표제지
목차
Chapter I. 서론 13
Chapter II. 이론적 배경 17
1. HCl의 물리적·화학적 특성 17
2. 푸리에변환 적외선분광기(FTIR) 18
3. 중량법 제조방법 21
Chapter III. 염화수소가스(HCl) 100 μmol/mol 인증표준물질 개발 26
1. 실험방법 및 재료 26
1.1. 인증표준물질 개발 절차 26
1.2. 원료가스 순도분석 및 재료 27
1.3. 전자저울의 성능 및 불확도 31
1.4. 제조 시스템 구성 33
1.5. HCl 혼합가스에 대한 분석 기술 34
1.6. 안정도 평가 방법 39
2. 결과 및 고찰 40
2.1. 원료가스의 순도분석 결과 40
2.2. 중량법 제조 결과 42
2.3. FTIR을 이용한 혼합가스의 농도 및 표준분산 평가 52
2.4. FTIR을 이용한 HCl 혼합가스의 내부일치성 평가 53
2.5. 온라인 IC법을 이용한 HCl 혼합가스 분석기술 확립 58
2.6. 임핀저 IC법을 이용한 HCl 혼합가스의 검증 60
2.7. HCl 100 μmol/mol 혼합가스의 안정도 평가 64
3. 결론 및 토의 64
Chapter IV. 독성가스(NO, NO₂, SO₂, HCl)의 흡착량 평가 67
1. 실험 및 방법 67
1.1. 원료가스 및 재료 67
1.2. 표준가스 제조 68
1.3. 가스시료의 흡착량 분석 69
2. 결과 및 고찰 73
2.1. NO, NO₂ 및 SO₂ 가스의 실린더 표면 흡착량 분석 73
2.2. HCl 혼합가스의 실린더 표면 흡착량 분석 75
2.3. 실린더 표면의 중금속 성분 분석 79
3. 결론 및 토의 82
Chapter V. 흡착성 가스의 장기 안정성 평가 84
1. 시료 도입부분의 변경 84
2. 안정성 규명에 관한 연구 85
3. HCl 혼합가스의 실린더 내 장기 안정성 평가 91
4. 인증표준물질의 인증값 및 불확도 평가 93
5. 결론 및 토의 96
VI. 결론 98
References 102
ABSTRACT 106
APPENDIX 109
Table 1. Physical properties of hydrogen chloride. 17
Table 2. Analytical condition for impurity test of high purity HCl. 30
Table 3. Uncertainty budget of the mass measurement. 33
Table 4. Analytic condition for the 100 μmol/mol HCl gas mixture by... 36
Table 5. Composition of the high purity HCl source gas used in this study. 40
Table 6. Composition of the pure nitrogen gas used in this study. 41
Table 7. List of gravimetrically prepared 1 cmol/mol HCl in N₂ gas... 43
Table 8. List of gravimetrically prepared 1000 μmol/mol HCl in N₂ gas... 44
Table 9. List of gravimetrically prepared 100 μmol/mol HCl in N₂ gas... 45
Table 10. The calculation equations for the first dilution step used in... 46
Table 11. The calculation equations for the second dilution step used in... 47
Table 12. The calculation equations for the third dilution step used in... 48
Table 13. List of the quantities used in calculation for the first dilution step. 49
Table 14. List of the quantities used in calculation for the second dilution step. 50
Table 15. List of the quantities used in calculation for the third dilution step. 51
Table 16. List of the selected HCl gas mixtures for the... 53
Table 17. FTIR measurement results of 1 cmol/mol HCl gas mixtures. 53
Table 18. FTIR measurement results of 1,000 μmol/mol HCl gas... 55
Table 19. FTIR measurement results of 100 μmol/mol HCl gas mixtures. 57
Table 20. HCl gas sampling conditions used in impinger system. 61
Table 21. Measurement results of 1 cmol/mol HCl gas mixtures by an... 62
Table 22. The amounts of HCl adsorbed inner surface of the aluminum... 78
Table 23. Uncertainty budget of 100 μmol/mol HCl standard gas mixture. 94
Table 24. Degree of equivalence for the HCl 100.23 μmol/mol standard gas... 95
Table 25. The uncertainty budget for 100 μmol/mol HCl measured by... 96
Figure 1. The electromagnetic spectrum for FTIR measurement. 19
Figure 2. The schematic diagram of Michelson interferometer. 20
Figure 3. Relationship of the signal outputs from interferometer... 20
Figure 4. The experimental procedure for preparation of certified... 27
Figure 5. Schematic diagram of system configuration for the back flushing... 29
Figure 6. Calibration curve for the inorganic impurity gases.[원문불량;p.17] 29
Figure 7. Chromatogram of standard gases by back flushing method... 30
Figure 8. Filling system for preparation of HCl gas. (a) front side and (b)... 34
Figure 9. Photo of the FTIR spectrometer. 35
Figure 10. Absorbance spectrum of HCl gas mixture. Four... 37
Figure 11. Schematic diagram of semi-continuous gas sampling... 38
Figure 12. Dilution scheme for gravimetric preparation from source gas to... 42
Figure 13. The effect of the integration ranges on the FTIR... 52
Figure 14. Results of the consistency test for the 1 cmol/mol HCl gas... 54
Figure 15. Results of the consistency test for the 1,000 μmol/mol HCl... 56
Figure 16. Results of the consistency test for the 100 μmol/mol HCl... 57
Figure 17. Verification of the concentration of HCl gas mixture with... 59
Figure 18. Temporal variations of Cl- concentrations in liquid measured by...(이미지참조) 60
Figure 19. Relative difference of 1 cmol/mol concentration level by... 61
Figure 20. Results of the measurement of 100 μmol/mol HCl gas... 63
Figure 21. Photo of the cylinder evacuation system for the removal of... 67
Figure 22. Dilution scheme for gravimetric preparation of (a) NO, (b) SO₂... 69
Figure 23. Dilution scheme for gravimetric preparation of HCl gases. 69
Figure 24. Sampling procedure of the IC/ICP analysis for adsorbed gases in... 70
Figure 25. Photos of the introducing with deionized water into evacuated... 71
Figure 26. Photo of the water samples. 72
Figure 27. The amounts adsorbed on the inner surfaces of the NO, NO₂ and... 74
Figure 28. The amounts of HCl adsorbed in the nickel-plated manganese... 76
Figure 29. The amounts of HCl adsorbed inner surface of the aluminum... 77
Figure 30. The adsorption amounts in the cylinder according to... 79
Figure 31. The amounts of leached Ni and Fe in the nickel-plated... 80
Figure 32. Comparison of the amounts of leached Al, Fe and Ni according... 81
Figure 33. Scheme of HCl analysis using purge valve. 84
Figure 34. Photo of the cross section of purge valve. 84
Figure 35. HCl measurement system using FTIR. 85
Figure 36. Photos of cross section of cylinder valves, spindle,... 86
Figure 37. A silconert coated regulator which has slow... 87
Figure 38. Unused Silconert coated Regulator with blue color and the more... 88
Figure 39. The unused nipples which coated with silconert and the used... 89
Figure 40. The photos of outlet of cylinder valve and nipple connector. 89
Figure 41. The photos of outlet of cylinder valve. (a) valves... 90
Figure 42. Comparison of HCl gas mixture for 100 μmol/mol... 92