COAL PREPARATION PLANT EMISSION TESTS
TEST NO. 1281-15
EASTERN ASSOCIATES COAL COMPANY
Keystone, West Virginia
PREPARED FOR
ENVIRONMENTAL PROTECTION AGENCY
Research Triangle Park
North Carolina 27711
Contract No 68-02-0233
SCOTT RESEARCH LABORATORIES, INC.
PLUMSTEADVILLE. PENNSYLVANIA 18949
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Test No. 1281-15
Eastern Associates Coal Company
Keystone, West Virginia, Norman R. Troxel
SCOTT RESEARCH LABORATORIES, INC.
Plumsteadville, Pennsylvania 18949
68-02-0233
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SRL 1281 15 0372
TABLE OF CONTENTS
1.0 INTRODUCTION
2.0 SUMMARY OF RESULTS
3.0 PROCESS' DESCRIPTION AND OPERATION
4.0 LOCATION OF SAMPLING POINTS
5.0 SAMPLING AND ANALYTICAL PROCEDURES
APPENDIX A SUMMARY OF PARTI.CULATE MATTER
AND SAMPLE CALCULATION
APPENDIX B RAW DATA SHEETS
APPENDIX C STANDARD SAMPLING PROCEDURES
APPENDIX D LABORATORY REPORT
APPENDIX E TEST LOG
APPENDIX F PROJECT PARTICIPANTS AND TITLES
Page
1-1
2-1
3-1
4-1
5-1
A-l
B-l
C-l
D-l
E-l
F-l
SCOTT RESEARCH LABORATORIES. INC.
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1-1
SRL 1281 15 0372
1.0 INTRODUCTION
Source sampling tests were performed at the Keystone, West
Virginia plant of Eastern Associated Coal Company on February 23 and
24, 1972. The company operates a coal preparation operation at this
site. In order to control the emissions to the atmosphere from this
operation, the exhaust gases pass through a Fangborn Baghouse collector
before entering the atmosphere.
It was the purpose of the test program to determine the
quantity of particulate matter being emitted to the atmosphere from the
collector. Triplicate tests were performed, running one test the first
day and two tests the next day. Figure 1 shows the location of the
sampling points.
SCOTT RESEARCH LABORATORIES, INC
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FIGURE 1
LOCATION OF SAMPLING POINTS
90
PI
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til Eirl
TRMH
L.
PLAN
1
I
.STACK
a A rat"
y
6LOUER
L.1CT
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o
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.. STACK.
. * ? '
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n^-. _„_„...'.' .._..ii t/^i...
I
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SECTION ON A A
V
s
A
r
»
1
S£
SECTION ON 6-6
FROM BA& HOUSE
ASSOCIATED COAL Co.
.ASTERN /ASSOCIATED
. Ul. \A.
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2-1
SRL 1281 15 0373
2.0 SUMMARY OF RESULTS
A summary of test results is presented in Table 1. Table 2
presents a summary of the particulate weights. All of the particulate
results are included in Appendix A and the raw data sheets are included
as Appendix B.
In observing Table 2 it is seen that there is no weight included
for Container 5 during Run 1. This was due to the fact that it was
discovered that the hydrocarbon stopcock grease used was attacked by
acetone. An acceptable type of stopcock grease was obtained and used
for the remaining two runs.
SCOTT RESEARCH LABORATORIES. INC.
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SRL 1281 15 0372
2-2
TABLE 1
SUMMARY OF.TEST RESULTS
Run Number:
Sample Gas Vol., scf
Moisture, %
Stack Gas Temp., °F
Stack Gas Vel., fpm
Stack Gas Vol., SCFM
Particulate Collected
Probe, cyclone, filter, mg.
Total, mg.
Particulate Concentration
Probe, cyclone, filter, gr/scf
Total, gr/scf
Particulate Emissions
Probe, cyclone, filter, Ib/hr.
Total, Ib/hr.
55.70
0.886
63
2230
25,918
39.3
54.5
0.011
0.015
2.41
3.35
53.71
0.988
65
2079
23,902
6.2 .
39.5
0.002
0.012
0.36
2.54
54.74
1.072
65
2172
24,902
9.5
25.8
0.003
0.007
0.57
1.56
SCOTT RESEARCH LABORATORIES, INC
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2-3
SRL 1281 15 0372
TABLE 2
PARTICULATE WEIGHTS SUMMARY
Run Number: 1 2 3
Container 1, mg. 0.5 0.0 0.0
Container 2, mg. 38.8 6.2 9.5
Container 3a, mg. 3.9 0.0** 1.0
Container 3b, mg. 11.3 0.0** 0.0**
Container 5, mg. * 37.0 15.5
Probe, cyclone, filter, mg. 39.3 6.2 9.5
Total, mg. 54.5 39.5 25.8
* No sample taken
** Blank was actually higher than sample value.
SCOTT RESEARCH LABORATORIES, INC
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3-1
SRL 1281 15 0372
3.0 PROCESS DESCRIPTION AND OPERATION
The Keystone Preparation Plant of Eastern Associated Coal
cleans No. 3 Pocahantas coal for metallurgical use by both wet and dry
methods. Minus 3/8 in. coal is processed through air tables with the
middlings recombined with plus 3/8 in. raw coal for wet processing.
Six R & S Super Airflo tables are used at approximately 30,000 cfm air
flow, 40 tons/hr. coal being cleaned per table.
Six Pangborn baghouses clean exhaust air, using 110 bags per
baghouse. Dynel bags are currently used in five baghouses. Cotton bags
were formerly used, but are gradually being phased out. The unit
tested had dynel bags. The bags are cleaned by shakers activated by
manual control at 2-3 hour intervals. There was no manual shaking of
the bags during any of the test runs.
The only process variables monitored were the coal moisture
content to the tables and the table feeder arm speed. The former was
measured with a probe developed by Consolidation Coal Company which
operates on a flow resistance principle. Assuming the charts were
calibrated properly, the moisture content of raw coal feed varied
from 3.2 percent to 6.5 percent during the tests. Table feed had been
set so that the six tables were fed coal at identical rates.
Loadout of cleaned coal was effected at the same rate as
production during the tests. This indicated a cleaned coal rate of
38 tons/hr. per table.
SCOTT RESEARCH LABORATORIES, INC.
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TCST i>ATfc.- 23-24 Ft-
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PROCESSING DIAGRAM
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SRL 1281 15 0372
4.0 LOCATION OF SAMPLING POINTS
From the baghouse collector the exhaust gases were emitted to
the atmosphere through a 42 in. by 42 in. stack. The sample ports were
all located on one side of the stack as shown in Figure 1. There were
three ports which were located at the distances shown in Figures 1 and 2,
These ports were located approximately 6 feet downstream from a fan and
approximately 6 to 12 inches upstream from the outlet of the stack (the
tope of the stack being inclined rather than flat).
Figure 2 shows the exact location of each sample point in the
cross section. Six points were sampled in each port giving a total of
eighteen points for the test. The three ports were labeled A, B, and C
starting at the east side of the stack and moving to the right. The
traverse points were numbered from 1 to 6 starting with 1 being nearest
to the port. The distance from the port to the first point was 3*5 in.
while the distances between the remaining points were each 7 in.
The testing was conducted from the roof of the building.
There was no requirement for any special scaffolding or platforms.
SCOTT RESEARCH LABORATORIES, INC
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FIGURE 2
j*Kt
W
8
90
So
n
ao
n
5:
DO
g
§
2
3
0
STACK
POINTS
N
EXACT LOCATION OF EACH SAMPLE POINT
EASTERN ASSOCIATE CO/\L Co. , KEYSTOMH, U1. VA.
^ +z'
; tf
.^ . y" > j -^ . . . 14? . -± < . \4~ - . >J . 7 >-
1 1 1
6— f- 6-- — 6 •--•
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1
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5-1
SRL 1281 15 0372
5.0 SAMPLING AND ANALYTICAL PROCEDURES
The sampling procedure used was the same as that specified by
Method 5 - "Determination of Particulate Emissions From Stationary
Sources" and published in the Federal Register, Volume 36, No. 247,
Thursday, December, 1971. This method is attached as Appendix E. In
addition, the impinger catch was analyzed.
Briefly, the method consists of withdrawing a sample iso-
kinetically from the stack through a heated glass probe into a filter
and impinger train. The sample volume is measured with a dry gas meter
and isokinetic conditions maintained by monitoring the stack gas velocity
with an "S" type pitot tube.
After testing, the train was thoroughly washed including the
probe. The washings were evaporated, dried and weighed along with the
filter in order to come up with a total weight of particulate matter
collected.
The stack gas velocity and flow rate was measured using
Method 2 - "Determination of Stack Gas Velocity and Volumetric Flow
Rate (Type S Pitot Tube)", and published in the Federal Register.
Using both the weight of sample collected and the flow rate determined,
a total particulate emission rate was calculated.
SCOTT RESEARCH LABORATORIES, INC.
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A-l
SRL 1281 15 0372
APPENDIX A
SUMMARY OF PARTICULATE MATTER
AND SAMPLE CALCULATION
SCOTT RESEARCH LABORATORIES, INC
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A-2
OF
SOl.'KCE TtSTll.'C CALCULAUO;; FORKS
Test. No. /
—/-
No. RIMIS 3
Name of Finn £OL £
Location of Plant ;
Type of Plant
A S 2 a C-X.cjU.-J '
Sampling ? o i n t Location s -^Q
<^^s
Pollutants Sampled ("aTft^'ci.. L-"tg.
Time of Pr.rticulate Test:
-Run No. I Date.
Run No. £ " Date_
Run No. 3 Date
gjj.s.ovu.
JO. \/
..a •
. _ __ ^
• 3
Begin //
Begin
tnd
/7
PART1CULATE EMISSION DATA
Run No.
p bc'iromstric pressure, "Hcj Absolute
p orifice pressure drop, "H?0
V - vo'Tuins of dry gas sans plod 0 meter
1 conditions, ft. 3
T Avorcc;.j CjcS Meter Temperature, °F
V VoUirnG of Dry Gas Sampled & Stcnderci
std. UdMuitionc/ft.3
V Total H..O collected, ml., Impi rigors
w & Silical Gel.
V_( " Volume 'of Water Vapor Collected
'o^s ft. 3 i? St.* no <">>•<•.! Cofidi tioi'i?*
/
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' * 70 F, 29.92" liy.
-------
A-3
Fi'ISSiO;; iiAVA (co:n:'d)
Hun !.'0. ....
£M - X-f'bisUirc i:: ••''.:: str-ok o^.s by voluiT.e
"M, - Mole fraction of dry CMS
:* C02 ^)
'* °2 <^)
% n2 ^)
f-i N , - rioVec'jVar weight of dry stacl: gas
M H - Molecular weight of stack gas
<^.Ps - Velocity Me-od of stack gas, In. HO
~T - Stack Temperature, °F
Upsx(V460)
j b b
P - Stack Pressure, "Hg. .Absolute
o
V - Stack Velocity 0 stack conditions, fpn1.
A - Stack Area, in.
Z>
Q - Stack Gas Volume (? A
s Standard Conditions. SCR'1.
T. - Net Time of Test, niin.
\f
D ^.- Sampling Nozzle Dic^ot.er, in.
n
**
%l ' - Percent isokinctic
m.r - ParticulstG - probe, cyclone
1 and filter, mg.
ni - Parti cul atn - total, ing.
\f
C - Participate •- probe, cyclone.
an and. filter, gr/SCF
C - Particulate.' - total, gr/SCF
so • '
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3 gr/cf « stsck conditions ^.o/&3a#)/?
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-1'-" f.-id f-i I •;.:;% }:.-/;•;:'.
C - P?.rtir;'.-lote - t;'t?.l, lb/!ir.
g EA - % Exfc-r.r> air f
s ;••:,•:[.! 1 ing point
/ K J3
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-------
A-5
PAI'-TICULAiE CALCULATE 0;-.'$
1. Voliwo of dry
l!(j, ft.3 '
samr-lc1;.! si siand-ivd conditions - 70°F, 29.92''--
n, 8
1T6"
-
2-. Vo.luiiie of water- vapor at 70°F :& 29.92" Ikj, Ft.
V = O.C47'1 X V. = Ft.
•-.gas--
3. X moisture -in stack gas
M = V ' + V
4. Mole fraction of dry gas
TOO - ffl
^ o,B8>(?
5. Average molecular weight of dry stack gas
.HHd - (scoz x
-------
A-6
0
7. Stack velocity (• ftnc.!: conditions, •{];:(
- 4350 X/-P x (V * < 60 ).-'•, -Trr-n
^/ S v S ;j / X h \>!
r
= fprn
;S vpluiii'a (? standard conditions, SCFH
Q B
(Ts + 160)
9. Per cent isokinetic
1032 X (T -i- /i60) X V
in.
V$XTtXPs XMdX (
XI2.6 X
10. Par.ticulGte - probe, cyclone, ft filter, gr/SCF
Car, ss°-01M'>fr :
Vstd
-------
'artki'UI'j total,
-------
'/. c ••:>.::•;•• •: ir ..rl f ;•• :;;'i 'iiv; p.'
A-8
TOO X % 0.,
0.266 X % N,, - % 02
-------
B-l
SRL 1281 15 0372
APPENDIX B
RAW DATA SHEETS
SCOTT RESEARCH LABORATORIES, INC.
-------
1 ' -
-A. /
Run
>ate
Sampling Train (Downstairs)
Sample | Time
Point j
Vol.
Pitot Tube
Press
Vac.
Total
Stack i Cal. Orifice
Temp. KAH in. HaO) I °F
0F.
Draft
(Ps in. HaO
Vac.
in. HR.
73
7.
: 7
.J-l,
,
tr
V
r
,3
CO
33
O
t
,£7
r
f
Probe Tip Dia. inches
X CV ")
Form 001
6/26/70
-------
Run
Sheet
Date
•jLYV'/J>U Sampling Train (Downstairs)
Sample
Point
.,- 1
5
if
y
Time
i
Vol.
(H3)
•^ ^ «^ j
S3 •••- ; f *
3^:
3r.g
;•>--
>A>
3*S>*
Pitot Tube »
Press
•^
7
y.
3
>>9
•
Vac.
Total
(£P in. H20)
), 1
,g
,r
/// ^
•JT"
»7"Z^
i
Stack i
Temp .
$f
. • • -^
'
/^^y
^ l.^-'
-><3
Cal. Orifice
|(AH in. HaO)
<-^
r
r &7
>;'(?
•" t" '"
//2,
op
/^r
//f
/, .'!
;/r
/ ; ->
/2.o
4
,- ^
//^
1 •• r'
' • ^
/ / ^ —
Draft
(Ps in. HaO
• ^<^
.- A."'
/ ••- {''
Vac.
in. Eg.
5
1
•'
r
Silica Gel I'umber J_
Correction
v *?
Filter Wt»t. * / , XC77 C?
^robe Tip Dia. inches
Form 001
6/26/70
-------
Run
Sheet
Date
1; S >
Sampling Train (Downstairs)
Sample j Time
Point I
Vol.
(H3)
Pitot Tube
Press
Vac.
Total
I
Stack ! Cal. Orifice
(&P in. HaO) I Temp. KAH in. HaO)
OF
Draft
(Ps in. H20
Vac.
in. Eg.
,73
Tr
7(9
&
,04,
.I/
70
t/O
80
&
5"
6
,0 (f
2_
7 W.2
fou
/(TO
f(fO
I o-o
rO(
7
//c;
Silica Gel I-'umber
Correction
. 7
Filter W<»t. 5»"2—
Probe Tip Dia. inches f_
»:-:
i
-•$$!
;. ?iiKa
^
Form 001
6/26/70
-------
Run
Sheet
Date
Sampling Train (Downstairs)
Sample | Time
Point 1
Vol.
(H3)
Pitot Tube
Press
Vac.
Total
in. H20)
Stack ! Cal. Orifice
Temp. KAH in. HaO)
Ti
OF
Draft
(Ps in. HaO
Vac
in.
(
Jj-L
Y
r
5T
, ?- -7
to
Ln
Silica Gel I'umber 2~_
Correction
'• /
Filter Wt»t. o
"J 7
''robe Tip Dia. inches
Form 001
6/26/70
-------
Run ^
1
«o O S •* *\ /**
3o£/;^2 £
Sample
Point
A~ '
-z
i
f
.6
'
^
I
Time
^7
,1
,
Vol.
(H3)
37/,
3fr,
xt.t
Vifc
W*
^3,3
* ' rv V "* ^ »
Total
(AP in. HaO)
,7T<
^/^
^r-
"°7
,/r
,^-/
iST?
,/7
/or
,0.^
'^i9
••^7
Stack i
Temp.
'' 6-$~
6 ^
r ^
t*~~
6 -T"
i? *
C -T
e.5^
^vf"
^'T
tf
b^
I-'unber ^ -b ' 2» / o.
, *. ^
^actftr / i P ^
Cal. Orifice
^AH in. H20)
/r3
t^3
J
fLJ.
,*?
,4f
., 1 "^
,^> 1-
JO f
,/7
,_^r
,«?^"
Ti
Op
*o
<*r
^r
fr
9T-
/6-0
^T
//r
x,r
//• -P
'^r
/,s-
Filter W^t. ?
T2
^o
fo
10
30
1 ^
/**
"0
ffO
1/0
/;/->
MO
Date " ' ^- ' ^-^
Draft
(Ps in. H20
/ 3 - :
.3
/a1?
^ ^
/O f
i ^ /
(
/ *~:-^
~^' "^
/O^
•Qb
•/ J
,^>
, Vac.
in. He.
3
z.
•o
6
c?
I
o
t>
•' ::^
^
<^)
2,.
t-^3 ,i.?7<7
w
ON
''robe Tip Dia. inches • 1 rTO
Form 001
6/26/70
s
*•» / Vi -
-------
Run
Sheet
Date
Sampling Train (Downstairs)
Sample j Time
Point I
Pitot Tube
Press
Vac.
Total
UP in. H20)
Stack i Cal. Orifice
Temp.
(AH in. H20)
T2
OF
Draft
(Ps in. H20
Vac.
in. HK.
C (
•Z-.
3
r
ttf
\\r
: 3-
3
/v-
w
Silica Gel I'umber
Correction
S
Fitter West. <» -^
,G> ~:
V
^robe Tip Dia. inches ,i ^
Form 001
6/26/70
-------
B-8
W A T E R V 0 L U It E
Rim Ko. / DAT'Ji
BulMoi # 1 /£>/?. Silica Gal No, / Wgt. fc JT/jf..#
t 2 /Q 0
t 3 Bubbler // 4 S •? <* • ^
Wat ei Added (-) 2~M? Gror;? Wgi.. (••) ,^//,
Net/.. -^ cc
'(A) ^
Het(A) °
Total KaLor
Form R & D 109
-------
B-9
W A T E R VOLUME
Run Ko. j DATE
/"<« 2
Bubbler // 1 ({TO ">"•« Silica Gal Ko. t>2> Wgt.
>-^
3 >^ Bubbler * A
Grccs
Water Added (-) _ .^Z__" ________ Grose Wgt. (-)
Het(A) c2 \AA cc Net(B) g
Het(A) ^.0
Total Water //^ '3
cc
Form R & D 109
-------
B-10
VI A T E R V 0 L U M E
Run No, 2>
DATE
^7
Bubblcr // 1
VX
Silica Gel Ko. __ Wgt. g
Bubbler // 4
Gross
W&.LC.V Added (-) __
Gros& V'Bfc' (-
cc
g
Het
(A)
Total Uatei1
cc
Fonc. R & D 109
-------
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 file of all measurements required by
this subpart. Appropriate measurements
shall be reduced to the units of the ap-
plicable standard daily and summarized
monthly. The record of any such meas-
urement and summary shall be retained
for at least 2 years following the date
of such measurements and summaries.
§ 60.85 Test methods and procedures.
(a) The provisions of this section are
applicable to performance tests for deter-
mining emissions of acid mist and sulfur
dioxide from sulfuric acid production
units.
(b) All performance tests shall be con-
ducted while the affected facility is oper-
ating at or above the maximum acid
production rate at which such facility
will be operated and under such other
relevant conditions as the Administrator
shall specify based on representative per-
formance of the affected facility.
(c) Test methods set forth in the ap-
pendix to this part or equivalent methods
as approved by the .Administrator shall
be used as follows:
(1) For each repetition the acid mist
and 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.'
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 lb:/hr. by the acid produced. The
emission rate shall be determined by
the equation, lb./hr.<=QsXc, where
Qa=volumetric flow rate of the effluent
in ft.'/hr. at standard conditions, dry
basis as determined in accordance with
paragraph (c) (2) of this section, and
c=acid mist and SO, concentrations in
lb./ft.8 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 VELOCITY TRAVERSES
FOR STATIONARY SOURCES
1. Principle and Applicability.
1.1 Principle. A sampling site and the
number of traverse points are selected to aid
in the extraction of a representative sample.
1.2 Applicability. This method should
be applied only when specified by the test
procedures for determining compliance with
the New Source Performance Standards. Un-
less otherwise specified, this method Is not
Intended to apply to gas streams other than
those emitted directly to the atmosphere
without further processing.
2. Procedure.
2.1 Selection of a sampling site and mini-
mum number of traverse points.
2.1.1 Select a sampling site that Is at least
eight stack or duct diameters downstream
and two diameters upstream from any flow
disturbance such as a bend, expansion, con-
traction, or visible flame. For rectangular
cross section, determine an equivalent diam-
eter from the following equation:
2.1.2 When the above sampling site
criteria can be met, the minimum number
of traverse points Is twelve (12).
2.1.3 Some sampling situations render the
above sampling site criteria Impractical.
When this Is the case, choose a convenient
sampling location and use Figure 1-1 to de-
termine the minimum number of traverse
points. Under no conditions should a sam-
pling point be selected within 1 Inch of the
stack wall. To obtain the number of traverse
points for stacks or ducts with a diameter
less than 2 feet, multiply the number of
points obtained from Figure 1-1 by 0.67.
2.1.4 To use Figure 1-1 first measure the
distance from the chosen sampling location
to the nearest upstream and downstream dis-
turbances. Determine the corresponding
number of traverse points for each distance
from Figure 1-1. Select the higher of the
two numbers of traverse points, or a greater
value, such that for circular stacks the num-
ber Is a multiple of 4, and for rectangular
stacks the number follows the criteria of
section 2.2.2.
2.2 Cross-sectional layout and location of
traverse points.
2.2.1 For circular stacks locate the tra-
verse points on at least two diameters ac-
cording to Figure 1-2 and Table 1-1. The
traverse axes shall divide the stack cross
section Into equal parts.
8
CO
NUMBER OF DUCT DIAMETERS UPSTREAM'
(DISTANCE A)
FROM POINT OF ANY TYPE OF
DISTURBANCE (BEND. EXPANSION, CONTRACTION. ETC.)
equivalent diameter=2l
/(length) (width)\
\ length+width /
equation 1-1
NUMBER OF DUCT DIAMETERS DOWNSTREAM*
(DISTANCE B)
Figure 1-1. Minimum number o! traverse points.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 73, 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
1
0
• •••__•• M
o
1
1
» 1 »
, 1
r— - ,
i
0 | ~ 0
1
, r 1
1
0 | 0
o
o
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
18
19
20
21
22
23
24
Number of traverse points on a diameter
Z
14.6
85.4
4
6.7
25.0
75.0
93.3
6
4.4
14.7
29.5
70.5
85.3
95.6
8
3.3
10.5
19.4
32.3
67.7
80.6
89.5
96.7
10
2.5
8.2
14.6
22.6
34.2
65.8
77.4
85.4
91.8
97.5
12
2.1
6.7
11.8
17.7
25.0
35.5
64.5
65.0
82.3
88.2
93.3
97.9
14
1.8
5.7
9.9
14.6
20.1
26.9
36.6
63.4
73.1
79.9
85.4
90.1
94.3
98.2
16
T.6
4.9
8.5
12.5
16.9
22.0
28.3
37.5
62.5
71.7'
78.0
83.1
87.5
91.5
95.1
98.4
18
1.4
4.4
7.5
10.9
14.6
18.8
23.6
29.6
38.2
61.8
70.4
76.4
81.2
85.4
89.1
92.5
95.6
93.6
20
1.3
3.9
6.7
9.7
12.9
16.5
20.4
25.0
30.6
38.8
61.2
69.4
75.0
79.6
83.5
87.1
90.3
93.3
96.1
98.7
22
J.I
3.5
6.0
8.7
11.6
14.6
18.0
21.8
26.1
31. 5
39.3
60.7
68.5
73.9
78.2
82.0
85.4
83.4
91.3
94.0
96.5
9S-.9
24
1.1
3.2
5.5
7.9
10.5
13.2
16.1
19.4
23.0
27.2
32.3
3.9.8
60.2
67.7
72.8
77.0
80.6
83.9
86.8
89.5
92.1
94.5
96.8
98.9
m
v*
1
o
I
o
No. 247—Pt. H 3
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
24884
RULES AND REGULATIONS
2.2.2 For rectangular stacks divide the
cross section Into as many equal rectangular
areas as traverse points, such that the ratio
of the length to the width of the elemental
areas is between one and two. Locate the
traverse points at the centroid of each equal
area according to Figure 1-3.
3. References.
Determining Dust Concentration in a Gas
Stream, ASME Performance Test Code #27,
New York, N.Y., 1957.
Devorkin, Howard, et al., Air Pollution
Source Testing Manual, Air Pollution Control
District, Los Angeles, Calif. November 1963.
Methods for Determination of Velocity,
Volume, Dust and Mist Content of Gases,
Western Precipitation Division of Joy Manu-
facturing Co., Los Angeles, Calif. Bulletin
WP-50, 1968.
Standard Method for Sampling Stacks for
Paniculate Matter, In: 1971 Book of ASTM
Standards, Part 23, Philadelphia, Pa. 1971,
ASTM Designation D-2928-71.
METHOD 2 DETERMINATION OF STACK OAS
VELOCITY AND VOLUMETRIC PLOW BATE (TYPE
S 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) pltot tube.
1.2 Applicability. This method should be
applied only when specified by the test pro-
cedures for determining compliance with the
New Source Performance Standards.
2. Apparatus.
2.1 Pttot tube—Type 8 (Figure 2-1), or
equivalent, with a coefficient within ±5%
over the working range.
2.2 Differential pressure gauge—Inclined
manometer, or equivalent, to measure velo-
city head to within 10% of the minimum
value.
2.3 Temperature gauge—Thermocouple or
equivalent attached to the pltot tube to
measure stack temperature to within 1.6% 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 Pilot tube—Standard type, to cali-
brate Type S pltot 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 L
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 pltot tube, measure
the velocity head at some point In a flowing
gas stream with both a Type 8 pltot tube and
a standard type pltot 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 pltot tube coefficient
using equation 2-1.
equation 2-1
where:
c"telt — Pltot tube coefficient of Type S
pltot tube.
Cp,,a=Pltot tube coefficient of standard
type pltot tube (If unknown, use
0.99).
Ap.tdzr Velocity head measured by stand-
ard type pltot tube.
Apt..t = Velocity head measured by Type S
pltot 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
pltot 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
^Figure 2-1. Pitot tube-manometer assembly.
Equation 2-2
where:
(V.)oTi.=Stack gas velocity, feet per second (f.p.s.).
Ib.
Ub. mole-°R>
when these units
Cp=Pltot tube coefficient, dlmenslonless.
(T.).,,.=Average absolute stack gas temperature,
°H.
(V3p).,,.=Average velocity head of stack gas, Inches
H,0 (see Fig. 2-2).
Pi= Absolute stack gas pressure, Inches Hg.
M.=Molecular weight of stack gas (wet basis),
Ib./lb.-mole.
Md(l-B.o)+18B,0
Md=Dry molecular weight of stack gas (from
Methods).
B.0= Proportion by volume of water vapor In
the gas stream (from Method 4).
Figure 2-2 shows a sample recording sheet
for velocity traverse data. Use the averages
In the last two columns of Figure 2-2 to de-
termine the average stack gas velocity from
Equation 2-2.
Use Equation 2-3 to calculate the stack
gas volumetric flow rate.
Q.=3600 (l-
itd
Equation 2-3
There:
Q,= Volume trie flow rate, dry basis, standard condi-
tions, ft.'/hr.
A=» Cross-sectional area of stack; ft.1
Tni=Absolute temperature at standard conditions,
830° H.
P.id~Absolutrj pressure at standard conditions, 29.98
inches Hg.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
RULES AND REGULATIONS
24885
6. References.
Mark, L. 8., Mechanical Engineers' Hand-
book, McGraw-Hill Book Ckx, Inc. New York,
N.T., 1951.
Perry, J. H., Chemical Engineers' Hand-
book, McGraw-Hill Book Co., Inc., New York,
N.Y., 1960.
Shlgehara, B. .T., W. P. Todd, and W. S.
Smith, Significance of Errors In Stack Sam-
PLANT_
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
Association, St. Louis, Mo., June 14-19, 1970.
Standard Method for Sampling Stacks for
Partlculate Matter, In: 1971 Book of ASTM
Standards, Part 23, Philadelphia, Pa., 1971,
ASTM Designation D-2928-71.
Vennard, J. K., Elementary Fluid Mechan-
ics, John Wiley & Sons, Inc., New York, N.Y.,
1947.
SCHEMATIC OF STACK
CROSS SECTION
Traverse point
number
Velocity head,
in. H20
Stack Temperature
AVERAGE:
Figure 2-2. Velocity traverse data.
FEDERAL REGISTER, VOL; 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
24888
RULES AND REGULATIONS
4.3 das volume.
*Is"
-
. Hg Tn equation 4-2
•where:
Vint =Dry gas volume through meter At
standard conditions, cu. ft.
VM =Dry gas volume measured by meter,
en. ft.
Pm = Barometric pressure at the dry gas
meter. Inches Hg.
P.td=Pressure at standard conditions, 29.93
inches Hg.
T.t,i= Absolute temperature at standard
conditions, 530* R.
Tm = Absolute temperature at meter ( • P +
460), ••&.
4.3 Moisture content.
V..
-+B.
Vw.+V.
-+(0.025)
equation 4-3
where:
B wo=Proportion by volume of water vapor
txx the gas stream., dlmenslonless.
Vwi = Volume of water vapor collected
(standard conditions), cu. ft.
• Vm. =Dry gas volume through meter
(standard conditions), cu. ft.
Bvn=Approximate volumetric proportion
of water vapor In the gas stream
leaving the Implngers, 0.025.
5. References.
Air Pollution Engineering Manual, Daniel-
eon, J. A. (ed.), VS. DHEW, PHS, National
Center for Air Pollution Control, Cincinnati,
Ohio, PHS Publication No. 999-AP-40, 1967.
Devorkin, Howard, et al., Air Pollution
Source Testing Manual, Air Pollution Con-
trol District, Los Angeles, Calif., November
1963.
Methods for Determination of Velocity,
Volume, Dust and Mist Content of Gases,
Western Precipitation Division of Joy Manu-
facturing Co., Los Angeles, Calif., Bulletin
WP-60, 1968.
METHOD 6—DETERMINATION or PABTTCULATE
EMISSIONS FROM STATIONARY SOURCES
1. Principle and applicability.
1.1 Principle. Partlculate matter is with-
drawn Isokinetioally from the source and its
weight is determined gravimetrically after re-
moval of uncomtolned water.
1.2 Applicability. This method Is applica-
ble for the determination of partlculate emis-
sions from stationary sources only when
specified by the test procedures for determin-
ing compliance with New Source Perform-
ance Standards.
2. Apparatus.
2.1 Sampling train. The design specifica-
tions of the partlculate sampling train used
by EPA (Figure 6-1) are described In APTD-
0581. Commercial models of this train are
available.
2.1.1 Nozzle—Stainless steel (316) with
sharp, tapered leading edge.
2.1.2 Probe—Pyrex1 glass with a heating
system capable of maintaining a minimum
gas temperature of 250' F. at the exit end
during sampling to prevent condensation
from occurring. When length limitations
(greater than about 8 ft.) are encountered at
temperatures less than 600* F., Incoloy 825 ',
or equivalent, may be used. Probes for sam-
pling gas streams at temperatures in excess
or 600* F. must have been approved by the
Administrator.
2.1.3 Pltot tube—Type S, or equivalent,
attached to probe to monitor stack gas
velocity.
3.1.4 Filter Holder—Pyrex1 glass with
heating system capable of maintaining mini-
mum temperature of 225* F.
2.1.5 Implngers / Condenser—Four impin- •
gers connected in series with glass ball Joint
fittings. The first, third, and fourth Impln-
gers are of the Greenburg-Smlth design,
modified by replacing the tip with a %-lnch
ID glass tube extending to one-half inch
from the bottom of the flask. The second tm-
plnger is of the Greeaburg-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 be determined.
2.1.6 Metering system—Vacuum gauge,
leak-free pump, thermometers capable of
measuring temperature to within 6* F., dry
gas meter with 2% accuracy, and related
equipment, or equivalent, as required to
maintain an isoklnetlc sampling rate and to
determine sample volume.
2.1.7 Barometer—To measure atmospheric
pressure to ±0.1 inches Hg.
2.2 Sample recovery.
2.2.1 Probe brush—At least as long as
probe.
2.2.2 Glass wash bottles—Two.
2.2.3 Glass sample storage containers.
2.2.4 Graduated cylinder—250 ml.
2.3 Analysis.
2.3.1 Glass weighing dishes.
2.3.2 Desiccator.
2.3.3 Analytical balance—To measure to
±0.1 mg.
2.3.4 Trip balance—300 g. capacity, to
measure to ±0.05 g.
3. Reagents.
3.1 Sampling.
3.1.1 Filters—Glass fiber, MSA 1106 BH».
or equivalent, numbered for Identification
and prewelghed.
3.1.2 Silica gel—Indicating type, 6-16
mesh, dried at 175° C. (350* F.) for 2 hours.
3.1.3 Water.
3.1.4 Crushed ice.
3.2 Sample recovery.
3.2.1 Acetone—Reagent grade.
3.3 Analysis.
3.3.1 Water.
IMPINGER TRAIN OPTIONAL. MAY BE REPLACED
BY AN EQUIVALENT CONDENSER
PROBE
REVERSE-TYPE
PITOT TUBE
HEATED AREA FILTER HOLDER / THERMOMETER CHECK
^VALVE
..VACUUM
LINE
IMPINGERS ICE BATH
BY-PASS.VALVE
THERMOMETERS'
VACUUM
V GAUGE
MAIN VALVE
DRV TEST METER
AIR-TIGHT
PUMP
Figure 5-1. particulate-sampling train.
3.3.2 Deslccant—Drlerlte,1 Indicating.
4. Procedure.
4.1 Sampling
4.1.1 After selecting the sampling site and
the minimum number of sampling .points,
determine the. stack pressure, temperature,
moisture, and range of velocity head.
4.1.2 Preparation of collection train.
Weigh to the nearest gram approximately 200
g. of silica gel. Label a filter of proper diam-
eter, desiccate' for at least 24 hours and
weigh to the nearest 0.5 mg. In a room where
the relative humidity is less than 50%. Place
100 ml. of water in each of the first two
Implngers, leave the third impinger empty,
and place approximately 200 g. of preweighed
silica gel in the fourth Impinger. Set up the
train without the probe as in Figure 5-1.
Leak check the sampling train at the sam-
pling site by plugging up the Inlet to the fil-
ter holder and pulling a 15 In. Hg vacuum. A
leakage rate not in excess of 0.02 c.f.m. at a
vacuum of 15 in. Hg is acceptable. Attach
the probe and adjust the heater to provide a
gas temperature oT about 250° F. at the probe
outlet. Turn on the filter heating system.
Place crushed Ice around the Implngers. Add
> Trade name.
1 Trade name.
"Dry using Driertte1 at 70° F.±10" F.
more ice during the run to keep the temper-
ature of the gases leaving the last Impinger
as low as possible and preferably at 70° F..
or less. Temperatures above 70° F. may result
in damage to the dry gas meter from either
moisture condensation or excessive heat.
4.1.3 Partlculate train operation. For each
run, record the data required on the example
sheet shown In Figure 5-2. Take readings at
each sampling point, at least every 5 minutes,
and when significant changes in stack con-
ditions necessitate additional adjustments
in flow rate. To begin .sampling, position the
nozzle at the first traverse point with the
tip pointing directly into the gas stream.
Immediately start the pump and adjust the
now to isokiiietic conditions. Sample for at
least 5 minutes at each traverse point; sam-
pling time must be the same for each point.
Maintain isolUnetlc 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
thesa 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
njujr_
LOCATION.
OPERATOR
DATE___
HUN NO.
UETER'Kn N0._
«ETERAH.__
AMBIENT TEMPERATURE.
trazat oourm. ta.
fKXt HEATER SETTING.
SCHEMATIC OF ITAC« CROSS SEaKH
HW VERSE POIW
NUU8EK
TOTAL
SAWIINO
TIME
M.lflta.
AVERAGE
STATIC
PRESSURE
|PSI. hi. Hg.
STAC!
TEMPEMTUC
.*P
VElOCtn
HEAD
I»PSI.
•
pBESsun
OtfFEBEHTIAL
ACROSS
OR1FICI
•ETEH '
UH).
ln-MjO
OASSAMFU
VOLUME
fM,
OAS SAMPLE TEMPERATUII
AT DRY GAS METER
WIST
IT«tol.«P
AX.
OUTLET
(T. J.V
lot.
Avg.
SAMPLE KH
TEMPERATURE.
•F
TEHPERATUIIt
OF GAS
LEAvne
COHOERSER OR
LAST BPOICER.
•f
Tm=Average dry gas meter temperature,
"R.
Pb.P=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, 26.02 Inches Hg.
6.3 Volume of water vapor.
f\im 5-2. Paniculate llgld dala.
4.2 Sample recovery. Exercise care In mov-
ing the collection train from the test site to
the sample recovery area to minimize the
loss of collected sample or the gain of
extraneous partlculate matter. Set aside a
portion of the acetone used in the sample
recovery as a blank for analysis. Measure the
volume of water from the first three Im-
plngers, then discard. Place the samples in
containers as follows:
Container No. 1. Remove the filter from
Its holder, place In this container, and seal.
Container No. 2. Place loose 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 Impinger 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 filter and
any loose partlculate matter from the sample
container to a tared glass weighing dish,
desiccate, and dry to a constant weight. Re-
port results to the nearest 0.6 mg.
Container No. 2. Transfer the acetone
washings to a tared beaker and evaporate to
dryness at ambient temperature and pres-
sure. Desiccate and dry to a constant weight.
Report results to the nearest 0.5 mg.
Container No. 3. Weigh the spent silica gel
and report to the nearest gram.
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 6-3).
6.2 Dry gas volume. Correct the sample
volume measured by the dry gas meter to
standard conditions (70° F., 29.92 Inches Hg)
by using Equation 6-1.
P"'t+i^6)
-
°R
equation 5-2
where:
V».td = Volume of water vapor in the gas
sample (standard conditions),
cu. ft.
Vi,=Total volume of liquid collected In
implngers and silica gel (see Fig-
ure 6-3), ml.
pa,o=Density of water, 1 g./mL
Maao=Molecular weight of water, 18 lb./
Ib.-mole.
R=Ideal gas constant, 21.83 Inches
Hg—cu. ft./lb.-mole-°R.
T,ta=Absolute temperature at standard
conditions, 630* R.
P,,4=Absolute pressure at standard con-
ditions, 29.92 Inches Hg.
6.4 Moisture content.
T> Vw.tJ
"•td~l~ *»«td
equation 5-3
where:
B,o
v*iid
in.
I>+£\
\-^-/
equation 5—1
where:
Vmgl
Volume of gas sample through the
dry gas meter (standard condi-
tions), cu.'ft.
Vm = Volume of gas sample through Che
dry gas meter (meter condi-
tions) , cu. ft.
T,ta=Absolute temperature at standard
conditions, 630* R.
Proportion by volume of wator vapor In the g:.s
stream, dimenslonless.
Volume of water In the gas sample (standard
conditions), cu. ft.
^"•w Volume of gas sample through the dry pas mot ur
(standard conditions), cu. ft.
6.6 Total partlculate weight. Determine
the total partlculate catch from the sum of
the weights on the analysis data sheet
(Figure 6-3) .
6.6 Concentration.
6.6.1 Concentration In gr./s.cJ.
equation 5-4
There:
c',= Concentration of partlculate matter In stack
gas, gr./s.o-f., dry basis.
M0=Total amount of partlculate matter collected,
mg.
V™,td= Volume of gas sample through dry gas meter
(standard conditions), cu. ft.
FEDERAL REGISTER, VOL. 36, NO. 247—THURSDAY, DECEMBER 23, 1971
-------
24890
RULES AND REGULATIONS
PLANT.
DATE
RUN N0._
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICULATE COLLECTED,
mg
FINAL WEIGHT
X
TARE WEIGHT
:XL
WEIGHT GAIN
FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME.
ml
SILICA GEL
WEIGHT.
9
9* ml
CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
INCREASE BY DENSITY OF WATER. (1 g. ml):
= VOLUME WATER, m.
Figure5-3. Analytical data.
6.6.2 Concentration in Ib./cu. ft.
/ 1 to^\M
_\453,600mgJM°
c. = -
= 2.205X10-"
Mn
v
Vlnitd
where:
equation 5-5
^Concentration of partlculate matter In stack M°=Tmg! am°Unt °'partlculate matter collected,
Iry basis. Vmitd=Volume of gas sample through dry gas meter
(standard conditions), cu. ft.
6.7 Isokinetic variation.
V..(PH,0)R
v/ , ^
T° V "+13.
9V.P.A0
X100
SV.P.A.
where:
I=Percent of Isoklnetlc sampling.
Vic=TotaI volume of liquid collected In tmplngers
and silica gel (See Fig. 6-3), ml.
PH]O=Density of water, 1 g./ml.
R=Ideal gas constant, 21.83 Inches Hg-cu. ft./lb.
mole-°R.
Mn,o=Molecular weight of water, 18 Ib./lb.-mole.
V0=Volume of gas sample through the dry gas meter
(meter conditions), cu. ft.
To,=Absolute average dry gas meter temperature
(see Figure &-2),°R.
Pi>.,=Bnrometric pressure at sampling site, inches
Hg.
AH=Average pressure drop across the orifice (see
Fig. 6-2), inches HjO.
T.=Absolute average stack gas temperature (see
Fig. 6-2), °R.
6=Total sampling time, mln.
V.=Stack gas velocity calculated by Method 2,
Equation 2-2, ft.&ec.
P,=Absolute stack gas pressure, Inches Hg.
AD=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 repeat.
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, APTD-0581.
Rom, Jerome J., Maintenance, Calibration,
and Operation of Isoklnetlc Source Sam-
pling Equipment. Environmental Protection
Agency, APTD-0576.
Smith, W. 8.. R. T. Shlgehara, and W. P.
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 14r-19, 1970.
Smith, W. S., et al., Stack Qas 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 trtoxlde, is sepa-
rated from the sulfur dioxide. The sulfur
dioxide fraction Is measured by the barium-
thorin titration 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—Pyrex1 glass, approximately
5 to 6 mm. ID, with a heating system to
prevent condensation and a filtering medium
to remove partlculate matter Including sul-
furlc acid mist.
2.1.2 Midget bubbler—One, with glass
wool packed in top to prevent sulfurlc acid
rnist carryover.
2.1.3 Glass wool.
2.1.4 Midget Impingers—Three.
2.1.5 Drying tube—Packed with 6 to 16
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 Pltot tube—Type 8, or equivalent,
Equation 5-6 1 Trade names.
FEDERAL REGISTER, VOL 36, NO. 247—THURSDAY, DECEMBER 23, 1971
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SRL 1281 15 0372
APPENDIX C
STANDARD SAMPLING PROCEDURES
The sampling procedures used during the test are the same
as those published in the Federal Register, Volume 36, Number 24,
Thursday, December 23, 1971. These methods are as follows (Methods
1, 2, 5). Additionally, the impinger catch was analyzed for
particulate content.
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APPENDIX D
LABORATORY REPORT
1. On Site Handling and Transfer
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 any possible contamination. At the laboratory facility, the
nozzle was disconnected from the probe and very carefully washed with
acetone, using a fine bristled brush. All acetone washings were collected
in a clean glass jar, the jar itself being placed on a large piece of
clean aluminum foil. The probe was then washed with acetone, using a
long-handled brush. The brush was rotated slowly and pushed through the
probe while a continuous stream of acetone was run through it. The brush
was also carefully cleaned and all washings collected in the glass jar.
The probe was finally eye-ball checked for transfer efficiency.
The impinger train was Initially wiped clean on the outside
and all glassware connectors, including the filter, removed carefully
and all exposed surfaces wiped clean. All the connectors were placed
on a piece of aluminum foil, ready for washing. The first three impingers
were then analyzed for water collection by transferring the water through
the outlet port into a graduated cylinder and noting the volume. The
impingers were not dismantled and all transfers and washings were performed
through the inlet and outlet ports. All of the glassware in the back half
of the filter, up to the fourth impinger was then carefully washed with
distilled water and the washings collected. This was followed by an
acetone wash which was again collected in a separate jar.
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Acetone washings from the glassware in the front half of the
filter were collected in the same jar as the probe and nozzle wash.
The filter was carefully removed from the holder and placed in a plastic
dish which was then sealed with tape. Silica gel in the fourth impinger
was weighed in a previously tared glass jar using a triple-beam balance.
All acetone jars had aluminum lined lids., or aluminum foil
was used before screwing on the lids. The following designations were
used for labeling the containers:
Container //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
2. Laboratory Handling and Analysis
a. Filter Transfer
Clean plastic dishes were desiccated for 24 hours, labeled and
tared on an electronic balance. The filter containers were unsealed
and desiccated for 24 hours before carefully transferring the filters
to the tared dishes using a fine pair of tweezers. Care was taken to
place a piece of aluminum foil under the transfer operation. A "static-
master" brush was used to brush any fine particles adhering to the
container or foil. All transfers were performed near the balance and
the weight reported to the nearest 0.1 mg. The plastic dishes were
then sealed for shipment.
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b. Acetone Washes
250 ml. beakers were used for acetone wash transfers. These
beakers were leached for 24 hours in 50% nitric acid, washed thoroughly
and oven dried overnight. These were then desiccated for 24 hours and
tared. Once tared, the beakers were sealed with "parafilm". Handling
of beakers was done as far as possible with tongs and "Kimwipes".
All acetone glass jars were left loosely covered in a hood
until the acetone was evaporated. This was found to be safer than
transferring the acetone into the tared beaker and evaporating. Once
the acetone was evaporated, the glass jar was rinsed with acetone,
using a rubber policeman, and the washings collected in the tared beaker.
Once the acetone evaporated in the beakers, the beakers were
desiccated for 24 hours and weighed to a constant weight.
In some cases where water was present in the acetone wash, the
water was evaporated in an oven at 90 C after the acetone had all evaporated.
c. Water Wash Extraction
Beakers tared as described before were used for collecting
the organic extract and the water wash after extraction. The amount of
water collected was marked and the volume later measured and reported.
The water wash was transferred into a 2000 ml. extraction flask and
three 25 cc portions of chloroform used for the initial extraction.
Often when a large volume of water was collected (above 500 cc), a
fourth portion was used. The extraction flask was shaken thoroughly,
and once the chloroform extract settled at the bottom, it was collected
directly in the tared beaker.
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Due to the large volume of water usually collected, three 50 ml.
portions of ether were used. The ether extract separated at the top
and the water portion was collected in the original jars. The ether
extract was then collected along with the chloroform extract. Once all
the ether extract was collected, the extract portion was transferred
back into the extraction flask and the funnel and sides of the flask
rinsed with distilled water. The chloroform and ether extract separating
at the bottom was then drained into the tared beaker and allowed to
evaporate in the hood before desiccating and weighing.
The water portion was transferred to tared beakers, oven dried
at 90°C, desiccated and weighed. All beakers were "parafilm" sealed for
shipment.
The Project Officer requested that particle size analysis not
be performed. Table D-l presents a summary of the measurements and
weight analysis for particulates.
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30
O
1
i
38
p? Container #1
** (Filter)
2
f Container 02
(Acetone wash front half)
Container l>3a
(Organic extract)
Container #3b
(Water after extraction)
Container 115
(Acetone wash back half
Run 1
TABLE D-l
SUMMARY OF WEIGHT MEASUREMENTS
Run 2
en
NJ
00
O
U)
Gross Blank Net
Final (g) Tare (g) (mg) (mg) (mg)
88.1375 8.1370 0.5
0.5
83.3790 83.3395 39.5 0.710 38.79
83.8845 83.8795 5.0 1.07 3.93
92.8184 92.8005 17.9 6.60 11.30
Probe, cyclone, filter, tng. : 39.29
Total, mg.: 54.52
Gross Blank Net
Final (g) Tare (g) (mg) (mg) (mg)
8.1508 8.1508 0.0
0.0
87.0653 87.0584 6.9 0.71 6.19
82.2180 32.3180 0.0 1.07 0.0
82.1840 82,1812 2.8 5.45 0.0
85.7350 85.6976 37.4 0.42 36.98
Probe, cyclone, filter, mg.: 6.19
Total, mg. : 43.17
Run 3
Gross Blank
Final (g) Tare (g) (rag) (mg)
7.5899 7.5899 0.0
82.9152 82.9050 10.2 0.75
85.8033 85.8015 1.8 0.8
Net
(mg)
0.0
9.45
1.00
82.9045 82.8992 5.3 5.45 0.0
88.7124 88.6965 15.9 0.38 15.52
Probe, cyclone, filter, mg. : 9.45
Total, rag. : 25.97
O
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SRL 1281 15 0372
APPENDIX E
TEST LOG
The Eastern Associates Coal Company plant was located on the
north side of the railroad tracks in Keystone, West Virginia. Figure 1
gives a rough schematic of the stack locations, the approximate dimensions
and the sampling setup used. The main building was approximately 70 feet
to the top of the flat roof where the ports were located. The sample
setup and transfer facilities were done in a relatively clean room
located in a single storied building about 100 feet east of the main
building.
Wednesday. February 23, 1972
All the necessary equipment was hauled up and set up for the
initial flow traverse by about 1300 hours. There was some shower activity
at this time, which increased in intensity by late afternoon.
Some electrical grounding problems were encountered, possibly
due to the rain. Grounding the meter box overcame this difficulty. A
leak test was performed after the initial traverse and the first run
started at 1435. Six points were sampled at each of three ports with
a time period of 7 minutes at each point. The first run ended at 1648.
No problems were encountered in port transfer.
The sample box configuration was modified for this site due
to the low height of the sample port from the flat roof (approximately 6").
The sample box had a special inlet on the backside and the impinger train
was placed facing away from the ports.
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SRL 1281 15 0372
The complete impinger train and the probe were carried to the
laboratory facilities where the sample transfer was accomplished. Very
low particulate collection was noticed in this and the other two runs
performed at this site. The halocarbon grease used for glassware
sealing was found to be attacked by acetone and hence it was advised
by the Project Officer not to collect a container #5 (acetone wash back
half) for this run. All glass ware cleanup and setup for the following
day were done at the Keystone laboratory facilities.
The Project Officer also advised that it would be satisfactory
to collect a minimum 60 cubic foot sample rather than a minimum 90 cubic
foot sample.
Thursday, February 24, 1972
Very heavy rain was encountered throughout most of the day.
Stopcock grease was obtained from the Bluefield State College and no
problems were encountered during sample transfer and glassware work.
Two runs were accomplished, the first one starting at 1155 and ending
at 1410, the second one from 1520 to 1735. All sample transfer and
glassware wash were done at the laboratory facility.
Friday. February 25. 1972
All equipment was unloaded, cleaned and packed for transfer
to next site by 1300 hours.
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SRL 1281 15 0372
Thomas Ward
Joseph Wilson
Jyotin Sachdev
Norman Troxel
Zenophon Tomaras
Louis Reckner
APPENDIX F
PROJECT PARTICIPANTS AND TITLES
Project Officer - EPA
Field Team Leader - SRL
Engineer - SRL
Senior Engineer - SRL
Chemist - SRL
Manager, Atmospheric Chemistry &
Industrial Emissions Dept. - SRL
SCOTT RESEARCH LABORATORIES, INC
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