반도체용 과산화수소 중 음이온 분석을 위한 헤드스페이스 고상마이크로 추출법을 활용한 기체크로마토그래피-질량분석법 개발

An ultrasensitive method to detect trace anions (fluoride, nitrite and nitrate) in hydrogen peroxide (H2O2) for semiconductor by headspace solid phase microextraction (HS-SPME) gas chromatography-mass spectrometry (GC-MS) was described. Fluoride, nitrite and nitrate in hydrogen peroxide reacted with pentafluorobenzyl bromide (PFB-Br) in a headspace vial and the formed PFB derivatives were vaporized and adsorbed onto a fiber. The optimal HS-SPME conditions were achieved with a 50/30 μm divinylbenzene-carboxen- polydimethylsiloxan (DVB-CAR-PDMS) fiber, 50 μL of PFB-Br (99%), 100 μL of 10% tetraoctylammonium bromide (10%) as a phase transfer catalyst, an extraction/derivatization temperature of 90oC, a heating time of 50 min, and a pH of 6.0. Under the established conditions, the method detection limits of fluoride, nitrite and nitrate were 2.8-4.0 μg/L in 30% H2O2 solutions (w/w) and the relative standard deviations were less than 4% at concentrations of 25 and 50 μg/L. The concentrations of anions in five concentrated H2O2 had detectable levels of 8.7 to 28.4 μg/L. The method was sensitive, reproducible and simple enough to permit the reliable routine analysis of anions in hydrogen peroxide for semiconductor