title: Simple determination of hydrazine in waste water by headspace solid-phase micro extraction and gas chromatography-tandem mass spectrometry after derivatization with trifluoro pentanedione.
abstract: 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-1TFPD, 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-1and 0.007 μg L-1by 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-1in 5 of 20 waste water samples.
authors.affiliation: Department of Environmental Science, Kongju National University, Kongju, 314-701, Republic of Korea.
authors.forename: Jin-Aa
authors.initials: JA
authors.lastname: Oh
authors.affiliation: Department of Environmental Education, Kongju National University, Kongju, 314-701, Republic of Korea. Electronic address: hshin@kongju.ac.kr.
authors.forename: Ho-Sang
authors.initials: HS
authors.lastname: Shin
keywords: Gas chromatography-tandem mass spectrometry; Headspace solid-phase micro extraction; Hydrazine; Industrial waste water