Indian Streams Research Journal
Vol - I , ISSUE - III [April 2011 ]
ISSN:-2230-7850 Available online at www.isrj.org
QUANTITATIVE ANALYSIS OF NITRITES USING ENVIRONMENTALLY
BENIGN PROCDURE
M. T. Bachute
Department of Chemistry, K. B. P. Mahavidyalaya, Pandharpur, Dist. Solapur(MS)
Abstract : An environmentally benign procedure has been developed for the quantitative
analysis of sodium nitrite and potassium nitrite. These nitrites were analysed quantitatively by
redox titration method in the presence of biocatalyst . The solution of nitrite was titrated
against 0.1 N potassium permanganate solution in the presence of paste of green peas as bio
catalyst and little volume of 2N sulphuric acid. The results obtained were comparable with
those obtained by routine procedure.
KEYWORDS : Quantitative , environmentally , municipal wastes, industrial wastes.
Introduction
Nitrite is present at trace level in soil, natural waters and plant and animal tissues. Their
presence in water can be a result of water processing or use of nitrite salts as corrosion inhibitors. To
surface waters they get from the same sources as nitrates, i.e. in municipal wastes, industrial wastes,
mining wastes and with water flowing in from artificially fertilized fields. Human saliva also small
amount of nitrite1
In pure form nitrite was first prepared by the Swedish Chemist Scheele2 by heating potassium nitrate at
red heat for half an hour [2 KNO3 KNO2 + O2].
Nitrites appear as intermediates in the nitrogen cycle. They are unstable and, depending on
conditions, are transformed into nitrates or ammonia. Nitrites are commonly used in preservatives. The
sources of ammonium ions in surface waters are reactions of biochemical decomposition of organic
nitrogen compounds, reduction of nitrites and nitrates by hydrogen sulfide, iron (II), humus substances
(or other reducing compounds) and, first of all, municipal wastes, industrial wastes and animal farm
wastes. Nitrogen compounds enhance eutrophication of surface waters. Organic nitrogen compounds
undergo biochemical decomposition into nitrites later oxidized to nitrates.3With realization of reaction
of nitrous acid with aromatic amines to form diazonium ions, nitrites gained importance in development
of organic chemistry in 19th century.4
The basic method for determination of nitrites in water samples, relies on the reaction of
nitrites with sulphanilic acid giving diazo compounds, which couples with 1-naphthylamine. The reaction
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Indian Streams Research Journal
Vol - I , ISSUE - III [April 2011 ]
ISSN:-2230-7850 Available online at www.isrj.org
gives an azo dye of intense red colour. There are other methods that are modifications of that proposed
by Griess, e.g.5,6 that involving the reaction with sulfanilamide and N-(1-naphthyl)-ethylenediamine).
HPLC7 with normal and reversed phase columns should also be mentioned. Ion chromatography has
become a standard method for determining anions and cations in water, air and solid samples. In 1984
the American Society for Testing Materials (ASTM)8 approved it as the standard method for determining
anions in water. There are a number of methods for determining NO2 - , NO3 - and NH4 + ions.
Determination of these analytes in the sample often poses analytical problems related to low selectivity
of the methods and the presence of many interfering factors.
There are reports3 on therapeutic uses of inorganic nitrites as vasodilator,antitode for cynide
and hydrogen sulphide poisoning,antimicrobial agents.
Therefore there is need to develop environmentally benign procedure for quantitative analysis
of inorganic nitrites. In view of this literature search revealed that biocatalyst like lipoxygenase enzyme
can be used as source of oxygen in redox volumetric analysis. Lipoxygenases are dioxygenating enzymes
found in plants9 like potato tuber, green peas, cucumber etc. and mammals like rats. They bring about
hydroperoxide formation fatty acids10 .Therefore we thought to use plant material containing
lipoxygenaseas catalyst in quantitative analysis of sodium nitrite and potassium nitrite.
PRESENT WORK
In the present work the solution of nitirite was titrated against 0.1NKMnO4 solution in the
presence of paste of green peas and little volume of sulphuric acid. It was necessary to heat the mixture
prior to titration
DETERMINATION OF AMOUNT OF NITRITE IN THE STOCK SOLUTION
Stock solution of nitrite was prepared by dissolving 1.1g of nitrite in 250cm3 distilled water.
Titration using routine procedure11
To potassium permanganate solution (0.1N, 10cm3) in a 500cm3 conical flask, was added
sulphuric acid solution (1N, 225cm3). This solution was heated to 40 to 500C and hot solution was
titrated against nitrite solution with constant stirring and slow addition till pink colour disappeared. Tip
of the burette was immersed deep in the KMnO4 solution. Three burette readings were recorded and CBR
was recorded as X cm3(Table III).
Table III
1 In Burette Nitrite solution
2 In conical flask 10 cm3 0.1N KMnO4 + 225 cm3 1N H2SO4
3 Indicator KMnO4 itself
4 End point Pink to colourless
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Indian Streams Research Journal
Vol - I , ISSUE - III [April 2011 ]
ISSN:-2230-7850 Available online at www.isrj.org
Burette Readings
For Sodium nitrite: Pilot Reading : 7.00 to 8.00 cm3
Level Burette Readings cm3 CBR Amount of
1 2 3 X cm3 NaNO2 found
Final 7.60 7.60 7.60
Initial 0.00 0.00 0.00 7.60 1.058g
Difference 7.60 7.60 7.60
For Potassium Nitrite: Pilot reading 11.00 to 12.00cm3
Level Burette Readings CBR Amount of
3
1 2 3 X cm KNO2 found
Final 11.60 11.60 11.40
Initial 0.00 0.00 0.00 11.60 1.099g
Difference 11.60 11.60 11.40
Titration using potato tuber pieces
To potassium permanganate solution (0.1N, 10cm3) in a 100cm3 conical flask, was added
sulphuric acid solution (1 N, 90cm3). To this solution potato pieces were added and the solution was
slowly titrated against nitrite solution with constant stirring till pink colour disappeared. Tip of the burette
was immersed deep in the KMnO4 solution. Three burette readings were recorded and CBR was recorded
as Y cm3 ( Table IV).
Table IV
1 In Burette Nitrite solution
2 In conical flask 10 cm3 0.1N KMnO4 + 90 cm3 1N H2SO4 + potato pieces( 0.5g
for NaNO2 and 2.00g for KNO2
3 Indicator KMnO4 itself
4 End point Pink to colourless
Burette Readings (In the presence of potato pieces)
For sodium Nitrite(Stock solution : 1.1g/250cm3) : Pilot Reading 7.00 to 9.00cm3
Level Burette Readings CBR Amount of
3 3 3 3
1 cm 2 cm 3 cm Y cm NaNO2 found
Final 7.90 7.90 7.80
Initial 0.00 0.00 0.00 7.90 1.098g
Difference 7.90 7.90 7.80
For potassium Nitrite(Stock solution : 1.1g/250cm3): Pilot Reading 11.00 to 12.00 cm3
Level Burette Readings CBR Amount of
3 3 3 3
1 cm 2 cm 3 cm X cm KNO2 found
Final 11.20 11.20 11.20
Initial 0.00 0.00 0.00 11.20 1.1g
Difference 11.20 11.20 11.20
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Indian Streams Research Journal
Vol - I , ISSUE - III [April 2011 ]
ISSN:-2230-7850 Available online at www.isrj.org
Calculations
A. For sodium nitrite
Factor used : 1 cm3 1N KMnO4 = 0.0345 g NaNO2
B. For potassium nitrite
Factor used 1 cm3 1N KMnO4 = 0.0445 g KNO2
DISCUSSION
Results show that results obtained from both procedure are nearly same. The catalysis of the reaction
may be probably due to the lipoxygenase enzyme present in the potato tuber. Lipoxygenase is a
dioxygenating enzyme because of which there may be increase in oxygen level in the reaction mixture.
Hence reaction occurs at room temperature.
Fuel saving:
Important thing in this procedure is that it is not necessary to heat the solution prior to
titration which is required in routine procedure. This saves a lot of fuel.
References
1. G. P. Uber, metadiamidobenzolals Regensaufsaltpetrigesaure, Chem Ber, 1878,11, 624.
2. C W Scheele, Chemische Abhandlung von der Luft und dem Feuer, Upsala Sweden: M.
Swerderus; 1777.
3. A. R. Butler, M. Feelisch, Circulation, 117, 2008, 2151.
4. DLH Williams, Nitrosation reactions and the chemistry of nitric oxide, London, UK : 2004.
5. M. J. Moorcroft , J. DAVIS and R G Compton, Detection and Determination of Nitrate and
Nitrite: A Review.Talanta, 54, 785, 2001.
6. H. Elbanowska H., J. Zerbeand J. Siepak, Physico-chemical analysis of water (in Polish),
UAM Printing House, Poznań, 1999.
7. M. C. Gennaro and S. Angelino Separation and Determination of Inorganic Anions by
Reversed-Phase High-Performance Liquid Chromatography (Review). J. Chromatogr. 789,
181, 1997).
8. American Society for Testing and Materials (ASTM), Philadelphia, PA. Annnual Book of
ASTM Standards, 1990.
9. Gillard T., Phytochemistry, 9, 1970, 1725.
10. Vick B. A. and Zimmerman D. C., Oxidative systems for the modification of fatty acids, 9,
1987, 53-90.
11. Vogel’s Text book of Inorganic Quantitative Chemical Analysis, revised by Jeffery G. H.,
Basset J., Mendham J.and Denny R. C.
