New Jersey Zinc Company
Feiro-Alloy Sinter Plant
East Plant Baghouse
Palmerton, Pennsylvania
Scott
Environmental Technology
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SRL 1425 01 0474
New Jersey Zinc Company
Ferro-Alloy Sinter Plant
- East Plant Baghouse
Palmerton, Pennsylvania
Prepared For:
Environmental Protection Agency
Research Triangle Park
North Carolina 27711
Contract No.: 68-02-0233
EPA Report No. 74-ZNC-l
Prepared By:
G. Rulings Darby
SCOTT RESEARCH LABORATORIES, INC.
Plumsteadville, Pennsylvania 18949
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SRL 1425 01 0474
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 SAMPLING POINTS 4-1
5.0 SAMPLING AND ANALYTICAL PROCEDURES 5-1
5.1 PARTICULATE 5-1
5.2 GASES 5-1
APPENDIX A COMPLETE PARTICULATE RESULTS WITH
SAMPLE CALCULATIONS ' A-l
APPENDIX B COMPLETE GASEOUS EMISSION RESULTS WITH
SAMPLE CALCULATIONS B-l
APPENDIX C FIELD DATA . C-l
APPENDIX D STANDARD SAMPLING PROCEDURES D-l
APPENDIX E LABORATORY REPORT E-l
APPENDIX F TEST LOG F-l
APPENDIX G PROJECT PARTICIPANTS AND TITLES G-l
SCOTT RESEARCH LABORATORIES, INC.
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SRL 1425 01 0474
1.0 INTRODUCTION
Scott Research Laboratories, Inc. performed source sampling tests
at the East Plant of New Jersey Zinc Company's Ferro-Alloy Sinter Plant
in Palmerton, Pennsylvania during the week of February 4, 1974. The plant
uses a baghouse to control the exhaust emissions from an ore roasting
operation.
The exhaust gases were sampled both at the inlet and outlet of the
baghouse, and were analyzed for total particulate loading, sulfur dioxide,
carbon dioxide, carbon monoxide, and oxygen.
As scheduled, the work program consisted of three pairs of
stationary particulate tests, each pair involving inlet and outlet measure-
ments. The first two pairs of tests were performed on February 6, 1974,
with the third pair being done February 7, 1974. The outlet measurement
portion of the third pair was invalidated by a loose impinger. Mr. Douglas
Bell, of the Emission Measurements Branch, directed that the test not be
redone, stating that the results obtained were sufficient. Figures 1-1 and
1-2 show the location of the sampling points at the baghouse inlet and
outlet.
SCOTT RESEARCH LABORATORIES, INC.
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Exhaust
Gas Flow
o
s
H
to
PI
t/i
Pi
>
90
O
SB
> Sample
Ports
o
39
C/l
3
I Test Platform
Test
Scaffold
T~T"T"T~r
D
' Gas
Exhaust
Stack
Test
Scaffold^
Baghouse
Sample
Ports
i
to
FIGURE 1-1 NEW JERSEY ZINC CO. EAST PLANT BAGHOUSE, SOUTH ELEVATION
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N
Test
Scaffold
Sample
tfPbrts
FIGURE 1-2 NEW JERSEY ZINC CO. EAST PLANT BAGHOUSE, PLAN.
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. 2-1
SRL 1425 01 0474
2.0 SUMMARY OF RESULTS
t
A summary of test results is presented in Tables 2-1 through 2-4.
The particulate weights are summarized and shown in Table 2-5. The
complete particulate results, including sample calculations, appear as
Appendix A.
'.'''• -It was learned after the test that while the sample runs were
being made, bypassing occurred in the baghouse. The bypassing was caused
by inadequate bag cleaning which caused a pressure buildup in the baghouse
which, in turn, caused a valve, used in keeping the bags hot during sinter
machine shutdown, to open and allow the inlet gas stream to bypass the
bags and pass directly into the outlet stack. The plant said this problem
would be corrected in a few months when a larger compressor for bag cleaning
is put on the baghouse and a stronger valve is installed. Meanwhile, however,
the results obtained at the outlet during this test are unusually high and
are not representative of normal emissions from the baghouse.
^^Jf^
SCOTT HKSKARCII LABORATORIES. INC.
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2-2
SRL 1425 01 0474
TABLE 2-1 SUMMARY OF TEST RESULTS
NEW JERSEY ZINC CO. EAST BAGHOUSE PLANT INLET
(British Units)
Run Number
Date
(a)
Volume of Gas Sampled - DSCF '
Percent Moisture by Volume
Average Stack Temperature - °F
Stack Volumetric Flow Rate - DSCFM^
(c)
Stack Volumetric Flow Rate - ACFM
Percent Isokinetic
Percent Excess Air
Percent Opacity
Feed Rate - ton/hr
Particulate - probe, cyclone &
filter catch
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
Particulate - total catch
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
Percent Impinger Catch
(a) Dry standard cubic feet at 70°F, 29.92
(b) Dry standard cubic feet per minute at
(c) Actual cubic feet per minute.
C\} SCOTT RESEARCH LABORATORIES, INC.
1
2/6/74
62.4
6.61
69
23906
32558
80.3
562
-
2051.1
0.5062
0.4764
103.7
2167.3
0.5349
0.5034
109.6
77.3
In.Hg.
70°F, 29
2
2/6/74
37.09
7.67
58
22890
30894
85.9
562
-
1297.6
0.5388
0.5087
105.7
1359.3
0.5644
0.5328
110.7
79.9
.92 in.Hg.
3
2/7/74
38.01
8.06
49
22395
30721
89.9
562 .
-
1748.4
0.7084
0.6697
135.3
1833.8
0.7430
0.7024
142.6
85.5
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2-3
SRL 1425 01 0474
TABLE 2-2 SUMMARY OF TEST RESULTS
NEW JERSEY ZINC CO. EAST BAGHOU6E PLANT INLET
(Metric Units)
Run Number .
Date (a)
Volume of Gas Sampled - Nm
Percent Moisture by Volume
Average Stack Temperature - °C
*•
Stack Volumetric Flow Rate - Nm"
Stack Volumetric Flow Rate - m /
Percent Isokinetic
Percent Excess Air
Percent Opacity
Feed Rate - M tqn/hr
Particulate - probe, cyclone &
filter catch
mg
mg/Nm
mg/m
kg/hr
kg/M ton feed
Particulates --total catch
mg
mg/Nm
mg/m
kg/hr
kg/M ton feed
Percent Impinger Catch
1
2/6/74
1.767
6.61
20.6
676.9
921.9
80.3
562
2051.1
1158
1090
47.0
2167.3
1224
1152
49.7
2
2/6/74
1.050
7.67
14.4
648.2
874.8
85.9
562
1297.6
1233
1164
47.9
1359.3
1291
1219
50.2
3
2/7/74
1.076
8.06
9.4
634.2
869.9
89.9
562
1748.4
1621
1532
61.4
1833.8
1700
1607
64.7
77.3
79.9
85.5
(a) Dry normal cubic meter at 21.1°C and 760 mm Hg.
(b) Dry normal cubic meters per minute'at 21.1°C and 760 mm Hg.
(c) Actual cubic meters per minute.
SCOTT RESEARCH LABORATORIES, INC.
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2-4
SRL 1425 01 0474
TABLE 2-3 SUMMARY OF TEST RESULTS
NEW JERSEY ZINC CO. EAST BAGHOUSE PLANT OUTLET
(British Units)
Run Number
(b)
Date
Volume of Gas Sampled - DSCF
Percent Moisture by Volume
Average Stack Temperature - °F
Stack Volumetric Flow Rate - DSCFM
fc)
Stack Volumetric Flow Rate - ACFMV
Percent Isokinetic
Percent Excess Air
Percent Opacity
Feed Rate - ton/hr
2/6/74
72.24
5.90
59
30682
37939
98.0
718
2/6/74
68.64
6.95
61
28694
36084
99.6
718
Particulate -
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
probe, cyclone &
filter catch
193.6
0.04127
0.03987
10.85
210.1
0.04714
0.04462
11.59
Particulate - total catch
mg
gr/DSCF
gr/ACF
Ib/hr
Ib/ton feed
Percent Impinger Catch
236.1
0.05033
0.0';862
13.23
81.6
269.4
0.06044
0.05720
14.86
84.0
(a) Dry standard cubic feet at 70°F, 29.92 in.Hg.
(b) Dry standard cubic feet per minute at 70°F, 29.92 in.Hg.
(c) Actual cubic feet per minute.
SCOTT RESEARCH LABORATORIES, INC.
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2-5
SRL 1425 01 0474
TABLE 2-4 SUMMARY OF TEST RESULTS
NEW JERSEY ZINC CO. EAST BAGHOUSE PLANT OUTLET
(Metric Units)
Run Number
,00
Date
Volume of Gas Sampled - Nm""
Percent Moisture by Volume
Average Stack Temperature - °C
o
Stack Volumetric Flow Rate - Nm /min
o (c
Stack Volumetric Flow Rate - m /min
Percent Isokinetic
Percent Excess Air
Percent Opacity
Feed Rate - M ton/hr
2/6/74
2.046
5.90
15.0
868.8
1074.3
98.0
718
2/6/74
1.944
6.95
16.1
812.5
1021.8
99.6
718
Particulate - probe, cyclone &
filter catch
mg
3
mg/Nm
o
mg/m
kg/hr
kg/M ton feed
193.6
94.43
91.22
4.92
210.1
107.9
102.1
5.26
Particulates - total catch
mg
3
mg/Nm
o
mg/m
kg/hr
kg/M ton feed
Percent Impinger Catch
236.1
115.2
111.2
6.00
81.6
269.4
138.3
130.9
6.74
84.0
(a) Dry normal cubic meter at 21.1°C and 760 mm Hg.
(b) Dry normal cubic meters per minute at 21.1°C and 760 mm Hg.
(c) Actual cubic meters per minute.
SCOTT RESEARCH LABORATORIES, INC.
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2-6
SRL 1425 01 0474
TABLE 2-5 SUMMARY OF PARTICULATE WEIGHTS
(All weights given in milligrams)
NEW JERSEY ZINC CO. EAST BAGHOUSE PLANT INLET
Weight
Filter
Front Wash
Probe, cyclone, and filter
Back Wash
Total
Run Number
1
1385.0
666.1
2051.2
116.2
2167.3
2
972.8
324.8
1297.6
61.7
1359.3
3
1069.9
678.5
1748.4
85.4
1833.8
NEW JERSEY ZINC CO. EAST BAGHOUSE PLANT OUTLET
Weight
Filter
Front Wash
I
Probe, cyclone, and filter
Run Number
132.1
61.5
193.6
161.3
48.8
210.1
Back Wash
Total
42.5
236.1
59.3
269.4
SCOTT RESEARCH LABORATORIES, INC.
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3-1
SRL 1425 01 0474
3.0 PROCESS DESCRIPTION
The baghouse tested served as the emission control device for the
zinc sintering machine.
The New Jersey Zinc Company has facilities for feeding two types
of feed to this sintering machine: an unroasted zinc oxide ore and
a roasted zinc sulfide concentrate. All other primary zinc smelters
feed the roasted zinc sulfide concentrate; therefore, during the emission
tests this type of feed was fed to the sintering machine. The primary
purpose of the sintering machine is to agglomerate the charge into a
hard permeable mass suitable for feed to.a reduction system. The
sintering machine also removes lead and cadmium impurities and residual
sulfur remaining after roasting.
The sintering machine incorporates bar- or grate-type pallets
which are joined to form a continuous metal conveyor system. The
concentrate is distributed on the pallets and ignited. The New Jersey
i
Zinc Company uses a downdraft-type sintering machine, which means
the air supply passes downward through the sinter bed and into wind
boxes. The effluent stream is then ducted to the baghouse from the
wind boxes.
The baghouse has 1320 bags made of Nomex felt with an air-to-cloth
ratio of 3.25:1. The effluent from the baghouse exits out a 60-foot stack.
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4-1
SRL 1425 01 0474
4.0 LOCATION OF SAMPLING POINTS
The exhaust gases from an ore-roasting operation exit through a
horizontal 36" I.D. insulated pipe located 33' above grade, pass through
the baghouse, and are drawn through a pump. They then pass into a 60'
high 48" O.D. steel stack.
Two ports separated by 90°, were cut into the inlet pipe 10'
before the 90° bend leading into the baghouse, about 30' from the outside
wall of the sintering machine building. One port was located on the top,
because buildup of solid material was expected to have collected within
the pipe; the other port was located in the west side of the pipe.
Two ports, separated by 90°, were cut into the east and south
sides of the outlet stack 24' above grade.
The upstream and downstream disturbances were located at the
following duct diameter distances:
Inlet
Number of duct diameters from upstream disturbance: 10
Number of duct diameters from downstream disturbance: 3.3
Outlet
Number of duct diameters from upstream disturbance: 7
Number of duct diameters from downstream disturbance: 1.8
Special scaffolding, constructed by Riebe Construction Company,
was required at both locations to accomplish the desired sampling. Figures
1-1 and 1-2, above, show the physical layout of the system and the location
of the scaffolding and sample ports.
The traverse points for the inlet and outlet sampling locations
are shown in Figures 4-1 and 4-2, respectively.
SCOTT RESEARCH LABORATORIES, INC.
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4-3
SRL 1425 01 0474
FIGURE 4-1 TRAVERSE POINTS FOR INLET SAMPLING LOCATIONS
(Observer facing flow)
SCOTT RESEARCH LABORATORIES. INC.
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SRL 1425 01 0474
4-4
FIGURE 4-2 TRAVERSE POINTS FOR OUTLET SAMPLING LOCATIONS
SCOTT RESEARCH LABORATORIES, INC.
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5-1
SRL 1425 01 0474
5.0 SAMPLING AND ANALYTICAL PROCEDURES
5.1 PARTICULATE
5.1.1 Sampling
Samples were collected for the determination of particulate
matter at the inlet and outlet of the baghouse. The sampling locations
are described in Section 4.0. The sampling and analytical procedures
used were the same as those specified by Method 5, "Determination of
Particulate Emissions from Stationary Sources," and published in the
Federal Register, 3£ (247), Thursday, December 23, 1971. 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 heated cyclone and filter,
and then into an iced impinger train. Isokinetic conditions are maintained
by monitoring the stack gas velocity with an "S" type pitot tube.
5.1.2 Analytical Procedures
After testing was completed, the train, including the probe,
was thoroughly washed with acetone. The washings were evaporated, dried,
and weighed along with the filter in order to obtain the total weight of
particulate matter collected.
The stack gas velocity and flow rate were measured using Method 2,
"Determination of Stack Gas Velocity and Volumetric Flow Rate (Type S
Pitot Tube)," published in the Federal Register. Using both the weight
of sample collected and the flow rate determined, a total particulate
emission rate was calculated.
5.2 GASES
The sampling and analytical procedures used were in accordance
with Federal Register _% (247), December 23, 1972, "Standards of Performance
for New Stationary Sources."
5.2.1 Carbon Oxides and Oxygen
Sampling
Grab samples, for analysis for carbon oxides and oxygen, were
taken in accordance with EPA Method No. 3 during the final particulate
sampling run at both the inlet and outlet locations. Briefly, sampling
was accomplished by withdrawing the gas through a glass-wool plug and a
SCOTT RESEARCH LABORATORIES. INC.
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5-2
SRL 1425 01 0474
one-way valve into a squeeze bulb, this bulb being so arranged as to deliver
the sample through another one-way valve and a length of Teflon tubing into
a Tedlar bag of approximately 5 liter capacity.
Analytical Procedure
The grab sample bags were analyzed by the Orsat method for CO,
C0_, and 0_. Repetitive analyses were performed on each bag to ensure
analytical reliability. The results were reported in percentages.
5.2.2 Sulfur Dioxide and Sulfur Trioxide
Sampling
Grab samples, for analysis for sulfur dioxide and sulfur
trioxide, were taken at approximately the same time and in exactly the
same manner as described in Section 5.2.1.
Analytical Procedure
The grab sample bags were analyzed for SO- and SO- by EPA Method 6.
The exact procedure used is described in detail in Appendix E.
SCOTT RESEARCH LABORATORIES. INC.
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A-l
SRL 1425 01 0474
APPENDIX A
COMPLETE PARTICULATE RESULTS WITH SAMPLE CALCULATIONS
SCOTT RESEARCH LABORATORIES, INC.
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REPORT NO. /'2.i> - ^ '
A-2
PAGE
OF
PAGES
SOURCE TESTING CALCULATION FORMS
Test No.
No. Runs
Name of
Location
Type of
Control
Sampling
i* urn? \
rr\ 1 o
of Plant \ 3. V\A«/r-4o-n , •> a .
«
Plant fc^-Sf W:;;
7s-. /.> ^/'
7.
2/.j.r
i.cte
a. s i
61
QZ/c1':
1C l.-_.
5.13
*70°F, 29.92" Hg.
SCOTT RKSEAr.Ci: UKORATOi'.lES. INC.
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A-3
PARTICULATE EMISSION' DATA (contcl)
Run No.
XM - % Moisture in the stack gas
bv volur.e
M. - Mole fraction of dry gas
% co2
%o2
%N2
M W, '- Molecular weight of dry
stack p.as
M V.T - Molecular v.'eight of stack
gas
AP - Velocity Head of stack
gas, In. HO
T - Stack Temperature, °F
S
"Y s v ~ s
P - Stack Pressure, "llg. Absolute
i
V - Stack Velocity @ stack
conditions, fpm
2
A - Stack Area, in."
S
Q - Stack Gas Volume @
S Stnnrlard Conditions. *SCFM
T. - Net Time' of Test, min.
D - Sampling Nozzle Diameter, in.
%I - Percent isokinetic
m, - Particulate - probe, cyclone
and filter, Kg.
m - Particulate - total, rag.
C - Particulate - probe, cyclone,
an and filter, gr/SCF
C - Particulate - total, gr/SCF
ao
C - Particulate - probe, cyclone, &
filter, gr/cf Q stack conditions
IN)
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bCOTT nESEAlICl! LABOUATOHinS. INC.
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A-4
PARTICULATE EMISSION DATA (coned)
Run No .
Cn - Particulatc, total, gr/cf
@ stack cond.
C - Particulnte, probe, cyclone,
av/ and filter, Ih/hr.
C - Particulnte - total, Ib/hr.
ax
7, EA - % Excess air (?
samplin?. point
1 N Lfc i
/
Wftf
/.v7i
ws?
*..«
0.
0/lr/y
/o5T7n
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t
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7/S.I3
2
Cl j-
(7 G *"
7,r.W
*70°F. 29.92" Hg.
SCOTT r.KSKAKCH LA):01i/.TO:u:-:s..INC.
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A-5
' PARTICULATE CALCULATIONS
1. Volui-e of dry gns sampled at standard conditions - 70°r, 29.92"
17.7 X V /P., + P
r.i B m
= Ft-
13.6
std
(T + 460)
m
1-
2. Volume of v.'atcr vapor at 70°F & 29;92" Hg, Ft
V = 0.0474 X V = Ft.'
w w
gas
- 0,0474
3. % Moisture in stack gas
100 X V
w
gas = %
%M = V + V
m , w
std gas
-- U\
4- .
/Mole fraction of dry gas
i
M. • IPO - %H -
100
5. Average molecular v;eight of dry stack gas
M W . = (%CO X 44 ) + (%0 X 32 ) +(%N X 28 ) + (%CO X 28 )
• 100 100 r 100 _ „ 100^
6. Molecular weight of stack g,as
M W = M W • X M. +18 (1 - M.)
ad a
SCOTT HEDEAllCi: UJJOUATOr.IUS. INC.
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A-6
7. Stack velocity & Stack conditions, fpm
V = 4350 X,/i.P X (T + 4
s V s . s
60)
1'
P X M W
s
1/2
8. Stack gas voluir.e @ standard conditions, SCFM
A 0.123 X V X A X M, X P „__
Q = s s d s = SCFM
S . (T + 460)
S
9. Per cent isokinctic
1032 X (T + 460) X V
m
std = %
V XT X P X M. X (D )
s t s d n
(32, ^X43r.
~l&
4m
10. Particulate - probe, cyclone, & filter, gr/SCF
C = 0.0154 X Mf = gr/SCF
' an r:
m std
11. Particulate total, gr/SCF
= 0.0154 X Mt = gr/SCF ._ (0,0|S"4
td
- 0.5349
12. Particulate - probe, cyclone & filter, gr/CF at stack conditions.
„ 17.7 X C X P X M. , .,
C = an s d = gp/CF ^
a . (T + 460)
s
GCOTT i;ns;::.r.cu LAnonATo:-:iss. IMC.
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A-7
13. Particulrte - total, gr/CF @ stack conditions
= 17>7 X Cno X Ps X Md = gr/CF -
3U (T + 460)
14. Particulate - probe, cyclone, & filter, lb/hr.
C = 0.00857 X C X Q = lb/hr. •=
aw an s
- /03-7/
15. Particulate - total, lb/hr.
C = 0.00857 X C X Q = lb/hr. -
ax • ,• ao s
16. % excess air at sampling point
% EA = 100 X % 02 .
0.266 X % N - %
' <
?COTT )»ESI;ARCII LAi:oRATor.ir.s. INC.
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B-l
SRL 1425 01 0474
APPENDIX B
COMPLETE GASEOUS EMISSION RESULTS WITH SAMPLE CALCULATION
SCOTT RESEARCH LABORATORIES. INC.
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B-2
SO,, EMISSION DATA
U C.M-» OA
Run No.
Date
_^^ JJLIl^
1Hg^g2 iv?, i>-.
G >
T - Average Gas Meter Temperature,
m o v.
P - Barometric Pressure, "Hg abs.
V - Volume of dry gas sampled @
m .meter conditions, ft.
jOpv.v 56^
V^'2 f^~<^
\ti U£T '
3
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L
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0,
^
^
^,^^
;y/
^,
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:t)'
»•?
.r
<1
n
).d,
5
__ 0.7332 X mg S0_
ppm S02 = _ b 2
P, X V
b m
/Ol?
SCOTT r.EEKAKCIl LAUOlUTO.IJtS, INC.
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C-l
SRL 1425 01 0474
APPENDIX .C
FIELD DATA
SCOTT RESEARCH LABORATORIES, INC.
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, v
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^ — •x
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TRAVERSE
POINT
NUMBER
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3 PLANT A/ a ^V~o l<-/^-/\
\(\Y DATE ' ,/fc/-7^/
VX N SAMPLING L(
SAMPLE TYP
RUN NUMBEF
OPERATOR
AKBIEHT TE
BAROMETRIC
STATIC PRE!
FILTER HUM
\. CLOCK TIME
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REFERENCE
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I 4'72 ' . .' .
-------
/
r
VATY.R VOLUME
Run No.
Date
Bubbler
Silica Gel No.
Gross
Water Added(-)
Bubbler
Gross Wftt.(-)
> 2-
(A)
(B)
Net
(A)
Net (+)
(B)
Total U-atcr
. 2.
cc
Forn ll&D 109
-------
FIELD DATA
(A
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-------
C-5
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WATER VOLUKE
Run No.
Date
Bubbler *1
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Gross
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cc
Forn USD 109
-------
FIELD DATA
TRAVERSE
POINT
NUMBER
/
2~
3
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REFERENCE
ATIC OF TRAVERSE POINT LAYOUT f~
CRD ALL DATA EVERY ^£? MINUTES / ^
ORIFICE PRESSURE
DIFFEREiNllAL
(AH), in. H20)
DESIRED
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EPA (Dur) 235
4'72 '
O
-------
:-?
WATER VOLUME
Run No.
Pate
Bubbler :/!l \4J"
Silica Gel X
3 Wftt. g. 5/
Bubbler 3?A
Gross
Water Added(-)
Gross Wg-t.(-)
(A)
(B)
Net
(A)
Net
(B)
Total V.'atcr
70.2—
cc
Fom RftD 109
-------
FIELD DATA
. 2, ^
PLANT__
DATE / /(, /~7J-t
SAMPLING LOCATION
SAMPLE TYPE ^
RUN NUMBER /
OPERATOR
AKBIENT TEMPERATURE .
BAROMETRIC PRESSURE .
STATIC PRESSURE, (Ps)_
FILTER NUMBER (s) I
O
// is
PROBE LENGTH AND TYPE
NOZZLE I.D..
ASSUMED KOISTURE.3
SAMPLE BOX NUMBER
METER BOX NUMBER .
METER AHg
CFACTOR_
/ O
PROBE HEATER SETTING
HEATER B.OX SETTING_
REFERENCED
SCHEMATIC OF TRAVERSE POINT LAYOUT
READ AND RECORD ALL DATA FVFRY 3 MINUTES
TRAVERSE
POINT
NUKI3ER
/ 1
IT-,
'
n
7-0
CLOCK TIME
/Z-
30
is
GAS METER READING
(Vm). I!3
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VELOCITY
HEAD
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ORIFICE PRESSURE
DIFFERENTIAL
(iH). in. H20)
DESIRED ACTUAL
,
-------
-—"Sf*" v
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6
TRAVERSE
POINT
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7. 7
3-fc-
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J3
-------
C-10
WATER VOLU1T.
Run No
. /
Pate J3 / U '7
-------
TRAVERSE
POINT
NUMBER
Jt-
7
f2_
n
11
FIELD DATA
PLANT.
DATE / / U / ^
PROBE LENGTH AND TYPE.
NOZZLE ID . 3-/
SAMPLING LOCATION
SAMPLE TYPE
RUN NUMBER
OPERATOR ___^_
AMBIENT TEMPERA'TU^E .
BAROMETRIC PRESSURE .
STATIC PRESSURE, (Ps)_
FILTER NUMBER (s)
ASSUMED MOISTURE, % /_k
SAMPLE BOX NUMBER
METER BOX NUMBER.
METER AH&, l_
CFACTOR
2-
PROBE HEATER SETTING.
HEATER BOX SETTING
REFERENCE Ap A-
SCHEMATIC OF TRAVERSE POINT LAYOUT
READ AND RECORD ALL DATA EVERY.
MINUTES
CLOCK TIME
6
GAS METER READ'ING
(Vm), H3
7-77
If,
Hi
•JL.
VELOCITY
HEAD
(Aps), in. H20
,37
^
L
-------
TRAVERSE
POINT
NUMBER*
CLOCK TIME
GAS METER READING
.vmut
3
VELOCITY
HEAD
IApK in. H0
ORIFICE PRESSURE
DIFFERENTIAL
IAH). in HOi
DESIRED ACTUAL
STACK
TEMPERATURE
(TS).°F
DRY GAS METER
TEMPERATURE
INLET OUTLET
PUMP
VACUUM.
in Hj
SAMPLE BOX
TEMPERATURE.
°F
IKPINGER
TEMPERATURE.
°F
3,*?
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-------
C-13
WATER VOLUME
Run No. k &UTC£T Hate
BubbleX^L-TN / <~c/ ^<- Silica Gel No. Wftt. g. $UO .
f 3 U 'V^it Bubbler /'A ^> ^ 7> 7
Gross
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Net- or
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Net
(A)
Net (+) ; 7> ^
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, 3
Total V.'ater . cc
Fom ll&D 109
-------
DRY MOLECULAR WEIGHT DETERMINATION
PLANT
DATE
/v
SAMPLING TI"iE (24-hr CLOCK).
SAPLING LOCATION.
SAMPLE TYPE (BAG, INTEGRATED, CONTINUOUS^
ANALYTICAL METHOD _
AMBIENT TEMPERATURE.
OPERATOR
COHHENTS:
^\^ RUN-
GAS ^"^\
C02
02 (NET IS ACTUAL 02
READHIG MINUS ACTUAL
C02 READING)
CO (NET IS ACTUAL CO
READING &1NUS ACTUAL
02 READING)
^2 (NET IS 100 MINUS
ACTUAL CO READING)
A
ACTUAL
READING
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•
3
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• ( •
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44/100
• 32/100 ' -
• iZTTl
28/ioo
23/lCO
KOLECULAR WEIGHT OF
STACK GAS (Dr.Y BASIS)
r,ld, lb/!b--c!a
*
"
•
i
TOTAL
i
h-'
J>
EPA (Dai) 239
4/72
-------
DRY MOLECULAR WEIGHT DETERMINATION
.ANT "/* ^' ^^-v
27
PL
DATE
SAMPLING TIME '(24-hr CLOCK)
SAMPLING LOCATION
COKMEHTS:
/
3 £>
SAMPLE TYPE (BAG, INTEGRATED, CONTINUOUS).
ANALYTICAL METHOD <0xv^-
AKBIENT TEMPERATURE
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( 0 to
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AVERAGE
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VOLUME
AS-?'
//.7y .
.vq
• i '
MULTIPLIER
44/100
: 32/100
• 1 !
28/ioo
23/ico
MOLECULAR WEIGHT OF
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MJ, lb/!b-mcle
"
•
TOTAL
o
I—•
Ui
EPA (Our) 230
4/72
-------
D-l
SRL 1425 01 0474
APPENDIX D
STANDARD SAMPLING PROCEDURES
The sampling procedures used during the test are the same as
those published in Federal Register 36^ (247), Thursday, December 23, 1971,
The methods used were those numbered 1, 2, 3, 5, and 6.
The only departure from the method outlined was that the SO
was collected in bags and analyzed at the laboratory.
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(s) specified or recommends cali-
bration at shorter Intervals, in which
case such specifications or recommenda-
tions shall be followed. The applicable
method specified in the appendix of this
part shall be the reference method.
(c) Production rate and hours of op-
eration shall be recorded daily.
(d) The owner or operator of any sul-
furlc acid production unit subject to the
provisions of this subpart shall maintain
a flle 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 procedure's.
(a) The provisions of this section are
applicable to performance tests for deter-
mining emissions of acid mist and sulfur
dioxide from sulfuric acid production
units.
(b) All performance-tests shall be con-
ducted while the affected facility Is oper-
ating at or above the maximum acid
production rate at which such facility
will be operated and under such other
relevant conditions as the Administrator
shall specify based on representative per-
formance of the affected facility.
(c) Test methods set forth in the ap-
pendix to this part or equivalent methods
as approved by the.Administrator shall
be used as follows:
(1) For each repetition the acid mist
and SO, concentrations shall be deter-
mined by using Method 8 and traversing
according to Method 1. The minimum
sampling time shall be 2 hours, and mini-
mum sampling volume shall be 40 ft.1
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
Q8=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=acid mist and SO, concentrations In
Ib./f t." as determined in accordance with
paragraph (c)(l) of this section, cor-
rected to standard conditions, dry basis.
APPENDIX—TEST METHODS
METHOD 1 SAMPLE AND VELOCTTT TBAVEBSES
TOR STATIONARY SOUCCE3
1. Principle and Applicability.
1.1 Principle. A sampling site and the
number of traverse points are selected to aid
In the extraction of a representative sample.
1.2 Applicability. Thla method should
be applied only when specified by the test
procedures for determining compliance with,
the New Source Performance Standards. TJn-
lesa otherwise specified, this method Is not
Intended to apply to gas streams other than
thoso emitted directly to the atmosphere
without further processing.
2. Procedure.
2.1 Selection of a sampling site and mini-
mum number of traverse points.
2.1.1 Select a sampling site that Is at least
eight stack or duct diameters downstream
and two diameters upstream from any flow
disturbance such a8 a bend, expansion, con-
traction, or visible flame. For rectangular
cross section, determine an equivalent diam-
eter from the following equation:
equivalent diameter=2
'(length) (width) \
, length+width /
equation 1-1
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 0.87.
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.
2.3 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 Ti«.ble 1-1. The
traverse axes shall divide the stack croea
section Into equal parts.
g
0.5
1.0
NUMBER OF DUCT DIAMETERS UPSTREAM'
(DISTANCE A)
1.5 2.0
2.8
50
i 40
o
1 30
20
10
\
A
1
B
J
I
1
i
^DISTURBANCE
. SAMPLINO
'"SITE
DISTURBANCE
•FROM POINT OF ANY TYPE OF .
DISTURBANCE (BEND. EXPANSION, CONTRACTION. ETC.)
10
NUMBER OF DUCT DIAMETERS DOWNSTREAM*
(DISTANCE B)
Figure 1-1. Minimum number of traverse points.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
Table 1-1. Location of traverse points in circular stacks
(Percent of stack diameter from inside wall to traverse point)
Figure 1-2. Cross section of circular stac'k divided Into 12 equal
areas, showing location of traverse points at centroid of each area.
o
o
o
1
1
• 1 »
1
„..„, i
1
0 1 ^ O
J
1
r r 1
1
0 I 0
1
1
0
' 0
o
Figure 1-3. Cross section of rectangular stack divided Into 12 equal
areas, with traverse points at centroid 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
13
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
1Z
2.1
6.7
11.8
17.7
25.0
35.5
64.5
65.0
S2.3
83.2
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
93.2
•
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
93.4
18
1.4
4.4
7.5
10.9
14.6
18.8
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
15.5.
20.4
25.0
30.6
38.8
61.2
69.4
75.0
79.6
83.5
87.1
90.3
93.3
96.1
93.7
'
22
T.I
3.5
6.0
8.7
11.6
14.6
13.0
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
S3-. 9
24
1.1
3.2
5.5
7.9
10.5
13.2
16.1
19.4
23.0
27.2
32.3
3.9.3
60.2
67.7
72.8
77.0
30.6
83.9
S6.3
89.5
92.1
94.5
96.8
93.9
o
No. 247—Ft.
FEOERAL REGISTER, VOt. 36, NO. 347—THURSDAY, DECEMBER 23, J97I
-------
24884
RULES AND REGULATIONS
2.2.2 For rectangular stacks divide the
cross section Into as many equal rectangular
areas as traverse points, such that the ratio
of the length to the width of the elemental
areas Is between one and two. Locate the
traverse points at the centrold of each equal
area according to Figure 1-3.
3. References.
Determining Dust Concentration In a Gas
Stream, ASME Performance Test Code #27,
New Tork. 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
Paniculate Matter, In: 1971 Book of ASTM
Standards. Part 23, Philadelphia, Pa. 1971,
ASTM Designation D-2928-71.
METHOD 2 DETERMINATION OP STACK CAS
VELOCITY AND VOLUMETRIC PLOW RATE (TTPE
8 PTTOT TUBE)
1. Principle and.applicability.
1.1 Principle. Stack gas velocity Is deter-
mined from the gas density and from meas-
urement of the velocity head using a Type S
(Stauschelbe or reverse type) 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 S pitot tube ana
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 coefflclent
using equation 2-1.
. = Gp.,dW— equation 2-1
where:
Cp,e., = Pitot tube coefflclent of Type.S
pitot tube.
Cp,l(1 = Pltot tube coefflclent of standard
type pitot tube (if unknown, use
0.99).
Ap,u= Velocity head measured by stand-
ard type pitot tube.
Apmtr: Velocity head measured by Type S
pitot tube.
4.3 Compare the coefficients of the Type S
pitot tube determined first with one leg and
then the other pointed downstream. Use the
pitot tube only if the two coefficients differ by
no more than 0.01.
5. Calculations. —
Use equation 2-2 to calculate the stack gas
velocity.
PIPE COUPLINC
TUBING ADAPTER
Equation 2-2
where:
(VO.,,.=Stack gas velocity, feat (>er second (f.p.s.).
aroused.
Cp=Pltot tube coefficient, dimenslonless.
(T.).,,.=Average absolute stack gas temperature,
(VSp).,,.=Averago velocity head of stack gas, Inches
HtO (see Fig. 2-2).
P.= Absolute stack gas pressure, Inches Hg.
M.=MoIecular weight of stack gas (wet basis),
Ib./lb.-mole.
Md(l-B.o)+18B.«
Md=Dry molecular weight of stack gas (from
Method 3).
B.0=Proportlon by volume of water vapor ID
the gas stream (from Method 4).
Figure 2-2 shows a simple recording sheet
for velocity traverse data. Use the averages
in the last two columns of Figure 2-2 to de-
termine the average stack gas velocity from
Equation 2-2.
Use Equation 2-3 to calculate the stack
gas volumetric flow rate.
.=o600 (l-'
^Figure 2-1. Pilot tube-manometer assembly.
Equation 2-3
Where:
Q.=YoIumetrlc flow rate, dry basis, standard condi-
tions, ft.'/hr.
A = Cross-sectional area of stack, ft.'
T,ui= Absolute temperature at standard conditions,
630° R.
P«d= Absolute pressure at standard conditions, 29.91
Inches Hg.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
RULES AND REGULATIONS
24885
6. References.
Mark, L. 8., 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.Y., I960.
Shlgehara, B. -T., W. P. Todd, and W. 8.
Smith, Significance of Errors In Stack 8am-
PLAIMT_
DATE
RUN NO.
STACK DIAMETER, in.
BAROMETRIC. PRESSURE, in.
STATIC PRESSURE IN STACK |Pg), in. Hg._
OPERATORS
pllng Measurements. Paper presented at the
Annual Meeting of the Air Pollution Control
Asaoclatlon, St. Louis, Mo!, June 14—19, 1970.
Standard Method for Sampling Stacks for
Partloulate Matter, In: 1971 Book of ASTM
Standards, Part 33. Philadelphia, Pa., 1971,
ASTM Designation r>-292»-71.
Vennard, J. K., Elementary Sluid Mechan-
ics, John Wiley & Sons, Inc., New York, N.Y.,
1947.
SCHEMATIC OF STACK
CROSS SECTION
Traverse point
number
Velocity head,
in. H20
Stack Temperature
AVERAGE:
Flgyra 2-2. Velocity traverse data.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
i
-------
24886
RULES AND REGULATIONS
METHOD 3—GAS ANALYSIS FOE CAEBON DIOXIDE,
EXCESS AIB, AND DBT 1IOLECULAB WKI1HT
1. Principle and applicability.
1.1 Principle. An Integrated or grab gas
sample Is extracted from a sampHug point
and analyzed for Its components using an
Great analyzer.
1.2 Applicability. This method should be
applied only when specified by the toot pro-
cedures for determining rompllanco 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 eteel or Pyrex1
glass, equipped with a filter to remove panic-
ulate matter.
2.1.3 Pump—One-way squeeze bulb, or
equivalent, to transport gas sample to
analyzer.
»Trade name.
2.2 Integrated sample (Figure 3-2).
2.2.1 Probe—Stainless steel or Pyrex1
glass, equipped with a filter to remove por-
Uculate matter.
222 Air-cooled condenser or equivalent—
To remove any excess moisture.
2.2.3 Needle valve-cTo adjust flow rate.
2.2.4 Pump—Leak-free, diaphragm type,
or equivalent, to pull gas.
2.2..'< Rate meter—To measure a flow
range from 0 to 0.035 cfm.
2.2.6 Flexible bag—Tedlar,1 or equivalent,
with a capacity of 2 to 3 cu. ft. Leak test the
bag In the laboratory before using.
2.2.7 Pilot tube—Type S, or equivalent,
attached to the probe so that the sampling
flow rate can be regulated proportional to
the stack gas velocity when velocity Is vary-
ing with time or a sample traverse Is
conducted.
2.3 Analysis.
2.3.1 Orsat analyzer, or equivalent.
KtOBE
'FLEXIBLE TUBING
TO ANALYZER
TER(G
! FILTER (GLASS HOOl)
SQUEEZE BULB
Figure 3*1. Grab-sampling train.
RATE METER
AIR-COOLED CONDENSER
[PROBE
\
FILTER (GLASS ROOM
3. Procedure.
3.1 Grab sampling.
8.1.1 .Set up tho equipment as shown In
Figure 3-1, making sure all connections are
leak-free. Place tho probe in the stack at &
sampling point and purge the sampling line.
3.V.2 'Draw cample Into the analyser.
3.2 Integrated sampling.
3.2.1 Evacuate the" flexible bog. 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 CO,, O,, and CO con-
centrations as soon as possfble.'Make as many
passes as are necessary to give constant read-.
ings. If more than ten passes are necessary,
replace the absorbing solution.
3.3.2 For grab sampling, repeat the sam-
pling, and analysis until three consecutive
samples vary no more than 0.6 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% COr
4.2 Excess air. TJse Equation 3-1 to calcu-
late excess air. and average the runs. Report
the result to 'the nearest 0.1% excels air.
%EA =
X100
(%Oa)-O.S(%CQ)
0.264(% N,)-(% Oa)+0.5C% CO)
equation 3-1
where:
%EA= Percent excess air.
%O3=Percent oxygen by volume, dry basis.
%N,=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 tho runs. Report the result to the
nearest tenth.
QUICK DISCONNECT Md=o.44(%co3) +o.32(%oa)
RIGID CONTAINER
i Figure 3-2. Integrated gas -sampling train.
equation 3-2
•where:
Mj==Dry molecular weight, Ib./lb-mole,
%CO:f=Percent carbon dioxide by volume,
•dry basis.
%Oj==Percent oxygen by volume, dry
basis.
%N»-=Percent nitrogen by volume, dry
basis.
0.44=Molecular weight of carbon dloxld*
divided by 100.
0.3I*=Molecular weight of oxygen divided
by 100.
0.28=Molecu]ar weight of nitrogen and
CO divided by 100.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
6. 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 19G4.
Devorkln, Howard, et al., Air Pollution
Source Testing Manual, Air Pollution Con-
trol District, Los Angeles. Calif., November
1963.
METHOD 4 DZTEEMINATION OF MOISTUBE
IN STACK CASES
1. Principle anil applicability.
1.1 Principle. Moisture Is removed from
the gas stream, condensed, and determined
volume trtcally.
1.2 Applicability. This method Is appli-
cable for the determination of moisture In
stack gas only when specified by test pro-
cedures for determining compliance with New
Source Performance Standards. This method
does not apply when liquid droplets are pres-
ent In the gas stream' and the moisture Is
subsequently used In the determination of
stack gas molecular weight.
Other methods such as drying tubes, wet
bulb-dry bulb techniques, and volumetric
condensation techniques may be used.
2. Apparatus.
2.1 Probe—Stainless steel or Pyrex 2 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 psychrometrlc chart to obtain an ap-
proximation of the moisture percentage.
• Trada .name.
v.,=-
where:
. Vwc=Volume of water' vapor collected
(standard conditions), cu. ft.
Vi=Final volume of Implnger contents,
ml.
Vi=Initial volume of Implnger con-
tents, ml.
R=Ideal gas constant, 21.83 Inches
and equipped with a filter to remove partlcu-
late matter.
2.2 Implngers—Two midget Implngera.
each with 30 ml. capacity, or equivalent.
2.3 Ice bath container—To . condense
moisture In Implngers.
• 2.4 Silica gel tube (optional)—To protect
pump and dry gas meter.
. 2.5 Needlo 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
17» of the total sample volume.
2.8 Eotarheter—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 .Pilot 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 Implnger. Assemble the apparatus with-
out the probe as shown In Figure 4-1. Leak
check by plugging the Inlet to the first Im-
plnger and drawing a vacuum. Insure that
flow through the dry gas meter Is less than
1% of the sampling rate.
3.2 Connect the probe and sample at a
constant rate of 0.075 c.f.m. or at a rate pro-
portional to the stack gas velocity. Continue
sampling until the dry gas meter registers 1
cubic foot or until visible liquid droplets are
carried over from the first Implnger 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.
-=0.0474m^(V,-Vi)
equation 4-1
Hg—cu. ft./lb. mole-'R.
pn»o=:Density of water, 1 g./ml.
Ti to=Absolute temperature at standard
conditions, 530° B.
P. id=Absolute pressure at standard con-
ditions. 29.92 Inches Hg.
Mn:o=Molecular weight of water, 18 lb./
Ib.-mole.
HEATED PROB1
FILTER'(GLASS WOOL)
ROTAMETER
ICE BATH
LOCATION.
TEST
DATE
OPERATOR
PUMP
Figure 4-1. Moisture-sampling train.
COMMENTS
DRY GAS METER
BAROMETRIC PRESSURE
m
v»
fa
m
O
CLOCK TIME
GAS VOLUME THROUGH
METER. (Vm),
ft3
ROTAMETER SETTING
ft3/min_
METER TEMPERATURE,
•r
Figure 4-2. Field moisture determination.
FEDERAL REGISTER, VOL 36, NO. 247—THURSDAY, DECEMBER 23, 1971
OO
23
-------
2-1888
RULES AND REGULATIONS
4.3 Gas volume.
17 71
1/'/1
--
ln. HgV. T
equation 4-2
where:
Vm. =Dry gas voUme through meter at
standard conditions, cu. ft.
VM =Dry gas volume measured by meter,
cu. ft.
Pm = Barometric pressure at the dry gas
meter; inches Hg.
P^ n = Pressure at standard conditions, 29.93
inches Hg.
T.u=Absolute temperature at standard
conditions, 630* R.
Tm =Absolute temperature at meter ( *F+
460), 'R.
4.3 Moisture content.
V..
"V..+V.
"V..+V
b~+ (0.025)
equation 4-3
vhcre:
B»o=Proportloh by volume of water viapor
in the gas stream, dimenslonlesa.
V». =Volume of water vapor collected
(standard conditions), cu. ft.
Vm. =Dry gas volume through meter
(standard conditions), cu. ft.
Bwii=Approximate volumetric proportion
of water vapor In the gas stream
•i leaving the Implngers, 0.025.
6. References.
Air Pollution Engineering Manual, Danlel-
Bon, J. A. (ed.), US. 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 Gases,
Western Precipitation Division of Joy Manu-
facturing Co., Los Angeles, Calif., Bulletin
WP-€0, 1968.
METHOD 6—DETERMINATION or PARTICULATB
EMISSIONS FBOM STATIONARY SOURCES
1. Principle and applicability.
1.1 Principle. Partlculate matter Is with-
drawn ifiokinetlcally from the source and its
weight Is determined gravlmetrically after re-
moval of uncombined water.
1.2 Applicability. This method is applica-
ble for the determination of participate 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 portlculate sampling train used
by EPA (Figure 6-1) are described In APTD-
0581. Commercial models at this train are
available.
2.1.1 Nozzle—Stainless steel (316) wltn
sharp, tapered leading edge.
2.1.2 Probe—Pjrex' glass with a heating
system capable of maintaining a minimum
gas temperature of 250° P. at the exit end
during sampling to prevent condensation
from occurring. When length limitations
(groater 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 Pitot tube—Type S, or equivalent,
attached to probe to monitor stack gas
velocity.
2.1.4 Filter Holder—Pyrex' glass with
beating system capable of maintaining mini-
mum temperature of 225 • F.
2.1* Implngers / Condenser—Four impln-
gera connected in series with glass ball Joint
ntttnge. The first, third, and fourth Impln-
gers are of the Greenburg-Smith design,
nvdifled by replacing the tip with a %-lnch
ID glass tube extending to one-half inch
from the bottom of the flask. The second 1m-
ptnger is of the Greenburg-Smlth design
with the standard tip. A condenser may be
used in place of the implngers provided.that
the moisture content of the stack gas can
still bo determined.
2.1.6 Metering system—Vacuum gauge,
leak-free pump, thermometers capable of
measuring temperature to within 6* P., dry
gas meter with 2% accuracy, anU 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 Glass wash bottles—Two.
2.2.3 Glass sample storage containers.
' 2.2.4 Graduated cylinder—250 ml.
2.3 Analysis.
2.3.1 Glass weighing dishes.
2.3.2 Desiccator.
2.3.3 Analytical balance—To measure to
±0.1 mg.
2.3.4 Trip balance—300 g. capacity, to
measure to ±0.05 g.
3. Reagents.
3.1 Sampling.
3.1.1 Filters—Glass fiber. MSA 1106 BH>,
or equivalent, numbered for Identification
and prewelghed.
3.1.2 Silica gel—Indicating type, fr-18
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.
IWPINGER TRAIN OPTIONAL HAY BE REPLACED
BY AN EQUIVALENT CONDENSER
HEATED AREA FILTER HOLDER / THERMOMETER
REVERSE-TYPE
PITOT TUBE
IMPINGERS ICE BATH
BY-PASS.VALVE
CHECK
,,VALVE
..VACUUM
' LINE
THERMOMETERS'
VACUUM
V GAUGE
MAIN VALVE
DRY TEST METER
AIR-TIGHT
PUMP
Figure 5-1. particulate-sampling train.
3.3.2 Desiccant—Drierite,1 indicating.
4. Procedure.
4.1 Sampling
4.1.1 After selecting the sampling site and
the minimum number of sampling points,
determine the stack pressure, temperature,
moisture, and range of velocity head.
4.1.2 Preparation of collection train.
Weigh to the nearest gram approximately 200
g. of silica gel. Label a filter of proper diam-
eter, desiccate • for at least 24 hours and
weigh to the nearest 0.5 n:g. in .1 room where
the relative humidity Is less than 50T». Place
100 ml. of water In each of the first two
Implngers, leave the third implnger empty,
and place approximately 200 g. of preweighcd
silica gel in the fourth implnger. 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.fjn. 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 Implngers. Add
> Trade name.
"Trade name.
•Dry using Drlerite» at 70' F.±10° F.
more ;.ce during the run to keep the temper-
ature of the gases leaving the last Impinger
as lovr as possible and preferably at 70° F.,
or loss.. Temperatures above 70" F. may result
In damage to the dry gas meter from either
moisture condensation or excessive heat.
4.l.:t Participate 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-
dlttOMS 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 Isoklnetic conditions. Sample for at
least 5 minutes at each traverse point; sam-
pling time must be the same for each point.
Maintain isokinctlc sampling throughout the
sampling period. Nomographs are available
which aid In the rapid adjustment of the
sampling rate without other computations.
APTD-0576 details the procedure for using
these nomographs. Turn off the pump at the
conclusion of each run and record the final
readings. Remove the probe and nozzle from
the stack and handle in accordance with the
sample recovery process described in section
4.2.
FEDERAL REGISTER, VOl. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
RULES AND REGULATIONS
24889
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SCHEMATIC of swot CKKS section
MAVirctMeit
NUKCK
TOTAL
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If jl. I"- HJ.
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"• ».'•"'
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OURIT
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Ait.
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suncKK
TUffflUTUK.
•F
(EWEPJITOSE
orcu
LE«vs«
COflEfWrR Oft
UUT WDICtK.
•f
Tm — Average dry gas meter temperature,
"R. •
?,,„•= Barometric pressure at the orifice
meter. Inches Hg.
AH =• Average pressure drop across the
orifice meter, inches HaO.
13.6-= Specific gravity of mercury.
P,-,, —Absolute pressure at standard con-
ditions, 28.92 inches Hg.
6.3 Volume of water vapor.
equation 5-2
water vapor In the ga»
(standard conditions) .
flgm!-2.
4.3 Sample recovery. Exercise care In mov-
ing the collection train from the test site to
the sample recovery area to minimize the
losa 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 Im-
pingers, then discard. Place the samples In
containers as follows:
Container No. 1. Remove the niter from
Its holder, place In this container, and seal.
Container No. 2. Place loose partlculate
matter and acetone washings from all
sample-exposed surfaces prior to the filter
In this container and seal. Use a razor blade,
brush, or rubber policeman to lose adhering
particles.
Container No. 3. Transfer the silica gel
from the fourth Implnger to the original con-
tainer and seal. Use a rubber policeman as
an aid In removing silica gel from the
Implnger.
4.3 Analysis. Record the data required on
the example sheet shown In Figure 6-3.
Handle each sample container as follows:
Container No. 1. Transfer the niter and
any loose partlculate matter from the sample
container to a tared glass weighing dish,
desiccate, and dry to a constant weight. Re-
port results to the nearest 0.6 mg.
Container No. Z. 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.
6. 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).
0.2 Dry gas volume. Correct the sample
volume measured by the dry gas meter to
standard conditions (70° P., 29.92 inches Hg)
by using Equation 6-1.
where:
Vw.w= Volume °
sample
cu. ft.
V i. = Total volume of liquid collected In
impingers and silica gel (see Fig-
ure 6-3) , ml.
pato** Density of water, 1 gyml.
MH3o«= Molecular weight of water, 10 lb./
Ib.-mole.
B= Ideal gas constant, 21.83 Inches
Hg — cu. ft./lb.-mole-'R.
Titd= Absolute temperature at standard
conditions, 630* B.
P.,4= Absolute pressure at standard con-
ditions, 29.92 Inches Hg.
6.4 Moisture content.
where:
B,,
"witd
equation 5-3
Proportion by voluinoof wntor vapor In thc^s
stream, dluienslonk'ss.
Voliiine of water In the gas sample (standard
conditions), cu. ft.
^«,id=Volumo o( pas sample tlirongh the dry gas mcliT
(standard conditions), cu. It. •
6.6 Total partlculate weight. Determine
the total partlculate 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.cJT .
(17.71
\ in.
equation 5-1
where:
=• Volume of gas sample through the
dry gas meter (standard condi-
tions), cu-'ft.
• Volume of gas sample through the
dry gas meter (meter condi-
tions) , cu. ft.
= Absolute temperature at standard
conditions, 630* R.
mi«dy
equation 5-4
where:
(^Concentration of paniculate matter In stack
gas, gr./s.c,f., dry basis.
M»=Tota! amount of partlculate matter collected,
mg.
v".w=Volmne of gas sample through dry gas meter
(.Hindard conditions), cu. ft.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 197)
-------
24890
> RULES AND REGULATIONS
PLANT.
DATE
RUN NO.
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICIPATE COLLECTED,
mg
FINAL'WEIGHT
•"• — -^__. -*
^-^=~^ — J
TARE WEIGHT
:x
WEIGHT GAIN
FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME.
ml
1
SILICA GEL
WEIGHT,
9
'
g" ml
CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
INCREASE BY DENSITY OF WATER. (1 g. ml):
= VOLUME ».TER.m,
Figure5-3. Analytical data.
6.6.2 Concentration In Ib./cu. ft.
/ i J
_V453,600mg.
= 2.205X10-':
Mn
itd
where:
i equation 5-5
(^Concentration of partlculate matter In stack M"=T?ng amount °' Parllculatematter collected,
«3,600-Mi$b'.lb'/8'C'f'' ^ UaSl3' V0.ld=Volume of gas sample through dry gas meter
(standard conditions), cu. ft.
6.7 Isoklnetlc variation.
XlOO
.P.An
ev.P.An
where:
I=Pprcent of Isoklnctlc sampling.
Vic=»Total volume of liquid collected In imnlngers
and silica gel (See Klg. 6-3), ml.
PH)0=Donslty of water, 1 g./nu.
R=Ideal gas constant, 21.83 Inches Hg-cu. ft./lb.
molo-°R.
Mn,o=Molccular weight of vrater, IS Ib./lb.-n'-olo.
Vn, = Volume of gas sample through theory gas meter
(motor conditions), cu. ft.
To,=Absolute average dry gas meter temperature
(sec Figure *-2),°R.
Pbir=Brj-ometric pressure at sampling slto, Inches
Hg-
AII-=Avcraee pressure drop across tho orifice (see
Klg. 5-2), inches IIjO.
T,=Absoluto average stack gas temperature (see
Fig. 5-2), »K.
»=Total sampling time, mln.
V.=Stack gas velocity calculated by Method 2
Equation 2-2, ft./sec.
P.=.\bsolute stack gas pressure, Inches Tip.
An = Cross-sectlonal area of nozzle, sq. ft.
6.8 Acceptable results. The following
range sets the limit on acceptable Isoklnetlc
sampling results:
If 90% < I < 110%, the results are acceptable,
otherwise, reject the results and repeal.
the test.
7. Reference.
Addendum to Specifications for Incinerator
Testing at Federal Facilities, PHS,. NCAPC,
Dec. 6, 1967.
Martin, Robert M., Construction Details of
Isoklnetlc Source Sampling Equipment, En-
vironmental Protection Agency, APTI>-0581.
Rom, Jerome J., Maintenance, Calibration,
and Operation of Isoklnetlc Source Sam-
pling Equipment. Environmental Protection
Agency, APTD-0576.
Smith, W. S., R. T. Shlgehara, and W. F.
Todd, A Method of Interpreting Stack Sam-
pling Data, Paper presented at the 63d An-
nual Meeting of the Air Pollution Control
Association, St. Louis, Mo., June 14-19, 1970.
Smith, W. S., et al.. Stack Oas Sampling
Improved and Simplified with New Equip-
ment, APCA paper No. 67-119, 1967.
Specifications for Incinerator Testing at
Federal Facilities, PHS, NCAPC. 1967.
METHOD 6 DETERMINATION OP SULFUR DIOXIDE
EMISSIONS FROM STATIONARY SOURCES
1. Principle and applicability.
1.1 Principle. A gas sample Is extracted
from the sampling point In the stack. The
acid mist, Including sulfur trtoxide, Is sepa-
rated from the sulfur dioxide. The sulfur
dioxide fraction. Is measured by the barium-
thorln tltratlon method.
1.2 Applicability. This method Is appli-
cable for the determination of sulfur dioxide
emissions from stationary sources only when
specified by the test procedures for determin-
ing compliance with New Source Performance
Standards.
2. Apparatus.
2.1 Sampling. See Figure 6-1.
2.1.1 Probe—Pyrex » glass, approximately
5 to 6 mm. ID, with a heating system to
prevent condensation and a filtering medium
to remove paniculate matter Including sul-
f uric acid mist.
2.1.2 Midget bubbler—One, with glass
wool packed In top to prevent sulfurlc acid
mist carryover.
2.1.3 Class wool.
. 2.1.4 Midget implngers—Three.
2.1.5 Drying tube—Packed with 6 to 18
mesh indicating-type silica gel, or equivalent,
to dry the sample.
•2.1.6 Valve—Needle valve, or equivalent,
to adjust flow rate.
2.1.7 Pump—Leak-free, vacuum type.
2.1.8 Rate meter—Rotameter or equiva-
lent, to measure a 0-10 s.c.f.h. flow range.
2.1.9 Dry gas meter—Sufficiently accurate
to measure the sample volume within 1%.
2.1.10 Pitot tube—Type S, or equivalent.
Equation 5-6 * Trade names.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, J971
-------
necessary only If a nampl* traverse Is re-
quired, or If stack gas velocity varies with
time.
2-3 Sample recovery.
PROBE (END PACKED
WITH QUARTZ OR
PYREX WOOL;
TVPESPITOT
3.2.1 Glass wash bottles—Two.
22.3 Polyethylene storage bottles—To
store Unplnger samples.
2.3 Analysis.
SILICA GEL DRYING TUBE
MIDGET BUBBLER MIDGET IMPINGERS
DRY GAS METER ROT;
Figure 6-1. SOg sampling train.
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 stock and disconnect It
from the train. Drain the Ice bath and purge
the remaining part or the train by drawing
clean ambient air through the eystem for 15
minutes.
4.2 Sample recovery. Disconnect the 1m-
plngers after purging. Discard the contents
of the midget bubbler. Pour the contents of
the midget Implngers Into a polyethylene
shipment bottle. Rinse the three rrddyet Im-
plngers and the connecting tubes" with dis-
tilled water and add these washings to the
same storage container.
4.3 Sample analysis. Transfer the contents
of the storage container to a 50 ml. volu-
metric flaak. Dilute to the mark with de-
lonlzed, distilled water. Pipette a 10 ml.
aliquot of this solution Into a 126 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. Bun a blank with each series
of samples.
6. Calibration.
5.1 Use standard methods and equipment
8.3.1 Pipettes—Transfer type. 5 ml. and
10 ml. olzes (0.1 ml. divisions) and 26 ml.
size (0.2 ml. divisions).
2.3.2 Volumetric flasks—50 ml., 100 ml.,
and 1.000ml.
2.3.3 Burettes—B 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 dally.
3.2 Sample recovery.
3.2.1 Water—Delonlzed, distilled.
'3.2.2 Isopropanol, 80%.
3.3 Analysis.
3.3.1 Water—Delonlzed, distilled.
3.3.2 Isopropanol.
3.3.3 Thorln Indicator—l-(o-arsonophen-
ylazo)-2-naphthol-3,6-dlsulfonlc acid, dlso-
dlum salt (or equivalent). Dissolve 0.20 g. In
100 ml. distilled water.
3.3.4 Barium perchlorate (0.01 N)—Dis-
solve 1.05 g. of barium pcrchlorato
[Ba(ClO4),«3H3O] In 200 ml. distilled water
No. 247—Ft. II 3
and dilute to 1 liter with Isopropanol. Stand-
ardize with BUlfurlc acid. Barium chloride
may be used.
3.3.5 Sulfurlo acid standard (0.01 N) —
Purchase or standardize to ±0.0002 N
against 0.01N NaOH which has previously
been standardized' against potassium acid
phthalate (primary standard grade).
4. Procedure.
4.1 Sampling.
4.1.1 Preparation of collection train. Pour
15 ml. of 80% Isopropanol Into the midget
bubbler and 15 ml. of 3% hydrogen peroxide
Into each of the first two midget Implngers.
Lea,ve the final midget Implnger 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 Eg 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' F. or
less.
4.1.2 Sample collection. Adjust the sam-
ple flow rate proportional to the steck gas
which have been approved by too Adminis-
trator to calibrate the rotameter, pltot tube,
dry gas meter, and probe heater.
5.2 Standardize the barium perchlorata
against 25 ml. of standard pulfurlo 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.
°R /VmPb,A
17-71 in. Hg \T^r) equation 6-1
where: ,
Vm.ta= Volume of gas sample through the
dry gas meter (standard condi-
tions), cu. ft.
- V,,," Volume of gas sample through the
dry gas meter (meter condi-
tions), cu. ft.
Tita= Absolute temperature at standard
conditions, 030* R.
Tm=. Average dry gas moter temperature,
P6.,= Barometric pressure at the orifice
meter, Inches Hg.
P,,4~ Absolute pressure at standard con-
ditions, 29.92 inches Hg.
6.2 Sulfur dioxide concentration.
/ ib-lN
(7.05X10-^7-)
where:
Cso3= Concentration of sulfur dioxide
at standard conditions, dry
basis, Ib./cu. ft.
7.05 X10-'= 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.
Vt= Volume of barium perchlorate
tltrant used for the sample,
ml.
Vlb=> Volume of barium perchlorate
tltrant used for the blank, ml.
W= Normality of barium perchlorate
tltrant, g.-cq./l. .
V10,0 = Total solution volume of sulfur
dioxide, 50 ml.
V.= Volume of sample aliquot ti-
trated, ml.
Vm,,d«" Volume of gas sample through
the dry gas meter (standard
conditions), cu. ft., see Equa-
tion 6-1.
equation 6-2
7. References.
Atmospheric Emissions from Sullurlc Acid
Manufacturing Processes. U.S. DIIEW, PHS,
Division of Air Pollution, Public Health Serv-
ice Publication No. 999-AP-13, Cincinnati.
Ohio. 1965.
Corbett, P. F.. The Determination of SO,
and SO, In Flue Gases. Journal of the Insti-
tute of Fuel, 24:237-243, 1961.
Matty. R. E. aud E. K. Dlebl, Measuring
Flue-Gas SO, and SO,. Power 101:94-97, No-
vember, 1957.
Patton. W. F. and J. A. Brink, Jr., New
Equipment and Techniques for Sampling
Clicmlcal Process Gases. J. Air Pollution Con-
trol Association. 13, 162 (19G3).
METHOD 7—DETERMINATION OT NITROGEN OXTJDS
EMISSIONS FBOM STATIONARY BOI7ECE3
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
m
O
c
o
z
FEDERAL REGISTER, VOL. 35, NO. 217--TilUSJOAY, P:CE,Y.';2R 23, 1971
8
-------
24892
nitrous oxide, are measure colorlmetrlcally
using the phenoldlsulfonlc acid (PDS)
procedure.
1.2 Applicability. This method Is applica-
ble for the measurement of nitrogen oxides
from stationary sourc«8 only when specified
by the test procedures for determining com-
pliance with New Source Performance
Standards.
' 2. Apparatus.
2.1 Sampling. See Figure 7-1.
2.1.1 Probe—Pyrex1 glass, heated, with
filter to remove partlculate 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 25" to 125* F.
2.1.5 Vacuum line—Tubing capable of
withstanding a vacuum of 3 Inches Hg abso-
lute pressure, with "T" connection and T-bore
stopcock, or equivalent.
2.1.6 Pressure gauge—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.
2.1.8 Squeeze bulb—Oneway.
2.2 Sample recovery.
2.2.1 Pipette or dropper.
2.2.2 Glass storage containers—Cushioned
for shipping. .
;SQUEEZE BUUi
PROBE
- flASK VALVE'
FILTER
GROUND-GLASS SOCI
5 NO. 12/6
J-WAV STOPCOCK.-
T-BOffi. I. PtREX.
2-mmBORE.I-romOO
FlASK
.FLASK SHIELtX. ,\
GROUND
STANDARD TAPER.
| SLEEVE NO. 24/40
GROUND-GLASS
SOCKET, 5 NO. 12/S
PVREX
— -FOAM ENCASEMENT
\V I .• ^BOILING FLASK •
V - J-' 2- LITER. ROUND-BOTTOM. SHOOT NECK.
*^ ' KITH j SLEEVE NO. 24/40
Figure 7-1. Sampling train, Ijask valve, and Mask.
3.2.3 Glass wash bottle.
2.3 Analysis.
2.3.1 Steam bath.
2.3.2 Beakers or casseroles—250 ml., one
for each sample and standard (blank).
2.3.3 Volumetric pipettes—1, 2, and 10 ml.
•3.3.4 Transfer pipette—10 ml. with 0.1 ml.
divisions.
2.3.5 Volumetric flask—100 ml., one for
each sample, and 1,000 mi. for the standard
(blank).
2.3.6 Spectrophotomoter—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. Rcagenti..
• 3.1 Sampling.
3.1.1 Absorbing solution—Add 2.8 ml. of
concentrated H.SO, 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 Bodlum hydroxide (IN)—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 sulfurlc acid—15 to 18% by
weight free sulfur trloxlde.
3.3.2 Phenol—White solid reagent grade.
3.3.3 Sulfurlc acid—Concentrated reagent
grade.
3.3.4 Standard solution—Dissolve 0.5495 g.
potassium nitrate (KNO,) In distilled water
and dilute to 1 liter. For the working stand-
ard solution, dilute 10 ml. of the resulting
solution to 100 ml. with distilled water. One
ml. of the working' standard solution Is
equivalent to 25 #g. nitrogen dioxide.
3.3.5 Water—Delonlzed, distilled.
3.3.6 Phenol dlsulfonlo acid solution-
Dissolve 25 g. of pure white phenol In 160 ml.
concentrated sulfurlo acid on a steam bath.
Cool, add 76 ml. fuming sulfurlo add, and
beat at 100° O. for 2 hours. Store in a dark,
stoppered bottle.
4. Procedure.
4.1 Sampling.
4.1.1 Pipette 25 ml. of absorbing solution
Into ft 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 ffask pressure and temperature along
with the barometric pressure. Transfer the
flask contents to a container for shipment
or to a 250 ml. beaker for analysis. Rinse the
flask with two portions of > distilled water
(approximately 10 ml.) and add rinse water
to the sample. For a blank use 25 ml. of ab-
sorbing solution and the same volume of dis-
tilled water as used In rinsing the flask. Prior
to shipping-or analysis, add sodium hydrox-
ide (IN) 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 sulfurlc acid. Heat the solu-
tion on a steam bath for 3 minutes with oc-
casional stirring. Cool, add 20 ml. distilled
water, mix well by stirring, and add concen-
trated ammonium hydroxide dropwlse with
constant stirring until alkaline to litmus
paper. Transfer the solution to a 100 ml.
volumetric flask and wash the beaker three
times with 4 to 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 or each sample at 420 nm. using the
blank .tolutlon as a zero. Dilute the sample
Eind tha blank with a suitable amount of
distilled water If absorbance falls outside the
range of calibration.
B. Calibration.
6.1 Flask volume. Assemble the flask and
flask valve and fill with water to the stop-
cock. Measure the volume of water to ±10
ml. Number and record the volume on the
flask.
6.2 Spectre-photometer. Add 0.0 to 16.0 ml.
of standard solution to a series of beakers. To
each beaker add 29 ml. of absorbing solutlou
and add sodium hydroxide (IN) dropwlsa
until alkaline to litmus paper (about 35 to
35 drops). Follow the analysis procedure of
section 4.3 to collect enough data to draw a
calibration curve of concentration In fig. NOt
per sample versus absorbance.
6. Calculations.
6.1 Sample volume.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
RULES AND REGULATIONS
24893
V..=
TitJ(V(-V.)
-
where:
V.c = Sample volume at standard condi-
tions (dry basis), mi,
T,ld = Absolute temperature at standard
conditions, 630* R.
P,,,, = Pressure at standard conditions,
29.92 inches Hg.
Vt— Volume of flask and valve, ml.
V, —Volume of absorbing solution, 25 ml.
'-«=)•
;1 Ib. v
cu. ft.
1.6X10^,
where:
C—Concentration of NO, as NOa (dry
basis), lb./s.c.f.
m=Mass of NO, In gas sample, //g.
V,c = 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 Gaseous Combustion Products
(Phenoldlsulfonlc Acid Procedure), In: 1968
Book of ASTM Standards. Part 23, Philadel-
phia, Pa. 19C8, 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 SOTJT7HIC ACID
MIST AND SUUtm DIOXIDE EMISSIONS FBOM
STATIONARY SOURCES
1. Principle and applicability.
1.1 Principle. A gas sample Is extracted
from a sampling point In the stack and the
acid mist Including sulfur trloxlde te sepa-
rated from sulfur dioxide. Both fractions are
measured separately by the barlum-thorln
titratlon method.
1.2 Applicability. This method Is applica-
ble to determination of sulfurlc acid mist
(Including sulfur trloxlde) and sulfur diox-
ide from stationary sources only when spe-
cified by the test procedures for determining
P,-= Final absolute pressure of flask.
Inches Hg.
P,-= Initial absolute pressure of flask.
Inches Hg.
T,-= Final absolute temperature of Cask,
•R.
T, •= Initial absolute temperature of flask,
°R.
6.2 Sample concentration. Read ;ig. NOZ
for each sample from the plot of us- NOa
versus absorbance.
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 gloss with a heating
system to prevent visible condensation dur-
ing sampling.
2.1.3 Pltot tube—Type S, or equivalent,
attached to probe to monitor stack gas
velocity.
2.1.4 Filter holder—Pyrex > glass.
2.1.5 Impingers—Four as shown In Figure
8-1. The first and third are of the Greenburg-
Smlth design with standard tip. The second
and fourth are of the Greenburg-Smith de-
sign, modified by replacing the standard tip
with a '/i-lnch ID glass tube extending to
one-half Inch from the bottom of the im-
plnger flask. Similar collection systems,
which have been approved by the Adminis-
trator, may be used.
2.1.6 Metering system—Vacuum gauge,
leak-freo 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
PROBE
REVERSE-TYPE
PITOTTUBE
THERMOMETER
CHECK
VALVE
VACUUM
LINE
VACUUM
GAUGE
•AIR-TIGHT
PUMP
DRY TEST METER
Figure 8-1. Sulfurlc 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—250 ml.
2.3 Analysis.
2.3.1 Pipette—25 ml., 100ml.
2.3.2 Burette—50 ml. •
2.3.3 Erienmeyer flask—250ml.
2.3.4 Graduated cylindor—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 1106
BH. or equivalent, of a suitable size to fit
in the filter holder..
3.1.2 Silica gel—Indicating type, 6-16
mesh, dried at 175° C. (350° F.) fur 2 hours.
3.1.3 Water—Delonlzed, distilled.
3.1.4 Isopropanol, 80%—Mix 800 ml. of
isopropanol with 200 ml. of deiouized, dis-
tilled water.
3.1.5 Hydrogen peroxide, 3%—Dilute 100
ml. of 30% hydrogen peroxide to 1 liter with
delonlzed, distilled water.
3.1.6 Crushed Ice.
3.2 Sample recovery.
3.2.1 .Water—Delonlzed, distilled.
3.2.2 Isopropanol, 80%.
3.3 Analysis.
3.3.1 Water—Delonlzed, distilled.
3.3.2 Isopropanol.
3.3.3 Thorln Indicator—l-(o-arsonophen-
yla?.o)-2-naphthol-3, 6-disulfon!c acid, di-
sodlum salt (or equivalent). Dissolve 0.20 g.
In 100 ml. distilled water.
3.3.4 Barium perchlorate (0.01 AT)—Dis-
solve 1.95 g. of barium perchlorate [Ba
(CO.I..3 H^O] in 200 ml. distilled water anc!
dllute'to 1 liter with Isopropanol. Standardize
with sulfuric acid.
3.3.5 Sulfuric acid standard (0.01/V) —
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
Implngcr. 100 ml..of 37o hydrogen peroxide In
both the second and third Implngers. and
about 200 g. of silica gel In the fourth 1m-
pinger. Retain a portion of the reagents for
use as blank solutions. Assemble the train
without tho probe as shown in Figure 8-1
with tho 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
cJ.m. at a vivcuum of 15 Inches Hg Is ac-
ceptable. Attach the probe and turn on the
probe heating system. Adjust the probe
heater setting during sampling to prevent
any visible condensation. Place crushed ice
around the Implngers. Add more Ice during
the run to keep the temperature of the gases
leaving the last Impinger at 70' F. or less.
4.1.3 Train operation. For each run, re-
cord the data required on the example sheet
shown In Figure 8-2. Take readings at each
sampling point at least every 5 minutes and
when significant changes in stack conditions
necessitate additional adjustments In flow
rate. To begin sampling, position the nozzle
at the first traverse point with the tip point-
Ing directly into the gas stream. Start the
.pump and Immediately adjust the flow to
Isokinotlc conditions. Maintain Isoklnetic
sampling throughout the sampling period.
Nomographs are available which aid la the
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
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SRL 1425 01 0474
APPENDIX E
LABORATORY REPORT
SCOTT RESEARCH LABORATORIES, INC.
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SRL 1425 01 0474
APPENDIX E
LABORATORY REPORT
E.I ON-SITE HANDLING AND TRANSFER, PARTICULATE
After the completion of a test run, the probe and nozzle were
disconnected from the impinger train and all open ends sealed immediately
to avoid contamination. At the laboratory facility, the nozzle was
disconnected from the probe and, with the aid of a fine-bristled brush,
very carefully washed with acetone. 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. In some cases this was
performed at the test site in order to minimize the time required between
tests.
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 collected in a separate jar.
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 Teflon lines lids. The following designa-
tions were used for labeling the containers:
SCOTT RESEARCH LABORATORIES. INC.
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SRL 1425 01 0474
Container //I: 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 a single-pan analytical 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.
the weight reported is to the nearest 0.1 mg.
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, then oven
dried overnight. These were then desiccated for 24 hours and labeled
and tared. Once tared, the beakers were sealed with plastic film and
handled with tongs or laboratory wiping tissue.
The acetone washes were transferred to the tared beakers,
rinsing the jar thoroughly with acetone from a wash bottle to collect any
particulate adhering to the jar. The beakers were covered'with watch
glasses and placed in a fume hood to evaporate the acetone.
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.
The chloroform extracts were collected directly in a tared beaker prepared
SCOTT RESEARCH LABORATORIES, INC.
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SRL 1425 01 0474
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 with
distilled water in the separately funnel, the organic layer being returned
to the tared beaker for evaporation.
The water portion was transferred to additional tared beakers,
oven dried at 90°C, desiccated, and weighed. A summary of weight measurements
is shown in Tables E-l and E-2.
E.2.4 Blank Analysis
. The amount of acetone wash and water wash used in each test is
measured. An average volume of acetone and water is determined from these
measurements. Blank samples of acetone and water, equivalent to the average
volumes, are then evaporated, dessicated and weighed in the same manner as the
test samples. If the blanks indicate a positive value, this value is then
adjusted proportionately to the volume of each sample and subtracted from the
sample weight.
E.2.5 EPA Sample Number Identification Log
Table E-3 lists the EPA Sample Number Identifications for the
different runs and sampling locations.
E.3 GAS ANALYSES BY ORSAT METHOD
Two grab samples were analyzed by the Orsat method during the two day
test period. The Tedlar sample bags had a capacity of about 5 liters and were
equipped with Teflon sample tubes fitted with air-tight syringe caps. Prior to
sampling, each bag was flushed with pure, dry nitrogen and sealed with the
syrxnge cap.
The two sample bags (one inlet and one outlet) were returned to the
field laboratory where they were analyzed for CO, CO^, and 02 by the Orsat method.
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 bypass. Successive 100 ml. samples
were drawn into the sample burette and then passed through each of the
three absorbing solutions, viz, potassium hydroxide for C02, alkaline
pyrogallate for 02, and cuprous chloride for CO. Repetitive passes were
made through each absorbing solution until good duplication of results
SCOTT RESEARCH LABORATORIES, INC.
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n
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B
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n
TABLE E-l SUMMARY OF WEIGHT MEASUREMENTS
(INLET)
CO
N3
U1
Container 91
(Filter)
Container 92
(Acetone wash front half)
Container 03a
(Organic Extract)
Container #3b
(Water after extraction)
Container 05
(Acetone wash back half)
Run 1
Gross Tare Net Blank Final
(g) (g) (mg) (mg) (mg)
2.3076 0.9226 1385.0 0 1385..0
96.5828 95.9167 666.1 0 666.1
86.7592 86.7523 6.9 0 6.9
85.1956 85.1018 93.8 0 93.8
93.9451 93.9296 15.5 0 15.5
.Probe, Cyclone, Filter 2051.1
Total 2167.3
Run 2
Gross Tare Net Blank Final
(g) (g) (mg) (mg) (mg)
1.4255 0.4527 972.8 0 972.8
85.8734 85.5486 324.8 0 324.8
100.6702 100.6638 6.4 0 6.4
89.1946 89.1431 51.5 0 51.5
96.6057 96.6019 3.8 0 3.8
Probe, Cyclone, Filter 1297.6
Total 1359.3
Run 3
Gross Tare Net Blank Final
(g) (g) (mg) (mg) (ing)
2.0022 0.9323 1069.9 0 1069.9
88.9804 88.3019 678.5 0 678.5
88.4884 88.4826 5.8 0 5.8
87.1368 87.0658 71.0 0 71.0
81.6047 81.5961 8.6 0 8.6
Probe, Cyclone, Filter 1748.4
Total 1833.8
O
i— •
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in
' t— •
-P-
o ro
O Ui
H TABLE E-2 SUMMARY OF WEIGHT MEASUREMENTS o
58 . >-
5 . (OUTLET) o
0 ' **
B
r-
C3
o
SI
58
*-.
M
Ui
O
Container 01
(Filter)
Container 62
(Acetone wash front half)
Container #3a
(Organic Extract)
Container #3b
(Water after extraction)
Container 05
(Acetone wash back half)
Run 1
Gross Tare Net Blank Final
(g) (g) fag) (mg) (mg)
0.5588 0.4267 132.1 - 132.1
89.5360 89.4745 61.5 0 61.5
94.7729 94.7643 8.6 0 8.6
82.5572 82.5279 29.3 0 29.3
94.7717 94.7671 4.6 0 4.6
Probe Cyclone, Filter 193.6
Total 236.1
Run 2
Gross Tare Net Blank Final
(g) (g) (mg) (mg) (mg)
0.6137 0.4524 161.3 - 161.3
96.1004 96.0516 48.8 0 48.8
-
87.6316 87.6235 8.1 0 8.1
89.6068 89.5566 50.2 - 50.2
81.6025 81.6015 1.0 - 1.0
Probe, Cyclone, Filter 210.0
Total . 269.4
W
ON
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SRL 1425 01 0474
TABLE E-3 EPA SAMPLE NUMBER IDENTIFICATION LOG
Sample //
Run //
Location
Contents
S-74-002 437
S-74-002 438
S-74-002 439
S-74-002 440
S-74-002 441
S-74-002 442
S-74-002 443
S-74-002 444
S-74-002 445
S-74-002 446
S-74-002 447
S-74-002 448
S-74-002 449
S-74-002 450
S-74-002 451
S-74-002 452
S-74-002 453
S-74-002 454
S-74-002 455
S-74-002 456
S-74-002 457
S-74-002 458
S-74-002 459
S-74-002 460
S-74-002 461
S-74-002 462
S-74-002 463
S-74-002 464
S-74-002 465
S-74-002 466
S-74-002 467 .
S-74-002 468
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
-
-
1
1
2
2
3
3
Inlet
Inlet
Inlet
Inlet
Outlet
Outlet
Outlet
Outlet
Inlet
Inlet
Inlet
Inlet
Outlet
Outlet
Outlet
Outlet
Inlet
Inlet
Inlet
Inlet
Outlet
Outlet
Outlet
Outlet
Blank
Blank
Sinter
Machine
Baghouse
Sinter
Machine
Baghouse
Sinter
Machine
Baghouse
Acetone wash of
Filter
Impinger catch
Acetone wash of
Acetone wash of
Filter
Impinger catch
Acetone wash of
Acetone wash of
Filter
Impinger catch
Acetone wash of
Acetone wash of
Filter
Impinger catch
Acetone wash of
Acetone wash of
Filter
Impinger catch
Acetone wash of
Acetone wash of
Filter
Impinger catch
Acetone wash of
Acetone blank
Water blank
Sinter feed
Baghouse dust
Sinter feed
Baghouse dust
Sinter feed
Baghouse dust
front
& H20 wash of
back half
front half
& H20 wash of
back half
front
& H20 wash of
back half
front half
& 1^0 wash of
back half
front half
& H20 wash of
back half
front half
& H20 wash of
back
back half
back half
back half
back half
back half
back half
SCOTT RESEARCH LABORATORIES. INC.
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SRL 1425 01 0474
occurred. At least three 100 ml. samples were analyzed from each Tedlar
sample bag. The data recorded for each Orsat analysis is included as
Table E-4.
E.4 SULFUR OXIDES ANALYSES
Bag samples for SO,, and SO ' were connected to a glass train
consisting of one midget bubbler followed by three midget impingers.
Fifteen milliliters of 80% isopropanol was placed in the midget bubbler, and
fifteen milliliters of 3% hydrogen peroxide into each of the first two
midget impingers. The third midget impinger was left dry.
A plug of glass wool was placed between the midget bubbler and
the first impinger to prevent carry-over of sulfuric acid mist into the
SO- impinger.
The samples were then transferred to the glass train using a
small vacuum pump. After removal of the bags, clean ambient air was
used to purge the system.
The SO and SO samples were analyzed by the Thorin titration
procedure.
The SO, bubblers were rinsed with a small amount of 80% isopropanol
and diluted to 20 ml.
The two SO„ impinger contents were combined, the impingers
rinsed with distilled water and diluted to 60 milliliters on the inlet
sample and 55 ml. on the outlet sample.
The entire 20 ml. from the midget bubbler and the glass wool
plug were transferred to a 125 ml. Erlenmeyer flask. Twenty milliliters
of 80% isopropanol and four drops of Thorin were added and the sample
titrated with a previously standardized solution of 0.01 N barium chloride.
Suitable aliquots from the S0_ sample were pipeted to 125 ml.
Erlenmeyer flasks. Anhydrous isopropanol was added to total 40 ml., and
the titration performed as for the SO .
A solution blank was titrated'with the samples; Tables E-5 and
E-6 list the titration data.
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SRL 1425 01 0474
TABLE E-4 GAS ANALYSIS DATA FROM ORSAT METHOD
Sample
Designation
Inlet
Component
co.
2
°0
2
CO
Analysis
Number
1
2
3
i
2
3
1
2
3
Burette Volume
Initial
100.0
100.0
100.0
98.0
98.0
98.0
80.0
79.7
80.2
Final
98.0
98.0
98.0
80.0
79.7
80.2
79.9
79.6
80.0
(ml.)
Difference
2.0
2.0
2.0
18.0
18.3
17.8
0.1
0.1
0.2
Outlet
°2
CO
1
2
3
1
2
3
1
2
3
100.0 .
100.0
100.0
99.6
99.4
99.3
81.0
80.5
80.5
96.6
99.4
99.3
81.0
80.5
80.5
80.7
80.4
80.1
0.4
0.6
0.7
18.6
18.9
18.8
0.3
0.1
0.4
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SRL 1425 01 0474
Sample
Location
Inlet
Outlet
TABLE E-5 SULFUR DIOXIDE ANALYSES DATA
Total
Volume (ml.)
60
55
Sample Titrant
Aliquot (ml.) Volume (ml.)
30
35
43.3
6.7
Sample
Normality
14.43x10
-3
1.91x10
-3
TABLE E-6 SULFUR TRIOXIDE ANALYSES DATA
Sample
Location
Inlet
Outlet
Total
Volume (ml.)
20
20
Sample
Aliquot (ml.)
20
20
Titrant
Volume (ml.)
0.1
0.3
Sample
Normality
5.0xlO~5
1.5xlO~4
SCOTT RESEARCH LABORATORIES. INC.
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SRL 1425 01 0474
The normality of each of the sample solutions was calculated
by using the following formula:
V x N
N = L „ X
s V
s
where: V = Volume of titrant (ml.)
N + Normality of titrant (0.01)
V = Volume of sample aliquot (ml.)
S
From this information the milligrams of SO per sample were calcualted
using the formula:
mg SO = V x N x meq. wt. SO,
t. Q S £
where: V = Sample dilution volume (ml.)
N = Normality of sample solution
S
meq. wt SO = 32
The amount of SO., expressed in milligrams as a result of the above calcu-
lation, may be converted to ppm by the formula shown in Appendix B.
SCOTT RESEARCH LABORATORIES, INC.
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SRL 1425 01 0474
APPENDIX F
TEST LOG
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SRL 1425 01 0474
APPENDIX F
TEST LOG
January 5, 1974
Scott crew arrived at the plant office at 1330; picked up Doug
Bell, the EPA representative; and proceeded to the sampling site. The
scaffolding was complete at the outlet, but the new sampling port had
not been installed. The inlet scaffolding was not complete, and the
ports had not been installed. The scaffolding contractor estimated
completion by the following morning.
Set-up was started but the failure of the 40' umbilical required
returning to Scott's Plumsteadville laboratory for a new umbilical.
January 6, 1974
Set-up was continued while scaffolding contractor finished work.
Preliminary traverses started at 1100. First tests started about 1350.
Excessive loading was encountered at the inlet location. Tests were
completed at about 1630.
Second test series was started at 1806. The inlet time was
reduced from two hour to one hour because of the high loading encountered
previously. This test was completed at about 1930. The outlet test was
completed at 1952.
January 7, 1974
The third series of tests was started at 1009 and the inlet
was completed at 1147. The outlet: was run with a defective impinger and
did not produce usable results.
Following the third series of tests, the equipment was immediately
dismantled, and the crew returned to Scott's Plumsteadville laboratory.
SCOTT RESEARCH LABORATORIES, INC.
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SRL 1425 01 0474
APPENDIX G
PROJECT PARTICIPANTS AND TITLES
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SRL 1425 01 0474
The following individuals participated in the activity at
Ferro-Alloy Sinter Plant-East Plant Baghouse of New Jersey Zinc Company
in Palmerton, Pennsylvania.
Douglas Bell
Charles Darvin
Thomas Ward
H. William Blakeslee
Renton B. Bethmann
G. Hulings Darby
Margaret Husic
Fred Lucrezi
William Prugh
Joseph Y. Wilson
EPA Project Coordinator
EPA
EPA
SRL Department Manager
SRL Field Technician
SRL Project Manager
SRL Laboratory Technician
SRL Field Technician
SRL Field Technician
SRL Field Team Supervisor
SCOTT RESEARCH LABORATORIES. INC.
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