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Validation data for the determination of perchlorate in water using ion chromatography with suppressed conductivity detection.
BACKGROUND: Perchlorate salts are relatively stable, soluble in water, and migrate into groundwater sources. Groundwater is an essential source for drinking water suppliers. Perchlorate bears health risks as it is identified to impair normal thyroid function by interfering with iodine uptake by the thyroid gland. The development of a sensitive analytical method for the determination of perchlorate is therefore of the highest interest or public health. Ion chromatography is a sensitive method suitable for perchlorate determinations. This manuscript describes the validation of an ion chromatographic method. Perchlorate is determined by ion chromatography (IC) with conductivity detection after suppression (CD) applying isocratic elution.
RESULTS: In this study, the suitability of IC-CD was tested for synthetic samples, selected environmental water, drinking water, and swimming pool water in order to evaluate potential matrix effects on the perchlorate signal even after sample preparation. A sample injection volume of 750 μL was applied to the selected 2-mm-IC column. In untreated samples, the perchlorate peak can be interfered by neighbouring signals from matrix ions like chloride, nitrate, carbonate, and sulphate. Depending on the concentration of the matrix ions, the perchlorate peak can show asymmetric shape in particular when the perchlorate concentration is low. Recovery is reduced with increasing matrix ion concentrations. Dedicated matrix elimination was applied to minimize such effects. A reporting limit of 1.5 μg/L perchlorate and an expanded measurement uncertainty of 13.2 % were achieved.
CONCLUSION: The extended method validation proves the applicability of IC based on the EPA 314.0 method for the determination of trace amounts of perchlorate in water samples of different origin. The results support the development of a respective international standard pursued by ISO. The approach evidenced its working robustness and ease of use in terms of eluent preparation, chromatographic resolution, column life time and sample preparation. Due to the simplified analytical workflow of the analytical procedure the application's integration into the collection of methods of interested laboratories should be facilitated.
RESULTS: In this study, the suitability of IC-CD was tested for synthetic samples, selected environmental water, drinking water, and swimming pool water in order to evaluate potential matrix effects on the perchlorate signal even after sample preparation. A sample injection volume of 750 μL was applied to the selected 2-mm-IC column. In untreated samples, the perchlorate peak can be interfered by neighbouring signals from matrix ions like chloride, nitrate, carbonate, and sulphate. Depending on the concentration of the matrix ions, the perchlorate peak can show asymmetric shape in particular when the perchlorate concentration is low. Recovery is reduced with increasing matrix ion concentrations. Dedicated matrix elimination was applied to minimize such effects. A reporting limit of 1.5 μg/L perchlorate and an expanded measurement uncertainty of 13.2 % were achieved.
CONCLUSION: The extended method validation proves the applicability of IC based on the EPA 314.0 method for the determination of trace amounts of perchlorate in water samples of different origin. The results support the development of a respective international standard pursued by ISO. The approach evidenced its working robustness and ease of use in terms of eluent preparation, chromatographic resolution, column life time and sample preparation. Due to the simplified analytical workflow of the analytical procedure the application's integration into the collection of methods of interested laboratories should be facilitated.
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