EL/SOP-A/03

AMBIENT NOx
IS-5182 (Part 6), 2006
(Modified Jacob & Hochheiser Method)
1. Principle
Ambient NO
2
is collected by bubbling Air through a solution of Sodium Hydroxide and Sodium
Arsenite. The concentration of Nitrite ion produce during sampling is determined calorimetrically
by reacting the Nitrite ion with Phosphoric Acid, Sulphamic Acid, NEDA (N-(1-Naphthyl)
Ethylenediamine di-hydrochoride) and measuring the Absorbance of highly colored azo dye at
540 nm.
2. Range
The nominal range of the method is 6-750 g NO2 /m3 (0.003-0.400 ppm)
The range of the analysis is 0.04 to 2.0 g NO2 /ml, following Beer's Law throughout this range
(0 to 1.0 absorbance units). Under the specified conditions of 50 ml of absorbing reagent, a
sampling rate of 200 cm
3
/min for 24 hours, and a sampling efficiency of 0.82, the range of the
method is, therefore, 6 to 420 g/NO
2
/m
3
(0.003 to 0.22 ppm). Nitrogen dioxide concentrations
in the range of 420 to 750 g/m3 (0.22 to 0.4 ppm) are accurately measured by 1:1 dilution of the
collected sample.
3. Interference

NO (Positive), CO
2
(Negative) interference. The average error resulting from normal Ambient
conc. On NO and CO2 is small for most Monitoring situation and does necessitate applying a
correction to measurement obtained with this method.

Potential interference from sulphur dioxide (SO

2
) is eliminated by converting any SO2 to
sulphate using Hydrogen peroxide during analysis.
4. Sample Preservation
Collected samples are stable for at list Six week at room Temperature 25
O
C + 2
O
C. Store
samples should be tightly sealed to prevent Absorption of NO
2
from the Atmosphere.
5. Reagent Preparation
Absorbing Reagent (Sodium - Arsenite) (0.1 N NaOH):-
4.0 gm NaOH + 1.0 Sodium Arsenite (NaAsO
2
) dissolved in 1000 ml. Distill Water (D.W.)
Sodium Arsenite is Highly Poisonous chemical so it is important to use it with care and to
protect them to come in skin contact.

Hydrogen Peroxide (H
2
O
2
) (0.02%)
0.2 ml H
2
O
2
(30%) make up 250ml. with Distill Water (D.W.)
This solution may be used for one month, if refrigerated and protected from light

Sulphanilamide (2.0%)- Melting Point 165

O
C to 167
O
C
20.0 gm. Sulphanilamide + 700 ml. D.W, then shake + 50.0 ml. of 85 % phosphoric acid (H
3
PO
4
)
make up 1000 ml. (1.0 Liter) with Distill Water (D.W.)
This Solution is stable for one month if refrigerated.

NEDA (0.1%)
0.5 gm. NEDA make up 500 ml. with Distill Water (D.W.)
1% Aqueous solution should have only one absorption peak at 320nm .over the range of
260-400nm. NEDA showing more than one absorbance peak over this range is impure and
should not in use.
This solution is stable for one month , if refrigerated and protected from light
6. Standard Solution (NaNO
2
):-
(i) Sodium Nitrite Stock Solution (1000 gNO
2
/ml solution)
1.5 gm Sodium Nitrite (NaNO
2
) dissolved in 1000 ml. (1.0 Liter) Distill Water (D.W.)
NaNO
2
(97% pure generally) we are using 1.5 gram for 100% pure NaNO
2
. If conc. Is less
than 100% purity than conc. Of sodium Nitrite calculated by Formula
G=1.5/A
Where G = amount of Sodium Nitrite
A=Assay percent (97%)
Stable for 6 weeks if Refrigerated.
(ii) Sodium Nitrite (10 gNO
2
/ml solution),
5.0 ml. Stock Solution make up 500ml. with Distilled water
(iii) Sodium Nitrite Working Solution (W.S.) (1 gNO
2
/ml solution),
25.0 ml. Sodium Nitrite Solution (10 gNO
2
/ml) make up 250 ml. with Absorbing Reagent
Prepare fresh daily.
5.1 Known Standard Solution
Reagent Blank 0.0 g NO
2
10 ml. Absorbing Solution. + 1.0 ml. H
2
O
2
+ 10.0 ml. Sulphanilamide + 1.4 ml. NEDA and make
up 50.0 ml. with Distilled Water , with mixing after the addition of each reagent
1.0 g NO
2
1.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
2.0 g NO
2

2.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent+ 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
. 3.0 g NO
2
3.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
4.0 g NO
2
4.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
5.0 g NO
2
5.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
6.0 g NO
2
6.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
7.0 g NO
2
7.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
8.0 g NO
2
8.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
9.0 g NO
2
9.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
10.0 g NO
2
10.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
12.0 g NO
2
12.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
15.0 g NO
2
15.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
20.0 g NO
2

20.0 ml. (W.S.) make up 20.0 ml. with Absorbing Reagent. + 1.0 ml. H
2
O
2
+ 10.0 ml.
Sulphanilamide + 1.4 ml. NEDA and make up 50.0 ml. with Distilled Water , with mixing after
the addition of each reagent
Note: Here W.S. is working solution
Wait for 10.0 minute to color development interval, measure the Absorbance of Standard and
reagent blank at 540.0 nm wavelength against the distilled water
7. Calculation For Calibration Factor

Subtract the absorbance of Reagent Blank from the absorbance of the Standards. Plot corrected
absorbances against the Concentration of Standard Solution

Calibration Factor(Kc) = Conc.(g NO

2
) / Absorbance
8. Sample Analysis

Reagent Blank
10.0 ml. of Abs. sol. + 1.0 ml. H
2
O
2
+ 10.0 ml. Sulphanilamide + 1.4 ml. NEDA and make up
50.0 ml. with Distilled Water , with mixing after the addition of each reagent

Sample
10.0 ml. of Sample + 1.0 ml. H
2
O
2
+ 10.0 ml. Sulphanilamide + 1.4 ml. NEDA and make up
50.0 ml. with Distilled Water , with mixing after the addition of each reagent
Note: - Wait for 10.0 minute to color development interval, measure the Absorbance of Sample
and reagent blank at 540.0 nm wavelength against the distilled water
9. NOx Calculation Formula:
NO
x
(g/m
3
) = (As-Ao) x Kc x Vs x 1000
V
a
(liter) x Vt x 0.82
Here:-
Vs = Taken Volume of Absorbing Solution for sampling
Vt = Taken Volume of Absorbing Solution for Analysis
Va

=

Volume of Air = Avg. Flow rate (LPM) x Time (min)
As = Absorbance of Sample by Spectrophotometer
Ao = Absorbance of Sample Reagent Blank by Spectrophotometer
Kc = Calibration Factor
10. References
IS 5182 (Part 6): 2006
CPCB Guidelines for the Measurement of Ambient Air Pollutants Volume-I