具有动态稀释功能的EA-IRMS联机系统在δ13C和δ15N测定中的应用

Application of Dynamic Dilution on δ13C and δ15N Measurements Using EA-IRMS System

  • 摘要: 自然界的样品中C、N元素含量或C/N变化极大,以往的元素分析稳定同位素比值质谱仪(EA-IRMS)大多采用固定比例稀释样品气,不仅需要预先了解样品中元素含量及C/N等信息,还需要精确控制取样量。为了提高样品分析效率,本实验初步建立了具有动态稀释功能的EA-IRMS联机系统,快速分析有机碳、总氮稳定同位素比值(δ13C和δ15N)。结果表明,该联机系统与传统的固定比例稀释方法的δ13C和δ15N测定结果一致性较好(p>0.05)。对于C/N差异较大或难以精确称重的9种样品,该联机系统的δ13C和δ15N测定结果具有良好的重复性。通过动态稀释,δ13C和δ15N的测定精度分别为0.07‰~0.32‰和0.05‰~0.27‰。该联机系统在不同时间(间隔45天)的测定结果再现性良好(p>0.05),δ13C和δ15N的测定偏差分别小于0.2‰和0.3‰。结合动态稀释功能的EA-IRMS,无需精确控制样品质量,省时、省力,具有一定的应用前景。

     

    Abstract: In natural environment, there are wide varieties in C and N element contents and carbon-nitrogen ratio (C/N) for different samples. Element analysis-stable isotope ratio mass spectrometry (EA-IRMS) is selected to dilute these sample gas through strict weight controls to keep the intensities of sample gas consistent with the reference gas. However, this kind of fixed dilution method is commonly time consuming and labor intensive. In this study, a fast analysis method of EA-IRMS equipped with a dynamic dilution component was established for the measurements of the bulk δ13C and δ15N, which was expected to improve the measurement efficiency. For comparison, different dilution ratios of 0 (no dilution), 57% (fixed dilution) and 0.96% (dynamic dilution) were set. To detect the repeatability of detection for δ13C and δ15N, nine kinds of samples (honey, pork fat, pork, chicken, hair, spinach, apple, soil and caffeine) were measured by the dynamic dilution method. As for reproducibility assessment at different times, the above samples were measured on 4th March and 19th April 2016, respectively. The results indicated that EA-IRMS had an identical measurement result for δ13C and δ15N through both the dynamic and fixed dilution methods (p>0.05). For the 9 kinds of samples with different mass and C/N values, the EA-IRMS gave good repetitions for δ13C and δ15N measurements. Based on the dynamic dilution method, the measurement precision ranged from 0.07‰ to 0.32‰ for δ13C, and 0.05‰ to 0.27‰ for δ15N, respectively. There was no significant time drifts for the new EA-IRMS equipped with the dynamic dilution component during the 45 days of study periods. During these two measurement periods, the differences were less than 0.2‰ for δ13C, and 0.3‰ for δ15N, respectively. Because it was unnecessary to accurately measure the mass of different kinds of samples, the new EA-IRMS equipped with a dynamic dilution component would have the advantages of time and labor saving. It should have a broad application prospect for the rapid measurements of δ13C and δ15N in future research.

     

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