加速溶剂萃取-气相色谱-质谱法测定固化涂料中有机挥发物残留量
GC-MS Determination of Residual Amounts of Volatile Organic Compounds in Solidified Paint with Accelerated Solvent Extraction
摘 要
提出了气相色谱-质谱法测定固化涂料中7种有机挥发物甲苯、乙苯、二甲苯、六甲基丙酮、3-乙氧基丙酸乙酯、6-甲基-2-庚酮和苯甲醇残留量的方法。样品经粉碎后用丙酮溶剂经加速溶剂萃取仪在50 ℃每次3 min连续萃取3次。采用HP-5MS色谱柱分离。7种有机挥发物的质量浓度分别在一定的范围内呈线性,方法的检出限(3S/N)在0.01~1.35 μg之间。以空白样品为基体,进行加标回收试验,回收率在84.4%~104%之间,测定值的相对标准偏差(n=6)在0.80%~13%之间。
有机挥发物
加速溶剂萃取
气相色谱-质谱法
Solidified paint
Volatile organic compounds
Accelerated solvent extraction
GC-MS
Abstract
Residual amounts of 7 volatile organic compounds, i.e., toluene, ethylbenzene, xylene, hexamethylacetone, 3-ethoxypropionate, 6-methyl-2-heptanone and benzylalcohol in solidified paint were determined by GC-MS. The sample was crushed and extracted (by ASE) thrice with acetone consecutively, at 50 ℃ for 3 min in each extraction. HP-5MS column was used for separation. Linear relationships between values of peak area and mass concentration of the 7 volatile organic compounds were kept in definite ranges, with detection limits (3S/N) in the range of 0.01-1.35 μg. Using blank sample as matrix, test for recovery was made by standard addition method, and values of recovery obtained were in the range of 84.4%-104%, with values of RSD′s (n=6) in the range of 0.80%-13%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 上海检验检疫科研专项(HK012-2012)
收稿日期 2013/4/9
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网络出版日期
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备注马腾洲(1980-),男,黑龙江哈尔滨人,工程师,硕士,研究方向为高分子材料检测。
引用该论文: MA Teng-zhou,CHEN Jun-shui,CHENG Yu-xiao,MA Ming,ZHANG Lin,SHEN Bo. GC-MS Determination of Residual Amounts of Volatile Organic Compounds in Solidified Paint with Accelerated Solvent Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(11): 1364～1367
马腾洲,陈俊水,程欲晓,马明,张琳,沈波. 加速溶剂萃取-气相色谱-质谱法测定固化涂料中有机挥发物残留量[J]. 理化检验－化学分册, 2013, 49(11): 1364～1367
被引情况:
【1】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)
【2】肖道清,马明,关荣发,曹国洲, "加速溶剂萃取-气相色谱法测定乙烯-乙酸乙烯共聚物塑料制品中甲酰胺残留量",理化检验－化学分册 52, 167-170(2016)
【3】肖道清,马 明,朱晓艳,曹国洲, "加速溶剂萃取-气相色谱-质谱法测定乙烯-乙酸乙烯共聚物制品中的苯乙酮",理化检验－化学分册 52, 463-465(2016)
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参考文献
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【4】DIN 55649-2001Paints and varnishes-determination of volatile organic compound contend in waterthinnable emulsion paints (In-can VOC)［S］.
【5】ASTM D3960-2005Standard practice for determining volatile organic compound (VOC) content of paints and related coatings［S］.
【2】BRUNO K, LESLIE S. Quality control system-requirements for a testing and inspection laboratory［M］. N.W.Washington: D.C. American Council of Independent Laboratories, 2006.
【3】LE SECH J, DUCRUET V, FEIGENBAUM A. Influence of dissolved gases in the dynamic headspace analysis of styrene and other volatile organic compounds and improvement of their determination［J］. Journal of Chromatography A, 1994,667(3):340-347.
【4】DIN 55649-2001Paints and varnishes-determination of volatile organic compound contend in waterthinnable emulsion paints (In-can VOC)［S］.
【5】ASTM D3960-2005Standard practice for determining volatile organic compound (VOC) content of paints and related coatings［S］.
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