Simple determination of hydrazine in waste water by headspace solid-phase micro extraction and gas chromatography-tandem mass spectrometry after derivatization with trifluoro pentanedione

- New single peak derivatization method of hydrazine with 1,1,1-trifluoro-2,4-pentanedione in wastewater for HS-SPME.
- Easy manipulation and amenable to automation.
- This method requires no solvent for sample extraction and is environmentally friendly.
- This method shows low interference due to the use of HS-GC-MS/MS.

A headspace solid-phase micro extraction (HS-SPME) and gas chromatography-tandem mass spectrometric (GC-MS/MS) method is described to detect hydrazine after derivatization with 1,1,1-trifluoro-2,4-pentanedione (1,1,1-TFPD) to 3-methyl-5-(trifluoromethyl) pyrazole in industrial waste water. The following optimal HS-SPME conditions were used: 85 μm-carboxen-polydimethylsiloxane fibre, 100 mg L−1 TFPD, saturated NaCl, an extraction/derivatization temperature of 80 °C, a heating time of 40 min, and a pH of 9.5. Under the established conditions, the detection and quantification limits were 0.002 μg L−1 and 0.007 μg L−1 by using 5 mL of waste water and the intra- and inter-day relative standard deviations were less than 10.2% at concentrations of 0.02 and 0.1 μg L−1. The calibration curve showed good linearity, with r2 = 0.998; the accuracy was in the range of 98.0-103%; and the precision of the assay was less than 10.2% in industrial waste water. Hydrazine was detected over a concentration range of 0.011-0.074 μg L−1 in 5 of 20 waste water samples.

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