吹扫捕集-气相色谱-质谱法同时测定土壤中27种挥发性有机物
GC-MS Determination of 27 Volatile Organic Compounds in Soil with Purge and Trap Concentrator
摘 要
应用吹扫捕集-气相色谱-质谱法测定土壤中27种挥发性有机物的含量。选定在25 ℃条件下吹扫捕集11 min,取样品溶液5 mL于吹扫瓶中,利用Tekmar Stratum吹扫捕集器直接进样,经TR-5MS毛细管色谱柱分离,电子轰击电离(EI)全扫描和选择离子扫描检测,内标法进行定量测定。27种挥发性有机物的质量浓度与其峰面积在一定的浓度范围内呈线性关系,方法检出限(3S/N)在0.077~0.69 μg·kg-1之间。样品加标平均回收率在86.5%~117.5%之间,相对标准偏差(n=7)在1.6%~8.2%之间。
吹扫捕集
挥发性有机物
土壤
GC-MS
Purge and trap
Volatile organic compounds
Soil
Abstract
The Tekmar Stratum purge and trap concentrator was used in GC-MS determination of 27 volatile organic compounds (VOC′s) in soil. Temperature and time for purge and trap were set at 25 ℃ and 11 min respectively. Five mL. of sample solution were transferred to the purge and trap bottle and introduced into the instrument for GC-MS analysis. The VOC′s were separated on the TR-5MS capillary column and detected by the modes of full-scanning and selective ion-scanning. Internal standard was adopted in the determination. Linear relationships between peak areas and mass concentration of 27 VOC′s were obtained in definite ranges, with detection limits (3S/N) in the range of 0.077-0.69 μg·kg-1. Tests for recovery were made by addition of standard VOC′s to sample matrixes; values of recovery obtained were in the range of 86.5%-117.5%. Values of RSD′s (n=7) found for the VOC′s were in the range of 1.6%-8.2%.
中图分类号 O657.63
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收稿日期 2010/7/14
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备注李丽君(1972-),女,辽宁朝阳人,硕士,高级工程师,主要从事有机分析工作。
引用该论文: LI Li-jun,SONG Li-hua,WANG Hai-jiao,ZHU Bin. GC-MS Determination of 27 Volatile Organic Compounds in Soil with Purge and Trap Concentrator[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(8): 937～941
李丽君,宋丽华,王海娇,祝彬. 吹扫捕集-气相色谱-质谱法同时测定土壤中27种挥发性有机物[J]. 理化检验－化学分册, 2011, 47(8): 937～941
被引情况:
【1】王娜,李丽君,宋丽华,马建生, "吹扫捕集-气相色谱-质谱法测定地下水中的挥发性有机物",理化检验－化学分册 52, 607-611(2016)
【2】赵历,莫少芳,钟少枢, "静态顶空-气相色谱法测定阅读材料中的总挥发性有机化合物",理化检验－化学分册 51, 987-990(2015)
【3】李永亮,李健,李桂莲,于亭亭, "吹扫捕集-气相色谱法测定水稻田土壤中的敌稗",理化检验－化学分册 52, 1073-1075(2016)
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参考文献
【1】EPA Method 5035Closed-system purge and trap and extraction for volatile organics in soil and waste samples［S］．
【2】EPA Method 8260BVolatile organic compounds by chromatography/mass spectrometry (GC/MS)［S］．
【3】LIGOR M, BUSZEWSKI B. Study of VOC distribution in citrus fruits by chromat ographic analysis［J］. Anal Bioanal Chem, 2003(376):668-672．
【4】RAO B P S, ANSARI F, ANKAM S, et al. Estimating fugitive emission budget of volatile organic carbon (VOC ) in a petroleumrefinery［J］. Environ Contam Toxicol, 2005(75):127-134．
【5】MASS OLD E, BAHR C, SALTHAMMER T, et al. Determination of VOC and T VOC in air using thermal desorption GC-MS practical implications for test chamber experiments ［J］. Chromatographia, 2005(62):75-85．
【6】GELDERMANN J, TREITZ M, SCHOLLENBERGER H, et al. Evaluati on of VOC recovery strategies［J］. OR Spectrum, 2006(28):3-20．
【7】孙华.顶空气相色谱法测定土壤中挥发性有机物［J］.环境科学与管理, 2003,33(6):134-137．
【8】贾静,饶竹.吹扫捕集-气相色谱/质谱法测定土壤中挥发性有机化合物［J］.岩矿测试, 2008,27(6):413-417．
【9】秦宏兵,顾海东,尹燕敏.吹扫捕集气相色谱质谱法测定土壤中挥发性有机物［J］.中国环境监测, 2009,25(4):38-41．
【10】刘慧,朱优峰,徐晓白,等.吹扫-捕集气质联用法测定北京郊区土壤中挥发性有机物［J］.复旦大学学报, 2003,42(6):856-860．
【11】刘劲松,孙晓慧,叶伟红,等.高速公路两侧农业土壤中挥发性有机化合物污染研究［J］.分析测试学报, 2007,26:213-214．
【12】刘梅,贾静,饶竹,等.土壤样品挥发性有机物定量分析时基体的选择及处理研究［J］.分析试验室, 2009,28(8):32-35．
【13】殷月芬,文凌飞,李必芬,等.土壤中挥发性有机化合物的GC-MS测定［J］.分析测试学报, 2003,22(1):86-88．
【14】卢迎红.土壤中挥发性有机物的测定-吹脱-捕集GC/MS法［J］.辽宁农业科学, 2005(2):22-24．
【2】EPA Method 8260BVolatile organic compounds by chromatography/mass spectrometry (GC/MS)［S］．
【3】LIGOR M, BUSZEWSKI B. Study of VOC distribution in citrus fruits by chromat ographic analysis［J］. Anal Bioanal Chem, 2003(376):668-672．
【4】RAO B P S, ANSARI F, ANKAM S, et al. Estimating fugitive emission budget of volatile organic carbon (VOC ) in a petroleumrefinery［J］. Environ Contam Toxicol, 2005(75):127-134．
【5】MASS OLD E, BAHR C, SALTHAMMER T, et al. Determination of VOC and T VOC in air using thermal desorption GC-MS practical implications for test chamber experiments ［J］. Chromatographia, 2005(62):75-85．
【6】GELDERMANN J, TREITZ M, SCHOLLENBERGER H, et al. Evaluati on of VOC recovery strategies［J］. OR Spectrum, 2006(28):3-20．
【7】孙华.顶空气相色谱法测定土壤中挥发性有机物［J］.环境科学与管理, 2003,33(6):134-137．
【8】贾静,饶竹.吹扫捕集-气相色谱/质谱法测定土壤中挥发性有机化合物［J］.岩矿测试, 2008,27(6):413-417．
【9】秦宏兵,顾海东,尹燕敏.吹扫捕集气相色谱质谱法测定土壤中挥发性有机物［J］.中国环境监测, 2009,25(4):38-41．
【10】刘慧,朱优峰,徐晓白,等.吹扫-捕集气质联用法测定北京郊区土壤中挥发性有机物［J］.复旦大学学报, 2003,42(6):856-860．
【11】刘劲松,孙晓慧,叶伟红,等.高速公路两侧农业土壤中挥发性有机化合物污染研究［J］.分析测试学报, 2007,26:213-214．
【12】刘梅,贾静,饶竹,等.土壤样品挥发性有机物定量分析时基体的选择及处理研究［J］.分析试验室, 2009,28(8):32-35．
【13】殷月芬,文凌飞,李必芬,等.土壤中挥发性有机化合物的GC-MS测定［J］.分析测试学报, 2003,22(1):86-88．
【14】卢迎红.土壤中挥发性有机物的测定-吹脱-捕集GC/MS法［J］.辽宁农业科学, 2005(2):22-24．
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