반도체용 과산화수소 중 음이온 분석을 위한 헤드스페이스 고상마이크로 추출법을 활용한 기체크로마토그래피-질량분석법 개발
Determinations of Trace Level Anions in Hydrogen Peroxide for Semiconductor by Headspace Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry
0
조회
0
다운로드
0
인용
0
참고문헌
키워드
초록
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
Abstract
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
참고문헌 (12)
- Occupational Safety & Health Research Institute, "Health management assistant for the workers in the semiconductor industry", 8~11 (2012)
- D. H. Yeum, "The behavior of hydrogen peroxide and ozone as oxidants in semiconductor wet cleaning chemicals", 석사, pp.1999
- I. J. Malik, "Particle removal from semiconductor surfaces by chemical-mechanical cleaning:setting the record straight", Particles on Surfaces:Detection, Adhesion and Removal, 6, pp.335~352 (1999)
- M. Ye, "Determination of trace anions in hydrogen peroxide by electrolysis treatment", Journal of Zhejiang University. Science edition, 31, pp.184~187 (2004)
- B. Zan, "Determination of trace anions in concentrated hydrogen peroxide using ion chromatography", Analytical Instrumentation, 139, pp.33~35 (2004)
- T. Meissner, "Capillary zone electrophoresis and ion chromatography in the low μg", L range applied to the determination of anions in hydrogen peroxide, 1998, pp.829, 351~357
- J. Kerth, "Determinations of trace anions in hydrogen peroxide", Journal of Chromatography A, 706, pp.191~198 (1995)
- D. Tsikas, "Determination of nitrite as pentafluorobenzyl derivative by RP-HPLC and UV detection with and without ion-pair extraction", Fresenius Journal of Analytical Chemistry, 344, pp.256~260 (1992)
- nitrosoalbumin as internal standard, "Journal of Chromatography B: Biomedical Sciences and Applications", 1999, 13~24
- Nitrite Enrichment and Concentration in Urine by Gas Chromatography Mass Spectrometry as Pentafluorobenzyl Derivatives, "Analytical Chemistry", 2010, 2585~2587
- X. Yang, "An improved mass spectrometrybased measurement of NO metabolites in biological fluids", Free Radical Biology & Medicine, 56, pp.1~8 (2013)