Control of Precision in Head-space GC Determination of Volatile Organic Compounds in Water
摘 要
试验证明在顶空采样-气相色谱法测定水中挥发性有机物时出现的分析结果重现性差的原因在于所采用HP 7694E型顶空自动进样器加热方法的设计缺陷,对此提出了改进措施。通过用水浴预加热使整批样品温度达到与检测室温度(25±2) ℃接近,并选择顶空采样条件为55 ℃及15 min。按此条件对三氯甲烷、一溴二氯甲烷、二溴一氯甲烷及三溴甲烷等4种组分进行了测定,得到结果的相对标准偏差(n=5)在2.2%~3.3%之间。
Abstract
It was found that the precision of the results of determination of volatile organic compounds (VOC′s) in water samples by GC using the HP 7694E head space automatic sampler was poor and unsatisfactory, and that the cause was the designing defect of its heating device. Measure for improvement was proposed by preheating the water samples to a temperature close to the temperature of the detection chamber (25±2) ℃ in water bath, and setting the conditions of head-space sampling at 55 ℃ and 15 min. Four VOC′s (i.e. CHCl3, BrCHCl2, Br2CHCl and CHBr3) were determined under the prescribed conditions. Values of RSD′s (n=5) found were in the range of 2.2% to 3.3%.
中图分类号 O657.7
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收稿日期 2010/10/19
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备注顾福权(1980-),男,浙江绍兴人,工程师,主要研究方向为水质检测。
引用该论文: GU Fu-quan,HUANG Zhong,ZHOU Xiao-yan,SHEN Yan,CAI Hai-jiang,ZHU Shui-shun,TENG Fei. Control of Precision in Head-space GC Determination of Volatile Organic Compounds in Water[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(12): 1417~1419
顾福权,黄中,周晓燕,沈雁,蔡海江,诸水顺,滕飞. 顶空气相色谱法测定水中挥发性有机物的精密度控制[J]. 理化检验-化学分册, 2011, 47(12): 1417~1419
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参考文献
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【3】HOU D Y, TANG J F. Determination of halocarbons in drinking water by direct aqueous injection gas chromatography[J]. Anal Chen, 1991,63(18):2078-2080.
【4】张莘民,徐朝.气相色谱法直接进样测定饮用水中挥发性氯代烃[J].色谱, 2000,18(3):274-276.
【5】焦中志,陈忠林,刘丽君,等.自动顶空进样测定饮用水中挥发性卤代烃[J].给水排水, 2006,32(7):20-22.
【6】高建民,高建国,靳春林,等.自动顶空气相色谱法测定化妆品中的甲醇[J].化学分析计量, 2003,(12)3:7-10.
【7】吴伟都,金世梅,朱慧.自动进样顶空气相色谱法测定浓缩果汁中的乙醇[J]中国食品添加剂, 2004,(5):97-98.
【8】张思群,王志元,许毅.自动进样顶空气相色谱法连续测定食品中丙酸盐[J].分析检验, 2002,23(11):104-106.
【9】吴孟李,范坤,聂锦风,等.自动静态顶空-毛细管气相色谱法测定污水中甲醛的研究[J].长春大学学报, 2006,16(3):76-78.
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