Hostname: page-component-cd9895bd7-q99xh Total loading time: 0 Render date: 2024-12-24T00:42:01.384Z Has data issue: false hasContentIssue false

Determination of nitrate in sea water by cadmium-copper reduction to nitrite

Published online by Cambridge University Press:  11 May 2009

E. D. Wood
Affiliation:
Department of Oceanography, University of Washington, Seattle
F. A. J. Armstrong
Affiliation:
The Plymouth Laboratory, England
F. A. Richards
Affiliation:
Department of Oceanography, University of Washington, Seattle

Extract

An accurate, dependable determination of 0–60 μg-at./l. of NO3-N in sea water has been developed. The sample is treated with tetrasodium ethylenediaminetetraacetate solution and passed through a column of copperized cadmium filings. A nearly quantitative reduction of nitrate to nitrite results. Nitrite is then determined by a diazotization method. Neither sulphide nor high nitrite concentrations interferes. Approximately eight samples per hour per column can be analysed with a standard deviation of 0.12 μg-at./l. at the 20 μg-at./l. level.

Introduction

Accurate determinations of nitrate ions in sea water have been difficult, especially under shipboard conditions.

The colorimetric method described by Harvey (1926, 1930) and improved by Cooper (1932), Zwicker & Robinson (1944), and others uses strychnidine in concentrated sulphuric acid to produce a red colour. The reagent lacks reliable sensitivity, because it is dependent on the rates of mixing and cooling.

In a method by Armstrong (1963), the absorbance of nitrosyl chloride in the UV region is measured with a spectrophotometer. While the method is good for small samples containing high concentrations of nitrate, the use of concentrated sulphuric acid and lack of sensitivity limit its use in routine analysis.

A method in which nitrate is quantitatively reduced to nitrite would be advantageous, because nitrite can be readily determined by the sensitive diazotization method proposed by Griess (1879). Several such methods have been proposed. FØyn (1951), Vatova (1956), and Chow & Johnstone (1962) used zinc powder for the reduction, but the reduction is sensitive to temperature, and it is necessary to centrifuge or filter each sample.

Type
Research Article
Copyright
Copyright © Marine Biological Association of the United Kingdom 1967

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Armstrong, F. A. J., 1963. The determination of nitrate in water by ultra-violet spectrophotometry. Analyt. Chem., Vol. 35, pp. 1292–4.CrossRefGoogle Scholar
Austin, K. H. & Strickland, J. D. H., 1959. The direct estimation of ammonia in sea water with notes on ‘reactive’ iron, nitrate, and inorganic phosphorus. J. Cons. perm. int. Explor. Mer, Vol. 24, pp. 446–9.Google Scholar
Bendschneider, K. & Robinson, R. J., 1952. A new spectrophotometric determination of nitrite in sea water. J. mar. Res., Vol. 11, pp. 8796.Google Scholar
Brewer, P. G. & Riley, J. P., 1965. The automatic determination of nitrate in sea water. Deep-Sea Res., Vol. 12, pp. 765–72.Google Scholar
Chow, T. J. & Johnstone, M. S., 1962. The determination of nitrate in sea water. Analytica chim. acta, Vol. 27, pp. 441–6.CrossRefGoogle Scholar
Cooper, L. H. N., 1932. The determination of nitrate in the sea by reduced strychnine. J. mar. biol. Ass. U.K., Vol. 18, pp. 161–6.CrossRefGoogle Scholar
Flaschka, H. A., 1959. EDTA Titrations. New York: Pergamon Press. 138 pp.Google Scholar
FØyn, E., 1951. Nitrogen determinations in sea-water. FiskDir. Skr., Ser. HavundersØk., Bd. 9, No. 14, pp. 17.Google Scholar
Grasshoff, K., 1964. Zur Bestimmung von Nitrat in Meer- und Trinkwasser. Kieler Meeresforsch., Bd. 20, No. 1, pp. 511.Google Scholar
Griess, P., 1879. Bemerkungen zu der Abandlung der H. N. Weselsky und Benedikt ‘Uber einige Azoverbindungen’. Ber. dt. chem. Ges., Bd. 12, pp. 426–8.CrossRefGoogle Scholar
Harvey, H. W., 1926. Nitrate in the sea. J. mar. biol. Ass. U.K., Vol. 14, pp. 7188.CrossRefGoogle Scholar
Harvey, H. W., 1930. Nitrate in the sea. II. J. mar. biol. Ass. U.K., Vol. 15, pp. 183190.CrossRefGoogle Scholar
Morris, A. W. & Riley, J. P., 1963. The determination of nitrate in sea-water. Analytica chim. acta, Vol. 29, pp. 272—279.CrossRefGoogle Scholar
Mullin, J. B. & Riley, J. P., 1955. The spectrophotometric determination of nitrate in natural waters with particular reference to sea water. Analytica chim. acta, Vol. 12, pp. 464–80.CrossRefGoogle Scholar
Pötzl, L. & Reiter, R., 1960. Eine einfache Methode zur Bestimmung von NitratIonen im atmospharischen Niederschlag und in Aerosol-Kondensaten mit Anwendungauf Probleme der Luftelektrizitat wahrend Niederschlagen. Z. Aerosol Forsch. u. -Ther., Bd. 8, pp. 252–64.Google Scholar
Shinn, M. B., 1941. A colorimetric method for the determination of nitrite. Ind. Engng Chem., analyt. Edn, Vol. 13, pp. 33–5.CrossRefGoogle Scholar
Strickland, J. D. H. & Parsons, T. R., 1965. A manual of seawater analysis, 2nd ed. revised. Bull. Fish. Res. Bd Can., No. 125, 203 pp.Google Scholar
Vatova, A., 1956. Elektrophotometrische Nitratbestimmung im Meerwasser mit dem Photometer ‘Elko II’. Dt. hydrogr. Z., Bd. 9, pp. 194–8.CrossRefGoogle Scholar
Zwicker, B. M. G. & Robinson, R. J., 1944. The photometric determination of nitrate in sea water with a strychnidine reagent. J. mar. Res., Vol. 5, pp. 214–32.Google Scholar