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荧光光谱法分析油气化探样品中的芳烃

Analysis of Aromatic Hydrocarbons in Oil and Gas Geochemical Exploration Samples by Fluorescence Spectrometry

  • 摘要: 荧光光谱法避免了色谱法所需的大量分离工作,具有灵敏度高、检测限低、分析速度快等特点,非常适用于油气化探样品分析。本文对常规荧光光谱分析的样品前处理方法和仪器测定参数进行优化,建立了适用于测定油气化探样品中芳烃的荧光光谱分析方法。实验采用农残级正己烷作为溶剂,简化了溶剂提纯操作,采用振荡器间歇振荡方式有效地提高了芳烃的提取效果。在优化的仪器条件下对油气化探样品中的芳烃进行检测,选择萘、菲、 (䓛) 三种标准物质,采用单点外标法对样品激发波长265 nm,发射波长为320 nm、360 nm、405 nm的三个特征光谱峰进行定量分析,测定结果采用量化后的浓度值代替常用的荧光强度值,使不同实验室、不同型号仪器间的荧光指标具有统一的定量标准,提高了数据的可比性。本方法检测限为1.8 ng/g(以萘计算),优于行业标准(SY/T 6009.8—2003)规定的检出限≤2 ng/g要求,方法精密度(RSD,n=12)为4.5%(320 nm)、9.6%(360 nm)、14.7%(405 nm)。通过质量控制与质量管理体系的完善,本方法已经在大庆地区油气化探工作中得到实际应用,荧光指标对样品采样深度确定及异常点发现具有良好的指示作用。

     

    Abstract: Fluorescence spectrometry, with the characteristics of high sensitivity, low detection limits and rapid analysis, avoids complex separating work in the chromatography method, and is suitable for oil and gas geochemical exploration samples requiring a large number of assays. In this paper, sample pretreatment methods and analytical conditions that were optimized in order to analyse aromatic hydrocarbons in oil samples by fluorescence spectrometry are reported. Ultra pesticide residue grade n-hexane was selected as the extraction solvent, which simplified the purification operation, and intermittent oscillation was selected to improve the extraction effect of aromatics. Through selecting proper standard materials (naphthalene, phenanthrene and chrysene) and adopting an external standard method, aromatic hydrocarbon in the samples was determined under the optimal analytical conditions. With the excitation wavelength of 265 nm and the emission wavelength of 320 nm, 360 nm and 405 nm, the fluorescent spectra of aromatic hydrocarbon were studied. The relative intensities were converted into the concentration of a certain standard material, which could then be used to compare the fluorescence data between different laboratories and different instruments. The detection limit of the method was 1.8 ng/g (naphthalene), which was lower than the limit of the national industry standard (2.0 ng/g, SY/T 6009.8—2003). The precision results of the method (RSD, n=12) were 4.5% (320 nm), 9.6% (360 nm) and 14.7% (405 nm), respectively. Through improving the quality control and management, the proposed method has been conducted successfully in the Daqin oil field, and it was found that the fluorescent data could effectively indicate sampling depth and anomalies.

     

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