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USEPA Method 29 - Determination of Metals Emissions PDF
USEPA Method 29 - Determination of Metals Emissions PDF
USEPA Method 29 - Determination of Metals Emissions PDF
1.1 Analytes.
Be, Cd, Cr, Co, Cu, Pb, Mn, Ni, P, Se, Ag, Tl, and Zn by
analysis of Sb, As, Cd, Co, Pb, Se, and Tl if these elements
used for analysis of Sb, As, Ba, Be, Cd, Cr, Co, Cu, Pb, Mn,
4.0 Interferences.
5.0 Safety.
burn.
body tissue. Will cause third degree burns. Eye damage may
limit exposure.
cool place.
1466
Method 5 train.
glass frit.
Section 6.1.1.6.
the fifth and sixth (both acidified KMnO4) impingers are the
then the fourth, fifth, and sixth impingers are not used.
holder.
reagents.
Section 16.0.
ng/ml.
equivalent.
equivalent.
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7.2.6 KMnO4.
equivalent.
Type II.
equivalent.
with water. Mix well. This reagent shall contain less than
Type II.
0.0, 1.0, 2.0, 3.0, 4.0, and 5.0 ml of the working standard
calibration range.
Solution Elements
I As, Be, Cd, Mn,
Pb, Se, Zn
1477
for Al, Cr and Pb, 15 µg/ml for Fe, and 10 µg/ml for the
by reference in §60.17(i).
7.5.35 GFAAS Standards. Sb, As, Cd, Co, Pb, Se, and
Suggested levels are 0, 10, 50, 75, and 100 ng/ml. Prepare
2 weeks.
with water.
Storage.
sampling train glassware with hot tap water and then wash in
hot soapy water. Next, rinse glassware three times with tap
Section 8.1.2.
silicone grease.
of Method 5.
site, remove the probe from the sampling train and cap the
might be present. Cap the filter inlet where the probe was
and cap the impinger. Cap the filter holder outlet and
cyclone inlet and loosely cap the open ends. Cap the probe
29-2b):
remove the filter from the filter holder and place it in its
directions on analysis.
container, tighten the lid so that acetone will not leak out
its contents.
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rinse. Rinse the probe nozzle and fitting, probe liner, and
rinses.
record the final total volume. Mark the height of the fluid
8.2.9.1 When sampling for Hg, pour all the liquid from
the sampled flue gas. Place the liquid in Container No. 5A.
in Section 7.3.2.
drilled in the container cap and Teflon liner has been used
successfully.
and stem with the HCl by turning the impinger on its side
impinger, then pour the actual rinse used for the first
during transport.
container and seal it. The tester may use a funnel to pour
0.5 g.
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once during each field test, place 300 ml of the 0.1 N HNO3
Section 8.2.9.2.
No. 12 three unused blank filters from the same lot as the
heat (do not heat the filters to speed the drying) and weigh
Method 5.
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sample.
Section 8.3.3.
and cover the beaker with a ribbed watch glass. Reduce the
1494
Nos. 5A, 5B, and 5C separate from each other. Measure and
Fraction 3C.
values.
1499
Analyze the blanks for Analytical Fractions 1B, 2B, 3A, 3B,
analyses).
Sb, As, Ba, Be, Cd, Cu, Cr, Co, Pb, Ni, Mn, Hg, P, Se, Ag,
Methods for Water and Wastewater Method 303F (for Hg). Run
for all desired metals except Hg, and five for Hg. A
contents and rinses from the empty impinger No. 4 and the
analysis.
200.7 (40 CFR 136, Appendix C). Calibrate the ICAP, and set
§60.17(i).
Section 9.2.2.
described.
12.1 Nomenclature.
curve, µg/ml.
curve, (µg/ml).
mg/dscm.
1508
Fraction 2, µg.
blanks, µg.
blank, µg.
train, µg.
µg.
blank, µg.
similarly).
applicable).
be 0.02 ml.
similarly).
1512
conditions, dscm.
K4 = 10-3 mg/µg.
12.2 Dry Gas Volume. Using the data from this test,
B
A× 'D Eq. 29-1
C
following equation:
emission sample value (Mfh); if Mfhb exceeds "A" µg, use the
greater of I or II:
I. "A" µg.
or II:
I. 1 µg.
29-5:
Qfh
Hgfh ' (Vsoln,1) Eq. 29-5
Vf1B
Half Hg.
1515
Qbh2
Hgbh2 ' (Vsoln,2) Eq. 29-6
Vf2B
Qbh3(A,B,C)
Hgbh3(A,B,C) ' Vsoln,3(A,B,C,) Eq. 29-7
Vf3(A,B,C)
Equation 29-9:
Hgt ' (Hgfh & Hgfhb) %(Hgbh &Hgbhb) Eq. 29-9
+ Hgbhb) is in the range of 0.0 to 0.6 µg, then use the total
I. 0.6 µg.
1516
Equation 29-10:
K4 Mt
Cs ' Eq. 29-10
Vm(std)
detection limits.
and Zn (5 ng/ml).
ng/ml).
for the back-half samples, and (4) a stack gas sample volume
data.
Table 29-1.
be as follows:
16.0 References.
Interferences
Metal Technique SW-8461 Wavelength
Method No. (nm) Cause Minimization
Interferences
Metal Technique SW-8461 Wavelength
Method No. (nm) Cause Minimization
Sb Aspiration 7040 217.6 1000 mg/ml Pb, Use secondary wavelength of 231.1 nm; match
Ni, Cu, or sample & standards acid concentration or
acid use nitrous oxide/acetylene flame
Sb Furnace 7041 217.6 High Pb Secondary wavelength or Zeeman correction
As Furnace 7060 193.7 Arsenic Spike samples and add nickel nitrate
Volatilization solution to digestates prior to analysis
Aluminum Use Zeeman background correction
Ba Aspiration 7080 553.6 Calcium High hollow cathode current and narrow band
set
Barium 2 ml of KCl per 100 ml of sample
Ionization
Be Aspiration 7090 234.9 500 ppm Al Add 0.1% fluoride
High Mg and Si
Be Furnace 7091 234.9 Be in optical Optimize parameters to minimize effects
path
Cd Aspiration 7130 228.8 Absorption and Background correction is required
light
scattering
Front Half of Filter support & 1st impinger 2nd & 3rd
Probe Liner Filter (empty at impingers
and Nozzle Filter back half of filter
Housing housing beginning of (HNO3/H2O2)
test)
FH AR F BH
(3)* (2) (1) (4)
Remove any
residue with
25 ml 8N HCl
solution
8N HCl
(5A) (5B) (5C)