Injector Split vs Splitless 6 pentane hexane heptane

Injector Split vs Splitless

6) 시료: pentane, hexane, heptane, octane, 미지시료(standard 혼합물) pentane 분자량(g/mol) 72. 15 hexane heptane octane 86. 18 100. 20 114. 23 밀도(g/m. L) 0. 626 0. 6548 0. 6795 0. 703 녹는점(°C) − 130. 5 to − 129. 1 °C − 96 to − 94 − 91. 0 to − 90. 1 − 57. 1 to − 56. 6 끓는점(°C) 35. 9 to 36. 3 68. 5 to 69. 1 98. 1 to 98. 7 125. 1 to 126. 1

4. 실험결과 및 분석 § 결과 비교 - Hexane Signals of Different Volumes - Hexane Signals at Different Temperatures - Signals of Pentane, Hexane and Octane at 70℃ § 결과 계산 § 미지시료 분석

Hexane: Signals of Different Volumes 2000000 Detector Response (m. V) 1800000 1600000 1400000 1200000 hexane (0. 5) 1000000 hexane (1. 0) hexane (1. 5) 800000 600000 400000 200000 0 0 20 40 60 80 100 Time (s) 120 140 160 180

Hexane: Signals at Different oven Temperatures 1800000 Detector Response (m. V) 1600000 1400000 1200000 1000000 hexane 50도 hexane 70도 800000 hexane 90도 600000 400000 200000 0 0 50 100 150 Time (s) 200 250 300

Signals of Pentane, Hexane and Octane at 70℃ 1600000 Detector Response (m. V) 1400000 1200000 1000000 Pentane 800000 hexane octane 600000 400000 200000 0 0 50 100 150 200 250 300 Time (s) 350 400 450 500 550

Peak 넓이 구하기 Example. n-Pentane 2000000 Peak h: 1806549 m. V ½ h: 903274. 5 m. V Detector Response (m. V) 1800000 1600000 1400000 1200000 d at ½ h: 67. 4 -57. 6=9. 8 s 1000000 800000 600000 400000 200000 0 0 50 100 시간 (초) 150 Peak 넓이: 1806549 X 9. 8 = 17704184 m. V*s

표준물질의 정량분석 표준물질 Peak Height 1/2 Height (m. V) d Area (m. V*s) (s) Area by Origin Program (m. V*s) Pentane 919657 459828. 5 7. 05 6483582 8552659 Hexane 1352913 676456. 5 7. 33 9916852. 3 10418426 Octane 307471 153735. 5 41. 7 12821541 13135892

Mol 구하기 Example. n-Pentane Molecular Weight: 72. 15 g/mol Density: 0. 626 g/ml Mass: 1㎕ X (10 -3 ml/㎕) X (0. 626 g/ml) = 6. 26 x 10 -4 g Mole: (6. 26 x 10 -4 g) / (72. 15 g/mol) =8. 68 x 10 -6 mol

표준물질의 정량분석 표준물질 M. W. (g/mol) Density (g/ml) Mass (g) Mole (mol) Pentane 72. 15 0. 626 6. 26. E-04 8. 67637 E-06 Hexane 86. 18 0. 659 6. 59. E-04 7. 64679 E-06 Octane 114. 23 0. 703 7. 03. E-04 6. 15425 E-06

Factor 구하기 Factor pentane= 1 Factor hexane =(6483582/9916852. 3) * (7. 65 X 10^-6 / 8. 68 X 10^-6) = 0. 576

Factor 계산 결과 　 Pentane Hexane Octane 　 Pentane Factor (반높이 나비법 사용) 1 0. 576 0. 359 Factor (프로그램 사용) 1 Hexane 0. 724 Octane 0. 462

Detector Response (m. V) 미지시료의 Retention Time 비교 분석 1200000 1000000 800000 600000 400000 200000 0 0 50 100 150 200 250 300 350 400 450 500 550 RT (s) (미지시료) RT (s) (Standard) Pentane 61. 30 69. 95 Hexane 106. 60 109. 5 Octane 420. 68 402

미지시료의 봉우리 넓이 Peak Height (m. V) 1/2 Height (m. V) d (s) Area (m. V*s) Area by Origin Program (m. V*s) Pentane 462056 231028 4. 43 2046908 2218328 Hexane 1017593 508796. 5 6. 84 6960336 7365026 Octane 130525. 8 65262. 9 23. 92 3122177 3369028

보정 넓이 백분율을 사용한 Mole % 구하기 Example. Pentane Peak Area * Factor pentane = 2046908 * 1 = 2046908 Hexane Peak Area * Factor hexane = 6960336 * 0. 576 = 4009154

보정 넓이 백분율을 사용한 Mole % 구하기 Area*Factor (반높이 나비법) Area*Factor (프로그램) Pentane 2046908 2218328 Hexane 4009154 5332279 Octane 1120862 1556491 Total 7176924 9107097

보정 넓이 백분율을 사용한 Mole % 구하기 Example. Pentane의 mole% = 2046908 / 7176924 * 100 = 28. 520687

미지시료 분석 결과 Mol % Ratio (반높이 나비법) Approx. Ratio Pentane 28. 52069 1 1. 8 Hexane 55. 86173 1. 958639 3. 6 Octane 15. 61758 0. 5475878 1 Mol % Ratio (프로그램) Approx. Ratio Pentane 24. 358234 1 1. 4 Hexane 58. 550809 2. 4037379 3. 4 Octane 17. 090957 0. 70165010 1

5. 참고문헌 1. 연세대학교 이과대학 화학과 <분석화학실험> 2. Quantitative Chemical Analysis 8 th Ed. , Freeman, Daniel C. Harris