Sensitive determination of hydrazine in water by gas chromatography–mass spectrometry after derivatization with ortho-phthalaldehyde

Abstract

A gas chromatography–mass spectrometric (GC–MS) method has been established for the determination of hydrazine in drinking water and surface water. This method is based on the derivatization of hydrazine with ortho-phthalaldehyde (OPA) in water. The following optimum reaction conditions were established: reagent dosage, 40mgmL−1 of OPA; pH 2; reaction for 20min at 70°C. The organic derivative was extracted with methylene chloride and then measured by GC–MS. Under the established condition, the detection and the quantification limits were 0.002μgL−1 and 0.007μgL−1 by using 5.0-mL of surface water or drinking water, respectively. The calibration curve showed good linearity with r2=0.9991 (for working range of 0.05–100μgL−1) and the accuracy was in a range of 95–106%, and the precision of the assay was less than 13% in water. Hydrazine was detected in a concentration range of 0.05–0.14μgL−1 in 2 samples of 10 raw drinking water samples and in a concentration range of 0.09–0.55μgL−1 in 4 samples of 10 treated drinking water samples.