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Test method for Analysis of HNO2 Content in Concentrated Nitric Acid
Scope
This method is applicable for measuring of HN02 content in CAN.
Principle of the Method
 | CNA Sample is titrated against 0.1 N KMnO4 in presence on 20% H2S04
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 | HNO2 Gets Oxidised to HNO3 and in the process Mn (7+) is reduced to Mn (2+). This leads to Discoloration of KMnO4 Solution.
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 | 5HNO2+2KMnO4+3H2SO4=> K2SO4+2MnSO4+5HNO3+3H2O i.e. 5NO2- +2MnO4- +6H = 2Mn+5NO3- +3H2O. |
Reference Document
Textbook of Quantitative Inorganic Analysis by Vogel, 4th Edition.
Reagents
KMn04 0.1 N Solution 20% H2S04.
Apparatus
1. Erlenmeyer Flask Size 250 ml.
2. Pipette 25 ml.
3. Burette
Procedure
Take 100 ml Distilled water in an Erlenmeyer flask. Add 25 ml of 20 % H2S04. Shake well & Add 25 ml CNA Sample. Quickly Titrate against 0.1 N KMn04 Solution to a distinct pink colour that persists for at least three minutes.
Calculation
%HNO2=(ml of KMnO4)*N of KMnO4*.0235*100 / (Simple Volume)*(Density of CNA )
Remarks
1. Density of CNA should be determined separately.
2. If CNA contains more HNO2 (Evident from Brown Colour) take 10 ml of sample.
3. Owing to the slow self-decomposition of CNA the HNO2 content increases during storage.
4. 0.1 N KMnO4 should be standardised daily with previously dried A.R. Grade Oxalic Acid / Mono sodium oxalate. |