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다중 모세관을 이용한 교정용 표준가스의 제조: 불확도와 유효성 평가

Generation of calibration standard gases using capillary gas divider: uncertainty measurement and method validation

  • 이상윤 ((주)리가스 가스분석과학연구소) ;
  • 황은진 ((주)리가스 가스분석과학연구소) ;
  • 정혜자 ((주)리가스 가스분석과학연구소) ;
  • 이광우 ((주)리가스 가스분석과학연구소) ;
  • 전기준 (한국표준과학연구원 삶의질표준부)
  • Lee, Sangyun (Research Institute of Gas Analytical Science Co.) ;
  • Hwang, Eun-Jin (Research Institute of Gas Analytical Science Co.) ;
  • Jung, Hye-Ja (Research Institute of Gas Analytical Science Co.) ;
  • Lee, Kwang-Woo (Research Institute of Gas Analytical Science Co.) ;
  • Chun, Ki-Joon (Korea Research Institute of Standard and Science)
  • Received : 2006.07.26
  • Accepted : 2006.08.11
  • Published : 2006.10.28

Abstract

ISO 6145-5에 의거한 동적 부피 측정법을 이용하여 교정용 혼합가스를 제조하고 그 불확도를 평가하였다. 내경 0.25 mm, 길이 50 cm 규격의 10개의 모세관을 병렬 배치하고, 성분 가스와 희석 가스가 흐르는 모세관 개수를 조절하는 방법으로 혼합 가스의 희석 비율을 결정하였다. 모세관은 각종 가스에 대하여 낮은 흡착 용량을 가진 PTFE 재질의 것을 사용하였으며, 유로의 설정은 열을 발생시키지 않는 mechanical valve를 사용하였다. ISO 6145-5의 요건을 구현하는 본 장치를 이용하여 제조된 희석 가스의 농도는 (주)리가스에서 제조한 마스터급 표준가스를 이용하여 비교 평가하였다. ISO 6143의 비교법을 이용한 교정 후 제조된 산소 표준가스의 농도 편차는 대부분의 희석 영역에서 상대비 0.2% 이내, 황화수소 표준가스의 농도 편차는 상대비 1% 이내임을 확인하였다. 이 결과는 본 장치를 통해 제조한 표준가스가 대기환경 측정용 등 저농도 표준가스를 이용한 교정 곡선 획득용으로 사용하는데 충분한 성능을 가지고 있음을 증명하는 것이다.

Calibration gas mixtures were prepared using dynamic volumetric method according to ISO 6145-5 and the uncertainty was evaluated. Ten identical capillaries with 0.25 mm in inner diameter and 50 cm in length were applied in this system. Dilution ratio of parent gas was determined by the number of capillaries that passes parent gas and that passes balance gas through. Capillaries were made of Teflon which had good chemical stability against adsorption of gaseous substances. Mechanical valves were introduced in this system in order to minimize the thermal effect of solenoid valves. Concentration of prepared gases were compared with master grade standard gases in cylinders made by RiGAS Co. and calibration of the instrument were completed using comparison method according to ISO 6143. Experimental results showed that the coefficient of variance of diluted oxygen standard gases showed less then 0.2% in most dilution range, that of diluted hydrogen sulfide standard gases showed less then 1.0%. Therefore, it is proven that the standard gases prepared by this system are appropriate to be used as a calibration standards in ambient monitoring, etc.

Keywords

References

  1. ISO 6142 Gas Analysis-Preparation of calibration gas mixtures-Gravimetric method
  2. ISO 6144 Gas analysis-Preparation of calibration gas mixtures-Static volumetric method
  3. ISO 6145 Gas Analysis-Preparation of calibration gas mixtures using dynamic volumetric methods
  4. ISO 6145-2 Gas analysis-Preparation of calibration gas mixtures using dynamic volumetric methods-Part 2: Volumetric pumps
  5. ISO 6145-4 Gas analysis-Preparation of calibration gas mixtures using dynamic volumetric methods-Part 4: Continuous syringe injection method
  6. ISO 6145-5 Gas analysis-Preparation of calibration gas mixtures using dynamic volumetric methods-Part 5: Capillary calibration devices
  7. ISO 6145-6 Gas analysis-Preparation of calibration gas mixtures using dynamic volumetric methods-Part 6: Critical orifices
  8. ISO 6145-7 Gas analysis-Preparation of calibration gas mixtures using dynamic volumetric methods-Part 7: Thermal mass-flow controllers
  9. ISO 6145-8 Gas analysis-Preparation of calibration gas mixtures using dynamic volumetric methods-Part 8: Diffusion method
  10. ISO 6145-9 Gas analysis-Preparation of calibration gas mixtures using dynamic volumetric methods-Part 9: Saturation method
  11. ISO 6145-10 Gas analysis-Preparation of calibration gas mixtures using dynamic volumetric methods-Part 10: Permeation method
  12. ISO 6143 Gas Analysis-Comparison methods for determining and checking the composition of calibration gas mixtures
  13. ISO Guide 35 Certification of reference materials-General and statistical principles