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  • Simultaneous determination of total nitrogen and total phosphorus in environmental waters using alkaline persulfate digestion and ion chromatography.

Simultaneous determination of total nitrogen and total phosphorus in environmental waters using alkaline persulfate digestion and ion chromatography.

Journal of chromatography. A (2014-12-03)
Brian M De Borba, Richard F Jack, Jeffrey S Rohrer, Joan Wirt, Dongmei Wang
ABSTRACT

An ion chromatography (IC) method was developed for the simultaneous determination of total nitrogen and total phosphorus after alkaline persulfate digestion. This study takes advantage of advances in construction of high-resolution, high-capacity anion-exchange columns that can better tolerate the matrices typically encountered when a determination of total nitrogen and total phosphorous is required. Here, we used an electrolytically generated hydroxide eluent combined with a high-capacity, hydroxide-selective, anion-exchange column for the determination of total nitrogen (as nitrate-N) and total phosphorus (as phosphate-P) in environmental samples by IC. This method yielded LODs for nitrate-N and phosphate-P of 1.0 and 1.3 μg/L, respectively. The LOQs determined for these analytes were 3.4 and 4.2 μg/L, respectively. Due to the dilution factor required and the blank nitrate-N concentration after the persulfate digestion, the quantification limits increased for nitrate-N and phosphate-P to 171 and 63 μg/L, respectively. The suitability of the method was evaluated by determining the nitrogen and phosphorus concentrations from known concentrations of organic-containing nitrogen and phosphorus compounds. In addition, environmental samples consisting of six different wastewaters and 48 reservoir samples were evaluated for total nitrogen and phosphorus. The recoveries of nitrogen and phosphorus from the organic-containing compounds ranged from 93.1 to 100.1% and 85.2 to 97.1%, respectively. In addition, good correlation between results obtained by the colorimetric method and IC was also observed. The linearity, accuracy, and evaluation of potential interferences for determining TN and TP will be discussed.

MATERIALS
Product Number
Brand
Product Description

Nicotinic acid, analytical standard
Glycine, ACS reagent, ≥98.5%
Glycine
Sigma-Aldrich
Urea-12C, 99.9 atom % 12C
Ammonium chloride, Molecular Biology, suitable for cell culture, ≥99.5%
Urea solution, 40 % (w/v) in H2O
Nicotinic acid, BioReagent, suitable for cell culture, suitable for insect cell culture, suitable for plant cell culture, ≥98%
Millipore
Urea solution, suitable for microbiology, 40% in H2O
Sodium hydroxide, reagent grade, ≥98%, pellets (anhydrous)
Sodium hydroxide solution, 50% in H2O
Sodium hydroxide, BioUltra, suitable for luminescence, ≥98.0% (T), pellets
Sodium hydroxide solution, 49-51% in water, eluent for IC
Sodium hydroxide, pellets, semiconductor grade, 99.99% trace metals basis
Sodium hydroxide solution, purum, ≥32%
Sodium hydroxide solution, 5.0 M
Sodium hydroxide, reagent grade, 97%, flakes
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
Sodium hydroxide, ACS reagent, ≥97.0%, pellets
Sodium hydroxide solution, BioUltra, Molecular Biology, 10 M in H2O
Sodium hydroxide, beads, 16-60 mesh, reagent grade, 97%
Sodium hydroxide, reagent grade, 97%, powder
Sodium hydroxide, puriss. p.a., ACS reagent, K ≤0.02%, ≥98.0% (T), pellets
Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture
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Ammonium chloride, 99.998% trace metals basis
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