Application of Stir Bar of Sorptive Extraction to Sampling of Residues of Combustion Adjuvants in Air over Fire Field
摘 要
对微吸附采样技术进行改进,采用带有活性炭/聚二甲基硅氧烷涂层的长度为20 mm的吸附萃取搅拌棒对火场空气中助燃剂残留物进行采集取样。将上述吸附萃取搅拌棒装于采集取样装置的前端,采集取样装置的后端与空气泵连接。在空气泵流量为50 mL·min-1,采集时间为60 s,采集温度为30℃的条件下进行采集取样。样品采集完成后,将吸附萃取搅拌棒直接放置于热分离进样杆中进样,对助燃剂残留物样品进行气相色谱-质谱法分析。当分析对象为汽油,采集时间为60 s时,方法的检出限(5S/N)为0.1 μL·L-1;当采集时间增加至300 s时,检出限(5S/N)可降至1 nL·L-1。分析95#汽油时,用AMDIS软件对总离子流色谱图进行分析,1 μL·L-1的汽油样品中检出400种特征化合物。除汽油外,还对航空煤油、柴油、乙醇和乙酸乙酯等助燃剂的残留物进行定性分析。
Abstract
As a modification for the micro-adsorption sampling technique, a stir bar of sorptive extraction, having a length of 20 mm and coated on its surface with activated carbon and poly-dimethylsiloxane, was used in the sampling of residues of combustion adjuvants in air over fire field. The stir bar of sorptive extraction was placed into the holder in the front position of the sampling device, which was connected with the air pump at the rear. Sampling of the sample was accomplished under the following conditions:(a) flow rate of air pump was 50 mL·min-1; (b) acquisition time was 60 s; and (c) acquisition temperature was 30℃. At the end of sampling, the stir bar of sorptive extraction was replaced into thermal separation probe of injection to have the sample of residues of combustion adjuvants for GC-MS analysis. As gasoline was the analyte and acquisition time of 60 s was taken, detection limit (5S/N) of the method of 0.1 μL·L-1 was attained, and detection limit (5S/N) could be lowered to 1 nL·L-1 when acquisition time of 300 s was taken. In analysis of 95# gasoline, with volume fraction of 1 μL·L-1, 400 characteristic compounds were detected from the TIC chromatogram with help of the soft ware AMDIS. Besides gasoline, aviation kerosene, diesel oil, ethanol and ethyl acetate were the 4 other combustion adjuvants, the residues of which were also be qualitatively analyzed by the proposed method.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201905004
所属栏目 工作简报
基金项目 上海市公安局科学技术发展基金(2016025)
收稿日期 2018/6/27
修改稿日期
网络出版日期
作者单位点击查看
备注赵晓雷,助理工程师,主要从事法庭科学理化检验工作,zhaoxiaolei1990@163.com
引用该论文: ZHAO Xiaolei,LÜ,Xiaobao,LI Yang,DAI Wei,SHEN Wenyi,WANG Changfu. Application of Stir Bar of Sorptive Extraction to Sampling of Residues of Combustion Adjuvants in Air over Fire Field[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(5): 520~525
赵晓雷,吕小宝,李阳,戴维,沈雯怡,王长富. 吸附萃取搅拌棒在火场空气中助燃剂残留物的采集取样中的应用[J]. 理化检验-化学分册, 2019, 55(5): 520~525
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】张怡,阳世群,祝兴华,等.汽油燃烧残留物标准样品制备及特征组分研究[J].化学研究与应用, 2017,29(6):836-840.
【2】SANDERCOCK P M L. Fire investigation and ignitable liquid residue analysis-A review:2001-2007[J]. Forensic Science International, 2008,176(2/3):93-110.
【3】祝兴华,王新刚,彭波.气相色谱-质谱联用仪分析火场残留物中的汽油成分[J].分析测试学报, 2007,26(增刊1):339-341.
【4】姜华.固相微萃取与气相色谱仪联用技术在火场助燃剂检验中的应用[J].刑事技术, 2006(6):25-26.
【5】邱榕.火场残留助燃剂的提取分离及气相色谱/质谱分析[J].中国安全生产科学技术, 2007,3(1):35-39.
【6】刁中文,邢若葵,王松才,等.自动热脱附气相色谱-质谱法分析火场助燃剂汽油成分[J].刑事技术, 2008(5):10-12.
【7】TOURON P, MALAQUIN P, GARDEBAS D, et al. Semi-automatic analysis of fire debris[J]. Forensic Science International, 2000,110(1):7-18.
【8】邢若葵,王松才,戴维列,等.纵火现场中汽油、煤油和柴油残留物的ATD/GC/MS法检测[J].中国司法鉴定, 2008(4):22-25.
【9】GORDIN A, AMIRAV A. SnifProbe:New method and device for vapor and gas sampling[J]. Journal of Chromatography A, 2000,903(1/2):155-172.
【10】夏攀,张成功,赵素丽,等.微吸附采样技术在测定放火现场助燃剂中的应用[J].理化检验-化学分册, 2014,50(10):1282-1285.
【11】张成功,王长富,凌友青,等.应用SPME-GC/MS检测放火现场中助燃剂的研究[J].中国司法鉴定, 2004(1):18-20.
【2】SANDERCOCK P M L. Fire investigation and ignitable liquid residue analysis-A review:2001-2007[J]. Forensic Science International, 2008,176(2/3):93-110.
【3】祝兴华,王新刚,彭波.气相色谱-质谱联用仪分析火场残留物中的汽油成分[J].分析测试学报, 2007,26(增刊1):339-341.
【4】姜华.固相微萃取与气相色谱仪联用技术在火场助燃剂检验中的应用[J].刑事技术, 2006(6):25-26.
【5】邱榕.火场残留助燃剂的提取分离及气相色谱/质谱分析[J].中国安全生产科学技术, 2007,3(1):35-39.
【6】刁中文,邢若葵,王松才,等.自动热脱附气相色谱-质谱法分析火场助燃剂汽油成分[J].刑事技术, 2008(5):10-12.
【7】TOURON P, MALAQUIN P, GARDEBAS D, et al. Semi-automatic analysis of fire debris[J]. Forensic Science International, 2000,110(1):7-18.
【8】邢若葵,王松才,戴维列,等.纵火现场中汽油、煤油和柴油残留物的ATD/GC/MS法检测[J].中国司法鉴定, 2008(4):22-25.
【9】GORDIN A, AMIRAV A. SnifProbe:New method and device for vapor and gas sampling[J]. Journal of Chromatography A, 2000,903(1/2):155-172.
【10】夏攀,张成功,赵素丽,等.微吸附采样技术在测定放火现场助燃剂中的应用[J].理化检验-化学分册, 2014,50(10):1282-1285.
【11】张成功,王长富,凌友青,等.应用SPME-GC/MS检测放火现场中助燃剂的研究[J].中国司法鉴定, 2004(1):18-20.
相关信息