE
THERMOMETER
CHECK
VALVE
.VACUUM
LINE
VACUUM
GAUGE
IR-TIGHT
PUMP
DRY TEST I
Figure 8-1. Sulfuric acid mist sampling train.
' 2.2 Sample recovery.
2.2.1 Wash bottles—Two.
2.2.2 Graduated cylinders—250 ml., 500
ml.
2.3.3 Glass sample storage containers.
2.2.4 Graduated cylinder—250ml.
2.3 Analysis.
2.3.1 Pipette—25 ml., 100 ml.
2.3 2 Burette—50ml. <
2.3.3 Erlenmeyer flask—250 ml.
2.3.4 Graduated cylinder—100 ml.
2.3.5 Trip balance—300 g. capacity, to
measure to ± 0.05 g.
•2.3.6 Dropping bottle—to add indicator
solution.
3. Reagents.
3.1 Sampling.
3.1.1 Filters—Glass fiber, MSA type 1106
BH, or equivalent, of a suitable size to fit
In the filter holder..
3.1.2 Silica gel—Indicating type, 6-16
mesh, dried at 175° C. (350° F.) for 2 hours.
3.113 Water—Deionized, distilled.
3.1,4 Isopropanol, 80%—Mix 800 ml. of
isopropanol with 200 ml. of deionized, dis-
tilled water.
3.1.5 Hydrogen peroxide, 3%—Dilute 100
ml. of 30% hydrogen peroxide to 1 liter with
deionized, distilled water.
3.1.6 Crushed Ice.
3.2 Sample recovery.
3.2.1 .Water—Deionized, distilled.
3.2.2 Isopropanol, 80%.
3.3 Analysis.
3.3.1 Water—Deionized, distilled.
3.3.2 Isopropanol.
3.3.3 Thorin Indicator—l-(o-arsonophen-
ylazo)-2-naphthol-3, 6-dlsulfonlc acid, dl-
sodiuxn salt (or equivalent). Dissolve 0.20 g.
in 100 ml. distilled water.
3.3.4 Barium perchlorate (0.012V)—Dis-
solve 1.95 g. of barium perchlorate [Ba
(COJ.,-3 H,O] In 200 ml. distilled water and
dilute to 1 liter with Isopropanol. Standardize
with sulfuric acid.
3.3.5 Sulfuric acid standard (0.012V) —
Purchase or standardize to + 0.0002 N against
0.01 N NaOH which has previously been
standardized against primary standard po-
tassium acid phthalate.
4. Procedure.
4.1 Sampling.
4.1.1 After selecting the sampling site and
the minimum number of sampling points,
determine the stack pressure, temperature,
moisture, and range of velocity head.
4.1.2 Preparation of collection train.
Place 100 ml. of 80% Isopropanol in the first
Implnger, 100 ml. of 3% hydrogen peroxide in
both the second and third Impingers, and
about 200 g. of silica gel in the fourth im-
pinger. Betain a portion of the reagents for
use as blank solutions. Assemble the train
without the probe as shown in Figure 8-1
with .the filter between the first and second
Impingers. Leak check the sampling train
at the sampling site by plugging the inlet to
the first Impinger and pulling a 15-inch Hg
vacuum. A leakage rate not in excess of 0.02
cjf.m. at a vacuum of 15 inches Hg is ac-
ceptable. Attach the probe and turn on the
probe heating system. Adjust the probe
heater setting during sampling to prevent
any visible condensation. Place crushed ice
around the implngers. Add more ice during
the run to keep the temperature of the gases
leaving the last Impinger at 70° F. or less.
4.1.3 Train operation. For each run, re-
cord the data required on the example sheet
shown in Figure 8-2. Take readings at each
sampling point at least every 5 minutes and
when significant changes in stack conditions
necessitate additional adjustments in flow
rate. To begin sampling, position the nozzle
at the first traverse point with the tip point-
Ing directly into the gas stream. Start the
• pump and Immediately adjust the flow to
isoklnetlc conditions. Maintain isokinetlc
sampling throughout the sampling period.
Nomographs are available which aid in the
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
E-l
SRL 1281 25 0472
APPENDIX E
LABORATORY REPORT
E.I ON-SITE HANDLING AND TRANSFER, PARTICULATE
After the completion of a test run, the probe and nozzle were
disconnected from the impinger train and all open ends sealed immediately
to avoid contamination. At the laboratory facility, the nozzle was
disconnected from the probe and very carefully washed with acetone,
using a fine bristled brush. All acetone washings were collected in a
clean glass jar, the jar itself being placed on a large piece of clean
aluminum foil. The probe was then washed using a long handled brush
rotated through it under a continuous stream of acetone. The brush
was also carefully cleaned, and all washings collected in the glass
jar. The probe was finally checked visually for any residue.
The impinger train was initially wiped clean on the outside
and all glassware connectors, including the filter, removed carefully
and all exposed surfaces wiped clean. All the connectors were placed
on a piece of aluminum foil ready for washing. The first three impingers
were then analyzed for water collection by transferring the water through
the outlet port into a graduated cylinder and noting the volume. The
impingers were not dismantled and all transfers and washings were
performed through the inlet and outlet ports. All of the glassware in
the back half of the filter, up to the fourth impinger was then carefully
washed with distilled water and the washings collected. This was
followed by an acetone wash which was again collected in a separate jar.
SCOTT RESEARCH LABORATORIES, INC
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E-2
SRL 1281 25 0472
Acetone washings from the glassware in the front half of the
filter were collected in the same jar as the probe and nozzle wash.
The filter was carefully removed from the holder and placed in a
plastic dish which was then sealed with tape. Silica gel in the fourth
impinger was weighed in a previously tared glass jar using a triple-
beam balance.
All acetone jars had aluminum lined lids, or aluminum foil
was used before screwing on the lids. The following designations were
used for labeling the containers:
Container #1: Filter
Container #2: Acetone wash front half from filter
Container #3: Water wash back half from filter
Container #4: Silica gel
Container #5: Acetone wash back half from filter
E.2 LABORATORY HANDLING AND ANALYSIS, PARTICULATE
E.2.1 Filter Transfer
Clean plastic dishes were.desiccated for 24 hours, labeled
and tared on an electronic balance. The filter containers were unsealed
and desiccated for 24 hours before carefully transferring the filters
to the tared dishes using a fine pair of tweezers. Care was taken to
place a piece of aluminum foil under the transfer operation. A
"staticmaster" brush was used to brush any fine particles adhering to
the container or foil. All transfers were performed near the balance
and the weight reported to the nearest 0.1 mg. The plastic dishes were
then sealed for shipment. .
SCOTT RESEARCH LABORATORIES, INC
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E-3
SRL 1281 25 0472
E.2.2 Acetone Washes
The 250 ml. beakers to be used for the acetone wash transfers
were leached for 24 hours in 50% nitric acid, washed thoroughly and oven
dried overnight. These were then desiccated for 24 hours and tared.
Once tared, the beakers were sealed with "parafilm" and handled with
tongs or "Kimwipes".
The jars containing the acetone washes were left loosely
covered in a hood until the acetone was evaporated. Once the acetone
was evaporated, the glass jar was rinsed with acetone, using a rubber
policeman, and the washings collected in the tared beaker. When the
acetone wash of the front half contained considerable particulate
matter, the dried particulate cake was transferred carefully with a
spatula into the tared beaker along with the final acetone rinse.
After the acetone had evaporated, the beakers were desiccated
for 24 hours and weighed to a constant weight. Where water was present
in the acetone wash, it was evaporated in an oven at 90 C after the
acetone had all evaporated.
E.2.3 Water Washes
The level of water in the collection bottles was marked for
later volume measurement. Each water wash was then transferred into
a 2000 ml. separatory funnel and extracted three times with 25 ml.
portions of chloroform. Often, where a large volume of water was
collected (above 500 ml.) a fourth extraction was used. The chloroform
extracts were collected directly in a tared beaker prepared in the same
manner as described in the previous section.
SCOTT RESEARCH LABORATORIES, INC
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E-4
SRL 1281 25 0472
Extraction with three 50 ml. portions of ether followed.
collecting the water portion in the original jars. The ether extracts
were combined with the chloroform extracts. These were then washed
with distilled water in the separatory funnel and returned to the
tared beaker for evaporation.
The water portion was transferred to tared beakers, oven
dried at 90 C, desiccated, and weighed. All beakers were "parafilm"
sealed for shipment. The Project Officer requested that particle size
analysis not be performed. A summary of weight measurements is shown
in Tables E-l and E-2.
E.3 ORSAT ANALYSIS
A total of six integrated bag samples were analyzed by
Orsat during the three day test period. The Tedlar sample bags had a
capacity of about 5 liters and were equipped with Teflon sample tubes
fitted with airtight syringe caps. Prior to sampling, each bag was
flushed with pure, dry nitrogen and sealed with the syringe cap.
At the end of each sampling day two sample bags (one inlet and
one outlet) were returned to the field laboratory where they were
analyzed for CO, C0« and 0^ by Orsat.
Each bag was connected to the Orsat analyzer by carefully
removing the syringe cap and inserting the Teflon tube securely into the
Orsat sample tube. The Orsat analyzer was then purged by squeezing the
Tedlar bag and forcing the sample through the Orsat bypass. Successive
100 ml. samples were drawn into the Orsat sample burette and then passed
SCOTT RESEARCH LABORATORIES, INC
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TABLE E-l
®
1
Run 1
Final Tare Gross Blank Net
PI
C/l
> Container #la 8.1980 7.9490 249.0 - 249.0
% (Filter)
2E
r Container //lb 0.1670 0.1425 24.5 - 24.5
03 (Filter)
so
*t Container 01c - - - -
O (Filter)
90
j» Container )?2a 164.2365 88.8970 55339.5 0.5 55339.0
~ (Acetone wash front half)
P
Container #2b -
(Acetone wash front half)
Container 03a 85.1300 85.1260 4.0 1.0 3.0
(Organic Extract)
Container «b 87.5585 87.5320 26.5 5.5 21.0
(Water after extraction)
Container 05 82.1360 82.0290 107.0 0 107.0
(Acetone wash back half)
Probe, cyclone, filter (mg) 55612.5
Total (mg) 55743.5
TJ-X. J. \J*. rvj-j j.vjj.1 j.
(INLET)
Final Tare
8.0475 7.9875
8.2605 8.2020
8.3600 8.2255
153.0405 88.6855
26.4980 7.4780
88.5230 88.4900
82.3830 82.3450
87.4180 87.4060
Probe, cyclone,
L lunu u tvi^riijiN j. o
Run 2
Gross Blank
(mg) (mg)
60.0
•
58.5
134.5
64354.0 1.0
19020.0 0
33.0 1.0
38.0 5.5
12.0 0
filter (mg)
Total (mg)
Net
(mg)
60.0
58.5
134.5
64353.0
19020.0
32.0
32.5
12.0
83626.0
83702.5
CO
i — •
t-o
Run 3 2
Final Tare Gross Blank Net
8.1905 8.0310 159.5 - 159.5 °
?j
8.2450 8.2025 42.5 - 42.5
134.5280 97.2925 37235.5 0.5 37235.0
82.1495 82.1425 7.0 1.0 6.0 M
Ui
80.8645 80.8910 26.5 4.5 22.0
89.3630 89.3540 9.0 0 9.0
Probe, cyclone, filter (nig) 37437.0
Total (mg) 37474.0
-------
Pi
GO
g
1
n
TABLE E-2 - SUMMARY OF WEIGHT MEASUREMENTS
(OUTLET)
Run 1
Container #1 •
(Filter)
Container #2
(Acetone wash front half)
Container #3a
(Organic Extract)
Container #3b
(Water after extraction)
Container 05
Final Tare Gross Blank Net
(g) (g) (mg) (mg) (mg)
7.9805 7.9407 39.80 .- 39'.80
86.2676 86.2092 58.40 0.14 58.26
86.3675 86.3630 4.50 1.47 3.03
88.9760 88.9620 14.00 5.93 8.07
97.3862 97.3740 12.20 0.07 12.13
Probe, cyclone, filter (mg) 98.06
Total (mg) 121.29
Run 2
Final Tare Gross Blank Net
(g) (g) (mg) (mg) (mg)
7.9885 7.9370 31.50
51.50
82.7500 82.7250 25.00 0.18 24.82
86.8954 86.8910 4.40 1.47 2.93
87.0973 87.0915 5.80 4.10 1.70
89.3688 89.3600 8.80 0.06 8.74
Probe, cyclone, filter (mg) 76.32
Total (mg) 89.69
Run 3 .
CD
Ul
Final Tare Gross Blank Net g
(S) (g) (mg) (mg) (mg) '5
7.7625 7.7325 30.00
30.00
85.3515 85.3040 47.50 0.14 47.36
86.8100 86.8090 1.00 1.47 0.00
84.6882 84.6810 7.20 4.11 3.09
83.5695 83.5606 8.90 0.07 8.83
Probe, cyclone, filter (mg) 77.36
Total (mg) 89.28
-------
E-7
SRL 1281 25 0472
through each of the three absorbing solutions (potassium hydroxide -
CO., alkaline pyrogallate - 0-, and cuprous chloride - CO). Repetitive
passes were made through each absorbing solution until good duplication
of results occurred. At least three 100 ml. samples were analyzed from
each Tedlar sample bag. The data recorded for each Orsat analysis is
included as Table E-3.
E.4 S02 ANALYSIS
A total of six S0« gas samples were taken during the course
of the test program. Following each sampling period the impinger train
was disconnected from the sample probe and purged with ambient air for
fifteen minutes at the same flow rate used during the test. The inlet
and outlet connections of the impinger train were then sealed with
tape to prevent contamination and transported to the field laboratory
for transfer. Upon arrival at the field laboratory, the outside surfaces
of the impinger train were washed with water and then wiped clean to
remove any coal dust that had accumulated during the test. The isopropanol
bubbler was then carefully disconnected from the impinger section of the
train and its contents discarded. The next two impingers were individually
disconnected and the hydrogen peroxide solutions were transferred to
separate polyethelene bottles with distilled water washes. The glass
connecting tubes were then rinsed with distilled water and the washes
added to their respective polyethelene bottles. The final transfer step
involved rinsing the third impinger with distilled water and adding this
wash to.the number two impinger solution. The polyethelene bottles were
tightly capped and labeled for shipment to the laboratory.
SCOTT RESEARCH LABORATORIES. INC
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E-8
SRL 1281 25 0472
Sample
Location
Inlet
Sample
Number
1
Outlet
TABLE E-3 - ORSAT ANALYSIS DATA
Run
Component
co2
°2
CO
°2
CO
°2
CO
CO,
°2
CO
°2
CO
°2
CO
- February 29, 1972
Analysis
Number
1
2
1
2
3
1
2
1
2
1
2
3
1
2
1
2
1
2
3
1
1
2
1
2
3
. 1
2
1
2
1
2
3
1
2
1
2
1
2
3
1
2
Burette Volume
Initial
100.0
99.1
79.7
100.0
99.1
79.1
100.0
99.1
79.5
100.0
99.1
80.0
100.0
99.0
79.8
100.0
99.0
79.8
Final
99.1
99.1
80.1
79.7
79.7
79.7
79.7
99.1
99.1
79.7
79.1
79.1
79.1
79.1
99.1
99.1
81.1
79.5
79.5
79.5
79.5
99.1
99.1
80.1
80.0
80.0
80.0
80.0
99.0
99.0
80.2
79.8
79.8
79.8
79.8
99.0
99.0
80.3
79.8
79.8
79.8
79.8
(ml.)
Difference
0.9
0.9
19.0
19.4
19.4
0.0
0.0
0.9
0.9
19.4
20.0
20.0
0.0
0.0
0.9
0.9
18.0
19.6
19.6
0.0
0.0
0.9
0.9
19.0
19.1
19.1
0.0
0.0
1.0
1.0
18.8
19.2
19.2
0.0
0.0
1.0
1.0
18.7
19.2
19.2
0.0
0.0
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SRL 1281 25 0472
E-9
TABLE E-3 - ORSAT ANALYSIS DATA
(continued)
Run #2 - March 1, 1972
Sample Sample Analysis
Location Number Component Number
Inlet 1 C00 1
2 2
0 1
Z 2
3
4
CO 1
2
2 CO 1
2
3
0-> 1
2
Z 2
3
CO 1
2
3 CO. 1
2
0 1
Z 2
3
CO 1
2
Outlet 1 C00 1
2 2
0- 1
2
3
CO 1
2
2 C00 1
2
2
3
4
0 1
2
3
4
CO 1
2
Burette
Volume
Initial Final
100.0
99.1
80.6
100.0
99.0
80.2
100.0
99.1
80.5
100.0
99.5
79.8
100.0
99.1
79.3
99.1
99.1
81.6
80.8
80.6
80.6
80.6
80.6
99.1
99.0
99.0
81.0
80.2
80.2
80.2
80.2
99.1
99.1
80.8
80.5
80.5
80.5
80.5
99.5
99.5
80.0
79.8
79.8
79.8
79.8
99.5
99.2
99.1
99.1
80.0
79.8
79.3
79.3
79.3
79.3
(ml.)
Difference
0.9
0.9
17.5
18.3
18.5
18.5
0.0
0.0
0.9
1.0
1.0
18.0
18.8
18.8
0.0
0.0
0.9
0.9
18.3
18.6
18.6
0.0
0.0
0.5
0.5
19.5
19.7
19.7
0.0
0.0
0.5
0.8
0.9
0.9
19.1
19.3
19.8
19.8
0.0
0.0
SCOTT RESEARCH LABORATORIES. INC
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E-10
SRL 1281 25 OA72
TABLE E-3 - ORSAT ANALYSIS DATA
Run #2 - March 1, 1972
(continued)
Burette Volume (ml.)
Sample Sample Analysis
Location Number Component Number "initial Final Difference
Outlet
CO,
CO
1
2
1
2
3
1
2
100.0
99.2
79.6
99,
99,
79.8
79.6
79,
79
,2
,2
,6
.6
79.6
0.8
0.8
19.4
19.6
19.6
0.0
0.0
SCOTT RESEARCH LABORATORIES, INC
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E-ll
SRL 1281 25 0472
TABLE E-3 - ORSAT ANALYSIS DATA
Run #3 - 'March 2, 1972
Sample Sample
Location Number Component
Inlet 1 C00
2
0-
9
^
CO
2 CO.
2
0-
9
£>
CO
3 C02
°2
CO
Outlet 1 C00
2
°2
CO
2 C09
°2
CO
3 CO-
°2
CO
Analysis
Number
1
2
1
2
3
4
1
2
1
2
1
2
3
1
2
1
2
1
2
3
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
Burette Volume
Initial
100.0
99.0
79.9
100.0
99.0
80.1
100.0
99.0
80.0
100.0
99.8
79.2
100.0
99.9
79.4
100.0
99.9
79.3
Final
99.0
99.0
80.5
80.3
79.9
79.9
79.9
79.9
99.0
99.0
80.8
80.1
80.1
80.1
80.1
99.0
99.0
80.2
80.0
80.0
80.0
80.0
99.8
99.8
79.2
79.2
79.2
79.2
99.9
99.9
79.4
79.4
79.4
79.4
99.9
99.9
79.3
79.3
79.3
79.3
(ml.)
Difference
1.0
1.0
18.5
18.7
19.1
19.1
0.0
0.0
1.0
. 1.0
18.2
18.9
18.9
0.0
0.0
1.0
1.0
18.8
19.0
19.0
0.0
0.0
0.2
0.2
20.6
20.6
0.0
0.0
0.1
0.1
20.5
20.5
0.0
0.0
0.1
0.1
20.6
20.6
0.0
0.0
SCOTT RESEARCH LABORATORIES. INC.
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E-12
SRL 1281 25 0472
All S02 samples were analyzed by the Barium-Thorin Titration
procedure. Each sample was transferred to either a 50 or 100 ml. volumetric
flask with distilled water washes and then diluted to volume. A suitable
aliquot of either 5 or 10 ml. was chosen and then pipeted to a 250 ml.
Erlenmeyer flask. Isopropanol was then added to each sample in 4 to 1
proportions (isopropanol to sample aliquot) by volume. The titration
was performed in the presence of four drops of Thorin indicator with a
previously standardized solution of 0.0111 N barium perchlorate. A
solution blank was titrated with each set of samples analyzed. Each sample
was titrated twice or until good duplication of results was obtained.
Table E-4 lists all titration data recorded. The titer volumes for each
impinger sample pair were then summed and the normality of the sample
solution was computed by the following formula:
Ns= —
s
where:
V = Volume of titer (ml.)
NT = Normality of titer (0.0111)
V = Volume of sample aliquot (ml.)
• ' "
From this information the milligrams of SO- per sample were calculated
using the formula:
mg SO- = Vd x N x meq. wt. SO-
where:
V, = Sample dilution volume (ml.)
N = Normality of sample solution
S
meq. wt. SO™ = 32
The mg SO- for each sample were then converted to ppm as shown in
Appendix B.
SCOTT RESEARCH LABORATORIES. INC
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SRL 1281 25 0472
E-13
TABLE E-4 -
S02 ANALYSIS DATA
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Impinger
Number
1
2
1
2
Dilution
Vol. (ml.)
Run #1 •
50
50
50
50
1
2
Run #2
50
50
100
100
Run #3
100
100
100
100
Sample
Analysis Aliq.
Number (ml.)
February 29
1
2
1
2
1
2
1
2
- March 1,
1
2
1
2
1
2
3
1
2
3
- March 2,
1
2
1
2
1
2
3
1
2
, 1972
10
10
10
10
10
10
10
10
1972
5
5
5
5
10
10
10
10
10
10
1972
10
10
10
10
10
10
10
10
10
Volume
Titer
(ml.)
0.90 •<
0.90
0.00
0.00 >
0.025
0.025
0.025
0.025
29.80 ^
29 . 94
38.70
39.00 >
39.30 ^
39.52
39.59
47.75
48.05
48.10.,
3.20^
3.22
4.20
4. 20 J
2.50'
2,44
2.44
3.48
3.51
9.99 x 10
n _, ._
°'56 X 10
10
-1
0.97 x 10
-2
,-2
0.66 x 10
-2
SCOTT RESEARCH LABORATORIES, INC
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E-14
SRL 1281 25 0472
E.5 NO ANALYSIS
X
Immediately after each NO flask sample was taken, the flask
X
containing the absorbing solution and the gas sample was shaken for five
minutes. The flask was then allowed to sit until the following morning
when it was shaken again for two minutes. Following this final shake, the
flask pressure was measured with a mercury manometer. Each flask was
then carefully wiped off and the stopcocks removed. The absorbing
solutions were then transferred to glass shipping bottles with two 10 ml.
washes of distilled water. Just prior to shipping, the samples were
neutralized with 1.0 N sodium hydroxide (approximately 40 drops). At
this time solution blanks were made for each set of samples. The blanks
contained 25 ml. of NO absorbing solution and 20 ml. of distilled water
X
and were neutralized with 1.0 N sodium hydroxide. At the end of the
test period all samples were transported to the laboratory for analysis.
All NO samples were analyzed by the Phenoldisulfonic acid
X
procedure. Prior to analysis, a calibration curve was established for a
suitable range of NO concentrations. From a standard potassium nitrate
X
solution with an equivalent concentration of 25 yg NO,, per ml. four
aliquots of 4, 8, 12 and 16 ml. were added to respective 250 ml. beakers.
Twenty-five ml. of NO absorbing solution was added to each of these
X
beakers and the analysis procedure described below was followed. These
solutions were read against a blank containing no standard solution and
a calibration curve of % absorbance versus yg N0~ was plotted.
SCOTT RESEARCH LABORATORIES. INC
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E-15
SRL 1281 25 0472
Upon arrival at the laboratory, each sample was transferred
to a 250 ml. beaker and evaporated to dryness on a steam bath. After
cooling, 2 ml. of phenoldisulfonic acid was added and each sample was
triturated thoroughly with a glass stirring rod. One ml. of distilled
water and four drops of concentrated sulfuric acid were added and the
samples were returned to the steam bath for three minutes. The samples
were then cooled and 20 ml. of distilled water was added. Concentrated
ammonium hydroxide was then added dropwise until each sample was alkaline
to litmus paper. The samples were transferred to 100 ml. volumetric
flasks with distilled water and portions of each solution were read at
420 mp on a Bausch and Lomb Spectronic 20 Colorimeter. The solution
blanks run with each set of samples were used for the colorimeter zero
reference. The absorbances read for each sample were then converted
to tag N00 via the previously established calibration curve. NO con-
£. X
centrations were calculated as ppm NO- following the procedure described
in Appendix B. Table E-5 lists all the absorbance data for NOX.
SCOTT RESEARCH LABORATORIES, INC
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E-16
SRL 1281 25 0472
TABLE E-5 - NO ANALYSIS DATA
x
Run Sample Sample Absorbance NOX Cone.
No. Date Location Port @ 420 my (yg NOJ
1 Feb. 29 Inlet A 0.298 222.5
A 0.296 221.0
B 0.288 215.0
Outlet A 0.231 172.5
. A 0.228 172.0
B 0.241 177.6
2 Mar. 1 Inlet A 0.310 231.0
A 0.320 238.0
B 0.258 192.5
Outlet Mid 0.280 208.0
Mid 0.143 107.5
Mid 0.249 186.0
3 Mar. 2 Inlet A 0.340 254.3
A 0.356 266.3
B 0.382 285.7
Outlet Mid 0.304 227.4
Mid 0.264 197.4
Mid 0.179 133.9
SCOTT RESEARCH UBORATORIES, INC
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F-l
SRL 1281 25 0472
APPENDIX F
TEST LOG
On Monday, February 28, 1972, the Scott team arrived at the
Bishop plant of Consolidation Coal Company in Bishop, West Virginia,
and began to set up the test equipment. The special testing platforms
which were required had been erected by Consolidation Coal Co. and
were in place.
Both particulate train control panels were set up in the
same area. This area was next to the inlet sample location. The
outlet sample location was approximately 30 feet above this area.
Once the equipment had been put in place, preliminary velocity
and temperature traverses were performed at both test locations. It was
discovered that the pump in the outlet control system was leaking. This
was corrected by substituting another pump which was satisfactory.
The equipment was then returned to the motel and prepared for the first
test. All of the glassware was set up in the sampling boxes before
going to the test site. An eight foot probe was used at both locations
for the particulate sample.
On Tuesday, February 29, 1972, the team arrived at the plant
and set the equipment in place for the test.
The particulate sample trains were started at 1140. Figure F-l,
"Summary of Test Program", shows the times that the various samples were
taken. The inlet sample probe was located at 36 different traverse
points for four minutes each. The outlet sample probe was located at
SCOTT RESEARCH LABORATORIES, INC
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F-2
SRL 1281 25 0472
48 traverse points for three minutes each. At 1200 the pitot tube in
the inlet stack became plugged with dirt and moisture. It was cleaned
and the test continued at 1205. Again at 1220 the pitot tube became
clogged and improper AP's were observed. The test was stopped and a new
umbilical line was attached. The pitot tube was cleaned and the test
was resumed at 1243. At 1320 the test was stopped and the probe was
moved from one port to the other. The filter in the inlet sample train
was also changed because the vacuum was becoming excessively high. The
test was resumed at 1346 and ran until 1505.
The Orsat sample system was set up at the inlet location and
was started at 1142. It was stopped from 1205 until 1218 and then ran
until 1255. The system was transferred to the outlet location and a
sample was collected from 1352 until 1452.
The S0_ sampling apparatus was set up at the inlet location
and a sample was collected from 1147 to 1230 except for the period from
1205 to 1218. The system was then moved to the outlet location and a
sample collected from 1356 to 1430. Grab NO samples were collected
X
from the inlet location at 1145, 1235, and 1410. NO samples were
collected from the outlet location at 1157, 1355, and 1434. All testing
was completed by 1505.
The sample boxes were removed and returned to the motel where
the particulate samples were transferred to sample bottles and the system
prepared for the next test. While cleaning the glassware it was observed
that the probe used at the inlet location was broken. Thus, a 10 foot
probe was prepared for the test the next day. The break did not have an
SCOTT RESEARCH LABORATORIES. INC.
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FIGURE F-l - SUMMARY OF TEST PROGRAM
Run #1 - February 29, 1972
SC
53
PJ
SO
O
BO
O
90
§
50
S
O
1140
o
Change
Filter
Changs
Ports
1205
1230
1255
1320
1345
1410
1435
25
50
75
100
125
150
175
Change
Ports
1500
200
2
00
I—*
K:
**
C
*•
•>J
K:
NO
Oraat
Particulates
1525 Time
—I
u>
225 Time
Klapsed
: (min.)
Particuiates
Orsat
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F-4
SRL 1281 25 0472
adverse effect on the first test as evidenced by the heating tape on the
outside of the probe not having been broken; and further, it is suspected
that the probe may have been broken during removal from the test site
following the test. It was also observed that a very slight amount of
particulate matter managed to get past the filter in both trains. It
was found that the filters were just a fraction too small. This was
corrected on later tests by using larger filters.
The Orsat samples were analyzed and the SO- samples were
transferred to sample bottles. The NO samples were transferred to
sample bottles the next morning.
On Wednesday, March 1, 1972, the team arrived at the plant
and set up the equipment for the second test. At this point it was
necessary to install additional scaffolding at the outlet location in
order that Research Cottrell personnel could perform tests simultaneously
with the Scott team.
The particulate test trains were started at 1156. Although the
pitot tube at the inlet location periodically became plugged with dirt
and moisture, the problem was easily corrected by blowing out the line
with an air supply which Consolidation Coal Co. provided.
SCOTT RESEARCH LABORATORIES. INC.
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FIGURE F-2 - SUMMARY OF TEST PROGRAM
©
8
30
PI
cn
Pi
30
O
X
E -
| i
I
z
r>
1156
0
.u
01
i-H
4J
O
Kun ffz - marcn i, ly/z OT
. „ so °°
to
O
• • • • XO --J
x to
Change
Chanse 4 . Filter Change
Filter " " Change Filtcr
Ports
1221 1246 1311 1336 1401 1426 1451 1516 1541 Time
. | • . I . I , j MJ
25 50 75 ICC 125 150 175 200 225 Time <-"
Elaosed
(nin.)
Change D ^ . 1
* *" * ". * Forts
NO
SO,,
-------
33
PI
U>
PI
§
FIGURE F-3 - SUMMARY OF TEST PROGRAM
Run #3 - March 2, 1972
CO
N3
00
O
NJ
3 5
M *""*
2
1011
0
Change
Filter
Change
Ports
1036 1101 1126 1151 1216 1241 1306 1331 1356 Time.
1 * . f 1 - 1 ' ! ! ... '
t 1 ! I i < J - , - - <
25 50 75 100 125 150 175 200 2^5 Time
Elapsed
* Ports " "* "r^ ^ul^tl-j
O
NO
-------
F-7
SRL 1281 25 0472
The inlet filter became heavily loaded with material so the
test was stopped at 1238 and the filter changed. The test .resumed at
1300 but had to be stopped at 1305 because the pump in the inlet system
apparently had been over taxed and stopped. The pump was dismantled
and the problem corrected. The test resumed at 1324 and ran until 1337.
The inlet pitot tube was cleaned and the test resumed at 1340 and run
until 1356 when it was stopped in order to change the sample probe from
one port to the other. The inlet filter was also changed at this time.
The test was resumed at 1415 and ran until 1451. , It was stopped at this
point in order to change the inlet filter which had become heavily loaded.
The test resumed at 1456 and ran until 1532 when the test was completed.
The times that the other samples were collected are summarized
in Figure F-2, "Summary of Test Program". An inlet Orsat sample was
collected from 1156 to 1256. An outlet Orsat sample was collected from
1421 to 1522. The inlet SO™ sample was collected from 1205 to 1236.
The outlet SO- sample was collected from 1431 to 1503. The inlet NO
£. ••""'* X •
samples were collected at 1159, 1240 and 1449 while the outlet NO
X
samples were collected at 1215, 1425, and 1509.
All sampling was completed by 1532. The sampling trains were
dismantled and returned to the motel for clean up and sample transfer.
All sample transfers and clean up operations were performed
as described for the first run. The entire system was prepared for the
test the next day.
The Scott team arrived at the test site on Thursday, March 2,
1972, and assembled the equipment for the third run. Leak tests were
performed on both the inlet and outlet trains and were found to be
SCOTT RESEARCH LABORATORIES. INC
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F-8
SRL 1281 25 0472
satisfactory. The particulate tests were started at 1011. The sample
continued until 1123 when it was stopped in order to change ports. In
addition, the filter was changed in the inlet sampling train because
of the high loading. When the leak test was performed a leak rate was
discovered. Although the leak test was acceptable it appears the slight
leak was due to the introduction of the new filter which was in a
different filter holder.
The particulate test was resumed in the other port at 1203
and ran until 1315. The other sampling times are summarized and
shown in Figure 3.
The inlet SO- sample was collected from 1036 to 1108 while the
outlet S02 sample was collected from 1204 to 1236. The inlet Orsat
sample was taken from 1030 to 1130 and the outlet Orsat sample was
taken from 1157 to 1257. The inlet N0x samples were taken at 1031, 1111,
and 1219. The outlet NO samples were taken at 1045, 1159, and 1253.
X
All testing was completed by 1315.
The sampling trains were removed and the remaining equipment
was disassembled and removed from the test site. The samples were
taken back to the motel where the sampling clean up procedures described
earlier were followed.
SCOTT RESEARCH LABORATORIES. INC
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G-l
SRL 1281 25 0472
APPENDIX G
PROJECT PARTICIPANTS AND TITLES
The personnel taking part in the project include:
Thomas Ward
Charles Sedman
Norman Troxel
Joseph Wilson
Nosh Mistry
Jyotin Sachdev
William Blakeslee
William Scott
Duane Gulick
Zenophon Tomaras
Margaret Husic
Louis Reckner
Project Officer - EPA
Project Engineer - EPA
Senior Engineer - SRL
Field Team Leader - SRL
Field Team Leader - SRL
Engineer - SRL
Chemist - SRL
Technician - SRL
Technician - SRL
Chemist - SRL
Technician - SRL
Manager, Atmospheric Chemistry and
Industrial Emissions Department - SRL
SCOTT RESEARCH LABORATORIES. INC
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