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악취측정용 10 μmol/mol 황화수소 표준가스 개발

Development of 10 μmol/mol Hydrogen Sulfide Primary Standard Gas for Odor Measurements

  • 김용두 (한국표준과학연구원 화학의료표준본부) ;
  • 배현길 (한국표준과학연구원 화학의료표준본부) ;
  • 김달호 (한국표준과학연구원 화학의료표준본부) ;
  • 오상협 (한국표준과학연구원 화학의료표준본부) ;
  • 이진홍 (충남대학교) ;
  • 이상일 (한국표준과학연구원 화학의료표준본부)
  • Kim, Yong-Doo (Center for Gas Analysis, Korea Research Institute of Standards and Scence (KRISS)) ;
  • Bae, Hyun-Kil (Center for Gas Analysis, Korea Research Institute of Standards and Scence (KRISS)) ;
  • Kim, Dalho (Center for Gas Analysis, Korea Research Institute of Standards and Scence (KRISS)) ;
  • Oh, Sang-Hyub (Center for Gas Analysis, Korea Research Institute of Standards and Scence (KRISS)) ;
  • Lee, Jin Hong (Department of Environmental Engineering, Chungnam National University) ;
  • Lee, Sangil (Center for Gas Analysis, Korea Research Institute of Standards and Scence (KRISS))
  • 투고 : 2017.12.21
  • 심사 : 2018.04.06
  • 발행 : 2018.04.30

초록

산업이 급속하게 발전함에 따라 자연 대기에서 악취를 유발하는 매우 적은 양의 황화수소가 존재합니다. 매립 및 하폐수처리장에서 나오는 황화수소 성분은 대기에 존재하므로 많은 민원이 발생됩니다. 민원이 발생하는 악취가스를 측정하기 위해 $10{\mu}mol/mol$ 농도 수준의 황화수소 인증표준물질(Certified reference material)을 개발하고자 하였다. 질소 안에 $10{\mu}mol/mol$ 수준의 황화수소 가스 제조는 ISO 6142에 의한 중량법을 사용하였다. 4 개의 알루미늄 실린더에 가스 CRM을 제조하고 GC-AED로 그 농도를 확인했습니다. 제조의 불확도는 0.50 % 미만이었고, 제조일치성은 0.22 %이었다. 실린더의 내부 흡착은 1500 psi에서 0.10 %이었고 1 년 동안 장기간 안정한 것으로 평가되었다. 이 황화수소 CRM의 제조 일치성, 실린더의 흡착 및 장기 안정성에 대한 상대 확장불확도는 1.05 %(신뢰도 95 %, k = 2) 이내로 개발되었다.

Hydrogen sulfide from landfill and sewage treatment plant is a major odor component and causes many civil petitions. Rapidly developing industries release hydrogen sulfide, an odorous gas, to the atmosphere. This study aims to develop a $10{\mu}mol/mol$ concentration level hydrogen sulfide primary standard gas for odor measurement. The hydrogen sulfide gas was prepared at a nominal concentration of $10{\mu}mol/mol$ in nitrogen using the gravimetric method described in ISO 6142. Replicate standard gases were produced in 4 aluminium cylinders, and their concentrations were verified by GC-AED. The uncertainty of production was less than 0.50 %, and the variation of the 4 replicates was 0.22 %. The wall adsorption of hydrogen sulfide in cylinders was 0.10 % at 1500 psi, and the concentration was estimated to be long-term stable for one year. The relative expanded uncertainty of the preparation consistency, adsorption and long-term stability of this hydrogen sulfide standard gas was less than 1.05 % (95 % of confidence level, k=2).

키워드

참고문헌

  1. "Clean air environment conservation act", Odor emission standards, (2005)
  2. Choi, Y. N., Kim, Y. D., Kim, M. R., Heo. G. S., "Development of on-line continuous measuring method for hydrogen sulfide in ambient air", Korean Journal of Odor Research and Engineering, Cheongju, 213-219, (2010)
  3. Poruthoor, S. K.; Dasgupta, P. K.; Genfa, Z., "Indoor air pollution and sick building syndrome. monitoring aerosol protein as a measure of bio aerosols", Environmental science & technology, 32(8);1147-1152, (1998) https://doi.org/10.1021/es9710058
  4. L.S.S. Nunes, T.M. Tavares, J. Dippel, W. Jaeschke., "Measurements of atmospheric aoncentrations of reduced sulphur compounds in the all saints bay area in bahia", Brazil, J. Atmos. Chem, 50, 79-100, (2005) https://doi.org/10.1007/s10874-005-3123-0
  5. Richard I. Masel., "Principles of adsorption and reaction on solid surfaces. Wiley interscience", New York, (1996)
  6. ISO 6142., "Gas analysis-preparation of calibration gas mixtures-weighing methods", (2001)
  7. Rhoderick, G.C., "Long-term stability of hydrocarbons in NIST gas standard reference material (SRM) 1800", Analytical and bioanalytical Chemistry, 383(1), 98-106. (2005) https://doi.org/10.1007/s00216-005-3381-3
  8. ISO/IEC., Guide 98-3 "Uncertainty of measurement, Guide to the expression of uncertainty in measurement", (2008)
  9. ASTM D7652-11., "Determination of trace hydrogen sulfide, carbonyl sulfide, methyl mercaptan, carbon disulfide and total sulfur in hydrogen fuel by gas chromatography and sulfur chemiluminescence detection", ASTM International, Pennsylvania, (2011)
  10. M.J.T. Milton, G.M. Vargha, A.S. Brown., "Gravimetric methods for the preparation of standard gas mixtures". Metrologia, 48, R1-R9, (2011) https://doi.org/10.1088/0026-1394/48/5/R01
  11. N. Matsumoto, T. Watanabe, M. Maruyama, Y. Horimoto, T. Maeda, K. Kato., "Development of massmeasurement equipment using an electronic mass comparator for gravimetric preparation of reference gasmixtures". Metrologia, 41, 178-188. (2004) https://doi.org/10.1088/0026-1394/41/3/011
  12. ISO 6143., "Gas Analysis-comparison methods for determining and checking the composition of calibration gas mixtures", (2001)
  13. Heo, G. S., You, Y. M., Y. D., Kim, "Evaluation of measurement uncertainties in analysis of trace sulfur compounds", Korean Journal of Odor Research and Engineering, 3(1), 31-40, (2004)
  14. Woo, J. C., Oh, S. H., Kim, B. M., Bae, H. K., Kim, K. S., Kim, Y. D., "Measurement uncertainty for QC/QA applied to the chemical analysis", Analytical science & technology, 18(6), 475-482, (2005)
  15. M.J.T.Milton, F.Guenther, W.R.Miller, A.S. Brown., "Validation of the gravimetric values and uncertainties of independently prepared primary standard gas mixtures", Metrologia, 43, L7-L10, (2006) https://doi.org/10.1088/0026-1394/43/3/N01
  16. Kim, Y. D., Heo, G. S., Lee, Sangil., Han, Wu, Konopelko, Kustikov, Malginov, Gromova, Pankratov, Pavlov, Botha., "Final report on international key comparison APMP.QM-K41(10 umol/mol Hydrogen sulfide in Nitrogen)". Metrlogia, Vol. 51, 08012, (2014) https://doi.org/10.1088/0026-1394/51/1A/08012
  17. "Development and dissemination of reference materials., Korea Research Institute of Standard and Science", KRISS/IR-2004-011, (2004)
  18. Franklin R Guenther, Walter R Miller, David L. Duewer, Gwi Suk Heo, Yongdoo Kim, M.H. van der Veen, Leonid Konopelko, Yury Kustikov, Nina Shor, Chris Adriaan Brookes, Martin Milton, Florbela Dias, Han Qiao., "International comparison CCQM-K41(Hydrogen sulfide in Nitrogen)", Metrlogia, 44, 08004, (2007) https://doi.org/10.1088/0026-1394/44/1A/08004