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Statistically sound calibration curves for chromatographic methods involving negative response data.

Journal of chromatographic science (2011-08-24)
L E Vanatta, D C Cowles
ABSTRACT

A statistical procedure is presented for calibrating chromatographic methods that generate negative chromatographic peaks. The technique is illustrated via data collected during the ion-chromatographic analysis of the ammonium ion in methansulfonic-acid solutions. A peak-integration protocol is explained and subsequent regression data are presented. For the concentration range of 1 to 5 ppb, a quadratic model could be fitted to the calibration data, using ordinary least squares as the fitting technique. The precision was approximately ± 0.5 ppb, at 95% confidence.

MATERIALS
Product Number
Brand
Product Description

Supelco
Methanesulfonic acid concentrate, 0.1 M CH3SO3H in water (0.1N), eluent concentrate for IC
Sigma-Aldrich
Methanesulfonic acid solution, 70 wt. % in H2O
Sigma-Aldrich
Silver methanesulfonate
Sigma-Aldrich
Methanesulfonic acid, ≥99.0%
Sigma-Aldrich
Methanesulfonic acid solution, 4 M (with 0.2% (w/v) tryptamine)
Sigma-Aldrich
Potassium methanesulfonate, ≥98.0% (dry substance, T)
Sigma-Aldrich
Sodium methanesulfonate, 98%