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Published:Journal of Chromatographic Science, ISSN 0021-9665 Volume 47, Number 7, August 2009, pp. 498-504

United States Environmental Protection Agency Perchlorate Method 332.0 via Microbore and Capillary Chromatographic Formats: Statistical Evaluation of the Use of 18O-Perchlorate Internal Standard with Deionized-Water Matrices

L.E. Vanatta1 and R.W. Slingsby2
1Air Liquide-Balazs, Dallas, TX and
2Dionex Corporation, Sunnyvale, CA

A statistically sound evaluation is made of the United States Environmental Protection Agency’s perchlorate Method 332.0 by tandem ion chromatography–mass spectrometry–mass spectrometry. Two microbore formats and one capillary format are used with a deionized-water matrix. The evaluation is made for raw peak-area data and for analyte responses scaled by the internal standard, over an analyte concentration range of 0.25 to 200 µg/L. Results indicate that: (i) the internal-standard signal is suppressed by the analyte in both microbore formats; (ii) the analyte signal is not affected by the internal standard; (iii) models for the calibration curves usually contain bias; (iv) the measurement uncertainty is similar in magnitude for both the peak-area- and ratio-based curves.

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