中文核心期刊

中国科技核心期刊

CSCD来源期刊

DOAJ 收录

Scopus 收录

刘玉龙, 黄燕高, 刘菲. 气相色谱法测试土壤中分段石油烃的标准化定量方法初探[J]. 岩矿测试, 2019, 38(1): 102-111. DOI: 10.15898/j.cnki.11-2131/td.201709040139
引用本文: 刘玉龙, 黄燕高, 刘菲. 气相色谱法测试土壤中分段石油烃的标准化定量方法初探[J]. 岩矿测试, 2019, 38(1): 102-111. DOI: 10.15898/j.cnki.11-2131/td.201709040139
Yu-long LIU, Yan-gao HUANG, Fei LIU. Analysis of Total Petroleum Hydrocarbon Fractions in Soils by Gas Chromatography: Standardized Calibration and Quantitation Method[J]. Rock and Mineral Analysis, 2019, 38(1): 102-111. DOI: 10.15898/j.cnki.11-2131/td.201709040139
Citation: Yu-long LIU, Yan-gao HUANG, Fei LIU. Analysis of Total Petroleum Hydrocarbon Fractions in Soils by Gas Chromatography: Standardized Calibration and Quantitation Method[J]. Rock and Mineral Analysis, 2019, 38(1): 102-111. DOI: 10.15898/j.cnki.11-2131/td.201709040139

气相色谱法测试土壤中分段石油烃的标准化定量方法初探

Analysis of Total Petroleum Hydrocarbon Fractions in Soils by Gas Chromatography: Standardized Calibration and Quantitation Method

  • 摘要: 目前土壤样品中分段石油烃的分析方法中石油烃包括的碳原子数范围和采用的校准物质不统一,造成不同实验室的量值不具有可比性。为保证不同实验室之间结果的可比性,本文尝试建立一种石油烃相邻碳原子数标准化定量方法。该方法主要包括:①规定了石油烃包括的碳原子数范围为气相色谱峰中正己烷和正四十碳烷之间所有的烃(含正己烷);②总石油烃(TPH)分为挥发性石油烃(VPH)和半挥发性石油烃(SPH),分别选取碳原子数为6~10的5个正构烷烃作为VPH校准物质,选取碳原子数为10~40的31个正构烷烃作为SPH校准物质。采用平均响应因子法或一次线性回归法,建立校准物质的峰面积-浓度的校准关系;③采用相邻峰标准化校准方法,逐一定量所有的目标色谱峰;④计算正构烷烃含量、总石油烃含量和任意分段的石油烃含量。该方法为环境样品中石油烃分析方法的标准化建设提供了数据基础。

     

    Abstract:
    BACKGROUNDInter-laboratory measurement results of total petroleum hydrocarbons (TPH) in soils determined by current Gas Chromatography-Flame Ionization Detector, are not comparable due to specified TPH ranges of alkanes and/or different calibration standards between laboratories.
    OBJECTIVESTo establish a standardized calibration and quantitation method of TPH and to develop the adjacent-peak calibration and quantitation method (APCQM).
    METHODSThe APCQM mainly includes:(1) defining TPH range as all compounds eluting between n-hexane and n-tetracontane; (2) division of TPHs into volatile petroleum hydrocarbons (VPH) and semivolatile petroleum hydrocarbons (SPH). Specify and calibrate procedure of TPH. Reference materials (RM) for VPH are 5 n-alkanes, from n-hexane to n-decane, whereas SPH RMs are 31 n-alkanes, from n-decane to n-tetracontane. Calibration equations of peak area and concentration of n-alkanes can be constructed by average response factor or linear regression methods; (3) quantitative concentrations of all target chromatographic peaks acquired by adjacent standard peak calibration; (4) calculation of the contents of n-alkanes, TPH and optional TPH fractions.
    RESULTSUsing the normal calibration and quantitation method, TPH recoveries of laboratory fortified blanks and laboratory fortified sample matrices could be underestimated or overestimated by 10%. By using the APCQM the paradox in quality control processes was resolved, and thus reliable measurement results of TPH were obtained in laboratories.
    CONCLUSIONSThe APCQM is applicable to standardization analysis of TPH fractions in environmental samples.

     

/

返回文章
返回