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S.D. Joshi
Scientist
Air Pollution Control Division, NEERI, N a g p u r - 440020
Nitric oxide (NO) and nitrogen dioxide (NO2) are the most prevalent
nitrogen oxide air pollutants. These pollutants are chiefly emitted from high
temperature combustion processes, with the major oxide in combustion
emissions being NO. Nitric oxide is oxidized to NO2 in the atmosphere.
measured as NO^ in this technique after conversion of the NO2 to NO. The
manual method (Saltzman method) is based on a specific reaction of nitrite ion
with diazotizing-coupling reagents to form a deeply colored azo dye, which is
measured colorimetrically. Nitric oxide can be measured by this method by
oxidizing it to NO2 prior to sampling. Although various solid and liquid oxidants
for the conversion of NO to NO2 have been used and tested, their reliability for
field use is not wholly satisfactory. Consequently the measurement of NO by this
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method is not recommended. The detector tube method is applicable only to the
semiquantitative measurement of NO2. There are currently no detector tubes
available for the measurement of NO; however, tubes are available for the
measurement of NO x (NO + NO2).
principles.
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The method is intended for the manual determination of NO2 in the
atmosphere in the concentration range of a few to about 9400 ug/m 3 (5 ppm) for
sampling periods up to 2 hours at flow rates up to 0.6 liter/minute. Sulfur dioxide,
ozone, and other gases may interfere; but in urban air, the extent of the
interference is normally minimal.
Apparatus
fritted disperses
Air-metering device - A flow meter capable of accurately measuring a flow
between 0.3 and 0.6 liter/minute is recommended.
Air pump - An appropriate suction pump capable of drawing the required sample
flow for intervals of up to 2 hours is suitable.
Mechanical stirrer.
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Spectrophotometer or colorimeter - A laboratory instrument suitable for
measuring the pink color at 550 nm, with stoppered tubes or cuvettes, is
recommended.
Reagents
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Standard sodium nitrite solution (stock solution) : Dissolve sufficient
desiccated sodium nitrite [NaNC^] (assay of 97 percent or greater)] and dilute
1.500
G = x 100
A
Where,
G = amount in g of sodium nitrite;
1.500= gravimetric factor in converting N 0 2 into sodium nitrite;
A= assay, percent
Sampling Procedure
Butt-to-butt glass connections with slightly greased tygon or pure gum rubber
tubing may also be used for connections without losses if lengths are kept
minimal. In areas of high particulate concentrations, a filter is recommended at
the intake of the absorber to remove particulate matter.
Calibration Curve
Take 12 sample impinger tubes and number them in series marking one of
then as control or blank. Add Step-lll solution in the volume ranging from 0.5 to
18 ml i.e. 0.5 to 18 ug NO2. Make up the volume to 20 ml by adding appropriate
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present in the sample will be converted to soluble sulfate. Add 5 ml of diazotizing
reagent and shake well and add 1 ml of coupling reagent adjust the final volume
to 30 ml with absorbing media shake well. Wait for 30 minutes. Using 1-cm path
length cells, the absorbance of the sample in each bubbler and the absorbance
of unexposed reagent is measured with a colorimeter or spectrophotometer at
550 nm, using distilled water as a reference. The absorbencies of the test
solutions are then corrected for the reading given by the unexposed reagent; the
corrected absorbance values for each pair of bubblers are then added together.
Plot the curve on graph paper taking transmittance/absorbance on Y axis and
NC>2 (ug) concentrations on X axis.
of mercury and 25°C; thus, only slight correction by means of the well-known
perfect gas equation is ordinarily required to get the standard volume of the air
sample.
It has been determined empirically that 0.74 mole of NaNC>2 produces the
calculated from :
F1 + F 2
V= x T x 10"6
2
Where,
50
Calculate the concentration of nitrogen dioxide as follows :
(ug/N0 2 /ml) x 50
3
Mass of nitrogen dioxide in ug/ per m =
V x 0.35
Where,
50 = volume of absorbing reagent used in sampling, ml;
V= volume of air sampled, m 2 ;and
0.35 = overall average efficiency
N02
Calibration Procedure
Add graduated amounts (0.2, 0.4, 0.6, 0.8, and 1.0 ml) of freshly prepared
standard NaNC>2 solution (0.0203 g/liter) to a series of 25-ml volumetric flasks,
and dilute to marks with absorbing reagent. Good results can be obtained with
these small volumes of standard solution if they are carefully measured. If
preferred, however, larger volumes may be used with correspondingly larger
volumetric flasks. Mix well and allow 15 minutes of unexposed reagent using
distilled water as a reference.
Plot the absorbances of the standard nitrite solutions, corrected for the
reagent blanks, against the nitrite concentrations.
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