顶空固相微萃取-气相色谱法测定废水中挥发性脂肪酸
GC Determination of Volatile Fatty Acids in Waste Water with HS-SPME
摘 要
提出了顶空固相微萃取-气相色谱法测定废水中挥发性脂肪酸(乙酸、丙酸、丁酸、戊酸、异戊酸和己酸)的含量。为使固相微萃取达到更高的效率,选择极性85 μm PA作为微萃取头的涂层,微萃取系在pH 1.5的试液中进行,萃取温度及时间为25 ℃和20 min,在20 mL试样溶液中加入氯化钠3.5 g作为盐析剂。用Stabilwax-DA毛细管色谱柱分离,火焰离子检测器检测。6种脂肪酸在一定的质量浓度范围内与其峰面积呈线性关系,相对标准偏差(n=10)均小于10.0%。
顶空固相微萃取
挥发性脂肪酸
废水
GC
HS-SPME
Volatile fatty acids
Waste water
Abstract
GC with headspace-solid phase micro-extraction (HS-SPME) was applied to the determination of 6 fatty acids, i.e., acetic acid, propionic acid, butyric acid, pentanoic acid, isopentanoic acid and hextanoic acid, in waste water. To attain a higher efficiency in SPME, the polar 85 μm PA coating was selected for the micro-extractor, and the extraction was carried out at 25 ℃ for 20 min from the sample solution having the acidity of pH 1.5, and with addition of 3.5 g of NaCl to 20 mL of sample solution as salting out agent. The analyte were separated with Stabilwax-DA capillary column and detected by FID. Linear relationships between values of peak area and mass concentration of 6 fatty acids were kept in definite ranges. Values of RSD′s (n=10) of the 6 fatty acids found were less than 10.0%.
中图分类号 O657.7
所属栏目
基金项目 重庆师范大学博士启动基金(09XLB023)
收稿日期 2009/11/19
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备注冯琳(1963-),女,四川温江人,博士,副教授,主要研究方向为环境分析化学。
引用该论文: FENG Lin. GC Determination of Volatile Fatty Acids in Waste Water with HS-SPME[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(1): 86～89
冯琳. 顶空固相微萃取-气相色谱法测定废水中挥发性脂肪酸[J]. 理化检验－化学分册, 2011, 47(1): 86～89
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参考文献
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【3】TAKAI T, HIRATA A, YAMAUCHI K, et al. Effects of temperature and volatile fatty acids on nitrification-denitrification activity in small-scale anaerobic-aerobic recirculation biofilm process［J］. Water Sci Technol, 1997,35(6):101-108.
【4】VENKATA M S, CANDRASEKHARA R N, KRISHNA P K, et al. Anaerobic treatment of complex chemical wastewater in a sequencing batch biofilm reactor: process optimization and evaluation of factor interactions using the taguchi dynamic DOE methodo-logy［J］. Biotechnology and Bioengineering, 2005,90(6):732-745.
【5】PAN L, PAWLISZYN J. Derivatization/solid-phase microextraction: new approach to polar analytes［J］. Anal Chem, 1997,69(2):196-205.
【6】张廉奉,李秀娟,刘翠霞,等.三甲基杯[6]芳烃固相微萃取气相色谱法测定土壤中的多环芳烃［J］.分析化学, 2007,35(9):1269-1273.
【7】PAN L, ADAMS M, PAWLISZYN J. Determination of fatty acids using solid-phase microextraction［J］. Anal Chem, 1995,67(23):4396-4400.
【8】YO S P. Analysis of volatile fatty acids in wastewater collected from a pig farm by a solid phase microextraction method［J］. Chemosphere,1999,38(4):823-834.
【9】ABALOS M, BAYONA J M, PAWLISZYN J. Deve-lopment of a headspace solid-phase microextraction procedure for the determination of free volatile fatty acids in waste waters［J］. J Chromatogr A, 2000,873(1):107-115.
【10】ABALOS M, BAYONA J M. Application of gas chromatography coupled to chemical ionization mass spectrometry following headspace solid-phase microextraction for the determination of free volatile fatty acids in aqueous samples［J］. J Chromatogr A, 2000,891(2):287-294.
【11】MILLS G A, WALKER V, MUGHAL H. Headspace solid-phase microextraction with 1-pyrenyldiazomethane in-fibre derivatisation for analysis of faecal short-chain fatty acids［J］. J Chromatogr B, 1999,730(1):113-122.
【12】PINHO O, FERREIRA I, FERREIRA M A. Solid-phase microextraction in combination with GC-MS for quantification of the major volatile free fatty acids in ewe cheese［J］. Anal Chem, 2002,74(20):5199-520.
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