표제지
목차
Ⅰ. 서론 9
Ⅱ. 이론적 배경 13
Ⅱ-1. 장비 및 이론 13
1) 기체크로마토그래피 13
2) 중량법 19
3) 측정불확도 및 검출 한계 20
Ⅲ. 실험 방법 21
Ⅲ-1. 재료 (시약 및 기구) 21
Ⅲ-2. 중량법을 통한 인증표준물질 제조 24
Ⅲ-3. 물질량 분율 및 제조 불확도 평가 30
Ⅲ-4. 제조된 인증표준물질의 검증과 내부일치성 확인 31
Ⅲ-5. 개발된 순도분석법과 장비 조건 33
Ⅲ-6. 불순물의 물질량 분율 및 불확도 계산 37
Ⅳ. 결과 및 고찰 38
Ⅳ-1. 제조된 인증표준물질의 내부일치성 검증 결과 38
Ⅳ-2. 고순도 질소의 순도분석 결과 43
Ⅴ. 결론 47
Ⅵ. 참고 문헌 49
Abstract 52
국문요약 54
Table 1. List of the type of detectors used in Gas Chromatography 14
Table 2. Analytical conditions of GC-FID 36
Table 3. The amount fractions of gravimetrically prepared 4 bottles of CRM (step 1) 41
Table 4. The amount fractions of gravimetrically prepared 3 bottles of CRM (step 2) 42
Table 5. The amount fractions of CO, CO₂, CH₄, as impurities in the high purity N₂ gases obtained of each method. The numbers in the parentheses are represented the expanded uncertainties in the last digit (k = 2) 46
Figure 1. Reverse peak chromatogram from GC-FID. 11
Figure 2. Thermal conductivity detector with a restrictor on the vent line. 16
Figure 3. Flame ionization detector which is widely used for the analysis of hydrocarbon. 17
Figure 4. Pulsed discharge helium ionization detector which is widely used for the analysis of low-concentration samples. 18
Figure 5. Gas cylinder which used in the preparation for the CRMs. 22
Figure 6. The gas evacuation system which consists of a rotary pump and a turbomolecular pump. 23
Figure 7. Schematic diagram of workflow for the CRM preparation and dilution steps. In each dilution step, the gas mixture was gravimetrically prepared. 25
Figure 8. A blow-off type gas mixture preparation system. 27
Figure 9. Automated weight balance system with a readability of 1 mg. 28
Figure 10. Schematic diagram of the experimental instrument. In method 1, the high purity N₂ and the CRM were used as the sample and ultra-h... 34
Figure 11. The internal consistency of gravimetrically prepared cylinders. 40
Figure 12. The chromatograms of CO, CH₄, and CO₂. The red line represents the chromatogram of CRM obtained using ultra-high purity nitroge... 44