Field measurement of nitrate in marine and estuarine waters with a flow analysis system utilizing on-line zinc reduction.

A sensitive reagent-injection flow analysis method for the spectrophotometric determination of nitrate in marine, estuarine and fresh water samples is described. The method is based on the reduction of nitrate in a micro column containing zinc granules at pH 6.5. The nitrite formed is reacted with sulfanilamide and N-(1-naphthyl)ethylene diamine (Griess reagent), and the resulting azo compound is quantified spectrophotometrically at 520 nm. Water samples in the range of 3-700 μg L(-1) NO(3)(-)-N can be processed with a throughput of up to 40 samples per hour, a detection limit of 1.3 μg L(-1) and reproducibility of 1.2% RSD (50 μg L(-1) NO(3)(-)-N, n=10). The proposed method was successfully applied for the determination of nitrate in estuarine waters and the reliability was assessed by the analyses of certified reference materials and recovery experiments. The method is suitable for waters with a wide range of salinities, and was successfully used for more than 3200 underway nitrate measurements aboard SV Pelican1 in the "Two Bays" cruise in January 2010.

[1]  S. Yao,et al.  A Novel Flow-Injection System for Simultaneous Determination of Nitrate and Nitrite Based on the Use of a Zinc Reductor and a Bulk Acoustic Wave Impedance Detector , 1998 .

[2]  J. Lambert,et al.  Differential Colorimetric Determination of Nitrite and Nitrate lons , 1960 .

[3]  Sarah M. Gray,et al.  Spectrophotometric Determination of Ammonia in Estuarine Waters by Hybrid Reagent‐Injection Gas‐Diffusion Flow Analysis , 2006 .

[4]  J. F. Staden Automated simultaneous determination of nitrate and nitrite by pre-valve reduction of nitrate in a flow-injection system , 1982 .

[5]  Paul J Worsfold,et al.  A compact flow injection analysis system for surface mapping of phosphate in marine waters. , 2002, Talanta.

[6]  P. Carr,et al.  Determinatlon of nitrate ion at the part per billion level in environmental samples with a continuous flow immobilized enzyme reaction. , 1976, Analytical chemistry.

[7]  B. Reis,et al.  Simultaneous determination of nitrate and nitrite by flow injection analysis , 1980 .

[8]  A. O. Rangel,et al.  Determination of nitrate and nitrite in dairy samples by sequential injection using an in-line cadmium-reducing column , 2006 .

[9]  Paul J. Worsfold,et al.  An automated spectrophotometric field monitor for water quality parameters: determination of nitrate , 1987 .

[10]  W. Horwath,et al.  Spectrophotometric Determination of Nitrate with a Single Reagent , 2003 .

[11]  A. Townshend,et al.  Spectrophotometric flow-injection determination of nitrate based on reduction with titanium(III) chloride , 1986 .

[12]  Henryk Temkin,et al.  Portable flow-injection analyzer with liquid-core waveguide based fluorescence, luminescence, and long path length absorbance detector , 2003 .

[13]  Paul J. Worsfold,et al.  Determination of carbon, phosphorus, nitrogen and silicon species in waters , 1994 .

[14]  S. Hirata,et al.  Portable flow-injection analyzer for nitrite and nitrate in natural water. , 2004, Analytical sciences : the international journal of the Japan Society for Analytical Chemistry.

[15]  K. Takeda,et al.  Determination of nitrate in natural waters with the photo-induced conversion of nitrate to nitrite , 1993 .

[16]  J. Miller,et al.  Statistics and chemometrics for analytical chemistry , 2005 .

[17]  Celio Pasquini,et al.  Flow-injection Determination Of Inorganic Forms Of Nitrogen By Gas Diffusion And Conductimetry , 1991 .

[18]  P. Nagaraja,et al.  Spectrophotometric Determination of Nitrate in Polluted Water Using a New Coupling Reagent , 2002, Analytical sciences : the international journal of the Japan Society for Analytical Chemistry.

[19]  C. E. López Pasquali,et al.  Two rapid and sensitive automated methods for the determination of nitrite and nitrate in soil samples , 2010 .

[20]  Sarah M. Gray,et al.  Underway determination of alkalinity in estuarine waters by reagent-injection gas-diffusion flow analysis , 2008 .

[21]  Leif G. Anderson,et al.  Simultaneous spectrophotometric determination of nitrite and nitrate by flow injection analysis , 1979 .

[22]  Pavel Mikusˇka,et al.  Flow-injection chemiluminescence determination of ultra low concentrations of nitrite in water , 1995 .

[23]  J. Lima,et al.  Construction and evaluation of ion selective electrodes for nitrate with a summing operational amplifier. Application to tobacco analysis. , 2001, Talanta.

[24]  A. Fischer,et al.  Corn leaf nitrate reductase--a nontoxic alternative to cadmium for photometric nitrate determinations in water samples by air-segmented continuous-flow analysis. , 2002, Environmental science & technology.

[25]  J. Lima,et al.  Sequential Injection Analysis-Based System for On-Line Monitoring of Nitrite and Nitrate in Wastewaters , 2000 .

[26]  S. Wakida,et al.  Simultaneous determination of nitrate and nitrite ions in seawater by capillary zone electrophoresis using artificial seawater as the carrier solution , 1999 .

[27]  F G Reyes,et al.  Polarographic determination of nitrate in vegetables. , 2000, Talanta.

[28]  P. Pratt,et al.  Simultaneous determination of nitrate and nitrite in biological samples by multichannel flow injection analysis. , 1995, Analytical biochemistry.

[29]  P. Worsfold,et al.  Multi-reflection photometric flow cell for use in flow injection analysis of estuarine waters , 2003 .

[30]  R. Carlson Continuous flow reduction of nitrate to ammonia with granular zinc , 1986 .

[31]  Wolfgang Frenzel,et al.  Re-Examination of the Cadmium Reduction Method and Optimisation of Conditions for the Determination of Nitrate by Flow Injection Analysis , 2004 .

[32]  F. R. Rocha,et al.  A green analytical procedure for flow-injection determination of nitrate in natural waters. , 2005, Talanta.

[33]  C. Stalikas,et al.  Ion chromatographic method for the simultaneous determination of nitrite and nitrate by post-column indirect fluorescence detection. , 2003, Journal of chromatography. A.

[34]  F. Nydahl On the reduction of oxygen in aqueous solution by electrolytically precipitated cadmium. , 1974, Talanta.

[35]  A. Vogel A text-book of quantitative inorganic analysis : including elementary instrumental analysis , 1961 .

[36]  H. V. Malmstadt,et al.  Automated determination of nitrate in waters with a reduction column in a microcomputer-based stopped-flow sample processing system , 1982 .

[37]  B. C. Madsen Utilization of flow injection with hydrazine reduction and photometric detection for the determination of nitrate in rain-water , 1981 .

[38]  J. A. Camargo,et al.  Nitrate toxicity to aquatic animals: a review with new data for freshwater invertebrates. , 2005, Chemosphere.

[39]  E. Gorodkiewicz,et al.  Simultaneous spectrophotometric determination of nitrite and nitrate in a flow-injection system , 1995 .

[40]  K. Kudo,et al.  Simultaneous determination of nitrate and nitrite in human plasma by gas chromatography-mass spectrometry. , 2002, Journal of analytical toxicology.