COAL PREPARATION PLANT EMISSION TESTS
TEST NO. 1281-35
WESTMORELAND COAL COMPANY
WENTZ PLANT
Stonega, Virginia
PREPARED FOR
ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park
North Carolina 27711
Contract No 68-02-0233
SCOTT RESEARCH LABORATORIES, INC.
PLUMSTEADVILLE, PENNSYLVANIA 18949
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SRL 1281 35 0472
Test No. 1281-35
Westmoreland Coal Company
Wentz Plant
Stonega, Virginia, Norman R. Troxel
SCOTT RESEARCH LABORATORIES, INC.
Plumsteadville, Pennsylvania 18949
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SRL 1281 35 0472
TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1-1
2.0 SUMMARY OF RESULTS 2-1
3.0 PROCESS DESCRIPTION 3-1
4.0 LOCATION OF SAMPLE POINTS 4-1
5.0 PROCESS OPERATION 5-1
6.0 SAMPLING AND ANALTYICAL PROCEDURES 6-1
6.1 PARTICULATE SAMPLING AND ANALYTICAL PROCEDURES 6-1
6.2 GASEOUS SAMPLING PROCEDURES 6-1
6.3 NO SAMPLING AND ANALYTICAL PROCEDURES 6-2
x
6.4 ORSAT SAMPLING AND ANALYTICAL PROCEDURES 6-3
6.5 TOTAL HYDROCARBON SAMPLING AND ANALYSIS PROCEDURES 6-3
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-2
E.2 LABORATORY HANDLING AND ANALYSIS, PARTICULATE E-3
E.3 NO ANALYSIS E-7
x
E.4 ORSAT ANALYSIS E-8
E.5 TOTAL HYDROCARBON ANALYSIS E-10
APPENDIX F TEST LOG F-l
APPENDIX G PROJECT PARTICIPANTS AND TITLES G-l
SCOTT RESEARCH LABORATORIES, INC
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SRL 1281 35 0472
1.0 INTRODUCTION
Scott Research Laboratories, Inc. performed source sampling
tests at the Wentz Plant of Westmoreland Coal Company during the week
of March 20, 1972. This plant is located in Stonega, Virginia. The
plant uses a Research Cottrell venturi scrubber to control the exhaust
gas emissions from a coal cleaning and preparation operation.
The exhaust gases, as they were being emitted to the atmos-
phere, were sampled and analyzed for the determination of total
particulate loading, oxides of nitrogen, total hydrocarbons, carbon
monoxide, carbon dioxide, and oxygen concentrations.
There are two types of coal processed at the plant, Osaka
coal and Wentz coal. The Osaka coal is a low sulfur, medium ash,
high volatile steam coal of 55 grindability index, while the Wentz
coal is a low sulfur, low ash, high volatile metallurgical coal of 55
grindability index. One sample run with Osaka coal being processed
was performed on March 20, 1972, and two other runs were conducted on
March 22, 1972. Two sample runs were performed with the Wentz coal
being processed on March 23, 1972. Figure 1 shows the location of the
sampling point at the plant.
SCOTT RESEARCH LABORATORIES, INC.
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SRL 1281 35 0472
WESTMORELAND COAL Cg.
STONEQA, VIRGINIA
BLOWER
LLEVATION
FIGUKK 1 - SAMPLE POINT LOCATION
.«. MIST
ELIMINATOR
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SRL 1281 35 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 during the three runs while Osaka coal was being processed
averaged approximately 40 percent more than what was collected during
the two runs performed while Wentz coal was being processed. This is
also shown in Table 1 where the particulate emission rate to the atmosphere
was approximately 50% higher for Osaka coal compared to Wentz coal.
A visible trail of brownish smoke was observed from the stack
during the processing of Osaka coal. It was difficult to compare this
occurrence with the visible emissions during processing of Wentz coal,
since it was snowing the day of the tests. However, there did appear
to also be somewhat of a brownish trail.
The NO concentrations were fairly consistent for all of the
x
tests. The total hydrocarbon concentrations, however, varied considerably.
They ranged from 18 ppm to 208 ppm.
SCOTT RESEARCH LABORATORIES, INC
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TABLE 1 - SUMMARY OF TEST RESULTS
OJ
g
§
SO
S
Run Number
Type of Coal
Sample Date
Sample Gas Vol., scf.
Moisture, %
Stack Gas Temp., °F
Stack Gas Vel., fpm.
Stack Gas Vol., SCFM
Partlculate Collected
Probe, cyclone, filter, mg.
Total, mg.
Particulate Concentration
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, %
Total Hydrocarbon (ppm-C)
NO , ppm
A.
1
Osaka
3/20/72
88.56
12.61
120
5165
137,310
261.5
337.0
0.046
0.059
53.54
68.96
87.89
0.0
0.2
18.2
208.2
52.8
2
Osaka
3/22/72
86.95
13.61
120
4961
128,520
206.5
280.5
0.037
0.050
40.31
54.74
92.19
0.0
0.3
19.6
102.0
54.4
3
Osaka
3/22/72
86.09
12.56
120
4847
127,100
242.0
314.0
0.043
0.056
47.16
61.22
92.30
0.0
0.2
19.4
48.0
37.6
4
Wentz
3/23/72
95.90
11.93
120
5120
135,450
169.5
220.5
0.027
0.035
31.57
41.09
96.48
0.0
0.3
19.8
31.5
59.6
5
Wentz
3/23/72
94.51
9.37
120
4998
136,070
173.0
225.0
0.028
0.037
32.88
42.80
94.65
0.0
0.4
19.8
18.0
44.6
CO
f
to
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o
to
NJ
I
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2-3
SRL 1281 35 0472
TABLE 2 - PARTICULATE WEIGHTS SUMMARY
Run Number 1 2 3 4 5
Container 1, mg. 92.0 101.5 94.0 64.0 78.0
Container 2, mg. 169.5 105.0 148.0 105.5 95.0
Container 3a, mg. 5.0 9.0 8.0 9.0 8.0
Container 3b, mg. 61.0 54.0 5.5 32.5 30.5
Container 5, mg. 9.5 11.0 13.5 9.5 13.5
Probe, cyclone filter, mg. 261.5 206.5 242.0 169.5 173.0
Total, mg. 337.0 280.5 314.0 220.5 225.0
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SRL 1281 35 0472
3.0 PROCESS DESCRIPTION
i
At the Wentz plant the coal from the mines is screened,
washed and then dried. The exhaust from the drier passes through a
Research Cottrell venturi scrubber before it is emitted to the
atmosphere. Figure 2 shows a flow diagram of the Wentz plant.
SCOTT RESEARCH LABORATORIES, INC
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o
s
n
i
Bd
O
»
25
2
StAM :
FIGURE 2 COAL FLOW IN WENTZ CLEANING PLANT
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SRL 1281 35 0472
4.0 LOCATION OF SAMPLE POINTS
The exhaust gases from the coal cleaning operation pass through
a Research Cottrell venturi scrubber to a mist eliminator and then are
emitted to the atmosphere through an 81 inch diameter stack. Two
sampling ports located at 90° apart were in the stack at a point
approximately 10 feet upstream from the top of the stack and approximately
25 feet downstream from the outlet of the mist eliminator.
There had been a platform installed at the sample point location
for some previous test work. An angle iron support rail extending ten
feet out from each port was used to hold the sample box. The sample
control unit was located in the same area. Figure 1 shows the physical
layout of the system and the location of the sample ports.
Figure 3 shows the traverse points used. A total of 48 traverse
points were sampled two and one half minutes each. 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 samples for five minutes each. The
traverse points were chosen in accordance with Method 1 published in
the Federal Register, Volume 36, No. 24.
The two ports were designated as A and B, with A being the
port on the left and B the port 90° to the right of A.
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SRL 1281 35 0472
WESTMORELAND COAL CO.
STONEGA, VIRGINIA
FIGURE 3 TRAVERSE POINT LOCATIONS
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SRL 1281 35 0472
5.0 PROCESS OPERATION
During the test all filter cake from flotation cells was fed
to the dryer. Measured loadout of rail cars indicated that the plant
production during our tests was 300 TPH, of which 200 TPH had been
thermally dried.
Process variables monitored during the tes.t were the furnace
combustion zone temperature. These were recorded as follows:
Dryer Temperature
Combustion Zone Exhaust Temperature
Date
3/22
3/22
3/23
3/23
Test No.
2
3
4
5
Hi
1300
1250
1200
1200
Lo
1100
1100
900
700
Avg.
1150
1150
1100
1050
Hi
180
180
150
155
Lo
155
170
140
140
Avg,
170
175
145
145
Process operating data was not obtained during the first test
on March 20, 1972.
SCOTT RESEARCH UBORATORIES. INC
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SRL 1281 35 0472
6.0 SAMPLING AND ANALYTICAL PROCEDURES
6.1 PARTICIPATE SAMPLING AND ANALYTICAL PROCEDURES
Samples were collected for the determination of particulate matter
from the outlet of the venturi scrubber. The sampling and analytical pro-
cedures 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. In addition, the
impinger catch was analyzed. This method is attached as Appendix D.
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 was 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.
6.2 GASEOUS SAMPLING PROCEDURES
Stack gas samples were taken at regular intervals during each
particulate sampling traverse to determine the concentrations of 0«,
SCOTT RESEARCH LABORATORIES. INC
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SRL 1281 35 0472
CO, C09, NO and total hydrocarbons present in the stack effluent. The
Z- X
sampling location was the same with respect to the venturi scrubber as
that 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".
6.3 NO SAMPLING AND ANALYTICAL PROCEDURES
x
All NO samples were taken through a ^ inch O.D. glass probe
x
heated to approximately 250 F. Each sample was drawn through this probe
into a previously evacuated 2 liter flask containing 25 ml. of NO
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
and the results were reported as parts per million N0_.
SCOTT RESEARCH LABORATORIES, INC
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6-3
SRL 1281 35 0472
6.4 ORSAT SAMPLING AND ANALYTICAL PROCEDURES
Integrated bag 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 flowmeter 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 rate
to approximately 80 cc per mintue, and inserting the hypodermic needle
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, C0~, and 0 . Repetitive analyses were performed on
each bag to insure satisfactory duplication. The results were reported
in percentages.
6.5 TOTAL HYDROCARBON SAMPLING AND ANALYSIS PROCEDURES
The same integrated bag sample that was taken for Orsat analysis
was analyzed for total hydrocarbons via a Beckman Model 108-A Total Hydro-
carbon Analyzer. Following each Orsat analysis the Tedlar sample bag was
connected to the hydrocarbon analyzer via a Teflon sample tube. The
sample was drawn into the instrument until a stable reading was recorded
on the meter. Before and after each analysis the instrument was zeroed
with hydrocarbon free air (<0.1 ppm-C) and spanned with a Scott close
SCOTT RESEARCH LABORATORIES, INC
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6-4
SRL 1281 35 0472
tolerance blend of 99.9 ppm propane in nitrogen (analysis: ±2.0%). The
meter readings for each sample were converted to ppm-C as shown in
Section E-5 of Appendix E.
SCOTT RESEARCH LABORATORIES, INC.
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A-l
SRL 1281 35 0472
APPENDIX A
COMPLETE PARTICULATE RESULTS WITH EXAMPLE CALCULATIONS
SCOTT RESEARCH LABORATORIES, INC
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A-2
• OF
SOURCE TESTING CALCULATION FORMS
Test. No.
No. Runs
Name of Firm
CM/..
Location of Plant
Type of Plant £-«P al
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7.77 ;
* 70°F, 29.92" Hg.
-------
A-3
ITVTC
' '
P.un I.'o. ...
/:M - % Krnst'jrc i-: IV? stack g<.s by volume
"M, - Mole fraction of dry gas
AC02 ( W r\ f d s f. i\
2 I ffss-) )
. -- . v i/ „
A N • / • \
* N2 -( *"j) .. ' •
M W . - Molecular weigiit. of dry steel: gas
. .
M W - Molecular weight of stack gas
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C. • - Parties: tLte, total ,-$r7'cf
. L-.U r, ,- .-. -. ... 1. ~r r ,.;
C.M - Pn rti f'U • atcT1 pvoo.';'. cyclone'^
-c" and filter, lo/hr.
C - Particulate - total > Ib/hr.
3X •
% EA - % Excess air &
samp 'ring point
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-------
1;
A-5
'ARTICULATE CALCULAT'JOi'.'S
Volume of dry ges sampled c.t standard conditions - 70°F, 29.92'''-
lig, ft. 3
17.7 X V /Pp •:• P]
"" K -ire-/
2% Volunie of water- vapor at 70°F & 29.92" lig, Ft.
« 0.0474 X
= Ft.3
3. % moisture -in stack gas
mstd wgas
4. Mole fraction of dry gas
100
5. Average molecular v/eight of dry stack gas
x
-------
A-6
- K W , X H . . is [I
7. Stack velocity P stack conditions.
v « 4350 xA T+
o)/,
I 1/2-
= fprn r
8.
Stack gas volume @ standard conditions, SCFM
0.123 X Vc X A, X Mj X P
+ 460)
S = SCFM
= . '/.3-73I.O
9. Per cent isokinetic
1032 X (T -i- 460) X V
YsXTtXPs XMdX -(Dj2
81. B
10. Panticulate - probe, cyclone, & filter, gr/SCF
Can = 0.0154 x;/ = gr/SCF
Vstd
x «?6/,
=- o.o
-------
A-7
';]. Pcirticin<'.li: tola], gr/'SCF
C --- 0.0154 X 7>--=.gr/SCF
3O m '
-. mst
-------
16. % c-ixcurj5.. sir ..re
:v; point
TOO X %
•-= %.
0.266 X
-------
B-l
SRL 1281 35 0472
APPENDIX B
COMPLETE GASEOUS RESULTS WITH EXAMPLE CALCULATIONS
SCOTT RESEARCH LABORATORIES, INC
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B-2
SRL 1281 35 0472
ORSAT ANALYSIS DATA SHEET
Run Analysis % % %
No. Date Number CO C00 00
-- ---.--. .-I---, . -^— ' Z ~~~~"Z"~~
1 3/20/72 1 0.0 0.2 18.2
2 0.0 0.2 18.1
3 0.0 0.2 18.2
Avg. 0.0 0.2 18.2
2 3/22/72 1
2
3
Avg.
3 3/22/72 1
2
3
Avg.
4 3/23/72 1
2
3
Avg.
5 3/23/72 1
2
3
Avg. 0.0 0.4 19.8
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
0.3
0.2
0.3
0.3
0.2
0.2
0.3
0.2
0.3
0.4
0.3
0.3
0.4
0.4
0.5
19.6
19.7
19.6
19.6
19.4
19.4
19.5
19.4
19.8
19.7
19.8
19.8
19.8
19.8
19.8
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B-3
SRL 1281 35 0472
TOTAL HYDROCARBON DATA
Run
No.
1
2
3
4
5
Date
3/20/72
3/22/72
3/22/72
3/24/72
3/23/72
Sample
No.
1
2
1
2
1
2
1
2
1
2
Range
100
100
100
100
100
100
100
100
100
100
Meter
Units
69.5
69.5
35.0
33.0
16.0
16.0
10.5
10.5
5.0
7.0
THC*
(ppm-C3HQ)
69.4
69.4
35.0
33.0
16.0
16.0
10.5
10.5
5.0
7.0
THC
(ppm-C)
208.2
208.2
105.0
99.0
48.0
48.0
31.5
31.5
15.0
21.0
* All spans were set at full scale on Range 100 using a 99.9
ppm C_HQ standard.
Sample calculation:
Run #1, Sample #1:
n ti meter units x 99.9 ppm-C0Hn
Ppm-C2Hg = 3-8
nraB
ppm-
(69.5H99.9)
-
38
ppm-C-H_ =69.4
J o
ppm-C = ppm-C_HQ x 3
J O
ppm-C = 208.2
SCOTT RESEARCH LABORATORIES. INC
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B-4
NO, MISSION CAM
Run io.
.Date -
ing K0?
T. - Fle.s!; Ten.pGraturc?, °F
Vf - Flr.sk Vclu:.ie, liters
P- - Initial Fliisk VACUUM, "Kj.
Pf- Final Flask Vacuum, "Hg.
ppni NC^
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29.63 x mg !!02 X (Tf * 460)
Vf X (P. - Pf)
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-------
B-5
i-;ox EMISSION'
"
Run io.
.Oats
°
Tf - Flo.?.!; Ter,i|>e>r£ture, F
Vf - Flask VcU;:ne, liters
P.. - Initial H^s'; Vocuu;:!, "Kj.
Pf- Final Flask Vacuum, "Hg.
ppm i.'Cp'
'"
ppm
29.63 x mg NO 2 X (Tf + 460)
Vf X
- P)
-------
r;fX.B~fcssjc:; DATA
Run io.
.Date
mg N0?
T,r - Flo?.!; Tempora lure, °F
Vf - Flask VcUi.-.ie, liters
P -. - I n i ti a 1 Fl as k V';; ci:u;n , !1 K j .
Pf- Final Flask Vacuum, "Hg.
ppni UCj
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-------
C-l
SRL 1281 35 0472
APPENDIX C
FIELD DATA
SCOTT RESEARCH LABORATORIES, INC
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-i I
-?
<—
ant
**< _
Location
Operator
Date,
Run No.
Sampl-e Box No.
Meter Box No.
er AHg
Fact9i»
Ambient; Temperature
Barometric Pressure
Assumed Moisture, %
Setting _
™3MM&...
Schematic Of Stack Cross Section
1,
ter, In. _
Setting _
t6$0
Traverse Point
Number
Sampling
Time
(6) min.
Static .« 0
Pressure"!,
'
"
'97
,'
,/
Avg.
-------
Plant
Location
Operator
Date
Run -No.
Sample Box Ho
Meter Box No.
Meter AHg
C Factor
Ambient Temperature
W - ~"
Barometric Pressure _
Assumed Moisture, X _
Heater Box Setting
Probe Length, m. _, ._
Nozzle Diameter, la.
Probe Heater Setting
of Stack Cross Section
-------
Plant - ^
' Location *
Operator
Date
Run No. / ' ^
Sample Box No. -
i
Traverse Point
Number
/t-Z
•\
;-i
z~~"
*
-.,
k
(. •**
• /a
^Tptal - ,.,.
Meter Box
Meter AHg
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' Location
Operator
Date
Run No.
Sample Box No.
Meter Box No.
Meter AHg
C Factor
Ambient Temperature
Barometric Pressure
Assumed Moisture, %
Heater Box Setting
Probe Length, m.,
Nozzle Dianeter,4ln.
Probe Heater Setting
Schematic of Stack Cross Section
Traverse Point
Number
Sampling
Tine
(0) min.
Static
Pressure
(Pfl) In. Hg.
Stack
Temperature
Velocity
Head
Pressure t
Differential
ross
rifice
Meter
(AH)
In. H20
Gas Sample
Volume.
(Vm) ftj
Temperature
DryGas Meter
/ Inlet.
Outlet
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out
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Temperature
'• Temperature
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C-6
7
WATER VOLUME
Run No
. /
Date
Bubbler *
Silica Gel No. 61 Wgt. g. t> ' ^> c 3>
n I b
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Gross
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Gross T,Jgt.(-)
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34.7
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cc
Fom R&D 109
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i
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Meter *Hg /.,
C Factor A
Ambient Temperature
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Operator
Date **
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Location
Operator
Date
Run No.
Sample Box No.
Meter Box Mo.
Heter AHg
C Factor
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Ambient Temperature _
Barometric Pressure
Assumed Moisture, %
Heater Box Setting
Probe Length, m.
Nozzle Diameter, In.
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Number
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In. H20
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Volume.
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Plant
Location
Operator
Date
Run Ho.
1. &
Sample Box No.
Meter Box No.
Meter AHg
C Factor
Ambient Temperature
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C-ll
WATER VOLUME
Run No.
Date
Bubbler /'
Silica Gel No.
Bubbler
Gross
VJater Added (-)
Net
(A)
cc
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Net
(B)
f.
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r-
Fom R&D 109
-------
Plant _
"Location
Operator
Date
IT ~!
O
Run No.
Sample Box No.
Meter Box No.
Meter AH0
g
1',
Ambient Temperature
Barometric Pressure.
Assumed Moisture, % /
Heater Box Setting
•
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O
Traverse Point
Number
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Time
(9) min.
Static
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°
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Head
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Across
Orifice
Miter
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In. *20
, C
Gas Sample
Volume.
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Gas Sample Temperature
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°
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Temperature
Temperature
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Plant .,
Location
Operator
Date
Run No. ^
Sample Box No.
Meter Box No.
Meter AHg
C Factor
Ambient Temperature _
Barometric Pressure _
Assumed Moisture, % _
Heater Box Setting
Probe Length, m.
Nozzle Diameter, In.
Protre Heater Setting
Schematic of Stack Cross Section
Traverse Point
Number
Sampling
Time
(6) rain.
Static
Pressure
(Ps) In. Hg.
Stack
Temperature
(T8) 5F
Velocity
Head ijg.
Pressure
Differential
Across
Orifice
Meter
(AH)
In.
H20
Gas Sample
Volume.
(Vm) ftj
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at Dry 'Ggg Hetet
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Plant
Location
Operator
Date
Run No.
•,*, :
Sample Box No.
Meter Box No.
Meter AHg
C Factor
Ambient Temperature _
.i. Barometric Pressure
•« * —
Assumed Moisture, % _
Heater Box Setting _J_
Probe Length, m.
Nozzle Diameter, In.
Setting
Schematic of Stack Cross Section
Traverse Point
Number
Sampling
Time
(9) min.
Static
Pressure
(P=) In. Hg.
Stack '
Temperature
(Ts) °F%
Velocity
Head
Pressure
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Across
Orifice
Meter
(AH)
In. H20
Gae Saople
Volume.
(Vn) ftj
Gas Sample Temperature
at Dry G s Meter
Inle
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Sample Box
Temperature
Temperature
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-------
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V
Plant
Location
Operator
Date
Run No.
Sample Box^No.
Meter Box No.
Meter AHg
C Factor
Ambient Temperature
Barometric Pressure _
Assumed Moisture, % _
Heater Box Setting
Probe Length, m.
Nozzle Diameter, In.
Probe Heater Setting
Schematic of Stack Cross Section
Traverse Point
Number
Sampling
Time
(6) min.
Static
Pressure
(P8) In. Hg.
Stack
Temperature
(T8) 6F
Velocity
Head
(AP8)
Pressure
Differential
Across
Orifice
Meter
(AH)
In.
H20
Gas Sample
Volume.
(Vm) ftj
Gas Sample Temperature
at Dry G s Meter
Inlet
Outlet
Sample Box
Temperature
°
. V
Temperature
Leaving
Condenser or
Last Implnger
a
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14-
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60
71
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77
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57
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-------
C-16
WATER VOLUTtE
Run No.
Date
Bubbler /(
H/vC
Silica Gel No. Wftt. g
Bubbler il
Gross
Water Added(-)
Gross TJgt.(-) <. /S>. g
Net
(A)
cc
Net
(B)
Net
(A)
Net (+)
(B)
Total Water
cc
Fom R&D 109
-------
Ambient Temperature
Barometric Pressure
Assumed Moisture, Z
Heater Box Setting _.
Probe Length, m
Istratinn
Operatbr
Date
Sample Box No
Meter Box No,
Mater AHg
CF
Nozzle Diameter, In.
Probe Heater Setting
Schematic of Stack Cross Section
Pressure
Differential
Temperature
Leaving
Condenser or
^Orifice
Meter
(AH)
Gas Sample Temperature
at Dry Gas -Meter
Velocity
Head
'
Last Jmpinger
-------
Plant
Location
Operator
Date
Run No.
Sample Box No.
Meter Box No.
Meter AHg
C Factor
Ambient Temperature
Barometric Pressure
Assumed Moisture, %
Heater Box Setting
Probe Length, m.
Nozzle Diameter, In.
Probe Heater Setting
Schematic of Stack Cross Section
Traverse Point
Number
Sampling
Time
(6) min.
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Pressure
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Plant
Location
Operator
Date
Run No. ff / C?
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Traverse Point
Number
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Plant
Location
-?,
Operator
Date
Run No. • /«i
Sample Box No. .
Traverse Point
Number
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1
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t
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C-21
WATER VOLUT1E
Run No.
Date
Bubbler $1 &. B
)?3 g
Silica Gel No. ft Wgt. e.
Bubbler g»"
Gross
Water Added (-)
Net if?
(A)
cc
Gross
Net
(B)
- /
Net
(A)
Net (+)
(B)
Total Water
cc
Fom R&D 109
-------
Plant
Location t
Operator
Date
Run No.
Sample Box No.
Meter Box No.
Meter AH
g
C Factor
~->
Ambient Temperature
Barometric Pressure
•Assumed Moisture, %
Heater Box Setting _
Probe Length, m.
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Plant
Location
Operator
Date
Run No.
Sample Box No.
Meter Box No.
Meter AH,
C Fac
tor
'g
*''
Ambient Temperature _
Barometric Pressure _
Assumed Moisture,.% _
Heater Box Setting
Probe Length, m.
Nozzle Diameter, In.
' t
Probe Heater Setting
Schematic of Stack Cross Section
Traverse Point
Number
Sampling
time
(6) min.
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Pressure
(Ps) In. Hg.
Stack
temperature
Velocity
Hea
-------
Plant
Ambient Temperature
Barometric Pressure
Assumed Moisture, Z
Heater Box Setting
Probe Length, m
Sample Box No.
Meter Box No.
MeterAHg
C Falter
Nozzle Diameter, In.
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AcrSfs
Orific^t
Meter ||
Temperature
Leaving
Condenser or
Gas Sample Temperature
at Dry G a Meter
Sampling-
Time
(6) min.
Static
Presence
In. Hg
Sample Box
Temperature
Traverse Point
Number
Last Impinger
-------
;•'. ' 11ilC?"~
"••t ::^g:;?fe''--v
•-^- "•.'•:.;.;,. >"-irf|£ "A.V
Plant
Location
Operator
Date
Run No. .
Sample Box No.
Meter Box No.
Meter AHg
C Factor
Temperature •-,"'.':
Barometric Pressure j.
Moisture, Z
Beater Box Setting
Probe Length, m. _^____
Noazle Diameter, "In. .
Probe Heater Setting
-
Schematic of Stack Cross Section
Traverse Point
Number
Sampling
Time
(6) min,
Static
Pressure
Stack
Temperature
(T.) 5P
Veloci
Head
Pressure
Differential
- . Across
Orifice
Meter
> ;••<*»>
in,
Gas Sample
Gas Sample Temperature
at Dry G s Meter
• Sample Box
rature
Temperature ,
t Leaving
CSindenser or
-------
c-26
WATER VOLUME
Run No. 6
Date
Bubbler *1 3. O 3.
Silica Gel No. 3 Wfct. g. ^> /^ 6>"
i?3
Bubbler g
Gross
Water Added (-)
Gross Wgt.(-)
Net
(A)
cc
Net
(B)
Net (+)
(B)
. I
Total Water
A 06.9
cc
< (e
Fom R&D 109
-------
C-27
LABORATORY TEST SHEET
LABORATORY
4NO-GEN- I I IB
-------
C-28
LABORATORY TEST SHEET
LABORATORY
4NO-GEN-I I 28
TEST ENGINEER
TEST EQUIPMENT
1
i
V 2-
C
OBSERVERS
2SL
1SPJ
6
0.2-
Q.3
0-3
M
-« TT
Wc
is.©
HC,
6.0
<*•
•*
.• ..;!,..
''""''
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*
-------
D-l
SRL 1281 35 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,
December 23, 1971. These methods are as follows: Methods 1, 2, 3, 4, 5,
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, hi 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 dally.
(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 add mist
and SO, concentrations shall be deter-
mined by using Method 8 and traversing
according to Method 1. The mtnimn^n
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 Ibi/hr. by the acid produced. The
emission rate shall be determined by
the equation, lb./hr.=QsXc, where
Qa=volumetric flow rate of the effluent
in ft.'/hr. at standard conditions, dry
basis as determined In accordance with
paragraph (c)(2) of this section, and
c=acld mist and SO, concentrations in
Ib./ft.' as determined in accordance with
paragraph (c)(l) of this section, cor-
rected to standard conditions, dry basis.
APPENDIX—TEST METHODS
METHOD 1—OUIFZJI AND VELOCITY TRAVERSES
1OB STATIONARY SOURCES
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.
1.3 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 ^^nyiing 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)
0.5
FROM POINT OF ANY TYPE OF
DISTURBANCE [BEND. EXPANSION, CONTRACTION. ETC.)
equivalent diameter=2i
/(length) (width) \
\ length+width /
equation 1-1
NUMBER OF DUCT DIAMETERS DOWNSTREAM*
(DISTANCE B)
FlfluraM. Minimum number of traverse points.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
Tabla 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 stac'k divided Into 12 equal
areas, showing location of traverse points at centroid of each area.
O
..-—-.-
0
o
1
i
o .[ 9
i
_.. i
r > i
i
O | " O
, r- — --^
I
O | O
1
0
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
13.8
23.6
29.6
33.2
61.8
70.4
76.4
81.2
85.4
89.1
92.5
95.6
93.6
20
1.3
3.9
6.7
9,7
12.9
16.6
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
98.7
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
83.4
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
i
SO
m
O
|
O
z
v>
No. 247—Pt. H
FEDERAL REGISTER, VOL. 36, NO. 347—THURSDAY, DECEMBER 23, 1971
-------
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 centroid of each equal
area according to Figure 1-3.
3. References.
Determining Dust Concentration In a Gas
Stream, ASME Performance Test Code #27,
New Tort, N.Y.. 1957.
Devorkln, 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
Particulate 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 PLOW RATE (TYPE
B PITOT 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
(Steuschelbe or reverse type) pitot 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 Pitot 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 pitot 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 Pitot 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.
4. Calibration.
4.1 To calibrate the pitot tube, measure
the velocity head at some point in a flowing
gas stream with both a Type 8 pitot 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.
equation 2-1
where :
CP ,,,„,= Pi tot tube coefficient of Type S
pitot tube.
Cp,,d=Pltot tube coefficient of standard
type pitot tube (if unknown, use
0.99) .
Apsttd=Absolute pressure at standard conditions, 29.98
Inches Hg.
FEDERAL REGISTER, VOL 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
RULES AND REGULATIONS
24885
6. References.
Mark, L. S., Mechanical Engineers' Hand-
book, McGraw-Hill Book Co., Inc., New York,
N.Y., 1951.
Perry, J. H., Chemical Engineers' Hand-
book, McGraw-Hill Book Co., Inc., New York,
N.T., 1960.
Shigehara, R. .T., W. P. Todd, and W. S.
Smith, Significance of Errors in Stack Sam-
pling 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
Particulate 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.
PLANT.
DATE
RUN NO.
STACK DIAMETER, in.
BAROMETRIC PRESSURE, in. Hg.
STATIC PRESSURE IN STACK (Pg), in. Hg.
OPERATORS
SCHEMATIC OF STACK
CROSS SECTION
Traverse point
number
Velocity head,
in. H20
Stack Temperature
AVERAGE:
Figyra 2-2. Velocity traverse data.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
24886
RULES AND REGULATIONS
METHOD 3 GAS ANALYSIS FOB CARBON DIOXIDE,
EXCESS AIB, AND DRY MOLECULAE WEIGHT
1. Principle and applicability.
1.1 Principle. An Integrated or grab gas
sample Is extracted from a sampling point
and analyzed for Its components using an
Great 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 steel 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.
i Trade name.
2.2 Integrated sample (Figure 5-2).
2.2.1 Probe—Stainless steel or Pyrex1
glass, equipped with a filter to remove par-
ticulate matter.
222 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 Bate 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 Pltot 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.
PROBE
FLEXIBLE TUBING
TO ANALYZER
[ FUTE/HG
(GLASS WOOL)
SQUEEZE BULB
Figure 3-1. Grab-sampling train.
RATE I
[ WOBE
RIGID CONTAINER"
, Figure 3-2. Integrated gas • sampling train.
3. Procedure.
3.1 Grab sampling.
8.1.1 Set up the equipment as shown In
Figure 8-1, making sure all connections are
leak-free. Place the probe In the stack 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 CO2, O2, and CO con-
centrations as soon as possible. Make as many
passes as are necessary to give constant read-
ings. If more than ten parses 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 For 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,.
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 =
(%02)-0.5(%CQ)
0.264(% N2) - (% Oa) +0.5(% CO)
equation 3-1
where:
%EA=Percent excess air.
%O2=Percent oxygen by volume, dry basis.
%Na=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. Use Equation
3-2 to calculate dry molecular weight and
average the runs. Report the result to tha
nearest tenth.
Ma=0.44(%CO.)+0.32(%02)
+ 0.28(%NS+%CO)
equation 3-2
where:
M*=3Dry molecular weight, Ib./lb-mole.
%CO*=Percent carbon dioxide by volume,
•dry basis.
%Os=Percent oxygen by volume, dry
basis.
%NiHPercent nitrogen by volume, dry
basis.
0.44=Molecular weight of carbon dioxide
divided by 100.
0.32=Molecular weight of oxygen divided
by 100.
0-28=Molecular weight of nitrogen and
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 OF MOISTURE
IN STACK GASES
I. 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 sxich 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.
and equipped with a filter to remove partlcu-
late matter.
2.2 Impingers—Two midget impingers,
each with 30 ml. capacity, or equivalent.
2.3 Ice bath container—To condense
moisture In Impingers.
• 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 8, 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 Im-
pinger 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.
Vwo =
(Vf-Vi)pH2oRTatd
ml.
equation 4-1
where:
Vwc=Volume of water vapor collected
(standard conditions), cu. ft.
Vt=Final volume of impinger contents,
ml.
Vi=Initial volume of Impinger con-
tents, ml.
R=Ideal gas constant, 21.83 Inches
Hg—cu. ft./lb. mole-°R.
pn'2o=:Density of water, 1 g./ml.
Tstd=Absolute temperature at standard
conditions, 530° R.
Pstd=Absolute pressure at standard con-
ditions, 29.92 Inches Hg.
MHOO=Molecular weight of water, 18 lb./
Ib.-mole.
HEATED PROB1
FILTER'(GLASS WOOL)
ROTAMETER
PUMP
DRY GAS METER
ICE BATH
Figure 4-1. Moisture-sampling train.
LOCATION.
TEST
COMMENTS
DATE
OPERATOR
BAROMETRIC PRESSURE
CLOCK TIME
GAS VOLUME THROUGH
METER, (Vm),
ft3
ROTAMETER SETTING
ft3/min
METER TEMPERATURE,
•r
V)
90
m
O
i
Figure 4-2. Field moisture determination.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
1x5
*»
oo
23
-------
24888
RULES AND REGULATIONS
4.2 Gas volume.
1771 CR
'•"in. HgV. Tm equation 4-2
•where:
Vine =Dry gas volume through meter at
standard conditions, cu. ft.
Vm =Dry gas volume measured by meter,
co. ft
Fm = Barometric pressure at the dry gas
meter, Inches Hg.
Pit«;=Pressure at standard conditions, 29.93
Inches Hg.
T.t«=Absolute temperature at standard
conditions, 530* R.
Tm —Absolute temperature at meter ( *F+
460), *R.
4.3 Moisture content.
-+8.,,,=
+ (0.025)
V^+Vm.
equation 4-3
where:
Bwo=Proportion by volume of water vapor
In the gas stream, dlmenslonless.
, Vw« = 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
;.: leaving the impingers, 0.025.
6. References.
Air Pollution Engineering Manual, Daniel-
eon. J. A. (ed.), UJS. DHEW, PHS, National
Center for Air Pollution Control, Cincinnati,
Ohio, PHS Publication No. 999-AP-40, 1967.
Devorkln, 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 Oases,
Western Precipitation Division of Joy Manu-
facturing Co., Los Angeles, Calif., Bulletin
WP-60, 1068.
METHOD E—DETERMINATION OF FABTICTTLATE
EMISSIONS FBOM STATIONAET SOURCES
1. Principle and applicability.
1.1 Principle. Partlculate matter Is with-
drawn Isoklnetioally from the source and Its
•weight Is determined gravimetrically after re-
moval of uncomlblned water.
12 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 partlculate sampling train used
by KPA (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° F., 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 &, or equivalent,
attached to probe to monitor stack gas
velocity.
3.1.4 Filter Holder— Pyrex » glass with
heating system capable of maintaining mini-
mum temperature of 225' F.
2.1.6 Implngers / Condenser — Pour Impln-
gers connected In series with glass ball joint
fittings. The first, third, and fourth Impln-
gers are of the Oreenburg-Smlth 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 Up. A condenser may be
used In place of the Implngers 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 isoklnetic 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 Olass wash bottles—Two.
2.2.3 Olass sample storage containers.
2.2.4 Graduated cylinder—250 ml.
2.3 Analysis.
2.3.1 Olass 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, tx>
measure to ±0.05 g.
3. Reagents.
3.1 Sampling.
3.1.1 Filters—Glass fiber, MSA 1106 BH*.
or equivalent, numbered for Identification
and prewelghed.
3.1.2 Silica gel—Indicating type, 6-16
mesh, dried at 175° C. (350* F.) for 2 hours.
3.1.3 Water.
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
PROBE
REVERSE-TYPE
PITOT TUBE
HEATED AREA FILTER HOLDER / THERMOMETER CHECK
..VALVE
..VACUUM
LINE
PITOT MANOMETER
ORIFICE
THERMOHETI
IMPINGERS ICE BATH
BY-PASS,VALVE
VACUUM
GAUGE
MAIN VALVE
DRY TEST METER
AIR-TIGHT
PUMP
Figure 5-1. partlculate-sampling train.
3.3.2 Desiccant—Drlerlte,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 o'f 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
Implngers, leave the third implnger empty,
and place approximately 200 g. of prewelghed
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 Drlerlte1 at 70° F.±10° F.
more ice during the run to keep the temper-
ature of the gases leaving the last Implnger
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 isokinetlc conditions. Sample for at
least 5 minutes at each traverse point; sam-
pling time must be the same for each point.
Maintain isoklnetic 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 oft 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
24889
RUN NO
SAMPLE KK Nq_
METER'BOX K0._
HETERtHj
CFACIOB
AMBIENT TEUPERA7URE_
Tm= Average dry gas meter temperature,
ASSUMED MOI$TME.*_
HUTES BOX S£TTINO_
ffiOBE LENGTH.*
NOZZLE aAMETO, !«._
PROBE Hf ATER SETT1NG_
SCHEMATIC OF STACK CROSS SECTION
TRAVERSE POINT
NUU8QI
TOTAL
SAMPLING
TIME
lel.ria.
AVERAGE
STATIC
PRESSURE
[Psl. ta. Mj.
STACK
TEUPEUTUC
(TS'-*f
vEiocm
HEAD
I»PS>.
PHESSUKE
DIFFERENTIAL
ACROSS
ORIFICE
METER '
I«HJ.
la-HjO
GAS SAMPLE
VOLUME
(Vml. It3
GAS SAMPLE TEMPERATURE
AT DOT GAS UETtR
INLET
IT" ».!•*'
Avg.
OUTLET
"" ««"••'
AX.
Avg.
SAMPLE KM
TEMPERATURE.
"F
TE»PER»niRE
OF GAS
LEAVING
CONDENSER OR
LAST WPfflGER.
•t
Figure 5-2. Parlici
4.2 Sample recovery. Exercise care in mov-
ing the collection train from the test site to
the sample recovery area to minimize the
loss of collected sample or the gain of
extraneous paniculate 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 participate
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 Impinger 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 participate 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 6-2).
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 5-1.
/
-V fT.tJ\(
""-M^WV
"+13.6 1
__ I =
equation 5-1
where:
Vm>td= 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.
TlU = Absolute temperature at standard
conditions, 530° R.
AH
Barometric pressure at the orifice
meter. Inches Hg.
Average pressure drop across the
orifice meter, Inches H=O.
13.6= Specific gravity of mercury.
P.,4= Absolute pressure at standard con-
ditions, 29.92 Inches Hg.
6.3 Volume of water vapor.
).0474
cu. :
equation 5-2
where:
Vvr.ld= 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.
pay) = Density of water, 1 g./mL
Maao=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.
P. td=Absolute pressure at standard con-
ditions, 29.92 inches Hg.
6.4 Moisture content.
„ *w»td
equation 5—3
where:
Bwo =Proportion by volume of water vapor in the £as
stream, dtmensionlcss.
^•«id=Volume of water in the gas sample (standard
conditions), cu. ft.
VmBtd = Volume of gas sample through the dry gas mot cr
(standard conditions) , cu. ft.
6.5 Total partlculate weight. Determine
the total participate catch from the sum of
the weights on the analysis data sheet
(Figure 5-3).
6.6 Concentration.
6.6.1 Concentration In gr./s.c.f .
c'.= 0.0154
-^ n
ing./ \
equation 5-4
where:
0",= Concentration of participate matter In stack
gas. gr./s.o,f., dry basis.
M0 = Total amount of paniculate matter collected,
mg.
Vm.i
-------
24890
RULES AND REGULATIONS
PLANT.
DATE_
RUN NO.
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICULATE COLLECTED.
mg
FINAL 'WEIGHT
x
TARE WEIGHT
:^^
WEIGHT GAIN
FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME.
ml
SILICA GEL
WEIGHT.
9
9»| ml
CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
INCREASE BY DENSITY OF WATER. (1 g ml):
= VOLUME WATER, ml
Figure5-3. Analytical data.
6.6.2 Concentration In lb./cu. ft.
Ci = V453i600mg^==2205><10_6M!,
Vm«td *mstd
equation 5-5
where:
-------
necessary only If a sample traverse la re-
quired, or It stack gas velocity varies with
time.
2.2 Sample recovery.
2.2.1 Glass wash bottles—Two.
2.2.2 Polyethylene storage bottles—To
store Implnger samples.
2.3 Analysis.
PROBE (END PACKED
WITH QUARTZ OR
PYREX WOOL]
TVPESP1TOT
STACK WALL
MIDGET BUBBLER MIDGET IMPINGERS
GLASS WOOL
SILICA GEL DRYING TUBE
TOEJWOHETER
'UMP
DRY GAS METER BOTAMETER
Figure 6-1. SOj sampling train.
2.3.1 Pipettes—Transfer type, 5 ml. and
10 ml. sizes (0.1 ml. divisions) and 25 ml.
size (0.2 ml. divisions).
2.3.2 Volumetric flasks—50 ml., 100 ml.,
and 1,000ml.
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—Delonlzed, distilled.
8.1.2 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—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-disulfonlc acid, dlso-
dium 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(ClO4)a.3H3O] In 200 ml. distilled water
No. 247—Pt. II 3
and dilute to 1 liter with isopropanol. Stand-
ardize with sulfurlc acid. Barium chloride
may be used.
3.3.5 Sulfurlc 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% isopropanpl 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 Implnger at 70° P. 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 the 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 1m-
pingers after purging. Discard the contents
of the midget bubbler. Pour the contents of
the midget Impingers into a polyethylene
shipment bottle. Rinse the three midget Im-
pingers 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 thorln 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, pilot tube,
dry gas meter, and probe heater.
5.2 Standardize the barium perchlorate
against 25 ml. of standard sulfurie 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° P. and 29.92 Inches
Hg) by using equation 6-1.
_ /T.td\ /Pb.,
-
1
vmp
in. Hg\ T
..\
/
equation 6-1
where:
Vmlltd= Volume of gas sample through the
dry gas meter (standard condi-
tions) , cu. ft.
• Vra= Volume of gas sample through the
dry gas meter (meter condi-
tions) , cu. ft.
Tata = Absolute temperature at standard
conditions, 530' R.
Tm= Average dry gas meter temperature,
°R.
Pbmr= Barometric pressure at the orifice
meter, Inches Hg.
P,ta= Absolute pressure at standard con-
ditions, 29.92 Inches Hg.
6.2 Sulfur dioxide concentration.
eoj
(7.05X10-'— \-
V g.-ml.
where:
Cso3= 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
titrant used for the sample,
ml.
Vtb = Volume of barium perchlorate
titrant used for the blank, ml.
W=Normality of barium perchlorate
titrant, g.-eq./l. ,
Vaoln = Total solution volume of sulfur
dioxide, 50 ml.
V, = Volume of sample aliquot ti-
trated, ml,
Vmltd= Volume of gas sample through
the dry gas meter (standard
conditions), cu. ft., see Equa-
tion 6-1.
c.
m
to
O
O
I
equation- 6-2 ij
Z
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. F., The Determination of SO2
and SO, in Flue Gases, Journal of the Insti-
tute of Fuel, 24:237-243, 1961.
Matty, R. E. and E. K. Dlehl, Measuring
Flue-Gas SO2 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 OP NITROGEN OXIDE
EMISSIONS FROM STATIONARY SOURCES
1. Principle and applicability.
1.1 Principle. A grab sample la collected
In an evacuated flask containing a dilute
sulfurlc acid-hydrogen peroxide absorbing
solution, and the nitrogen oxides, except 10
FEDERAL REGISTER, VOL. 35, HO. 257- 7i;:j5;OAY, DKEiV.DIil 23, 1971
-------
24892
nitrous oxide, are measure colorlmetrtcally
using the phenoldlsulfonlc acid (PDS)
procedure.
1.2 Applicability. This method IB applica-
ble for the measurement of nitrogen oxides
from stationary sources only when specified
by the test procedures for determining com-.
pllance 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.
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—Dial-type ther,
mometer, or equivalent, capable of measur-
ing 2° F. Intervals from 28" 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—TJ-tube manometer,
36 Inches, with 0.1-lnch divisions, or
equivalent.
2.1.7 Pump—Capable of producing a vac-
uum of 3 Inches Hg absolute pressure.
3.1.8 Squeeze bulb—Oneway.
2.2 Sample recovery.
2.2.1 Pipette or dropper.
2.2.2 Glass storage containers—Cushioned
for shipping. «
- SQUEEZE BULI
PROBE
- FLASK VALVI
FILTER
GROUND-GLASS
§ NO. 12/5
8-WAY STOPCOCKr
T-BORE. I. PYREX.
2-irmBORE, 8-mmOO
FLASK
.FLASK SHIEltX. .\
GROUND"
STANDARD TAPER,
3 SLEEVE NO. 24/40
GROUND-GLASS
SOCKET, S NO. K/6
PYREX
0AM ENCASEMENT
•BOILING FLASK •
2- LITER. ROUND-BOTTOM. SHOOT MECX.
WITH { SLEEVE NO. 24/40
Figure 7-1. Sampling train, flask valve, and llask.
2.2.3 Glass wash bottle.
2.3 Analysis.
2.3.1 Steam bath.
2.3.2 Beakers or casseroles—260 ml., one
for each sample and standard (blank).
2.8.3 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 ml. with
1.0 ml. divisions.
2.3.8 Analytical balance—To measure to
0.1 mg.
3. Seagents..
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 (12V)—Dissolve
40 g. NaOH in distilled water and dilute to 1
liter.
3.2.2 Red litmus paper.
3.2.3 Water—Delonlzed, distilled.
3.3 Analysis.
3.3.1 Fuming sulfuric acid—15 to 18% by
weight free sulfur trloxide.
3.3.2 Phenol—White solid reagent grade.
3.3.3 Sulfuric acid—Concentrated reagent
grade.
3.3.4 Standard solution—Dissolve 0.6495 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 IB
equivalent to 25 /ig. nitrogen dioxide.
3.3.5 Water—Delonlzed, distilled.
3.3.6 Phenoldlsulfonlc 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 nask 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 4 distilled water
(approximately 10 ml.) and add rinse water
to the sample. For a blank use 26 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) drop-wise 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-
dlsulfonlc 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 drbpwlse 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 6 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.
5.1 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.
6.2 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 pg. NOa
per sample versus absorbance.
6. Calculations.
6.1 Sample volume.
FEDERAL REGISTER, VOl. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
RULES AND REGULATIONS
24893
where:
V,c=Sample volume at standard condi-
tions (dry basis), ml.
Tala= Absolute temperature at standard
conditions, 530° R.
P,tJ — Pressure at standard conditions,
29.92 Inches Hg.
Vf = Volume of flask and valve, ml.
Va = Volume of absorbing solution, 25 ml.
Pt—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,
°R.
6.2 Sample concentration. Read /ig. NO2
for each sample from the plot of ng. NOa
versus absorbance.
Ci
= I ^7—
1.6X10'^
ml./
where:
C = Concentration of NOX as NOa (dry
basis), Ib./s.c.f.
m=Masf of NO2 In gas sample, /ig.
Vac = 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
(Phenoldlsulfonlo 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 OF SULFTTRIC 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 trloxide (s sepa-
rated from sulfur dioxide. Both fractions are
measured separately by the barlum-thorln
tltration method.
1.2 Applicability. This method Is applica-
ble to determination of sulfuric acid mist
(Including sulfur trloxide) 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 Pltot tube—Type 8, or equivalent,
attached to probe to monitor stack gas
velocity.
2.1.4 Filter holder—Pyrex1 glass.
2.1.5 Implngers—Four as shown in Figure
8-1. The first and third are of the Greenburg-
Smith design with standard tip. The second
and fourth are of the Greenburg-Smlth de-
sign, modified by replacing the standard tip
with a %-inch 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 isoklnetic 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
THERMOMETER
CHECK
VALVE
REVERSE-TYPE
PITOTTUBE
ICE BATH IMPINQERS
BY-PASS VALVE
VACUUM
LINE
VACUUM
GAUGE
•AIR-TIGHT
PUMP
DRY TEST METER
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.
2.2.3 Glass sample storage containers.
2.2.4 Graduated cylinder—260 ml.
2.3 Analysis.
2.3.1 Pipette—25 ml., 100ml.
2.3.2 Burette—50ml.
2.3.3 Erlenmeyer flask—260 ml.
2.3.4 Graduated cylinder—100ml.
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 1108
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.
3.1.3 Water—Delonized, distilled.
3.1.4 Isopropanol, 80%—Mix 800 ml. of
Isopropanol with 200 ml. of deionlzed, dis-
tilled water.
3.1.5 Hydrogen peroxide, 3%—Dilute 100
ml. of 30% hydrogen peroxide to 1 liter with
delonized, 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—Deionlzed, distilled.
3.3.2 Isopropanol.
3.3.3 Thorin indicator—l-(o-arsonophen-
ylazo)-2-naphthol-3, 6-disulfonlc acid, di-
sodlum salt (or equivalent). Dissolve 0.20 g.
In 100 ml. distilled water.
3.3.4 Barium perchlorate (0.01N)—Dis-
solve 1.95 g. of barium perchlorate [Ba
(CO,).,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 (0.01AT) —
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 1m-
plnger. Retain 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
Implngers. 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
c.f.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 Implnger 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
isoklnetic conditions. Maintain Isoklnetic
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 35 0472
APPENDIX E
LABORATORY REPORT
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SRL 1281 35 0472
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.
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SRL 1281 35 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 lid , 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.
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SRL 1281 35 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.
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.
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
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SRL 1281 35 0472
with distilled water in the separatory funnel and returned to the
tared beaker for evaporation in the hood. The residues were desiccated
and weighed.
The water portion was transferred to tared beakers, oven dried
at 90 C, desiccated, and weighed. All beakers were "parafilm" sealed for
shipment. Particle size analysis was not performed per instruction
from the Project Officer. A summary of weight measurements is shown
in Table E-l.
SCOTT RESEARCH LABORATORIES. INC
1
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TABLE E-l - SUMMARY OF WEIGHT MEASUREMENTS
30
n
po
20
n
t-
oo
O
ao
I
so
H
O
Run 1
Final
Tare Gross Blank Net
(g) (mg) (mg) (nig)
Container #1
(Filter)
Container #2
(Acetone wash front half)
Container "3a
(Organic excract)
Container #3b
(Water after extraction)
Container US
(Acetone wash back half)
8.1710 8.0790 92.0 - 92.0
88.0860 87.9135 172.5 3.0 169.5
99.5340 99.5290 5.0 0.0 5.0
100.5075 100.4465 61.0 0.0 61.0
94.5905 94.5805 10.0 0.5 9.5
Probe, cyclone, filter, mg. 261.5
Total, mg. 337.0
Run 2
Final Tare Gross Blank Net
(g) (g) (mg) (mg) (mg)
8.2030 8.1015 101.5
101.5
93.8415 93.7345 107.0 2.0 105.0
99.5090 99.5000 9.0 0.0 9.0
99.4915 99.4375 54.0 0.0 54.0
98.3490 98.3370 12.0 1.0 11.0
Probe, cyclone, filter, mg. 206.5
Total, mg. 280.5
Run 3
Final Tare Gross Blank Net
(g) (g) (gm) (mg) (mg)
00
8.2085 8.1145 94.0
94'°
91.8990 91.7500 149.0 1.0 148.0
96.5790 96.5710 8.0 0.0 - 8.0
97.9745 97.9240 50.5 0.0 50.5
101.6575 101.6430 14.5 1.0 13.5
Probe, cyclone, filter, mg. 242.0
Total, mg. 314.0
Run 4
Final Tare Gross Blank Net
(g) (g) (mg) (mg) (mg)
Container //I
(Filter)
7.7760 7.7120 64.0
64.0
Container #2 96.0070 95.8995 107.5 2.0 105.5
(Acetone wash front half)
Container #3a
(Organic Extract)
Container #3b
(Water after extraction)
Container //5
(Acetone wash back half)
97.3620 97.3530 9.0 0.0 9.0
98.1750 98.1425 32.5 0.0 32.5
95.5405 95.5300 10.5 1.0 9.5
Probe, cyclone, filter, mg. . 169.5
Total, mg. 220.5
Run 5
Final Tare Gross Blank Net
(g) (g) (mg) (mg) (mg)
7.7905 7.7125 78.0
78.0
93.4980 93.4020 96.0 1.0 95.0
99.3770 99.3690 8.0 0.0 8.0
98.5585 98.5280 30.5 0.0 30.5
98.5695 98.5550 14.5 1.0 13.5
Probe, cyclone, filter, mg. 173.0
Total, mg. 225.0
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E-7
SRL 1281 35 0472
E.3 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
X
distilled water 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 pg N0« 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 ug N0« was plotted.
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SRL 1281 35 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 my on a Bausch and Lomb Spectronic 20 Colorimeter. The solution
blanks run with each set of samples were used for a colorimeter zero
reference. The absorbances read for each sample were then converted
to yg N09 via the previously established calibration curve. NO con-
Z. X.
centrations were calculated as ppm N0_ following the procedure described
in Appendix B. The laboratory data recorded for each analysis is included
as Table E-2.
E.4 ORSAT ANALYSIS
A total of five integrated bag samples were analyzed by Orsat
during the three day test period. Each five liter Tedlar sample bag
was equipped with a Teflon sample tube fitted with an airtight syringe
cap. Prior to sampling, each bag was flushed with pure, dry nitrogen
and sealed with the syringe cap.
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SRL 1281 35 0472
TABLE E-2 - NO ANALYSIS DATA
Run
No.
1
Date
3/20/72
3/22/72
3/22/72
3/23/72
3/23/72
Sample
Number
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
Absorbance
@ 420 my
0.160
0.227
0.205
0.242
0.240
0.170
0.208
0.050
0.256
0.037
0.230
0.93
0.260
0.199
NOX
Concentration
N02)
119.7
169.8
153.3
181.0
179.5
(lost)
127.1
155.6
37.4
191.5
27.7
172.0
69.6
194.4
148.8
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SRL 1281 35 0472
At the end of each sampling day the sample bags were returned
to the field laboratory where they were analyzed for CO, CCL 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
through each of the three absorbing solutions (potassium hydroxide - CO-,
alkaline pyrogallate - 0~, and acid 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 in Table E-3.
E.5 TOTAL HYDROCARBON ANALYSIS
Immediately following each Orsat analysis the remainder of the
sample contained in each Tedlar bag was analyzed for hydrocarbons via
a Beckman Model 108-A Total Hydrocarbon Analyzer. This instrument
utilized a flame ionization detector and the following operating
conditions were maintained during each analysis:
Sample Backpressure: 2.50 psi
Fuel Pressure: 23.0 psi
Oxidant Pressure: 11.0 psi
Range: 100 X
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SRL 1281 35 0472
TABLE E-3 - ORSAT ANALYSIS DATA
Run Sample
No. Date Number Component
1 3/20/72 1 C02
°2
CO
2 C02
°2
CO
3 C02
°2
CO
2 3/22/72 1 C02
°2
CO
2 C0_
°2
CO
3 C0_
°2
CO
Analysis
Number
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
Bunette Volume (ml)
Initial
100.0
99.8
81.6
1100.0
99.8
81.7
100.0
99.8
81.6
100.0
99.7
80.1
100.0
99.8
80.1
100.0
99.7
80.1
Final
99.8
99.8
81.6
81.6
81.6
81.6
99.8
99.8
81.7
81.7
81.7
81.7
99.8
99.8
81.6
81.6
81.6
81.6
99.7
99.7
80.1
80.1
80.1
80.1
99.8
99.8
80.1
80.1
80.1
80.1
99.7
99.7
80.1
80.1
80.1
80.1
Difference
0.2
0.2
18.2
18.2
0.0
0.0
0.2
0.2
18.1
18.1
0.0
0.0
0.2
0.2
18.2
18.2
0.0
0.0
0.3
0.3
19.6
19.6
0.0
0.0
0.2
0.2
19.7
19.7
0.0
0.0
0.3
0.3
19.6
19.6
0.0
0.0
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SRL 1281 35 0472
TABLE E-3 - ORSAT ANALYSIS DATA
(continued)
Run
No.
Date
Sample
Number
3 7/22/72 1
4 7/23/72 1
Component
co2
°2
CO
co2
°2
CO
co2
°2
CO
co2
°2
CO
co2
°2
CO
co2
°2
CO
Analysis
Numb er
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
Bunette Volume (ml)
Initial
100.0
99.8
80.4
100.0
99.8
80.4
100.0
99.7
80.3
100.0
99.7
79.9
100.0
99.6
79.9
100.0
99.7
99.9
Final
99.8
99.8
80.4
80.4
80.4
80.4
99.8
99.8
80.4
80.4
80.4
80.4
99.7
99.7
80.3
80.3
80.3
80.3
99.7
99.7
79.9
79.9
79.9
79.9
99.6
99.6
79.9
79.9
79.9
79.9
99.7
99.7
79.9
79.9
79.9
79.9
Difference
0.2
0.2
19.4
19.4
0.4
0.0
0.2
0.2
19.4
19.4
0.0
0.0
0.3
0.3
19.5
19.5
0.0
0.0
0.3
0.3
19.8
19.8
0.0
0.0
0.4
0.4
19.7
19.7
0.0
0.0
0.3
0.3
19.8
19.8
0.0
0.0
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SRL 1281 35 0472
TABLE E-3 - ORSAT ANALYSIS DATA
(continued)
Run Sample Analysis Analysis
No. Date Number Component Number
5 3/23/72 1 C02
°2
CO
2 C0_
°2
CO
3 CO
.
°2
CO
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
Bunette Volume (ml)
Initial
100.0
99.6
79.8
100.0
99.6
79.8
100.0
99.5
79.7
Final
99.6
99.6
79.8
79.8
79.8
79.8
99.6
99.6
79.8
79.8
79.8
79.8
99.5
99.5
79.7
79.7
79.7
79.7
Difference
0.4
0.4
19.8
19.8
0.0
0.0
0.4
0.4
19.8
19.8
0.0
0.0
0.5
0.5
19.8
19 . 8
0.0
0.0
SCOTT RESEARCH LABORATORIES, INC
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E-14
SRL 1281 35 0472
The Scott compressed gases used during each analysis were:
Fuel: 40% hydrogen in nitrogen
Oxidant: Blended Air
Zero: Hydrocarbon Free Air (<0.1 ppm-C)
Span: 99.9 ppm propane (±2.0% analysis) in nitrogen
Just prior to introducing each sample into the analyzer,
the instrument was zeroed and spanned on range 100. The Tedlar sample
bag was then connected to the analyzer via a Teflon tube and the sample
was drawn into the analyzer until a stable reading was recorded on the
meter. The bag was then disconnected and resealed with the syringe cap.
The instrument zero and span points were rechecked to insure that the
calibration had not changed during the analysis. The complete analytical
procedure was then repeated until good duplication of results were obtained.
All meter readings recorded for each sample are included as Table E-4.
The meter readings were then converted to parts per million
carbon by the following formula:
99.9 ppm-C3HR 3 ppm-C
ppm-C = meter units x -r^— . ~ — x rr, „
vv 100 units-Span ppm-C-Hg
The final data with example calculations are included in Appendix B of
this report.
SCOTT RESEARCH LABORATORIES, INC
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E-15
SRL 1281 35 0472
TABLE E-4 - TOTAL HYDROCARBON DATA
Run
No.
Date
3/20/72
3/22/72
3/22/72
3/23/72
3/23/72
Sample
No.
1
2
1
2
1
2
1
2
1
2
Range
100
100
100
100
100
100
100
100
100
100
Meter Units
Sample
69.5
69.5
35.0
33.0
16.0
16.0
10.5
10.5
5.0
7.0
Span
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
SCOTT RESEARCH LABORATORIES, INC
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F-l
SRL 1281 35 0472
APPENDIX F
TEST LOG
SCOTT RESEARCH LABORATORIES. INC
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F-2
SRL 1281 35 0472
TEST LOG
On Monday, March 20, 1972, the Scott test team arrived at
the Wentz Plant of Westmoreland Coal Company in Stonega, Virginia,
and began to set up the test equipment. Upon arrival at the site it
was learned that a wildcat strike had just started, but that there
was enough Osaka coal to continue processing for 8 or 9 hours. The
process was switched to Osaka coal around noon by which time Scott was
set up and prepared to start testing. Preliminary velocity and
temperature traverses were performed and a nozzle size selected.
The first run was started at 1523. Twenty-four points were traversed
in each port for a period of 2% minutes each. The pitot line became
clogged with water at one point and had to be blown out. The first run
was completed at 1825. An Orsat and total hydrocarbon sample was
collected from 1512 to 1607. NO samples were collected at 1540, 1628,
X
and 1807. During the test a brownish plume was observed trailing off
from the stack.
The sample train was dismantled and the spare system was
assembled for the second run. A leak test was performed and found to be
satisfactory. When the pump was turned on to start the test, all of the
power went off. Apparently the plant had turned on night lights between
the tests and the circuit was not large enough to carry everything.
Several attempts were made to supply alternate power but with no success.
Thus, it was decided to be ready for a test early the next morning. The
samples were returned to the motel where all sample transfers were
performed and a new system, as well as a backup unit were prepared. The
Orsat and hydrocarbon samples were analyzed and the NO samples trans-
X
ferred to sample bottles.
SCOTT RESEARCH LABORATORIES, INC.
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F-3
SRL 1281 35 0472
It was believed that there would be enough coal to perform a
run first thing Tuesday morning even if the strike continued. Thus,
the Scott team arrived at the plant early and began setting up for a
test run. It was soon learned that the entire plant was now striking
and that no testing could be performed. The strike was settled late
in the afternoon and preparations were made to test on Wednesday.
Wednesday the Scott team arrived at the plant and prepared
to run a test while the plant was processing Osaka coal. A leak test
was performed and the filter holder was found to leak slightly, but it
was acceptable. The run was started at 940 and continued to 1142.
The Orsat and hydrocarbon sample was collected from 935 to 1030. NO
samples were collected at 950, 1025, and 1115. The sample train was
disassembled and the second system was set up and leak tested.
The third run was then started at 1305 and ran until 1515.
The Orsat and hydrocarbon sample was collected from 1304 to 1404.
The first sample for NO was collected at 1325. Other NO samples
X X
were taken at 1430 and 1520. During both tests a slight brownish
plume was observed trailing off from the stack.
The sample train was dismantled and taken back to the motel
where both sample trains were cleaned and the samples transferred to
sample bottles. During the cleanup and transfer, it was noted that the
filters were being torn by the gasket in the filter holder. This did
not affect the test, but made the cleanup procedure difficult. The
Orsat and hydrocarbon samples were analyzed while the NO samples were
X
transferred. The sample trains were then prepared for more tests.
SCOTT RESEARCH LABORATORIES, INC.
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F-4
SRL 1281 35 0472
On Thursday the Scott team arrived at the plant and set up to
perform tests while the plant was processing Wentz coal. The sample
train was put in place and a leak test performed. It was found to be
satisfactory and the test was started at 925 and ran until 1130. It
was snowing and very windy during the test. At 1045 the wind blew over
the manometer being used to measure the draft. Thus, no readings were
taken after 1045. The Orsat and hydrocarbon sample was collected from
925 to 1025. The NO samples were collected at 950, 1020, and 1115.
X
The sample train was disassembled and the second unit prepared to start
testing.
A leak test was performed and found to be satisfactory. The
test was started at 1144. It had to be stopped at 1254 because of a
coal blockage in the plant operation. The test was restarted at 1336
and continued until 1430. The Orsat and hydrocarbon sample, was collected
from 1138 to 1238. The NO samples were taken at 1205, 1340, and 1415.
X.
Because of the weather conditions it was difficult to obtain a good
visible description of the stack plume.
The sampling train was disassembled and all of the test
equipment was removed from the test site. Back at the motel the sample
transfer and analyses were performed. The Scott team traveled home on
Friday.
Figure F-l illustrates the test program schedule.
SCOTT RESEARCH LABORATORIES, INC.
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FIGURE F-l SUMMARY OF TEST PROGRAM
®
M 1500
S
H
90
n
en
tn
ft
SB
» 0925
o
90
O
90
M
ft
1300
0900
1125
15*12 1607 °rSat & HC Sample
Change
1523 1620 X*~\ Ports 1725
1701 1704
1540 1628
933 1025
Change
940 • 104o'"1fortS 1042 1142
• • *
950 1025 1115
1304 1404
Change
1305 1405 °rtS 1415 1515
» • «
1325 1430 1520
925 1025
Change
09*^ -"'""i* O T t S^
J^ 1025 1030 1130
• • •
950 1020 1115
1138 1238
Change
1144 /forfcs "\ ' .
1244 1246 1254 1336
• • • •
1205 1340
RUN 1 - 3/20/72
1825
• NO
1807 x
RUN 2 - 3/22/72
1220
NO
X
RUN 3 - 3/22/72
1555
NO
*
RUN 4 - 3/23/72
1155
NO
X
RUN 5 - 3/23/72
1445
1430
• NO-
1415 X
UJ
P
1845 g
'Particulate i—
w
Ui
o
Ni
Particulate
Particulate
Particulate
Particulate
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G-l
SRL 1281 35 0472
APPENDIX G
PROJECT PARTICIPANTS AND TITLES
SCOTT RESEARCH LABORATORIES, INC
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G-2
SRL 1281 35 0472
PROJECT PARTICIPANTS AND TITLES
The personnel taking part in the project include:
Thomas Ward
Charles Sedman
Larry Jones
Norman Troxel
Joseph Wilson
Jyotin Sachdev
William Scott
Zenophon Tomaras
Margaret Husic
Louis Reckner
Project Officer - EPA
Project Engineer - EPA
Project Engineer - EPA
Senior Engineer - SRL
Field Team Leader - SRL
Engineer - SRL
Technician - SRL
Chemist - SRL
Technician - SRL
Manager, Atmospheric Chemistry &
Industrial Emissions Dept.
SCOTT RESEARCH LABORATORIES. INC
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