Electron capture detector based on a non-radioactive electron source: Operating parameters vs. Analytical performance

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Abstract

Gas chromatographs with electron capture detectors are widely used for the analysis of electron affine substances such as pesticides or chlorofluorocarbons. With detection limits in the low pptv range, electron capture detectors are the most sensitive detectors available for such compounds. Based on their operating principle, they require free electrons at atmospheric pressure, which are usually generated by a β- decay. However, the use of radioactive materials leads to regulatory restrictions regarding purchase, operation, and disposal. Here, we present a novel electron capture detector based on a non-radioactive electron source that shows similar detection limits compared to radioactive detectors but that is not subject to these limitations and offers further advantages such as adjustable electron densities and energies. In this work we show first experimental results using 1,1,2-trichloroethane and sevoflurane, and investigate the effect of several operating parameters on the analytical performance of this new non-radioactive electron capture detector (ECD).

Figures

  • Figure 1. Schematic of our electron capture detector with our nonradioactive electron source with orthogonal (a) and axial (b) gas flow.
  • Figure 2. SNR over the electron emission current from 10 to 40 nA with an applied collector voltage of 3 V and 50 ppbv 1,1,2- trichloroethane. The electron source acceleration voltage is Uacc = 10 kV.
  • Figure 3. SNR over the acceleration voltage from 8 to 12 kV with an applied collector voltage of 3 V and 50 ppbv 1,1,2- trichloroethane. The electron emission current is constantly controlled to Iemis = 40 nA.
  • Figure 5. Signal amplitude of the detector response over collector voltage calculated by the difference between the detector signals with pure nitrogen as carrier gas and nitrogen containing 220 ppbv 1,1,2-trichloroethane.
  • Figure 4. Detector signals with pure nitrogen as carrier gas (solid red line) and nitrogen containing 220 ppbv 1,1,2-trichloroethane (dashed blue line) over collector voltage.
  • Figure 6. Standard deviation σ of the measured noise (black dots) and the resulting signal-to-noise ratio (red triangles) over collector voltage.
  • Figure 7. Resulting signal amplitudes over the analyte concentration for 1,1,2-trichloroethane (a) and sevoflurane (b) for sample gas flows of 5, 10 and 30 mls min−1.
  • Table 1. LoDs for 1,1,2-trichloroethane and sevoflurane for sample gas flows between 5 and 30 mls min−1 for a measuring time of 200 ms and Ucol = 5 V.

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CITATION STYLE

APA

Bunert, E., Kirk, A. T., Oermann, J., & Zimmermann, S. (2017). Electron capture detector based on a non-radioactive electron source: Operating parameters vs. Analytical performance. Journal of Sensors and Sensor Systems, 6(2), 381–387. https://doi.org/10.5194/jsss-6-381-2017

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