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Selection of Calibration Approaches and Their Impact on the Quantification of Unknown Samples: Case Study on Reduced Sulfur Gases

환원황화합물의 분석과 검량기준의 선택에 따른 오차발생의 특성

  • Jo, Hyo-Jae (Department of Environment & Energy, Sejong University) ;
  • Hong, One-Feel (Department of Environment & Energy, Sejong University) ;
  • Kim, Ki-Hyun (Department of Environment & Energy, Sejong University)
  • 조효재 (세종대학교 환경에너지융합학과) ;
  • 홍원필 (세종대학교 환경에너지융합학과) ;
  • 김기현 (세종대학교 환경에너지융합학과)
  • Received : 2010.06.16
  • Accepted : 2011.01.12
  • Published : 2011.04.30

Abstract

In this study, different calibration approaches for reduced sulfur compounds (RSCs) were investigated by using thermal desorption coupled with gas chromatography (GC) and pulsed flame photometric detection (PFPD). To evaluate the effects of calibration procedures, gaseous standards of 4 RSCs ($H_2S$, $CH_3SH$, DMS, and DMDS) prepared at 10 ppm level were analyzed at 7 loading injection volumes (40, 60, 80, 100, 160, 240, and 320 ${\mu}L$). The results were then compared with calibration curves made with the Z (zero offset) and N (non-zero offset) method. The concentrations of unknown samples were then quantified by using R (ratio) method in which the slope values are compared between standards and samples. Secondly, in A (average) method, results obtained from a multi-point analysis of unknown samples were also averaged to extract representative values for each sample. Results of both experiments showed that analytical error of low molecular weight components (such as $H_2S$ and $CH_3SH$) was greatly expanded with the Z method. In conclusion, the combined application of N-A method was the more realistic approach to reduce biases in the quantification of RSCs.

Keywords

References

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