-------
Date: f
Run number:
Operator: _
5 ^"
Sample box number:
PARTICULATE CLEANUP SHEET
"•.' : "•'.' Plant: /^n>
Location of sample port:
Barometric pressure; 3
-------
APPENDIX E
STANDARD SAMPLING PROCEDURES
-------
15708
PROPOSED RULE MAKING
Subporl E—Standards of Perform-
ance for Nitric Acid Plant*
S 466.50 Applicability and designation
of affected facility.
(a) The provisions of this subpart are
applicable to nitric acid plants.
"Weak nitric acid" means acid
which is SO to 70 percent In strength.
§ 466.52 Standard for nitrogen oxides.
No person subject to the provisions of
this subpart shall cause or allow the dis-
charge Into the atmosphere of nitrogen
oxides in the effluent which are:
(a) In excess of 3 Ibs. per ton of acid
produced (1.5 Kgm. per metric ton),
maximum 2-hour average, expressed as
NO.
(b) A visible .emission within the
meaning of this part.
§466.53 Emission monitoring.
(a) There shall be Installed, cali-
brated, maintained, and operated, in any
nitric acid plant subject to the provisions
of this subpart, an instrument for con-
tinuously monitoring and recording
emissions of nitrogen oxides.
(b) The Instrument installed and used,
pursuant to this section shall have a
confidence level of at least 95 percent and
be accurate within ±20 percent and shall
be calibrated Jn accordance with the
method(s) prescribed by the manufac-
turer^) of such instrument; the instru-
ment shall be calibrated at least once
per year unless the manufacturer(s)
specifies or recommends calibration at
shorter Intervals, in which case such
specifications or recommendations shall
be followed.
(c) The owner or operator of any
nitric acid plant subject to the provisions
of this subpart shall maintain a file of all
measurements required by this subpart
and shall retain the record of any such
measurement for at least 1 year follow-
ing the date of such measurement.
§ 466.54 Test methods and procedures.
(a) The provisions of this section are
applicable to performance tests for deter-
mining emissions of nitrogen oxides from
nitric acid plants.
(b) All performance tests shall be con-
ducted while the affected facility is
operating at or above the acid product
rate for which such facility was designed.
(c) Test methods set forth In the ap-
pendix to this part shall be used as
follows:
(1) For each repetition the NO. con-
centration shall be determined by using
Method 7. The sampling location shall be
selected according to Method 1 and the
sampling point shall be the centroid of
the stack or duct. The sampling time
shall be 2 hours and four samples shall
be taken during each 2-hour period.
(2) The volumetric flow rate of the
total effluent shall be determined by us-
ing Method 2 and traversing according
to Method 1. Gas analysis shall be per-
formed by Method 3, and moisture con-
tent shall be determined by Method 4.
(d) Acid produced, expressed In tons
per hour of 100 percent weak nitric 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, nitrogen ox-
Ides emissions, expressed in Ib./ton of
weak nitric acid, shall be determined by
dividing the emission rate in Ib./hr. by
the acid produced. The emission rate
shall be determined by the equation, lb./
hr.=QxC, where Q=volumetric flow
rate of the effluent in ft.'/hr. at standard
conditions, dry basis, as determined In
accordance with J 466.54(d) (2), and
C=NO, concentration In Ib./f t.', as deter-
mined in accordance with i 466.54(d) (1),
corrected to standard conditions, dry
basis. • •'
Subpart F—Standards of Perform-
ance for Sulfuric Acid Plants
g 466.60 Applicability and designation
of affected facility.
(a) The provisions of this subpart are
applicable to sulfur acid plants.
(b) For purposes of ! 466.11(e) the en-
tire plant Is the affected facility.
§ 466.61 Definitions.
As used In this part, all terms not
denned herein shall have the meaning
given them in the Act:
(a) "Sulfuric acid plant" means any
facility producing sulfuric acid by the
contact process by burning elemental sul-
fur, alkylatlon acid, hydrogen sulfide,
organic sulfldes and mercaptans, or acid
sludge.
(b) "Acid mist" means sulfur acid mist,
as measured by test methods set forth
in this part.
§ 466.62 Standard for sulfur dioxide.
No person subject to the provisions of
this subpart shall cause or allow the dis-
charge into the atmosphere of sulfur di-
oxide in the effluent in excess of 4 Ibs.
per ton of acid produced (2 kgm. per
metric ton), maximum 2-hour average.
§ 466.63 Standard for acid mist.
No person subject to the provisions of
this subpart shall cause or allow the dis-
charge into the atmosphere of acid mist
in the effluent which is:
(a) In excess of 0.15 lb. per ton of acid
produced (0.075 Kgm. per metric ton),
maximum 2-hour average, expressed as
H.SO,.
(b) A visible emission within the
meaning of this part.
§ 466.64 Emission monitoring.
(a) There shall be installed, calibrated,
maintained, and operated, in any *^fv.ric
acid plant subject to the provisions of
this subpart, an Instrument for continu-
ously monitoring and recording emis-
sions of sulfur dioxide.
(b) The instrument Installed and used
pursuant to this section shall have a con-
fidence level of at least 95 percent and be
accurate within ±20 percent end shall
be calibrated in accordance with the
method (s) prescribed by the manufac-
turer^) of such instrument, the instru-
ment shall be calibrated at least once per
year unless the manufacturer (s) speci-
fies or recommends calibration at shorter
intervals, in which case such specifica-
tions or recommendations shall be fol-
lowed.
(c) The owner or operator of any sul-
furic acid plant subject to the provisions
of this subpart shall maintain a file of
all measurements required by this sub-
part and shall retain the record of any
such measurement for at least 1 year
following the date of such measurement.
§ 466.65 Test methods and procedures.
(a) The provisions of this section are
applicable to performance tests for de-
termining emissions of acid mist and sul-
fur dioxide from sulfuric acid plants.
(b) All performance tests shall be con-
ducted while the affected facility is op-
erating at or above the acid production
rate for which such facility was designed.
(c) Test methods set forth in the
appendix to this part 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 sampling
time shall be 2 hours, and sampling vol-
ume shall be 40 ft.3 corrected to standard
conditions.
(2) The volumetric flow rate of the
total effluent shall be determined by us-
ing Method 2 and traversing according
to Method 1. Gas analysis shall be per-
formed by 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
Ib./ton of sulfuric acid shall be deter-
mined by dividing the emission rate in
Ib./hr. by the acid produced. The emis-
sion rate shall be determined by the
equation, lb./hr.=QxC, where Q=volu-
metric flow rate of the effluent in ft.'/hr.
at standard conditions, dry basis, as de-
termined in accordance with § 466.65 (d)
(2), and C=acid mist and SO, concen-
trations in lb./ft.' as determined in ac-
cordance with 5 466.65(d) (1), corrected
to standard conditions, dry basis.
APPENDIX—TEST METHODS
METHOD 1—SAMPLE AND VELOCITY TRAVERSES
FOB 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 pro-
cedures for determining compliance with
FEOHAl REGISTER, VOL. 36, NO. IS*—TUESDAY, AUGUST 17, 1971
E-l
-------
I
ro
New Source Performance Standards. This
method Is not Intended to apply to gas
streams other than those emitted directly to
the atmosphere without further processing.
2. Procedure.
3.1 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 down-
stream and two diameters upstream from
any flow disturbance such as a bend, expan-
sion, contraction, or visible flame. For a
rectangular cross section, determine an
equivalent diameter from the following
equation:
equivalent diamcter=2
,[• (length) (width) "I
L length+width J
equation 1-1
2.1.3 When the above sampling site cri-
teria can be met, the minimum number of
traverse points Is twelve (12).
2.1.8 Some sampling situations reader the
above sampling site criteria Impractical.
When this Is the case, choose a convenient
sampling location and use Figure l-l to
determine the minimum number of traverse
points.
2.1.4 To use Figure 1-1 first measure the
distance from the chosen sampling location
to the nearest upstream and downstream
disturbances. 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 number is
a multiple of four, and for rectangular staples
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 traverse
points on two perpendicular diameters ac-
cording to Figure 1-2 and Table 1-1.
NUMBER OF DUCT DIAMETERS UPSTREAM'
(DISTANCE A)
•FROM POINT Of ANY TYPE OF
DISTURBANCE (BEND. EXPANSION, CONTRACTION, ETC.)
Figure 1-2. Cross section of circular stack showing location of
traverse points on perpendicular diameters.
b
. 0
______
0
1
1
•° i °
**• — t — "
i
O 1 O
1
1
r r -1
1
01 0
1
!
o •
c
i
i
I
Figure 1-3. Cross section of rectangular stack divided Into 12 equal
areas, with traverse points at centroid of each area.
10
NUMBER OF OUaOIAMETm DOWNSTREAM*
(DISTANCE •)
Figure 1*1. Minimum mimbar of Invent polnti.
FEDERAL RECISTER, VOl. 36, NO. 159—TUESDAY, AUGUST 17, W1
-------
Table 1-1. Location of traverse points in circular stacks
(Percent of stack diameter from inside wall to traverse point)
i
CO
Traverse
point
number
on a
diameter
1
2
3
4
6
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
' 21
22
23
24
Number of traverse
6 8 10
4.4 3.3 2.5
14.7 10.5 8.2
29.5 19.4 14.6
70.5 32.3 22.6
85.3 67.7 34.2
95.6 80.6 65.8
89.5 77.4
96.7 85.4
91.8
97.5
12
2.%
6.7
11.8
17.7
25.0
35.5
64.5
75.0
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
points
16
1.6
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
on a diameter
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
1.1
3.5
6.0
8.7
11.6
14.6
18.0
21.8
26.1
31.5
39.3
60.7
68.5
73.9
78.2
82.0
85.4
88.4
91.3
94.0
96.5
98.9
24
1.1
3.2
5.5
7.9
10.5
13.2
16.1
19.4
23.0
27.2
32.3
39.8
60.2
67.7
72.8
77.0
80.6
83.9 :
86.8
89.5
92.1
94.5
96.8
98.9
S.2.2. Tor rectangular stack! divide the
erou section Into as many equal rectangular
areas aa traverse points, such that the ratio
of the length to the width of the elemental
area* Is between one and two. locate the tra-
verse points at the centrold of each equal
area according to Figure 1-3.
3. References. Determining Dust Concen-
tration In a Gas Stream. ASME Performance
Test Code #27. New York. 1957.
Devorkln, Howard, et al. Air Pollution
Source Testing Manual. Air Pollution Con-
trol District. Los Angeles. November 1983.
Methods for Determination of Velocity,
Volume, Dust and Mist Content of Gases.
Western Precipitation Division of Joy *tanu-
facturlng Co. Los Angeles. Bulletin V'P-50.
1908.
not be used In the case of nbndlrectlonal
flow.
2. Apparatus.
2.1 Pltot tube—Type S (Figure 3-1),.or
, equivalent.
2.2 Differential pressure gauge—Inclined
manometer, or equivalent, to measure ve-
locity head to within 10 percent of .the mini-
mum valve.
2.3. Temperature gauge—Thermocouples.
bimetallic thermometers, liquid filled sys-
tems, or equivalent, to measure stack tem-
perature to within 1.5 percent of the mini-
mum 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.
' standard Method for Sampling Stacks for
Partlculate Matter. In: 1971 Book of ASTM
Standards, Part 23. Philadelphia, 1971. ASTM
Designation D-2928-71.
METHOD 2—DETERMINATION Or STACK CAS
VELOCITY (TYPE 8 PITOT TUBE)
1. Principle and applicability.
1.1 Principle. Stack gas velocity Is de-
termined from the gas density and from
measurement 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
New Source Performance Standards. Being a
directional Instrument, a pltot tube should
3.0 Gas analyzer—To analyze gas compo-
sition for determining molecular weight.
3.7 Pltot 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 at
the traverse points specified by Method 1.
'3.2 Measure the temperature of the stack
/as. If the total temperature variation with
time Is less than 60* P., a point measurement
will suffice. -Otherwise, conduct a tempera-
ture traverse.
• 3.3 Measure the static pressure in the
•stack.
3.4 Determine the stack gas molecular
weight by gas analysis and appropriate cal-
culation as Indicated In Method 3.
PIPE COUPLING
TUBING ADAPTER
O
8
I
I
Figure 2-1. Pitot tube - manometer assembly.
4. Calibration.
4.1 To calibrate the pltot tube, measure
the velocity head at some point in a flowing
gas stream with both a Type S pltot tube and
a standard type pltot tube with known co-
efficient. The velocity of the flowing gas
stream should be within the normal working
range.
FEDERAL REGISTER,-VOL. 36, NO. 159—TUESDAY, AUGUST 17, 1971
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PROPOSED RULE MAKING
15711
4.3 Calculate the pltot tube coefficient
using Equation 9-1.
where:
c»i..«=Plto* tube coefficient of Type 8
pltot tube.
C».u=Pltot tube coefficient of standard
type pltot tube (If unknown, use
0.99).
AP.,4=Veloclty bead measured by stand-
ard type pltot tube.
AP, ,=Velocity head measured by Type S
pltot tube.
C3 Compare the coefficients of the Type S
pltot tube determined first with one leg and
then the other pointed downstream. Use the
pilot tube only If the two coefficients differ
by no more than 0.01.
« Oaioulations.
equation 2-1 Uae Equation 2-2 to calculate the stack gas
velocity.
V.-K.CV1
equation 2-2
»here:
V.=Stack gas velocity, feet per second (f.p.s.).
Ks=86.48
ft. / lb. \V>
eeo. Mb-mote-'B/
when these units
•ranged.
fc
p.-
M,=
Pltot tube coefficient, dlmensiocless.
'Absolute stack gas temperature, °K.
•Velocity head o! stack gas, In HiO (see fig. 2-2).
Absolute stack gas pressure, In Hg.
Molecular weight of stack gas, Ib./lb.-mole.
PLANT_
DATE i
RUN NO.
STACK DIAMETER. In.
BAROMETRIC PRESSURE, In.
STATIC PRESSURE IN STACK (Pg), In. Hg._
OPERATORS .
SCHEMATIC OF STACK
CROSS SECTION
Traverse point
Velocity head,
in. H20
AVERAGE:
Stack Temperature
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 deter-
mine the average stack gas velocity from
Equation 2-2.
C. References.
Mark, L. 8. Mechanical Engineers' Hand-
book. McGraw-Hill Book Co., Inc., New York,
1951.
Perry, J. H. Chemical Engineers' Handbook.
McGraw-Hill Book Co., Inc., New York, 1960.
Shlgehara, R. T., W. F. Todd, and W. S.
Smith. Significance of Errors In Stack Sam-
pling Measurements. Paper presented at the
Annual Meeting of the Air Pollution Control
Association, St. Louis, Mo., June 14-19, 1970.
Standard Method for Sampling Stacks for
Partlculate Matter. In: 1971 Book of ASTM
standards, Part 23. Philadelphia, 1971. ASTM
Designation D-2928-71.
Vennard, J. K. Elementary Fluid Mechanics.
John Wiley and Sons, Inc., New York, 1947.
METHOD 3—CAS ANALYSIS FOB CARBON DIOXIDE.
' KJCCESS ADI, AND DRT MOLECU1AE WEIGHT •
1. Principle and applicability.
1.1 Principle. An integrated or grab gas
sample is extracted from a sampling point
and analyzed for its components using an
Orsat analyzer.
1.2 Applicability. This method should be
applied only when specified by the test pro-
cedures for determining compliance with New
Source Performance Standards.
2. Apparatus.
2.1 Grab sample (Figure 3-1).
2.1.1 Probe—Stainless steel or Pyrex1
glass, equipped with a filter to remove par-
ticulate matter.
2.1.2 Pump—One-way squeeze bulb, or
equivalent, to transport gas sample to ana-
lyzer..
2.2 Integrated sample (Figure 3-2).
2.2.1 Probe—Stainless steel or Pyrex1
glass equipped with a filter to remove par-
ticulate matter.
2.2.2 Air-cooled condenser—To remove
any excess moisture.
2.2.3 Needle valve—To adjust flow rate.
2.2.4 Pump—Leak-free, diaphragm type.
or equivalent, to pull gas.
2.2.5 Rate meter—To measure a flow range
from 0 to 0.035 c.f m. •
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 Pitot 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 la varying
with time or a sample traverse is conducted.
2.3 Analysis.
2.3.1 Orsat analyzer, or equivalent.
3. Procedure.
3.1 Grab sampling.
3.1.1 Set up the equipment as shown In
Figure 3-1. Place the probe In the stack at a
campling point and purge the sampling line.
Figure 2-2. Velocity traverse data.
1 Trade name.
FEDERAL REGISTER, VOL. 36, NO. 159—TUESDAY, AUGUST 17, 1971
No. 150—Pt n-
E-4
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15712
PROPOSED RULE MAKING
PROBE
FLEXIBLE TUBING
T£R(G
FILTER (GLASS WOOL!
SQUEEZE BULB
Figure 3-1. Grab-sampling train.
RATE METER
VALVE
AIR-COOLED CONDENSER / PUMP
PROBE
QUICK DISCONNECT
FILTER (GLASS WOOL)
RIGID CONTAINER'
Figure 3-2. Integrated gas - sampling train.
3.1.2 Draw sample into the analyzer.
3.2 Integrated sampling.
3.2.1 Evacuate the flexible bag. Set up the
equipment as shown In Figure 3-2 with the
bag disconnected. Place the probe In the
stack and purge the sampling line. Connect
the bag, making sure that all connections
are tight and that there are no leaks.
3.2.2 Sample at a rate proportional to the
stack gas velocity.
3.3 Analysis.
3.3.1 Determine the CO2. CK, and CO con-
centrations as soon as possible. Make as many
passes as are necessary to give constant read-
Ings. If more than 10 passes are necessary,
replace the absorbing solution.
3.3.2 For Integrated sampling, repeat the
analysis until three consecutive run* vary
no more than 0.2 percent by volume for e&h
component being analyzed.
4. Calculations.
4.1 Carbon dioxide. Average the three
consecutive runs and report result to the
nearest 0.1 percent CO*.
4.2 Excess air. Use Equation 3-1 to cal-
culate excess air, and average the runs. Re-
port the result to the nearest 0.1 ; rcent
excess air.
%KA =
(%0.)-0.5(%CO) '
0.264(% N,)-(% 0,)+0.5(
equation 3-1
where:
%EA= Percent excess air.
%O,= 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 the runs. Report the result to the
nearest tenth.
CO,) +0.32(% O,)
+0.28(% N,+ %CO)
Equation 3-1
where:
Md=Dry molecular weight, lb./lb.-
mole.
% CO, = Percent carbon dioxide by volume,
dry basis.
%O,= Percent oxygen by volume, dry
. basis.
%N,= Percent nitrogen by volume, dry
basis.
0.44= Molecular weight of carbon dioxide
divided by 100.
0.32= Molecular weight of oxygen
divided by 100.
0.28= Molecular weight of nitrogen
divided by 100.
6. References
TO ANALYZER AltshuUer, A. P., et al. Storage of Oases
and Vapors In Plastic Bags. Int. J. Air &
Water Pollution. 6.76-81.1963.
Conner, William D., and J. S. Nader Air
Sampling with Plastic Bags. Journal of the
American Industrial Hygiene Association.
25:291-297. May-June 1964. ,
Devorkln, Howard, et al. Air Pollution
Source Testing Manual. Air Pollution Con-
trol District. Los Angeles. November 1963.
METHOD 4 DETERMINATION OF MOISTUBE IK
STACK CASES
1. Principle and applicability.
1.1 Principle. Moisture Is removed from
the gas stream, condensed, and determined
gravlmetrlcally.
1.2 Applicability. This method Is appli-
cable for the determination of moisture in
stack gas only when specified by test proce-
dures for determining compliance with New
Source Performance Standards. This method
does not apply when liquid droplets are pres-
ent In the gas stream.'
Other methods such as drying tubes, wet
bulb-dry bulb techniques, and volumetric
condensation techniques may be used sub-
ject to the approval of the Administrator.
2. Apparatus.
2.1 Probe—Stainless steel or Pyrex> glass
sufficiently heated to prevent condensation
and equipped with a filter to remove par-
ticulate matter.
2.2 Implngers—Two midget Implngers,
each with 30 ml. capacity, or equivalent.
2.3 Ice bath container—To condense
moisture In Implngers.
2.4 Silica gel tube—To protect pump and
dry gas meter.
2.6 Needle valve—To regulate gas flow
rate.
2.6 Pump—Leak-free, <«••»»"•»•"» type, or '
equivalent, to pull pas through train.
2.7 Dry gas meter—To measure to within
» percent of the total sample volume.
2.8 Rotameter—To measure a flow range
from 0 to 0.1 c.f.m.
2.9 Balance—Capable of measuring to the
nearest 0.1 g.
2.10 Barometer—Sufficient to read to
within 0.1 in. Hg.
2.11 Pilot tube—Type S, or equivalent, at-
tached 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 about 5 ml. distilled water In
each Implnger and weigh the Implnger and
contents to the nearest 0.1 g. Assemble the
apparatus without the probe as shown in Flg-
•ure 4-1. Leak check by plugging the inlet to
the first impinger and drawing a vacuum. In-
sure that flow through the dry gas meter is
Mess than 1 percent 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 not to ex-
ceed 0.075 c.f.m. Continue sampling until the
dry gas meter registers 1 cu. ft. or until visible
liquid droplets are carried over from the first
impinger to the second. Record temperature,
pressure, and dry gas meter reading as re-
quired by Figure 4-2.
3.3 After collecting the sample, weigh the
impingers and their contents again to the
nearest 0.1 g.
i Trade name.
: If liquid droplets are present in the gas
stream, assume the stream to be saturated,
determine the average stack gas temperature
(Method 1), and use a psychrometrle chart
to obtain an approximation of the moisture
percentage.
FEDERAL REGISTER, VOL. 36, NO. 159—TUESDAY, AUGUST 17, 1971
E-5
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4. Calculation!.
4.1 Volume of water collected.
, (W,-W.)HT.M.
equation 4-1
where:
V»«=Volume of water vapor collected
(standard conditions), cu. ft.
PROPOSED RULE MAKING
Wt=nnal weight of Impingen and
contents, g.
Wi=Inltial weight of Implngers and
contents, g.
B=Ideal gas constant, 21.83-ln. Hg—
cu. ft./lb. mole-' B.
T.u=Absolute temperature at standard
conditions, 630* B.
P.I4=Pressure at standard conditions,
39.92 In. Hg.
M,=Molecular weight of water, 18
Ib./lb. mole.
SILICA GEL TUBE
HEATED
FILTER '(GLASS WOOL)
ICE BATH
LOCATION.
TEST
DATE
OPERATOR.
POMP
Figure 4-1. Moisture-sampling train.
COMMENTS
DRY GAS METER
BAROMETRIC PRESSURE.
CLOCK TIME
GAS VOLUME THROUGH
METER, (Vm).
ft*
ROTAMETER SETTING,
ftVmin
-
-
METER TEMPERATURE,
•F
43 Gas volume.
15713
l-
' in. Hg/ T. equation 4-2
where:
V.«=Dry gas volume through meter at
standard conditions, cu. ft.
V»=Dry gas volume measured by meter.
cu. ft.
Pm = Barometric pressure at the dry gas
meter, In. Hg.
P.u=Pressure at standard conditions.
29.92-ln. Hg.
T.,j= Absolute temperature at standard
conditions, 530° R.
T»= Absolute temperature at meter
(•P.+460). 'R.
4.3 Moisture content.
Y..
'V..
"V..+V..
-f (0.025)
Figure 4-2. Field ir.clslure determination.
equation 4-3
where:
Bw.=Proportion by volume of water
vapor In the gas stream, dlmen-
slonless.
Vw«=Volume of water vapor collected
(standard conditions), cu. ft.
V»«=Dry gas volume through meter
(standard conditions), cu. ft.
BwB=Approxlmate volumetric proportion
of water vapor In the gas stream
leaving the Impingers, 0.025.
5. References.
Air Pollution Engineering Manual,
Danlelson, J. A.
-------
15714
PROPOSED RULE MAKING
3.1.3 Pltot tube—Typ« 8. or equivalent,
attached to probe to monitor (tack gas
Telocity.
3.1.4 Filter holder—Pyrex1 glass with
beating system capable ol maintaining any
temperature to a maximum of 225* F.
2.1.5 Implngers—Four Implngers con-
nected in series with glass ball Joint fittings.
The first, third, and fourth Implngers are of
the Greenhurg-Smlth design, modified by re-
HEATED AREA
PROBE
REVERSE-TYPE
PITOT TUBE
placing the tip with a Vi-lnch ID glass tube
extending to '/i-lnch from the bottom of the
flask. The second Implnger Is of the Qreen-
burg-Smlth design with the standard tip.
2.1.8 Metering system—Vacuum -gauge,
leak-free pump, thermometers capable of
measuring temperature to within 5' F., dry
gas meter with 2 percent accuracy, and re-
lated equipment, or equivalent, as required
to maintain an isoklnetic sampling rate and
to determine sample volume.
FJLTER HOLDER THERMOMETER CHECK
VALVE
VACUUM
LINE
IMPIMGERS ICE BATH
PASS.VALVE
VACUUM
\ GAUGE
MAIN VALVE
DRY TEST METER
AIR-TIGHT
PUMP
Figure 5-1. Paniculate-sampling train.
3.1.T Barometer—To measure atmospheric
pressure to ±0.1 In. Hg.
13 Sample recovery.
3.3.1 Probe brush—At least as long as
probe.
2.2.2 Qlaw ~ash bottles—Two.
2.2.3 Glass sample storage containers.
3.2.4 ursduated cylinder—260 mU
2.3 Analysis.
2.3.1 Qlw« -relghlng dishes.
2.3.2 'Desiccator.
2.3.3 Analytical balance—To measure to
±0.1 mg.
2.3.4 Beakers—250 ml.
1 Trade name..
2.3.5 Separator? funnels—600 ml. and
1,000 ml.
2.3.8 Trip balance—300 g. capacity, to
measure to ±0.05 g.
2.3.7 Graduated cylinder—25 ml.
3. Reagents.
3.1 Sampling
3.1.1 Filters—Glass fiber, MSA 1106 BH,
or equivalent, numbered for identification
and prewelghed.
3.13 Silica gel—Indicating type, « to 18
mesh, dried at 175* O. (350' F.) for 2 hours.
•3.1.3 Water—Dainnlzed, distilled.
3.1.4 Cninhe
-------
PROPOSED RULE MAKING
15715
PLANT
LOCATION.
OPERATOR.
DATE
RUN NO.
SAMPLE BOX N0j_
METER BOX N0._
METER AHg
C FACTOR
AMBIENT TEMPERATURE.
BAROMETRIC PRESSURED
ASSUMED MOISTURE, «_
HEATER BOX SETTING
PROBE LENGTH, in.
NOZZLE DIAMETER, in. _
PROBE HEATER SETTING.
SCHEMATIC OF STACK CROSS SECTION
TRAVERSE POINT
NUMBER
TOTAL
SAMPLING
TIME
(«), min.
AVERAGE
STATIC
PRESSURE
(Ps). in. Hg.
STACK
TEMPERATURE
). h3
GAS SAMPLE TEMPERATURE
AT DRV GAS METER
INLET
ITm ,„.).- F
Avg.
OUTLET
(Tmoul).eF
Avg.
Avg.
SAMPLE BOX
TEMPERATURE,
»F
IMPINGER
TEMPERATURE,
"F
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
participate matter. Set aside portions of the
water and acetone used in the sample recov-
ery as blanks for analysis. 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 particulate
matter and acetone washings from all sam-
ple-exposed surfaces prior to the filter In this
container and seal. Use a razor blade, brush.
or rubber policeman to loosen adhering par-
ticles.
Container No. 3. Measure the volume of
water from the first three Impingers and
place the water in this container. Place water
Figure 5-2. Particulate field data.
rinsings of all sample-exposed surfaces be-
tween the filter and fourth Impinger In this
container prior to sealing.
Container No. 4. Transfer the slllcft gel
from the fourth impinger to the original
container and seal. Use a rubber policeman
as an aid in removing silica gel from the
Impinger.
Container No. 5. Thoroughly rinse all sam-
ple-exposed surfaces between the filter and
fourth Impinger with acetone, place the
washings In this container, and seal.
4.3 Analysis. Record the data required on
the example sheet shown In Figure 5-3.
Handle each sample container as follows:
Container No. 1. Transfer the filter and any
loose particulate matter from the sample
container to a tared glass weighing dish, des-
sicate, and dry to a constant weight. Report
results to the nearest 0.5 mg.
Container No. 2. Transfer the acetone
washings to a tared beaker and evaporate to
dryness at ambient temperature and pres-
sure. Dessicate and dry to a constant weight.
Report results to the nearest 0.5 mg.
Container No. 3. Extract organic particulate
from the Impinger solution with three 26 ml.
portions of chloroform. Complete the ex-
traction with three 25 ml. portions of ethyl
ether. Combine the ether and chloroform ex-
tracts, transfer to a tared beaker and evapo-
rate at 70° P. until no solvent remains. Des-
sicate, dry to a constant weight, and report
the results to the nearest 0.5 mg.
Container No. 4. Weigh the spent silica
gel and report to the nearest gram.
FEDERAL REGISTER, VOl. 36, NO. 159—TUESDAY, AUGUST 17, 1971
E-8
-------
15716
PROPOSED RULE MAKING
PIANT_
OATE__
RUN NO,
CONTAINER
NUMBER
1
2
3a«
3b«»
S
TOTAL
WEIGHT OF PARTICIPATE COLLECTED.
mg
FINAL WEIGHT
X,
TARE WEIGHT
;x^
WEIGHT GAIN
•
where:
V-.,«=Volum« of gas sample through the
dry gas meter (standard condi-
tions) , cu. ft.
V»=Volume of gas sample through the
dry gas meter (meter conditions),
eu. ft.
T,a=Absolute temperature at standard
conditions, 630 °B.
T.=Aver age dry gits meter temperature,
•B.
P,,,=Barometric pressure at the orifice
meter, In. Hg.
AH=Pressure drop across the orifice
meter, in HO.
13.6=Specific gravity of mercury.
PM1=Absolute pressure at standard con-
ditions, 29.92 In. Hg.
6.14 Volume of Water vapor.
cu. ft.
1.0474
*3a • ORGANIC EXTRACT FRACTION.
"3b • RESIDUAL WATER FRACTION.
FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME.
ml
-
SILICA GEL
WEIGHT.
9
9* ml
ml.
equation 5-2
where:
Vw.t4=Volume of water vapor In the gas
sample (standard conditions) , cu.
' ft.
Vi.rrToUl Tolume of liquid collected in
Unpingers and silica gel (see Fig-
ure 5-3), ml.
»H,o=Denslty of water, l g./mL
Mn,o= Molecular weight of water, 18 Ib./lb.
mole.
B= Ideal gas constant, 21.83 in Hg-cu.
ft./lb. mole-°B.
Tita=Ab6olute temperature at standard
conditions, 530° R.
P td=Absolute pressure at standard con-
ditions. 29.92 In. Hg.
6.1.4 Total gas volume.
"tottl= * m»td~t" V wltd
•CONVERT WEIGHT Of WATER TO VOLUME BY DIVIDING TOTAL WEIGHT"
INCREASE BY DENSITY OF WATER. (1 g/ml):
INCREASE, g
(1 g/ml)
VOLUME WATER, ml
equation 5-3
where:
V,,,ll=Total volume of gas sample (stand-
ard conditions) , cu. ft.
V»i,ia= Volume of gas through dry gas
meter (standard conditions), cu.
ft.
• V.mlJ= Volume of water vapor in the gas
sample (standard conditions) , cu.
ft.
6.1.6 Total particulate weight. Determine
tli« total particulate catch from the sum of
the weights on the analysis data sheet (Fig-
ure 5-3).
6.1.6 Concentration.
Figure 5-3. Analytical data.
IL.\(™±\
Container No. 5. Transfer the acetone
washings to a tared beaker and evaporate to
dryuess at ambient temperature and pres-
sure. Desiccate, dry to a constant weight, and
report the results to the nearest 0.5 mg.
5. Calibration.
Use standard methods and equipment ap-
proved by the Administrator to calibrate
the orince meter, pilot tube, dry gas meter,
and probe heater.
6. Calculations.
6.1 Sample concentration method.
6.1.1 Average dry gas meter temperature.
See data sheet (Figure 5-2).
6.1.2 Dry gas volume. Correct the sample
volume measured by the dry gas meter to
standard conditions (70° P., 29.92 in. Hg) by
using Equation 5-1.
v
equation 5-1
c.'
equation 5-4
where;
c'.=Concentration of particulate matter
In stack gas (Sample Concentra-
tion Method), gr./s.c.f.
M.=Total amount of particulate mat-
ter collected, mg.
V,.1.,=Total volume of gas sample (stand-
ard conditions), cu. ft.
6.3 Ratio of area method.
6 J.I Stock gas velocity. Collect the neces-
sary data as detailed in Method 2. Correct the
FIOKAL K6ISTEI. VOL 34, NO. 159—TUESDAY, AUGUST 17, If71
E-9
-------
stack gas velocity to standard conditions
(29.92 in. Hg, 530° R.) as follows:
S
i
a
mi '
1' in. Hg/ \ T. / equation 5-5
where:
V.iM=Stack gas velocity at standard con-
ditions, ft. /sec.
V.=Stack gas velocity calculated by
Method 2, Equation 2-3, ft./sec.
P.=Absolute stack gas pressure. In. Hg.
P,tt=Absolute pressure at standard oon-
tlons, 39.92 In. Hg.
Tlt<=Absolute temperature at standard
conditions, 530* R.
T.= Absolute stack gas temperature
(average), *R.
t
6.2.2 Concentration.
'•=0:'
Mj A.
e A_
where:
Ci=Concentration of partlculate matter
In the stack gas (Ratio of Area
Method), gr./s.c.f.
M.=Partlculate mass now rate through
the stack (standard conditions),
mass/time.
Qi= Volumetric flow rate of gas stream
through the stack (standard con-
ditions) , volume/time.
Mr. = Total amount of partlculate matter
collected by train, mg.
. I=Total sampling time, mln.
A.=Cross-sectional area of stack, sq. ft.
A.=Cross-sectlonal area of nozzle, sq. ft.
V.,ta=Stack gaa velocity at standard con-
ditions, ft./sec.
6.3 Isokinetlc variation.
c.
^XlOO--
9V.P.A.
X100 =
min.
AH
c'.=Concentration of paniculate matter
In the stack gaa (Sample Concentra-
tion Method). gr./s.c.f.
7. References.
Addendum to Specifications for Incinerator
Testing at Federal Facilities PBS, KCAPC.
Dec. 6,1867.
Martin, Robert M. Construction Details of
Isoklnetlo Source Sampling Equipment. En-
vironmental Protection Agency, APTD-0581.
Bom, Jerome J. Maintenance, Calibration,
and Operation of Isoklnetlo Source Sampling
Equipment. Environmental Protection
Agency, APTD-0676.
Smith, W. S.; R. T. Bhlgehara, and W. F.
Todd. A Method of Interpreting Stack Sam-
pling Data. Paper presented at the 63d
Annual Meeting of the Air Pollution Control
Association, St. Louis. June 14-19, 1970.
Smith, W. S., et al. Stack Gas Sampling Im-
proved and Simplified with New Equipment.
APCA Paper No. 67-119.1967.
Specifications for Incinerator Testing at
Federal Facilities. PHS, NCAPC. 1967.
METHOD S—DETERMINATION OF STOTOB DIOXIDE
EMISSIONS FROM 8TATIONABT SOUftCES
1. Principle and applicability.
1.1 Principle. A gas sample Is extracted
from the sampling point In the stack, and
the acid mist Including sulfur trloxlde Is
separated from the sulfur dioxide. The sulfur
dioxide fraction Is measured by the barium*
thorln tltratlon method.
1.3 Applicability. This method Is appllca-
9V.P.A.
where: '
I=Percent of isoklnetlc sampling.
Ci=Concentratlon of participate matter
in the stack gas (Ratio of Area
Method), gr./s.c.f.
C 4 = Concentration of partlculate matter .
In the stack gaa (Sample Concen-
tration Method), gr./s.c.f.
Vi.sTotal volume of liquid collected In
Implngers and silica gel (see Fig-
ure 5-3), ml.
»H.o=Density of water, 1 g./ml.
R=r Ideal gas constant, 31.83 In. Hg-cu.
ft./lb. mole-'R.
Mnao=Molecular weight of water, 18 Ib./lb.
mole.
Vm— Volume of gas sample through the
dry gas meter (meter conditions),
cu. ft.
T»=Absolute average dry gas meter tem-
perature (see Figure 5-2), *R.
Pblr=Barometrlc pressure at sampling
site. In Hg.
AH=Aver age pressure drop across the ori-
fice (see Figure 5-2), in H3O.
Ti=Absolute average stack gas tempera-
ture (see Figure 6-2), 'R.
equation 5-7
*=Total sampling time, mln.
V.=Stack gaa velocity calculated by
Method 2, Equation 2-2, rt./sec.
P.=Absolute stack gas pressure. In. Hg.
A.=Cross-sectional area of nozzle, sq. ft.
6.4 Acceptable results. The following
range sets the limit on acceptable Isoklnetlc
sampling results:
If 83 percent .c.f.h. flow rang*.
2.1.8 Dry gas meter—Sufficiently accurate
to measure the sample volume within 1
percent.
2.1.9 Pltot tube—Type S, or equivalent,
necessary only If a sample traverse Is re-
quired or if stack gas velocity varies with
time.
2.2 Sample recovery.
2.2.1 Glass wash bottles—Two.
2.2.2 Polyethylene storage bottles—To
store Implnger samples.
2.3 Analysis.
1 Trade name.
PROBE (END PACKED
WITH QUARTZ OR
PYREX WOOL)
TYPE S PITOT TUBE
HCKWALL
ri
MIDGET BUBBLER MIDGET IMPINGERS
GLASS WOOL
SILICA GEL DRYING TUB!
PITOT MANOMETER
• <• +c ' Equation 8-8
where :
c.= Average partlculate concentration la
the stack gas, gr./s.c.f.
c«= Concentration of partlculate matter
In the stack gas (Ratio of Area
Method) , gr./s.c.f.
'PUMP
DRY GAS METER ROT,
Figure 6*1. SOa sampling train.
O
S
m
O
JO
O
FEDERAL REGISTER, VOL. 36, NO. 159— TUESDAY, AUGUST 17, 1971
-------
APPENDIX F
LABORATORY REPORT
-------
All laboratory analyses were supervised and performed by EPA personnel
Complete sample boxes were shipped by air freight, directly to the EPA
facilities in Durham, M. C. Results are presented in this section.
F-1
-------
ENVIRONMENTAL PROTECTION AGENCY
Office of A1r Programs
Research Triangle Park, North Carolina 27711
Reply to
Attnof: ATD Date April 10, 1972
Subject-. Mass Analysis of Participate Samples from Chromium Mining and Smelting-
Woodstock, Tenn.
To: Hlnton Kelly, Chemical Engineer, Petroleum & Chemical Section, ETB, ATD
Particulate samples from six tests at the Chromium Mining and Smelting
Company, Woodstock, Tenn. were analyzed for mass as specified 1n the
Federal Register. Listed below 1n Table I are the results of the analysis,
listed according to EPA code number and Source test numbers.
TABLE I
MASS ANALYSIS OF SOURCE SAMPLES FROM
CHROMIUM MINING & SMELTING-WOODSTOCK, TENN.
EPA Code f
1013
1012
1016
1015
1014
Total
1017
Test I
CSE-1
CSE-1
CSE-1
CSE-1
CSE-1
CSE-1
CSE-1
Sample
Fraction
F
C
B
C-E
H20
S-G
Mass (mg)
109.5
11.9
8.6
5.1
12.1
147.2
14.0 gm.
1027 CSE-2 F 256.9
1026 CSE-2 C 9.9
1030 CSE-2 B 4.3
1029 CSE-2 C-E 3.9
1028 CSE-2 H20 13.5
Total CSE-2 288.5
1031 CSE-2 S-G 22.3 gm.
F-2
-------
TABLE I (Continued)
EPA Code 1
1041
1040
1044
1043
1042
Total
1045
1004
1002
1003
1005
1001
1008
1007
1006
Total
1009
1019
1020
1021
1018
1024
1023
1022
Total
1025
Test 1
CSE-3
CSE-3
CSE-3
CSE-3
CSE-3
CSE-3
CSE-3
CSD-1
CSD-1
CSD-1
CSD-1
CSD-1
CSD-1
CSD-1
CSD-1
CSD-i
CSD-1
CSD«2
CSD-2
CSD-2
CSD-2
CSD-2
CSD-2
CSD-2
CSD-2
CSD-2
Sample
Fraction
F
C
B
C-E
H20
S-G
F
F
F
F
C
B
C-E
H20
S-G
F
F
F
C
B
C-E
H20
S-G
Mass (mg)
286.6
15.4
10.6
1.9
2.9
317.4
29.1
-------
TABLE I (Continued)
EPA Code 1
1033
1035
1034
1032
1038
1037
1036
Total
1039
1010
1011
Test 1
CSD-3
CSD-3
CSD-3
CSD-3
CSD-3
CSD-3
CSD-3
CSD-3
CSD-3
H20 Blank
Acetone Blank
Sample
Fraction
F
F
F
C
B
C-E
H20
S-G
120 ml.
95 ml .
Mass (mq)
2122.8
1808.0
480.2
2004.2
11.1
1.6
99.1
6527.0
28.5 gm.
0.0
0.3
where: F - filter fraction; c - front half (acetone);
B - back half (acetone); C-E - organic extraction;
HpO - Implnger water residue. Each value has been adjusted to
correct for the appropriate blank weight.
These samples have been sealed to prevent contamination and are
being held for any further desired analyses at the IRL Building.
Frank W11shire
Chemist
Petroleum & Chemical Section
Emission Testing Branch, ATD
F-4
-------
APPENDIX G
TEST LOG
-------
APPENDIX G - TEST LOG
Date (1972)
2/1/72
2/2/72
2/2/72
Time
1430-1648
1430-1631
0850-1038
0849-1033
1255-1438
1254-1440
Location
Exhaust
Inlet
Exhaust
Inlet
Exhaust
Inlet
Sample No.
CSE-1
CSD-1
CSE-2
CSD-2
CSE-3
CSD-3
Particulate
X
X
X
X
X
X
Orsat
X
X
X
X
X
X
Notes: On Monday (1/31) all RRI field personnel arrived at the test
site, unpacked and checked equipment. On Tuesday (2/1) equipment
was set up and preliminary measurements made. The first efficiency
test was carried out by mid-afternoon that day after a delay caused
by Chromasco having to build a test platform at the exhaust stack.
On Tuesday (2/1) two particulate efficiency tests were carried
out without any difficulty. Gas sample bags were collected along
with each particulate to be analyzed for 02, C02 and CO at the
site. Late in the afternoon a group of RRI personnel returned home.
On Wednesday (2/2) the remainder of RRI personnel returned
home after completing packing and shipping of the test equipment.
6-1
-------
APPENDIX H
RELATED REPORTS
-------
Related reports covering emissions from reactive metals furnaces,
under this same contract for the Environmental Protection Agency, are
as follows:
Test Number
FA-1
FA-2
FA-3
FA-4
FA-5
FA-6
Survey Location
Foote Mineral Company,
Steubenville, Ohio
Union Carbide Corporation
Marietta, Ohio
Airco Alloys and Carbide
Niagara Falls, New York
Ai rco
Charleston, S. C.
Union Carbide Corporation
Alloy, West Virginia
Chromium Mining & Smelting
Corporation
Memphis, Tennessee
Control Device
None
Venturi Scrubber
Baghouse
Electrostatic
Precipitator
Baghouse
ADTEC
Scrubber System
Status
Issued
Aug., 1971
Issued
Oct., 1971
Issued Oct., 1971
(Rev. Dec., 1971)
Issued Nov., 1971
Draft Issued
Mar., 1972
This Report
H-l
-------
APPENDIX I
PROJECT PARTICIPANTS AND TITLES
-------
PROJECT PARTICIPANTS AND TITLES
R. N. Allen, P.E., Project Manager
C. C. Gonzalez, Chemist, Crew Leader
T. E. Eggleston, Industrial Hygienist
G. B. Patchell, Senior Technician
J. R. Avery, Technician
L. W. Baxley, Technician
B. M. Brown, Technician
0. R. McReynolds, Technician
1-1
-------