High-precision analysis of SF 6 at ambient level

  • Lim J
  • Moon D
  • Kim J
  • et al.
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Abstract

Abstract. This work reports on the development of a technique for the precise analysis of ambient SF6. This technique, which involves a gas chromatograph/electron capture detector (GC-ECD) coupled with an Activated Alumina-F1 (AA-F1) column, performed well in the measurements, particularly in terms of accuracy, which complies with the World Meteorological Organization (WMO)-recommended compatibility of 0.02 ppt. Compared to the Porapak Q technique, we observed a sharper peak shape for the SF6 stream, which substantiates the improvement in the analytical precision. The traceability to the WMO scale was tested by calibrating the GC-ECD/AA-F1 analyser using five SF6 standards provided by the WMO/Global Atmosphere Watch (GAW) Central Calibration Laboratory (CCL) for SF6 (NOAA, United States of America). After calibration by various methods, the GC-ECD/AA-F1 accurately estimated the mole fraction of SF6 in the working standard prepared by the World Calibration Centre for SF6 operated by the Korea Meteorological Administration (KMA)/Korea Research Institute of Standards and Science (KRISS). Among the calibration methods, the two-point calibration method emerged to be the most economical procedure in terms of the data quality and measurement time. It was found that the KRISS scale of SF6/N2 was biased by 0.13 ppt when compared to the WMO scale of SF6/air; this bias is probably due to a different matrix.

Figures

  • Fig. 1. Schematic diagram of the experimental setup. Using the regulator without a gauge, the unwanted contribution of gases moored in the dead volume was expected to be reduced. Two restrictors virtually isolated the instrument from variation in the ambient conditions of the lab and, therefore, lead to reasonable repeatability of the measur ment results. EPC and ECD stand for the el ctronic pr ssure controller and electron capture detector, respectively. A series of measurements were performed while manually switching the left cylinder betweem sample and standard.
  • Fig. 2. Chromatograms taken using the GC-ECD coupled with two different types of columns installed in the GC.
  • Table 1. Repeated measurement of reference and sample in order to compensate for instrumental drift between measurement cycles; every area data point is a result of three successive analyses.
  • Fig. 3. Pe k rea plot as a function of the assigned mole fraction of the WMO standards. The response curve was approximated by a least square fit of a second-order polynomial with an agreement of R2 = 0.99981. Residuals are listed in Table 2.
  • Table 2. Analytical results of SF6 standard gases from the NOAA.
  • Fig. 5. Chromatogram of a working standard (CC315007, red) overlaid on one of the five WMO cylinders (FB03443, blue)
  • Fig. 4. Trace bility chain of SF6 from the C stations.
  • Table 3. Calculated result of SF6 in the working standard CC315007 depending on the calibration methods that are referred to the WMO scale. Unit is ppt.

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APA

Lim, J. S., Moon, D. M., Kim, J. S., Yun, W.-T., & Lee, J. (2013). High-precision analysis of SF 6 at ambient level. Atmospheric Measurement Techniques, 6(9), 2293–2299. https://doi.org/10.5194/amt-6-2293-2013

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