Analysis of

NOx in
Ambient Air

Envirotech Centre for Research & Development

New Delhi
Principle
 Modified Jacobs & Hochheiser Method (IS 5182 Part 6
Methods for Measurement of Air Pollution: Oxides of
nitrogen).
 Ambient nitrogen dioxide (NO2) is collected by
bubbling air through a solution of sodium hydroxide
and sodium arsenite.
 The concentration of nitrite ion (NO2-) produced
during sampling is determined colorimetrically by
reacting the nitrite ion with phosphoric acid,
sulfanilamide, and N-(1-naphthyl)-ethylenediamine
di-hydrochloride (NEDA) and measuring the
absorbance of the highly coloured azo-dye at 540
nm.
Requirements:
 Analytical balance
 Gaseous Sampler that can maintain a flow rate up to
3 litre/min.
 Calibrated flow measuring device to control the air
flow from 1 litre/min.
 Absorber: a midget impinger or a fritted bubbler
 Spectrophotometer: Capable of measuring
absorbance at 540 nm equipped with 1 cm path
length cells.
 Glass wares: low actinic glassware must be used for
analysis
Absorbing Media
Dissolve 4.0 gm Sodium hydroxide
+
1.0 gm Sodium arsenite

And make upto 1000ml with distilled water

Reagents required for analysis

Sulfanilamide Solution

Dissolve 20.0 gm Sulfanilamide

+
50 ml of 85% phosphoric acid

And make upto 1000ml with distilled water

(This solution is stable for one month, if kept in refrigerator)

Reagents required for analysis

Hydrogen peroxide Solution

Dilute 0.2 ml of 30% H2O2 solution

And make upto 250ml with distilled water

(This solution is stable for one month, if kept in

refrigerator & protected for light.)
Reagents required for analysis

N-(1-Napthyl)-ethyenediamine di-
hydrochloride (NEDA) Solution

Dissolve 0.5 gm of NEDA

And make upto 500ml with distilled water

(This solution is stable for one month, if kept in

refrigerator & protected for light.)
Preparation of Calibration Curve
Stock Sodium nitrite solution
(1000ug NO2/ml)

Dissolve 1.5 gm of Sodium nitrite

And make upto 1000ml with distilled water

The amount of Sodium nitrite to be used, if the assay percent is less

than 100%, is calculated by
G=1.5/A

Where G= Amount of Sodium nitrite in gm

1.5= Gravimetric conversion factor
A= Assay percentage (should be greater than 97%)
(This solution is stable for six weeks, if kept in refrigerator.)
Preparation of Calibration Curve
Working Sodium nitrite solution

Solution A (10ug NO2/ml)

Dilute 5 ml of Stock Sodium nitrite solution

And make upto 500ml with distilled water

Solution B (1.0ug NO2/ml)

Dilute 25 ml of Solution A

And make upto 250ml with absorbing solution

(Prepare freshly)
Preparation of Calibration Curve
Volumetric 50ml 50ml 50ml 50ml 50ml 50ml
Flask Blank Sample1 Sample2 Sample3 Sample4 Sample5
Working 0 ml 1ml 3ml 5ml 7ml 9ml
NaNO2
Solution B
Absorbing 10ml 9ml 7ml 5ml 3ml 1ml
Media
H2O2 Sol. 1ml 1ml 1ml 1ml 1ml 1ml

Sulfanilami 10ml 10ml 10ml 10ml 10ml 10ml

de Sol.
NEDA Sol. 1.4ml 1.4ml 1.4ml 1.4ml 1.4ml 1.4ml

Make upto 50ml with distill water, Mix thoroughly , After 10 minutes measure
absorbance of each flask at 540nm wavelength
Preparation of Calibration Curve
Plot calibration curve with absorbance
versus concentration of NO2
Preparation of Calibration Curve
Plot a calibration curve absorbance (Y axis)
versus concentration (X axis). Draw a line of
best fit and determine the slope. The
reciprocal of slope gives the calibration
factor (CF).
Sampling Procedure
 Place 20 ml of absorbing solution in an
impinger
 Place this impinger in Gaseous sampler
and sample for one hour at the flow rate
of 1 L/min.
 After sampling measure the volume of
sample and transfer to a sample storage
bottle.
Sample analysis
Volumetric Flask 50ml 50ml
For Blank For sample
Exposed absorbing Media 0 ml 10ml

Absorbing Media 10ml 0ml

H2O2 Sol. 1ml 1ml

Sulfanilamide Sol. 10ml 10ml

NEDA Sol. 1.4ml 1.4ml

Make upto 50ml with distill water, Mix thoroughly , After 10 minutes measure
absorbance of each flask at 540nm wavelength
Calculation
Total volume of air passed through Nox
impinger (V, in liter)

Avg. Flow Rate (lpm) X Time (minute)

Calculation
Concentration (ug NO2/m3)
=
C x A x 1000 x D
V x B x 0.82

Where:
C= NO2 Curve value
A= Absorbing reagent taken for sampling, ml
V= Volume of sampled air
B= Volume taken for sample analysis, ml
D= Dilution factor
1000 for conversion from liter to m3
0.82= sampling efficiency